# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1501321'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-11-06 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 Bi2 Ga O11 Pb2'
_chemical_formula_weight         1110.49

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'
Ga Ga 0.2307 1.6083 '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'
Bi Bi -4.1077 10.2566 '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                   17.318(5)
_cell_length_b                   8.868(3)
_cell_length_c                   6.779(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.238(4)
_cell_angle_gamma                90.00
_cell_volume                     1041.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1070
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.10

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    7.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    68.539
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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            3148
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         27.54
_reflns_number_total             1207
_reflns_number_gt                1042
_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)+(0.0636P)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       0.00136(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1207
_refine_ls_number_parameters     90
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.168
_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
Bi1 Bi 0.43383(3) 0.29934(7) -0.00681(9) 0.0129(3) Uani 1 1 d . . .
Pb1 Pb 0.15756(3) 0.59263(7) 0.05990(10) 0.0165(3) Uani 1 1 d . . .
Ga1 Ga 0.2500 0.2500 0.0000 0.0092(5) Uani 1 2 d S . .
B1 B 0.0000 0.517(2) 0.2500 0.005(4) Uani 1 2 d SU . .
B2 B 0.3249(9) 0.5078(19) 0.239(3) 0.008(3) Uani 1 1 d . . .
O1 O 0.0644(7) 0.4390(13) 0.1941(18) 0.018(3) Uani 1 1 d U . .
O2 O 0.1798(7) 0.1524(12) 0.1876(17) 0.013(2) Uani 1 1 d . . .
O3 O 0.2587(7) 0.4369(13) 0.1777(18) 0.015(2) Uani 1 1 d U . .
O4 O 0.3966(7) 0.4466(13) 0.2323(19) 0.021(3) Uani 1 1 d U . .
O5 O 0.5000 0.171(2) 0.2500 0.030(5) Uani 1 2 d S . .
O6 O 0.3419(6) 0.1552(12) 0.0995(16) 0.009(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Bi1 0.0094(4) 0.0151(4) 0.0143(4) -0.0009(2) 0.0004(2) 0.0028(2)
Pb1 0.0103(4) 0.0212(4) 0.0181(4) 0.0035(2) -0.0010(3) -0.0009(2)
Ga1 0.0043(11) 0.0099(11) 0.0133(13) 0.0019(9) 0.0007(9) 0.0013(9)
B1 0.005(4) 0.005(4) 0.005(4) 0.000 -0.0001(10) 0.000
B2 0.003(7) 0.011(8) 0.011(8) -0.007(7) 0.001(6) -0.001(6)
O1 0.018(3) 0.018(3) 0.018(3) -0.0001(10) 0.0003(10) -0.0002(10)
O2 0.013(6) 0.013(5) 0.014(6) 0.002(5) 0.004(4) 0.000(4)
O3 0.015(3) 0.015(3) 0.015(3) -0.0005(10) -0.0004(10) 0.0003(10)
O4 0.020(3) 0.021(3) 0.021(3) -0.0006(10) -0.0003(10) 0.0002(10)
O5 0.033(12) 0.023(10) 0.035(12) 0.000 -0.016(9) 0.000
O6 0.006(5) 0.013(5) 0.009(6) 0.001(4) 0.004(4) -0.001(4)

_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
Bi1 O6 2.167(10) . ?
Bi1 O4 2.181(13) . ?
Bi1 O2 2.354(12) 7 ?
Bi1 O5 2.370(9) . ?
Bi1 O1 2.466(12) 7 ?
Pb1 O1 2.302(12) . ?
Pb1 O3 2.367(12) . ?
Pb1 O6 2.375(11) 4 ?
Pb1 O6 2.449(10) 7 ?
Ga1 O6 1.920(11) . ?
Ga1 O6 1.920(11) 7 ?
Ga1 O2 1.964(11) . ?
Ga1 O2 1.964(11) 7 ?
Ga1 O3 2.054(12) 7 ?
Ga1 O3 2.054(12) . ?
Ga1 Bi1 3.2140(11) 7 ?
B1 O1 1.368(16) 2 ?
B1 O1 1.368(16) . ?
B1 O5 1.37(3) 3_455 ?
B2 O4 1.36(2) . ?
B2 O3 1.370(19) . ?
B2 O2 1.379(19) 4 ?
O1 Bi1 2.466(12) 7 ?
O2 B2 1.379(19) 4_545 ?
O2 Bi1 2.354(12) 7 ?
O5 B1 1.37(3) 3_545 ?
O5 Bi1 2.370(9) 2_655 ?
O6 Pb1 2.375(11) 4_545 ?
O6 Pb1 2.449(10) 7 ?

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
O6 Bi1 O4 83.5(4) . . ?
O6 Bi1 O2 70.5(4) . 7 ?
O4 Bi1 O2 91.7(4) . 7 ?
O6 Bi1 O5 80.0(4) . . ?
O4 Bi1 O5 83.4(4) . . ?
O2 Bi1 O5 150.5(3) 7 . ?
O6 Bi1 O1 71.1(4) . 7 ?
O4 Bi1 O1 154.2(4) . 7 ?
O2 Bi1 O1 84.2(4) 7 7 ?
O5 Bi1 O1 87.8(5) . 7 ?
O1 Pb1 O3 92.3(4) . . ?
O1 Pb1 O6 75.8(4) . 4 ?
O3 Pb1 O6 79.0(4) . 4 ?
O1 Pb1 O6 69.3(4) . 7 ?
O3 Pb1 O6 67.7(4) . 7 ?
O6 Pb1 O6 129.7(3) 4 7 ?
O6 Ga1 O6 180.0(3) . 7 ?
O6 Ga1 O2 95.4(5) . . ?
O6 Ga1 O2 84.6(5) 7 . ?
O6 Ga1 O2 84.6(5) . 7 ?
O6 Ga1 O2 95.4(5) 7 7 ?
O2 Ga1 O2 180.0(8) . 7 ?
O6 Ga1 O3 84.9(5) . 7 ?
O6 Ga1 O3 95.1(5) 7 7 ?
O2 Ga1 O3 88.9(5) . 7 ?
O2 Ga1 O3 91.1(5) 7 7 ?
O6 Ga1 O3 95.1(5) . . ?
O6 Ga1 O3 84.9(5) 7 . ?
O2 Ga1 O3 91.1(5) . . ?
O2 Ga1 O3 88.9(5) 7 . ?
O3 Ga1 O3 180.0(7) 7 . ?
O6 Ga1 Bi1 139.0(3) . 7 ?
O6 Ga1 Bi1 41.0(3) 7 7 ?
O2 Ga1 Bi1 46.8(3) . 7 ?
O2 Ga1 Bi1 133.2(3) 7 7 ?
O3 Ga1 Bi1 80.1(3) 7 7 ?
O3 Ga1 Bi1 99.9(3) . 7 ?
O1 B1 O1 119.2(19) 2 . ?
O1 B1 O5 120.4(9) 2 3_455 ?
O1 B1 O5 120.4(9) . 3_455 ?
O4 B2 O3 124.9(14) . . ?
O4 B2 O2 116.1(13) . 4 ?
O3 B2 O2 119.0(13) . 4 ?
B1 O1 Pb1 112.6(10) . . ?
B1 O1 Bi1 126.0(10) . 7 ?
Pb1 O1 Bi1 107.1(5) . 7 ?
B2 O2 Ga1 133.1(10) 4_545 . ?
B2 O2 Bi1 107.8(9) 4_545 7 ?
Ga1 O2 Bi1 95.8(5) . 7 ?
B2 O3 Ga1 127.3(10) . . ?
B2 O3 Pb1 116.8(9) . . ?
Ga1 O3 Pb1 102.7(5) . . ?
B2 O4 Bi1 122.5(10) . . ?
B1 O5 Bi1 118.6(4) 3_545 2_655 ?
B1 O5 Bi1 118.6(4) 3_545 . ?
Bi1 O5 Bi1 122.8(8) 2_655 . ?
Ga1 O6 Bi1 103.5(5) . . ?
Ga1 O6 Pb1 116.3(5) . 4_545 ?
Bi1 O6 Pb1 117.5(5) . 4_545 ?
Ga1 O6 Pb1 104.0(4) . 7 ?
Bi1 O6 Pb1 112.2(4) . 7 ?
Pb1 O6 Pb1 102.7(4) 4_545 7 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         4.659
_refine_diff_density_min         -5.432
_refine_diff_density_rms         2.519
