# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_11

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 O5 Pb'
_chemical_formula_weight         445.42

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'
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   Iba2

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

_cell_length_a                   16.2354(8)
_cell_length_b                   19.1181(10)
_cell_length_c                   8.2268(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2553.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2991
_cell_measurement_theta_min      3.6680
_cell_measurement_theta_max      27.668

_exptl_crystal_description       needle-like
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    13.224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0661
_exptl_absorpt_correction_T_max  0.2998
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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  'Xcalibur, Eos, Gemini'
_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            14881
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         26.37
_reflns_number_total             2608
_reflns_number_gt                1698
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;

_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)+(0.0265P)²+9.6047P] where P=(Fo²+2Fc²)/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       0.00164(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_number_reflns         2608
_refine_ls_number_parameters     155
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0798
_refine_ls_wR_factor_gt          0.0678
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.024
_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
Pb1 Pb -0.00001(3) 0.878750(13) 0.6728(5) 0.02510(16) Uani 1 1 d . . .
O1 O 0.1097(4) 0.9112(3) 0.4186(12) 0.0341(15) Uani 1 1 d . . .
O2 O 0.1377(5) 0.8391(5) 0.6153(10) 0.052(2) Uani 1 1 d . . .
O3 O 0.4058(5) 0.7159(4) 0.6389(10) 0.054(2) Uani 1 1 d . . .
O4 O 0.4706(4) 0.6959(3) 0.4072(12) 0.0361(17) Uani 1 1 d . . .
O5 O 0.1044(6) 0.9486(4) 0.9176(18) 0.080(3) Uani 1 1 d . . .
H5A H 0.1009 0.9929 0.9166 0.097 Uiso 1 1 d R . .
H5B H 0.1333 0.9316 0.8410 0.097 Uiso 1 1 d R . .
C1 C 0.1590(7) 0.8675(5) 0.4820(13) 0.031(3) Uani 1 1 d . . .
C2 C 0.2378(5) 0.8480(4) 0.4072(15) 0.0208(19) Uani 1 1 d . . .
C3 C 0.2875(6) 0.7997(5) 0.4834(12) 0.028(2) Uani 1 1 d . . .
H3 H 0.2719 0.7799 0.5819 0.034 Uiso 1 1 calc R . .
C4 C 0.3612(5) 0.7811(4) 0.4102(15) 0.027(2) Uani 1 1 d . . .
C5 C 0.4163(8) 0.7275(6) 0.4872(15) 0.049(2) Uani 1 1 d . . .
C6 C 0.3854(7) 0.8124(5) 0.2622(12) 0.028(2) Uani 1 1 d . . .
H6 H 0.4344 0.7987 0.2130 0.033 Uiso 1 1 calc R . .
C7 C 0.3383(7) 0.8621(5) 0.1908(13) 0.028(2) Uani 1 1 d . . .
C8 C 0.2622(9) 0.8803(6) 0.2625(15) 0.049(2) Uani 1 1 d . . .
H8 H 0.2285 0.9136 0.2137 0.058 Uiso 1 1 calc R . .
C9 C 0.3644(7) 0.8996(6) 0.0330(14) 0.039(3) Uani 1 1 d . . .
C10 C 0.4563(8) 0.8963(6) 0.0113(15) 0.049(2) Uani 1 1 d . . .
H10A H 0.4698 0.8587 -0.0614 0.073 Uiso 1 1 calc R . .
H10B H 0.4820 0.8883 0.1147 0.073 Uiso 1 1 calc R . .
H10C H 0.4756 0.9396 -0.0333 0.073 Uiso 1 1 calc R . .
C11 C 0.3224(16) 0.8621(9) -0.1064(19) 0.119(8) Uani 1 1 d . . .
H11B H 0.2647 0.8576 -0.0836 0.178 Uiso 1 1 calc R . .
H11A H 0.3462 0.8164 -0.1192 0.178 Uiso 1 1 calc R . .
H11C H 0.3298 0.8884 -0.2047 0.178 Uiso 1 1 calc R . .
C12 C 0.3401(10) 0.9741(7) 0.0259(18) 0.065(4) Uani 1 1 d . . .
H12B H 0.3526 0.9963 0.1277 0.098 Uiso 1 1 calc R . .
H12A H 0.2821 0.9775 0.0050 0.098 Uiso 1 1 calc R . .
H12C H 0.3699 0.9970 -0.0597 0.098 Uiso 1 1 calc R . .


_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 2.385(7) 8_464 ?
Pb1 O2 2.408(8) . ?
Pb1 O4 2.446(10) 6_565 ?
Pb1 O4 2.653(10) 8_464 ?
O1 C1 1.269(12) . ?
O2 C1 1.271(12) . ?
O3 C5 1.279(13) . ?
O3 Pb1 2.385(7) 8_564 ?
O4 C5 1.254(14) . ?
O4 Pb1 2.446(10) 6_564 ?
O4 Pb1 2.653(10) 8_564 ?
C1 C2 1.469(14) . ?
C2 C3 1.377(13) . ?
C2 C8 1.398(16) . ?
C3 C4 1.386(13) . ?
C4 C6 1.412(15) . ?
C4 C5 1.501(14) . ?
C6 C7 1.354(14) . ?
C7 C8 1.412(16) . ?
C7 C9 1.542(15) . ?
C9 C12 1.480(16) . ?
C9 C10 1.504(16) . ?
C9 C11 1.51(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 O2 109.5(3) 8_464 . ?
O3 Pb1 O4 77.0(3) 8_464 6_565 ?
O2 Pb1 O4 77.9(3) . 6_565 ?
O3 Pb1 O4 51.7(3) 8_464 8_464 ?
O2 Pb1 O4 80.6(3) . 8_464 ?
O4 Pb1 O4 111.8(2) 6_565 8_464 ?
C1 O2 Pb1 106.7(7) . . ?
C5 O3 Pb1 99.2(7) . 8_564 ?
C5 O4 Pb1 146.3(8) . 6_564 ?
C5 O4 Pb1 87.3(7) . 8_564 ?
Pb1 O4 Pb1 107.5(2) 6_564 8_564 ?
O1 C1 O2 117.7(10) . . ?
O1 C1 C2 123.0(10) . . ?
O2 C1 C2 119.3(10) . . ?
C3 C2 C8 121.2(10) . . ?
C3 C2 C1 119.3(11) . . ?
C8 C2 C1 119.5(9) . . ?
C2 C3 C4 118.7(10) . . ?
C3 C4 C6 120.4(9) . . ?
C3 C4 C5 120.4(11) . . ?
C6 C4 C5 119.2(9) . . ?
O4 C5 O3 121.5(11) . . ?
O4 C5 C4 121.7(10) . . ?
O3 C5 C4 116.8(11) . . ?
C7 C6 C4 120.9(10) . . ?
C6 C7 C8 119.1(10) . . ?
C6 C7 C9 122.4(10) . . ?
C8 C7 C9 118.5(10) . . ?
C2 C8 C7 119.6(10) . . ?
C12 C9 C10 107.5(11) . . ?
C12 C9 C11 107.9(14) . . ?
C10 C9 C11 109.6(13) . . ?
C12 C9 C7 114.1(10) . . ?
C10 C9 C7 110.7(10) . . ?
C11 C9 C7 107.1(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Pb1 O2 C1 109.5(7) 8_464 . . . ?
O4 Pb1 O2 C1 -179.2(8) 6_565 . . . ?
O4 Pb1 O2 C1 65.9(7) 8_464 . . . ?
Pb1 O2 C1 O1 4.8(12) . . . . ?
Pb1 O2 C1 C2 -174.4(7) . . . . ?
O1 C1 C2 C3 -179.5(10) . . . . ?
O2 C1 C2 C3 -0.3(15) . . . . ?
O1 C1 C2 C8 2.3(16) . . . . ?
O2 C1 C2 C8 -178.6(11) . . . . ?
C8 C2 C3 C4 -2.7(15) . . . . ?
C1 C2 C3 C4 179.1(9) . . . . ?
C2 C3 C4 C6 1.3(14) . . . . ?
C2 C3 C4 C5 -178.6(10) . . . . ?
Pb1 O4 C5 O3 123.3(14) 6_564 . . . ?
Pb1 O4 C5 O3 5.2(12) 8_564 . . . ?
Pb1 O4 C5 C4 -57.3(18) 6_564 . . . ?
Pb1 O4 C5 C4 -175.4(10) 8_564 . . . ?
Pb1 O3 C5 O4 -5.8(14) 8_564 . . . ?
Pb1 O3 C5 C4 174.8(8) 8_564 . . . ?
C3 C4 C5 O4 160.5(11) . . . . ?
C6 C4 C5 O4 -19.5(16) . . . . ?
C3 C4 C5 O3 -20.1(15) . . . . ?
C6 C4 C5 O3 160.0(11) . . . . ?
C3 C4 C6 C7 1.5(16) . . . . ?
C5 C4 C6 C7 -178.5(10) . . . . ?
C4 C6 C7 C8 -2.9(16) . . . . ?
C4 C6 C7 C9 177.4(10) . . . . ?
C3 C2 C8 C7 1.3(17) . . . . ?
C1 C2 C8 C7 179.5(10) . . . . ?
C6 C7 C8 C2 1.5(16) . . . . ?
C9 C7 C8 C2 -178.8(11) . . . . ?
C6 C7 C9 C12 -144.2(12) . . . . ?
C8 C7 C9 C12 36.1(16) . . . . ?
C6 C7 C9 C10 -22.8(16) . . . . ?
C8 C7 C9 C10 157.5(11) . . . . ?
C6 C7 C9 C11 96.6(16) . . . . ?
C8 C7 C9 C11 -83.1(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.362
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.164
_database_code_depnum_ccdc_archive 'CCDC 1019800'
#######################################################################
#
#                 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_Pb2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 O9 Pb3'
_chemical_formula_weight         1078.00

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'
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   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                   18.7933(9)
_cell_length_b                   17.7755(6)
_cell_length_c                   8.2471(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.723(4)
_cell_angle_gamma                90.00
_cell_volume                     2715.46(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4315
_cell_measurement_theta_min      3.2730
_cell_measurement_theta_max      27.8990

_exptl_crystal_description       sheet-like
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    18.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0613
_exptl_absorpt_correction_T_max  0.2137
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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  'Xcalibur, Eos, Gemini'
_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            16537
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5542
_reflns_number_gt                3824
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_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.The largest residual density peak (4.763) in the final difference Fourier map is 0.985 ? from atom Pb1. The highest peak is due to the so-called heavy atom effect, since extremely heavy elements are present in this structure: Zmax = 82  
;

_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)+(0.0721P)²+0.0000P] where P=(Fo²+2Fc²)/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         5542
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1551
_refine_ls_wR_factor_gt          0.1319
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.18177(3) 0.51952(2) 0.04343(5) 0.02739(12) Uani 1 1 d . . .
Pb2 Pb 0.01333(3) 0.45338(2) 0.20498(5) 0.02699(12) Uani 1 1 d . . .
Pb3 Pb 0.05987(3) 0.65952(2) 0.16916(6) 0.03468(14) Uani 1 1 d . . .
O9 O 0.0616(4) 0.5459(4) 0.0430(8) 0.0237(19) Uani 1 1 d . . .
O6 O -0.1025(5) 0.5103(4) 0.2604(9) 0.033(2) Uani 1 1 d . . .
O1 O 0.1631(5) 0.5701(5) 0.3096(9) 0.044(3) Uani 1 1 d . . .
O5 O -0.0113(5) 0.5844(5) 0.3627(9) 0.038(2) Uani 1 1 d . . .
C16 C -0.2014(7) 0.6131(6) 0.3554(13) 0.028(3) Uani 1 1 d . . .
H16 H -0.2166 0.5634 0.3408 0.034 Uiso 1 1 calc R . .
O2 O 0.2792(6) 0.5651(6) 0.3018(11) 0.062(3) Uani 1 1 d . . .
C4 C 0.1879(7) 0.6374(6) 0.6231(13) 0.030(3) Uani 1 1 d . . .
H4 H 0.1402 0.6353 0.5698 0.036 Uiso 1 1 calc R . .
C15 C -0.1048(7) 0.7038(6) 0.3935(12) 0.029(3) Uani 1 1 d . . .
H15 H -0.0559 0.7148 0.4044 0.035 Uiso 1 1 calc R . .
C13 C -0.0789(7) 0.5705(7) 0.3287(13) 0.030(3) Uani 1 1 d . . .
C14 C -0.1295(7) 0.6310(7) 0.3635(14) 0.032(3) Uani 1 1 d . . .
C7 C 0.2758(8) 0.6645(6) 0.8635(14) 0.035(3) Uani 1 1 d . . .
H7 H 0.2856 0.6810 0.9720 0.042 Uiso 1 1 calc R . .
C3 C 0.3160(7) 0.6187(7) 0.6253(13) 0.036(3) Uani 1 1 d . . .
H3 H 0.3527 0.6052 0.5683 0.043 Uiso 1 1 calc R . .
C6 C 0.2050(7) 0.6631(7) 0.7835(13) 0.032(3) Uani 1 1 d . . .
C2 C 0.2434(8) 0.6152(7) 0.5451(12) 0.032(3) Uani 1 1 d . . .
C8 C 0.3332(7) 0.6419(7) 0.7867(15) 0.034(3) Uani 1 1 d . . .
C20 C -0.2521(7) 0.6708(7) 0.3693(14) 0.035(3) Uani 1 1 d . . .
C1 C 0.2282(9) 0.5827(7) 0.3740(16) 0.045(4) Uani 1 1 d . . .
C21 C -0.3306(8) 0.6475(7) 0.3646(18) 0.048(4) Uani 1 1 d . . .
C11 C 0.4124(9) 0.5946(10) 1.0398(16) 0.066(3) Uani 1 1 d . . .
H11B H 0.3807 0.6157 1.1075 0.099 Uiso 1 1 calc R . .
H11C H 0.4608 0.5934 1.1003 0.099 Uiso 1 1 calc R . .
H11A H 0.3972 0.5444 1.0084 0.099 Uiso 1 1 calc R . .
C9 C 0.4104(8) 0.6435(8) 0.8839(15) 0.043(4) Uani 1 1 d . . .
C12 C 0.4296(9) 0.7247(10) 0.9398(17) 0.066(3) Uani 1 1 d . . .
H12A H 0.4289 0.7562 0.8450 0.099 Uiso 1 1 calc R . .
H12C H 0.4769 0.7256 1.0054 0.099 Uiso 1 1 calc R . .
H12B H 0.3950 0.7428 1.0037 0.099 Uiso 1 1 calc R . .
C24 C -0.3816(9) 0.7140(9) 0.347(2) 0.075(3) Uani 1 1 d . . .
H24C H -0.3763 0.7407 0.4500 0.113 Uiso 1 1 calc R . .
H24A H -0.4304 0.6965 0.3181 0.113 Uiso 1 1 calc R . .
H24B H -0.3704 0.7471 0.2632 0.113 Uiso 1 1 calc R . .
C10 C 0.4660(9) 0.6165(11) 0.7820(17) 0.066(3) Uani 1 1 d . . .
H10A H 0.4530 0.5672 0.7393 0.099 Uiso 1 1 calc R . .
H10C H 0.5128 0.6146 0.8502 0.099 Uiso 1 1 calc R . .
H10B H 0.4673 0.6507 0.6925 0.099 Uiso 1 1 calc R . .
C22 C -0.3398(9) 0.6013(10) 0.521(2) 0.075(3) Uani 1 1 d . . .
H22A H -0.3059 0.5605 0.5347 0.113 Uiso 1 1 calc R . .
H22B H -0.3880 0.5817 0.5080 0.113 Uiso 1 1 calc R . .
H22C H -0.3310 0.6334 0.6157 0.113 Uiso 1 1 calc R . .
C23 C -0.3562(9) 0.5969(10) 0.212(2) 0.075(3) Uani 1 1 d . . .
H23B H -0.3550 0.6254 0.1133 0.113 Uiso 1 1 calc R . .
H23C H -0.4046 0.5801 0.2133 0.113 Uiso 1 1 calc R . .
H23A H -0.3248 0.5542 0.2144 0.113 Uiso 1 1 calc R . .
C18 C -0.1552(7) 0.7606(6) 0.4071(13) 0.027(3) Uani 1 1 d . . .
C17 C -0.1317(9) 0.8411(7) 0.4223(16) 0.0454(17) Uani 1 1 d . . .
C19 C -0.2269(8) 0.7427(6) 0.3941(15) 0.040(4) Uani 1 1 d . . .
H19 H -0.2598 0.7811 0.4024 0.048 Uiso 1 1 calc R . .
O7 O -0.0676(6) 0.8553(5) 0.4825(11) 0.0454(17) Uani 1 1 d . . .
O8 O -0.1764(5) 0.8920(5) 0.3730(10) 0.0454(17) Uani 1 1 d . . .
O3 O 0.1624(6) 0.6760(5) 1.0335(11) 0.0499(17) Uani 1 1 d . . .
O4 O 0.0803(6) 0.6858(5) 0.8097(11) 0.0499(17) Uani 1 1 d . . .
C5 C 0.1461(9) 0.6778(8) 0.8812(17) 0.0499(17) Uani 1 1 d . . .


_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 O9 2.306(8) . ?
Pb1 O8 2.376(8) 2_545 ?
Pb1 O1 2.452(8) . ?
Pb1 O2 2.688(9) . ?
Pb1 O6 2.742(7) 3_565 ?
Pb1 Pb3 3.6496(7) . ?
Pb2 O9 2.279(7) 3_565 ?
Pb2 O9 2.393(7) . ?
Pb2 O6 2.510(9) . ?
Pb2 O7 2.646(9) 2_545 ?
Pb2 O5 2.744(8) . ?
Pb3 O9 2.274(7) . ?
Pb3 O3 2.403(10) 1_554 ?
Pb3 O5 2.615(9) . ?
Pb3 O1 2.622(9) . ?
Pb3 O7 2.634(9) 4_575 ?
O9 Pb2 2.279(7) 3_565 ?
O6 C13 1.256(13) . ?
O6 Pb1 2.742(7) 3_565 ?
O1 C1 1.268(17) . ?
O5 C13 1.277(15) . ?
C16 C14 1.378(17) . ?
C16 C20 1.417(17) . ?
C16 H16 0.9300 . ?
O2 C1 1.250(18) . ?
C4 C2 1.373(18) . ?
C4 C6 1.385(15) . ?
C4 H4 0.9300 . ?
C15 C14 1.384(15) . ?
C15 C18 1.402(16) . ?
C15 H15 0.9300 . ?
C13 C14 1.495(18) . ?
C7 C6 1.382(18) . ?
C7 C8 1.399(19) . ?
C7 H7 0.9300 . ?
C3 C8 1.378(16) . ?
C3 C2 1.413(17) . ?
C3 H3 0.9300 . ?
C6 C5 1.50(2) . ?
C2 C1 1.507(17) . ?
C8 C9 1.534(17) . ?
C20 C19 1.367(17) . ?
C20 C21 1.53(2) . ?
C21 C24 1.51(2) . ?
C21 C23 1.56(2) . ?
C21 C22 1.56(2) . ?
C11 C9 1.547(19) . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 H11A 0.9600 . ?
C9 C10 1.52(2) . ?
C9 C12 1.54(2) . ?
C12 H12A 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10C 0.9600 . ?
C10 H10B 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C23 H23A 0.9600 . ?
C18 C19 1.371(18) . ?
C18 C17 1.496(17) . ?
C17 O7 1.247(17) . ?
C17 O8 1.255(16) . ?
C19 H19 0.9300 . ?
O7 Pb3 2.634(9) 4_576 ?
O7 Pb2 2.646(9) 2 ?
O8 Pb1 2.376(8) 2 ?
O3 C5 1.242(15) . ?
O3 Pb3 2.403(10) 1_556 ?
O4 C5 1.285(18) . ?

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 Pb1 O8 96.0(3) . 2_545 ?
O9 Pb1 O1 68.8(3) . . ?
O8 Pb1 O1 94.0(3) 2_545 . ?
O9 Pb1 O2 118.4(3) . . ?
O8 Pb1 O2 96.6(3) 2_545 . ?
O1 Pb1 O2 50.3(3) . . ?
O9 Pb1 O6 69.9(3) . 3_565 ?
O8 Pb1 O6 92.1(3) 2_545 3_565 ?
O1 Pb1 O6 138.7(3) . 3_565 ?
O2 Pb1 O6 167.1(3) . 3_565 ?
O9 Pb1 Pb3 36.86(17) . . ?
O8 Pb1 Pb3 120.6(2) 2_545 . ?
O1 Pb1 Pb3 45.9(2) . . ?
O2 Pb1 Pb3 86.9(2) . . ?
O6 Pb1 Pb3 96.94(17) 3_565 . ?
O9 Pb2 O9 74.4(3) 3_565 . ?
O9 Pb2 O6 74.8(2) 3_565 . ?
O9 Pb2 O6 104.3(2) . . ?
O9 Pb2 O7 73.7(3) 3_565 2_545 ?
O9 Pb2 O7 84.6(3) . 2_545 ?
O6 Pb2 O7 143.5(3) . 2_545 ?
O9 Pb2 O5 107.0(2) 3_565 . ?
O9 Pb2 O5 77.9(2) . . ?
O6 Pb2 O5 49.5(3) . . ?
O7 Pb2 O5 161.5(3) 2_545 . ?
O9 Pb3 O3 79.6(3) . 1_554 ?
O9 Pb3 O5 82.8(3) . . ?
O3 Pb3 O5 151.5(3) 1_554 . ?
O9 Pb3 O1 66.2(3) . . ?
O3 Pb3 O1 71.8(3) 1_554 . ?
O5 Pb3 O1 80.6(3) . . ?
O9 Pb3 O7 74.1(3) . 4_575 ?
O3 Pb3 O7 117.5(3) 1_554 4_575 ?
O5 Pb3 O7 78.3(3) . 4_575 ?
O1 Pb3 O7 136.9(3) . 4_575 ?
O9 Pb3 Pb1 37.5(2) . . ?
O3 Pb3 Pb1 50.2(2) 1_554 . ?
O5 Pb3 Pb1 103.61(18) . . ?
O1 Pb3 Pb1 42.17(18) . . ?
O7 Pb3 Pb1 108.57(19) 4_575 . ?
Pb3 O9 Pb2 110.6(3) . 3_565 ?
Pb3 O9 Pb1 105.7(3) . . ?
Pb2 O9 Pb1 117.3(3) 3_565 . ?
Pb3 O9 Pb2 108.6(3) . . ?
Pb2 O9 Pb2 105.6(3) 3_565 . ?
Pb1 O9 Pb2 108.8(3) . . ?
C13 O6 Pb2 100.0(8) . . ?
C13 O6 Pb1 132.2(7) . 3_565 ?
Pb2 O6 Pb1 96.3(2) . 3_565 ?
C1 O1 Pb1 99.6(9) . . ?
C1 O1 Pb3 131.9(8) . . ?
Pb1 O1 Pb3 91.9(2) . . ?
C13 O5 Pb3 123.8(7) . . ?
C13 O5 Pb2 88.5(7) . . ?
Pb3 O5 Pb2 90.0(3) . . ?
C14 C16 C20 119.7(11) . . ?
C14 C16 H16 120.1 . . ?
C20 C16 H16 120.1 . . ?
C1 O2 Pb1 88.8(8) . . ?
C2 C4 C6 118.1(12) . . ?
C2 C4 H4 121.0 . . ?
C6 C4 H4 121.0 . . ?
C14 C15 C18 118.5(12) . . ?
C14 C15 H15 120.7 . . ?
C18 C15 H15 120.7 . . ?
O6 C13 O5 121.7(12) . . ?
O6 C13 C14 120.7(11) . . ?
O5 C13 C14 117.5(10) . . ?
C16 C14 C15 121.4(12) . . ?
C16 C14 C13 118.4(10) . . ?
C15 C14 C13 120.1(12) . . ?
C6 C7 C8 122.2(11) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C8 C3 C2 121.1(13) . . ?
C8 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C7 C6 C4 120.7(12) . . ?
C7 C6 C5 118.6(11) . . ?
C4 C6 C5 119.9(12) . . ?
C4 C2 C3 121.1(10) . . ?
C4 C2 C1 120.7(12) . . ?
C3 C2 C1 118.1(13) . . ?
C3 C8 C7 116.7(12) . . ?
C3 C8 C9 123.8(12) . . ?
C7 C8 C9 119.4(11) . . ?
C19 C20 C16 118.0(13) . . ?
C19 C20 C21 124.4(12) . . ?
C16 C20 C21 117.5(11) . . ?
O2 C1 O1 121.2(12) . . ?
O2 C1 C2 120.2(13) . . ?
O1 C1 C2 118.5(13) . . ?
C24 C21 C20 112.6(12) . . ?
C24 C21 C23 105.7(12) . . ?
C20 C21 C23 110.0(13) . . ?
C24 C21 C22 109.4(14) . . ?
C20 C21 C22 111.2(11) . . ?
C23 C21 C22 107.6(12) . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
H11B C11 H11A 109.5 . . ?
H11C C11 H11A 109.5 . . ?
C10 C9 C8 112.5(11) . . ?
C10 C9 C12 108.1(13) . . ?
C8 C9 C12 109.1(11) . . ?
C10 C9 C11 111.0(12) . . ?
C8 C9 C11 108.2(12) . . ?
C12 C9 C11 107.8(11) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24C C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10C C10 H10B 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
C19 C18 C15 119.7(11) . . ?
C19 C18 C17 120.1(11) . . ?
C15 C18 C17 120.0(12) . . ?
O7 C17 O8 122.0(12) . . ?
O7 C17 C18 118.7(12) . . ?
O8 C17 C18 119.3(13) . . ?
C20 C19 C18 122.6(12) . . ?
C20 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
C17 O7 Pb3 159.0(8) . 4_576 ?
C17 O7 Pb2 110.0(8) . 2 ?
Pb3 O7 Pb2 90.3(3) 4_576 2 ?
C17 O8 Pb1 130.8(8) . 2 ?
C5 O3 Pb3 113.3(10) . 1_556 ?
O3 C5 O4 121.3(14) . . ?
O3 C5 C6 117.5(13) . . ?
O4 C5 C6 120.9(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 Pb1 Pb3 O9 -54.2(4) 2_545 . . . ?
O1 Pb1 Pb3 O9 -117.0(4) . . . . ?
O2 Pb1 Pb3 O9 -150.0(4) . . . . ?
O6 Pb1 Pb3 O9 42.4(3) 3_565 . . . ?
O9 Pb1 Pb3 O3 -134.7(4) . . . 1_554 ?
O8 Pb1 Pb3 O3 171.1(4) 2_545 . . 1_554 ?
O1 Pb1 Pb3 O3 108.3(4) . . . 1_554 ?
O2 Pb1 Pb3 O3 75.3(4) . . . 1_554 ?
O6 Pb1 Pb3 O3 -92.3(3) 3_565 . . 1_554 ?
O9 Pb1 Pb3 O5 58.1(3) . . . . ?
O8 Pb1 Pb3 O5 3.8(3) 2_545 . . . ?
O1 Pb1 Pb3 O5 -58.9(4) . . . . ?
O2 Pb1 Pb3 O5 -91.9(3) . . . . ?
O6 Pb1 Pb3 O5 100.5(3) 3_565 . . . ?
O9 Pb1 Pb3 O1 117.0(4) . . . . ?
O8 Pb1 Pb3 O1 62.7(4) 2_545 . . . ?
O2 Pb1 Pb3 O1 -33.0(4) . . . . ?
O6 Pb1 Pb3 O1 159.4(4) 3_565 . . . ?
O9 Pb1 Pb3 O7 -23.9(4) . . . 4_575 ?
O8 Pb1 Pb3 O7 -78.2(3) 2_545 . . 4_575 ?
O1 Pb1 Pb3 O7 -140.9(4) . . . 4_575 ?
O2 Pb1 Pb3 O7 -173.9(3) . . . 4_575 ?
O6 Pb1 Pb3 O7 18.5(3) 3_565 . . 4_575 ?
O3 Pb3 O9 Pb2 -94.2(4) 1_554 . . 3_565 ?
O5 Pb3 O9 Pb2 108.3(3) . . . 3_565 ?
O1 Pb3 O9 Pb2 -168.7(4) . . . 3_565 ?
O7 Pb3 O9 Pb2 28.5(3) 4_575 . . 3_565 ?
Pb1 Pb3 O9 Pb2 -127.9(5) . . . 3_565 ?
O3 Pb3 O9 Pb1 33.7(3) 1_554 . . . ?
O5 Pb3 O9 Pb1 -123.7(3) . . . . ?
O1 Pb3 O9 Pb1 -40.8(3) . . . . ?
O7 Pb3 O9 Pb1 156.4(3) 4_575 . . . ?
O3 Pb3 O9 Pb2 150.4(3) 1_554 . . . ?
O5 Pb3 O9 Pb2 -7.1(3) . . . . ?
O1 Pb3 O9 Pb2 75.8(3) . . . . ?
O7 Pb3 O9 Pb2 -86.9(3) 4_575 . . . ?
Pb1 Pb3 O9 Pb2 116.6(4) . . . . ?
O8 Pb1 O9 Pb3 135.4(3) 2_545 . . . ?
O1 Pb1 O9 Pb3 43.3(3) . . . . ?
O2 Pb1 O9 Pb3 34.5(4) . . . . ?
O6 Pb1 O9 Pb3 -134.6(3) 3_565 . . . ?
O8 Pb1 O9 Pb2 -100.9(3) 2_545 . . 3_565 ?
O1 Pb1 O9 Pb2 167.1(4) . . . 3_565 ?
O2 Pb1 O9 Pb2 158.3(3) . . . 3_565 ?
O6 Pb1 O9 Pb2 -10.8(3) 3_565 . . 3_565 ?
Pb3 Pb1 O9 Pb2 123.8(5) . . . 3_565 ?
O8 Pb1 O9 Pb2 18.9(3) 2_545 . . . ?
O1 Pb1 O9 Pb2 -73.1(3) . . . . ?
O2 Pb1 O9 Pb2 -81.9(4) . . . . ?
O6 Pb1 O9 Pb2 109.0(3) 3_565 . . . ?
Pb3 Pb1 O9 Pb2 -116.5(4) . . . . ?
O9 Pb2 O9 Pb3 118.6(4) 3_565 . . . ?
O6 Pb2 O9 Pb3 49.2(3) . . . . ?
O7 Pb2 O9 Pb3 -166.8(3) 2_545 . . . ?
O5 Pb2 O9 Pb3 6.9(3) . . . . ?
O9 Pb2 O9 Pb2 0.0 3_565 . . 3_565 ?
O6 Pb2 O9 Pb2 -69.4(3) . . . 3_565 ?
O7 Pb2 O9 Pb2 74.6(3) 2_545 . . 3_565 ?
O5 Pb2 O9 Pb2 -111.7(3) . . . 3_565 ?
O9 Pb2 O9 Pb1 -126.8(4) 3_565 . . . ?
O6 Pb2 O9 Pb1 163.8(3) . . . . ?
O7 Pb2 O9 Pb1 -52.2(3) 2_545 . . . ?
O5 Pb2 O9 Pb1 121.5(3) . . . . ?
O9 Pb2 O6 C13 -126.3(7) 3_565 . . . ?
O9 Pb2 O6 C13 -57.2(7) . . . . ?
O7 Pb2 O6 C13 -157.6(6) 2_545 . . . ?
O5 Pb2 O6 C13 2.8(6) . . . . ?
O9 Pb2 O6 Pb1 8.6(2) 3_565 . . 3_565 ?
O9 Pb2 O6 Pb1 77.7(3) . . . 3_565 ?
O7 Pb2 O6 Pb1 -22.8(5) 2_545 . . 3_565 ?
O5 Pb2 O6 Pb1 137.7(4) . . . 3_565 ?
O9 Pb1 O1 C1 -168.0(8) . . . . ?
O8 Pb1 O1 C1 97.1(8) 2_545 . . . ?
O2 Pb1 O1 C1 1.9(7) . . . . ?
O6 Pb1 O1 C1 -165.1(7) 3_565 . . . ?
Pb3 Pb1 O1 C1 -133.1(9) . . . . ?
O9 Pb1 O1 Pb3 -35.0(2) . . . . ?
O8 Pb1 O1 Pb3 -129.9(3) 2_545 . . . ?
O2 Pb1 O1 Pb3 134.9(5) . . . . ?
O6 Pb1 O1 Pb3 -32.0(5) 3_565 . . . ?
O9 Pb3 O1 C1 141.0(12) . . . . ?
O3 Pb3 O1 C1 54.6(12) 1_554 . . . ?
O5 Pb3 O1 C1 -132.8(12) . . . . ?
O7 Pb3 O1 C1 165.7(11) 4_575 . . . ?
Pb1 Pb3 O1 C1 104.7(12) . . . . ?
O9 Pb3 O1 Pb1 36.3(3) . . . . ?
O3 Pb3 O1 Pb1 -50.1(3) 1_554 . . . ?
O5 Pb3 O1 Pb1 122.5(3) . . . . ?
O7 Pb3 O1 Pb1 61.0(5) 4_575 . . . ?
O9 Pb3 O5 C13 -82.3(9) . . . . ?
O3 Pb3 O5 C13 -134.5(9) 1_554 . . . ?
O1 Pb3 O5 C13 -149.3(9) . . . . ?
O7 Pb3 O5 C13 -7.1(9) 4_575 . . . ?
Pb1 Pb3 O5 C13 -113.7(9) . . . . ?
O9 Pb3 O5 Pb2 5.9(2) . . . . ?
O3 Pb3 O5 Pb2 -46.3(7) 1_554 . . . ?
O1 Pb3 O5 Pb2 -61.1(3) . . . . ?
O7 Pb3 O5 Pb2 81.0(3) 4_575 . . . ?
Pb1 Pb3 O5 Pb2 -25.5(2) . . . . ?
O9 Pb2 O5 C13 48.9(7) 3_565 . . . ?
O9 Pb2 O5 C13 118.2(7) . . . . ?
O6 Pb2 O5 C13 -2.7(6) . . . . ?
O7 Pb2 O5 C13 138.4(9) 2_545 . . . ?
O9 Pb2 O5 Pb3 -75.0(3) 3_565 . . . ?
O9 Pb2 O5 Pb3 -5.7(2) . . . . ?
O6 Pb2 O5 Pb3 -126.6(4) . . . . ?
O7 Pb2 O5 Pb3 14.6(9) 2_545 . . . ?
O9 Pb1 O2 C1 8.8(9) . . . . ?
O8 Pb1 O2 C1 -91.7(8) 2_545 . . . ?
O1 Pb1 O2 C1 -1.9(7) . . . . ?
O6 Pb1 O2 C1 136.3(12) 3_565 . . . ?
Pb3 Pb1 O2 C1 28.7(8) . . . . ?
Pb2 O6 C13 O5 -5.4(12) . . . . ?
Pb1 O6 C13 O5 -113.5(11) 3_565 . . . ?
Pb2 O6 C13 C14 170.6(9) . . . . ?
Pb1 O6 C13 C14 62.5(15) 3_565 . . . ?
Pb3 O5 C13 O6 93.9(12) . . . . ?
Pb2 O5 C13 O6 4.9(10) . . . . ?
Pb3 O5 C13 C14 -82.3(12) . . . . ?
Pb2 O5 C13 C14 -171.3(9) . . . . ?
C20 C16 C14 C15 3.3(17) . . . . ?
C20 C16 C14 C13 -172.9(10) . . . . ?
C18 C15 C14 C16 -3.4(17) . . . . ?
C18 C15 C14 C13 172.8(10) . . . . ?
O6 C13 C14 C16 15.0(17) . . . . ?
O5 C13 C14 C16 -168.8(10) . . . . ?
O6 C13 C14 C15 -161.3(10) . . . . ?
O5 C13 C14 C15 14.9(16) . . . . ?
C8 C7 C6 C4 1.4(18) . . . . ?
C8 C7 C6 C5 171.5(11) . . . . ?
C2 C4 C6 C7 -1.6(17) . . . . ?
C2 C4 C6 C5 -171.6(11) . . . . ?
C6 C4 C2 C3 -0.3(17) . . . . ?
C6 C4 C2 C1 176.6(11) . . . . ?
C8 C3 C2 C4 2.5(18) . . . . ?
C8 C3 C2 C1 -174.5(11) . . . . ?
C2 C3 C8 C7 -2.6(18) . . . . ?
C2 C3 C8 C9 177.0(11) . . . . ?
C6 C7 C8 C3 0.7(18) . . . . ?
C6 C7 C8 C9 -178.9(11) . . . . ?
C14 C16 C20 C19 -1.3(17) . . . . ?
C14 C16 C20 C21 -178.2(11) . . . . ?
Pb1 O2 C1 O1 3.3(13) . . . . ?
Pb1 O2 C1 C2 179.5(11) . . . . ?
Pb1 O1 C1 O2 -3.7(14) . . . . ?
Pb3 O1 C1 O2 -105.0(14) . . . . ?
Pb1 O1 C1 C2 -179.9(9) . . . . ?
Pb3 O1 C1 C2 78.7(14) . . . . ?
C4 C2 C1 O2 177.5(12) . . . . ?
C3 C2 C1 O2 -5.5(18) . . . . ?
C4 C2 C1 O1 -6.2(18) . . . . ?
C3 C2 C1 O1 170.8(11) . . . . ?
C19 C20 C21 C24 14.4(19) . . . . ?
C16 C20 C21 C24 -168.9(12) . . . . ?
C19 C20 C21 C23 132.1(13) . . . . ?
C16 C20 C21 C23 -51.2(15) . . . . ?
C19 C20 C21 C22 -108.8(14) . . . . ?
C16 C20 C21 C22 67.8(15) . . . . ?
C3 C8 C9 C10 0.0(18) . . . . ?
C7 C8 C9 C10 179.6(12) . . . . ?
C3 C8 C9 C12 120.0(14) . . . . ?
C7 C8 C9 C12 -60.5(16) . . . . ?
C3 C8 C9 C11 -123.0(14) . . . . ?
C7 C8 C9 C11 56.6(16) . . . . ?
C14 C15 C18 C19 1.4(16) . . . . ?
C14 C15 C18 C17 -173.8(11) . . . . ?
C19 C18 C17 O7 158.6(12) . . . . ?
C15 C18 C17 O7 -26.2(18) . . . . ?
C19 C18 C17 O8 -22.1(18) . . . . ?
C15 C18 C17 O8 153.1(12) . . . . ?
C16 C20 C19 C18 -0.6(18) . . . . ?
C21 C20 C19 C18 176.1(12) . . . . ?
C15 C18 C19 C20 0.5(18) . . . . ?
C17 C18 C19 C20 175.7(11) . . . . ?
O8 C17 O7 Pb3 148.7(18) . . . 4_576 ?
C18 C17 O7 Pb3 -32(3) . . . 4_576 ?
O8 C17 O7 Pb2 -47.0(16) . . . 2 ?
C18 C17 O7 Pb2 132.2(10) . . . 2 ?
O7 C17 O8 Pb1 -27(2) . . . 2 ?
C18 C17 O8 Pb1 153.3(9) . . . 2 ?
Pb3 O3 C5 O4 13.4(17) 1_556 . . . ?
Pb3 O3 C5 C6 -160.9(9) 1_556 . . . ?
C7 C6 C5 O3 -13.8(18) . . . . ?
C4 C6 C5 O3 156.4(12) . . . . ?
C7 C6 C5 O4 171.9(12) . . . . ?
C4 C6 C5 O4 -17.9(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         4.763
_refine_diff_density_min         -2.910
_refine_diff_density_rms         0.386
_database_code_depnum_ccdc_archive 'CCDC 1019801'
#######################################################################
#
#                 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_Pb3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 O13 Pb4'
_chemical_formula_weight         1505.41

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'
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   Pna21

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

_cell_length_a                   18.4043(5)
_cell_length_b                   30.9956(9)
_cell_length_c                   6.9963(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3991.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5171
_cell_measurement_theta_min      3.6970
_cell_measurement_theta_max      28.6680

_exptl_crystal_description       prism-shaped
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2736
_exptl_absorpt_coefficient_mu    16.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2365
_exptl_absorpt_correction_T_max  0.4307
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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  'Xcalibur, Eos, Gemini'
_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            6388
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.02
_reflns_number_total             6388
_reflns_number_gt                5912
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_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)+(0.0374P)²+12.4369P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.038(13)
_refine_ls_number_reflns         6388
_refine_ls_number_parameters     526
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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 0.84720(2) 0.609348(12) 0.59338(9) 0.02196(11) Uani 1 1 d . . .
Pb2 Pb 1.03673(2) 0.659179(13) 0.57909(8) 0.02099(11) Uani 1 1 d . . .
Pb3 Pb 0.87300(2) 0.731954(12) 0.58826(9) 0.02146(11) Uani 1 1 d . . .
Pb4 Pb 1.08259(3) 0.333701(16) 0.50869(7) 0.02687(12) Uani 1 1 d . . .
O1 O 0.9583(5) 0.6089(3) 0.3871(14) 0.032(2) Uani 1 1 d . . .
O2 O 1.0661(6) 0.5775(3) 0.3800(17) 0.044(3) Uani 1 1 d . . .
O3 O 1.0746(5) 0.4150(3) 0.4172(13) 0.029(2) Uani 1 1 d . . .
O4 O 0.9702(5) 0.3794(3) 0.4064(13) 0.027(2) Uani 1 1 d . . .
O5 O 0.8159(5) 0.6705(3) 0.3892(13) 0.028(2) Uani 1 1 d . . .
O6 O 0.7146(6) 0.6335(3) 0.4376(16) 0.047(3) Uani 1 1 d . . .
O7 O 0.4762(6) 0.7138(3) 0.4129(16) 0.045(3) Uani 1 1 d . . .
O8 O 0.4817(5) 0.7840(3) 0.3830(12) 0.027(2) Uani 1 1 d . . .
O9 O 0.5476(6) 0.7841(3) 0.8331(18) 0.047(3) Uani 1 1 d . . .
O10 O 0.4448(5) 0.7476(3) 0.8701(15) 0.038(3) Uani 1 1 d . . .
O11 O 0.7866(5) 0.7082(3) 0.8581(14) 0.037(2) Uani 1 1 d . . .
O12 O 0.7899(5) 0.6384(3) 0.9047(13) 0.031(2) Uani 1 1 d . . .
O13 O 0.9188(4) 0.6667(2) 0.6825(12) 0.0174(18) Uani 1 1 d . . .
C1 C 1.0006(8) 0.5745(4) 0.3667(18) 0.023(3) Uani 1 1 d . . .
C2 C 0.9621(7) 0.5320(4) 0.3395(16) 0.021(3) Uani 1 1 d . . .
C3 C 0.8894(8) 0.5297(4) 0.2804(19) 0.028(3) Uani 1 1 d . . .
H3 H 0.8645 0.5552 0.2538 0.033 Uiso 1 1 calc R . .
C4 C 1.0007(9) 0.4946(4) 0.3737(17) 0.021(3) Uani 1 1 d . . .
H4 H 1.0499 0.4958 0.4042 0.026 Uiso 1 1 calc R . .
C5 C 0.9648(7) 0.4549(4) 0.3617(17) 0.022(3) Uani 1 1 d . . .
C6 C 1.0055(8) 0.4142(4) 0.4001(18) 0.022(3) Uani 1 1 d . . .
C7 C 0.8922(8) 0.4533(5) 0.310(2) 0.031(3) Uani 1 1 d . . .
H7 H 0.8687 0.4268 0.3076 0.038 Uiso 1 1 calc R . .
C8 C 0.8534(7) 0.4905(4) 0.2605(19) 0.028(3) Uani 1 1 d . A .
C9 C 0.7761(9) 0.4888(5) 0.188(2) 0.037(4) Uani 1 1 d . . .
C10 C 0.744(2) 0.4435(10) 0.197(6) 0.046(7) Uani 0.58(4) 1 d P A 1
H10A H 0.7752 0.4236 0.1338 0.069 Uiso 0.58(4) 1 calc PR A 1
H10B H 0.6969 0.4435 0.1360 0.069 Uiso 0.58(4) 1 calc PR A 1
H10C H 0.7380 0.4351 0.3287 0.069 Uiso 0.58(4) 1 calc PR A 1
C11 C 0.7265(17) 0.5193(13) 0.301(6) 0.049(7) Uani 0.58(4) 1 d P A 1
H11A H 0.7306 0.5132 0.4346 0.073 Uiso 0.58(4) 1 calc PR A 1
H11B H 0.6771 0.5153 0.2604 0.073 Uiso 0.58(4) 1 calc PR A 1
H11C H 0.7408 0.5487 0.2772 0.073 Uiso 0.58(4) 1 calc PR A 1
C12 C 0.776(2) 0.5036(14) -0.021(6) 0.056(8) Uani 0.58(4) 1 d P A 1
H12A H 0.8117 0.5256 -0.0391 0.084 Uiso 0.58(4) 1 calc PR A 1
H12B H 0.7287 0.5149 -0.0529 0.084 Uiso 0.58(4) 1 calc PR A 1
H12C H 0.7865 0.4795 -0.1027 0.084 Uiso 0.58(4) 1 calc PR A 1
C10' C 0.762(3) 0.5228(16) 0.034(7) 0.046(7) Uani 0.42(4) 1 d P A 2
H10D H 0.7712 0.5510 0.0855 0.069 Uiso 0.42(4) 1 calc PR A 2
H10E H 0.7119 0.5211 -0.0058 0.069 Uiso 0.42(4) 1 calc PR A 2
H10F H 0.7929 0.5177 -0.0733 0.069 Uiso 0.42(4) 1 calc PR A 2
C11' C 0.758(2) 0.4449(13) 0.102(11) 0.049(7) Uani 0.42(4) 1 d P A 2
H11D H 0.7979 0.4349 0.0269 0.073 Uiso 0.42(4) 1 calc PR A 2
H11E H 0.7155 0.4475 0.0222 0.073 Uiso 0.42(4) 1 calc PR A 2
H11F H 0.7480 0.4247 0.2029 0.073 Uiso 0.42(4) 1 calc PR A 2
C12' C 0.724(3) 0.4976(19) 0.352(8) 0.056(8) Uani 0.42(4) 1 d P A 2
H12D H 0.7216 0.4728 0.4345 0.084 Uiso 0.42(4) 1 calc PR A 2
H12E H 0.6760 0.5033 0.3018 0.084 Uiso 0.42(4) 1 calc PR A 2
H12F H 0.7400 0.5222 0.4237 0.084 Uiso 0.42(4) 1 calc PR A 2
C13 C 0.7449(8) 0.6671(5) 0.3858(19) 0.025(3) Uani 1 1 d . . .
C14 C 0.7028(7) 0.7064(4) 0.3321(18) 0.024(3) Uani 1 1 d . . .
C15 C 0.6298(8) 0.7078(5) 0.363(2) 0.025(3) Uani 1 1 d . . .
H15 H 0.6063 0.6836 0.4113 0.030 Uiso 1 1 calc R . .
C16 C 0.7379(8) 0.7434(4) 0.2588(18) 0.025(3) Uani 1 1 d . . .
H16 H 0.7877 0.7425 0.2375 0.030 Uiso 1 1 calc R . .
C17 C 0.5902(7) 0.7446(4) 0.3238(18) 0.024(3) Uani 1 1 d . . .
C18 C 0.5103(9) 0.7456(5) 0.3741(19) 0.026(3) Uani 1 1 d . . .
C19 C 0.6261(7) 0.7805(4) 0.2521(18) 0.027(3) Uani 1 1 d . . .
H19 H 0.5995 0.8054 0.2261 0.033 Uiso 1 1 calc R . .
C20 C 0.7007(7) 0.7806(4) 0.2180(17) 0.022(3) Uani 1 1 d . B .
C21 C 0.7398(8) 0.8209(4) 0.140(2) 0.031(3) Uani 1 1 d . . .
C22 C 0.8219(15) 0.8154(9) 0.134(5) 0.048(7) Uani 0.56(2) 1 d P B 1
H22A H 0.8447 0.8432 0.1281 0.072 Uiso 0.56(2) 1 calc PR B 1
H22B H 0.8351 0.7989 0.0230 0.072 Uiso 0.56(2) 1 calc PR B 1
H22C H 0.8378 0.8005 0.2468 0.072 Uiso 0.56(2) 1 calc PR B 1
C23 C 0.714(2) 0.8252(11) -0.068(5) 0.056(7) Uani 0.56(2) 1 d P B 1
H23A H 0.6614 0.8261 -0.0708 0.084 Uiso 0.56(2) 1 calc PR B 1
H23B H 0.7302 0.8010 -0.1413 0.084 Uiso 0.56(2) 1 calc PR B 1
H23C H 0.7325 0.8513 -0.1227 0.084 Uiso 0.56(2) 1 calc PR B 1
C24 C 0.7199(19) 0.8620(10) 0.246(5) 0.051(7) Uani 0.56(2) 1 d P B 1
H24A H 0.7503 0.8852 0.2025 0.076 Uiso 0.56(2) 1 calc PR B 1
H24B H 0.7268 0.8578 0.3805 0.076 Uiso 0.56(2) 1 calc PR B 1
H24C H 0.6699 0.8690 0.2211 0.076 Uiso 0.56(2) 1 calc PR B 1
C22' C 0.691(2) 0.8607(12) 0.142(6) 0.048(7) Uani 0.44(2) 1 d P B 2
H22D H 0.6654 0.8622 0.2613 0.072 Uiso 0.44(2) 1 calc PR B 2
H22E H 0.6561 0.8586 0.0392 0.072 Uiso 0.44(2) 1 calc PR B 2
H22F H 0.7197 0.8862 0.1250 0.072 Uiso 0.44(2) 1 calc PR B 2
C23' C 0.806(2) 0.8322(14) 0.264(7) 0.056(7) Uani 0.44(2) 1 d P B 2
H23D H 0.8296 0.8574 0.2130 0.084 Uiso 0.44(2) 1 calc PR B 2
H23E H 0.8398 0.8085 0.2629 0.084 Uiso 0.44(2) 1 calc PR B 2
H23F H 0.7908 0.8378 0.3925 0.084 Uiso 0.44(2) 1 calc PR B 2
C24' C 0.767(3) 0.8142(13) -0.063(6) 0.051(7) Uani 0.44(2) 1 d P B 2
H24D H 0.7292 0.8016 -0.1387 0.076 Uiso 0.44(2) 1 calc PR B 2
H24E H 0.8084 0.7953 -0.0610 0.076 Uiso 0.44(2) 1 calc PR B 2
H24F H 0.7809 0.8415 -0.1166 0.076 Uiso 0.44(2) 1 calc PR B 2
C25 C 0.5151(9) 0.7485(5) 0.858(2) 0.029(4) Uani 1 1 d . . .
C26 C 0.5580(8) 0.7083(4) 0.873(2) 0.031(3) Uani 1 1 d . . .
C27 C 0.6331(8) 0.7093(5) 0.861(2) 0.028(4) Uani 1 1 d . . .
H27 H 0.6564 0.7355 0.8387 0.034 Uiso 1 1 calc R . .
C28 C 0.5216(9) 0.6685(5) 0.894(3) 0.046(4) Uani 1 1 d . . .
H28 H 0.4711 0.6677 0.8943 0.056 Uiso 1 1 calc R . .
C29 C 0.6741(8) 0.6721(4) 0.883(2) 0.028(3) Uani 1 1 d . . .
C30 C 0.7548(8) 0.6736(5) 0.8797(19) 0.027(3) Uani 1 1 d . . .
C31 C 0.6365(9) 0.6333(5) 0.906(3) 0.046(4) Uani 1 1 d . . .
H31 H 0.6630 0.6079 0.9165 0.055 Uiso 1 1 calc R . .
C32 C 0.5604(10) 0.6310(5) 0.914(3) 0.057(5) Uani 1 1 d . C .
C33 C 0.5229(13) 0.5878(8) 0.935(4) 0.082(7) Uani 1 1 d . . .
C34 C 0.5662(19) 0.5489(11) 0.865(7) 0.076(9) Uani 0.582(19) 1 d P C 1
H34A H 0.5750 0.5517 0.7302 0.114 Uiso 0.582(19) 1 calc PR C 1
H34B H 0.5390 0.5230 0.8886 0.114 Uiso 0.582(19) 1 calc PR C 1
H34C H 0.6117 0.5475 0.9316 0.114 Uiso 0.582(19) 1 calc PR C 1
C35 C 0.510(2) 0.5831(13) 1.149(7) 0.093(12) Uani 0.582(19) 1 d P C 1
H35A H 0.5534 0.5906 1.2169 0.140 Uiso 0.582(19) 1 calc PR C 1
H35B H 0.4968 0.5539 1.1771 0.140 Uiso 0.582(19) 1 calc PR C 1
H35C H 0.4712 0.6021 1.1871 0.140 Uiso 0.582(19) 1 calc PR C 1
C36 C 0.449(2) 0.5873(12) 0.833(8) 0.087(10) Uani 0.582(19) 1 d P C 1
H36A H 0.4173 0.6077 0.8922 0.130 Uiso 0.582(19) 1 calc PR C 1
H36B H 0.4285 0.5589 0.8416 0.130 Uiso 0.582(19) 1 calc PR C 1
H36C H 0.4560 0.5948 0.7010 0.130 Uiso 0.582(19) 1 calc PR C 1
C34' C 0.444(3) 0.5907(14) 1.004(10) 0.076(9) Uani 0.418(19) 1 d P C 2
H34D H 0.4430 0.6033 1.1293 0.114 Uiso 0.418(19) 1 calc PR C 2
H34E H 0.4234 0.5624 1.0084 0.114 Uiso 0.418(19) 1 calc PR C 2
H34F H 0.4168 0.6084 0.9172 0.114 Uiso 0.418(19) 1 calc PR C 2
C35' C 0.526(3) 0.5737(18) 0.727(9) 0.093(12) Uani 0.418(19) 1 d P C 2
H35D H 0.4846 0.5844 0.6597 0.140 Uiso 0.418(19) 1 calc PR C 2
H35E H 0.5273 0.5428 0.7199 0.140 Uiso 0.418(19) 1 calc PR C 2
H35F H 0.5697 0.5851 0.6687 0.140 Uiso 0.418(19) 1 calc PR C 2
C36' C 0.566(3) 0.5569(15) 1.063(11) 0.087(10) Uani 0.418(19) 1 d P C 2
H36D H 0.6024 0.5428 0.9895 0.130 Uiso 0.418(19) 1 calc PR C 2
H36E H 0.5331 0.5358 1.1158 0.130 Uiso 0.418(19) 1 calc PR C 2
H36F H 0.5878 0.5729 1.1654 0.130 Uiso 0.418(19) 1 calc PR C 2


_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 O13 2.298(7) . ?
Pb1 O5 2.443(9) . ?
Pb1 O1 2.502(9) . ?
Pb1 O12 2.582(9) . ?
Pb1 Pb4 3.6370(8) 2_765 ?
Pb2 O13 2.299(8) . ?
Pb2 O8 2.452(9) 4_565 ?
Pb2 O9 2.508(10) 4_565 ?
Pb2 O1 2.514(9) . ?
Pb2 O4 2.587(9) 2_765 ?
Pb3 O13 2.289(7) . ?
Pb3 O10 2.457(10) 4_565 ?
Pb3 O8 2.511(9) 4_565 ?
Pb3 O11 2.576(9) . ?
Pb3 O5 2.583(9) . ?
Pb3 Pb4 3.6690(8) 2_765 ?
Pb4 O13 2.283(9) 2_764 ?
Pb4 O3 2.604(8) . ?
Pb4 O12 2.605(9) 2_764 ?
Pb4 O4 2.608(9) . ?
Pb4 Pb1 3.6370(8) 2_764 ?
Pb4 Pb3 3.6690(8) 2_764 ?
O1 C1 1.328(16) . ?
O2 C1 1.214(17) . ?
O3 C6 1.278(16) . ?
O4 C6 1.258(16) . ?
O4 Pb2 2.587(9) 2_764 ?
O5 C13 1.311(17) . ?
O6 C13 1.234(16) . ?
O7 C18 1.199(18) . ?
O8 C18 1.305(17) . ?
O8 Pb2 2.452(9) 4_465 ?
O8 Pb3 2.511(9) 4_465 ?
O9 C25 1.267(18) . ?
O9 Pb2 2.508(10) 4_465 ?
O10 C25 1.297(18) . ?
O10 Pb3 2.457(10) 4_465 ?
O11 C30 1.233(16) . ?
O12 C30 1.280(16) . ?
O12 Pb4 2.605(9) 2_765 ?
O13 Pb4 2.283(9) 2_765 ?
C1 C2 1.506(18) . ?
C2 C4 1.381(19) . ?
C2 C3 1.403(18) . ?
C3 C8 1.393(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(19) . ?
C4 H4 0.9300 . ?
C5 C7 1.385(19) . ?
C5 C6 1.491(18) . ?
C7 C8 1.400(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.51(2) . ?
C9 C11' 1.52(5) . ?
C9 C10 1.53(4) . ?
C9 C12' 1.53(5) . ?
C9 C10' 1.53(5) . ?
C9 C12 1.53(4) . ?
C9 C11 1.53(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?
C11' H11D 0.9600 . ?
C11' H11E 0.9600 . ?
C11' H11F 0.9600 . ?
C12' H12D 0.9600 . ?
C12' H12E 0.9600 . ?
C12' H12F 0.9600 . ?
C13 C14 1.493(18) . ?
C14 C15 1.362(19) . ?
C14 C16 1.411(18) . ?
C15 C17 1.381(19) . ?
C15 H15 0.9300 . ?
C16 C20 1.372(18) . ?
C16 H16 0.9300 . ?
C17 C19 1.389(19) . ?
C17 C18 1.51(2) . ?
C19 C20 1.394(18) . ?
C19 H19 0.9300 . ?
C20 C21 1.541(18) . ?
C21 C24 1.52(3) . ?
C21 C24' 1.52(4) . ?
C21 C22 1.52(3) . ?
C21 C22' 1.53(4) . ?
C21 C23' 1.54(5) . ?
C21 C23 1.54(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C22' H22D 0.9600 . ?
C22' H22E 0.9600 . ?
C22' H22F 0.9600 . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?
C25 C26 1.48(2) . ?
C26 C27 1.38(2) . ?
C26 C28 1.41(2) . ?
C27 C29 1.39(2) . ?
C27 H27 0.9300 . ?
C28 C32 1.37(2) . ?
C28 H28 0.9300 . ?
C29 C31 1.40(2) . ?
C29 C30 1.49(2) . ?
C31 C32 1.40(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.51(3) . ?
C33 C35 1.52(5) . ?
C33 C35' 1.53(6) . ?
C33 C34 1.53(4) . ?
C33 C36' 1.53(6) . ?
C33 C34' 1.53(6) . ?
C33 C36 1.53(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C34' H34D 0.9600 . ?
C34' H34E 0.9600 . ?
C34' H34F 0.9600 . ?
C35' H35D 0.9600 . ?
C35' H35E 0.9600 . ?
C35' H35F 0.9600 . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?

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 Pb1 O5 72.2(3) . . ?
O13 Pb1 O1 72.1(3) . . ?
O5 Pb1 O1 82.0(3) . . ?
O13 Pb1 O12 74.7(3) . . ?
O5 Pb1 O12 97.3(3) . . ?
O1 Pb1 O12 145.3(3) . . ?
O13 Pb1 Pb4 37.3(2) . 2_765 ?
O5 Pb1 Pb4 100.0(2) . 2_765 ?
O1 Pb1 Pb4 100.0(2) . 2_765 ?
O12 Pb1 Pb4 45.7(2) . 2_765 ?
O13 Pb2 O8 73.3(3) . 4_565 ?
O13 Pb2 O9 77.4(3) . 4_565 ?
O8 Pb2 O9 85.8(3) 4_565 4_565 ?
O13 Pb2 O1 71.8(3) . . ?
O8 Pb2 O1 84.8(3) 4_565 . ?
O9 Pb2 O1 149.2(3) 4_565 . ?
O13 Pb2 O4 73.8(3) . 2_765 ?
O8 Pb2 O4 143.8(3) 4_565 2_765 ?
O9 Pb2 O4 72.6(3) 4_565 2_765 ?
O1 Pb2 O4 99.1(3) . 2_765 ?
O13 Pb3 O10 78.4(3) . 4_565 ?
O13 Pb3 O8 72.4(3) . 4_565 ?
O10 Pb3 O8 94.7(3) 4_565 4_565 ?
O13 Pb3 O11 76.4(3) . . ?
O10 Pb3 O11 79.5(3) 4_565 . ?
O8 Pb3 O11 148.7(3) 4_565 . ?
O13 Pb3 O5 69.7(3) . . ?
O10 Pb3 O5 147.3(3) 4_565 . ?
O8 Pb3 O5 82.6(3) 4_565 . ?
O11 Pb3 O5 86.2(3) . . ?
O13 Pb3 Pb4 36.6(2) . 2_765 ?
O10 Pb3 Pb4 51.7(2) 4_565 2_765 ?
O8 Pb3 Pb4 99.9(2) 4_565 2_765 ?
O11 Pb3 Pb4 52.5(2) . 2_765 ?
O5 Pb3 Pb4 96.5(2) . 2_765 ?
O13 Pb4 O3 76.0(3) 2_764 . ?
O13 Pb4 O12 74.5(3) 2_764 2_764 ?
O3 Pb4 O12 70.2(3) . 2_764 ?
O13 Pb4 O4 73.7(3) 2_764 . ?
O3 Pb4 O4 50.3(3) . . ?
O12 Pb4 O4 117.2(3) 2_764 . ?
O13 Pb4 Pb1 37.59(18) 2_764 2_764 ?
O3 Pb4 Pb1 49.8(2) . 2_764 ?
O12 Pb4 Pb1 45.2(2) 2_764 2_764 ?
O4 Pb4 Pb1 78.4(2) . 2_764 ?
O13 Pb4 Pb3 36.70(18) 2_764 2_764 ?
O3 Pb4 Pb3 110.6(2) . 2_764 ?
O12 Pb4 Pb3 76.1(2) 2_764 2_764 ?
O4 Pb4 Pb3 104.95(19) . 2_764 ?
Pb1 Pb4 Pb3 63.230(14) 2_764 2_764 ?
C1 O1 Pb1 123.1(8) . . ?
C1 O1 Pb2 102.6(8) . . ?
Pb1 O1 Pb2 99.1(3) . . ?
C6 O3 Pb4 93.4(7) . . ?
C6 O4 Pb2 113.0(8) . 2_764 ?
C6 O4 Pb4 93.8(8) . . ?
Pb2 O4 Pb4 91.8(3) 2_764 . ?
C13 O5 Pb1 100.5(8) . . ?
C13 O5 Pb3 118.4(8) . . ?
Pb1 O5 Pb3 99.3(3) . . ?
C18 O8 Pb2 121.0(9) . 4_465 ?
C18 O8 Pb3 99.8(8) . 4_465 ?
Pb2 O8 Pb3 98.7(3) 4_465 4_465 ?
C25 O9 Pb2 132.0(9) . 4_465 ?
C25 O10 Pb3 118.6(9) . 4_465 ?
C30 O11 Pb3 129.2(9) . . ?
C30 O12 Pb1 112.8(8) . . ?
C30 O12 Pb4 102.1(8) . 2_765 ?
Pb1 O12 Pb4 89.0(3) . 2_765 ?
Pb4 O13 Pb3 106.7(3) 2_765 . ?
Pb4 O13 Pb1 105.1(3) 2_765 . ?
Pb3 O13 Pb1 113.2(3) . . ?
Pb4 O13 Pb2 109.0(3) 2_765 . ?
Pb3 O13 Pb2 110.3(3) . . ?
Pb1 O13 Pb2 112.2(3) . . ?
O2 C1 O1 120.8(13) . . ?
O2 C1 C2 123.0(12) . . ?
O1 C1 C2 116.1(12) . . ?
C4 C2 C3 119.9(12) . . ?
C4 C2 C1 118.0(13) . . ?
C3 C2 C1 122.0(12) . . ?
C8 C3 C2 121.9(12) . . ?
C8 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C2 C4 C5 119.1(14) . . ?
C2 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C7 C5 C4 120.1(13) . . ?
C7 C5 C6 120.1(12) . . ?
C4 C5 C6 119.8(13) . . ?
O4 C6 O3 121.8(12) . . ?
O4 C6 C5 118.1(13) . . ?
O3 C6 C5 120.0(12) . . ?
C5 C7 C8 121.9(13) . . ?
C5 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C3 C8 C7 116.8(13) . . ?
C3 C8 C9 120.8(12) . . ?
C7 C8 C9 122.4(13) . . ?
C8 C9 C11' 112(2) . . ?
C8 C9 C10 112.7(17) . . ?
C11' C9 C10 27(2) . . ?
C8 C9 C12' 110(2) . . ?
C11' C9 C12' 108(3) . . ?
C10 C9 C12' 83(2) . . ?
C8 C9 C10' 112(2) . . ?
C11' C9 C10' 107(3) . . ?
C10 C9 C10' 127(2) . . ?
C12' C9 C10' 107(3) . . ?
C8 C9 C12 108(2) . . ?
C11' C9 C12 84(3) . . ?
C10 C9 C12 108(2) . . ?
C12' C9 C12 132(3) . . ?
C10' C9 C12 28.7(18) . . ?
C8 C9 C11 111.4(18) . . ?
C11' C9 C11 128(2) . . ?
C10 C9 C11 108(2) . . ?
C12' C9 C11 29.0(19) . . ?
C10' C9 C11 80(2) . . ?
C12 C9 C11 108(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
C9 C10' H10D 109.5 . . ?
C9 C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
C9 C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
C9 C11' H11D 109.5 . . ?
C9 C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
C9 C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
C9 C12' H12D 109.5 . . ?
C9 C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
C9 C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
O6 C13 O5 121.0(13) . . ?
O6 C13 C14 121.9(13) . . ?
O5 C13 C14 117.0(12) . . ?
C15 C14 C16 118.9(12) . . ?
C15 C14 C13 119.8(12) . . ?
C16 C14 C13 121.2(12) . . ?
C14 C15 C17 121.0(13) . . ?
C14 C15 H15 119.5 . . ?
C17 C15 H15 119.5 . . ?
C20 C16 C14 122.1(13) . . ?
C20 C16 H16 119.0 . . ?
C14 C16 H16 119.0 . . ?
C15 C17 C19 118.9(13) . . ?
C15 C17 C18 118.9(13) . . ?
C19 C17 C18 122.0(12) . . ?
O7 C18 O8 121.8(14) . . ?
O7 C18 C17 123.0(14) . . ?
O8 C18 C17 115.0(13) . . ?
C17 C19 C20 122.1(13) . . ?
C17 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
C16 C20 C19 117.0(13) . . ?
C16 C20 C21 121.5(12) . . ?
C19 C20 C21 121.5(12) . . ?
C24 C21 C24' 131(2) . . ?
C24 C21 C22 110.4(19) . . ?
C24' C21 C22 68(2) . . ?
C24 C21 C22' 34.6(18) . . ?
C24' C21 C22' 108(2) . . ?
C22 C21 C22' 133(2) . . ?
C24 C21 C23' 74(2) . . ?
C24' C21 C23' 107(3) . . ?
C22 C21 C23' 41.6(19) . . ?
C22' C21 C23' 106(2) . . ?
C24 C21 C20 113.2(16) . . ?
C24' C21 C20 112.0(19) . . ?
C22 C21 C20 112.5(14) . . ?
C22' C21 C20 112.0(17) . . ?
C23' C21 C20 110.9(18) . . ?
C24 C21 C23 108(2) . . ?
C24' C21 C23 40(2) . . ?
C22 C21 C23 107(2) . . ?
C22' C21 C23 76(2) . . ?
C23' C21 C23 140(2) . . ?
C20 C21 C23 105.0(16) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
C21 C22' H22D 109.5 . . ?
C21 C22' H22E 109.5 . . ?
H22D C22' H22E 109.5 . . ?
C21 C22' H22F 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C21 C23' H23D 109.5 . . ?
C21 C23' H23E 109.5 . . ?
H23D C23' H23E 109.5 . . ?
C21 C23' H23F 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C21 C24' H24D 109.5 . . ?
C21 C24' H24E 109.5 . . ?
H24D C24' H24E 109.5 . . ?
C21 C24' H24F 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
O9 C25 O10 120.0(13) . . ?
O9 C25 C26 119.4(14) . . ?
O10 C25 C26 120.6(13) . . ?
C27 C26 C28 119.9(13) . . ?
C27 C26 C25 120.7(14) . . ?
C28 C26 C25 119.4(14) . . ?
C26 C27 C29 121.2(14) . . ?
C26 C27 H27 119.4 . . ?
C29 C27 H27 119.4 . . ?
C32 C28 C26 120.3(16) . . ?
C32 C28 H28 119.8 . . ?
C26 C28 H28 119.8 . . ?
C27 C29 C31 117.3(14) . . ?
C27 C29 C30 121.2(13) . . ?
C31 C29 C30 121.5(13) . . ?
O11 C30 O12 121.3(13) . . ?
O11 C30 C29 120.1(13) . . ?
O12 C30 C29 118.5(12) . . ?
C29 C31 C32 122.9(15) . . ?
C29 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C28 C32 C31 118.2(16) . . ?
C28 C32 C33 121.6(17) . . ?
C31 C32 C33 120.2(17) . . ?
C32 C33 C35 105(3) . . ?
C32 C33 C35' 98(3) . . ?
C35 C33 C35' 157(3) . . ?
C32 C33 C34 115(2) . . ?
C35 C33 C34 109(3) . . ?
C35' C33 C34 56(3) . . ?
C32 C33 C36' 112(3) . . ?
C35 C33 C36' 56(3) . . ?
C35' C33 C36' 111(4) . . ?
C34 C33 C36' 55(3) . . ?
C32 C33 C34' 114(2) . . ?
C35 C33 C34' 63(3) . . ?
C35' C33 C34' 111(4) . . ?
C34 C33 C34' 130(3) . . ?
C36' C33 C34' 110(4) . . ?
C32 C33 C36 111(2) . . ?
C35 C33 C36 109(3) . . ?
C35' C33 C36 66(3) . . ?
C34 C33 C36 108(3) . . ?
C36' C33 C36 136(3) . . ?
C34' C33 C36 46(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
C33 C34' H34D 109.5 . . ?
C33 C34' H34E 109.5 . . ?
H34D C34' H34E 109.5 . . ?
C33 C34' H34F 109.5 . . ?
H34D C34' H34F 109.5 . . ?
H34E C34' H34F 109.5 . . ?
C33 C35' H35D 109.5 . . ?
C33 C35' H35E 109.5 . . ?
H35D C35' H35E 109.5 . . ?
C33 C35' H35F 109.5 . . ?
H35D C35' H35F 109.5 . . ?
H35E C35' H35F 109.5 . . ?
C33 C36' H36D 109.5 . . ?
C33 C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C33 C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.811
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.193
_database_code_depnum_ccdc_archive 'CCDC 1019802'
