# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_pboi_cs_fulldata_0m
_database_code_depnum_ccdc_archive 'CCDC 1920738'
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B3 I3 O13 Pb10'
_chemical_formula_weight         2693.03

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'
I I -0.4742 1.8119 '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   Cc
_symmetry_space_group_name_Hall  C_-2yc
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'

_cell_length_a                   16.6423(5)
_cell_length_b                   9.0277(3)
_cell_length_c                   16.9746(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.6580(10)
_cell_angle_gamma                90.00
_cell_volume                     2298.82(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4723
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      27.50

_exptl_crystal_description       strip
_exptl_crystal_colour            transparent
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.027
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    7.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4392
_exptl_absorpt_coefficient_mu    77.019
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.4471
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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            16455
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5081
_reflns_number_gt                4898
_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)+(0.0199P)²+6.7846P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   no
_refine_ls_hydrogen_treatment    no
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000035(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.368(8)
_refine_ls_number_reflns         5081
_refine_ls_number_parameters     264
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0559
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.034
_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 0.67144(4) 0.46922(7) 0.21917(4) 0.00767(13) Uani 1 1 d . . .
Pb2 Pb 0.78417(4) 1.03954(7) 0.31703(4) 0.00630(12) Uani 1 1 d . . .
Pb3 Pb 1.11503(4) 1.53201(6) 0.42790(4) 0.00743(12) Uani 1 1 d . . .
Pb4 Pb 1.00242(4) 0.96812(6) 0.32757(4) 0.00604(12) Uani 1 1 d . . .
Pb5 Pb 0.98940(4) 1.25341(6) 0.48961(3) 0.00658(12) Uani 1 1 d . . .
Pb6 Pb 0.80285(4) 0.74744(6) 0.16053(3) 0.00642(12) Uani 1 1 d . . .
Pb7 Pb 0.91581(4) 1.35162(7) 0.26664(4) 0.00663(12) Uani 1 1 d . . .
Pb8 Pb 0.87645(4) 0.66332(6) 0.39126(4) 0.00613(12) Uani 1 1 d . . .
Pb9 Pb 0.55866(4) 0.82159(7) 0.12217(4) 0.00848(13) Uani 1 1 d . . .
Pb10 Pb 1.24027(4) 1.16085(7) 0.53401(4) 0.00852(13) Uani 1 1 d . . .
I1 I 0.77129(8) 0.64946(12) 0.93229(7) 0.0101(2) Uani 1 1 d . . .
I2 I 0.02001(7) 0.35270(12) 0.71465(7) 0.0101(2) Uani 1 1 d . . .
I3 I 0.89824(9) 0.95681(8) 0.57940(10) 0.01140(15) Uani 1 1 d . . .
B1 B 0.6449(13) 0.750(2) 0.3330(11) 0.005(2) Uani 1 1 d U . .
B2 B 0.6982(12) 1.090(2) 0.1311(11) 0.007(3) Uani 1 1 d U . .
B3 B 0.5919(14) 0.587(2) 0.0082(14) 0.019(4) Uani 1 1 d U . .
O1 O 0.9185(7) 1.1492(12) 0.3568(7) 0.006(2) Uani 1 1 d U . .
O2 O 0.8675(8) 0.8560(13) 0.2920(8) 0.010(2) Uani 1 1 d U . .
O3 O 1.0386(7) 0.8167(13) 0.4489(7) 0.007(2) Uani 1 1 d U . .
O4 O 0.7480(9) 1.1815(15) 0.1971(9) 0.017(3) Uani 1 1 d U . .
O5 O 1.1002(7) 1.0587(13) 0.4866(7) 0.010(2) Uani 1 1 d . . .
O6 O 1.1571(7) 1.3585(12) 0.5434(7) 0.004(2) Uani 1 1 d U . .
O7 O 0.8069(7) 0.5531(12) 0.2575(7) 0.007(2) Uani 1 1 d U . .
O8 O 0.9768(6) 1.4646(11) 0.4039(7) 0.007(2) Uani 1 1 d U . .
O9 O 0.6363(8) 0.6301(13) 0.0950(8) 0.012(2) Uani 1 1 d . . .
O10 O 0.6895(8) 0.9423(13) 0.1471(8) 0.010(2) Uani 1 1 d U . .
O11 O 0.6374(6) 0.7081(11) 0.2505(7) 0.012(2) Uani 1 1 d U . .
O12 O 0.5794(7) 0.8238(12) 0.3406(8) 0.017(2) Uani 1 1 d . . .
O13 O 0.7252(6) 0.7259(11) 0.4034(6) 0.0110(19) 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 O7 2.193(10) . ?
Pb1 O11 2.349(10) . ?
Pb1 O9 2.413(12) . ?
Pb2 O4 2.255(14) . ?
Pb2 O1 2.264(11) . ?
Pb2 O2 2.316(12) . ?
Pb3 O8 2.240(10) . ?
Pb3 O12 2.307(11) 3 ?
Pb3 O6 2.366(11) . ?
Pb3 I2 3.4248(12) 2_674 ?
Pb4 O2 2.292(12) . ?
Pb4 O3 2.324(11) . ?
Pb4 O1 2.339(11) . ?
Pb4 O5 2.608(11) . ?
Pb4 B3 2.81(2) 4_565 ?
Pb5 O1 2.249(11) . ?
Pb5 O8 2.352(10) . ?
Pb5 O5 2.563(11) . ?
Pb5 O6 2.705(11) . ?
Pb6 O2 2.240(12) . ?
Pb6 O7 2.387(10) . ?
Pb6 O10 2.516(12) . ?
Pb6 O9 2.716(13) . ?
Pb7 O8 2.335(10) . ?
Pb7 O1 2.371(11) . ?
Pb7 O12 2.469(10) 3 ?
Pb7 O7 2.525(10) 1_565 ?
Pb8 O7 2.282(10) . ?
Pb8 O2 2.381(12) . ?
Pb8 O8 2.397(10) 1_545 ?
Pb8 O13 2.674(10) . ?
Pb9 O11 2.245(10) . ?
Pb9 O10 2.305(12) . ?
Pb9 O9 2.321(11) . ?
Pb10 O13 2.200(10) 3 ?
Pb10 O5 2.304(12) . ?
Pb10 O6 2.306(11) . ?
I2 Pb3 3.4248(13) 2_475 ?
B1 O12 1.33(2) . ?
B1 O13 1.37(2) . ?
B1 O11 1.40(2) . ?
B2 O4 1.35(2) . ?
B2 O10 1.38(2) . ?
B2 O6 1.42(2) 4_474 ?
B3 O3 1.34(2) 4_464 ?
B3 O5 1.39(2) 4_464 ?
B3 O9 1.39(2) . ?
B3 Pb4 2.81(2) 4_464 ?
O3 B3 1.34(2) 4_565 ?
O5 B3 1.39(2) 4_565 ?
O6 B2 1.42(2) 4_575 ?
O7 Pb7 2.525(10) 1_545 ?
O8 Pb8 2.397(10) 1_565 ?
O12 Pb3 2.307(11) 3_445 ?
O12 Pb7 2.469(10) 3_445 ?
O13 Pb10 2.200(10) 3_445 ?

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
O7 Pb1 O11 86.2(4) . . ?
O7 Pb1 O9 83.2(4) . . ?
O11 Pb1 O9 69.8(4) . . ?
O4 Pb2 O1 82.2(4) . . ?
O4 Pb2 O2 100.8(5) . . ?
O1 Pb2 O2 77.0(4) . . ?
O8 Pb3 O12 72.8(4) . 3 ?
O8 Pb3 O6 83.3(4) . . ?
O12 Pb3 O6 84.0(4) 3 . ?
O8 Pb3 I2 85.6(3) . 2_674 ?
O12 Pb3 I2 72.3(3) 3 2_674 ?
O6 Pb3 I2 155.9(3) . 2_674 ?
O2 Pb4 O3 79.7(4) . . ?
O2 Pb4 O1 76.0(4) . . ?
O3 Pb4 O1 99.9(4) . . ?
O2 Pb4 O5 120.8(4) . . ?
O3 Pb4 O5 57.4(4) . . ?
O1 Pb4 O5 73.9(4) . . ?
O2 Pb4 B3 101.9(6) . 4_565 ?
O3 Pb4 B3 28.2(5) . 4_565 ?
O1 Pb4 B3 88.6(5) . 4_565 ?
O5 Pb4 B3 29.3(5) . 4_565 ?
O1 Pb5 O8 81.4(4) . . ?
O1 Pb5 O5 76.3(4) . . ?
O8 Pb5 O5 114.6(4) . . ?
O1 Pb5 O6 120.1(4) . . ?
O8 Pb5 O6 74.2(3) . . ?
O5 Pb5 O6 66.5(4) . . ?
O2 Pb6 O7 77.1(4) . . ?
O2 Pb6 O10 78.6(4) . . ?
O7 Pb6 O10 111.9(4) . . ?
O2 Pb6 O9 122.9(4) . . ?
O7 Pb6 O9 73.4(3) . . ?
O10 Pb6 O9 69.1(4) . . ?
O8 Pb7 O1 79.3(4) . . ?
O8 Pb7 O12 68.3(4) . 3 ?
O1 Pb7 O12 83.4(4) . 3 ?
O8 Pb7 O7 74.7(3) . 1_565 ?
O1 Pb7 O7 114.0(4) . 1_565 ?
O12 Pb7 O7 135.2(3) 3 1_565 ?
O7 Pb8 O2 76.4(4) . . ?
O7 Pb8 O8 78.2(3) . 1_545 ?
O2 Pb8 O8 115.9(4) . 1_545 ?
O7 Pb8 O13 94.6(3) . . ?
O2 Pb8 O13 97.4(4) . . ?
O8 Pb8 O13 142.6(3) 1_545 . ?
O11 Pb9 O10 86.0(4) . . ?
O11 Pb9 O9 73.2(4) . . ?
O10 Pb9 O9 80.0(4) . . ?
O13 Pb10 O5 95.6(4) 3 . ?
O13 Pb10 O6 93.1(4) 3 . ?
O5 Pb10 O6 77.7(4) . . ?
O12 B1 O13 121.7(15) . . ?
O12 B1 O11 120.6(15) . . ?
O13 B1 O11 117.3(15) . . ?
O4 B2 O10 120.3(15) . . ?
O4 B2 O6 121.2(15) . 4_474 ?
O10 B2 O6 118.4(14) . 4_474 ?
O3 B3 O5 121.9(17) 4_464 4_464 ?
O3 B3 O9 119.3(17) 4_464 . ?
O5 B3 O9 118.7(17) 4_464 . ?
O3 B3 Pb4 55.2(9) 4_464 4_464 ?
O5 B3 Pb4 67.1(9) 4_464 4_464 ?
O9 B3 Pb4 173.7(15) . 4_464 ?
Pb5 O1 Pb2 120.2(5) . . ?
Pb5 O1 Pb4 113.7(5) . . ?
Pb2 O1 Pb4 103.5(4) . . ?
Pb5 O1 Pb7 100.4(4) . . ?
Pb2 O1 Pb7 113.9(5) . . ?
Pb4 O1 Pb7 104.4(5) . . ?
Pb6 O2 Pb4 116.7(6) . . ?
Pb6 O2 Pb2 115.3(5) . . ?
Pb4 O2 Pb2 103.4(5) . . ?
Pb6 O2 Pb8 104.0(5) . . ?
Pb4 O2 Pb8 112.5(5) . . ?
Pb2 O2 Pb8 104.6(5) . . ?
B3 O3 Pb4 96.7(11) 4_565 . ?
B2 O4 Pb2 103.4(11) . . ?
B3 O5 Pb10 119.2(11) 4_565 . ?
B3 O5 Pb5 119.3(12) 4_565 . ?
Pb10 O5 Pb5 110.3(4) . . ?
B3 O5 Pb4 83.6(10) 4_565 . ?
Pb10 O5 Pb4 124.8(5) . . ?
Pb5 O5 Pb4 96.0(3) . . ?
B2 O6 Pb10 107.0(9) 4_575 . ?
B2 O6 Pb3 119.3(9) 4_575 . ?
Pb10 O6 Pb3 115.2(5) . . ?
B2 O6 Pb5 115.2(10) 4_575 . ?
Pb10 O6 Pb5 105.5(4) . . ?
Pb3 O6 Pb5 93.5(3) . . ?
Pb1 O7 Pb8 117.4(5) . . ?
Pb1 O7 Pb6 109.3(4) . . ?
Pb8 O7 Pb6 102.5(4) . . ?
Pb1 O7 Pb7 112.8(4) . 1_545 ?
Pb8 O7 Pb7 102.2(4) . 1_545 ?
Pb6 O7 Pb7 112.1(4) . 1_545 ?
Pb3 O8 Pb7 105.6(4) . . ?
Pb3 O8 Pb5 107.4(4) . . ?
Pb7 O8 Pb5 98.5(4) . . ?
Pb3 O8 Pb8 115.7(4) . 1_565 ?
Pb7 O8 Pb8 104.6(4) . 1_565 ?
Pb5 O8 Pb8 122.3(4) . 1_565 ?
B3 O9 Pb9 109.6(11) . . ?
B3 O9 Pb1 125.0(12) . . ?
Pb9 O9 Pb1 102.7(5) . . ?
B3 O9 Pb6 121.6(12) . . ?
Pb9 O9 Pb6 100.7(4) . . ?
Pb1 O9 Pb6 93.4(4) . . ?
B2 O10 Pb9 126.2(10) . . ?
B2 O10 Pb6 123.7(10) . . ?
Pb9 O10 Pb6 107.3(5) . . ?
B1 O11 Pb9 127.4(10) . . ?
B1 O11 Pb1 123.2(10) . . ?
Pb9 O11 Pb1 107.2(4) . . ?
B1 O12 Pb3 118.5(10) . 3_445 ?
B1 O12 Pb7 140.5(11) . 3_445 ?
Pb3 O12 Pb7 99.4(4) 3_445 3_445 ?
B1 O13 Pb10 124.3(10) . 3_445 ?
B1 O13 Pb8 124.2(10) . . ?
Pb10 O13 Pb8 108.7(4) 3_445 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.827
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.390
