# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_vb59
_database_code_depnum_ccdc_archive 'CCDC 920801'
#TrackingRef '17026_web_deposit_cif_file_0_PhilAndrews_1358575216.Compound1.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H42 Bi2 O24'
_chemical_formula_sum            'C54 H42 Bi2 O24'
_chemical_formula_weight         1492.84
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Bi Bi -4.028 10.608 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   12.631(3)
_cell_length_b                   18.890(4)
_cell_length_c                   11.552(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.82(3)
_cell_angle_gamma                90.00
_cell_volume                     2592.9(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    38098
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      29.61
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    6.867
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_T_max  0.8205
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'MX2 beamline, Australian Synchrotron'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'ADSC Quantum 315r CCD'
_diffrn_measurement_method       '\f scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0-
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48984
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         29.61
_reflns_number_total             6938
_reflns_number_gt                6435
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Blue Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabasch, 1993)'
_computing_data_reduction        'XDS (Kabasch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_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^)+(0.0304P)^2^+5.4134P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6938
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0712
_refine_ls_wR_factor_gt          0.0700
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.003
_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 0.076677(8) 0.497979(5) 0.849895(9) 0.01876(5) Uani 1 1 d . . .
O1 O 0.12688(17) 0.62530(11) 0.85432(18) 0.0227(4) Uani 1 1 d . . .
O2 O 0.20180(17) 0.55496(10) 1.01250(19) 0.0221(4) Uani 1 1 d . . .
O3 O 0.30463(18) 0.62217(12) 1.23633(19) 0.0261(4) Uani 1 1 d . . .
O4 O 0.1167(2) 0.62339(14) 1.1981(2) 0.0350(5) Uani 1 1 d . . .
O5 O 0.17973(17) 0.40443(11) 0.94851(19) 0.0222(4) Uani 1 1 d . . .
O6 O 0.06420(17) 0.43124(10) 1.04818(19) 0.0227(4) Uani 1 1 d . . .
O7 O 0.36102(17) 0.32047(10) 1.07737(19) 0.0232(4) Uani 1 1 d . . .
O8 O 0.4066(2) 0.42093(13) 1.1880(2) 0.0354(5) Uani 1 1 d . . .
O9 O 0.2202(2) 0.50124(10) 0.7798(2) 0.0239(4) Uani 1 1 d . . .
O10 O 0.09116(16) 0.42696(11) 0.66842(19) 0.0222(4) Uani 1 1 d . . .
O11 O 0.14059(16) 0.34829(10) 0.49670(18) 0.0206(4) Uani 1 1 d . . .
O12 O 0.03962(18) 0.43555(11) 0.3776(2) 0.0265(4) Uani 1 1 d . . .
C1 C 0.1894(2) 0.61707(14) 0.9640(3) 0.0203(5) Uani 1 1 d . . .
C2 C 0.2496(2) 0.67930(14) 1.0350(3) 0.0206(5) Uani 1 1 d . . .
C3 C 0.2541(3) 0.74042(16) 0.9685(3) 0.0263(6) Uani 1 1 d . . .
H3 H 0.2165 0.7412 0.8820 0.032 Uiso 1 1 calc R . .
C4 C 0.3125(3) 0.79982(17) 1.0266(3) 0.0321(7) Uani 1 1 d . . .
H4 H 0.3160 0.8407 0.9801 0.039 Uiso 1 1 calc R . .
C5 C 0.3659(3) 0.79937(17) 1.1531(3) 0.0328(7) Uani 1 1 d . . .
H5 H 0.4062 0.8400 1.1932 0.039 Uiso 1 1 calc R . .
C6 C 0.3606(3) 0.73991(17) 1.2211(3) 0.0276(6) Uani 1 1 d . . .
H6 H 0.3970 0.7399 1.3078 0.033 Uiso 1 1 calc R . .
C7 C 0.3022(2) 0.68039(15) 1.1625(3) 0.0233(5) Uani 1 1 d . . .
C8 C 0.2065(3) 0.59576(18) 1.2428(3) 0.0293(6) Uani 1 1 d . . .
C9 C 0.2305(3) 0.5284(2) 1.3141(4) 0.0432(9) Uani 1 1 d . . .
H9A H 0.1674 0.5171 1.3420 0.065 Uiso 1 1 calc R . .
H9B H 0.2994 0.5338 1.3855 0.065 Uiso 1 1 calc R . .
H9C H 0.2407 0.4901 1.2616 0.065 Uiso 1 1 calc R . .
C10 C 0.1397(2) 0.39224(13) 1.0349(2) 0.0195(5) Uani 1 1 d . . .
C11 C 0.1833(2) 0.33063(14) 1.1187(3) 0.0203(5) Uani 1 1 d . . .
C12 C 0.1134(2) 0.30146(15) 1.1779(3) 0.0230(5) Uani 1 1 d . . .
H12 H 0.0417 0.3220 1.1656 0.028 Uiso 1 1 calc R . .
C13 C 0.1471(3) 0.24288(15) 1.2545(3) 0.0248(5) Uani 1 1 d . . .
H13 H 0.0977 0.2228 1.2918 0.030 Uiso 1 1 calc R . .
C14 C 0.2524(3) 0.21400(14) 1.2762(3) 0.0237(5) Uani 1 1 d . . .
H14 H 0.2760 0.1746 1.3300 0.028 Uiso 1 1 calc R . .
C15 C 0.3238(2) 0.24228(14) 1.2197(3) 0.0225(5) Uani 1 1 d . . .
H15 H 0.3967 0.2228 1.2357 0.027 Uiso 1 1 calc R . .
C16 C 0.2885(2) 0.29913(14) 1.1398(3) 0.0217(5) Uani 1 1 d . . .
C17 C 0.4119(3) 0.38461(16) 1.1055(3) 0.0269(6) Uani 1 1 d . . .
C18 C 0.4742(3) 0.4015(2) 1.0189(3) 0.0374(7) Uani 1 1 d . . .
H18A H 0.4248 0.4280 0.9484 0.056 Uiso 1 1 calc R . .
H18B H 0.4976 0.3573 0.9900 0.056 Uiso 1 1 calc R . .
H18C H 0.5408 0.4300 1.0618 0.056 Uiso 1 1 calc R . .
C19 C 0.1846(2) 0.45557(13) 0.6910(2) 0.0182(5) Uani 1 1 d . . .
C20 C 0.2629(2) 0.43901(14) 0.6230(2) 0.0186(5) Uani 1 1 d . . .
C21 C 0.3683(2) 0.47200(15) 0.6594(3) 0.0230(5) Uani 1 1 d . . .
H21 H 0.3859 0.5070 0.7221 0.028 Uiso 1 1 calc R . .
C22 C 0.4475(3) 0.45453(17) 0.6057(3) 0.0286(6) Uani 1 1 d . . .
H22 H 0.5191 0.4768 0.6324 0.034 Uiso 1 1 calc R . .
C23 C 0.4218(3) 0.40434(18) 0.5129(3) 0.0299(6) Uani 1 1 d . . .
H23 H 0.4761 0.3924 0.4759 0.036 Uiso 1 1 calc R . .
C24 C 0.3173(2) 0.37135(15) 0.4734(3) 0.0244(5) Uani 1 1 d . . .
H24 H 0.2996 0.3373 0.4090 0.029 Uiso 1 1 calc R . .
C25 C 0.2391(2) 0.38867(14) 0.5288(2) 0.0192(5) Uani 1 1 d . . .
C26 C 0.0428(2) 0.37937(15) 0.4279(3) 0.0227(5) Uani 1 1 d . . .
C27 C -0.0550(3) 0.33435(19) 0.4256(3) 0.0330(7) Uani 1 1 d . . .
H27A H -0.0604 0.3326 0.5082 0.049 Uiso 1 1 calc R . .
H27B H -0.0444 0.2864 0.3992 0.049 Uiso 1 1 calc R . .
H27C H -0.1243 0.3546 0.3680 0.049 Uiso 1 1 calc R . .
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 0.01979(6) 0.02168(6) 0.01698(7) 0.00013(3) 0.00908(5) 0.00210(3)
O1 0.0240(10) 0.0271(9) 0.0174(9) -0.0003(7) 0.0077(8) -0.0008(7)
O2 0.0243(9) 0.0227(9) 0.0209(10) 0.0002(7) 0.0097(8) 0.0008(7)
O3 0.0233(10) 0.0326(11) 0.0223(10) 0.0036(8) 0.0075(8) -0.0054(8)
O4 0.0284(12) 0.0508(14) 0.0293(12) 0.0016(10) 0.0145(10) -0.0027(10)
O5 0.0268(10) 0.0245(9) 0.0193(10) 0.0024(7) 0.0130(8) 0.0067(7)
O6 0.0254(10) 0.0243(9) 0.0223(10) 0.0008(7) 0.0133(8) 0.0050(7)
O7 0.0237(9) 0.0246(9) 0.0245(10) 0.0011(7) 0.0123(8) 0.0004(7)
O8 0.0388(13) 0.0324(12) 0.0338(13) -0.0077(10) 0.0105(11) -0.0087(10)
O9 0.0246(11) 0.0282(11) 0.0232(12) -0.0052(7) 0.0137(10) -0.0024(7)
O10 0.0199(9) 0.0284(10) 0.0210(10) -0.0026(7) 0.0107(8) -0.0015(7)
O11 0.0213(9) 0.0222(9) 0.0203(9) -0.0009(7) 0.0096(8) -0.0022(7)
O12 0.0243(10) 0.0313(10) 0.0228(10) 0.0055(8) 0.0064(9) -0.0009(8)
C1 0.0202(12) 0.0232(12) 0.0203(13) -0.0022(9) 0.0106(11) -0.0004(9)
C2 0.0178(11) 0.0255(12) 0.0217(13) -0.0013(10) 0.0107(11) -0.0018(9)
C3 0.0251(13) 0.0303(14) 0.0258(15) 0.0020(11) 0.0115(12) -0.0034(11)
C4 0.0328(16) 0.0303(15) 0.0328(17) 0.0039(12) 0.0105(14) -0.0067(12)
C5 0.0327(16) 0.0312(15) 0.0341(17) -0.0041(12) 0.0109(14) -0.0108(12)
C6 0.0230(13) 0.0364(15) 0.0235(15) -0.0020(11) 0.0079(12) -0.0058(11)
C7 0.0212(12) 0.0271(13) 0.0228(14) 0.0029(10) 0.0092(11) -0.0018(10)
C8 0.0289(15) 0.0406(16) 0.0193(14) -0.0008(11) 0.0093(12) -0.0109(12)
C9 0.044(2) 0.046(2) 0.0319(19) 0.0117(15) 0.0035(16) -0.0197(16)
C10 0.0230(12) 0.0195(11) 0.0178(12) -0.0017(9) 0.0093(11) -0.0003(9)
C11 0.0247(13) 0.0194(11) 0.0197(12) -0.0005(9) 0.0112(11) 0.0017(9)
C12 0.0254(13) 0.0245(12) 0.0228(13) -0.0015(10) 0.0128(12) 0.0021(10)
C13 0.0313(14) 0.0235(12) 0.0232(14) -0.0012(10) 0.0142(12) -0.0005(10)
C14 0.0313(14) 0.0202(11) 0.0202(13) 0.0009(9) 0.0097(12) 0.0004(10)
C15 0.0239(13) 0.0224(12) 0.0220(13) -0.0001(10) 0.0087(11) 0.0019(10)
C16 0.0258(13) 0.0209(12) 0.0201(13) -0.0027(9) 0.0101(11) -0.0014(10)
C17 0.0225(13) 0.0285(14) 0.0261(15) 0.0036(11) 0.0036(12) -0.0013(10)
C18 0.0353(17) 0.0425(18) 0.0363(18) 0.0033(14) 0.0147(16) -0.0112(14)
C19 0.0203(12) 0.0216(11) 0.0161(12) 0.0008(9) 0.0105(10) 0.0024(9)
C20 0.0196(12) 0.0220(11) 0.0172(12) 0.0015(9) 0.0102(10) 0.0013(9)
C21 0.0228(13) 0.0274(13) 0.0211(13) -0.0033(10) 0.0101(11) -0.0030(10)
C22 0.0218(13) 0.0386(16) 0.0286(15) -0.0037(12) 0.0129(12) -0.0045(11)
C23 0.0254(14) 0.0398(16) 0.0316(16) -0.0021(12) 0.0189(13) 0.0026(12)
C24 0.0268(14) 0.0276(13) 0.0240(14) -0.0019(10) 0.0151(12) 0.0030(10)
C25 0.0199(12) 0.0211(11) 0.0191(12) 0.0014(9) 0.0098(10) 0.0008(9)
C26 0.0219(12) 0.0299(13) 0.0177(12) -0.0011(10) 0.0085(11) -0.0025(10)
C27 0.0240(14) 0.0463(18) 0.0281(16) 0.0033(13) 0.0081(13) -0.0100(13)
_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 O9 2.223(2) . ?
Bi1 O5 2.260(2) . ?
Bi1 O2 2.274(2) . ?
Bi1 O1 2.483(2) . ?
Bi1 O10 2.547(2) . ?
Bi1 O6 2.666(2) . ?
Bi1 C1 2.748(3) . ?
Bi1 O6 2.7860(19) 3_567 ?
Bi1 O12 2.833(2) 3_566 ?
Bi1 O12 9.605(3) 3_567 ?
O1 C1 1.255(4) . ?
O2 C1 1.286(3) . ?
O3 C8 1.361(4) . ?
O3 C7 1.386(3) . ?
O4 C8 1.195(4) . ?
O5 C10 1.283(3) . ?
O6 C10 1.255(3) . ?
O7 C17 1.358(4) . ?
O7 C16 1.403(3) . ?
O8 C17 1.195(4) . ?
O9 C19 1.298(3) . ?
O10 C19 1.243(3) . ?
O11 C26 1.355(3) . ?
O11 C25 1.399(3) . ?
O12 C26 1.204(3) . ?
C1 C2 1.486(4) . ?
C2 C7 1.396(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.385(4) . ?
C4 C5 1.386(5) . ?
C5 C6 1.385(5) . ?
C6 C7 1.389(4) . ?
C8 C9 1.489(5) . ?
C10 C11 1.494(4) . ?
C11 C16 1.400(4) . ?
C11 C12 1.401(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.379(4) . ?
C14 C15 1.387(4) . ?
C15 C16 1.387(4) . ?
C17 C18 1.501(5) . ?
C19 C20 1.490(3) . ?
C20 C25 1.399(4) . ?
C20 C21 1.400(4) . ?
C21 C22 1.383(4) . ?
C22 C23 1.385(4) . ?
C23 C24 1.389(4) . ?
C24 C25 1.386(3) . ?
C26 C27 1.492(4) . ?
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
O9 Bi1 O5 78.70(8) . . ?
O9 Bi1 O2 82.17(8) . . ?
O5 Bi1 O2 80.43(8) . . ?
O9 Bi1 O1 75.32(7) . . ?
O5 Bi1 O1 130.34(7) . . ?
O2 Bi1 O1 54.79(7) . . ?
O9 Bi1 O10 54.52(7) . . ?
O5 Bi1 O10 79.23(7) . . ?
O2 Bi1 O10 134.86(7) . . ?
O1 Bi1 O10 115.97(6) . . ?
O9 Bi1 O6 128.28(8) . . ?
O5 Bi1 O6 52.33(6) . . ?
O2 Bi1 O6 75.00(7) . . ?
O1 Bi1 O6 121.97(6) . . ?
O10 Bi1 O6 119.99(7) . . ?
O9 Bi1 C1 78.36(8) . . ?
O5 Bi1 C1 106.38(9) . . ?
O2 Bi1 C1 27.67(8) . . ?
O1 Bi1 C1 27.16(8) . . ?
O10 Bi1 C1 130.97(7) . . ?
O6 Bi1 C1 98.45(8) . . ?
O9 Bi1 O6 149.02(6) . 3_567 ?
O5 Bi1 O6 120.23(6) . 3_567 ?
O2 Bi1 O6 77.78(7) . 3_567 ?
O1 Bi1 O6 73.84(6) . 3_567 ?
O10 Bi1 O6 146.62(7) . 3_567 ?
O6 Bi1 O6 68.37(7) . 3_567 ?
C1 Bi1 O6 72.89(7) . 3_567 ?
O9 Bi1 O12 83.10(8) . 3_566 ?
O5 Bi1 O12 147.45(7) . 3_566 ?
O2 Bi1 O12 123.58(7) . 3_566 ?
O1 Bi1 O12 68.79(7) . 3_566 ?
O10 Bi1 O12 68.23(7) . 3_566 ?
O6 Bi1 O12 147.54(6) . 3_566 ?
C1 Bi1 O12 95.95(8) . 3_566 ?
O6 Bi1 O12 88.56(6) 3_567 3_566 ?
O9 Bi1 O12 137.35(7) . 3_567 ?
O5 Bi1 O12 82.96(5) . 3_567 ?
O2 Bi1 O12 56.85(5) . 3_567 ?
O1 Bi1 O12 88.44(5) . 3_567 ?
O10 Bi1 O12 155.47(5) . 3_567 ?
O6 Bi1 O12 36.03(4) . 3_567 ?
C1 Bi1 O12 70.43(6) . 3_567 ?
O6 Bi1 O12 39.08(5) 3_567 3_567 ?
O12 Bi1 O12 127.56(5) 3_566 3_567 ?
C1 O1 Bi1 88.27(16) . . ?
C1 O2 Bi1 97.15(17) . . ?
C8 O3 C7 119.6(2) . . ?
C10 O5 Bi1 102.77(16) . . ?
C10 O6 Bi1 84.49(15) . . ?
C17 O7 C16 118.2(2) . . ?
C19 O9 Bi1 99.37(16) . . ?
C19 O10 Bi1 85.78(15) . . ?
C26 O11 C25 118.1(2) . . ?
O1 C1 O2 119.6(3) . . ?
O1 C1 C2 119.2(2) . . ?
O2 C1 C2 121.2(3) . . ?
O1 C1 Bi1 64.58(15) . . ?
O2 C1 Bi1 55.18(14) . . ?
C2 C1 Bi1 175.45(19) . . ?
C7 C2 C3 118.3(3) . . ?
C7 C2 C1 124.4(2) . . ?
C3 C2 C1 117.3(3) . . ?
C4 C3 C2 121.1(3) . . ?
C3 C4 C5 119.7(3) . . ?
C6 C5 C4 120.2(3) . . ?
C5 C6 C7 120.0(3) . . ?
O3 C7 C6 116.4(3) . . ?
O3 C7 C2 122.8(3) . . ?
C6 C7 C2 120.7(3) . . ?
O4 C8 O3 124.4(3) . . ?
O4 C8 C9 126.7(3) . . ?
O3 C8 C9 109.0(3) . . ?
O6 C10 O5 120.4(2) . . ?
O6 C10 C11 120.4(2) . . ?
O5 C10 C11 119.2(2) . . ?
C16 C11 C12 117.8(2) . . ?
C16 C11 C10 124.3(2) . . ?
C12 C11 C10 117.9(2) . . ?
C13 C12 C11 121.0(3) . . ?
C14 C13 C12 120.0(3) . . ?
C13 C14 C15 120.2(3) . . ?
C14 C15 C16 119.9(3) . . ?
C15 C16 C11 121.1(3) . . ?
C15 C16 O7 116.5(2) . . ?
C11 C16 O7 122.3(2) . . ?
O8 C17 O7 123.5(3) . . ?
O8 C17 C18 126.4(3) . . ?
O7 C17 C18 110.0(3) . . ?
O10 C19 O9 120.3(2) . . ?
O10 C19 C20 123.5(2) . . ?
O9 C19 C20 116.2(2) . . ?
C25 C20 C21 117.9(2) . . ?
C25 C20 C19 123.2(2) . . ?
C21 C20 C19 118.9(2) . . ?
C22 C21 C20 121.2(3) . . ?
C21 C22 C23 119.7(3) . . ?
C22 C23 C24 120.6(3) . . ?
C25 C24 C23 119.2(3) . . ?
C24 C25 C20 121.4(3) . . ?
C24 C25 O11 117.2(2) . . ?
C20 C25 O11 120.9(2) . . ?
O12 C26 O11 122.7(3) . . ?
O12 C26 C27 127.0(3) . . ?
O11 C26 C27 110.3(3) . . ?
_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.956
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.921
_refine_diff_density_rms         0.114


data_vbmerge
_database_code_depnum_ccdc_archive 'CCDC 920802'
#TrackingRef '17027_web_deposit_cif_file_1_PhilAndrews_1358575216.Compound2.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H28 Bi K O16'
_chemical_formula_sum            'C36 H28 Bi K O16'
_chemical_formula_weight         964.66
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.028 10.608 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.243(2)
_cell_length_b                   11.341(2)
_cell_length_c                   16.047(3)
_cell_angle_alpha                106.16(3)
_cell_angle_beta                 104.71(3)
_cell_angle_gamma                103.86(3)
_cell_volume                     1791.8(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    28417
_cell_measurement_theta_min      1.41
_cell_measurement_theta_max      28.78
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    5.112
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8216
_exptl_absorpt_correction_T_max  0.8617
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'MX1 beamline, Australian Synchrotron'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'ADSC Quantum 210r CCD'
_diffrn_measurement_method       '\f scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            58724
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         28.78
_reflns_number_total             8732
_reflns_number_gt                8395
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Blue Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabasch, 1993)'
_computing_data_reduction        'XDS (Kabasch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_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^)+(0.0290P)^2^+3.5081P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0231(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         8732
_refine_ls_number_parameters     492
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0633
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.048
_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 0.653889(9) 0.567624(10) 0.631182(7) 0.01637(5) Uani 1 1 d . . .
K1 K 0.52325(7) 0.84966(7) 0.57587(5) 0.02504(13) Uani 1 1 d . . .
O1 O 0.5709(2) 0.3245(2) 0.60705(17) 0.0287(5) Uani 1 1 d . . .
O2 O 0.7614(2) 0.4610(2) 0.70982(16) 0.0233(4) Uani 1 1 d . . .
O3 O 0.4459(3) 0.1818(2) 0.69463(17) 0.0294(5) Uani 1 1 d . . .
O4 O 0.4117(3) 0.0420(2) 0.55327(17) 0.0309(5) Uani 1 1 d . . .
O5 O 0.5650(2) 0.7499(2) 0.71170(16) 0.0250(4) Uani 1 1 d . . .
O6 O 0.6125(2) 0.6050(2) 0.77084(15) 0.0234(4) Uani 1 1 d . . .
O7 O 0.6308(2) 0.6628(2) 0.95136(16) 0.0259(5) Uani 1 1 d . . .
O8 O 0.4754(3) 0.4637(3) 0.88894(19) 0.0355(6) Uani 1 1 d . . .
O9 O 0.7765(2) 0.4982(3) 0.53566(17) 0.0306(5) Uani 1 1 d . . .
O10 O 0.6101(2) 0.5249(3) 0.44389(16) 0.0307(5) Uani 1 1 d . . .
O11 O 0.9123(2) 0.3653(2) 0.44805(16) 0.0241(4) Uani 1 1 d . . .
O12 O 0.7163(2) 0.2143(3) 0.40960(19) 0.0332(5) Uani 1 1 d . . .
O13 O 0.8456(2) 0.7256(2) 0.71801(15) 0.0218(4) Uani 1 1 d . . .
O14 O 0.7586(2) 0.8088(2) 0.61760(16) 0.0250(5) Uani 1 1 d . . .
O15 O 1.0516(2) 0.8843(2) 0.86856(16) 0.0255(5) Uani 1 1 d . . .
O16 O 0.8794(3) 0.9231(3) 0.90438(18) 0.0326(5) Uani 1 1 d . . .
C1 C 0.6693(3) 0.3507(3) 0.6762(2) 0.0239(6) Uani 1 1 d . . .
C2 C 0.6794(3) 0.2558(3) 0.7241(2) 0.0253(6) Uani 1 1 d . . .
C3 C 0.8023(4) 0.2523(4) 0.7689(2) 0.0315(7) Uani 1 1 d . . .
H3 H 0.8786 0.3103 0.7686 0.038 Uiso 1 1 calc R . .
C4 C 0.8137(4) 0.1646(4) 0.8138(3) 0.0353(8) Uani 1 1 d . . .
H4 H 0.8975 0.1624 0.8434 0.042 Uiso 1 1 calc R . .
C5 C 0.7033(4) 0.0805(4) 0.8154(3) 0.0375(8) Uani 1 1 d . . .
H5 H 0.7112 0.0193 0.8447 0.045 Uiso 1 1 calc R . .
C6 C 0.5811(4) 0.0855(3) 0.7743(2) 0.0336(8) Uani 1 1 d . . .
H6 H 0.5056 0.0304 0.7776 0.040 Uiso 1 1 calc R . .
C7 C 0.5698(4) 0.1717(3) 0.7282(2) 0.0276(7) Uani 1 1 d . . .
C8 C 0.3759(4) 0.1148(3) 0.6037(2) 0.0274(7) Uani 1 1 d . . .
C9 C 0.2525(4) 0.1444(4) 0.5762(3) 0.0367(8) Uani 1 1 d . . .
H9A H 0.2576 0.1941 0.5353 0.055 Uiso 1 1 calc R . .
H9B H 0.2402 0.1958 0.6315 0.055 Uiso 1 1 calc R . .
H9C H 0.1788 0.0628 0.5437 0.055 Uiso 1 1 calc R . .
C10 C 0.5665(3) 0.6979(3) 0.7717(2) 0.0202(5) Uani 1 1 d . . .
C11 C 0.5100(3) 0.7441(3) 0.8444(2) 0.0220(6) Uani 1 1 d . . .
C12 C 0.4217(3) 0.8093(3) 0.8269(2) 0.0246(6) Uani 1 1 d . . .
H12 H 0.4012 0.8250 0.7706 0.030 Uiso 1 1 calc R . .
C13 C 0.3632(3) 0.8519(3) 0.8905(3) 0.0305(7) Uani 1 1 d . . .
H13 H 0.3016 0.8946 0.8772 0.037 Uiso 1 1 calc R . .
C14 C 0.3950(4) 0.8317(4) 0.9738(3) 0.0336(8) Uani 1 1 d . . .
H14 H 0.3562 0.8621 1.0178 0.040 Uiso 1 1 calc R . .
C15 C 0.4827(3) 0.7678(4) 0.9926(2) 0.0304(7) Uani 1 1 d . . .
H15 H 0.5049 0.7547 1.0498 0.036 Uiso 1 1 calc R . .
C16 C 0.5385(3) 0.7227(3) 0.9277(2) 0.0234(6) Uani 1 1 d . . .
C17 C 0.5881(3) 0.5299(3) 0.9240(2) 0.0283(7) Uani 1 1 d . . .
C18 C 0.7019(4) 0.4826(4) 0.9443(3) 0.0387(8) Uani 1 1 d . . .
H18A H 0.6707 0.3910 0.9380 0.058 Uiso 1 1 calc R . .
H18B H 0.7617 0.5349 1.0075 0.058 Uiso 1 1 calc R . .
H18C H 0.7477 0.4909 0.9007 0.058 Uiso 1 1 calc R . .
C19 C 0.7133(3) 0.4986(3) 0.4580(2) 0.0214(6) Uani 1 1 d . . .
C20 C 0.7699(3) 0.4747(3) 0.3814(2) 0.0205(6) Uani 1 1 d . . .
C21 C 0.7295(3) 0.5188(3) 0.3099(2) 0.0228(6) Uani 1 1 d . . .
H21 H 0.6638 0.5583 0.3086 0.027 Uiso 1 1 calc R . .
C22 C 0.7837(3) 0.5062(3) 0.2403(2) 0.0268(6) Uani 1 1 d . . .
H22 H 0.7557 0.5379 0.1925 0.032 Uiso 1 1 calc R . .
C23 C 0.8785(3) 0.4474(4) 0.2408(2) 0.0294(7) Uani 1 1 d . . .
H23 H 0.9166 0.4400 0.1939 0.035 Uiso 1 1 calc R . .
C24 C 0.9179(3) 0.3989(3) 0.3103(2) 0.0264(6) Uani 1 1 d . . .
H24 H 0.9816 0.3570 0.3103 0.032 Uiso 1 1 calc R . .
C25 C 0.8639(3) 0.4123(3) 0.3791(2) 0.0220(6) Uani 1 1 d . . .
C26 C 0.8276(3) 0.2716(3) 0.4610(2) 0.0267(6) Uani 1 1 d . . .
C27 C 0.8911(4) 0.2494(4) 0.5465(3) 0.0375(8) Uani 1 1 d . . .
H27A H 0.8311 0.1752 0.5514 0.056 Uiso 1 1 calc R . .
H27B H 0.9127 0.3275 0.6007 0.056 Uiso 1 1 calc R . .
H27C H 0.9710 0.2310 0.5434 0.056 Uiso 1 1 calc R . .
C28 C 0.8471(3) 0.8183(3) 0.6864(2) 0.0207(6) Uani 1 1 d . . .
C29 C 0.9630(3) 0.9423(3) 0.7358(2) 0.0220(6) Uani 1 1 d . . .
C30 C 0.9777(3) 1.0344(3) 0.6937(2) 0.0270(6) Uani 1 1 d . . .
H30 H 0.9160 1.0167 0.6351 0.032 Uiso 1 1 calc R . .
C31 C 1.0810(4) 1.1518(3) 0.7357(3) 0.0308(7) Uani 1 1 d . . .
H31 H 1.0889 1.2138 0.7062 0.037 Uiso 1 1 calc R . .
C32 C 1.1728(3) 1.1778(3) 0.8210(3) 0.0322(7) Uani 1 1 d . . .
H32 H 1.2447 1.2568 0.8494 0.039 Uiso 1 1 calc R . .
C33 C 1.1588(3) 1.0877(3) 0.8645(2) 0.0290(7) Uani 1 1 d . . .
H33 H 1.2203 1.1059 0.9232 0.035 Uiso 1 1 calc R . .
C34 C 1.0553(3) 0.9715(3) 0.8223(2) 0.0236(6) Uani 1 1 d . . .
C35 C 0.9522(3) 0.8617(3) 0.9032(2) 0.0264(6) Uani 1 1 d . . .
C36 C 0.9499(4) 0.7491(4) 0.9344(3) 0.0321(7) Uani 1 1 d . . .
H36A H 0.9040 0.7522 0.9790 0.048 Uiso 1 1 calc R . .
H36B H 1.0395 0.7536 0.9637 0.048 Uiso 1 1 calc R . .
H36C H 0.9047 0.6675 0.8811 0.048 Uiso 1 1 calc R . .
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 0.01584(7) 0.01467(7) 0.01772(7) 0.00541(4) 0.00598(4) 0.00387(4)
K1 0.0264(3) 0.0278(3) 0.0253(3) 0.0128(3) 0.0109(3) 0.0105(3)
O1 0.0282(12) 0.0243(11) 0.0301(12) 0.0124(10) 0.0064(9) 0.0034(9)
O2 0.0221(10) 0.0212(10) 0.0262(11) 0.0093(9) 0.0071(8) 0.0071(9)
O3 0.0341(13) 0.0251(11) 0.0285(12) 0.0079(9) 0.0137(10) 0.0082(10)
O4 0.0427(14) 0.0224(11) 0.0297(12) 0.0104(10) 0.0164(11) 0.0094(10)
O5 0.0310(12) 0.0237(11) 0.0259(11) 0.0109(9) 0.0151(9) 0.0106(9)
O6 0.0272(11) 0.0240(11) 0.0232(10) 0.0101(9) 0.0118(9) 0.0106(9)
O7 0.0245(11) 0.0260(11) 0.0226(10) 0.0083(9) 0.0067(9) 0.0027(9)
O8 0.0322(13) 0.0307(13) 0.0377(14) 0.0139(11) 0.0096(11) 0.0013(11)
O9 0.0330(12) 0.0426(14) 0.0250(11) 0.0148(10) 0.0136(10) 0.0210(11)
O10 0.0225(11) 0.0434(14) 0.0242(11) 0.0069(10) 0.0080(9) 0.0134(10)
O11 0.0193(10) 0.0239(11) 0.0282(11) 0.0101(9) 0.0077(8) 0.0054(9)
O12 0.0248(12) 0.0335(13) 0.0383(14) 0.0179(11) 0.0067(10) 0.0030(10)
O13 0.0189(10) 0.0169(10) 0.0246(10) 0.0059(8) 0.0052(8) 0.0018(8)
O14 0.0217(10) 0.0252(11) 0.0240(11) 0.0093(9) 0.0065(8) 0.0017(9)
O15 0.0236(11) 0.0229(11) 0.0292(11) 0.0107(9) 0.0076(9) 0.0064(9)
O16 0.0346(13) 0.0368(14) 0.0294(12) 0.0103(10) 0.0137(10) 0.0163(11)
C1 0.0291(15) 0.0215(14) 0.0263(15) 0.0104(12) 0.0130(12) 0.0114(12)
C2 0.0357(17) 0.0200(14) 0.0242(14) 0.0084(12) 0.0132(13) 0.0123(13)
C3 0.0365(18) 0.0325(18) 0.0295(16) 0.0123(14) 0.0133(14) 0.0150(15)
C4 0.047(2) 0.039(2) 0.0280(17) 0.0122(15) 0.0136(15) 0.0276(17)
C5 0.059(2) 0.0319(18) 0.0266(17) 0.0142(14) 0.0142(16) 0.0200(18)
C6 0.051(2) 0.0236(16) 0.0281(16) 0.0111(13) 0.0168(15) 0.0095(15)
C7 0.0367(17) 0.0214(14) 0.0236(15) 0.0061(12) 0.0115(13) 0.0089(13)
C8 0.0359(17) 0.0200(14) 0.0280(16) 0.0112(12) 0.0146(13) 0.0055(13)
C9 0.040(2) 0.038(2) 0.0344(18) 0.0114(16) 0.0162(16) 0.0155(17)
C10 0.0200(13) 0.0184(13) 0.0195(13) 0.0040(10) 0.0081(11) 0.0035(11)
C11 0.0218(13) 0.0187(13) 0.0199(13) 0.0026(11) 0.0085(11) 0.0007(11)
C12 0.0241(14) 0.0183(13) 0.0282(15) 0.0050(12) 0.0108(12) 0.0035(12)
C13 0.0274(16) 0.0235(15) 0.0384(18) 0.0054(13) 0.0148(14) 0.0075(13)
C14 0.0328(17) 0.0329(18) 0.0321(17) 0.0031(14) 0.0204(14) 0.0057(15)
C15 0.0289(16) 0.0326(17) 0.0226(15) 0.0045(13) 0.0121(13) 0.0014(14)
C16 0.0212(14) 0.0207(14) 0.0226(14) 0.0054(11) 0.0075(11) -0.0002(11)
C17 0.0320(17) 0.0289(16) 0.0243(15) 0.0121(13) 0.0113(13) 0.0062(14)
C18 0.0370(19) 0.0351(19) 0.046(2) 0.0179(17) 0.0158(17) 0.0109(16)
C19 0.0210(13) 0.0197(13) 0.0218(14) 0.0044(11) 0.0104(11) 0.0046(11)
C20 0.0185(13) 0.0172(13) 0.0226(14) 0.0047(11) 0.0085(11) 0.0019(11)
C21 0.0207(13) 0.0192(13) 0.0253(14) 0.0068(11) 0.0068(11) 0.0035(11)
C22 0.0290(16) 0.0220(14) 0.0250(15) 0.0095(12) 0.0071(12) 0.0016(12)
C23 0.0262(15) 0.0320(17) 0.0260(15) 0.0086(13) 0.0117(13) 0.0019(13)
C24 0.0202(14) 0.0262(15) 0.0306(16) 0.0068(13) 0.0114(12) 0.0052(12)
C25 0.0181(13) 0.0209(14) 0.0248(14) 0.0083(11) 0.0067(11) 0.0037(11)
C26 0.0263(15) 0.0227(15) 0.0311(16) 0.0114(13) 0.0092(13) 0.0069(13)
C27 0.0374(19) 0.0342(19) 0.0379(19) 0.0200(16) 0.0064(15) 0.0057(16)
C28 0.0182(13) 0.0200(13) 0.0212(13) 0.0043(11) 0.0090(11) 0.0027(11)
C29 0.0207(13) 0.0177(13) 0.0259(14) 0.0063(11) 0.0091(11) 0.0043(11)
C30 0.0269(15) 0.0245(15) 0.0253(15) 0.0086(12) 0.0082(12) 0.0022(13)
C31 0.0321(17) 0.0231(15) 0.0354(18) 0.0118(14) 0.0132(14) 0.0031(13)
C32 0.0250(16) 0.0212(15) 0.0406(19) 0.0080(14) 0.0073(14) -0.0013(13)
C33 0.0228(15) 0.0213(15) 0.0318(17) 0.0043(13) 0.0021(12) 0.0021(12)
C34 0.0227(14) 0.0181(13) 0.0291(15) 0.0080(12) 0.0095(12) 0.0052(11)
C35 0.0255(15) 0.0247(15) 0.0228(14) 0.0051(12) 0.0064(12) 0.0035(12)
C36 0.0330(17) 0.0335(18) 0.0307(17) 0.0149(14) 0.0121(14) 0.0074(15)
_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 O13 2.243(2) . ?
Bi1 O2 2.300(2) . ?
Bi1 O6 2.348(2) . ?
Bi1 O9 2.407(3) . ?
Bi1 O1 2.572(3) . ?
Bi1 O5 2.664(2) . ?
Bi1 O10 2.711(3) 2_666 ?
Bi1 O10 2.799(3) . ?
K1 O12 2.704(3) 2_666 ?
K1 O5 2.713(2) . ?
K1 O14 2.744(3) . ?
K1 O1 2.798(3) 2_666 ?
K1 O4 2.826(3) 1_565 ?
K1 O4 2.845(3) 2_666 ?
K1 C6 3.330(4) 1_565 ?
K1 C8 3.441(3) 2_666 ?
O1 C1 1.256(4) . ?
O1 K1 2.798(3) 2_666 ?
O2 C1 1.284(4) . ?
O3 C8 1.356(4) . ?
O3 C7 1.405(4) . ?
O4 C8 1.205(4) . ?
O4 K1 2.826(3) 1_545 ?
O4 K1 2.845(3) 2_666 ?
O5 C10 1.260(4) . ?
O6 C10 1.278(4) . ?
O7 C17 1.369(4) . ?
O7 C16 1.401(4) . ?
O8 C17 1.197(4) . ?
O9 C19 1.271(4) . ?
O10 C19 1.248(4) . ?
O10 Bi1 2.711(3) 2_666 ?
O11 C26 1.348(4) . ?
O11 C25 1.402(4) . ?
O12 C26 1.206(4) . ?
O12 K1 2.704(3) 2_666 ?
O13 C28 1.287(4) . ?
O14 C28 1.242(4) . ?
O15 C35 1.372(4) . ?
O15 C34 1.392(4) . ?
O16 C35 1.194(4) . ?
C1 C2 1.496(4) . ?
C2 C7 1.395(5) . ?
C2 C3 1.402(5) . ?
C3 C4 1.392(5) . ?
C4 C5 1.383(6) . ?
C5 C6 1.387(6) . ?
C6 C7 1.390(5) . ?
C6 K1 3.330(4) 1_545 ?
C8 C9 1.492(5) . ?
C8 K1 3.441(3) 2_666 ?
C10 C11 1.496(4) . ?
C11 C12 1.392(5) . ?
C11 C16 1.396(4) . ?
C12 C13 1.388(5) . ?
C13 C14 1.390(6) . ?
C14 C15 1.379(6) . ?
C15 C16 1.388(5) . ?
C17 C18 1.498(6) . ?
C19 C20 1.511(4) . ?
C20 C21 1.391(4) . ?
C20 C25 1.407(4) . ?
C21 C22 1.392(5) . ?
C22 C23 1.385(5) . ?
C23 C24 1.396(5) . ?
C24 C25 1.379(4) . ?
C26 C27 1.495(5) . ?
C28 C29 1.510(4) . ?
C29 C30 1.394(4) . ?
C29 C34 1.400(4) . ?
C30 C31 1.392(5) . ?
C31 C32 1.392(5) . ?
C32 C33 1.390(5) . ?
C33 C34 1.384(4) . ?
C35 C36 1.494(5) . ?
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
O13 Bi1 O2 78.56(8) . . ?
O13 Bi1 O6 84.38(9) . . ?
O2 Bi1 O6 73.19(8) . . ?
O13 Bi1 O9 82.97(9) . . ?
O2 Bi1 O9 78.51(8) . . ?
O6 Bi1 O9 150.77(8) . . ?
O13 Bi1 O1 132.03(8) . . ?
O2 Bi1 O1 53.69(8) . . ?
O6 Bi1 O1 85.85(9) . . ?
O9 Bi1 O1 83.27(9) . . ?
O13 Bi1 O5 81.22(8) . . ?
O2 Bi1 O5 122.94(8) . . ?
O6 Bi1 O5 52.05(8) . . ?
O9 Bi1 O5 149.65(8) . . ?
O1 Bi1 O5 126.17(8) . . ?
O13 Bi1 O10 153.10(8) . 2_666 ?
O2 Bi1 O10 119.92(9) . 2_666 ?
O6 Bi1 O10 83.10(8) . 2_666 ?
O9 Bi1 O10 118.14(9) . 2_666 ?
O1 Bi1 O10 70.57(9) . 2_666 ?
O5 Bi1 O10 72.30(8) . 2_666 ?
O13 Bi1 O10 110.03(9) . . ?
O2 Bi1 O10 123.63(8) . . ?
O6 Bi1 O10 158.95(8) . . ?
O9 Bi1 O10 49.54(8) . . ?
O1 Bi1 O10 94.73(9) . . ?
O5 Bi1 O10 113.41(8) . . ?
O10 Bi1 O10 77.31(9) 2_666 . ?
O12 K1 O5 79.07(8) 2_666 . ?
O12 K1 O14 144.09(8) 2_666 . ?
O5 K1 O14 66.70(7) . . ?
O12 K1 O1 92.03(9) 2_666 2_666 ?
O5 K1 O1 117.59(8) . 2_666 ?
O14 K1 O1 94.30(8) . 2_666 ?
O12 K1 O4 70.80(8) 2_666 1_565 ?
O5 K1 O4 132.05(8) . 1_565 ?
O14 K1 O4 141.80(8) . 1_565 ?
O1 K1 O4 100.24(8) 2_666 1_565 ?
O12 K1 O4 124.73(9) 2_666 2_666 ?
O5 K1 O4 156.13(8) . 2_666 ?
O14 K1 O4 89.61(8) . 2_666 ?
O1 K1 O4 64.77(7) 2_666 2_666 ?
O4 K1 O4 65.85(9) 1_565 2_666 ?
O12 K1 C6 80.43(10) 2_666 1_565 ?
O5 K1 C6 72.39(8) . 1_565 ?
O14 K1 C6 98.49(10) . 1_565 ?
O1 K1 C6 166.33(9) 2_666 1_565 ?
O4 K1 C6 66.58(9) 1_565 1_565 ?
O4 K1 C6 110.32(8) 2_666 1_565 ?
O12 K1 C8 131.85(9) 2_666 2_666 ?
O5 K1 C8 142.21(8) . 2_666 ?
O14 K1 C8 77.44(8) . 2_666 ?
O1 K1 C8 52.08(8) 2_666 2_666 ?
O4 K1 C8 84.06(8) 1_565 2_666 ?
O4 K1 C8 19.27(8) 2_666 2_666 ?
C6 K1 C8 126.41(9) 1_565 2_666 ?
O12 K1 K1 98.35(7) 2_666 2_676 ?
O5 K1 K1 160.76(6) . 2_676 ?
O14 K1 K1 117.54(6) . 2_676 ?
O1 K1 K1 81.41(6) 2_666 2_676 ?
O4 K1 K1 33.05(5) 1_565 2_676 ?
O4 K1 K1 32.79(6) 2_666 2_676 ?
C6 K1 K1 88.37(7) 1_565 2_676 ?
C8 K1 K1 51.27(6) 2_666 2_676 ?
C1 O1 Bi1 85.91(19) . . ?
C1 O1 K1 134.0(2) . 2_666 ?
Bi1 O1 K1 116.08(9) . 2_666 ?
C1 O2 Bi1 97.71(19) . . ?
C8 O3 C7 117.2(3) . . ?
C8 O4 K1 132.1(2) . 1_545 ?
C8 O4 K1 109.5(2) . 2_666 ?
K1 O4 K1 114.15(9) 1_545 2_666 ?
C10 O5 Bi1 85.82(18) . . ?
C10 O5 K1 171.6(2) . . ?
Bi1 O5 K1 97.50(8) . . ?
C10 O6 Bi1 100.05(18) . . ?
C17 O7 C16 117.7(3) . . ?
C19 O9 Bi1 102.8(2) . . ?
C19 O10 Bi1 146.9(2) . 2_666 ?
C19 O10 Bi1 84.89(18) . . ?
Bi1 O10 Bi1 102.69(9) 2_666 . ?
C26 O11 C25 118.1(2) . . ?
C26 O12 K1 137.3(2) . 2_666 ?
C28 O13 Bi1 105.67(18) . . ?
C28 O14 K1 139.1(2) . . ?
C35 O15 C34 117.0(3) . . ?
O1 C1 O2 121.3(3) . . ?
O1 C1 C2 120.6(3) . . ?
O2 C1 C2 118.1(3) . . ?
C7 C2 C3 118.1(3) . . ?
C7 C2 C1 122.0(3) . . ?
C3 C2 C1 119.9(3) . . ?
C4 C3 C2 120.7(4) . . ?
C5 C4 C3 120.1(4) . . ?
C4 C5 C6 120.1(3) . . ?
C5 C6 C7 119.6(4) . . ?
C5 C6 K1 93.9(2) . 1_545 ?
C7 C6 K1 90.2(2) . 1_545 ?
C6 C7 C2 121.3(4) . . ?
C6 C7 O3 117.7(3) . . ?
C2 C7 O3 120.6(3) . . ?
O4 C8 O3 123.0(3) . . ?
O4 C8 C9 125.8(3) . . ?
O3 C8 C9 111.2(3) . . ?
O4 C8 K1 51.19(17) . 2_666 ?
O3 C8 K1 125.2(2) . 2_666 ?
C9 C8 K1 97.8(2) . 2_666 ?
O5 C10 O6 121.8(3) . . ?
O5 C10 C11 119.0(3) . . ?
O6 C10 C11 119.2(3) . . ?
C12 C11 C16 118.3(3) . . ?
C12 C11 C10 118.0(3) . . ?
C16 C11 C10 123.7(3) . . ?
C13 C12 C11 120.9(3) . . ?
C12 C13 C14 119.7(3) . . ?
C15 C14 C13 120.3(3) . . ?
C14 C15 C16 119.7(3) . . ?
C15 C16 C11 121.1(3) . . ?
C15 C16 O7 117.7(3) . . ?
C11 C16 O7 121.1(3) . . ?
O8 C17 O7 123.6(3) . . ?
O8 C17 C18 126.3(4) . . ?
O7 C17 C18 110.1(3) . . ?
O10 C19 O9 122.6(3) . . ?
O10 C19 C20 118.6(3) . . ?
O9 C19 C20 118.6(3) . . ?
C21 C20 C25 117.8(3) . . ?
C21 C20 C19 118.6(3) . . ?
C25 C20 C19 123.6(3) . . ?
C20 C21 C22 121.2(3) . . ?
C23 C22 C21 120.0(3) . . ?
C22 C23 C24 119.9(3) . . ?
C25 C24 C23 119.6(3) . . ?
C24 C25 O11 116.0(3) . . ?
C24 C25 C20 121.5(3) . . ?
O11 C25 C20 122.5(3) . . ?
O12 C26 O11 123.8(3) . . ?
O12 C26 C27 125.5(3) . . ?
O11 C26 C27 110.6(3) . . ?
O14 C28 O13 122.7(3) . . ?
O14 C28 C29 119.8(3) . . ?
O13 C28 C29 117.4(3) . . ?
C30 C29 C34 117.9(3) . . ?
C30 C29 C28 118.1(3) . . ?
C34 C29 C28 124.0(3) . . ?
C31 C30 C29 121.4(3) . . ?
C30 C31 C32 119.7(3) . . ?
C33 C32 C31 119.7(3) . . ?
C34 C33 C32 120.1(3) . . ?
C33 C34 O15 116.5(3) . . ?
C33 C34 C29 121.2(3) . . ?
O15 C34 C29 122.3(3) . . ?
O16 C35 O15 123.2(3) . . ?
O16 C35 C36 127.6(3) . . ?
O15 C35 C36 109.1(3) . . ?
_diffrn_measured_fraction_theta_max 0.936
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.130