 
data_shelx
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H5.02 Ca0.98 Na1.02 O30 Pb10' 
_chemical_formula_weight          2715.77

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.0362   0.0249
 '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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       hexagonal
_space_group_IT_number            194
_space_group_name_H-M_alt         'P 63/m m c'
_space_group_name_Hall            '-P 6c 2c'
 
_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, x, z+1/2'
 '-y, x-y, z'
 '-x, -y, z+1/2'
 '-x+y, -x, z'
 'y, -x+y, z+1/2'
 '-y, -x, -z+1/2'
 'x-y, -y, -z'
 'x, x-y, -z+1/2'
 'y, x, -z'
 '-x+y, y, -z+1/2'
 '-x, -x+y, -z'
 '-x, -y, -z'
 '-x+y, -x, -z-1/2'
 'y, -x+y, -z'
 'x, y, -z-1/2'
 'x-y, x, -z'
 '-y, x-y, -z-1/2'
 'y, x, z-1/2'
 '-x+y, y, z'
 '-x, -x+y, z-1/2'
 '-y, -x, z'
 'x-y, -y, z-1/2'
 'x, x-y, z'
 
_cell_length_a                    5.2533(11)
_cell_length_b                    5.2533(11)
_cell_length_c                    29.425(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      703.3(3)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     6.413          
_exptl_crystal_F_000              1144
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     59.929
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             7062
_diffrn_reflns_av_unetI/netI      0.0317
_diffrn_reflns_av_R_equivalents   0.0535
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        3
_diffrn_reflns_limit_k_min        -3
_diffrn_reflns_limit_k_max        6
_diffrn_reflns_limit_l_min        -38
_diffrn_reflns_limit_l_max        36
_diffrn_reflns_theta_min          4.155
_diffrn_reflns_theta_max          27.992
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.971
_diffrn_measured_fraction_theta_full  0.973
_diffrn_reflns_Laue_measured_fraction_max    0.971
_diffrn_reflns_Laue_measured_fraction_full   0.973
_diffrn_reflns_point_group_measured_fraction_max   0.971
_diffrn_reflns_point_group_measured_fraction_full  0.973
_reflns_number_total              372
_reflns_number_gt                 363
_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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1057P)²+49.6807P] 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      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0009(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          372
_refine_ls_number_parameters      40
_refine_ls_number_restraints      12
_refine_ls_R_factor_all           0.0475
_refine_ls_R_factor_gt            0.0470
_refine_ls_wR_factor_ref          0.1417
_refine_ls_wR_factor_gt           0.1412
_refine_ls_goodness_of_fit_ref    0.990
_refine_ls_restrained_S_all       0.972
_refine_ls_shift/su_max           0.046
_refine_ls_shift/su_mean          0.002
 
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
Pb1 Pb 0.3333 -0.3333 0.09508(4) 0.0182(5) Uani 1 6 d S T P . .
Pb2 Pb 0.0841(4) -0.0841(4) 0.00087(16) 0.0250(13) Uani 0.1667 2 d S T P . .
O1 O 0.386(3) 0.1931(13) 0.0822(4) 0.018(3) Uani 1 2 d S T P . .
OH1 O 0.3333 -0.3333 0.0172(9) 0.032(6) Uani 1 6 d S T P . .
C1 C 0.6667 0.3333 0.0819(12) 0.018(6) Uani 1 6 d S T P . .
Pb3 Pb 0.0000 0.0000 0.17308(4) 0.0186(5) Uani 1 6 d S T P . .
Na Na 0.3333 0.6667 0.2500 0.0269(12) Uani 0.51 12 d S TU P . .
Ca Ca 0.3333 0.6667 0.2500 0.0269(12) Uani 0.4896 12 d S T P . .
OH2 O 0.0000 0.0000 0.2500 0.0574(14) Uani 1 12 d S TU P . .
O2 O 0.5265(13) 0.053(3) 0.1916(5) 0.020(3) Uani 1 2 d S T P . .
C2 C 0.6667 0.3333 0.1888(15) 0.024(7) Uani 1 6 d S T P . .
 
 
_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 OH1 2.29(3) . ?
Pb1 O1 2.665(2) . ?
Pb1 O1 2.665(2) 5 ?
Pb1 O1 2.665(2) 3_545 ?
Pb1 O1 2.665(2) 3_655 ?
Pb1 O1 2.665(2) 1_545 ?
Pb1 O1 2.665(2) 5_655 ?
Pb1 C1 3.058(5) 1_545 ?
Pb1 C1 3.058(5) . ?
Pb1 C1 3.058(5) 1_445 ?
Pb1 Pb2 3.581(5) . ?
Pb1 Pb2 3.581(5) 3_545 ?
Pb2 Pb2 0.767(4) 15 ?
Pb2 Pb2 0.767(4) 17 ?
Pb2 Pb2 1.326(7) 5 ?
Pb2 Pb2 1.326(7) 3 ?
Pb2 Pb2 1.532(8) 13 ?
Pb2 OH1 2.318(7) . ?
Pb2 O1 2.638(14) 15 ?
Pb2 OH1 2.783(6) 13_545 ?
Pb2 OH1 2.783(6) 13_655 ?
Pb2 O1 2.838(13) 5 ?
Pb2 O1 2.838(13) . ?
O1 C1 1.276(12) . ?
O1 Pb2 2.638(14) 17 ?
O1 Pb1 2.665(2) 1_565 ?
O1 Pb2 2.838(13) 3 ?
OH1 Pb2 2.318(7) 3_545 ?
OH1 Pb2 2.318(7) 5_655 ?
OH1 Pb2 2.783(6) 15 ?
OH1 Pb2 2.783(6) 17 ?
OH1 Pb2 2.783(6) 13_545 ?
OH1 Pb2 2.783(6) 13_655 ?
OH1 Pb2 2.783(6) 17_545 ?
OH1 Pb2 2.783(6) 15_655 ?
C1 O1 1.276(12) 3_655 ?
C1 O1 1.276(12) 5_665 ?
C1 Pb1 3.058(5) 1_565 ?
C1 Pb1 3.058(5) 1_665 ?
Pb3 OH2 2.2633(13) . ?
Pb3 O2 2.693(3) 5_665 ?
Pb3 O2 2.693(3) 5 ?
Pb3 O2 2.693(3) 3 ?
Pb3 O2 2.693(3) 3_545 ?
Pb3 O2 2.693(3) 1_455 ?
Pb3 O2 2.693(3) . ?
Pb3 C2 3.068(7) 1_445 ?
Pb3 C2 3.068(7) . ?
Pb3 C2 3.068(7) 1_455 ?
Pb3 Na 3.7844(9) 1_445 ?
Pb3 Ca 3.7844(9) 1_445 ?
Na O2 2.459(12) 16_566 ?
Na O2 2.459(12) 3 ?
Na O2 2.459(12) 18_556 ?
Na O2 2.459(12) 1_565 ?
Na O2 2.459(12) 5_665 ?
Na O2 2.459(12) 14_666 ?
Na Pb3 3.7844(9) 14_566 ?
Na Pb3 3.7844(9) 14_666 ?
Na Pb3 3.7844(9) 1_565 ?
Na Pb3 3.7844(9) 1_665 ?
Na Pb3 3.7844(9) 14_556 ?
OH2 Pb3 2.2633(13) 14_556 ?
OH2 Ca 3.0330(6) 1_445 ?
OH2 Ca 3.0330(6) 1_545 ?
O2 C2 1.278(12) . ?
O2 Ca 2.459(12) 1_545 ?
O2 Na 2.459(12) 1_545 ?
O2 Pb3 2.693(3) 1_655 ?
C2 O2 1.278(12) 3_655 ?
C2 O2 1.278(12) 5_665 ?
C2 Pb3 3.068(7) 1_655 ?
C2 Pb3 3.068(7) 1_665 ?
 
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
OH1 Pb1 O1 81.8(3) . . ?
OH1 Pb1 O1 81.8(3) . 5 ?
O1 Pb1 O1 69.6(5) . 5 ?
OH1 Pb1 O1 81.8(3) . 3_545 ?
O1 Pb1 O1 118.02(13) . 3_545 ?
O1 Pb1 O1 49.0(5) 5 3_545 ?
OH1 Pb1 O1 81.8(3) . 3_655 ?
O1 Pb1 O1 49.0(5) . 3_655 ?
O1 Pb1 O1 118.02(13) 5 3_655 ?
O1 Pb1 O1 160.6(6) 3_545 3_655 ?
OH1 Pb1 O1 81.8(3) . 1_545 ?
O1 Pb1 O1 160.6(6) . 1_545 ?
O1 Pb1 O1 118.02(13) 5 1_545 ?
O1 Pb1 O1 69.6(5) 3_545 1_545 ?
O1 Pb1 O1 118.02(13) 3_655 1_545 ?
OH1 Pb1 O1 81.8(3) . 5_655 ?
O1 Pb1 O1 118.02(13) . 5_655 ?
O1 Pb1 O1 160.6(6) 5 5_655 ?
O1 Pb1 O1 118.02(13) 3_545 5_655 ?
O1 Pb1 O1 69.6(5) 3_655 5_655 ?
O1 Pb1 O1 49.0(5) 1_545 5_655 ?
OH1 Pb1 C1 82.7(7) . 1_545 ?
O1 Pb1 C1 141.6(3) . 1_545 ?
O1 Pb1 C1 141.6(3) 5 1_545 ?
O1 Pb1 C1 94.1(3) 3_545 1_545 ?
O1 Pb1 C1 94.1(3) 3_655 1_545 ?
O1 Pb1 C1 24.6(3) 1_545 1_545 ?
O1 Pb1 C1 24.6(3) 5_655 1_545 ?
OH1 Pb1 C1 82.7(7) . . ?
O1 Pb1 C1 24.6(3) . . ?
O1 Pb1 C1 94.1(3) 5 . ?
O1 Pb1 C1 141.6(3) 3_545 . ?
O1 Pb1 C1 24.6(3) 3_655 . ?
O1 Pb1 C1 141.6(3) 1_545 . ?
O1 Pb1 C1 94.1(3) 5_655 . ?
C1 Pb1 C1 118.4(3) 1_545 . ?
OH1 Pb1 C1 82.7(7) . 1_445 ?
O1 Pb1 C1 94.1(3) . 1_445 ?
O1 Pb1 C1 24.6(3) 5 1_445 ?
O1 Pb1 C1 24.6(3) 3_545 1_445 ?
O1 Pb1 C1 141.6(3) 3_655 1_445 ?
O1 Pb1 C1 94.1(3) 1_545 1_445 ?
O1 Pb1 C1 141.6(3) 5_655 1_445 ?
C1 Pb1 C1 118.4(3) 1_545 1_445 ?
C1 Pb1 C1 118.4(3) . 1_445 ?
OH1 Pb1 Pb2 39.28(7) . . ?
O1 Pb1 Pb2 51.5(3) . . ?
O1 Pb1 Pb2 51.5(3) 5 . ?
O1 Pb1 Pb2 80.4(3) 3_545 . ?
O1 Pb1 Pb2 80.4(3) 3_655 . ?
O1 Pb1 Pb2 117.3(3) 1_545 . ?
O1 Pb1 Pb2 117.3(3) 5_655 . ?
C1 Pb1 Pb2 122.0(7) 1_545 . ?
C1 Pb1 Pb2 65.6(5) . . ?
C1 Pb1 Pb2 65.6(5) 1_445 . ?
OH1 Pb1 Pb2 39.28(7) . 3_545 ?
O1 Pb1 Pb2 117.3(3) . 3_545 ?
O1 Pb1 Pb2 80.4(3) 5 3_545 ?
O1 Pb1 Pb2 51.5(3) 3_545 3_545 ?
O1 Pb1 Pb2 117.3(3) 3_655 3_545 ?
O1 Pb1 Pb2 51.5(3) 1_545 3_545 ?
O1 Pb1 Pb2 80.4(3) 5_655 3_545 ?
C1 Pb1 Pb2 65.6(5) 1_545 3_545 ?
C1 Pb1 Pb2 122.0(7) . 3_545 ?
C1 Pb1 Pb2 65.6(5) 1_445 3_545 ?
Pb2 Pb1 Pb2 66.51(11) . 3_545 ?
Pb2 Pb2 Pb2 119.56(17) 15 17 ?
Pb2 Pb2 Pb2 30.22(9) 15 5 ?
Pb2 Pb2 Pb2 90.000(2) 17 5 ?
Pb2 Pb2 Pb2 90.000(2) 15 3 ?
Pb2 Pb2 Pb2 30.22(9) 17 3 ?
Pb2 Pb2 Pb2 60.0 5 3 ?
Pb2 Pb2 Pb2 59.94(2) 15 13 ?
Pb2 Pb2 Pb2 59.94(2) 17 13 ?
Pb2 Pb2 Pb2 30.06(2) 5 13 ?
Pb2 Pb2 Pb2 30.06(2) 3 13 ?
Pb2 Pb2 OH1 120.13(15) 15 . ?
Pb2 Pb2 OH1 120.13(15) 17 . ?
Pb2 Pb2 OH1 147.9(2) 5 . ?
Pb2 Pb2 OH1 147.9(2) 3 . ?
Pb2 Pb2 OH1 170.0(8) 13 . ?
Pb2 Pb2 O1 97.2(7) 15 15 ?
Pb2 Pb2 O1 97.2(7) 17 15 ?
Pb2 Pb2 O1 109.0(2) 5 15 ?
Pb2 Pb2 O1 109.0(2) 3 15 ?
Pb2 Pb2 O1 110.2(5) 13 15 ?
OH1 Pb2 O1 79.9(7) . 15 ?
Pb2 Pb2 OH1 46.08(16) 15 13_545 ?
Pb2 Pb2 OH1 159.6(7) 17 13_545 ?
Pb2 Pb2 OH1 76.22(8) 5 13_545 ?
Pb2 Pb2 OH1 134.88(14) 3 13_545 ?
Pb2 Pb2 OH1 105.27(12) 13 13_545 ?
OH1 Pb2 OH1 77.0(3) . 13_545 ?
O1 Pb2 OH1 73.9(5) 15 13_545 ?
Pb2 Pb2 OH1 159.6(7) 15 13_655 ?
Pb2 Pb2 OH1 46.08(16) 17 13_655 ?
Pb2 Pb2 OH1 134.88(14) 5 13_655 ?
Pb2 Pb2 OH1 76.22(8) 3 13_655 ?
Pb2 Pb2 OH1 105.27(12) 13 13_655 ?
OH1 Pb2 OH1 77.0(3) . 13_655 ?
O1 Pb2 OH1 73.9(5) 15 13_655 ?
OH1 Pb2 OH1 141.4(6) 13_545 13_655 ?
Pb2 Pb2 O1 67.2(7) 15 5 ?
Pb2 Pb2 O1 122.6(8) 17 5 ?
Pb2 Pb2 O1 76.49(9) 5 5 ?
Pb2 Pb2 O1 107.6(2) 3 5 ?
Pb2 Pb2 O1 93.9(3) 13 5 ?
OH1 Pb2 O1 77.7(6) . 5 ?
O1 Pb2 O1 140.0(4) 15 5 ?
OH1 Pb2 O1 69.2(6) 13_545 5 ?
OH1 Pb2 O1 131.0(6) 13_655 5 ?
Pb2 Pb2 O1 122.6(8) 15 . ?
Pb2 Pb2 O1 67.2(7) 17 . ?
Pb2 Pb2 O1 107.6(2) 5 . ?
Pb2 Pb2 O1 76.49(9) 3 . ?
Pb2 Pb2 O1 93.9(3) 13 . ?
OH1 Pb2 O1 77.7(6) . . ?
O1 Pb2 O1 140.0(4) 15 . ?
OH1 Pb2 O1 131.0(6) 13_545 . ?
OH1 Pb2 O1 69.2(6) 13_655 . ?
O1 Pb2 O1 64.8(5) 5 . ?
Pb2 Pb2 Pb1 111.6(6) 15 . ?
Pb2 Pb2 Pb1 111.6(6) 17 . ?
Pb2 Pb2 Pb1 123.25(6) 5 . ?
Pb2 Pb2 Pb1 123.25(6) 3 . ?
Pb2 Pb2 Pb1 131.2(4) 13 . ?
OH1 Pb2 Pb1 38.8(7) . . ?
O1 Pb2 Pb1 118.6(3) 15 . ?
OH1 Pb2 Pb1 88.7(5) 13_545 . ?
OH1 Pb2 Pb1 88.7(5) 13_655 . ?
O1 Pb2 Pb1 47.32(10) 5 . ?
O1 Pb2 Pb1 47.32(10) . . ?
C1 O1 Pb2 111.6(18) . 17 ?
C1 O1 Pb1 95.2(3) . 1_565 ?
Pb2 O1 Pb1 95.6(3) 17 1_565 ?
C1 O1 Pb1 95.2(3) . . ?
Pb2 O1 Pb1 95.6(3) 17 . ?
Pb1 O1 Pb1 160.6(6) 1_565 . ?
C1 O1 Pb2 118.5(18) . . ?
Pb2 O1 Pb2 15.55(12) 17 . ?
Pb1 O1 Pb2 107.8(3) 1_565 . ?
Pb1 O1 Pb2 81.1(2) . . ?
C1 O1 Pb2 118.5(18) . 3 ?
Pb2 O1 Pb2 15.55(12) 17 3 ?
Pb1 O1 Pb2 81.1(2) 1_565 3 ?
Pb1 O1 Pb2 107.8(3) . 3 ?
Pb2 O1 Pb2 27.01(19) . 3 ?
Pb1 OH1 Pb2 101.9(7) . . ?
Pb1 OH1 Pb2 101.9(7) . 3_545 ?
Pb2 OH1 Pb2 115.8(5) . 3_545 ?
Pb1 OH1 Pb2 101.9(7) . 5_655 ?
Pb2 OH1 Pb2 115.8(5) . 5_655 ?
Pb2 OH1 Pb2 115.8(5) 3_545 5_655 ?
Pb1 OH1 Pb2 101.0(6) . 15 ?
Pb2 OH1 Pb2 13.79(8) . 15 ?
Pb2 OH1 Pb2 103.0(3) 3_545 15 ?
Pb2 OH1 Pb2 128.9(5) 5_655 15 ?
Pb1 OH1 Pb2 101.0(6) . 17 ?
Pb2 OH1 Pb2 13.79(8) . 17 ?
Pb2 OH1 Pb2 128.9(5) 3_545 17 ?
Pb2 OH1 Pb2 103.0(3) 5_655 17 ?
Pb2 OH1 Pb2 27.56(16) 15 17 ?
Pb1 OH1 Pb2 101.0(6) . 13_545 ?
Pb2 OH1 Pb2 103.0(3) . 13_545 ?
Pb2 OH1 Pb2 13.79(8) 3_545 13_545 ?
Pb2 OH1 Pb2 128.9(5) 5_655 13_545 ?
Pb2 OH1 Pb2 89.8(3) 15 13_545 ?
Pb2 OH1 Pb2 116.5(4) 17 13_545 ?
Pb1 OH1 Pb2 101.0(6) . 13_655 ?
Pb2 OH1 Pb2 103.0(3) . 13_655 ?
Pb2 OH1 Pb2 128.9(5) 3_545 13_655 ?
Pb2 OH1 Pb2 13.79(8) 5_655 13_655 ?
Pb2 OH1 Pb2 116.5(4) 15 13_655 ?
Pb2 OH1 Pb2 89.8(3) 17 13_655 ?
Pb2 OH1 Pb2 141.4(6) 13_545 13_655 ?
Pb1 OH1 Pb2 101.0(6) . 17_545 ?
Pb2 OH1 Pb2 128.9(5) . 17_545 ?
Pb2 OH1 Pb2 13.79(8) 3_545 17_545 ?
Pb2 OH1 Pb2 103.0(3) 5_655 17_545 ?
Pb2 OH1 Pb2 116.5(4) 15 17_545 ?
Pb2 OH1 Pb2 141.4(6) 17 17_545 ?
Pb2 OH1 Pb2 27.56(16) 13_545 17_545 ?
Pb2 OH1 Pb2 116.5(4) 13_655 17_545 ?
Pb1 OH1 Pb2 101.0(6) . 15_655 ?
Pb2 OH1 Pb2 128.9(5) . 15_655 ?
Pb2 OH1 Pb2 103.0(3) 3_545 15_655 ?
Pb2 OH1 Pb2 13.79(8) 5_655 15_655 ?
Pb2 OH1 Pb2 141.4(6) 15 15_655 ?
Pb2 OH1 Pb2 116.5(4) 17 15_655 ?
Pb2 OH1 Pb2 116.5(4) 13_545 15_655 ?
Pb2 OH1 Pb2 27.56(16) 13_655 15_655 ?
Pb2 OH1 Pb2 89.8(3) 17_545 15_655 ?
O1 C1 O1 119.99(6) 3_655 5_665 ?
O1 C1 O1 119.99(6) 3_655 . ?
O1 C1 O1 119.99(6) 5_665 . ?
O1 C1 Pb1 172(2) 3_655 1_565 ?
O1 C1 Pb1 60.2(2) 5_665 1_565 ?
O1 C1 Pb1 60.2(2) . 1_565 ?
O1 C1 Pb1 60.2(2) 3_655 . ?
O1 C1 Pb1 172(2) 5_665 . ?
O1 C1 Pb1 60.2(2) . . ?
Pb1 C1 Pb1 118.4(3) 1_565 . ?
O1 C1 Pb1 60.2(2) 3_655 1_665 ?
O1 C1 Pb1 60.2(2) 5_665 1_665 ?
O1 C1 Pb1 172(2) . 1_665 ?
Pb1 C1 Pb1 118.4(3) 1_565 1_665 ?
Pb1 C1 Pb1 118.4(3) . 1_665 ?
OH2 Pb3 O2 78.4(3) . 5_665 ?
OH2 Pb3 O2 78.4(3) . 5 ?
O2 Pb3 O2 154.5(6) 5_665 5 ?
OH2 Pb3 O2 78.4(3) . 3 ?
O2 Pb3 O2 68.8(5) 5_665 3 ?
O2 Pb3 O2 116.04(18) 5 3 ?
OH2 Pb3 O2 78.4(3) . 3_545 ?
O2 Pb3 O2 116.04(18) 5_665 3_545 ?
O2 Pb3 O2 48.4(5) 5 3_545 ?
O2 Pb3 O2 154.5(6) 3 3_545 ?
OH2 Pb3 O2 78.4(3) . 1_455 ?
O2 Pb3 O2 116.04(18) 5_665 1_455 ?
O2 Pb3 O2 68.8(5) 5 1_455 ?
O2 Pb3 O2 48.4(5) 3 1_455 ?
O2 Pb3 O2 116.04(18) 3_545 1_455 ?
OH2 Pb3 O2 78.4(3) . . ?
O2 Pb3 O2 48.4(5) 5_665 . ?
O2 Pb3 O2 116.04(18) 5 . ?
O2 Pb3 O2 116.04(18) 3 . ?
O2 Pb3 O2 68.8(5) 3_545 . ?
O2 Pb3 O2 154.5(6) 1_455 . ?
OH2 Pb3 C2 81.3(8) . 1_445 ?
O2 Pb3 C2 139.5(5) 5_665 1_445 ?
O2 Pb3 C2 24.5(3) 5 1_445 ?
O2 Pb3 C2 139.5(5) 3 1_445 ?
O2 Pb3 C2 24.5(3) 3_545 1_445 ?
O2 Pb3 C2 93.3(3) 1_455 1_445 ?
O2 Pb3 C2 93.3(3) . 1_445 ?
OH2 Pb3 C2 81.3(8) . . ?
O2 Pb3 C2 24.5(3) 5_665 . ?
O2 Pb3 C2 139.5(5) 5 . ?
O2 Pb3 C2 93.3(3) 3 . ?
O2 Pb3 C2 93.3(3) 3_545 . ?
O2 Pb3 C2 139.5(5) 1_455 . ?
O2 Pb3 C2 24.5(3) . . ?
C2 Pb3 C2 117.8(4) 1_445 . ?
OH2 Pb3 C2 81.3(8) . 1_455 ?
O2 Pb3 C2 93.3(3) 5_665 1_455 ?
O2 Pb3 C2 93.3(3) 5 1_455 ?
O2 Pb3 C2 24.5(3) 3 1_455 ?
O2 Pb3 C2 139.5(5) 3_545 1_455 ?
O2 Pb3 C2 24.5(3) 1_455 1_455 ?
O2 Pb3 C2 139.5(5) . 1_455 ?
C2 Pb3 C2 117.8(4) 1_445 1_455 ?
C2 Pb3 C2 117.8(4) . 1_455 ?
OH2 Pb3 Na 53.269(16) . 1_445 ?
O2 Pb3 Na 126.3(3) 5_665 1_445 ?
O2 Pb3 Na 40.4(3) 5 1_445 ?
O2 Pb3 Na 78.9(3) 3 1_445 ?
O2 Pb3 Na 78.9(3) 3_545 1_445 ?
O2 Pb3 Na 40.4(3) 1_455 1_445 ?
O2 Pb3 Na 126.3(3) . 1_445 ?
C2 Pb3 Na 60.9(5) 1_445 1_445 ?
C2 Pb3 Na 134.6(8) . 1_445 ?
C2 Pb3 Na 60.9(5) 1_455 1_445 ?
OH2 Pb3 Ca 53.269(16) . 1_445 ?
O2 Pb3 Ca 126.3(3) 5_665 1_445 ?
O2 Pb3 Ca 40.4(3) 5 1_445 ?
O2 Pb3 Ca 78.9(3) 3 1_445 ?
O2 Pb3 Ca 78.9(3) 3_545 1_445 ?
O2 Pb3 Ca 40.4(3) 1_455 1_445 ?
O2 Pb3 Ca 126.3(3) . 1_445 ?
C2 Pb3 Ca 60.9(5) 1_445 1_445 ?
C2 Pb3 Ca 134.6(8) . 1_445 ?
C2 Pb3 Ca 60.9(5) 1_455 1_445 ?
Na Pb3 Ca 0.0 1_445 1_445 ?
O2 Na O2 138.1(2) 16_566 3 ?
O2 Na O2 76.5(5) 16_566 18_556 ?
O2 Na O2 88.8(6) 3 18_556 ?
O2 Na O2 88.8(6) 16_566 1_565 ?
O2 Na O2 76.5(5) 3 1_565 ?
O2 Na O2 138.1(2) 18_556 1_565 ?
O2 Na O2 138.1(2) 16_566 5_665 ?
O2 Na O2 76.5(5) 3 5_665 ?
O2 Na O2 138.1(2) 18_556 5_665 ?
O2 Na O2 76.5(5) 1_565 5_665 ?
O2 Na O2 76.5(5) 16_566 14_666 ?
O2 Na O2 138.1(2) 3 14_666 ?
O2 Na O2 76.5(5) 18_556 14_666 ?
O2 Na O2 138.1(2) 1_565 14_666 ?
O2 Na O2 88.8(6) 5_665 14_666 ?
O2 Na Pb3 172.3(3) 16_566 . ?
O2 Na Pb3 45.19(6) 3 . ?
O2 Na Pb3 97.6(2) 18_556 . ?
O2 Na Pb3 98.9(3) 1_565 . ?
O2 Na Pb3 45.19(6) 5_665 . ?
O2 Na Pb3 97.6(2) 14_666 . ?
O2 Na Pb3 45.19(6) 16_566 14_566 ?
O2 Na Pb3 97.6(2) 3 14_566 ?
O2 Na Pb3 45.19(6) 18_556 14_566 ?
O2 Na Pb3 97.6(2) 1_565 14_566 ?
O2 Na Pb3 172.3(3) 5_665 14_566 ?
O2 Na Pb3 98.9(3) 14_666 14_566 ?
Pb3 Na Pb3 132.753(11) . 14_566 ?
O2 Na Pb3 45.19(6) 16_566 14_666 ?
O2 Na Pb3 172.3(3) 3 14_666 ?
O2 Na Pb3 98.9(3) 18_556 14_666 ?
O2 Na Pb3 97.6(2) 1_565 14_666 ?
O2 Na Pb3 97.6(2) 5_665 14_666 ?
O2 Na Pb3 45.19(6) 14_666 14_666 ?
Pb3 Na Pb3 132.753(11) . 14_666 ?
Pb3 Na Pb3 87.91(2) 14_566 14_666 ?
O2 Na Pb3 97.6(2) 16_566 1_565 ?
O2 Na Pb3 45.19(6) 3 1_565 ?
O2 Na Pb3 97.6(2) 18_556 1_565 ?
O2 Na Pb3 45.19(6) 1_565 1_565 ?
O2 Na Pb3 98.9(3) 5_665 1_565 ?
O2 Na Pb3 172.3(3) 14_666 1_565 ?
Pb3 Na Pb3 87.91(2) . 1_565 ?
Pb3 Na Pb3 73.46(3) 14_566 1_565 ?
Pb3 Na Pb3 132.753(11) 14_666 1_565 ?
O2 Na Pb3 97.6(2) 16_566 1_665 ?
O2 Na Pb3 98.9(3) 3 1_665 ?
O2 Na Pb3 172.3(3) 18_556 1_665 ?
O2 Na Pb3 45.19(6) 1_565 1_665 ?
O2 Na Pb3 45.19(6) 5_665 1_665 ?
O2 Na Pb3 97.6(2) 14_666 1_665 ?
Pb3 Na Pb3 87.91(2) . 1_665 ?
Pb3 Na Pb3 132.753(11) 14_566 1_665 ?
Pb3 Na Pb3 73.46(3) 14_666 1_665 ?
Pb3 Na Pb3 87.91(2) 1_565 1_665 ?
O2 Na Pb3 98.9(3) 16_566 14_556 ?
O2 Na Pb3 97.6(2) 3 14_556 ?
O2 Na Pb3 45.19(6) 18_556 14_556 ?
O2 Na Pb3 172.3(3) 1_565 14_556 ?
O2 Na Pb3 97.6(2) 5_665 14_556 ?
O2 Na Pb3 45.19(6) 14_666 14_556 ?
Pb3 Na Pb3 73.46(3) . 14_556 ?
Pb3 Na Pb3 87.91(2) 14_566 14_556 ?
Pb3 Na Pb3 87.91(2) 14_666 14_556 ?
Pb3 Na Pb3 132.753(11) 1_565 14_556 ?
Pb3 Na Pb3 132.753(11) 1_665 14_556 ?
Pb3 OH2 Pb3 180.0 . 14_556 ?
Pb3 OH2 Ca 90.0 . 1_445 ?
Pb3 OH2 Ca 90.0 14_556 1_445 ?
Pb3 OH2 Ca 90.0 . 1_545 ?
Pb3 OH2 Ca 90.0 14_556 1_545 ?
Ca OH2 Ca 120.0 1_445 1_545 ?
C2 O2 Ca 139(2) . 1_545 ?
C2 O2 Na 139(2) . 1_545 ?
Ca O2 Na 0.0 1_545 1_545 ?
C2 O2 Pb3 94.4(5) . . ?
Ca O2 Pb3 94.4(3) 1_545 . ?
Na O2 Pb3 94.4(3) 1_545 . ?
C2 O2 Pb3 94.4(5) . 1_655 ?
Ca O2 Pb3 94.4(3) 1_545 1_655 ?
Na O2 Pb3 94.4(3) 1_545 1_655 ?
Pb3 O2 Pb3 154.5(6) . 1_655 ?
O2 C2 O2 119.6(5) 3_655 . ?
O2 C2 O2 119.6(5) 3_655 5_665 ?
O2 C2 O2 119.6(5) . 5_665 ?
O2 C2 Pb3 175(3) 3_655 . ?
O2 C2 Pb3 61.1(3) . . ?
O2 C2 Pb3 61.1(3) 5_665 . ?
O2 C2 Pb3 61.1(3) 3_655 1_655 ?
O2 C2 Pb3 61.1(3) . 1_655 ?
O2 C2 Pb3 175(3) 5_665 1_655 ?
Pb3 C2 Pb3 117.8(4) . 1_655 ?
O2 C2 Pb3 61.1(3) 3_655 1_665 ?
O2 C2 Pb3 175(3) . 1_665 ?
O2 C2 Pb3 61.1(3) 5_665 1_665 ?
Pb3 C2 Pb3 117.8(4) . 1_665 ?
Pb3 C2 Pb3 117.8(4) 1_655 1_665 ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
Pb2 O1 C1 O1 -91(3) 17 . . 3_655 ?
Pb1 O1 C1 O1 171(3) 1_565 . . 3_655 ?
Pb1 O1 C1 O1 7(3) . . . 3_655 ?
Pb2 O1 C1 O1 -75(3) . . . 3_655 ?
Pb2 O1 C1 O1 -106(3) 3 . . 3_655 ?
Pb2 O1 C1 O1 91(3) 17 . . 5_665 ?
Pb1 O1 C1 O1 -7(3) 1_565 . . 5_665 ?
Pb1 O1 C1 O1 -171(3) . . . 5_665 ?
Pb2 O1 C1 O1 106(3) . . . 5_665 ?
Pb2 O1 C1 O1 75(3) 3 . . 5_665 ?
Pb2 O1 C1 Pb1 98.2(4) 17 . . 1_565 ?
Pb1 O1 C1 Pb1 -163.7(8) . . . 1_565 ?
Pb2 O1 C1 Pb1 113.6(7) . . . 1_565 ?
Pb2 O1 C1 Pb1 82.7(2) 3 . . 1_565 ?
Pb2 O1 C1 Pb1 -98.2(4) 17 . . . ?
Pb1 O1 C1 Pb1 163.7(8) 1_565 . . . ?
Pb2 O1 C1 Pb1 -82.7(2) . . . . ?
Pb2 O1 C1 Pb1 -113.6(7) 3 . . . ?
Ca O2 C2 O2 84(4) 1_545 . . 3_655 ?
Na O2 C2 O2 84(4) 1_545 . . 3_655 ?
Pb3 O2 C2 O2 -174(3) . . . 3_655 ?
Pb3 O2 C2 O2 -18(4) 1_655 . . 3_655 ?
Ca O2 C2 O2 -84(4) 1_545 . . 5_665 ?
Na O2 C2 O2 -84(4) 1_545 . . 5_665 ?
Pb3 O2 C2 O2 18(4) . . . 5_665 ?
Pb3 O2 C2 O2 174(3) 1_655 . . 5_665 ?
Ca O2 C2 Pb3 -102.0(4) 1_545 . . . ?
Na O2 C2 Pb3 -102.0(4) 1_545 . . . ?
Pb3 O2 C2 Pb3 156.0(7) 1_655 . . . ?
Ca O2 C2 Pb3 102.0(4) 1_545 . . 1_655 ?
Na O2 C2 Pb3 102.0(4) 1_545 . . 1_655 ?
Pb3 O2 C2 Pb3 -156.0(7) . . . 1_655 ?
 
_refine_diff_density_max    4.758
_refine_diff_density_min   -2.777
_refine_diff_density_rms    0.638



