# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_whp

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B6 F2 O11 Pb3'
_chemical_formula_weight         900.43

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'
F F 0.0171 0.0103 '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           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.4274(13)
_cell_length_b                   8.3282(17)
_cell_length_c                   9.4891(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.19(3)
_cell_angle_gamma                90.00
_cell_volume                     498.28(17)
_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       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    50.655
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2032
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         20.00
_reflns_number_total             915
_reflns_number_gt                900
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0282(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_number_reflns         915
_refine_ls_number_parameters     105
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          2.347
_refine_ls_shift/su_mean         0.058

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 -0.02133(13) 0.3560(2) 0.27323(11) 0.0074(5) Uani 1 1 d . . .
Pb2 Pb 0.46270(16) 0.68140(11) 0.45339(11) 0.0084(5) Uani 1 1 d . . .
Pb3 Pb 0.54782(15) 0.70226(12) 0.02756(12) 0.0080(6) Uani 1 1 d . . .
F1 F -0.130(2) 0.558(2) 0.4266(17) 0.021(4) Uiso 1 1 d . . .
F2 F 0.616(2) 0.429(2) 0.1211(18) 0.023(5) Uiso 1 1 d . . .
O1 O -0.069(2) 0.312(3) 0.5393(19) 0.009(5) Uiso 1 1 d . . .
O2 O 1.091(2) 0.546(2) 0.6593(18) 0.000(5) Uiso 1 1 d . . .
O3 O 0.333(2) 0.393(2) 0.4046(18) 0.000(4) Uiso 1 1 d . . .
O4 O 0.811(3) 0.579(2) -0.1244(18) 0.003(4) Uiso 1 1 d . . .
O5 O 0.016(2) 0.645(3) 0.2386(17) 0.005(6) Uiso 1 1 d . . .
O6 O 0.153(2) 0.623(2) 0.0260(19) 0.007(5) Uiso 1 1 d . . .
O7 O 0.710(2) 0.508(2) 0.6272(16) 0.000(4) Uiso 1 1 d . . .
O8 O 0.054(2) 0.361(3) -0.0607(18) 0.005(4) Uiso 1 1 d . . .
O9 O 0.454(2) 0.540(2) 0.7715(15) 0.000(4) Uiso 1 1 d . . .
O10 O 0.724(3) 0.798(3) 0.307(2) 0.010(5) Uiso 1 1 d . . .
O11 O 0.693(3) 0.319(3) 0.8068(19) 0.009(5) Uiso 1 1 d . . .
B1 B 0.012(5) 0.524(4) -0.057(3) 0.002(7) Uiso 1 1 d . . .
B2 B 0.889(5) 0.473(4) 0.564(3) 0.002(7) Uiso 1 1 d . . .
B3 B 0.076(5) 0.213(4) 0.644(3) 0.001(8) Uiso 1 1 d . . .
B4 B 0.272(5) 0.463(4) 0.705(3) 0.000(8) Uiso 1 1 d . . .
B5 B 0.669(5) 0.483(4) 0.759(3) 0.000(8) Uiso 1 1 d . . .
B6 B 0.107(5) 0.745(5) 0.131(3) 0.000(7) Uiso 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
Pb1 0.0069(7) 0.0081(10) 0.0066(8) -0.0022(7) -0.0003(5) -0.0003(6)
Pb2 0.0055(8) 0.0086(11) 0.0106(9) 0.0033(6) 0.0002(6) -0.0020(5)
Pb3 0.0048(8) 0.0112(12) 0.0078(8) -0.0011(6) 0.0008(5) 0.0010(5)

_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 O3 2.395(15) . ?
Pb1 F1 2.416(18) . ?
Pb1 O5 2.45(3) . ?
Pb1 F2 2.566(14) 1_455 ?
Pb1 O1 2.627(19) . ?
Pb1 O2 2.721(18) 2_646 ?
Pb2 O3 2.438(17) 2_656 ?
Pb2 O7 2.515(15) . ?
Pb2 O3 2.558(19) . ?
Pb2 O10 2.57(2) . ?
Pb2 O11 2.730(18) 2_656 ?
Pb3 F2 2.454(18) . ?
Pb3 F2 2.464(17) 2_655 ?
Pb3 O11 2.597(19) 2_656 ?
Pb3 O6 2.620(17) . ?
Pb3 O4 2.63(2) . ?
Pb3 O9 2.744(16) 1_554 ?
F1 B2 1.47(4) 1_455 ?
F1 B3 1.52(4) 2_556 ?
F2 Pb3 2.464(17) 2_645 ?
F2 Pb1 2.566(14) 1_655 ?
O1 B2 1.40(4) 1_455 ?
O1 B3 1.48(4) . ?
O2 B4 1.35(3) 1_655 ?
O2 B2 1.55(3) . ?
O2 Pb1 2.721(18) 2_656 ?
O3 Pb2 2.438(17) 2_646 ?
O4 B1 1.41(3) 1_655 ?
O4 B5 1.52(3) 1_554 ?
O5 B3 1.47(4) 2_556 ?
O5 B6 1.52(4) . ?
O6 B1 1.36(4) . ?
O6 B6 1.49(4) . ?
O7 B5 1.34(4) . ?
O7 B2 1.43(4) . ?
O8 B1 1.38(4) . ?
O8 B6 1.48(4) 2_545 ?
O9 B4 1.38(3) . ?
O9 B5 1.49(3) . ?
O9 Pb3 2.744(16) 1_556 ?
O10 B4 1.38(4) 2_656 ?
O10 B3 1.46(4) 2_656 ?
O11 B5 1.44(4) . ?
O11 B6 1.45(4) 2_646 ?
O11 Pb3 2.597(19) 2_646 ?
O11 Pb2 2.730(18) 2_646 ?
B1 O4 1.41(3) 1_455 ?
B2 O1 1.40(4) 1_655 ?
B2 F1 1.47(4) 1_655 ?
B3 O10 1.46(4) 2_646 ?
B3 O5 1.47(4) 2_546 ?
B3 F1 1.52(4) 2_546 ?
B4 O2 1.35(3) 1_455 ?
B4 O10 1.38(4) 2_646 ?
B5 O4 1.52(3) 1_556 ?
B6 O11 1.45(4) 2_656 ?
B6 O8 1.48(4) 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
O3 Pb1 F1 87.4(6) . . ?
O3 Pb1 O5 80.6(5) . . ?
F1 Pb1 O5 56.1(6) . . ?
O3 Pb1 F2 158.8(7) . 1_455 ?
F1 Pb1 F2 80.6(5) . 1_455 ?
O5 Pb1 F2 78.1(5) . 1_455 ?
O3 Pb1 O1 78.1(5) . . ?
F1 Pb1 O1 54.4(6) . . ?
O5 Pb1 O1 107.4(6) . . ?
F2 Pb1 O1 108.2(5) 1_455 . ?
O3 Pb1 O2 100.5(5) . 2_646 ?
F1 Pb1 O2 116.1(6) . 2_646 ?
O5 Pb1 O2 172.2(6) . 2_646 ?
F2 Pb1 O2 100.5(5) 1_455 2_646 ?
O1 Pb1 O2 65.5(6) . 2_646 ?
O3 Pb2 O7 81.3(5) 2_656 . ?
O3 Pb2 O3 154.1(4) 2_656 . ?
O7 Pb2 O3 73.7(5) . . ?
O3 Pb2 O10 71.9(6) 2_656 . ?
O7 Pb2 O10 100.1(5) . . ?
O3 Pb2 O10 118.8(6) . . ?
O3 Pb2 O11 105.1(6) 2_656 2_656 ?
O7 Pb2 O11 155.3(6) . 2_656 ?
O3 Pb2 O11 100.5(6) . 2_656 ?
O10 Pb2 O11 60.9(6) . 2_656 ?
F2 Pb3 F2 160.7(4) . 2_655 ?
F2 Pb3 O11 102.4(6) . 2_656 ?
F2 Pb3 O11 79.7(6) 2_655 2_656 ?
F2 Pb3 O6 82.7(5) . . ?
F2 Pb3 O6 83.3(5) 2_655 . ?
O11 Pb3 O6 53.7(6) 2_656 . ?
F2 Pb3 O4 75.5(6) . . ?
F2 Pb3 O4 103.4(6) 2_655 . ?
O11 Pb3 O4 176.1(5) 2_656 . ?
O6 Pb3 O4 128.6(5) . . ?
F2 Pb3 O9 81.7(5) . 1_554 ?
F2 Pb3 O9 82.8(5) 2_655 1_554 ?
O11 Pb3 O9 131.8(5) 2_656 1_554 ?
O6 Pb3 O9 79.9(5) . 1_554 ?
O4 Pb3 O9 51.5(4) . 1_554 ?
B2 F1 B3 144(2) 1_455 2_556 ?
B2 F1 Pb1 102.5(16) 1_455 . ?
B3 F1 Pb1 101.9(15) 2_556 . ?
Pb3 F2 Pb3 118.5(6) . 2_645 ?
Pb3 F2 Pb1 120.0(7) . 1_655 ?
Pb3 F2 Pb1 112.5(7) 2_645 1_655 ?
B2 O1 B3 123(2) 1_455 . ?
B2 O1 Pb1 95.1(16) 1_455 . ?
B3 O1 Pb1 123.3(17) . . ?
B4 O2 B2 124(2) 1_655 . ?
B4 O2 Pb1 125.5(16) 1_655 2_656 ?
B2 O2 Pb1 110.4(15) . 2_656 ?
Pb1 O3 Pb2 123.5(8) . 2_646 ?
Pb1 O3 Pb2 117.2(7) . . ?
Pb2 O3 Pb2 117.2(6) 2_646 . ?
B1 O4 B5 122(2) 1_655 1_554 ?
B1 O4 Pb3 120.7(17) 1_655 . ?
B5 O4 Pb3 104.3(13) 1_554 . ?
B3 O5 B6 124(3) 2_556 . ?
B3 O5 Pb1 102.0(19) 2_556 . ?
B6 O5 Pb1 133.5(19) . . ?
B1 O6 B6 127(2) . . ?
B1 O6 Pb3 134(2) . . ?
B6 O6 Pb3 98.2(14) . . ?
B5 O7 B2 133(2) . . ?
B5 O7 Pb2 119.1(17) . . ?
B2 O7 Pb2 107.4(14) . . ?
B1 O8 B6 122(2) . 2_545 ?
B4 O9 B5 122(2) . . ?
B4 O9 Pb3 131.1(17) . 1_556 ?
B5 O9 Pb3 100.4(11) . 1_556 ?
B4 O10 B3 119(2) 2_656 2_656 ?
B4 O10 Pb2 116(2) 2_656 . ?
B3 O10 Pb2 105.6(17) 2_656 . ?
B5 O11 B6 124(2) . 2_646 ?
B5 O11 Pb3 120.7(16) . 2_646 ?
B6 O11 Pb3 100.4(17) 2_646 2_646 ?
B5 O11 Pb2 96.6(14) . 2_646 ?
B6 O11 Pb2 109.2(17) 2_646 2_646 ?
Pb3 O11 Pb2 103.5(6) 2_646 2_646 ?
O6 B1 O8 120(2) . . ?
O6 B1 O4 121(3) . 1_455 ?
O8 B1 O4 118(3) . 1_455 ?
O1 B2 O7 117(2) 1_655 . ?
O1 B2 F1 107(2) 1_655 1_655 ?
O7 B2 F1 110(2) . 1_655 ?
O1 B2 O2 108(2) 1_655 . ?
O7 B2 O2 109(2) . . ?
F1 B2 O2 104(2) 1_655 . ?
O10 B3 O5 114(2) 2_646 2_546 ?
O10 B3 O1 110(3) 2_646 . ?
O5 B3 O1 115(2) 2_546 . ?
O10 B3 F1 107(2) 2_646 2_546 ?
O5 B3 F1 100(2) 2_546 2_546 ?
O1 B3 F1 110(2) . 2_546 ?
O2 B4 O9 121(3) 1_455 . ?
O2 B4 O10 121(2) 1_455 2_646 ?
O9 B4 O10 118(3) . 2_646 ?
O7 B5 O11 114(3) . . ?
O7 B5 O9 112(2) . . ?
O11 B5 O9 109(2) . . ?
O7 B5 O4 114(2) . 1_556 ?
O11 B5 O4 105.1(19) . 1_556 ?
O9 B5 O4 102(2) . 1_556 ?
O11 B6 O8 113(3) 2_656 2 ?
O11 B6 O6 107(2) 2_656 . ?
O8 B6 O6 111(2) 2 . ?
O11 B6 O5 113(2) 2_656 . ?
O8 B6 O5 110(2) 2 . ?
O6 B6 O5 103(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        20.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.503
_refine_diff_density_min         -2.135
_refine_diff_density_rms         0.534
_database_code_depnum_ccdc_archive 'CCDC 965533'