data_global
_audit_creation_method                  'APEX3 v2017.3-0'

_publ_requested_journal                 ?

_publ_contact_author_name               ?
_publ_contact_author_address            
;
;
_publ_contact_author_email              ?
_publ_contact_author_fax                ?
_publ_contact_author_phone              ?

_publ_section_title                     
;
;
_publ_section_abstract                  
;
;
_publ_section_references                
;
;
_publ_section_comment                   
;
;

data_20200608PbNbOH21
_chemical_name_systematic               ?
_chemical_name_common                   Pb1.34Ca0.06Nb2O6.61
_chemical_formula_moiety                ?
_chemical_formula_sum                   'Ca0.06 Nb2 O6.61 Pb1.34'
_chemical_formula_iupac                 ?
_chemical_formula_weight                572.74

_chemical_melting_point                 ?

_space_group_crystal_system             cubic
_space_group_name_H-M_alt               'F d -3 m'
_space_group_name_Hall                  '-F 4vw 2vw 3'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-x+3/4, -y+1/4, z+1/2'
    '-x+1/4, y+1/2, -z+3/4'
    'x+1/2, -y+3/4, -z+1/4'
    'z, x, y'
    'z+1/2, -x+3/4, -y+1/4'
    '-z+3/4, -x+1/4, y+1/2'
    '-z+1/4, x+1/2, -y+3/4'
    'y, z, x'
    '-y+1/4, z+1/2, -x+3/4'
    'y+1/2, -z+3/4, -x+1/4'
    '-y+3/4, -z+1/4, x+1/2'
    'y+3/4, x+1/4, -z+1/2'
    '-y, -x, -z'
    'y+1/4, -x+1/2, z+3/4'
    '-y+1/2, x+3/4, z+1/4'
    'x+3/4, z+1/4, -y+1/2'
    '-x+1/2, z+3/4, y+1/4'
    '-x, -z, -y'
    'x+1/4, -z+1/2, y+3/4'
    'z+3/4, y+1/4, -x+1/2'
    'z+1/4, -y+1/2, x+3/4'
    '-z+1/2, y+3/4, x+1/4'
    '-z, -y, -x'
    'x, y+1/2, z+1/2'
    '-x+3/4, -y+3/4, z+1'
    '-x+1/4, y+1, -z+5/4'
    'x+1/2, -y+5/4, -z+3/4'
    'z, x+1/2, y+1/2'
    'z+1/2, -x+5/4, -y+3/4'
    '-z+3/4, -x+3/4, y+1'
    '-z+1/4, x+1, -y+5/4'
    'y, z+1/2, x+1/2'
    '-y+1/4, z+1, -x+5/4'
    'y+1/2, -z+5/4, -x+3/4'
    '-y+3/4, -z+3/4, x+1'
    'y+3/4, x+3/4, -z+1'
    '-y, -x+1/2, -z+1/2'
    'y+1/4, -x+1, z+5/4'
    '-y+1/2, x+5/4, z+3/4'
    'x+3/4, z+3/4, -y+1'
    '-x+1/2, z+5/4, y+3/4'
    '-x, -z+1/2, -y+1/2'
    'x+1/4, -z+1, y+5/4'
    'z+3/4, y+3/4, -x+1'
    'z+1/4, -y+1, x+5/4'
    '-z+1/2, y+5/4, x+3/4'
    '-z, -y+1/2, -x+1/2'
    'x+1/2, y, z+1/2'
    '-x+5/4, -y+1/4, z+1'
    '-x+3/4, y+1/2, -z+5/4'
    'x+1, -y+3/4, -z+3/4'
    'z+1/2, x, y+1/2'
    'z+1, -x+3/4, -y+3/4'
    '-z+5/4, -x+1/4, y+1'
    '-z+3/4, x+1/2, -y+5/4'
    'y+1/2, z, x+1/2'
    '-y+3/4, z+1/2, -x+5/4'
    'y+1, -z+3/4, -x+3/4'
    '-y+5/4, -z+1/4, x+1'
    'y+5/4, x+1/4, -z+1'
    '-y+1/2, -x, -z+1/2'
    'y+3/4, -x+1/2, z+5/4'
    '-y+1, x+3/4, z+3/4'
    'x+5/4, z+1/4, -y+1'
    '-x+1, z+3/4, y+3/4'
    '-x+1/2, -z, -y+1/2'
    'x+3/4, -z+1/2, y+5/4'
    'z+5/4, y+1/4, -x+1'
    'z+3/4, -y+1/2, x+5/4'
    '-z+1, y+3/4, x+3/4'
    '-z+1/2, -y, -x+1/2'
    'x+1/2, y+1/2, z'
    '-x+5/4, -y+3/4, z+1/2'
    '-x+3/4, y+1, -z+3/4'
    'x+1, -y+5/4, -z+1/4'
    'z+1/2, x+1/2, y'
    'z+1, -x+5/4, -y+1/4'
    '-z+5/4, -x+3/4, y+1/2'
    '-z+3/4, x+1, -y+3/4'
    'y+1/2, z+1/2, x'
    '-y+3/4, z+1, -x+3/4'
    'y+1, -z+5/4, -x+1/4'
    '-y+5/4, -z+3/4, x+1/2'
    'y+5/4, x+3/4, -z+1/2'
    '-y+1/2, -x+1/2, -z'
    'y+3/4, -x+1, z+3/4'
    '-y+1, x+5/4, z+1/4'
    'x+5/4, z+3/4, -y+1/2'
    '-x+1, z+5/4, y+1/4'
    '-x+1/2, -z+1/2, -y'
    'x+3/4, -z+1, y+3/4'
    'z+5/4, y+3/4, -x+1/2'
    'z+3/4, -y+1, x+3/4'
    '-z+1, y+5/4, x+1/4'
    '-z+1/2, -y+1/2, -x'
    '-x, -y, -z'
    'x-3/4, y-1/4, -z-1/2'
    'x-1/4, -y-1/2, z-3/4'
    '-x-1/2, y-3/4, z-1/4'
    '-z, -x, -y'
    '-z-1/2, x-3/4, y-1/4'
    'z-3/4, x-1/4, -y-1/2'
    'z-1/4, -x-1/2, y-3/4'
    '-y, -z, -x'
    'y-1/4, -z-1/2, x-3/4'
    '-y-1/2, z-3/4, x-1/4'
    'y-3/4, z-1/4, -x-1/2'
    '-y-3/4, -x-1/4, z-1/2'
    'y, x, z'
    '-y-1/4, x-1/2, -z-3/4'
    'y-1/2, -x-3/4, -z-1/4'
    '-x-3/4, -z-1/4, y-1/2'
    'x-1/2, -z-3/4, -y-1/4'
    'x, z, y'
    '-x-1/4, z-1/2, -y-3/4'
    '-z-3/4, -y-1/4, x-1/2'
    '-z-1/4, y-1/2, -x-3/4'
    'z-1/2, -y-3/4, -x-1/4'
    'z, y, x'
    '-x, -y+1/2, -z+1/2'
    'x-3/4, y+1/4, -z'
    'x-1/4, -y, z-1/4'
    '-x-1/2, y-1/4, z+1/4'
    '-z, -x+1/2, -y+1/2'
    '-z-1/2, x-1/4, y+1/4'
    'z-3/4, x+1/4, -y'
    'z-1/4, -x, y-1/4'
    '-y, -z+1/2, -x+1/2'
    'y-1/4, -z, x-1/4'
    '-y-1/2, z-1/4, x+1/4'
    'y-3/4, z+1/4, -x'
    '-y-3/4, -x+1/4, z'
    'y, x+1/2, z+1/2'
    '-y-1/4, x, -z-1/4'
    'y-1/2, -x-1/4, -z+1/4'
    '-x-3/4, -z+1/4, y'
    'x-1/2, -z-1/4, -y+1/4'
    'x, z+1/2, y+1/2'
    '-x-1/4, z, -y-1/4'
    '-z-3/4, -y+1/4, x'
    '-z-1/4, y, -x-1/4'
    'z-1/2, -y-1/4, -x+1/4'
    'z, y+1/2, x+1/2'
    '-x+1/2, -y, -z+1/2'
    'x-1/4, y-1/4, -z'
    'x+1/4, -y-1/2, z-1/4'
    '-x, y-3/4, z+1/4'
    '-z+1/2, -x, -y+1/2'
    '-z, x-3/4, y+1/4'
    'z-1/4, x-1/4, -y'
    'z+1/4, -x-1/2, y-1/4'
    '-y+1/2, -z, -x+1/2'
    'y+1/4, -z-1/2, x-1/4'
    '-y, z-3/4, x+1/4'
    'y-1/4, z-1/4, -x'
    '-y-1/4, -x-1/4, z'
    'y+1/2, x, z+1/2'
    '-y+1/4, x-1/2, -z-1/4'
    'y, -x-3/4, -z+1/4'
    '-x-1/4, -z-1/4, y'
    'x, -z-3/4, -y+1/4'
    'x+1/2, z, y+1/2'
    '-x+1/4, z-1/2, -y-1/4'
    '-z-1/4, -y-1/4, x'
    '-z+1/4, y-1/2, -x-1/4'
    'z, -y-3/4, -x+1/4'
    'z+1/2, y, x+1/2'
    '-x+1/2, -y+1/2, -z'
    'x-1/4, y+1/4, -z-1/2'
    'x+1/4, -y, z-3/4'
    '-x, y-1/4, z-1/4'
    '-z+1/2, -x+1/2, -y'
    '-z, x-1/4, y-1/4'
    'z-1/4, x+1/4, -y-1/2'
    'z+1/4, -x, y-3/4'
    '-y+1/2, -z+1/2, -x'
    'y+1/4, -z, x-3/4'
    '-y, z-1/4, x-1/4'
    'y-1/4, z+1/4, -x-1/2'
    '-y-1/4, -x+1/4, z-1/2'
    'y+1/2, x+1/2, z'
    '-y+1/4, x, -z-3/4'
    'y, -x-1/4, -z-1/4'
    '-x-1/4, -z+1/4, y-1/2'
    'x, -z-1/4, -y-1/4'
    'x+1/2, z+1/2, y'
    '-x+1/4, z, -y-3/4'
    '-z-1/4, -y+1/4, x-1/2'
    '-z+1/4, y, -x-3/4'
    'z, -y-1/4, -x-1/4'
    'z+1/2, y+1/2, x'

_cell_length_a                          10.5456(6)
_cell_length_b                          10.5456(6)
_cell_length_c                          10.5456(6)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            1172.8(2)
_cell_formula_units_Z                   8
_cell_measurement_reflns_used           224
_cell_measurement_theta_min             3.3450
_cell_measurement_theta_max             25.2311
_cell_measurement_temperature           296.(2)

_exptl_crystal_description              octahedron
_exptl_crystal_colour                   'lustrous light yellow'
_exptl_crystal_size_max                 0.112
_exptl_crystal_size_mid                 0.100
_exptl_crystal_size_min                 0.082
_exptl_crystal_density_diffrn           6.474
_exptl_crystal_density_meas             ?
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1967

_exptl_absorpt_coefficient_mu           42.221
_exptl_absorpt_correction_type          Multi-Scan
_exptl_absorpt_process_details          
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min         0.03
_exptl_absorpt_correction_T_max         0.13

_exptl_special_details                  
;
; 

_diffrn_ambient_temperature             296.(2)

_diffrn_source                          'Incoatec Ims 2.0'
_diffrn_source_type                     Microfocus

_diffrn_radiation_type                  MoK\a
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_monochromator         'multi layer optic'

_diffrn_measurement_device_type         'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method              'φ and ω scans'

_diffrn_detector_area_resol_mean        10.4167

_diffrn_reflns_number                   10876
_diffrn_reflns_av_R_equivalents         0.0432
_diffrn_reflns_av_unetI/netI            0.0186
_diffrn_reflns_theta_min                3.35
_diffrn_reflns_theta_max                47.78
_diffrn_reflns_theta_full               47.78
_diffrn_measured_fraction_theta_max     0.993
_diffrn_measured_fraction_theta_full    0.993
_diffrn_reflns_limit_h_min              -21
_diffrn_reflns_limit_h_max              21
_diffrn_reflns_limit_k_min              -21
_diffrn_reflns_limit_k_max              21
_diffrn_reflns_limit_l_min              -21
_diffrn_reflns_limit_l_max              21

_refine_special_details                 
;
;

_reflns_number_total                    303
_reflns_number_gt                       226
_reflns_threshold_expression            'I > 2σ(I)'

_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_R_factor_all                 0.0422
_refine_ls_R_factor_gt                  0.0317
_refine_ls_wR_factor_gt                 0.1234
_refine_ls_wR_factor_ref                0.1349
_refine_ls_goodness_of_fit_ref          1.136
_refine_ls_restrained_S_all             1.136
_refine_ls_number_reflns                303
_refine_ls_number_parameters            10
_refine_ls_number_restraints            0
_refine_ls_number_constraints           ?
_refine_ls_hydrogen_treatment           undef
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details            
    'w=1/[σ²(Fo²)+(0.0609P)²+8.8260P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens          ?
_atom_sites_solution_primary            ?
_atom_sites_solution_secondary          ?

_refine_ls_shift/su_max                 0.000
_refine_ls_shift/su_mean                0.000
_refine_diff_density_max                0.819
_refine_diff_density_min                -1.139
_refine_ls_extinction_method            none
_refine_ls_extinction_coef              ?

loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    H H 0.0000 0.0000 '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'
    Pb Pb -3.3944 10.1111
     'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    Ca Ca 0.2262 0.3064
     'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection              'Bruker Instrument Service vV6.2.6'
_computing_cell_refinement              'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_reduction               'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution           'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement         'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics           'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material         ?

loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags_adp
    _atom_site_refinement_flags_occupancy
    _atom_site_refinement_flags_posn
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Pb Pb 0.25 0.5 0.25 0.0291(2) Uani d T P S 0.67 . .
    Ca Ca 0.25 0.5 0.25 0.0291(2) Uani d T P S 0.03 . .
    O O1 0.375 0.375 0.375 0.06 Uiso d U P S 0.61(3) . .
    O O2 0.4362(3) 0.625 0.125 0.0198(5) Uani d T P S 1.0 . .
    Nb Nb 0.5 0.75 0.25 0.01494(17) Uani d T P S 1.0 . .


_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Pb O1 145_565 2.28319(13) ?
    Pb O1 . 2.28319(13) ?
    Pb O2 . 2.708(2) ?
    Pb O2 102_665 2.708(2) ?
    Pb O2 54_455 2.708(2) ?
    Pb O2 145_565 2.708(2) ?
    Pb O2 129_655 2.708(2) ?
    Pb O2 81_455 2.708(2) ?
    O2 Nb . 1.9819(12) ?
    O2 Nb 76_455 1.9819(12) ?

loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 Pb O1 145_565 . 180.0 ?
    O1 Pb O2 145_565 . 81.75(5) ?
    O1 Pb O2 . . 98.25(5) ?
    O1 Pb O2 145_565 102_665 98.25(5) ?
    O1 Pb O2 . 102_665 81.75(5) ?
    O2 Pb O2 . 102_665 62.02(2) ?
    O1 Pb O2 145_565 54_455 81.75(5) ?
    O1 Pb O2 . 54_455 98.25(5) ?
    O2 Pb O2 . 54_455 117.98(2) ?
    O2 Pb O2 102_665 54_455 180.0 ?
    O1 Pb O2 145_565 145_565 98.25(5) ?
    O1 Pb O2 . 145_565 81.75(5) ?
    O2 Pb O2 . 145_565 180.00(10) ?
    O2 Pb O2 102_665 145_565 117.98(2) ?
    O2 Pb O2 54_455 145_565 62.02(2) ?
    O1 Pb O2 145_565 129_655 98.25(5) ?
    O1 Pb O2 . 129_655 81.75(5) ?
    O2 Pb O2 . 129_655 62.02(2) ?
    O2 Pb O2 102_665 129_655 117.98(2) ?
    O2 Pb O2 54_455 129_655 62.02(2) ?
    O2 Pb O2 145_565 129_655 117.98(2) ?
    O1 Pb O2 145_565 81_455 81.75(5) ?
    O1 Pb O2 . 81_455 98.25(5) ?
    O2 Pb O2 . 81_455 117.98(2) ?
    O2 Pb O2 102_665 81_455 62.02(2) ?
    O2 Pb O2 54_455 81_455 117.98(2) ?
    O2 Pb O2 145_565 81_455 62.02(2) ?
    O2 Pb O2 129_655 81_455 180.0 ?
    Pb O1 Pb 75_545 52_455 109.4710(10) ?
    Pb O1 Pb 75_545 26_554 109.4710(10) ?
    Pb O1 Pb 52_455 26_554 109.5 ?
    Pb O1 Pb 75_545 . 109.4710(10) ?
    Pb O1 Pb 52_455 . 109.5 ?
    Pb O1 Pb 26_554 . 109.5 ?
    Nb O2 Nb . 76_455 140.31(19) ?
    Nb O2 Pb . . 104.25(5) ?
    Nb O2 Pb 76_455 . 104.25(5) ?
    Nb O2 Pb . 76_455 104.25(5) ?
    Nb O2 Pb 76_455 76_455 104.25(5) ?
    Pb O2 Pb . 76_455 87.03(10) ?
    O2 Nb O2 121_665 130_565 90.53(13) ?
    O2 Nb O2 121_665 10_655 89.47(13) ?
    O2 Nb O2 130_565 10_655 180.0 ?
    O2 Nb O2 121_665 102_665 90.53(13) ?
    O2 Nb O2 130_565 102_665 90.53(13) ?
    O2 Nb O2 10_655 102_665 89.47(13) ?
    O2 Nb O2 121_665 30 89.47(13) ?
    O2 Nb O2 130_565 30 89.47(13) ?
    O2 Nb O2 10_655 30 90.53(13) ?
    O2 Nb O2 102_665 30 180.0 ?
    O2 Nb O2 121_665 . 180.0 ?
    O2 Nb O2 130_565 . 89.47(13) ?
    O2 Nb O2 10_655 . 90.53(13) ?
    O2 Nb O2 102_665 . 89.47(13) ?
    O2 Nb O2 30 . 90.53(13) ?
    O2 Nb Ca 121_665 28 44.74(7) ?
    O2 Nb Ca 130_565 28 135.26(7) ?
    O2 Nb Ca 10_655 28 44.74(7) ?
    O2 Nb Ca 102_665 28 90.0 ?
    O2 Nb Ca 30 28 90.0 ?
    O2 Nb Ca . 28 135.26(7) ?
    O2 Nb Ca 121_665 73 44.74(7) ?
    O2 Nb Ca 130_565 73 90.0 ?
    O2 Nb Ca 10_655 73 90.0 ?
    O2 Nb Ca 102_665 73 135.26(7) ?
    O2 Nb Ca 30 73 44.74(7) ?
    O2 Nb Ca . 73 135.26(7) ?
    Ca Nb Ca 28 73 60.0 ?
    O2 Nb Ca 121_665 51_554 90.0 ?
    O2 Nb Ca 130_565 51_554 44.74(7) ?
    O2 Nb Ca 10_655 51_554 135.26(7) ?
    O2 Nb Ca 102_665 51_554 135.26(7) ?
    O2 Nb Ca 30 51_554 44.74(7) ?
    O2 Nb Ca . 51_554 90.0 ?
    Ca Nb Ca 28 51_554 120.0 ?
    Ca Nb Ca 73 51_554 60.0 ?



