# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.

#==============================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_coden_Cambridge         0182
#CCDC numbers 640883, 640884 and 640885
#==============================================================================

# 1. SUBMISSION DETAILS

_publ_contact_author             
# Name and address of author for correspondence
;
Dr. Jagadese J. Vittal
Department of Chemistry
National University of Singapore
3 Science Drive 3
SINGAPORE 117543
;
_publ_contact_author_phone       '(65) 6516 2677'
_publ_contact_author_fax         '(65) 6779 1691'
_publ_contact_author_email       chmjjv@nus.edu.sg

_publ_requested_coeditor_name    ' '

_publ_contact_letter             
;
''
;
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?
_journal_suppl_publ_number       ?
_journal_suppl_publ_pages        ?

#==============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;Photodimerization of 1D Hydrogen-bonded zwitter-ionic Lead(II) complex and its
isomerization in solution
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address

'Abdul Malik Puthan Peedikakal'
; Department of Chemistry
National University of Singapore
SINGAPORE 117543
;
'Lip Lin Koh'
; Department of Chemistry
National University of Singapore
SINGAPORE 117543
;
'Jagadese J. Vittal'
; Department of Chemistry
National University of Singapore
SINGAPORE 117543
;
_publ_contact_author_name        'Dr. Jagadese J. Vittal'
#==============================================================================
# CCDC 640883

data_compound_1
_database_code_depnum_ccdc_archive 'CCDC 640883'

#data_pam1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H22 F12 N4 O8 Pb'
_chemical_formula_weight         1025.73

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   11.916(4)
_cell_length_b                   15.793(6)
_cell_length_c                   19.578(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.828(8)
_cell_angle_gamma                90.00
_cell_volume                     3606(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5640
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      25.41

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.42
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_exptl_absorpt_coefficient_mu    4.796
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.49143
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10015
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3164
_reflns_number_gt                3014
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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.

The F atoms were disordered. Four disordered models were resolved for each
CF3 group. The geometry was restrained by using SADI and isotropic thermal
parameters were refined for each model. The occupancy factor was fixed at
0.25 for each model and was not refined.

The 4,4'-bipyridylethylene-H is also found to be disordered. The occupancy
of two disordered models were refined to 0.62(2) and 0.38(2). Only individual
isotropic thermal parameters were refined for non-hydrogen atoms. All the
hydrogen atoms were placed in ideal positions using AFIX option.
;

_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^)+(0.0676P)^2^+21.9265P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3164
_refine_ls_number_parameters     268
_refine_ls_number_restraints     405
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.174
_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 0.5000 0.557350(18) 0.2500 0.02606(15) Uiso 1 2 d S . .
N1 N 0.4977(11) 0.4341(9) 0.1587(8) 0.031(4) Uiso 0.618(17) 1 d PD A 1
C1 C 0.4597(11) 0.4528(10) 0.0916(7) 0.039(4) Uiso 0.618(17) 1 d PD A 1
H1 H 0.4213 0.5038 0.0803 0.047 Uiso 0.618(17) 1 calc PR A 1
C2 C 0.4744(10) 0.4007(9) 0.0390(7) 0.040(3) Uiso 0.618(17) 1 d PD A 1
H2C H 0.4441 0.4164 -0.0069 0.048 Uiso 0.618(17) 1 calc PR A 1
C3 C 0.5328(9) 0.3256(8) 0.0516(6) 0.033(3) Uiso 0.618(17) 1 d PD A 1
C4 C 0.5697(10) 0.3051(7) 0.1205(7) 0.036(3) Uiso 0.618(17) 1 d PD A 1
H4 H 0.6066 0.2537 0.1325 0.043 Uiso 0.618(17) 1 calc PR A 1
C5 C 0.5524(12) 0.3603(9) 0.1723(8) 0.036(4) Uiso 0.618(17) 1 d PD A 1
H5 H 0.5801 0.3453 0.2186 0.043 Uiso 0.618(17) 1 calc PR A 1
N2 N 0.6960(10) 0.0706(8) -0.1710(7) 0.030(3) Uiso 0.618(17) 1 d PD A 1
H2 H 0.7125 0.0418 -0.2049 0.036 Uiso 0.618(17) 1 calc PR A 1
C6 C 0.7228(13) 0.0388(11) -0.1073(10) 0.046(5) Uiso 0.618(17) 1 d PD A 1
H6 H 0.7594 -0.0135 -0.1004 0.055 Uiso 0.618(17) 1 calc PR A 1
C7 C 0.6973(12) 0.0820(9) -0.0501(7) 0.035(3) Uiso 0.618(17) 1 d PD A 1
H7 H 0.7167 0.0591 -0.0055 0.042 Uiso 0.618(17) 1 calc PR A 1
C8 C 0.6427(9) 0.1598(7) -0.0611(6) 0.031(3) Uiso 0.618(17) 1 d PD A 1
C9 C 0.6174(12) 0.1904(9) -0.1290(8) 0.040(4) Uiso 0.618(17) 1 d PD A 1
H9 H 0.5810 0.2426 -0.1377 0.048 Uiso 0.618(17) 1 calc PR A 1
C10 C 0.6452(12) 0.1445(10) -0.1849(8) 0.035(4) Uiso 0.618(17) 1 d PD A 1
H10 H 0.6282 0.1657 -0.2302 0.042 Uiso 0.618(17) 1 calc PR A 1
C11 C 0.5553(10) 0.2758(7) -0.0063(6) 0.040(3) Uiso 0.618(17) 1 d PD A 1
H11 H 0.5211 0.2943 -0.0508 0.048 Uiso 0.618(17) 1 calc PR A 1
C12 C 0.6184(10) 0.2076(8) -0.0025(6) 0.038(3) Uiso 0.618(17) 1 d PD A 1
H12 H 0.6507 0.1879 0.0419 0.046 Uiso 0.618(17) 1 calc PR A 1
N1A N 0.5060(17) 0.4228(15) 0.1669(11) 0.031(7) Uiso 0.382(17) 1 d PD A 2
C1A C 0.5682(16) 0.3567(12) 0.1906(12) 0.030(6) Uiso 0.382(17) 1 d PD A 2
H1A H 0.5965 0.3513 0.2384 0.036 Uiso 0.382(17) 1 calc PR A 2
C2A C 0.5926(14) 0.2952(10) 0.1463(9) 0.026(4) Uiso 0.382(17) 1 d PD A 2
H2AC H 0.6349 0.2480 0.1649 0.031 Uiso 0.382(17) 1 calc PR A 2
C3A C 0.5563(11) 0.3013(9) 0.0754(8) 0.023(4) Uiso 0.382(17) 1 d PD A 2
C4A C 0.4900(16) 0.3703(13) 0.0511(9) 0.036(5) Uiso 0.382(17) 1 d PD A 2
H4A H 0.4624 0.3776 0.0035 0.043 Uiso 0.382(17) 1 calc PR A 2
C5A C 0.4643(18) 0.4300(15) 0.0990(12) 0.037(6) Uiso 0.382(17) 1 d PD A 2
H5A H 0.4169 0.4755 0.0826 0.044 Uiso 0.382(17) 1 calc PR A 2
N2A N 0.7051(15) 0.0568(11) -0.1580(11) 0.027(5) Uiso 0.382(17) 1 d PD A 2
H2A H 0.7282 0.0195 -0.1840 0.032 Uiso 0.382(17) 1 calc PR A 2
C6A C 0.6601(19) 0.1276(17) -0.1877(14) 0.045(9) Uiso 0.382(17) 1 d PD A 2
H6A H 0.6550 0.1353 -0.2353 0.054 Uiso 0.382(17) 1 calc PR A 2
C7A C 0.6199(16) 0.1909(12) -0.1490(11) 0.031(5) Uiso 0.382(17) 1 d PD A 2
H7A H 0.5894 0.2409 -0.1701 0.038 Uiso 0.382(17) 1 calc PR A 2
C8A C 0.6266(13) 0.1774(10) -0.0790(9) 0.025(4) Uiso 0.382(17) 1 d PD A 2
C9A C 0.6756(19) 0.1027(13) -0.0518(11) 0.041(6) Uiso 0.382(17) 1 d PD A 2
H9A H 0.6819 0.0929 -0.0043 0.050 Uiso 0.382(17) 1 calc PR A 2
C10A C 0.7166(17) 0.0402(13) -0.0915(12) 0.027(6) Uiso 0.382(17) 1 d PD A 2
H10A H 0.7499 -0.0097 -0.0718 0.032 Uiso 0.382(17) 1 calc PR A 2
C11A C 0.5914(15) 0.2378(11) 0.0304(9) 0.036(5) Uiso 0.382(17) 1 d PD A 2
H11A H 0.6223 0.1885 0.0525 0.044 Uiso 0.382(17) 1 calc PR A 2
C12A C 0.5855(15) 0.2407(11) -0.0367(9) 0.033(5) Uiso 0.382(17) 1 d PD A 2
H12A H 0.5512 0.2884 -0.0598 0.040 Uiso 0.382(17) 1 calc PR A 2
O1 O 0.7154(4) 0.5060(3) 0.2725(2) 0.0409(12) Uani 1 1 d . A .
O2 O 0.7149(5) 0.5834(4) 0.3663(3) 0.0510(14) Uani 1 1 d . A .
C13 C 0.7608(6) 0.5386(4) 0.3296(3) 0.0348(15) Uani 1 1 d D . .
C14 C 0.8859(7) 0.5180(5) 0.3568(4) 0.066(3) Uani 1 1 d D A .
F1 F 0.9439(14) 0.5016(17) 0.3059(8) 0.061(4) Uiso 0.25 1 d PD A 3
F2 F 0.8920(16) 0.4390(10) 0.3903(13) 0.061(4) Uiso 0.25 1 d PD A 3
F3 F 0.9461(15) 0.5692(12) 0.4019(10) 0.061(4) Uiso 0.25 1 d PD A 3
F1A F 0.9280(16) 0.4546(11) 0.3269(11) 0.060(4) Uiso 0.25 1 d PD A 4
F2A F 0.9173(16) 0.5114(17) 0.4257(6) 0.060(4) Uiso 0.25 1 d PD A 4
F3A F 0.9493(13) 0.5886(10) 0.3427(14) 0.060(4) Uiso 0.25 1 d PD A 4
F1C F 0.9364(13) 0.4712(12) 0.3174(9) 0.043(3) Uiso 0.25 1 d PD A 5
F2C F 0.8937(13) 0.4720(14) 0.4192(8) 0.043(3) Uiso 0.25 1 d PD A 5
F3C F 0.9505(11) 0.5862(9) 0.3780(12) 0.043(3) Uiso 0.25 1 d PD A 5
F1D F 0.9079(17) 0.4340(10) 0.3445(15) 0.074(4) Uiso 0.25 1 d PD A 6
F2D F 0.9415(16) 0.5440(16) 0.4096(10) 0.074(4) Uiso 0.25 1 d PD A 6
F3D F 0.9444(16) 0.5531(17) 0.3005(12) 0.074(4) Uiso 0.25 1 d PD A 6
O3 O 0.3863(6) 0.6067(4) 0.3607(3) 0.0633(17) Uani 1 1 d . . .
O4 O 0.3757(7) 0.7031(4) 0.2808(4) 0.076(2) Uani 1 1 d . . .
C15 C 0.3448(6) 0.6700(4) 0.3295(3) 0.0381(15) Uani 1 1 d D . .
C16 C 0.2459(8) 0.7105(5) 0.3536(4) 0.071(3) Uani 1 1 d D . .
F4 F 0.1474(12) 0.6631(13) 0.3256(17) 0.074(5) Uiso 0.25 1 d PD B 7
F5 F 0.2198(18) 0.7882(8) 0.3380(13) 0.074(5) Uiso 0.25 1 d PD B 7
F6 F 0.257(2) 0.7001(19) 0.4241(8) 0.074(5) Uiso 0.25 1 d PD B 7
F4A F 0.1604(19) 0.735(3) 0.3015(11) 0.110(8) Uiso 0.25 1 d PD B 8
F5A F 0.282(2) 0.7859(16) 0.388(2) 0.110(8) Uiso 0.25 1 d PD B 8
F6A F 0.200(3) 0.6655(17) 0.3982(17) 0.110(8) Uiso 0.25 1 d PD B 8
F4C F 0.1601(18) 0.6667(19) 0.359(2) 0.097(6) Uiso 0.25 1 d PD B 9
F5C F 0.218(2) 0.7868(11) 0.3219(15) 0.097(6) Uiso 0.25 1 d PD B 9
F6C F 0.290(2) 0.738(2) 0.4241(9) 0.097(6) Uiso 0.25 1 d PD B 9
F4D F 0.253(2) 0.7962(7) 0.3537(16) 0.063(4) Uiso 0.25 1 d PD B 10
F5D F 0.223(2) 0.6837(15) 0.4123(9) 0.063(4) Uiso 0.25 1 d PD B 10
F6D F 0.1463(11) 0.695(2) 0.3029(10) 0.063(4) Uiso 0.25 1 d PD B 10

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
O1 0.032(2) 0.055(3) 0.033(2) -0.013(2) 0.0003(19) 0.008(2)
O2 0.049(3) 0.061(3) 0.044(3) -0.016(3) 0.013(3) 0.010(3)
C13 0.031(3) 0.038(4) 0.033(4) -0.005(3) 0.004(3) 0.002(3)
C14 0.047(5) 0.078(7) 0.063(6) -0.041(5) -0.011(4) 0.013(5)
O3 0.083(4) 0.054(4) 0.050(3) 0.006(3) 0.006(3) 0.030(3)
O4 0.099(5) 0.054(4) 0.090(5) 0.012(4) 0.055(4) 0.007(4)
C15 0.042(4) 0.033(4) 0.039(4) 0.001(3) 0.006(3) 0.000(3)
C16 0.082(7) 0.055(6) 0.083(7) 0.021(5) 0.034(6) 0.022(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.639(16) . ?
Pb1 N1 2.639(16) 6_656 ?
Pb1 O1 2.642(5) 6_656 ?
Pb1 O1 2.642(5) . ?
Pb1 N1A 2.69(3) . ?
Pb1 N1A 2.69(3) 6_656 ?
N1 C1 1.332(18) . ?
N1 C5 1.336(17) . ?
C1 C2 1.357(17) . ?
C2 C3 1.372(15) . ?
C3 C4 1.368(15) . ?
C3 C11 1.450(15) . ?
C4 C5 1.384(17) . ?
N2 C10 1.318(18) . ?
N2 C6 1.322(19) . ?
C6 C7 1.397(19) . ?
C7 C8 1.386(16) . ?
C8 C9 1.388(15) . ?
C8 C12 1.451(15) . ?
C9 C10 1.409(18) . ?
C11 C12 1.306(19) . ?
N1A C1A 1.31(3) . ?
N1A C5A 1.33(2) . ?
C1A C2A 1.37(2) . ?
C2A C3A 1.370(19) . ?
C3A C4A 1.37(2) . ?
C3A C11A 1.45(2) . ?
C4A C5A 1.41(2) . ?
N2A C10A 1.31(3) . ?
N2A C6A 1.32(3) . ?
C6A C7A 1.40(3) . ?
C7A C8A 1.37(2) . ?
C8A C9A 1.37(2) . ?
C8A C12A 1.45(2) . ?
C9A C10A 1.40(3) . ?
C11A C12A 1.30(3) . ?
O1 C13 1.249(8) . ?
O2 C13 1.216(9) . ?
C13 C14 1.512(11) . ?
C14 F2D 1.182(17) . ?
C14 F3 1.299(12) . ?
C14 F1C 1.301(12) . ?
C14 F1A 1.310(12) . ?
C14 F2A 1.328(12) . ?
C14 F3C 1.340(12) . ?
C14 F1 1.350(12) . ?
C14 F1D 1.383(16) . ?
C14 F2 1.404(12) . ?
C14 F3A 1.405(12) . ?
C14 F2C 1.409(12) . ?
O3 C15 1.222(9) . ?
O4 C15 1.208(9) . ?
C15 C16 1.500(12) . ?
C16 F4C 1.26(2) . ?
C16 F5 1.287(13) . ?
C16 F5D 1.304(13) . ?
C16 F6A 1.331(13) . ?
C16 F4A 1.340(14) . ?
C16 F4D 1.355(13) . ?
C16 F5C 1.365(13) . ?
C16 F6 1.371(13) . ?
C16 F5A 1.388(14) . ?
C16 F6D 1.404(13) . ?
C16 F4 1.405(13) . ?
C16 F6C 1.443(14) . ?

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
N1 Pb1 N1 85.0(6) . 6_656 ?
N1 Pb1 O1 77.6(3) . 6_656 ?
N1 Pb1 O1 76.2(3) 6_656 6_656 ?
N1 Pb1 O1 76.2(3) . . ?
N1 Pb1 O1 77.6(3) 6_656 . ?
O1 Pb1 O1 144.2(2) 6_656 . ?
N1 Pb1 N1A 5.2(5) . . ?
N1 Pb1 N1A 80.2(4) 6_656 . ?
O1 Pb1 N1A 78.6(5) 6_656 . ?
O1 Pb1 N1A 73.3(4) . . ?
N1 Pb1 N1A 80.2(4) . 6_656 ?
N1 Pb1 N1A 5.2(5) 6_656 6_656 ?
O1 Pb1 N1A 73.3(4) 6_656 6_656 ?
O1 Pb1 N1A 78.6(4) . 6_656 ?
N1A Pb1 N1A 75.4(8) . 6_656 ?
C1 N1 C5 116.3(16) . . ?
C1 N1 Pb1 117.4(10) . . ?
C5 N1 Pb1 124.9(10) . . ?
N1 C1 C2 123.0(15) . . ?
C1 C2 C3 121.7(13) . . ?
C4 C3 C2 115.6(11) . . ?
C4 C3 C11 124.7(10) . . ?
C2 C3 C11 119.7(9) . . ?
C3 C4 C5 120.4(12) . . ?
N1 C5 C4 122.9(13) . . ?
C10 N2 C6 122.9(15) . . ?
N2 C6 C7 121.3(15) . . ?
C8 C7 C6 118.8(13) . . ?
C7 C8 C9 117.4(11) . . ?
C7 C8 C12 120.2(10) . . ?
C9 C8 C12 122.4(10) . . ?
C8 C9 C10 121.7(12) . . ?
N2 C10 C9 117.8(13) . . ?
C12 C11 C3 126.8(11) . . ?
C11 C12 C8 126.2(11) . . ?
C1A N1A C5A 119(3) . . ?
C1A N1A Pb1 120.0(15) . . ?
C5A N1A Pb1 119.3(16) . . ?
N1A C1A C2A 121(2) . . ?
C3A C2A C1A 121.8(17) . . ?
C2A C3A C4A 116.5(15) . . ?
C2A C3A C11A 119.7(12) . . ?
C4A C3A C11A 123.7(13) . . ?
C3A C4A C5A 119.3(17) . . ?
N1A C5A C4A 122(2) . . ?
C10A N2A C6A 124(2) . . ?
N2A C6A C7A 121(2) . . ?
C8A C7A C6A 118.3(18) . . ?
C7A C8A C9A 117.0(17) . . ?
C7A C8A C12A 120.5(13) . . ?
C9A C8A C12A 122.5(14) . . ?
C8A C9A C10A 123.8(19) . . ?
N2A C10A C9A 115.7(19) . . ?
C12A C11A C3A 128.8(16) . . ?
C11A C12A C8A 126.8(16) . . ?
C13 O1 Pb1 104.5(4) . . ?
O2 C13 O1 127.2(7) . . ?
O2 C13 C14 116.6(6) . . ?
O1 C13 C14 116.2(6) . . ?
F2D C14 F3 19.3(16) . . ?
F2D C14 F1C 118.1(14) . . ?
F3 C14 F1C 119.8(14) . . ?
F2D C14 F1A 117.3(17) . . ?
F3 C14 F1A 124.7(14) . . ?
F1C C14 F1A 15.3(14) . . ?
F2D C14 F2A 31.5(13) . . ?
F3 C14 F2A 50.0(14) . . ?
F1C C14 F2A 119.2(14) . . ?
F1A C14 F2A 109.7(11) . . ?
F2D C14 F3C 42.8(14) . . ?
F3 C14 F3C 24.1(11) . . ?
F1C C14 F3C 109.5(10) . . ?
F1A C14 F3C 120.3(14) . . ?
F2A C14 F3C 74.0(11) . . ?
F2D C14 F1 115.7(17) . . ?
F3 C14 F1 109.0(11) . . ?
F1C C14 F1 23.7(11) . . ?
F1A C14 F1 39.0(13) . . ?
F2A C14 F1 130.9(13) . . ?
F3C C14 F1 92.0(13) . . ?
F2D C14 F1D 113.2(13) . . ?
F3 C14 F1D 128.1(15) . . ?
F1C C14 F1D 39.2(12) . . ?
F1A C14 F1D 23.9(13) . . ?
F2A C14 F1D 94.4(15) . . ?
F3C C14 F1D 135.1(13) . . ?
F1 C14 F1D 62.8(12) . . ?
F2D C14 F2 86.2(16) . . ?
F3 C14 F2 105.4(11) . . ?
F1C C14 F2 77.6(11) . . ?
F1A C14 F2 62.7(13) . . ?
F2A C14 F2 58.5(13) . . ?
F3C C14 F2 126.7(12) . . ?
F1 C14 F2 100.9(10) . . ?
F1D C14 F2 40.1(12) . . ?
F2D C14 F3A 70.7(14) . . ?
F3 C14 F3A 52.8(13) . . ?
F1C C14 F3A 90.1(13) . . ?
F1A C14 F3A 104.3(11) . . ?
F2A C14 F3A 102.2(10) . . ?
F3C C14 F3A 29.0(9) . . ?
F1 C14 F3A 68.2(13) . . ?
F1D C14 F3A 126.7(14) . . ?
F2 C14 F3A 144.8(13) . . ?
F2D C14 F2C 59.6(14) . . ?
F3 C14 F2C 78.6(12) . . ?
F1C C14 F2C 105.3(10) . . ?
F1A C14 F2C 91.7(13) . . ?
F2A C14 F2C 28.7(10) . . ?
F3C C14 F2C 102.4(9) . . ?
F1 C14 F2C 126.1(12) . . ?
F1D C14 F2C 71.0(12) . . ?
F2 C14 F2C 31.6(9) . . ?
F3A C14 F2C 129.5(11) . . ?
F2D C14 C13 124.7(12) . . ?
F3 C14 C13 118.3(10) . . ?
F1C C14 C13 117.1(9) . . ?
F1A C14 C13 116.6(10) . . ?
F2A C14 C13 115.3(9) . . ?
F3C C14 C13 113.5(9) . . ?
F1 C14 C13 113.5(9) . . ?
F1D C14 C13 110.7(10) . . ?
F2 C14 C13 107.9(9) . . ?
F3A C14 C13 107.0(9) . . ?
F2C C14 C13 107.5(8) . . ?
O4 C15 O3 126.2(8) . . ?
O4 C15 C16 116.7(6) . . ?
O3 C15 C16 117.1(6) . . ?
F4C C16 F5 112.7(19) . . ?
F4C C16 F5D 54.7(18) . . ?
F5 C16 F5D 115.8(17) . . ?
F4C C16 F6A 36.2(16) . . ?
F5 C16 F6A 123.5(16) . . ?
F5D C16 F6A 19.8(18) . . ?
F4C C16 F4A 73.9(19) . . ?
F5 C16 F4A 55.9(18) . . ?
F5D C16 F4A 120.0(17) . . ?
F6A C16 F4A 107.4(13) . . ?
F4C C16 F4D 126.9(18) . . ?
F5 C16 F4D 20.0(14) . . ?
F5D C16 F4D 110.3(11) . . ?
F6A C16 F4D 124.5(17) . . ?
F4A C16 F4D 75.7(15) . . ?
F4C C16 F5C 113.6(19) . . ?
F5 C16 F5C 13.1(17) . . ?
F5D C16 F5C 127.7(15) . . ?
F6A C16 F5C 132.4(16) . . ?
F4A C16 F5C 47.6(15) . . ?
F4D C16 F5C 29.4(12) . . ?
F4C C16 F6 75.6(16) . . ?
F5 C16 F6 108.7(12) . . ?
F5D C16 F6 21.0(14) . . ?
F6A C16 F6 40.5(16) . . ?
F4A C16 F6 134.4(16) . . ?
F4D C16 F6 97.2(16) . . ?
F5C C16 F6 121.9(16) . . ?
F4C C16 F5A 127.1(17) . . ?
F5 C16 F5A 48.1(18) . . ?
F5D C16 F5A 87.3(17) . . ?
F6A C16 F5A 105.6(12) . . ?
F4A C16 F5A 103.4(12) . . ?
F4D C16 F5A 29.7(14) . . ?
F5C C16 F5A 59.0(15) . . ?
F6 C16 F5A 70.3(16) . . ?
F4C C16 F6D 51.9(17) . . ?
F5 C16 F6D 82.8(14) . . ?
F5D C16 F6D 105.5(11) . . ?
F6A C16 F6D 88.0(17) . . ?
F4A C16 F6D 27.5(14) . . ?
F4D C16 F6D 102.8(10) . . ?
F5C C16 F6D 75.1(13) . . ?
F6 C16 F6D 125.6(14) . . ?
F5A C16 F6D 128.6(14) . . ?
F4C C16 F4 27.6(14) . . ?
F5 C16 F4 105.9(12) . . ?
F5D C16 F4 82.1(14) . . ?
F6A C16 F4 63.0(16) . . ?
F4A C16 F4 54.0(15) . . ?
F4D C16 F4 125.4(13) . . ?
F5C C16 F4 100.8(11) . . ?
F6 C16 F4 103.1(10) . . ?
F5A C16 F4 142.6(15) . . ?
F6D C16 F4 27.5(11) . . ?
F4C C16 F6C 103.0(13) . . ?
F5 C16 F6C 87.7(17) . . ?
F5D C16 F6C 50.0(16) . . ?
F6A C16 F6C 69.8(16) . . ?
F4A C16 F6C 135.6(16) . . ?
F4D C16 F6C 71.6(15) . . ?
F5C C16 F6C 100.1(11) . . ?
F6 C16 F6C 29.7(13) . . ?
F5A C16 F6C 42.5(14) . . ?
F6D C16 F6C 145.3(14) . . ?
F4 C16 F6C 130.4(14) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.565
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.145

#===#END
#CCDC 640884
data_compound_2a
_database_code_depnum_ccdc_archive 'CCDC 640884'
#data_7093

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 F6 N4 O4 Pb'
_chemical_formula_weight         797.67

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Ia-3d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-1/4'

_cell_length_a                   34.8486(4)
_cell_length_b                   34.8486(4)
_cell_length_c                   34.8486(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     42321.0(8)
_cell_formula_units_Z            48
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    6584
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      18.61

_exptl_crystal_description       'half sphere'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             18432
_exptl_absorpt_coefficient_mu    4.849
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2742
_exptl_absorpt_correction_T_max  0.5938
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2005)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            118018
_diffrn_reflns_av_R_equivalents  0.1476
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3110
_reflns_number_gt                2195
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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.

The F atoms in CF3 group were found to be disordered. Two models were resolved
and DFIX option was used to contraint the geometry. The occupancy was fixed
at 0.5 and not refined.
;

_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^)+(0.0969P)^2^+352.1093P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3110
_refine_ls_number_parameters     204
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1778
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_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 0.860154(10) 0.8750 0.110154(10) 0.0681(3) Uani 1 2 d S . .
N1 N 0.8899(2) 0.9149(2) 0.1619(3) 0.064(2) Uani 1 1 d . . .
N2 N 1.0518(3) 0.9084(3) 0.1699(3) 0.085(3) Uani 1 1 d . . .
O1 O 0.9146(4) 0.9009(4) 0.0737(3) 0.134(5) Uani 1 1 d . . .
O2 O 0.9357(4) 0.8473(4) 0.0436(4) 0.145(5) Uani 1 1 d . . .
C1 C 0.8917(3) 0.9019(3) 0.1977(3) 0.071(3) Uani 1 1 d . . .
H1 H 0.8803 0.8784 0.2033 0.086 Uiso 1 1 calc R . .
C2 C 0.9097(3) 0.9216(3) 0.2271(3) 0.067(3) Uani 1 1 d . . .
H2 H 0.9105 0.9117 0.2518 0.080 Uiso 1 1 calc R . .
C3 C 0.9264(3) 0.9561(3) 0.2189(3) 0.058(2) Uani 1 1 d . . .
C4 C 0.9242(3) 0.9707(3) 0.1806(3) 0.069(3) Uani 1 1 d . . .
H4 H 0.9343 0.9946 0.1742 0.083 Uiso 1 1 calc R . .
C5 C 0.9064(3) 0.9480(3) 0.1533(3) 0.066(3) Uani 1 1 d . . .
H5 H 0.9061 0.9563 0.1279 0.079 Uiso 1 1 calc R . .
C6 C 0.9462(3) 0.9783(3) 0.2511(3) 0.064(3) Uani 1 1 d . . .
H6 H 0.9360 0.9701 0.2759 0.077 Uiso 1 1 calc R . .
C7 C 0.9923(3) 0.9779(3) 0.2523(3) 0.068(3) Uani 1 1 d . . .
H7 H 1.0013 0.9708 0.2780 0.081 Uiso 1 1 calc R . .
C10 C 1.0128(3) 0.9548(3) 0.2225(3) 0.064(3) Uani 1 1 d . . .
C9 C 1.0182(3) 0.9668(4) 0.1852(4) 0.092(4) Uani 1 1 d . . .
H9 H 1.0091 0.9904 0.1768 0.110 Uiso 1 1 calc R . .
C8 C 1.0383(4) 0.9417(4) 0.1602(4) 0.095(4) Uani 1 1 d . . .
H8 H 1.0421 0.9498 0.1350 0.114 Uiso 1 1 calc R . .
C12 C 1.0453(3) 0.8977(3) 0.2054(4) 0.085(4) Uani 1 1 d . . .
H12 H 1.0540 0.8736 0.2129 0.102 Uiso 1 1 calc R . .
C11 C 1.0263(3) 0.9195(3) 0.2323(4) 0.080(3) Uani 1 1 d . . .
H11 H 1.0228 0.9103 0.2571 0.097 Uiso 1 1 calc R . .
C13 C 0.9336(5) 0.8835(6) 0.0504(5) 0.110(5) Uani 1 1 d D A .
C14 C 0.9626(4) 0.9107(4) 0.0312(4) 0.193(12) Uani 1 1 d D . .
F1 F 0.9928(6) 0.8950(6) 0.0136(6) 0.140(6) Uani 0.50 1 d PD A 1
F2 F 0.9775(9) 0.9357(10) 0.0567(9) 0.276(16) Uani 0.50 1 d PD A 1
F3 F 0.9415(7) 0.9297(8) 0.0057(9) 0.236(14) Uani 0.50 1 d PD A 1
F1A F 0.9534(6) 0.9468(5) 0.0219(6) 0.140(6) Uani 0.50 1 d PD A 2
F2A F 0.9685(10) 0.8933(8) -0.0028(7) 0.276(16) Uani 0.50 1 d PD A 2
F3A F 0.9949(8) 0.9115(7) 0.0520(10) 0.236(14) Uani 0.50 1 d PD A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0809(4) 0.0425(3) 0.0809(4) -0.0094(2) -0.0461(3) 0.0094(2)
N1 0.057(5) 0.058(5) 0.077(6) -0.017(4) -0.028(4) 0.004(4)
N2 0.059(6) 0.091(8) 0.106(8) -0.042(7) 0.004(6) 0.015(5)
O1 0.132(9) 0.169(11) 0.102(8) 0.042(7) 0.027(7) 0.063(8)
O2 0.155(11) 0.145(10) 0.134(10) -0.010(9) -0.003(8) -0.051(9)
C1 0.066(7) 0.075(7) 0.074(8) -0.015(6) -0.012(6) -0.011(5)
C2 0.077(7) 0.062(7) 0.061(6) -0.012(5) -0.004(5) -0.006(5)
C3 0.061(6) 0.063(6) 0.048(6) -0.020(5) -0.009(4) 0.015(5)
C4 0.062(7) 0.048(6) 0.097(8) -0.016(5) -0.014(6) -0.003(5)
C5 0.064(6) 0.061(6) 0.073(7) -0.011(5) -0.026(5) 0.004(5)
C6 0.064(6) 0.057(5) 0.070(6) -0.010(5) -0.001(5) 0.005(5)
C7 0.053(6) 0.075(6) 0.075(7) -0.031(6) -0.008(5) 0.008(5)
C10 0.046(6) 0.090(8) 0.057(6) -0.028(6) -0.011(5) 0.002(5)
C9 0.070(8) 0.097(9) 0.107(10) -0.036(8) -0.017(7) 0.034(7)
C8 0.087(9) 0.119(12) 0.079(9) -0.026(8) -0.004(7) 0.023(8)
C12 0.069(8) 0.071(8) 0.116(11) -0.024(7) 0.029(7) 0.006(6)
C11 0.065(7) 0.066(7) 0.110(10) -0.022(7) 0.021(6) -0.001(6)
C13 0.091(11) 0.144(16) 0.095(11) 0.014(11) 0.014(9) 0.002(11)
C14 0.25(3) 0.16(2) 0.16(2) -0.039(19) 0.05(2) 0.07(2)
F1 0.140(14) 0.129(12) 0.150(12) -0.002(10) 0.039(11) -0.022(10)
F2 0.23(3) 0.18(2) 0.42(5) -0.02(3) 0.11(3) -0.04(2)
F3 0.19(2) 0.136(16) 0.38(4) 0.10(2) -0.05(2) -0.001(16)
F1A 0.140(14) 0.129(12) 0.150(12) -0.002(10) 0.039(11) -0.022(10)
F2A 0.23(3) 0.18(2) 0.42(5) -0.02(3) 0.11(3) -0.04(2)
F3A 0.19(2) 0.136(16) 0.38(4) 0.10(2) -0.05(2) -0.001(16)

_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 O1 2.457(12) 46_563 ?
Pb1 O1 2.457(12) . ?
Pb1 N1 2.500(8) . ?
Pb1 N1 2.500(8) 46_563 ?
N1 C5 1.325(13) . ?
N1 C1 1.330(14) . ?
N2 C8 1.299(17) . ?
N2 C12 1.313(16) . ?
O1 C13 1.210(18) . ?
O2 C13 1.285(19) . ?
C1 C2 1.385(14) . ?
C2 C3 1.364(14) . ?
C3 C4 1.431(14) . ?
C3 C6 1.528(13) . ?
C4 C5 1.384(14) . ?
C6 C6 1.513(19) 28_465 ?
C6 C7 1.608(14) . ?
C7 C10 1.497(14) . ?
C7 C7 1.55(2) 28_465 ?
C10 C11 1.361(15) . ?
C10 C9 1.375(17) . ?
C9 C8 1.422(16) . ?
C12 C11 1.377(15) . ?
C13 C14 1.539(15) . ?
C14 F3 1.331(10) . ?
C14 F1 1.335(10) . ?
C14 F1A 1.338(10) . ?
C14 F3A 1.340(10) . ?
C14 F2A 1.346(10) . ?
C14 F2 1.350(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 159.2(5) 46_563 . ?
O1 Pb1 N1 82.1(3) 46_563 . ?
O1 Pb1 N1 81.3(4) . . ?
O1 Pb1 N1 81.3(4) 46_563 46_563 ?
O1 Pb1 N1 82.1(3) . 46_563 ?
N1 Pb1 N1 73.2(4) . 46_563 ?
C5 N1 C1 119.2(9) . . ?
C5 N1 Pb1 120.1(7) . . ?
C1 N1 Pb1 120.5(7) . . ?
C8 N2 C12 115.9(11) . . ?
C13 O1 Pb1 125.7(12) . . ?
N1 C1 C2 123.2(11) . . ?
C3 C2 C1 118.4(10) . . ?
C2 C3 C4 119.2(9) . . ?
C2 C3 C6 118.9(9) . . ?
C4 C3 C6 121.9(9) . . ?
C5 C4 C3 117.4(10) . . ?
N1 C5 C4 122.6(10) . . ?
C6 C6 C3 118.1(10) 28_465 . ?
C6 C6 C7 90.5(5) 28_465 . ?
C3 C6 C7 117.8(8) . . ?
C10 C7 C7 117.6(12) . 28_465 ?
C10 C7 C6 117.5(8) . . ?
C7 C7 C6 89.4(5) 28_465 . ?
C11 C10 C9 117.7(10) . . ?
C11 C10 C7 118.4(11) . . ?
C9 C10 C7 123.8(11) . . ?
C10 C9 C8 117.4(12) . . ?
N2 C8 C9 124.6(14) . . ?
N2 C12 C11 124.6(13) . . ?
C10 C11 C12 119.6(13) . . ?
O1 C13 O2 130.4(16) . . ?
O1 C13 C14 109.9(17) . . ?
O2 C13 C14 119.2(15) . . ?
F3 C14 F1 109.6(15) . . ?
F3 C14 F1A 40.2(14) . . ?
F1 C14 F1A 117.6(18) . . ?
F3 C14 F3A 144.5(19) . . ?
F1 C14 F3A 66.1(17) . . ?
F1A C14 F3A 108.1(14) . . ?
F3 C14 F2A 73.8(17) . . ?
F1 C14 F2A 45.0(15) . . ?
F1A C14 F2A 104.3(14) . . ?
F3A C14 F2A 111.0(15) . . ?
F3 C14 F2 109.2(15) . . ?
F1 C14 F2 105.3(14) . . ?
F1A C14 F2 69.1(16) . . ?
F3A C14 F2 46.0(15) . . ?
F2A C14 F2 144(2) . . ?
F3 C14 C13 103.6(17) . . ?
F1 C14 C13 117.7(15) . . ?
F1A C14 C13 121.8(16) . . ?
F3A C14 C13 109.3(19) . . ?
F2A C14 C13 101.9(19) . . ?
F2 C14 C13 111(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.155

#===#END
#CCDC No. 640885
data_compound_3
_database_code_depnum_ccdc_archive 'CCDC 640885'
#data_abdul5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 F6 N4 O4 Pb'
_chemical_formula_weight         797.67

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   15.8071(8)
_cell_length_b                   10.1994(5)
_cell_length_c                   18.2899(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.518(2)
_cell_angle_gamma                90.00
_cell_volume                     2935.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3563
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      20.69

_exptl_crystal_description       block,
_exptl_crystal_colour            cream
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    5.826
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5793
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16990
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5168
_reflns_number_gt                4194
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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.

The F atoms in the two CF3 groups were disordered. Two disordered models
were resolved with fixed occupancy of 0.5 and included in the refinement
cycles. Only isotropic thermal parameters were refined for these F atoms.
;

_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^)+(0.0548P)^2^+4.4344P] 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    consr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5168
_refine_ls_number_parameters     382
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_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 0.651888(16) 0.32815(3) 0.743845(15) 0.04212(12) Uani 1 1 d . . .
N1 N 0.5124(4) 0.2772(6) 0.6731(3) 0.0438(15) Uani 1 1 d . . .
C1 C 0.4919(4) 0.1527(7) 0.6544(4) 0.0412(17) Uani 1 1 d . . .
H1 H 0.5303 0.0865 0.6690 0.049 Uiso 1 1 calc R . .
C2 C 0.4176(4) 0.1195(7) 0.6151(4) 0.0412(17) Uani 1 1 d . . .
H2 H 0.4062 0.0321 0.6034 0.049 Uiso 1 1 calc R . .
C3 C 0.3590(4) 0.2151(7) 0.5924(4) 0.0357(15) Uani 1 1 d . . .
C4 C 0.3796(5) 0.3427(7) 0.6117(5) 0.051(2) Uani 1 1 d . . .
H4 H 0.3421 0.4106 0.5979 0.061 Uiso 1 1 calc R . .
C5 C 0.4561(5) 0.3685(8) 0.6515(5) 0.056(2) Uani 1 1 d . . .
H5 H 0.4690 0.4551 0.6640 0.067 Uiso 1 1 calc R . .
N2 N 0.3124(4) -0.2000(6) 0.3690(3) 0.0447(15) Uani 1 1 d . . .
C6 C 0.3239(5) -0.2404(7) 0.4379(5) 0.054(2) Uani 1 1 d . . .
H6 H 0.3485 -0.3223 0.4472 0.065 Uiso 1 1 calc R . .
C7 C 0.3016(5) -0.1688(7) 0.4961(4) 0.0479(19) Uani 1 1 d . . .
H7 H 0.3105 -0.2023 0.5435 0.058 Uiso 1 1 calc R . .
C8 C 0.2657(4) -0.0459(6) 0.4842(3) 0.0320(14) Uani 1 1 d . . .
C9 C 0.2552(5) -0.0040(7) 0.4127(4) 0.0458(18) Uani 1 1 d . . .
H9 H 0.2324 0.0784 0.4015 0.055 Uiso 1 1 calc R . .
C10 C 0.2782(5) -0.0829(8) 0.3584(4) 0.054(2) Uani 1 1 d . . .
H10 H 0.2693 -0.0524 0.3104 0.064 Uiso 1 1 calc R . .
N3 N -0.0336(4) -0.0711(7) 0.6734(4) 0.0583(18) Uani 1 1 d . . .
C11 C -0.0384(4) 0.0525(8) 0.6502(4) 0.0472(18) Uani 1 1 d . . .
H11 H -0.0827 0.1037 0.6643 0.057 Uiso 1 1 calc R . .
C12 C 0.0176(4) 0.1100(8) 0.6069(4) 0.0457(18) Uani 1 1 d . . .
H12 H 0.0098 0.1962 0.5910 0.055 Uiso 1 1 calc R . .
C13 C 0.0867(4) 0.0361(7) 0.5870(3) 0.0355(15) Uani 1 1 d . . .
C14 C 0.0904(5) -0.0914(8) 0.6105(5) 0.054(2) Uani 1 1 d . . .
H14 H 0.1343 -0.1453 0.5980 0.065 Uiso 1 1 calc R . .
C15 C 0.0305(6) -0.1404(8) 0.6519(5) 0.065(2) Uani 1 1 d . . .
H15 H 0.0349 -0.2280 0.6660 0.078 Uiso 1 1 calc R . .
N4 N 0.1751(7) 0.3457(11) 0.7964(6) 0.101(3) Uani 1 1 d . . .
C16 C 0.2110(7) 0.2328(12) 0.7777(5) 0.082(3) Uani 1 1 d . . .
H16 H 0.2350 0.1798 0.8155 0.098 Uiso 1 1 calc R . .
C17 C 0.2151(6) 0.1895(9) 0.7068(5) 0.067(2) Uani 1 1 d . . .
H17 H 0.2376 0.1074 0.6980 0.080 Uiso 1 1 calc R . .
C18 C 0.1852(5) 0.2698(8) 0.6487(4) 0.0485(19) Uani 1 1 d . . .
C19 C 0.1492(6) 0.3853(10) 0.6673(6) 0.073(3) Uani 1 1 d . . .
H19 H 0.1272 0.4418 0.6303 0.088 Uiso 1 1 calc R . .
C20 C 0.1447(8) 0.4196(15) 0.7390(7) 0.110(5) Uani 1 1 d . . .
H20 H 0.1190 0.4990 0.7486 0.131 Uiso 1 1 calc R . .
C21 C 0.2766(4) 0.1831(6) 0.5468(4) 0.0363(16) Uani 1 1 d . . .
H21 H 0.2814 0.2110 0.4961 0.044 Uiso 1 1 calc R . .
C22 C 0.2423(4) 0.0408(6) 0.5457(3) 0.0323(15) Uani 1 1 d . . .
H22 H 0.2582 -0.0016 0.5931 0.039 Uiso 1 1 calc R . .
C23 C 0.1516(4) 0.0997(6) 0.5443(4) 0.0349(15) Uani 1 1 d . . .
H23 H 0.1278 0.1085 0.4931 0.042 Uiso 1 1 calc R . .
C24 C 0.1902(4) 0.2338(7) 0.5707(4) 0.0416(17) Uani 1 1 d . . .
H24 H 0.1677 0.3046 0.5382 0.050 Uiso 1 1 calc R . .
O1 O 0.6249(5) 0.5318(7) 0.6623(5) 0.118(3) Uani 1 1 d . . .
O2 O 0.6862(5) 0.7108(10) 0.7088(5) 0.126(3) Uani 1 1 d . . .
C25 C 0.6345(5) 0.6482(9) 0.6716(5) 0.060(2) Uani 1 1 d D A .
C26 C 0.5662(7) 0.7270(10) 0.6292(6) 0.098(4) Uani 1 1 d D . .
F1 F 0.5383(10) 0.6616(14) 0.5656(7) 0.138(6) Uiso 0.50 1 d PD A 1
F2 F 0.5851(8) 0.8406(10) 0.6037(8) 0.099(4) Uiso 0.50 1 d PD A 1
F3 F 0.4987(7) 0.7369(15) 0.6653(8) 0.121(5) Uiso 0.50 1 d PD A 1
F1A F 0.5809(10) 0.7571(19) 0.5621(7) 0.154(6) Uiso 0.50 1 d PD A 2
F2A F 0.5627(11) 0.8503(12) 0.6603(10) 0.160(7) Uiso 0.50 1 d PD A 2
F3A F 0.4885(6) 0.6872(11) 0.6275(8) 0.094(4) Uiso 0.50 1 d PD A 2
O3 O 0.6140(4) 0.1167(6) 0.7903(3) 0.0649(16) Uani 1 1 d . . .
O4 O 0.6628(5) 0.2009(6) 0.8977(3) 0.079(2) Uani 1 1 d . . .
C27 C 0.6357(5) 0.1127(8) 0.8579(4) 0.052(2) Uani 1 1 d D B .
C28 C 0.6212(6) -0.0213(11) 0.8971(6) 0.097(4) Uani 1 1 d D . .
F4 F 0.6554(9) -0.0278(13) 0.9640(6) 0.112(5) Uiso 0.50 1 d PD B 3
F5 F 0.6557(9) -0.1172(10) 0.8585(7) 0.102(4) Uiso 0.50 1 d PD B 3
F6 F 0.5391(7) -0.0467(14) 0.8929(9) 0.129(5) Uiso 0.50 1 d PD B 3
F4A F 0.6884(8) -0.0459(13) 0.9444(7) 0.118(5) Uiso 0.50 1 d PD B 4
F5A F 0.6019(10) -0.1163(11) 0.8529(7) 0.127(5) Uiso 0.50 1 d PD B 4
F6A F 0.5540(8) -0.0045(14) 0.9364(8) 0.128(5) Uiso 0.50 1 d PD B 4

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.03742(18) 0.04709(19) 0.04147(19) -0.01562(12) 0.00191(11) -0.00449(13)
N1 0.039(4) 0.046(4) 0.047(4) -0.012(3) 0.004(3) -0.008(3)
C1 0.035(4) 0.041(4) 0.046(4) -0.007(3) -0.001(3) -0.003(3)
C2 0.044(4) 0.038(4) 0.041(4) -0.007(3) 0.001(3) -0.014(3)
C3 0.028(4) 0.044(4) 0.035(4) -0.005(3) 0.004(3) -0.004(3)
C4 0.037(4) 0.051(5) 0.062(5) 0.002(4) -0.007(4) 0.000(4)
C5 0.048(5) 0.038(4) 0.079(6) -0.010(4) -0.003(4) -0.006(4)
N2 0.049(4) 0.051(4) 0.034(4) -0.005(3) 0.005(3) 0.000(3)
C6 0.071(6) 0.035(4) 0.058(5) 0.001(4) 0.015(4) 0.002(4)
C7 0.067(5) 0.044(4) 0.034(4) 0.007(3) 0.007(3) 0.007(4)
C8 0.025(3) 0.041(4) 0.030(4) -0.004(3) 0.005(3) -0.005(3)
C9 0.053(5) 0.055(5) 0.029(4) 0.000(3) -0.002(3) 0.018(4)
C10 0.055(5) 0.075(6) 0.028(4) -0.005(4) -0.008(3) 0.027(4)
N3 0.042(4) 0.073(5) 0.061(5) 0.014(4) 0.016(3) -0.008(3)
C11 0.032(4) 0.055(5) 0.055(5) -0.002(4) 0.009(3) 0.006(3)
C12 0.028(4) 0.055(5) 0.053(5) 0.005(4) 0.001(3) -0.004(3)
C13 0.032(4) 0.048(4) 0.027(3) -0.008(3) 0.004(3) -0.005(3)
C14 0.043(5) 0.057(5) 0.066(6) 0.004(4) 0.022(4) 0.003(4)
C15 0.058(6) 0.056(5) 0.084(7) 0.018(5) 0.027(5) 0.005(4)
N4 0.097(7) 0.141(10) 0.067(6) -0.055(6) 0.021(5) -0.017(6)
C16 0.081(7) 0.116(9) 0.048(6) -0.016(6) 0.001(5) -0.007(7)
C17 0.085(7) 0.078(6) 0.037(5) -0.007(4) 0.006(4) 0.003(5)
C18 0.038(4) 0.060(5) 0.047(5) -0.019(4) 0.003(3) -0.008(4)
C19 0.068(6) 0.071(6) 0.080(7) -0.030(5) 0.004(5) 0.009(5)
C20 0.114(11) 0.129(11) 0.086(10) -0.062(9) 0.015(8) -0.002(8)
C21 0.028(4) 0.046(4) 0.034(4) -0.009(3) 0.003(3) 0.001(3)
C22 0.027(3) 0.044(4) 0.025(3) -0.005(3) 0.001(2) -0.003(3)
C23 0.032(4) 0.043(4) 0.029(4) -0.005(3) 0.001(3) 0.002(3)
C24 0.036(4) 0.048(4) 0.041(4) 0.000(3) 0.005(3) -0.003(3)
O1 0.105(6) 0.067(5) 0.178(9) 0.036(5) -0.002(6) -0.007(4)
O2 0.065(5) 0.187(9) 0.119(7) -0.034(6) -0.016(5) -0.019(6)
C25 0.041(5) 0.074(6) 0.064(6) 0.012(5) -0.001(4) -0.003(4)
C26 0.083(8) 0.076(7) 0.140(12) 0.027(8) 0.027(8) -0.028(6)
O3 0.082(4) 0.067(4) 0.042(3) -0.008(3) -0.012(3) -0.020(3)
O4 0.122(6) 0.068(4) 0.046(4) -0.015(3) 0.004(4) -0.024(4)
C27 0.050(5) 0.052(5) 0.054(5) 0.001(4) 0.004(4) -0.001(4)
C28 0.090(8) 0.089(8) 0.105(9) -0.039(7) -0.022(7) 0.022(7)

_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 2.414(6) . ?
Pb1 N1 2.501(6) . ?
Pb1 N2 2.551(6) 3_656 ?
Pb1 O1 2.569(7) . ?
Pb1 N3 2.718(6) 2_556 ?
N1 C5 1.321(10) . ?
N1 C1 1.346(8) . ?
C1 C2 1.360(9) . ?
C2 C3 1.381(10) . ?
C3 C4 1.379(10) . ?
C3 C21 1.513(9) . ?
C4 C5 1.377(10) . ?
N2 C10 1.317(9) . ?
N2 C6 1.321(10) . ?
N2 Pb1 2.551(6) 3_656 ?
C6 C7 1.366(10) . ?
C7 C8 1.385(9) . ?
C8 C9 1.370(9) . ?
C8 C22 1.504(8) . ?
C9 C10 1.355(10) . ?
N3 C15 1.326(10) . ?
N3 C11 1.331(10) . ?
N3 Pb1 2.718(6) 2_546 ?
C11 C12 1.374(10) . ?
C12 C13 1.404(10) . ?
C13 C14 1.369(10) . ?
C13 C23 1.496(9) . ?
C14 C15 1.363(11) . ?
N4 C16 1.342(13) . ?
N4 C20 1.344(16) . ?
C16 C17 1.376(12) . ?
C17 C18 1.388(11) . ?
C18 C19 1.366(12) . ?
C18 C24 1.482(10) . ?
C19 C20 1.366(14) . ?
C21 C22 1.549(9) . ?
C21 C24 1.561(9) . ?
C22 C23 1.553(9) . ?
C23 C24 1.555(9) . ?
O1 C25 1.207(10) . ?
O2 C25 1.195(11) . ?
C25 C26 1.501(15) . ?
C26 F3A 1.290(11) . ?
C26 F2 1.295(11) . ?
C26 F1A 1.308(12) . ?
C26 F3 1.310(11) . ?
C26 F1 1.377(12) . ?
C26 F2A 1.383(12) . ?
O3 C27 1.251(9) . ?
O4 C27 1.209(9) . ?
C27 C28 1.570(15) . ?
C28 F5A 1.279(11) . ?
C28 F4 1.292(11) . ?
C28 F6 1.318(11) . ?
C28 F4A 1.328(11) . ?
C28 F6A 1.349(12) . ?
C28 F5 1.350(11) . ?

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 N1 76.1(2) . . ?
O3 Pb1 N2 84.75(19) . 3_656 ?
N1 Pb1 N2 74.2(2) . 3_656 ?
O3 Pb1 O1 153.4(2) . . ?
N1 Pb1 O1 77.2(2) . . ?
N2 Pb1 O1 89.0(3) 3_656 . ?
O3 Pb1 N3 86.3(2) . 2_556 ?
N1 Pb1 N3 75.3(2) . 2_556 ?
N2 Pb1 N3 149.5(2) 3_656 2_556 ?
O1 Pb1 N3 86.2(3) . 2_556 ?
C5 N1 C1 116.7(6) . . ?
C5 N1 Pb1 122.9(5) . . ?
C1 N1 Pb1 120.4(5) . . ?
N1 C1 C2 122.9(7) . . ?
C1 C2 C3 120.2(7) . . ?
C4 C3 C2 117.0(6) . . ?
C4 C3 C21 120.9(6) . . ?
C2 C3 C21 122.1(6) . . ?
C5 C4 C3 119.3(7) . . ?
N1 C5 C4 123.7(7) . . ?
C10 N2 C6 116.1(6) . . ?
C10 N2 Pb1 117.7(5) . 3_656 ?
C6 N2 Pb1 126.2(5) . 3_656 ?
N2 C6 C7 123.7(7) . . ?
C6 C7 C8 119.6(7) . . ?
C9 C8 C7 116.3(6) . . ?
C9 C8 C22 121.0(6) . . ?
C7 C8 C22 122.7(6) . . ?
C10 C9 C8 119.9(7) . . ?
N2 C10 C9 124.5(7) . . ?
C15 N3 C11 115.6(7) . . ?
C15 N3 Pb1 123.4(5) . 2_546 ?
C11 N3 Pb1 121.0(5) . 2_546 ?
N3 C11 C12 124.7(7) . . ?
C11 C12 C13 118.7(7) . . ?
C14 C13 C12 116.1(7) . . ?
C14 C13 C23 124.4(6) . . ?
C12 C13 C23 119.4(6) . . ?
C15 C14 C13 120.8(8) . . ?
N3 C15 C14 124.1(8) . . ?
C16 N4 C20 114.2(10) . . ?
N4 C16 C17 125.1(11) . . ?
C16 C17 C18 119.2(9) . . ?
C19 C18 C17 115.9(8) . . ?
C19 C18 C24 121.0(8) . . ?
C17 C18 C24 123.1(7) . . ?
C20 C19 C18 121.4(11) . . ?
N4 C20 C19 124.0(12) . . ?
C3 C21 C22 119.4(6) . . ?
C3 C21 C24 120.3(6) . . ?
C22 C21 C24 90.0(5) . . ?
C8 C22 C21 116.7(5) . . ?
C8 C22 C23 120.5(5) . . ?
C21 C22 C23 87.7(5) . . ?
C13 C23 C22 120.1(6) . . ?
C13 C23 C24 119.2(5) . . ?
C22 C23 C24 90.0(5) . . ?
C18 C24 C23 117.4(6) . . ?
C18 C24 C21 118.7(6) . . ?
C23 C24 C21 87.1(5) . . ?
C25 O1 Pb1 134.6(8) . . ?
O2 C25 O1 132.5(10) . . ?
O2 C25 C26 115.2(9) . . ?
O1 C25 C26 112.3(8) . . ?
F3A C26 F2 121.7(13) . . ?
F3A C26 F1A 107.8(12) . . ?
F2 C26 F1A 51.9(9) . . ?
F3A C26 F3 38.6(8) . . ?
F2 C26 F3 109.9(11) . . ?
F1A C26 F3 133.0(14) . . ?
F3A C26 F1 66.4(9) . . ?
F2 C26 F1 101.2(10) . . ?
F1A C26 F1 52.5(9) . . ?
F3 C26 F1 104.7(10) . . ?
F3A C26 F2A 102.8(10) . . ?
F2 C26 F2A 49.8(8) . . ?
F1A C26 F2A 101.0(10) . . ?
F3 C26 F2A 70.0(10) . . ?
F1 C26 F2A 140.0(14) . . ?
F3A C26 C25 118.7(9) . . ?
F2 C26 C25 119.0(9) . . ?
F1A C26 C25 115.2(10) . . ?
F3 C26 C25 111.2(10) . . ?
F1 C26 C25 109.4(9) . . ?
F2A C26 C25 109.2(10) . . ?
C27 O3 Pb1 108.9(5) . . ?
O4 C27 O3 128.1(8) . . ?
O4 C27 C28 115.6(7) . . ?
O3 C27 C28 116.2(7) . . ?
F5A C28 F4 127.8(14) . . ?
F5A C28 F6 69.0(9) . . ?
F4 C28 F6 111.4(12) . . ?
F5A C28 F4A 113.4(11) . . ?
F4 C28 F4A 30.4(8) . . ?
F6 C28 F4A 136.2(14) . . ?
F5A C28 F6A 106.3(11) . . ?
F4 C28 F6A 77.3(10) . . ?
F6 C28 F6A 40.1(8) . . ?
F4A C28 F6A 107.3(11) . . ?
F5A C28 F5 37.4(8) . . ?
F4 C28 F5 107.8(10) . . ?
F6 C28 F5 105.8(10) . . ?
F4A C28 F5 82.3(9) . . ?
F6A C28 F5 138.4(13) . . ?
F5A C28 C27 114.0(10) . . ?
F4 C28 C27 114.3(9) . . ?
F6 C28 C27 109.3(9) . . ?
F4A C28 C27 108.6(9) . . ?
F6A C28 C27 106.8(9) . . ?
F5 C28 C27 107.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.124
#===#END