# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_AB(djhnmr)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H19 N7 O'
_chemical_formula_sum            'C14 H19 N7 O'
_chemical_formula_weight         301.36

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'

_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                   11.7201(15)
_cell_length_b                   8.1454(10)
_cell_length_c                   15.683(3)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 100.962(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     1469.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    2615
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.98

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8707
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            9733
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2673
_reflns_number_gt                2139
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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)+(0.0633P)²+1.7424P] 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         2673
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1563
_refine_ls_wR_factor_gt          0.1444
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
C1 C 0.52586(19) 0.6803(3) 0.57467(17) 0.0222(6) Uani 1 1 d . . .
H1A H 0.5037 0.6757 0.5119 0.027 Uiso 1 1 calc R . .
H1B H 0.5409 0.7942 0.5912 0.027 Uiso 1 1 calc R . .
C2 C 0.4268(2) 0.6171(3) 0.61473(17) 0.0191(5) Uani 1 1 d . . .
C3 C 0.4255(2) 0.6437(3) 0.70205(18) 0.0240(6) Uani 1 1 d . . .
H3 H 0.4854 0.7015 0.7368 0.029 Uiso 1 1 calc R . .
C4 C 0.3335(2) 0.5828(3) 0.73659(17) 0.0249(6) Uani 1 1 d . . .
H4 H 0.3317 0.5972 0.7952 0.030 Uiso 1 1 calc R . .
C5 C 0.2448(2) 0.5006(3) 0.68332(16) 0.0218(6) Uani 1 1 d . . .
H5 H 0.1817 0.4606 0.7051 0.026 Uiso 1 1 calc R . .
C6 C 0.25119(19) 0.4785(3) 0.59615(16) 0.0191(5) Uani 1 1 d . . .
C7 C 0.16361(19) 0.3911(3) 0.53383(16) 0.0189(5) Uani 1 1 d . . .
H7 H 0.1748 0.3753 0.4773 0.023 Uiso 1 1 calc R . .
C8 C 0.0117(2) 0.2235(3) 0.40963(17) 0.0244(6) Uani 1 1 d . . .
H8A H 0.0161 0.3271 0.3813 0.037 Uiso 1 1 calc R . .
H8B H -0.0518 0.1607 0.3779 0.037 Uiso 1 1 calc R . .
H8C H 0.0830 0.1643 0.4116 0.037 Uiso 1 1 calc R . .
C9 C -0.10957(19) 0.2027(3) 0.52311(16) 0.0183(5) Uani 1 1 d . . .
C10 C -0.13700(19) 0.2567(3) 0.60053(16) 0.0178(5) Uani 1 1 d . . .
H10 H -0.0885 0.3269 0.6378 0.021 Uiso 1 1 calc R . .
C11 C -0.2416(2) 0.1997(3) 0.61932(16) 0.0185(5) Uani 1 1 d . . .
C12 C -0.2776(2) 0.0588(3) 0.49178(16) 0.0191(5) Uani 1 1 d . . .
C14 C -0.3574(2) -0.0477(3) 0.42921(17) 0.0232(6) Uani 1 1 d . . .
H14A H -0.3259 -0.1566 0.4303 0.035 Uiso 1 1 calc R . .
H14B H -0.3653 -0.0032 0.3717 0.035 Uiso 1 1 calc R . .
H14C H -0.4323 -0.0515 0.4455 0.035 Uiso 1 1 calc R . .
C15 C -0.3982(2) 0.2210(3) 0.70359(18) 0.0246(6) Uani 1 1 d . . .
H15A H -0.4425 0.3142 0.6787 0.037 Uiso 1 1 calc R . .
H15B H -0.4022 0.2127 0.7640 0.037 Uiso 1 1 calc R . .
H15C H -0.4295 0.1230 0.6740 0.037 Uiso 1 1 calc R . .
N1 N 0.34220(16) 0.5345(2) 0.56251(13) 0.0177(5) Uani 1 1 d . . .
N2 N 0.07054(16) 0.3355(2) 0.55674(13) 0.0195(5) Uani 1 1 d . . .
N3 N -0.00687(17) 0.2511(2) 0.49748(14) 0.0196(5) Uani 1 1 d . . .
N4 N -0.17931(16) 0.1047(2) 0.46700(13) 0.0192(5) Uani 1 1 d . . .
N5 N -0.31296(16) 0.0984(2) 0.56521(13) 0.0190(5) Uani 1 1 d . . .
N6 N -0.27775(17) 0.2407(2) 0.69460(14) 0.0212(5) Uani 1 1 d . . .
N7 N -0.21377(18) 0.3635(3) 0.74568(14) 0.0261(5) Uani 1 1 d . . .
H7A H -0.1554 0.4086 0.7290 0.031 Uiso 1 1 calc R . .
H7B H -0.2331 0.3935 0.7936 0.031 Uiso 1 1 calc R . .
O1 O 0.62980(13) 0.5865(2) 0.60182(11) 0.0243(4) Uani 1 1 d . . .
H1 H 0.6285 0.5056 0.5706 0.036 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.432(3) . ?
C1 C2 1.512(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.340(3) . ?
C2 C3 1.389(4) . ?
C3 C4 1.388(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(3) . ?
C5 H5 0.9300 . ?
C6 N1 1.356(3) . ?
C6 C7 1.461(3) . ?
C7 N2 1.293(3) . ?
C7 H7 0.9300 . ?
C8 N3 1.453(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.344(3) . ?
C9 C10 1.385(3) . ?
C9 N3 1.396(3) . ?
C10 C11 1.394(3) . ?
C10 H10 0.9300 . ?
C11 N5 1.353(3) . ?
C11 N6 1.369(3) . ?
C12 N5 1.335(3) . ?
C12 N4 1.338(3) . ?
C12 C14 1.497(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N6 1.454(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 N3 1.356(3) . ?
N6 N7 1.406(3) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
O1 H1 0.8200 . ?

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 C1 C2 111.8(2) . . ?
O1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
O1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C3 122.4(2) . . ?
N1 C2 C1 117.0(2) . . ?
C3 C2 C1 120.6(2) . . ?
C4 C3 C2 118.9(2) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 118.8(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
N1 C6 C5 122.1(2) . . ?
N1 C6 C7 114.1(2) . . ?
C5 C6 C7 123.8(2) . . ?
N2 C7 C6 120.5(2) . . ?
N2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 123.3(2) . . ?
N4 C9 N3 115.4(2) . . ?
C10 C9 N3 121.3(2) . . ?
C9 C10 C11 116.1(2) . . ?
C9 C10 H10 122.0 . . ?
C11 C10 H10 122.0 . . ?
N5 C11 N6 115.7(2) . . ?
N5 C11 C10 122.3(2) . . ?
N6 C11 C10 122.0(2) . . ?
N5 C12 N4 127.5(2) . . ?
N5 C12 C14 116.6(2) . . ?
N4 C12 C14 115.9(2) . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C2 N1 C6 118.4(2) . . ?
C7 N2 N3 118.5(2) . . ?
N2 N3 C9 116.5(2) . . ?
N2 N3 C8 121.82(19) . . ?
C9 N3 C8 121.5(2) . . ?
C12 N4 C9 115.2(2) . . ?
C12 N5 C11 115.60(19) . . ?
C11 N6 N7 116.49(19) . . ?
C11 N6 C15 121.5(2) . . ?
N7 N6 C15 116.47(19) . . ?
N6 N7 H7A 120.0 . . ?
N6 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C1 O1 H1 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 976898'
#######################################################################
#
#                 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_L1(sdjh485)

# start Validation Reply Form
_vrf_THETM01_L1sdjh485           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Weak diffracting crystal. See _expl_special_details
;
_vrf_PLAT029_L1sdjh485           
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.822       
RESPONSE: Weak diffracting crystal. See _expl_special_details
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H42 N16 O2'
_chemical_formula_sum            'C40 H42 N16 O2'
_chemical_formula_weight         778.90

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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I4(1)/a  '

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

_cell_length_a                   33.8887(17)
_cell_length_b                   33.8887
_cell_length_c                   15.8396(10)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     18191.1(13)
_cell_formula_units_Z            16
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    8236
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      23.84

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_min          0.24
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_max          0.59
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6560
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8627
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
;
Crystals of L1 were difficult to grow and diffracted poorly. 
The report structure contained diffuse disordered solvent which 
contributed to the poor diffraction. No meaningful data could be
obtained beyond theta 23.99. This dataset was the best of the three 
that were collected and solved.
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            91123
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         23.99
_reflns_number_total             5861
_reflns_number_gt                5387
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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)+(0.0545P)²+55.7759P] 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       0.00050(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5861
_refine_ls_number_parameters     530
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1648
_refine_ls_wR_factor_gt          0.1621
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.013
_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
C1 C 0.19800(12) -0.22364(11) 0.2770(3) 0.0510(10) Uani 1 1 d . . .
H1A H 0.2068 -0.2464 0.3090 0.061 Uiso 1 1 calc R . .
H1B H 0.1709 -0.2181 0.2926 0.061 Uiso 1 1 calc R . .
C2 C 0.22344(11) -0.18867(10) 0.2985(2) 0.0403(9) Uani 1 1 d . . .
C3 C 0.20943(11) -0.15042(10) 0.2912(2) 0.0410(9) Uani 1 1 d . . .
H3 H 0.1836 -0.1458 0.2738 0.049 Uiso 1 1 calc R . .
C4 C 0.23398(11) -0.11927(10) 0.3098(2) 0.0403(9) Uani 1 1 d . . .
H4 H 0.2250 -0.0934 0.3055 0.048 Uiso 1 1 calc R . .
C5 C 0.27214(10) -0.12703(10) 0.3350(2) 0.0387(9) Uani 1 1 d . . .
H5 H 0.2891 -0.1065 0.3496 0.046 Uiso 1 1 calc R . .
C6 C 0.28491(10) -0.16581(9) 0.3383(2) 0.0352(8) Uani 1 1 d . . .
C7 C 0.32608(11) -0.17658(10) 0.3578(2) 0.0428(9) Uani 1 1 d . . .
H7 H 0.3345 -0.2027 0.3544 0.051 Uiso 1 1 calc R . .
C8 C 0.40474(12) -0.19677(11) 0.3812(3) 0.0680(13) Uani 1 1 d . . .
H8A H 0.3905 -0.2156 0.4147 0.102 Uiso 1 1 calc R . .
H8B H 0.4320 -0.1970 0.3974 0.102 Uiso 1 1 calc R . .
H8C H 0.4025 -0.2036 0.3226 0.102 Uiso 1 1 calc R . .
C9 C 0.41110(10) -0.12565(10) 0.4223(2) 0.0382(8) Uani 1 1 d . . .
C10 C 0.39380(10) -0.09012(9) 0.4420(2) 0.0351(8) Uani 1 1 d . . .
H10 H 0.3668 -0.0861 0.4354 0.042 Uiso 1 1 calc R . .
C11 C 0.41813(9) -0.06090(10) 0.4719(2) 0.0358(8) Uani 1 1 d . . .
C12 C 0.47152(10) -0.10057(11) 0.4551(2) 0.0428(9) Uani 1 1 d . . .
C13 C 0.51566(10) -0.10571(13) 0.4569(3) 0.0589(11) Uani 1 1 d . . .
H13A H 0.5260 -0.0946 0.5080 0.088 Uiso 1 1 calc R . .
H13B H 0.5271 -0.0925 0.4092 0.088 Uiso 1 1 calc R . .
H13C H 0.5220 -0.1333 0.4546 0.088 Uiso 1 1 calc R . .
C14 C 0.42811(10) 0.00791(10) 0.5247(3) 0.0431(9) Uani 1 1 d . . .
H14A H 0.4553 0.0002 0.5222 0.065 Uiso 1 1 calc R . .
H14B H 0.4214 0.0149 0.5817 0.065 Uiso 1 1 calc R . .
H14C H 0.4239 0.0302 0.4884 0.065 Uiso 1 1 calc R . .
C15 C 0.34694(10) 0.01222(10) 0.5090(2) 0.0361(8) Uani 1 1 d . . .
H15 H 0.3620 0.0336 0.5269 0.043 Uiso 1 1 calc R . .
C16 C 0.30438(9) 0.01606(9) 0.5003(2) 0.0320(8) Uani 1 1 d . . .
C17 C 0.27873(9) -0.01550(9) 0.4865(2) 0.0326(8) Uani 1 1 d . . .
H17 H 0.2877 -0.0414 0.4849 0.039 Uiso 1 1 calc R . .
C18 C 0.23874(9) -0.00609(9) 0.4753(2) 0.0314(8) Uani 1 1 d . . .
C19 C 0.25268(10) 0.05942(9) 0.4942(2) 0.0329(8) Uani 1 1 d . . .
C20 C 0.23790(10) 0.10048(10) 0.5032(2) 0.0383(9) Uani 1 1 d . . .
C21 C 0.20258(10) 0.11200(10) 0.4662(2) 0.0442(9) Uani 1 1 d . . .
H21 H 0.1882 0.0943 0.4335 0.053 Uiso 1 1 calc R . .
C22 C 0.18885(12) 0.15042(11) 0.4786(3) 0.0556(12) Uani 1 1 d . . .
H22 H 0.1655 0.1584 0.4532 0.067 Uiso 1 1 calc R . .
C23 C 0.20982(13) 0.17665(11) 0.5284(3) 0.0561(12) Uani 1 1 d . . .
H23 H 0.2002 0.2020 0.5373 0.067 Uiso 1 1 calc R . .
C24 C 0.24481(12) 0.16511(10) 0.5646(3) 0.0526(11) Uani 1 1 d . . .
H24 H 0.2590 0.1828 0.5978 0.063 Uiso 1 1 calc R . .
C25 C 0.25888(10) 0.12761(9) 0.5519(2) 0.0412(9) Uani 1 1 d . . .
H25 H 0.2827 0.1202 0.5762 0.049 Uiso 1 1 calc R . .
C26 C 0.20766(9) -0.03530(9) 0.4595(2) 0.0324(8) Uani 1 1 d . . .
H26 H 0.1845 -0.0275 0.4329 0.039 Uiso 1 1 calc R . .
C27 C 0.14659(9) -0.08601(10) 0.4225(2) 0.0390(9) Uani 1 1 d . . .
H27A H 0.1333 -0.0649 0.4513 0.059 Uiso 1 1 calc R . .
H27B H 0.1293 -0.1083 0.4184 0.059 Uiso 1 1 calc R . .
H27C H 0.1540 -0.0775 0.3669 0.059 Uiso 1 1 calc R . .
C28 C 0.18942(9) -0.13657(9) 0.4898(2) 0.0304(8) Uani 1 1 d . . .
C29 C 0.22561(9) -0.14871(9) 0.5202(2) 0.0311(8) Uani 1 1 d . . .
H29 H 0.2456 -0.1309 0.5334 0.037 Uiso 1 1 calc R . .
C30 C 0.23029(9) -0.18878(9) 0.5300(2) 0.0323(8) Uani 1 1 d . . .
C31 C 0.16695(10) -0.19976(10) 0.4899(2) 0.0372(8) Uani 1 1 d . . .
C32 C 0.13339(10) -0.22810(10) 0.4760(3) 0.0495(10) Uani 1 1 d . . .
H32A H 0.1135 -0.2238 0.5181 0.074 Uiso 1 1 calc R . .
H32B H 0.1430 -0.2547 0.4800 0.074 Uiso 1 1 calc R . .
H32C H 0.1223 -0.2239 0.4209 0.074 Uiso 1 1 calc R . .
C33 C 0.27412(11) -0.24694(10) 0.5566(3) 0.0497(10) Uani 1 1 d . . .
H33A H 0.2905 -0.2540 0.5096 0.075 Uiso 1 1 calc R . .
H33B H 0.2496 -0.2610 0.5532 0.075 Uiso 1 1 calc R . .
H33C H 0.2873 -0.2537 0.6083 0.075 Uiso 1 1 calc R . .
C34 C 0.33058(9) -0.19028(9) 0.5849(2) 0.0357(8) Uani 1 1 d . . .
H34 H 0.3367 -0.2168 0.5783 0.043 Uiso 1 1 calc R . .
C35 C 0.36120(9) -0.16196(9) 0.6090(2) 0.0332(8) Uani 1 1 d . . .
C36 C 0.35310(10) -0.12272(9) 0.6288(2) 0.0392(9) Uani 1 1 d . . .
H36 H 0.3275 -0.1129 0.6254 0.047 Uiso 1 1 calc R . .
C37 C 0.38372(10) -0.09891(10) 0.6532(2) 0.0437(9) Uani 1 1 d . . .
H37 H 0.3790 -0.0727 0.6677 0.052 Uiso 1 1 calc R . .
C38 C 0.42159(10) -0.11395(10) 0.6563(2) 0.0415(9) Uani 1 1 d . . .
H38 H 0.4427 -0.0980 0.6720 0.050 Uiso 1 1 calc R . .
C39 C 0.42766(9) -0.15309(9) 0.6357(2) 0.0354(8) Uani 1 1 d . . .
C40 C 0.46807(9) -0.17193(10) 0.6362(3) 0.0419(9) Uani 1 1 d . . .
H40A H 0.4661 -0.1989 0.6564 0.050 Uiso 1 1 calc R . .
H40B H 0.4785 -0.1726 0.5792 0.050 Uiso 1 1 calc R . .
N1 N 0.26103(9) -0.19635(8) 0.32087(18) 0.0403(7) Uani 1 1 d . . .
N2 N 0.35022(8) -0.14887(8) 0.37970(19) 0.0393(7) Uani 1 1 d . . .
N3 N 0.38840(8) -0.15742(8) 0.3948(2) 0.0427(8) Uani 1 1 d . . .
N4 N 0.45056(8) -0.13175(9) 0.42903(19) 0.0434(8) Uani 1 1 d . . .
N5 N 0.45771(8) -0.06573(9) 0.47897(19) 0.0427(8) Uani 1 1 d . . .
N6 N 0.40356(8) -0.02451(8) 0.49729(19) 0.0378(7) Uani 1 1 d . . .
N7 N 0.36361(7) -0.02112(8) 0.49173(18) 0.0346(7) Uani 1 1 d . . .
N8 N 0.29127(7) 0.05361(7) 0.50534(18) 0.0329(7) Uani 1 1 d . . .
N9 N 0.22592(7) 0.03135(7) 0.47696(18) 0.0334(7) Uani 1 1 d . . .
N10 N 0.21203(7) -0.07144(8) 0.48188(17) 0.0317(7) Uani 1 1 d . . .
N11 N 0.18172(7) -0.09707(7) 0.46940(17) 0.0315(7) Uani 1 1 d . . .
N12 N 0.15922(8) -0.16162(8) 0.47523(18) 0.0361(7) Uani 1 1 d . . .
N13 N 0.20135(8) -0.21527(8) 0.51548(19) 0.0373(7) Uani 1 1 d . . .
N14 N 0.26651(8) -0.20480(7) 0.55477(19) 0.0385(7) Uani 1 1 d . . .
N15 N 0.29522(8) -0.17807(8) 0.57289(18) 0.0347(7) Uani 1 1 d . . .
N16 N 0.39811(8) -0.17689(7) 0.61298(19) 0.0357(7) Uani 1 1 d . . .
O1 O 0.19999(8) -0.23224(7) 0.18943(17) 0.0534(7) Uani 1 1 d . . .
H1 H 0.2230 -0.2364 0.1760 0.080 Uiso 1 1 calc R . .
O2 O 0.49361(7) -0.15053(8) 0.6884(2) 0.0656(9) Uani 1 1 d . . .
H2 H 0.5159 -0.1509 0.6683 0.098 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.419(5) . ?
C1 C2 1.504(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.348(5) . ?
C2 C3 1.385(5) . ?
C3 C4 1.376(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(5) . ?
C5 H5 0.9300 . ?
C6 N1 1.343(4) . ?
C6 C7 1.475(5) . ?
C7 N2 1.293(4) . ?
C7 H7 0.9300 . ?
C8 N3 1.460(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.358(4) . ?
C9 C10 1.375(5) . ?
C9 N3 1.393(4) . ?
C10 C11 1.373(5) . ?
C10 H10 0.9300 . ?
C11 N5 1.356(4) . ?
C11 N6 1.388(4) . ?
C12 N5 1.325(5) . ?
C12 N4 1.339(5) . ?
C12 C13 1.506(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N6 1.445(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N7 1.292(4) . ?
C15 C16 1.455(5) . ?
C15 H15 0.9300 . ?
C16 N8 1.350(4) . ?
C16 C17 1.395(4) . ?
C17 C18 1.403(4) . ?
C17 H17 0.9300 . ?
C18 N9 1.341(4) . ?
C18 C26 1.467(4) . ?
C19 N8 1.334(4) . ?
C19 N9 1.343(4) . ?
C19 C20 1.485(5) . ?
C20 C21 1.389(5) . ?
C20 C25 1.395(5) . ?
C21 C22 1.396(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.374(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.372(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 N10 1.284(4) . ?
C26 H26 0.9300 . ?
C27 N11 1.452(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N12 1.349(4) . ?
C28 C29 1.381(4) . ?
C28 N11 1.401(4) . ?
C29 C30 1.376(4) . ?
C29 H29 0.9300 . ?
C30 N13 1.349(4) . ?
C30 N14 1.399(4) . ?
C31 N12 1.339(4) . ?
C31 N13 1.341(4) . ?
C31 C32 1.505(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N14 1.451(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N15 1.282(4) . ?
C34 C35 1.465(5) . ?
C34 H34 0.9300 . ?
C35 N16 1.351(4) . ?
C35 C36 1.393(5) . ?
C36 C37 1.370(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.382(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.381(5) . ?
C38 H38 0.9300 . ?
C39 N16 1.335(4) . ?
C39 C40 1.511(5) . ?
C40 O2 1.400(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
N2 N3 1.348(4) . ?
N6 N7 1.362(4) . ?
N10 N11 1.360(4) . ?
N14 N15 1.360(4) . ?
O1 H1 0.8200 . ?
O2 H2 0.8200 . ?

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 C1 C2 110.8(3) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C3 121.8(3) . . ?
N1 C2 C1 116.7(3) . . ?
C3 C2 C1 121.5(3) . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
N1 C6 C5 122.4(3) . . ?
N1 C6 C7 115.0(3) . . ?
C5 C6 C7 122.6(3) . . ?
N2 C7 C6 118.4(3) . . ?
N2 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 122.4(3) . . ?
N4 C9 N3 116.8(3) . . ?
C10 C9 N3 120.8(3) . . ?
C11 C10 C9 117.0(3) . . ?
C11 C10 H10 121.5 . . ?
C9 C10 H10 121.5 . . ?
N5 C11 C10 122.4(3) . . ?
N5 C11 N6 115.8(3) . . ?
C10 C11 N6 121.8(3) . . ?
N5 C12 N4 127.2(3) . . ?
N5 C12 C13 116.7(3) . . ?
N4 C12 C13 116.2(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 119.4(3) . . ?
N7 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
N8 C16 C17 121.8(3) . . ?
N8 C16 C15 113.9(3) . . ?
C17 C16 C15 124.3(3) . . ?
C16 C17 C18 116.6(3) . . ?
C16 C17 H17 121.7 . . ?
C18 C17 H17 121.7 . . ?
N9 C18 C17 121.7(3) . . ?
N9 C18 C26 114.1(3) . . ?
C17 C18 C26 124.2(3) . . ?
N8 C19 N9 125.8(3) . . ?
N8 C19 C20 117.1(3) . . ?
N9 C19 C20 117.1(3) . . ?
C21 C20 C25 119.2(3) . . ?
C21 C20 C19 120.9(3) . . ?
C25 C20 C19 119.9(3) . . ?
C20 C21 C22 119.3(4) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C23 C22 C21 120.5(4) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C25 C24 C23 120.2(4) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C20 120.9(4) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?
N10 C26 C18 120.9(3) . . ?
N10 C26 H26 119.5 . . ?
C18 C26 H26 119.5 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N12 C28 C29 123.1(3) . . ?
N12 C28 N11 114.9(3) . . ?
C29 C28 N11 122.0(3) . . ?
C30 C29 C28 115.8(3) . . ?
C30 C29 H29 122.1 . . ?
C28 C29 H29 122.1 . . ?
N13 C30 C29 123.6(3) . . ?
N13 C30 N14 115.3(3) . . ?
C29 C30 N14 121.0(3) . . ?
N12 C31 N13 126.9(3) . . ?
N12 C31 C32 116.3(3) . . ?
N13 C31 C32 116.8(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N14 C33 H33A 109.5 . . ?
N14 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N14 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N15 C34 C35 119.3(3) . . ?
N15 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
N16 C35 C36 122.0(3) . . ?
N16 C35 C34 115.0(3) . . ?
C36 C35 C34 123.0(3) . . ?
C37 C36 C35 118.4(3) . . ?
C37 C36 H36 120.8 . . ?
C35 C36 H36 120.8 . . ?
C36 C37 C38 119.8(3) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C39 C38 C37 119.0(3) . . ?
C39 C38 H38 120.5 . . ?
C37 C38 H38 120.5 . . ?
N16 C39 C38 122.1(3) . . ?
N16 C39 C40 115.2(3) . . ?
C38 C39 C40 122.6(3) . . ?
O2 C40 C39 110.2(3) . . ?
O2 C40 H40A 109.6 . . ?
C39 C40 H40A 109.6 . . ?
O2 C40 H40B 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
C6 N1 C2 118.4(3) . . ?
C7 N2 N3 119.9(3) . . ?
N2 N3 C9 114.8(3) . . ?
N2 N3 C8 122.3(3) . . ?
C9 N3 C8 122.9(3) . . ?
C12 N4 C9 115.3(3) . . ?
C12 N5 C11 115.7(3) . . ?
N7 N6 C11 114.2(3) . . ?
N7 N6 C14 121.9(3) . . ?
C11 N6 C14 123.9(3) . . ?
C15 N7 N6 119.6(3) . . ?
C19 N8 C16 117.0(3) . . ?
C18 N9 C19 117.1(3) . . ?
C26 N10 N11 118.8(3) . . ?
N10 N11 C28 115.9(2) . . ?
N10 N11 C27 121.9(3) . . ?
C28 N11 C27 121.1(2) . . ?
C31 N12 C28 115.4(3) . . ?
C31 N13 C30 115.0(3) . . ?
N15 N14 C30 115.4(2) . . ?
N15 N14 C33 121.6(3) . . ?
C30 N14 C33 122.9(3) . . ?
C34 N15 N14 119.0(3) . . ?
C39 N16 C35 118.7(3) . . ?
C1 O1 H1 109.5 . . ?
C40 O2 H2 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.822
_diffrn_reflns_theta_full        23.99
_diffrn_measured_fraction_theta_full 0.822
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.055

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.250 0.625 868.9 202.7
2 0.000 0.750 0.375 868.8 202.6
3 0.500 0.250 0.875 868.9 202.6
4 0.500 0.750 0.125 869.0 202.7
_platon_squeeze_details          
; ?
;
_database_code_depnum_ccdc_archive 'CCDC 976899'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1(djh558)

# start Validation Reply Form
_vrf_THETM01_1djh558             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Weak diffracting crystal. See _expl_special_details
;
_vrf_REFNR01_1djh558             
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: Weak diffracting crystal, large structure. See _expl_special_details
;
_vrf_PLAT780_1djh558             
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do ! 
RESPONSE: The atoms from ligand L1 are connected to each other and the donor
atoms are connected to the four Pb atoms. Seven of the eight ClO4- anions are
also connected to the Pb atoms as are two H2O molecules.
;
_vrf_PLAT088_1djh558             
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.76       
RESPONSE: Weak diffracting crystal, large structure. See _expl_special_details
;
_vrf_PLAT230_1djh558             
;
PROBLEM: Hirshfeld Test Diff for    Cl2    --  O22     ..        7.9 su    
RESPONSE: Disordered ClO4- anion. See _refine_special_details
;
_vrf_PLAT232_1djh558             
;
PROBLEM: Hirshfeld Test Diff (M-X)  Pb1    --  O21     ..       13.5 su    
RESPONSE: Disordered ClO4- anion. See _refine_special_details
;
_vrf_PLAT241_1djh558             
;
PROBLEM: High      Ueq as Compared to Neighbors for .....        O21 Check 
RESPONSE: Disordered ClO4- anion. See _refine_special_details
;
_vrf_PLAT342_1djh558             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0272 Ang.  
RESPONSE: Weak diffracting crystal, large structure. See _expl_special_details
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C41 H49 Cl7 N17 O34 Pb4, 3(C H3 N O2), (Cl O4)'
_chemical_formula_sum            'C44 H58 Cl8 N20 O44 Pb4'
_chemical_formula_weight         2683.46

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'
Cl Cl 0.1484 0.1585 '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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2296(10)
_cell_length_b                   17.3147(18)
_cell_length_c                   25.755(3)
_cell_angle_alpha                102.491(4)
_cell_angle_beta                 93.675(4)
_cell_angle_gamma                104.479(4)
_cell_volume                     3860.3(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    7074
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      21.21

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_min          0.03
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2556
_exptl_absorpt_coefficient_mu    9.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
;
Crystals of complex 1 were difficult to grow and were very small 
in two dimensions. The structure of complex 1 was large and contained
solvent molecules. As a result the crystals did not diffract well and
no meaningful data could be obtained beyond theta 21.24. This dataset
was the better of two collections.
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39972
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         21.24
_reflns_number_total             8364
_reflns_number_gt                7006
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

Several of components of complex 1 showed large or elongated thermal ellipsoids
due to disorder, including several of the anions, the CH3NO2 and H2O molecules,
and the terminal pyridine rings. The ellipsoids were restrained with ISOR
restraints. The disorder was not modelled further. 
;

_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)+(0.0512P)²+132.8490P] where P=(Fo²+2Fc²)/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         8364
_refine_ls_number_parameters     1106
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1390
_refine_ls_wR_factor_gt          0.1297
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.024
_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
C1 C 0.666(3) 0.0596(14) 0.5890(10) 0.065(6) Uani 1 1 d U . .
H1A H 0.7430 0.0511 0.6130 0.078 Uiso 1 1 calc R . .
H1B H 0.7122 0.0744 0.5584 0.078 Uiso 1 1 calc R . .
C2 C 0.543(3) -0.0158(15) 0.5711(8) 0.059(7) Uani 1 1 d . . .
C3 C 0.551(2) -0.0799(14) 0.5267(8) 0.054(6) Uani 1 1 d U . .
H3 H 0.6365 -0.0733 0.5089 0.065 Uiso 1 1 calc R . .
C4 C 0.439(2) -0.1493(13) 0.5104(8) 0.051(5) Uani 1 1 d U . .
H4 H 0.4450 -0.1901 0.4812 0.061 Uiso 1 1 calc R . .
C5 C 0.312(3) -0.1597(16) 0.5382(8) 0.062(7) Uani 1 1 d . . .
H5 H 0.2315 -0.2068 0.5275 0.074 Uiso 1 1 calc R . .
C6 C 0.310(3) -0.0984(14) 0.5816(7) 0.053(6) Uani 1 1 d . . .
C7 C 0.184(2) -0.1095(12) 0.6139(7) 0.038(5) Uani 1 1 d . . .
H7 H 0.1059 -0.1579 0.6051 0.045 Uiso 1 1 calc R . .
C8 C -0.0641(19) -0.1343(12) 0.6683(7) 0.042(5) Uani 1 1 d . . .
H8A H -0.0375 -0.1822 0.6742 0.063 Uiso 1 1 calc R . .
H8B H -0.0963 -0.1424 0.6308 0.063 Uiso 1 1 calc R . .
H8C H -0.1446 -0.1254 0.6886 0.063 Uiso 1 1 calc R . .
C9 C 0.0821(18) -0.0057(11) 0.7341(6) 0.027(4) Uani 1 1 d . . .
C10 C -0.0066(17) -0.0228(10) 0.7732(6) 0.028(4) Uani 1 1 d . . .
H10 H -0.0775 -0.0731 0.7692 0.033 Uiso 1 1 calc R . .
C11 C 0.0167(19) 0.0394(11) 0.8186(6) 0.031(4) Uani 1 1 d . . .
C12 C 0.2040(19) 0.1236(11) 0.7854(6) 0.030(4) Uani 1 1 d . . .
C13 C 0.321(2) 0.2038(11) 0.7917(7) 0.042(5) Uani 1 1 d . . .
H13A H 0.3195 0.2204 0.7585 0.064 Uiso 1 1 calc R . .
H13B H 0.4185 0.1975 0.8014 0.064 Uiso 1 1 calc R . .
H13C H 0.2990 0.2449 0.8193 0.064 Uiso 1 1 calc R . .
C14 C -0.1589(19) -0.0552(10) 0.8628(7) 0.033(4) Uani 1 1 d . . .
H14A H -0.2598 -0.0646 0.8461 0.049 Uiso 1 1 calc R . .
H14B H -0.1613 -0.0584 0.8995 0.049 Uiso 1 1 calc R . .
H14C H -0.1147 -0.0962 0.8442 0.049 Uiso 1 1 calc R . .
C15 C -0.1568(18) 0.0852(10) 0.9367(6) 0.029(4) Uani 1 1 d . . .
H15 H -0.2297 0.0360 0.9341 0.035 Uiso 1 1 calc R . .
C16 C -0.1447(19) 0.1569(11) 0.9811(6) 0.032(4) Uani 1 1 d . . .
C17 C -0.2553(19) 0.1558(11) 1.0145(6) 0.035(5) Uani 1 1 d . . .
H17 H -0.3362 0.1097 1.0108 0.042 Uiso 1 1 calc R . .
C18 C -0.240(2) 0.2268(10) 1.0540(7) 0.032(4) Uani 1 1 d . . .
C19 C -0.0147(19) 0.2869(11) 1.0264(6) 0.030(4) Uani 1 1 d . . .
C20 C 0.120(2) 0.3594(10) 1.0342(6) 0.030(4) Uani 1 1 d U . .
C21 C 0.261(2) 0.3465(12) 1.0307(7) 0.042(5) Uani 1 1 d . . .
H21 H 0.2722 0.2934 1.0234 0.050 Uiso 1 1 calc R . .
C22 C 0.387(2) 0.4149(14) 1.0386(8) 0.055(6) Uani 1 1 d . . .
H22 H 0.4848 0.4093 1.0376 0.067 Uiso 1 1 calc R . .
C23 C 0.357(3) 0.4944(14) 1.0481(9) 0.070(8) Uani 1 1 d . . .
H23 H 0.4386 0.5407 1.0531 0.084 Uiso 1 1 calc R . .
C24 C 0.218(3) 0.5056(13) 1.0503(8) 0.062(7) Uani 1 1 d . . .
H24 H 0.2041 0.5579 1.0558 0.074 Uiso 1 1 calc R . .
C25 C 0.100(2) 0.4380(11) 1.0443(7) 0.042(5) Uani 1 1 d . . .
H25 H 0.0033 0.4445 1.0469 0.050 Uiso 1 1 calc R . .
C26 C -0.3553(19) 0.2373(11) 1.0901(7) 0.033(4) Uani 1 1 d . . .
H26 H -0.4495 0.1992 1.0838 0.039 Uiso 1 1 calc R . .
C27 C -0.5909(19) 0.2631(11) 1.1438(8) 0.043(5) Uani 1 1 d . . .
H27A H -0.6567 0.2941 1.1596 0.064 Uiso 1 1 calc R . .
H27B H -0.6097 0.2120 1.1545 0.064 Uiso 1 1 calc R . .
H27C H -0.6095 0.2523 1.1055 0.064 Uiso 1 1 calc R . .
C28 C -0.3927(18) 0.3634(10) 1.2107(6) 0.031(4) Uani 1 1 d . . .
C29 C -0.4947(17) 0.3694(11) 1.2483(7) 0.030(4) Uani 1 1 d . . .
H29 H -0.5933 0.3361 1.2412 0.036 Uiso 1 1 calc R . .
C30 C -0.4422(18) 0.4274(11) 1.2966(6) 0.030(4) Uani 1 1 d . . .
C31 C -0.2078(18) 0.4660(10) 1.2705(6) 0.029(4) Uani 1 1 d . . .
C32 C -0.0462(18) 0.5161(11) 1.2829(7) 0.036(5) Uani 1 1 d . . .
H32A H -0.0269 0.5462 1.3198 0.054 Uiso 1 1 calc R . .
H32B H -0.0267 0.5538 1.2602 0.054 Uiso 1 1 calc R . .
H32C H 0.0185 0.4802 1.2767 0.054 Uiso 1 1 calc R . .
C33 C -0.692(2) 0.3884(14) 1.3304(9) 0.069(7) Uani 1 1 d U . .
H33A H -0.7119 0.3428 1.2997 0.103 Uiso 1 1 calc R . .
H33B H -0.7581 0.4222 1.3261 0.103 Uiso 1 1 calc R . .
H33C H -0.7092 0.3684 1.3621 0.103 Uiso 1 1 calc R . .
C34 C -0.563(2) 0.5119(10) 1.4174(7) 0.033(4) Uani 1 1 d . . .
H34 H -0.6566 0.4746 1.4154 0.039 Uiso 1 1 calc R . .
C35 C -0.508(2) 0.5843(11) 1.4644(7) 0.035(5) Uani 1 1 d . . .
C36 C -0.5888(19) 0.5938(10) 1.5071(6) 0.026(4) Uani 1 1 d . . .
H36 H -0.6797 0.5556 1.5072 0.031 Uiso 1 1 calc R . .
C37 C -0.535(2) 0.6586(11) 1.5484(7) 0.035(5) Uani 1 1 d . . .
H37 H -0.5901 0.6667 1.5772 0.042 Uiso 1 1 calc R . .
C38 C -0.399(2) 0.7137(12) 1.5483(7) 0.040(5) Uani 1 1 d . . .
H38 H -0.3578 0.7570 1.5780 0.047 Uiso 1 1 calc R . .
C39 C -0.323(2) 0.7043(11) 1.5038(7) 0.036(5) Uani 1 1 d . . .
C40 C -0.181(2) 0.7667(12) 1.5011(8) 0.053(6) Uani 1 1 d . . .
H40A H -0.2041 0.8180 1.4999 0.064 Uiso 1 1 calc R . .
H40B H -0.1125 0.7765 1.5335 0.064 Uiso 1 1 calc R . .
C43 C 0.353(4) 0.9998(17) 0.8498(12) 0.114(11) Uani 1 1 d D . .
H43A H 0.2772 0.9715 0.8199 0.171 Uiso 1 1 calc R . .
H43B H 0.4284 1.0411 0.8395 0.171 Uiso 1 1 calc R . .
H43C H 0.3079 1.0252 0.8789 0.171 Uiso 1 1 calc R . .
C44 C 0.222(3) 0.5435(16) 1.2071(11) 0.090(8) Uani 1 1 d DU . .
H44A H 0.2086 0.5819 1.1866 0.135 Uiso 1 1 calc R . .
H44B H 0.2540 0.5719 1.2440 0.135 Uiso 1 1 calc R . .
H44C H 0.1275 0.5027 1.2045 0.135 Uiso 1 1 calc R . .
C45 C 0.925(3) 0.2200(18) 0.7282(10) 0.096(9) Uani 1 1 d U . .
H45A H 0.9813 0.2429 0.7632 0.143 Uiso 1 1 calc R . .
H45B H 0.8952 0.1611 0.7215 0.143 Uiso 1 1 calc R . .
H45C H 0.8366 0.2396 0.7265 0.143 Uiso 1 1 calc R . .
C46 C 0.653(3) 0.2058(17) 0.2873(10) 0.082(8) Uani 1 1 d . . .
H46A H 0.6477 0.2151 0.2519 0.123 Uiso 1 1 calc R . .
H46B H 0.6942 0.1602 0.2874 0.123 Uiso 1 1 calc R . .
H46C H 0.7160 0.2541 0.3119 0.123 Uiso 1 1 calc R . .
N1 N 0.4209(18) -0.0259(12) 0.5975(6) 0.048(4) Uani 1 1 d . . .
N2 N 0.1821(14) -0.0517(9) 0.6544(5) 0.032(4) Uani 1 1 d . . .
N3 N 0.0657(15) -0.0635(9) 0.6852(5) 0.033(4) Uani 1 1 d . . .
N4 N 0.1901(16) 0.0650(10) 0.7407(5) 0.035(4) Uani 1 1 d . . .
N5 N 0.1147(14) 0.1137(8) 0.8249(5) 0.026(3) Uani 1 1 d . . .
N6 N -0.0691(15) 0.0261(8) 0.8608(6) 0.038(4) Uani 1 1 d . . .
N7 N -0.0645(14) 0.0920(8) 0.9017(5) 0.026(3) Uani 1 1 d . . .
N8 N -0.0271(14) 0.2214(9) 0.9866(5) 0.026(3) Uani 1 1 d . . .
N9 N -0.1187(16) 0.2923(8) 1.0599(5) 0.031(4) Uani 1 1 d . . .
N10 N -0.3236(15) 0.2995(9) 1.1303(5) 0.034(4) Uani 1 1 d . . .
N11 N -0.4367(15) 0.3093(9) 1.1616(5) 0.035(4) Uani 1 1 d . . .
N12 N -0.2500(14) 0.4108(8) 1.2218(5) 0.027(3) Uani 1 1 d U . .
N13 N -0.2987(15) 0.4746(8) 1.3072(5) 0.029(3) Uani 1 1 d . . .
N14 N -0.5357(15) 0.4369(9) 1.3355(6) 0.037(4) Uani 1 1 d . . .
N15 N -0.4780(15) 0.5017(9) 1.3792(5) 0.035(4) Uani 1 1 d . . .
N16 N -0.3764(16) 0.6385(8) 1.4624(6) 0.032(4) Uani 1 1 d . . .
N17 N 0.421(3) 0.9435(15) 0.8661(10) 0.088(7) Uani 1 1 d DU . .
N18 N 0.330(2) 0.5053(14) 1.1872(9) 0.082(7) Uani 1 1 d D . .
N19 N 1.015(2) 0.2438(11) 0.6894(7) 0.054(4) Uani 1 1 d U . .
N20 N 0.496(3) 0.1870(17) 0.3039(9) 0.089(8) Uani 1 1 d . . .
O1 O 0.6079(14) 0.1226(11) 0.6155(5) 0.071(5) Uani 1 1 d . . .
H1 H 0.6619 0.1672 0.6137 0.085 Uiso 1 1 calc R . .
O2 O -0.1107(13) 0.7432(8) 1.4575(5) 0.043(3) Uani 1 1 d . . .
O3 O -0.1051(16) 0.2273(9) 0.8527(5) 0.051(4) Uani 1 1 d D . .
O4 O -0.1079(18) 0.5594(9) 1.4291(6) 0.069(5) Uani 1 1 d D . .
O5 O 0.503(3) 0.9687(17) 0.9140(11) 0.148(9) Uani 1 1 d . . .
O6 O 0.441(2) 0.8845(11) 0.8381(8) 0.097(6) Uani 1 1 d . . .
O7 O 0.278(2) 0.4402(19) 1.1781(13) 0.176(15) Uani 1 1 d . . .
O8 O 0.455(4) 0.565(2) 1.1845(13) 0.205(13) Uani 1 1 d U . .
O9 O 1.1441(18) 0.2801(13) 0.7002(8) 0.106(7) Uani 1 1 d . . .
O10 O 0.9402(18) 0.2475(10) 0.6467(6) 0.074(5) Uani 1 1 d . . .
O11 O 0.1916(12) 0.0562(9) 0.5651(5) 0.049(4) Uani 1 1 d . . .
O12 O -0.0203(15) 0.1035(8) 0.5472(6) 0.057(4) Uani 1 1 d . . .
O13 O -0.0569(14) -0.0259(7) 0.5669(5) 0.048(3) Uani 1 1 d . . .
O14 O 0.0557(15) 0.0929(8) 0.6363(5) 0.053(4) Uani 1 1 d . . .
O21 O 0.580(3) 0.1093(18) 0.7349(12) 0.167(10) Uani 1 1 d U . .
O22 O 0.677(2) 0.0597(13) 0.8008(9) 0.114(7) Uani 1 1 d U . .
O23 O 0.728(2) 0.0199(12) 0.7078(8) 0.106(6) Uani 1 1 d U . .
O24 O 0.472(3) -0.0085(15) 0.7276(9) 0.128(7) Uani 1 1 d U . .
O31 O 0.2628(15) 0.1367(10) 0.9480(7) 0.078(5) Uani 1 1 d . . .
O32 O 0.371(2) 0.0767(15) 1.0101(12) 0.166(13) Uani 1 1 d . . .
O33 O 0.1403(17) 0.0128(9) 0.9659(7) 0.075(5) Uani 1 1 d . . .
O34 O 0.162(3) 0.1313(12) 1.0309(7) 0.141(10) Uani 1 1 d . . .
O41 O 0.4555(14) 0.2931(8) 0.9180(5) 0.053(4) Uani 1 1 d . . .
O42 O 0.682(2) 0.3075(9) 0.9684(7) 0.093(6) Uani 1 1 d . . .
O43 O 0.5737(15) 0.1841(7) 0.9058(6) 0.056(4) Uani 1 1 d . . .
O44 O 0.6713(18) 0.3068(10) 0.8766(7) 0.083(5) Uani 1 1 d . . .
O51 O -0.2239(15) 0.4790(9) 1.1092(6) 0.062(4) Uani 1 1 d . . .
O52 O -0.076(2) 0.6001(10) 1.0843(6) 0.081(5) Uani 1 1 d . . .
O53 O -0.225(2) 0.6191(12) 1.1515(8) 0.104(6) Uani 1 1 d U . .
O54 O -0.024(3) 0.5751(10) 1.1660(7) 0.112(8) Uani 1 1 d . . .
O61 O -0.005(2) 0.2539(10) 1.1574(7) 0.083(5) Uani 1 1 d U . .
O62 O -0.009(2) 0.3251(11) 1.2405(7) 0.093(5) Uani 1 1 d U . .
O63 O 0.1470(13) 0.2358(8) 1.2254(5) 0.043(3) Uani 1 1 d . . .
O64 O -0.1048(19) 0.1822(13) 1.2166(13) 0.154(11) Uani 1 1 d . . .
O71 O 0.484(2) 0.6139(10) 0.3156(8) 0.092(6) Uani 1 1 d U . .
O72 O 0.585(2) 0.7428(11) 0.3781(6) 0.083(5) Uani 1 1 d . . .
O73 O 0.333(3) 0.6798(17) 0.3681(11) 0.160(10) Uani 1 1 d U . .
O74 O 0.4239(18) 0.7335(9) 0.2996(6) 0.072(5) Uani 1 1 d . . .
O81 O 0.095(2) 0.4415(11) 0.4368(9) 0.129(9) Uani 1 1 d . . .
O82 O 0.027(2) 0.3050(11) 0.3973(9) 0.116(8) Uani 1 1 d . . .
O83 O -0.0798(16) 0.3558(11) 0.4732(6) 0.080(5) Uani 1 1 d . . .
O84 O -0.140(2) 0.3865(13) 0.3950(8) 0.102(6) Uani 1 1 d . . .
O110 O 0.401(3) 0.1868(17) 0.2719(12) 0.154(9) Uani 1 1 d U . .
O120 O 0.497(2) 0.1830(14) 0.3477(8) 0.112(7) Uani 1 1 d U . .
Cl1 Cl 0.0403(5) 0.0546(3) 0.5784(2) 0.0475(13) Uani 1 1 d . . .
Cl2 Cl 0.6230(7) 0.0341(4) 0.7447(2) 0.0717(17) Uani 1 1 d . . .
Cl3 Cl 0.2417(7) 0.0899(3) 0.9884(2) 0.0678(17) Uani 1 1 d . . .
Cl4 Cl 0.5923(6) 0.2700(3) 0.9213(2) 0.0590(15) Uani 1 1 d . . .
Cl5 Cl -0.1409(6) 0.5699(3) 1.1268(2) 0.0531(14) Uani 1 1 d . . .
Cl6 Cl 0.0077(5) 0.2492(3) 1.2098(2) 0.0540(14) Uani 1 1 d . . .
Cl7 Cl 0.4506(7) 0.6899(5) 0.3394(3) 0.082(2) Uani 1 1 d . . .
Cl8 Cl -0.0226(5) 0.3697(3) 0.4245(2) 0.0431(12) Uani 1 1 d . . .
Pb1 Pb 0.36423(8) 0.09027(5) 0.66145(3) 0.0416(2) Uani 1 1 d . . .
Pb2 Pb 0.13197(7) 0.22735(4) 0.90749(3) 0.0324(2) Uani 1 1 d . . .
Pb3 Pb -0.06719(7) 0.39780(4) 1.15202(2) 0.0263(2) Uani 1 1 d . . .
Pb4 Pb -0.25242(8) 0.62348(4) 1.37862(3) 0.0345(2) Uani 1 1 d . . .
H2 H -0.067(19) 0.788(11) 1.441(7) 0.041 Uiso 1 1 d . . .
H3A H -0.156(18) 0.266(8) 0.855(7) 0.052 Uiso 1 1 d D . .
H3B H -0.14(2) 0.1721(18) 0.842(7) 0.052 Uiso 1 1 d D . .
H4A H -0.09(2) 0.512(6) 1.414(7) 0.052 Uiso 1 1 d D . .
H4B H -0.04(2) 0.577(12) 1.455(8) 0.052 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.40(3) . ?
C1 C2 1.46(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.35(2) . ?
C2 C3 1.43(3) . ?
C3 C4 1.34(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.41(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(3) . ?
C5 H5 0.9300 . ?
C6 N1 1.37(3) . ?
C6 C7 1.47(3) . ?
C7 N2 1.28(2) . ?
C7 H7 0.9300 . ?
C8 N3 1.45(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.34(2) . ?
C9 C10 1.37(2) . ?
C9 N3 1.40(2) . ?
C10 C11 1.37(2) . ?
C10 H10 0.9300 . ?
C11 N5 1.35(2) . ?
C11 N6 1.41(2) . ?
C12 N4 1.33(2) . ?
C12 N5 1.36(2) . ?
C12 C13 1.50(2) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N6 1.46(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N7 1.28(2) . ?
C15 C16 1.47(2) . ?
C15 H15 0.9300 . ?
C16 N8 1.32(2) . ?
C16 C17 1.38(2) . ?
C17 C18 1.39(2) . ?
C17 H17 0.9300 . ?
C18 N9 1.35(2) . ?
C18 C26 1.48(2) . ?
C19 N8 1.33(2) . ?
C19 N9 1.34(2) . ?
C19 C20 1.50(2) . ?
C20 C21 1.38(3) . ?
C20 C25 1.39(2) . ?
C21 C22 1.41(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.45(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.34(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.36(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 N10 1.28(2) . ?
C26 H26 0.9300 . ?
C27 N11 1.44(2) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N12 1.34(2) . ?
C28 N11 1.37(2) . ?
C28 C29 1.40(2) . ?
C29 C30 1.39(2) . ?
C29 H29 0.9300 . ?
C30 N13 1.35(2) . ?
C30 N14 1.37(2) . ?
C31 N13 1.31(2) . ?
C31 N12 1.37(2) . ?
C31 C32 1.50(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N14 1.46(2) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N15 1.31(2) . ?
C34 C35 1.50(2) . ?
C34 H34 0.9300 . ?
C35 N16 1.35(2) . ?
C35 C36 1.37(2) . ?
C36 C37 1.33(2) . ?
C36 H36 0.9300 . ?
C37 C38 1.38(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.38(2) . ?
C38 H38 0.9300 . ?
C39 N16 1.34(2) . ?
C39 C40 1.49(3) . ?
C40 O2 1.37(2) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C43 N17 1.400(2) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 N18 1.399(2) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 N19 1.40(3) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 N20 1.51(3) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
N1 Pb1 2.497(17) . ?
N2 N3 1.376(18) . ?
N2 Pb1 2.570(14) . ?
N4 Pb1 2.720(13) . ?
N5 Pb2 2.532(13) . ?
N6 N7 1.364(18) . ?
N7 Pb2 2.548(13) . ?
N8 Pb2 2.591(12) . ?
N9 Pb3 2.596(13) . ?
N10 N11 1.380(18) . ?
N10 Pb3 2.493(13) . ?
N12 Pb3 2.556(13) . ?
N13 Pb4 2.740(13) . ?
N14 N15 1.374(19) . ?
N15 Pb4 2.569(14) . ?
N16 Pb4 2.501(13) . ?
N17 O6 1.18(2) . ?
N17 O5 1.33(3) . ?
N18 O7 1.08(3) . ?
N18 O8 1.36(3) . ?
N19 O9 1.19(2) . ?
N19 O10 1.28(2) . ?
N20 O120 1.14(2) . ?
N20 O110 1.16(3) . ?
O1 Pb1 2.602(12) . ?
O1 H1 0.8200 . ?
O2 Pb4 2.572(12) . ?
O2 H2 0.98(18) . ?
O3 Pb2 2.526(13) . ?
O3 H3A 0.90(2) . ?
O3 H3B 0.90(2) . ?
O4 Pb4 2.417(14) . ?
O4 H4A 0.90(2) . ?
O4 H4B 0.9(2) . ?
O11 Cl1 1.454(12) . ?
O11 Pb1 2.727(12) . ?
O12 Cl1 1.464(13) . ?
O13 Cl1 1.413(12) . ?
O14 Cl1 1.478(13) . ?
O21 Cl2 1.52(3) . ?
O21 Pb1 2.56(3) . ?
O22 Cl2 1.43(2) . ?
O23 Cl2 1.43(2) . ?
O24 Cl2 1.40(2) . ?
O31 Cl3 1.446(14) . ?
O31 Pb2 2.550(13) . ?
O32 Cl3 1.378(19) . ?
O33 Cl3 1.402(15) . ?
O34 Cl3 1.51(2) . ?
O41 Cl4 1.419(13) . ?
O42 Cl4 1.356(16) . ?
O43 Cl4 1.416(13) . ?
O44 Cl4 1.568(15) . ?
O51 Cl5 1.521(15) . ?
O51 Pb3 2.602(13) . ?
O52 Cl5 1.417(15) . ?
O53 Cl5 1.38(2) . ?
O54 Cl5 1.403(17) . ?
O61 Cl6 1.369(17) . ?
O61 Pb3 2.722(17) . ?
O62 Cl6 1.429(19) . ?
O63 Cl6 1.411(12) . ?
O64 Cl6 1.401(17) . ?
O71 Cl7 1.444(19) . ?
O72 Cl7 1.500(18) . ?
O73 Cl7 1.35(3) . ?
O74 Cl7 1.438(14) . ?
O81 Cl8 1.390(16) . ?
O82 Cl8 1.385(17) . ?
O83 Cl8 1.436(15) . ?
O84 Cl8 1.407(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
O1 C1 C2 108.5(18) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C3 119(2) . . ?
N1 C2 C1 120(2) . . ?
C3 C2 C1 121(2) . . ?
C4 C3 C2 121(2) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 118(2) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C5 C6 N1 123(2) . . ?
C5 C6 C7 120(2) . . ?
N1 C6 C7 117.0(17) . . ?
N2 C7 C6 119.3(18) . . ?
N2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 122.6(15) . . ?
N4 C9 N3 116.6(14) . . ?
C10 C9 N3 120.8(15) . . ?
C11 C10 C9 115.4(15) . . ?
C11 C10 H10 122.3 . . ?
C9 C10 H10 122.3 . . ?
N5 C11 C10 123.7(14) . . ?
N5 C11 N6 117.6(14) . . ?
C10 C11 N6 118.7(15) . . ?
N4 C12 N5 122.5(15) . . ?
N4 C12 C13 118.5(14) . . ?
N5 C12 C13 118.9(15) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 118.5(15) . . ?
N7 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
N8 C16 C17 122.3(15) . . ?
N8 C16 C15 117.8(14) . . ?
C17 C16 C15 119.8(16) . . ?
C16 C17 C18 116.8(16) . . ?
C16 C17 H17 121.6 . . ?
C18 C17 H17 121.6 . . ?
N9 C18 C17 120.6(15) . . ?
N9 C18 C26 116.3(15) . . ?
C17 C18 C26 123.0(16) . . ?
N8 C19 N9 123.2(15) . . ?
N8 C19 C20 119.3(14) . . ?
N9 C19 C20 117.4(15) . . ?
C21 C20 C25 121.7(17) . . ?
C21 C20 C19 119.1(16) . . ?
C25 C20 C19 119.2(17) . . ?
C20 C21 C22 118.8(19) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C21 C22 C23 116(2) . . ?
C21 C22 H22 121.9 . . ?
C23 C22 H22 121.9 . . ?
C24 C23 C22 124(2) . . ?
C24 C23 H23 118.0 . . ?
C22 C23 H23 118.0 . . ?
C23 C24 C25 118(2) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C24 C25 C20 121.3(19) . . ?
C24 C25 H25 119.4 . . ?
C20 C25 H25 119.4 . . ?
N10 C26 C18 119.0(15) . . ?
N10 C26 H26 120.5 . . ?
C18 C26 H26 120.5 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N12 C28 N11 118.6(14) . . ?
N12 C28 C29 120.8(14) . . ?
N11 C28 C29 120.6(15) . . ?
C30 C29 C28 117.1(15) . . ?
C30 C29 H29 121.5 . . ?
C28 C29 H29 121.5 . . ?
N13 C30 N14 118.1(14) . . ?
N13 C30 C29 121.4(14) . . ?
N14 C30 C29 120.4(15) . . ?
N13 C31 N12 123.6(15) . . ?
N13 C31 C32 119.0(14) . . ?
N12 C31 C32 117.3(14) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N14 C33 H33A 109.5 . . ?
N14 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N14 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N15 C34 C35 119.0(16) . . ?
N15 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
N16 C35 C36 122.5(16) . . ?
N16 C35 C34 116.8(15) . . ?
C36 C35 C34 120.7(17) . . ?
C37 C36 C35 119.0(17) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C36 C37 C38 119.9(16) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C37 C38 C39 119.6(17) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
N16 C39 C38 120.3(17) . . ?
N16 C39 C40 119.1(15) . . ?
C38 C39 C40 120.6(17) . . ?
O2 C40 C39 113.1(15) . . ?
O2 C40 H40A 109.0 . . ?
C39 C40 H40A 109.0 . . ?
O2 C40 H40B 109.0 . . ?
C39 C40 H40B 109.0 . . ?
H40A C40 H40B 107.8 . . ?
N17 C43 H43A 109.5 . . ?
N17 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N17 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N18 C44 H44A 109.5 . . ?
N18 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N18 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N19 C45 H45A 109.5 . . ?
N19 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N19 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N20 C46 H46A 109.5 . . ?
N20 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N20 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C2 N1 C6 118.6(19) . . ?
C2 N1 Pb1 122.6(16) . . ?
C6 N1 Pb1 117.7(11) . . ?
C7 N2 N3 118.9(15) . . ?
C7 N2 Pb1 117.2(11) . . ?
N3 N2 Pb1 122.6(10) . . ?
N2 N3 C9 116.9(14) . . ?
N2 N3 C8 120.9(13) . . ?
C9 N3 C8 122.2(13) . . ?
C12 N4 C9 118.6(14) . . ?
C12 N4 Pb1 121.3(11) . . ?
C9 N4 Pb1 120.0(11) . . ?
C11 N5 C12 116.7(13) . . ?
C11 N5 Pb2 120.7(10) . . ?
C12 N5 Pb2 122.6(10) . . ?
N7 N6 C11 118.3(13) . . ?
N7 N6 C14 119.2(13) . . ?
C11 N6 C14 122.5(14) . . ?
C15 N7 N6 120.3(14) . . ?
C15 N7 Pb2 121.0(11) . . ?
N6 N7 Pb2 118.7(9) . . ?
C16 N8 C19 118.6(13) . . ?
C16 N8 Pb2 117.8(10) . . ?
C19 N8 Pb2 122.1(11) . . ?
C19 N9 C18 118.4(14) . . ?
C19 N9 Pb3 123.6(11) . . ?
C18 N9 Pb3 115.2(10) . . ?
C26 N10 N11 117.2(14) . . ?
C26 N10 Pb3 121.4(11) . . ?
N11 N10 Pb3 121.3(9) . . ?
C28 N11 N10 116.2(13) . . ?
C28 N11 C27 122.4(14) . . ?
N10 N11 C27 121.3(13) . . ?
C28 N12 C31 118.3(13) . . ?
C28 N12 Pb3 119.7(10) . . ?
C31 N12 Pb3 122.0(10) . . ?
C31 N13 C30 118.8(14) . . ?
C31 N13 Pb4 119.6(11) . . ?
C30 N13 Pb4 115.6(10) . . ?
C30 N14 N15 115.7(13) . . ?
C30 N14 C33 124.3(14) . . ?
N15 N14 C33 119.8(13) . . ?
C34 N15 N14 117.3(14) . . ?
C34 N15 Pb4 117.2(11) . . ?
N14 N15 Pb4 123.2(10) . . ?
C39 N16 C35 118.6(14) . . ?
C39 N16 Pb4 121.4(11) . . ?
C35 N16 Pb4 119.7(11) . . ?
O6 N17 O5 115(2) . . ?
O6 N17 C43 126(3) . . ?
O5 N17 C43 117(3) . . ?
O7 N18 O8 146(3) . . ?
O7 N18 C44 106(2) . . ?
O8 N18 C44 108(3) . . ?
O9 N19 O10 119.9(19) . . ?
O9 N19 C45 122(2) . . ?
O10 N19 C45 114(2) . . ?
O120 N20 O110 133(3) . . ?
O120 N20 C46 112(2) . . ?
O110 N20 C46 115(2) . . ?
C1 O1 Pb1 121.2(14) . . ?
C1 O1 H1 109.5 . . ?
Pb1 O1 H1 129.3 . . ?
C40 O2 Pb4 120.5(11) . . ?
C40 O2 H2 114(10) . . ?
Pb4 O2 H2 105(10) . . ?
Pb2 O3 H3A 130(10) . . ?
Pb2 O3 H3B 93(10) . . ?
H3A O3 H3B 132(10) . . ?
Pb4 O4 H4A 122(10) . . ?
Pb4 O4 H4B 135(10) . . ?
H4A O4 H4B 97(10) . . ?
Cl1 O11 Pb1 104.8(6) . . ?
Cl2 O21 Pb1 119.0(16) . . ?
Cl3 O31 Pb2 138.4(9) . . ?
Cl5 O51 Pb3 108.2(7) . . ?
Cl6 O61 Pb3 109.2(9) . . ?
O13 Cl1 O11 112.7(8) . . ?
O13 Cl1 O12 109.5(8) . . ?
O11 Cl1 O12 107.7(8) . . ?
O13 Cl1 O14 110.0(8) . . ?
O11 Cl1 O14 106.7(8) . . ?
O12 Cl1 O14 110.3(9) . . ?
O24 Cl2 O23 116.5(13) . . ?
O24 Cl2 O22 119.9(14) . . ?
O23 Cl2 O22 118.2(13) . . ?
O24 Cl2 O21 86.3(15) . . ?
O23 Cl2 O21 104.8(14) . . ?
O22 Cl2 O21 101.7(15) . . ?
O32 Cl3 O33 107.5(12) . . ?
O32 Cl3 O31 115.0(12) . . ?
O33 Cl3 O31 109.0(10) . . ?
O32 Cl3 O34 112.0(17) . . ?
O33 Cl3 O34 104.7(13) . . ?
O31 Cl3 O34 108.2(11) . . ?
O42 Cl4 O43 113.9(9) . . ?
O42 Cl4 O41 113.1(10) . . ?
O43 Cl4 O41 114.1(9) . . ?
O42 Cl4 O44 107.3(11) . . ?
O43 Cl4 O44 106.3(9) . . ?
O41 Cl4 O44 100.8(9) . . ?
O53 Cl5 O54 105.7(13) . . ?
O53 Cl5 O52 110.9(11) . . ?
O54 Cl5 O52 108.2(13) . . ?
O53 Cl5 O51 114.5(11) . . ?
O54 Cl5 O51 105.0(9) . . ?
O52 Cl5 O51 112.0(10) . . ?
O61 Cl6 O64 109.8(15) . . ?
O61 Cl6 O63 111.4(10) . . ?
O64 Cl6 O63 106.5(10) . . ?
O61 Cl6 O62 105.9(11) . . ?
O64 Cl6 O62 111.3(14) . . ?
O63 Cl6 O62 112.0(10) . . ?
O73 Cl7 O74 109.4(14) . . ?
O73 Cl7 O71 113.4(15) . . ?
O74 Cl7 O71 111.6(11) . . ?
O73 Cl7 O72 106.2(15) . . ?
O74 Cl7 O72 108.3(10) . . ?
O71 Cl7 O72 107.6(10) . . ?
O82 Cl8 O81 109.7(11) . . ?
O82 Cl8 O84 114.0(14) . . ?
O81 Cl8 O84 105.9(14) . . ?
O82 Cl8 O83 112.6(11) . . ?
O81 Cl8 O83 108.8(12) . . ?
O84 Cl8 O83 105.4(11) . . ?
N1 Pb1 O21 96.2(8) . . ?
N1 Pb1 N2 65.0(5) . . ?
O21 Pb1 N2 106.7(7) . . ?
N1 Pb1 O1 62.3(6) . . ?
O21 Pb1 O1 75.2(7) . . ?
N2 Pb1 O1 127.1(5) . . ?
N1 Pb1 N4 121.8(5) . . ?
O21 Pb1 N4 83.1(7) . . ?
N2 Pb1 N4 59.9(5) . . ?
O1 Pb1 N4 158.4(4) . . ?
N1 Pb1 O11 69.9(4) . . ?
O21 Pb1 O11 163.6(7) . . ?
N2 Pb1 O11 75.8(4) . . ?
O1 Pb1 O11 90.3(4) . . ?
N4 Pb1 O11 111.2(4) . . ?
O3 Pb2 N5 77.7(4) . . ?
O3 Pb2 N7 71.9(4) . . ?
N5 Pb2 N7 63.8(4) . . ?
O3 Pb2 O31 143.8(5) . . ?
N5 Pb2 O31 80.2(5) . . ?
N7 Pb2 O31 72.6(4) . . ?
O3 Pb2 N8 86.5(4) . . ?
N5 Pb2 N8 127.4(4) . . ?
N7 Pb2 N8 63.5(4) . . ?
O31 Pb2 N8 84.6(4) . . ?
N10 Pb3 N12 62.7(4) . . ?
N10 Pb3 N9 64.3(4) . . ?
N12 Pb3 N9 127.0(4) . . ?
N10 Pb3 O51 77.4(5) . . ?
N12 Pb3 O51 81.3(4) . . ?
N9 Pb3 O51 87.7(5) . . ?
N10 Pb3 O61 78.4(5) . . ?
N12 Pb3 O61 102.0(5) . . ?
N9 Pb3 O61 66.8(5) . . ?
O51 Pb3 O61 150.6(5) . . ?
O4 Pb4 N16 81.1(5) . . ?
O4 Pb4 N15 85.6(5) . . ?
N16 Pb4 N15 65.5(5) . . ?
O4 Pb4 O2 77.2(5) . . ?
N16 Pb4 O2 64.0(5) . . ?
N15 Pb4 O2 128.4(4) . . ?
O4 Pb4 N13 80.3(4) . . ?
N16 Pb4 N13 122.0(4) . . ?
N15 Pb4 N13 58.7(4) . . ?
O2 Pb4 N13 155.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        21.24
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         2.569
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.214
_database_code_depnum_ccdc_archive 'CCDC 976900'
#######################################################################
#
#                 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_2(djh840)

# start Validation Reply Form
_vrf_DIFMX01_2djh840             
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: Insufficient absorption correction due to strongly absorbing crystal.
See _exptl_special_details
;
_vrf_PLAT234_2djh840             
;
PROBLEM: Large Hirshfeld Difference F131   --  C93     ..       0.32 Ang.  
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT780_2djh840             
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do ! 
RESPONSE: The atoms of each L1 ligands are connected to each other and the donor
atoms are connected to the eight Pb atoms. All sixteen of the SO3CF3- anions are
connected to the Pb atoms. The two L1 atoms are connected through bridging SO3CF3-
anions
;
_vrf_PLAT094_2djh840             
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.34 Why ? 
RESPONSE: Strongly absorbing crystal. See _exptl_special_details
;
_vrf_PLAT097_2djh840             
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      14.63 eA-3  
RESPONSE: Insufficient absorption correction due to strongly absorbing crystal.
See _exptl_special_details
;
_vrf_PLAT112_2djh840             
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem...          I Check 
RESPONSE: ...
;
_vrf_PLAT213_2djh840             
;
PROBLEM: Atom O153            has ADP max/min Ratio .....        4.7 prolat
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT220_2djh840             
;
PROBLEM: Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        7.6 Ratio 
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT230_2djh840             
;
PROBLEM: Hirshfeld Test Diff for    S13    --  O131    ..        7.4 su    
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT232_2djh840             
;
PROBLEM: Hirshfeld Test Diff (M-X)  Pb6    --  O151    ..       11.3 su    
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT241_2djh840             
;
PROBLEM: High      Ueq as Compared to Neighbors for .....        O92 Check 
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT242_2djh840             
;
PROBLEM: Low       Ueq as Compared to Neighbors for .....        S15 Check 
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT306_2djh840             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check 
RESPONSE: The H atoms of O5 could not be located as there was no residual
electron density within 1.2 A of O5
;
_vrf_PLAT342_2djh840             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0228 Ang.  
RESPONSE: Large structure
;
_vrf_PLAT415_2djh840             
;
PROBLEM: Short Inter D-H..H-X       H4A    ..  H10D    ..       2.04 Ang.  
RESPONSE: H4A on one of the hydroxymethyl arms is orientated towards H10D on one
of the methyl groups of a symmetry related ligand. 
;
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C102 H93 F48 N35 O52 Pb8 S16, 4(C2 H3 N), O'
_chemical_formula_sum            'C110 H105 F48 N39 O53 Pb8 S16'
_chemical_formula_weight         5904.00

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'
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'
S S 0.1246 0.1234 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   18.0882(18)
_cell_length_b                   19.955(3)
_cell_length_c                   26.553(3)
_cell_angle_alpha                70.191(5)
_cell_angle_beta                 87.643(5)
_cell_angle_gamma                87.432(5)
_cell_volume                     9004.7(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9784
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      31.65

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.15
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_max          0.47
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5612
_exptl_absorpt_coefficient_mu    7.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_T_max  0.312
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
;
The crystal was a large plate and strongly absorbed X-rays.  The standard 
multi-scan absorption correction left residual electron density in close
proximity to the Pb atoms.  Further attempts to improve the 
multi-scan absorption correction did not yeild better results.
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            93775
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         0.82
_diffrn_reflns_theta_max         25.50
_reflns_number_total             33396
_reflns_number_gt                25009
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

Several of components of complex 2 showed large or elongated thermal ellipsoids
due to disorder, including several of the SO3CF3- anions. The ellipsoids were 
restrained with ISOR restraints. The disorder was not modelled further. 
;

_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)+(0.0350P)²+433.6655P] where P=(Fo²+2Fc²)/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         33396
_refine_ls_number_parameters     2486
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.1804
_refine_ls_wR_factor_gt          0.1694
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001

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
C1 C 0.5432(9) 0.5887(8) 0.1204(7) 0.029(4) Uani 1 1 d . . .
H1A H 0.5243 0.6017 0.1507 0.035 Uiso 1 1 calc R . .
H1B H 0.5353 0.6294 0.0882 0.035 Uiso 1 1 calc R . .
C2 C 0.6245(9) 0.5717(8) 0.1263(6) 0.023(3) Uani 1 1 d . . .
C3 C 0.6723(10) 0.6258(8) 0.1230(6) 0.028(4) Uani 1 1 d . . .
H3 H 0.6540 0.6720 0.1172 0.033 Uiso 1 1 calc R . .
C4 C 0.7465(10) 0.6102(8) 0.1285(6) 0.028(4) Uani 1 1 d . . .
H4 H 0.7793 0.6460 0.1256 0.034 Uiso 1 1 calc R . .
C5 C 0.7722(9) 0.5410(8) 0.1385(6) 0.027(4) Uani 1 1 d . . .
H5 H 0.8225 0.5294 0.1425 0.032 Uiso 1 1 calc R . .
C6 C 0.7217(9) 0.4883(8) 0.1424(5) 0.020(3) Uani 1 1 d . . .
C7 C 0.7495(9) 0.4135(7) 0.1537(6) 0.021(3) Uani 1 1 d . . .
H7 H 0.8000 0.4020 0.1558 0.025 Uiso 1 1 calc R . .
C8 C 0.8055(9) 0.2799(8) 0.1635(7) 0.030(4) Uani 1 1 d . . .
H8A H 0.8324 0.2797 0.1940 0.046 Uiso 1 1 calc R . .
H8B H 0.8244 0.3157 0.1320 0.046 Uiso 1 1 calc R . .
H8C H 0.8112 0.2340 0.1593 0.046 Uiso 1 1 calc R . .
C9 C 0.6752(8) 0.2442(8) 0.1887(6) 0.021(3) Uani 1 1 d . . .
C10 C 0.6936(9) 0.1723(8) 0.2030(6) 0.022(3) Uani 1 1 d . . .
H10 H 0.7424 0.1564 0.2011 0.027 Uiso 1 1 calc R . .
C11 C 0.6374(9) 0.1256(8) 0.2200(6) 0.022(3) Uani 1 1 d . . .
C12 C 0.5536(8) 0.2173(7) 0.2121(6) 0.017(3) Uani 1 1 d . . .
C13 C 0.4761(8) 0.2449(8) 0.2171(7) 0.025(3) Uani 1 1 d . . .
H13A H 0.4557 0.2652 0.1822 0.037 Uiso 1 1 calc R . .
H13B H 0.4768 0.2807 0.2337 0.037 Uiso 1 1 calc R . .
H13C H 0.4463 0.2064 0.2386 0.037 Uiso 1 1 calc R . .
C14 C 0.7229(8) 0.0219(7) 0.2210(6) 0.019(3) Uani 1 1 d . . .
H14A H 0.7523 0.0062 0.2524 0.029 Uiso 1 1 calc R . .
H14B H 0.7486 0.0577 0.1929 0.029 Uiso 1 1 calc R . .
H14C H 0.7145 -0.0178 0.2095 0.029 Uiso 1 1 calc R . .
C15 C 0.6092(9) -0.0590(7) 0.2776(6) 0.024(4) Uani 1 1 d . . .
H15 H 0.6574 -0.0768 0.2764 0.028 Uiso 1 1 calc R . .
C16 C 0.5498(8) -0.1074(7) 0.3015(6) 0.020(3) Uani 1 1 d . . .
C17 C 0.5675(9) -0.1791(7) 0.3276(6) 0.023(3) Uani 1 1 d . . .
H17 H 0.6164 -0.1961 0.3312 0.028 Uiso 1 1 calc R . .
C18 C 0.5096(9) -0.2241(7) 0.3478(6) 0.021(3) Uani 1 1 d . . .
C19 C 0.4257(9) -0.1293(7) 0.3195(6) 0.020(3) Uani 1 1 d . . .
C20 C 0.3471(8) -0.1030(7) 0.3164(6) 0.022(3) Uani 1 1 d . . .
C21 C 0.2972(9) -0.1298(8) 0.3592(7) 0.027(4) Uani 1 1 d . . .
H21 H 0.3127 -0.1653 0.3902 0.032 Uiso 1 1 calc R . .
C22 C 0.2241(10) -0.1039(9) 0.3559(8) 0.038(4) Uani 1 1 d . . .
H22 H 0.1910 -0.1210 0.3847 0.046 Uiso 1 1 calc R . .
C23 C 0.2016(9) -0.0520(8) 0.3088(8) 0.037(5) Uani 1 1 d . . .
H23 H 0.1529 -0.0344 0.3061 0.045 Uiso 1 1 calc R . .
C24 C 0.2507(9) -0.0259(8) 0.2656(8) 0.034(4) Uani 1 1 d . . .
H24 H 0.2344 0.0085 0.2343 0.041 Uiso 1 1 calc R . .
C25 C 0.3234(8) -0.0504(8) 0.2688(7) 0.023(3) Uani 1 1 d . . .
H25 H 0.3564 -0.0326 0.2399 0.028 Uiso 1 1 calc R . .
C26 C 0.5262(9) -0.3013(7) 0.3740(6) 0.023(3) Uani 1 1 d . . .
H26 H 0.5738 -0.3174 0.3850 0.028 Uiso 1 1 calc R . .
C27 C 0.5648(9) -0.4378(8) 0.4262(7) 0.032(4) Uani 1 1 d . . .
H27A H 0.6011 -0.4306 0.3976 0.048 Uiso 1 1 calc R . .
H27B H 0.5650 -0.4874 0.4478 0.048 Uiso 1 1 calc R . .
H27C H 0.5763 -0.4099 0.4478 0.048 Uiso 1 1 calc R . .
C28 C 0.4367(8) -0.4632(7) 0.4057(6) 0.019(3) Uani 1 1 d . . .
C29 C 0.4514(8) -0.5363(8) 0.4271(6) 0.023(3) Uani 1 1 d . . .
H29 H 0.4976 -0.5551 0.4401 0.028 Uiso 1 1 calc R . .
C30 C 0.3922(8) -0.5798(7) 0.4277(6) 0.018(3) Uani 1 1 d . . .
C31 C 0.3171(8) -0.4818(8) 0.3906(6) 0.021(3) Uani 1 1 d . . .
C32 C 0.2413(9) -0.4514(9) 0.3720(7) 0.032(4) Uani 1 1 d . . .
H32A H 0.2156 -0.4380 0.3997 0.048 Uiso 1 1 calc R . .
H32B H 0.2139 -0.4866 0.3642 0.048 Uiso 1 1 calc R . .
H32C H 0.2460 -0.4102 0.3403 0.048 Uiso 1 1 calc R . .
C33 C 0.4780(9) -0.6871(9) 0.4516(8) 0.034(4) Uani 1 1 d . . .
H33A H 0.4898 -0.7044 0.4888 0.052 Uiso 1 1 calc R . .
H33B H 0.5136 -0.6530 0.4319 0.052 Uiso 1 1 calc R . .
H33C H 0.4792 -0.7262 0.4382 0.052 Uiso 1 1 calc R . .
C34 C 0.3527(9) -0.7627(7) 0.4739(6) 0.021(3) Uani 1 1 d . . .
H34 H 0.3995 -0.7821 0.4845 0.025 Uiso 1 1 calc R . .
C35 C 0.2910(9) -0.8093(8) 0.4802(6) 0.022(3) Uani 1 1 d . . .
C36 C 0.3015(9) -0.8821(8) 0.4973(6) 0.024(3) Uani 1 1 d . . .
H36 H 0.3485 -0.9026 0.5064 0.029 Uiso 1 1 calc R . .
C37 C 0.2423(10) -0.9245(8) 0.5008(7) 0.029(4) Uani 1 1 d . . .
H37 H 0.2483 -0.9739 0.5132 0.035 Uiso 1 1 calc R . .
C38 C 0.1736(10) -0.8923(9) 0.4855(6) 0.032(4) Uani 1 1 d . . .
H38 H 0.1333 -0.9200 0.4864 0.039 Uiso 1 1 calc R . .
C39 C 0.1650(9) -0.8180(9) 0.4688(6) 0.023(3) Uani 1 1 d . . .
C40 C 0.0922(9) -0.7831(9) 0.4513(8) 0.034(4) Uani 1 1 d . . .
H40A H 0.0810 -0.7876 0.4172 0.041 Uiso 1 1 calc R . .
H40B H 0.0541 -0.8067 0.4773 0.041 Uiso 1 1 calc R . .
C41 C 0.9757(11) 0.9066(9) 0.3898(8) 0.041(5) Uani 1 1 d . . .
H41A H 0.9826 0.8729 0.4256 0.050 Uiso 1 1 calc R . .
H41B H 0.9951 0.8844 0.3644 0.050 Uiso 1 1 calc R . .
C42 C 0.8945(11) 0.9237(8) 0.3810(6) 0.030(4) Uani 1 1 d . . .
C43 C 0.8486(12) 0.8680(9) 0.3860(7) 0.038(5) Uani 1 1 d . . .
H43 H 0.8677 0.8217 0.3933 0.046 Uiso 1 1 calc R . .
C44 C 0.7732(13) 0.8835(8) 0.3799(7) 0.041(5) Uani 1 1 d . . .
H44 H 0.7408 0.8469 0.3842 0.049 Uiso 1 1 calc R . .
C45 C 0.7454(11) 0.9540(9) 0.3672(6) 0.034(4) Uani 1 1 d . . .
H45 H 0.6951 0.9652 0.3627 0.041 Uiso 1 1 calc R . .
C46 C 0.7963(11) 1.0066(8) 0.3618(6) 0.030(4) Uani 1 1 d . . .
C47 C 0.7695(10) 1.0808(8) 0.3480(6) 0.027(4) Uani 1 1 d . . .
H47 H 0.7190 1.0920 0.3464 0.032 Uiso 1 1 calc R . .
C48 C 0.7127(9) 1.2167(9) 0.3353(8) 0.038(5) Uani 1 1 d . . .
H48A H 0.6839 1.2052 0.3100 0.057 Uiso 1 1 calc R . .
H48B H 0.7061 1.2665 0.3302 0.057 Uiso 1 1 calc R . .
H48C H 0.6968 1.1892 0.3710 0.057 Uiso 1 1 calc R . .
C49 C 0.8449(9) 1.2513(7) 0.3100(6) 0.021(3) Uani 1 1 d . . .
C50 C 0.8259(9) 1.3236(7) 0.2968(6) 0.019(3) Uani 1 1 d . . .
H50 H 0.7770 1.3397 0.2979 0.023 Uiso 1 1 calc R . .
C51 C 0.8838(9) 1.3703(7) 0.2820(5) 0.020(3) Uani 1 1 d . . .
C52 C 0.9651(9) 1.2772(7) 0.2879(6) 0.022(3) Uani 1 1 d . . .
C53 C 1.0432(9) 1.2504(8) 0.2802(7) 0.032(4) Uani 1 1 d . . .
H53A H 1.0412 1.2077 0.2713 0.049 Uiso 1 1 calc R . .
H53B H 1.0697 1.2404 0.3126 0.049 Uiso 1 1 calc R . .
H53C H 1.0682 1.2862 0.2516 0.049 Uiso 1 1 calc R . .
C54 C 0.8018(9) 1.4726(8) 0.2855(7) 0.031(4) Uani 1 1 d . . .
H54A H 0.8121 1.5115 0.2975 0.047 Uiso 1 1 calc R . .
H54B H 0.7774 1.4362 0.3140 0.047 Uiso 1 1 calc R . .
H54C H 0.7702 1.4895 0.2553 0.047 Uiso 1 1 calc R . .
C55 C 0.9139(9) 1.5546(7) 0.2287(6) 0.022(3) Uani 1 1 d . . .
H55 H 0.8669 1.5727 0.2334 0.027 Uiso 1 1 calc R . .
C56 C 0.9737(8) 1.6027(7) 0.2026(6) 0.018(3) Uani 1 1 d . . .
C57 C 0.9580(8) 1.6730(8) 0.1756(6) 0.022(3) Uani 1 1 d . . .
H57 H 0.9093 1.6906 0.1731 0.027 Uiso 1 1 calc R . .
C58 C 1.0147(8) 1.7177(8) 0.1523(6) 0.020(3) Uani 1 1 d . . .
C59 C 1.0983(8) 1.6226(7) 0.1824(6) 0.016(3) Uani 1 1 d . . .
C60 C 1.1771(8) 1.5970(7) 0.1861(6) 0.018(3) Uani 1 1 d . . .
C61 C 1.1998(8) 1.5468(8) 0.2339(6) 0.021(3) Uani 1 1 d . . .
H61 H 1.1660 1.5284 0.2621 0.025 Uiso 1 1 calc R . .
C62 C 1.2742(9) 1.5245(8) 0.2391(7) 0.027(4) Uani 1 1 d . . .
H62 H 1.2903 1.4916 0.2712 0.033 Uiso 1 1 calc R . .
C63 C 1.3240(9) 1.5510(9) 0.1969(7) 0.028(4) Uani 1 1 d . . .
H63 H 1.3733 1.5353 0.2005 0.033 Uiso 1 1 calc R . .
C64 C 1.3012(9) 1.6011(8) 0.1489(7) 0.025(3) Uani 1 1 d . . .
H64 H 1.3352 1.6192 0.1208 0.030 Uiso 1 1 calc R . .
C65 C 1.2276(9) 1.6238(8) 0.1433(7) 0.025(4) Uani 1 1 d . . .
H65 H 1.2117 1.6567 0.1112 0.030 Uiso 1 1 calc R . .
C66 C 0.9973(8) 1.7938(7) 0.1255(6) 0.022(3) Uani 1 1 d . . .
H66 H 0.9496 1.8096 0.1143 0.027 Uiso 1 1 calc R . .
C67 C 0.9582(8) 1.9309(8) 0.0719(6) 0.021(3) Uani 1 1 d . . .
H67A H 0.9463 1.9025 0.0507 0.032 Uiso 1 1 calc R . .
H67B H 0.9578 1.9803 0.0499 0.032 Uiso 1 1 calc R . .
H67C H 0.9223 1.9241 0.1007 0.032 Uiso 1 1 calc R . .
C68 C 1.0858(8) 1.9583(7) 0.0923(6) 0.015(3) Uani 1 1 d . . .
C69 C 1.0676(8) 2.0300(7) 0.0761(5) 0.014(3) Uani 1 1 d U . .
H69 H 1.0200 2.0473 0.0657 0.017 Uiso 1 1 calc R . .
C70 C 1.1239(7) 2.0756(7) 0.0762(6) 0.016(3) Uani 1 1 d . . .
C71 C 1.2057(8) 1.9802(7) 0.1037(6) 0.019(3) Uani 1 1 d . . .
C72 C 1.2825(8) 1.9518(8) 0.1192(7) 0.029(4) Uani 1 1 d . . .
H72A H 1.3055 1.9368 0.0914 0.043 Uiso 1 1 calc R . .
H72B H 1.2804 1.9119 0.1520 0.043 Uiso 1 1 calc R . .
H72C H 1.3108 1.9884 0.1243 0.043 Uiso 1 1 calc R . .
C73 C 1.0331(8) 2.1778(8) 0.0608(6) 0.023(3) Uani 1 1 d U . .
H73A H 1.0160 2.1901 0.0250 0.034 Uiso 1 1 calc R . .
H73B H 1.0326 2.2197 0.0708 0.034 Uiso 1 1 calc R . .
H73C H 1.0012 2.1434 0.0850 0.034 Uiso 1 1 calc R . .
C74 C 1.1530(8) 2.2598(8) 0.0304(6) 0.020(3) Uani 1 1 d . . .
H74 H 1.1043 2.2767 0.0244 0.024 Uiso 1 1 calc R . .
C75 C 1.2131(8) 2.3096(8) 0.0182(6) 0.019(3) Uani 1 1 d . . .
C76 C 1.1983(9) 2.3822(8) -0.0015(6) 0.022(3) Uani 1 1 d . . .
H76 H 1.1503 2.4000 -0.0102 0.026 Uiso 1 1 calc R . .
C77 C 1.2566(9) 2.4285(8) -0.0082(6) 0.026(4) Uani 1 1 d . . .
H77 H 1.2480 2.4775 -0.0213 0.031 Uiso 1 1 calc R . .
C78 C 1.3260(9) 2.4009(8) 0.0047(6) 0.022(3) Uani 1 1 d . . .
H78 H 1.3651 2.4310 0.0012 0.026 Uiso 1 1 calc R . .
C79 C 1.3384(8) 2.3275(8) 0.0232(6) 0.020(3) Uani 1 1 d . . .
C80 C 1.4137(9) 2.2956(8) 0.0390(7) 0.025(4) Uani 1 1 d . . .
H80A H 1.4503 2.3228 0.0133 0.030 Uiso 1 1 calc R . .
H80B H 1.4245 2.2981 0.0738 0.030 Uiso 1 1 calc R . .
C81 C 0.5602(15) 0.4785(12) 0.2912(8) 0.058(7) Uani 1 1 d . . .
C82 C 0.5616(9) 0.0230(10) 0.1046(8) 0.034(4) Uani 1 1 d . . .
C83 C 0.4488(10) -0.1841(10) 0.1897(8) 0.042(5) Uani 1 1 d . . .
C84 C 0.2709(13) -0.3882(13) 0.5314(10) 0.058(6) Uani 1 1 d . . .
C85 C 0.3198(9) -0.6901(9) 0.3016(6) 0.027(4) Uani 1 1 d U . .
C86 C 0.9590(11) 1.0193(11) 0.2121(7) 0.041(5) Uani 1 1 d . . .
C87 C 1.2214(10) 1.8893(10) -0.0425(7) 0.038(5) Uani 1 1 d . . .
C88 C 1.2013(9) 2.1897(9) 0.1965(6) 0.026(4) Uani 1 1 d . . .
C89 C 0.5034(11) 0.1377(10) 0.3893(7) 0.040(5) Uani 1 1 d . . .
C90 C 0.1881(12) -0.6162(12) 0.6007(7) 0.047(5) Uani 1 1 d . . .
C91 C 1.2833(12) 2.1223(10) -0.1070(8) 0.044(5) Uani 1 1 d . . .
C92 C 0.7045(10) 0.3720(10) 0.0032(8) 0.038(4) Uani 1 1 d U . .
C93 C 1.0127(18) 1.3703(19) 0.1061(12) 0.087(10) Uani 1 1 d . . .
C94 C 0.853(3) 1.1780(18) 0.4773(12) 0.110(13) Uani 1 1 d . . .
C95 C 0.9559(16) 1.4412(16) 0.3901(12) 0.072(7) Uani 1 1 d U . .
C96 C 0.0780(17) 0.7974(16) 0.2846(12) 0.078(8) Uani 1 1 d U . .
C97 C 0.3396(11) 0.4122(9) 0.1304(7) 0.030(4) Uani 1 1 d . . .
C98 C 0.2601(9) 0.4121(10) 0.1404(7) 0.035(4) Uani 1 1 d . . .
H98A H 0.2396 0.4595 0.1243 0.052 Uiso 1 1 calc R . .
H98B H 0.2499 0.3962 0.1783 0.052 Uiso 1 1 calc R . .
H98C H 0.2383 0.3806 0.1251 0.052 Uiso 1 1 calc R . .
C99 C 0.1802(11) 0.0925(8) 0.3597(7) 0.032(4) Uani 1 1 d . . .
C100 C 0.2591(11) 0.0909(10) 0.3568(7) 0.041(5) Uani 1 1 d . . .
H10A H 0.2771 0.1252 0.3710 0.061 Uiso 1 1 calc R . .
H10B H 0.2756 0.1022 0.3201 0.061 Uiso 1 1 calc R . .
H10C H 0.2776 0.0441 0.3773 0.061 Uiso 1 1 calc R . .
C101 C 1.3713(12) 1.7948(10) 0.0598(7) 0.041(5) Uani 1 1 d . . .
C102 C 1.4384(12) 1.7796(12) 0.0341(9) 0.057(6) Uani 1 1 d . . .
H10D H 1.4341 1.7997 -0.0041 0.086 Uiso 1 1 calc R . .
H10E H 1.4466 1.7289 0.0442 0.086 Uiso 1 1 calc R . .
H10F H 1.4794 1.8000 0.0449 0.086 Uiso 1 1 calc R . .
C103 C 0.7106(10) 0.6680(9) 0.2479(7) 0.030(4) Uani 1 1 d . . .
C104 C 0.6352(12) 0.6911(12) 0.2538(11) 0.062(7) Uani 1 1 d . . .
H10G H 0.6315 0.7422 0.2405 0.094 Uiso 1 1 calc R . .
H10H H 0.6203 0.6740 0.2910 0.094 Uiso 1 1 calc R . .
H10I H 0.6035 0.6725 0.2340 0.094 Uiso 1 1 calc R . .
C105 C 0.0217(14) 0.6420(10) 0.0465(8) 0.046(5) Uani 1 1 d . . .
C106 C 0.0906(13) 0.6163(12) 0.0291(9) 0.056(6) Uani 1 1 d . . .
H10J H 0.0807 0.5815 0.0128 0.084 Uiso 1 1 calc R . .
H10K H 0.1214 0.5948 0.0594 0.084 Uiso 1 1 calc R . .
H10L H 0.1156 0.6554 0.0036 0.084 Uiso 1 1 calc R . .
C107 C 0.4609(17) 0.8707(10) 0.4536(8) 0.052(7) Uani 1 1 d . . .
C108 C 0.3977(16) 0.8992(15) 0.4712(11) 0.079(8) Uani 1 1 d . . .
H10M H 0.3692 0.8614 0.4951 0.118 Uiso 1 1 calc R . .
H10N H 0.3686 0.9257 0.4411 0.118 Uiso 1 1 calc R . .
H10O H 0.4117 0.9303 0.4898 0.118 Uiso 1 1 calc R . .
C109 C 0.2020(12) 0.1827(9) 0.7424(7) 0.035(4) Uani 1 1 d . . .
C110 C 0.1290(12) 0.2057(13) 0.7548(11) 0.064(7) Uani 1 1 d . . .
H11A H 0.1184 0.2533 0.7311 0.095 Uiso 1 1 calc R . .
H11B H 0.1268 0.2051 0.7912 0.095 Uiso 1 1 calc R . .
H11C H 0.0932 0.1742 0.7505 0.095 Uiso 1 1 calc R . .
N1 N 0.6492(7) 0.5036(6) 0.1367(5) 0.018(3) Uani 1 1 d . . .
N2 N 0.7015(7) 0.3651(6) 0.1607(5) 0.020(3) Uani 1 1 d . . .
N3 N 0.7276(7) 0.2954(6) 0.1716(5) 0.024(3) Uani 1 1 d . . .
N4 N 0.6052(7) 0.2668(6) 0.1938(5) 0.019(3) Uani 1 1 d . . .
N5 N 0.5658(7) 0.1474(6) 0.2253(5) 0.020(3) Uani 1 1 d . . .
N6 N 0.6518(7) 0.0518(6) 0.2332(5) 0.023(3) Uani 1 1 d . . .
N7 N 0.5953(7) 0.0080(6) 0.2583(5) 0.017(3) Uani 1 1 d . . .
N8 N 0.4790(7) -0.0832(6) 0.2991(5) 0.019(3) Uani 1 1 d . . .
N9 N 0.4384(7) -0.2004(6) 0.3432(5) 0.021(3) Uani 1 1 d . . .
N10 N 0.4741(6) -0.3460(6) 0.3815(5) 0.018(3) Uani 1 1 d . . .
N11 N 0.4919(7) -0.4160(6) 0.4038(5) 0.019(3) Uani 1 1 d . . .
N12 N 0.3710(7) -0.4360(6) 0.3865(5) 0.021(3) Uani 1 1 d . . .
N13 N 0.3250(7) -0.5531(6) 0.4105(5) 0.020(3) Uani 1 1 d . . .
N14 N 0.4041(7) -0.6532(6) 0.4452(5) 0.023(3) Uani 1 1 d . . .
N15 N 0.3428(7) -0.6946(6) 0.4538(5) 0.019(3) Uani 1 1 d . . .
N16 N 0.2234(7) -0.7772(6) 0.4658(5) 0.022(3) Uani 1 1 d . . .
N17 N 0.8689(9) 0.9920(7) 0.3681(5) 0.033(3) Uani 1 1 d . . .
N18 N 0.8169(7) 1.1304(6) 0.3382(5) 0.026(3) Uani 1 1 d . . .
N19 N 0.7916(8) 1.2000(7) 0.3272(6) 0.031(3) Uani 1 1 d . . .
N20 N 0.9148(8) 1.2281(6) 0.3051(5) 0.024(3) Uani 1 1 d . . .
N21 N 0.9540(7) 1.3477(6) 0.2768(5) 0.022(3) Uani 1 1 d . . .
N22 N 0.8705(7) 1.4435(6) 0.2702(5) 0.020(3) Uani 1 1 d . . .
N23 N 0.9278(7) 1.4865(6) 0.2452(5) 0.018(3) Uani 1 1 d . . .
N24 N 1.0448(6) 1.5769(6) 0.2058(5) 0.018(3) Uani 1 1 d . . .
N25 N 1.0860(7) 1.6939(6) 0.1552(5) 0.022(3) Uani 1 1 d . . .
N26 N 1.0499(6) 1.8384(6) 0.1179(5) 0.016(3) Uani 1 1 d . . .
N27 N 1.0317(6) 1.9094(6) 0.0939(5) 0.018(3) Uani 1 1 d . . .
N28 N 1.1551(7) 1.9322(6) 0.1060(5) 0.020(3) Uani 1 1 d . . .
N29 N 1.1937(7) 2.0503(6) 0.0877(5) 0.020(3) Uani 1 1 d . . .
N30 N 1.1082(6) 2.1476(6) 0.0635(5) 0.017(3) Uani 1 1 d . . .
N31 N 1.1675(6) 2.1924(6) 0.0495(4) 0.013(2) Uani 1 1 d U . .
N32 N 1.2819(7) 2.2816(6) 0.0306(5) 0.018(3) Uani 1 1 d . . .
N33 N 0.4020(9) 0.4131(8) 0.1205(6) 0.037(4) Uani 1 1 d . . .
N34 N 0.1170(10) 0.0937(8) 0.3635(7) 0.044(4) Uani 1 1 d . . .
N35 N 1.3187(8) 1.8067(11) 0.0800(7) 0.052(5) Uani 1 1 d . . .
N36 N 0.7695(9) 0.6509(8) 0.2423(7) 0.042(4) Uani 1 1 d . . .
N37 N -0.0320(13) 0.6615(10) 0.0599(8) 0.061(6) Uani 1 1 d . . .
N38 N 0.5135(15) 0.8467(10) 0.4391(7) 0.068(7) Uani 1 1 d . . .
N39 N 0.2576(10) 0.1631(9) 0.7331(8) 0.053(5) Uani 1 1 d . . .
O1 O 0.5028(6) 0.5301(5) 0.1175(5) 0.033(3) Uani 1 1 d . . .
H1 H 0.4539 0.5376 0.1068 0.040 Uiso 1 1 calc R . .
O2 O 0.0918(9) -0.7104(9) 0.4460(6) 0.064(4) Uani 1 1 d U . .
H2 H 0.0467 -0.6852 0.4418 0.077 Uiso 1 1 calc R . .
O3 O 1.0150(8) 0.9678(6) 0.3834(5) 0.047(4) Uani 1 1 d . . .
H3A H 1.0662 0.9635 0.3866 0.056 Uiso 1 1 calc R . .
O4 O 1.4187(6) 2.2238(5) 0.0412(5) 0.027(3) Uani 1 1 d . . .
H4A H 1.4651 2.2019 0.0409 0.032 Uiso 1 1 calc R . .
O11 O 0.5370(6) 0.4075(7) 0.2319(5) 0.035(3) Uani 1 1 d . . .
O12 O 0.5443(10) 0.3439(9) 0.3277(6) 0.073(5) Uani 1 1 d . . .
O13 O 0.6556(7) 0.3905(7) 0.2732(5) 0.042(3) Uani 1 1 d . . .
O21 O 0.4715(6) 0.0249(6) 0.1828(5) 0.034(3) Uani 1 1 d . . .
O22 O 0.4242(5) 0.0619(5) 0.0929(4) 0.023(2) Uani 1 1 d . . .
O23 O 0.5060(7) 0.1392(6) 0.1179(5) 0.041(3) Uani 1 1 d . . .
O31 O 0.4417(8) -0.3044(7) 0.2675(5) 0.045(3) Uani 1 1 d . . .
O32 O 0.3361(8) -0.2650(8) 0.2104(6) 0.054(4) Uani 1 1 d U . .
O33 O 0.4504(9) -0.3055(7) 0.1761(6) 0.058(4) Uani 1 1 d . . .
O41 O 0.3128(7) -0.3148(6) 0.4356(5) 0.041(3) Uani 1 1 d . . .
O42 O 0.4046(6) -0.3899(6) 0.4945(5) 0.033(3) Uani 1 1 d . . .
O43 O 0.3565(8) -0.2811(7) 0.5086(7) 0.060(4) Uani 1 1 d . . .
O52 O 0.2293(6) -0.6317(5) 0.3530(4) 0.026(2) Uani 1 1 d . . .
O53 O 0.1967(6) -0.7454(5) 0.3462(4) 0.028(3) Uani 1 1 d . . .
O54 O 0.1906(6) -0.6373(5) 0.2683(4) 0.023(2) Uani 1 1 d . . .
O61 O 0.9800(6) 1.0861(6) 0.2758(4) 0.031(3) Uani 1 1 d . . .
O62 O 0.9749(8) 1.1559(8) 0.1818(6) 0.058(4) Uani 1 1 d . . .
O63 O 0.8629(6) 1.1055(6) 0.2322(5) 0.036(3) Uani 1 1 d . . .
O71 O 1.1682(6) 1.7981(6) 0.0455(5) 0.032(3) Uani 1 1 d . . .
O72 O 1.1304(6) 1.7928(6) -0.0397(5) 0.035(3) Uani 1 1 d . . .
O73 O 1.0856(6) 1.8909(6) -0.0084(5) 0.031(3) Uani 1 1 d . . .
O81 O 1.2904(6) 2.1347(5) 0.1414(4) 0.019(2) Uani 1 1 d . . .
O82 O 1.3325(6) 2.1360(5) 0.2263(4) 0.023(2) Uani 1 1 d . . .
O83 O 1.3236(6) 2.2473(5) 0.1510(4) 0.024(2) Uani 1 1 d . . .
O91 O 0.5596(8) 0.0143(6) 0.4386(5) 0.048(4) Uani 1 1 d . . .
O92 O 0.4692(11) 0.0254(11) 0.3726(8) 0.088(6) Uani 1 1 d U . .
O93 O 0.5870(14) 0.0691(10) 0.3448(7) 0.111(9) Uani 1 1 d . . .
O101 O 0.2992(7) -0.7033(7) 0.6202(5) 0.042(3) Uani 1 1 d . . .
O102 O 0.2936(6) -0.6119(6) 0.5321(5) 0.034(3) Uani 1 1 d . . .
O103 O 0.2132(7) -0.7102(6) 0.5554(4) 0.030(3) Uani 1 1 d . . .
O111 O 1.1819(7) 2.2200(6) -0.1231(5) 0.039(3) Uani 1 1 d . . .
O112 O 1.1842(7) 2.1257(6) -0.0362(5) 0.037(3) Uani 1 1 d . . .
O113 O 1.2753(6) 2.2161(6) -0.0602(4) 0.026(3) Uani 1 1 d . . .
O121 O 0.6098(7) 0.4444(6) 0.0373(5) 0.036(3) Uani 1 1 d . . .
O122 O 0.5914(8) 0.3181(7) 0.0641(5) 0.044(3) Uani 1 1 d . . .
O123 O 0.5723(7) 0.3947(6) -0.0294(5) 0.035(3) Uani 1 1 d . . .
O131 O 1.0265(10) 1.4853(9) 0.1302(7) 0.073(5) Uani 1 1 d U . .
O132 O 0.9343(10) 1.4833(7) 0.0680(6) 0.063(5) Uani 1 1 d . . .
O133 O 0.9271(10) 1.4144(11) 0.1612(6) 0.081(6) Uani 1 1 d . . .
O141 O 0.8631(9) 1.0644(9) 0.4544(7) 0.066(4) Uani 1 1 d U . .
O142 O 0.8693(9) 1.0572(9) 0.5452(6) 0.066(4) Uani 1 1 d . . .
O143 O 0.9689(10) 1.0992(10) 0.4819(8) 0.084(6) Uani 1 1 d . . .
O151 O 1.0534(11) 1.4448(11) 0.3243(8) 0.093(6) Uani 1 1 d U . .
O152 O 1.0829(7) 1.4504(7) 0.4080(5) 0.043(3) Uani 1 1 d . . .
O153 O 0.997(2) 1.573(2) 0.3279(14) 0.24(2) Uani 1 1 d . . .
O161 O 0.1531(12) 0.7159(11) 0.2445(8) 0.103(8) Uani 1 1 d . . .
O162 O 0.1940(14) 0.8329(9) 0.2294(7) 0.102(8) Uani 1 1 d . . .
O163 O 0.1991(7) 0.7472(9) 0.3181(5) 0.054(4) Uani 1 1 d . . .
F11 F 0.5902(9) 0.4782(9) 0.3364(6) 0.083(5) Uani 1 1 d . . .
F12 F 0.4862(8) 0.4910(10) 0.2979(6) 0.092(6) Uani 1 1 d . . .
F13 F 0.5883(11) 0.5324(7) 0.2507(5) 0.095(6) Uani 1 1 d . . .
F21 F 0.5454(6) -0.0444(6) 0.1134(6) 0.062(4) Uani 1 1 d . . .
F22 F 0.5766(6) 0.0548(6) 0.0532(4) 0.044(3) Uani 1 1 d . . .
F23 F 0.6205(6) 0.0245(7) 0.1313(5) 0.056(3) Uani 1 1 d . . .
F31 F 0.4103(10) -0.1476(7) 0.2175(5) 0.082(5) Uani 1 1 d . . .
F32 F 0.5175(8) -0.1829(8) 0.2006(7) 0.090(6) Uani 1 1 d . . .
F33 F 0.4387(6) -0.1501(5) 0.1386(4) 0.046(3) Uani 1 1 d . . .
F41 F 0.2115(7) -0.3459(8) 0.5315(6) 0.083(5) Uani 1 1 d . . .
F42 F 0.2936(9) -0.4161(9) 0.5810(6) 0.098(6) Uani 1 1 d . . .
F43 F 0.2527(8) -0.4395(7) 0.5126(7) 0.086(5) Uani 1 1 d . . .
F51 F 0.3249(7) -0.7315(6) 0.2719(5) 0.056(3) Uani 1 1 d . . .
F53 F 0.3530(6) -0.6308(6) 0.2749(5) 0.049(3) Uani 1 1 d . . .
F54 F 0.3575(6) -0.7231(7) 0.3455(5) 0.055(3) Uani 1 1 d . . .
F61 F 0.9311(9) 0.9641(6) 0.2513(5) 0.067(4) Uani 1 1 d . . .
F62 F 1.0312(7) 1.0066(8) 0.2066(5) 0.068(4) Uani 1 1 d . . .
F63 F 0.9281(7) 1.0219(7) 0.1668(5) 0.061(3) Uani 1 1 d . . .
F71 F 1.2418(6) 1.9316(6) -0.0152(5) 0.058(3) Uani 1 1 d . . .
F72 F 1.2796(6) 1.8483(6) -0.0467(5) 0.052(3) Uani 1 1 d . . .
F73 F 1.2023(7) 1.9311(7) -0.0909(5) 0.065(4) Uani 1 1 d . . .
F81 F 1.1632(6) 2.2286(6) 0.1543(4) 0.046(3) Uani 1 1 d . . .
F82 F 1.1979(6) 2.2246(6) 0.2310(4) 0.050(3) Uani 1 1 d . . .
F83 F 1.1685(5) 2.1293(5) 0.2192(4) 0.041(3) Uani 1 1 d . . .
F91 F 0.4495(7) 0.1348(8) 0.4249(6) 0.074(4) Uani 1 1 d . . .
F92 F 0.5572(7) 0.1709(6) 0.4024(5) 0.058(3) Uani 1 1 d . . .
F93 F 0.4768(9) 0.1785(7) 0.3424(5) 0.084(5) Uani 1 1 d . . .
F101 F 0.1453(7) -0.6608(8) 0.6387(5) 0.074(4) Uani 1 1 d . . .
F102 F 0.1442(8) -0.5771(7) 0.5614(6) 0.073(4) Uani 1 1 d . . .
F103 F 0.2193(9) -0.5733(7) 0.6211(5) 0.075(4) Uani 1 1 d . . .
F111 F 1.2429(8) 2.0841(6) -0.1274(5) 0.063(4) Uani 1 1 d . . .
F112 F 1.3291(6) 2.1614(8) -0.1443(5) 0.065(4) Uani 1 1 d . . .
F113 F 1.3221(8) 2.0764(7) -0.0673(5) 0.074(4) Uani 1 1 d . . .
F121 F 0.7281(6) 0.4298(6) -0.0355(4) 0.047(3) Uani 1 1 d . . .
F122 F 0.7471(7) 0.3610(8) 0.0464(5) 0.068(4) Uani 1 1 d . . .
F123 F 0.7157(7) 0.3148(6) -0.0126(4) 0.051(3) Uani 1 1 d . . .
F131 F 1.0562(14) 1.3358(14) 0.1473(10) 0.152(8) Uani 1 1 d U . .
F132 F 0.9678(11) 1.3285(8) 0.0953(7) 0.094(6) Uani 1 1 d . . .
F133 F 1.0593(16) 1.3824(15) 0.0686(12) 0.163(9) Uani 1 1 d U . .
F141 F 0.8806(12) 1.2110(8) 0.5106(7) 0.107(6) Uani 1 1 d . . .
F142 F 0.7779(9) 1.1807(10) 0.4899(11) 0.142(10) Uani 1 1 d . . .
F143 F 0.8779(11) 1.2145(11) 0.4280(6) 0.119(7) Uani 1 1 d . . .
F151 F 0.9443(12) 1.4449(16) 0.4485(9) 0.154(9) Uani 1 1 d . . .
F152 F 0.9526(11) 1.3531(17) 0.4154(11) 0.189(13) Uani 1 1 d . . .
F153 F 0.8965(15) 1.4563(11) 0.3742(7) 0.144(9) Uani 1 1 d . . .
F161 F 0.0341(8) 0.7549(10) 0.3136(6) 0.102(6) Uani 1 1 d . . .
F162 F 0.0788(10) 0.8503(12) 0.3060(8) 0.117(7) Uani 1 1 d . . .
F163 F 0.0402(9) 0.8380(10) 0.2345(7) 0.099(6) Uani 1 1 d . . .
S1 S 0.5771(3) 0.3958(3) 0.28033(19) 0.0373(11) Uani 1 1 d . . .
S2 S 0.4820(2) 0.0673(2) 0.12684(17) 0.0258(9) Uani 1 1 d . . .
S3 S 0.4141(3) -0.2747(2) 0.21207(18) 0.0355(10) Uani 1 1 d . . .
S4 S 0.3453(2) -0.3375(2) 0.48824(18) 0.0303(9) Uani 1 1 d . . .
S5 S 0.2233(2) -0.67551(19) 0.31916(15) 0.0194(8) Uani 1 1 d . . .
S6 S 0.9419(2) 1.1020(2) 0.22605(16) 0.0264(9) Uani 1 1 d . . .
S7 S 1.1420(2) 1.8372(2) -0.00787(16) 0.0249(9) Uani 1 1 d . . .
S8 S 1.2979(2) 2.17658(18) 0.17661(14) 0.0169(7) Uani 1 1 d . . .
S9 S 0.5344(3) 0.0518(2) 0.38700(19) 0.0446(13) Uani 1 1 d . . .
S10 S 0.2564(2) -0.6659(2) 0.57470(16) 0.0235(8) Uani 1 1 d . . .
S11 S 1.2237(2) 2.17761(19) -0.07863(15) 0.0194(8) Uani 1 1 d . . .
S12 S 0.6093(3) 0.3841(2) 0.01986(17) 0.0315(10) Uani 1 1 d . . .
S13 S 0.9716(2) 1.4475(2) 0.11602(17) 0.0288(9) Uani 1 1 d . . .
S14 S 0.8896(3) 1.0971(3) 0.4888(2) 0.0476(13) Uani 1 1 d . . .
S15 S 1.0310(2) 1.4697(2) 0.36517(17) 0.0299(9) Uani 1 1 d . . .
S16 S 0.1640(3) 0.7663(3) 0.2692(2) 0.0424(12) Uani 1 1 d . . .
Pb1 Pb 0.56309(3) 0.40564(3) 0.14106(2) 0.01819(13) Uani 1 1 d . . .
Pb2 Pb 0.46691(3) 0.05671(3) 0.26616(2) 0.02230(14) Uani 1 1 d . . .
Pb3 Pb 0.34835(3) -0.30163(3) 0.34274(2) 0.02267(14) Uani 1 1 d . . .
Pb4 Pb 0.20865(3) -0.64506(3) 0.44744(2) 0.01968(13) Uani 1 1 d . . .
Pb5 Pb 0.95315(4) 1.08946(3) 0.36393(2) 0.02468(14) Uani 1 1 d . . .
Pb6 Pb 1.05356(3) 1.43732(3) 0.23508(2) 0.01940(13) Uani 1 1 d . . .
Pb7 Pb 1.18690(3) 1.79624(3) 0.13780(2) 0.02074(14) Uani 1 1 d . . .
Pb8 Pb 1.29997(3) 2.15080(3) 0.04593(2) 0.01494(12) Uani 1 1 d . . .
O5 O 0.003(2) 0.2922(18) 0.5496(12) 0.198(17) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.432(18) . ?
C1 C2 1.50(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.350(19) . ?
C2 C3 1.39(2) . ?
C3 C4 1.36(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.40(2) . ?
C5 H5 0.9300 . ?
C6 N1 1.34(2) . ?
C6 C7 1.49(2) . ?
C7 N2 1.290(18) . ?
C7 H7 0.9300 . ?
C8 N3 1.45(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.342(19) . ?
C9 N3 1.373(18) . ?
C9 C10 1.38(2) . ?
C10 C11 1.37(2) . ?
C10 H10 0.9300 . ?
C11 N5 1.37(2) . ?
C11 N6 1.408(18) . ?
C12 N5 1.327(18) . ?
C12 N4 1.344(18) . ?
C12 C13 1.50(2) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N6 1.465(19) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N7 1.275(18) . ?
C15 C16 1.45(2) . ?
C15 H15 0.9300 . ?
C16 N8 1.346(19) . ?
C16 C17 1.390(19) . ?
C17 C18 1.38(2) . ?
C17 H17 0.9300 . ?
C18 N9 1.348(19) . ?
C18 C26 1.482(19) . ?
C19 N8 1.330(19) . ?
C19 N9 1.356(18) . ?
C19 C20 1.49(2) . ?
C20 C21 1.39(2) . ?
C20 C25 1.41(2) . ?
C21 C22 1.39(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.39(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.39(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.38(2) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 N10 1.288(18) . ?
C26 H26 0.9300 . ?
C27 N11 1.456(19) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N12 1.331(19) . ?
C28 N11 1.391(18) . ?
C28 C29 1.39(2) . ?
C29 C30 1.406(19) . ?
C29 H29 0.9300 . ?
C30 N13 1.339(18) . ?
C30 N14 1.388(17) . ?
C31 N12 1.340(18) . ?
C31 N13 1.343(18) . ?
C31 C32 1.51(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N14 1.461(19) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N15 1.287(18) . ?
C34 C35 1.45(2) . ?
C34 H34 0.9300 . ?
C35 N16 1.36(2) . ?
C35 C36 1.37(2) . ?
C36 C37 1.38(2) . ?
C36 H36 0.9300 . ?
C37 C38 1.38(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.40(2) . ?
C38 H38 0.9300 . ?
C39 N16 1.346(18) . ?
C39 C40 1.48(2) . ?
C40 O2 1.41(2) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 O3 1.40(2) . ?
C41 C42 1.50(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 N17 1.35(2) . ?
C42 C43 1.38(2) . ?
C43 C44 1.39(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.41(2) . ?
C44 H44 0.9300 . ?
C45 C46 1.39(2) . ?
C45 H45 0.9300 . ?
C46 N17 1.34(2) . ?
C46 C47 1.46(2) . ?
C47 N18 1.29(2) . ?
C47 H47 0.9300 . ?
C48 N19 1.47(2) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 N20 1.34(2) . ?
C49 N19 1.39(2) . ?
C49 C50 1.395(19) . ?
C50 C51 1.39(2) . ?
C50 H50 0.9300 . ?
C51 N21 1.35(2) . ?
C51 N22 1.399(18) . ?
C52 N20 1.32(2) . ?
C52 N21 1.345(18) . ?
C52 C53 1.52(2) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 N22 1.45(2) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 N23 1.294(18) . ?
C55 C56 1.47(2) . ?
C55 H55 0.9300 . ?
C56 N24 1.360(18) . ?
C56 C57 1.37(2) . ?
C57 C58 1.37(2) . ?
C57 H57 0.9300 . ?
C58 N25 1.349(19) . ?
C58 C66 1.47(2) . ?
C59 N24 1.341(18) . ?
C59 N25 1.373(18) . ?
C59 C60 1.49(2) . ?
C60 C61 1.39(2) . ?
C60 C65 1.40(2) . ?
C61 C62 1.40(2) . ?
C61 H61 0.9300 . ?
C62 C63 1.38(2) . ?
C62 H62 0.9300 . ?
C63 C64 1.39(2) . ?
C63 H63 0.9300 . ?
C64 C65 1.39(2) . ?
C64 H64 0.9300 . ?
C65 H65 0.9300 . ?
C66 N26 1.295(18) . ?
C66 H66 0.9300 . ?
C67 N27 1.461(17) . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 N28 1.350(18) . ?
C68 C69 1.376(19) . ?
C68 N27 1.403(17) . ?
C69 C70 1.396(18) . ?
C69 H69 0.9300 . ?
C70 N29 1.346(18) . ?
C70 N30 1.377(18) . ?
C71 N29 1.328(18) . ?
C71 N28 1.339(18) . ?
C71 C72 1.50(2) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 N30 1.456(19) . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 N31 1.285(18) . ?
C74 C75 1.458(19) . ?
C74 H74 0.9300 . ?
C75 N32 1.347(19) . ?
C75 C76 1.38(2) . ?
C76 C77 1.40(2) . ?
C76 H76 0.9300 . ?
C77 C78 1.36(2) . ?
C77 H77 0.9300 . ?
C78 C79 1.39(2) . ?
C78 H78 0.9300 . ?
C79 N32 1.367(17) . ?
C79 C80 1.49(2) . ?
C80 O4 1.414(18) . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C81 F11 1.34(2) . ?
C81 F13 1.34(3) . ?
C81 F12 1.37(3) . ?
C81 S1 1.78(2) . ?
C82 F23 1.31(2) . ?
C82 F22 1.32(2) . ?
C82 F21 1.33(2) . ?
C82 S2 1.838(18) . ?
C83 F32 1.29(2) . ?
C83 F33 1.31(2) . ?
C83 F31 1.36(2) . ?
C83 S3 1.833(19) . ?
C84 F42 1.32(3) . ?
C84 F41 1.34(2) . ?
C84 F43 1.34(3) . ?
C84 S4 1.83(2) . ?
C85 F53 1.311(19) . ?
C85 F51 1.320(19) . ?
C85 F54 1.328(19) . ?
C85 S5 1.825(17) . ?
C86 F62 1.33(2) . ?
C86 F63 1.33(2) . ?
C86 F61 1.34(2) . ?
C86 S6 1.820(19) . ?
C87 F73 1.32(2) . ?
C87 F72 1.33(2) . ?
C87 F71 1.36(2) . ?
C87 S7 1.834(18) . ?
C88 F83 1.309(19) . ?
C88 F82 1.323(19) . ?
C88 F81 1.325(18) . ?
C88 S8 1.837(16) . ?
C89 F91 1.32(2) . ?
C89 F92 1.32(2) . ?
C89 F93 1.33(2) . ?
C89 S9 1.798(19) . ?
C90 F103 1.31(2) . ?
C90 F102 1.34(2) . ?
C90 F101 1.34(2) . ?
C90 S10 1.810(19) . ?
C91 F112 1.32(2) . ?
C91 F111 1.33(2) . ?
C91 F113 1.34(2) . ?
C91 S11 1.83(2) . ?
C92 F121 1.33(2) . ?
C92 F123 1.35(2) . ?
C92 F122 1.36(2) . ?
C92 S12 1.79(2) . ?
C93 F133 1.24(4) . ?
C93 F132 1.29(4) . ?
C93 F131 1.34(3) . ?
C93 S13 1.78(3) . ?
C94 F143 1.34(3) . ?
C94 F142 1.38(4) . ?
C94 F141 1.39(3) . ?
C94 S14 1.65(4) . ?
C95 F153 1.16(3) . ?
C95 S15 1.53(3) . ?
C95 F151 1.58(4) . ?
C95 F152 1.66(4) . ?
C96 F161 1.23(3) . ?
C96 F162 1.36(3) . ?
C96 F163 1.48(3) . ?
C96 S16 1.73(3) . ?
C97 N33 1.15(2) . ?
C97 C98 1.45(2) . ?
C98 H98A 0.9600 . ?
C98 H98B 0.9600 . ?
C98 H98C 0.9600 . ?
C99 N34 1.14(2) . ?
C99 C100 1.42(3) . ?
C100 H10A 0.9600 . ?
C100 H10B 0.9600 . ?
C100 H10C 0.9600 . ?
C101 N35 1.13(2) . ?
C101 C102 1.44(3) . ?
C102 H10D 0.9600 . ?
C102 H10E 0.9600 . ?
C102 H10F 0.9600 . ?
C103 N36 1.12(2) . ?
C103 C104 1.44(3) . ?
C104 H10G 0.9600 . ?
C104 H10H 0.9600 . ?
C104 H10I 0.9600 . ?
C105 N37 1.12(3) . ?
C105 C106 1.45(3) . ?
C106 H10J 0.9600 . ?
C106 H10K 0.9600 . ?
C106 H10L 0.9600 . ?
C107 N38 1.15(3) . ?
C107 C108 1.39(4) . ?
C108 H10M 0.9600 . ?
C108 H10N 0.9600 . ?
C108 H10O 0.9600 . ?
C109 N39 1.11(2) . ?
C109 C110 1.44(3) . ?
C110 H11A 0.9600 . ?
C110 H11B 0.9600 . ?
C110 H11C 0.9600 . ?
N1 Pb1 2.523(11) . ?
N2 N3 1.386(16) . ?
N2 Pb1 2.614(13) . ?
N4 Pb1 2.735(11) . ?
N5 Pb2 2.540(12) . ?
N6 N7 1.372(17) . ?
N7 Pb2 2.506(12) . ?
N8 Pb2 2.629(11) . ?
N9 Pb3 2.654(12) . ?
N10 N11 1.349(16) . ?
N10 Pb3 2.532(11) . ?
N12 Pb3 2.557(11) . ?
N13 Pb4 2.777(11) . ?
N14 N15 1.376(16) . ?
N15 Pb4 2.570(12) . ?
N16 Pb4 2.518(12) . ?
N17 Pb5 2.494(14) . ?
N18 N19 1.378(18) . ?
N18 Pb5 2.606(14) . ?
N20 Pb5 2.750(12) . ?
N21 Pb6 2.540(13) . ?
N22 N23 1.374(16) . ?
N23 Pb6 2.478(12) . ?
N24 Pb6 2.625(11) . ?
N25 Pb7 2.709(12) . ?
N26 N27 1.373(16) . ?
N26 Pb7 2.597(11) . ?
N28 Pb7 2.599(11) . ?
N29 Pb8 2.759(11) . ?
N30 N31 1.385(15) . ?
N31 Pb8 2.509(11) . ?
N32 Pb8 2.510(11) . ?
N35 Pb7 2.759(15) . ?
O1 Pb1 2.552(10) . ?
O1 H1 0.9300 . ?
O2 Pb4 2.541(16) . ?
O2 H2 0.9300 . ?
O3 Pb5 2.523(12) . ?
O3 H3A 0.9300 . ?
O4 Pb8 2.623(10) . ?
O4 H4A 0.9300 . ?
O11 S1 1.446(12) . ?
O11 Pb1 2.451(11) . ?
O12 S1 1.455(14) . ?
O13 S1 1.428(13) . ?
O21 S2 1.450(12) . ?
O21 Pb2 2.497(12) . ?
O22 S2 1.439(11) . ?
O23 S2 1.455(12) . ?
O31 S3 1.486(13) . ?
O31 Pb3 2.577(14) . ?
O32 S3 1.415(15) . ?
O33 S3 1.425(14) . ?
O41 S4 1.457(13) . ?
O41 Pb3 2.450(13) . ?
O42 S4 1.438(11) . ?
O43 S4 1.430(14) . ?
O52 S5 1.460(11) . ?
O52 Pb4 2.445(11) . ?
O53 S5 1.430(11) . ?
O54 S5 1.442(11) . ?
O61 S6 1.446(12) . ?
O61 Pb5 2.394(11) . ?
O62 S6 1.428(13) . ?
O63 S6 1.432(12) . ?
O71 S7 1.454(12) . ?
O71 Pb7 2.475(11) . ?
O72 S7 1.442(12) . ?
O73 S7 1.443(11) . ?
O81 S8 1.462(10) . ?
O81 Pb8 2.445(10) . ?
O82 S8 1.445(10) . ?
O83 S8 1.432(10) . ?
O91 S9 1.404(13) . ?
O92 S9 1.43(2) . ?
O92 Pb2 2.68(2) . ?
O93 S9 1.40(2) . ?
O101 S10 1.424(12) . ?
O102 S10 1.438(12) . ?
O103 S10 1.434(11) . ?
O103 Pb4 2.720(10) . ?
O111 S11 1.421(12) . ?
O112 S11 1.436(11) . ?
O113 S11 1.435(11) . ?
O113 Pb8 2.721(10) . ?
O121 S12 1.427(12) . ?
O121 Pb1 2.708(11) . ?
O122 S12 1.476(13) . ?
O123 S12 1.439(12) . ?
O131 S13 1.409(17) . ?
O131 Pb6 2.679(17) . ?
O132 S13 1.414(13) . ?
O133 S13 1.398(16) . ?
O141 S14 1.400(17) . ?
O141 Pb5 2.758(16) . ?
O142 S14 1.478(16) . ?
O143 S14 1.441(19) . ?
O151 S15 1.38(2) . ?
O151 Pb6 2.42(2) . ?
O152 S15 1.443(13) . ?
O153 S15 2.05(5) . ?
O161 S16 1.399(16) . ?
O162 S16 1.50(2) . ?
O163 S16 1.395(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
O1 C1 C2 112.5(13) . . ?
O1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N1 C2 C3 121.7(15) . . ?
N1 C2 C1 119.0(13) . . ?
C3 C2 C1 119.3(14) . . ?
C4 C3 C2 119.3(15) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.4(14) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 119.1(15) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
N1 C6 C5 121.5(14) . . ?
N1 C6 C7 119.5(13) . . ?
C5 C6 C7 119.0(14) . . ?
N2 C7 C6 117.9(14) . . ?
N2 C7 H7 121.1 . . ?
C6 C7 H7 121.1 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 N3 116.9(13) . . ?
N4 C9 C10 121.0(13) . . ?
N3 C9 C10 122.0(14) . . ?
C11 C10 C9 117.5(15) . . ?
C11 C10 H10 121.3 . . ?
C9 C10 H10 121.3 . . ?
N5 C11 C10 122.5(13) . . ?
N5 C11 N6 117.0(13) . . ?
C10 C11 N6 120.5(14) . . ?
N5 C12 N4 125.5(14) . . ?
N5 C12 C13 118.6(13) . . ?
N4 C12 C13 115.9(12) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 120.0(14) . . ?
N7 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
N8 C16 C17 120.5(13) . . ?
N8 C16 C15 120.6(13) . . ?
C17 C16 C15 119.0(14) . . ?
C18 C17 C16 117.5(14) . . ?
C18 C17 H17 121.3 . . ?
C16 C17 H17 121.3 . . ?
N9 C18 C17 122.1(13) . . ?
N9 C18 C26 118.9(13) . . ?
C17 C18 C26 119.0(14) . . ?
N8 C19 N9 123.8(14) . . ?
N8 C19 C20 119.3(12) . . ?
N9 C19 C20 116.9(13) . . ?
C21 C20 C25 120.0(14) . . ?
C21 C20 C19 121.2(14) . . ?
C25 C20 C19 118.7(14) . . ?
C20 C21 C22 120.5(16) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C23 C22 C21 118.8(16) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C22 C23 C24 121.0(16) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 120.6(16) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C20 119.0(15) . . ?
C24 C25 H25 120.5 . . ?
C20 C25 H25 120.5 . . ?
N10 C26 C18 119.6(14) . . ?
N10 C26 H26 120.2 . . ?
C18 C26 H26 120.2 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N12 C28 N11 118.0(12) . . ?
N12 C28 C29 122.3(13) . . ?
N11 C28 C29 119.8(13) . . ?
C28 C29 C30 115.7(14) . . ?
C28 C29 H29 122.1 . . ?
C30 C29 H29 122.1 . . ?
N13 C30 N14 118.5(12) . . ?
N13 C30 C29 122.5(13) . . ?
N14 C30 C29 119.0(13) . . ?
N12 C31 N13 125.2(13) . . ?
N12 C31 C32 118.0(13) . . ?
N13 C31 C32 116.8(13) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N14 C33 H33A 109.5 . . ?
N14 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N14 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N15 C34 C35 120.4(14) . . ?
N15 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
N16 C35 C36 121.9(14) . . ?
N16 C35 C34 116.7(13) . . ?
C36 C35 C34 121.2(15) . . ?
C35 C36 C37 119.6(16) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C36 C37 C38 118.7(14) . . ?
C36 C37 H37 120.6 . . ?
C38 C37 H37 120.6 . . ?
C37 C38 C39 120.0(14) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
N16 C39 C38 120.6(15) . . ?
N16 C39 C40 119.1(14) . . ?
C38 C39 C40 120.3(14) . . ?
O2 C40 C39 111.0(14) . . ?
O2 C40 H40A 109.4 . . ?
C39 C40 H40A 109.4 . . ?
O2 C40 H40B 109.4 . . ?
C39 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
O3 C41 C42 111.6(14) . . ?
O3 C41 H41A 109.3 . . ?
C42 C41 H41A 109.3 . . ?
O3 C41 H41B 109.3 . . ?
C42 C41 H41B 109.3 . . ?
H41A C41 H41B 108.0 . . ?
N17 C42 C43 122.4(18) . . ?
N17 C42 C41 119.6(15) . . ?
C43 C42 C41 117.9(15) . . ?
C42 C43 C44 117.8(16) . . ?
C42 C43 H43 121.1 . . ?
C44 C43 H43 121.1 . . ?
C43 C44 C45 120.5(16) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C46 C45 C44 117.3(18) . . ?
C46 C45 H45 121.3 . . ?
C44 C45 H45 121.3 . . ?
N17 C46 C45 122.5(16) . . ?
N17 C46 C47 118.6(15) . . ?
C45 C46 C47 118.8(17) . . ?
N18 C47 C46 119.2(16) . . ?
N18 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
N19 C48 H48A 109.5 . . ?
N19 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N19 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N20 C49 N19 116.8(13) . . ?
N20 C49 C50 122.1(14) . . ?
N19 C49 C50 121.1(15) . . ?
C51 C50 C49 116.4(14) . . ?
C51 C50 H50 121.8 . . ?
C49 C50 H50 121.8 . . ?
N21 C51 C50 121.9(13) . . ?
N21 C51 N22 117.4(13) . . ?
C50 C51 N22 120.6(14) . . ?
N20 C52 N21 126.5(15) . . ?
N20 C52 C53 116.0(13) . . ?
N21 C52 C53 117.5(14) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N22 C54 H54A 109.5 . . ?
N22 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
N22 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N23 C55 C56 118.9(14) . . ?
N23 C55 H55 120.6 . . ?
C56 C55 H55 120.6 . . ?
N24 C56 C57 120.2(13) . . ?
N24 C56 C55 119.6(12) . . ?
C57 C56 C55 120.2(13) . . ?
C56 C57 C58 119.5(14) . . ?
C56 C57 H57 120.3 . . ?
C58 C57 H57 120.3 . . ?
N25 C58 C57 121.8(13) . . ?
N25 C58 C66 119.4(12) . . ?
C57 C58 C66 118.8(13) . . ?
N24 C59 N25 124.3(13) . . ?
N24 C59 C60 119.9(12) . . ?
N25 C59 C60 115.8(12) . . ?
C61 C60 C65 120.7(14) . . ?
C61 C60 C59 118.0(13) . . ?
C65 C60 C59 121.3(13) . . ?
C60 C61 C62 119.0(14) . . ?
C60 C61 H61 120.5 . . ?
C62 C61 H61 120.5 . . ?
C63 C62 C61 120.3(15) . . ?
C63 C62 H62 119.9 . . ?
C61 C62 H62 119.9 . . ?
C62 C63 C64 120.7(15) . . ?
C62 C63 H63 119.7 . . ?
C64 C63 H63 119.7 . . ?
C65 C64 C63 119.6(15) . . ?
C65 C64 H64 120.2 . . ?
C63 C64 H64 120.2 . . ?
C64 C65 C60 119.8(15) . . ?
C64 C65 H65 120.1 . . ?
C60 C65 H65 120.1 . . ?
N26 C66 C58 118.4(13) . . ?
N26 C66 H66 120.8 . . ?
C58 C66 H66 120.8 . . ?
N27 C67 H67A 109.5 . . ?
N27 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
N27 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N28 C68 C69 122.6(13) . . ?
N28 C68 N27 117.5(12) . . ?
C69 C68 N27 119.9(13) . . ?
C68 C69 C70 116.9(13) . . ?
C68 C69 H69 121.6 . . ?
C70 C69 H69 121.6 . . ?
N29 C70 N30 119.6(12) . . ?
N29 C70 C69 120.7(13) . . ?
N30 C70 C69 119.7(13) . . ?
N29 C71 N28 125.5(13) . . ?
N29 C71 C72 117.8(13) . . ?
N28 C71 C72 116.7(12) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N30 C73 H73A 109.5 . . ?
N30 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
N30 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N31 C74 C75 119.8(14) . . ?
N31 C74 H74 120.1 . . ?
C75 C74 H74 120.1 . . ?
N32 C75 C76 122.4(13) . . ?
N32 C75 C74 116.9(13) . . ?
C76 C75 C74 120.4(14) . . ?
C75 C76 C77 118.8(15) . . ?
C75 C76 H76 120.6 . . ?
C77 C76 H76 120.6 . . ?
C78 C77 C76 119.2(14) . . ?
C78 C77 H77 120.4 . . ?
C76 C77 H77 120.4 . . ?
C77 C78 C79 119.8(14) . . ?
C77 C78 H78 120.1 . . ?
C79 C78 H78 120.1 . . ?
N32 C79 C78 121.7(14) . . ?
N32 C79 C80 117.2(13) . . ?
C78 C79 C80 120.9(13) . . ?
O4 C80 C79 111.0(12) . . ?
O4 C80 H80A 109.4 . . ?
C79 C80 H80A 109.4 . . ?
O4 C80 H80B 109.4 . . ?
C79 C80 H80B 109.4 . . ?
H80A C80 H80B 108.0 . . ?
F11 C81 F13 108(2) . . ?
F11 C81 F12 104.9(17) . . ?
F13 C81 F12 110(2) . . ?
F11 C81 S1 111.5(16) . . ?
F13 C81 S1 111.1(14) . . ?
F12 C81 S1 111.1(18) . . ?
F23 C82 F22 108.3(14) . . ?
F23 C82 F21 109.2(15) . . ?
F22 C82 F21 109.5(16) . . ?
F23 C82 S2 110.5(13) . . ?
F22 C82 S2 110.8(12) . . ?
F21 C82 S2 108.6(12) . . ?
F32 C83 F33 110.2(18) . . ?
F32 C83 F31 106.2(17) . . ?
F33 C83 F31 107.7(15) . . ?
F32 C83 S3 112.4(13) . . ?
F33 C83 S3 112.6(12) . . ?
F31 C83 S3 107.4(15) . . ?
F42 C84 F41 108(2) . . ?
F42 C84 F43 111(2) . . ?
F41 C84 F43 109(2) . . ?
F42 C84 S4 109.7(16) . . ?
F41 C84 S4 110.9(15) . . ?
F43 C84 S4 108.3(17) . . ?
F53 C85 F51 107.6(14) . . ?
F53 C85 F54 108.2(14) . . ?
F51 C85 F54 106.8(14) . . ?
F53 C85 S5 113.1(11) . . ?
F51 C85 S5 110.7(11) . . ?
F54 C85 S5 110.2(11) . . ?
F62 C86 F63 107.0(15) . . ?
F62 C86 F61 108.5(17) . . ?
F63 C86 F61 107.5(17) . . ?
F62 C86 S6 111.0(15) . . ?
F63 C86 S6 111.5(14) . . ?
F61 C86 S6 111.1(12) . . ?
F73 C87 F72 109.4(16) . . ?
F73 C87 F71 107.7(16) . . ?
F72 C87 F71 108.0(15) . . ?
F73 C87 S7 109.7(13) . . ?
F72 C87 S7 112.4(13) . . ?
F71 C87 S7 109.5(13) . . ?
F83 C88 F82 107.4(13) . . ?
F83 C88 F81 108.8(14) . . ?
F82 C88 F81 107.1(13) . . ?
F83 C88 S8 112.2(11) . . ?
F82 C88 S8 110.6(12) . . ?
F81 C88 S8 110.5(11) . . ?
F91 C89 F92 105.3(16) . . ?
F91 C89 F93 105.6(17) . . ?
F92 C89 F93 109.2(17) . . ?
F91 C89 S9 113.7(14) . . ?
F92 C89 S9 111.7(13) . . ?
F93 C89 S9 110.9(13) . . ?
F103 C90 F102 108.4(18) . . ?
F103 C90 F101 109.0(16) . . ?
F102 C90 F101 107.8(18) . . ?
F103 C90 S10 111.5(15) . . ?
F102 C90 S10 109.8(13) . . ?
F101 C90 S10 110.3(15) . . ?
F112 C91 F111 109.7(17) . . ?
F112 C91 F113 109.7(17) . . ?
F111 C91 F113 107.3(16) . . ?
F112 C91 S11 111.3(14) . . ?
F111 C91 S11 110.6(14) . . ?
F113 C91 S11 108.1(14) . . ?
F121 C92 F123 109.3(15) . . ?
F121 C92 F122 107.9(15) . . ?
F123 C92 F122 106.9(15) . . ?
F121 C92 S12 110.3(13) . . ?
F123 C92 S12 111.7(13) . . ?
F122 C92 S12 110.6(13) . . ?
F133 C93 F132 103(3) . . ?
F133 C93 F131 100(3) . . ?
F132 C93 F131 113(3) . . ?
F133 C93 S13 115(3) . . ?
F132 C93 S13 116(2) . . ?
F131 C93 S13 109(2) . . ?
F143 C94 F142 120(3) . . ?
F143 C94 F141 106(3) . . ?
F142 C94 F141 100(3) . . ?
F143 C94 S14 104(3) . . ?
F142 C94 S14 115(2) . . ?
F141 C94 S14 112(3) . . ?
F153 C95 S15 131(3) . . ?
F153 C95 F151 100(2) . . ?
S15 C95 F151 112(2) . . ?
F153 C95 F152 101(2) . . ?
S15 C95 F152 115(2) . . ?
F151 C95 F152 90(2) . . ?
F161 C96 F162 104(3) . . ?
F161 C96 F163 108(2) . . ?
F162 C96 F163 98(2) . . ?
F161 C96 S16 119(2) . . ?
F162 C96 S16 116(2) . . ?
F163 C96 S16 109.4(19) . . ?
N33 C97 C98 177.5(18) . . ?
C97 C98 H98A 109.5 . . ?
C97 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C97 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N34 C99 C100 178(2) . . ?
C99 C100 H10A 109.5 . . ?
C99 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C99 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
N35 C101 C102 180(3) . . ?
C101 C102 H10D 109.5 . . ?
C101 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
C101 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
N36 C103 C104 179(2) . . ?
C103 C104 H10G 109.5 . . ?
C103 C104 H10H 109.5 . . ?
H10G C104 H10H 109.5 . . ?
C103 C104 H10I 109.5 . . ?
H10G C104 H10I 109.5 . . ?
H10H C104 H10I 109.5 . . ?
N37 C105 C106 179(2) . . ?
C105 C106 H10J 109.5 . . ?
C105 C106 H10K 109.5 . . ?
H10J C106 H10K 109.5 . . ?
C105 C106 H10L 109.5 . . ?
H10J C106 H10L 109.5 . . ?
H10K C106 H10L 109.5 . . ?
N38 C107 C108 180(3) . . ?
C107 C108 H10M 109.5 . . ?
C107 C108 H10N 109.5 . . ?
H10M C108 H10N 109.5 . . ?
C107 C108 H10O 109.5 . . ?
H10M C108 H10O 109.5 . . ?
H10N C108 H10O 109.5 . . ?
N39 C109 C110 178(2) . . ?
C109 C110 H11A 109.5 . . ?
C109 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C109 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
C6 N1 C2 119.0(12) . . ?
C6 N1 Pb1 119.1(9) . . ?
C2 N1 Pb1 121.8(10) . . ?
C7 N2 N3 117.7(13) . . ?
C7 N2 Pb1 118.3(10) . . ?
N3 N2 Pb1 123.5(9) . . ?
C9 N3 N2 115.7(13) . . ?
C9 N3 C8 123.7(12) . . ?
N2 N3 C8 120.6(12) . . ?
C9 N4 C12 117.7(12) . . ?
C9 N4 Pb1 120.0(9) . . ?
C12 N4 Pb1 119.8(9) . . ?
C12 N5 C11 115.8(13) . . ?
C12 N5 Pb2 123.5(10) . . ?
C11 N5 Pb2 120.5(9) . . ?
N7 N6 C11 116.8(12) . . ?
N7 N6 C14 120.5(11) . . ?
C11 N6 C14 122.7(12) . . ?
C15 N7 N6 118.5(13) . . ?
C15 N7 Pb2 120.1(10) . . ?
N6 N7 Pb2 121.4(8) . . ?
C19 N8 C16 119.0(12) . . ?
C19 N8 Pb2 127.6(10) . . ?
C16 N8 Pb2 112.7(9) . . ?
C18 N9 C19 117.0(12) . . ?
C18 N9 Pb3 111.6(9) . . ?
C19 N9 Pb3 125.7(9) . . ?
C26 N10 N11 117.9(12) . . ?
C26 N10 Pb3 119.2(9) . . ?
N11 N10 Pb3 122.3(8) . . ?
N10 N11 C28 116.5(11) . . ?
N10 N11 C27 119.5(11) . . ?
C28 N11 C27 124.0(12) . . ?
C28 N12 C31 117.6(12) . . ?
C28 N12 Pb3 121.3(9) . . ?
C31 N12 Pb3 121.2(9) . . ?
C30 N13 C31 116.6(12) . . ?
C30 N13 Pb4 116.0(9) . . ?
C31 N13 Pb4 124.5(9) . . ?
N15 N14 C30 117.4(12) . . ?
N15 N14 C33 119.7(11) . . ?
C30 N14 C33 122.8(12) . . ?
C34 N15 N14 118.0(13) . . ?
C34 N15 Pb4 117.1(10) . . ?
N14 N15 Pb4 124.1(8) . . ?
C39 N16 C35 119.1(13) . . ?
C39 N16 Pb4 121.9(11) . . ?
C35 N16 Pb4 118.4(9) . . ?
C46 N17 C42 119.4(15) . . ?
C46 N17 Pb5 119.4(10) . . ?
C42 N17 Pb5 121.0(13) . . ?
C47 N18 N19 119.1(14) . . ?
C47 N18 Pb5 116.5(11) . . ?
N19 N18 Pb5 122.6(10) . . ?
N18 N19 C49 115.8(13) . . ?
N18 N19 C48 120.7(12) . . ?
C49 N19 C48 123.4(13) . . ?
C52 N20 C49 116.6(12) . . ?
C52 N20 Pb5 121.2(10) . . ?
C49 N20 Pb5 118.2(9) . . ?
C52 N21 C51 116.2(13) . . ?
C52 N21 Pb6 123.0(10) . . ?
C51 N21 Pb6 120.2(9) . . ?
N23 N22 C51 116.1(12) . . ?
N23 N22 C54 121.5(12) . . ?
C51 N22 C54 122.3(13) . . ?
C55 N23 N22 116.9(13) . . ?
C55 N23 Pb6 121.1(10) . . ?
N22 N23 Pb6 122.0(8) . . ?
C59 N24 C56 118.1(12) . . ?
C59 N24 Pb6 127.2(9) . . ?
C56 N24 Pb6 112.4(9) . . ?
C58 N25 C59 116.2(12) . . ?
C58 N25 Pb7 114.9(9) . . ?
C59 N25 Pb7 125.4(9) . . ?
C66 N26 N27 117.2(12) . . ?
C66 N26 Pb7 122.0(9) . . ?
N27 N26 Pb7 120.5(8) . . ?
N26 N27 C68 117.2(11) . . ?
N26 N27 C67 119.8(11) . . ?
C68 N27 C67 123.0(11) . . ?
C71 N28 C68 116.2(12) . . ?
C71 N28 Pb7 122.1(9) . . ?
C68 N28 Pb7 121.7(9) . . ?
C71 N29 C70 117.9(12) . . ?
C71 N29 Pb8 125.4(10) . . ?
C70 N29 Pb8 113.9(9) . . ?
C70 N30 N31 117.1(11) . . ?
C70 N30 C73 123.1(12) . . ?
N31 N30 C73 119.6(11) . . ?
C74 N31 N30 117.5(12) . . ?
C74 N31 Pb8 117.6(9) . . ?
N30 N31 Pb8 124.2(8) . . ?
C75 N32 C79 117.9(12) . . ?
C75 N32 Pb8 116.4(9) . . ?
C79 N32 Pb8 124.2(10) . . ?
C101 N35 Pb7 164.4(18) . . ?
C1 O1 Pb1 120.9(9) . . ?
C1 O1 H1 119.6 . . ?
Pb1 O1 H1 119.6 . . ?
C40 O2 Pb4 123.1(12) . . ?
C40 O2 H2 118.5 . . ?
Pb4 O2 H2 118.5 . . ?
C41 O3 Pb5 122.8(11) . . ?
C41 O3 H3A 118.6 . . ?
Pb5 O3 H3A 118.6 . . ?
C80 O4 Pb8 121.6(9) . . ?
C80 O4 H4A 119.2 . . ?
Pb8 O4 H4A 119.2 . . ?
S1 O11 Pb1 137.9(7) . . ?
S2 O21 Pb2 132.1(7) . . ?
S3 O31 Pb3 115.9(8) . . ?
S4 O41 Pb3 139.5(7) . . ?
S5 O52 Pb4 137.2(6) . . ?
S6 O61 Pb5 137.7(7) . . ?
S7 O71 Pb7 148.0(7) . . ?
S8 O81 Pb8 138.8(6) . . ?
S9 O92 Pb2 110.3(11) . . ?
S10 O103 Pb4 105.9(5) . . ?
S11 O113 Pb8 110.9(5) . . ?
S12 O121 Pb1 109.3(6) . . ?
S13 O131 Pb6 113.3(9) . . ?
S14 O141 Pb5 111.2(9) . . ?
S15 O151 Pb6 156.2(13) . . ?
O13 S1 O11 113.7(8) . . ?
O13 S1 O12 116.8(10) . . ?
O11 S1 O12 114.0(9) . . ?
O13 S1 C81 104.9(11) . . ?
O11 S1 C81 101.4(9) . . ?
O12 S1 C81 103.7(11) . . ?
O22 S2 O21 114.4(7) . . ?
O22 S2 O23 115.4(7) . . ?
O21 S2 O23 114.1(8) . . ?
O22 S2 C82 102.6(7) . . ?
O21 S2 C82 103.7(8) . . ?
O23 S2 C82 104.5(8) . . ?
O32 S3 O33 118.3(10) . . ?
O32 S3 O31 113.1(9) . . ?
O33 S3 O31 113.3(9) . . ?
O32 S3 C83 104.6(9) . . ?
O33 S3 C83 103.2(10) . . ?
O31 S3 C83 101.9(8) . . ?
O43 S4 O42 116.9(8) . . ?
O43 S4 O41 114.5(9) . . ?
O42 S4 O41 113.4(8) . . ?
O43 S4 C84 104.0(11) . . ?
O42 S4 C84 103.3(9) . . ?
O41 S4 C84 102.2(9) . . ?
O53 S5 O54 115.7(7) . . ?
O53 S5 O52 114.9(6) . . ?
O54 S5 O52 113.0(6) . . ?
O53 S5 C85 104.7(7) . . ?
O54 S5 C85 103.9(7) . . ?
O52 S5 C85 102.6(7) . . ?
O62 S6 O63 117.1(8) . . ?
O62 S6 O61 114.3(8) . . ?
O63 S6 O61 113.6(7) . . ?
O62 S6 C86 105.3(9) . . ?
O63 S6 C86 103.0(8) . . ?
O61 S6 C86 101.0(8) . . ?
O72 S7 O73 117.5(7) . . ?
O72 S7 O71 113.8(7) . . ?
O73 S7 O71 113.0(7) . . ?
O72 S7 C87 102.5(9) . . ?
O73 S7 C87 103.6(8) . . ?
O71 S7 C87 104.2(7) . . ?
O83 S8 O82 115.8(6) . . ?
O83 S8 O81 115.4(6) . . ?
O82 S8 O81 112.5(6) . . ?
O83 S8 C88 104.4(7) . . ?
O82 S8 C88 104.2(7) . . ?
O81 S8 C88 102.5(7) . . ?
O93 S9 O91 117.5(12) . . ?
O93 S9 O92 111.1(13) . . ?
O91 S9 O92 115.4(11) . . ?
O93 S9 C89 102.9(10) . . ?
O91 S9 C89 105.0(8) . . ?
O92 S9 C89 102.8(11) . . ?
O101 S10 O103 114.8(7) . . ?
O101 S10 O102 116.4(7) . . ?
O103 S10 O102 112.5(7) . . ?
O101 S10 C90 103.3(8) . . ?
O103 S10 C90 103.9(9) . . ?
O102 S10 C90 103.8(9) . . ?
O111 S11 O113 114.7(7) . . ?
O111 S11 O112 116.9(8) . . ?
O113 S11 O112 113.7(7) . . ?
O111 S11 C91 103.0(8) . . ?
O113 S11 C91 103.3(9) . . ?
O112 S11 C91 102.7(8) . . ?
O121 S12 O123 116.1(8) . . ?
O121 S12 O122 112.2(7) . . ?
O123 S12 O122 115.4(7) . . ?
O121 S12 C92 102.9(8) . . ?
O123 S12 C92 103.6(8) . . ?
O122 S12 C92 104.6(9) . . ?
O133 S13 O131 109.1(11) . . ?
O133 S13 O132 116.3(11) . . ?
O131 S13 O132 116.8(10) . . ?
O133 S13 C93 98.9(15) . . ?
O131 S13 C93 109.4(14) . . ?
O132 S13 C93 104.4(11) . . ?
O141 S14 O143 107.6(11) . . ?
O141 S14 O142 111.1(10) . . ?
O143 S14 O142 109.9(11) . . ?
O141 S14 C94 112.2(14) . . ?
O143 S14 C94 110.8(17) . . ?
O142 S14 C94 105.2(14) . . ?
O151 S15 O152 112.5(11) . . ?
O151 S15 C95 112.2(14) . . ?
O152 S15 C95 107.0(13) . . ?
O151 S15 O153 105.2(11) . . ?
O152 S15 O153 121.6(11) . . ?
C95 S15 O153 97.4(14) . . ?
O163 S16 O161 121.0(13) . . ?
O163 S16 O162 112.1(11) . . ?
O161 S16 O162 110.3(11) . . ?
O163 S16 C96 102.0(11) . . ?
O161 S16 C96 108.2(14) . . ?
O162 S16 C96 100.9(13) . . ?
O11 Pb1 N1 82.8(4) . . ?
O11 Pb1 O1 81.1(4) . . ?
N1 Pb1 O1 64.6(4) . . ?
O11 Pb1 N2 93.1(4) . . ?
N1 Pb1 N2 64.7(4) . . ?
O1 Pb1 N2 129.3(4) . . ?
O11 Pb1 O121 161.7(4) . . ?
N1 Pb1 O121 79.6(4) . . ?
O1 Pb1 O121 86.7(4) . . ?
N2 Pb1 O121 84.0(4) . . ?
O11 Pb1 N4 83.3(4) . . ?
N1 Pb1 N4 119.5(4) . . ?
O1 Pb1 N4 163.3(4) . . ?
N2 Pb1 N4 57.7(4) . . ?
O121 Pb1 N4 109.9(4) . . ?
O21 Pb2 N7 73.6(4) . . ?
O21 Pb2 N5 89.4(4) . . ?
N7 Pb2 N5 63.5(4) . . ?
O21 Pb2 N8 74.8(4) . . ?
N7 Pb2 N8 65.5(4) . . ?
N5 Pb2 N8 129.0(4) . . ?
O21 Pb2 O92 153.5(5) . . ?
N7 Pb2 O92 94.9(5) . . ?
N5 Pb2 O92 107.1(5) . . ?
N8 Pb2 O92 78.7(5) . . ?
O41 Pb3 N10 83.7(4) . . ?
O41 Pb3 N12 80.4(4) . . ?
N10 Pb3 N12 61.9(4) . . ?
O41 Pb3 O31 153.7(4) . . ?
N10 Pb3 O31 70.1(4) . . ?
N12 Pb3 O31 88.6(4) . . ?
O41 Pb3 N9 88.0(4) . . ?
N10 Pb3 N9 65.0(4) . . ?
N12 Pb3 N9 126.5(4) . . ?
O31 Pb3 N9 79.4(4) . . ?
O52 Pb4 N16 86.3(4) . . ?
O52 Pb4 O2 87.9(4) . . ?
N16 Pb4 O2 63.4(5) . . ?
O52 Pb4 N15 82.3(4) . . ?
N16 Pb4 N15 64.6(4) . . ?
O2 Pb4 N15 127.5(5) . . ?
O52 Pb4 O103 157.1(3) . . ?
N16 Pb4 O103 72.4(4) . . ?
O2 Pb4 O103 89.7(4) . . ?
N15 Pb4 O103 81.1(4) . . ?
O52 Pb4 N13 73.6(4) . . ?
N16 Pb4 N13 122.6(4) . . ?
O2 Pb4 N13 159.5(4) . . ?
N15 Pb4 N13 59.9(4) . . ?
O103 Pb4 N13 110.8(3) . . ?
O61 Pb5 N17 82.5(4) . . ?
O61 Pb5 O3 78.0(4) . . ?
N17 Pb5 O3 64.8(5) . . ?
O61 Pb5 N18 90.4(4) . . ?
N17 Pb5 N18 64.8(4) . . ?
O3 Pb5 N18 129.3(4) . . ?
O61 Pb5 N20 80.6(4) . . ?
N17 Pb5 N20 119.7(5) . . ?
O3 Pb5 N20 157.4(4) . . ?
N18 Pb5 N20 57.8(4) . . ?
O61 Pb5 O141 152.2(4) . . ?
N17 Pb5 O141 71.9(5) . . ?
O3 Pb5 O141 99.9(5) . . ?
N18 Pb5 O141 69.3(4) . . ?
N20 Pb5 O141 102.5(4) . . ?
O151 Pb6 N23 77.0(6) . . ?
O151 Pb6 N21 82.6(6) . . ?
N23 Pb6 N21 63.3(4) . . ?
O151 Pb6 N24 83.2(6) . . ?
N23 Pb6 N24 65.9(4) . . ?
N21 Pb6 N24 129.1(4) . . ?
O151 Pb6 O131 154.8(6) . . ?
N23 Pb6 O131 84.8(5) . . ?
N21 Pb6 O131 104.7(5) . . ?
N24 Pb6 O131 73.6(5) . . ?
O71 Pb7 N26 74.7(4) . . ?
O71 Pb7 N28 88.8(4) . . ?
N26 Pb7 N28 61.7(3) . . ?
O71 Pb7 N25 78.7(4) . . ?
N26 Pb7 N25 62.9(4) . . ?
N28 Pb7 N25 124.5(4) . . ?
O71 Pb7 N35 68.0(4) . . ?
N26 Pb7 N35 136.8(5) . . ?
N28 Pb7 N35 95.9(5) . . ?
N25 Pb7 N35 126.7(5) . . ?
O81 Pb8 N31 81.9(3) . . ?
O81 Pb8 N32 86.0(4) . . ?
N31 Pb8 N32 65.3(4) . . ?
O81 Pb8 O4 87.4(3) . . ?
N31 Pb8 O4 127.3(3) . . ?
N32 Pb8 O4 62.6(4) . . ?
O81 Pb8 O113 156.3(3) . . ?
N31 Pb8 O113 79.4(3) . . ?
N32 Pb8 O113 73.0(4) . . ?
O4 Pb8 O113 92.4(3) . . ?
O81 Pb8 N29 74.7(4) . . ?
N31 Pb8 N29 61.3(4) . . ?
N32 Pb8 N29 125.0(4) . . ?
O4 Pb8 N29 159.2(4) . . ?
O113 Pb8 N29 108.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         14.631
_refine_diff_density_min         -3.372
_refine_diff_density_rms         0.295
_database_code_depnum_ccdc_archive 'CCDC 976901'
#######################################################################
#
#                 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_3(sdjh878)

# start Validation Reply Form
_vrf_PLAT415_3sdjh878            
;
PROBLEM: Short Inter D-H..H-X       H2     ..  H46B    ..       1.77 Ang.  
RESPONSE: A CH3CN molecule resides in close proximity to the hydroxymethyl
arm containing H2.
;
_vrf_PLAT213_3sdjh878            
;
PROBLEM: Atom O14             has ADP max/min Ratio .....        4.6 oblate
RESPONSE: Disordered ClO4- anion. See _refine_special_details
;
_vrf_PLAT220_3sdjh878            
;
PROBLEM: Large Non-Solvent    O     Ueq(max)/Ueq(min) ...        4.2 Ratio 
RESPONSE: Disordered ClO4- anion. See _refine_special_details
;
_vrf_PLAT306_3sdjh878            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O4 Check 
RESPONSE: The H atoms of O4 could not be located as there was no residual
electron density within 1.2 A of O4
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C42 H45 Cl4 N17 O19 Pb2), C4 H10 O, 4(C2 H3 N), 2(O)'
_chemical_formula_sum            'C96 H112 Cl8 N38 O41 Pb4'
_chemical_formula_weight         3566.64

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'
Cl Cl 0.1484 0.1585 '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                   29.752(3)
_cell_length_b                   10.5359(9)
_cell_length_c                   44.383(4)
_cell_angle_alpha                90.000
_cell_angle_beta                 109.239(3)
_cell_angle_gamma                90.000
_cell_volume                     13135(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.58

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.07
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6984
_exptl_absorpt_coefficient_mu    5.368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43553
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         25.69
_reflns_number_total             12429
_reflns_number_gt                10521
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

Some of the components of complex 3 showed large thermal ellipsoids due to
disorder including two of the ClO4- anions and one of the terminal pyridine 
rings. The worst ellipsoids were restrained with ISOR restraints. The disorder
was not modelled further. 
;

_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)+(0.0340P)²+424.2833P] 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         12429
_refine_ls_number_parameters     900
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1493
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_restrained_S_all      1.235
_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
C1 C 0.1765(4) 0.9718(15) 0.9475(3) 0.041(3) Uani 1 1 d . . .
H1A H 0.1772 0.9175 0.9652 0.049 Uiso 1 1 calc R . .
H1B H 0.1725 1.0586 0.9534 0.049 Uiso 1 1 calc R . .
C2 C 0.2230(4) 0.9605(10) 0.9414(3) 0.024(2) Uani 1 1 d . . .
C3 C 0.2653(4) 0.9832(11) 0.9659(3) 0.029(3) Uani 1 1 d . . .
H3 H 0.2651 1.0022 0.9863 0.035 Uiso 1 1 calc R . .
C4 C 0.3078(4) 0.9773(12) 0.9597(3) 0.032(3) Uani 1 1 d . . .
H4 H 0.3366 0.9867 0.9761 0.038 Uiso 1 1 calc R . .
C5 C 0.3069(4) 0.9572(10) 0.9287(3) 0.022(2) Uani 1 1 d . . .
H5 H 0.3349 0.9590 0.9237 0.027 Uiso 1 1 calc R . .
C6 C 0.2630(4) 0.9340(10) 0.9049(3) 0.021(2) Uani 1 1 d . . .
C7 C 0.2611(4) 0.9154(10) 0.8718(3) 0.021(2) Uani 1 1 d . . .
H7 H 0.2888 0.9168 0.8665 0.025 Uiso 1 1 calc R . .
C8 C 0.2626(4) 0.8854(11) 0.8118(3) 0.025(3) Uani 1 1 d . . .
H8A H 0.2740 0.9714 0.8141 0.037 Uiso 1 1 calc R . .
H8B H 0.2568 0.8581 0.7902 0.037 Uiso 1 1 calc R . .
H8C H 0.2861 0.8314 0.8260 0.037 Uiso 1 1 calc R . .
C9 C 0.1740(4) 0.8602(10) 0.7964(3) 0.021(2) Uani 1 1 d . . .
C10 C 0.1690(4) 0.8394(9) 0.7648(3) 0.018(2) Uani 1 1 d . . .
H10 H 0.1950 0.8323 0.7577 0.021 Uiso 1 1 calc R . .
C11 C 0.1226(4) 0.8299(10) 0.7442(3) 0.022(2) Uani 1 1 d . . .
C12 C 0.0933(4) 0.8579(10) 0.7849(2) 0.020(2) Uani 1 1 d . . .
C13 C 0.0513(4) 0.8701(13) 0.7966(2) 0.028(3) Uani 1 1 d . . .
H13A H 0.0228 0.8818 0.7787 0.042 Uiso 1 1 calc R . .
H13B H 0.0559 0.9418 0.8106 0.042 Uiso 1 1 calc R . .
H13C H 0.0485 0.7944 0.8078 0.042 Uiso 1 1 calc R . .
C14 C 0.0632(4) 0.7957(12) 0.6892(3) 0.027(3) Uani 1 1 d . . .
H14A H 0.0593 0.8535 0.6718 0.041 Uiso 1 1 calc R . .
H14B H 0.0407 0.8161 0.6997 0.041 Uiso 1 1 calc R . .
H14C H 0.0578 0.7105 0.6811 0.041 Uiso 1 1 calc R . .
C15 C 0.1437(4) 0.7769(10) 0.6725(2) 0.017(2) Uani 1 1 d . . .
H15 H 0.1133 0.7780 0.6576 0.020 Uiso 1 1 calc R . .
C16 C 0.1860(4) 0.7572(10) 0.6625(3) 0.023(2) Uani 1 1 d . . .
C17 C 0.2295(4) 0.7279(10) 0.6842(3) 0.024(2) Uani 1 1 d . . .
H17 H 0.2336 0.7165 0.7057 0.029 Uiso 1 1 calc R . .
C18 C 0.2674(4) 0.7159(10) 0.6725(2) 0.020(2) Uani 1 1 d . . .
C19 C 0.2191(4) 0.7590(10) 0.6228(2) 0.023(3) Uani 1 1 d . . .
C20 C 0.2142(4) 0.7796(10) 0.5885(2) 0.019(2) Uani 1 1 d . . .
C21 C 0.1693(4) 0.7770(11) 0.5644(3) 0.028(3) Uani 1 1 d . . .
H21 H 0.1419 0.7638 0.5696 0.034 Uiso 1 1 calc R . .
C22 C 0.1661(4) 0.7940(11) 0.5330(3) 0.030(3) Uani 1 1 d . . .
H22 H 0.1363 0.7920 0.5173 0.035 Uiso 1 1 calc R . .
C23 C 0.2057(5) 0.8140(12) 0.5243(3) 0.037(3) Uani 1 1 d . . .
H23 H 0.2027 0.8262 0.5030 0.045 Uiso 1 1 calc R . .
C24 C 0.2507(5) 0.8157(12) 0.5479(3) 0.032(3) Uani 1 1 d . . .
H24 H 0.2779 0.8270 0.5422 0.039 Uiso 1 1 calc R . .
C25 C 0.2543(4) 0.8004(12) 0.5798(3) 0.029(3) Uani 1 1 d . . .
H25 H 0.2841 0.8041 0.5955 0.035 Uiso 1 1 calc R . .
C26 C 0.3172(4) 0.6970(10) 0.6938(3) 0.021(2) Uani 1 1 d . . .
H26 H 0.3422 0.7023 0.6857 0.025 Uiso 1 1 calc R . .
C27 C 0.4122(4) 0.6831(12) 0.7311(3) 0.031(3) Uani 1 1 d . . .
H27A H 0.4110 0.6239 0.7144 0.047 Uiso 1 1 calc R . .
H27B H 0.4415 0.6721 0.7484 0.047 Uiso 1 1 calc R . .
H27C H 0.4105 0.7681 0.7230 0.047 Uiso 1 1 calc R . .
C28 C 0.3785(4) 0.6402(10) 0.7744(3) 0.021(2) Uani 1 1 d . . .
C29 C 0.3409(4) 0.6190(10) 0.7864(2) 0.020(2) Uani 1 1 d . . .
H29 H 0.3094 0.6153 0.7731 0.024 Uiso 1 1 calc R . .
C30 C 0.3531(4) 0.6040(10) 0.8189(3) 0.020(2) Uani 1 1 d . . .
C31 C 0.4321(4) 0.6239(10) 0.8246(3) 0.021(2) Uani 1 1 d . . .
C32 C 0.4832(4) 0.6283(12) 0.8461(3) 0.030(3) Uani 1 1 d . . .
H32A H 0.5037 0.6131 0.8337 0.045 Uiso 1 1 calc R . .
H32B H 0.4884 0.5643 0.8623 0.045 Uiso 1 1 calc R . .
H32C H 0.4899 0.7104 0.8560 0.045 Uiso 1 1 calc R . .
C33 C 0.2699(4) 0.5539(10) 0.8157(3) 0.020(2) Uani 1 1 d . . .
H33A H 0.2588 0.4871 0.8261 0.031 Uiso 1 1 calc R . .
H33B H 0.2677 0.5272 0.7946 0.031 Uiso 1 1 calc R . .
H33C H 0.2507 0.6283 0.8144 0.031 Uiso 1 1 calc R . .
C34 C 0.3014(4) 0.5964(10) 0.8800(3) 0.024(2) Uani 1 1 d . . .
H34 H 0.2695 0.5809 0.8686 0.029 Uiso 1 1 calc R . .
C35 C 0.3165(4) 0.6179(10) 0.9145(2) 0.019(2) Uani 1 1 d . . .
C36 C 0.2824(4) 0.6190(10) 0.9297(3) 0.025(3) Uani 1 1 d . . .
H36 H 0.2506 0.6018 0.9185 0.030 Uiso 1 1 calc R . .
C37 C 0.2970(4) 0.6463(11) 0.9621(3) 0.028(3) Uani 1 1 d . . .
H37 H 0.2751 0.6484 0.9730 0.034 Uiso 1 1 calc R . .
C38 C 0.3447(4) 0.6707(12) 0.9778(3) 0.030(3) Uani 1 1 d . . .
H38 H 0.3553 0.6904 0.9995 0.036 Uiso 1 1 calc R . .
C39 C 0.3760(4) 0.6653(11) 0.9614(3) 0.025(2) Uani 1 1 d . . .
C40 C 0.4283(4) 0.6922(13) 0.9779(3) 0.033(3) Uani 1 1 d . . .
H40A H 0.4325 0.7406 0.9972 0.040 Uiso 1 1 calc R . .
H40B H 0.4456 0.6129 0.9838 0.040 Uiso 1 1 calc R . .
C41 C 0.1146(5) 1.1764(15) 0.8731(4) 0.048(4) Uani 1 1 d . . .
C42 C 0.1041(5) 1.2757(15) 0.8920(4) 0.056(4) Uani 1 1 d . . .
H42A H 0.1132 1.2490 0.9138 0.084 Uiso 1 1 calc R . .
H42B H 0.0706 1.2937 0.8842 0.084 Uiso 1 1 calc R . .
H42C H 0.1216 1.3507 0.8905 0.084 Uiso 1 1 calc R . .
C43 C 0.1676(5) 0.4988(15) 0.7380(3) 0.043(3) Uani 1 1 d . . .
C44 C 0.1173(4) 0.4848(12) 0.7308(3) 0.035(3) Uani 1 1 d . . .
H44A H 0.1069 0.5365 0.7451 0.052 Uiso 1 1 calc R . .
H44B H 0.1100 0.3975 0.7333 0.052 Uiso 1 1 calc R . .
H44C H 0.1012 0.5110 0.7092 0.052 Uiso 1 1 calc R . .
C45 C 0.0547(5) 0.4618(16) 0.9901(5) 0.054(4) Uani 1 1 d . . .
C46 C 0.0396(7) 0.4297(18) 0.9575(4) 0.072(5) Uani 1 1 d . . .
H46A H 0.0230 0.5002 0.9451 0.108 Uiso 1 1 calc R . .
H46B H 0.0187 0.3576 0.9538 0.108 Uiso 1 1 calc R . .
H46C H 0.0668 0.4093 0.9514 0.108 Uiso 1 1 calc R . .
C47 C 0.9863(6) 0.4121(19) 0.6940(4) 0.071(5) Uani 1 1 d . . .
H47B H 1.0124 0.3534 0.6990 0.107 Uiso 1 1 calc R . .
H47A H 0.9860 0.4624 0.6759 0.107 Uiso 1 1 calc R . .
H47C H 0.9570 0.3660 0.6891 0.107 Uiso 1 1 calc R . .
C48 C 0.9919(5) 0.4971(17) 0.7220(5) 0.067(5) Uani 1 1 d . . .
H48A H 1.0184 0.5544 0.7245 0.081 Uiso 1 1 calc R . .
H48B H 0.9634 0.5477 0.7182 0.081 Uiso 1 1 calc R . .
N1 N 0.2220(3) 0.9375(8) 0.9116(2) 0.021(2) Uani 1 1 d . . .
N2 N 0.2209(3) 0.8972(8) 0.8504(2) 0.0188(19) Uani 1 1 d . . .
N3 N 0.2188(3) 0.8784(9) 0.8192(2) 0.021(2) Uani 1 1 d . . .
N4 N 0.1362(3) 0.8699(9) 0.8067(2) 0.021(2) Uani 1 1 d . . .
N5 N 0.0837(3) 0.8381(9) 0.7538(2) 0.021(2) Uani 1 1 d . . .
N6 N 0.1120(3) 0.8067(9) 0.7120(2) 0.021(2) Uani 1 1 d . . .
N7 N 0.1501(3) 0.7922(8) 0.7017(2) 0.021(2) Uani 1 1 d . . .
N8 N 0.1799(3) 0.7772(8) 0.6314(2) 0.0195(19) Uani 1 1 d . . .
N9 N 0.2625(3) 0.7318(8) 0.6418(2) 0.021(2) Uani 1 1 d . . .
N10 N 0.3256(3) 0.6732(8) 0.7237(2) 0.0191(19) Uani 1 1 d . . .
N11 N 0.3714(3) 0.6601(9) 0.7427(2) 0.025(2) Uani 1 1 d . . .
N12 N 0.4247(3) 0.6398(9) 0.7938(2) 0.023(2) Uani 1 1 d . . .
N13 N 0.3988(3) 0.6080(8) 0.8385(2) 0.020(2) Uani 1 1 d . . .
N14 N 0.3186(3) 0.5826(8) 0.8336(2) 0.0192(19) Uani 1 1 d . . .
N15 N 0.3324(3) 0.5992(8) 0.86579(19) 0.0150(18) Uani 1 1 d . . .
N16 N 0.3622(3) 0.6387(8) 0.9303(2) 0.0191(19) Uani 1 1 d . . .
N17 N 0.1273(5) 1.0933(11) 0.8594(3) 0.056(4) Uani 1 1 d . . .
N18 N 0.2072(5) 0.509(2) 0.7438(3) 0.093(7) Uani 1 1 d . . .
N19 N 0.0680(6) 0.4905(16) 1.0170(4) 0.079(5) Uani 1 1 d . . .
O1 O 0.1382(3) 0.9387(8) 0.92122(18) 0.032(2) Uani 1 1 d . . .
H1 H 0.1077 0.9488 0.9222 0.039 Uiso 1 1 calc R . .
O2 O 0.4470(3) 0.7624(12) 0.9571(2) 0.059(3) Uani 1 1 d . . .
H2 H 0.4649 0.8366 0.9620 0.071 Uiso 1 1 calc R . .
O3 O 0.4099(3) 0.4027(7) 0.90091(18) 0.0287(19) Uani 1 1 d . . .
O4 O 0.4581(6) 0.267(2) 0.9520(5) 0.161(9) Uani 1 1 d . . .
O5 O 1.0000 0.4274(15) 0.7500 0.063(4) Uani 1 2 d S . .
O11 O 0.1261(3) 0.3568(8) 0.6205(2) 0.038(2) Uani 1 1 d . . .
O12 O 0.0493(4) 0.3959(10) 0.6182(4) 0.075(4) Uani 1 1 d . . .
O13 O 0.1100(7) 0.4971(16) 0.6561(3) 0.121(6) Uani 1 1 d . . .
O14 O 0.0932(5) 0.5475(10) 0.6051(4) 0.089(5) Uani 1 1 d . . .
O21 O 0.1875(3) 1.6288(8) 0.85273(19) 0.0287(19) Uani 1 1 d . . .
O22 O 0.1464(4) 1.5484(11) 0.8022(2) 0.059(3) Uani 1 1 d . . .
O23 O 0.1528(3) 1.4263(8) 0.8481(2) 0.047(2) Uani 1 1 d . . .
O24 O 0.1041(3) 1.6096(8) 0.8361(2) 0.036(2) Uani 1 1 d . . .
O31 O 0.1926(4) 0.6728(15) 0.9675(3) 0.083(4) Uani 1 1 d . . .
O32 O 0.1518(5) 0.4868(11) 0.9516(3) 0.080(4) Uani 1 1 d . . .
O33 O 0.1103(3) 0.6806(9) 0.9470(2) 0.045(2) Uani 1 1 d . . .
O34 O 0.1568(4) 0.6358(10) 0.9138(2) 0.058(3) Uani 1 1 d . . .
Cl1 Cl 0.09479(11) 0.4510(3) 0.62510(8) 0.0363(7) Uani 1 1 d . . .
Cl2 Cl 0.14717(10) 1.5505(3) 0.83463(7) 0.0266(6) Uani 1 1 d . . .
Cl3 Cl 0.15113(12) 0.6162(3) 0.94381(8) 0.0380(8) Uani 1 1 d . . .
Pb1 Pb 0.147739(14) 0.84929(4) 0.869185(10) 0.02058(12) Uani 1 1 d . . .
Pb2 Pb 0.419969(14) 0.63680(4) 0.900280(10) 0.02103(12) Uani 1 1 d . . .
Cl4 Cl 0.0404(4) 0.0460(11) 0.9539(2) 0.037(2) Uani 0.55(2) 1 d P A 1
O41 O 0.0677(19) -0.061(5) 0.9525(12) 0.071(16) Uani 0.55(2) 1 d P A 1
O42 O 0.0375(11) 0.130(3) 0.9286(10) 0.056(9) Uani 0.55(2) 1 d P A 1
O43 O 0.0435(11) 0.093(4) 0.9830(8) 0.047(8) Uani 0.55(2) 1 d PU A 1
O44 O -0.0060(5) 0.0000(15) 0.9515(4) 0.041(5) Uani 0.55(2) 1 d P A 1
Cl4A Cl 0.0592(5) 0.0736(13) 0.9545(3) 0.032(3) Uani 0.45(2) 1 d P A 2
O41A O 0.074(2) -0.057(5) 0.9540(13) 0.037(12) Uani 0.45(2) 1 d PU A 2
O42A O 0.0223(11) 0.103(3) 0.9256(9) 0.031(8) Uani 0.45(2) 1 d PU A 2
O43A O 0.0577(14) 0.111(5) 0.9818(13) 0.061(13) Uani 0.45(2) 1 d PU A 2
O44A O 0.0994(6) 0.1571(19) 0.9588(5) 0.043(7) Uani 0.45(2) 1 d P A 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.379(14) . ?
C1 C2 1.498(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.332(14) . ?
C2 C3 1.387(16) . ?
C3 C4 1.380(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.405(15) . ?
C5 H5 0.9300 . ?
C6 N1 1.349(13) . ?
C6 C7 1.465(15) . ?
C7 N2 1.272(13) . ?
C7 H7 0.9300 . ?
C8 N3 1.448(13) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.353(13) . ?
C9 C10 1.376(15) . ?
C9 N3 1.398(14) . ?
C10 C11 1.383(15) . ?
C10 H10 0.9300 . ?
C11 N5 1.360(13) . ?
C11 N6 1.380(14) . ?
C12 N4 1.330(14) . ?
C12 N5 1.330(13) . ?
C12 C13 1.508(14) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N6 1.477(14) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N7 1.258(13) . ?
C15 C16 1.480(15) . ?
C15 H15 0.9300 . ?
C16 N8 1.351(13) . ?
C16 C17 1.369(16) . ?
C17 C18 1.392(15) . ?
C17 H17 0.9300 . ?
C18 N9 1.336(13) . ?
C18 C26 1.485(16) . ?
C19 N9 1.317(14) . ?
C19 N8 1.354(14) . ?
C19 C20 1.500(14) . ?
C20 C25 1.388(16) . ?
C20 C21 1.409(15) . ?
C21 C22 1.374(15) . ?
C21 H21 0.9300 . ?
C22 C23 1.372(18) . ?
C22 H22 0.9300 . ?
C23 C24 1.401(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.396(15) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 N10 1.292(13) . ?
C26 H26 0.9300 . ?
C27 N11 1.487(14) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N12 1.360(14) . ?
C28 N11 1.366(14) . ?
C28 C29 1.409(15) . ?
C29 C30 1.373(15) . ?
C29 H29 0.9300 . ?
C30 N13 1.354(14) . ?
C30 N14 1.403(13) . ?
C31 N12 1.322(14) . ?
C31 N13 1.337(13) . ?
C31 C32 1.504(16) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N14 1.435(13) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N15 1.279(13) . ?
C34 C35 1.464(15) . ?
C34 H34 0.9300 . ?
C35 N16 1.327(13) . ?
C35 C36 1.391(15) . ?
C36 C37 1.385(16) . ?
C36 H36 0.9300 . ?
C37 C38 1.385(17) . ?
C37 H37 0.9300 . ?
C38 C39 1.357(15) . ?
C38 H38 0.9300 . ?
C39 N16 1.336(13) . ?
C39 C40 1.514(16) . ?
C40 O2 1.431(15) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 N17 1.195(18) . ?
C41 C42 1.44(2) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 N18 1.125(18) . ?
C43 C44 1.433(19) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 N19 1.16(2) . ?
C45 C46 1.41(2) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.50(2) . ?
C47 H47B 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47C 0.9600 . ?
C48 O5 1.393(18) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
N1 Pb1 2.558(9) . ?
N2 N3 1.380(12) . ?
N2 Pb1 2.623(8) . ?
N4 Pb1 2.688(9) . ?
N6 N7 1.361(12) . ?
N10 N11 1.353(12) . ?
N13 Pb2 2.621(9) . ?
N14 N15 1.363(11) . ?
N15 Pb2 2.581(8) . ?
N16 Pb2 2.496(8) . ?
N17 Pb1 2.645(11) . ?
O1 Pb1 2.595(8) . ?
O1 H1 0.9300 . ?
O2 Pb2 2.724(10) . ?
O2 H2 0.9300 . ?
O3 Pb2 2.486(8) . ?
O5 C48 1.393(18) 2_756 ?
O11 Cl1 1.420(8) . ?
O11 Pb2 2.696(8) 4_546 ?
O12 Cl1 1.411(10) . ?
O13 Cl1 1.388(13) . ?
O14 Cl1 1.341(11) . ?
O21 Cl2 1.458(8) . ?
O22 Cl2 1.432(10) . ?
O23 Cl2 1.426(10) . ?
O24 Cl2 1.444(8) . ?
O31 Cl3 1.460(11) . ?
O32 Cl3 1.405(11) . ?
O33 Cl3 1.438(9) . ?
O34 Cl3 1.413(9) . ?
Pb2 O11 2.696(8) 4_556 ?
Cl4 O43 1.36(4) . ?
Cl4 O41 1.40(5) . ?
Cl4 O42 1.41(4) . ?
Cl4 O44 1.43(2) . ?
Cl4A O43A 1.29(6) . ?
Cl4A O42A 1.42(4) . ?
Cl4A O44A 1.45(3) . ?
Cl4A O41A 1.45(6) . ?

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 C1 C2 112.5(10) . . ?
O1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N1 C2 C3 121.9(11) . . ?
N1 C2 C1 118.2(10) . . ?
C3 C2 C1 119.8(10) . . ?
C4 C3 C2 119.2(11) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.2(10) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 118.8(11) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
N1 C6 C5 120.9(10) . . ?
N1 C6 C7 119.1(9) . . ?
C5 C6 C7 119.8(10) . . ?
N2 C7 C6 119.0(10) . . ?
N2 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 122.2(10) . . ?
N4 C9 N3 116.4(9) . . ?
C10 C9 N3 121.3(9) . . ?
C9 C10 C11 115.7(10) . . ?
C9 C10 H10 122.1 . . ?
C11 C10 H10 122.1 . . ?
N5 C11 N6 114.0(9) . . ?
N5 C11 C10 123.7(10) . . ?
N6 C11 C10 122.3(10) . . ?
N4 C12 N5 126.6(10) . . ?
N4 C12 C13 116.5(9) . . ?
N5 C12 C13 116.9(9) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 118.1(10) . . ?
N7 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
N8 C16 C17 122.1(10) . . ?
N8 C16 C15 116.3(10) . . ?
C17 C16 C15 121.5(10) . . ?
C16 C17 C18 116.9(10) . . ?
C16 C17 H17 121.5 . . ?
C18 C17 H17 121.5 . . ?
N9 C18 C17 122.7(10) . . ?
N9 C18 C26 114.7(9) . . ?
C17 C18 C26 122.4(10) . . ?
N9 C19 N8 127.3(9) . . ?
N9 C19 C20 115.3(9) . . ?
N8 C19 C20 117.3(10) . . ?
C25 C20 C21 118.7(10) . . ?
C25 C20 C19 119.9(10) . . ?
C21 C20 C19 121.4(10) . . ?
C22 C21 C20 119.9(11) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C23 C22 C21 121.7(12) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C22 C23 C24 119.4(11) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 119.4(12) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C20 C25 C24 120.9(11) . . ?
C20 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
N10 C26 C18 119.7(9) . . ?
N10 C26 H26 120.2 . . ?
C18 C26 H26 120.2 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N12 C28 N11 115.8(9) . . ?
N12 C28 C29 121.4(10) . . ?
N11 C28 C29 122.8(10) . . ?
C30 C29 C28 116.7(10) . . ?
C30 C29 H29 121.6 . . ?
C28 C29 H29 121.6 . . ?
N13 C30 C29 122.1(10) . . ?
N13 C30 N14 116.2(9) . . ?
C29 C30 N14 121.7(10) . . ?
N12 C31 N13 126.5(10) . . ?
N12 C31 C32 116.1(9) . . ?
N13 C31 C32 117.3(10) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N14 C33 H33A 109.5 . . ?
N14 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N14 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N15 C34 C35 119.3(10) . . ?
N15 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
N16 C35 C36 121.8(10) . . ?
N16 C35 C34 119.0(9) . . ?
C36 C35 C34 119.1(10) . . ?
C37 C36 C35 118.4(11) . . ?
C37 C36 H36 120.8 . . ?
C35 C36 H36 120.8 . . ?
C38 C37 C36 118.8(10) . . ?
C38 C37 H37 120.6 . . ?
C36 C37 H37 120.6 . . ?
C39 C38 C37 119.4(11) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
N16 C39 C38 122.2(11) . . ?
N16 C39 C40 117.0(9) . . ?
C38 C39 C40 120.7(10) . . ?
O2 C40 C39 109.9(10) . . ?
O2 C40 H40A 109.7 . . ?
C39 C40 H40A 109.7 . . ?
O2 C40 H40B 109.7 . . ?
C39 C40 H40B 109.7 . . ?
H40A C40 H40B 108.2 . . ?
N17 C41 C42 174.2(16) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N18 C43 C44 179(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N19 C45 C46 178.2(19) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C48 C47 H47A 109.5 . . ?
H47B C47 H47A 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
O5 C48 C47 111.4(16) . . ?
O5 C48 H48A 109.3 . . ?
C47 C48 H48A 109.3 . . ?
O5 C48 H48B 109.3 . . ?
C47 C48 H48B 109.3 . . ?
H48A C48 H48B 108.0 . . ?
C2 N1 C6 119.8(10) . . ?
C2 N1 Pb1 121.9(7) . . ?
C6 N1 Pb1 116.8(7) . . ?
C7 N2 N3 119.3(9) . . ?
C7 N2 Pb1 117.8(7) . . ?
N3 N2 Pb1 121.6(6) . . ?
N2 N3 C9 117.7(8) . . ?
N2 N3 C8 118.5(8) . . ?
C9 N3 C8 123.8(9) . . ?
C12 N4 C9 116.8(9) . . ?
C12 N4 Pb1 120.7(7) . . ?
C9 N4 Pb1 120.4(7) . . ?
C12 N5 C11 114.9(9) . . ?
N7 N6 C11 115.8(9) . . ?
N7 N6 C14 119.9(9) . . ?
C11 N6 C14 124.2(9) . . ?
C15 N7 N6 120.1(9) . . ?
C16 N8 C19 115.2(9) . . ?
C19 N9 C18 115.7(9) . . ?
C26 N10 N11 118.2(9) . . ?
N10 N11 C28 116.0(9) . . ?
N10 N11 C27 122.6(9) . . ?
C28 N11 C27 120.9(9) . . ?
C31 N12 C28 116.5(9) . . ?
C31 N13 C30 116.6(9) . . ?
C31 N13 Pb2 120.5(7) . . ?
C30 N13 Pb2 121.3(7) . . ?
N15 N14 C30 116.9(8) . . ?
N15 N14 C33 120.5(8) . . ?
C30 N14 C33 122.4(9) . . ?
C34 N15 N14 119.9(9) . . ?
C34 N15 Pb2 117.5(7) . . ?
N14 N15 Pb2 122.6(6) . . ?
C35 N16 C39 119.4(9) . . ?
C35 N16 Pb2 118.9(7) . . ?
C39 N16 Pb2 121.6(7) . . ?
C41 N17 Pb1 136.3(11) . . ?
C1 O1 Pb1 122.8(7) . . ?
C1 O1 H1 118.6 . . ?
Pb1 O1 H1 118.6 . . ?
C40 O2 Pb2 106.7(8) . . ?
C40 O2 H2 126.6 . . ?
Pb2 O2 H2 126.6 . . ?
C48 O5 C48 116(2) . 2_756 ?
Cl1 O11 Pb2 111.5(4) . 4_546 ?
O14 Cl1 O13 108.7(10) . . ?
O14 Cl1 O12 110.3(8) . . ?
O13 Cl1 O12 109.6(10) . . ?
O14 Cl1 O11 108.4(7) . . ?
O13 Cl1 O11 111.8(9) . . ?
O12 Cl1 O11 108.0(6) . . ?
O23 Cl2 O22 111.6(7) . . ?
O23 Cl2 O24 111.0(6) . . ?
O22 Cl2 O24 109.4(6) . . ?
O23 Cl2 O21 109.1(6) . . ?
O22 Cl2 O21 107.5(6) . . ?
O24 Cl2 O21 108.2(5) . . ?
O32 Cl3 O34 112.2(7) . . ?
O32 Cl3 O33 112.2(7) . . ?
O34 Cl3 O33 113.0(6) . . ?
O32 Cl3 O31 106.2(9) . . ?
O34 Cl3 O31 106.5(7) . . ?
O33 Cl3 O31 106.1(7) . . ?
N1 Pb1 O1 62.2(3) . . ?
N1 Pb1 N2 63.8(3) . . ?
O1 Pb1 N2 123.9(3) . . ?
N1 Pb1 N17 82.2(4) . . ?
O1 Pb1 N17 72.9(3) . . ?
N2 Pb1 N17 86.0(4) . . ?
N1 Pb1 N4 121.1(3) . . ?
O1 Pb1 N4 151.0(3) . . ?
N2 Pb1 N4 59.6(3) . . ?
N17 Pb1 N4 78.9(3) . . ?
O3 Pb2 N16 84.0(3) . . ?
O3 Pb2 N15 75.7(3) . . ?
N16 Pb2 N15 65.1(3) . . ?
O3 Pb2 N13 84.8(3) . . ?
N16 Pb2 N13 126.1(3) . . ?
N15 Pb2 N13 61.0(3) . . ?
O3 Pb2 O11 143.9(3) . 4_556 ?
N16 Pb2 O11 79.3(3) . 4_556 ?
N15 Pb2 O11 68.2(3) . 4_556 ?
N13 Pb2 O11 79.7(3) . 4_556 ?
O3 Pb2 O2 118.1(3) . . ?
N16 Pb2 O2 63.1(3) . . ?
N15 Pb2 O2 123.8(3) . . ?
N13 Pb2 O2 157.0(3) . . ?
O11 Pb2 O2 82.0(3) 4_556 . ?
O43 Cl4 O41 119(3) . . ?
O43 Cl4 O42 120(2) . . ?
O41 Cl4 O42 111(3) . . ?
O43 Cl4 O44 87.6(16) . . ?
O41 Cl4 O44 107(2) . . ?
O42 Cl4 O44 110.5(17) . . ?
O43A Cl4A O42A 122(3) . . ?
O43A Cl4A O44A 88(2) . . ?
O42A Cl4A O44A 110(2) . . ?
O43A Cl4A O41A 115(3) . . ?
O42A Cl4A O41A 110(3) . . ?
O44A Cl4A O41A 109(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.69
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         3.555
_refine_diff_density_min         -3.170
_refine_diff_density_rms         0.213

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.019 0.307 0.116 67.5 20.1
2 0.019 0.307 0.384 67.5 21.3
3 -0.019 0.693 0.616 67.5 20.8
4 0.019 0.693 0.884 67.4 21.0
5 0.481 0.807 0.116 67.5 20.1
6 0.481 0.193 0.616 67.5 20.8
7 0.519 0.807 0.384 67.5 21.3
8 0.519 0.193 0.884 67.4 21.0
_database_code_depnum_ccdc_archive 'CCDC 976902'
#######################################################################
#
#                 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_4(dh1211)

# start Validation Reply Form
_vrf_PLAT780_4dh1211             
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do ! 
RESPONSE: The atoms of ligand L1 are connected to each other and the donor
atoms are connected to the Cu atoms.Three of the six SO3CF3- anions are also
connected to the Cu atoms as are two CH3CN molecules and a H2O molecule
;
_vrf_PLAT213_4dh1211             
;
PROBLEM: Atom O13             has ADP max/min Ratio .....        4.5 prolat
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT214_4dh1211             
;
PROBLEM: Atom O52     (Anion/Solvent) ADP max/min Ratio          5.6 prolat
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT220_4dh1211             
;
PROBLEM: Large Non-Solvent    F     Ueq(max)/Ueq(min) ...        4.7 Ratio 
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT242_4dh1211             
;
PROBLEM: Low       Ueq as Compared to Neighbors for .....         S1 Check 
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT417_4dh1211             
;
PROBLEM: Short Inter D-H..H-D       H5B    ..  H6A     ..       1.87 Ang.  
RESPONSE: The H5B and H6A H2O molecules are H-bonded to each other.
;
_vrf_PLAT431_4dh1211             
;
PROBLEM: Short Inter HL..A  Contact F42    ..  O53     ..       2.58 Ang.  
RESPONSE: Two of the unbound SO3CF3- anions are in close proximity to
each other
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C54 H54 Cu3 F12 N18 O17 S4, 2(C F3 O3 S), 2(C2 H3 N), H2 O'
_chemical_formula_sum            'C60 H62 Cu3 F18 N20 O24 S6'
_chemical_formula_weight         2172.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_space_group_name_H-M   'P -1'
_symmetry_cell_setting           triclinic

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.93796(15)
_cell_length_b                   18.6842(2)
_cell_length_c                   21.6335(2)
_cell_angle_alpha                113.9013(11)
_cell_angle_beta                 92.2282(9)
_cell_angle_gamma                105.8198(11)
_cell_volume                     4182.87(9)
_cell_formula_units_Z            2.00000
_cell_measurement_temperature    100.01(10)
_cell_measurement_reflns_used    47395
_cell_measurement_theta_min      4.1400
_cell_measurement_theta_max      76.3080

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.3892
_exptl_crystal_size_mid          0.1447
_exptl_crystal_size_min          0.0735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2198
_exptl_absorpt_coefficient_mu    3.413
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.01(10)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1725
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            96122
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.91
_diffrn_reflns_theta_max         66.99
_reflns_number_total             14909
_reflns_number_gt                13185
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

Some of the components of complex 4 showed large or elongated thermal ellipsoids
due to disorder, including several of the SO3CF3- anions. The disorder was not 
modelled further. 
;

_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)+(0.1571P)²+10.6915P] where P=(Fo²+2Fc²)/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         14909
_refine_ls_number_parameters     1206
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.2487
_refine_ls_wR_factor_gt          0.2397
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 1.1275(7) 0.2183(5) 1.1393(5) 0.078(2) Uani 1 1 d . . .
H1A H 1.1069 0.2001 1.0923 0.093 Uiso 1 1 calc R . .
H1B H 1.1854 0.2029 1.1560 0.093 Uiso 1 1 calc R . .
C2 C 1.0748(6) 0.2660(5) 1.1821(4) 0.0676(17) Uani 1 1 d . . .
H2 H 1.0962 0.2838 1.2290 0.081 Uiso 1 1 calc R . .
C3 C 0.9833(5) 0.2917(4) 1.1580(3) 0.0563(13) Uani 1 1 d . . .
C4 C 0.8233(5) 0.3418(4) 1.1867(3) 0.0562(14) Uani 1 1 d . . .
H4A H 0.7653 0.2916 1.1531 0.067 Uiso 1 1 calc R . .
H4B H 0.8490 0.3790 1.1654 0.067 Uiso 1 1 calc R . .
C5 C 0.7688(5) 0.3814(3) 1.2478(2) 0.0459(11) Uani 1 1 d . . .
C6 C 0.8222(5) 0.4057(3) 1.3147(3) 0.0500(12) Uani 1 1 d . . .
H6 H 0.8946 0.3986 1.3228 0.060 Uiso 1 1 calc R . .
C7 C 0.7669(5) 0.4405(3) 1.3686(3) 0.0526(13) Uani 1 1 d . . .
H7 H 0.8011 0.4560 1.4134 0.063 Uiso 1 1 calc R . .
C8 C 0.6606(5) 0.4520(3) 1.3559(2) 0.0476(12) Uani 1 1 d . . .
H8 H 0.6229 0.4763 1.3919 0.057 Uiso 1 1 calc R . .
C9 C 0.6111(5) 0.4266(3) 1.2884(2) 0.0440(11) Uani 1 1 d . . .
C10 C 0.4979(5) 0.4339(3) 1.2700(2) 0.0432(11) Uani 1 1 d . . .
H10 H 0.4573 0.4616 1.3025 0.052 Uiso 1 1 calc R . .
C11 C 0.2905(6) 0.4495(4) 1.2183(3) 0.0566(14) Uani 1 1 d . . .
H11A H 0.2598 0.4268 1.2491 0.085 Uiso 1 1 calc R . .
H11B H 0.2264 0.4488 1.1897 0.085 Uiso 1 1 calc R . .
H11C H 0.3410 0.5053 1.2443 0.085 Uiso 1 1 calc R . .
C12 C 0.3345(4) 0.3591(3) 1.1052(2) 0.0394(10) Uani 1 1 d . . .
C13 C 0.2380(4) 0.3552(3) 1.0662(2) 0.0412(10) Uani 1 1 d . . .
H13 H 0.1838 0.3813 1.0860 0.049 Uiso 1 1 calc R . .
C14 C 0.2249(4) 0.3106(3) 0.9960(2) 0.0390(10) Uani 1 1 d . . .
C15 C 0.3911(4) 0.2732(3) 1.0081(2) 0.0411(10) Uani 1 1 d . . .
C16 C 0.4685(5) 0.2219(4) 0.9790(2) 0.0499(13) Uani 1 1 d . . .
H16A H 0.4223 0.1701 0.9425 0.075 Uiso 1 1 calc R . .
H16B H 0.5041 0.2123 1.0143 0.075 Uiso 1 1 calc R . .
H16C H 0.5292 0.2502 0.9615 0.075 Uiso 1 1 calc R . .
C17 C 0.0404(6) 0.3411(5) 0.9729(3) 0.0641(17) Uani 1 1 d . . .
H17A H 0.0419 0.3788 0.9529 0.096 Uiso 1 1 calc R . .
H17B H 0.0537 0.3705 1.0220 0.096 Uiso 1 1 calc R . .
H17C H -0.0353 0.2991 0.9575 0.096 Uiso 1 1 calc R . .
C18 C 0.0531(4) 0.2454(3) 0.8365(3) 0.0436(10) Uani 1 1 d . . .
H18 H -0.0078 0.2685 0.8444 0.052 Uiso 1 1 calc R . .
C19 C 0.0694(4) 0.1946(3) 0.7679(3) 0.0420(10) Uani 1 1 d . . .
C20 C 0.0060(4) 0.1867(3) 0.7102(3) 0.0460(11) Uani 1 1 d . . .
H20 H -0.0549 0.2094 0.7128 0.055 Uiso 1 1 calc R . .
C21 C 0.0362(4) 0.1433(3) 0.6474(3) 0.0442(11) Uani 1 1 d . . .
C22 C 0.1737(4) 0.1137(3) 0.7019(2) 0.0429(10) Uani 1 1 d . . .
C23 C 0.2617(5) 0.0697(3) 0.6933(2) 0.0453(11) Uani 1 1 d . . .
C24 C 0.3356(5) 0.0741(4) 0.6458(3) 0.0554(13) Uani 1 1 d . . .
H24 H 0.3277 0.1036 0.6210 0.067 Uiso 1 1 calc R . .
C25 C 0.4212(6) 0.0346(4) 0.6352(4) 0.0657(16) Uani 1 1 d . . .
H25 H 0.4712 0.0377 0.6039 0.079 Uiso 1 1 calc R . .
C26 C 0.4302(6) -0.0100(4) 0.6726(4) 0.0658(16) Uani 1 1 d . . .
H26 H 0.4875 -0.0362 0.6665 0.079 Uiso 1 1 calc R . .
C27 C 0.3559(6) -0.0156(4) 0.7182(3) 0.0603(15) Uani 1 1 d . . .
H27 H 0.3623 -0.0462 0.7423 0.072 Uiso 1 1 calc R . .
C28 C 0.2712(5) 0.0241(3) 0.7287(3) 0.0516(12) Uani 1 1 d . . .
H28 H 0.2207 0.0201 0.7597 0.062 Uiso 1 1 calc R . .
C29 C -0.0147(4) 0.1365(3) 0.5817(3) 0.0455(11) Uani 1 1 d . . .
H29 H 0.0099 0.1075 0.5414 0.055 Uiso 1 1 calc R . .
C30 C -0.0969(5) 0.1228(3) 0.4559(2) 0.0461(11) Uani 1 1 d . . .
H30A H -0.1397 0.1244 0.4182 0.069 Uiso 1 1 calc R . .
H30B H -0.1096 0.0665 0.4476 0.069 Uiso 1 1 calc R . .
H30C H -0.0141 0.1497 0.4603 0.069 Uiso 1 1 calc R . .
C31 C -0.2306(4) 0.1961(3) 0.5203(2) 0.0385(10) Uani 1 1 d . . .
C32 C -0.2823(4) 0.2242(3) 0.5790(2) 0.0416(10) Uani 1 1 d . . .
H32 H -0.2541 0.2248 0.6199 0.050 Uiso 1 1 calc R . .
C33 C -0.3768(4) 0.2508(3) 0.5728(2) 0.0389(10) Uani 1 1 d . . .
C34 C -0.3605(4) 0.2245(3) 0.4605(2) 0.0383(9) Uani 1 1 d . . .
C35 C -0.4005(5) 0.2263(3) 0.3948(3) 0.0463(11) Uani 1 1 d . . .
H35A H -0.3803 0.2824 0.4011 0.069 Uiso 1 1 calc R . .
H35B H -0.4845 0.2008 0.3818 0.069 Uiso 1 1 calc R . .
H35C H -0.3622 0.1967 0.3594 0.069 Uiso 1 1 calc R . .
C36 C -0.4126(6) 0.2818(5) 0.6940(3) 0.0628(15) Uani 1 1 d . . .
H36A H -0.4098 0.3353 0.7278 0.094 Uiso 1 1 calc R . .
H36B H -0.3375 0.2737 0.6995 0.094 Uiso 1 1 calc R . .
H36C H -0.4728 0.2401 0.6999 0.094 Uiso 1 1 calc R . .
C37 C -0.6034(5) 0.3209(3) 0.6519(3) 0.0492(12) Uani 1 1 d . . .
H37 H -0.5916 0.3303 0.6976 0.059 Uiso 1 1 calc R . .
C38 C -0.7029(5) 0.3337(3) 0.6210(3) 0.0514(12) Uani 1 1 d . . .
C39 C -0.7925(5) 0.3535(4) 0.6562(4) 0.0603(14) Uani 1 1 d . . .
H39 H -0.7886 0.3633 0.7021 0.072 Uiso 1 1 calc R . .
C40 C -0.8874(6) 0.3582(4) 0.6220(4) 0.0705(18) Uani 1 1 d . . .
H40 H -0.9487 0.3716 0.6445 0.085 Uiso 1 1 calc R . .
C41 C -0.8911(5) 0.3429(4) 0.5537(4) 0.0650(16) Uani 1 1 d . . .
H41 H -0.9558 0.3449 0.5298 0.078 Uiso 1 1 calc R . .
C42 C -0.7993(5) 0.3249(3) 0.5211(3) 0.0548(13) Uani 1 1 d . . .
C43 C -0.7990(5) 0.3056(4) 0.4471(3) 0.0570(14) Uani 1 1 d . . .
H43A H -0.7499 0.3532 0.4423 0.068 Uiso 1 1 calc R . .
H43B H -0.7685 0.2599 0.4252 0.068 Uiso 1 1 calc R . .
C44 C -0.9424(7) 0.2415(4) 0.3473(4) 0.0709(19) Uani 1 1 d . . .
C45 C -1.0733(8) 0.2205(7) 0.3225(6) 0.110(4) Uani 1 1 d . . .
H45 H -1.1216 0.2429 0.3522 0.132 Uiso 1 1 calc R . .
C46 C -1.1159(9) 0.1701(8) 0.2582(7) 0.132(5) Uani 1 1 d . . .
H46A H -1.0666 0.1481 0.2290 0.158 Uiso 1 1 calc R . .
H46B H -1.1956 0.1561 0.2416 0.158 Uiso 1 1 calc R . .
C47 C 0.5007(14) 0.0814(7) 1.1234(6) 0.120(4) Uani 1 1 d . . .
C48 C 0.1802(10) 0.0401(10) 0.9642(7) 0.117(4) Uani 1 1 d . . .
C49 C -0.6702(6) 0.0363(4) 0.4498(3) 0.0575(14) Uani 1 1 d . . .
C50 C 0.5013(7) 0.4307(5) 0.8961(3) 0.077(2) Uani 1 1 d . . .
C51 C 0.9680(12) 0.4228(6) 0.7765(6) 0.108(3) Uani 1 1 d . . .
C52 C 0.8427(5) 0.4642(4) 0.5742(3) 0.0587(14) Uani 1 1 d . . .
C53 C 0.7263(5) 0.3961(3) 1.0496(2) 0.0449(11) Uani 1 1 d . . .
C54 C 0.7909(6) 0.4230(4) 1.0040(3) 0.0610(15) Uani 1 1 d . . .
H54A H 0.7925 0.3758 0.9639 0.092 Uiso 1 1 calc R . .
H54B H 0.8703 0.4561 1.0269 0.092 Uiso 1 1 calc R . .
H54C H 0.7531 0.4550 0.9907 0.092 Uiso 1 1 calc R . .
C55 C 0.4981(5) 0.1977(4) 0.8207(3) 0.0514(13) Uani 1 1 d . . .
C56 C 0.6131(6) 0.1941(7) 0.8046(4) 0.085(3) Uani 1 1 d . . .
H56A H 0.6619 0.2479 0.8117 0.128 Uiso 1 1 calc R . .
H56B H 0.6051 0.1559 0.7576 0.128 Uiso 1 1 calc R . .
H56C H 0.6488 0.1762 0.8338 0.128 Uiso 1 1 calc R . .
C57 C 0.8024(7) 0.0304(5) 0.7690(4) 0.0761(19) Uani 1 1 d . . .
C58 C 0.7918(12) -0.0570(6) 0.7438(5) 0.110(3) Uani 1 1 d . . .
H58A H 0.8431 -0.0705 0.7108 0.165 Uiso 1 1 calc R . .
H58B H 0.7116 -0.0900 0.7226 0.165 Uiso 1 1 calc R . .
H58C H 0.8137 -0.0679 0.7815 0.165 Uiso 1 1 calc R . .
C59 C 0.2374(6) 0.8255(5) 0.0380(4) 0.0706(17) Uani 1 1 d . . .
C60 C 0.2017(9) 0.8866(7) 0.0245(7) 0.109(3) Uani 1 1 d . . .
H60A H 0.2224 0.8850 -0.0184 0.163 Uiso 1 1 calc R . .
H60B H 0.2411 0.9404 0.0607 0.163 Uiso 1 1 calc R . .
H60C H 0.1178 0.8749 0.0221 0.163 Uiso 1 1 calc R . .
N1 N 0.6659(4) 0.3922(3) 1.23520(19) 0.0424(9) Uani 1 1 d . . .
N2 N 0.4582(4) 0.3988(2) 1.20511(19) 0.0403(8) Uani 1 1 d . . .
N3 N 0.3580(4) 0.4005(3) 1.1757(2) 0.0429(9) Uani 1 1 d . . .
N4 N 0.4135(4) 0.3196(3) 1.07647(19) 0.0408(9) Uani 1 1 d . . .
N5 N 0.3017(3) 0.2697(3) 0.9666(2) 0.0404(8) Uani 1 1 d . . .
N6 N 0.1329(4) 0.3030(3) 0.9518(2) 0.0421(9) Uani 1 1 d . . .
N7 N 0.1295(3) 0.2557(3) 0.8850(2) 0.0396(8) Uani 1 1 d . . .
N8 N 0.1567(3) 0.1595(2) 0.7651(2) 0.0403(8) Uani 1 1 d . . .
N9 N 0.1178(4) 0.1063(3) 0.6436(2) 0.0459(9) Uani 1 1 d . . .
N10 N -0.0932(4) 0.1707(2) 0.5806(2) 0.0411(9) Uani 1 1 d . . .
N11 N -0.1387(4) 0.1654(2) 0.51943(19) 0.0410(9) Uani 1 1 d . . .
N12 N -0.2703(4) 0.1966(2) 0.4616(2) 0.0405(8) Uani 1 1 d . . .
N13 N -0.4172(4) 0.2522(2) 0.5137(2) 0.0391(8) Uani 1 1 d . . .
N14 N -0.4393(4) 0.2764(3) 0.6261(2) 0.0450(9) Uani 1 1 d . . .
N15 N -0.5337(4) 0.2954(3) 0.6105(2) 0.0446(9) Uani 1 1 d . . .
N16 N -0.7043(4) 0.3216(3) 0.5553(2) 0.0471(10) Uani 1 1 d . . .
N17 N 0.6744(4) 0.3731(3) 1.08471(19) 0.0416(9) Uani 1 1 d . . .
N18 N 0.4082(4) 0.2005(3) 0.8342(2) 0.0424(9) Uani 1 1 d . . .
N19 N 0.8105(6) 0.0975(5) 0.7893(4) 0.090(2) Uani 1 1 d . . .
N20 N 0.2618(6) 0.7774(4) 0.0483(3) 0.0754(16) Uani 1 1 d . . .
O1 O 0.9622(4) 0.2866(4) 1.1015(2) 0.0778(14) Uani 1 1 d . . .
O2 O 0.9219(4) 0.3230(3) 1.20817(19) 0.0566(9) Uani 1 1 d . . .
O3 O -0.9213(4) 0.2838(3) 0.4160(3) 0.0714(13) Uani 1 1 d . . .
O4 O -0.8685(5) 0.2257(3) 0.3133(3) 0.0733(13) Uani 1 1 d . . .
O5 O -0.5362(4) 0.3519(3) 0.4624(2) 0.0496(9) Uani 1 1 d . . .
O6 O -0.6117(4) 0.2968(4) 0.3315(3) 0.0709(12) Uani 1 1 d D . .
O11 O 0.5417(4) 0.2247(2) 1.12889(18) 0.0545(9) Uani 1 1 d . . .
O12 O 0.3955(13) 0.1799(12) 1.1851(11) 0.303(12) Uani 1 1 d . . .
O13 O 0.5874(13) 0.2115(5) 1.2319(3) 0.213(7) Uani 1 1 d . . .
O21 O 0.1912(4) 0.0906(2) 0.8713(2) 0.0603(10) Uani 1 1 d . . .
O22 O 0.0684(5) 0.1350(3) 0.9546(3) 0.0804(14) Uani 1 1 d . . .
O23 O 0.0063(7) -0.0060(4) 0.8666(4) 0.119(2) Uani 1 1 d . . .
O31 O -0.6723(3) 0.1677(2) 0.4392(2) 0.0512(8) Uani 1 1 d . . .
O32 O -0.7527(5) 0.1452(3) 0.5321(3) 0.0835(16) Uani 1 1 d . . .
O33 O -0.8609(4) 0.0622(3) 0.4166(4) 0.0899(17) Uani 1 1 d . . .
O41 O 0.2884(5) 0.4296(3) 0.9034(3) 0.0847(16) Uani 1 1 d . . .
O42 O 0.3258(4) 0.3257(3) 0.8025(2) 0.0637(10) Uani 1 1 d . . .
O43 O 0.3842(5) 0.4671(3) 0.8185(2) 0.0712(12) Uani 1 1 d . . .
O51 O 0.8859(15) 0.3597(9) 0.8515(7) 0.262(10) Uani 1 1 d . . .
O52 O 0.9555(17) 0.5020(15) 0.8916(7) 0.46(2) Uani 1 1 d . . .
O53 O 0.7909(8) 0.4339(9) 0.8303(7) 0.190(6) Uani 1 1 d . . .
O61 O 0.6330(4) 0.4405(2) 0.60702(18) 0.0511(9) Uani 1 1 d . . .
O62 O 0.7560(4) 0.5804(2) 0.63594(19) 0.0620(11) Uani 1 1 d . . .
O63 O 0.6713(4) 0.4855(3) 0.51709(19) 0.0540(9) Uani 1 1 d . . .
F11 F 0.4671(8) 0.0361(4) 1.1584(4) 0.150(3) Uani 1 1 d . . .
F12 F 0.4408(15) 0.0509(4) 1.0674(4) 0.260(8) Uani 1 1 d . . .
F13 F 0.6022(17) 0.0788(12) 1.1142(10) 0.327(12) Uani 1 1 d . . .
F21 F 0.1151(6) 0.0163(5) 1.0027(4) 0.137(3) Uani 1 1 d . . .
F22 F 0.2286(10) -0.0138(7) 0.9291(6) 0.208(6) Uani 1 1 d . . .
F23 F 0.2695(7) 0.1123(7) 1.0086(5) 0.169(4) Uani 1 1 d . . .
F31 F -0.7188(4) -0.0145(2) 0.4781(2) 0.0779(11) Uani 1 1 d . . .
F32 F -0.6751(4) -0.0101(3) 0.3840(2) 0.0831(12) Uani 1 1 d . . .
F33 F -0.5598(3) 0.0732(2) 0.4800(2) 0.0696(9) Uani 1 1 d . . .
F41 F 0.4953(4) 0.3850(3) 0.9311(2) 0.0850(12) Uani 1 1 d . . .
F42 F 0.5764(4) 0.4119(5) 0.8528(3) 0.116(2) Uani 1 1 d . . .
F43 F 0.5479(6) 0.5090(3) 0.9403(2) 0.120(2) Uani 1 1 d . . .
F51 F 0.9102(10) 0.3567(6) 0.7206(4) 0.213(6) Uani 1 1 d . . .
F52 F 0.9835(10) 0.4837(5) 0.7610(5) 0.183(4) Uani 1 1 d . . .
F53 F 1.0754(7) 0.4243(11) 0.7876(5) 0.262(8) Uani 1 1 d . . .
F61 F 0.8895(4) 0.4653(4) 0.6311(3) 0.0999(16) Uani 1 1 d . . .
F62 F 0.8191(3) 0.3893(2) 0.5246(3) 0.0849(13) Uani 1 1 d . . .
F63 F 0.9250(3) 0.5148(2) 0.5580(2) 0.0720(10) Uani 1 1 d . . .
S1 S 0.5104(2) 0.18604(11) 1.17404(9) 0.0776(5) Uani 1 1 d . . .
S2 S 0.10192(16) 0.06763(11) 0.90852(9) 0.0687(4) Uani 1 1 d . . .
S3 S -0.74864(13) 0.10948(10) 0.45964(9) 0.0594(4) Uani 1 1 d . . .
S4 S 0.35843(15) 0.41142(9) 0.84987(8) 0.0594(4) Uani 1 1 d . . .
S5 S 0.89109(15) 0.42113(13) 0.84019(10) 0.0730(5) Uani 1 1 d . . .
S6 S 0.71093(12) 0.49639(7) 0.58530(6) 0.0439(3) Uani 1 1 d . . .
Cu1 Cu 0.55977(6) 0.35096(5) 1.14360(3) 0.0423(2) Uani 1 1 d . . .
Cu2 Cu 0.25434(6) 0.20562(4) 0.86136(3) 0.0398(2) Uani 1 1 d . . .
Cu3 Cu -0.55975(6) 0.29032(4) 0.51891(4) 0.0415(2) Uani 1 1 d . . .
H5A H -0.484(7) 0.387(5) 0.475(4) 0.06(2) Uiso 1 1 d . . .
H5B H -0.559(6) 0.330(4) 0.417(4) 0.06(2) Uiso 1 1 d . . .
H6A H -0.661(5) 0.250(3) 0.336(3) 0.037(13) Uiso 1 1 d D . .
H6B H -0.604(8) 0.258(4) 0.296(3) 0.11(3) Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 C2 1.315(11) . ?
C1 H1A 0.9300 . ?
C1 H1B 0.9300 . ?
C2 C3 1.464(9) . ?
C2 H2 0.9300 . ?
C3 O1 1.196(7) . ?
C3 O2 1.357(7) . ?
C4 O2 1.428(7) . ?
C4 C5 1.503(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.334(7) . ?
C5 C6 1.394(7) . ?
C6 C7 1.378(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.379(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.389(7) . ?
C8 H8 0.9300 . ?
C9 N1 1.361(6) . ?
C9 C10 1.449(8) . ?
C10 N2 1.289(6) . ?
C10 H10 0.9300 . ?
C11 N3 1.453(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.369(7) . ?
C12 N4 1.369(6) . ?
C12 N3 1.377(6) . ?
C13 C14 1.383(7) . ?
C13 H13 0.9300 . ?
C14 N6 1.365(6) . ?
C14 N5 1.365(6) . ?
C15 N5 1.336(6) . ?
C15 N4 1.348(6) . ?
C15 C16 1.487(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N6 1.462(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N7 1.279(6) . ?
C18 C19 1.458(7) . ?
C18 H18 0.9300 . ?
C19 N8 1.365(6) . ?
C19 C20 1.367(7) . ?
C20 C21 1.393(8) . ?
C20 H20 0.9300 . ?
C21 N9 1.327(7) . ?
C21 C29 1.467(7) . ?
C22 N9 1.340(6) . ?
C22 N8 1.345(7) . ?
C22 C23 1.475(7) . ?
C23 C28 1.378(8) . ?
C23 C24 1.394(8) . ?
C24 C25 1.390(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.395(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.369(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(8) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 N10 1.275(7) . ?
C29 H29 0.9300 . ?
C30 N11 1.469(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N12 1.344(6) . ?
C31 N11 1.367(6) . ?
C31 C32 1.402(7) . ?
C32 C33 1.372(7) . ?
C32 H32 0.9300 . ?
C33 N13 1.362(6) . ?
C33 N14 1.389(6) . ?
C34 N12 1.321(6) . ?
C34 N13 1.349(6) . ?
C34 C35 1.497(6) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N14 1.447(7) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N15 1.284(7) . ?
C37 C38 1.462(8) . ?
C37 H37 0.9300 . ?
C38 N16 1.346(8) . ?
C38 C39 1.383(8) . ?
C39 C40 1.372(10) . ?
C39 H39 0.9300 . ?
C40 C41 1.383(11) . ?
C40 H40 0.9300 . ?
C41 C42 1.371(9) . ?
C41 H41 0.9300 . ?
C42 N16 1.358(7) . ?
C42 C43 1.491(9) . ?
C43 O3 1.459(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O4 1.192(10) . ?
C44 O3 1.345(10) . ?
C44 C45 1.522(11) . ?
C45 C46 1.304(17) . ?
C45 H45 0.9300 . ?
C46 H46A 0.9300 . ?
C46 H46B 0.9300 . ?
C47 F12 1.206(13) . ?
C47 F13 1.246(19) . ?
C47 F11 1.345(12) . ?
C47 S1 1.780(12) . ?
C48 F21 1.288(10) . ?
C48 F22 1.288(14) . ?
C48 F23 1.402(17) . ?
C48 S2 1.807(9) . ?
C49 F33 1.309(7) . ?
C49 F32 1.323(7) . ?
C49 F31 1.346(8) . ?
C49 S3 1.808(6) . ?
C50 F43 1.322(8) . ?
C50 F42 1.332(9) . ?
C50 F41 1.342(9) . ?
C50 S4 1.811(9) . ?
C51 F52 1.281(12) . ?
C51 F53 1.285(15) . ?
C51 F51 1.313(13) . ?
C51 S5 1.691(10) . ?
C52 F62 1.317(7) . ?
C52 F61 1.321(8) . ?
C52 F63 1.330(7) . ?
C52 S6 1.823(7) . ?
C53 N17 1.140(7) . ?
C53 C54 1.440(8) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 N18 1.132(7) . ?
C55 C56 1.441(9) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 N19 1.123(10) . ?
C57 C58 1.463(12) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 N20 1.116(10) . ?
C59 C60 1.448(12) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N1 Cu1 2.040(4) . ?
N2 N3 1.348(6) . ?
N2 Cu1 1.947(4) . ?
N4 Cu1 2.014(4) . ?
N5 Cu2 2.064(4) . ?
N6 N7 1.346(6) . ?
N7 Cu2 1.947(4) . ?
N8 Cu2 2.061(4) . ?
N10 N11 1.365(5) . ?
N13 Cu3 2.006(4) . ?
N14 N15 1.342(6) . ?
N15 Cu3 1.952(4) . ?
N16 Cu3 2.055(4) . ?
N17 Cu1 1.980(4) . ?
N18 Cu2 1.965(4) . ?
O5 Cu3 1.971(4) . ?
O5 H5A 0.72(8) . ?
O5 H5B 0.90(8) . ?
O6 H6A 0.95(5) . ?
O6 H6B 0.85(5) . ?
O11 S1 1.438(4) . ?
O11 Cu1 2.196(4) . ?
O12 S1 1.384(9) . ?
O13 S1 1.352(8) . ?
O21 S2 1.438(5) . ?
O21 Cu2 2.176(4) . ?
O22 S2 1.424(6) . ?
O23 S2 1.439(7) . ?
O31 S3 1.446(4) . ?
O31 Cu3 2.229(4) . ?
O32 S3 1.442(5) . ?
O33 S3 1.427(6) . ?
O41 S4 1.438(5) . ?
O42 S4 1.437(4) . ?
O43 S4 1.432(5) . ?
O51 S5 1.253(8) . ?
O52 S5 1.431(14) . ?
O53 S5 1.308(7) . ?
O61 S6 1.441(4) . ?
O62 S6 1.434(4) . ?
O63 S6 1.447(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
C1 C2 C3 121.7(7) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 H2 119.1 . . ?
O1 C3 O2 122.3(5) . . ?
O1 C3 C2 126.1(6) . . ?
O2 C3 C2 111.5(5) . . ?
O2 C4 C5 109.3(4) . . ?
O2 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
O2 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
N1 C5 C6 121.2(5) . . ?
N1 C5 C4 116.7(4) . . ?
C6 C5 C4 122.1(5) . . ?
C7 C6 C5 119.4(5) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 119.7(5) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C7 C8 C9 118.6(5) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
N1 C9 C8 121.5(5) . . ?
N1 C9 C10 116.0(4) . . ?
C8 C9 C10 122.4(5) . . ?
N2 C10 C9 114.5(4) . . ?
N2 C10 H10 122.7 . . ?
C9 C10 H10 122.7 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N4 121.9(4) . . ?
C13 C12 N3 123.2(4) . . ?
N4 C12 N3 115.0(4) . . ?
C12 C13 C14 116.9(4) . . ?
C12 C13 H13 121.6 . . ?
C14 C13 H13 121.6 . . ?
N6 C14 N5 115.8(4) . . ?
N6 C14 C13 122.2(4) . . ?
N5 C14 C13 122.0(4) . . ?
N5 C15 N4 123.3(4) . . ?
N5 C15 C16 119.6(4) . . ?
N4 C15 C16 117.1(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N7 C18 C19 114.5(4) . . ?
N7 C18 H18 122.8 . . ?
C19 C18 H18 122.8 . . ?
N8 C19 C20 122.3(5) . . ?
N8 C19 C18 115.7(4) . . ?
C20 C19 C18 121.9(5) . . ?
C19 C20 C21 117.4(5) . . ?
C19 C20 H20 121.3 . . ?
C21 C20 H20 121.3 . . ?
N9 C21 C20 121.0(4) . . ?
N9 C21 C29 114.9(5) . . ?
C20 C21 C29 124.1(5) . . ?
N9 C22 N8 124.5(4) . . ?
N9 C22 C23 115.3(4) . . ?
N8 C22 C23 120.2(4) . . ?
C28 C23 C24 119.8(5) . . ?
C28 C23 C22 123.0(5) . . ?
C24 C23 C22 117.2(5) . . ?
C25 C24 C23 120.4(6) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 118.5(6) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
C27 C26 C25 121.0(6) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C28 120.1(6) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C23 C28 C27 120.0(6) . . ?
C23 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
N10 C29 C21 119.2(5) . . ?
N10 C29 H29 120.4 . . ?
C21 C29 H29 120.4 . . ?
N11 C30 H30A 109.5 . . ?
N11 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N11 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N12 C31 N11 116.5(4) . . ?
N12 C31 C32 121.6(4) . . ?
N11 C31 C32 121.9(4) . . ?
C33 C32 C31 116.5(4) . . ?
C33 C32 H32 121.7 . . ?
C31 C32 H32 121.7 . . ?
N13 C33 C32 122.4(4) . . ?
N13 C33 N14 115.5(4) . . ?
C32 C33 N14 122.1(4) . . ?
N12 C34 N13 125.3(4) . . ?
N12 C34 C35 116.5(4) . . ?
N13 C34 C35 118.2(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N14 C36 H36A 109.5 . . ?
N14 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N14 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N15 C37 C38 114.3(5) . . ?
N15 C37 H37 122.8 . . ?
C38 C37 H37 122.8 . . ?
N16 C38 C39 122.1(6) . . ?
N16 C38 C37 115.8(5) . . ?
C39 C38 C37 122.1(6) . . ?
C40 C39 C38 118.5(7) . . ?
C40 C39 H39 120.7 . . ?
C38 C39 H39 120.7 . . ?
C39 C40 C41 119.5(6) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 H40 120.3 . . ?
C42 C41 C40 120.0(6) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
N16 C42 C41 120.6(6) . . ?
N16 C42 C43 116.6(5) . . ?
C41 C42 C43 122.8(6) . . ?
O3 C43 C42 106.7(5) . . ?
O3 C43 H43A 110.4 . . ?
C42 C43 H43A 110.4 . . ?
O3 C43 H43B 110.4 . . ?
C42 C43 H43B 110.4 . . ?
H43A C43 H43B 108.6 . . ?
O4 C44 O3 124.3(6) . . ?
O4 C44 C45 127.6(8) . . ?
O3 C44 C45 108.0(8) . . ?
C46 C45 C44 118.1(12) . . ?
C46 C45 H45 121.0 . . ?
C44 C45 H45 121.0 . . ?
C45 C46 H46A 120.0 . . ?
C45 C46 H46B 120.0 . . ?
H46A C46 H46B 120.0 . . ?
F12 C47 F13 106.9(16) . . ?
F12 C47 F11 112.3(11) . . ?
F13 C47 F11 104.3(11) . . ?
F12 C47 S1 114.1(9) . . ?
F13 C47 S1 108.1(13) . . ?
F11 C47 S1 110.6(9) . . ?
F21 C48 F22 111.8(10) . . ?
F21 C48 F23 106.1(11) . . ?
F22 C48 F23 108.5(10) . . ?
F21 C48 S2 113.0(7) . . ?
F22 C48 S2 110.5(9) . . ?
F23 C48 S2 106.5(7) . . ?
F33 C49 F32 109.6(5) . . ?
F33 C49 F31 106.6(5) . . ?
F32 C49 F31 107.3(5) . . ?
F33 C49 S3 111.7(4) . . ?
F32 C49 S3 110.1(4) . . ?
F31 C49 S3 111.2(4) . . ?
F43 C50 F42 107.7(6) . . ?
F43 C50 F41 107.7(6) . . ?
F42 C50 F41 106.9(7) . . ?
F43 C50 S4 111.5(7) . . ?
F42 C50 S4 110.5(5) . . ?
F41 C50 S4 112.2(5) . . ?
F52 C51 F53 100.5(11) . . ?
F52 C51 F51 106.0(11) . . ?
F53 C51 F51 109.8(12) . . ?
F52 C51 S5 118.7(8) . . ?
F53 C51 S5 114.5(9) . . ?
F51 C51 S5 106.8(8) . . ?
F62 C52 F61 108.4(6) . . ?
F62 C52 F63 107.5(5) . . ?
F61 C52 F63 107.2(5) . . ?
F62 C52 S6 111.4(4) . . ?
F61 C52 S6 111.5(5) . . ?
F63 C52 S6 110.6(4) . . ?
N17 C53 C54 178.6(6) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N18 C55 C56 179.1(6) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N19 C57 C58 178.9(9) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N20 C59 C60 178.1(9) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C5 N1 C9 119.6(4) . . ?
C5 N1 Cu1 129.3(3) . . ?
C9 N1 Cu1 110.7(3) . . ?
C10 N2 N3 125.2(4) . . ?
C10 N2 Cu1 117.6(4) . . ?
N3 N2 Cu1 116.7(3) . . ?
N2 N3 C12 114.6(4) . . ?
N2 N3 C11 119.4(4) . . ?
C12 N3 C11 125.8(4) . . ?
C15 N4 C12 117.9(4) . . ?
C15 N4 Cu1 128.6(3) . . ?
C12 N4 Cu1 113.1(3) . . ?
C15 N5 C14 117.9(4) . . ?
C15 N5 Cu2 129.6(3) . . ?
C14 N5 Cu2 112.5(3) . . ?
N7 N6 C14 115.6(4) . . ?
N7 N6 C17 119.9(4) . . ?
C14 N6 C17 124.4(4) . . ?
C18 N7 N6 123.9(4) . . ?
C18 N7 Cu2 118.6(4) . . ?
N6 N7 Cu2 117.4(3) . . ?
C22 N8 C19 116.0(4) . . ?
C22 N8 Cu2 132.7(3) . . ?
C19 N8 Cu2 110.4(3) . . ?
C21 N9 C22 118.6(4) . . ?
C29 N10 N11 118.9(4) . . ?
N10 N11 C31 116.1(4) . . ?
N10 N11 C30 121.2(4) . . ?
C31 N11 C30 122.5(4) . . ?
C34 N12 C31 117.8(4) . . ?
C34 N13 C33 116.3(4) . . ?
C34 N13 Cu3 130.2(3) . . ?
C33 N13 Cu3 113.4(3) . . ?
N15 N14 C33 114.7(4) . . ?
N15 N14 C36 119.3(4) . . ?
C33 N14 C36 126.0(4) . . ?
C37 N15 N14 125.3(5) . . ?
C37 N15 Cu3 118.1(4) . . ?
N14 N15 Cu3 116.5(3) . . ?
C38 N16 C42 119.2(5) . . ?
C38 N16 Cu3 111.4(4) . . ?
C42 N16 Cu3 129.1(4) . . ?
C53 N17 Cu1 165.3(4) . . ?
C55 N18 Cu2 177.7(4) . . ?
C3 O2 C4 114.8(4) . . ?
C44 O3 C43 113.9(6) . . ?
Cu3 O5 H5A 115(6) . . ?
Cu3 O5 H5B 125(5) . . ?
H5A O5 H5B 113(7) . . ?
H6A O6 H6B 80(5) . . ?
S1 O11 Cu1 130.1(2) . . ?
S2 O21 Cu2 128.7(3) . . ?
S3 O31 Cu3 119.7(2) . . ?
O13 S1 O12 113.2(10) . . ?
O13 S1 O11 118.4(5) . . ?
O12 S1 O11 111.2(5) . . ?
O13 S1 C47 105.8(6) . . ?
O12 S1 C47 102.5(10) . . ?
O11 S1 C47 103.7(4) . . ?
O22 S2 O21 113.8(3) . . ?
O22 S2 O23 115.7(4) . . ?
O21 S2 O23 113.8(4) . . ?
O22 S2 C48 103.9(5) . . ?
O21 S2 C48 102.3(4) . . ?
O23 S2 C48 105.4(6) . . ?
O33 S3 O32 114.7(4) . . ?
O33 S3 O31 115.6(3) . . ?
O32 S3 O31 112.3(3) . . ?
O33 S3 C49 105.6(3) . . ?
O32 S3 C49 103.6(3) . . ?
O31 S3 C49 103.4(3) . . ?
O43 S4 O42 114.4(3) . . ?
O43 S4 O41 116.3(3) . . ?
O42 S4 O41 114.5(3) . . ?
O43 S4 C50 103.0(3) . . ?
O42 S4 C50 103.4(3) . . ?
O41 S4 C50 102.7(4) . . ?
O51 S5 O53 116.7(9) . . ?
O51 S5 O52 119.4(16) . . ?
O53 S5 O52 98.4(13) . . ?
O51 S5 C51 112.1(5) . . ?
O53 S5 C51 110.2(6) . . ?
O52 S5 C51 98.0(9) . . ?
O62 S6 O61 115.2(2) . . ?
O62 S6 O63 115.1(2) . . ?
O61 S6 O63 114.3(2) . . ?
O62 S6 C52 103.0(3) . . ?
O61 S6 C52 105.0(3) . . ?
O63 S6 C52 102.1(3) . . ?
N2 Cu1 N17 142.86(18) . . ?
N2 Cu1 N4 78.90(16) . . ?
N17 Cu1 N4 96.24(16) . . ?
N2 Cu1 N1 80.84(17) . . ?
N17 Cu1 N1 102.60(17) . . ?
N4 Cu1 N1 159.26(16) . . ?
N2 Cu1 O11 112.17(16) . . ?
N17 Cu1 O11 104.94(16) . . ?
N4 Cu1 O11 95.62(17) . . ?
N1 Cu1 O11 87.90(16) . . ?
N7 Cu2 N18 154.84(18) . . ?
N7 Cu2 N8 80.20(16) . . ?
N18 Cu2 N8 98.50(16) . . ?
N7 Cu2 N5 78.62(16) . . ?
N18 Cu2 N5 100.98(16) . . ?
N8 Cu2 N5 158.80(16) . . ?
N7 Cu2 O21 104.63(18) . . ?
N18 Cu2 O21 100.53(18) . . ?
N8 Cu2 O21 94.69(17) . . ?
N5 Cu2 O21 89.91(17) . . ?
N15 Cu3 O5 146.56(19) . . ?
N15 Cu3 N13 79.72(17) . . ?
O5 Cu3 N13 103.13(17) . . ?
N15 Cu3 N16 79.99(18) . . ?
O5 Cu3 N16 96.33(17) . . ?
N13 Cu3 N16 159.19(17) . . ?
N15 Cu3 O31 114.36(16) . . ?
O5 Cu3 O31 98.93(17) . . ?
N13 Cu3 O31 91.96(15) . . ?
N16 Cu3 O31 92.22(17) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        66.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.286
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.126
_database_code_depnum_ccdc_archive 'CCDC 976903'
#######################################################################
#
#                 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_5(djh466)

# start Validation Reply Form
_vrf_REFNR01_5djh466             
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: Weak diffracting crystal, large structure. See _expl_special_details
;
_vrf_THETM01_5djh466             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Weak diffracting crystal. See _expl_special_details
;
_vrf_PLAT088_5djh466             
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.37       
RESPONSE: Weak diffracting crystal, large structure. See _expl_special_details
;
_vrf_PLAT415_5djh466             
;
PROBLEM: Short Inter D-H..H-X       H2A    ..  H48A    ..       1.82 Ang.  
RESPONSE: Disordered hydroxymethyl arm. See _refine_special_details
;
_vrf_PLAT213_5djh466             
;
PROBLEM: Atom C68             has ADP max/min Ratio .....        5.0 prolat
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT220_5djh466             
;
PROBLEM: Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        9.6 Ratio 
RESPONSE: Disordered hydroxymethyl arm and phenyl ring. See _refine_special_details
;
_vrf_PLAT222_5djh466             
;
PROBLEM: Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        8.7 Ratio 
RESPONSE: Disordered hydroxymethyl arm and phenyl ring. See _refine_special_details
;
_vrf_PLAT231_5djh466             
;
PROBLEM: Hirshfeld Test (Solvent)   S2     --  O21     ..       13.6 su    
RESPONSE: Disordered SO3CF3- anion. See _refine_special_details
;
_vrf_PLAT332_5djh466             
;
PROBLEM: Large Phenyl C-C Range           C20    -C25           0.28 Ang.  
RESPONSE: Disordered hydroxymethyl arm and phenyl ring. See _refine_special_details
;
_vrf_PLAT420_5djh466             
;
PROBLEM: D-H Without Acceptor       O1     -   H1     ...     Please Check 
RESPONSE: H1 is in a calculated position which is not aligned along a possible H-bond
between O1-O22. However, there is no additional electron density around O1 which 
could be used to give H1 an appropriate position.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C80 H84 Ag2 N32 O4, 2(C F3 O3 S), C2 H3 N, H2 O'
_chemical_formula_sum            'C84 H89 Ag2 F6 N33 O11 S2'
_chemical_formula_weight         2130.77

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.957(3)
_cell_length_b                   16.872(3)
_cell_length_c                   17.655(3)
_cell_angle_alpha                90.879(8)
_cell_angle_beta                 104.340(8)
_cell_angle_gamma                99.074(8)
_cell_volume                     4540.1(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    7143
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      18.82

_exptl_crystal_description       rhomb
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_max          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
;
Crystals of complex 5 were difficult to grow and were very small 
in two dimensions. The structure of complex 5 was large and contained
a CH3CN and H2O molecule. As a result the crystals did not diffract well and
no meaningful data could be obtained beyond theta 18.82. In spite of this
the reported structure clearly revealed full details of complex 5's 
structure and crystal packing.
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22229
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.19
_diffrn_reflns_theta_max         18.82
_reflns_number_total             7056
_reflns_number_gt                6174
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

Some of the components of complex 5 showed large or elongated thermal ellipsoids
due to disorder, including the SO3CF3- anions, one of the central phenyl ring and one
of the terminal hydroxymethyl arms. The disordered phenyl ring (C21-C25) was modelled
as being disordered over two sites with site occupancy factors of 0.69 and 0.31, 
while the O2 containing hydroxymethyl arm was disordered over two sites with occupancy
factors of 0.51 and 0.49. Several of the ellipsoids were also restrained with
ISOR restraints.
;

_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)+(0.0520P)²+60.8872P] where P=(Fo²+2Fc²)/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         7056
_refine_ls_number_parameters     1327
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1691
_refine_ls_wR_factor_gt          0.1599
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.007
_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
C1 C 0.6098(7) 0.3656(7) 0.5267(7) 0.033(3) Uani 1 1 d . . .
H1A H 0.5944 0.3979 0.5654 0.040 Uiso 1 1 calc R . .
H1B H 0.5881 0.3864 0.4759 0.040 Uiso 1 1 calc R . .
C2 C 0.7085(7) 0.3755(7) 0.5442(6) 0.020(3) Uani 1 1 d . . .
C3 C 0.7573(8) 0.4511(7) 0.5647(6) 0.026(3) Uani 1 1 d . . .
H3 H 0.7298 0.4953 0.5674 0.031 Uiso 1 1 calc R . .
C4 C 0.8476(9) 0.4603(7) 0.5813(6) 0.033(3) Uani 1 1 d . . .
H4 H 0.8820 0.5105 0.5971 0.039 Uiso 1 1 calc R . .
C5 C 0.8855(8) 0.3940(7) 0.5740(6) 0.027(3) Uani 1 1 d . . .
H5 H 0.9462 0.3990 0.5845 0.033 Uiso 1 1 calc R . .
C6 C 0.8340(8) 0.3206(7) 0.5512(6) 0.019(3) Uani 1 1 d . . .
C7 C 0.8740(7) 0.2491(8) 0.5409(6) 0.024(3) Uani 1 1 d . . .
H7 H 0.9324 0.2484 0.5663 0.028 Uiso 1 1 calc R . .
C8 C 0.9513(7) 0.1136(7) 0.5390(7) 0.031(3) Uani 1 1 d . . .
H8A H 0.9941 0.1548 0.5270 0.047 Uiso 1 1 calc R . .
H8B H 0.9646 0.0618 0.5278 0.047 Uiso 1 1 calc R . .
H8C H 0.9526 0.1193 0.5935 0.047 Uiso 1 1 calc R . .
C9 C 0.8137(8) 0.0622(7) 0.4362(7) 0.020(3) Uani 1 1 d . . .
C10 C 0.7518(8) 0.0817(7) 0.3735(7) 0.019(3) Uani 1 1 d . . .
H10 H 0.7449 0.1348 0.3650 0.023 Uiso 1 1 calc R . .
C11 C 0.6998(8) 0.0187(8) 0.3231(7) 0.022(3) Uani 1 1 d . . .
C12 C 0.7737(9) -0.0703(7) 0.3968(8) 0.023(3) Uani 1 1 d . . .
C13 C 0.7858(8) -0.1565(7) 0.4115(7) 0.034(3) Uani 1 1 d . . .
H13A H 0.7442 -0.1808 0.4389 0.051 Uiso 1 1 calc R . .
H13B H 0.8443 -0.1574 0.4425 0.051 Uiso 1 1 calc R . .
H13C H 0.7767 -0.1860 0.3624 0.051 Uiso 1 1 calc R . .
C14 C 0.5682(7) -0.0341(6) 0.2161(6) 0.025(3) Uani 1 1 d . . .
H14A H 0.5115 -0.0254 0.2204 0.038 Uiso 1 1 calc R . .
H14B H 0.5797 -0.0845 0.2374 0.038 Uiso 1 1 calc R . .
H14C H 0.5694 -0.0353 0.1620 0.038 Uiso 1 1 calc R . .
C15 C 0.5798(8) 0.1290(7) 0.1850(7) 0.018(3) Uani 1 1 d . . .
H15 H 0.5286 0.0935 0.1620 0.022 Uiso 1 1 calc R . .
C16 C 0.5948(8) 0.2123(7) 0.1618(6) 0.018(3) Uani 1 1 d . . .
C17 C 0.6775(8) 0.2550(7) 0.1700(6) 0.022(3) Uani 1 1 d . . .
H17 H 0.7268 0.2314 0.1894 0.026 Uiso 1 1 calc R . .
C18 C 0.6860(8) 0.3334(7) 0.1490(6) 0.024(3) Uani 1 1 d . . .
C19 C 0.5354(8) 0.3214(8) 0.1139(7) 0.039(3) Uani 1 1 d U A .
C26 C 0.7726(9) 0.3823(7) 0.1537(7) 0.028(3) Uani 1 1 d . . .
H26 H 0.7783 0.4376 0.1495 0.034 Uiso 1 1 calc R . .
C27 C 0.9305(8) 0.4809(6) 0.1749(7) 0.032(3) Uani 1 1 d . . .
H27A H 0.8977 0.4984 0.1267 0.048 Uiso 1 1 calc R . .
H27B H 0.9915 0.5028 0.1828 0.048 Uiso 1 1 calc R . .
H27C H 0.9098 0.4990 0.2176 0.048 Uiso 1 1 calc R . .
C28 C 0.9894(8) 0.3532(7) 0.1796(6) 0.018(3) Uani 1 1 d . . .
C29 C 0.9789(7) 0.2699(7) 0.1690(6) 0.023(3) Uani 1 1 d . . .
H29 H 0.9237 0.2379 0.1544 0.027 Uiso 1 1 calc R . .
C30 C 1.0552(8) 0.2373(7) 0.1814(6) 0.020(3) Uani 1 1 d . . .
C31 C 1.1372(8) 0.3605(8) 0.2121(6) 0.025(3) Uani 1 1 d . . .
C32 C 1.2265(7) 0.4123(6) 0.2385(7) 0.029(3) Uani 1 1 d . . .
H32A H 1.2581 0.3943 0.2869 0.044 Uiso 1 1 calc R . .
H32B H 1.2197 0.4672 0.2459 0.044 Uiso 1 1 calc R . .
H32C H 1.2583 0.4083 0.1994 0.044 Uiso 1 1 calc R . .
C33 C 1.1256(7) 0.1161(7) 0.2172(6) 0.030(3) Uani 1 1 d . . .
H33A H 1.1011 0.0763 0.2474 0.044 Uiso 1 1 calc R . .
H33B H 1.1681 0.1559 0.2517 0.044 Uiso 1 1 calc R . .
H33C H 1.1535 0.0909 0.1832 0.044 Uiso 1 1 calc R . .
C34 C 0.9858(7) 0.0349(8) 0.1063(6) 0.025(3) Uani 1 1 d . . .
H34 H 1.0290 0.0109 0.1386 0.030 Uiso 1 1 calc R . .
C35 C 0.9187(7) -0.0142(7) 0.0470(7) 0.025(3) Uani 1 1 d U . .
C36 C 0.9081(8) -0.0981(7) 0.0480(8) 0.036(3) Uani 1 1 d . . .
H36 H 0.9459 -0.1229 0.0854 0.043 Uiso 1 1 calc R . .
C37 C 0.8403(9) -0.1434(7) -0.0078(8) 0.043(4) Uani 1 1 d . . .
H37 H 0.8329 -0.1992 -0.0082 0.051 Uiso 1 1 calc R . .
C38 C 0.7856(8) -0.1084(8) -0.0608(8) 0.038(3) Uani 1 1 d U B .
H38 H 0.7399 -0.1392 -0.0979 0.046 Uiso 1 1 calc R . .
C39 C 0.7978(8) -0.0251(8) -0.0600(7) 0.035(3) Uani 1 1 d . . .
C41 C 0.7090(8) 0.0437(7) 0.6109(7) 0.032(3) Uani 1 1 d . . .
H41A H 0.7611 0.0739 0.5996 0.039 Uiso 1 1 calc R . .
H41B H 0.6800 0.0817 0.6324 0.039 Uiso 1 1 calc R . .
C42 C 0.6494(8) 0.0068(7) 0.5362(7) 0.025(3) Uani 1 1 d . . .
C43 C 0.6299(8) -0.0772(8) 0.5205(7) 0.031(3) Uani 1 1 d . . .
H43 H 0.6581 -0.1112 0.5552 0.037 Uiso 1 1 calc R . .
C44 C 0.5691(8) -0.1078(7) 0.4536(8) 0.030(3) Uani 1 1 d . . .
H44 H 0.5559 -0.1631 0.4425 0.036 Uiso 1 1 calc R . .
C45 C 0.5277(7) -0.0582(8) 0.4032(7) 0.027(3) Uani 1 1 d . . .
H45 H 0.4849 -0.0790 0.3583 0.033 Uiso 1 1 calc R . .
C46 C 0.5503(8) 0.0250(8) 0.4198(8) 0.025(3) Uani 1 1 d . . .
C47 C 0.5087(7) 0.0797(8) 0.3661(7) 0.024(3) Uani 1 1 d . . .
H47 H 0.4564 0.0607 0.3291 0.028 Uiso 1 1 calc R . .
C48 C 0.4069(7) 0.1844(7) 0.2818(6) 0.026(3) Uani 1 1 d . . .
H48A H 0.4027 0.1474 0.2386 0.040 Uiso 1 1 calc R . .
H48B H 0.3841 0.2315 0.2624 0.040 Uiso 1 1 calc R . .
H48C H 0.3737 0.1593 0.3161 0.040 Uiso 1 1 calc R . .
C49 C 0.5440(8) 0.2843(8) 0.3258(6) 0.020(3) Uani 1 1 d . . .
C50 C 0.6345(8) 0.3006(7) 0.3410(6) 0.019(3) Uani 1 1 d . . .
H50 H 0.6687 0.2604 0.3521 0.023 Uiso 1 1 calc R . .
C51 C 0.6710(8) 0.3802(8) 0.3389(6) 0.021(3) Uani 1 1 d . . .
C52 C 0.5374(9) 0.4156(8) 0.3111(8) 0.040(4) Uani 1 1 d . . .
C53 C 0.4809(8) 0.4803(8) 0.2937(10) 0.073(5) Uani 1 1 d . . .
H53A H 0.4643 0.4947 0.3400 0.109 Uiso 1 1 calc R . .
H53B H 0.4292 0.4605 0.2529 0.109 Uiso 1 1 calc R . .
H53C H 0.5133 0.5267 0.2770 0.109 Uiso 1 1 calc R . .
C54 C 0.8002(7) 0.4902(6) 0.3567(7) 0.030(3) Uani 1 1 d . . .
H54A H 0.8365 0.5048 0.4086 0.045 Uiso 1 1 calc R . .
H54B H 0.7544 0.5222 0.3453 0.045 Uiso 1 1 calc R . .
H54C H 0.8352 0.4994 0.3196 0.045 Uiso 1 1 calc R . .
C55 C 0.8960(8) 0.3685(6) 0.3725(5) 0.015(3) Uani 1 1 d . . .
H55 H 0.9204 0.4225 0.3833 0.018 Uiso 1 1 calc R . .
C56 C 0.9532(8) 0.3086(6) 0.3742(6) 0.016(3) Uani 1 1 d . . .
C57 C 0.9216(7) 0.2310(7) 0.3414(6) 0.016(3) Uani 1 1 d . . .
H57 H 0.8624 0.2148 0.3174 0.019 Uiso 1 1 calc R . .
C58 C 0.9804(8) 0.1789(7) 0.3454(6) 0.015(3) Uani 1 1 d . . .
C59 C 1.0923(8) 0.2797(7) 0.4085(6) 0.019(3) Uani 1 1 d . . .
C60 C 1.1877(7) 0.3050(6) 0.4444(7) 0.020(3) Uani 1 1 d . . .
C61 C 1.2504(8) 0.2808(7) 0.4108(7) 0.030(3) Uani 1 1 d . . .
H61 H 1.2329 0.2486 0.3646 0.036 Uiso 1 1 calc R . .
C62 C 1.3386(7) 0.3045(7) 0.4460(7) 0.027(3) Uani 1 1 d . . .
H62 H 1.3802 0.2911 0.4216 0.033 Uiso 1 1 calc R . .
C63 C 1.3649(8) 0.3474(7) 0.5163(7) 0.031(3) Uani 1 1 d . . .
H63 H 1.4244 0.3611 0.5408 0.038 Uiso 1 1 calc R . .
C64 C 1.3031(8) 0.3705(7) 0.5514(8) 0.039(3) Uani 1 1 d . . .
H64 H 1.3207 0.4000 0.5992 0.047 Uiso 1 1 calc R . .
C65 C 1.2147(7) 0.3490(6) 0.5141(7) 0.025(3) Uani 1 1 d . . .
H65 H 1.1731 0.3649 0.5371 0.030 Uiso 1 1 calc R . .
C66 C 0.9540(8) 0.0973(7) 0.3148(7) 0.017(3) Uani 1 1 d . . .
H66 H 0.9850 0.0570 0.3357 0.020 Uiso 1 1 calc R . .
C67 C 0.8945(7) -0.0615(6) 0.2567(7) 0.029(3) Uani 1 1 d . . .
H67A H 0.9502 -0.0591 0.2446 0.043 Uiso 1 1 calc R . .
H67B H 0.8567 -0.1104 0.2335 0.043 Uiso 1 1 calc R . .
H67C H 0.9027 -0.0603 0.3125 0.043 Uiso 1 1 calc R . .
C68 C 0.7852(7) 0.0016(7) 0.1603(7) 0.015(3) Uani 1 1 d . . .
C69 C 0.7595(7) 0.0691(7) 0.1237(7) 0.017(3) Uani 1 1 d . . .
H69 H 0.7880 0.1207 0.1421 0.020 Uiso 1 1 calc R . .
C70 C 0.6904(7) 0.0557(7) 0.0595(7) 0.019(3) Uani 1 1 d . . .
C71 C 0.6754(7) -0.0788(7) 0.0730(7) 0.021(3) Uani 1 1 d U . .
C72 C 0.6301(7) -0.1621(6) 0.0451(7) 0.030(3) Uani 1 1 d . . .
H72A H 0.6730 -0.1959 0.0440 0.045 Uiso 1 1 calc R . .
H72B H 0.5929 -0.1614 -0.0067 0.045 Uiso 1 1 calc R . .
H72C H 0.5953 -0.1827 0.0799 0.045 Uiso 1 1 calc R . .
C73 C 0.5761(7) 0.1224(7) -0.0310(7) 0.034(3) Uani 1 1 d . . .
H73A H 0.5540 0.1662 -0.0117 0.051 Uiso 1 1 calc R . .
H73B H 0.5389 0.0727 -0.0274 0.051 Uiso 1 1 calc R . .
H73C H 0.5768 0.1295 -0.0847 0.051 Uiso 1 1 calc R . .
C74 C 0.7142(8) 0.2455(8) -0.0231(7) 0.028(3) Uani 1 1 d . . .
H74 H 0.6568 0.2539 -0.0429 0.034 Uiso 1 1 calc R . .
C75 C 0.7882(8) 0.3042(7) -0.0325(6) 0.025(3) Uani 1 1 d . . .
C76 C 0.7767(8) 0.3828(8) -0.0485(8) 0.045(4) Uani 1 1 d . . .
H76 H 0.7223 0.3981 -0.0532 0.054 Uiso 1 1 calc R . .
C77 C 0.8468(9) 0.4377(7) -0.0574(8) 0.048(4) Uani 1 1 d . . .
H77 H 0.8405 0.4906 -0.0678 0.058 Uiso 1 1 calc R . .
C78 C 0.9277(8) 0.4123(8) -0.0506(7) 0.040(3) Uani 1 1 d . . .
H78 H 0.9757 0.4481 -0.0572 0.048 Uiso 1 1 calc R . .
C79 C 0.9354(8) 0.3345(7) -0.0342(6) 0.024(3) Uani 1 1 d . . .
C80 C 1.0196(8) 0.3023(7) -0.0265(7) 0.037(3) Uani 1 1 d . . .
H80A H 1.0395 0.2869 0.0268 0.044 Uiso 1 1 calc R . .
H80B H 1.0077 0.2542 -0.0608 0.044 Uiso 1 1 calc R . .
C81 C 1.1985(10) 0.3187(9) 0.7752(9) 0.058(4) Uani 1 1 d . . .
C82 C 0.5010(16) 0.717(2) 0.2232(17) 0.151(9) Uani 1 1 d DU . .
C83 C 0.8758(10) 0.1670(11) 0.7794(10) 0.067(5) Uani 1 1 d . . .
C84 C 0.8386(11) 0.2371(11) 0.7474(10) 0.091(6) Uani 1 1 d . . .
H84A H 0.8116 0.2265 0.6924 0.137 Uiso 1 1 calc R . .
H84B H 0.8845 0.2830 0.7549 0.137 Uiso 1 1 calc R . .
H84C H 0.7954 0.2478 0.7738 0.137 Uiso 1 1 calc R . .
N1 N 0.7447(6) 0.3105(6) 0.5362(5) 0.024(2) Uani 1 1 d . . .
N2 N 0.8289(6) 0.1883(6) 0.4976(5) 0.018(2) Uani 1 1 d . . .
N3 N 0.8652(6) 0.1209(6) 0.4920(5) 0.024(2) Uani 1 1 d . . .
N4 N 0.8276(6) -0.0138(6) 0.4483(5) 0.021(2) Uani 1 1 d . . .
N5 N 0.7103(6) -0.0588(6) 0.3351(5) 0.020(2) Uani 1 1 d . . .
N6 N 0.6349(6) 0.0305(6) 0.2593(5) 0.019(2) Uani 1 1 d . . .
N7 N 0.6406(6) 0.1079(6) 0.2383(6) 0.020(2) Uani 1 1 d . . .
N8 N 0.5233(6) 0.2451(5) 0.1339(5) 0.026(2) Uani 1 1 d . . .
N9 N 0.6159(7) 0.3681(6) 0.1207(6) 0.040(3) Uani 1 1 d . . .
N10 N 0.8392(7) 0.3473(5) 0.1636(5) 0.021(2) Uani 1 1 d . . .
N11 N 0.9194(6) 0.3940(5) 0.1712(5) 0.022(2) Uani 1 1 d . . .
N12 N 1.0683(7) 0.3993(5) 0.2000(5) 0.023(2) Uani 1 1 d . . .
N13 N 1.1351(6) 0.2810(6) 0.2046(5) 0.023(2) Uani 1 1 d . . .
N14 N 1.0552(6) 0.1548(6) 0.1698(5) 0.018(2) Uani 1 1 d . . .
N15 N 0.9881(6) 0.1110(6) 0.1162(5) 0.020(2) Uani 1 1 d . B .
N16 N 0.8639(6) 0.0214(5) -0.0076(6) 0.027(2) Uani 1 1 d . B .
N17 N 0.6111(7) 0.0565(5) 0.4851(6) 0.025(2) Uani 1 1 d . . .
N18 N 0.5433(5) 0.1542(6) 0.3693(5) 0.020(2) Uani 1 1 d . . .
N19 N 0.4994(6) 0.2071(6) 0.3251(5) 0.020(2) Uani 1 1 d . . .
N20 N 0.6231(7) 0.4398(6) 0.3272(6) 0.030(2) Uani 1 1 d . . .
N21 N 0.4933(6) 0.3410(6) 0.3084(5) 0.027(2) Uani 1 1 d . . .
N22 N 0.7615(6) 0.4052(5) 0.3514(5) 0.021(2) Uani 1 1 d . . .
N23 N 0.8118(7) 0.3473(5) 0.3564(5) 0.017(2) Uani 1 1 d . . .
N24 N 1.0392(7) 0.3335(5) 0.4071(5) 0.021(2) Uani 1 1 d . . .
N25 N 1.0670(6) 0.2024(5) 0.3805(5) 0.016(2) Uani 1 1 d . . .
N26 N 0.8854(7) 0.0823(5) 0.2570(6) 0.018(2) Uani 1 1 d . . .
N27 N 0.8547(6) 0.0073(6) 0.2256(6) 0.019(2) Uani 1 1 d . . .
N28 N 0.7443(6) -0.0726(6) 0.1335(5) 0.024(2) Uani 1 1 d . . .
N29 N 0.6445(5) -0.0180(6) 0.0332(5) 0.018(2) Uani 1 1 d . . .
N30 N 0.6648(6) 0.1204(6) 0.0156(5) 0.023(2) Uani 1 1 d . . .
N31 N 0.7306(6) 0.1811(6) 0.0135(5) 0.021(2) Uani 1 1 d . B .
N32 N 0.8666(7) 0.2800(5) -0.0249(5) 0.025(2) Uani 1 1 d . B .
N33 N 0.9031(9) 0.1115(9) 0.8046(10) 0.099(6) Uani 1 1 d . . .
O1 O 0.5669(5) 0.2858(4) 0.5262(4) 0.031(2) Uani 1 1 d . . .
H1 H 0.5125 0.2707 0.5368 0.037 Uiso 1 1 calc R . .
O3 O 0.7350(5) -0.0099(4) 0.6679(4) 0.033(2) Uani 1 1 d . . .
H3A H 0.7608 -0.0417 0.6510 0.049 Uiso 1 1 calc R . .
O4 O 1.0876(5) 0.3563(4) -0.0445(5) 0.037(2) Uani 1 1 d . . .
H4A H 1.0718 0.3693 -0.0897 0.056 Uiso 1 1 calc R . .
O5 O 0.8529(5) 0.9372(5) 0.6025(5) 0.036(2) Uani 1 1 d . . .
H5A H 0.853(7) 0.946(7) 0.545(8) 0.053 Uiso 1 1 d . . .
H5B H 0.877(8) 0.890(7) 0.595(7) 0.053 Uiso 1 1 d . . .
O11 O 1.0585(6) 0.2270(5) 0.6983(5) 0.063(3) Uani 1 1 d . . .
O12 O 1.0445(7) 0.3206(7) 0.7975(6) 0.092(4) Uani 1 1 d . . .
O13 O 1.0749(5) 0.3678(5) 0.6804(6) 0.061(3) Uani 1 1 d . . .
O21 O 0.3487(13) 0.6560(10) 0.2438(12) 0.203(8) Uani 1 1 d DU . .
O22 O 0.4001(10) 0.7752(9) 0.3307(10) 0.145(5) Uani 1 1 d U . .
O23 O 0.3791(12) 0.7975(12) 0.2088(12) 0.174(7) Uani 1 1 d U . .
F11 F 1.2145(8) 0.2664(5) 0.8323(7) 0.137(5) Uani 1 1 d . . .
F12 F 1.2421(6) 0.3112(7) 0.7240(7) 0.122(5) Uani 1 1 d . . .
F13 F 1.2290(5) 0.3903(5) 0.8127(4) 0.061(2) Uani 1 1 d . . .
F21 F 0.4729(17) 0.6786(15) 0.1491(13) 0.37(2) Uani 1 1 d D . .
F22 F 0.5556(16) 0.7748(9) 0.2244(16) 0.343(18) Uani 1 1 d D . .
F23 F 0.5314(15) 0.6651(14) 0.2692(17) 0.57(4) Uani 1 1 d D . .
S1 S 1.0823(2) 0.30562(19) 0.73355(19) 0.0380(9) Uani 1 1 d . . .
S2 S 0.4059(5) 0.7384(4) 0.2567(3) 0.121(2) Uani 1 1 d D . .
Ag1 Ag 0.66232(5) 0.18896(5) 0.49167(5) 0.0268(3) Uani 1 1 d . . .
Ag2 Ag 0.87858(5) 0.15542(5) 0.00653(5) 0.0280(3) Uani 1 1 d . . .
C20 C 0.4551(9) 0.3562(8) 0.0827(8) 0.051(4) Uani 1 1 d U . .
C21 C 0.4528(14) 0.4112(13) 0.0212(14) 0.073(9) Uani 0.69(2) 1 d P A 1
H21 H 0.5031 0.4271 0.0040 0.088 Uiso 0.69(2) 1 calc PR A 1
C22 C 0.3780(15) 0.4404(14) -0.0123(17) 0.094(11) Uani 0.69(2) 1 d P A 1
H22 H 0.3788 0.4797 -0.0486 0.113 Uiso 0.69(2) 1 calc PR A 1
C23 C 0.3009(12) 0.4110(15) 0.0081(16) 0.045(6) Uani 0.69(2) 1 d P A 1
H23 H 0.2482 0.4277 -0.0156 0.054 Uiso 0.69(2) 1 calc PR A 1
C24 C 0.3051(16) 0.3640(17) 0.0565(17) 0.016(8) Uani 0.69(2) 1 d PU A 1
H24 H 0.2549 0.3495 0.0743 0.019 Uiso 0.69(2) 1 calc PR A 1
C25 C 0.3799(17) 0.3259(16) 0.0920(15) 0.011(8) Uani 0.69(2) 1 d PU A 1
H25 H 0.3732 0.2806 0.1207 0.013 Uiso 0.69(2) 1 calc PR A 1
C22A C 0.400(3) 0.495(3) 0.079(3) 0.059(15) Uani 0.31(2) 1 d PU A 2
H21A H 0.4065 0.5507 0.0798 0.071 Uiso 0.31(2) 1 calc PR A 2
C21A C 0.474(3) 0.455(3) 0.105(3) 0.055(15) Uani 0.31(2) 1 d PU A 2
H22A H 0.5285 0.4824 0.1319 0.066 Uiso 0.31(2) 1 calc PR A 2
C23A C 0.318(3) 0.446(3) 0.051(3) 0.023(13) Uani 0.31(2) 1 d PU A 2
H23A H 0.2722 0.4697 0.0226 0.028 Uiso 0.31(2) 1 calc PR A 2
C24A C 0.293(4) 0.344(3) 0.066(3) 0.016(19) Uani 0.31(2) 1 d PU A 2
H24A H 0.2393 0.3107 0.0585 0.019 Uiso 0.31(2) 1 calc PR A 2
C25A C 0.360(6) 0.330(6) 0.087(5) 0.07(3) Uani 0.31(2) 1 d PU A 2
H25A H 0.3581 0.2864 0.1194 0.082 Uiso 0.31(2) 1 calc PR A 2
O2 O 0.6464(9) -0.0331(8) -0.1291(8) 0.028(6) Uani 0.500(19) 1 d P B 3
H2 H 0.6335 -0.0407 -0.0873 0.042 Uiso 0.500(19) 1 calc PR B 3
C40 C 0.741(2) 0.0045(19) -0.1137(19) 0.024(9) Uani 0.500(19) 1 d PU B 3
H40A H 0.7579 0.0015 -0.1625 0.029 Uiso 0.500(19) 1 calc PR B 3
H40B H 0.7452 0.0611 -0.0993 0.029 Uiso 0.500(19) 1 calc PR B 3
O2A O 0.6911(11) -0.0179(10) -0.1935(10) 0.049(7) Uani 0.500(19) 1 d P B 4
H2A H 0.6591 -0.0562 -0.1818 0.074 Uiso 0.500(19) 1 calc PR B 4
C40A C 0.7335(19) 0.0297(18) -0.1283(16) 0.023(10) Uani 0.500(19) 1 d PU B 4
H40C H 0.6910 0.0496 -0.1053 0.028 Uiso 0.500(19) 1 calc PR B 4
H40D H 0.7706 0.0755 -0.1421 0.028 Uiso 0.500(19) 1 calc PR B 4


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.409(13) . ?
C1 C2 1.508(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.340(13) . ?
C2 C3 1.377(14) . ?
C3 C4 1.380(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(14) . ?
C5 H5 0.9300 . ?
C6 N1 1.365(13) . ?
C6 C7 1.480(15) . ?
C7 N2 1.275(13) . ?
C7 H7 0.9300 . ?
C8 N3 1.444(13) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.347(13) . ?
C9 C10 1.372(15) . ?
C9 N3 1.393(14) . ?
C10 C11 1.393(15) . ?
C10 H10 0.9300 . ?
C11 N5 1.357(13) . ?
C11 N6 1.369(14) . ?
C12 N5 1.330(14) . ?
C12 N4 1.343(14) . ?
C12 C13 1.515(15) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N6 1.453(13) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N7 1.271(13) . ?
C15 C16 1.471(15) . ?
C15 H15 0.9300 . ?
C16 N8 1.335(13) . ?
C16 C17 1.372(14) . ?
C17 C18 1.374(15) . ?
C17 H17 0.9300 . ?
C18 N9 1.335(14) . ?
C18 C26 1.476(16) . ?
C19 N8 1.336(14) . ?
C19 N9 1.374(15) . ?
C19 C20 1.480(18) . ?
C26 N10 1.272(13) . ?
C26 H26 0.9300 . ?
C27 N11 1.446(13) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N12 1.334(13) . ?
C28 N11 1.381(13) . ?
C28 C29 1.394(15) . ?
C29 C30 1.384(15) . ?
C29 H29 0.9300 . ?
C30 N13 1.332(13) . ?
C30 N14 1.404(13) . ?
C31 N13 1.339(14) . ?
C31 N12 1.342(14) . ?
C31 C32 1.508(15) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N14 1.472(13) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N15 1.285(13) . ?
C34 C35 1.438(16) . ?
C34 H34 0.9300 . ?
C35 N16 1.349(14) . ?
C35 C36 1.400(15) . ?
C36 C37 1.384(16) . ?
C36 H36 0.9300 . ?
C37 C38 1.327(16) . ?
C37 H37 0.9300 . ?
C38 C39 1.387(17) . ?
C38 H38 0.9300 . ?
C39 C40 1.31(3) . ?
C39 N16 1.348(14) . ?
C39 C40A 1.76(3) . ?
C41 O3 1.395(12) . ?
C41 C42 1.483(16) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 N17 1.342(14) . ?
C42 C43 1.411(16) . ?
C43 C44 1.363(16) . ?
C43 H43 0.9300 . ?
C44 C45 1.356(15) . ?
C44 H44 0.9300 . ?
C45 C46 1.400(15) . ?
C45 H45 0.9300 . ?
C46 N17 1.348(14) . ?
C46 C47 1.448(16) . ?
C47 N18 1.285(13) . ?
C47 H47 0.9300 . ?
C48 N19 1.470(13) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 N21 1.341(13) . ?
C49 N19 1.381(13) . ?
C49 C50 1.383(15) . ?
C50 C51 1.383(15) . ?
C50 H50 0.9300 . ?
C51 N20 1.346(14) . ?
C51 N22 1.399(13) . ?
C52 N20 1.321(15) . ?
C52 N21 1.336(15) . ?
C52 C53 1.510(16) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 N22 1.460(13) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 N23 1.292(12) . ?
C55 C56 1.462(14) . ?
C55 H55 0.9300 . ?
C56 N24 1.346(13) . ?
C56 C57 1.388(14) . ?
C57 C58 1.374(14) . ?
C57 H57 0.9300 . ?
C58 N25 1.359(13) . ?
C58 C66 1.431(14) . ?
C59 N24 1.332(13) . ?
C59 N25 1.351(13) . ?
C59 C60 1.486(15) . ?
C60 C65 1.365(15) . ?
C60 C61 1.389(15) . ?
C61 C62 1.382(15) . ?
C61 H61 0.9300 . ?
C62 C63 1.364(15) . ?
C62 H62 0.9300 . ?
C63 C64 1.387(15) . ?
C63 H63 0.9300 . ?
C64 C65 1.388(15) . ?
C64 H64 0.9300 . ?
C65 H65 0.9300 . ?
C66 N26 1.287(13) . ?
C66 H66 0.9300 . ?
C67 N27 1.459(13) . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 N28 1.338(13) . ?
C68 N27 1.378(13) . ?
C68 C69 1.385(14) . ?
C69 C70 1.359(14) . ?
C69 H69 0.9300 . ?
C70 N29 1.351(13) . ?
C70 N30 1.402(13) . ?
C71 N28 1.320(13) . ?
C71 N29 1.342(13) . ?
C71 C72 1.491(15) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 N30 1.457(13) . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 N31 1.301(13) . ?
C74 C75 1.462(16) . ?
C74 H74 0.9300 . ?
C75 N32 1.353(13) . ?
C75 C76 1.390(16) . ?
C76 C77 1.377(16) . ?
C76 H76 0.9300 . ?
C77 C78 1.401(17) . ?
C77 H77 0.9300 . ?
C78 C79 1.367(16) . ?
C78 H78 0.9300 . ?
C79 N32 1.361(13) . ?
C79 C80 1.502(16) . ?
C80 O4 1.405(13) . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C81 F12 1.284(18) . ?
C81 F13 1.330(14) . ?
C81 F11 1.354(16) . ?
C81 S1 1.794(16) . ?
C82 F22 1.19(3) . ?
C82 F23 1.28(3) . ?
C82 F21 1.39(3) . ?
C82 S2 1.840(17) . ?
C83 N33 1.144(19) . ?
C83 C84 1.47(2) . ?
C84 H84A 0.9600 . ?
C84 H84B 0.9600 . ?
C84 H84C 0.9600 . ?
N1 Ag1 2.267(9) . ?
N2 N3 1.367(12) . ?
N2 Ag1 2.637(8) . ?
N6 N7 1.358(12) . ?
N10 N11 1.368(12) . ?
N14 N15 1.349(12) . ?
N15 Ag2 2.479(9) . ?
N16 Ag2 2.240(9) . ?
N17 Ag1 2.246(9) . ?
N18 N19 1.359(12) . ?
N18 Ag1 2.489(9) . ?
N22 N23 1.349(11) . ?
N26 N27 1.342(11) . ?
N30 N31 1.354(12) . ?
N31 Ag2 2.499(8) . ?
N32 Ag2 2.208(9) . ?
O1 Ag1 2.564(7) . ?
O1 H1 0.9300 . ?
O3 H3A 0.8200 . ?
O4 H4A 0.8200 . ?
O5 H5A 1.03(13) . ?
O5 H5B 0.96(12) . ?
O11 S1 1.411(8) . ?
O12 S1 1.443(10) . ?
O13 S1 1.417(9) . ?
O21 S2 1.519(15) . ?
O22 S2 1.467(16) . ?
O23 S2 1.368(19) . ?
C20 C25 1.28(3) . ?
C20 C21 1.44(2) . ?
C20 C25A 1.53(9) . ?
C20 C21A 1.67(5) . ?
C21 C22 1.36(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.39(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.17(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.45(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C22A C23A 1.41(6) . ?
C22A C21A 1.42(6) . ?
C22A H21A 0.9300 . ?
C21A H22A 0.9300 . ?
C23A C24A 1.74(7) . ?
C23A H23A 0.9300 . ?
C24A C25A 1.10(10) . ?
C24A H24A 0.9300 . ?
C25A H25A 0.9300 . ?
O2 C40 1.49(3) . ?
O2 H2 0.8200 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
O2A C40A 1.36(3) . ?
O2A H2A 0.8200 . ?
C40A H40C 0.9700 . ?
C40A H40D 0.9700 . ?

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 C1 C2 114.8(9) . . ?
O1 C1 H1A 108.6 . . ?
C2 C1 H1A 108.6 . . ?
O1 C1 H1B 108.6 . . ?
C2 C1 H1B 108.6 . . ?
H1A C1 H1B 107.5 . . ?
N1 C2 C3 122.7(10) . . ?
N1 C2 C1 118.2(10) . . ?
C3 C2 C1 119.0(11) . . ?
C2 C3 C4 119.2(10) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.6(10) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C6 C5 C4 120.0(11) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
N1 C6 C5 121.9(10) . . ?
N1 C6 C7 117.6(10) . . ?
C5 C6 C7 120.5(11) . . ?
N2 C7 C6 120.4(10) . . ?
N2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 122.7(11) . . ?
N4 C9 N3 116.2(11) . . ?
C10 C9 N3 121.1(10) . . ?
C9 C10 C11 117.2(11) . . ?
C9 C10 H10 121.4 . . ?
C11 C10 H10 121.4 . . ?
N5 C11 N6 116.1(11) . . ?
N5 C11 C10 121.4(11) . . ?
N6 C11 C10 122.5(11) . . ?
N5 C12 N4 127.1(9) . . ?
N5 C12 C13 116.7(11) . . ?
N4 C12 C13 116.2(11) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 116.5(10) . . ?
N7 C15 H15 121.8 . . ?
C16 C15 H15 121.8 . . ?
N8 C16 C17 121.5(10) . . ?
N8 C16 C15 116.2(10) . . ?
C17 C16 C15 122.2(10) . . ?
C16 C17 C18 118.7(10) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
N9 C18 C17 121.4(10) . . ?
N9 C18 C26 116.7(10) . . ?
C17 C18 C26 121.8(11) . . ?
N8 C19 N9 124.7(10) . . ?
N8 C19 C20 116.2(11) . . ?
N9 C19 C20 119.2(12) . . ?
N10 C26 C18 118.8(10) . . ?
N10 C26 H26 120.6 . . ?
C18 C26 H26 120.6 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N12 C28 N11 115.0(10) . . ?
N12 C28 C29 122.2(10) . . ?
N11 C28 C29 122.8(11) . . ?
C30 C29 C28 116.2(10) . . ?
C30 C29 H29 121.9 . . ?
C28 C29 H29 121.9 . . ?
N13 C30 C29 123.4(10) . . ?
N13 C30 N14 113.8(10) . . ?
C29 C30 N14 122.8(11) . . ?
N13 C31 N12 127.1(10) . . ?
N13 C31 C32 116.9(11) . . ?
N12 C31 C32 116.0(11) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N14 C33 H33A 109.5 . . ?
N14 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N14 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N15 C34 C35 122.2(11) . . ?
N15 C34 H34 118.9 . . ?
C35 C34 H34 118.9 . . ?
N16 C35 C36 120.4(11) . . ?
N16 C35 C34 119.3(10) . . ?
C36 C35 C34 120.2(12) . . ?
C37 C36 C35 118.6(12) . . ?
C37 C36 H36 120.7 . . ?
C35 C36 H36 120.7 . . ?
C38 C37 C36 121.0(12) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C37 C38 C39 118.9(12) . . ?
C37 C38 H38 120.5 . . ?
C39 C38 H38 120.5 . . ?
C40 C39 N16 122.8(16) . . ?
C40 C39 C38 115.0(17) . . ?
N16 C39 C38 122.2(12) . . ?
C40 C39 C40A 9.5(18) . . ?
N16 C39 C40A 113.6(13) . . ?
C38 C39 C40A 124.2(15) . . ?
O3 C41 C42 115.5(10) . . ?
O3 C41 H41A 108.4 . . ?
C42 C41 H41A 108.4 . . ?
O3 C41 H41B 108.4 . . ?
C42 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
N17 C42 C43 120.8(11) . . ?
N17 C42 C41 117.3(11) . . ?
C43 C42 C41 121.8(12) . . ?
C44 C43 C42 119.1(11) . . ?
C44 C43 H43 120.5 . . ?
C42 C43 H43 120.5 . . ?
C45 C44 C43 120.4(11) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 118.9(11) . . ?
C44 C45 H45 120.5 . . ?
C46 C45 H45 120.5 . . ?
N17 C46 C45 121.6(11) . . ?
N17 C46 C47 118.2(11) . . ?
C45 C46 C47 120.2(12) . . ?
N18 C47 C46 120.6(11) . . ?
N18 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
N19 C48 H48A 109.5 . . ?
N19 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N19 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N21 C49 N19 115.2(10) . . ?
N21 C49 C50 123.0(11) . . ?
N19 C49 C50 121.8(11) . . ?
C51 C50 C49 116.0(10) . . ?
C51 C50 H50 122.0 . . ?
C49 C50 H50 122.0 . . ?
N20 C51 C50 122.9(10) . . ?
N20 C51 N22 114.8(11) . . ?
C50 C51 N22 122.3(11) . . ?
N20 C52 N21 128.6(10) . . ?
N20 C52 C53 116.4(12) . . ?
N21 C52 C53 114.9(11) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N22 C54 H54A 109.5 . . ?
N22 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
N22 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N23 C55 C56 120.8(10) . . ?
N23 C55 H55 119.6 . . ?
C56 C55 H55 119.6 . . ?
N24 C56 C57 121.5(10) . . ?
N24 C56 C55 116.3(10) . . ?
C57 C56 C55 122.1(10) . . ?
C58 C57 C56 118.1(10) . . ?
C58 C57 H57 121.0 . . ?
C56 C57 H57 121.0 . . ?
N25 C58 C57 121.1(10) . . ?
N25 C58 C66 116.6(10) . . ?
C57 C58 C66 122.3(10) . . ?
N24 C59 N25 125.5(10) . . ?
N24 C59 C60 118.6(10) . . ?
N25 C59 C60 115.9(10) . . ?
C65 C60 C61 119.0(10) . . ?
C65 C60 C59 119.4(11) . . ?
C61 C60 C59 121.5(11) . . ?
C62 C61 C60 120.1(11) . . ?
C62 C61 H61 119.9 . . ?
C60 C61 H61 119.9 . . ?
C63 C62 C61 120.4(11) . . ?
C63 C62 H62 119.8 . . ?
C61 C62 H62 119.8 . . ?
C62 C63 C64 120.0(11) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 C65 119.1(11) . . ?
C63 C64 H64 120.4 . . ?
C65 C64 H64 120.4 . . ?
C60 C65 C64 121.2(11) . . ?
C60 C65 H65 119.4 . . ?
C64 C65 H65 119.4 . . ?
N26 C66 C58 116.7(10) . . ?
N26 C66 H66 121.6 . . ?
C58 C66 H66 121.6 . . ?
N27 C67 H67A 109.5 . . ?
N27 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
N27 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N28 C68 N27 116.4(10) . . ?
N28 C68 C69 121.7(10) . . ?
N27 C68 C69 121.9(10) . . ?
C70 C69 C68 116.4(10) . . ?
C70 C69 H69 121.8 . . ?
C68 C69 H69 121.8 . . ?
N29 C70 C69 123.6(10) . . ?
N29 C70 N30 116.6(10) . . ?
C69 C70 N30 119.8(11) . . ?
N28 C71 N29 126.3(10) . . ?
N28 C71 C72 116.1(10) . . ?
N29 C71 C72 117.6(10) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N30 C73 H73A 109.5 . . ?
N30 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
N30 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N31 C74 C75 118.3(11) . . ?
N31 C74 H74 120.8 . . ?
C75 C74 H74 120.8 . . ?
N32 C75 C76 121.8(10) . . ?
N32 C75 C74 118.4(11) . . ?
C76 C75 C74 119.8(11) . . ?
C77 C76 C75 119.4(11) . . ?
C77 C76 H76 120.3 . . ?
C75 C76 H76 120.3 . . ?
C76 C77 C78 118.8(11) . . ?
C76 C77 H77 120.6 . . ?
C78 C77 H77 120.6 . . ?
C79 C78 C77 119.4(11) . . ?
C79 C78 H78 120.3 . . ?
C77 C78 H78 120.3 . . ?
N32 C79 C78 122.2(10) . . ?
N32 C79 C80 115.1(10) . . ?
C78 C79 C80 122.7(11) . . ?
O4 C80 C79 114.8(10) . . ?
O4 C80 H80A 108.6 . . ?
C79 C80 H80A 108.6 . . ?
O4 C80 H80B 108.6 . . ?
C79 C80 H80B 108.6 . . ?
H80A C80 H80B 107.5 . . ?
F12 C81 F13 107.8(14) . . ?
F12 C81 F11 111.9(13) . . ?
F13 C81 F11 103.8(11) . . ?
F12 C81 S1 113.1(10) . . ?
F13 C81 S1 111.5(10) . . ?
F11 C81 S1 108.4(12) . . ?
F22 C82 F23 111(2) . . ?
F22 C82 F21 111(2) . . ?
F23 C82 F21 106(2) . . ?
F22 C82 S2 114(2) . . ?
F23 C82 S2 104(2) . . ?
F21 C82 S2 110(2) . . ?
N33 C83 C84 178.6(18) . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C2 N1 C6 117.6(9) . . ?
C2 N1 Ag1 122.0(7) . . ?
C6 N1 Ag1 120.3(8) . . ?
C7 N2 N3 119.8(9) . . ?
C7 N2 Ag1 107.8(7) . . ?
N3 N2 Ag1 125.0(7) . . ?
N2 N3 C9 114.6(9) . . ?
N2 N3 C8 121.8(9) . . ?
C9 N3 C8 123.5(9) . . ?
C12 N4 C9 115.4(9) . . ?
C12 N5 C11 116.0(10) . . ?
N7 N6 C11 113.8(9) . . ?
N7 N6 C14 123.0(9) . . ?
C11 N6 C14 123.2(9) . . ?
C15 N7 N6 120.3(9) . . ?
C16 N8 C19 117.2(9) . . ?
C18 N9 C19 116.5(10) . . ?
C26 N10 N11 118.0(9) . . ?
N10 N11 C28 115.8(9) . . ?
N10 N11 C27 121.8(9) . . ?
C28 N11 C27 122.3(9) . . ?
C28 N12 C31 116.0(9) . . ?
C30 N13 C31 115.2(9) . . ?
N15 N14 C30 118.7(9) . . ?
N15 N14 C33 120.5(9) . . ?
C30 N14 C33 120.8(9) . . ?
C34 N15 N14 119.6(9) . . ?
C34 N15 Ag2 109.1(8) . . ?
N14 N15 Ag2 129.8(7) . . ?
C39 N16 C35 118.9(10) . . ?
C39 N16 Ag2 124.1(8) . . ?
C35 N16 Ag2 116.4(7) . . ?
C42 N17 C46 119.2(10) . . ?
C42 N17 Ag1 122.2(8) . . ?
C46 N17 Ag1 117.6(8) . . ?
C47 N18 N19 120.4(9) . . ?
C47 N18 Ag1 110.4(7) . . ?
N19 N18 Ag1 125.7(7) . . ?
N18 N19 C49 117.1(9) . . ?
N18 N19 C48 121.4(9) . . ?
C49 N19 C48 121.4(9) . . ?
C52 N20 C51 114.7(10) . . ?
C52 N21 C49 114.5(9) . . ?
N23 N22 C51 117.1(9) . . ?
N23 N22 C54 121.0(8) . . ?
C51 N22 C54 121.8(9) . . ?
C55 N23 N22 118.5(8) . . ?
C59 N24 C56 117.0(9) . . ?
C59 N25 C58 116.7(9) . . ?
C66 N26 N27 120.9(9) . . ?
N26 N27 C68 114.2(9) . . ?
N26 N27 C67 122.3(9) . . ?
C68 N27 C67 123.4(9) . . ?
C71 N28 C68 117.1(9) . . ?
C71 N29 C70 114.7(9) . . ?
N31 N30 C70 115.4(9) . . ?
N31 N30 C73 119.9(9) . . ?
C70 N30 C73 124.5(9) . . ?
C74 N31 N30 120.7(9) . . ?
C74 N31 Ag2 109.1(7) . . ?
N30 N31 Ag2 121.8(7) . . ?
C75 N32 C79 118.4(9) . . ?
C75 N32 Ag2 118.6(7) . . ?
C79 N32 Ag2 122.9(8) . . ?
C1 O1 Ag1 109.3(6) . . ?
C1 O1 H1 125.3 . . ?
Ag1 O1 H1 125.3 . . ?
C41 O3 H3A 109.5 . . ?
C80 O4 H4A 109.5 . . ?
H5A O5 H5B 85(9) . . ?
O11 S1 O13 114.9(6) . . ?
O11 S1 O12 115.7(6) . . ?
O13 S1 O12 111.2(7) . . ?
O11 S1 C81 105.6(6) . . ?
O13 S1 C81 102.2(6) . . ?
O12 S1 C81 105.8(7) . . ?
O23 S2 O22 98.1(11) . . ?
O23 S2 O21 118.3(12) . . ?
O22 S2 O21 107.9(11) . . ?
O23 S2 C82 101.7(13) . . ?
O22 S2 C82 131.2(12) . . ?
O21 S2 C82 101.0(14) . . ?
N17 Ag1 N1 160.3(4) . . ?
N17 Ag1 N18 71.2(4) . . ?
N1 Ag1 N18 128.5(3) . . ?
N17 Ag1 O1 118.0(3) . . ?
N1 Ag1 O1 69.5(3) . . ?
N18 Ag1 O1 85.6(3) . . ?
N17 Ag1 N2 100.9(3) . . ?
N1 Ag1 N2 69.0(3) . . ?
N18 Ag1 N2 122.7(3) . . ?
O1 Ag1 N2 138.4(3) . . ?
N32 Ag2 N16 159.0(3) . . ?
N32 Ag2 N15 127.4(3) . . ?
N16 Ag2 N15 72.3(4) . . ?
N32 Ag2 N31 71.3(4) . . ?
N16 Ag2 N31 104.7(3) . . ?
N15 Ag2 N31 124.9(3) . . ?
C25 C20 C21 114.8(18) . . ?
C25 C20 C19 123.3(17) . . ?
C21 C20 C19 119.5(14) . . ?
C25 C20 C25A 8(5) . . ?
C21 C20 C25A 107(4) . . ?
C19 C20 C25A 131(4) . . ?
C25 C20 C21A 109(2) . . ?
C21 C20 C21A 60.3(18) . . ?
C19 C20 C21A 110.6(19) . . ?
C25A C20 C21A 104(4) . . ?
C22 C21 C20 121.0(19) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 120(2) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 117(2) . . ?
C24 C23 H23 121.5 . . ?
C22 C23 H23 121.5 . . ?
C23 C24 C25 127(2) . . ?
C23 C24 H24 116.3 . . ?
C25 C24 H24 116.3 . . ?
C20 C25 C24 118(2) . . ?
C20 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
C23A C22A C21A 117(4) . . ?
C23A C22A H21A 121.6 . . ?
C21A C22A H21A 121.6 . . ?
C22A C21A C20 116(4) . . ?
C22A C21A H22A 122.2 . . ?
C20 C21A H22A 122.2 . . ?
C22A C23A C24A 126(4) . . ?
C22A C23A H23A 117.1 . . ?
C24A C23A H23A 117.1 . . ?
C25A C24A C23A 100(7) . . ?
C25A C24A H24A 129.8 . . ?
C23A C24A H24A 129.8 . . ?
C24A C25A C20 142(10) . . ?
C24A C25A H25A 108.9 . . ?
C20 C25A H25A 108.9 . . ?
C40 O2 H2 109.5 . . ?
C39 C40 O2 118(2) . . ?
C39 C40 H40A 107.8 . . ?
O2 C40 H40A 107.8 . . ?
C39 C40 H40B 107.8 . . ?
O2 C40 H40B 107.8 . . ?
H40A C40 H40B 107.2 . . ?
C40A O2A H2A 109.5 . . ?
O2A C40A C39 110(2) . . ?
O2A C40A H40C 109.7 . . ?
C39 C40A H40C 109.7 . . ?
O2A C40A H40D 109.7 . . ?
C39 C40A H40D 109.7 . . ?
H40C C40A H40D 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        18.82
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.105

#===END
_database_code_depnum_ccdc_archive 'CCDC 976904'
