# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1543156'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/c7nj00203c 2017
_audit_update_record             
;
2017-04-10 deposited with the CCDC.
2017-04-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B8 O16 Pb4'
_chemical_formula_weight         1171.24

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'
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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5502(12)
_cell_length_b                   6.7414(12)
_cell_length_c                   17.087(3)
_cell_angle_alpha                78.799(12)
_cell_angle_beta                 80.592(12)
_cell_angle_gamma                61.228(11)
_cell_volume                     646.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3230
_cell_measurement_theta_min      3.48
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.068
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    52.016
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.3421
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   Face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10786
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2964
_reflns_number_gt                2443
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0279P)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       0.00179(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2964
_refine_ls_number_parameters     134
_refine_ls_number_restraints     464
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0848
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      0.962
_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 1.14915(7) -0.22773(7) 0.17686(3) 0.01427(13) Uani 1 1 d U . .
Pb2 Pb 0.60084(8) 0.24591(7) 0.33959(3) 0.01121(13) Uani 1 1 d U . .
Pb3 Pb -0.14639(8) 0.57353(7) 0.40856(3) 0.01288(13) Uani 1 1 d U . .
Pb4 Pb 1.26667(8) 0.24023(7) 0.04075(3) 0.01327(13) Uani 1 1 d U . .
B1 B 0.485(2) 0.076(2) 0.2191(8) 0.0095(15) Uiso 1 1 d U . .
B2 B 0.737(2) 0.281(2) 0.1491(8) 0.0085(15) Uiso 1 1 d U . .
B3 B 0.258(2) -0.009(2) 0.4912(8) 0.0091(18) Uiso 1 1 d U . .
B4 B 0.239(2) -0.301(2) 0.4340(8) 0.010(2) Uiso 1 1 d U . .
B5 B 0.803(2) 0.246(2) -0.0030(8) 0.0127(17) Uiso 1 1 d U . .
B6 B 1.045(2) 0.311(2) 0.2161(8) 0.0102(16) Uiso 1 1 d U . .
B7 B 0.669(2) 0.657(2) 0.1868(8) 0.0104(17) Uiso 1 1 d U . .
B8 B 0.219(2) 0.040(2) 0.3442(8) 0.0093(17) Uiso 1 1 d U . .
O1 O 0.9839(13) 0.2286(12) 0.1537(5) 0.0100(12) Uiso 1 1 d U . .
O2 O 0.5159(12) -0.1125(12) 0.1797(4) 0.0090(13) Uiso 1 1 d U . .
O3 O 0.2763(12) 0.2901(12) 0.1911(5) 0.0093(13) Uiso 1 1 d U . .
O4 O 0.6906(12) 0.1178(12) 0.2128(4) 0.0094(12) Uiso 1 1 d U . .
O5 O 0.1776(13) 0.1321(12) 0.4215(5) 0.0108(13) Uiso 1 1 d U . .
O6 O 0.8806(12) 0.5625(12) 0.2167(4) 0.0070(13) Uiso 1 1 d U . .
O7 O 0.4461(12) 0.0234(12) 0.3081(4) 0.0082(12) Uiso 1 1 d U . .
O8 O 0.5832(13) 0.5225(12) 0.1679(5) 0.0104(12) Uiso 1 1 d U . .
O9 O 1.0291(13) 0.1888(12) 0.2948(5) 0.0115(13) Uiso 1 1 d U . .
O10 O 0.1903(13) -0.4789(12) 0.4542(5) 0.0110(15) Uiso 1 1 d U . .
O11 O 0.2686(13) 0.0573(13) 0.5576(5) 0.0131(14) Uiso 1 1 d U . .
O12 O 0.3123(13) -0.2389(13) 0.4945(5) 0.0121(15) Uiso 1 1 d U . .
O13 O 0.2303(13) -0.1894(12) 0.3595(5) 0.0110(13) Uiso 1 1 d U . .
O14 O 0.6897(13) 0.2586(13) 0.0745(5) 0.0140(13) Uiso 1 1 d U . .
O15 O 0.9343(14) 0.3568(13) -0.0306(5) 0.0165(14) Uiso 1 1 d U . .
O16 O 0.7642(14) 0.1310(14) -0.0503(5) 0.0181(15) Uiso 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 O16 2.198(8) 2_755 ?
Pb1 O8 2.508(7) 1_645 ?
Pb1 O6 2.681(7) 1_545 ?
Pb1 O1 2.693(7) . ?
Pb2 O11 2.326(8) 2_656 ?
Pb2 O7 2.350(7) . ?
Pb2 O4 2.367(8) . ?
Pb2 O9 2.642(7) . ?
Pb3 O10 2.302(7) 1_565 ?
Pb3 O10 2.316(8) 2_556 ?
Pb3 O11 2.379(8) 2_566 ?
Pb3 O5 2.688(7) . ?
Pb4 O15 2.365(8) 2_765 ?
Pb4 O15 2.386(8) . ?
Pb4 O1 2.465(7) . ?
Pb4 O16 2.579(8) 2_755 ?
Pb4 O3 2.669(8) 1_655 ?
B1 O2 1.466(14) . ?
B1 O4 1.487(14) . ?
B1 O3 1.493(14) . ?
B1 O7 1.501(15) . ?
B2 O14 1.411(14) . ?
B2 O1 1.491(14) . ?
B2 O4 1.495(13) . ?
B2 O8 1.514(14) . ?
B3 O11 1.324(15) . ?
B3 O5 1.373(14) . ?
B3 O12 1.402(14) . ?
B4 O13 1.342(14) . ?
B4 O10 1.352(13) . ?
B4 O12 1.414(15) . ?
B5 O16 1.348(15) . ?
B5 O15 1.367(14) . ?
B5 O14 1.406(15) . ?
B6 O3 1.449(14) 1_655 ?
B6 O9 1.450(14) . ?
B6 O1 1.481(14) . ?
B6 O6 1.510(14) . ?
B7 O6 1.358(14) . ?
B7 O2 1.377(14) 1_565 ?
B7 O8 1.382(14) . ?
B8 O9 1.444(14) 1_455 ?
B8 O7 1.471(14) . ?
B8 O13 1.489(14) . ?
B8 O5 1.495(15) . ?
O2 B7 1.377(14) 1_545 ?
O3 B6 1.449(14) 1_455 ?
O3 Pb4 2.669(8) 1_455 ?
O6 Pb1 2.681(6) 1_565 ?
O8 Pb1 2.508(7) 1_465 ?
O9 B8 1.444(14) 1_655 ?
O10 Pb3 2.302(7) 1_545 ?
O10 Pb3 2.316(8) 2_556 ?
O11 Pb2 2.326(8) 2_656 ?
O11 Pb3 2.379(8) 2_566 ?
O15 Pb4 2.365(8) 2_765 ?
O16 Pb1 2.198(8) 2_755 ?
O16 Pb4 2.579(8) 2_755 ?

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
O16 Pb1 O8 80.1(3) 2_755 1_645 ?
O16 Pb1 O6 120.2(3) 2_755 1_545 ?
O8 Pb1 O6 117.0(2) 1_645 1_545 ?
O16 Pb1 O1 72.8(3) 2_755 . ?
O8 Pb1 O1 118.6(2) 1_645 . ?
O6 Pb1 O1 124.4(2) 1_545 . ?
O11 Pb2 O7 79.8(3) 2_656 . ?
O11 Pb2 O4 111.7(3) 2_656 . ?
O7 Pb2 O4 58.7(2) . . ?
O11 Pb2 O9 91.9(2) 2_656 . ?
O7 Pb2 O9 124.9(2) . . ?
O4 Pb2 O9 75.3(2) . . ?
O11 Pb2 B1 104.9(3) 2_656 . ?
O7 Pb2 B1 31.1(3) . . ?
O4 Pb2 B1 30.8(3) . . ?
O9 Pb2 B1 105.5(3) . . ?
O10 Pb3 O10 75.4(3) 1_565 2_556 ?
O10 Pb3 O11 79.2(3) 1_565 2_566 ?
O10 Pb3 O11 83.5(3) 2_556 2_566 ?
O10 Pb3 O5 68.5(2) 1_565 . ?
O10 Pb3 O5 80.9(2) 2_556 . ?
O11 Pb3 O5 146.7(2) 2_566 . ?
O10 Pb3 Pb3 37.84(19) 1_565 2_566 ?
O10 Pb3 Pb3 37.57(18) 2_556 2_566 ?
O11 Pb3 Pb3 79.02(19) 2_566 2_566 ?
O5 Pb3 Pb3 70.65(16) . 2_566 ?
O15 Pb4 O15 74.4(3) 2_765 . ?
O15 Pb4 O1 88.3(3) 2_765 . ?
O15 Pb4 O1 80.3(3) . . ?
O15 Pb4 O16 146.7(3) 2_765 2_755 ?
O15 Pb4 O16 76.6(3) . 2_755 ?
O1 Pb4 O16 71.0(3) . 2_755 ?
O15 Pb4 O3 80.5(3) 2_765 1_655 ?
O15 Pb4 O3 128.3(3) . 1_655 ?
O1 Pb4 O3 54.3(2) . 1_655 ?
O16 Pb4 O3 105.7(2) 2_755 1_655 ?
O15 Pb4 Pb4 145.83(19) 2_765 2_855 ?
O15 Pb4 Pb4 107.2(2) . 2_855 ?
O1 Pb4 Pb4 125.90(17) . 2_855 ?
O16 Pb4 Pb4 59.86(18) 2_755 2_855 ?
O3 Pb4 Pb4 118.45(16) 1_655 2_855 ?
O2 B1 O4 116.5(9) . . ?
O2 B1 O3 110.0(9) . . ?
O4 B1 O3 110.3(9) . . ?
O2 B1 O7 110.0(8) . . ?
O4 B1 O7 101.4(8) . . ?
O3 B1 O7 108.0(9) . . ?
O2 B1 Pb2 151.0(8) . . ?
O4 B1 Pb2 54.5(5) . . ?
O3 B1 Pb2 98.5(7) . . ?
O7 B1 Pb2 53.9(5) . . ?
O14 B2 O1 114.4(9) . . ?
O14 B2 O4 109.2(9) . . ?
O1 B2 O4 106.5(8) . . ?
O14 B2 O8 109.9(9) . . ?
O1 B2 O8 107.2(8) . . ?
O4 B2 O8 109.6(9) . . ?
O11 B3 O5 125.1(10) . . ?
O11 B3 O12 117.3(10) . . ?
O5 B3 O12 117.3(10) . . ?
O13 B4 O10 123.3(11) . . ?
O13 B4 O12 119.3(10) . . ?
O10 B4 O12 117.4(10) . . ?
O16 B5 O15 121.7(11) . . ?
O16 B5 O14 116.7(10) . . ?
O15 B5 O14 121.5(11) . . ?
O3 B6 O9 113.6(9) 1_655 . ?
O3 B6 O1 106.6(9) 1_655 . ?
O9 B6 O1 111.6(9) . . ?
O3 B6 O6 106.7(8) 1_655 . ?
O9 B6 O6 109.3(9) . . ?
O1 B6 O6 108.8(9) . . ?
O6 B7 O2 123.9(10) . 1_565 ?
O6 B7 O8 121.0(10) . . ?
O2 B7 O8 114.9(10) 1_565 . ?
O9 B8 O7 113.3(9) 1_455 . ?
O9 B8 O13 107.7(9) 1_455 . ?
O7 B8 O13 110.1(9) . . ?
O9 B8 O5 109.9(9) 1_455 . ?
O7 B8 O5 105.6(8) . . ?
O13 B8 O5 110.2(9) . . ?
B6 O1 B2 120.6(9) . . ?
B6 O1 Pb4 101.9(6) . . ?
B2 O1 Pb4 127.0(6) . . ?
B6 O1 Pb1 112.7(6) . . ?
B2 O1 Pb1 94.7(5) . . ?
Pb4 O1 Pb1 96.6(3) . . ?
B7 O2 B1 133.7(9) 1_545 . ?
B6 O3 B1 119.2(8) 1_455 . ?
B6 O3 Pb4 94.1(6) 1_455 1_455 ?
B1 O3 Pb4 103.0(6) . 1_455 ?
B1 O4 B2 124.7(8) . . ?
B1 O4 Pb2 94.7(6) . . ?
B2 O4 Pb2 111.2(6) . . ?
B3 O5 B8 121.7(9) . . ?
B3 O5 Pb3 126.4(7) . . ?
B8 O5 Pb3 110.3(6) . . ?
B7 O6 B6 120.2(8) . . ?
B7 O6 Pb1 119.8(6) . 1_565 ?
B6 O6 Pb1 105.7(6) . 1_565 ?
B8 O7 B1 120.3(8) . . ?
B8 O7 Pb2 122.4(6) . . ?
B1 O7 Pb2 95.0(6) . . ?
B7 O8 B2 123.4(9) . . ?
B7 O8 Pb1 103.5(7) . 1_465 ?
B2 O8 Pb1 133.1(6) . 1_465 ?
B8 O9 B6 126.6(9) 1_655 . ?
B8 O9 Pb2 121.1(6) 1_655 . ?
B6 O9 Pb2 112.2(6) . . ?
B4 O10 Pb3 115.7(7) . 1_545 ?
B4 O10 Pb3 112.6(7) . 2_556 ?
Pb3 O10 Pb3 104.6(3) 1_545 2_556 ?
B3 O11 Pb2 111.6(7) . 2_656 ?
B3 O11 Pb3 131.6(7) . 2_566 ?
Pb2 O11 Pb3 116.6(3) 2_656 2_566 ?
B3 O12 B4 118.4(9) . . ?
B4 O13 B8 121.0(9) . . ?
B5 O14 B2 135.0(9) . . ?
B5 O15 Pb4 116.3(7) . 2_765 ?
B5 O15 Pb4 115.8(7) . . ?
Pb4 O15 Pb4 105.6(3) 2_765 . ?
B5 O16 Pb1 110.6(7) . 2_755 ?
B5 O16 Pb4 139.1(8) . 2_755 ?
Pb1 O16 Pb4 107.3(3) 2_755 2_755 ?

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
O11 Pb2 B1 O2 -26.5(16) 2_656 . . . ?
O7 Pb2 B1 O2 -63.8(14) . . . . ?
O4 Pb2 B1 O2 81.2(16) . . . . ?
O9 Pb2 B1 O2 69.8(16) . . . . ?
O11 Pb2 B1 O4 -107.7(6) 2_656 . . . ?
O7 Pb2 B1 O4 -145.0(9) . . . . ?
O9 Pb2 B1 O4 -11.4(6) . . . . ?
O11 Pb2 B1 O3 143.4(6) 2_656 . . . ?
O7 Pb2 B1 O3 106.1(9) . . . . ?
O4 Pb2 B1 O3 -108.9(9) . . . . ?
O9 Pb2 B1 O3 -120.3(6) . . . . ?
O11 Pb2 B1 O7 37.3(6) 2_656 . . . ?
O4 Pb2 B1 O7 145.0(9) . . . . ?
O9 Pb2 B1 O7 133.6(5) . . . . ?
O3 B6 O1 B2 -164.2(8) 1_655 . . . ?
O9 B6 O1 B2 71.3(12) . . . . ?
O6 B6 O1 B2 -49.4(12) . . . . ?
O3 B6 O1 Pb4 -17.2(9) 1_655 . . . ?
O9 B6 O1 Pb4 -141.7(7) . . . . ?
O6 B6 O1 Pb4 97.6(7) . . . . ?
O3 B6 O1 Pb1 85.3(8) 1_655 . . . ?
O9 B6 O1 Pb1 -39.2(10) . . . . ?
O6 B6 O1 Pb1 -159.9(6) . . . . ?
O14 B2 O1 B6 160.7(9) . . . . ?
O4 B2 O1 B6 -78.6(11) . . . . ?
O8 B2 O1 B6 38.6(12) . . . . ?
O14 B2 O1 Pb4 22.5(12) . . . . ?
O4 B2 O1 Pb4 143.2(6) . . . . ?
O8 B2 O1 Pb4 -99.6(9) . . . . ?
O14 B2 O1 Pb1 -79.4(8) . . . . ?
O4 B2 O1 Pb1 41.3(8) . . . . ?
O8 B2 O1 Pb1 158.5(7) . . . . ?
O15 Pb4 O1 B6 -68.6(6) 2_765 . . . ?
O15 Pb4 O1 B6 -143.0(6) . . . . ?
O16 Pb4 O1 B6 137.9(7) 2_755 . . . ?
O3 Pb4 O1 B6 10.9(6) 1_655 . . . ?
Pb4 Pb4 O1 B6 112.7(6) 2_855 . . . ?
O15 Pb4 O1 B2 75.5(8) 2_765 . . . ?
O15 Pb4 O1 B2 1.1(7) . . . . ?
O16 Pb4 O1 B2 -78.1(8) 2_755 . . . ?
O3 Pb4 O1 B2 155.0(8) 1_655 . . . ?
Pb4 Pb4 O1 B2 -103.2(7) 2_855 . . . ?
O15 Pb4 O1 Pb1 176.5(3) 2_765 . . . ?
O15 Pb4 O1 Pb1 102.1(3) . . . . ?
O16 Pb4 O1 Pb1 23.0(2) 2_755 . . . ?
O3 Pb4 O1 Pb1 -104.0(3) 1_655 . . . ?
Pb4 Pb4 O1 Pb1 -2.2(3) 2_855 . . . ?
O16 Pb1 O1 B6 -132.8(7) 2_755 . . . ?
O8 Pb1 O1 B6 -64.8(7) 1_645 . . . ?
O6 Pb1 O1 B6 111.9(7) 1_545 . . . ?
O16 Pb1 O1 B2 101.1(6) 2_755 . . . ?
O8 Pb1 O1 B2 169.2(6) 1_645 . . . ?
O6 Pb1 O1 B2 -14.1(7) 1_545 . . . ?
O16 Pb1 O1 Pb4 -26.9(3) 2_755 . . . ?
O8 Pb1 O1 Pb4 41.1(3) 1_645 . . . ?
O6 Pb1 O1 Pb4 -142.2(2) 1_545 . . . ?
O4 B1 O2 B7 57.6(16) . . . 1_545 ?
O3 B1 O2 B7 -175.9(10) . . . 1_545 ?
O7 B1 O2 B7 -57.0(15) . . . 1_545 ?
Pb2 B1 O2 B7 -6(2) . . . 1_545 ?
O2 B1 O3 B6 70.6(12) . . . 1_455 ?
O4 B1 O3 B6 -159.5(9) . . . 1_455 ?
O7 B1 O3 B6 -49.5(12) . . . 1_455 ?
Pb2 B1 O3 B6 -104.2(8) . . . 1_455 ?
O2 B1 O3 Pb4 -31.7(9) . . . 1_455 ?
O4 B1 O3 Pb4 98.2(8) . . . 1_455 ?
O7 B1 O3 Pb4 -151.8(6) . . . 1_455 ?
Pb2 B1 O3 Pb4 153.5(3) . . . 1_455 ?
O2 B1 O4 B2 92.5(12) . . . . ?
O3 B1 O4 B2 -33.8(14) . . . . ?
O7 B1 O4 B2 -148.1(9) . . . . ?
Pb2 B1 O4 B2 -119.9(10) . . . . ?
O2 B1 O4 Pb2 -147.7(8) . . . . ?
O3 B1 O4 Pb2 86.0(8) . . . . ?
O7 B1 O4 Pb2 -28.2(7) . . . . ?
O14 B2 O4 B1 -42.7(13) . . . . ?
O1 B2 O4 B1 -166.7(9) . . . . ?
O8 B2 O4 B1 77.7(12) . . . . ?
O14 B2 O4 Pb2 -154.7(7) . . . . ?
O1 B2 O4 Pb2 81.3(8) . . . . ?
O8 B2 O4 Pb2 -34.3(9) . . . . ?
O11 Pb2 O4 B1 82.5(6) 2_656 . . . ?
O7 Pb2 O4 B1 20.3(6) . . . . ?
O9 Pb2 O4 B1 168.7(6) . . . . ?
O11 Pb2 O4 B2 -147.4(6) 2_656 . . . ?
O7 Pb2 O4 B2 150.4(7) . . . . ?
O9 Pb2 O4 B2 -61.2(6) . . . . ?
B1 Pb2 O4 B2 130.1(9) . . . . ?
O11 B3 O5 B8 166.1(10) . . . . ?
O12 B3 O5 B8 -19.8(14) . . . . ?
O11 B3 O5 Pb3 -29.7(15) . . . . ?
O12 B3 O5 Pb3 144.4(7) . . . . ?
O9 B8 O5 B3 149.2(9) 1_455 . . . ?
O7 B8 O5 B3 -88.3(11) . . . . ?
O13 B8 O5 B3 30.6(13) . . . . ?
O9 B8 O5 Pb3 -17.4(10) 1_455 . . . ?
O7 B8 O5 Pb3 105.2(7) . . . . ?
O13 B8 O5 Pb3 -135.9(7) . . . . ?
O10 Pb3 O5 B3 67.6(8) 1_565 . . . ?
O10 Pb3 O5 B3 -10.2(8) 2_556 . . . ?
O11 Pb3 O5 B3 52.8(9) 2_566 . . . ?
Pb3 Pb3 O5 B3 27.2(8) 2_566 . . . ?
O10 Pb3 O5 B8 -126.6(6) 1_565 . . . ?
O10 Pb3 O5 B8 155.6(6) 2_556 . . . ?
O11 Pb3 O5 B8 -141.4(6) 2_566 . . . ?
Pb3 Pb3 O5 B8 -167.0(6) 2_566 . . . ?
O2 B7 O6 B6 -175.1(10) 1_565 . . . ?
O8 B7 O6 B6 10.9(16) . . . . ?
O2 B7 O6 Pb1 -41.1(15) 1_565 . . 1_565 ?
O8 B7 O6 Pb1 144.9(8) . . . 1_565 ?
O3 B6 O6 B7 137.2(10) 1_655 . . . ?
O9 B6 O6 B7 -99.6(11) . . . . ?
O1 B6 O6 B7 22.5(13) . . . . ?
O3 B6 O6 Pb1 -2.4(9) 1_655 . . 1_565 ?
O9 B6 O6 Pb1 120.8(7) . . . 1_565 ?
O1 B6 O6 Pb1 -117.1(7) . . . 1_565 ?
O9 B8 O7 B1 -22.8(13) 1_455 . . . ?
O13 B8 O7 B1 97.9(10) . . . . ?
O5 B8 O7 B1 -143.1(9) . . . . ?
O9 B8 O7 Pb2 96.6(9) 1_455 . . . ?
O13 B8 O7 Pb2 -142.8(7) . . . . ?
O5 B8 O7 Pb2 -23.8(11) . . . . ?
O2 B1 O7 B8 -75.2(12) . . . . ?
O4 B1 O7 B8 160.9(8) . . . . ?
O3 B1 O7 B8 44.9(12) . . . . ?
Pb2 B1 O7 B8 132.4(9) . . . . ?
O2 B1 O7 Pb2 152.4(7) . . . . ?
O4 B1 O7 Pb2 28.5(7) . . . . ?
O3 B1 O7 Pb2 -87.5(7) . . . . ?
O11 Pb2 O7 B8 85.6(8) 2_656 . . . ?
O4 Pb2 O7 B8 -151.0(8) . . . . ?
O9 Pb2 O7 B8 170.8(7) . . . . ?
B1 Pb2 O7 B8 -130.9(10) . . . . ?
O11 Pb2 O7 B1 -143.5(6) 2_656 . . . ?
O4 Pb2 O7 B1 -20.1(6) . . . . ?
O9 Pb2 O7 B1 -58.3(6) . . . . ?
O6 B7 O8 B2 -23.2(16) . . . . ?
O2 B7 O8 B2 162.3(9) 1_565 . . . ?
O6 B7 O8 Pb1 155.7(9) . . . 1_465 ?
O2 B7 O8 Pb1 -18.8(11) 1_565 . . 1_465 ?
O14 B2 O8 B7 -126.0(11) . . . . ?
O1 B2 O8 B7 -1.2(14) . . . . ?
O4 B2 O8 B7 114.0(11) . . . . ?
O14 B2 O8 Pb1 55.4(12) . . . 1_465 ?
O1 B2 O8 Pb1 -179.7(5) . . . 1_465 ?
O4 B2 O8 Pb1 -64.5(11) . . . 1_465 ?
O3 B6 O9 B8 -5.5(15) 1_655 . . 1_655 ?
O1 B6 O9 B8 115.0(11) . . . 1_655 ?
O6 B6 O9 B8 -124.6(10) . . . 1_655 ?
O3 B6 O9 Pb2 177.8(7) 1_655 . . . ?
O1 B6 O9 Pb2 -61.7(10) . . . . ?
O6 B6 O9 Pb2 58.7(9) . . . . ?
O11 Pb2 O9 B8 -11.6(8) 2_656 . . 1_655 ?
O7 Pb2 O9 B8 -90.4(8) . . . 1_655 ?
O4 Pb2 O9 B8 -123.5(8) . . . 1_655 ?
B1 Pb2 O9 B8 -117.5(8) . . . 1_655 ?
O11 Pb2 O9 B6 165.4(7) 2_656 . . . ?
O7 Pb2 O9 B6 86.5(7) . . . . ?
O4 Pb2 O9 B6 53.4(7) . . . . ?
B1 Pb2 O9 B6 59.4(7) . . . . ?
O13 B4 O10 Pb3 -47.4(14) . . . 1_545 ?
O12 B4 O10 Pb3 135.5(8) . . . 1_545 ?
O13 B4 O10 Pb3 -167.6(9) . . . 2_556 ?
O12 B4 O10 Pb3 15.3(12) . . . 2_556 ?
O5 B3 O11 Pb2 177.1(9) . . . 2_656 ?
O12 B3 O11 Pb2 3.0(12) . . . 2_656 ?
O5 B3 O11 Pb3 3.9(17) . . . 2_566 ?
O12 B3 O11 Pb3 -170.2(6) . . . 2_566 ?
O11 B3 O12 B4 161.9(10) . . . . ?
O5 B3 O12 B4 -12.6(14) . . . . ?
O13 B4 O12 B3 33.2(15) . . . . ?
O10 B4 O12 B3 -149.6(10) . . . . ?
O10 B4 O13 B8 162.8(10) . . . . ?
O12 B4 O13 B8 -20.2(16) . . . . ?
O9 B8 O13 B4 -129.8(10) 1_455 . . . ?
O7 B8 O13 B4 106.2(11) . . . . ?
O5 B8 O13 B4 -10.0(13) . . . . ?
O16 B5 O14 B2 152.2(11) . . . . ?
O15 B5 O14 B2 -31.8(19) . . . . ?
O1 B2 O14 B5 -16.5(17) . . . . ?
O4 B2 O14 B5 -135.7(11) . . . . ?
O8 B2 O14 B5 104.1(13) . . . . ?
O16 B5 O15 Pb4 112.9(11) . . . 2_765 ?
O14 B5 O15 Pb4 -62.9(13) . . . 2_765 ?
O16 B5 O15 Pb4 -122.1(10) . . . . ?
O14 B5 O15 Pb4 62.1(13) . . . . ?
O15 Pb4 O15 B5 -130.3(9) 2_765 . . . ?
O1 Pb4 O15 B5 -39.4(8) . . . . ?
O16 Pb4 O15 B5 33.2(8) 2_755 . . . ?
O3 Pb4 O15 B5 -66.4(9) 1_655 . . . ?
Pb4 Pb4 O15 B5 85.3(8) 2_855 . . . ?
O15 Pb4 O15 Pb4 0.0 2_765 . . 2_765 ?
O1 Pb4 O15 Pb4 90.9(3) . . . 2_765 ?
O16 Pb4 O15 Pb4 163.5(4) 2_755 . . 2_765 ?
O3 Pb4 O15 Pb4 63.9(4) 1_655 . . 2_765 ?
Pb4 Pb4 O15 Pb4 -144.4(2) 2_855 . . 2_765 ?
O15 B5 O16 Pb1 -15.5(14) . . . 2_755 ?
O14 B5 O16 Pb1 160.5(8) . . . 2_755 ?
O15 B5 O16 Pb4 141.5(9) . . . 2_755 ?
O14 B5 O16 Pb4 -42.5(17) . . . 2_755 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.729
_refine_diff_density_min         -2.970
_refine_diff_density_rms         0.561
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1543157'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/c7nj00203c 2017
_audit_update_record             
;
2017-04-10 deposited with the CCDC.
2017-04-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B10 O21 Pb6'
_chemical_formula_weight         1687.24

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'
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                   21.185(2)
_cell_length_b                   4.7866(5)
_cell_length_c                   19.549(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.572(6)
_cell_angle_gamma                90.00
_cell_volume                     1843.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5247
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.085
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2840
_exptl_absorpt_coefficient_mu    54.712
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.2407
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   Face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14219
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.54
_reflns_number_total             2125
_reflns_number_gt                1948
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0453P)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       0.00112(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2125
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0881
_refine_ls_wR_factor_gt          0.0854
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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 0.838371(17) 0.79821(7) 0.098214(19) 0.01252(14) Uani 1 1 d . . .
Pb2 Pb 0.914503(18) 0.78761(7) -0.051024(18) 0.01182(14) Uani 1 1 d . . .
Pb3 Pb 0.951789(19) 0.78086(7) 0.30791(2) 0.01247(14) Uani 1 1 d . . .
B1 B 0.9356(5) 0.2792(17) 0.1977(5) 0.0073(18) Uiso 1 1 d . . .
B2 B 0.9321(5) 1.3115(19) 0.0618(5) 0.0099(18) Uiso 1 1 d . . .
B3 B 0.8203(5) 1.2572(18) 0.2163(6) 0.0089(18) Uiso 1 1 d . . .
B4 B 0.7183(5) 0.404(2) 0.1053(5) 0.0137(18) Uiso 1 1 d . . .
B5 B 0.7070(5) 1.095(2) 0.1988(5) 0.0126(18) Uiso 1 1 d . . .
O1 O 0.8828(3) 1.1265(11) 0.2187(3) 0.0092(11) Uiso 1 1 d . . .
O2 O 0.9333(3) 0.5740(11) 0.2002(3) 0.0101(11) Uiso 1 1 d . . .
O3 O 0.9286(3) 1.1680(13) 0.1228(3) 0.0109(12) Uiso 1 1 d . . .
O4 O 0.7747(3) 1.0551(11) 0.2280(3) 0.0103(11) Uiso 1 1 d . . .
O5 O 0.6769(4) 0.2499(12) 0.1339(4) 0.0161(14) Uiso 1 1 d . . .
O6 O 1.0000 1.1480(17) 0.2500 0.0119(16) Uiso 1 2 d S . .
O7 O 0.8381(3) 0.4764(12) 0.2741(3) 0.0135(12) Uiso 1 1 d . . .
O8 O 0.9129(3) 0.5875(13) 0.0522(3) 0.0169(12) Uiso 1 1 d . . .
O9 O 0.7880(3) 0.3839(12) 0.1420(3) 0.0125(11) Uiso 1 1 d . . .
O10 O 0.9538(3) 1.1798(12) 0.0145(3) 0.0131(12) Uiso 1 1 d . . .
O11 O 0.6901(3) 0.5636(13) 0.0462(3) 0.0200(13) Uiso 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 O8 2.315(6) . ?
Pb1 O2 2.495(6) . ?
Pb1 O3 2.518(6) . ?
Pb1 O9 2.544(6) . ?
Pb1 O1 2.697(5) . ?
Pb1 O11 2.742(6) 7_665 ?
Pb2 O8 2.246(6) . ?
Pb2 O10 2.252(6) . ?
Pb2 O11 2.362(6) 7_665 ?
Pb2 O10 2.618(6) 5_775 ?
Pb3 O2 2.228(5) . ?
Pb3 O1 2.458(6) . ?
Pb3 O6 2.503(6) . ?
Pb3 O7 2.682(6) . ?
Pb3 O2 2.685(5) 2_755 ?
Pb3 Pb3 3.5637(7) 2_755 ?
B1 O2 1.413(9) . ?
B1 O6 1.508(11) 1_545 ?
B1 O3 1.512(11) 1_545 ?
B1 O1 1.515(10) 1_545 ?
B2 O10 1.333(11) . ?
B2 O8 1.375(10) 1_565 ?
B2 O3 1.402(11) . ?
B3 O4 1.443(11) . ?
B3 O1 1.448(11) . ?
B3 O7 1.485(11) 1_565 ?
B3 O9 1.488(11) 1_565 ?
B4 O11 1.330(11) . ?
B4 O9 1.388(11) . ?
B4 O5 1.409(11) . ?
B5 O4 1.348(11) . ?
B5 O7 1.376(10) 4_655 ?
B5 O5 1.403(11) 1_565 ?
O1 B1 1.515(10) 1_565 ?
O2 Pb3 2.685(5) 2_755 ?
O3 B1 1.512(11) 1_565 ?
O5 B5 1.403(11) 1_545 ?
O6 B1 1.508(11) 2_765 ?
O6 B1 1.508(11) 1_565 ?
O6 Pb3 2.503(6) 2_755 ?
O7 B5 1.376(10) 4_645 ?
O7 B3 1.485(11) 1_545 ?
O8 B2 1.375(10) 1_545 ?
O9 B3 1.488(11) 1_545 ?
O10 Pb2 2.618(6) 5_775 ?
O11 Pb2 2.362(6) 7_665 ?
O11 Pb1 2.742(6) 7_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
O8 Pb1 O2 70.00(19) . . ?
O8 Pb1 O3 78.61(19) . . ?
O2 Pb1 O3 79.47(18) . . ?
O8 Pb1 O9 102.76(19) . . ?
O2 Pb1 O9 73.18(18) . . ?
O3 Pb1 O9 150.02(19) . . ?
O8 Pb1 O1 121.6(2) . . ?
O2 Pb1 O1 68.47(17) . . ?
O3 Pb1 O1 55.04(16) . . ?
O9 Pb1 O1 102.43(17) . . ?
O8 Pb1 O11 68.20(19) . 7_665 ?
O2 Pb1 O11 137.20(17) . 7_665 ?
O3 Pb1 O11 83.76(18) . 7_665 ?
O9 Pb1 O11 125.00(18) . 7_665 ?
O1 Pb1 O11 129.25(17) . 7_665 ?
O8 Pb2 O10 88.2(2) . . ?
O8 Pb2 O11 76.6(2) . 7_665 ?
O10 Pb2 O11 83.2(2) . 7_665 ?
O8 Pb2 O10 98.5(2) . 5_775 ?
O10 Pb2 O10 70.2(2) . 5_775 ?
O11 Pb2 O10 153.2(2) 7_665 5_775 ?
O2 Pb3 O1 77.09(18) . . ?
O2 Pb3 O6 80.99(17) . . ?
O1 Pb3 O6 56.06(14) . . ?
O2 Pb3 O7 72.28(18) . . ?
O1 Pb3 O7 86.82(18) . . ?
O6 Pb3 O7 138.49(12) . . ?
O2 Pb3 O2 68.2(2) . 2_755 ?
O1 Pb3 O2 121.47(16) . 2_755 ?
O6 Pb3 O2 72.71(15) . 2_755 ?
O7 Pb3 O2 122.44(16) . 2_755 ?
O2 Pb3 Pb3 48.83(14) . 2_755 ?
O1 Pb3 Pb3 83.09(12) . 2_755 ?
O6 Pb3 Pb3 44.60(13) . 2_755 ?
O7 Pb3 Pb3 121.06(11) . 2_755 ?
O2 Pb3 Pb3 38.65(11) 2_755 2_755 ?
O2 B1 O6 115.2(8) . 1_545 ?
O2 B1 O3 113.1(7) . 1_545 ?
O6 B1 O3 104.6(6) 1_545 1_545 ?
O2 B1 O1 115.7(7) . 1_545 ?
O6 B1 O1 100.9(6) 1_545 1_545 ?
O3 B1 O1 105.9(6) 1_545 1_545 ?
O10 B2 O8 121.4(8) . 1_565 ?
O10 B2 O3 119.9(8) . . ?
O8 B2 O3 118.7(7) 1_565 . ?
O4 B3 O1 111.2(7) . . ?
O4 B3 O7 110.5(7) . 1_565 ?
O1 B3 O7 107.9(7) . 1_565 ?
O4 B3 O9 109.5(8) . 1_565 ?
O1 B3 O9 107.1(7) . 1_565 ?
O7 B3 O9 110.6(6) 1_565 1_565 ?
O11 B4 O9 122.8(8) . . ?
O11 B4 O5 120.0(8) . . ?
O9 B4 O5 117.2(8) . . ?
O4 B5 O7 124.0(8) . 4_655 ?
O4 B5 O5 121.2(7) . 1_565 ?
O7 B5 O5 114.7(8) 4_655 1_565 ?
B3 O1 B1 122.7(6) . 1_565 ?
B3 O1 Pb3 127.7(5) . . ?
B1 O1 Pb3 102.2(5) 1_565 . ?
B3 O1 Pb1 101.6(5) . . ?
B1 O1 Pb1 95.7(4) 1_565 . ?
Pb3 O1 Pb1 98.79(18) . . ?
B1 O2 Pb3 118.7(5) . . ?
B1 O2 Pb1 115.4(5) . . ?
Pb3 O2 Pb1 111.9(2) . . ?
B1 O2 Pb3 108.8(5) . 2_755 ?
Pb3 O2 Pb3 92.52(19) . 2_755 ?
Pb1 O2 Pb3 106.05(18) . 2_755 ?
B2 O3 B1 129.4(7) . 1_565 ?
B2 O3 Pb1 117.1(5) . . ?
B1 O3 Pb1 103.3(4) 1_565 . ?
B5 O4 B3 120.4(7) . . ?
B5 O5 B4 119.5(8) 1_545 . ?
B1 O6 B1 130.8(9) 2_765 1_565 ?
B1 O6 Pb3 100.5(4) 2_765 2_755 ?
B1 O6 Pb3 113.8(4) 1_565 2_755 ?
B1 O6 Pb3 113.8(4) 2_765 . ?
B1 O6 Pb3 100.5(4) 1_565 . ?
Pb3 O6 Pb3 90.8(3) 2_755 . ?
B5 O7 B3 124.6(7) 4_645 1_545 ?
B5 O7 Pb3 111.6(5) 4_645 . ?
B3 O7 Pb3 121.7(5) 1_545 . ?
B2 O8 Pb2 115.5(5) 1_545 . ?
B2 O8 Pb1 125.2(5) 1_545 . ?
Pb2 O8 Pb1 113.6(3) . . ?
B4 O9 B3 123.5(7) . 1_545 ?
B4 O9 Pb1 105.7(5) . . ?
B3 O9 Pb1 123.1(5) 1_545 . ?
B2 O10 Pb2 129.7(6) . . ?
B2 O10 Pb2 112.8(6) . 5_775 ?
Pb2 O10 Pb2 109.8(2) . 5_775 ?
B4 O11 Pb2 105.5(5) . 7_665 ?
B4 O11 Pb1 153.1(5) . 7_665 ?
Pb2 O11 Pb1 96.6(2) 7_665 7_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.604
_refine_diff_density_min         -3.609
_refine_diff_density_rms         0.700
