 
data_compound1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B N O10 Pb6' 
_chemical_formula_weight          1427.96 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 
_symmetry_cell_setting             'Orthorhombic' 
_symmetry_space_group_name_H-M     'Pmmn' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y+1/2, z' 
 'x+1/2, -y, -z' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y-1/2, -z' 
 '-x-1/2, y, z' 
 'x, -y-1/2, z' 
 
_cell_length_a                    5.7534(3) 
_cell_length_b                    9.4518(5) 
_cell_length_c                    11.2735(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      613.05(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description       'Needle' 
_exptl_crystal_colour             'Colorless'
_exptl_crystal_size_max           0.1000
_exptl_crystal_size_mid           0.0600
_exptl_crystal_size_min           0.0500
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     7.735 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1168 
_exptl_absorpt_coefficient_mu     82.130 
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_min   0.08161
_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          'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator   'mirror' 
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <1.0% 
_diffrn_reflns_number             1670 
_diffrn_reflns_av_R_equivalents   0.1130 
_diffrn_reflns_av_sigmaI/netI     0.0820 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        5 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.81 
_diffrn_reflns_theta_max          24.99 
_reflns_number_total              633 
_reflns_number_gt                 562 
_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)+(0.0141P)²+0.0000P] 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        0.00197(16) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          633 
_refine_ls_number_parameters      59 
_refine_ls_number_restraints      18 
_refine_ls_R_factor_all           0.0511 
_refine_ls_R_factor_gt            0.0409 
_refine_ls_wR_factor_ref          0.0817 
_refine_ls_wR_factor_gt           0.0778 
_refine_ls_goodness_of_fit_ref    1.086 
_refine_ls_restrained_S_all       1.070 
_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 -0.2500 -0.05578(8) 0.32052(10) 0.0164(4) Uani 1 2 d S . . 
Pb2 Pb -0.2500 0.2500 0.14327(14) 0.0153(4) Uani 1 4 d S . . 
Pb3 Pb 0.2500 0.01261(9) 0.11943(9) 0.0167(3) Uani 1 2 d S . . 
Pb4 Pb 0.2500 0.2500 0.36558(14) 0.0163(4) Uani 1 4 d S . . 
B1 B 0.2500 0.2500 -0.072(4) 0.007(7) Uani 1 4 d SU . . 
N1 N 0.2500 0.7500 0.412(4) 0.034(8) Uani 1 4 d SU . . 
O1 O 0.2500 0.2500 0.049(2) 0.015(5) Uani 1 4 d S . . 
O2 O 0.2500 0.1210(19) -0.1293(19) 0.037(5) Uani 1 2 d S . . 
O3 O 0.2500 0.7500 0.299(4) 0.051(10) Uani 1 4 d S . . 
O4 O 0.2500 0.640(2) 0.464(2) 0.063(7) Uani 1 2 d S . . 
O5 O 0.0033(16) 0.1054(10) 0.2514(10) 0.016(3) Uani 1 1 d U . . 
 
 
_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 2.24(2) 5 ? 
Pb1 O5 2.248(10) . ? 
Pb1 O5 2.248(10) 7 ? 
Pb1 Pb2 3.5137(13) . ? 
Pb1 Pb1 3.6715(16) 2_445 ? 
Pb2 O5 2.340(10) 8_565 ? 
Pb2 O5 2.340(10) . ? 
Pb2 O5 2.340(10) 7 ? 
Pb2 O5 2.340(10) 2_455 ? 
Pb2 Pb1 3.5137(13) 2_455 ? 
Pb2 Pb3 3.6582(6) 1_455 ? 
Pb2 Pb3 3.6582(6) 2 ? 
Pb2 Pb3 3.6582(6) 2_455 ? 
Pb2 Pb3 3.6582(6) . ? 
Pb3 O5 2.235(10) 7_655 ? 
Pb3 O5 2.235(10) . ? 
Pb3 O1 2.379(9) . ? 
Pb3 Pb4 3.5686(15) . ? 
Pb3 Pb2 3.6582(6) 1_655 ? 
Pb4 O5 2.353(10) . ? 
Pb4 O5 2.353(10) 8_565 ? 
Pb4 O5 2.353(10) 2 ? 
Pb4 O5 2.353(10) 7_655 ? 
Pb4 Pb3 3.5686(15) 2 ? 
B1 O2 1.38(3) . ? 
B1 O2 1.38(3) 2 ? 
B1 O1 1.36(5) . ? 
N1 O4 1.19(3) . ? 
N1 O4 1.19(3) 2_565 ? 
N1 O3 1.27(5) . ? 
O1 Pb3 2.379(9) 2 ? 
O2 Pb1 2.24(2) 5 ? 
 
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 81.6(5) 5 . ? 
O2 Pb1 O5 81.6(5) 5 7 ? 
O5 Pb1 O5 80.8(5) . 7 ? 
O2 Pb1 Pb2 71.3(5) 5 . ? 
O5 Pb1 Pb2 41.0(2) . . ? 
O5 Pb1 Pb2 41.0(2) 7 . ? 
O2 Pb1 Pb1 74.0(5) 5 2_445 ? 
O5 Pb1 Pb1 132.7(2) . 2_445 ? 
O5 Pb1 Pb1 132.7(2) 7 2_445 ? 
Pb2 Pb1 Pb1 145.34(3) . 2_445 ? 
O5 Pb2 O5 71.4(5) 8_565 . ? 
O5 Pb2 O5 117.2(5) 8_565 7 ? 
O5 Pb2 O5 77.0(5) . 7 ? 
O5 Pb2 O5 77.0(5) 8_565 2_455 ? 
O5 Pb2 O5 117.2(5) . 2_455 ? 
O5 Pb2 O5 71.4(5) 7 2_455 ? 
O5 Pb2 Pb1 39.1(2) 8_565 2_455 ? 
O5 Pb2 Pb1 100.6(3) . 2_455 ? 
O5 Pb2 Pb1 100.6(3) 7 2_455 ? 
O5 Pb2 Pb1 39.1(2) 2_455 2_455 ? 
O5 Pb2 Pb1 100.6(3) 8_565 . ? 
O5 Pb2 Pb1 39.1(2) . . ? 
O5 Pb2 Pb1 39.1(2) 7 . ? 
O5 Pb2 Pb1 100.6(3) 2_455 . ? 
Pb1 Pb2 Pb1 110.68(5) 2_455 . ? 
O5 Pb2 Pb3 152.4(3) 8_565 1_455 ? 
O5 Pb2 Pb3 99.8(2) . 1_455 ? 
O5 Pb2 Pb3 35.9(3) 7 1_455 ? 
O5 Pb2 Pb3 84.6(2) 2_455 1_455 ? 
Pb1 Pb2 Pb3 123.11(3) 2_455 1_455 ? 
Pb1 Pb2 Pb3 62.436(18) . 1_455 ? 
O5 Pb2 Pb3 35.9(3) 8_565 2 ? 
O5 Pb2 Pb3 84.6(2) . 2 ? 
O5 Pb2 Pb3 152.4(3) 7 2 ? 
O5 Pb2 Pb3 99.8(2) 2_455 2 ? 
Pb1 Pb2 Pb3 62.436(18) 2_455 2 ? 
Pb1 Pb2 Pb3 123.11(3) . 2 ? 
Pb3 Pb2 Pb3 171.57(6) 1_455 2 ? 
O5 Pb2 Pb3 99.8(2) 8_565 2_455 ? 
O5 Pb2 Pb3 152.4(3) . 2_455 ? 
O5 Pb2 Pb3 84.6(2) 7 2_455 ? 
O5 Pb2 Pb3 35.9(3) 2_455 2_455 ? 
Pb1 Pb2 Pb3 62.436(18) 2_455 2_455 ? 
Pb1 Pb2 Pb3 123.11(3) . 2_455 ? 
Pb3 Pb2 Pb3 75.67(2) 1_455 2_455 ? 
Pb3 Pb2 Pb3 103.70(2) 2 2_455 ? 
O5 Pb2 Pb3 84.6(2) 8_565 . ? 
O5 Pb2 Pb3 35.9(3) . . ? 
O5 Pb2 Pb3 99.8(2) 7 . ? 
O5 Pb2 Pb3 152.4(3) 2_455 . ? 
Pb1 Pb2 Pb3 123.11(3) 2_455 . ? 
Pb1 Pb2 Pb3 62.436(18) . . ? 
Pb3 Pb2 Pb3 103.70(2) 1_455 . ? 
Pb3 Pb2 Pb3 75.67(2) 2 . ? 
Pb3 Pb2 Pb3 171.57(6) 2_455 . ? 
O5 Pb3 O5 78.8(5) 7_655 . ? 
O5 Pb3 O1 81.4(5) 7_655 . ? 
O5 Pb3 O1 81.4(5) . . ? 
O5 Pb3 Pb4 40.2(2) 7_655 . ? 
O5 Pb3 Pb4 40.2(2) . . ? 
O1 Pb3 Pb4 70.4(6) . . ? 
O5 Pb3 Pb2 37.9(3) 7_655 1_655 ? 
O5 Pb3 Pb2 102.1(2) . 1_655 ? 
O1 Pb3 Pb2 56.3(2) . 1_655 ? 
Pb4 Pb3 Pb2 63.72(3) . 1_655 ? 
O5 Pb3 Pb2 102.1(2) 7_655 . ? 
O5 Pb3 Pb2 37.9(3) . . ? 
O1 Pb3 Pb2 56.3(2) . . ? 
Pb4 Pb3 Pb2 63.72(3) . . ? 
Pb2 Pb3 Pb2 103.70(2) 1_655 . ? 
O5 Pb4 O5 71.0(5) . 8_565 ? 
O5 Pb4 O5 113.7(5) . 2 ? 
O5 Pb4 O5 74.2(5) 8_565 2 ? 
O5 Pb4 O5 74.2(5) . 7_655 ? 
O5 Pb4 O5 113.7(5) 8_565 7_655 ? 
O5 Pb4 O5 71.0(5) 2 7_655 ? 
O5 Pb4 Pb3 37.8(2) . . ? 
O5 Pb4 Pb3 86.5(3) 8_565 . ? 
O5 Pb4 Pb3 86.5(3) 2 . ? 
O5 Pb4 Pb3 37.8(2) 7_655 . ? 
O5 Pb4 Pb3 86.5(3) . 2 ? 
O5 Pb4 Pb3 37.8(2) 8_565 2 ? 
O5 Pb4 Pb3 37.8(2) 2 2 ? 
O5 Pb4 Pb3 86.5(3) 7_655 2 ? 
Pb3 Pb4 Pb3 77.92(5) . 2 ? 
O2 B1 O2 124(4) . 2 ? 
O2 B1 O1 118.1(18) . . ? 
O2 B1 O1 118.1(18) 2 . ? 
O4 N1 O4 122(5) . 2_565 ? 
O4 N1 O3 119(3) . . ? 
O4 N1 O3 119(3) 2_565 . ? 
B1 O1 Pb3 109.4(6) . 2 ? 
B1 O1 Pb3 109.4(6) . . ? 
Pb3 O1 Pb3 141.2(12) 2 . ? 
B1 O2 Pb1 134(2) . 5 ? 
Pb3 O5 Pb1 112.1(4) . . ? 
Pb3 O5 Pb2 106.1(5) . . ? 
Pb1 O5 Pb2 99.9(3) . . ? 
Pb3 O5 Pb4 102.1(4) . . ? 
Pb1 O5 Pb4 126.5(5) . . ? 
Pb2 O5 Pb4 108.7(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              24.99 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    5.484 
_refine_diff_density_min   -3.861 
_refine_diff_density_rms    1.076 

#===end 
data_compound2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H B2 N3 O17 Pb6' 
_chemical_formula_weight          1579.80 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'B'  'B'   0.0013   0.0007 
 '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' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'C2/c'
 
loop_ 
 _symmetry_equiv_pos_as_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                    12.589(7) 
_cell_length_b                    15.197(7) 
_cell_length_c                    9.669(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  115.502(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      1669.6(15) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        'Prism'
_exptl_crystal_colour            'Colorless'
_exptl_crystal_size_max          0.1600 
_exptl_crystal_size_mid          0.0900
_exptl_crystal_size_min          0.0700 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     6.285 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2639 
_exptl_absorpt_coefficient_mu     60.380 
_exptl_absorpt_correction_type     'Multi-scan'
_exptl_absorpt_correction_T_min   0.3212
_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          'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator   'mirror' 
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <1.0% 
_diffrn_reflns_number             7293 
_diffrn_reflns_av_R_equivalents   0.0789 
_diffrn_reflns_av_sigmaI/netI     0.0707 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.24 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              1903 
_reflns_number_gt                 1451 
_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)+(0.0492P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1903 
_refine_ls_number_parameters      128 
_refine_ls_number_restraints      32 
_refine_ls_R_factor_all           0.0583 
_refine_ls_R_factor_gt            0.0472 
_refine_ls_wR_factor_ref          0.1151 
_refine_ls_wR_factor_gt           0.1116 
_refine_ls_goodness_of_fit_ref    0.979 
_refine_ls_restrained_S_all       0.978 
_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 0.07821(5) 0.10521(4) 0.00375(6) 0.01546(19) Uani 1 1 d . . . 
Pb2 Pb 0.26748(6) -0.10962(4) 0.02599(7) 0.01800(19) Uani 1 1 d . . . 
Pb3 Pb 0.42477(5) 0.10199(4) -0.00172(6) 0.0215(2) Uani 1 1 d . . . 
B1 B 0.1873(14) -0.0410(12) 0.2688(16) 0.020(4) Uani 1 1 d DU . . 
N1 N 0.3439(13) -0.2255(10) -0.2299(16) 0.035(4) Uani 1 1 d DU . . 
N2 N 0.5000 -0.2709(11) 0.2500 0.017(4) Uani 1 2 d SD . . 
O1 O 0.1968(11) -0.0300(7) 0.4134(11) 0.029(3) Uani 1 1 d D . . 
O2 O 0.0933(9) -0.0269(7) 0.1333(11) 0.022(2) Uani 1 1 d DU . . 
O3 O 0.2951(9) -0.0601(8) 0.2617(11) 0.028(3) Uani 1 1 d D . . 
O4 O 0.3808(14) -0.2532(9) -0.0902(17) 0.060(4) Uani 1 1 d D . . 
O5 O 0.329(2) -0.2756(13) -0.334(2) 0.025(5) Uani 0.50 1 d PDU . . 
O6 O 0.3155(12) -0.1457(10) -0.2515(13) 0.045(4) Uani 1 1 d D . . 
O7 O 0.5000 -0.3528(10) 0.2500 0.031(4) Uani 1 2 d SD . . 
O8 O 0.4156(12) -0.2304(8) 0.2543(14) 0.041(3) Uani 1 1 d D . . 
O9 O 0.4417(8) -0.0420(7) 0.0912(11) 0.020(2) 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 
Pb1 O2 2.318(10) 5 ? 
Pb1 O1 2.328(11) 6 ? 
Pb1 O2 2.330(10) . ? 
Pb2 O9 2.253(10) . ? 
Pb2 O3 2.280(10) . ? 
Pb2 O1 2.375(10) 6 ? 
Pb3 O3 2.256(10) 6 ? 
Pb3 O9 2.340(10) . ? 
Pb3 O9 2.379(9) 5_655 ? 
Pb3 Pb3 3.6255(18) 5_655 ? 
B1 O2 1.352(16) . ? 
B1 O1 1.361(15) . ? 
B1 O3 1.418(17) . ? 
N1 O5 1.210(19) . ? 
N1 O6 1.255(17) . ? 
N1 O4 1.296(16) . ? 
N2 O7 1.245(18) . ? 
N2 O8 1.245(13) . ? 
N2 O8 1.245(13) 2_655 ? 
O1 Pb1 2.328(11) 6_556 ? 
O1 Pb2 2.375(10) 6_556 ? 
O2 Pb1 2.318(10) 5 ? 
O3 Pb3 2.256(10) 6_556 ? 
O9 Pb3 2.379(9) 5_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 
O2 Pb1 O1 97.1(4) 5 6 ? 
O2 Pb1 O2 72.9(4) 5 . ? 
O1 Pb1 O2 82.0(3) 6 . ? 
O9 Pb2 O3 81.9(4) . . ? 
O9 Pb2 O1 81.3(4) . 6 ? 
O3 Pb2 O1 91.7(4) . 6 ? 
O3 Pb3 O9 91.8(4) 6 . ? 
O3 Pb3 O9 80.7(4) 6 5_655 ? 
O9 Pb3 O9 79.6(4) . 5_655 ? 
O3 Pb3 Pb3 85.1(3) 6 5_655 ? 
O9 Pb3 Pb3 40.2(2) . 5_655 ? 
O9 Pb3 Pb3 39.4(2) 5_655 5_655 ? 
O2 B1 O1 129.0(14) . . ? 
O2 B1 O3 116.2(12) . . ? 
O1 B1 O3 114.4(12) . . ? 
O5 N1 O6 122.6(17) . . ? 
O5 N1 O4 121.3(18) . . ? 
O6 N1 O4 115.8(14) . . ? 
O7 N2 O8 119.7(9) . . ? 
O7 N2 O8 119.7(9) . 2_655 ? 
O8 N2 O8 120.6(18) . 2_655 ? 
B1 O1 Pb1 122.5(10) . 6_556 ? 
B1 O1 Pb2 115.5(10) . 6_556 ? 
Pb1 O1 Pb2 116.2(4) 6_556 6_556 ? 
B1 O2 Pb1 133.1(10) . 5 ? 
B1 O2 Pb1 119.5(9) . . ? 
Pb1 O2 Pb1 107.1(4) 5 . ? 
B1 O3 Pb3 107.3(8) . 6_556 ? 
B1 O3 Pb2 112.3(8) . . ? 
Pb3 O3 Pb2 130.8(5) 6_556 . ? 
Pb2 O9 Pb3 113.7(4) . . ? 
Pb2 O9 Pb3 118.6(4) . 5_655 ? 
Pb3 O9 Pb3 100.4(4) . 5_655 ? 
 
_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    3.522 
_refine_diff_density_min   -6.265 
_refine_diff_density_rms    0.641 

#===end 

data_compound3 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H B2 N3 O19 Pb8' 
_chemical_formula_weight          2026.18 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'N'  'N'   0.0061   0.0033 
 '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' 
 'B'  'B'   0.0013   0.0007 
 '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' 
 
_symmetry_cell_setting            'triclinic' 
_symmetry_space_group_name_H-M    'P-1'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    9.0637(3) 
_cell_length_b                    9.9713(4) 
_cell_length_c                    11.6123(5) 
_cell_angle_alpha                 85.559(3) 
_cell_angle_beta                  79.021(3) 
_cell_angle_gamma                 88.640(3) 
_cell_volume                      1027.14(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        'Prism'
_exptl_crystal_colour             'Colorless'
_exptl_crystal_size_max            0.1600
_exptl_crystal_size_mid           0.0800
_exptl_crystal_size_min           0.0600
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     6.551 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1680 
_exptl_absorpt_coefficient_mu     65.403 
_exptl_absorpt_correction_type    'analytical'
_exptl_absorpt_correction_T_min   0.20390
_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          'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator   'mirror' 
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <1.0% 
_diffrn_reflns_number             13780 
_diffrn_reflns_av_R_equivalents   0.0480 
_diffrn_reflns_av_sigmaI/netI     0.0442 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.62 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3614 
_reflns_number_gt                 3208 
_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)+(0.0000P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3614 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0268 
_refine_ls_R_factor_gt            0.0218 
_refine_ls_wR_factor_ref          0.0364 
_refine_ls_wR_factor_gt           0.0342 
_refine_ls_goodness_of_fit_ref    0.924 
_refine_ls_restrained_S_all       0.924 
_refine_ls_shift/su_max           0.001 
_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 0.12076(3) 0.04805(3) 0.10451(3) 0.01475(9) Uani 1 1 d . . . 
Pb2 Pb 0.03535(3) -0.31379(3) 0.10021(3) 0.01485(9) Uani 1 1 d . . . 
Pb3 Pb 0.30412(3) 0.09849(3) -0.20107(3) 0.01603(9) Uani 1 1 d . . . 
Pb4 Pb 0.41726(3) -0.51831(3) 0.80595(3) 0.01424(9) Uani 1 1 d . . . 
Pb5 Pb 0.46609(3) -0.17559(3) -0.02445(3) 0.01438(9) Uani 1 1 d . . . 
Pb6 Pb 0.50247(3) -0.67679(3) 0.51166(3) 0.01588(9) Uani 1 1 d . . . 
Pb7 Pb 0.18889(3) -0.52218(4) 0.38716(3) 0.01659(9) Uani 1 1 d . . . 
Pb8 Pb 0.06377(4) -0.17475(4) 0.42192(4) 0.01979(9) Uani 1 1 d . . . 
B1 B 0.3308(10) -0.2364(10) 0.2231(10) 0.014(2) Uani 1 1 d . . . 
B2 B -0.1714(10) -0.3509(10) 0.3273(10) 0.013(2) Uani 1 1 d U . . 
N1 N 0.7887(8) -0.3901(7) -0.1053(7) 0.0152(18) Uani 1 1 d . . . 
N2 N -0.1986(8) 0.2109(9) 0.2625(8) 0.025(2) Uani 1 1 d . . . 
N3 N 0.3412(10) 0.1282(9) -0.6842(8) 0.031(2) Uani 1 1 d . . . 
O1 O 0.2774(6) -0.2588(6) 0.3381(6) 0.0192(15) Uani 1 1 d . . . 
O2 O 0.4810(6) -0.2595(6) 0.1728(6) 0.0164(15) Uani 1 1 d . . . 
O3 O 0.2401(6) -0.1878(6) 0.1397(6) 0.0174(15) Uani 1 1 d . . . 
O4 O -0.2479(6) -0.3654(6) 0.4404(5) 0.0204(16) Uani 1 1 d . . . 
O5 O -0.0181(6) -0.3207(6) 0.3050(6) 0.0200(16) Uani 1 1 d . . . 
O6 O -0.2341(6) -0.3484(6) 0.2299(6) 0.0175(15) Uani 1 1 d . . . 
O7 O 0.9120(7) -0.3731(8) -0.1739(7) 0.045(2) Uani 1 1 d . . . 
O8 O 0.7083(7) -0.4893(7) -0.1174(7) 0.0341(19) Uani 1 1 d . . . 
O9 O 0.7529(7) -0.3208(7) -0.0239(7) 0.0337(19) Uani 1 1 d . . . 
O10 O -0.2045(7) 0.1817(7) 0.1606(7) 0.036(2) Uani 1 1 d . . . 
O11 O -0.2358(7) 0.3290(7) 0.2933(7) 0.0321(19) Uani 1 1 d . . . 
O12 O -0.1588(9) 0.1250(8) 0.3356(8) 0.054(2) Uani 1 1 d . . . 
O13 O 0.3858(8) 0.0427(8) -0.7539(8) 0.044(2) Uani 1 1 d . . . 
O14 O 0.2380(14) 0.1039(14) -0.6032(13) 0.150(7) Uani 1 1 d . . . 
O15 O 0.3927(10) 0.2414(9) -0.6968(8) 0.060(3) Uani 1 1 d . . . 
O16 O 0.0685(6) -0.3711(6) 0.5315(5) 0.0136(14) Uani 1 1 d . . . 
O17 O 0.5280(6) -0.5015(6) 0.6170(5) 0.0139(14) Uani 1 1 d . . . 
O18 O 0.3555(5) 0.0380(6) -0.0264(5) 0.0114(13) Uani 1 1 d . . . 
O19 O -0.0642(6) -0.1087(6) 0.0823(6) 0.0158(14) 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 
Pb1 O19 2.354(6) 2 ? 
Pb1 O18 2.373(5) . ? 
Pb1 O19 2.381(5) . ? 
Pb1 O3 2.602(6) . ? 
Pb1 Pb3 3.6227(6) . ? 
Pb2 O19 2.226(6) . ? 
Pb2 O5 2.330(6) . ? 
Pb2 O3 2.399(5) . ? 
Pb2 O6 2.628(6) . ? 
Pb3 O18 2.202(6) . ? 
Pb3 O19 2.348(6) 2 ? 
Pb3 O6 2.569(6) 2 ? 
Pb3 O2 2.636(5) 2_655 ? 
Pb4 O17 2.227(6) . ? 
Pb4 O6 2.269(5) 2_546 ? 
Pb4 O2 2.393(6) 2_646 ? 
Pb5 O18 2.332(5) . ? 
Pb5 O18 2.333(5) 2_655 ? 
Pb5 O2 2.405(6) . ? 
Pb5 O3 2.516(6) . ? 
Pb5 Pb5 3.6750(7) 2_655 ? 
Pb6 O17 2.250(6) . ? 
Pb6 O17 2.279(6) 2_646 ? 
Pb6 O4 2.305(5) 2_546 ? 
Pb6 Pb6 3.5150(7) 2_646 ? 
Pb6 Pb7 3.6820(5) . ? 
Pb7 O4 2.363(6) 2_546 ? 
Pb7 O16 2.425(6) . ? 
Pb7 O16 2.567(5) 2_546 ? 
Pb7 O17 2.573(5) 2_646 ? 
Pb7 O1 2.749(6) . ? 
Pb7 Pb8 3.6477(5) . ? 
Pb8 O1 2.175(6) . ? 
Pb8 O16 2.255(6) . ? 
Pb8 O5 2.292(5) . ? 
B1 O1 1.334(12) . ? 
B1 O2 1.396(11) . ? 
B1 O3 1.435(11) . ? 
B2 O4 1.361(12) . ? 
B2 O6 1.358(11) . ? 
B2 O5 1.400(11) . ? 
N1 O9 1.204(9) . ? 
N1 O7 1.249(10) . ? 
N1 O8 1.274(9) . ? 
N2 O10 1.251(10) . ? 
N2 O12 1.255(11) . ? 
N2 O11 1.276(9) . ? 
N3 O14 1.208(13) . ? 
N3 O15 1.220(11) . ? 
N3 O13 1.228(10) . ? 
O2 Pb4 2.393(6) 2_646 ? 
O2 Pb3 2.636(5) 2_655 ? 
O4 Pb6 2.305(5) 2_546 ? 
O4 Pb7 2.363(6) 2_546 ? 
O6 Pb4 2.269(5) 2_546 ? 
O6 Pb3 2.569(6) 2 ? 
O16 Pb7 2.567(5) 2_546 ? 
O17 Pb6 2.279(6) 2_646 ? 
O17 Pb7 2.573(5) 2_646 ? 
O18 Pb5 2.333(5) 2_655 ? 
O19 Pb3 2.348(6) 2 ? 
O19 Pb1 2.354(6) 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 
O19 Pb1 O18 75.55(18) 2 . ? 
O19 Pb1 O19 75.2(2) 2 . ? 
O18 Pb1 O19 116.54(19) . . ? 
O19 Pb1 O3 118.18(19) 2 . ? 
O18 Pb1 O3 71.86(19) . . ? 
O19 Pb1 O3 74.78(17) . . ? 
O19 Pb1 Pb3 39.53(13) 2 . ? 
O18 Pb1 Pb3 36.02(13) . . ? 
O19 Pb1 Pb3 98.45(15) . . ? 
O3 Pb1 Pb3 95.20(14) . . ? 
O19 Pb2 O5 92.6(2) . . ? 
O19 Pb2 O3 81.80(18) . . ? 
O5 Pb2 O3 78.5(2) . . ? 
O19 Pb2 O6 78.6(2) . . ? 
O5 Pb2 O6 55.39(17) . . ? 
O3 Pb2 O6 128.3(2) . . ? 
O18 Pb3 O19 78.98(19) . 2 ? 
O18 Pb3 O6 114.1(2) . 2 ? 
O19 Pb3 O6 77.8(2) 2 2 ? 
O18 Pb3 O2 73.9(2) . 2_655 ? 
O19 Pb3 O2 120.58(19) 2 2_655 ? 
O6 Pb3 O2 67.40(16) 2 2_655 ? 
O18 Pb3 Pb1 39.32(13) . . ? 
O19 Pb3 Pb1 39.67(14) 2 . ? 
O6 Pb3 Pb1 96.79(14) 2 . ? 
O2 Pb3 Pb1 97.98(14) 2_655 . ? 
O17 Pb4 O6 92.1(2) . 2_546 ? 
O17 Pb4 O2 89.9(2) . 2_646 ? 
O6 Pb4 O2 76.52(18) 2_546 2_646 ? 
O18 Pb5 O18 76.05(18) . 2_655 ? 
O18 Pb5 O2 110.91(19) . . ? 
O18 Pb5 O2 76.4(2) 2_655 . ? 
O18 Pb5 O3 74.1(2) . . ? 
O18 Pb5 O3 108.60(19) 2_655 . ? 
O2 Pb5 O3 57.60(17) . . ? 
O18 Pb5 Pb5 38.03(12) . 2_655 ? 
O18 Pb5 Pb5 38.02(13) 2_655 2_655 ? 
O2 Pb5 Pb5 94.41(13) . 2_655 ? 
O3 Pb5 Pb5 91.63(13) . 2_655 ? 
O17 Pb6 O17 78.2(2) . 2_646 ? 
O17 Pb6 O4 85.7(2) . 2_546 ? 
O17 Pb6 O4 77.8(2) 2_646 2_546 ? 
O17 Pb6 Pb6 39.39(15) . 2_646 ? 
O17 Pb6 Pb6 38.81(14) 2_646 2_646 ? 
O4 Pb6 Pb6 79.33(16) 2_546 2_646 ? 
O17 Pb6 Pb7 94.28(13) . . ? 
O17 Pb6 Pb7 43.71(13) 2_646 . ? 
O4 Pb6 Pb7 38.49(15) 2_546 . ? 
Pb6 Pb6 Pb7 65.111(11) 2_646 . ? 
O4 Pb7 O16 80.2(2) 2_546 . ? 
O4 Pb7 O16 81.99(18) 2_546 2_546 ? 
O16 Pb7 O16 76.05(19) . 2_546 ? 
O4 Pb7 O17 71.20(19) 2_546 2_646 ? 
O16 Pb7 O17 104.72(17) . 2_646 ? 
O16 Pb7 O17 152.45(18) 2_546 2_646 ? 
O4 Pb7 O1 116.90(19) 2_546 . ? 
O16 Pb7 O1 65.79(19) . . ? 
O16 Pb7 O1 132.11(17) 2_546 . ? 
O17 Pb7 O1 68.75(17) 2_646 . ? 
O4 Pb7 Pb8 113.93(15) 2_546 . ? 
O16 Pb7 Pb8 37.15(14) . . ? 
O16 Pb7 Pb8 96.04(12) 2_546 . ? 
O17 Pb7 Pb8 100.47(13) 2_646 . ? 
O1 Pb7 Pb8 36.45(12) . . ? 
O4 Pb7 Pb6 37.37(13) 2_546 . ? 
O16 Pb7 Pb6 104.81(12) . . ? 
O16 Pb7 Pb6 114.86(12) 2_546 . ? 
O17 Pb7 Pb6 37.73(14) 2_646 . ? 
O1 Pb7 Pb6 102.38(10) . . ? 
Pb8 Pb7 Pb6 123.739(12) . . ? 
O1 Pb8 O16 79.2(2) . . ? 
O1 Pb8 O5 79.7(2) . . ? 
O16 Pb8 O5 78.9(2) . . ? 
O1 Pb8 Pb7 48.67(17) . . ? 
O16 Pb8 Pb7 40.51(15) . . ? 
O5 Pb8 Pb7 53.75(14) . . ? 
O1 B1 O2 122.6(8) . . ? 
O1 B1 O3 123.5(8) . . ? 
O2 B1 O3 113.8(8) . . ? 
O4 B2 O6 125.4(8) . . ? 
O4 B2 O5 119.6(8) . . ? 
O6 B2 O5 114.5(9) . . ? 
O9 N1 O7 120.4(7) . . ? 
O9 N1 O8 120.8(8) . . ? 
O7 N1 O8 118.5(8) . . ? 
O10 N2 O12 120.9(8) . . ? 
O10 N2 O11 119.7(9) . . ? 
O12 N2 O11 119.4(9) . . ? 
O14 N3 O15 117.5(10) . . ? 
O14 N3 O13 120.2(10) . . ? 
O15 N3 O13 122.2(10) . . ? 
B1 O1 Pb8 122.0(5) . . ? 
B1 O1 Pb7 109.7(6) . . ? 
Pb8 O1 Pb7 94.9(2) . . ? 
B1 O2 Pb4 118.7(6) . 2_646 ? 
B1 O2 Pb5 97.0(5) . . ? 
Pb4 O2 Pb5 115.9(2) 2_646 . ? 
B1 O2 Pb3 121.5(5) . 2_655 ? 
Pb4 O2 Pb3 104.92(17) 2_646 2_655 ? 
Pb5 O2 Pb3 96.9(2) . 2_655 ? 
B1 O3 Pb2 122.6(5) . . ? 
B1 O3 Pb5 91.3(5) . . ? 
Pb2 O3 Pb5 114.2(2) . . ? 
B1 O3 Pb1 130.7(5) . . ? 
Pb2 O3 Pb1 95.84(17) . . ? 
Pb5 O3 Pb1 100.2(2) . . ? 
B2 O4 Pb6 121.9(5) . 2_546 ? 
B2 O4 Pb7 132.4(5) . 2_546 ? 
Pb6 O4 Pb7 104.1(2) 2_546 2_546 ? 
B2 O5 Pb8 117.8(5) . . ? 
B2 O5 Pb2 100.7(5) . . ? 
Pb8 O5 Pb2 127.1(3) . . ? 
B2 O6 Pb4 128.4(6) . 2_546 ? 
B2 O6 Pb3 101.9(5) . 2 ? 
Pb4 O6 Pb3 110.98(19) 2_546 2 ? 
B2 O6 Pb2 88.8(5) . . ? 
Pb4 O6 Pb2 126.5(3) 2_546 . ? 
Pb3 O6 Pb2 92.7(2) 2 . ? 
Pb8 O16 Pb7 102.3(2) . . ? 
Pb8 O16 Pb7 115.4(2) . 2_546 ? 
Pb7 O16 Pb7 103.95(19) . 2_546 ? 
Pb4 O17 Pb6 116.8(3) . . ? 
Pb4 O17 Pb6 124.1(2) . 2_646 ? 
Pb6 O17 Pb6 101.8(2) . 2_646 ? 
Pb4 O17 Pb7 106.4(2) . 2_646 ? 
Pb6 O17 Pb7 106.7(2) . 2_646 ? 
Pb6 O17 Pb7 98.6(2) 2_646 2_646 ? 
Pb3 O18 Pb5 110.7(2) . . ? 
Pb3 O18 Pb5 112.7(2) . 2_655 ? 
Pb5 O18 Pb5 103.95(18) . 2_655 ? 
Pb3 O18 Pb1 104.66(18) . . ? 
Pb5 O18 Pb1 113.1(2) . . ? 
Pb5 O18 Pb1 112.0(2) 2_655 . ? 
Pb2 O19 Pb3 110.6(3) . 2 ? 
Pb2 O19 Pb1 114.3(2) . 2 ? 
Pb3 O19 Pb1 100.80(18) 2 2 ? 
Pb2 O19 Pb1 107.38(19) . . ? 
Pb3 O19 Pb1 118.9(2) 2 . ? 
Pb1 O19 Pb1 104.8(2) 2 . ? 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    1.507 
_refine_diff_density_min   -1.353 
_refine_diff_density_rms    0.307 

#===end 