# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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.
#
data_123

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B O8 P Pb4'
_chemical_formula_weight         998.54

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'
P P 0.1023 0.0942 '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   P2(1)/c

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

_cell_length_a                   10.202(2)
_cell_length_b                   7.0047(16)
_cell_length_c                   12.921(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.057(15)
_cell_angle_gamma                90.00
_cell_volume                     849.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2278
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      27.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    7.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    79.227
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.0230
_exptl_absorpt_correction_T_max  0.0345
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9130
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1500
_reflns_number_gt                1291
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0873P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1500
_refine_ls_number_parameters     127
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1258
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.052
_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 0.86999(9) 0.22743(11) 0.06858(7) 0.0133(3) Uani 1 1 d . . .
Pb2 Pb 0.45093(9) 0.19882(11) 0.07416(7) 0.0163(3) Uani 1 1 d . . .
Pb3 Pb 0.75925(10) -0.00917(10) 0.29334(7) 0.0158(3) Uani 1 1 d . . .
Pb4 Pb 0.76925(9) 0.49161(10) 0.26588(7) 0.0144(3) Uani 1 1 d . . .
B1 B 0.458(3) 0.730(3) 0.1345(18) 0.008(5) Uani 1 1 d U . .
P1 P 0.8992(7) -0.2502(7) 0.1018(5) 0.0144(13) Uani 1 1 d . . .
O1 O 0.7088(16) 0.2177(17) 0.1629(11) 0.012(3) Uani 1 1 d U . .
O2 O 0.9342(18) -0.140(2) 0.2120(12) 0.027(4) Uani 1 1 d . . .
O3 O 1.0349(17) -0.326(2) 0.0953(12) 0.023(3) Uani 1 1 d U . .
O4 O 0.8278(16) -0.1157(18) 0.0032(12) 0.020(3) Uani 1 1 d . . .
O5 O 0.6854(17) 0.2497(16) -0.1129(12) 0.014(3) Uani 1 1 d U . .
O6 O 0.7937(15) 0.5859(18) 0.0881(11) 0.016(3) Uani 1 1 d . . .
O7 O 0.5291(18) 0.589(2) 0.2056(16) 0.036(4) Uani 1 1 d . . .
O8 O 0.4729(17) 0.133(2) -0.0971(11) 0.023(4) 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 0.0047(5) 0.0147(5) 0.0192(5) -0.0001(3) 0.0032(4) 0.0002(3)
Pb2 0.0105(6) 0.0180(5) 0.0223(5) -0.0014(3) 0.0085(4) -0.0008(3)
Pb3 0.0150(6) 0.0096(5) 0.0239(5) 0.0025(3) 0.0087(4) 0.0000(3)
Pb4 0.0099(5) 0.0100(5) 0.0236(5) -0.0031(3) 0.0069(4) -0.0019(3)
B1 0.010(6) 0.007(6) 0.007(6) 0.004(4) 0.003(5) 0.000(4)
P1 0.008(3) 0.016(3) 0.018(3) 0.001(2) 0.003(2) -0.001(2)
O1 0.019(7) 0.006(5) 0.014(5) 0.002(4) 0.008(5) -0.005(5)
O2 0.037(11) 0.024(8) 0.026(8) -0.007(7) 0.018(8) 0.005(8)
O3 0.019(7) 0.029(6) 0.029(6) 0.001(5) 0.018(5) 0.001(5)
O4 0.024(9) 0.009(7) 0.026(8) -0.009(6) 0.007(7) -0.006(7)
O5 0.018(7) 0.006(5) 0.016(6) 0.001(4) 0.006(5) 0.001(5)
O6 0.008(8) 0.017(8) 0.022(8) 0.008(6) 0.006(6) 0.004(6)
O7 0.021(10) 0.033(10) 0.068(13) 0.025(9) 0.031(9) 0.011(8)
O8 0.030(10) 0.022(8) 0.018(8) -0.005(6) 0.010(7) -0.005(8)

_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 O5 2.368(15) . ?
Pb1 O1 2.401(13) . ?
Pb1 O4 2.528(13) . ?
Pb1 O6 2.670(13) . ?
Pb1 O3 2.741(14) 3_755 ?
Pb2 O8 2.354(13) . ?
Pb2 O1 2.427(15) . ?
Pb2 O8 2.434(15) 3_655 ?
Pb2 O4 2.683(15) 3_655 ?
Pb3 O1 2.225(12) . ?
Pb3 O3 2.400(16) 2_755 ?
Pb3 O5 2.460(13) 4_566 ?
Pb3 O2 2.568(14) . ?
Pb3 Pb4 3.5204(13) 1_545 ?
Pb4 O1 2.278(12) . ?
Pb4 O7 2.362(16) . ?
Pb4 O6 2.495(13) . ?
Pb4 O5 2.663(13) 4_566 ?
Pb4 Pb3 3.5204(13) 1_565 ?
B1 O7 1.35(3) . ?
B1 O5 1.38(3) 3_665 ?
B1 O8 1.39(3) 3_665 ?
P1 O3 1.515(16) . ?
P1 O4 1.521(15) . ?
P1 O2 1.535(14) . ?
P1 O6 1.536(14) 1_545 ?
O3 Pb3 2.400(16) 2_745 ?
O3 Pb1 2.741(14) 3_755 ?
O4 Pb2 2.683(15) 3_655 ?
O5 B1 1.38(3) 3_665 ?
O5 Pb3 2.460(13) 4_565 ?
O5 Pb4 2.663(13) 4_565 ?
O6 P1 1.536(14) 1_565 ?
O8 B1 1.39(3) 3_665 ?
O8 Pb2 2.434(15) 3_655 ?

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
O5 Pb1 O1 93.9(5) . . ?
O5 Pb1 O4 76.5(4) . . ?
O1 Pb1 O4 94.7(4) . . ?
O5 Pb1 O6 83.3(4) . . ?
O1 Pb1 O6 72.3(4) . . ?
O4 Pb1 O6 155.2(5) . . ?
O5 Pb1 O3 66.6(5) . 3_755 ?
O1 Pb1 O3 156.8(5) . 3_755 ?
O4 Pb1 O3 92.7(5) . 3_755 ?
O6 Pb1 O3 92.3(4) . 3_755 ?
O8 Pb2 O1 88.3(5) . . ?
O8 Pb2 O8 77.6(5) . 3_655 ?
O1 Pb2 O8 76.1(5) . 3_655 ?
O8 Pb2 O4 94.8(5) . 3_655 ?
O1 Pb2 O4 169.2(4) . 3_655 ?
O8 Pb2 O4 94.5(5) 3_655 3_655 ?
O1 Pb3 O3 87.8(5) . 2_755 ?
O1 Pb3 O5 79.7(5) . 4_566 ?
O3 Pb3 O5 71.0(5) 2_755 4_566 ?
O1 Pb3 O2 86.4(5) . . ?
O3 Pb3 O2 81.4(5) 2_755 . ?
O5 Pb3 O2 149.4(5) 4_566 . ?
O1 Pb3 Pb4 129.8(3) . 1_545 ?
O3 Pb3 Pb4 122.6(4) 2_755 1_545 ?
O5 Pb3 Pb4 144.1(3) 4_566 1_545 ?
O2 Pb3 Pb4 63.4(3) . 1_545 ?
O1 Pb4 O7 92.4(6) . . ?
O1 Pb4 O6 77.7(4) . . ?
O7 Pb4 O6 94.9(5) . . ?
O1 Pb4 O5 74.5(4) . 4_566 ?
O7 Pb4 O5 81.2(5) . 4_566 ?
O6 Pb4 O5 151.7(4) . 4_566 ?
O1 Pb4 Pb3 152.1(3) . 1_565 ?
O7 Pb4 Pb3 71.3(4) . 1_565 ?
O6 Pb4 Pb3 81.2(3) . 1_565 ?
O5 Pb4 Pb3 122.9(3) 4_566 1_565 ?
O7 B1 O5 117.2(18) . 3_665 ?
O7 B1 O8 122(2) . 3_665 ?
O5 B1 O8 120.2(17) 3_665 3_665 ?
O3 P1 O4 108.7(9) . . ?
O3 P1 O2 110.0(9) . . ?
O4 P1 O2 109.1(8) . . ?
O3 P1 O6 110.2(8) . 1_545 ?
O4 P1 O6 106.4(8) . 1_545 ?
O2 P1 O6 112.3(9) . 1_545 ?
Pb3 O1 Pb4 103.3(5) . . ?
Pb3 O1 Pb1 113.8(6) . . ?
Pb4 O1 Pb1 101.0(5) . . ?
Pb3 O1 Pb2 101.8(5) . . ?
Pb4 O1 Pb2 108.5(5) . . ?
Pb1 O1 Pb2 126.4(6) . . ?
P1 O2 Pb3 127.8(9) . . ?
P1 O3 Pb3 139.3(8) . 2_745 ?
P1 O3 Pb1 124.1(8) . 3_755 ?
Pb3 O3 Pb1 96.1(5) 2_745 3_755 ?
P1 O4 Pb1 110.2(7) . . ?
P1 O4 Pb2 105.5(7) . 3_655 ?
Pb1 O4 Pb2 110.4(5) . 3_655 ?
B1 O5 Pb1 125.0(12) 3_665 . ?
B1 O5 Pb3 109.1(11) 3_665 4_565 ?
Pb1 O5 Pb3 105.0(5) . 4_565 ?
B1 O5 Pb4 120.2(12) 3_665 4_565 ?
Pb1 O5 Pb4 103.1(5) . 4_565 ?
Pb3 O5 Pb4 87.1(4) 4_565 4_565 ?
P1 O6 Pb4 114.2(7) 1_565 . ?
P1 O6 Pb1 119.8(7) 1_565 . ?
Pb4 O6 Pb1 88.6(4) . . ?
B1 O7 Pb4 130.4(14) . . ?
B1 O8 Pb2 116.3(12) 3_665 . ?
B1 O8 Pb2 121.3(13) 3_665 3_655 ?
Pb2 O8 Pb2 102.4(5) . 3_655 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.551
_refine_diff_density_min         -4.948
_refine_diff_density_rms         0.988
_database_code_depnum_ccdc_archive 'CCDC 981388'
#######################################################################
#
#                 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.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Bi4 O10 P'
_chemical_formula_weight         1037.70

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'
P P 0.1023 0.0942 '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           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                   5.536(6)
_cell_length_b                   14.102(14)
_cell_length_c                   22.62(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1766(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1401
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.29

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    7.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3456
_exptl_absorpt_coefficient_mu    79.715
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.0172
_exptl_absorpt_correction_T_max  0.0925
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9635
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         27.38
_reflns_number_total             1988
_reflns_number_gt                1472
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0388P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1988
_refine_ls_number_parameters     145
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.020
_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
Bi1 Bi 0.05342(10) 0.71229(4) 0.30675(2) 0.01281(16) Uani 1 1 d U . .
Bi2 Bi 0.54041(11) 0.52313(4) 0.30828(3) 0.01728(17) Uani 1 1 d U . .
Bi3 Bi 0.03571(10) 0.54061(4) 0.42524(2) 0.01204(16) Uani 1 1 d U . .
Bi4 Bi 0.56453(10) 0.73778(4) 0.41555(3) 0.01621(16) Uani 1 1 d U . .
B1 B 0.537(3) 0.3862(12) 0.1878(8) 0.015(4) Uani 1 1 d U . .
P1 P 0.0091(7) 0.8760(3) 0.45401(18) 0.0127(8) Uani 1 1 d U . .
O1 O 0.2619(18) 0.6271(6) 0.3697(4) 0.013(2) Uani 1 1 d U . .
O2 O 0.2979(18) 0.6189(6) 0.2494(4) 0.011(2) Uani 1 1 d U . .
O3 O 0.7719(18) 0.6332(6) 0.3697(4) 0.014(2) Uani 1 1 d U . .
O4 O -0.0383(18) 0.7913(7) 0.4121(5) 0.018(2) Uani 1 1 d U . .
O5 O 0.207(2) 0.8511(7) 0.4980(5) 0.022(3) Uani 1 1 d U . .
O6 O 0.093(2) 0.9607(8) 0.4163(5) 0.026(3) Uani 1 1 d U . .
O7 O -0.232(2) 0.8930(8) 0.4853(5) 0.030(3) Uani 1 1 d U . .
O8 O 0.698(2) 0.4201(8) 0.2286(6) 0.031(3) Uani 1 1 d U . .
O9 O -0.074(2) 0.4414(9) 0.3534(5) 0.030(3) Uani 1 1 d U . .
O10 O 0.480(2) 0.7866(9) 0.3195(6) 0.029(3) Uani 1 1 d U . .

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 0.0117(3) 0.0125(3) 0.0142(3) 0.0011(2) -0.0021(2) 0.0005(2)
Bi2 0.0133(3) 0.0205(3) 0.0181(3) 0.0069(2) -0.0014(2) -0.0010(2)
Bi3 0.0125(3) 0.0131(3) 0.0106(3) 0.0006(2) 0.0010(2) 0.0002(2)
Bi4 0.0142(3) 0.0175(3) 0.0169(3) -0.0044(2) -0.0011(2) 0.0048(2)
B1 0.015(4) 0.015(4) 0.015(4) -0.0002(10) -0.0002(10) 0.0003(10)
P1 0.0126(11) 0.0130(11) 0.0125(11) 0.0009(9) 0.0002(9) 0.0004(8)
O1 0.013(2) 0.013(2) 0.013(2) 0.0005(10) 0.0001(10) 0.0006(10)
O2 0.011(2) 0.011(2) 0.011(2) 0.0004(10) 0.0006(10) 0.0000(10)
O3 0.014(2) 0.014(2) 0.014(2) 0.0002(10) 0.0000(10) 0.0002(10)
O4 0.018(3) 0.018(3) 0.018(3) -0.0006(10) -0.0003(10) 0.0002(10)
O5 0.022(3) 0.022(3) 0.022(3) 0.0002(10) -0.0004(10) -0.0003(10)
O6 0.026(3) 0.026(3) 0.026(3) 0.0004(10) -0.0001(10) -0.0005(10)
O7 0.030(3) 0.030(3) 0.030(3) -0.0002(10) 0.0002(10) 0.0000(10)
O8 0.031(3) 0.031(3) 0.031(3) -0.0004(10) 0.0001(10) -0.0002(10)
O9 0.030(3) 0.030(3) 0.030(3) -0.0009(10) -0.0003(10) 0.0002(10)
O10 0.029(3) 0.028(3) 0.029(3) 0.0003(10) -0.0005(10) -0.0002(10)

_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 O1 2.191(10) . ?
Bi1 O2 2.291(10) . ?
Bi1 O2 2.312(10) 6_556 ?
Bi1 O3 2.387(10) 1_455 ?
Bi1 O10 2.597(13) . ?
Bi1 O4 2.680(11) . ?
Bi1 Bi4 3.676(3) 1_455 ?
Bi2 O2 2.325(10) . ?
Bi2 O2 2.357(10) 6_656 ?
Bi2 O3 2.445(10) . ?
Bi2 O8 2.474(12) . ?
Bi2 O8 2.530(12) 6_556 ?
Bi2 O1 2.540(10) . ?
Bi2 O9 2.632(12) 1_655 ?
Bi2 O6 2.700(12) 8_655 ?
Bi3 O1 2.153(10) . ?
Bi3 O9 2.229(12) . ?
Bi3 O3 2.328(10) 1_455 ?
Bi3 O6 2.353(11) 8_655 ?
Bi3 O7 2.575(13) 4_566 ?
Bi3 Bi3 3.592(3) 5_566 ?
Bi4 O3 2.138(10) . ?
Bi4 O4 2.326(11) 1_655 ?
Bi4 O10 2.327(13) . ?
Bi4 O5 2.453(11) 4_566 ?
Bi4 O1 2.515(10) . ?
Bi4 Bi1 3.675(3) 1_655 ?
B1 O9 1.36(2) 6_656 ?
B1 O8 1.37(2) . ?
B1 O10 1.42(2) 3_645 ?
P1 O5 1.519(11) . ?
P1 O7 1.527(13) . ?
P1 O6 1.539(12) . ?
P1 O4 1.547(11) . ?
O2 Bi1 2.312(9) 6_656 ?
O2 Bi2 2.357(9) 6_556 ?
O3 Bi3 2.328(10) 1_655 ?
O3 Bi1 2.387(10) 1_655 ?
O4 Bi4 2.326(10) 1_455 ?
O5 Bi4 2.453(11) 4_466 ?
O6 Bi3 2.353(11) 8_665 ?
O6 Bi2 2.700(12) 8_665 ?
O7 Bi3 2.575(12) 4_466 ?
O8 Bi2 2.530(12) 6_656 ?
O9 B1 1.36(2) 6_556 ?
O9 Bi2 2.632(12) 1_455 ?
O10 B1 1.42(2) 3_655 ?

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
O1 Bi1 O2 75.0(4) . . ?
O1 Bi1 O2 111.5(3) . 6_556 ?
O2 Bi1 O2 73.9(2) . 6_556 ?
O1 Bi1 O3 72.6(4) . 1_455 ?
O2 Bi1 O3 117.1(3) . 1_455 ?
O2 Bi1 O3 70.2(3) 6_556 1_455 ?
O1 Bi1 O10 70.8(4) . . ?
O2 Bi1 O10 76.0(4) . . ?
O2 Bi1 O10 147.8(4) 6_556 . ?
O3 Bi1 O10 135.7(4) 1_455 . ?
O1 Bi1 O4 75.5(3) . . ?
O2 Bi1 O4 148.7(3) . . ?
O2 Bi1 O4 127.5(3) 6_556 . ?
O3 Bi1 O4 62.6(3) 1_455 . ?
O10 Bi1 O4 84.6(4) . . ?
O1 Bi1 Bi4 90.4(3) . 1_455 ?
O2 Bi1 Bi4 150.5(2) . 1_455 ?
O2 Bi1 Bi4 88.4(3) 6_556 1_455 ?
O3 Bi1 Bi4 33.5(2) 1_455 1_455 ?
O10 Bi1 Bi4 123.7(3) . 1_455 ?
O4 Bi1 Bi4 39.1(2) . 1_455 ?
O2 Bi2 O2 72.48(19) . 6_656 ?
O2 Bi2 O3 105.0(3) . . ?
O2 Bi2 O3 68.5(3) 6_656 . ?
O2 Bi2 O8 97.3(4) . . ?
O2 Bi2 O8 73.8(3) 6_656 . ?
O3 Bi2 O8 127.0(4) . . ?
O2 Bi2 O8 73.3(3) . 6_556 ?
O2 Bi2 O8 126.9(4) 6_656 6_556 ?
O3 Bi2 O8 160.8(4) . 6_556 ?
O8 Bi2 O8 71.7(3) . 6_556 ?
O2 Bi2 O1 68.1(3) . . ?
O2 Bi2 O1 109.8(3) 6_656 . ?
O3 Bi2 O1 69.0(3) . . ?
O8 Bi2 O1 162.0(4) . . ?
O8 Bi2 O1 93.3(4) 6_556 . ?
O2 Bi2 O9 160.9(4) . 1_655 ?
O2 Bi2 O9 88.6(4) 6_656 1_655 ?
O3 Bi2 O9 68.5(3) . 1_655 ?
O8 Bi2 O9 74.9(4) . 1_655 ?
O8 Bi2 O9 118.9(4) 6_556 1_655 ?
O1 Bi2 O9 122.2(4) . 1_655 ?
O2 Bi2 O6 123.4(3) . 8_655 ?
O2 Bi2 O6 148.5(3) 6_656 8_655 ?
O3 Bi2 O6 80.6(3) . 8_655 ?
O8 Bi2 O6 124.3(4) . 8_655 ?
O8 Bi2 O6 84.6(4) 6_556 8_655 ?
O1 Bi2 O6 61.8(3) . 8_655 ?
O9 Bi2 O6 74.2(3) 1_655 8_655 ?
O1 Bi3 O9 95.0(4) . . ?
O1 Bi3 O3 74.4(4) . 1_455 ?
O9 Bi3 O3 77.7(4) . 1_455 ?
O1 Bi3 O6 73.3(4) . 8_655 ?
O9 Bi3 O6 82.8(4) . 8_655 ?
O3 Bi3 O6 140.4(4) 1_455 8_655 ?
O1 Bi3 O7 87.8(4) . 4_566 ?
O9 Bi3 O7 159.6(4) . 4_566 ?
O3 Bi3 O7 122.3(3) 1_455 4_566 ?
O6 Bi3 O7 78.7(4) 8_655 4_566 ?
O1 Bi3 Bi3 142.6(3) . 5_566 ?
O9 Bi3 Bi3 117.2(3) . 5_566 ?
O3 Bi3 Bi3 128.2(3) 1_455 5_566 ?
O6 Bi3 Bi3 91.4(3) 8_655 5_566 ?
O7 Bi3 Bi3 55.3(3) 4_566 5_566 ?
O3 Bi4 O4 72.5(4) . 1_655 ?
O3 Bi4 O10 81.9(4) . . ?
O4 Bi4 O10 93.7(4) 1_655 . ?
O3 Bi4 O5 82.1(4) . 4_566 ?
O4 Bi4 O5 83.6(4) 1_655 4_566 ?
O10 Bi4 O5 163.8(4) . 4_566 ?
O3 Bi4 O1 74.3(3) . . ?
O4 Bi4 O1 144.8(3) 1_655 . ?
O10 Bi4 O1 70.3(4) . . ?
O5 Bi4 O1 103.0(3) 4_566 . ?
O3 Bi4 Bi1 38.0(3) . 1_655 ?
O4 Bi4 Bi1 46.6(3) 1_655 1_655 ?
O10 Bi4 Bi1 63.4(3) . 1_655 ?
O5 Bi4 Bi1 104.4(3) 4_566 1_655 ?
O1 Bi4 Bi1 98.8(2) . 1_655 ?
O9 B1 O8 123.8(15) 6_656 . ?
O9 B1 O10 117.3(15) 6_656 3_645 ?
O8 B1 O10 117.7(14) . 3_645 ?
O5 P1 O7 111.2(7) . . ?
O5 P1 O6 109.0(6) . . ?
O7 P1 O6 113.4(6) . . ?
O5 P1 O4 110.1(6) . . ?
O7 P1 O4 104.9(6) . . ?
O6 P1 O4 108.1(6) . . ?
Bi3 O1 Bi1 112.6(4) . . ?
Bi3 O1 Bi4 119.9(4) . . ?
Bi1 O1 Bi4 106.2(3) . . ?
Bi3 O1 Bi2 110.2(4) . . ?
Bi1 O1 Bi2 106.3(4) . . ?
Bi4 O1 Bi2 100.3(3) . . ?
Bi1 O2 Bi1 110.2(4) . 6_656 ?
Bi1 O2 Bi2 110.5(4) . . ?
Bi1 O2 Bi2 107.0(4) 6_656 . ?
Bi1 O2 Bi2 106.6(4) . 6_556 ?
Bi1 O2 Bi2 113.1(4) 6_656 6_556 ?
Bi2 O2 Bi2 109.5(4) . 6_556 ?
Bi4 O3 Bi3 117.5(4) . 1_655 ?
Bi4 O3 Bi1 108.5(4) . 1_655 ?
Bi3 O3 Bi1 100.0(4) 1_655 1_655 ?
Bi4 O3 Bi2 115.6(4) . . ?
Bi3 O3 Bi2 106.2(3) 1_655 . ?
Bi1 O3 Bi2 107.5(4) 1_655 . ?
P1 O4 Bi4 113.0(6) . 1_455 ?
P1 O4 Bi1 146.5(6) . . ?
Bi4 O4 Bi1 94.2(4) 1_455 . ?
P1 O5 Bi4 114.2(6) . 4_466 ?
P1 O6 Bi3 126.0(6) . 8_665 ?
P1 O6 Bi2 132.2(6) . 8_665 ?
Bi3 O6 Bi2 99.2(4) 8_665 8_665 ?
P1 O7 Bi3 149.0(7) . 4_466 ?
B1 O8 Bi2 117.8(10) . . ?
B1 O8 Bi2 117.8(10) . 6_656 ?
Bi2 O8 Bi2 99.6(4) . 6_656 ?
B1 O9 Bi3 137.4(11) 6_556 . ?
B1 O9 Bi2 110.5(10) 6_556 1_455 ?
Bi3 O9 Bi2 103.2(4) . 1_455 ?
B1 O10 Bi4 114.5(10) 3_655 . ?
B1 O10 Bi1 109.2(10) 3_655 . ?
Bi4 O10 Bi1 99.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.38
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         3.088
_refine_diff_density_min         -3.155
_refine_diff_density_rms         0.550
_database_code_depnum_ccdc_archive 'CCDC 981389'
