# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_111
_database_code_depnum_ccdc_archive 'CCDC 1834067'
_audit_update_record             
;
2018-04-02 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B5 F O8 Pb'
_chemical_formula_weight         408.24

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'
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           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

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

_cell_length_a                   10.885(3)
_cell_length_b                   9.108(2)
_cell_length_c                   13.576(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1345.9(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2204
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.029
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    25.110
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.1167
_exptl_absorpt_correction_T_max  0.2109
_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            7621
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.53
_reflns_number_total             1550
_reflns_number_gt                1259
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0183P)²+1.9478P] 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       0.00022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1550
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0481
_refine_ls_wR_factor_gt          0.0444
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.038395(18) 0.67997(2) 0.885215(17) 0.01515(9) Uani 1 1 d . . .
B1 B -0.2714(6) 0.7906(6) 0.9062(5) 0.0115(13) Uani 1 1 d . . .
B2 B -0.0092(6) 0.3457(6) 0.8678(5) 0.0094(12) Uani 1 1 d . . .
B3 B 0.3025(5) 0.8739(6) 0.9575(5) 0.0090(12) Uani 1 1 d . . .
B4 B 0.3302(5) 0.6975(6) 0.8212(5) 0.0098(12) Uani 1 1 d . . .
B5 B -0.3149(5) 0.9729(6) 0.7871(5) 0.0106(12) Uani 1 1 d . . .
O1 O 0.0488(3) 0.2256(4) 0.8129(3) 0.0110(8) Uani 1 1 d . . .
O2 O 0.2535(3) 0.7755(4) 0.8804(3) 0.0115(8) Uani 1 1 d . . .
O3 O -0.1836(3) 0.7065(4) 0.9497(3) 0.0124(8) Uani 1 1 d . . .
O4 O 0.0775(3) 0.4269(4) 0.9283(3) 0.0109(8) Uani 1 1 d . . .
O5 O -0.2321(3) 0.8820(4) 0.8307(3) 0.0114(8) Uani 1 1 d . . .
O6 O -0.1074(3) 0.2843(4) 0.9323(3) 0.0116(8) Uani 1 1 d . . .
O7 O 0.2692(3) 0.5896(3) 0.7668(3) 0.0103(8) Uani 1 1 d . . .
O8 O -0.0632(3) 0.4532(4) 0.7986(3) 0.0124(8) Uani 1 1 d . . .
F1 F 0.2212(3) 0.9904(3) 0.9688(2) 0.0149(7) 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
Pb1 0.01136(12) 0.01454(12) 0.01954(14) 0.00097(9) -0.00049(9) -0.00188(8)
B1 0.011(3) 0.012(3) 0.011(4) 0.000(2) 0.000(2) -0.002(2)
B2 0.011(3) 0.011(3) 0.006(3) -0.001(2) 0.002(2) 0.004(2)
B3 0.008(3) 0.011(3) 0.009(3) 0.000(2) 0.003(2) 0.000(2)
B4 0.011(3) 0.007(3) 0.012(3) 0.003(2) 0.000(2) -0.002(2)
B5 0.011(3) 0.013(3) 0.008(3) -0.002(3) 0.003(2) -0.001(2)
O1 0.0082(18) 0.0144(17) 0.010(2) -0.0045(15) -0.0017(15) 0.0008(14)
O2 0.0087(19) 0.0137(17) 0.012(2) -0.0037(16) 0.0002(15) -0.0032(14)
O3 0.0079(18) 0.0187(19) 0.011(2) 0.0020(16) 0.0017(15) 0.0037(14)
O4 0.0080(18) 0.0118(18) 0.013(2) -0.0023(16) -0.0047(15) 0.0051(14)
O5 0.0086(18) 0.0137(16) 0.012(2) 0.0035(16) 0.0019(15) 0.0034(14)
O6 0.0087(18) 0.0129(17) 0.013(2) 0.0067(15) 0.0028(16) -0.0001(14)
O7 0.0065(18) 0.0088(17) 0.016(2) -0.0034(15) 0.0024(15) -0.0018(14)
O8 0.0075(18) 0.0147(17) 0.015(2) 0.0076(17) 0.0009(15) -0.0007(14)
F1 0.0156(16) 0.0093(14) 0.020(2) 0.0004(13) 0.0012(14) 0.0056(12)

_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 O4 2.416(3) . ?
Pb1 O2 2.499(4) . ?
Pb1 O3 2.581(4) . ?
Pb1 O6 2.610(4) 5_567 ?
Pb1 O8 2.622(4) . ?
B1 O3 1.359(7) . ?
B1 O6 1.366(7) 8_565 ?
B1 O5 1.389(7) . ?
B2 O4 1.454(7) . ?
B2 O1 1.467(7) . ?
B2 O8 1.478(7) . ?
B2 O6 1.491(7) . ?
B3 F1 1.390(6) . ?
B3 O4 1.448(7) 8_665 ?
B3 O3 1.465(7) 4_567 ?
B3 O2 1.478(7) . ?
B4 O1 1.346(6) 8_665 ?
B4 O2 1.360(7) . ?
B4 O7 1.397(7) . ?
B5 O8 1.348(7) 8_565 ?
B5 O5 1.359(7) . ?
B5 O7 1.382(7) 3_556 ?
O1 B4 1.346(6) 8_655 ?
O3 B3 1.465(7) 4_467 ?
O4 B3 1.448(7) 8_655 ?
O6 B1 1.366(7) 8 ?
O6 Pb1 2.610(4) 5_567 ?
O7 B5 1.382(7) 3_546 ?
O8 B5 1.348(7) 8 ?

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
O4 Pb1 O2 99.98(12) . . ?
O4 Pb1 O3 99.92(12) . . ?
O2 Pb1 O3 148.60(12) . . ?
O4 Pb1 O6 80.70(12) . 5_567 ?
O2 Pb1 O6 73.25(12) . 5_567 ?
O3 Pb1 O6 86.33(12) . 5_567 ?
O4 Pb1 O8 55.34(12) . . ?
O2 Pb1 O8 131.13(11) . . ?
O3 Pb1 O8 80.27(11) . . ?
O6 Pb1 O8 130.22(11) 5_567 . ?
O3 B1 O6 122.9(5) . 8_565 ?
O3 B1 O5 116.2(5) . . ?
O6 B1 O5 120.9(5) 8_565 . ?
O4 B2 O1 112.7(4) . . ?
O4 B2 O8 106.3(4) . . ?
O1 B2 O8 110.0(4) . . ?
O4 B2 O6 108.9(5) . . ?
O1 B2 O6 109.1(4) . . ?
O8 B2 O6 109.7(4) . . ?
F1 B3 O4 110.5(4) . 8_665 ?
F1 B3 O3 110.6(4) . 4_567 ?
O4 B3 O3 108.0(4) 8_665 4_567 ?
F1 B3 O2 108.2(4) . . ?
O4 B3 O2 109.5(4) 8_665 . ?
O3 B3 O2 110.1(4) 4_567 . ?
O1 B4 O2 123.4(5) 8_665 . ?
O1 B4 O7 123.7(5) 8_665 . ?
O2 B4 O7 112.8(5) . . ?
O8 B5 O5 121.4(5) 8_565 . ?
O8 B5 O7 121.2(5) 8_565 3_556 ?
O5 B5 O7 117.4(5) . 3_556 ?
B4 O1 B2 121.4(4) 8_655 . ?
B4 O2 B3 121.0(4) . . ?
B4 O2 Pb1 114.1(3) . . ?
B3 O2 Pb1 122.0(3) . . ?
B1 O3 B3 125.6(4) . 4_467 ?
B1 O3 Pb1 124.3(3) . . ?
B3 O3 Pb1 110.0(3) 4_467 . ?
B3 O4 B2 124.8(4) 8_655 . ?
B3 O4 Pb1 122.9(3) 8_655 . ?
B2 O4 Pb1 103.5(3) . . ?
B5 O5 B1 118.8(4) . . ?
B1 O6 B2 121.6(5) 8 . ?
B1 O6 Pb1 121.2(4) 8 5_567 ?
B2 O6 Pb1 107.7(3) . 5_567 ?
B5 O7 B4 130.5(4) 3_546 . ?
B5 O8 B2 123.6(4) 8 . ?
B5 O8 Pb1 111.2(3) 8 . ?
B2 O8 Pb1 94.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.196
