# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'David Gordon Billing'
_publ_contact_author_email       DAVE.BILLING@WITS.AC.ZA

_publ_section_title              
;
Inorganic-organic hybrid materials incorporating
primary cyclic ammonium cations: The lead bromide and chloride series
;
_publ_requested_category         FM
loop_
_publ_author_name
'David G. Billing'
'Andreas Lemmerer'

# Attachment 'combined_cif_corrected.cif'

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2004-11-29 at 10:30:28
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.2
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac17l_a smart

data_1
_database_code_depnum_ccdc_archive 'CCDC 708560'

_audit_creation_date             2004-11-29T10:30:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclopropylammonium)tetrabromoplumbate(II)
;
_chemical_formula_sum            'C6 H16 Br4 N2 Pb'
_chemical_formula_moiety         'Br4 Pb, 2(C3 H8 N)'
_chemical_formula_weight         643.04

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.400(3)
_cell_length_b                   7.8407(19)
_cell_length_c                   8.385(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.177(4)
_cell_angle_gamma                90
_cell_volume                     774.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    863
_cell_measurement_theta_min      3.4585
_cell_measurement_theta_max      28.2715

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rectangle
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    2.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.03
-1 0 0 0.03
0 0 1 0.105
1 0 -4 0.105
-2 3 4 0.16
0 1 -1 0.16
0 -1 0 0.2

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    21.178
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0169
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_number            4820
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             1867
_reflns_number_gt                1577
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.
;
_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)+(0.0760P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1867
_refine_ls_number_parameters     61
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.045
_refine_ls_wR_factor_ref         0.1206
_refine_ls_wR_factor_gt          0.1128
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.31
_refine_diff_density_min         -3.98
_refine_diff_density_rms         0.363

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.6816(8) 0.5951(13) 0.3120(12) 0.0399(19) Uani 1 1 d DU . .
H1 H 0.6827 0.7168 0.2768 0.048 Uiso 1 1 calc R . .
C2 C 0.5709(9) 0.5057(14) 0.2544(15) 0.053(3) Uani 1 1 d DU . .
H2A H 0.5045 0.5702 0.1837 0.063 Uiso 1 1 calc R . .
H2B H 0.5712 0.3828 0.2275 0.063 Uiso 1 1 calc R . .
C3 C 0.6197(9) 0.5573(19) 0.4322(13) 0.056(3) Uani 1 1 d DU . .
H3A H 0.5837 0.6538 0.4724 0.067 Uiso 1 1 calc R . .
H3B H 0.6503 0.4665 0.5162 0.067 Uiso 1 1 calc R . .
N1 N 0.7837(8) 0.4920(9) 0.3242(12) 0.0338(18) Uani 1 1 d U . .
H1A H 0.814 0.5258 0.2434 0.051 Uiso 1 1 calc R . .
H1B H 0.7642 0.3799 0.3094 0.051 Uiso 1 1 calc R . .
H1C H 0.8357 0.507 0.4272 0.051 Uiso 1 1 calc R . .
Br1 Br 1.24770(7) 0.58241(10) 1.08268(11) 0.0299(2) Uani 1 1 d . . .
Br2 Br 0.95317(8) 0.68780(10) 0.67325(9) 0.0278(2) Uani 1 1 d . . .
Pb1 Pb 1 0.5 1 0.01908(16) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.474(12) . ?
C1 N1 1.478(13) . ?
C1 C2 1.481(12) . ?
C1 H1 1 . ?
C2 C3 1.480(13) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
Br1 Pb1 3.0005(11) . ?
Br2 Pb1 2.9944(9) 4_575 ?
Br2 Pb1 3.0033(9) . ?
Pb1 Br2 2.9944(9) 4_576 ?
Pb1 Br2 2.9944(9) 2_746 ?
Pb1 Br1 3.0005(11) 3_767 ?
Pb1 Br2 3.0033(9) 3_767 ?

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
C3 C1 N1 117.4(9) . . ?
C3 C1 C2 60.1(4) . . ?
N1 C1 C2 116.8(9) . . ?
C3 C1 H1 116.8 . . ?
N1 C1 H1 116.8 . . ?
C2 C1 H1 116.8 . . ?
C3 C2 C1 59.7(4) . . ?
C3 C2 H2A 117.8 . . ?
C1 C2 H2A 117.8 . . ?
C3 C2 H2B 117.8 . . ?
C1 C2 H2B 117.8 . . ?
H2A C2 H2B 114.9 . . ?
C1 C3 C2 60.2(4) . . ?
C1 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C1 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Br2 Pb1 146.29(3) 4_575 . ?
Br2 Pb1 Br2 180 4_576 2_746 ?
Br2 Pb1 Br1 92.94(3) 4_576 . ?
Br2 Pb1 Br1 87.06(2) 2_746 . ?
Br2 Pb1 Br1 87.06(2) 4_576 3_767 ?
Br2 Pb1 Br1 92.94(3) 2_746 3_767 ?
Br1 Pb1 Br1 180 . 3_767 ?
Br2 Pb1 Br2 88.267(19) 4_576 3_767 ?
Br2 Pb1 Br2 91.733(19) 2_746 3_767 ?
Br1 Pb1 Br2 90.12(2) . 3_767 ?
Br1 Pb1 Br2 89.88(2) 3_767 3_767 ?
Br2 Pb1 Br2 91.733(19) 4_576 . ?
Br2 Pb1 Br2 88.267(19) 2_746 . ?
Br1 Pb1 Br2 89.88(2) . . ?
Br1 Pb1 Br2 90.12(2) 3_767 . ?
Br2 Pb1 Br2 180.0000(10) 3_767 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 107.7(10) . . . . ?
N1 C1 C3 C2 -106.7(10) . . . . ?
Pb1 Br2 Pb1 Br2 49.30(7) 4_575 . . 4_576 ?
Pb1 Br2 Pb1 Br2 -130.70(7) 4_575 . . 2_746 ?
Pb1 Br2 Pb1 Br1 -43.64(6) 4_575 . . . ?
Pb1 Br2 Pb1 Br1 136.36(6) 4_575 . . 3_767 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A

N1 H1A Br1 0.91 2.73 3.362(9) 127 3_766
N1 H1B Br1 0.91 2.52 3.357(7) 152.5 2_746
N1 H1C Br2 0.91 2.55 3.392(9) 153.6 .
_chemical_name_common            
bis(cyclopropylammonium)tetrabromoplumbate(ii)

### END

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2004-11-29 at 10:12:08
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.2
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac18l_a smart

data_2
_database_code_depnum_ccdc_archive 'CCDC 708561'

_audit_creation_date             2004-11-29T10:12:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclobutylammonium)tetrabromoplumbate(II)
;
_chemical_formula_sum            'C8 H20 Br4 N2 Pb'
_chemical_formula_moiety         'Br4 Pb, 2(C4 H10 N)'
_chemical_formula_weight         671.09

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.278(3)
_cell_length_b                   7.9463(18)
_cell_length_c                   8.4703(19)
_cell_angle_alpha                90
_cell_angle_beta                 108.430(4)
_cell_angle_gamma                90
_cell_volume                     847.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    937
_cell_measurement_theta_min      3.2345
_cell_measurement_theta_max      27.956

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    2.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.02
1 0 0 0.02
0 1 -1 0.06
0 -3 2 0.06
1 -1 -2 0.1
-1 1 2 0.1

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    19.352
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0551
_exptl_absorpt_correction_T_max  0.4444
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_number            5321
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             2050
_reflns_number_gt                1514
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.

;
_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)+(0.0424P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2050
_refine_ls_number_parameters     70
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.082
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.96
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.26
_refine_diff_density_min         -3.275
_refine_diff_density_rms         0.267

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'

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 0.7109(7) 0.5808(13) -0.1127(11) 0.042(2) Uani 1 1 d DU . .
H1 H 0.7252 0.7031 -0.0879 0.05 Uiso 1 1 calc R . .
C2 C 0.6586(9) 0.5506(17) -0.2952(12) 0.064(3) Uani 1 1 d U . .
H2A H 0.6722 0.4372 -0.3324 0.077 Uiso 1 1 calc R . .
H2B H 0.6739 0.6389 -0.367 0.077 Uiso 1 1 calc R . .
C3 C 0.5504(9) 0.568(2) -0.2714(12) 0.075(3) Uani 1 1 d DU . .
H3A H 0.4978 0.4834 -0.3321 0.09 Uiso 1 1 calc R . .
H3B H 0.5205 0.6834 -0.2906 0.09 Uiso 1 1 calc R . .
C4 C 0.6063(7) 0.5252(15) -0.0861(11) 0.053(3) Uani 1 1 d DU . .
H4A H 0.5842 0.5967 -0.0072 0.064 Uiso 1 1 calc R . .
H4B H 0.6039 0.4044 -0.0591 0.064 Uiso 1 1 calc R . .
N1 N 0.8046(6) 0.4776(9) -0.0309(8) 0.0352(16) Uani 1 1 d U . .
H1A H 0.8295 0.5043 0.0791 0.053 Uiso 1 1 calc R . .
H1B H 0.8559 0.4976 -0.0787 0.053 Uiso 1 1 calc R . .
H1C H 0.7863 0.3668 -0.0423 0.053 Uiso 1 1 calc R . .
Br1 Br 0.76894(7) 0.07438(11) -0.15254(9) 0.0324(2) Uani 1 1 d . . .
Br2 Br 1.04322(7) 0.19450(10) -0.27801(9) 0.0290(2) Uani 1 1 d . . .
Pb1 Pb 1 0 0 0.02046(13) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.468(11) . ?
C1 C2 1.500(13) . ?
C1 C4 1.540(11) . ?
C1 H1 1 . ?
C2 C3 1.520(15) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 C4 1.547(11) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
Br1 Pb1 2.9876(11) . ?
Br2 Pb1 3.0126(9) 2_754 ?
Br2 Pb1 3.0196(8) . ?
Pb1 Br1 2.9876(11) 3_755 ?
Pb1 Br2 3.0126(9) 2_744 ?
Pb1 Br2 3.0126(9) 4_566 ?
Pb1 Br2 3.0196(8) 3_755 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 116.4(8) . . ?
N1 C1 C4 116.0(8) . . ?
C2 C1 C4 87.7(7) . . ?
N1 C1 H1 111.6 . . ?
C2 C1 H1 111.6 . . ?
C4 C1 H1 111.6 . . ?
C1 C2 C3 89.9(7) . . ?
C1 C2 H2A 113.7 . . ?
C3 C2 H2A 113.7 . . ?
C1 C2 H2B 113.7 . . ?
C3 C2 H2B 113.7 . . ?
H2A C2 H2B 110.9 . . ?
C2 C3 C4 86.7(7) . . ?
C2 C3 H3A 114.2 . . ?
C4 C3 H3A 114.2 . . ?
C2 C3 H3B 114.2 . . ?
C4 C3 H3B 114.2 . . ?
H3A C3 H3B 111.4 . . ?
C1 C4 C3 87.4(7) . . ?
C1 C4 H4A 114.1 . . ?
C3 C4 H4A 114.1 . . ?
C1 C4 H4B 114.1 . . ?
C3 C4 H4B 114.1 . . ?
H4A C4 H4B 111.3 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Br2 Pb1 148.60(3) 2_754 . ?
Br1 Pb1 Br1 180.000(16) 3_755 . ?
Br1 Pb1 Br2 94.44(2) 3_755 2_744 ?
Br1 Pb1 Br2 85.56(2) . 2_744 ?
Br1 Pb1 Br2 85.56(2) 3_755 4_566 ?
Br1 Pb1 Br2 94.44(2) . 4_566 ?
Br2 Pb1 Br2 180.000(19) 2_744 4_566 ?
Br1 Pb1 Br2 90.92(2) 3_755 . ?
Br1 Pb1 Br2 89.08(2) . . ?
Br2 Pb1 Br2 88.360(18) 2_744 . ?
Br2 Pb1 Br2 91.640(18) 4_566 . ?
Br1 Pb1 Br2 89.08(2) 3_755 3_755 ?
Br1 Pb1 Br2 90.92(2) . 3_755 ?
Br2 Pb1 Br2 91.640(18) 2_744 3_755 ?
Br2 Pb1 Br2 88.360(18) 4_566 3_755 ?
Br2 Pb1 Br2 180.00(4) . 3_755 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 139.9(9) . . . . ?
C4 C1 C2 C3 21.8(9) . . . . ?
C1 C2 C3 C4 -21.8(9) . . . . ?
N1 C1 C4 C3 -139.9(9) . . . . ?
C2 C1 C4 C3 -21.5(9) . . . . ?
C2 C3 C4 C1 21.2(9) . . . . ?
Pb1 Br2 Pb1 Br1 -137.25(6) 2_754 . . 3_755 ?
Pb1 Br2 Pb1 Br1 42.75(6) 2_754 . . . ?
Pb1 Br2 Pb1 Br2 128.34(7) 2_754 . . 2_744 ?
Pb1 Br2 Pb1 Br2 -51.66(7) 2_754 . . 4_566 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br1 0.91 2.71 3.409(7) 134.1 4_566
N1 H1B Br2 0.91 2.6 3.427(7) 152 2_754
N1 H1C Br1 0.91 2.49 3.353(7) 159 .
_chemical_name_common            bis(cyclobutylammonium)tetrabromoplumbate(ii)

### END

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2004-11-29 at 09:55:05
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.2
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac8l_a smart

data_3
_database_code_depnum_ccdc_archive 'CCDC 708562'

_audit_creation_date             2004-11-29T09:55:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclopentylammonium)tetrabromoplumbate(II)
;
_chemical_formula_sum            'C10 H24 Br4 N2 Pb'
_chemical_formula_moiety         '2(C5 H12 N), Br4 Pb'
_chemical_formula_weight         699.14

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.429(3)
_cell_length_b                   7.9862(19)
_cell_length_c                   8.800(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.163(4)
_cell_angle_gamma                90
_cell_volume                     906.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    967
_cell_measurement_theta_min      3.159
_cell_measurement_theta_max      28.265

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.06
1 0 0 0.065
-1 -1 2 0.19
0 -2 -3 0.185
3 3 -2 0.16
-1 2 2 0.19

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    18.108
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0181
_exptl_absorpt_correction_T_max  0.1321
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_number            5745
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_reflns_number_total             2169
_reflns_number_gt                1959
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.

;
_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)+(0.0596P)²+7.7798P] 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_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0091(8)
_refine_ls_number_reflns         2169
_refine_ls_number_parameters     90
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_restrained_S_all      1.05
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.17
_refine_diff_density_min         -2.656
_refine_diff_density_rms         0.299

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'

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 0.7267(6) 0.9630(10) 0.9312(8) 0.0251(13) Uani 1 1 d DU A .
H1 H 0.737 0.8513 0.9846 0.03 Uiso 1 1 calc R . .
C2 C 0.6181(6) 1.0276(13) 0.9233(10) 0.0379(19) Uani 1 1 d DU . .
H2A H 0.584 0.9544 0.9847 0.045 Uiso 0.52(3) 1 calc PR A 1
H2B H 0.6212 1.143 0.9654 0.045 Uiso 0.52(3) 1 calc PR A 1
H2C H 0.5991 1.0006 1.0215 0.045 Uiso 0.48(3) 1 calc PR A 2
H2D H 0.6132 1.1501 0.906 0.045 Uiso 0.48(3) 1 calc PR A 2
C3A C 0.5600(15) 1.023(3) 0.7476(13) 0.044(4) Uani 0.52(3) 1 d PDU A 1
H3A1 H 0.4873 0.9878 0.7322 0.053 Uiso 0.52(3) 1 calc PR A 1
H3A2 H 0.5603 1.1353 0.6995 0.053 Uiso 0.52(3) 1 calc PR A 1
C3B C 0.5493(11) 0.934(4) 0.782(2) 0.045(4) Uani 0.48(3) 1 d PDU A 2
H3B1 H 0.489 1.0032 0.7267 0.054 Uiso 0.48(3) 1 calc PR A 2
H3B2 H 0.5236 0.8282 0.8164 0.054 Uiso 0.48(3) 1 calc PR A 2
C4 C 0.6175(6) 0.8971(16) 0.6729(11) 0.050(2) Uani 1 1 d DU . .
H4A H 0.6007 0.7803 0.6942 0.059 Uiso 0.52(3) 1 calc PR A 1
H4B H 0.6029 0.9143 0.5574 0.059 Uiso 0.52(3) 1 calc PR A 1
H4C H 0.6128 0.7771 0.6436 0.059 Uiso 0.48(3) 1 calc PR A 2
H4D H 0.594 0.9642 0.5749 0.059 Uiso 0.48(3) 1 calc PR A 2
C5 C 0.7291(6) 0.9419(13) 0.7600(8) 0.0335(16) Uani 1 1 d DU A .
H5A H 0.7505 1.047 0.7185 0.04 Uiso 1 1 calc R . .
H5B H 0.7772 0.8512 0.7505 0.04 Uiso 1 1 calc R . .
N1 N 0.8081(5) 1.0801(9) 1.0206(7) 0.0259(12) Uani 1 1 d U . .
H1A H 0.8047 1.0881 1.1222 0.039 Uiso 1 1 calc R A .
H1B H 0.7979 1.1829 0.9743 0.039 Uiso 1 1 calc R . .
H1C H 0.8716 1.0409 1.02 0.039 Uiso 1 1 calc R . .
Br1 Br 0.76898(6) 1.02630(10) 0.37567(9) 0.0265(2) Uani 1 1 d . . .
Br2 Br 1.00251(6) 0.68679(9) 0.69656(8) 0.0258(2) Uani 1 1 d . . .
Pb1 Pb 1 1 0.5 0.01838(17) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.487(10) . ?
C1 C5 1.525(7) . ?
C1 C2 1.530(7) . ?
C1 H1 1 . ?
C2 C3B 1.525(9) . ?
C2 C3A 1.526(8) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C2 H2C 0.99 . ?
C2 H2D 0.99 . ?
C3A C4 1.525(9) . ?
C3A H3A1 0.99 . ?
C3A H3A2 0.99 . ?
C3B C4 1.527(9) . ?
C3B H3B1 0.99 . ?
C3B H3B2 0.99 . ?
C4 C5 1.523(8) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C4 H4C 0.99 . ?
C4 H4D 0.99 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
Br1 Pb1 2.9959(11) . ?
Br2 Pb1 3.0360(9) . ?
Br2 Pb1 3.0671(9) 2_746 ?
Pb1 Br1 2.9959(11) 3_776 ?
Pb1 Br2 3.0360(9) 3_776 ?
Pb1 Br2 3.0671(9) 4_575 ?
Pb1 Br2 3.0671(9) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag

N1 C1 C5 112.2(6) . . ?
N1 C1 C2 111.3(6) . . ?
C5 C1 C2 105.9(6) . . ?
N1 C1 H1 109.1 . . ?
C5 C1 H1 109.1 . . ?
C2 C1 H1 109.1 . . ?
C3B C2 C1 103.0(9) . . ?
C3A C2 C1 104.5(8) . . ?
C3A C2 H2A 110.9 . . ?
C1 C2 H2A 110.9 . . ?
C3A C2 H2B 110.9 . . ?
C1 C2 H2B 110.9 . . ?
H2A C2 H2B 108.9 . . ?
C3B C2 H2C 111.2 . . ?
C3A C2 H2C 134.1 . . ?
C1 C2 H2C 111.2 . . ?
C3B C2 H2D 111.2 . . ?
C1 C2 H2D 111.2 . . ?
H2C C2 H2D 109.1 . . ?
C4 C3A C2 105.9(8) . . ?
C4 C3A H3A1 110.6 . . ?
C2 C3A H3A1 110.6 . . ?
C4 C3A H3A2 110.6 . . ?
C2 C3A H3A2 110.6 . . ?
H3A1 C3A H3A2 108.7 . . ?
C2 C3B C4 105.9(8) . . ?
C2 C3B H3B1 110.6 . . ?
C4 C3B H3B1 110.6 . . ?
C2 C3B H3B2 110.6 . . ?
C4 C3B H3B2 110.6 . . ?
H3B1 C3B H3B2 108.7 . . ?
C5 C4 C3A 100.0(10) . . ?
C5 C4 C3B 108.5(7) . . ?
C5 C4 H4A 111.8 . . ?
C3A C4 H4A 111.8 . . ?
C5 C4 H4B 111.8 . . ?
C3A C4 H4B 111.8 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 110 . . ?
C3B C4 H4C 110 . . ?
C5 C4 H4D 110 . . ?
C3B C4 H4D 110 . . ?
H4C C4 H4D 108.4 . . ?
C4 C5 C1 103.6(6) . . ?
C4 C5 H5A 111 . . ?
C1 C5 H5A 111 . . ?
C4 C5 H5B 111 . . ?
C1 C5 H5B 111 . . ?
H5A C5 H5B 109 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Br2 Pb1 153.60(3) . 2_746 ?
Br1 Pb1 Br1 180 3_776 . ?
Br1 Pb1 Br2 96.43(2) 3_776 3_776 ?
Br1 Pb1 Br2 83.57(2) . 3_776 ?
Br1 Pb1 Br2 83.57(2) 3_776 . ?
Br1 Pb1 Br2 96.43(2) . . ?
Br2 Pb1 Br2 180.000(16) 3_776 . ?
Br1 Pb1 Br2 91.30(2) 3_776 4_575 ?
Br1 Pb1 Br2 88.70(2) . 4_575 ?
Br2 Pb1 Br2 84.592(18) 3_776 4_575 ?
Br2 Pb1 Br2 95.408(18) . 4_575 ?
Br1 Pb1 Br2 88.70(2) 3_776 2_756 ?
Br1 Pb1 Br2 91.30(2) . 2_756 ?
Br2 Pb1 Br2 95.408(18) 3_776 2_756 ?
Br2 Pb1 Br2 84.592(18) . 2_756 ?
Br2 Pb1 Br2 180 4_575 2_756 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

N1 C1 C2 C3B 159.2(12) . . . . ?
C5 C1 C2 C3B 37.0(14) . . . . ?
N1 C1 C2 C3A 127.8(12) . . . . ?
C5 C1 C2 C3A 5.6(14) . . . . ?
C3B C2 C3A C4 -68.9(11) . . . . ?
C1 C2 C3A C4 22.2(18) . . . . ?
C3A C2 C3B C4 68.6(11) . . . . ?
C1 C2 C3B C4 -28(2) . . . . ?
C2 C3A C4 C5 -40.9(18) . . . . ?
C2 C3A C4 C3B 68.7(10) . . . . ?
C2 C3B C4 C5 9(2) . . . . ?
C2 C3B C4 C3A -68.8(11) . . . . ?
C3A C4 C5 C1 43.7(12) . . . . ?
C3B C4 C5 C1 13.4(16) . . . . ?
N1 C1 C5 C4 -152.8(8) . . . . ?
C2 C1 C5 C4 -31.2(10) . . . . ?
Pb1 Br2 Pb1 Br1 91.23(6) 2_746 . . 3_776 ?
Pb1 Br2 Pb1 Br1 -88.77(6) 2_746 . . . ?
Pb1 Br2 Pb1 Br2 -178.07(4) 2_746 . . 4_575 ?
Pb1 Br2 Pb1 Br2 1.93(4) 2_746 . . 2_756 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br1 0.91 2.46 3.338(6) 162.3 1_556
N1 H1B Br1 0.91 2.47 3.378(7) 174 4_586
N1 H1C Br2 0.91 2.7 3.392(7) 133.6 4_576
_chemical_name_common            
bis(cyclopentylammonium)tetrabromoplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2006-02-03 at 09:40:59
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac3l_a smart

data_4
_database_code_depnum_ccdc_archive 'CCDC 708563'

_audit_creation_date             2006-02-03T09:40:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclohexylammonium)tetrabromoplumbate(II)
;
_chemical_formula_sum            'C12 H28 Br4 N2 Pb'
_chemical_formula_moiety         'Br4 Pb, 2(C6 H14 N)'
_chemical_formula_weight         727.19
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmc2(1)
_symmetry_space_group_name_Hall  'C 2c -2'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   27.788(5)
_cell_length_b                   8.6541(14)
_cell_length_c                   8.2367(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1980.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    944
_cell_measurement_theta_min      2.465
_cell_measurement_theta_max      27.8935

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'light brown'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.025
1 0 0 0.025
-1 -1 -1 0.085
1 1 1 0.085
-1 -1 1 0.1
1 1 -1 0.1
1 0 -1 0.1
-1 0 1 0.1

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    16.578
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0729
_exptl_absorpt_correction_T_max  0.4516
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_number            9382
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_full        27.99
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             2346
_reflns_number_gt                2163
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

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

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.

;
_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)+(0.0473P)²+19.2395P] 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_number_reflns         2346
_refine_ls_number_parameters     91
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.036
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.006
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.215(14)
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.92
_refine_diff_density_rms         0.187

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'

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 0.1321(3) 0.6906(13) 0.4501(19) 0.070(3) Uani 1 1 d DU . .
H1 H 0.1305 0.6325 0.3454 0.084 Uiso 1 1 calc R . .
C2 C 0.1303(4) 0.8602(13) 0.4173(18) 0.074(3) Uani 1 1 d DU . .
H2A H 0.1284 0.9174 0.5212 0.089 Uiso 1 1 calc R . .
H2B H 0.1012 0.8849 0.3528 0.089 Uiso 1 1 calc R . .
C3 C 0.1748(3) 0.9095(17) 0.3249(18) 0.075(3) Uani 1 1 d DU . .
H3A H 0.1737 0.8646 0.2144 0.09 Uiso 1 1 calc R . .
H3B H 0.1747 1.0234 0.3137 0.09 Uiso 1 1 calc R . .
C4 C 0.2211(4) 0.8601(15) 0.407(2) 0.083(3) Uani 1 1 d DU . .
H4A H 0.2488 0.8885 0.3371 0.099 Uiso 1 1 calc R . .
H4B H 0.2246 0.9156 0.5112 0.099 Uiso 1 1 calc R . .
C5 C 0.2218(4) 0.6904(15) 0.4370(18) 0.081(3) Uani 1 1 d DU . .
H5A H 0.2517 0.6612 0.4948 0.097 Uiso 1 1 calc R . .
H5B H 0.2208 0.6338 0.3326 0.097 Uiso 1 1 calc R . .
C6 C 0.1781(3) 0.6490(18) 0.5394(17) 0.073(3) Uani 1 1 d DU . .
H6A H 0.1784 0.5369 0.5633 0.087 Uiso 1 1 calc R . .
H6B H 0.1795 0.7055 0.6438 0.087 Uiso 1 1 calc R . .
N1 N 0.0897(3) 0.6469(11) 0.5560(11) 0.050(2) Uani 1 1 d U . .
H1A H 0.0896 0.5429 0.5722 0.075 Uiso 1 1 calc R . .
H1B H 0.0618 0.6756 0.5062 0.075 Uiso 1 1 calc R . .
H1C H 0.0921 0.696 0.6534 0.075 Uiso 1 1 calc R . .
Br1 Br 0.10590(4) 0.27394(13) 0.4543(2) 0.0531(4) Uani 1 1 d . . .
Br2 Br 0 0.54668(13) 0.27566(18) 0.0284(3) Uani 1 2 d S . .
Br3 Br 0 0.07416(14) 0.1516(2) 0.0368(3) Uani 1 2 d S . .
Pb1 Pb 0 0.23368(4) 0.47561(5) 0.03086(13) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.493(9) . ?
C1 N1 1.514(14) . ?
C1 C6 1.519(8) . ?
C1 H1 1 . ?
C2 C3 1.514(8) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 C4 1.514(9) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 C5 1.490(9) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.521(9) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
Br1 Pb1 2.9686(11) . ?
Br2 Pb1 3.1178(15) 2_564 ?
Br2 Pb1 3.1702(14) . ?
Br3 Pb1 3.0048(17) . ?
Br3 Pb1 3.0328(14) 2_554 ?
Pb1 Br1 2.9686(11) 4 ?
Pb1 Br3 3.0328(14) 2 ?
Pb1 Br2 3.1178(15) 2_565 ?

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 N1 108.9(9) . . ?
C2 C1 C6 110.4(10) . . ?
N1 C1 C6 108.5(9) . . ?
C2 C1 H1 109.7 . . ?
N1 C1 H1 109.7 . . ?
C6 C1 H1 109.7 . . ?
C1 C2 C3 109.9(10) . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 113.0(10) . . ?
C4 C3 H3A 109 . . ?
C2 C3 H3A 109 . . ?
C4 C3 H3B 109 . . ?
C2 C3 H3B 109 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 111.3(11) . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108 . . ?
C4 C5 C6 108.4(10) . . ?
C4 C5 H5A 110 . . ?
C6 C5 H5A 110 . . ?
C4 C5 H5B 110 . . ?
C6 C5 H5B 110 . . ?
H5A C5 H5B 108.4 . . ?
C1 C6 C5 110.4(10) . . ?
C1 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C1 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Br2 Pb1 158.86(5) 2_564 . ?
Pb1 Br3 Pb1 145.90(6) . 2_554 ?
Br1 Pb1 Br1 164.90(5) 4 . ?
Br1 Pb1 Br3 90.08(3) 4 . ?
Br1 Pb1 Br3 90.08(3) . . ?
Br1 Pb1 Br3 97.55(2) 4 2 ?
Br1 Pb1 Br3 97.55(2) . 2 ?
Br3 Pb1 Br3 91.20(2) . 2 ?
Br1 Pb1 Br2 88.59(3) 4 2_565 ?
Br1 Pb1 Br2 88.59(3) . 2_565 ?
Br3 Pb1 Br2 169.79(4) . 2_565 ?
Br3 Pb1 Br2 99.01(5) 2 2_565 ?
Br1 Pb1 Br2 82.47(2) 4 . ?
Br1 Pb1 Br2 82.47(2) . . ?
Br3 Pb1 Br2 86.05(4) . . ?
Br3 Pb1 Br2 177.25(5) 2 . ?
Br2 Pb1 Br2 83.735(18) 2_565 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

N1 C1 C2 C3 174.7(11) . . . . ?
C6 C1 C2 C3 55.6(17) . . . . ?
C1 C2 C3 C4 -53.1(19) . . . . ?
C2 C3 C4 C5 54.8(19) . . . . ?
C3 C4 C5 C6 -57.2(17) . . . . ?
C2 C1 C6 C5 -60.9(17) . . . . ?
N1 C1 C6 C5 179.8(11) . . . . ?
C4 C5 C6 C1 60.8(17) . . . . ?
Pb1 Br3 Pb1 Br1 -97.55(2) 2_554 . . 4 ?
Pb1 Br3 Pb1 Br1 97.55(2) 2_554 . . . ?
Pb1 Br3 Pb1 Br3 0 2_554 . . 2 ?
Pb1 Br3 Pb1 Br2 180 2_554 . . 2_565 ?
Pb1 Br3 Pb1 Br2 180 2_554 . . . ?
Pb1 Br2 Pb1 Br1 -90.60(3) 2_564 . . 4 ?
Pb1 Br2 Pb1 Br1 90.60(3) 2_564 . . . ?
Pb1 Br2 Pb1 Br3 0 2_564 . . . ?
Pb1 Br2 Pb1 Br2 180 2_564 . . 2_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br1 0.91 2.56 3.365(10) 147.4 .
N1 H1B Br2 0.91 2.79 3.506(9) 136.1 .
N1 H1C Br1 0.91 2.52 3.381(10) 157.8 3_565
_chemical_name_common            bis(cyclohexylammonium)tetrabromoplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2006-02-04 at 09:45:40
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac13r_a smart

data_5
_database_code_depnum_ccdc_archive 'CCDC 708564'

_audit_creation_date             2006-02-04T09:45:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
tris(cycloheptylammonium)pentabromoplumbate(II)
;
_chemical_formula_sum            'C21 H50 Br5 N3 O Pb'
_chemical_formula_moiety         '3(C7 H16 N), Br5 Pb, H2 O'
_chemical_formula_weight         967.38

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.0888(4)
_cell_length_b                   27.1707(15)
_cell_length_c                   28.9932(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6372.1(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    919
_cell_measurement_theta_min      2.7195
_cell_measurement_theta_max      24.925

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'long rectangle'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.04
0 0 -1 0.04
0 1 0 0.05
0 -1 0 0.05
-1 0 0 0.2
1 0 0 0.2

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    11.584
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.1572
_exptl_absorpt_correction_T_max  0.4218
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.078
_diffrn_reflns_number            28684
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.4
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             5927
_reflns_number_gt                4811
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C---C bonds do not have normal carbon distances as a result of thermal
motion
of the hydrocarbon rings. All carbon distances and angles were then
restrained in
SHELX to reasonable molecular geometries usiing DFIX and DANG instructions
and the anisotropic displacement parameters
restrained to be equal in the direction of the bonds.
;
_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)+(0.0000P)²+865.2066P] 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_number_reflns         5927
_refine_ls_number_parameters     280
_refine_ls_number_restraints     222
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_gt           0.1401
_refine_ls_wR_factor_ref         0.27
_refine_ls_wR_factor_gt          0.2619
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_restrained_S_all      1.311
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.543
_refine_diff_density_min         -5.316
_refine_diff_density_rms         0.416

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.476(3) 0.3258(7) 0.1193(7) 0.036(5) Uani 1 1 d DU . .
H1 H 0.3608 0.3323 0.108 0.043 Uiso 1 1 calc R . .
C2 C 0.460(3) 0.2783(9) 0.1463(8) 0.044(5) Uani 1 1 d DU . .
H2D H 0.3526 0.2771 0.1626 0.053 Uiso 1 1 calc R . .
H2E H 0.4669 0.2497 0.1253 0.053 Uiso 1 1 calc R . .
C3 C 0.601(3) 0.2773(10) 0.1805(8) 0.052(6) Uani 1 1 d DU . .
H3D H 0.6946 0.2974 0.1691 0.062 Uiso 1 1 calc R . .
H3E H 0.6397 0.2431 0.1853 0.062 Uiso 1 1 calc R . .
C4 C 0.533(4) 0.2985(8) 0.2251(7) 0.054(6) Uani 1 1 d DU . .
H4A H 0.413 0.2923 0.2276 0.065 Uiso 1 1 calc R . .
H4B H 0.5892 0.2836 0.252 0.065 Uiso 1 1 calc R . .
C5 C 0.568(4) 0.3533(8) 0.2229(8) 0.054(6) Uani 1 1 d DU . .
H5A H 0.5536 0.3685 0.2537 0.065 Uiso 1 1 calc R . .
H5B H 0.6826 0.3594 0.2123 0.065 Uiso 1 1 calc R . .
C6 C 0.445(3) 0.3747(9) 0.1890(7) 0.044(5) Uani 1 1 d DU . .
H6A H 0.3425 0.3549 0.1887 0.052 Uiso 1 1 calc R . .
H6B H 0.4167 0.4089 0.1977 0.052 Uiso 1 1 calc R . .
C7 C 0.526(3) 0.3737(8) 0.1420(7) 0.036(5) Uani 1 1 d DU . .
H7A H 0.6478 0.3754 0.1451 0.044 Uiso 1 1 calc R . .
H7B H 0.4885 0.4021 0.1233 0.044 Uiso 1 1 calc R . .
C8 C 0.143(3) 0.5060(16) -0.1047(10) 0.056(6) Uani 1 1 d DU . .
H8 H 0.1789 0.5406 -0.0985 0.067 Uiso 1 1 calc R . .
C9 C -0.044(4) 0.5033(14) -0.1081(12) 0.061(7) Uani 1 1 d DU . .
H9A H -0.075 0.47 -0.119 0.074 Uiso 1 1 calc R . .
H9B H -0.091 0.5076 -0.0769 0.074 Uiso 1 1 calc R . .
C10 C -0.122(5) 0.5411(15) -0.1400(9) 0.070(7) Uani 1 1 d DU . .
H10A H -0.2407 0.5433 -0.1325 0.084 Uiso 1 1 calc R . .
H10B H -0.0718 0.5735 -0.1331 0.084 Uiso 1 1 calc R . .
C11 C -0.105(5) 0.5319(18) -0.1913(10) 0.075(7) Uani 1 1 d DU . .
H11A H -0.1986 0.5104 -0.2002 0.09 Uiso 1 1 calc R . .
H11B H -0.1243 0.564 -0.2067 0.09 Uiso 1 1 calc R . .
C12 C 0.048(4) 0.5101(19) -0.2131(13) 0.083(8) Uani 1 1 d DU . .
H12A H 0.0596 0.5253 -0.244 0.099 Uiso 1 1 calc R . .
H12B H 0.025 0.4747 -0.2183 0.099 Uiso 1 1 calc R . .
C13 C 0.217(4) 0.5130(17) -0.1903(11) 0.075(7) Uani 1 1 d DU . .
H13A H 0.3001 0.5007 -0.2125 0.089 Uiso 1 1 calc R . .
H13B H 0.2419 0.5481 -0.1844 0.089 Uiso 1 1 calc R . .
C14 C 0.238(5) 0.4851(15) -0.1454(9) 0.068(7) Uani 1 1 d DU . .
H14A H 0.3572 0.4845 -0.1375 0.082 Uiso 1 1 calc R . .
H14B H 0.2026 0.4506 -0.1503 0.082 Uiso 1 1 calc R . .
C15 C 0.598(7) 0.3204(13) -0.1241(13) 0.084(8) Uani 1 1 d DU . .
H15 H 0.713 0.3082 -0.1196 0.101 Uiso 1 1 calc R . .
C16 C 0.598(7) 0.3761(13) -0.1185(15) 0.090(8) Uani 1 1 d DU . .
H16A H 0.6476 0.3838 -0.0881 0.108 Uiso 1 1 calc R . .
H16B H 0.4816 0.3873 -0.1175 0.108 Uiso 1 1 calc R . .
C17 C 0.688(7) 0.4062(19) -0.1548(14) 0.102(9) Uani 1 1 d DU . .
H17A H 0.7017 0.4403 -0.1434 0.122 Uiso 1 1 calc R . .
H17B H 0.7993 0.3921 -0.1597 0.122 Uiso 1 1 calc R . .
C18 C 0.596(8) 0.4073(16) -0.2004(14) 0.106(9) Uani 1 1 d DU . .
H18A H 0.6409 0.4355 -0.2181 0.128 Uiso 1 1 calc R . .
H18B H 0.4795 0.4152 -0.1934 0.128 Uiso 1 1 calc R . .
C19 C 0.595(8) 0.3635(14) -0.2328(15) 0.111(9) Uani 1 1 d DU . .
H19A H 0.6669 0.3706 -0.2595 0.133 Uiso 1 1 calc R . .
H19B H 0.481 0.3586 -0.2445 0.133 Uiso 1 1 calc R . .
C20 C 0.653(7) 0.3166(17) -0.2096(15) 0.105(9) Uani 1 1 d DU . .
H20A H 0.7659 0.3215 -0.197 0.127 Uiso 1 1 calc R . .
H20B H 0.6579 0.2896 -0.2325 0.127 Uiso 1 1 calc R . .
C21 C 0.536(6) 0.3026(18) -0.1708(12) 0.091(8) Uani 1 1 d DU . .
H21A H 0.5234 0.2664 -0.17 0.109 Uiso 1 1 calc R . .
H21B H 0.4258 0.3171 -0.177 0.109 Uiso 1 1 calc R . .
N1 N 0.580(3) 0.3212(10) 0.0744(9) 0.037(5) Uani 1 1 d U . .
H1A H 0.5508 0.2931 0.0593 0.055 Uiso 1 1 calc R . .
H1B H 0.6889 0.3201 0.0817 0.055 Uiso 1 1 calc R . .
H1C H 0.5597 0.3476 0.0559 0.055 Uiso 1 1 calc R . .
N2 N 0.195(3) 0.4733(10) -0.0660(9) 0.038(6) Uani 1 1 d U . .
H2A H 0.3069 0.4724 -0.0644 0.058 Uiso 1 1 calc R . .
H2B H 0.1552 0.4423 -0.071 0.058 Uiso 1 1 calc R . .
H2C H 0.1531 0.4851 -0.039 0.058 Uiso 1 1 calc R . .
N3 N 0.493(4) 0.3003(12) -0.0865(11) 0.063(8) Uani 1 1 d U . .
H3A H 0.4869 0.267 -0.0891 0.094 Uiso 1 1 calc R . .
H3B H 0.3891 0.3133 -0.0886 0.094 Uiso 1 1 calc R . .
H3C H 0.5373 0.3083 -0.0587 0.094 Uiso 1 1 calc R . .
O1 O 0.535(3) 0.4898(9) -0.0602(9) 0.051(7) Uani 1 1 d . . .
H101 H 0.6153 0.4709 -0.0438 0.061 Uiso 1 1 d R . .
H102 H 0.5689 0.5207 -0.0481 0.061 Uiso 1 1 d R . .
Br1 Br 0.8285(4) 0.42138(13) 0.00016(12) 0.0474(9) Uani 1 1 d . . .
Br2 Br 0.9834(3) 0.32459(11) 0.10643(11) 0.0328(7) Uani 1 1 d . . .
Br3 Br 1.3436(4) 0.40042(12) 0.01674(13) 0.0461(10) Uani 1 1 d . . .
Br4 Br 1.1126(4) 0.34940(12) -0.09769(12) 0.0382(8) Uani 1 1 d . . .
Br5 Br 1.2912(3) 0.24581(10) 0.01246(8) 0.0211(6) Uani 1 1 d . . .
Pb1 Pb 1.05424(12) 0.33827(4) 0.00440(4) 0.0235(3) Uani 1 1 d . . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C7 1.514(10) . ?
C1 C2 1.514(10) . ?
C1 N1 1.55(3) . ?
C1 H1 1 . ?
C2 C3 1.511(10) . ?
C2 H2D 0.99 . ?
C2 H2E 0.99 . ?
C3 C4 1.518(10) . ?
C3 H3D 0.99 . ?
C3 H3E 0.99 . ?
C4 C5 1.517(10) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.514(10) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.512(10) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 N2 1.49(4) . ?
C8 C9 1.517(10) . ?
C8 C14 1.520(10) . ?
C8 H8 1 . ?
C9 C10 1.517(10) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C10 C11 1.515(10) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 C12 1.514(10) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 C13 1.517(10) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C13 C14 1.517(10) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 N3 1.49(5) . ?
C15 C16 1.520(10) . ?
C15 C21 1.522(10) . ?
C15 H15 1 . ?
C16 C17 1.520(10) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 C18 1.515(10) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C18 C19 1.516(10) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.518(10) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 C21 1.520(10) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
N2 H2A 0.91 . ?
N2 H2B 0.91 . ?
N2 H2C 0.91 . ?
N3 H3A 0.91 . ?
N3 H3B 0.91 . ?
N3 H3C 0.91 . ?
O1 H101 0.9528 . ?
O1 H102 0.9497 . ?
Br1 Pb1 2.907(3) . ?
Br2 Pb1 3.036(3) . ?
Br3 Pb1 2.908(3) . ?
Br4 Pb1 3.012(4) . ?
Br5 Pb1 3.160(3) 4 ?
Br5 Pb1 3.168(3) . ?
Pb1 Br5 3.160(3) 4_455 ?

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
C7 C1 C2 122.0(17) . . ?
C7 C1 N1 106.7(18) . . ?
C2 C1 N1 114(2) . . ?
C7 C1 H1 104 . . ?
C2 C1 H1 104 . . ?
N1 C1 H1 104 . . ?
C3 C2 C1 107.0(13) . . ?
C3 C2 H2D 110.3 . . ?
C1 C2 H2D 110.3 . . ?
C3 C2 H2E 110.3 . . ?
C1 C2 H2E 110.3 . . ?
H2D C2 H2E 108.6 . . ?
C2 C3 C4 106.3(13) . . ?
C2 C3 H3D 110.5 . . ?
C4 C3 H3D 110.5 . . ?
C2 C3 H3E 110.5 . . ?
C4 C3 H3E 110.5 . . ?
H3D C3 H3E 108.7 . . ?
C5 C4 C3 105.7(13) . . ?
C5 C4 H4A 110.6 . . ?
C3 C4 H4A 110.6 . . ?
C5 C4 H4B 110.6 . . ?
C3 C4 H4B 110.6 . . ?
H4A C4 H4B 108.7 . . ?
C6 C5 C4 106.4(13) . . ?
C6 C5 H5A 110.5 . . ?
C4 C5 H5A 110.5 . . ?
C6 C5 H5B 110.5 . . ?
C4 C5 H5B 110.5 . . ?
H5A C5 H5B 108.6 . . ?
C7 C6 C5 107.1(13) . . ?
C7 C6 H6A 110.3 . . ?
C5 C6 H6A 110.3 . . ?
C7 C6 H6B 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?
C6 C7 C1 106.9(13) . . ?
C6 C7 H7A 110.3 . . ?
C1 C7 H7A 110.3 . . ?
C6 C7 H7B 110.3 . . ?
C1 C7 H7B 110.3 . . ?
H7A C7 H7B 108.6 . . ?
N2 C8 C9 107(3) . . ?
N2 C8 C14 103(3) . . ?
C9 C8 C14 116(3) . . ?
N2 C8 H8 110.2 . . ?
C9 C8 H8 110.2 . . ?
C14 C8 H8 110.2 . . ?
C10 C9 C8 115(3) . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C11 C10 C9 117(3) . . ?
C11 C10 H10A 108.1 . . ?
C9 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
C9 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
C12 C11 C10 123(3) . . ?
C12 C11 H11A 106.6 . . ?
C10 C11 H11A 106.6 . . ?
C12 C11 H11B 106.6 . . ?
C10 C11 H11B 106.6 . . ?
H11A C11 H11B 106.5 . . ?
C11 C12 C13 122(3) . . ?
C11 C12 H12A 106.8 . . ?
C13 C12 H12A 106.8 . . ?
C11 C12 H12B 106.8 . . ?
C13 C12 H12B 106.8 . . ?
H12A C12 H12B 106.6 . . ?
C14 C13 C12 117(3) . . ?
C14 C13 H13A 108.1 . . ?
C12 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
C12 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 C8 115(3) . . ?
C13 C14 H14A 108.5 . . ?
C8 C14 H14A 108.5 . . ?
C13 C14 H14B 108.5 . . ?
C8 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
N3 C15 C16 107(3) . . ?
N3 C15 C21 110(3) . . ?
C16 C15 C21 114(4) . . ?
N3 C15 H15 108.4 . . ?
C16 C15 H15 108.4 . . ?
C21 C15 H15 108.4 . . ?
C15 C16 C17 118(4) . . ?
C15 C16 H16A 107.9 . . ?
C17 C16 H16A 107.9 . . ?
C15 C16 H16B 107.9 . . ?
C17 C16 H16B 107.9 . . ?
H16A C16 H16B 107.2 . . ?
C18 C17 C16 112(4) . . ?
C18 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C19 122(5) . . ?
C17 C18 H18A 106.9 . . ?
C19 C18 H18A 106.9 . . ?
C17 C18 H18B 106.9 . . ?
C19 C18 H18B 106.9 . . ?
H18A C18 H18B 106.7 . . ?
C18 C19 C20 113(4) . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 C21 110(4) . . ?
C19 C20 H20A 109.7 . . ?
C21 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C21 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C20 C21 C15 112(4) . . ?
C20 C21 H21A 109.2 . . ?
C15 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C15 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C8 N2 H2A 109.5 . . ?
C8 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C8 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C15 N3 H3A 109.5 . . ?
C15 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C15 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
H101 O1 H102 95.5 . . ?
Pb1 Br5 Pb1 165.72(9) 4 . ?
Br1 Pb1 Br3 93.42(11) . . ?
Br1 Pb1 Br4 88.79(10) . . ?
Br3 Pb1 Br4 86.37(10) . . ?
Br1 Pb1 Br2 91.02(9) . . ?
Br3 Pb1 Br2 95.91(9) . . ?
Br4 Pb1 Br2 177.72(9) . . ?
Br1 Pb1 Br5 97.59(9) . 4_455 ?
Br3 Pb1 Br5 168.74(10) . 4_455 ?
Br4 Pb1 Br5 91.49(8) . 4_455 ?
Br2 Pb1 Br5 86.28(7) . 4_455 ?
Br1 Pb1 Br5 177.57(10) . . ?
Br3 Pb1 Br5 87.97(9) . . ?
Br4 Pb1 Br5 93.29(8) . . ?
Br2 Pb1 Br5 86.86(7) . . ?
Br5 Pb1 Br5 81.11(3) 4_455 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

C7 C1 C2 C3 -39(3) . . . . ?
N1 C1 C2 C3 91(2) . . . . ?
C1 C2 C3 C4 94(2) . . . . ?
C2 C3 C4 C5 -91(2) . . . . ?
C3 C4 C5 C6 74(2) . . . . ?
C4 C5 C6 C7 -91(2) . . . . ?
C5 C6 C7 C1 93(2) . . . . ?
C2 C1 C7 C6 -38(3) . . . . ?
N1 C1 C7 C6 -171.6(18) . . . . ?
N2 C8 C9 C10 170(3) . . . . ?
C14 C8 C9 C10 -76(4) . . . . ?
C8 C9 C10 C11 75(5) . . . . ?
C9 C10 C11 C12 -37(7) . . . . ?
C10 C11 C12 C13 -23(8) . . . . ?
C11 C12 C13 C14 66(6) . . . . ?
C12 C13 C14 C8 -69(5) . . . . ?
N2 C8 C14 C13 -177(3) . . . . ?
C9 C8 C14 C13 66(5) . . . . ?
N3 C15 C16 C17 -176(4) . . . . ?
C21 C15 C16 C17 -54(7) . . . . ?
C15 C16 C17 C18 72(6) . . . . ?
C16 C17 C18 C19 -75(7) . . . . ?
C17 C18 C19 C20 15(8) . . . . ?
C18 C19 C20 C21 63(7) . . . . ?
C19 C20 C21 C15 -97(5) . . . . ?
N3 C15 C21 C20 -172(4) . . . . ?
C16 C15 C21 C20 67(6) . . . . ?
Pb1 Br5 Pb1 Br3 -73.8(4) 4 . . . ?
Pb1 Br5 Pb1 Br4 12.4(4) 4 . . . ?
Pb1 Br5 Pb1 Br2 -169.9(4) 4 . . . ?
Pb1 Br5 Pb1 Br5 103.4(4) 4 . . 4_455 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br5 0.91 2.81 3.59(3) 143.7 1_455
N1 H1B Br2 0.91 2.49 3.40(2) 174.3 .
N1 H1C Br3 0.91 2.53 3.33(3) 146.4 1_455
N2 H2A O1 0.91 1.91 2.80(3) 164.2 .
N2 H2B Br4 0.91 2.66 3.55(3) 165.2 1_455
N2 H2C Br1 0.91 2.78 3.45(3) 130.6 5_665
N3 H3A Br2 0.91 2.54 3.44(3) 173.1 4_455
N3 H3B Br4 0.91 2.46 3.37(3) 177.6 1_455
N3 H3C Br5 0.91 2.86 3.47(3) 125.3 4_455
O1 H101 Br1 0.95 2.53 3.48(2) 179.5 .
O1 H102 Br3 0.95 2.43 3.38(2) 179.6 5_765
_chemical_name_common            
tris(cycloheptylammonium)pentabromoplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2009-03-30 at 17:29:43
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac16r_a smart

data_6
_database_code_depnum_ccdc_archive 'CCDC 708565'

_audit_creation_date             2009-03-30T17:29:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
dekakis(cyclooctylammonium)octadecabromotetraplumbate(II)
;
_chemical_formula_moiety         'Br18 Pb4, 10(C8 H18 N)'
_chemical_formula_sum            'C80 H180 Br18 N10 Pb4'
_chemical_formula_weight         3549.48

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7861(11)
_cell_length_b                   16.0354(16)
_cell_length_c                   31.135(3)
_cell_angle_alpha                92.891(4)
_cell_angle_beta                 96.420(4)
_cell_angle_gamma                100.267(4)
_cell_volume                     5739.0(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    941
_cell_measurement_theta_min      2.8135
_cell_measurement_theta_max      26.1845

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3376
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.025
0 0 1 0.025
0 -1 0 0.04
0 1 0 0.04
-2 1 -1 0.1
2 -1 1 0.1

_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)

;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    12.157
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.1436
_exptl_absorpt_correction_T_max  0.5675
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_number            50853
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.29
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_reflns_number_total             20609
_reflns_number_gt                12794
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI,
DFIX and DANG instructions
in SHELX to be within 0.01 Å of each other.
The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.
;
_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)+(0.0657P)²] 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_number_reflns         20609
_refine_ls_number_parameters     1009
_refine_ls_number_restraints     948
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1393
_refine_ls_wR_factor_gt          0.123
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.473
_refine_diff_density_min         -2.929
_refine_diff_density_rms         0.264

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'

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
C1A C 0.4938(13) 0.7677(9) 0.3147(4) 0.057(2) Uani 1 1 d DU . .
H1 H 0.4194 0.7643 0.2952 0.068 Uiso 1 1 calc R . .
C1B C 0.4821(15) 0.7932(8) 0.3621(4) 0.067(2) Uani 1 1 d DU . .
H1B1 H 0.4158 0.7529 0.3705 0.081 Uiso 1 1 calc R . .
H1B2 H 0.5527 0.7831 0.3799 0.081 Uiso 1 1 calc R . .
C1C C 0.4653(13) 0.8813(8) 0.3756(6) 0.072(3) Uani 1 1 d DU . .
H1C1 H 0.4391 0.8807 0.4047 0.086 Uiso 1 1 calc R . .
H1C2 H 0.4029 0.8965 0.3552 0.086 Uiso 1 1 calc R . .
C1D C 0.5744(13) 0.9499(10) 0.3770(5) 0.072(3) Uani 1 1 d DU . .
H1D1 H 0.5849 0.9862 0.4043 0.086 Uiso 1 1 calc R . .
H1D2 H 0.6434 0.9228 0.3762 0.086 Uiso 1 1 calc R . .
C1E C 0.5641(15) 1.0046(9) 0.3385(4) 0.070(3) Uani 1 1 d DU . .
H1E1 H 0.5959 1.0647 0.3485 0.084 Uiso 1 1 calc R . .
H1E2 H 0.4809 1.0004 0.3278 0.084 Uiso 1 1 calc R . .
C1F C 0.6276(14) 0.9794(9) 0.3010(5) 0.068(3) Uani 1 1 d DU . .
H1F1 H 0.708 0.9765 0.3132 0.081 Uiso 1 1 calc R . .
H1F2 H 0.6331 1.0262 0.2813 0.081 Uiso 1 1 calc R . .
C1G C 0.5781(14) 0.8964(7) 0.2733(4) 0.060(2) Uani 1 1 d DU . .
H1G1 H 0.6135 0.8981 0.2459 0.072 Uiso 1 1 calc R . .
H1G2 H 0.4934 0.8929 0.2658 0.072 Uiso 1 1 calc R . .
C1H C 0.5987(12) 0.8158(9) 0.2953(5) 0.058(2) Uani 1 1 d DU . .
H1H1 H 0.6643 0.8318 0.3187 0.069 Uiso 1 1 calc R . .
H1H2 H 0.6222 0.7768 0.2737 0.069 Uiso 1 1 calc R . .
C2A C 0.0272(11) 0.7646(9) 0.3118(5) 0.050(2) Uani 1 1 d DU . .
H2 H 0.0629 0.7516 0.2851 0.06 Uiso 1 1 calc R . .
C2B C -0.0641(12) 0.8183(8) 0.2977(5) 0.051(2) Uani 1 1 d DU . .
H2B1 H -0.0961 0.8368 0.3239 0.061 Uiso 1 1 calc R . .
H2B2 H -0.1285 0.7812 0.2788 0.061 Uiso 1 1 calc R . .
C2C C -0.0240(13) 0.8977(8) 0.2735(5) 0.053(2) Uani 1 1 d DU . .
H2C1 H 0.0017 0.8781 0.2461 0.064 Uiso 1 1 calc R . .
H2C2 H -0.0932 0.9234 0.2654 0.064 Uiso 1 1 calc R . .
C2D C 0.0720(13) 0.9685(10) 0.2955(4) 0.061(2) Uani 1 1 d DU . .
H2D1 H 0.0773 1.0177 0.2773 0.073 Uiso 1 1 calc R . .
H2D2 H 0.1469 0.9484 0.2966 0.073 Uiso 1 1 calc R . .
C2E C 0.0556(15) 0.9985(10) 0.3413(4) 0.066(2) Uani 1 1 d DU . .
H2E1 H 0.0882 1.0601 0.3454 0.079 Uiso 1 1 calc R . .
H2E2 H -0.029 0.9921 0.3427 0.079 Uiso 1 1 calc R . .
C2F C 0.1066(16) 0.9569(9) 0.3796(5) 0.065(2) Uani 1 1 d DU . .
H2F1 H 0.07 0.975 0.4048 0.078 Uiso 1 1 calc R . .
H2F2 H 0.1897 0.984 0.3852 0.078 Uiso 1 1 calc R . .
C2G C 0.1035(16) 0.8619(8) 0.3822(5) 0.066(2) Uani 1 1 d DU . .
H2G1 H 0.159 0.8557 0.4076 0.079 Uiso 1 1 calc R . .
H2G2 H 0.0252 0.8374 0.3893 0.079 Uiso 1 1 calc R . .
C2H C 0.1276(12) 0.8041(10) 0.3457(5) 0.060(2) Uani 1 1 d DU . .
H2H1 H 0.1607 0.7574 0.3587 0.073 Uiso 1 1 calc R . .
H2H2 H 0.1885 0.837 0.3305 0.073 Uiso 1 1 calc R . .
C3A C 0.9293(10) 0.2714(8) 0.4745(3) 0.0284(16) Uani 1 1 d DU . .
H3 H 0.8483 0.2379 0.4709 0.034 Uiso 1 1 calc R . .
C3B C 0.9775(11) 0.2670(7) 0.4307(4) 0.0314(18) Uani 1 1 d DU . .
H3B1 H 0.9339 0.2987 0.4102 0.038 Uiso 1 1 calc R . .
H3B2 H 1.0596 0.2967 0.4348 0.038 Uiso 1 1 calc R . .
C3C C 0.9723(10) 0.1776(7) 0.4096(4) 0.0357(19) Uani 1 1 d DU . .
H3C1 H 1.0377 0.1538 0.4238 0.043 Uiso 1 1 calc R . .
H3C2 H 0.9841 0.1825 0.3787 0.043 Uiso 1 1 calc R . .
C3D C 0.8585(10) 0.1145(8) 0.4118(4) 0.039(2) Uani 1 1 d DU . .
H3D1 H 0.8368 0.0808 0.3837 0.047 Uiso 1 1 calc R . .
H3D2 H 0.7964 0.1474 0.4158 0.047 Uiso 1 1 calc R . .
C3E C 0.8623(13) 0.0527(8) 0.4481(3) 0.042(2) Uani 1 1 d DU . .
H3E1 H 0.9247 0.0203 0.4436 0.05 Uiso 1 1 calc R . .
H3E2 H 0.7881 0.0114 0.4437 0.05 Uiso 1 1 calc R . .
C3F C 0.8817(10) 0.0874(8) 0.4960(4) 0.038(2) Uani 1 1 d DU . .
H3F1 H 0.8194 0.1193 0.5012 0.046 Uiso 1 1 calc R . .
H3F2 H 0.8744 0.0387 0.5145 0.046 Uiso 1 1 calc R . .
C3G C 1.0004(9) 0.1460(6) 0.5101(4) 0.0339(19) Uani 1 1 d DU . .
H3G1 H 1.0321 0.1303 0.5388 0.041 Uiso 1 1 calc R . .
H3G2 H 1.0545 0.1351 0.4892 0.041 Uiso 1 1 calc R . .
C3H C 0.9984(10) 0.2415(7) 0.5132(4) 0.0302(18) Uani 1 1 d DU . .
H3H1 H 0.9648 0.2556 0.5398 0.036 Uiso 1 1 calc R . .
H3H2 H 1.0794 0.2732 0.5162 0.036 Uiso 1 1 calc R . .
C4A C -0.1033(11) 0.3419(9) 0.2701(3) 0.039(2) Uani 1 1 d DU . .
H4 H -0.0386 0.312 0.264 0.047 Uiso 1 1 calc R . .
C4B C -0.1615(13) 0.3003(7) 0.3073(4) 0.044(2) Uani 1 1 d DU . .
H4B1 H -0.2294 0.3268 0.3116 0.052 Uiso 1 1 calc R . .
H4B2 H -0.106 0.3137 0.3341 0.052 Uiso 1 1 calc R . .
C4C C -0.2030(12) 0.2029(7) 0.3015(5) 0.051(2) Uani 1 1 d DU . .
H4C1 H -0.2177 0.1819 0.3301 0.061 Uiso 1 1 calc R . .
H4C2 H -0.2777 0.1905 0.2823 0.061 Uiso 1 1 calc R . .
C4D C -0.1175(13) 0.1530(10) 0.2824(4) 0.057(2) Uani 1 1 d DU . .
H4D1 H -0.0386 0.1882 0.2878 0.069 Uiso 1 1 calc R . .
H4D2 H -0.1162 0.101 0.2981 0.069 Uiso 1 1 calc R . .
C4E C -0.1456(16) 0.1272(9) 0.2337(4) 0.060(2) Uani 1 1 d DU . .
H4E1 H -0.2258 0.0941 0.2286 0.072 Uiso 1 1 calc R . .
H4E2 H -0.0932 0.0883 0.2262 0.072 Uiso 1 1 calc R . .
C4F C -0.1366(13) 0.1973(9) 0.2015(5) 0.055(2) Uani 1 1 d DU . .
H4F1 H -0.1456 0.1704 0.1717 0.066 Uiso 1 1 calc R . .
H4F2 H -0.0581 0.2331 0.2071 0.066 Uiso 1 1 calc R . .
C4G C -0.2279(12) 0.2548(8) 0.2042(5) 0.049(2) Uani 1 1 d DU . .
H4G1 H -0.2912 0.2254 0.2195 0.058 Uiso 1 1 calc R . .
H4G2 H -0.262 0.2621 0.1744 0.058 Uiso 1 1 calc R . .
C4H C -0.1813(12) 0.3434(8) 0.2275(4) 0.043(2) Uani 1 1 d DU . .
H4H1 H -0.1368 0.3793 0.2079 0.052 Uiso 1 1 calc R . .
H4H2 H -0.248 0.37 0.2336 0.052 Uiso 1 1 calc R . .
C5A C 0.3882(11) 0.3354(9) 0.2708(3) 0.0383(18) Uani 1 1 d DU . .
H5 H 0.3054 0.3054 0.2651 0.046 Uiso 1 1 calc R . .
C5B C 0.4419(12) 0.3338(7) 0.2282(3) 0.041(2) Uani 1 1 d DU . .
H5B1 H 0.5246 0.3616 0.2341 0.05 Uiso 1 1 calc R . .
H5B2 H 0.4026 0.3685 0.208 0.05 Uiso 1 1 calc R . .
C5C C 0.4356(11) 0.2459(7) 0.2051(4) 0.048(2) Uani 1 1 d DU . .
H5C1 H 0.4519 0.2539 0.1749 0.058 Uiso 1 1 calc R . .
H5C2 H 0.4982 0.2196 0.2195 0.058 Uiso 1 1 calc R . .
C5D C 0.3202(12) 0.1837(9) 0.2038(4) 0.057(2) Uani 1 1 d DU . .
H5D1 H 0.2587 0.2173 0.2073 0.068 Uiso 1 1 calc R . .
H5D2 H 0.3021 0.1536 0.1747 0.068 Uiso 1 1 calc R . .
C5E C 0.3126(15) 0.1168(9) 0.2373(4) 0.061(2) Uani 1 1 d DU . .
H5E1 H 0.3737 0.0829 0.2335 0.074 Uiso 1 1 calc R . .
H5E2 H 0.2368 0.0779 0.2302 0.074 Uiso 1 1 calc R . .
C5F C 0.3246(12) 0.1472(10) 0.2853(4) 0.058(2) Uani 1 1 d DU . .
H5F1 H 0.3078 0.0966 0.3021 0.069 Uiso 1 1 calc R . .
H5F2 H 0.2639 0.1814 0.2891 0.069 Uiso 1 1 calc R . .
C5G C 0.4421(11) 0.2001(7) 0.3055(5) 0.049(2) Uani 1 1 d DU . .
H5G1 H 0.461 0.1815 0.3348 0.058 Uiso 1 1 calc R . .
H5G2 H 0.5028 0.1876 0.2878 0.058 Uiso 1 1 calc R . .
C5H C 0.4478(12) 0.2968(7) 0.3091(4) 0.041(2) Uani 1 1 d DU . .
H5H1 H 0.4129 0.3113 0.3353 0.05 Uiso 1 1 calc R . .
H5H2 H 0.5306 0.3247 0.3137 0.05 Uiso 1 1 calc R . .
C6A C 0.4454(9) 0.2765(8) 0.4759(3) 0.0265(18) Uani 1 1 d DU . .
H6 H 0.5066 0.2417 0.4722 0.032 Uiso 1 1 calc R . .
C6B C 0.3860(11) 0.2492(7) 0.5156(4) 0.0306(18) Uani 1 1 d DU . .
H6B1 H 0.3228 0.2816 0.5183 0.037 Uiso 1 1 calc R . .
H6B2 H 0.4432 0.2644 0.5418 0.037 Uiso 1 1 calc R . .
C6C C 0.3349(10) 0.1540(6) 0.5140(4) 0.0333(18) Uani 1 1 d DU . .
H6C1 H 0.3143 0.1405 0.5432 0.04 Uiso 1 1 calc R . .
H6C2 H 0.2619 0.1428 0.4938 0.04 Uiso 1 1 calc R . .
C6D C 0.4125(11) 0.0934(8) 0.5002(3) 0.0354(19) Uani 1 1 d DU . .
H6D1 H 0.4063 0.0458 0.5194 0.043 Uiso 1 1 calc R . .
H6D2 H 0.4941 0.124 0.5048 0.043 Uiso 1 1 calc R . .
C6E C 0.3843(12) 0.0564(8) 0.4529(3) 0.0362(19) Uani 1 1 d DU . .
H6E1 H 0.3036 0.0241 0.4493 0.043 Uiso 1 1 calc R . .
H6E2 H 0.4357 0.015 0.4486 0.043 Uiso 1 1 calc R . .
C6F C 0.3949(11) 0.1175(8) 0.4159(4) 0.0344(18) Uani 1 1 d DU . .
H6F1 H 0.4758 0.1493 0.4191 0.041 Uiso 1 1 calc R . .
H6F2 H 0.3818 0.0825 0.3881 0.041 Uiso 1 1 calc R . .
C6G C 0.3133(10) 0.1820(6) 0.4128(4) 0.0311(19) Uani 1 1 d DU . .
H6G1 H 0.2449 0.1606 0.4276 0.037 Uiso 1 1 calc R . .
H6G2 H 0.2852 0.1853 0.3819 0.037 Uiso 1 1 calc R . .
C6H C 0.3674(10) 0.2725(7) 0.4325(3) 0.0284(18) Uani 1 1 d DU . .
H6H1 H 0.414 0.3022 0.4114 0.034 Uiso 1 1 calc R . .
H6H2 H 0.3039 0.3038 0.4368 0.034 Uiso 1 1 calc R . .
C7A C 0.2694(14) 0.3939(9) 0.0893(4) 0.064(2) Uani 1 1 d DU . .
H7 H 0.1871 0.3987 0.0922 0.077 Uiso 1 1 calc R . .
C7B C 0.2882(12) 0.4132(12) 0.0428(4) 0.070(2) Uani 1 1 d DU . .
H7B1 H 0.2321 0.3704 0.0234 0.084 Uiso 1 1 calc R . .
H7B2 H 0.2662 0.4691 0.0379 0.084 Uiso 1 1 calc R . .
C7C C 0.4070(12) 0.4157(10) 0.0276(5) 0.074(3) Uani 1 1 d DU . .
H7C1 H 0.4637 0.4591 0.0464 0.089 Uiso 1 1 calc R . .
H7C2 H 0.4034 0.4352 -0.0022 0.089 Uiso 1 1 calc R . .
C7D C 0.4545(13) 0.3328(9) 0.0270(6) 0.078(3) Uani 1 1 d DU . .
H7D1 H 0.4841 0.323 0.057 0.093 Uiso 1 1 calc R . .
H7D2 H 0.5206 0.3388 0.0097 0.093 Uiso 1 1 calc R . .
C7E C 0.3633(15) 0.2555(10) 0.0081(5) 0.078(3) Uani 1 1 d DU . .
H7E1 H 0.3005 0.2759 -0.0099 0.094 Uiso 1 1 calc R . .
H7E2 H 0.4 0.2205 -0.0113 0.094 Uiso 1 1 calc R . .
C7F C 0.3083(15) 0.1986(10) 0.0411(5) 0.077(3) Uani 1 1 d DU . .
H7F1 H 0.3724 0.1833 0.0607 0.093 Uiso 1 1 calc R . .
H7F2 H 0.2657 0.1453 0.025 0.093 Uiso 1 1 calc R . .
C7G C 0.2250(13) 0.2312(10) 0.0695(5) 0.074(3) Uani 1 1 d DU . .
H7G1 H 0.1883 0.1836 0.0853 0.089 Uiso 1 1 calc R . .
H7G2 H 0.1626 0.2499 0.0506 0.089 Uiso 1 1 calc R . .
C7H C 0.2834(15) 0.3053(9) 0.1027(5) 0.066(2) Uani 1 1 d DU . .
H7H1 H 0.2508 0.296 0.1304 0.08 Uiso 1 1 calc R . .
H7H2 H 0.3674 0.3038 0.108 0.08 Uiso 1 1 calc R . .
C8A C -0.0670(19) 0.4098(10) 0.0854(5) 0.106(3) Uani 1 1 d DU . .
H8 H 0.0172 0.4175 0.0815 0.128 Uiso 1 1 calc R . .
C8B C -0.110(2) 0.3242(10) 0.1005(5) 0.110(3) Uani 1 1 d DU . .
H8B1 H -0.0585 0.318 0.1271 0.132 Uiso 1 1 calc R . .
H8B2 H -0.1879 0.3252 0.1093 0.132 Uiso 1 1 calc R . .
C8C C -0.1206(18) 0.2447(10) 0.0719(5) 0.123(4) Uani 1 1 d DU . .
H8C1 H -0.124 0.1957 0.0901 0.147 Uiso 1 1 calc R . .
H8C2 H -0.0502 0.2481 0.0569 0.147 Uiso 1 1 calc R . .
C8D C -0.2281(17) 0.2292(14) 0.0379(5) 0.131(4) Uani 1 1 d DU . .
H8D1 H -0.2491 0.1669 0.0314 0.157 Uiso 1 1 calc R . .
H8D2 H -0.2917 0.2461 0.0525 0.157 Uiso 1 1 calc R . .
C8E C -0.2336(19) 0.2678(10) -0.0054(5) 0.135(4) Uani 1 1 d DU . .
H8E1 H -0.2987 0.2994 -0.0071 0.162 Uiso 1 1 calc R . .
H8E2 H -0.2547 0.2204 -0.0282 0.162 Uiso 1 1 calc R . .
C8F C -0.128(2) 0.3269(11) -0.0175(5) 0.136(4) Uani 1 1 d DU . .
H8F1 H -0.0594 0.3004 -0.0111 0.163 Uiso 1 1 calc R . .
H8F2 H -0.1396 0.3328 -0.0491 0.163 Uiso 1 1 calc R . .
C8G C -0.105(2) 0.4130(11) 0.0052(5) 0.127(4) Uani 1 1 d DU . .
H8G1 H -0.1375 0.4492 -0.0159 0.153 Uiso 1 1 calc R . .
H8G2 H -0.0193 0.4311 0.0074 0.153 Uiso 1 1 calc R . .
C8H C -0.1364(18) 0.4424(10) 0.0482(5) 0.118(3) Uani 1 1 d DU . .
H8H1 H -0.1216 0.5053 0.0511 0.142 Uiso 1 1 calc R . .
H8H2 H -0.2203 0.422 0.0493 0.142 Uiso 1 1 calc R . .
C9A C 0.423(2) 0.8656(10) 0.1310(5) 0.100(3) Uani 1 1 d DU . .
H9 H 0.3369 0.8526 0.1234 0.12 Uiso 1 1 calc R . .
C9B C 0.4420(17) 0.9485(10) 0.1584(6) 0.103(3) Uani 1 1 d DU . .
H9B1 H 0.3792 0.9793 0.1487 0.123 Uiso 1 1 calc R . .
H9B2 H 0.4338 0.9352 0.1888 0.123 Uiso 1 1 calc R . .
C9C C 0.5570(16) 1.0076(11) 0.1580(6) 0.111(3) Uani 1 1 d DU . .
H9C1 H 0.6142 0.9741 0.1488 0.134 Uiso 1 1 calc R . .
H9C2 H 0.5854 1.0324 0.1879 0.134 Uiso 1 1 calc R . .
C9D C 0.551(2) 1.0792(10) 0.1282(5) 0.117(4) Uani 1 1 d DU . .
H9D1 H 0.6143 1.1275 0.1386 0.14 Uiso 1 1 calc R . .
H9D2 H 0.4762 1.0988 0.1296 0.14 Uiso 1 1 calc R . .
C9E C 0.5608(17) 1.0527(10) 0.0811(5) 0.121(4) Uani 1 1 d DU . .
H9E1 H 0.6172 1.0139 0.0799 0.145 Uiso 1 1 calc R . .
H9E2 H 0.588 1.1033 0.0655 0.145 Uiso 1 1 calc R . .
C9F C 0.4395(17) 1.0074(10) 0.0600(6) 0.119(3) Uani 1 1 d DU . .
H9F1 H 0.3812 1.0241 0.0776 0.143 Uiso 1 1 calc R . .
H9F2 H 0.4251 1.0288 0.031 0.143 Uiso 1 1 calc R . .
C9G C 0.4191(19) 0.9138(10) 0.0547(5) 0.115(3) Uani 1 1 d DU . .
H9G1 H 0.4483 0.899 0.0273 0.138 Uiso 1 1 calc R . .
H9G2 H 0.3338 0.8946 0.0501 0.138 Uiso 1 1 calc R . .
C9H C 0.4656(18) 0.8580(9) 0.0880(5) 0.106(3) Uani 1 1 d DU . .
H9H1 H 0.4436 0.798 0.0763 0.127 Uiso 1 1 calc R . .
H9H2 H 0.5515 0.8727 0.092 0.127 Uiso 1 1 calc R . .
C10A C 0.9900(17) 0.8555(11) 0.1301(6) 0.081(3) Uani 1 1 d DU . .
H10 H 0.9073 0.8499 0.1171 0.097 Uiso 1 1 calc R . .
C10B C 1.0216(19) 0.9425(10) 0.1562(6) 0.084(3) Uani 1 1 d DU . .
H10D H 0.9611 0.9462 0.1755 0.101 Uiso 1 1 calc R . .
H10E H 1.0957 0.9443 0.1749 0.101 Uiso 1 1 calc R . .
C10C C 1.0345(16) 1.0218(12) 0.1301(7) 0.094(3) Uani 1 1 d DU . .
H10F H 1.0999 1.0215 0.1128 0.112 Uiso 1 1 calc R . .
H10G H 1.0547 1.073 0.1506 0.112 Uiso 1 1 calc R . .
C10D C 0.9253(17) 1.0289(13) 0.0994(6) 0.100(3) Uani 1 1 d DU . .
H10H H 0.8603 1.0235 0.1173 0.12 Uiso 1 1 calc R . .
H10I H 0.9373 1.0877 0.0903 0.12 Uiso 1 1 calc R . .
C10E C 0.8812(18) 0.9703(13) 0.0581(6) 0.101(3) Uani 1 1 d DU . .
H10J H 0.8182 0.9256 0.0654 0.121 Uiso 1 1 calc R . .
H10K H 0.8452 1.0044 0.0367 0.121 Uiso 1 1 calc R . .
C10F C 0.9645(19) 0.9255(13) 0.0352(7) 0.102(3) Uani 1 1 d DU . .
H10L H 0.934 0.9187 0.004 0.123 Uiso 1 1 calc R . .
H10M H 1.0395 0.9657 0.0379 0.123 Uiso 1 1 calc R . .
C10G C 0.9928(19) 0.8395(12) 0.0473(6) 0.097(3) Uani 1 1 d DU . .
H10N H 1.0397 0.8197 0.0257 0.116 Uiso 1 1 calc R . .
H10O H 0.9192 0.7978 0.0454 0.116 Uiso 1 1 calc R . .
C10H C 1.0590(16) 0.8405(14) 0.0927(5) 0.088(3) Uani 1 1 d DU . .
H10P H 1.0852 0.7855 0.0956 0.106 Uiso 1 1 calc R . .
H10Q H 1.1293 0.8856 0.0953 0.106 Uiso 1 1 calc R . .
N1 N 0.5212(9) 0.6823(8) 0.3226(4) 0.043(2) Uani 1 1 d U . .
H1A H 0.4615 0.6507 0.3342 0.065 Uiso 1 1 calc R . .
H1B H 0.5874 0.6882 0.3414 0.065 Uiso 1 1 calc R . .
H1C H 0.5313 0.6559 0.2971 0.065 Uiso 1 1 calc R . .
N2 N -0.0321(10) 0.6838(7) 0.3238(3) 0.038(2) Uani 1 1 d U . .
H2A H -0.0914 0.6617 0.3028 0.057 Uiso 1 1 calc R . .
H2B H -0.061 0.6915 0.3493 0.057 Uiso 1 1 calc R . .
H2C H 0.0188 0.6474 0.3269 0.057 Uiso 1 1 calc R . .
N3 N 0.9247(9) 0.3632(7) 0.4854(3) 0.031(2) Uani 1 1 d U . .
H3A H 0.8834 0.3834 0.4631 0.047 Uiso 1 1 calc R . .
H3B H 0.9981 0.3941 0.4899 0.047 Uiso 1 1 calc R . .
H3C H 0.8897 0.3676 0.5098 0.047 Uiso 1 1 calc R . .
N4 N -0.0516(10) 0.4327(7) 0.2859(4) 0.039(3) Uani 1 1 d U . .
H4A H -0.0045 0.4336 0.3112 0.058 Uiso 1 1 calc R . .
H4B H -0.1097 0.4615 0.2903 0.058 Uiso 1 1 calc R . .
H4C H -0.0095 0.4578 0.2657 0.058 Uiso 1 1 calc R . .
N5 N 0.3896(10) 0.4284(7) 0.2850(3) 0.036(2) Uani 1 1 d U . .
H5A H 0.3544 0.4535 0.263 0.054 Uiso 1 1 calc R . .
H5B H 0.4644 0.456 0.2919 0.054 Uiso 1 1 calc R . .
H5C H 0.3509 0.4309 0.3086 0.054 Uiso 1 1 calc R . .
N6 N 0.5033(9) 0.3690(6) 0.4852(3) 0.027(2) Uani 1 1 d U . .
H6A H 0.552 0.375 0.5105 0.041 Uiso 1 1 calc R . .
H6B H 0.4481 0.4014 0.4876 0.041 Uiso 1 1 calc R . .
H6C H 0.5446 0.386 0.4632 0.041 Uiso 1 1 calc R . .
N7 N 0.3428(9) 0.4583(8) 0.1210(4) 0.046(3) Uani 1 1 d U . .
H7A H 0.3348 0.5112 0.1134 0.069 Uiso 1 1 calc R . .
H7B H 0.4185 0.4528 0.1215 0.069 Uiso 1 1 calc R . .
H7C H 0.3205 0.4507 0.1478 0.069 Uiso 1 1 calc R . .
N8 N -0.0873(12) 0.4682(10) 0.1240(4) 0.067(3) Uani 1 1 d U . .
H8A H -0.0498 0.454 0.149 0.1 Uiso 1 1 calc R . .
H8B H -0.1648 0.4615 0.1261 0.1 Uiso 1 1 calc R . .
H8C H -0.0592 0.5233 0.1196 0.1 Uiso 1 1 calc R . .
N9 N 0.4446(11) 0.7961(9) 0.1567(4) 0.059(3) Uani 1 1 d U . .
H9A H 0.4134 0.8003 0.182 0.088 Uiso 1 1 calc R . .
H9B H 0.5225 0.7984 0.1625 0.088 Uiso 1 1 calc R . .
H9C H 0.4113 0.7459 0.1417 0.088 Uiso 1 1 calc R . .
N10 N 0.9928(10) 0.7877(9) 0.1589(4) 0.055(3) Uani 1 1 d U . .
H10A H 0.9503 0.7957 0.1809 0.083 Uiso 1 1 calc R . .
H10B H 1.0676 0.7876 0.17 0.083 Uiso 1 1 calc R . .
H10C H 0.9623 0.737 0.1439 0.083 Uiso 1 1 calc R . .
Br1 Br -0.06641(10) 0.60143(9) 0.21675(4) 0.0282(3) Uani 1 1 d U . .
Br2 Br 0.16880(11) 0.62273(9) 0.12276(4) 0.0323(3) Uani 1 1 d U . .
Br3 Br 0.44831(10) 0.60035(9) 0.21592(4) 0.0302(3) Uani 1 1 d U . .
Br4 Br 0.21964(10) 0.59413(9) 0.31618(4) 0.0271(3) Uani 1 1 d U . .
Br5 Br 0.14474(11) 0.42134(9) 0.19858(4) 0.0328(3) Uani 1 1 d U . .
Br6 Br 0.24269(11) 0.80535(9) 0.22518(4) 0.0308(3) Uani 1 1 d U . .
Br7 Br -0.02304(10) 0.52383(9) 0.40143(5) 0.0328(3) Uani 1 1 d U . .
Br8 Br 0.23594(10) 0.45635(8) 0.49538(4) 0.0260(3) Uani 1 1 d U . .
Br9 Br 0.47649(10) 0.52458(9) 0.40251(4) 0.0311(3) Uani 1 1 d U . .
Br10 Br 0.27854(11) 0.69111(9) 0.44561(4) 0.0283(3) Uani 1 1 d U . .
Br11 Br 0.16809(11) 0.35523(9) 0.34419(4) 0.0298(3) Uani 1 1 d U . .
Br12 Br 0.69469(11) 0.51550(9) 0.30570(4) 0.0298(3) Uani 1 1 d U . .
Br13 Br 0.77251(10) 0.71911(8) 0.39048(4) 0.0276(3) Uani 1 1 d U . .
Br14 Br 0.68518(10) 0.34349(8) 0.40940(4) 0.0269(3) Uani 1 1 d U . .
Br15 Br 0.49684(11) 0.63861(10) 0.09180(4) 0.0379(3) Uani 1 1 d U . .
Br16 Br 0.82124(12) 0.64280(11) 0.09069(5) 0.0432(4) Uani 1 1 d U . .
Br17 Br 0.72937(11) 0.80749(10) 0.18400(5) 0.0399(3) Uani 1 1 d U . .
Br18 Br 0.62584(11) 0.42864(10) 0.14086(5) 0.0382(3) Uani 1 1 d U . .
Pb1 Pb 0.19445(4) 0.61278(3) 0.214270(15) 0.02365(13) Uani 1 1 d U . .
Pb2 Pb 0.22518(3) 0.51764(3) 0.402549(14) 0.01827(12) Uani 1 1 d U . .
Pb3 Pb 0.72736(4) 0.52784(3) 0.400369(14) 0.01917(12) Uani 1 1 d U . .
Pb4 Pb 0.67374(4) 0.61849(4) 0.157538(17) 0.03192(14) Uani 1 1 d U . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1A N1 1.49(2) . ?
C1A C1H 1.537(8) . ?
C1A C1B 1.539(8) . ?
C1A H1 1 . ?
C1B C1C 1.507(9) . ?
C1B H1B1 0.99 . ?
C1B H1B2 0.99 . ?
C1C C1D 1.531(8) . ?
C1C H1C1 0.99 . ?
C1C H1C2 0.99 . ?
C1D C1E 1.526(9) . ?
C1D H1D1 0.99 . ?
C1D H1D2 0.99 . ?
C1E C1F 1.531(8) . ?
C1E H1E1 0.99 . ?
C1E H1E2 0.99 . ?
C1F C1G 1.533(8) . ?
C1F H1F1 0.99 . ?
C1F H1F2 0.99 . ?
C1G C1H 1.537(9) . ?
C1G H1G1 0.99 . ?
C1G H1G2 0.99 . ?
C1H H1H1 0.99 . ?
C1H H1H2 0.99 . ?
C2A N2 1.448(17) . ?
C2A C2H 1.517(9) . ?
C2A C2B 1.534(9) . ?
C2A H2 1 . ?
C2B C2C 1.540(9) . ?
C2B H2B1 0.99 . ?
C2B H2B2 0.99 . ?
C2C C2D 1.526(9) . ?
C2C H2C1 0.99 . ?
C2C H2C2 0.99 . ?
C2D C2E 1.527(10) . ?
C2D H2D1 0.99 . ?
C2D H2D2 0.99 . ?
C2E C2F 1.515(10) . ?
C2E H2E1 0.99 . ?
C2E H2E2 0.99 . ?
C2F C2G 1.524(10) . ?
C2F H2F1 0.99 . ?
C2F H2F2 0.99 . ?
C2G C2H 1.514(10) . ?
C2G H2G1 0.99 . ?
C2G H2G2 0.99 . ?
C2H H2H1 0.99 . ?
C2H H2H2 0.99 . ?
C3A N3 1.506(16) . ?
C3A C3H 1.527(9) . ?
C3A C3B 1.538(9) . ?
C3A H3 1 . ?
C3B C3C 1.535(9) . ?
C3B H3B1 0.99 . ?
C3B H3B2 0.99 . ?
C3C C3D 1.540(9) . ?
C3C H3C1 0.99 . ?
C3C H3C2 0.99 . ?
C3D C3E 1.542(9) . ?
C3D H3D1 0.99 . ?
C3D H3D2 0.99 . ?
C3E C3F 1.544(9) . ?
C3E H3E1 0.99 . ?
C3E H3E2 0.99 . ?
C3F C3G 1.545(9) . ?
C3F H3F1 0.99 . ?
C3F H3F2 0.99 . ?
C3G C3H 1.533(9) . ?
C3G H3G1 0.99 . ?
C3G H3G2 0.99 . ?
C3H H3H1 0.99 . ?
C3H H3H2 0.99 . ?
C4A N4 1.510(17) . ?
C4A C4H 1.530(9) . ?
C4A C4B 1.532(9) . ?
C4A H4 1 . ?
C4B C4C 1.546(9) . ?
C4B H4B1 0.99 . ?
C4B H4B2 0.99 . ?
C4C C4D 1.543(9) . ?
C4C H4C1 0.99 . ?
C4C H4C2 0.99 . ?
C4D C4E 1.535(9) . ?
C4D H4D1 0.99 . ?
C4D H4D2 0.99 . ?
C4E C4F 1.540(9) . ?
C4E H4E1 0.99 . ?
C4E H4E2 0.99 . ?
C4F C4G 1.542(9) . ?
C4F H4F1 0.99 . ?
C4F H4F2 0.99 . ?
C4G C4H 1.542(9) . ?
C4G H4G1 0.99 . ?
C4G H4G2 0.99 . ?
C4H H4H1 0.99 . ?
C4H H4H2 0.99 . ?
C5A C5H 1.530(8) . ?
C5A N5 1.531(17) . ?
C5A C5B 1.535(8) . ?
C5A H5 1 . ?
C5B C5C 1.535(8) . ?
C5B H5B1 0.99 . ?
C5B H5B2 0.99 . ?
C5C C5D 1.532(8) . ?
C5C H5C1 0.99 . ?
C5C H5C2 0.99 . ?
C5D C5E 1.530(8) . ?
C5D H5D1 0.99 . ?
C5D H5D2 0.99 . ?
C5E C5F 1.532(8) . ?
C5E H5E1 0.99 . ?
C5E H5E2 0.99 . ?
C5F C5G 1.538(8) . ?
C5F H5F1 0.99 . ?
C5F H5F2 0.99 . ?
C5G C5H 1.538(8) . ?
C5G H5G1 0.99 . ?
C5G H5G2 0.99 . ?
C5H H5H1 0.99 . ?
C5H H5H2 0.99 . ?
C6A N6 1.517(15) . ?
C6A C6B 1.532(9) . ?
C6A C6H 1.539(9) . ?
C6A H6 1 . ?
C6B C6C 1.534(9) . ?
C6B H6B1 0.99 . ?
C6B H6B2 0.99 . ?
C6C C6D 1.526(9) . ?
C6C H6C1 0.99 . ?
C6C H6C2 0.99 . ?
C6D C6E 1.537(9) . ?
C6D H6D1 0.99 . ?
C6D H6D2 0.99 . ?
C6E C6F 1.550(9) . ?
C6E H6E1 0.99 . ?
C6E H6E2 0.99 . ?
C6F C6G 1.532(9) . ?
C6F H6F1 0.99 . ?
C6F H6F2 0.99 . ?
C6G C6H 1.543(9) . ?
C6G H6G1 0.99 . ?
C6G H6G2 0.99 . ?
C6H H6H1 0.99 . ?
C6H H6H2 0.99 . ?
C7A N7 1.476(18) . ?
C7A C7B 1.528(8) . ?
C7A C7H 1.532(9) . ?
C7A H7 1 . ?
C7B C7C 1.522(8) . ?
C7B H7B1 0.99 . ?
C7B H7B2 0.99 . ?
C7C C7D 1.531(9) . ?
C7C H7C1 0.99 . ?
C7C H7C2 0.99 . ?
C7D C7E 1.532(8) . ?
C7D H7D1 0.99 . ?
C7D H7D2 0.99 . ?
C7E C7F 1.529(9) . ?
C7E H7E1 0.99 . ?
C7E H7E2 0.99 . ?
C7F C7G 1.534(9) . ?
C7F H7F1 0.99 . ?
C7F H7F2 0.99 . ?
C7G C7H 1.541(8) . ?
C7G H7G1 0.99 . ?
C7G H7G2 0.99 . ?
C7H H7H1 0.99 . ?
C7H H7H2 0.99 . ?
C8A C8B 1.494(9) . ?
C8A C8H 1.513(10) . ?
C8A N8 1.55(2) . ?
C8A H8 1 . ?
C8B C8C 1.495(10) . ?
C8B H8B1 0.99 . ?
C8B H8B2 0.99 . ?
C8C C8D 1.532(10) . ?
C8C H8C1 0.99 . ?
C8C H8C2 0.99 . ?
C8D C8E 1.511(9) . ?
C8D H8D1 0.99 . ?
C8D H8D2 0.99 . ?
C8E C8F 1.515(10) . ?
C8E H8E1 0.99 . ?
C8E H8E2 0.99 . ?
C8F C8G 1.482(9) . ?
C8F H8F1 0.99 . ?
C8F H8F2 0.99 . ?
C8G C8H 1.506(10) . ?
C8G H8G1 0.99 . ?
C8G H8G2 0.99 . ?
C8H H8H1 0.99 . ?
C8H H8H2 0.99 . ?
C9A N9 1.45(2) . ?
C9A C9H 1.488(10) . ?
C9A C9B 1.511(9) . ?
C9A H9 1 . ?
C9B C9C 1.510(10) . ?
C9B H9B1 0.99 . ?
C9B H9B2 0.99 . ?
C9C C9D 1.518(10) . ?
C9C H9C1 0.99 . ?
C9C H9C2 0.99 . ?
C9D C9E 1.531(10) . ?
C9D H9D1 0.99 . ?
C9D H9D2 0.99 . ?
C9E C9F 1.541(10) . ?
C9E H9E1 0.99 . ?
C9E H9E2 0.99 . ?
C9F C9G 1.475(9) . ?
C9F H9F1 0.99 . ?
C9F H9F2 0.99 . ?
C9G C9H 1.520(10) . ?
C9G H9G1 0.99 . ?
C9G H9G2 0.99 . ?
C9H H9H1 0.99 . ?
C9H H9H2 0.99 . ?
C10A N10 1.45(2) . ?
C10A C10H 1.526(10) . ?
C10A C10B 1.542(10) . ?
C10A H10 1 . ?
C10B C10C 1.538(10) . ?
C10B H10D 0.99 . ?
C10B H10E 0.99 . ?
C10C C10D 1.539(10) . ?
C10C H10F 0.99 . ?
C10C H10G 0.99 . ?
C10D C10E 1.536(10) . ?
C10D H10H 0.99 . ?
C10D H10I 0.99 . ?
C10E C10F 1.532(10) . ?
C10E H10J 0.99 . ?
C10E H10K 0.99 . ?
C10F C10G 1.530(10) . ?
C10F H10L 0.99 . ?
C10F H10M 0.99 . ?
C10G C10H 1.536(10) . ?
C10G H10N 0.99 . ?
C10G H10O 0.99 . ?
C10H H10P 0.99 . ?
C10H H10Q 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
N2 H2A 0.91 . ?
N2 H2B 0.91 . ?
N2 H2C 0.91 . ?
N3 H3A 0.91 . ?
N3 H3B 0.91 . ?
N3 H3C 0.91 . ?
N4 H4A 0.91 . ?
N4 H4B 0.91 . ?
N4 H4C 0.91 . ?
N5 H5A 0.91 . ?
N5 H5B 0.91 . ?
N5 H5C 0.91 . ?
N6 H6A 0.91 . ?
N6 H6B 0.91 . ?
N6 H6C 0.91 . ?
N7 H7A 0.91 . ?
N7 H7B 0.91 . ?
N7 H7C 0.91 . ?
N8 H8A 0.91 . ?
N8 H8B 0.91 . ?
N8 H8C 0.91 . ?
N9 H9A 0.91 . ?
N9 H9B 0.91 . ?
N9 H9C 0.91 . ?
N10 H10A 0.91 . ?
N10 H10B 0.91 . ?
N10 H10C 0.91 . ?
Br1 Pb1 3.0572(13) . ?
Br1 Pb4 3.4554(14) 1_455 ?
Br2 Pb1 2.8469(14) . ?
Br3 Pb1 3.0289(13) . ?
Br3 Pb4 3.3623(13) . ?
Br4 Pb2 3.0104(13) . ?
Br4 Pb1 3.1877(13) . ?
Br5 Pb1 3.0249(15) . ?
Br6 Pb1 3.0330(15) . ?
Br7 Pb2 2.9412(12) . ?
Br7 Pb3 2.9505(12) 1_455 ?
Br8 Pb2 3.0960(13) . ?
Br8 Pb3 3.2172(13) 2_666 ?
Br9 Pb2 2.9443(12) . ?
Br9 Pb3 2.9562(12) . ?
Br10 Pb2 2.9567(15) . ?
Br11 Pb2 3.0268(14) . ?
Br12 Pb3 2.9216(13) . ?
Br13 Pb3 3.0554(14) . ?
Br14 Pb3 2.9421(14) . ?
Br15 Pb4 2.8271(15) . ?
Br16 Pb4 2.8558(15) . ?
Br17 Pb4 3.0353(16) . ?
Br18 Pb4 3.0031(16) . ?
Pb3 Br7 2.9505(13) 1_655 ?
Pb3 Br8 3.2172(13) 2_666 ?
Pb4 Br1 3.4554(14) 1_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1A C1H 105.5(11) . . ?
N1 C1A C1B 96.2(11) . . ?
C1H C1A C1B 117.0(11) . . ?
N1 C1A H1 112.2 . . ?
C1H C1A H1 112.2 . . ?
C1B C1A H1 112.2 . . ?
C1C C1B C1A 121.1(13) . . ?
C1C C1B H1B1 107 . . ?
C1A C1B H1B1 107 . . ?
C1C C1B H1B2 107 . . ?
C1A C1B H1B2 107 . . ?
H1B1 C1B H1B2 106.8 . . ?
C1B C1C C1D 114.3(12) . . ?
C1B C1C H1C1 108.7 . . ?
C1D C1C H1C1 108.7 . . ?
C1B C1C H1C2 108.7 . . ?
C1D C1C H1C2 108.7 . . ?
H1C1 C1C H1C2 107.6 . . ?
C1E C1D C1C 110.5(12) . . ?
C1E C1D H1D1 109.5 . . ?
C1C C1D H1D1 109.5 . . ?
C1E C1D H1D2 109.5 . . ?
C1C C1D H1D2 109.6 . . ?
H1D1 C1D H1D2 108.1 . . ?
C1D C1E C1F 113.7(13) . . ?
C1D C1E H1E1 108.8 . . ?
C1F C1E H1E1 108.8 . . ?
C1D C1E H1E2 108.8 . . ?
C1F C1E H1E2 108.8 . . ?
H1E1 C1E H1E2 107.7 . . ?
C1E C1F C1G 119.1(12) . . ?
C1E C1F H1F1 107.5 . . ?
C1G C1F H1F1 107.5 . . ?
C1E C1F H1F2 107.5 . . ?
C1G C1F H1F2 107.5 . . ?
H1F1 C1F H1F2 107 . . ?
C1F C1G C1H 114.3(12) . . ?
C1F C1G H1G1 108.7 . . ?
C1H C1G H1G1 108.7 . . ?
C1F C1G H1G2 108.7 . . ?
C1H C1G H1G2 108.7 . . ?
H1G1 C1G H1G2 107.6 . . ?
C1G C1H C1A 115.1(12) . . ?
C1G C1H H1H1 108.5 . . ?
C1A C1H H1H1 108.5 . . ?
C1G C1H H1H2 108.5 . . ?
C1A C1H H1H2 108.5 . . ?
H1H1 C1H H1H2 107.5 . . ?
N2 C2A C2H 111.6(12) . . ?
N2 C2A C2B 108.5(11) . . ?
C2H C2A C2B 118.2(13) . . ?
N2 C2A H2 105.9 . . ?
C2H C2A H2 105.9 . . ?
C2B C2A H2 105.9 . . ?
C2A C2B C2C 117.3(13) . . ?
C2A C2B H2B1 108 . . ?
C2C C2B H2B1 108 . . ?
C2A C2B H2B2 108 . . ?
C2C C2B H2B2 108 . . ?
H2B1 C2B H2B2 107.2 . . ?
C2D C2C C2B 119.9(12) . . ?
C2D C2C H2C1 107.4 . . ?
C2B C2C H2C1 107.4 . . ?
C2D C2C H2C2 107.4 . . ?
C2B C2C H2C2 107.4 . . ?
H2C1 C2C H2C2 106.9 . . ?
C2C C2D C2E 114.9(13) . . ?
C2C C2D H2D1 108.5 . . ?
C2E C2D H2D1 108.5 . . ?
C2C C2D H2D2 108.5 . . ?
C2E C2D H2D2 108.5 . . ?
H2D1 C2D H2D2 107.5 . . ?
C2F C2E C2D 119.5(15) . . ?
C2F C2E H2E1 107.4 . . ?
C2D C2E H2E1 107.4 . . ?
C2F C2E H2E2 107.4 . . ?
C2D C2E H2E2 107.4 . . ?
H2E1 C2E H2E2 107 . . ?
C2E C2F C2G 125.6(14) . . ?
C2E C2F H2F1 105.9 . . ?
C2G C2F H2F1 105.9 . . ?
C2E C2F H2F2 105.9 . . ?
C2G C2F H2F2 105.9 . . ?
H2F1 C2F H2F2 106.2 . . ?
C2H C2G C2F 124.0(15) . . ?
C2H C2G H2G1 106.3 . . ?
C2F C2G H2G1 106.3 . . ?
C2H C2G H2G2 106.3 . . ?
C2F C2G H2G2 106.3 . . ?
H2G1 C2G H2G2 106.4 . . ?
C2G C2H C2A 118.2(14) . . ?
C2G C2H H2H1 107.8 . . ?
C2A C2H H2H1 107.8 . . ?
C2G C2H H2H2 107.8 . . ?
C2A C2H H2H2 107.8 . . ?
H2H1 C2H H2H2 107.1 . . ?
N3 C3A C3H 106.8(9) . . ?
N3 C3A C3B 107.0(9) . . ?
C3H C3A C3B 117.1(10) . . ?
N3 C3A H3 108.6 . . ?
C3H C3A H3 108.6 . . ?
C3B C3A H3 108.6 . . ?
C3C C3B C3A 116.1(10) . . ?
C3C C3B H3B1 108.3 . . ?
C3A C3B H3B1 108.3 . . ?
C3C C3B H3B2 108.3 . . ?
C3A C3B H3B2 108.3 . . ?
H3B1 C3B H3B2 107.4 . . ?
C3B C3C C3D 115.2(10) . . ?
C3B C3C H3C1 108.5 . . ?
C3D C3C H3C1 108.5 . . ?
C3B C3C H3C2 108.5 . . ?
C3D C3C H3C2 108.5 . . ?
H3C1 C3C H3C2 107.5 . . ?
C3C C3D C3E 115.5(11) . . ?
C3C C3D H3D1 108.4 . . ?
C3E C3D H3D1 108.4 . . ?
C3C C3D H3D2 108.4 . . ?
C3E C3D H3D2 108.4 . . ?
H3D1 C3D H3D2 107.5 . . ?
C3D C3E C3F 119.8(11) . . ?
C3D C3E H3E1 107.4 . . ?
C3F C3E H3E1 107.4 . . ?
C3D C3E H3E2 107.4 . . ?
C3F C3E H3E2 107.4 . . ?
H3E1 C3E H3E2 106.9 . . ?
C3G C3F C3E 114.6(10) . . ?
C3G C3F H3F1 108.6 . . ?
C3E C3F H3F1 108.6 . . ?
C3G C3F H3F2 108.6 . . ?
C3E C3F H3F2 108.6 . . ?
H3F1 C3F H3F2 107.6 . . ?
C3H C3G C3F 115.5(10) . . ?
C3H C3G H3G1 108.4 . . ?
C3F C3G H3G1 108.4 . . ?
C3H C3G H3G2 108.4 . . ?
C3F C3G H3G2 108.4 . . ?
H3G1 C3G H3G2 107.5 . . ?
C3A C3H C3G 114.1(10) . . ?
C3A C3H H3H1 108.7 . . ?
C3G C3H H3H1 108.7 . . ?
C3A C3H H3H2 108.7 . . ?
C3G C3H H3H2 108.7 . . ?
H3H1 C3H H3H2 107.6 . . ?
N4 C4A C4H 107.7(10) . . ?
N4 C4A C4B 107.1(10) . . ?
C4H C4A C4B 116.7(11) . . ?
N4 C4A H4 108.4 . . ?
C4H C4A H4 108.4 . . ?
C4B C4A H4 108.4 . . ?
C4A C4B C4C 116.4(11) . . ?
C4A C4B H4B1 108.2 . . ?
C4C C4B H4B1 108.2 . . ?
C4A C4B H4B2 108.2 . . ?
C4C C4B H4B2 108.2 . . ?
H4B1 C4B H4B2 107.3 . . ?
C4D C4C C4B 115.0(12) . . ?
C4D C4C H4C1 108.5 . . ?
C4B C4C H4C1 108.5 . . ?
C4D C4C H4C2 108.5 . . ?
C4B C4C H4C2 108.5 . . ?
H4C1 C4C H4C2 107.5 . . ?
C4E C4D C4C 115.0(13) . . ?
C4E C4D H4D1 108.5 . . ?
C4C C4D H4D1 108.5 . . ?
C4E C4D H4D2 108.5 . . ?
C4C C4D H4D2 108.5 . . ?
H4D1 C4D H4D2 107.5 . . ?
C4D C4E C4F 118.8(13) . . ?
C4D C4E H4E1 107.6 . . ?
C4F C4E H4E1 107.6 . . ?
C4D C4E H4E2 107.6 . . ?
C4F C4E H4E2 107.6 . . ?
H4E1 C4E H4E2 107 . . ?
C4E C4F C4G 113.7(13) . . ?
C4E C4F H4F1 108.8 . . ?
C4G C4F H4F1 108.8 . . ?
C4E C4F H4F2 108.8 . . ?
C4G C4F H4F2 108.8 . . ?
H4F1 C4F H4F2 107.7 . . ?
C4F C4G C4H 115.0(12) . . ?
C4F C4G H4G1 108.5 . . ?
C4H C4G H4G1 108.5 . . ?
C4F C4G H4G2 108.5 . . ?
C4H C4G H4G2 108.5 . . ?
H4G1 C4G H4G2 107.5 . . ?
C4A C4H C4G 113.8(11) . . ?
C4A C4H H4H1 108.8 . . ?
C4G C4H H4H1 108.8 . . ?
C4A C4H H4H2 108.8 . . ?
C4G C4H H4H2 108.8 . . ?
H4H1 C4H H4H2 107.7 . . ?
C5H C5A N5 106.9(9) . . ?
C5H C5A C5B 117.1(11) . . ?
N5 C5A C5B 107.7(9) . . ?
C5H C5A H5 108.3 . . ?
N5 C5A H5 108.3 . . ?
C5B C5A H5 108.3 . . ?
C5A C5B C5C 116.4(10) . . ?
C5A C5B H5B1 108.2 . . ?
C5C C5B H5B1 108.2 . . ?
C5A C5B H5B2 108.2 . . ?
C5C C5B H5B2 108.2 . . ?
H5B1 C5B H5B2 107.3 . . ?
C5D C5C C5B 116.0(11) . . ?
C5D C5C H5C1 108.3 . . ?
C5B C5C H5C1 108.3 . . ?
C5D C5C H5C2 108.3 . . ?
C5B C5C H5C2 108.3 . . ?
H5C1 C5C H5C2 107.4 . . ?
C5E C5D C5C 117.6(12) . . ?
C5E C5D H5D1 107.9 . . ?
C5C C5D H5D1 107.9 . . ?
C5E C5D H5D2 107.9 . . ?
C5C C5D H5D2 107.9 . . ?
H5D1 C5D H5D2 107.2 . . ?
C5D C5E C5F 118.2(12) . . ?
C5D C5E H5E1 107.7 . . ?
C5F C5E H5E1 107.7 . . ?
C5D C5E H5E2 107.8 . . ?
C5F C5E H5E2 107.8 . . ?
H5E1 C5E H5E2 107.1 . . ?
C5E C5F C5G 117.4(12) . . ?
C5E C5F H5F1 107.9 . . ?
C5G C5F H5F1 107.9 . . ?
C5E C5F H5F2 107.9 . . ?
C5G C5F H5F2 108 . . ?
H5F1 C5F H5F2 107.2 . . ?
C5H C5G C5F 115.3(11) . . ?
C5H C5G H5G1 108.5 . . ?
C5F C5G H5G1 108.5 . . ?
C5H C5G H5G2 108.5 . . ?
C5F C5G H5G2 108.5 . . ?
H5G1 C5G H5G2 107.5 . . ?
C5A C5H C5G 117.1(10) . . ?
C5A C5H H5H1 108 . . ?
C5G C5H H5H1 108 . . ?
C5A C5H H5H2 108 . . ?
C5G C5H H5H2 108 . . ?
H5H1 C5H H5H2 107.3 . . ?
N6 C6A C6B 107.2(9) . . ?
N6 C6A C6H 105.6(9) . . ?
C6B C6A C6H 117.3(10) . . ?
N6 C6A H6 108.8 . . ?
C6B C6A H6 108.8 . . ?
C6H C6A H6 108.8 . . ?
C6A C6B C6C 114.3(10) . . ?
C6A C6B H6B1 108.7 . . ?
C6C C6B H6B1 108.7 . . ?
C6A C6B H6B2 108.7 . . ?
C6C C6B H6B2 108.7 . . ?
H6B1 C6B H6B2 107.6 . . ?
C6D C6C C6B 116.3(10) . . ?
C6D C6C H6C1 108.2 . . ?
C6B C6C H6C1 108.2 . . ?
C6D C6C H6C2 108.2 . . ?
C6B C6C H6C2 108.2 . . ?
H6C1 C6C H6C2 107.4 . . ?
C6C C6D C6E 115.1(11) . . ?
C6C C6D H6D1 108.5 . . ?
C6E C6D H6D1 108.5 . . ?
C6C C6D H6D2 108.5 . . ?
C6E C6D H6D2 108.5 . . ?
H6D1 C6D H6D2 107.5 . . ?
C6D C6E C6F 119.2(11) . . ?
C6D C6E H6E1 107.5 . . ?
C6F C6E H6E1 107.5 . . ?
C6D C6E H6E2 107.5 . . ?
C6F C6E H6E2 107.5 . . ?
H6E1 C6E H6E2 107 . . ?
C6G C6F C6E 117.3(11) . . ?
C6G C6F H6F1 108 . . ?
C6E C6F H6F1 108 . . ?
C6G C6F H6F2 108 . . ?
C6E C6F H6F2 108 . . ?
H6F1 C6F H6F2 107.2 . . ?
C6F C6G C6H 115.2(10) . . ?
C6F C6G H6G1 108.5 . . ?
C6H C6G H6G1 108.5 . . ?
C6F C6G H6G2 108.5 . . ?
C6H C6G H6G2 108.5 . . ?
H6G1 C6G H6G2 107.5 . . ?
C6A C6H C6G 114.9(10) . . ?
C6A C6H H6H1 108.5 . . ?
C6G C6H H6H1 108.5 . . ?
C6A C6H H6H2 108.5 . . ?
C6G C6H H6H2 108.5 . . ?
H6H1 C6H H6H2 107.5 . . ?
N7 C7A C7B 111.6(12) . . ?
N7 C7A C7H 109.0(11) . . ?
C7B C7A C7H 116.7(12) . . ?
N7 C7A H7 106.3 . . ?
C7B C7A H7 106.3 . . ?
C7H C7A H7 106.3 . . ?
C7C C7B C7A 120.5(13) . . ?
C7C C7B H7B1 107.2 . . ?
C7A C7B H7B1 107.2 . . ?
C7C C7B H7B2 107.2 . . ?
C7A C7B H7B2 107.2 . . ?
H7B1 C7B H7B2 106.8 . . ?
C7B C7C C7D 117.2(13) . . ?
C7B C7C H7C1 108 . . ?
C7D C7C H7C1 108 . . ?
C7B C7C H7C2 108 . . ?
C7D C7C H7C2 108 . . ?
H7C1 C7C H7C2 107.2 . . ?
C7C C7D C7E 113.1(13) . . ?
C7C C7D H7D1 109 . . ?
C7E C7D H7D1 109 . . ?
C7C C7D H7D2 109 . . ?
C7E C7D H7D2 109 . . ?
H7D1 C7D H7D2 107.8 . . ?
C7F C7E C7D 115.9(13) . . ?
C7F C7E H7E1 108.3 . . ?
C7D C7E H7E1 108.3 . . ?
C7F C7E H7E2 108.3 . . ?
C7D C7E H7E2 108.3 . . ?
H7E1 C7E H7E2 107.4 . . ?
C7E C7F C7G 119.6(14) . . ?
C7E C7F H7F1 107.4 . . ?
C7G C7F H7F1 107.4 . . ?
C7E C7F H7F2 107.4 . . ?
C7G C7F H7F2 107.4 . . ?
H7F1 C7F H7F2 106.9 . . ?
C7F C7G C7H 114.2(12) . . ?
C7F C7G H7G1 108.7 . . ?
C7H C7G H7G1 108.7 . . ?
C7F C7G H7G2 108.7 . . ?
C7H C7G H7G2 108.7 . . ?
H7G1 C7G H7G2 107.6 . . ?
C7A C7H C7G 115.3(12) . . ?
C7A C7H H7H1 108.4 . . ?
C7G C7H H7H1 108.4 . . ?
C7A C7H H7H2 108.4 . . ?
C7G C7H H7H2 108.5 . . ?
H7H1 C7H H7H2 107.5 . . ?
C8B C8A C8H 119.6(13) . . ?
C8B C8A N8 100.7(13) . . ?
C8H C8A N8 101.0(14) . . ?
C8B C8A H8 111.4 . . ?
C8H C8A H8 111.4 . . ?
N8 C8A H8 111.5 . . ?
C8C C8B C8A 121.7(13) . . ?
C8C C8B H8B1 106.8 . . ?
C8A C8B H8B1 106.8 . . ?
C8C C8B H8B2 107.3 . . ?
C8A C8B H8B2 106.8 . . ?
H8B1 C8B H8B2 106.7 . . ?
C8B C8C C8D 113.2(13) . . ?
C8B C8C H8C1 108.7 . . ?
C8D C8C H8C1 108.5 . . ?
C8B C8C H8C2 109.3 . . ?
C8D C8C H8C2 109.2 . . ?
H8C1 C8C H8C2 107.7 . . ?
C8E C8D C8C 124.5(11) . . ?
C8E C8D H8D1 106.3 . . ?
C8C C8D H8D1 106.5 . . ?
C8E C8D H8D2 105.7 . . ?
C8C C8D H8D2 106.4 . . ?
H8D1 C8D H8D2 106.4 . . ?
C8D C8E C8F 120.0(11) . . ?
C8D C8E H8E1 107.9 . . ?
C8F C8E H8E1 107.1 . . ?
C8D C8E H8E2 107.2 . . ?
C8F C8E H8E2 107.1 . . ?
H8E1 C8E H8E2 106.9 . . ?
C8G C8F C8E 114.9(10) . . ?
C8G C8F H8F1 107.8 . . ?
C8E C8F H8F1 108.3 . . ?
C8G C8F H8F2 109 . . ?
C8E C8F H8F2 109.1 . . ?
H8F1 C8F H8F2 107.6 . . ?
C8F C8G C8H 130.0(10) . . ?
C8F C8G H8G1 104.2 . . ?
C8H C8G H8G1 104.5 . . ?
C8F C8G H8G2 105.5 . . ?
C8H C8G H8G2 104.9 . . ?
H8G1 C8G H8G2 105.8 . . ?
C8A C8H C8G 111.4(13) . . ?
C8A C8H H8H1 109.3 . . ?
C8G C8H H8H1 109.5 . . ?
C8A C8H H8H2 109.3 . . ?
C8G C8H H8H2 109.4 . . ?
H8H1 C8H H8H2 108 . . ?
N9 C9A C9H 111.3(14) . . ?
N9 C9A C9B 111.7(14) . . ?
C9H C9A C9B 123.1(12) . . ?
N9 C9A H9 102.5 . . ?
C9H C9A H9 102.6 . . ?
C9B C9A H9 102.6 . . ?
C9C C9B C9A 116.6(13) . . ?
C9C C9B H9B1 108.1 . . ?
C9A C9B H9B1 108.1 . . ?
C9C C9B H9B2 108.2 . . ?
C9A C9B H9B2 108.2 . . ?
H9B1 C9B H9B2 107.3 . . ?
C9B C9C C9D 113.7(13) . . ?
C9B C9C H9C1 108.8 . . ?
C9D C9C H9C1 108.8 . . ?
C9B C9C H9C2 108.8 . . ?
C9D C9C H9C2 108.8 . . ?
H9C1 C9C H9C2 107.7 . . ?
C9C C9D C9E 112.8(13) . . ?
C9C C9D H9D1 109 . . ?
C9E C9D H9D1 109.1 . . ?
C9C C9D H9D2 109 . . ?
C9E C9D H9D2 109 . . ?
H9D1 C9D H9D2 107.8 . . ?
C9D C9E C9F 107.7(12) . . ?
C9D C9E H9E1 110.1 . . ?
C9F C9E H9E1 110.2 . . ?
C9D C9E H9E2 110.2 . . ?
C9F C9E H9E2 110.2 . . ?
H9E1 C9E H9E2 108.5 . . ?
C9G C9F C9E 116.9(12) . . ?
C9G C9F H9F1 108.2 . . ?
C9E C9F H9F1 108.1 . . ?
C9G C9F H9F2 108 . . ?
C9E C9F H9F2 108 . . ?
H9F1 C9F H9F2 107.3 . . ?
C9F C9G C9H 124.2(11) . . ?
C9F C9G H9G1 106.4 . . ?
C9H C9G H9G1 106.4 . . ?
C9F C9G H9G2 106.1 . . ?
C9H C9G H9G2 106.2 . . ?
H9G1 C9G H9G2 106.4 . . ?
C9A C9H C9G 114.6(13) . . ?
C9A C9H H9H1 108.6 . . ?
C9G C9H H9H1 108.6 . . ?
C9A C9H H9H2 108.7 . . ?
C9G C9H H9H2 108.6 . . ?
H9H1 C9H H9H2 107.6 . . ?
N10 C10A C10H 109.2(15) . . ?
N10 C10A C10B 110.3(14) . . ?
C10H C10A C10B 117.8(17) . . ?
N10 C10A H10 106.3 . . ?
C10H C10A H10 106.3 . . ?
C10B C10A H10 106.3 . . ?
C10C C10B C10A 116.9(17) . . ?
C10C C10B H10D 108.1 . . ?
C10A C10B H10D 108.1 . . ?
C10C C10B H10E 108.1 . . ?
C10A C10B H10E 108.1 . . ?
H10D C10B H10E 107.3 . . ?
C10B C10C C10D 114.4(16) . . ?
C10B C10C H10F 108.7 . . ?
C10D C10C H10F 108.6 . . ?
C10B C10C H10G 108.7 . . ?
C10D C10C H10G 108.7 . . ?
H10F C10C H10G 107.6 . . ?
C10E C10D C10C 123.5(19) . . ?
C10E C10D H10H 106.4 . . ?
C10C C10D H10H 106.4 . . ?
C10E C10D H10I 106.4 . . ?
C10C C10D H10I 106.4 . . ?
H10H C10D H10I 106.5 . . ?
C10F C10E C10D 120.7(19) . . ?
C10F C10E H10J 107.1 . . ?
C10D C10E H10J 107.1 . . ?
C10F C10E H10K 107.1 . . ?
C10D C10E H10K 107.2 . . ?
H10J C10E H10K 106.8 . . ?
C10G C10F C10E 123.1(19) . . ?
C10G C10F H10L 106.6 . . ?
C10E C10F H10L 106.5 . . ?
C10G C10F H10M 106.5 . . ?
C10E C10F H10M 106.5 . . ?
H10L C10F H10M 106.5 . . ?
C10F C10G C10H 114.5(17) . . ?
C10F C10G H10N 108.6 . . ?
C10H C10G H10N 108.7 . . ?
C10F C10G H10O 108.6 . . ?
C10H C10G H10O 108.6 . . ?
H10N C10G H10O 107.6 . . ?
C10A C10H C10G 115.1(16) . . ?
C10A C10H H10P 108.5 . . ?
C10G C10H H10P 108.5 . . ?
C10A C10H H10Q 108.5 . . ?
C10G C10H H10Q 108.5 . . ?
H10P C10H H10Q 107.5 . . ?
C1A N1 H1A 109.5 . . ?
C1A N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1A N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2A N2 H2A 109.5 . . ?
C2A N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C2A N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C3A N3 H3A 109.5 . . ?
C3A N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C3A N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C4A N4 H4A 109.5 . . ?
C4A N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4A N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C5A N5 H5A 109.5 . . ?
C5A N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C5A N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C6A N6 H6A 109.5 . . ?
C6A N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C6A N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C7A N7 H7A 109.5 . . ?
C7A N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C7A N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C8A N8 H8A 109.5 . . ?
C8A N8 H8B 109.5 . . ?
H8A N8 H8B 109.5 . . ?
C8A N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C9A N9 H9A 109.5 . . ?
C9A N9 H9B 109.5 . . ?
H9A N9 H9B 109.5 . . ?
C9A N9 H9C 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
C10A N10 H10A 109.5 . . ?
C10A N10 H10B 109.5 . . ?
H10A N10 H10B 109.5 . . ?
C10A N10 H10C 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
Pb1 Br1 Pb4 144.96(4) . 1_455 ?
Pb1 Br3 Pb4 144.70(5) . . ?
Pb2 Br4 Pb1 161.71(5) . . ?
Pb2 Br7 Pb3 179.32(6) . 1_455 ?
Pb2 Br8 Pb3 157.39(5) . 2_666 ?
Pb2 Br9 Pb3 178.37(6) . . ?
Br2 Pb1 Br5 88.07(4) . . ?
Br2 Pb1 Br3 91.68(4) . . ?
Br5 Pb1 Br3 86.12(4) . . ?
Br2 Pb1 Br6 89.09(4) . . ?
Br5 Pb1 Br6 177.16(4) . . ?
Br3 Pb1 Br6 94.03(4) . . ?
Br2 Pb1 Br1 91.61(4) . . ?
Br5 Pb1 Br1 87.11(4) . . ?
Br3 Pb1 Br1 172.37(4) . . ?
Br6 Pb1 Br1 92.91(4) . . ?
Br2 Pb1 Br4 177.84(4) . . ?
Br5 Pb1 Br4 89.80(4) . . ?
Br3 Pb1 Br4 88.52(3) . . ?
Br6 Pb1 Br4 93.04(4) . . ?
Br1 Pb1 Br4 87.94(3) . . ?
Br7 Pb2 Br9 175.86(4) . . ?
Br7 Pb2 Br10 88.23(4) . . ?
Br9 Pb2 Br10 88.43(4) . . ?
Br7 Pb2 Br4 88.82(4) . . ?
Br9 Pb2 Br4 88.67(4) . . ?
Br10 Pb2 Br4 89.01(4) . . ?
Br7 Pb2 Br11 91.06(4) . . ?
Br9 Pb2 Br11 91.80(4) . . ?
Br10 Pb2 Br11 170.19(4) . . ?
Br4 Pb2 Br11 81.19(4) . . ?
Br7 Pb2 Br8 90.97(4) . . ?
Br9 Pb2 Br8 91.22(4) . . ?
Br10 Pb2 Br8 85.57(4) . . ?
Br4 Pb2 Br8 174.59(4) . . ?
Br11 Pb2 Br8 104.23(4) . . ?
Br12 Pb3 Br14 95.75(4) . . ?
Br12 Pb3 Br7 91.04(4) . 1_655 ?
Br14 Pb3 Br7 88.70(4) . 1_655 ?
Br12 Pb3 Br9 90.89(4) . . ?
Br14 Pb3 Br9 88.76(4) . . ?
Br7 Pb3 Br9 176.96(4) 1_655 . ?
Br12 Pb3 Br13 83.96(4) . . ?
Br14 Pb3 Br13 179.55(4) . . ?
Br7 Pb3 Br13 90.96(4) 1_655 . ?
Br9 Pb3 Br13 91.59(4) . . ?
Br12 Pb3 Br8 179.37(4) . 2_666 ?
Br14 Pb3 Br8 84.87(4) . 2_666 ?
Br7 Pb3 Br8 88.93(4) 1_655 2_666 ?
Br9 Pb3 Br8 89.16(4) . 2_666 ?
Br13 Pb3 Br8 95.42(4) . 2_666 ?
Br15 Pb4 Br16 84.36(4) . . ?
Br15 Pb4 Br18 92.68(4) . . ?
Br16 Pb4 Br18 92.97(5) . . ?
Br15 Pb4 Br17 92.31(5) . . ?
Br16 Pb4 Br17 90.55(5) . . ?
Br18 Pb4 Br17 174.15(5) . . ?
Br15 Pb4 Br3 80.76(4) . . ?
Br16 Pb4 Br3 165.08(4) . . ?
Br18 Pb4 Br3 88.85(4) . . ?
Br17 Pb4 Br3 88.94(4) . . ?
Br15 Pb4 Br1 165.37(4) . 1_655 ?
Br16 Pb4 Br1 81.01(4) . 1_655 ?
Br18 Pb4 Br1 88.06(4) . 1_655 ?
Br17 Pb4 Br1 87.88(4) . 1_655 ?
Br3 Pb4 Br1 113.86(3) . 1_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

N1 C1A C1B C1C 173.8(14) . . . . ?
C1H C1A C1B C1C 63(2) . . . . ?
C1A C1B C1C C1D -73(2) . . . . ?
C1B C1C C1D C1E 105.8(16) . . . . ?
C1C C1D C1E C1F -98.9(15) . . . . ?
C1D C1E C1F C1G 72(2) . . . . ?
C1E C1F C1G C1H -75.6(19) . . . . ?
C1F C1G C1H C1A 101.0(15) . . . . ?
N1 C1A C1H C1G 164.6(12) . . . . ?
C1B C1A C1H C1G -89.9(17) . . . . ?
N2 C2A C2B C2C -166.0(12) . . . . ?
C2H C2A C2B C2C 65.7(19) . . . . ?
C2A C2B C2C C2D -60(2) . . . . ?
C2B C2C C2D C2E -49(2) . . . . ?
C2C C2D C2E C2F 90.9(19) . . . . ?
C2D C2E C2F C2G -43(3) . . . . ?
C2E C2F C2G C2H 43(3) . . . . ?
C2F C2G C2H C2A -87(2) . . . . ?
N2 C2A C2H C2G -89.5(17) . . . . ?
C2B C2A C2H C2G 37(2) . . . . ?
N3 C3A C3B C3C -170.9(10) . . . . ?
C3H C3A C3B C3C 69.4(15) . . . . ?
C3A C3B C3C C3D 42.3(16) . . . . ?
C3B C3C C3D C3E -99.1(15) . . . . ?
C3C C3D C3E C3F 64.4(17) . . . . ?
C3D C3E C3F C3G -63.4(17) . . . . ?
C3E C3F C3G C3H 101.6(14) . . . . ?
N3 C3A C3H C3G 173.3(10) . . . . ?
C3B C3A C3H C3G -66.8(14) . . . . ?
C3F C3G C3H C3A -46.3(15) . . . . ?
N4 C4A C4B C4C -170.1(12) . . . . ?
C4H C4A C4B C4C 69.1(18) . . . . ?
C4A C4B C4C C4D 42.3(18) . . . . ?
C4B C4C C4D C4E -99.3(15) . . . . ?
C4C C4D C4E C4F 66(2) . . . . ?
C4D C4E C4F C4G -66.9(19) . . . . ?
C4E C4F C4G C4H 103.9(15) . . . . ?
N4 C4A C4H C4G 172.4(11) . . . . ?
C4B C4A C4H C4G -67.2(17) . . . . ?
C4F C4G C4H C4A -45.6(17) . . . . ?
C5H C5A C5B C5C 66.8(17) . . . . ?
N5 C5A C5B C5C -172.8(11) . . . . ?
C5A C5B C5C C5D 42.2(18) . . . . ?
C5B C5C C5D C5E -99.0(16) . . . . ?
C5C C5D C5E C5F 64(2) . . . . ?
C5D C5E C5F C5G -65(2) . . . . ?
C5E C5F C5G C5H 99.0(16) . . . . ?
N5 C5A C5H C5G 171.5(11) . . . . ?
C5B C5A C5H C5G -67.7(16) . . . . ?
C5F C5G C5H C5A -40.7(17) . . . . ?
N6 C6A C6B C6C -173.1(10) . . . . ?
C6H C6A C6B C6C 68.4(15) . . . . ?
C6A C6B C6C C6D 45.8(15) . . . . ?
C6B C6C C6D C6E -100.9(13) . . . . ?
C6C C6D C6E C6F 61.9(16) . . . . ?
C6D C6E C6F C6G -63.7(16) . . . . ?
C6E C6F C6G C6H 99.3(13) . . . . ?
N6 C6A C6H C6G 171.2(10) . . . . ?
C6B C6A C6H C6G -69.4(15) . . . . ?
C6F C6G C6H C6A -41.6(15) . . . . ?
N7 C7A C7B C7C 61.6(19) . . . . ?
C7H C7A C7B C7C -65(2) . . . . ?
C7A C7B C7C C7D 64(2) . . . . ?
C7B C7C C7D C7E 44(2) . . . . ?
C7C C7D C7E C7F -101.0(18) . . . . ?
C7D C7E C7F C7G 70(2) . . . . ?
C7E C7F C7G C7H -67(2) . . . . ?
N7 C7A C7H C7G -172.2(12) . . . . ?
C7B C7A C7H C7G -45(2) . . . . ?
C7F C7G C7H C7A 99.1(18) . . . . ?
C8H C8A C8B C8C 64(3) . . . . ?
N8 C8A C8B C8C 173.4(18) . . . . ?
C8A C8B C8C C8D -78(2) . . . . ?
C8B C8C C8D C8E 84(2) . . . . ?
C8C C8D C8E C8F -1(3) . . . . ?
C8D C8E C8F C8G -74(2) . . . . ?
C8E C8F C8G C8H 25(3) . . . . ?
C8B C8A C8H C8G -87(2) . . . . ?
N8 C8A C8H C8G 164.2(13) . . . . ?
C8F C8G C8H C8A 70(3) . . . . ?
N9 C9A C9B C9C 99.4(17) . . . . ?
C9H C9A C9B C9C -37(3) . . . . ?
C9A C9B C9C C9D 99.8(19) . . . . ?
C9B C9C C9D C9E -84(2) . . . . ?
C9C C9D C9E C9F 82.6(18) . . . . ?
C9D C9E C9F C9G -102.0(19) . . . . ?
C9E C9F C9G C9H 39(3) . . . . ?
N9 C9A C9H C9G 164.6(14) . . . . ?
C9B C9A C9H C9G -59(3) . . . . ?
C9F C9G C9H C9A 61(3) . . . . ?
N10 C10A C10B C10C 174.1(16) . . . . ?
C10H C10A C10B C10C 48(3) . . . . ?
C10A C10B C10C C10D 58(3) . . . . ?
C10B C10C C10D C10E -70(3) . . . . ?
C10C C10D C10E C10F -24(3) . . . . ?
C10D C10E C10F C10G 87(3) . . . . ?
C10E C10F C10G C10H -66(3) . . . . ?
N10 C10A C10H C10G 125.7(18) . . . . ?
C10B C10A C10H C10G -107(2) . . . . ?
C10F C10G C10H C10A 68(2) . . . . ?
Pb4 Br3 Pb1 Br2 10.76(9) . . . . ?
Pb4 Br3 Pb1 Br5 98.71(9) . . . . ?
Pb4 Br3 Pb1 Br6 -78.45(9) . . . . ?
Pb4 Br3 Pb1 Br4 -171.39(9) . . . . ?
Pb4 Br1 Pb1 Br2 -9.59(9) 1_455 . . . ?
Pb4 Br1 Pb1 Br5 -97.58(8) 1_455 . . . ?
Pb4 Br1 Pb1 Br6 79.58(8) 1_455 . . . ?
Pb4 Br1 Pb1 Br4 172.52(8) 1_455 . . . ?
Pb2 Br4 Pb1 Br5 -1.08(15) . . . . ?
Pb2 Br4 Pb1 Br3 -87.20(15) . . . . ?
Pb2 Br4 Pb1 Br6 178.85(14) . . . . ?
Pb2 Br4 Pb1 Br1 86.04(15) . . . . ?
Pb1 Br4 Pb2 Br7 -90.71(15) . . . . ?
Pb1 Br4 Pb2 Br9 92.59(15) . . . . ?
Pb1 Br4 Pb2 Br10 -178.96(15) . . . . ?
Pb1 Br4 Pb2 Br11 0.55(14) . . . . ?
Pb3 Br8 Pb2 Br7 -90.52(12) 2_666 . . . ?
Pb3 Br8 Pb2 Br9 85.97(12) 2_666 . . . ?
Pb3 Br8 Pb2 Br10 -2.37(12) 2_666 . . . ?
Pb3 Br8 Pb2 Br11 178.14(11) 2_666 . . . ?
Pb1 Br3 Pb4 Br15 -6.11(9) . . . . ?
Pb1 Br3 Pb4 Br16 -1.8(2) . . . . ?
Pb1 Br3 Pb4 Br18 -99.01(9) . . . . ?
Pb1 Br3 Pb4 Br17 86.40(9) . . . . ?
Pb1 Br3 Pb4 Br1 173.62(8) . . . 1_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br4 0.91 2.82 3.562(11) 140 .
N1 H1A Br9 0.91 3.02 3.649(12) 127.6 .
N1 H1B Br13 0.91 2.48 3.382(11) 174.1 .
N1 H1C Br3 0.91 2.66 3.467(12) 148.9 .
N2 H2A Br1 0.91 2.87 3.476(11) 125.6 .
N2 H2A Br12 0.91 3.13 3.783(11) 129.9 1_455
N2 H2B Br13 0.91 2.55 3.368(11) 150 1_455
N2 H2C Br4 0.91 2.7 3.546(12) 154.2 .
N3 H3A Br14 0.91 2.67 3.432(10) 141.5 .
N3 H3B Br8 0.91 2.79 3.679(10) 167.2 1_655
N3 H3C Br10 0.91 2.61 3.421(11) 148.4 2_666
N4 H4A Br11 0.91 2.71 3.444(12) 138.5 .
N4 H4B Br12 0.91 2.69 3.582(12) 168.4 1_455
N4 H4C Br1 0.91 2.96 3.558(11) 124.8 .
N4 H4C Br5 0.91 3.02 3.780(12) 142.2 .
N5 H5A Br5 0.91 2.95 3.702(11) 140.4 .
N5 H5A Br3 0.91 2.95 3.600(11) 129.8 .
N5 H5B Br12 0.91 2.69 3.591(11) 170.7 .
N5 H5C Br11 0.91 2.66 3.433(10) 143.3 .
N6 H6A Br10 0.91 2.7 3.469(10) 143.2 2_666
N6 H6B Br8 0.91 2.83 3.708(11) 163.6 .
N6 H6C Br14 0.91 2.63 3.418(10) 145.2 .
N7 H7A Br15 0.91 2.7 3.354(13) 129.2 .
N7 H7A Br2 0.91 2.9 3.619(13) 136.5 .
N7 H7B Br18 0.91 2.55 3.445(11) 166.6 .
N7 H7C Br5 0.91 2.73 3.541(11) 148.6 .
N8 H8A Br5 0.91 2.76 3.594(15) 152.4 .
N8 H8B Br18 0.91 2.53 3.431(13) 171.5 1_455
N8 H8C Br16 0.91 2.71 3.346(16) 128.3 1_455
N8 H8C Br2 0.91 2.86 3.553(13) 134.1 .
N9 H9A Br6 0.91 2.55 3.385(12) 152.4 .
N9 H9B Br17 0.91 2.43 3.339(13) 175.5 .
N9 H9C Br15 0.91 2.66 3.341(13) 131.9 .
N10 H10A Br17 0.91 2.66 3.350(13) 133.7 .
N10 H10B Br6 0.91 2.5 3.361(12) 158.3 1_655
N10 H10C Br16 0.91 2.45 3.296(13) 153.8 .
_chemical_name_common            
dekakis(cyclooctylammonium)octadecabromotetraplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2005-03-01 at 18:40:45
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac28l_a smart

data_7
_database_code_depnum_ccdc_archive 'CCDC 708566'

_audit_creation_date             2005-03-01T18:40:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclopropylammonium)tetrachloroplumbate(II)
;
_chemical_formula_sum            'C6 H16 Cl4 N2 Pb'
_chemical_formula_moiety         'Cl4 Pb, 2(C3 H8 N)'
_chemical_formula_weight         465.2

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.187(5)
_cell_length_b                   7.508(3)
_cell_length_c                   8.054(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.141(6)
_cell_angle_gamma                90
_cell_volume                     696.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    966
_cell_measurement_theta_min      3.8125
_cell_measurement_theta_max      28.262

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -3 -3 0.14
-1 3 3 0.14
-1 0 0 0.02
1 0 0 0.02
1 2 -2 0.18
-1 -2 2 0.18

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    12.848
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0782
_exptl_absorpt_correction_T_max  0.5993
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_number            4555
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             1601
_reflns_number_gt                1332
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.1745P] 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_number_reflns         1601
_refine_ls_number_parameters     61
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.682
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.253

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.3192(5) -0.0915(9) -0.3675(7) 0.0266(12) Uani 1 1 d . . .
H1 H 0.32 -0.2202 -0.3992 0.032 Uiso 1 1 calc R . .
C2 C 0.4324(7) 0.0059(8) -0.3190(13) 0.042(2) Uani 1 1 d . . .
H2A H 0.5018 -0.0612 -0.3214 0.051 Uiso 1 1 calc R . .
H2B H 0.431 0.1328 -0.3528 0.051 Uiso 1 1 calc R . .
C3 C 0.3795(8) -0.0431(13) -0.1823(11) 0.049(2) Uani 1 1 d . . .
H3A H 0.4166 -0.1401 -0.0997 0.059 Uiso 1 1 calc R . .
H3B H 0.3458 0.0538 -0.1311 0.059 Uiso 1 1 calc R . .
N1 N 0.2150(6) 0.0100(5) -0.4607(10) 0.0289(15) Uani 1 1 d . . .
H1A H 0.1852 -0.0304 -0.5732 0.043 Uiso 1 1 calc R . .
H1B H 0.2335 0.1273 -0.4617 0.043 Uiso 1 1 calc R . .
H1C H 0.1613 -0.0036 -0.4055 0.043 Uiso 1 1 calc R . .
Cl1 Cl 0.24098(11) 0.0827(2) 0.16075(16) 0.0257(3) Uani 1 1 d . . .
Cl2 Cl -0.04342(12) 0.18682(19) 0.28432(16) 0.0269(3) Uani 1 1 d . . .
Pb1 Pb 0 0 0 0.01607(13) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.460(8) . ?
C1 C3 1.475(10) . ?
C1 C2 1.496(10) . ?
C1 H1 1 . ?
C2 C3 1.492(12) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
Cl1 Pb1 2.8625(16) . ?
Cl2 Pb1 2.8678(15) 2 ?
Cl2 Pb1 2.8786(14) . ?
Pb1 Cl1 2.8625(16) 3 ?
Pb1 Cl2 2.8678(15) 4_565 ?
Pb1 Cl2 2.8678(15) 2_545 ?
Pb1 Cl2 2.8786(14) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C3 116.9(6) . . ?
N1 C1 C2 116.8(5) . . ?
C3 C1 C2 60.3(6) . . ?
N1 C1 H1 116.9 . . ?
C3 C1 H1 116.9 . . ?
C2 C1 H1 116.9 . . ?
C3 C2 C1 59.2(5) . . ?
C3 C2 H2A 117.9 . . ?
C1 C2 H2A 117.9 . . ?
C3 C2 H2B 117.9 . . ?
C1 C2 H2B 117.9 . . ?
H2A C2 H2B 115 . . ?
C1 C3 C2 60.5(5) . . ?
C1 C3 H3A 117.7 . . ?
C2 C3 H3A 117.7 . . ?
C1 C3 H3B 117.7 . . ?
C2 C3 H3B 117.7 . . ?
H3A C3 H3B 114.8 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Cl2 Pb1 146.71(5) 2 . ?
Cl1 Pb1 Cl1 180 3 . ?
Cl1 Pb1 Cl2 86.89(4) 3 4_565 ?
Cl1 Pb1 Cl2 93.11(4) . 4_565 ?
Cl1 Pb1 Cl2 93.11(4) 3 2_545 ?
Cl1 Pb1 Cl2 86.89(4) . 2_545 ?
Cl2 Pb1 Cl2 180.00(3) 4_565 2_545 ?
Cl1 Pb1 Cl2 87.90(4) 3 3 ?
Cl1 Pb1 Cl2 92.10(4) . 3 ?
Cl2 Pb1 Cl2 87.89(3) 4_565 3 ?
Cl2 Pb1 Cl2 92.11(3) 2_545 3 ?
Cl1 Pb1 Cl2 92.10(4) 3 . ?
Cl1 Pb1 Cl2 87.90(4) . . ?
Cl2 Pb1 Cl2 92.11(3) 4_565 . ?
Cl2 Pb1 Cl2 87.89(3) 2_545 . ?
Cl2 Pb1 Cl2 180.00(5) 3 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 107.2(7) . . . . ?
N1 C1 C3 C2 -107.0(6) . . . . ?
Pb1 Cl2 Pb1 Cl1 -133.77(10) 2 . . 3 ?
Pb1 Cl2 Pb1 Cl1 46.23(10) 2 . . . ?
Pb1 Cl2 Pb1 Cl2 -46.81(12) 2 . . 4_565 ?
Pb1 Cl2 Pb1 Cl2 133.19(12) 2 . . 2_545 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl1 0.91 2.59 3.214(8) 125.9 1_554
N1 H1B Cl1 0.91 2.38 3.194(5) 149.1 4_565
N1 H1C Cl2 0.91 2.41 3.244(7) 151.7 3
_chemical_name_common            
bis(cyclopropylammonium)tetrachloroplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2005-03-01 at 17:55:12
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 5ac29l_a smart

data_8
_database_code_depnum_ccdc_archive 'CCDC 708567'

_audit_creation_date             2005-03-01T17:55:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclobutylammonium)tetrachloroplumbate(II)
;
_chemical_formula_moiety         'Cl4 Pb, 2(C4 H10 N)'
_chemical_formula_sum            'C8 H20 Cl4 N2 Pb'
_chemical_formula_weight         493.25

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.219(5)
_cell_length_b                   7.618(3)
_cell_length_c                   8.093(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.828(7)
_cell_angle_gamma                90
_cell_volume                     780.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    791
_cell_measurement_theta_min      3.2185
_cell_measurement_theta_max      28.284

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    2.1
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             464
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.015
-1 0 0 0.015
3 1 -2 0.065
-5 -3 3 0.075
1 -1 -1 0.115
-1 1 1 0.12

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    11.474
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_absorpt_correction_T_min  0.1263
_exptl_absorpt_correction_T_max  0.7112
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_number            4843
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_full        27.99
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             1885
_reflns_number_gt                1726
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.

;
_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)+(0.0000P)²+54.0170P] 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_number_reflns         1885
_refine_ls_number_parameters     70
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.1942
_refine_ls_wR_factor_gt          0.1927
_refine_ls_goodness_of_fit_ref   1.491
_refine_ls_restrained_S_all      1.478
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.124
_refine_diff_density_min         -5.934
_refine_diff_density_rms         0.372

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
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'

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 0.2901(17) 0.579(4) 0.118(3) 0.051(5) Uani 1 1 d DU . .
H1 H 0.2768 0.7076 0.0977 0.061 Uiso 1 1 calc R . .
C2 C 0.3440(16) 0.542(4) 0.307(3) 0.065(6) Uani 1 1 d DU . .
H2A H 0.3322 0.4214 0.3446 0.078 Uiso 1 1 calc R . .
H2B H 0.331 0.6312 0.3874 0.078 Uiso 1 1 calc R . .
C3 C 0.447(2) 0.565(5) 0.263(3) 0.071(6) Uani 1 1 d DU . .
H3A H 0.4761 0.6857 0.2817 0.086 Uiso 1 1 calc R . .
H3B H 0.5021 0.4775 0.318 0.086 Uiso 1 1 calc R . .
C4 C 0.3902(14) 0.524(4) 0.075(3) 0.053(5) Uani 1 1 d DU . .
H4A H 0.4098 0.6018 -0.0095 0.064 Uiso 1 1 calc R . .
H4B H 0.3921 0.3991 0.0429 0.064 Uiso 1 1 calc R . .
N1 N 0.1909(13) 0.474(2) 0.032(2) 0.030(3) Uani 1 1 d U . .
H1A H 0.1359 0.5157 0.066 0.045 Uiso 1 1 calc R . .
H1B H 0.202 0.3588 0.0625 0.045 Uiso 1 1 calc R . .
H1C H 0.1758 0.4834 -0.0851 0.045 Uiso 1 1 calc R . .
Cl1 Cl 0.2190(3) 1.0722(6) 0.1494(6) 0.0230(8) Uani 1 1 d . . .
Cl2 Cl -0.0392(3) 1.1915(6) 0.2840(5) 0.0213(8) Uani 1 1 d . . .
Pb1 Pb 0 1 0 0.0151(2) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.521(19) . ?
C1 C2 1.521(19) . ?
C1 N1 1.52(3) . ?
C1 H1 1 . ?
C2 C3 1.523(19) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 C4 1.522(19) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
Cl1 Pb1 2.849(4) . ?
Cl2 Pb1 2.885(4) 2 ?
Cl2 Pb1 2.893(4) . ?
Pb1 Cl1 2.849(4) 3_575 ?
Pb1 Cl2 2.885(4) 2_545 ?
Pb1 Cl2 2.885(4) 4_585 ?
Pb1 Cl2 2.893(4) 3_575 ?

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
C4 C1 C2 89.7(15) . . ?
C4 C1 N1 116.2(18) . . ?
C2 C1 N1 116.9(19) . . ?
C4 C1 H1 110.8 . . ?
C2 C1 H1 110.8 . . ?
N1 C1 H1 110.8 . . ?
C1 C2 C3 85.9(16) . . ?
C1 C2 H2A 114.3 . . ?
C3 C2 H2A 114.3 . . ?
C1 C2 H2B 114.3 . . ?
C3 C2 H2B 114.3 . . ?
H2A C2 H2B 111.5 . . ?
C4 C3 C2 89.6(15) . . ?
C4 C3 H3A 113.7 . . ?
C2 C3 H3A 113.7 . . ?
C4 C3 H3B 113.7 . . ?
C2 C3 H3B 113.7 . . ?
H3A C3 H3B 111 . . ?
C1 C4 C3 85.9(16) . . ?
C1 C4 H4A 114.3 . . ?
C3 C4 H4A 114.3 . . ?
C1 C4 H4B 114.3 . . ?
C3 C4 H4B 114.3 . . ?
H4A C4 H4B 111.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Cl2 Pb1 148.22(16) 2 . ?
Cl1 Pb1 Cl1 180 3_575 . ?
Cl1 Pb1 Cl2 94.71(13) 3_575 2_545 ?
Cl1 Pb1 Cl2 85.29(13) . 2_545 ?
Cl1 Pb1 Cl2 85.29(13) 3_575 4_585 ?
Cl1 Pb1 Cl2 94.71(13) . 4_585 ?
Cl2 Pb1 Cl2 180.00(10) 2_545 4_585 ?
Cl1 Pb1 Cl2 92.34(12) 3_575 . ?
Cl1 Pb1 Cl2 87.66(12) . . ?
Cl2 Pb1 Cl2 88.37(5) 2_545 . ?
Cl2 Pb1 Cl2 91.63(5) 4_585 . ?
Cl1 Pb1 Cl2 87.66(12) 3_575 3_575 ?
Cl1 Pb1 Cl2 92.34(12) . 3_575 ?
Cl2 Pb1 Cl2 91.63(5) 2_545 3_575 ?
Cl2 Pb1 Cl2 88.37(5) 4_585 3_575 ?
Cl2 Pb1 Cl2 180.00(9) . 3_575 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C1 C2 C3 22(2) . . . . ?
N1 C1 C2 C3 142(2) . . . . ?
C1 C2 C3 C4 -22(2) . . . . ?
C2 C1 C4 C3 -22(2) . . . . ?
N1 C1 C4 C3 -142(2) . . . . ?
C2 C3 C4 C1 22(2) . . . . ?
Pb1 Cl2 Pb1 Cl1 -133.5(3) 2 . . 3_575 ?
Pb1 Cl2 Pb1 Cl1 46.5(3) 2 . . . ?
Pb1 Cl2 Pb1 Cl2 131.9(4) 2 . . 2_545 ?
Pb1 Cl2 Pb1 Cl2 -48.1(4) 2 . . 4_585 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl2 0.91 2.41 3.277(18) 159.8 2_545
N1 H1B Cl1 0.91 2.29 3.193(17) 175.5 1_545
N1 H1C Cl1 0.91 2.41 3.239(18) 150.6 4_575
_chemical_name_common            
bis(cyclobutylammonium)tetrachloroplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2005-11-13 at 16:34:19
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 5ac43_a apex

data_9
_database_code_depnum_ccdc_archive 'CCDC 708568'

_audit_creation_date             2005-11-13T16:34:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclopentylammonium)tetrachloroplumbate(II)
;
_chemical_formula_sum            'C10 H24 Cl4 N2 Pb'
_chemical_formula_moiety         'Cl4 Pb, C10 H24 N2'
_chemical_formula_weight         521.3

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmca
_symmetry_space_group_name_Hall  '-C 2bc 2'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x-1/2, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z-1/2'

_cell_length_a                   25.8420(10)
_cell_length_b                   8.5174(3)
_cell_length_c                   7.6956(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1693.85(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2939
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      28.19

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 0 0.015
2 0 0 0.015
1 -1 -1 0.105
0 -2 0 0.15
1 3 1 0.08
3 1 1 0.1
2 4 -3 0.21

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    10.575
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0642
_exptl_absorpt_correction_T_max  0.7182
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_number            5933
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             1051
_reflns_number_gt                817
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.

;
_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)+(0.0639P)²+30.5208P] 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_number_reflns         1051
_refine_ls_number_parameters     59
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         4.747
_refine_diff_density_min         -2.927
_refine_diff_density_rms         0.258

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
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'

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 0.1325(3) 0.4510(10) -0.0405(11) 0.028(2) Uani 0.5 1 d PGU . .
H1 H 0.1271 0.4042 -0.1554 0.033 Uiso 0.5 1 calc PR . .
C2 C 0.1327(4) 0.6290(11) -0.0578(19) 0.040(3) Uani 0.5 1 d PGU . .
H2A H 0.1124 0.6605 -0.158 0.047 Uiso 0.5 1 calc PR . .
H2B H 0.1176 0.6765 0.045 0.047 Uiso 0.5 1 calc PR . .
C3 C 0.1884(4) 0.6820(13) -0.079(2) 0.068(5) Uani 0.5 1 d PGU . .
H3A H 0.1978 0.6877 -0.2009 0.081 Uiso 0.5 1 calc PR . .
H3B H 0.1938 0.784 -0.0261 0.081 Uiso 0.5 1 calc PR . .
C4 C 0.2193(3) 0.5565(18) 0.014(2) 0.074(5) Uani 0.5 1 d PGU . .
H4A H 0.2511 0.5353 -0.0494 0.089 Uiso 0.5 1 calc PR . .
H4B H 0.2283 0.5915 0.1298 0.089 Uiso 0.5 1 calc PR . .
C5 C 0.1865(3) 0.4096(14) 0.023(2) 0.055(4) Uani 0.5 1 d PGU . .
H5A H 0.185 0.3715 0.1416 0.067 Uiso 0.5 1 calc PR . .
H5B H 0.2013 0.328 -0.0495 0.067 Uiso 0.5 1 calc PR . .
N1 N 0.0927(4) 0.3939(13) 0.0775(15) 0.033(3) Uani 0.5 1 d PGU . .
H1A H 0.0617 0.4211 0.0374 0.05 Uiso 0.5 1 calc PR . .
H1B H 0.0974 0.436 0.1822 0.05 Uiso 0.5 1 calc PR . .
H1C H 0.0947 0.2898 0.0851 0.05 Uiso 0.5 1 calc PR . .
Cl1 Cl 0.10935(17) 0 0 0.102(3) Uani 1 2 d S . .
Cl2 Cl 0 0.1981(4) 0.3104(4) 0.0365(6) Uani 1 2 d S . .
Pb1 Pb 0 0 0 0.0215(2) Uani 1 4 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.4554 . ?
C1 C5 1.5201 . ?
C1 C2 1.5218 . ?
C1 H1 0.98 . ?
C2 C3 1.5173 . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 C4 1.5139 . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 C5 1.5134 . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
N1 H1A 0.89 . ?
N1 H1B 0.89 . ?
N1 H1C 0.89 . ?
Cl1 Pb1 2.826(4) . ?
Cl2 Pb1 2.925(3) . ?
Cl2 Pb1 2.957(3) 2 ?
Pb1 Cl1 2.826(4) 9 ?
Pb1 Cl2 2.925(3) 9 ?
Pb1 Cl2 2.957(3) 2_554 ?
Pb1 Cl2 2.957(3) 10_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C5 111.8 . . ?
N1 C1 C2 112.9 . . ?
C5 C1 C2 104.8 . . ?
N1 C1 H1 109.1 . . ?
C5 C1 H1 109.1 . . ?
C2 C1 H1 109.1 . . ?
C3 C2 C1 108 . . ?
C3 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
C3 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C4 C3 C2 103.9 . . ?
C4 C3 H3A 111 . . ?
C2 C3 H3A 111 . . ?
C4 C3 H3B 111 . . ?
C2 C3 H3B 111 . . ?
H3A C3 H3B 109 . . ?
C5 C4 C3 108 . . ?
C5 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C5 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
C4 C5 C1 107.9 . . ?
C4 C5 H5A 110.1 . . ?
C1 C5 H5A 110.1 . . ?
C4 C5 H5B 110.1 . . ?
C1 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pb1 Cl2 Pb1 154.80(12) . 2 ?
Cl1 Pb1 Cl1 180 . 9 ?
Cl1 Pb1 Cl2 90 . 9 ?
Cl1 Pb1 Cl2 90 9 9 ?
Cl1 Pb1 Cl2 90 . . ?
Cl1 Pb1 Cl2 90 9 . ?
Cl2 Pb1 Cl2 180.00(7) 9 . ?
Cl1 Pb1 Cl2 90 . 2_554 ?
Cl1 Pb1 Cl2 90 9 2_554 ?
Cl2 Pb1 Cl2 95.66(2) 9 2_554 ?
Cl2 Pb1 Cl2 84.34(2) . 2_554 ?
Cl1 Pb1 Cl2 90 . 10_556 ?
Cl1 Pb1 Cl2 90 9 10_556 ?
Cl2 Pb1 Cl2 84.34(2) 9 10_556 ?
Cl2 Pb1 Cl2 95.66(2) . 10_556 ?
Cl2 Pb1 Cl2 180.00(6) 2_554 10_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

N1 C1 C2 C3 144.9 . . . . ?
C5 C1 C2 C3 23 . . . . ?
C1 C2 C3 C4 -27.7 . . . . ?
C2 C3 C4 C5 21.7 . . . . ?
C3 C4 C5 C1 -8 . . . . ?
N1 C1 C5 C4 -131.7 . . . . ?
C2 C1 C5 C4 -9 . . . . ?
Pb1 Cl2 Pb1 Cl1 90 2 . . . ?
Pb1 Cl2 Pb1 Cl1 -90 2 . . 9 ?
Pb1 Cl2 Pb1 Cl2 0 2 . . 2_554 ?
Pb1 Cl2 Pb1 Cl2 180 2 . . 10_556 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl2 0.89 2.57 3.252(11) 133.7 2_554
N1 H1B Cl1 0.89 2.52 3.402(12) 168.7 10_566
N1 H1C Cl1 0.89 2.58 3.435(12) 160.8 .
_chemical_name_common            
bis(cyclopentylammonium)tetrachloroplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2005-09-05 at 06:17:50
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 5ac42a_a smart

data_10
_database_code_depnum_ccdc_archive 'CCDC 708569'

_audit_creation_date             2005-09-05T06:17:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
bis(cyclohexylammonium)tetrachloroplumbate(II)
;
_chemical_formula_sum            'C24 H56 Cl8 N4 Pb2'
_chemical_formula_moiety         'Cl8 Pb2, 4(C6 H14 N)'
_chemical_formula_weight         1098.71

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/m
_symmetry_space_group_name_Hall  '-P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   11.4446(11)
_cell_length_b                   28.306(3)
_cell_length_c                   11.5206(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.031(6)
_cell_angle_gamma                90
_cell_volume                     3732.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    975
_cell_measurement_theta_min      2.8785
_cell_measurement_theta_max      28.2275

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.08
0 1 0 0.08
-4 -1 -5 0.11
3 1 3 0.11
1 0 -1 0.12
-3 -2 3 0.12

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    9.605
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.1598
_exptl_absorpt_correction_T_max  0.2797
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_number            23552
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         0.72
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             6980
_reflns_number_gt                6348
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection       'Bruker SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+ (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.
The twin law applied, as suggested by PLATON, is
[1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00]
and the batch scale factor is 0.73.

;
_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)+(0.0223P)²+17.2800P] 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_number_reflns         6980
_refine_ls_number_parameters     362
_refine_ls_number_restraints     303
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.032
_refine_ls_wR_factor_ref         0.0767
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.13
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.966
_refine_diff_density_rms         0.218

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
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'

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 0.3327(7) 0.8798(3) 0.6904(6) 0.0204(15) Uani 1 1 d DU . .
H1 H 0.3712 0.8771 0.7681 0.025 Uiso 1 1 calc R . .
C2 C 0.4268(7) 0.8810(3) 0.5962(7) 0.0228(16) Uani 1 1 d DU . .
H2D H 0.478 0.853 0.6039 0.027 Uiso 1 1 calc R . .
H2E H 0.3895 0.88 0.5187 0.027 Uiso 1 1 calc R . .
C3 C 0.4992(6) 0.9256(3) 0.6073(7) 0.0253(16) Uani 1 1 d DU . .
H3D H 0.5556 0.9269 0.5422 0.03 Uiso 1 1 calc R . .
H3E H 0.5446 0.9241 0.6804 0.03 Uiso 1 1 calc R . .
C4 C 0.4269(7) 0.9709(3) 0.6071(7) 0.0248(16) Uani 1 1 d DU . .
H4D H 0.3893 0.975 0.5304 0.03 Uiso 1 1 calc R . .
H4E H 0.4785 0.9984 0.6211 0.03 Uiso 1 1 calc R . .
C5 C 0.3336(7) 0.9685(3) 0.7014(7) 0.0265(16) Uani 1 1 d DU . .
H5A H 0.2838 0.997 0.697 0.032 Uiso 1 1 calc R . .
H5B H 0.3718 0.9681 0.7786 0.032 Uiso 1 1 calc R . .
C6 C 0.2572(6) 0.9244(2) 0.6885(7) 0.0234(16) Uani 1 1 d DU . .
H6A H 0.1998 0.9232 0.7527 0.028 Uiso 1 1 calc R . .
H6B H 0.2135 0.926 0.6144 0.028 Uiso 1 1 calc R . .
C7 C 0.3154(6) 0.8786(3) 0.1829(6) 0.0181(15) Uani 1 1 d DU . .
H7 H 0.2339 0.8778 0.1515 0.022 Uiso 1 1 calc R . .
C8 C 0.3280(7) 0.9218(3) 0.2602(6) 0.0214(14) Uani 1 1 d DU . .
H8A H 0.4051 0.9211 0.2993 0.026 Uiso 1 1 calc R . .
H8B H 0.2667 0.9212 0.3209 0.026 Uiso 1 1 calc R . .
C9 C 0.3169(7) 0.9670(3) 0.1885(7) 0.0246(16) Uani 1 1 d DU . .
H9A H 0.2367 0.9693 0.1567 0.03 Uiso 1 1 calc R . .
H9B H 0.3304 0.9947 0.2391 0.03 Uiso 1 1 calc R . .
C10 C 0.4048(7) 0.9675(3) 0.0889(7) 0.0280(17) Uani 1 1 d DU . .
H10A H 0.3935 0.9965 0.042 0.034 Uiso 1 1 calc R . .
H10B H 0.4851 0.9681 0.1208 0.034 Uiso 1 1 calc R . .
C11 C 0.3895(8) 0.9245(3) 0.0128(6) 0.0273(16) Uani 1 1 d DU . .
H11A H 0.4491 0.9251 -0.0495 0.033 Uiso 1 1 calc R . .
H11B H 0.3116 0.9257 -0.0245 0.033 Uiso 1 1 calc R . .
C12 C 0.4009(7) 0.8786(3) 0.0809(6) 0.0246(16) Uani 1 1 d DU . .
H12A H 0.4818 0.8753 0.1102 0.03 Uiso 1 1 calc R . .
H12B H 0.384 0.8514 0.0294 0.03 Uiso 1 1 calc R . .
C13 C 0.8938(7) 0.8779(3) 0.6579(6) 0.0188(15) Uani 1 1 d DU . .
H13 H 0.9761 0.8746 0.63 0.023 Uiso 1 1 calc R . .
C14 C 0.8147(7) 0.8760(3) 0.5528(6) 0.0215(16) Uani 1 1 d DU . .
H14A H 0.7321 0.8757 0.5782 0.026 Uiso 1 1 calc R . .
H14B H 0.8299 0.8467 0.5087 0.026 Uiso 1 1 calc R . .
C15 C 0.8359(8) 0.9187(3) 0.4749(6) 0.0257(16) Uani 1 1 d DU . .
H15A H 0.7781 0.9187 0.411 0.031 Uiso 1 1 calc R . .
H15B H 0.9148 0.9163 0.4401 0.031 Uiso 1 1 calc R . .
C16 C 0.8263(7) 0.9653(3) 0.5423(7) 0.0256(17) Uani 1 1 d DU . .
H16A H 0.8456 0.9919 0.49 0.031 Uiso 1 1 calc R . .
H16B H 0.7448 0.9695 0.5691 0.031 Uiso 1 1 calc R . .
C17 C 0.9075(7) 0.9662(3) 0.6458(7) 0.0256(17) Uani 1 1 d DU . .
H17A H 0.8953 0.9957 0.6901 0.031 Uiso 1 1 calc R . .
H17B H 0.9896 0.9656 0.6187 0.031 Uiso 1 1 calc R . .
C18 C 0.8853(7) 0.9240(3) 0.7243(6) 0.0211(15) Uani 1 1 d DU . .
H18A H 0.9432 0.924 0.7882 0.025 Uiso 1 1 calc R . .
H18B H 0.8065 0.9268 0.7591 0.025 Uiso 1 1 calc R . .
C19 C 0.8217(7) 0.8753(3) 0.0887(7) 0.0203(15) Uani 1 1 d DU . .
H19 H 0.856 0.8714 0.0094 0.024 Uiso 1 1 calc R . .
C20 C 0.7515(6) 0.9210(3) 0.0902(7) 0.0215(15) Uani 1 1 d DU . .
H20A H 0.6903 0.9198 0.0295 0.026 Uiso 1 1 calc R . .
H20B H 0.7125 0.9246 0.1664 0.026 Uiso 1 1 calc R . .
C21 C 0.8308(8) 0.9629(3) 0.0687(7) 0.0283(17) Uani 1 1 d DU . .
H21A H 0.7847 0.9925 0.0736 0.034 Uiso 1 1 calc R . .
H21B H 0.8639 0.9608 -0.0104 0.034 Uiso 1 1 calc R . .
C22 C 0.9308(8) 0.9647(3) 0.1579(7) 0.0263(17) Uani 1 1 d DU . .
H22A H 0.9843 0.991 0.1383 0.032 Uiso 1 1 calc R . .
H22B H 0.8981 0.9708 0.236 0.032 Uiso 1 1 calc R . .
C23 C 0.9986(7) 0.9188(3) 0.1597(8) 0.0279(17) Uani 1 1 d DU . .
H23A H 1.0569 0.9201 0.2231 0.033 Uiso 1 1 calc R . .
H23B H 1.0417 0.9156 0.0856 0.033 Uiso 1 1 calc R . .
C24 C 0.9219(7) 0.8752(3) 0.1768(7) 0.0241(16) Uani 1 1 d DU . .
H24A H 0.8896 0.8751 0.2565 0.029 Uiso 1 1 calc R . .
H24B H 0.9695 0.8462 0.1667 0.029 Uiso 1 1 calc R . .
N1 N 0.2547(6) 0.8378(3) 0.6724(6) 0.0218(14) Uani 1 1 d U . .
H1A H 0.2984 0.811 0.6737 0.033 Uiso 1 1 calc R . .
H1B H 0.2181 0.8404 0.6026 0.033 Uiso 1 1 calc R . .
H1C H 0.2005 0.8367 0.73 0.033 Uiso 1 1 calc R . .
N2 N 0.3348(6) 0.8355(2) 0.2547(5) 0.0213(13) Uani 1 1 d U . .
H2A H 0.3277 0.8093 0.2093 0.032 Uiso 1 1 calc R . .
H2B H 0.2808 0.8344 0.3126 0.032 Uiso 1 1 calc R . .
H2C H 0.4078 0.8364 0.2861 0.032 Uiso 1 1 calc R . .
N3 N 0.8685(6) 0.8368(2) 0.7359(6) 0.0218(14) Uani 1 1 d U . .
H3A H 0.8746 0.8094 0.6948 0.033 Uiso 1 1 calc R . .
H3B H 0.7948 0.8395 0.7648 0.033 Uiso 1 1 calc R . .
H3C H 0.9207 0.8364 0.7955 0.033 Uiso 1 1 calc R . .
N4 N 0.7424(6) 0.8349(2) 0.1104(6) 0.0210(14) Uani 1 1 d U . .
H4A H 0.6832 0.8352 0.0575 0.032 Uiso 1 1 calc R . .
H4B H 0.7122 0.8372 0.1832 0.032 Uiso 1 1 calc R . .
H4C H 0.783 0.8074 0.1038 0.032 Uiso 1 1 calc R . .
Cl1 Cl -0.1438(2) 0.75 -0.0537(2) 0.0214(6) Uani 1 2 d S . .
Cl2 Cl 0.1578(3) 0.75 0.1678(2) 0.0254(6) Uani 1 2 d S . .
Cl3 Cl 0.3522(3) 0.75 -0.1723(3) 0.0281(7) Uani 1 2 d S . .
Cl4 Cl 0.6758(3) 0.75 -0.3567(2) 0.0292(7) Uani 1 2 d S . .
Cl5 Cl -0.1709(3) 0.75 0.3133(3) 0.0289(7) Uani 1 2 d S . .
Cl6 Cl -0.4625(3) 0.75 0.1440(2) 0.0249(6) Uani 1 2 d S . .
Cl7 Cl 0.0490(2) 0.75 -0.3338(2) 0.0200(6) Uani 1 2 d S . .
Cl8 Cl 0.3247(2) 0.75 0.4579(2) 0.0227(6) Uani 1 2 d S . .
Cl9 Cl 0.11691(18) 0.84974(7) 0.42953(17) 0.0253(4) Uani 1 1 d . . .
Cl10 Cl 0.09500(17) 0.84911(7) -0.09755(16) 0.0230(4) Uani 1 1 d . . .
Cl11 Cl 0.61660(18) 0.84977(7) -0.13969(17) 0.0217(4) Uani 1 1 d . . .
Cl12 Cl -0.40224(18) 0.84955(8) 0.34727(16) 0.0254(4) Uani 1 1 d . . .
Pb1 Pb 0.10429(3) 0.75 -0.07266(3) 0.01542(10) Uani 1 2 d S . .
Pb2 Pb -0.39596(4) 0.75 0.38357(3) 0.01834(10) Uani 1 2 d S . .
Pb3 Pb 0.08471(3) 0.75 0.41546(3) 0.01618(10) Uani 1 2 d S . .
Pb4 Pb 0.59143(4) 0.75 -0.13257(3) 0.01680(10) Uani 1 2 d S . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.500(10) . ?
C1 C6 1.529(7) . ?
C1 C2 1.530(9) . ?
C1 H1 1 . ?
C2 C3 1.516(9) . ?
C2 H2D 0.99 . ?
C2 H2E 0.99 . ?
C3 C4 1.525(9) . ?
C3 H3D 0.99 . ?
C3 H3E 0.99 . ?
C4 C5 1.526(7) . ?
C4 H4D 0.99 . ?
C4 H4E 0.99 . ?
C5 C6 1.532(7) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 N2 1.492(10) . ?
C7 C8 1.519(9) . ?
C7 C12 1.529(9) . ?
C7 H7 1 . ?
C8 C9 1.529(9) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 C10 1.526(10) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C10 C11 1.512(10) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 C12 1.523(9) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C13 N3 1.500(10) . ?
C13 C14 1.512(9) . ?
C13 C18 1.516(9) . ?
C13 H13 1 . ?
C14 C15 1.525(9) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.533(10) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.513(9) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 C18 1.519(9) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 N4 1.482(10) . ?
C19 C20 1.524(9) . ?
C19 C24 1.531(9) . ?
C19 H19 1 . ?
C20 C21 1.515(10) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.538(9) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 C23 1.513(10) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 C24 1.529(10) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
N2 H2A 0.91 . ?
N2 H2B 0.91 . ?
N2 H2C 0.91 . ?
N3 H3A 0.91 . ?
N3 H3B 0.91 . ?
N3 H3C 0.91 . ?
N4 H4A 0.91 . ?
N4 H4B 0.91 . ?
N4 H4C 0.91 . ?
Cl1 Pb1 2.848(3) . ?
Cl1 Pb4 3.163(3) 1_455 ?
Cl2 Pb1 2.836(3) . ?
Cl2 Pb3 2.974(3) . ?
Cl3 Pb4 2.776(3) . ?
Cl3 Pb1 3.061(3) . ?
Cl4 Pb4 2.758(3) . ?
Cl4 Pb2 3.102(3) 1_654 ?
Cl5 Pb2 2.700(3) . ?
Cl5 Pb3 3.153(3) . ?
Cl6 Pb2 2.863(3) . ?
Cl6 Pb4 3.246(3) 1_455 ?
Cl7 Pb3 2.917(3) 1_554 ?
Cl7 Pb1 3.074(3) . ?
Cl8 Pb3 2.789(3) . ?
Cl8 Pb2 3.310(3) 1_655 ?
Cl9 Pb3 2.852(2) . ?
Cl10 Pb1 2.822(2) . ?
Cl11 Pb4 2.840(2) . ?
Cl12 Pb2 2.850(2) . ?
Pb1 Cl10 2.822(2) 4_575 ?
Pb2 Cl12 2.850(2) 4_575 ?
Pb2 Cl4 3.102(3) 1_456 ?
Pb2 Cl8 3.310(3) 1_455 ?
Pb3 Cl9 2.852(2) 4_575 ?
Pb3 Cl7 2.917(3) 1_556 ?
Pb4 Cl11 2.840(2) 4_575 ?
Pb4 Cl1 3.163(3) 1_655 ?
Pb4 Cl6 3.246(3) 1_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C6 108.4(6) . . ?
N1 C1 C2 109.8(6) . . ?
C6 C1 C2 111.7(6) . . ?
N1 C1 H1 109 . . ?
C6 C1 H1 109 . . ?
C2 C1 H1 109 . . ?
C3 C2 C1 110.1(6) . . ?
C3 C2 H2D 109.6 . . ?
C1 C2 H2D 109.6 . . ?
C3 C2 H2E 109.6 . . ?
C1 C2 H2E 109.6 . . ?
H2D C2 H2E 108.1 . . ?
C2 C3 C4 113.7(6) . . ?
C2 C3 H3D 108.8 . . ?
C4 C3 H3D 108.8 . . ?
C2 C3 H3E 108.8 . . ?
C4 C3 H3E 108.8 . . ?
H3D C3 H3E 107.7 . . ?
C3 C4 C5 110.0(6) . . ?
C3 C4 H4D 109.7 . . ?
C5 C4 H4D 109.7 . . ?
C3 C4 H4E 109.7 . . ?
C5 C4 H4E 109.7 . . ?
H4D C4 H4E 108.2 . . ?
C4 C5 C6 111.5(6) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108 . . ?
C1 C6 C5 110.4(6) . . ?
C1 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C1 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 C8 108.5(6) . . ?
N2 C7 C12 109.3(6) . . ?
C8 C7 C12 113.0(6) . . ?
N2 C7 H7 108.6 . . ?
C8 C7 H7 108.6 . . ?
C12 C7 H7 108.6 . . ?
C7 C8 C9 110.3(6) . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 111.2(7) . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108 . . ?
C11 C10 C9 110.6(7) . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C10 C11 C12 112.2(6) . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C7 109.9(6) . . ?
C11 C12 H12A 109.7 . . ?
C7 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C7 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N3 C13 C14 109.7(6) . . ?
N3 C13 C18 110.7(6) . . ?
C14 C13 C18 113.3(6) . . ?
N3 C13 H13 107.6 . . ?
C14 C13 H13 107.6 . . ?
C18 C13 H13 107.6 . . ?
C13 C14 C15 110.4(6) . . ?
C13 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15 C16 111.8(6) . . ?
C14 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 111.7(6) . . ?
C17 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 C18 110.7(6) . . ?
C16 C17 H17A 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C13 C18 C17 111.4(6) . . ?
C13 C18 H18A 109.3 . . ?
C17 C18 H18A 109.3 . . ?
C13 C18 H18B 109.3 . . ?
C17 C18 H18B 109.3 . . ?
H18A C18 H18B 108 . . ?
N4 C19 C20 109.3(6) . . ?
N4 C19 C24 110.2(6) . . ?
C20 C19 C24 112.9(6) . . ?
N4 C19 H19 108.1 . . ?
C20 C19 H19 108.1 . . ?
C24 C19 H19 108.1 . . ?
C21 C20 C19 110.3(6) . . ?
C21 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C20 C21 C22 111.2(6) . . ?
C20 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108 . . ?
C23 C22 C21 111.3(6) . . ?
C23 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108 . . ?
C22 C23 C24 113.6(7) . . ?
C22 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 C19 110.0(6) . . ?
C23 C24 H24A 109.7 . . ?
C19 C24 H24A 109.7 . . ?
C23 C24 H24B 109.7 . . ?
C19 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C7 N2 H2A 109.5 . . ?
C7 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C7 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C13 N3 H3A 109.5 . . ?
C13 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C13 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C19 N4 H4A 109.5 . . ?
C19 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C19 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
Pb1 Cl1 Pb4 158.90(10) . 1_455 ?
Pb1 Cl2 Pb3 151.19(12) . . ?
Pb4 Cl3 Pb1 148.50(12) . . ?
Pb4 Cl4 Pb2 144.16(13) . 1_654 ?
Pb2 Cl5 Pb3 140.64(11) . . ?
Pb2 Cl6 Pb4 153.63(11) . 1_455 ?
Pb3 Cl7 Pb1 160.06(10) 1_554 . ?
Pb3 Cl8 Pb2 154.91(10) . 1_655 ?
Cl10 Pb1 Cl10 167.56(8) . 4_575 ?
Cl10 Pb1 Cl2 96.16(4) . . ?
Cl10 Pb1 Cl2 96.16(4) 4_575 . ?
Cl10 Pb1 Cl1 88.30(4) . . ?
Cl10 Pb1 Cl1 88.30(4) 4_575 . ?
Cl2 Pb1 Cl1 98.04(9) . . ?
Cl10 Pb1 Cl3 89.82(4) . . ?
Cl10 Pb1 Cl3 89.82(4) 4_575 . ?
Cl2 Pb1 Cl3 99.57(8) . . ?
Cl1 Pb1 Cl3 162.39(8) . . ?
Cl10 Pb1 Cl7 83.85(4) . . ?
Cl10 Pb1 Cl7 83.85(4) 4_575 . ?
Cl2 Pb1 Cl7 179.41(9) . . ?
Cl1 Pb1 Cl7 82.55(7) . . ?
Cl3 Pb1 Cl7 79.84(8) . . ?
Cl5 Pb2 Cl12 88.85(4) . . ?
Cl5 Pb2 Cl12 88.85(4) . 4_575 ?
Cl12 Pb2 Cl12 162.87(8) . 4_575 ?
Cl5 Pb2 Cl6 87.94(9) . . ?
Cl12 Pb2 Cl6 81.48(4) . . ?
Cl12 Pb2 Cl6 81.48(4) 4_575 . ?
Cl5 Pb2 Cl4 92.13(9) . 1_456 ?
Cl12 Pb2 Cl4 98.52(4) . 1_456 ?
Cl12 Pb2 Cl4 98.52(4) 4_575 1_456 ?
Cl6 Pb2 Cl4 179.93(10) . 1_456 ?
Cl5 Pb2 Cl8 177.55(8) . 1_455 ?
Cl12 Pb2 Cl8 90.78(4) . 1_455 ?
Cl12 Pb2 Cl8 90.78(4) 4_575 1_455 ?
Cl6 Pb2 Cl8 89.61(8) . 1_455 ?
Cl4 Pb2 Cl8 90.33(8) 1_456 1_455 ?
Cl8 Pb3 Cl9 82.12(4) . 4_575 ?
Cl8 Pb3 Cl9 82.12(4) . . ?
Cl9 Pb3 Cl9 163.77(8) 4_575 . ?
Cl8 Pb3 Cl7 87.99(8) . 1_556 ?
Cl9 Pb3 Cl7 87.82(4) 4_575 1_556 ?
Cl9 Pb3 Cl7 87.82(4) . 1_556 ?
Cl8 Pb3 Cl2 83.72(8) . . ?
Cl9 Pb3 Cl2 91.04(4) 4_575 . ?
Cl9 Pb3 Cl2 91.04(4) . . ?
Cl7 Pb3 Cl2 171.72(8) 1_556 . ?
Cl8 Pb3 Cl5 168.18(8) . . ?
Cl9 Pb3 Cl5 98.11(4) 4_575 . ?
Cl9 Pb3 Cl5 98.11(4) . . ?
Cl7 Pb3 Cl5 103.83(8) 1_556 . ?
Cl2 Pb3 Cl5 84.45(8) . . ?
Cl4 Pb4 Cl3 101.04(9) . . ?
Cl4 Pb4 Cl11 86.41(4) . . ?
Cl3 Pb4 Cl11 95.47(4) . . ?
Cl4 Pb4 Cl11 86.41(4) . 4_575 ?
Cl3 Pb4 Cl11 95.47(4) . 4_575 ?
Cl11 Pb4 Cl11 167.89(9) . 4_575 ?
Cl4 Pb4 Cl1 86.17(9) . 1_655 ?
Cl3 Pb4 Cl1 172.79(8) . 1_655 ?
Cl11 Pb4 Cl1 84.90(4) . 1_655 ?
Cl11 Pb4 Cl1 84.90(4) 4_575 1_655 ?
Cl4 Pb4 Cl6 170.46(9) . 1_655 ?
Cl3 Pb4 Cl6 88.50(8) . 1_655 ?
Cl11 Pb4 Cl6 92.73(4) . 1_655 ?
Cl11 Pb4 Cl6 92.73(4) 4_575 1_655 ?
Cl1 Pb4 Cl6 84.29(7) 1_655 1_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

N1 C1 C2 C3 175.0(6) . . . . ?
C6 C1 C2 C3 54.7(8) . . . . ?
C1 C2 C3 C4 -54.4(9) . . . . ?
C2 C3 C4 C5 54.7(9) . . . . ?
C3 C4 C5 C6 -55.1(9) . . . . ?
N1 C1 C6 C5 -177.6(6) . . . . ?
C2 C1 C6 C5 -56.6(9) . . . . ?
C4 C5 C6 C1 56.9(9) . . . . ?
N2 C7 C8 C9 176.2(6) . . . . ?
C12 C7 C8 C9 54.7(8) . . . . ?
C7 C8 C9 C10 -55.4(9) . . . . ?
C8 C9 C10 C11 56.8(8) . . . . ?
C9 C10 C11 C12 -56.9(9) . . . . ?
C10 C11 C12 C7 54.8(9) . . . . ?
N2 C7 C12 C11 -175.0(6) . . . . ?
C8 C7 C12 C11 -54.0(8) . . . . ?
N3 C13 C14 C15 177.7(6) . . . . ?
C18 C13 C14 C15 53.5(10) . . . . ?
C13 C14 C15 C16 -53.2(9) . . . . ?
C14 C15 C16 C17 55.4(9) . . . . ?
C15 C16 C17 C18 -55.5(9) . . . . ?
N3 C13 C18 C17 -178.5(6) . . . . ?
C14 C13 C18 C17 -54.8(9) . . . . ?
C16 C17 C18 C13 54.8(9) . . . . ?
N4 C19 C20 C21 179.7(6) . . . . ?
C24 C19 C20 C21 56.8(9) . . . . ?
C19 C20 C21 C22 -56.5(9) . . . . ?
C20 C21 C22 C23 55.0(10) . . . . ?
C21 C22 C23 C24 -53.1(10) . . . . ?
C22 C23 C24 C19 51.8(9) . . . . ?
N4 C19 C24 C23 -176.0(7) . . . . ?
C20 C19 C24 C23 -53.5(9) . . . . ?
Pb3 Cl2 Pb1 Cl10 89.14(4) . . . . ?
Pb3 Cl2 Pb1 Cl10 -89.14(4) . . . 4_575 ?
Pb3 Cl2 Pb1 Cl1 0.000(2) . . . . ?
Pb3 Cl2 Pb1 Cl3 180.000(2) . . . . ?
Pb4 Cl1 Pb1 Cl10 84.02(4) 1_455 . . . ?
Pb4 Cl1 Pb1 Cl10 -84.02(4) 1_455 . . 4_575 ?
Pb4 Cl1 Pb1 Cl2 180 1_455 . . . ?
Pb4 Cl1 Pb1 Cl3 0 1_455 . . . ?
Pb4 Cl1 Pb1 Cl7 0 1_455 . . . ?
Pb4 Cl3 Pb1 Cl10 96.22(4) . . . . ?
Pb4 Cl3 Pb1 Cl10 -96.22(4) . . . 4_575 ?
Pb4 Cl3 Pb1 Cl2 0 . . . . ?
Pb4 Cl3 Pb1 Cl1 180 . . . . ?
Pb4 Cl3 Pb1 Cl7 180 . . . . ?
Pb3 Cl7 Pb1 Cl10 90.92(4) 1_554 . . . ?
Pb3 Cl7 Pb1 Cl10 -90.92(4) 1_554 . . 4_575 ?
Pb3 Cl7 Pb1 Cl1 180 1_554 . . . ?
Pb3 Cl7 Pb1 Cl3 0 1_554 . . . ?
Pb3 Cl5 Pb2 Cl12 98.49(4) . . . . ?
Pb3 Cl5 Pb2 Cl12 -98.49(4) . . . 4_575 ?
Pb3 Cl5 Pb2 Cl6 180 . . . . ?
Pb3 Cl5 Pb2 Cl4 0 . . . 1_456 ?
Pb4 Cl6 Pb2 Cl5 0.000(2) 1_455 . . . ?
Pb4 Cl6 Pb2 Cl12 89.15(4) 1_455 . . . ?
Pb4 Cl6 Pb2 Cl12 -89.15(4) 1_455 . . 4_575 ?
Pb4 Cl6 Pb2 Cl8 180.000(2) 1_455 . . 1_455 ?
Pb2 Cl8 Pb3 Cl9 91.93(4) 1_655 . . 4_575 ?
Pb2 Cl8 Pb3 Cl9 -91.93(4) 1_655 . . . ?
Pb2 Cl8 Pb3 Cl7 180 1_655 . . 1_556 ?
Pb2 Cl8 Pb3 Cl2 0 1_655 . . . ?
Pb2 Cl8 Pb3 Cl5 0 1_655 . . . ?
Pb1 Cl2 Pb3 Cl8 180.000(2) . . . . ?
Pb1 Cl2 Pb3 Cl9 98.05(4) . . . 4_575 ?
Pb1 Cl2 Pb3 Cl9 -98.05(4) . . . . ?
Pb1 Cl2 Pb3 Cl5 0.000(2) . . . . ?
Pb2 Cl5 Pb3 Cl8 180 . . . . ?
Pb2 Cl5 Pb3 Cl9 89.74(4) . . . 4_575 ?
Pb2 Cl5 Pb3 Cl9 -89.74(4) . . . . ?
Pb2 Cl5 Pb3 Cl7 0 . . . 1_556 ?
Pb2 Cl5 Pb3 Cl2 180 . . . . ?
Pb2 Cl4 Pb4 Cl3 0 1_654 . . . ?
Pb2 Cl4 Pb4 Cl11 -94.88(4) 1_654 . . . ?
Pb2 Cl4 Pb4 Cl11 94.88(4) 1_654 . . 4_575 ?
Pb2 Cl4 Pb4 Cl1 180 1_654 . . 1_655 ?
Pb1 Cl3 Pb4 Cl4 180 . . . . ?
Pb1 Cl3 Pb4 Cl11 -92.60(4) . . . . ?
Pb1 Cl3 Pb4 Cl11 92.60(4) . . . 4_575 ?
Pb1 Cl3 Pb4 Cl6 0 . . . 1_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl3 0.91 2.55 3.259(7) 135.1 1_556
N1 H1B Cl9 0.91 2.32 3.229(7) 176.7 .
N1 H1C Cl10 0.91 2.35 3.236(7) 164.1 1_556
N2 H2A Cl2 0.91 2.61 3.311(7) 134 .
N2 H2B Cl9 0.91 2.35 3.231(7) 163 .
N2 H2C Cl12 0.91 2.32 3.217(7) 170.7 1_655
N3 H3A Cl7 0.91 2.63 3.309(7) 131.9 1_656
N3 H3B Cl11 0.91 2.34 3.241(7) 172.8 1_556
N3 H3C Cl10 0.91 2.37 3.243(7) 160.4 1_656
N4 H4A Cl11 0.91 2.43 3.247(7) 149.3 .
N4 H4B Cl12 0.91 2.33 3.219(7) 167 1_655
N4 H4C Cl1 0.91 2.57 3.323(7) 139.9 1_655
_chemical_name_common            
bis(cyclohexylammonium)tetrachloroplumbate(ii)

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2006-06-16 at 09:19:45
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac24la smart

data_11
_database_code_depnum_ccdc_archive 'CCDC 708570'

_audit_creation_date             2006-06-16T09:19:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
heptadecakis(cycloheptylammonium)hentriacontachloroheptaplumbate(II) dihydrate
;
_chemical_formula_moiety         'Cl31 Pb7, 17(C7 H16 N), 2(H2 O)'
_chemical_formula_sum            'C119 H276 Cl31 N17 O2 Pb7'
_chemical_formula_weight         4526.85
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.7667(15)
_cell_length_b                   46.043(5)
_cell_length_c                   14.9592(15)
_cell_angle_alpha                90
_cell_angle_beta                 94.385(5)
_cell_angle_gamma                90
_cell_volume                     8767.6(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    987
_cell_measurement_theta_min      2.732
_cell_measurement_theta_max      24.939

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4452
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -1 0.135
0 1 0 0.14
0 -1 0 0.14
-1 -1 0 0.11
1 2 0 0.1
0 1 1 0.145
0 -1 1 0.155

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.214
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.1632
_exptl_absorpt_correction_T_max  0.3113
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_number            68260
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_reflns_number_total             29908
_reflns_number_gt                21702
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+, (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+, (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other for all cations except for #10,
which were
restrained using DFIX and DANG instructions instead.
The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction for all cycloheptylammonium
cations.
DIFX and DANG instructions were applied to the water molecule to
give reasonable O-H distances and H-O-H angles.

;
_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)+(0.0522P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         29908
_refine_ls_number_parameters     1582
_refine_ls_number_restraints     2955
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1069
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.94
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(5)
_refine_diff_density_max         3.694
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.167

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1A C 0.6296(12) 0.1531(3) 0.0354(8) 0.049(2) Uani 1 1 d DU . .
H1 H 0.5623 0.1446 0.0083 0.059 Uiso 1 1 calc R . .
C1B C 0.7058(12) 0.1289(3) 0.0575(9) 0.051(2) Uani 1 1 d DU . .
H1B1 H 0.7777 0.137 0.0597 0.062 Uiso 1 1 calc R . .
H1B2 H 0.6995 0.1147 0.0077 0.062 Uiso 1 1 calc R . .
C1C C 0.6938(13) 0.1129(3) 0.1435(8) 0.055(2) Uani 1 1 d DU . .
H1C1 H 0.6181 0.1112 0.1528 0.066 Uiso 1 1 calc R . .
H1C2 H 0.7219 0.0929 0.138 0.066 Uiso 1 1 calc R . .
C1D C 0.7488(13) 0.1271(3) 0.2243(9) 0.057(2) Uani 1 1 d DU . .
H1D1 H 0.7459 0.1136 0.2753 0.069 Uiso 1 1 calc R . .
H1D2 H 0.8237 0.1293 0.2126 0.069 Uiso 1 1 calc R . .
C1E C 0.7112(14) 0.1562(3) 0.2542(9) 0.056(2) Uani 1 1 d DU . .
H1E1 H 0.7636 0.1639 0.3003 0.067 Uiso 1 1 calc R . .
H1E2 H 0.6449 0.1532 0.2832 0.067 Uiso 1 1 calc R . .
C1F C 0.6923(12) 0.1788(3) 0.1826(9) 0.054(2) Uani 1 1 d DU . .
H1F1 H 0.6764 0.1974 0.2117 0.065 Uiso 1 1 calc R . .
H1F2 H 0.7583 0.1815 0.1528 0.065 Uiso 1 1 calc R . .
C1G C 0.6058(11) 0.1725(3) 0.1117(9) 0.051(2) Uani 1 1 d DU . .
H1G1 H 0.5806 0.1913 0.0861 0.061 Uiso 1 1 calc R . .
H1G2 H 0.5468 0.1638 0.1415 0.061 Uiso 1 1 calc R . .
N1 N 0.6776(11) 0.1724(3) -0.0350(9) 0.052(3) Uani 1 1 d U . .
H1A H 0.6329 0.1873 -0.0504 0.079 Uiso 1 1 calc R . .
H1B H 0.6882 0.1616 -0.0845 0.079 Uiso 1 1 calc R . .
H1C H 0.7401 0.1797 -0.0117 0.079 Uiso 1 1 calc R . .
C2A C 0.2689(10) 0.2225(4) 0.1020(9) 0.050(2) Uani 1 1 d DU . .
H2 H 0.2691 0.2442 0.0987 0.061 Uiso 1 1 calc R . .
C2B C 0.1773(10) 0.2139(4) 0.1530(11) 0.057(2) Uani 1 1 d DU . .
H2B1 H 0.1622 0.2301 0.1936 0.069 Uiso 1 1 calc R . .
H2B2 H 0.1153 0.2117 0.1097 0.069 Uiso 1 1 calc R . .
C2C C 0.1883(12) 0.1875(4) 0.2060(10) 0.060(2) Uani 1 1 d DU . .
H2C1 H 0.221 0.1727 0.1691 0.072 Uiso 1 1 calc R . .
H2C2 H 0.1167 0.1806 0.2156 0.072 Uiso 1 1 calc R . .
C2D C 0.2503(10) 0.1881(4) 0.2971(10) 0.058(2) Uani 1 1 d DU . .
H2D1 H 0.2181 0.2029 0.3345 0.07 Uiso 1 1 calc R . .
H2D2 H 0.2415 0.1691 0.3261 0.07 Uiso 1 1 calc R . .
C2E C 0.3662(10) 0.1944(4) 0.2987(10) 0.054(2) Uani 1 1 d DU . .
H2E1 H 0.4025 0.1767 0.28 0.065 Uiso 1 1 calc R . .
H2E2 H 0.3926 0.1988 0.3612 0.065 Uiso 1 1 calc R . .
C2F C 0.3962(12) 0.2194(3) 0.2394(8) 0.051(2) Uani 1 1 d DU . .
H2F1 H 0.4716 0.2239 0.2529 0.061 Uiso 1 1 calc R . .
H2F2 H 0.3556 0.2369 0.2543 0.061 Uiso 1 1 calc R . .
C2G C 0.3767(10) 0.2133(4) 0.1389(8) 0.049(2) Uani 1 1 d DU . .
H2G1 H 0.43 0.2237 0.1063 0.058 Uiso 1 1 calc R . .
H2G2 H 0.3853 0.1922 0.1283 0.058 Uiso 1 1 calc R . .
N2 N 0.2585(10) 0.2115(3) 0.0083(8) 0.047(3) Uani 1 1 d U . .
H2A H 0.1947 0.2167 -0.0182 0.071 Uiso 1 1 calc R . .
H2B H 0.264 0.1918 0.0086 0.071 Uiso 1 1 calc R . .
H2C H 0.3102 0.2192 -0.0229 0.071 Uiso 1 1 calc R . .
C3A C -0.0930(13) 0.2689(3) 0.1659(9) 0.054(2) Uani 1 1 d DU . .
H3 H -0.0211 0.2766 0.1577 0.064 Uiso 1 1 calc R . .
C3B C -0.1635(12) 0.2932(3) 0.1920(10) 0.060(2) Uani 1 1 d DU . .
H3B1 H -0.1809 0.3054 0.1385 0.072 Uiso 1 1 calc R . .
H3B2 H -0.2299 0.2845 0.2096 0.072 Uiso 1 1 calc R . .
C3C C -0.1210(14) 0.3123(3) 0.2659(9) 0.069(3) Uani 1 1 d DU . .
H3C1 H -0.0689 0.3252 0.2407 0.082 Uiso 1 1 calc R . .
H3C2 H -0.1796 0.3248 0.2825 0.082 Uiso 1 1 calc R . .
C3D C -0.0712(15) 0.3003(3) 0.3493(10) 0.075(3) Uani 1 1 d DU . .
H3D1 H -0.0907 0.3132 0.3983 0.09 Uiso 1 1 calc R . .
H3D2 H 0.0056 0.3024 0.346 0.09 Uiso 1 1 calc R . .
C3E C -0.0900(15) 0.2701(3) 0.3788(10) 0.073(3) Uani 1 1 d DU . .
H3E1 H -0.1661 0.2657 0.372 0.087 Uiso 1 1 calc R . .
H3E2 H -0.0654 0.2678 0.4428 0.087 Uiso 1 1 calc R . .
C3F C -0.0304(14) 0.2493(3) 0.3215(9) 0.065(3) Uani 1 1 d DU . .
H3F1 H 0.04 0.2574 0.3136 0.079 Uiso 1 1 calc R . .
H3F2 H -0.0206 0.2306 0.3536 0.079 Uiso 1 1 calc R . .
C3G C -0.0860(14) 0.2438(3) 0.2309(9) 0.058(2) Uani 1 1 d DU . .
H3G1 H -0.1583 0.2373 0.2398 0.07 Uiso 1 1 calc R . .
H3G2 H -0.05 0.2275 0.2026 0.07 Uiso 1 1 calc R . .
N3 N -0.1432(9) 0.2576(3) 0.0766(8) 0.037(2) Uani 1 1 d U . .
H3A H -0.1044 0.2427 0.0572 0.055 Uiso 1 1 calc R . .
H3B H -0.1457 0.2722 0.0354 0.055 Uiso 1 1 calc R . .
H3C H -0.2096 0.2513 0.0841 0.055 Uiso 1 1 calc R . .
C4A C 0.4396(15) 0.0440(3) -0.0470(10) 0.067(2) Uani 1 1 d DU . .
H4 H 0.3661 0.0457 -0.0748 0.081 Uiso 1 1 calc R . .
C4B C 0.4533(14) 0.0135(3) -0.0169(11) 0.070(3) Uani 1 1 d DU . .
H4B1 H 0.3863 0.0068 0.0053 0.084 Uiso 1 1 calc R . .
H4B2 H 0.4667 0.0015 -0.0696 0.084 Uiso 1 1 calc R . .
C4C C 0.5381(13) 0.0080(4) 0.0537(10) 0.073(3) Uani 1 1 d DU . .
H4C1 H 0.5957 0.0222 0.048 0.087 Uiso 1 1 calc R . .
H4C2 H 0.5669 -0.0117 0.0462 0.087 Uiso 1 1 calc R . .
C4D C 0.4969(15) 0.0107(3) 0.1471(10) 0.073(3) Uani 1 1 d DU . .
H4D1 H 0.4298 0 0.1477 0.088 Uiso 1 1 calc R . .
H4D2 H 0.5478 0.0015 0.1917 0.088 Uiso 1 1 calc R . .
C4E C 0.4796(15) 0.0413(4) 0.1742(10) 0.073(3) Uani 1 1 d DU . .
H4E1 H 0.5491 0.0509 0.1834 0.088 Uiso 1 1 calc R . .
H4E2 H 0.4487 0.0411 0.2329 0.088 Uiso 1 1 calc R . .
C4F C 0.4107(14) 0.0599(4) 0.1112(10) 0.069(3) Uani 1 1 d DU . .
H4F1 H 0.3421 0.05 0.0999 0.083 Uiso 1 1 calc R . .
H4F2 H 0.3976 0.0785 0.1419 0.083 Uiso 1 1 calc R . .
C4G C 0.4521(15) 0.0667(3) 0.0227(10) 0.068(3) Uani 1 1 d DU . .
H4G1 H 0.4168 0.0845 -0.0012 0.082 Uiso 1 1 calc R . .
H4G2 H 0.5279 0.0712 0.0332 0.082 Uiso 1 1 calc R . .
N4 N 0.5111(13) 0.0470(4) -0.1222(10) 0.076(4) Uani 1 1 d U . .
H4A H 0.4986 0.0322 -0.1619 0.114 Uiso 1 1 calc R . .
H4B H 0.5792 0.0463 -0.0994 0.114 Uiso 1 1 calc R . .
H4C H 0.4986 0.0642 -0.1506 0.114 Uiso 1 1 calc R . .
C5A C 0.2729(14) 0.2541(3) -0.3150(9) 0.052(2) Uani 1 1 d DU . .
H5 H 0.3476 0.2544 -0.2895 0.063 Uiso 1 1 calc R . .
C5B C 0.2676(14) 0.2310(3) -0.3842(9) 0.052(2) Uani 1 1 d DU . .
H5B1 H 0.1929 0.2258 -0.3976 0.062 Uiso 1 1 calc R . .
H5B2 H 0.304 0.2137 -0.3582 0.062 Uiso 1 1 calc R . .
C5C C 0.3135(13) 0.2380(3) -0.4716(9) 0.056(2) Uani 1 1 d DU . .
H5C1 H 0.38 0.2488 -0.4582 0.067 Uiso 1 1 calc R . .
H5C2 H 0.331 0.2195 -0.5007 0.067 Uiso 1 1 calc R . .
C5D C 0.2447(13) 0.2554(3) -0.5364(9) 0.057(2) Uani 1 1 d DU . .
H5D1 H 0.2805 0.2566 -0.5927 0.069 Uiso 1 1 calc R . .
H5D2 H 0.1795 0.2441 -0.55 0.069 Uiso 1 1 calc R . .
C5E C 0.2130(14) 0.2853(3) -0.5137(9) 0.056(2) Uani 1 1 d DU . .
H5E1 H 0.1592 0.2921 -0.5602 0.068 Uiso 1 1 calc R . .
H5E2 H 0.2748 0.2982 -0.5156 0.068 Uiso 1 1 calc R . .
C5F C 0.1695(12) 0.2884(3) -0.4228(9) 0.056(2) Uani 1 1 d DU . .
H5F1 H 0.1365 0.3077 -0.4191 0.067 Uiso 1 1 calc R . .
H5F2 H 0.1138 0.2736 -0.4176 0.067 Uiso 1 1 calc R . .
C5G C 0.2497(13) 0.2849(3) -0.3457(9) 0.054(2) Uani 1 1 d DU . .
H5G1 H 0.226 0.296 -0.2943 0.064 Uiso 1 1 calc R . .
H5G2 H 0.3161 0.2939 -0.3622 0.064 Uiso 1 1 calc R . .
N5 N 0.2097(11) 0.2461(3) -0.2387(9) 0.050(3) Uani 1 1 d U . .
H5A H 0.2143 0.2605 -0.1969 0.075 Uiso 1 1 calc R . .
H5B H 0.235 0.2293 -0.2134 0.075 Uiso 1 1 calc R . .
H5C H 0.1414 0.2436 -0.2592 0.075 Uiso 1 1 calc R . .
C6A C -0.3228(14) 0.2027(3) -0.3492(10) 0.067(2) Uani 1 1 d DU . .
H6 H -0.2612 0.2105 -0.3115 0.08 Uiso 1 1 calc R . .
C6B C -0.2797(14) 0.1841(4) -0.4186(9) 0.070(3) Uani 1 1 d DU . .
H6B1 H -0.2707 0.1642 -0.3944 0.084 Uiso 1 1 calc RD . .
H6B2 H -0.2091 0.1915 -0.4301 0.084 Uiso 1 1 calc R . .
C6C C -0.3446(15) 0.1826(3) -0.5056(10) 0.070(3) Uani 1 1 d DU . .
H6C1 H -0.4193 0.1806 -0.4931 0.084 Uiso 1 1 calc R . .
H6C2 H -0.3246 0.165 -0.538 0.084 Uiso 1 1 calc R . .
C6D C -0.3340(15) 0.2089(3) -0.5668(10) 0.071(3) Uani 1 1 d DU . .
H6D1 H -0.2581 0.2127 -0.5706 0.085 Uiso 1 1 calc R . .
H6D2 H -0.3634 0.2035 -0.6276 0.085 Uiso 1 1 calc R . .
C6E C -0.3848(15) 0.2365(3) -0.5412(10) 0.069(3) Uani 1 1 d DU . .
H6E1 H -0.4619 0.2338 -0.5491 0.082 Uiso 1 1 calc R . .
H6E2 H -0.3662 0.2518 -0.5839 0.082 Uiso 1 1 calc R . .
C6F C -0.3571(15) 0.2478(3) -0.4462(9) 0.068(3) Uani 1 1 d DU . .
H6F1 H -0.2801 0.2506 -0.4375 0.082 Uiso 1 1 calc R . .
H6F2 H -0.3908 0.267 -0.4397 0.082 Uiso 1 1 calc R . .
C6G C -0.3912(14) 0.2277(4) -0.3741(11) 0.067(3) Uani 1 1 d DU . .
H6G1 H -0.3984 0.2394 -0.3194 0.08 Uiso 1 1 calc R . .
H6G2 H -0.4618 0.2202 -0.3938 0.08 Uiso 1 1 calc R . .
N6 N -0.3754(12) 0.1811(4) -0.2920(9) 0.071(3) Uani 1 1 d U . .
H6A H -0.3306 0.1661 -0.2778 0.106 Uiso 1 1 calc RD . .
H6B H -0.4345 0.1742 -0.3226 0.106 Uiso 1 1 calc R . .
H6C H -0.3928 0.19 -0.2408 0.106 Uiso 1 1 calc R . .
C7A C -0.1708(18) 0.3150(4) -0.2813(10) 0.089(3) Uani 1 1 d DU . .
H7 H -0.2366 0.3032 -0.2883 0.107 Uiso 1 1 calc R . .
C7B C -0.1994(17) 0.3434(4) -0.2422(11) 0.092(3) Uani 1 1 d DU . .
H7B1 H -0.1356 0.3557 -0.2349 0.111 Uiso 1 1 calc R . .
H7B2 H -0.2237 0.3399 -0.1818 0.111 Uiso 1 1 calc R . .
C7C C -0.2836(15) 0.3597(4) -0.2975(12) 0.097(3) Uani 1 1 d DU . .
H7C1 H -0.3403 0.3459 -0.3165 0.116 Uiso 1 1 calc R . .
H7C2 H -0.3138 0.3744 -0.2587 0.116 Uiso 1 1 calc R . .
C7D C -0.2500(18) 0.3748(4) -0.3792(11) 0.101(3) Uani 1 1 d DU . .
H7D1 H -0.3131 0.3846 -0.4075 0.121 Uiso 1 1 calc R . .
H7D2 H -0.2006 0.3903 -0.3578 0.121 Uiso 1 1 calc R . .
C7E C -0.2007(19) 0.3594(4) -0.4513(12) 0.102(3) Uani 1 1 d DU . .
H7E1 H -0.1297 0.3678 -0.455 0.122 Uiso 1 1 calc R . .
H7E2 H -0.2416 0.3642 -0.5083 0.122 Uiso 1 1 calc R . .
C7F C -0.1885(18) 0.3271(4) -0.4481(11) 0.101(3) Uani 1 1 d DU . .
H7F1 H -0.2593 0.3182 -0.4498 0.121 Uiso 1 1 calc R . .
H7F2 H -0.1558 0.3207 -0.5027 0.121 Uiso 1 1 calc R . .
C7G C -0.1266(16) 0.3158(4) -0.3709(10) 0.094(3) Uani 1 1 d DU . .
H7G1 H -0.0611 0.3274 -0.3641 0.113 Uiso 1 1 calc R . .
H7G2 H -0.1063 0.2957 -0.3854 0.113 Uiso 1 1 calc R . .
N7 N -0.0978(12) 0.2997(3) -0.2163(10) 0.067(3) Uani 1 1 d U . .
H7A H -0.1268 0.2984 -0.1627 0.101 Uiso 1 1 calc R . .
H7B H -0.0363 0.3098 -0.209 0.101 Uiso 1 1 calc R . .
H7C H -0.0851 0.2816 -0.237 0.101 Uiso 1 1 calc R . .
C8A C 0.5441(11) 0.3195(2) 0.2096(8) 0.0420(19) Uani 1 1 d DU . .
H8 H 0.6143 0.3201 0.1842 0.05 Uiso 1 1 calc R . .
C8B C 0.5115(11) 0.3504(3) 0.2277(8) 0.044(2) Uani 1 1 d DU . .
H8B1 H 0.5253 0.3624 0.1751 0.052 Uiso 1 1 calc R . .
H8B2 H 0.4348 0.3507 0.2337 0.052 Uiso 1 1 calc R . .
C8C C 0.5662(12) 0.3640(3) 0.3104(8) 0.048(2) Uani 1 1 d DU . .
H8C1 H 0.6397 0.3569 0.3165 0.057 Uiso 1 1 calc R . .
H8C2 H 0.5687 0.3853 0.3012 0.057 Uiso 1 1 calc R . .
C8D C 0.5173(13) 0.3582(3) 0.3969(8) 0.051(2) Uani 1 1 d DU . .
H8D1 H 0.4444 0.3657 0.3907 0.061 Uiso 1 1 calc R . .
H8D2 H 0.556 0.3697 0.4445 0.061 Uiso 1 1 calc R . .
C8E C 0.5133(13) 0.3268(3) 0.4291(8) 0.050(2) Uani 1 1 d DU . .
H8E1 H 0.4664 0.326 0.4788 0.06 Uiso 1 1 calc R . .
H8E2 H 0.5846 0.3214 0.4544 0.06 Uiso 1 1 calc R . .
C8F C 0.4765(11) 0.3035(3) 0.3602(9) 0.048(2) Uani 1 1 d DU . .
H8F1 H 0.4672 0.2849 0.3916 0.057 Uiso 1 1 calc R . .
H8F2 H 0.4073 0.3093 0.3311 0.057 Uiso 1 1 calc R . .
C8G C 0.5524(11) 0.2991(3) 0.2891(8) 0.044(2) Uani 1 1 d DU . .
H8G1 H 0.5437 0.279 0.2663 0.053 Uiso 1 1 calc R . .
H8G2 H 0.6245 0.3007 0.3182 0.053 Uiso 1 1 calc R . .
N8 N 0.4658(9) 0.3073(3) 0.1385(8) 0.036(2) Uani 1 1 d U . .
H8A H 0.4605 0.3194 0.0904 0.053 Uiso 1 1 calc R . .
H8B H 0.402 0.3055 0.1612 0.053 Uiso 1 1 calc R . .
H8C H 0.4878 0.2895 0.1211 0.053 Uiso 1 1 calc R . .
C9A C 0.3613(11) -0.0747(3) -0.1486(9) 0.049(2) Uani 1 1 d DU . .
H9 H 0.4093 -0.0856 -0.1863 0.059 Uiso 1 1 calc R . .
C9B C 0.4120(10) -0.0717(3) -0.0559(8) 0.051(2) Uani 1 1 d DU . .
H9B1 H 0.4613 -0.0551 -0.0558 0.061 Uiso 1 1 calc R . .
H9B2 H 0.4547 -0.0894 -0.0427 0.061 Uiso 1 1 calc R . .
C9C C 0.3435(12) -0.0674(3) 0.0204(9) 0.054(2) Uani 1 1 d DU . .
H9C1 H 0.2827 -0.0552 -0.0008 0.065 Uiso 1 1 calc R . .
H9C2 H 0.384 -0.0566 0.0688 0.065 Uiso 1 1 calc R . .
C9D C 0.3028(12) -0.0954(3) 0.0590(9) 0.058(2) Uani 1 1 d DU . .
H9D1 H 0.3617 -0.1093 0.0685 0.07 Uiso 1 1 calc R . .
H9D2 H 0.2761 -0.0912 0.1181 0.07 Uiso 1 1 calc R . .
C9E C 0.2165(12) -0.1091(3) -0.0011(9) 0.060(2) Uani 1 1 d DU . .
H9E1 H 0.1547 -0.0961 -0.0042 0.072 Uiso 1 1 calc R . .
H9E2 H 0.1958 -0.1276 0.0265 0.072 Uiso 1 1 calc R . .
C9F C 0.2451(13) -0.1153(3) -0.0954(9) 0.058(2) Uani 1 1 d DU . .
H9F1 H 0.3131 -0.1257 -0.0918 0.07 Uiso 1 1 calc R . .
H9F2 H 0.1915 -0.1285 -0.1242 0.07 Uiso 1 1 calc R . .
C9G C 0.2539(11) -0.0894(3) -0.1545(10) 0.053(2) Uani 1 1 d DU . .
H9G1 H 0.2008 -0.075 -0.1393 0.064 Uiso 1 1 calc R . .
H9G2 H 0.2365 -0.0955 -0.2174 0.064 Uiso 1 1 calc R . .
N9 N 0.3416(9) -0.0439(2) -0.1888(8) 0.037(2) Uani 1 1 d U . .
H9A H 0.3099 -0.0454 -0.2452 0.056 Uiso 1 1 calc R . .
H9B H 0.4039 -0.0344 -0.191 0.056 Uiso 1 1 calc R . .
H9C H 0.2993 -0.0337 -0.1538 0.056 Uiso 1 1 calc R . .
N10 N 0.3792(10) 0.3435(2) -0.1761(7) 0.064(3) Uani 1 1 d U . .
H10A H 0.3585 0.3292 -0.2153 0.096 Uiso 1 1 calc R . .
H10B H 0.3323 0.345 -0.1335 0.096 Uiso 1 1 calc R . .
H10C H 0.4438 0.3392 -0.1494 0.096 Uiso 1 1 calc R . .
C10A C 0.3839(10) 0.3700(2) -0.2224(7) 0.092(3) Uani 1 1 d DU . .
H10 H 0.459 0.3662 -0.2333 0.11 Uiso 1 1 calc R . .
C10B C 0.415(2) 0.3959(3) -0.1689(11) 0.093(3) Uani 1 1 d DU . .
H10N H 0.4848 0.3918 -0.1378 0.112 Uiso 1 1 calc R . .
H10O H 0.3649 0.3978 -0.1219 0.112 Uiso 1 1 calc R . .
C10C C 0.4218(18) 0.4247(3) -0.2131(12) 0.095(3) Uani 1 1 d DU . .
H10D H 0.4556 0.4382 -0.168 0.114 Uiso 1 1 calc R . .
H10E H 0.3489 0.4317 -0.2264 0.114 Uiso 1 1 calc R . .
C10D C 0.4772(18) 0.4284(4) -0.2971(10) 0.096(3) Uani 1 1 d DU . .
H10F H 0.4802 0.4495 -0.3079 0.115 Uiso 1 1 calc R . .
H10G H 0.5505 0.422 -0.282 0.115 Uiso 1 1 calc R . .
C10E C 0.445(2) 0.4151(3) -0.3845(12) 0.097(3) Uani 1 1 d DU . .
H10H H 0.5038 0.4175 -0.4232 0.116 Uiso 1 1 calc R . .
H10I H 0.3853 0.4266 -0.412 0.116 Uiso 1 1 calc R . .
C10F C 0.4134(18) 0.3843(4) -0.3886(12) 0.097(3) Uani 1 1 d DU . .
H10J H 0.4791 0.3731 -0.3928 0.116 Uiso 1 1 calc R . .
H10K H 0.3721 0.3818 -0.4468 0.116 Uiso 1 1 calc R . .
C10G C 0.3542(17) 0.3689(4) -0.3215(8) 0.096(3) Uani 1 1 d DU . .
H10L H 0.3529 0.3482 -0.3386 0.115 Uiso 1 1 calc R . .
H10M H 0.2808 0.3759 -0.3301 0.115 Uiso 1 1 calc R . .
C11A C 0.8024(14) 0.0272(3) -0.5287(9) 0.055(2) Uani 1 1 d DU . .
H11 H 0.7284 0.0224 -0.5168 0.066 Uiso 1 1 calc R . .
C11B C 0.7989(14) 0.0518(3) -0.5957(9) 0.060(2) Uani 1 1 d DU . .
H11N H 0.7648 0.0688 -0.5696 0.073 Uiso 1 1 calc R . .
H11O H 0.8717 0.0575 -0.6065 0.073 Uiso 1 1 calc R . .
C11C C 0.7411(14) 0.0445(4) -0.6835(9) 0.069(3) Uani 1 1 d DU . .
H11D H 0.7189 0.0628 -0.7139 0.083 Uiso 1 1 calc R . .
H11E H 0.6766 0.0337 -0.6714 0.083 Uiso 1 1 calc R . .
C11D C 0.8010(16) 0.0268(3) -0.7465(10) 0.076(3) Uani 1 1 d DU . .
H11F H 0.7615 0.0275 -0.806 0.091 Uiso 1 1 calc R . .
H11G H 0.8688 0.0368 -0.7526 0.091 Uiso 1 1 calc R . .
C11E C 0.8240(16) -0.0038(3) -0.7255(10) 0.078(3) Uani 1 1 d DU . .
H11H H 0.9005 -0.0068 -0.7285 0.093 Uiso 1 1 calc R . .
H11I H 0.7882 -0.0158 -0.7737 0.093 Uiso 1 1 calc R . .
C11F C 0.7941(14) -0.0158(4) -0.6366(9) 0.073(3) Uani 1 1 d DU . .
H11J H 0.7176 -0.0134 -0.6322 0.087 Uiso 1 1 calc R . .
H11K H 0.8105 -0.0368 -0.6332 0.087 Uiso 1 1 calc R . .
C11G C 0.8531(13) -0.0002(3) -0.5591(10) 0.063(2) Uani 1 1 d DU . .
H11L H 0.8617 -0.0137 -0.5076 0.075 Uiso 1 1 calc R . .
H11M H 0.9242 0.0047 -0.5768 0.075 Uiso 1 1 calc R . .
N11 N 0.8585(10) 0.0381(3) -0.4404(8) 0.045(3) Uani 1 1 d U . .
H11A H 0.8269 0.0547 -0.4229 0.068 Uiso 1 1 calc R . .
H11B H 0.9271 0.0418 -0.4487 0.068 Uiso 1 1 calc R . .
H11C H 0.8547 0.0243 -0.3973 0.068 Uiso 1 1 calc R . .
C12A C 0.2284(16) -0.0237(4) -0.5989(11) 0.092(3) Uani 1 1 d DU . .
H12 H 0.2881 -0.0366 -0.6128 0.11 Uiso 1 1 calc R . .
C12B C 0.1407(16) -0.0431(4) -0.5839(11) 0.096(3) Uani 1 1 d DU . .
H12N H 0.0906 -0.0322 -0.5491 0.115 Uiso 1 1 calc R . .
H12O H 0.1683 -0.0593 -0.5458 0.115 Uiso 1 1 calc R . .
C12C C 0.0808(16) -0.0557(5) -0.6636(11) 0.098(3) Uani 1 1 d DU . .
H12D H 0.0168 -0.0437 -0.6755 0.117 Uiso 1 1 calc R . .
H12E H 0.0573 -0.0752 -0.6464 0.117 Uiso 1 1 calc R . .
C12D C 0.1303(18) -0.0589(4) -0.7511(11) 0.099(3) Uani 1 1 d DU . .
H12F H 0.1998 -0.0681 -0.7382 0.119 Uiso 1 1 calc R . .
H12G H 0.0867 -0.0726 -0.7889 0.119 Uiso 1 1 calc R . .
C12E C 0.1461(17) -0.0322(4) -0.8057(11) 0.098(3) Uani 1 1 d DU . .
H12H H 0.162 -0.0381 -0.8669 0.118 Uiso 1 1 calc R . .
H12I H 0.0802 -0.0208 -0.8108 0.118 Uiso 1 1 calc R . .
C12F C 0.2324(16) -0.0138(4) -0.7660(11) 0.096(3) Uani 1 1 d DU . .
H12J H 0.2422 0.0026 -0.8074 0.116 Uiso 1 1 calc R . .
H12K H 0.298 -0.0254 -0.7624 0.116 Uiso 1 1 calc R . .
C12G C 0.2180(18) -0.0014(4) -0.6737(10) 0.095(3) Uani 1 1 d DU . .
H12L H 0.2708 0.0141 -0.6607 0.114 Uiso 1 1 calc R . .
H12M H 0.1476 0.0076 -0.6745 0.114 Uiso 1 1 calc R . .
N12 N 0.2617(12) -0.0094(3) -0.5085(10) 0.066(3) Uani 1 1 d U . .
H12A H 0.3171 0.0027 -0.5149 0.099 Uiso 1 1 calc R . .
H12B H 0.2808 -0.0234 -0.4674 0.099 Uiso 1 1 calc R . .
H12C H 0.207 0.001 -0.4895 0.099 Uiso 1 1 calc R . .
C13A C 0.8907(14) -0.0158(3) -0.0785(9) 0.061(2) Uani 1 1 d DU . .
H13 H 0.9576 -0.0044 -0.0779 0.073 Uiso 1 1 calc R . .
C13B C 0.8603(13) -0.0138(3) 0.0177(9) 0.062(2) Uani 1 1 d DU . .
H13N H 0.9249 -0.0144 0.0587 0.074 Uiso 1 1 calc R . .
H13O H 0.8257 0.0052 0.0262 0.074 Uiso 1 1 calc R . .
C13C C 0.7872(12) -0.0379(3) 0.0432(11) 0.067(2) Uani 1 1 d DU . .
H13D H 0.7413 -0.0305 0.0886 0.08 Uiso 1 1 calc R . .
H13E H 0.7417 -0.0437 -0.0104 0.08 Uiso 1 1 calc R . .
C13D C 0.8465(14) -0.0643(3) 0.0807(11) 0.072(3) Uani 1 1 d DU . .
H13F H 0.8979 -0.0578 0.1294 0.086 Uiso 1 1 calc R . .
H13G H 0.7959 -0.0773 0.1077 0.086 Uiso 1 1 calc R . .
C13E C 0.9030(14) -0.0813(3) 0.0159(11) 0.073(3) Uani 1 1 d DU . .
H13H H 0.8501 -0.0927 -0.021 0.087 Uiso 1 1 calc R . .
H13I H 0.9484 -0.0954 0.0506 0.087 Uiso 1 1 calc R . .
C13F C 0.9703(13) -0.0658(3) -0.0472(11) 0.071(3) Uani 1 1 d DU . .
H13J H 1.0255 -0.0551 -0.0104 0.085 Uiso 1 1 calc R . .
H13K H 1.0061 -0.0807 -0.0814 0.085 Uiso 1 1 calc R . .
C13G C 0.9198(15) -0.0451(3) -0.1124(10) 0.065(2) Uani 1 1 d DU . .
H13L H 0.8551 -0.0543 -0.14 0.078 Uiso 1 1 calc R . .
H13M H 0.9676 -0.0421 -0.1606 0.078 Uiso 1 1 calc R . .
N13 N 0.8177(11) 0.0002(3) -0.1427(9) 0.056(3) Uani 1 1 d U . .
H13A H 0.8027 0.0178 -0.1192 0.084 Uiso 1 1 calc R . .
H13B H 0.7574 -0.0102 -0.1531 0.084 Uiso 1 1 calc R . .
H13C H 0.8483 0.0028 -0.1951 0.084 Uiso 1 1 calc R . .
C14A C 0.0820(13) 0.1439(3) -0.4009(9) 0.058(2) Uani 1 1 d DU . .
H14 H 0.1502 0.1517 -0.3735 0.07 Uiso 1 1 calc R . .
C14B C 0.1081(13) 0.1241(4) -0.4728(10) 0.059(2) Uani 1 1 d DU . .
H14N H 0.1297 0.1053 -0.445 0.071 Uiso 1 1 calc R . .
H14O H 0.17 0.1321 -0.5004 0.071 Uiso 1 1 calc R . .
C14C C 0.0245(13) 0.1182(3) -0.5462(10) 0.058(2) Uani 1 1 d DU . .
H14D H -0.0439 0.1161 -0.5197 0.069 Uiso 1 1 calc R . .
H14E H 0.04 0.0995 -0.5754 0.069 Uiso 1 1 calc R . .
C14D C 0.0152(15) 0.1418(3) -0.6167(9) 0.059(2) Uani 1 1 d DU . .
H14F H 0.0861 0.1455 -0.6368 0.071 Uiso 1 1 calc R . .
H14G H -0.0288 0.1343 -0.6691 0.071 Uiso 1 1 calc R . .
C14E C -0.0300(14) 0.1705(3) -0.5903(10) 0.060(2) Uani 1 1 d DU . .
H14H H -0.104 0.1674 -0.5769 0.072 Uiso 1 1 calc R . .
H14I H -0.0303 0.1838 -0.6421 0.072 Uiso 1 1 calc R . .
C14F C 0.0278(14) 0.1850(3) -0.5100(9) 0.059(2) Uani 1 1 d DU . .
H14J H 0.0025 0.2053 -0.5059 0.071 Uiso 1 1 calc R . .
H14K H 0.1037 0.1857 -0.5194 0.071 Uiso 1 1 calc R . .
C14G C 0.0132(13) 0.1695(3) -0.4210(9) 0.058(2) Uani 1 1 d DU . .
H14L H 0.0256 0.1837 -0.3717 0.069 Uiso 1 1 calc R . .
H14M H -0.0609 0.1631 -0.4213 0.069 Uiso 1 1 calc R . .
N14 N 0.0359(11) 0.1264(3) -0.3302(9) 0.058(3) Uani 1 1 d U . .
H14A H 0.0187 0.1383 -0.2851 0.087 Uiso 1 1 calc R . .
H14B H 0.0837 0.1131 -0.3083 0.087 Uiso 1 1 calc R . .
H14C H -0.0227 0.1172 -0.354 0.087 Uiso 1 1 calc R . .
C15A C 0.0374(15) 0.0957(3) -0.0138(10) 0.065(2) Uani 1 1 d DU . .
H15 H -0.0238 0.0871 -0.0503 0.078 Uiso 1 1 calc R . .
C15B C 0.1098(14) 0.0711(3) 0.0111(11) 0.068(3) Uani 1 1 d DU . .
H15N H 0.178 0.0791 0.0357 0.082 Uiso 1 1 calc R . .
H15O H 0.1226 0.06 -0.0438 0.082 Uiso 1 1 calc R . .
C15C C 0.0693(15) 0.0503(3) 0.0791(10) 0.070(3) Uani 1 1 d DU . .
H15D H -0.0077 0.0485 0.0671 0.084 Uiso 1 1 calc R . .
H15E H 0.1003 0.0309 0.07 0.084 Uiso 1 1 calc R . .
C15D C 0.0928(16) 0.0589(3) 0.1761(10) 0.072(3) Uani 1 1 d DU . .
H15F H 0.0694 0.0428 0.2138 0.086 Uiso 1 1 calc R . .
H15G H 0.17 0.0604 0.1875 0.086 Uiso 1 1 calc R . .
C15E C 0.0458(16) 0.0862(3) 0.2077(11) 0.073(3) Uani 1 1 d DU . .
H15H H 0.0784 0.0907 0.2683 0.087 Uiso 1 1 calc R . .
H15I H -0.03 0.0829 0.2133 0.087 Uiso 1 1 calc R . .
C15F C 0.0576(15) 0.1129(3) 0.1478(10) 0.070(3) Uani 1 1 d DU . .
H15J H 0.0384 0.1304 0.1812 0.084 Uiso 1 1 calc R . .
H15K H 0.1323 0.1148 0.1353 0.084 Uiso 1 1 calc R . .
C15G C -0.0077(14) 0.1119(4) 0.0612(10) 0.067(3) Uani 1 1 d DU . .
H15L H -0.0217 0.1321 0.0411 0.08 Uiso 1 1 calc R . .
H15M H -0.0761 0.103 0.072 0.08 Uiso 1 1 calc R . .
N15 N 0.0908(12) 0.1163(3) -0.0767(10) 0.063(3) Uani 1 1 d U . .
H15A H 0.117 0.1059 -0.1217 0.095 Uiso 1 1 calc R . .
H15B H 0.1442 0.1259 -0.0453 0.095 Uiso 1 1 calc R . .
H15C H 0.0431 0.1294 -0.1004 0.095 Uiso 1 1 calc R . .
C16A C 0.1223(11) 0.3681(3) 0.2982(9) 0.048(2) Uani 1 1 d DU . .
H16 H 0.075 0.3507 0.2951 0.058 Uiso 1 1 calc R . .
C16B C 0.1941(10) 0.3648(3) 0.3817(8) 0.051(2) Uani 1 1 d DU . .
H16N H 0.243 0.3815 0.3857 0.062 Uiso 1 1 calc R . .
H16O H 0.2367 0.347 0.3758 0.062 Uiso 1 1 calc R . .
C16C C 0.1411(12) 0.3629(3) 0.4682(9) 0.053(2) Uani 1 1 d DU . .
H16D H 0.1908 0.3539 0.5141 0.064 Uiso 1 1 calc R . .
H16E H 0.0798 0.3498 0.4588 0.064 Uiso 1 1 calc R . .
C16D C 0.1040(12) 0.3913(3) 0.5049(9) 0.056(2) Uani 1 1 d DU . .
H16F H 0.072 0.387 0.5617 0.067 Uiso 1 1 calc R . .
H16G H 0.1671 0.4033 0.5206 0.067 Uiso 1 1 calc R . .
C16E C 0.0274(12) 0.4099(3) 0.4492(9) 0.056(2) Uani 1 1 d DU . .
H16H H -0.0302 0.4151 0.4868 0.067 Uiso 1 1 calc R . .
H16I H 0.0638 0.4282 0.4354 0.067 Uiso 1 1 calc R . .
C16F C -0.0214(11) 0.3980(3) 0.3628(9) 0.051(2) Uani 1 1 d DU . .
H16J H -0.0789 0.4111 0.3403 0.062 Uiso 1 1 calc R . .
H16K H -0.0532 0.3789 0.3748 0.062 Uiso 1 1 calc R . .
C16G C 0.0528(11) 0.3942(3) 0.2907(9) 0.051(2) Uani 1 1 d DU . .
H16L H 0.0109 0.3934 0.2323 0.061 Uiso 1 1 calc R . .
H16M H 0.0979 0.4117 0.2902 0.061 Uiso 1 1 calc R . .
N16 N 0.1835(10) 0.3669(3) 0.2166(8) 0.048(3) Uani 1 1 d U . .
H16A H 0.2278 0.3514 0.2206 0.071 Uiso 1 1 calc R . .
H16B H 0.2216 0.3836 0.2129 0.071 Uiso 1 1 calc R . .
H16C H 0.1384 0.3652 0.1668 0.071 Uiso 1 1 calc R . .
C17A C 0.4464(10) 0.0749(4) -0.4714(9) 0.054(2) Uani 1 1 d DU . .
H17 H 0.4568 0.0533 -0.4685 0.065 Uiso 1 1 calc R . .
C17B C 0.3383(11) 0.0796(4) -0.5120(9) 0.055(2) Uani 1 1 d DU . .
H17L H 0.2925 0.0656 -0.4832 0.066 Uiso 1 1 calc R . .
H17M H 0.317 0.0992 -0.4933 0.066 Uiso 1 1 calc R . .
C17C C 0.3117(12) 0.0776(4) -0.6086(9) 0.057(2) Uani 1 1 d DU . .
H17J H 0.2345 0.0754 -0.6181 0.069 Uiso 1 1 calc R . .
H17K H 0.3432 0.0595 -0.63 0.069 Uiso 1 1 calc R . .
C17D C 0.3435(12) 0.1019(4) -0.6676(11) 0.065(3) Uani 1 1 d DU . .
H17H H 0.3196 0.0968 -0.7302 0.078 Uiso 1 1 calc R . .
H17I H 0.3041 0.1195 -0.6518 0.078 Uiso 1 1 calc R . .
C17E C 0.4573(11) 0.1099(4) -0.6658(10) 0.067(3) Uani 1 1 d DU . .
H17F H 0.4601 0.13 -0.6891 0.081 Uiso 1 1 calc R . .
H17G H 0.4888 0.0973 -0.7101 0.081 Uiso 1 1 calc R . .
C17F C 0.5296(13) 0.1090(4) -0.5821(10) 0.069(3) Uani 1 1 d DU . .
H17D H 0.6013 0.1109 -0.6024 0.082 Uiso 1 1 calc R . .
H17E H 0.516 0.1271 -0.5495 0.082 Uiso 1 1 calc R . .
C17G C 0.5370(11) 0.0868(4) -0.5158(10) 0.062(2) Uani 1 1 d DU . .
H17N H 0.5874 0.0939 -0.4671 0.074 Uiso 1 1 calc R . .
H17O H 0.571 0.07 -0.5432 0.074 Uiso 1 1 calc R . .
N17 N 0.4548(10) 0.0858(3) -0.3732(8) 0.044(3) Uani 1 1 d U . .
H17A H 0.5216 0.0831 -0.3487 0.067 Uiso 1 1 calc R . .
H17B H 0.4094 0.0756 -0.3411 0.067 Uiso 1 1 calc R . .
H17C H 0.4384 0.105 -0.3721 0.067 Uiso 1 1 calc R . .
O1 O 0.8380(7) 0.3071(2) -0.0378(6) 0.037(2) Uani 1 1 d . . .
H1AA H 0.7734 0.3116 -0.0382 0.044 Uiso 1 1 d R . .
H1AB H 0.883 0.3207 -0.0335 0.044 Uiso 1 1 d R . .
O2 O 0.8765(8) -0.0104(2) -0.3185(7) 0.046(3) Uani 1 1 d D . .
H2AA H 0.8302 -0.0218 -0.3429 0.055 Uiso 1 1 d RD . .
H2AB H 0.9413 -0.0145 -0.32 0.055 Uiso 1 1 d RD . .
Pb1 Pb 0.16170(4) 0.028922(12) -0.26790(5) 0.03804(16) Uani 1 1 d U . .
Pb2 Pb 0.54726(4) -0.015688(12) -0.37747(4) 0.02683(13) Uani 1 1 d U . .
Pb3 Pb 0.76903(4) 0.089429(11) -0.21904(4) 0.02503(13) Uani 1 1 d U . .
Pb4 Pb 0.35880(5) 0.148808(14) -0.18214(4) 0.02635(11) Uani 1 1 d U . .
Pb5 Pb -0.05260(4) 0.208352(11) -0.14735(4) 0.02487(13) Uani 1 1 d U . .
Pb6 Pb 0.16953(4) 0.313471(12) 0.00236(4) 0.02943(14) Uani 1 1 d U . .
Pb7 Pb 0.55505(4) 0.268849(12) -0.10338(4) 0.03145(14) Uani 1 1 d U . .
Cl1 Cl 0.1894(4) 0.00285(10) -0.0988(3) 0.0582(11) Uani 1 1 d U . .
Cl2 Cl 0.1052(3) 0.04267(9) -0.4599(3) 0.0487(9) Uani 1 1 d U . .
Cl3 Cl 0.5888(3) -0.02841(8) -0.1813(3) 0.0386(8) Uani 1 1 d U . .
Cl4 Cl 0.4985(3) 0.00264(9) -0.5529(3) 0.0400(8) Uani 1 1 d U . .
Cl5 Cl 0.7573(3) 0.05954(9) -0.0525(3) 0.0450(9) Uani 1 1 d U . .
Cl6 Cl 0.7929(3) 0.10700(9) -0.3982(3) 0.0402(8) Uani 1 1 d U . .
Cl7 Cl 0.3187(3) 0.14243(9) 0.0043(3) 0.0441(9) Uani 1 1 d U . .
Cl8 Cl 0.3977(3) 0.15563(8) -0.3679(3) 0.0398(8) Uani 1 1 d U . .
Cl9 Cl -0.0744(3) 0.19034(8) 0.0311(3) 0.0366(8) Uani 1 1 d U . .
Cl10 Cl -0.0382(3) 0.23958(8) -0.3126(3) 0.0402(8) Uani 1 1 d U . .
Cl11 Cl 0.2289(3) 0.29802(8) 0.1925(3) 0.0356(7) Uani 1 1 d U . .
Cl12 Cl 0.1285(3) 0.33253(9) -0.1771(3) 0.0492(9) Uani 1 1 d U . .
Cl13 Cl 0.6080(3) 0.25260(8) 0.0831(3) 0.0405(8) Uani 1 1 d U . .
Cl14 Cl 0.5219(4) 0.29677(10) -0.2696(3) 0.0523(10) Uani 1 1 d U . .
Cl15 Cl 0.1203(3) -0.02567(8) -0.3271(3) 0.0423(9) Uani 1 1 d U . .
Cl16 Cl 0.3692(3) 0.02183(8) -0.3024(3) 0.0342(7) Uani 1 1 d U . .
Cl17 Cl 0.4008(3) -0.05740(8) -0.3922(3) 0.0368(8) Uani 1 1 d U . .
Cl18 Cl 0.7065(3) -0.05222(8) -0.4111(3) 0.0426(9) Uani 1 1 d U . .
Cl19 Cl 0.6581(3) 0.04443(8) -0.3013(3) 0.0331(7) Uani 1 1 d U . .
Cl20 Cl 0.9593(3) 0.06163(10) -0.2323(3) 0.0452(10) Uani 1 1 d U . .
Cl21 Cl 0.5594(3) 0.11858(9) -0.1818(3) 0.0372(8) Uani 1 1 d U . .
Cl22 Cl 0.2498(3) 0.09456(8) -0.2290(3) 0.0416(8) Uani 1 1 d U . .
Cl23 Cl 0.4636(3) 0.20395(9) -0.1373(3) 0.0438(8) Uani 1 1 d U . .
Cl24 Cl 0.1568(3) 0.17873(9) -0.1814(3) 0.0391(8) Uani 1 1 d U . .
Cl25 Cl -0.1440(4) 0.14953(10) -0.1838(3) 0.0461(8) Uani 1 1 d U . .
Cl26 Cl -0.2406(3) 0.23682(10) -0.1335(3) 0.0436(9) Uani 1 1 d U . .
Cl27 Cl 0.0589(3) 0.25439(8) -0.0642(3) 0.0362(7) Uani 1 1 d U . .
Cl28 Cl 0.0115(3) 0.34634(9) 0.0625(3) 0.0441(9) Uani 1 1 d U . .
Cl29 Cl 0.3126(3) 0.35584(8) 0.0295(2) 0.0335(7) Uani 1 1 d U . .
Cl30 Cl 0.3486(3) 0.27678(8) -0.0656(3) 0.0364(7) Uani 1 1 d U . .
Cl31 Cl 0.5955(3) 0.32374(8) -0.0397(3) 0.0360(8) Uani 1 1 d U . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1A C1B 1.499(5) . ?
C1A C1G 1.501(5) . ?
C1A N1 1.541(19) . ?
C1A H1 1 . ?
C1B C1C 1.502(5) . ?
C1B H1B1 0.99 . ?
C1B H1B2 0.99 . ?
C1C C1D 1.502(5) . ?
C1C H1C1 0.99 . ?
C1C H1C2 0.99 . ?
C1D C1E 1.500(5) . ?
C1D H1D1 0.99 . ?
C1D H1D2 0.99 . ?
C1E C1F 1.500(5) . ?
C1E H1E1 0.99 . ?
C1E H1E2 0.99 . ?
C1F C1G 1.499(5) . ?
C1F H1F1 0.99 . ?
C1F H1F2 0.99 . ?
C1G H1G1 0.99 . ?
C1G H1G2 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
C2A N2 1.486(19) . ?
C2A C2B 1.498(12) . ?
C2A C2G 1.503(13) . ?
C2A H2 1 . ?
C2B C2C 1.450(13) . ?
C2B H2B1 0.99 . ?
C2B H2B2 0.99 . ?
C2C C2D 1.522(13) . ?
C2C H2C1 0.99 . ?
C2C H2C2 0.99 . ?
C2D C2E 1.507(12) . ?
C2D H2D1 0.99 . ?
C2D H2D2 0.99 . ?
C2E C2F 1.520(12) . ?
C2E H2E1 0.99 . ?
C2E H2E2 0.99 . ?
C2F C2G 1.531(13) . ?
C2F H2F1 0.99 . ?
C2F H2F2 0.99 . ?
C2G H2G1 0.99 . ?
C2G H2G2 0.99 . ?
N2 H2A 0.91 . ?
N2 H2B 0.91 . ?
N2 H2C 0.91 . ?
C3A C3B 1.505(13) . ?
C3A C3G 1.508(13) . ?
C3A N3 1.527(17) . ?
C3A H3 1 . ?
C3B C3C 1.483(12) . ?
C3B H3B1 0.99 . ?
C3B H3B2 0.99 . ?
C3C C3D 1.464(13) . ?
C3C H3C1 0.99 . ?
C3C H3C2 0.99 . ?
C3D C3E 1.482(13) . ?
C3D H3D1 0.99 . ?
C3D H3D2 0.99 . ?
C3E C3F 1.528(13) . ?
C3E H3E1 0.99 . ?
C3E H3E2 0.99 . ?
C3F C3G 1.503(13) . ?
C3F H3F1 0.99 . ?
C3F H3F2 0.99 . ?
C3G H3G1 0.99 . ?
C3G H3G2 0.99 . ?
N3 H3A 0.91 . ?
N3 H3B 0.91 . ?
N3 H3C 0.91 . ?
C4A C4G 1.477(13) . ?
C4A C4B 1.481(13) . ?
C4A N4 1.51(2) . ?
C4A H4 1 . ?
C4B C4C 1.476(13) . ?
C4B H4B1 0.99 . ?
C4B H4B2 0.99 . ?
C4C C4D 1.535(13) . ?
C4C H4C1 0.99 . ?
C4C H4C2 0.99 . ?
C4D C4E 1.487(13) . ?
C4D H4D1 0.99 . ?
C4D H4D2 0.99 . ?
C4E C4F 1.506(13) . ?
C4E H4E1 0.99 . ?
C4E H4E2 0.99 . ?
C4F C4G 1.496(13) . ?
C4F H4F1 0.99 . ?
C4F H4F2 0.99 . ?
C4G H4G1 0.99 . ?
C4G H4G2 0.99 . ?
N4 H4A 0.91 . ?
N4 H4B 0.91 . ?
N4 H4C 0.91 . ?
C5A C5B 1.483(12) . ?
C5A N5 1.495(19) . ?
C5A C5G 1.512(12) . ?
C5A H5 1 . ?
C5B C5C 1.507(13) . ?
C5B H5B1 0.99 . ?
C5B H5B2 0.99 . ?
C5C C5D 1.491(13) . ?
C5C H5C1 0.99 . ?
C5C H5C2 0.99 . ?
C5D C5E 1.482(12) . ?
C5D H5D1 0.99 . ?
C5D H5D2 0.99 . ?
C5E C5F 1.513(13) . ?
C5E H5E1 0.99 . ?
C5E H5E2 0.99 . ?
C5F C5G 1.492(13) . ?
C5F H5F1 0.99 . ?
C5F H5F2 0.99 . ?
C5G H5G1 0.99 . ?
C5G H5G2 0.99 . ?
N5 H5A 0.91 . ?
N5 H5B 0.91 . ?
N5 H5C 0.91 . ?
C6A C6G 1.478(13) . ?
C6A C6B 1.481(13) . ?
C6A N6 1.50(2) . ?
C6A H6 1 . ?
C6B C6C 1.491(13) . ?
C6B H6B1 0.99 . ?
C6B H6B2 0.99 . ?
C6C C6D 1.527(13) . ?
C6C H6C1 0.99 . ?
C6C H6C2 0.99 . ?
C6D C6E 1.492(13) . ?
C6D H6D1 0.99 . ?
C6D H6D2 0.99 . ?
C6E C6F 1.528(13) . ?
C6E H6E1 0.99 . ?
C6E H6E2 0.99 . ?
C6F C6G 1.509(13) . ?
C6F H6F1 0.99 . ?
C6F H6F2 0.99 . ?
C6G H6G1 0.99 . ?
C6G H6G2 0.99 . ?
N6 H6A 0.91 . ?
N6 H6B 0.91 . ?
N6 H6C 0.91 . ?
C7A N7 1.47(2) . ?
C7A C7B 1.489(13) . ?
C7A C7G 1.494(13) . ?
C7A H7 1 . ?
C7B C7C 1.507(13) . ?
C7B H7B1 0.99 . ?
C7B H7B2 0.99 . ?
C7C C7D 1.495(13) . ?
C7C H7C1 0.99 . ?
C7C H7C2 0.99 . ?
C7D C7E 1.473(13) . ?
C7D H7D1 0.99 . ?
C7D H7D2 0.99 . ?
C7E C7F 1.496(13) . ?
C7E H7E1 0.99 . ?
C7E H7E2 0.99 . ?
C7F C7G 1.443(13) . ?
C7F H7F1 0.99 . ?
C7F H7F2 0.99 . ?
C7G H7G1 0.99 . ?
C7G H7G2 0.99 . ?
N7 H7A 0.91 . ?
N7 H7B 0.91 . ?
N7 H7C 0.91 . ?
C8A C8G 1.510(12) . ?
C8A N8 1.511(17) . ?
C8A C8B 1.513(12) . ?
C8A H8 1 . ?
C8B C8C 1.510(12) . ?
C8B H8B1 0.99 . ?
C8B H8B2 0.99 . ?
C8C C8D 1.503(12) . ?
C8C H8C1 0.99 . ?
C8C H8C2 0.99 . ?
C8D C8E 1.526(12) . ?
C8D H8D1 0.99 . ?
C8D H8D2 0.99 . ?
C8E C8F 1.534(12) . ?
C8E H8E1 0.99 . ?
C8E H8E2 0.99 . ?
C8F C8G 1.506(12) . ?
C8F H8F1 0.99 . ?
C8F H8F2 0.99 . ?
C8G H8G1 0.99 . ?
C8G H8G2 0.99 . ?
N8 H8A 0.91 . ?
N8 H8B 0.91 . ?
N8 H8C 0.91 . ?
C9A C9B 1.491(12) . ?
C9A C9G 1.526(12) . ?
C9A N9 1.556(18) . ?
C9A H9 1 . ?
C9B C9C 1.504(13) . ?
C9B H9B1 0.99 . ?
C9B H9B2 0.99 . ?
C9C C9D 1.521(12) . ?
C9C H9C1 0.99 . ?
C9C H9C2 0.99 . ?
C9D C9E 1.506(12) . ?
C9D H9D1 0.99 . ?
C9D H9D2 0.99 . ?
C9E C9F 1.511(13) . ?
C9E H9E1 0.99 . ?
C9E H9E2 0.99 . ?
C9F C9G 1.491(12) . ?
C9F H9F1 0.99 . ?
C9F H9F2 0.99 . ?
C9G H9G1 0.99 . ?
C9G H9G2 0.99 . ?
N9 H9A 0.91 . ?
N9 H9B 0.91 . ?
N9 H9C 0.91 . ?
N10 C10A 1.4058 . ?
N10 H10A 0.91 . ?
N10 H10B 0.91 . ?
N10 H10C 0.91 . ?
C10A C10B 1.473(9) . ?
C10A C10G 1.502(9) . ?
C10A H10 1 . ?
C10B C10C 1.490(9) . ?
C10B H10N 0.99 . ?
C10B H10O 0.99 . ?
C10C C10D 1.497(10) . ?
C10C H10D 0.99 . ?
C10C H10E 0.99 . ?
C10D C10E 1.474(10) . ?
C10D H10F 0.99 . ?
C10D H10G 0.99 . ?
C10E C10F 1.474(10) . ?
C10E H10H 0.99 . ?
C10E H10I 0.99 . ?
C10F C10G 1.481(10) . ?
C10F H10J 0.99 . ?
C10F H10K 0.99 . ?
C10G H10L 0.99 . ?
C10G H10M 0.99 . ?
C11A C11G 1.504(13) . ?
C11A C11B 1.512(13) . ?
C11A N11 1.538(18) . ?
C11A H11 1 . ?
C11B C11C 1.496(13) . ?
C11B H11N 0.99 . ?
C11B H11O 0.99 . ?
C11C C11D 1.496(13) . ?
C11C H11D 0.99 . ?
C11C H11E 0.99 . ?
C11D C11E 1.471(13) . ?
C11D H11F 0.99 . ?
C11D H11G 0.99 . ?
C11E C11F 1.516(13) . ?
C11E H11H 0.99 . ?
C11E H11I 0.99 . ?
C11F C11G 1.514(13) . ?
C11F H11J 0.99 . ?
C11F H11K 0.99 . ?
C11G H11L 0.99 . ?
C11G H11M 0.99 . ?
N11 H11A 0.91 . ?
N11 H11B 0.91 . ?
N11 H11C 0.91 . ?
C12A C12B 1.463(13) . ?
C12A C12G 1.517(13) . ?
C12A N12 1.53(2) . ?
C12A H12 1 . ?
C12B C12C 1.484(13) . ?
C12B H12N 0.99 . ?
C12B H12O 0.99 . ?
C12C C12D 1.503(14) . ?
C12C H12D 0.99 . ?
C12C H12E 0.99 . ?
C12D C12E 1.496(13) . ?
C12D H12F 0.99 . ?
C12D H12G 0.99 . ?
C12E C12F 1.480(13) . ?
C12E H12H 0.99 . ?
C12E H12I 0.99 . ?
C12F C12G 1.518(14) . ?
C12F H12J 0.99 . ?
C12F H12K 0.99 . ?
C12G H12L 0.99 . ?
C12G H12M 0.99 . ?
N12 H12A 0.91 . ?
N12 H12B 0.91 . ?
N12 H12C 0.91 . ?
C13A N13 1.481(19) . ?
C13A C13G 1.498(13) . ?
C13A C13B 1.521(13) . ?
C13A H13 1 . ?
C13B C13C 1.517(13) . ?
C13B H13N 0.99 . ?
C13B H13O 0.99 . ?
C13C C13D 1.517(13) . ?
C13C H13D 0.99 . ?
C13C H13E 0.99 . ?
C13D C13E 1.475(13) . ?
C13D H13F 0.99 . ?
C13D H13G 0.99 . ?
C13E C13F 1.504(13) . ?
C13E H13H 0.99 . ?
C13E H13I 0.99 . ?
C13F C13G 1.477(13) . ?
C13F H13J 0.99 . ?
C13F H13K 0.99 . ?
C13G H13L 0.99 . ?
C13G H13M 0.99 . ?
N13 H13A 0.91 . ?
N13 H13B 0.91 . ?
N13 H13C 0.91 . ?
C14A C14B 1.469(13) . ?
C14A N14 1.48(2) . ?
C14A C14G 1.485(13) . ?
C14A H14 1 . ?
C14B C14C 1.498(13) . ?
C14B H14N 0.99 . ?
C14B H14O 0.99 . ?
C14C C14D 1.515(13) . ?
C14C H14D 0.99 . ?
C14C H14E 0.99 . ?
C14D C14E 1.503(13) . ?
C14D H14F 0.99 . ?
C14D H14G 0.99 . ?
C14E C14F 1.517(13) . ?
C14E H14H 0.99 . ?
C14E H14I 0.99 . ?
C14F C14G 1.536(13) . ?
C14F H14J 0.99 . ?
C14F H14K 0.99 . ?
C14G H14L 0.99 . ?
C14G H14M 0.99 . ?
N14 H14A 0.91 . ?
N14 H14B 0.91 . ?
N14 H14C 0.91 . ?
C15A C15B 1.492(13) . ?
C15A C15G 1.498(13) . ?
C15A N15 1.53(2) . ?
C15A H15 1 . ?
C15B C15C 1.514(13) . ?
C15B H15N 0.99 . ?
C15B H15O 0.99 . ?
C15C C15D 1.512(13) . ?
C15C H15D 0.99 . ?
C15C H15E 0.99 . ?
C15D C15E 1.487(13) . ?
C15D H15F 0.99 . ?
C15D H15G 0.99 . ?
C15E C15F 1.532(13) . ?
C15E H15H 0.99 . ?
C15E H15I 0.99 . ?
C15F C15G 1.487(13) . ?
C15F H15J 0.99 . ?
C15F H15K 0.99 . ?
C15G H15L 0.99 . ?
C15G H15M 0.99 . ?
N15 H15A 0.91 . ?
N15 H15B 0.91 . ?
N15 H15C 0.91 . ?
C16A C16G 1.496(12) . ?
C16A C16B 1.499(12) . ?
C16A N16 1.499(17) . ?
C16A H16 1 . ?
C16B C16C 1.509(13) . ?
C16B H16N 0.99 . ?
C16B H16O 0.99 . ?
C16C C16D 1.509(12) . ?
C16C H16D 0.99 . ?
C16C H16E 0.99 . ?
C16D C16E 1.503(12) . ?
C16D H16F 0.99 . ?
C16D H16G 0.99 . ?
C16E C16F 1.494(12) . ?
C16E H16H 0.99 . ?
C16E H16I 0.99 . ?
C16F C16G 1.499(12) . ?
C16F H16J 0.99 . ?
C16F H16K 0.99 . ?
C16G H16L 0.99 . ?
C16G H16M 0.99 . ?
N16 H16A 0.91 . ?
N16 H16B 0.91 . ?
N16 H16C 0.91 . ?
C17A C17B 1.481(12) . ?
C17A C17G 1.481(12) . ?
C17A N17 1.550(19) . ?
C17A H17 1 . ?
C17B C17C 1.463(12) . ?
C17B H17L 0.99 . ?
C17B H17M 0.99 . ?
C17C C17D 1.499(13) . ?
C17C H17J 0.99 . ?
C17C H17K 0.99 . ?
C17D C17E 1.498(13) . ?
C17D H17H 0.99 . ?
C17D H17I 0.99 . ?
C17E C17F 1.498(13) . ?
C17E H17F 0.99 . ?
C17E H17G 0.99 . ?
C17F C17G 1.423(13) . ?
C17F H17D 0.99 . ?
C17F H17E 0.99 . ?
C17G H17N 0.99 . ?
C17G H17O 0.99 . ?
N17 H17A 0.91 . ?
N17 H17B 0.91 . ?
N17 H17C 0.91 . ?
O1 H1AA 0.8499 . ?
O1 H1AB 0.8501 . ?
O2 H2AA 0.8497 . ?
O2 H2AB 0.8498 . ?
Pb1 Cl15 2.704(4) . ?
Pb1 Cl16 2.756(3) . ?
Pb1 Cl1 2.798(5) . ?
Pb1 Cl2 2.976(5) . ?
Pb1 Cl20 3.073(4) 1_455 ?
Pb1 Cl22 3.261(4) . ?
Pb2 Cl17 2.678(4) . ?
Pb2 Cl18 2.715(3) . ?
Pb2 Cl4 2.781(4) . ?
Pb2 Cl3 2.999(4) . ?
Pb2 Cl16 3.131(3) . ?
Pb2 Cl19 3.273(4) . ?
Pb3 Cl19 2.747(4) . ?
Pb3 Cl20 2.766(4) . ?
Pb3 Cl6 2.838(4) . ?
Pb3 Cl5 2.860(4) . ?
Pb3 Cl25 3.013(5) 1_655 ?
Pb3 Cl21 3.082(4) . ?
Pb4 Cl8 2.877(4) . ?
Pb4 Cl7 2.888(4) . ?
Pb4 Cl21 2.915(4) . ?
Pb4 Cl22 2.919(4) . ?
Pb4 Cl23 2.924(4) . ?
Pb4 Cl24 2.924(4) . ?
Pb5 Cl26 2.756(4) . ?
Pb5 Cl27 2.793(4) . ?
Pb5 Cl9 2.829(4) . ?
Pb5 Cl10 2.877(4) . ?
Pb5 Cl25 2.983(4) . ?
Pb5 Cl24 3.078(4) . ?
Pb6 Cl29 2.682(3) . ?
Pb6 Cl28 2.729(4) . ?
Pb6 Cl12 2.834(4) . ?
Pb6 Cl11 2.974(4) . ?
Pb6 Cl30 3.077(3) . ?
Pb6 Cl27 3.189(4) . ?
Pb7 Cl31 2.736(4) . ?
Pb7 Cl30 2.762(3) . ?
Pb7 Cl14 2.802(4) . ?
Pb7 Cl13 2.917(4) . ?
Pb7 Cl26 3.060(4) 1_655 ?
Pb7 Cl23 3.234(4) . ?
Cl20 Pb1 3.073(4) 1_655 ?
Cl25 Pb3 3.013(5) 1_455 ?
Cl26 Pb7 3.060(4) 1_455 ?

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
C1B C1A C1G 116.2(10) . . ?
C1B C1A N1 107.1(11) . . ?
C1G C1A N1 106.8(12) . . ?
C1B C1A H1 108.8 . . ?
C1G C1A H1 108.8 . . ?
N1 C1A H1 108.8 . . ?
C1A C1B C1C 116.6(11) . . ?
C1A C1B H1B1 108.2 . . ?
C1C C1B H1B1 108.2 . . ?
C1A C1B H1B2 108.2 . . ?
C1C C1B H1B2 108.2 . . ?
H1B1 C1B H1B2 107.3 . . ?
C1D C1C C1B 113.7(11) . . ?
C1D C1C H1C1 108.8 . . ?
C1B C1C H1C1 108.8 . . ?
C1D C1C H1C2 108.8 . . ?
C1B C1C H1C2 108.8 . . ?
H1C1 C1C H1C2 107.7 . . ?
C1E C1D C1C 119.3(12) . . ?
C1E C1D H1D1 107.5 . . ?
C1C C1D H1D1 107.5 . . ?
C1E C1D H1D2 107.5 . . ?
C1C C1D H1D2 107.5 . . ?
H1D1 C1D H1D2 107 . . ?
C1D C1E C1F 116.3(11) . . ?
C1D C1E H1E1 108.2 . . ?
C1F C1E H1E1 108.2 . . ?
C1D C1E H1E2 108.2 . . ?
C1F C1E H1E2 108.2 . . ?
H1E1 C1E H1E2 107.4 . . ?
C1G C1F C1E 116.2(12) . . ?
C1G C1F H1F1 108.2 . . ?
C1E C1F H1F1 108.2 . . ?
C1G C1F H1F2 108.2 . . ?
C1E C1F H1F2 108.2 . . ?
H1F1 C1F H1F2 107.4 . . ?
C1F C1G C1A 118.1(11) . . ?
C1F C1G H1G1 107.8 . . ?
C1A C1G H1G1 107.8 . . ?
C1F C1G H1G2 107.8 . . ?
C1A C1G H1G2 107.8 . . ?
H1G1 C1G H1G2 107.1 . . ?
C1A N1 H1A 109.5 . . ?
C1A N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1A N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N2 C2A C2B 111.9(13) . . ?
N2 C2A C2G 105.3(12) . . ?
C2B C2A C2G 117.8(11) . . ?
N2 C2A H2 107.1 . . ?
C2B C2A H2 107.1 . . ?
C2G C2A H2 107.1 . . ?
C2C C2B C2A 116.9(12) . . ?
C2C C2B H2B1 108.1 . . ?
C2A C2B H2B1 108.1 . . ?
C2C C2B H2B2 108.1 . . ?
C2A C2B H2B2 108.1 . . ?
H2B1 C2B H2B2 107.3 . . ?
C2B C2C C2D 119.7(14) . . ?
C2B C2C H2C1 107.4 . . ?
C2D C2C H2C1 107.4 . . ?
C2B C2C H2C2 107.4 . . ?
C2D C2C H2C2 107.4 . . ?
H2C1 C2C H2C2 106.9 . . ?
C2E C2D C2C 117.4(12) . . ?
C2E C2D H2D1 107.9 . . ?
C2C C2D H2D1 107.9 . . ?
C2E C2D H2D2 107.9 . . ?
C2C C2D H2D2 107.9 . . ?
H2D1 C2D H2D2 107.2 . . ?
C2D C2E C2F 115.3(12) . . ?
C2D C2E H2E1 108.4 . . ?
C2F C2E H2E1 108.4 . . ?
C2D C2E H2E2 108.4 . . ?
C2F C2E H2E2 108.4 . . ?
H2E1 C2E H2E2 107.5 . . ?
C2E C2F C2G 113.8(12) . . ?
C2E C2F H2F1 108.8 . . ?
C2G C2F H2F1 108.8 . . ?
C2E C2F H2F2 108.8 . . ?
C2G C2F H2F2 108.8 . . ?
H2F1 C2F H2F2 107.7 . . ?
C2A C2G C2F 112.6(11) . . ?
C2A C2G H2G1 109.1 . . ?
C2F C2G H2G1 109.1 . . ?
C2A C2G H2G2 109.1 . . ?
C2F C2G H2G2 109.1 . . ?
H2G1 C2G H2G2 107.8 . . ?
C2A N2 H2A 109.5 . . ?
C2A N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C2A N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C3B C3A C3G 114.1(13) . . ?
C3B C3A N3 105.1(11) . . ?
C3G C3A N3 107.7(11) . . ?
C3B C3A H3 109.9 . . ?
C3G C3A H3 109.9 . . ?
N3 C3A H3 109.9 . . ?
C3C C3B C3A 116.3(12) . . ?
C3C C3B H3B1 108.2 . . ?
C3A C3B H3B1 108.2 . . ?
C3C C3B H3B2 108.2 . . ?
C3A C3B H3B2 108.2 . . ?
H3B1 C3B H3B2 107.4 . . ?
C3D C3C C3B 121.4(12) . . ?
C3D C3C H3C1 107 . . ?
C3B C3C H3C1 107 . . ?
C3D C3C H3C2 107 . . ?
C3B C3C H3C2 107 . . ?
H3C1 C3C H3C2 106.7 . . ?
C3C C3D C3E 122.5(13) . . ?
C3C C3D H3D1 106.7 . . ?
C3E C3D H3D1 106.7 . . ?
C3C C3D H3D2 106.7 . . ?
C3E C3D H3D2 106.7 . . ?
H3D1 C3D H3D2 106.6 . . ?
C3D C3E C3F 108.9(13) . . ?
C3D C3E H3E1 109.9 . . ?
C3F C3E H3E1 109.9 . . ?
C3D C3E H3E2 109.9 . . ?
C3F C3E H3E2 109.9 . . ?
H3E1 C3E H3E2 108.3 . . ?
C3G C3F C3E 113.0(13) . . ?
C3G C3F H3F1 109 . . ?
C3E C3F H3F1 109 . . ?
C3G C3F H3F2 109 . . ?
C3E C3F H3F2 109 . . ?
H3F1 C3F H3F2 107.8 . . ?
C3F C3G C3A 117.0(12) . . ?
C3F C3G H3G1 108 . . ?
C3A C3G H3G1 108 . . ?
C3F C3G H3G2 108 . . ?
C3A C3G H3G2 108 . . ?
H3G1 C3G H3G2 107.3 . . ?
C3A N3 H3A 109.5 . . ?
C3A N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C3A N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C4G C4A C4B 116.9(12) . . ?
C4G C4A N4 115.0(14) . . ?
C4B C4A N4 104.4(14) . . ?
C4G C4A H4 106.6 . . ?
C4B C4A H4 106.6 . . ?
N4 C4A H4 106.6 . . ?
C4C C4B C4A 116.3(14) . . ?
C4C C4B H4B1 108.2 . . ?
C4A C4B H4B1 108.2 . . ?
C4C C4B H4B2 108.2 . . ?
C4A C4B H4B2 108.2 . . ?
H4B1 C4B H4B2 107.4 . . ?
C4B C4C C4D 110.7(13) . . ?
C4B C4C H4C1 109.5 . . ?
C4D C4C H4C1 109.5 . . ?
C4B C4C H4C2 109.5 . . ?
C4D C4C H4C2 109.5 . . ?
H4C1 C4C H4C2 108.1 . . ?
C4E C4D C4C 113.2(13) . . ?
C4E C4D H4D1 108.9 . . ?
C4C C4D H4D1 108.9 . . ?
C4E C4D H4D2 108.9 . . ?
C4C C4D H4D2 108.9 . . ?
H4D1 C4D H4D2 107.8 . . ?
C4D C4E C4F 117.4(14) . . ?
C4D C4E H4E1 108 . . ?
C4F C4E H4E1 108 . . ?
C4D C4E H4E2 108 . . ?
C4F C4E H4E2 108 . . ?
H4E1 C4E H4E2 107.2 . . ?
C4G C4F C4E 116.3(14) . . ?
C4G C4F H4F1 108.2 . . ?
C4E C4F H4F1 108.2 . . ?
C4G C4F H4F2 108.2 . . ?
C4E C4F H4F2 108.2 . . ?
H4F1 C4F H4F2 107.4 . . ?
C4A C4G C4F 116.7(13) . . ?
C4A C4G H4G1 108.1 . . ?
C4F C4G H4G1 108.1 . . ?
C4A C4G H4G2 108.1 . . ?
C4F C4G H4G2 108.1 . . ?
H4G1 C4G H4G2 107.3 . . ?
C4A N4 H4A 109.5 . . ?
C4A N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4A N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C5B C5A N5 110.9(12) . . ?
C5B C5A C5G 117.6(11) . . ?
N5 C5A C5G 111.1(12) . . ?
C5B C5A H5 105.4 . . ?
N5 C5A H5 105.4 . . ?
C5G C5A H5 105.4 . . ?
C5A C5B C5C 117.0(12) . . ?
C5A C5B H5B1 108.1 . . ?
C5C C5B H5B1 108.1 . . ?
C5A C5B H5B2 108.1 . . ?
C5C C5B H5B2 108.1 . . ?
H5B1 C5B H5B2 107.3 . . ?
C5D C5C C5B 115.4(12) . . ?
C5D C5C H5C1 108.4 . . ?
C5B C5C H5C1 108.4 . . ?
C5D C5C H5C2 108.4 . . ?
C5B C5C H5C2 108.4 . . ?
H5C1 C5C H5C2 107.5 . . ?
C5E C5D C5C 120.4(13) . . ?
C5E C5D H5D1 107.2 . . ?
C5C C5D H5D1 107.2 . . ?
C5E C5D H5D2 107.2 . . ?
C5C C5D H5D2 107.2 . . ?
H5D1 C5D H5D2 106.8 . . ?
C5D C5E C5F 114.7(12) . . ?
C5D C5E H5E1 108.6 . . ?
C5F C5E H5E1 108.6 . . ?
C5D C5E H5E2 108.6 . . ?
C5F C5E H5E2 108.6 . . ?
H5E1 C5E H5E2 107.6 . . ?
C5G C5F C5E 114.0(12) . . ?
C5G C5F H5F1 108.7 . . ?
C5E C5F H5F1 108.7 . . ?
C5G C5F H5F2 108.7 . . ?
C5E C5F H5F2 108.7 . . ?
H5F1 C5F H5F2 107.6 . . ?
C5F C5G C5A 116.1(12) . . ?
C5F C5G H5G1 108.3 . . ?
C5A C5G H5G1 108.3 . . ?
C5F C5G H5G2 108.3 . . ?
C5A C5G H5G2 108.3 . . ?
H5G1 C5G H5G2 107.4 . . ?
C5A N5 H5A 109.5 . . ?
C5A N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C5A N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C6G C6A C6B 121.1(13) . . ?
C6G C6A N6 112.3(14) . . ?
C6B C6A N6 103.1(13) . . ?
C6G C6A H6 106.5 . . ?
C6B C6A H6 106.5 . . ?
N6 C6A H6 106.5 . . ?
C6A C6B C6C 115.3(13) . . ?
C6A C6B H6B1 108.5 . . ?
C6C C6B H6B1 108.5 . . ?
C6A C6B H6B2 108.5 . . ?
C6C C6B H6B2 108.5 . . ?
H6B1 C6B H6B2 107.5 . . ?
C6B C6C C6D 114.7(14) . . ?
C6B C6C H6C1 108.6 . . ?
C6D C6C H6C1 108.6 . . ?
C6B C6C H6C2 108.6 . . ?
C6D C6C H6C2 108.6 . . ?
H6C1 C6C H6C2 107.6 . . ?
C6E C6D C6C 117.5(13) . . ?
C6E C6D H6D1 107.9 . . ?
C6C C6D H6D1 107.9 . . ?
C6E C6D H6D2 107.9 . . ?
C6C C6D H6D2 107.9 . . ?
H6D1 C6D H6D2 107.2 . . ?
C6D C6E C6F 117.0(13) . . ?
C6D C6E H6E1 108.1 . . ?
C6F C6E H6E1 108.1 . . ?
C6D C6E H6E2 108.1 . . ?
C6F C6E H6E2 108.1 . . ?
H6E1 C6E H6E2 107.3 . . ?
C6G C6F C6E 113.5(13) . . ?
C6G C6F H6F1 108.9 . . ?
C6E C6F H6F1 108.9 . . ?
C6G C6F H6F2 108.9 . . ?
C6E C6F H6F2 108.9 . . ?
H6F1 C6F H6F2 107.7 . . ?
C6A C6G C6F 117.5(13) . . ?
C6A C6G H6G1 107.9 . . ?
C6F C6G H6G1 107.9 . . ?
C6A C6G H6G2 107.9 . . ?
C6F C6G H6G2 107.9 . . ?
H6G1 C6G H6G2 107.2 . . ?
C6A N6 H6A 109.5 . . ?
C6A N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C6A N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
N7 C7A C7B 108.7(14) . . ?
N7 C7A C7G 109.9(14) . . ?
C7B C7A C7G 116.8(15) . . ?
N7 C7A H7 107 . . ?
C7B C7A H7 107 . . ?
C7G C7A H7 107 . . ?
C7A C7B C7C 114.1(14) . . ?
C7A C7B H7B1 108.7 . . ?
C7C C7B H7B1 108.7 . . ?
C7A C7B H7B2 108.7 . . ?
C7C C7B H7B2 108.7 . . ?
H7B1 C7B H7B2 107.6 . . ?
C7D C7C C7B 116.3(15) . . ?
C7D C7C H7C1 108.2 . . ?
C7B C7C H7C1 108.2 . . ?
C7D C7C H7C2 108.2 . . ?
C7B C7C H7C2 108.2 . . ?
H7C1 C7C H7C2 107.4 . . ?
C7E C7D C7C 122.8(14) . . ?
C7E C7D H7D1 106.6 . . ?
C7C C7D H7D1 106.6 . . ?
C7E C7D H7D2 106.6 . . ?
C7C C7D H7D2 106.6 . . ?
H7D1 C7D H7D2 106.6 . . ?
C7D C7E C7F 120.3(14) . . ?
C7D C7E H7E1 107.3 . . ?
C7F C7E H7E1 107.3 . . ?
C7D C7E H7E2 107.3 . . ?
C7F C7E H7E2 107.3 . . ?
H7E1 C7E H7E2 106.9 . . ?
C7G C7F C7E 115.5(15) . . ?
C7G C7F H7F1 108.4 . . ?
C7E C7F H7F1 108.4 . . ?
C7G C7F H7F2 108.4 . . ?
C7E C7F H7F2 108.4 . . ?
H7F1 C7F H7F2 107.5 . . ?
C7F C7G C7A 120.4(15) . . ?
C7F C7G H7G1 107.2 . . ?
C7A C7G H7G1 107.2 . . ?
C7F C7G H7G2 107.2 . . ?
C7A C7G H7G2 107.2 . . ?
H7G1 C7G H7G2 106.9 . . ?
C7A N7 H7A 109.5 . . ?
C7A N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C7A N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C8G C8A N8 109.1(11) . . ?
C8G C8A C8B 116.5(10) . . ?
N8 C8A C8B 107.4(10) . . ?
C8G C8A H8 107.9 . . ?
N8 C8A H8 107.9 . . ?
C8B C8A H8 107.9 . . ?
C8C C8B C8A 114.8(11) . . ?
C8C C8B H8B1 108.6 . . ?
C8A C8B H8B1 108.6 . . ?
C8C C8B H8B2 108.6 . . ?
C8A C8B H8B2 108.6 . . ?
H8B1 C8B H8B2 107.5 . . ?
C8D C8C C8B 115.8(11) . . ?
C8D C8C H8C1 108.3 . . ?
C8B C8C H8C1 108.3 . . ?
C8D C8C H8C2 108.3 . . ?
C8B C8C H8C2 108.3 . . ?
H8C1 C8C H8C2 107.4 . . ?
C8C C8D C8E 117.8(11) . . ?
C8C C8D H8D1 107.9 . . ?
C8E C8D H8D1 107.9 . . ?
C8C C8D H8D2 107.9 . . ?
C8E C8D H8D2 107.9 . . ?
H8D1 C8D H8D2 107.2 . . ?
C8D C8E C8F 117.6(11) . . ?
C8D C8E H8E1 107.9 . . ?
C8F C8E H8E1 107.9 . . ?
C8D C8E H8E2 107.9 . . ?
C8F C8E H8E2 107.9 . . ?
H8E1 C8E H8E2 107.2 . . ?
C8G C8F C8E 112.8(11) . . ?
C8G C8F H8F1 109 . . ?
C8E C8F H8F1 109 . . ?
C8G C8F H8F2 109 . . ?
C8E C8F H8F2 109 . . ?
H8F1 C8F H8F2 107.8 . . ?
C8F C8G C8A 117.5(11) . . ?
C8F C8G H8G1 107.9 . . ?
C8A C8G H8G1 107.9 . . ?
C8F C8G H8G2 107.9 . . ?
C8A C8G H8G2 107.9 . . ?
H8G1 C8G H8G2 107.2 . . ?
C8A N8 H8A 109.5 . . ?
C8A N8 H8B 109.5 . . ?
H8A N8 H8B 109.5 . . ?
C8A N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C9B C9A C9G 114.7(11) . . ?
C9B C9A N9 108.8(12) . . ?
C9G C9A N9 105.4(11) . . ?
C9B C9A H9 109.3 . . ?
C9G C9A H9 109.3 . . ?
N9 C9A H9 109.3 . . ?
C9A C9B C9C 118.8(12) . . ?
C9A C9B H9B1 107.6 . . ?
C9C C9B H9B1 107.6 . . ?
C9A C9B H9B2 107.6 . . ?
C9C C9B H9B2 107.6 . . ?
H9B1 C9B H9B2 107 . . ?
C9B C9C C9D 114.2(12) . . ?
C9B C9C H9C1 108.7 . . ?
C9D C9C H9C1 108.7 . . ?
C9B C9C H9C2 108.7 . . ?
C9D C9C H9C2 108.7 . . ?
H9C1 C9C H9C2 107.6 . . ?
C9E C9D C9C 112.6(11) . . ?
C9E C9D H9D1 109.1 . . ?
C9C C9D H9D1 109.1 . . ?
C9E C9D H9D2 109.1 . . ?
C9C C9D H9D2 109.1 . . ?
H9D1 C9D H9D2 107.8 . . ?
C9D C9E C9F 114.7(12) . . ?
C9D C9E H9E1 108.6 . . ?
C9F C9E H9E1 108.6 . . ?
C9D C9E H9E2 108.6 . . ?
C9F C9E H9E2 108.6 . . ?
H9E1 C9E H9E2 107.6 . . ?
C9G C9F C9E 116.0(13) . . ?
C9G C9F H9F1 108.3 . . ?
C9E C9F H9F1 108.3 . . ?
C9G C9F H9F2 108.3 . . ?
C9E C9F H9F2 108.3 . . ?
H9F1 C9F H9F2 107.4 . . ?
C9F C9G C9A 115.4(11) . . ?
C9F C9G H9G1 108.4 . . ?
C9A C9G H9G1 108.4 . . ?
C9F C9G H9G2 108.4 . . ?
C9A C9G H9G2 108.4 . . ?
H9G1 C9G H9G2 107.5 . . ?
C9A N9 H9A 109.5 . . ?
C9A N9 H9B 109.5 . . ?
H9A N9 H9B 109.5 . . ?
C9A N9 H9C 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
C10A N10 H10A 109.5 . . ?
C10A N10 H10B 109.5 . . ?
H10A N10 H10B 109.5 . . ?
C10A N10 H10C 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
N10 C10A C10B 116.9(7) . . ?
N10 C10A C10G 116.2(8) . . ?
C10B C10A C10G 126.9(12) . . ?
N10 C10A H10 90.4 . . ?
C10B C10A H10 90.4 . . ?
C10G C10A H10 90.4 . . ?
C10A C10B C10C 120.1(14) . . ?
C10A C10B H10N 107.3 . . ?
C10C C10B H10N 107.3 . . ?
C10A C10B H10O 107.3 . . ?
C10C C10B H10O 107.3 . . ?
H10N C10B H10O 106.9 . . ?
C10B C10C C10D 121.3(18) . . ?
C10B C10C H10D 107 . . ?
C10D C10C H10D 107 . . ?
C10B C10C H10E 107 . . ?
C10D C10C H10E 107 . . ?
H10D C10C H10E 106.7 . . ?
C10E C10D C10C 125.5(19) . . ?
C10E C10D H10F 105.9 . . ?
C10C C10D H10F 105.9 . . ?
C10E C10D H10G 105.9 . . ?
C10C C10D H10G 105.9 . . ?
H10F C10D H10G 106.3 . . ?
C10D C10E C10F 119.5(16) . . ?
C10D C10E H10H 107.4 . . ?
C10F C10E H10H 107.4 . . ?
C10D C10E H10I 107.4 . . ?
C10F C10E H10I 107.4 . . ?
H10H C10E H10I 107 . . ?
C10E C10F C10G 125.6(19) . . ?
C10E C10F H10J 105.9 . . ?
C10G C10F H10J 105.9 . . ?
C10E C10F H10K 105.9 . . ?
C10G C10F H10K 105.9 . . ?
H10J C10F H10K 106.2 . . ?
C10F C10G C10A 123.3(15) . . ?
C10F C10G H10L 106.5 . . ?
C10A C10G H10L 106.5 . . ?
C10F C10G H10M 106.5 . . ?
C10A C10G H10M 106.5 . . ?
H10L C10G H10M 106.5 . . ?
C11G C11A C11B 114.8(12) . . ?
C11G C11A N11 110.6(12) . . ?
C11B C11A N11 108.2(12) . . ?
C11G C11A H11 107.7 . . ?
C11B C11A H11 107.7 . . ?
N11 C11A H11 107.7 . . ?
C11C C11B C11A 113.5(13) . . ?
C11C C11B H11N 108.9 . . ?
C11A C11B H11N 108.9 . . ?
C11C C11B H11O 108.9 . . ?
C11A C11B H11O 108.9 . . ?
H11N C11B H11O 107.7 . . ?
C11B C11C C11D 115.8(14) . . ?
C11B C11C H11D 108.3 . . ?
C11D C11C H11D 108.3 . . ?
C11B C11C H11E 108.3 . . ?
C11D C11C H11E 108.3 . . ?
H11D C11C H11E 107.4 . . ?
C11E C11D C11C 119.3(13) . . ?
C11E C11D H11F 107.5 . . ?
C11C C11D H11F 107.5 . . ?
C11E C11D H11G 107.5 . . ?
C11C C11D H11G 107.5 . . ?
H11F C11D H11G 107 . . ?
C11D C11E C11F 118.4(13) . . ?
C11D C11E H11H 107.7 . . ?
C11F C11E H11H 107.7 . . ?
C11D C11E H11I 107.7 . . ?
C11F C11E H11I 107.7 . . ?
H11H C11E H11I 107.1 . . ?
C11G C11F C11E 110.8(13) . . ?
C11G C11F H11J 109.5 . . ?
C11E C11F H11J 109.5 . . ?
C11G C11F H11K 109.5 . . ?
C11E C11F H11K 109.5 . . ?
H11J C11F H11K 108.1 . . ?
C11A C11G C11F 115.4(13) . . ?
C11A C11G H11L 108.4 . . ?
C11F C11G H11L 108.4 . . ?
C11A C11G H11M 108.4 . . ?
C11F C11G H11M 108.4 . . ?
H11L C11G H11M 107.5 . . ?
C11A N11 H11A 109.5 . . ?
C11A N11 H11B 109.5 . . ?
H11A N11 H11B 109.5 . . ?
C11A N11 H11C 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
C12B C12A C12G 120.0(15) . . ?
C12B C12A N12 106.9(14) . . ?
C12G C12A N12 111.3(14) . . ?
C12B C12A H12 105.9 . . ?
C12G C12A H12 105.9 . . ?
N12 C12A H12 105.9 . . ?
C12A C12B C12C 118.0(13) . . ?
C12A C12B H12N 107.8 . . ?
C12C C12B H12N 107.8 . . ?
C12A C12B H12O 107.8 . . ?
C12C C12B H12O 107.8 . . ?
H12N C12B H12O 107.1 . . ?
C12B C12C C12D 120.8(15) . . ?
C12B C12C H12D 107.1 . . ?
C12D C12C H12D 107.1 . . ?
C12B C12C H12E 107.1 . . ?
C12D C12C H12E 107.1 . . ?
H12D C12C H12E 106.8 . . ?
C12E C12D C12C 118.6(16) . . ?
C12E C12D H12F 107.7 . . ?
C12C C12D H12F 107.7 . . ?
C12E C12D H12G 107.7 . . ?
C12C C12D H12G 107.7 . . ?
H12F C12D H12G 107.1 . . ?
C12F C12E C12D 112.3(14) . . ?
C12F C12E H12H 109.2 . . ?
C12D C12E H12H 109.2 . . ?
C12F C12E H12I 109.2 . . ?
C12D C12E H12I 109.2 . . ?
H12H C12E H12I 107.9 . . ?
C12E C12F C12G 116.2(15) . . ?
C12E C12F H12J 108.2 . . ?
C12G C12F H12J 108.2 . . ?
C12E C12F H12K 108.2 . . ?
C12G C12F H12K 108.2 . . ?
H12J C12F H12K 107.4 . . ?
C12A C12G C12F 114.1(14) . . ?
C12A C12G H12L 108.7 . . ?
C12F C12G H12L 108.7 . . ?
C12A C12G H12M 108.7 . . ?
C12F C12G H12M 108.7 . . ?
H12L C12G H12M 107.6 . . ?
C12A N12 H12A 109.5 . . ?
C12A N12 H12B 109.5 . . ?
H12A N12 H12B 109.5 . . ?
C12A N12 H12C 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
N13 C13A C13G 112.8(13) . . ?
N13 C13A C13B 112.9(12) . . ?
C13G C13A C13B 117.5(11) . . ?
N13 C13A H13 103.9 . . ?
C13G C13A H13 103.9 . . ?
C13B C13A H13 103.9 . . ?
C13C C13B C13A 113.6(12) . . ?
C13C C13B H13N 108.8 . . ?
C13A C13B H13N 108.8 . . ?
C13C C13B H13O 108.8 . . ?
C13A C13B H13O 108.8 . . ?
H13N C13B H13O 107.7 . . ?
C13D C13C C13B 112.4(13) . . ?
C13D C13C H13D 109.1 . . ?
C13B C13C H13D 109.1 . . ?
C13D C13C H13E 109.1 . . ?
C13B C13C H13E 109.1 . . ?
H13D C13C H13E 107.9 . . ?
C13E C13D C13C 116.0(13) . . ?
C13E C13D H13F 108.3 . . ?
C13C C13D H13F 108.3 . . ?
C13E C13D H13G 108.3 . . ?
C13C C13D H13G 108.3 . . ?
H13F C13D H13G 107.4 . . ?
C13D C13E C13F 119.4(13) . . ?
C13D C13E H13H 107.5 . . ?
C13F C13E H13H 107.5 . . ?
C13D C13E H13I 107.5 . . ?
C13F C13E H13I 107.5 . . ?
H13H C13E H13I 107 . . ?
C13G C13F C13E 118.7(14) . . ?
C13G C13F H13J 107.6 . . ?
C13E C13F H13J 107.6 . . ?
C13G C13F H13K 107.6 . . ?
C13E C13F H13K 107.6 . . ?
H13J C13F H13K 107.1 . . ?
C13F C13G C13A 117.7(13) . . ?
C13F C13G H13L 107.9 . . ?
C13A C13G H13L 107.9 . . ?
C13F C13G H13M 107.9 . . ?
C13A C13G H13M 107.9 . . ?
H13L C13G H13M 107.2 . . ?
C13A N13 H13A 109.5 . . ?
C13A N13 H13B 109.5 . . ?
H13A N13 H13B 109.5 . . ?
C13A N13 H13C 109.5 . . ?
H13A N13 H13C 109.5 . . ?
H13B N13 H13C 109.5 . . ?
C14B C14A N14 108.0(14) . . ?
C14B C14A C14G 120.5(12) . . ?
N14 C14A C14G 108.3(13) . . ?
C14B C14A H14 106.4 . . ?
N14 C14A H14 106.4 . . ?
C14G C14A H14 106.4 . . ?
C14A C14B C14C 117.4(13) . . ?
C14A C14B H14N 107.9 . . ?
C14C C14B H14N 107.9 . . ?
C14A C14B H14O 107.9 . . ?
C14C C14B H14O 107.9 . . ?
H14N C14B H14O 107.2 . . ?
C14B C14C C14D 113.2(13) . . ?
C14B C14C H14D 108.9 . . ?
C14D C14C H14D 108.9 . . ?
C14B C14C H14E 108.9 . . ?
C14D C14C H14E 108.9 . . ?
H14D C14C H14E 107.8 . . ?
C14E C14D C14C 117.3(12) . . ?
C14E C14D H14F 108 . . ?
C14C C14D H14F 108 . . ?
C14E C14D H14G 108 . . ?
C14C C14D H14G 108 . . ?
H14F C14D H14G 107.2 . . ?
C14D C14E C14F 115.0(12) . . ?
C14D C14E H14H 108.5 . . ?
C14F C14E H14H 108.5 . . ?
C14D C14E H14I 108.5 . . ?
C14F C14E H14I 108.5 . . ?
H14H C14E H14I 107.5 . . ?
C14E C14F C14G 113.3(12) . . ?
C14E C14F H14J 108.9 . . ?
C14G C14F H14J 108.9 . . ?
C14E C14F H14K 108.9 . . ?
C14G C14F H14K 108.9 . . ?
H14J C14F H14K 107.7 . . ?
C14A C14G C14F 115.9(12) . . ?
C14A C14G H14L 108.3 . . ?
C14F C14G H14L 108.3 . . ?
C14A C14G H14M 108.3 . . ?
C14F C14G H14M 108.3 . . ?
H14L C14G H14M 107.4 . . ?
C14A N14 H14A 109.5 . . ?
C14A N14 H14B 109.5 . . ?
H14A N14 H14B 109.5 . . ?
C14A N14 H14C 109.5 . . ?
H14A N14 H14C 109.5 . . ?
H14B N14 H14C 109.5 . . ?
C15B C15A C15G 117.2(12) . . ?
C15B C15A N15 109.2(13) . . ?
C15G C15A N15 111.4(14) . . ?
C15B C15A H15 106.1 . . ?
C15G C15A H15 106.1 . . ?
N15 C15A H15 106.1 . . ?
C15A C15B C15C 114.3(13) . . ?
C15A C15B H15N 108.7 . . ?
C15C C15B H15N 108.7 . . ?
C15A C15B H15O 108.7 . . ?
C15C C15B H15O 108.7 . . ?
H15N C15B H15O 107.6 . . ?
C15D C15C C15B 115.3(14) . . ?
C15D C15C H15D 108.5 . . ?
C15B C15C H15D 108.5 . . ?
C15D C15C H15E 108.5 . . ?
C15B C15C H15E 108.5 . . ?
H15D C15C H15E 107.5 . . ?
C15E C15D C15C 118.1(13) . . ?
C15E C15D H15F 107.8 . . ?
C15C C15D H15F 107.8 . . ?
C15E C15D H15G 107.8 . . ?
C15C C15D H15G 107.8 . . ?
H15F C15D H15G 107.1 . . ?
C15D C15E C15F 115.6(13) . . ?
C15D C15E H15H 108.4 . . ?
C15F C15E H15H 108.4 . . ?
C15D C15E H15I 108.4 . . ?
C15F C15E H15I 108.4 . . ?
H15H C15E H15I 107.4 . . ?
C15G C15F C15E 114.3(14) . . ?
C15G C15F H15J 108.7 . . ?
C15E C15F H15J 108.7 . . ?
C15G C15F H15K 108.7 . . ?
C15E C15F H15K 108.7 . . ?
H15J C15F H15K 107.6 . . ?
C15F C15G C15A 116.5(13) . . ?
C15F C15G H15L 108.2 . . ?
C15A C15G H15L 108.2 . . ?
C15F C15G H15M 108.2 . . ?
C15A C15G H15M 108.2 . . ?
H15L C15G H15M 107.3 . . ?
C15A N15 H15A 109.5 . . ?
C15A N15 H15B 109.5 . . ?
H15A N15 H15B 109.5 . . ?
C15A N15 H15C 109.5 . . ?
H15A N15 H15C 109.5 . . ?
H15B N15 H15C 109.5 . . ?
C16G C16A C16B 117.7(11) . . ?
C16G C16A N16 108.1(11) . . ?
C16B C16A N16 110.6(11) . . ?
C16G C16A H16 106.6 . . ?
C16B C16A H16 106.6 . . ?
N16 C16A H16 106.6 . . ?
C16A C16B C16C 115.8(12) . . ?
C16A C16B H16N 108.3 . . ?
C16C C16B H16N 108.3 . . ?
C16A C16B H16O 108.3 . . ?
C16C C16B H16O 108.3 . . ?
H16N C16B H16O 107.4 . . ?
C16B C16C C16D 115.9(12) . . ?
C16B C16C H16D 108.3 . . ?
C16D C16C H16D 108.3 . . ?
C16B C16C H16E 108.3 . . ?
C16D C16C H16E 108.3 . . ?
H16D C16C H16E 107.4 . . ?
C16E C16D C16C 120.0(12) . . ?
C16E C16D H16F 107.3 . . ?
C16C C16D H16F 107.3 . . ?
C16E C16D H16G 107.3 . . ?
C16C C16D H16G 107.3 . . ?
H16F C16D H16G 106.9 . . ?
C16F C16E C16D 118.8(12) . . ?
C16F C16E H16H 107.6 . . ?
C16D C16E H16H 107.6 . . ?
C16F C16E H16I 107.6 . . ?
C16D C16E H16I 107.6 . . ?
H16H C16E H16I 107 . . ?
C16E C16F C16G 114.8(12) . . ?
C16E C16F H16J 108.6 . . ?
C16G C16F H16J 108.6 . . ?
C16E C16F H16K 108.6 . . ?
C16G C16F H16K 108.6 . . ?
H16J C16F H16K 107.5 . . ?
C16A C16G C16F 116.4(11) . . ?
C16A C16G H16L 108.2 . . ?
C16F C16G H16L 108.2 . . ?
C16A C16G H16M 108.2 . . ?
C16F C16G H16M 108.2 . . ?
H16L C16G H16M 107.4 . . ?
C16A N16 H16A 109.5 . . ?
C16A N16 H16B 109.5 . . ?
H16A N16 H16B 109.5 . . ?
C16A N16 H16C 109.5 . . ?
H16A N16 H16C 109.5 . . ?
H16B N16 H16C 109.5 . . ?
C17B C17A C17G 119.8(12) . . ?
C17B C17A N17 109.6(12) . . ?
C17G C17A N17 107.7(13) . . ?
C17B C17A H17 106.3 . . ?
C17G C17A H17 106.3 . . ?
N17 C17A H17 106.3 . . ?
C17C C17B C17A 122.3(13) . . ?
C17C C17B H17L 106.8 . . ?
C17A C17B H17L 106.8 . . ?
C17C C17B H17M 106.8 . . ?
C17A C17B H17M 106.8 . . ?
H17L C17B H17M 106.6 . . ?
C17B C17C C17D 118.8(13) . . ?
C17B C17C H17J 107.6 . . ?
C17D C17C H17J 107.6 . . ?
C17B C17C H17K 107.6 . . ?
C17D C17C H17K 107.6 . . ?
H17J C17C H17K 107 . . ?
C17E C17D C17C 118.7(13) . . ?
C17E C17D H17H 107.6 . . ?
C17C C17D H17H 107.6 . . ?
C17E C17D H17I 107.6 . . ?
C17C C17D H17I 107.6 . . ?
H17H C17D H17I 107.1 . . ?
C17D C17E C17F 122.9(13) . . ?
C17D C17E H17F 106.6 . . ?
C17F C17E H17F 106.6 . . ?
C17D C17E H17G 106.6 . . ?
C17F C17E H17G 106.6 . . ?
H17F C17E H17G 106.6 . . ?
C17G C17F C17E 127.4(14) . . ?
C17G C17F H17D 105.5 . . ?
C17E C17F H17D 105.5 . . ?
C17G C17F H17E 105.5 . . ?
C17E C17F H17E 105.5 . . ?
H17D C17F H17E 106 . . ?
C17F C17G C17A 124.5(13) . . ?
C17F C17G H17N 106.2 . . ?
C17A C17G H17N 106.2 . . ?
C17F C17G H17O 106.2 . . ?
C17A C17G H17O 106.2 . . ?
H17N C17G H17O 106.4 . . ?
C17A N17 H17A 109.5 . . ?
C17A N17 H17B 109.5 . . ?
H17A N17 H17B 109.5 . . ?
C17A N17 H17C 109.5 . . ?
H17A N17 H17C 109.5 . . ?
H17B N17 H17C 109.5 . . ?
H1AA O1 H1AB 118.1 . . ?
H2AA O2 H2AB 120.1 . . ?
Cl15 Pb1 Cl16 89.74(11) . . ?
Cl15 Pb1 Cl1 84.57(13) . . ?
Cl16 Pb1 Cl1 93.53(13) . . ?
Cl15 Pb1 Cl2 81.63(12) . . ?
Cl16 Pb1 Cl2 90.58(11) . . ?
Cl1 Pb1 Cl2 165.58(13) . . ?
Cl15 Pb1 Cl20 111.48(12) . 1_455 ?
Cl16 Pb1 Cl20 157.45(12) . 1_455 ?
Cl1 Pb1 Cl20 95.93(13) . 1_455 ?
Cl2 Pb1 Cl20 85.30(11) . 1_455 ?
Cl15 Pb1 Cl22 167.44(11) . . ?
Cl16 Pb1 Cl22 79.63(10) . . ?
Cl1 Pb1 Cl22 102.61(12) . . ?
Cl2 Pb1 Cl22 91.73(11) . . ?
Cl20 Pb1 Cl22 78.35(11) 1_455 . ?
Cl17 Pb2 Cl18 93.91(12) . . ?
Cl17 Pb2 Cl4 92.02(12) . . ?
Cl18 Pb2 Cl4 97.48(12) . . ?
Cl17 Pb2 Cl3 90.61(11) . . ?
Cl18 Pb2 Cl3 88.93(11) . . ?
Cl4 Pb2 Cl3 172.89(11) . . ?
Cl17 Pb2 Cl16 84.48(10) . . ?
Cl18 Pb2 Cl16 169.32(11) . . ?
Cl4 Pb2 Cl16 93.14(11) . . ?
Cl3 Pb2 Cl16 80.54(10) . . ?
Cl17 Pb2 Cl19 156.29(10) . . ?
Cl18 Pb2 Cl19 106.19(11) . . ?
Cl4 Pb2 Cl19 97.55(11) . . ?
Cl3 Pb2 Cl19 77.60(10) . . ?
Cl16 Pb2 Cl19 73.43(9) . . ?
Cl19 Pb3 Cl20 92.54(12) . . ?
Cl19 Pb3 Cl6 83.17(11) . . ?
Cl20 Pb3 Cl6 84.59(12) . . ?
Cl19 Pb3 Cl5 88.14(12) . . ?
Cl20 Pb3 Cl5 86.82(12) . . ?
Cl6 Pb3 Cl5 167.48(12) . . ?
Cl19 Pb3 Cl25 160.31(12) . 1_655 ?
Cl20 Pb3 Cl25 97.11(14) . 1_655 ?
Cl6 Pb3 Cl25 80.71(12) . 1_655 ?
Cl5 Pb3 Cl25 109.44(12) . 1_655 ?
Cl19 Pb3 Cl21 89.09(10) . . ?
Cl20 Pb3 Cl21 173.59(12) . . ?
Cl6 Pb3 Cl21 101.76(11) . . ?
Cl5 Pb3 Cl21 87.04(11) . . ?
Cl25 Pb3 Cl21 83.22(12) 1_655 . ?
Cl8 Pb4 Cl7 179.49(14) . . ?
Cl8 Pb4 Cl21 80.63(11) . . ?
Cl7 Pb4 Cl21 99.83(11) . . ?
Cl8 Pb4 Cl22 88.62(11) . . ?
Cl7 Pb4 Cl22 91.61(12) . . ?
Cl21 Pb4 Cl22 89.69(11) . . ?
Cl8 Pb4 Cl23 90.99(11) . . ?
Cl7 Pb4 Cl23 88.77(12) . . ?
Cl21 Pb4 Cl23 91.58(11) . . ?
Cl22 Pb4 Cl23 178.59(14) . . ?
Cl8 Pb4 Cl24 99.77(11) . . ?
Cl7 Pb4 Cl24 79.78(11) . . ?
Cl21 Pb4 Cl24 179.48(14) . . ?
Cl22 Pb4 Cl24 89.98(11) . . ?
Cl23 Pb4 Cl24 88.76(12) . . ?
Cl26 Pb5 Cl27 91.31(12) . . ?
Cl26 Pb5 Cl9 85.40(12) . . ?
Cl27 Pb5 Cl9 83.42(11) . . ?
Cl26 Pb5 Cl10 86.56(12) . . ?
Cl27 Pb5 Cl10 86.53(11) . . ?
Cl9 Pb5 Cl10 166.97(11) . . ?
Cl26 Pb5 Cl25 96.59(14) . . ?
Cl27 Pb5 Cl25 161.75(13) . . ?
Cl9 Pb5 Cl25 80.86(12) . . ?
Cl10 Pb5 Cl25 110.28(12) . . ?
Cl26 Pb5 Cl24 174.50(12) . . ?
Cl27 Pb5 Cl24 89.45(11) . . ?
Cl9 Pb5 Cl24 100.10(11) . . ?
Cl10 Pb5 Cl24 88.06(11) . . ?
Cl25 Pb5 Cl24 84.26(12) . . ?
Cl29 Pb6 Cl28 93.36(11) . . ?
Cl29 Pb6 Cl12 89.57(12) . . ?
Cl28 Pb6 Cl12 93.02(13) . . ?
Cl29 Pb6 Cl11 84.76(11) . . ?
Cl28 Pb6 Cl11 87.59(11) . . ?
Cl12 Pb6 Cl11 174.32(11) . . ?
Cl29 Pb6 Cl30 86.27(10) . . ?
Cl28 Pb6 Cl30 179.61(12) . . ?
Cl12 Pb6 Cl30 86.85(12) . . ?
Cl11 Pb6 Cl30 92.50(10) . . ?
Cl29 Pb6 Cl27 161.42(10) . . ?
Cl28 Pb6 Cl27 104.78(11) . . ?
Cl12 Pb6 Cl27 85.60(11) . . ?
Cl11 Pb6 Cl27 99.71(10) . . ?
Cl30 Pb6 Cl27 75.58(9) . . ?
Cl31 Pb7 Cl30 87.96(11) . . ?
Cl31 Pb7 Cl14 84.07(12) . . ?
Cl30 Pb7 Cl14 92.22(13) . . ?
Cl31 Pb7 Cl13 83.12(11) . . ?
Cl30 Pb7 Cl13 89.63(11) . . ?
Cl14 Pb7 Cl13 166.98(12) . . ?
Cl31 Pb7 Cl26 110.87(11) . 1_655 ?
Cl30 Pb7 Cl26 158.68(12) . 1_655 ?
Cl14 Pb7 Cl26 99.38(12) . 1_655 ?
Cl13 Pb7 Cl26 83.09(11) . 1_655 ?
Cl31 Pb7 Cl23 164.65(11) . . ?
Cl30 Pb7 Cl23 79.37(10) . . ?
Cl14 Pb7 Cl23 104.87(12) . . ?
Cl13 Pb7 Cl23 88.13(11) . . ?
Cl26 Pb7 Cl23 80.39(11) 1_655 . ?
Pb1 Cl16 Pb2 150.09(13) . . ?
Pb3 Cl19 Pb2 171.11(14) . . ?
Pb3 Cl20 Pb1 173.76(16) . 1_655 ?
Pb4 Cl21 Pb3 169.31(15) . . ?
Pb4 Cl22 Pb1 170.92(14) . . ?
Pb4 Cl23 Pb7 172.59(16) . . ?
Pb4 Cl24 Pb5 170.63(15) . . ?
Pb5 Cl25 Pb3 178.5(2) . 1_455 ?
Pb5 Cl26 Pb7 175.77(16) . 1_455 ?
Pb5 Cl27 Pb6 170.10(15) . . ?
Pb7 Cl30 Pb6 152.23(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

C1G C1A C1B C1C 42(2) . . . . ?
N1 C1A C1B C1C 161.3(12) . . . . ?
C1A C1B C1C C1D -84.9(18) . . . . ?
C1B C1C C1D C1E 66(2) . . . . ?
C1C C1D C1E C1F -48(2) . . . . ?
C1D C1E C1F C1G 65(2) . . . . ?
C1E C1F C1G C1A -82.1(18) . . . . ?
C1B C1A C1G C1F 35(2) . . . . ?
N1 C1A C1G C1F -84.9(15) . . . . ?
N2 C2A C2B C2C 94.1(16) . . . . ?
C2G C2A C2B C2C -28(2) . . . . ?
C2A C2B C2C C2D 79(2) . . . . ?
C2B C2C C2D C2E -65(2) . . . . ?
C2C C2D C2E C2F 45(2) . . . . ?
C2D C2E C2F C2G -68.0(19) . . . . ?
N2 C2A C2G C2F -172.7(12) . . . . ?
C2B C2A C2G C2F -47(2) . . . . ?
C2E C2F C2G C2A 90.6(16) . . . . ?
C3G C3A C3B C3C 75.4(19) . . . . ?
N3 C3A C3B C3C -166.9(14) . . . . ?
C3A C3B C3C C3D -47(2) . . . . ?
C3B C3C C3D C3E -21(3) . . . . ?
C3C C3D C3E C3F 75(2) . . . . ?
C3D C3E C3F C3G -79.3(18) . . . . ?
C3E C3F C3G C3A 68(2) . . . . ?
C3B C3A C3G C3F -68.8(19) . . . . ?
N3 C3A C3G C3F 175.0(13) . . . . ?
C4G C4A C4B C4C -39(2) . . . . ?
N4 C4A C4B C4C 89.1(17) . . . . ?
C4A C4B C4C C4D 90.1(19) . . . . ?
C4B C4C C4D C4E -75(2) . . . . ?
C4C C4D C4E C4F 54(2) . . . . ?
C4D C4E C4F C4G -67(2) . . . . ?
C4B C4A C4G C4F -38(2) . . . . ?
N4 C4A C4G C4F -160.8(15) . . . . ?
C4E C4F C4G C4A 80(2) . . . . ?
N5 C5A C5B C5C 170.9(13) . . . . ?
C5G C5A C5B C5C 42(2) . . . . ?
C5A C5B C5C C5D -81(2) . . . . ?
C5B C5C C5D C5E 63(2) . . . . ?
C5C C5D C5E C5F -50(2) . . . . ?
C5D C5E C5F C5G 70.7(19) . . . . ?
C5E C5F C5G C5A -85.0(17) . . . . ?
C5B C5A C5G C5F 34(2) . . . . ?
N5 C5A C5G C5F -95.5(15) . . . . ?
C6G C6A C6B C6C -28(3) . . . . ?
N6 C6A C6B C6C 98.3(16) . . . . ?
C6A C6B C6C C6D 79(2) . . . . ?
C6B C6C C6D C6E -73(2) . . . . ?
C6C C6D C6E C6F 53(2) . . . . ?
C6D C6E C6F C6G -63(2) . . . . ?
C6B C6A C6G C6F -46(3) . . . . ?
N6 C6A C6G C6F -167.9(14) . . . . ?
C6E C6F C6G C6A 81(2) . . . . ?
N7 C7A C7B C7C -173.3(17) . . . . ?
C7G C7A C7B C7C 62(3) . . . . ?
C7A C7B C7C C7D -77(2) . . . . ?
C7B C7C C7D C7E 58(3) . . . . ?
C7C C7D C7E C7F 4(4) . . . . ?
C7D C7E C7F C7G -60(3) . . . . ?
C7E C7F C7G C7A 74(3) . . . . ?
N7 C7A C7G C7F 173.7(19) . . . . ?
C7B C7A C7G C7F -62(3) . . . . ?
C8G C8A C8B C8C 44.9(17) . . . . ?
N8 C8A C8B C8C 167.5(11) . . . . ?
C8A C8B C8C C8D -85.9(16) . . . . ?
C8B C8C C8D C8E 63.0(19) . . . . ?
C8C C8D C8E C8F -46(2) . . . . ?
C8D C8E C8F C8G 67.4(18) . . . . ?
C8E C8F C8G C8A -84.3(16) . . . . ?
N8 C8A C8G C8F -87.9(14) . . . . ?
C8B C8A C8G C8F 33.8(18) . . . . ?
C9G C9A C9B C9C -33(2) . . . . ?
N9 C9A C9B C9C 85.1(14) . . . . ?
C9A C9B C9C C9D 85.8(17) . . . . ?
C9B C9C C9D C9E -74.5(18) . . . . ?
C9C C9D C9E C9F 55.9(19) . . . . ?
C9D C9E C9F C9G -72.2(19) . . . . ?
C9E C9F C9G C9A 86.8(18) . . . . ?
C9B C9A C9G C9F -42(2) . . . . ?
N9 C9A C9G C9F -161.5(12) . . . . ?
N10 C10A C10B C10C -180.0(17) . . . . ?
C10G C10A C10B C10C -1(3) . . . . ?
C10A C10B C10C C10D -47(3) . . . . ?
C10B C10C C10D C10E 65(3) . . . . ?
C10C C10D C10E C10F -45(4) . . . . ?
C10D C10E C10F C10G 37(4) . . . . ?
C10E C10F C10G C10A -50(3) . . . . ?
N10 C10A C10G C10F -137.0(18) . . . . ?
C10B C10A C10G C10F 45(3) . . . . ?
C11G C11A C11B C11C 59(2) . . . . ?
N11 C11A C11B C11C -177.0(13) . . . . ?
C11A C11B C11C C11D -79.3(19) . . . . ?
C11B C11C C11D C11E 71(2) . . . . ?
C11C C11D C11E C11F -5(3) . . . . ?
C11D C11E C11F C11G -62(2) . . . . ?
C11B C11A C11G C11F -67(2) . . . . ?
N11 C11A C11G C11F 170.1(13) . . . . ?
C11E C11F C11G C11A 86.7(18) . . . . ?
C12G C12A C12B C12C 41(3) . . . . ?
N12 C12A C12B C12C 169.3(19) . . . . ?
C12A C12B C12C C12D 24(3) . . . . ?
C12B C12C C12D C12E -74(3) . . . . ?
C12C C12D C12E C12F 73(2) . . . . ?
C12D C12E C12F C12G -62(2) . . . . ?
C12B C12A C12G C12F -79(3) . . . . ?
N12 C12A C12G C12F 154.8(17) . . . . ?
C12E C12F C12G C12A 72(2) . . . . ?
N13 C13A C13B C13C 90.1(16) . . . . ?
C13G C13A C13B C13C -44(2) . . . . ?
C13A C13B C13C C13D 89.5(17) . . . . ?
C13B C13C C13D C13E -70(2) . . . . ?
C13C C13D C13E C13F 47(3) . . . . ?
C13D C13E C13F C13G -62(2) . . . . ?
C13E C13F C13G C13A 77(2) . . . . ?
N13 C13A C13G C13F -165.4(14) . . . . ?
C13B C13A C13G C13F -31(2) . . . . ?
N14 C14A C14B C14C 88.8(16) . . . . ?
C14G C14A C14B C14C -36(2) . . . . ?
C14A C14B C14C C14D 81(2) . . . . ?
C14B C14C C14D C14E -71(2) . . . . ?
C14C C14D C14E C14F 57(2) . . . . ?
C14D C14E C14F C14G -70.8(19) . . . . ?
C14B C14A C14G C14F -37(2) . . . . ?
N14 C14A C14G C14F -162.3(13) . . . . ?
C14E C14F C14G C14A 81.8(19) . . . . ?
C15G C15A C15B C15C 48(2) . . . . ?
N15 C15A C15B C15C 175.4(14) . . . . ?
C15A C15B C15C C15D -86(2) . . . . ?
C15B C15C C15D C15E 64(2) . . . . ?
C15C C15D C15E C15F -48(2) . . . . ?
C15D C15E C15F C15G 71(2) . . . . ?
C15E C15F C15G C15A -84(2) . . . . ?
C15B C15A C15G C15F 29(2) . . . . ?
N15 C15A C15G C15F -97.4(17) . . . . ?
C16G C16A C16B C16C 60.2(18) . . . . ?
N16 C16A C16B C16C -174.8(12) . . . . ?
C16A C16B C16C C16D -78.3(18) . . . . ?
C16B C16C C16D C16E 58(2) . . . . ?
C16C C16D C16E C16F 8(2) . . . . ?
C16D C16E C16F C16G -69(2) . . . . ?
C16B C16A C16G C16F -58.5(19) . . . . ?
N16 C16A C16G C16F 175.4(12) . . . . ?
C16E C16F C16G C16A 78.6(17) . . . . ?
C17G C17A C17B C17C 41(3) . . . . ?
N17 C17A C17B C17C 166.1(14) . . . . ?
C17A C17B C17C C17D -75(2) . . . . ?
C17B C17C C17D C17E 57(2) . . . . ?
C17C C17D C17E C17F -36(3) . . . . ?
C17D C17E C17F C17G 44(3) . . . . ?
C17E C17F C17G C17A -51(3) . . . . ?
C17B C17A C17G C17F 17(3) . . . . ?
N17 C17A C17G C17F -108.7(19) . . . . ?
Cl15 Pb1 Cl16 Pb2 4.2(3) . . . . ?
Cl1 Pb1 Cl16 Pb2 88.8(3) . . . . ?
Cl2 Pb1 Cl16 Pb2 -77.4(3) . . . . ?
Cl20 Pb1 Cl16 Pb2 -156.5(2) 1_455 . . . ?
Cl22 Pb1 Cl16 Pb2 -169.1(3) . . . . ?
Cl17 Pb2 Cl16 Pb1 -8.2(3) . . . . ?
Cl18 Pb2 Cl16 Pb1 -90.0(7) . . . . ?
Cl4 Pb2 Cl16 Pb1 83.5(3) . . . . ?
Cl3 Pb2 Cl16 Pb1 -99.7(3) . . . . ?
Cl19 Pb2 Cl16 Pb1 -179.5(3) . . . . ?
Cl8 Pb4 Cl21 Pb3 -0.5(8) . . . . ?
Cl7 Pb4 Cl21 Pb3 179.7(8) . . . . ?
Cl22 Pb4 Cl21 Pb3 88.1(8) . . . . ?
Cl23 Pb4 Cl21 Pb3 -91.3(8) . . . . ?
Cl19 Pb3 Cl21 Pb4 -75.0(8) . . . . ?
Cl6 Pb3 Cl21 Pb4 7.9(9) . . . . ?
Cl5 Pb3 Cl21 Pb4 -163.2(9) . . . . ?
Cl25 Pb3 Cl21 Pb4 86.9(9) 1_655 . . . ?
Cl31 Pb7 Cl30 Pb6 1.2(3) . . . . ?
Cl14 Pb7 Cl30 Pb6 -82.8(3) . . . . ?
Cl13 Pb7 Cl30 Pb6 84.3(3) . . . . ?
Cl26 Pb7 Cl30 Pb6 154.0(3) 1_655 . . . ?
Cl23 Pb7 Cl30 Pb6 172.5(3) . . . . ?
Cl29 Pb6 Cl30 Pb7 1.0(3) . . . . ?
Cl28 Pb6 Cl30 Pb7 19(19) . . . . ?
Cl12 Pb6 Cl30 Pb7 90.8(3) . . . . ?
Cl11 Pb6 Cl30 Pb7 -83.6(3) . . . . ?
Cl27 Pb6 Cl30 Pb7 177.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl23 0.91 2.55 3.358(15) 147.7 .
N1 H1B Cl25 0.91 2.76 3.468(14) 135.9 1_655
N1 H1C Cl9 0.91 2.46 3.348(14) 166.8 1_655
N2 H2A Cl27 0.91 2.51 3.338(14) 151.4 .
N2 H2B Cl7 0.91 2.38 3.273(14) 167.1 .
N2 H2C Cl30 0.91 2.78 3.432(14) 129.7 .
N2 H2C Cl23 0.91 2.79 3.549(14) 142 .
N3 H3A Cl9 0.91 2.47 3.305(13) 151.9 .
N3 H3B O1 0.91 1.95 2.847(16) 170.5 1_455
N3 H3C Cl13 0.91 2.33 3.193(12) 158.6 1_455
N4 H4A Cl16 0.91 2.62 3.338(16) 136.8 .
N4 H4B Cl5 0.91 2.41 3.286(16) 162.8 .
N4 H4C Cl21 0.91 2.67 3.483(17) 149 .
N5 H5A Cl30 0.91 2.62 3.338(14) 136.8 .
N5 H5B Cl24 0.91 2.59 3.301(13) 135.4 .
N5 H5C Cl10 0.91 2.38 3.285(15) 177.2 .
N6 H6A Cl25 0.91 2.78 3.568(17) 145.5 .
N6 H6B Cl8 0.91 2.36 3.249(16) 166.4 1_455
N6 H6C Cl23 0.91 2.57 3.379(15) 148.3 1_455
N7 H7A O1 0.91 2 2.873(17) 161.3 1_455
N7 H7B Cl12 0.91 2.37 3.272(17) 173.9 .
N7 H7C Cl10 0.91 2.34 3.239(15) 169 .
N8 H8A Cl29 0.91 2.64 3.317(13) 132.3 .
N8 H8A Cl31 0.91 2.7 3.332(12) 126.9 .
N8 H8B Cl11 0.91 2.32 3.219(12) 169.3 .
N8 H8C Cl13 0.91 2.39 3.248(12) 157.9 .
N9 H9A Cl17 0.91 2.62 3.251(12) 126.9 .
N9 H9A Cl15 0.91 2.78 3.474(12) 133.8 .
N9 H9B Cl3 0.91 2.37 3.229(12) 157.5 .
N9 H9C Cl1 0.91 2.38 3.258(12) 162.8 .
N10 H10A Cl14 0.91 2.74 3.209(14) 113.4 .
N10 H10B Cl29 0.91 2.52 3.302(11) 144.3 .
N10 H10B Cl12 0.91 2.7 3.240(13) 119.3 .
N10 H10C Cl31 0.91 2.54 3.428(12) 164.6 .
N11 H11A Cl6 0.91 2.48 3.353(13) 160.5 .
N11 H11B Cl2 0.91 2.29 3.192(13) 169.4 1_655
N11 H11C O2 0.91 1.99 2.882(17) 165.4 .
N12 H12A Cl4 0.91 2.43 3.192(16) 142 .
N12 H12B Cl17 0.91 2.41 3.254(15) 154.5 .
N12 H12C Cl2 0.91 2.38 3.239(16) 157.8 .
N13 H13A Cl5 0.91 2.26 3.167(14) 175.1 .
N13 H13B Cl3 0.91 2.32 3.218(15) 169.6 .
N13 H13C O2 0.91 2 2.833(17) 150.9 .
N14 H14A Cl25 0.91 2.71 3.460(15) 140.2 .
N14 H14C Cl6 0.91 2.44 3.313(14) 160.7 1_455
N14 H14B Cl22 0.91 2.5 3.357(14) 157.3 .
N15 H15A Cl22 0.91 2.48 3.320(15) 153.9 .
N15 H15B Cl7 0.91 2.42 3.291(16) 161.1 .
N15 H15C Cl25 0.91 2.77 3.627(16) 157.9 .
N16 H16A Cl11 0.91 2.49 3.251(12) 140.8 .
N16 H16C Cl28 0.91 2.33 3.203(13) 161.1 .
N17 H17A Cl19 0.91 2.55 3.330(14) 143.5 .
N17 H17B Cl16 0.91 2.6 3.342(13) 138.6 .
N17 H17C Cl8 0.91 2.39 3.300(13) 179.1 .
O1 H1AA Cl31 0.85 2.34 3.188(10) 179.8 .
O1 H1AB Cl28 0.85 2.4 3.149(11) 146.4 1_655
O2 H2AA Cl18 0.85 2.29 3.142(11) 179 .
O2 H2AB Cl15 0.85 2.35 3.203(11) 178.9 1_655
_chemical_name_common            
;heptadecakis(cycloheptylammonium)hentriacontachloroheptaplumba
te(ii) dihydrate
;

### END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2006-06-13 at 14:58:02
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 4ac23l_a smart

data_12
_database_code_depnum_ccdc_archive 'CCDC 708571'

_audit_creation_date             2006-06-13T14:58:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
octadecakis(cyclooctylammonium)tetracontachloroundecaplumbate(II)
;
_chemical_formula_moiety         'Cl40 Pb11, 18(C8 H18 N)'
_chemical_formula_sum            'C144 H324 Cl40 N18 Pb11'
_chemical_formula_weight         6005.3

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.365(3)
_cell_length_b                   19.016(4)
_cell_length_c                   19.357(4)
_cell_angle_alpha                63.476(3)
_cell_angle_beta                 70.493(4)
_cell_angle_gamma                88.146(4)
_cell_volume                     5339.0(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    981
_cell_measurement_theta_min      3.4465
_cell_measurement_theta_max      27.4215

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.03
0 1 0 0.03
0 -1 -3 0.105
0 1 3 0.105
-1 0 -1 0.205
1 0 0 0.26

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    9.182
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker XPREP (Bruker, 1999)'
_exptl_absorpt_correction_T_min  0.0946
_exptl_absorpt_correction_T_max  0.5551
_exptl_special_details           
;
Numerical integration absorption corrections based on indexed crystal faces
were applied using the XPREP routine (Bruker, 1999)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_number            28276
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             18557
_reflns_number_gt                13579
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT+, (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT+, (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003)
;

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The C-C bond lengths and bond angles were restrained using the SADI instruction
in SHELX to be within 0.01 Å of each other. The anisotropic displacement
parameters were restrained to be equal in the direction
of the bonds using the SIMU and DELU instruction.

;
_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)+(0.0767P)²+114.9580P] 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_number_reflns         18557
_refine_ls_number_parameters     964
_refine_ls_number_restraints     1348
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1669
_refine_ls_wR_factor_gt          0.1429
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_diff_density_max         5.011
_refine_diff_density_min         -2.521
_refine_diff_density_rms         0.29

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
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'

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 0.4986(9) -0.2120(7) -0.0134(8) 0.0368(19) Uani 1 1 d DU . .
H1 H 0.4604 -0.2024 0.0323 0.044 Uiso 1 1 calc R . .
C2 C 0.5307(8) -0.2889(6) 0.0271(9) 0.040(2) Uani 1 1 d DU . .
H2D H 0.581 -0.2915 -0.0147 0.048 Uiso 1 1 calc R . .
H2E H 0.5472 -0.288 0.071 0.048 Uiso 1 1 calc R . .
C3 C 0.4711(9) -0.3634(7) 0.0647(8) 0.044(2) Uani 1 1 d DU . .
H3D H 0.4743 -0.3996 0.1193 0.053 Uiso 1 1 calc R . .
H3E H 0.4146 -0.3489 0.0745 0.053 Uiso 1 1 calc R . .
C4 C 0.4832(11) -0.4090(8) 0.0157(8) 0.047(2) Uani 1 1 d DU . .
H4D H 0.5408 -0.4206 0.0031 0.056 Uiso 1 1 calc R . .
H4E H 0.4469 -0.4605 0.0518 0.056 Uiso 1 1 calc R . .
C5 C 0.4671(10) -0.3707(8) -0.0642(7) 0.046(2) Uani 1 1 d DU . .
H5D H 0.4097 -0.3584 -0.0517 0.055 Uiso 1 1 calc R . .
H5E H 0.4705 -0.4102 -0.0849 0.055 Uiso 1 1 calc R . .
C6 C 0.5231(9) -0.2958(6) -0.1331(8) 0.042(2) Uani 1 1 d DU . .
H6D H 0.5759 -0.2958 -0.124 0.05 Uiso 1 1 calc R . .
H6E H 0.5351 -0.2982 -0.1856 0.05 Uiso 1 1 calc R . .
C7 C 0.4925(9) -0.2178(7) -0.1438(7) 0.039(2) Uani 1 1 d DU . .
H7D H 0.4532 -0.2088 -0.1731 0.047 Uiso 1 1 calc R . .
H7E H 0.54 -0.1753 -0.1805 0.047 Uiso 1 1 calc R . .
C8 C 0.4507(8) -0.2080(9) -0.0670(8) 0.0383(19) Uani 1 1 d DU . .
H8D H 0.4299 -0.1561 -0.0844 0.046 Uiso 1 1 calc R . .
H8E H 0.4018 -0.2494 -0.0317 0.046 Uiso 1 1 calc R . .
N1 N 0.5691(8) -0.1466(7) -0.0600(7) 0.034(2) Uani 1 1 d U . .
H1A H 0.5974 -0.1502 -0.0268 0.052 Uiso 1 1 calc R . .
H1B H 0.5496 -0.099 -0.0767 0.052 Uiso 1 1 calc R . .
H1C H 0.6033 -0.1506 -0.1051 0.052 Uiso 1 1 calc R . .
C9 C 0.5943(11) 0.2285(9) -0.2668(10) 0.053(2) Uani 1 1 d DU . .
H9 H 0.6528 0.2358 -0.3037 0.064 Uiso 1 1 calc R . .
C10 C 0.5861(11) 0.2939(9) -0.2425(10) 0.058(2) Uani 1 1 d DU . .
H10A H 0.5315 0.3113 -0.2408 0.069 Uiso 1 1 calc R . .
H10B H 0.5866 0.2715 -0.1856 0.069 Uiso 1 1 calc R . .
C11 C 0.6504(13) 0.3657(10) -0.2965(10) 0.069(3) Uani 1 1 d DU . .
H11A H 0.6377 0.4023 -0.2717 0.083 Uiso 1 1 calc R . .
H11B H 0.7039 0.3484 -0.293 0.083 Uiso 1 1 calc R . .
C12 C 0.6630(15) 0.4129(11) -0.3856(10) 0.078(3) Uani 1 1 d DU . .
H12A H 0.6118 0.4362 -0.3893 0.094 Uiso 1 1 calc R . .
H12B H 0.7072 0.4576 -0.4095 0.094 Uiso 1 1 calc R . .
C13 C 0.6843(11) 0.3742(13) -0.4394(12) 0.077(3) Uani 1 1 d DU . .
H13A H 0.7111 0.3274 -0.4145 0.092 Uiso 1 1 calc R . .
H13B H 0.7254 0.4116 -0.4935 0.092 Uiso 1 1 calc R . .
C14 C 0.6134(12) 0.3474(12) -0.4544(11) 0.078(3) Uani 1 1 d DU . .
H14A H 0.5947 0.396 -0.4888 0.094 Uiso 1 1 calc R . .
H14B H 0.6364 0.3204 -0.4888 0.094 Uiso 1 1 calc R . .
C15 C 0.5397(11) 0.2956(11) -0.3867(10) 0.074(3) Uani 1 1 d DU . .
H15A H 0.5085 0.2782 -0.4121 0.088 Uiso 1 1 calc R . .
H15B H 0.5059 0.3299 -0.3661 0.088 Uiso 1 1 calc R . .
C16 C 0.5405(12) 0.2222(10) -0.3112(10) 0.059(3) Uani 1 1 d DU . .
H16A H 0.4832 0.2038 -0.2711 0.071 Uiso 1 1 calc R . .
H16B H 0.5578 0.1802 -0.3279 0.071 Uiso 1 1 calc R . .
N2 N 0.5794(9) 0.1500(8) -0.1911(8) 0.042(3) Uani 1 1 d U . .
H2A H 0.612 0.1518 -0.1635 0.063 Uiso 1 1 calc R . .
H2B H 0.5917 0.111 -0.2065 0.063 Uiso 1 1 calc R . .
H2C H 0.5255 0.1398 -0.1577 0.063 Uiso 1 1 calc R . .
C17 C 0.8540(12) 0.2774(11) -0.5858(16) 0.084(3) Uani 1 1 d DU . .
H17 H 0.885 0.2724 -0.6369 0.1 Uiso 1 1 calc R . .
C18 C 0.7878(13) 0.3118(11) -0.6153(15) 0.090(4) Uani 1 1 d DU . .
H18A H 0.7359 0.291 -0.5666 0.108 Uiso 1 1 calc R . .
H18B H 0.7833 0.29 -0.6519 0.108 Uiso 1 1 calc R . .
C19 C 0.7895(13) 0.4002(11) -0.6609(13) 0.094(4) Uani 1 1 d DU . .
H19A H 0.7323 0.411 -0.6562 0.112 Uiso 1 1 calc R . .
H19B H 0.8079 0.4245 -0.6322 0.112 Uiso 1 1 calc R . .
C20 C 0.8425(12) 0.4411(14) -0.7500(13) 0.099(4) Uani 1 1 d DU . .
H20A H 0.8173 0.4232 -0.7793 0.118 Uiso 1 1 calc R . .
H20B H 0.8385 0.4985 -0.7701 0.118 Uiso 1 1 calc R . .
C21 C 0.9304(12) 0.4334(16) -0.7773(13) 0.100(4) Uani 1 1 d DU . .
H21A H 0.9553 0.4736 -0.836 0.12 Uiso 1 1 calc R . .
H21B H 0.9343 0.3808 -0.776 0.12 Uiso 1 1 calc R . .
C22 C 0.9838(14) 0.4409(14) -0.7345(13) 0.101(4) Uani 1 1 d DU . .
H22A H 1.0384 0.4293 -0.7616 0.121 Uiso 1 1 calc R . .
H22B H 0.9913 0.4979 -0.7495 0.121 Uiso 1 1 calc R . .
C23 C 0.9681(16) 0.3986(12) -0.6469(12) 0.097(4) Uani 1 1 d DU . .
H23A H 0.9367 0.4323 -0.6237 0.117 Uiso 1 1 calc R . .
H23B H 1.0227 0.4004 -0.6417 0.117 Uiso 1 1 calc R . .
C24 C 0.9265(13) 0.3161(11) -0.5879(14) 0.090(4) Uani 1 1 d DU . .
H24A H 0.9698 0.2816 -0.5928 0.108 Uiso 1 1 calc R . .
H24B H 0.9121 0.3121 -0.5322 0.108 Uiso 1 1 calc R . .
N3 N 0.8381(10) 0.1925(9) -0.5331(9) 0.055(3) Uani 1 1 d U . .
H3A H 0.8807 0.1765 -0.5147 0.082 Uiso 1 1 calc R . .
H3B H 0.8333 0.1674 -0.5622 0.082 Uiso 1 1 calc R . .
H3C H 0.7905 0.1802 -0.4891 0.082 Uiso 1 1 calc R . .
C25 C 0.8601(10) -0.1844(9) -0.0875(10) 0.053(3) Uani 1 1 d DU . .
H25 H 0.8249 -0.1713 -0.1221 0.064 Uiso 1 1 calc R . .
C26 C 0.8060(11) -0.2371(9) 0.0005(10) 0.063(3) Uani 1 1 d DU . .
H26A H 0.7659 -0.2058 0.0199 0.075 Uiso 1 1 calc R . .
H26B H 0.8408 -0.2537 0.035 0.075 Uiso 1 1 calc R . .
C27 C 0.7588(11) -0.3109(9) 0.0144(14) 0.072(3) Uani 1 1 d DU . .
H27A H 0.702 -0.3187 0.0537 0.086 Uiso 1 1 calc R . .
H27B H 0.7546 -0.3018 -0.0386 0.086 Uiso 1 1 calc R . .
C28 C 0.7959(11) -0.3855(10) 0.0471(13) 0.081(3) Uani 1 1 d DU . .
H28A H 0.7828 -0.404 0.1068 0.097 Uiso 1 1 calc R . .
H28B H 0.768 -0.4265 0.0417 0.097 Uiso 1 1 calc R . .
C29 C 0.8861(12) -0.3820(13) 0.0084(11) 0.082(3) Uani 1 1 d DU . .
H29A H 0.9018 -0.4342 0.0397 0.099 Uiso 1 1 calc R . .
H29B H 0.9143 -0.3422 0.015 0.099 Uiso 1 1 calc R . .
C30 C 0.9189(15) -0.3620(10) -0.0815(11) 0.083(3) Uani 1 1 d DU . .
H30A H 0.9766 -0.3732 -0.0952 0.099 Uiso 1 1 calc R . .
H30B H 0.8871 -0.3994 -0.0881 0.099 Uiso 1 1 calc R . .
C31 C 0.9184(14) -0.2807(9) -0.1447(11) 0.071(3) Uani 1 1 d DU . .
H31A H 0.8638 -0.2781 -0.1508 0.085 Uiso 1 1 calc R . .
H31B H 0.9602 -0.2717 -0.1983 0.085 Uiso 1 1 calc R . .
C32 C 0.9355(10) -0.2127(10) -0.1277(12) 0.063(3) Uani 1 1 d DU . .
H32A H 0.9688 -0.2301 -0.0917 0.076 Uiso 1 1 calc R . .
H32B H 0.9691 -0.1673 -0.1807 0.076 Uiso 1 1 calc R . .
N4 N 0.8893(9) -0.1072(8) -0.0915(9) 0.046(3) Uani 1 1 d U . .
H4A H 0.845 -0.0876 -0.0687 0.069 Uiso 1 1 calc R . .
H4B H 0.9161 -0.0712 -0.1452 0.069 Uiso 1 1 calc R . .
H4C H 0.9242 -0.1169 -0.0631 0.069 Uiso 1 1 calc R . .
C33 C 0.9114(12) 0.2203(12) -0.2664(10) 0.071(3) Uani 1 1 d DU . .
H33 H 0.8642 0.248 -0.2791 0.086 Uiso 1 1 calc R . .
C34 C 0.9748(13) 0.2336(11) -0.3472(10) 0.078(3) Uani 1 1 d DU . .
H34A H 0.9535 0.2024 -0.368 0.093 Uiso 1 1 calc R . .
H34B H 1.0249 0.2123 -0.337 0.093 Uiso 1 1 calc R . .
C35 C 0.9997(13) 0.3190(11) -0.4145(12) 0.091(4) Uani 1 1 d DU . .
H35A H 1.0463 0.3419 -0.409 0.109 Uiso 1 1 calc R . .
H35B H 1.021 0.3181 -0.4683 0.109 Uiso 1 1 calc R . .
C36 C 0.9368(15) 0.3745(13) -0.4186(13) 0.097(4) Uani 1 1 d DU . .
H36A H 0.9511 0.4122 -0.478 0.116 Uiso 1 1 calc R . .
H36B H 0.8838 0.3423 -0.4016 0.116 Uiso 1 1 calc R . .
C37 C 0.9183(17) 0.4227(12) -0.3753(12) 0.100(4) Uani 1 1 d DU . .
H37A H 0.8728 0.4518 -0.3889 0.12 Uiso 1 1 calc R . .
H37B H 0.9673 0.4629 -0.4003 0.12 Uiso 1 1 calc R . .
C38 C 0.8950(15) 0.3867(13) -0.2834(12) 0.096(4) Uani 1 1 d DU . .
H38A H 0.887 0.4302 -0.268 0.115 Uiso 1 1 calc R . .
H38B H 0.8411 0.3528 -0.2573 0.115 Uiso 1 1 calc R . .
C39 C 0.9534(14) 0.3385(10) -0.2473(14) 0.085(3) Uani 1 1 d DU . .
H39A H 0.954 0.3485 -0.2014 0.102 Uiso 1 1 calc R . .
H39B H 1.0095 0.3573 -0.29 0.102 Uiso 1 1 calc R . .
C40 C 0.9352(14) 0.2495(10) -0.2145(11) 0.076(3) Uani 1 1 d DU . .
H40A H 0.9847 0.2259 -0.2052 0.091 Uiso 1 1 calc R . .
H40B H 0.8901 0.2282 -0.1599 0.091 Uiso 1 1 calc R . .
N5 N 0.8795(9) 0.1359(9) -0.2145(9) 0.054(3) Uani 1 1 d U . .
H5A H 0.8391 0.1288 -0.1667 0.081 Uiso 1 1 calc R . .
H5B H 0.9211 0.1083 -0.2027 0.081 Uiso 1 1 calc R . .
H5C H 0.8583 0.1181 -0.2418 0.081 Uiso 1 1 calc R . .
C41 C 0.7605(18) -0.2760(12) 0.6720(12) 0.095(3) Uani 1 1 d DU . .
H41 H 0.6998 -0.2905 0.704 0.115 Uiso 1 1 calc R . .
C42 C 0.8047(16) -0.3145(12) 0.7317(12) 0.101(4) Uani 1 1 d DU . .
H42A H 0.8536 -0.3336 0.7046 0.121 Uiso 1 1 calc R . .
H42B H 0.8251 -0.2732 0.7417 0.121 Uiso 1 1 calc R . .
C43 C 0.7564(19) -0.3823(12) 0.8136(12) 0.112(4) Uani 1 1 d DU . .
H43A H 0.791 -0.398 0.8483 0.134 Uiso 1 1 calc R . .
H43B H 0.7077 -0.3632 0.8409 0.134 Uiso 1 1 calc R . .
C44 C 0.727(2) -0.4540(13) 0.8126(15) 0.118(4) Uani 1 1 d DU . .
H44A H 0.7765 -0.4813 0.8036 0.141 Uiso 1 1 calc R . .
H44B H 0.6899 -0.4884 0.87 0.141 Uiso 1 1 calc R . .
C45 C 0.6867(16) -0.4589(16) 0.7606(13) 0.118(4) Uani 1 1 d DU . .
H45A H 0.6443 -0.4227 0.7601 0.141 Uiso 1 1 calc R . .
H45B H 0.6563 -0.5133 0.7905 0.141 Uiso 1 1 calc R . .
C46 C 0.7281(18) -0.4430(13) 0.6738(13) 0.116(4) Uani 1 1 d DU . .
H46A H 0.7482 -0.4929 0.6756 0.139 Uiso 1 1 calc R . .
H46B H 0.6846 -0.434 0.6494 0.139 Uiso 1 1 calc R . .
C47 C 0.7966(16) -0.3794(11) 0.6144(14) 0.108(4) Uani 1 1 d DU . .
H47A H 0.813 -0.3798 0.5605 0.129 Uiso 1 1 calc R . .
H47B H 0.8442 -0.3912 0.6332 0.129 Uiso 1 1 calc R . .
C48 C 0.7793(19) -0.2957(11) 0.6011(12) 0.101(4) Uani 1 1 d DU . .
H48A H 0.8278 -0.2581 0.5554 0.121 Uiso 1 1 calc R . .
H48B H 0.7322 -0.2844 0.5817 0.121 Uiso 1 1 calc R . .
N6 N 0.7822(12) -0.1889(10) 0.6402(10) 0.068(4) Uani 1 1 d U . .
H6A H 0.7734 -0.1784 0.6835 0.102 Uiso 1 1 calc R . .
H6B H 0.7501 -0.1617 0.611 0.102 Uiso 1 1 calc R . .
H6C H 0.8362 -0.1736 0.6067 0.102 Uiso 1 1 calc R . .
C49 C 0.7473(19) -0.1926(12) 0.2769(14) 0.102(4) Uani 1 1 d DU . .
H49 H 0.6861 -0.2038 0.3062 0.122 Uiso 1 1 calc R . .
C50 C 0.7792(17) -0.2366(10) 0.3455(14) 0.107(4) Uani 1 1 d DU . .
H50A H 0.7801 -0.2028 0.3721 0.129 Uiso 1 1 calc R . .
H50B H 0.8371 -0.2433 0.3207 0.129 Uiso 1 1 calc R . .
C51 C 0.7332(18) -0.3169(12) 0.4121(13) 0.118(4) Uani 1 1 d DU . .
H51A H 0.7378 -0.325 0.4647 0.142 Uiso 1 1 calc R . .
H51B H 0.6741 -0.3163 0.419 0.142 Uiso 1 1 calc R . .
C52 C 0.760(2) -0.3858(12) 0.3987(14) 0.120(4) Uani 1 1 d DU . .
H52A H 0.7101 -0.4246 0.4227 0.144 Uiso 1 1 calc R . .
H52B H 0.7948 -0.4108 0.4325 0.144 Uiso 1 1 calc R . .
C53 C 0.8067(16) -0.3774(13) 0.3139(15) 0.121(4) Uani 1 1 d DU . .
H53A H 0.8507 -0.3314 0.2839 0.145 Uiso 1 1 calc R . .
H53B H 0.8336 -0.4254 0.3196 0.145 Uiso 1 1 calc R . .
C54 C 0.754(2) -0.3662(13) 0.2631(17) 0.118(4) Uani 1 1 d DU . .
H54A H 0.7895 -0.3663 0.2111 0.142 Uiso 1 1 calc R . .
H54B H 0.7119 -0.4139 0.2933 0.142 Uiso 1 1 calc R . .
C55 C 0.7102(17) -0.2971(12) 0.2402(18) 0.110(4) Uani 1 1 d DU . .
H55A H 0.6598 -0.3068 0.2883 0.132 Uiso 1 1 calc R . .
H55B H 0.6925 -0.2927 0.195 0.132 Uiso 1 1 calc R . .
C56 C 0.7591(18) -0.2175(12) 0.2123(13) 0.107(4) Uani 1 1 d DU . .
H56A H 0.8185 -0.2204 0.1887 0.128 Uiso 1 1 calc R . .
H56B H 0.7438 -0.1758 0.1674 0.128 Uiso 1 1 calc R . .
N7 N 0.7649(14) -0.1083(11) 0.2481(14) 0.090(4) Uani 1 1 d U . .
H7A H 0.7554 -0.0988 0.2921 0.135 Uiso 1 1 calc R . .
H7B H 0.7317 -0.0821 0.2198 0.135 Uiso 1 1 calc R . .
H7C H 0.8186 -0.0909 0.2141 0.135 Uiso 1 1 calc R . .
C57 C 0.5347(13) 0.2827(10) 0.3652(12) 0.079(3) Uani 1 1 d DU . .
H57 H 0.5699 0.2879 0.3948 0.095 Uiso 1 1 calc R . .
C58 C 0.6025(13) 0.3171(10) 0.2864(11) 0.084(4) Uani 1 1 d DU . .
H58A H 0.5997 0.282 0.2618 0.1 Uiso 1 1 calc R . .
H58B H 0.6526 0.3076 0.3011 0.1 Uiso 1 1 calc R . .
C59 C 0.6231(13) 0.3976(10) 0.2166(12) 0.078(3) Uani 1 1 d DU . .
H59A H 0.6363 0.3917 0.1658 0.093 Uiso 1 1 calc R . .
H59B H 0.6748 0.4216 0.2134 0.093 Uiso 1 1 calc R . .
C60 C 0.5646(14) 0.4572(11) 0.2121(12) 0.077(3) Uani 1 1 d DU . .
H60A H 0.5788 0.4959 0.1531 0.092 Uiso 1 1 calc R . .
H60B H 0.5088 0.4291 0.2311 0.092 Uiso 1 1 calc R . .
C61 C 0.5592(15) 0.5029(10) 0.2581(10) 0.078(3) Uani 1 1 d DU . .
H61A H 0.5128 0.5341 0.2532 0.094 Uiso 1 1 calc R . .
H61B H 0.6103 0.5412 0.2301 0.094 Uiso 1 1 calc R . .
C62 C 0.5474(13) 0.4577(11) 0.3480(10) 0.077(3) Uani 1 1 d DU . .
H62A H 0.5974 0.4322 0.3521 0.092 Uiso 1 1 calc R . .
H62B H 0.5448 0.4967 0.3692 0.092 Uiso 1 1 calc R . .
C63 C 0.4754(13) 0.3961(10) 0.4038(13) 0.079(3) Uani 1 1 d DU . .
H63A H 0.4265 0.4207 0.3938 0.095 Uiso 1 1 calc R . .
H63B H 0.4693 0.3843 0.4608 0.095 Uiso 1 1 calc R . .
C64 C 0.4690(12) 0.3176(10) 0.4037(14) 0.083(3) Uani 1 1 d DU . .
H64A H 0.4454 0.2777 0.4627 0.1 Uiso 1 1 calc R . .
H64B H 0.4258 0.3192 0.3803 0.1 Uiso 1 1 calc R . .
N8 N 0.5269(9) 0.1950(8) 0.4075(9) 0.048(3) Uani 1 1 d U . .
H8A H 0.5703 0.1788 0.3788 0.073 Uiso 1 1 calc R . .
H8B H 0.479 0.1742 0.4102 0.073 Uiso 1 1 calc R . .
H8C H 0.5268 0.1781 0.4596 0.073 Uiso 1 1 calc R . .
C65 C 0.7935(13) 0.2086(9) 0.0799(10) 0.059(2) Uani 1 1 d DU . .
H65 H 0.733 0.1984 0.1126 0.071 Uiso 1 1 calc R . .
C66 C 0.8359(12) 0.2378(10) 0.1196(11) 0.060(2) Uani 1 1 d DU . .
H66A H 0.8954 0.2518 0.0854 0.071 Uiso 1 1 calc R . .
H66B H 0.8304 0.1934 0.1742 0.071 Uiso 1 1 calc R . .
C67 C 0.8065(13) 0.3079(9) 0.1321(11) 0.068(3) Uani 1 1 d DU . .
H67A H 0.7486 0.3093 0.1346 0.082 Uiso 1 1 calc R . .
H67B H 0.8063 0.2988 0.1867 0.082 Uiso 1 1 calc R . .
C68 C 0.8542(14) 0.3882(10) 0.0688(10) 0.078(3) Uani 1 1 d DU . .
H68A H 0.817 0.4282 0.0715 0.093 Uiso 1 1 calc R . .
H68B H 0.8994 0.397 0.0856 0.093 Uiso 1 1 calc R . .
C69 C 0.8912(12) 0.4048(12) -0.0194(10) 0.078(3) Uani 1 1 d DU . .
H69A H 0.9252 0.3627 -0.0222 0.094 Uiso 1 1 calc R . .
H69B H 0.9286 0.4557 -0.0508 0.094 Uiso 1 1 calc R . .
C70 C 0.8314(13) 0.4095(10) -0.0617(13) 0.081(3) Uani 1 1 d DU . .
H70A H 0.7985 0.4523 -0.059 0.097 Uiso 1 1 calc R . .
H70B H 0.8643 0.4272 -0.1208 0.097 Uiso 1 1 calc R . .
C71 C 0.7722(12) 0.3392(9) -0.0337(14) 0.078(3) Uani 1 1 d DU . .
H71A H 0.7512 0.3492 -0.0785 0.094 Uiso 1 1 calc R . .
H71B H 0.7247 0.3349 0.0145 0.094 Uiso 1 1 calc R . .
C72 C 0.8045(13) 0.2596(9) -0.0097(10) 0.064(3) Uani 1 1 d DU . .
H72A H 0.7774 0.2283 -0.0267 0.077 Uiso 1 1 calc R . .
H72B H 0.8642 0.2696 -0.0426 0.077 Uiso 1 1 calc R . .
N9 N 0.8208(11) 0.1297(9) 0.0888(10) 0.059(3) Uani 1 1 d U . .
H9A H 0.7943 0.1097 0.0666 0.088 Uiso 1 1 calc R . .
H9B H 0.8083 0.0953 0.1433 0.088 Uiso 1 1 calc R . .
H9C H 0.8762 0.1366 0.0617 0.088 Uiso 1 1 calc R . .
Pb1 Pb 0.94147(3) 0.00429(3) 0.41858(3) 0.02841(14) Uani 1 1 d U . .
Pb2 Pb 0.68560(3) 0.00544(3) 0.46721(3) 0.02988(14) Uani 1 1 d U . .
Pb3 Pb 0.52528(3) 0.00261(3) 0.33343(3) 0.02724(13) Uani 1 1 d U . .
Pb4 Pb 0.65850(3) 0.00366(3) 0.02094(3) 0.02334(13) Uani 1 1 d U . .
Pb5 Pb 1 0 0 0.03018(19) Uani 1 2 d SU . .
Pb6 Pb 0.75235(3) -0.00078(3) -0.28343(3) 0.02399(13) Uani 1 1 d U . .
Cl1 Cl 0.9797(3) -0.1269(3) 0.5533(3) 0.0493(10) Uani 1 1 d U . .
Cl2 Cl 0.8542(3) 0.1241(2) 0.3372(2) 0.0404(7) Uani 1 1 d U . .
Cl3 Cl 0.8210(2) -0.0978(2) 0.4323(2) 0.0387(7) Uani 1 1 d U . .
Cl4 Cl 0.5 0 0.5 0.0254(7) Uani 1 2 d SU . .
Cl5 Cl 0.3632(2) -0.1200(2) 0.4782(2) 0.0345(7) Uani 1 1 d U . .
Cl6 Cl 0.3907(2) 0.1181(2) 0.3738(2) 0.0335(8) Uani 1 1 d . . .
Cl7 Cl 0.6128(3) -0.1124(3) 0.4060(3) 0.0481(9) Uani 1 1 d U . .
Cl8 Cl 0.6473(2) 0.1164(2) 0.3003(2) 0.0353(6) Uani 1 1 d U . .
Cl9 Cl 0.6384(2) 0.0099(3) 0.1788(2) 0.0425(8) Uani 1 1 d U . .
Cl10 Cl 0.5 0 0 0.0329(9) Uani 1 2 d SU . .
Cl11 Cl 0.7287(2) -0.0163(2) -0.1219(2) 0.0298(6) Uani 1 1 d U . .
Cl12 Cl 0.8262(2) -0.0021(3) 0.0176(2) 0.0384(8) Uani 1 1 d U . .
Cl13 Cl 0.6139(2) -0.1615(2) 0.0968(2) 0.0358(7) Uani 1 1 d U . .
Cl14 Cl 0.7028(2) 0.1685(2) -0.1017(2) 0.0377(7) Uani 1 1 d U . .
Cl15 Cl 1.0097(3) 0.1633(3) -0.0316(3) 0.0558(11) Uani 1 1 d U . .
Cl16 Cl 0.9645(3) -0.0511(3) 0.1709(3) 0.0562(11) Uani 1 1 d U . .
Cl17 Cl 0.5810(2) 0.0041(2) -0.2344(2) 0.0303(7) Uani 1 1 d U . .
Cl18 Cl 0.9233(2) -0.0004(3) -0.2867(2) 0.0386(8) Uani 1 1 d U . .
Cl19 Cl 0.8019(2) 0.0023(2) -0.4452(2) 0.0301(7) Uani 1 1 d U . .
Cl20 Cl 0.7830(2) 0.1650(2) -0.3484(2) 0.0352(7) Uani 1 1 d U . .
Cl21 Cl 0.7195(2) -0.1722(2) -0.1956(2) 0.0327(7) Uani 1 1 d U . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.489(18) . ?
C1 C8 1.510(6) . ?
C1 C2 1.510(6) . ?
C1 H1 1 . ?
C2 C3 1.510(6) . ?
C2 H2D 0.99 . ?
C2 H2E 0.99 . ?
C3 C4 1.510(6) . ?
C3 H3D 0.99 . ?
C3 H3E 0.99 . ?
C4 C5 1.507(6) . ?
C4 H4D 0.99 . ?
C4 H4E 0.99 . ?
C5 C6 1.510(6) . ?
C5 H5D 0.99 . ?
C5 H5E 0.99 . ?
C6 C7 1.507(6) . ?
C6 H6D 0.99 . ?
C6 H6E 0.99 . ?
C7 C8 1.514(6) . ?
C7 H7D 0.99 . ?
C7 H7E 0.99 . ?
C8 H8D 0.99 . ?
C8 H8E 0.99 . ?
N1 H1A 0.91 . ?
N1 H1B 0.91 . ?
N1 H1C 0.91 . ?
C9 C10 1.501(14) . ?
C9 N2 1.50(2) . ?
C9 C16 1.503(14) . ?
C9 H9 1 . ?
C10 C11 1.500(14) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 C12 1.485(15) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 C13 1.474(15) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C13 C14 1.507(15) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 C15 1.461(15) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.510(14) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
N2 H2A 0.91 . ?
N2 H2B 0.91 . ?
N2 H2C 0.91 . ?
C17 N3 1.45(2) . ?
C17 C24 1.459(14) . ?
C17 C18 1.461(14) . ?
C17 H17 1 . ?
C18 C19 1.505(15) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.488(15) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 C21 1.465(15) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.482(15) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 C23 1.444(15) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 C24 1.486(15) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
N3 H3A 0.91 . ?
N3 H3B 0.91 . ?
N3 H3C 0.91 . ?
C25 C32 1.501(14) . ?
C25 C26 1.502(14) . ?
C25 N4 1.53(2) . ?
C25 H25 1 . ?
C26 C27 1.519(15) . ?
C26 H26A 0.99 . ?
C26 H26B 0.99 . ?
C27 C28 1.497(15) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
C28 C29 1.483(15) . ?
C28 H28A 0.99 . ?
C28 H28B 0.99 . ?
C29 C30 1.503(15) . ?
C29 H29A 0.99 . ?
C29 H29B 0.99 . ?
C30 C31 1.485(15) . ?
C30 H30A 0.99 . ?
C30 H30B 0.99 . ?
C31 C32 1.529(14) . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
C32 H32A 0.99 . ?
C32 H32B 0.99 . ?
N4 H4A 0.91 . ?
N4 H4B 0.91 . ?
N4 H4C 0.91 . ?
C33 N5 1.46(2) . ?
C33 C34 1.495(15) . ?
C33 C40 1.509(14) . ?
C33 H33 1 . ?
C34 C35 1.516(15) . ?
C34 H34A 0.99 . ?
C34 H34B 0.99 . ?
C35 C36 1.491(15) . ?
C35 H35A 0.99 . ?
C35 H35B 0.99 . ?
C36 C37 1.461(15) . ?
C36 H36A 0.99 . ?
C36 H36B 0.99 . ?
C37 C38 1.498(15) . ?
C37 H37A 0.99 . ?
C37 H37B 0.99 . ?
C38 C39 1.483(16) . ?
C38 H38A 0.99 . ?
C38 H38B 0.99 . ?
C39 C40 1.520(15) . ?
C39 H39A 0.99 . ?
C39 H39B 0.99 . ?
C40 H40A 0.99 . ?
C40 H40B 0.99 . ?
N5 H5A 0.91 . ?
N5 H5B 0.91 . ?
N5 H5C 0.91 . ?
C41 N6 1.50(3) . ?
C41 C42 1.504(15) . ?
C41 C48 1.509(15) . ?
C41 H41 1 . ?
C42 C43 1.496(15) . ?
C42 H42A 0.99 . ?
C42 H42B 0.99 . ?
C43 C44 1.479(15) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 C45 1.444(16) . ?
C44 H44A 0.99 . ?
C44 H44B 0.99 . ?
C45 C46 1.479(16) . ?
C45 H45A 0.99 . ?
C45 H45B 0.99 . ?
C46 C47 1.462(16) . ?
C46 H46A 0.99 . ?
C46 H46B 0.99 . ?
C47 C48 1.531(15) . ?
C47 H47A 0.99 . ?
C47 H47B 0.99 . ?
C48 H48A 0.99 . ?
C48 H48B 0.99 . ?
N6 H6A 0.91 . ?
N6 H6B 0.91 . ?
N6 H6C 0.91 . ?
C49 N7 1.45(3) . ?
C49 C56 1.476(15) . ?
C49 C50 1.497(15) . ?
C49 H49 1 . ?
C50 C51 1.505(16) . ?
C50 H50A 0.99 . ?
C50 H50B 0.99 . ?
C51 C52 1.479(15) . ?
C51 H51A 0.99 . ?
C51 H51B 0.99 . ?
C52 C53 1.504(16) . ?
C52 H52A 0.99 . ?
C52 H52B 0.99 . ?
C53 C54 1.502(16) . ?
C53 H53A 0.99 . ?
C53 H53B 0.99 . ?
C54 C55 1.462(16) . ?
C54 H54A 0.99 . ?
C54 H54B 0.99 . ?
C55 C56 1.534(16) . ?
C55 H55A 0.99 . ?
C55 H55B 0.99 . ?
C56 H56A 0.99 . ?
C56 H56B 0.99 . ?
N7 H7A 0.91 . ?
N7 H7B 0.91 . ?
N7 H7C 0.91 . ?
C57 C58 1.448(14) . ?
C57 C64 1.458(14) . ?
C57 N8 1.48(2) . ?
C57 H57 1 . ?
C58 C59 1.470(14) . ?
C58 H58A 0.99 . ?
C58 H58B 0.99 . ?
C59 C60 1.489(15) . ?
C59 H59A 0.99 . ?
C59 H59B 0.99 . ?
C60 C61 1.479(15) . ?
C60 H60A 0.99 . ?
C60 H60B 0.99 . ?
C61 C62 1.498(15) . ?
C61 H61A 0.99 . ?
C61 H61B 0.99 . ?
C62 C63 1.471(15) . ?
C62 H62A 0.99 . ?
C62 H62B 0.99 . ?
C63 C64 1.501(14) . ?
C63 H63A 0.99 . ?
C63 H63B 0.99 . ?
C64 H64A 0.99 . ?
C64 H64B 0.99 . ?
N8 H8A 0.91 . ?
N8 H8B 0.91 . ?
N8 H8C 0.91 . ?
C65 C66 1.492(14) . ?
C65 C72 1.508(14) . ?
C65 N9 1.51(2) . ?
C65 H65 1 . ?
C66 C67 1.504(14) . ?
C66 H66A 0.99 . ?
C66 H66B 0.99 . ?
C67 C68 1.500(15) . ?
C67 H67A 0.99 . ?
C67 H67B 0.99 . ?
C68 C69 1.492(15) . ?
C68 H68A 0.99 . ?
C68 H68B 0.99 . ?
C69 C70 1.500(15) . ?
C69 H69A 0.99 . ?
C69 H69B 0.99 . ?
C70 C71 1.485(15) . ?
C70 H70A 0.99 . ?
C70 H70B 0.99 . ?
C71 C72 1.521(15) . ?
C71 H71A 0.99 . ?
C71 H71B 0.99 . ?
C72 H72A 0.99 . ?
C72 H72B 0.99 . ?
N9 H9A 0.91 . ?
N9 H9B 0.91 . ?
N9 H9C 0.91 . ?
Pb1 Cl3 2.765(4) . ?
Pb1 Cl2 2.852(4) . ?
Pb1 Cl18 2.863(4) 2_755 ?
Pb1 Cl19 2.912(3) 1_556 ?
Pb1 Cl1 2.949(4) . ?
Pb1 Cl1 3.073(5) 2_756 ?
Pb2 Cl6 2.786(4) 2_656 ?
Pb2 Cl5 2.814(4) 2_656 ?
Pb2 Cl19 3.024(4) 1_556 ?
Pb2 Cl4 3.0656(8) . ?
Pb2 Cl3 3.109(4) . ?
Pb2 Cl2 3.230(4) . ?
Pb2 Cl8 3.254(4) . ?
Pb3 Cl7 2.745(4) . ?
Pb3 Cl8 2.781(4) . ?
Pb3 Cl9 2.926(4) . ?
Pb3 Cl4 3.0829(8) . ?
Pb3 Cl17 3.113(3) 2_655 ?
Pb3 Cl5 3.245(4) . ?
Pb4 Cl13 2.811(4) . ?
Pb4 Cl11 2.817(3) . ?
Pb4 Cl14 2.889(4) . ?
Pb4 Cl12 2.891(3) . ?
Pb4 Cl10 2.9201(7) . ?
Pb4 Cl9 3.014(4) . ?
Pb5 Cl16 2.841(4) 2_755 ?
Pb5 Cl16 2.841(4) . ?
Pb5 Cl15 2.884(4) 2_755 ?
Pb5 Cl15 2.884(4) . ?
Pb5 Cl12 2.922(3) 2_755 ?
Pb5 Cl12 2.922(3) . ?
Pb6 Cl20 2.815(4) . ?
Pb6 Cl17 2.818(4) . ?
Pb6 Cl11 2.890(3) . ?
Pb6 Cl21 2.893(4) . ?
Pb6 Cl19 2.931(3) . ?
Pb6 Cl18 2.948(4) . ?
Cl1 Pb1 3.073(5) 2_756 ?
Cl4 Pb2 3.0656(8) 2_656 ?
Cl4 Pb3 3.0829(8) 2_656 ?
Cl5 Pb2 2.814(4) 2_656 ?
Cl6 Pb2 2.786(4) 2_656 ?
Cl10 Pb4 2.9201(7) 2_655 ?
Cl17 Pb3 3.113(3) 2_655 ?
Cl18 Pb1 2.863(4) 2_755 ?
Cl19 Pb1 2.912(3) 1_554 ?
Cl19 Pb2 3.024(4) 1_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C8 110.8(11) . . ?
N1 C1 C2 108.2(10) . . ?
C8 C1 C2 117.5(10) . . ?
N1 C1 H1 106.6 . . ?
C8 C1 H1 106.6 . . ?
C2 C1 H1 106.6 . . ?
C3 C2 C1 115.5(11) . . ?
C3 C2 H2D 108.4 . . ?
C1 C2 H2D 108.4 . . ?
C3 C2 H2E 108.4 . . ?
C1 C2 H2E 108.4 . . ?
H2D C2 H2E 107.5 . . ?
C4 C3 C2 117.0(12) . . ?
C4 C3 H3D 108 . . ?
C2 C3 H3D 108 . . ?
C4 C3 H3E 108 . . ?
C2 C3 H3E 108 . . ?
H3D C3 H3E 107.3 . . ?
C5 C4 C3 117.7(12) . . ?
C5 C4 H4D 107.9 . . ?
C3 C4 H4D 107.9 . . ?
C5 C4 H4E 107.9 . . ?
C3 C4 H4E 107.9 . . ?
H4D C4 H4E 107.2 . . ?
C4 C5 C6 117.3(12) . . ?
C4 C5 H5D 108 . . ?
C6 C5 H5D 108 . . ?
C4 C5 H5E 108 . . ?
C6 C5 H5E 108 . . ?
H5D C5 H5E 107.2 . . ?
C7 C6 C5 117.4(11) . . ?
C7 C6 H6D 107.9 . . ?
C5 C6 H6D 107.9 . . ?
C7 C6 H6E 107.9 . . ?
C5 C6 H6E 107.9 . . ?
H6D C6 H6E 107.2 . . ?
C6 C7 C8 117.9(11) . . ?
C6 C7 H7D 107.8 . . ?
C8 C7 H7D 107.8 . . ?
C6 C7 H7E 107.8 . . ?
C8 C7 H7E 107.8 . . ?
H7D C7 H7E 107.2 . . ?
C1 C8 C7 119.6(11) . . ?
C1 C8 H8D 107.4 . . ?
C7 C8 H8D 107.4 . . ?
C1 C8 H8E 107.4 . . ?
C7 C8 H8E 107.4 . . ?
H8D C8 H8E 106.9 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C10 C9 N2 109.3(12) . . ?
C10 C9 C16 118.2(14) . . ?
N2 C9 C16 107.5(12) . . ?
C10 C9 H9 107.1 . . ?
N2 C9 H9 107.1 . . ?
C16 C9 H9 107.1 . . ?
C11 C10 C9 116.9(14) . . ?
C11 C10 H10A 108.1 . . ?
C9 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
C9 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
C12 C11 C10 120.4(15) . . ?
C12 C11 H11A 107.2 . . ?
C10 C11 H11A 107.2 . . ?
C12 C11 H11B 107.2 . . ?
C10 C11 H11B 107.2 . . ?
H11A C11 H11B 106.9 . . ?
C13 C12 C11 119.6(16) . . ?
C13 C12 H12A 107.4 . . ?
C11 C12 H12A 107.4 . . ?
C13 C12 H12B 107.4 . . ?
C11 C12 H12B 107.4 . . ?
H12A C12 H12B 107 . . ?
C12 C13 C14 115.9(16) . . ?
C12 C13 H13A 108.3 . . ?
C14 C13 H13A 108.3 . . ?
C12 C13 H13B 108.3 . . ?
C14 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C15 C14 C13 122.2(15) . . ?
C15 C14 H14A 106.8 . . ?
C13 C14 H14A 106.8 . . ?
C15 C14 H14B 106.8 . . ?
C13 C14 H14B 106.8 . . ?
H14A C14 H14B 106.6 . . ?
C14 C15 C16 124.6(16) . . ?
C14 C15 H15A 106.2 . . ?
C16 C15 H15A 106.2 . . ?
C14 C15 H15B 106.2 . . ?
C16 C15 H15B 106.2 . . ?
H15A C15 H15B 106.4 . . ?
C9 C16 C15 117.9(13) . . ?
C9 C16 H16A 107.8 . . ?
C15 C16 H16A 107.8 . . ?
C9 C16 H16B 107.8 . . ?
C15 C16 H16B 107.8 . . ?
H16A C16 H16B 107.2 . . ?
C9 N2 H2A 109.5 . . ?
C9 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C9 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N3 C17 C24 113.8(15) . . ?
N3 C17 C18 115.1(14) . . ?
C24 C17 C18 130.0(16) . . ?
N3 C17 H17 93.5 . . ?
C24 C17 H17 93.5 . . ?
C18 C17 H17 93.5 . . ?
C17 C18 C19 121.6(16) . . ?
C17 C18 H18A 106.9 . . ?
C19 C18 H18A 106.9 . . ?
C17 C18 H18B 106.9 . . ?
C19 C18 H18B 106.9 . . ?
H18A C18 H18B 106.7 . . ?
C20 C19 C18 117.0(17) . . ?
C20 C19 H19A 108 . . ?
C18 C19 H19A 108 . . ?
C20 C19 H19B 108 . . ?
C18 C19 H19B 108 . . ?
H19A C19 H19B 107.3 . . ?
C21 C20 C19 121.1(16) . . ?
C21 C20 H20A 107 . . ?
C19 C20 H20A 107 . . ?
C21 C20 H20B 107.1 . . ?
C19 C20 H20B 107.1 . . ?
H20A C20 H20B 106.8 . . ?
C20 C21 C22 121.3(18) . . ?
C20 C21 H21A 107 . . ?
C22 C21 H21A 107 . . ?
C20 C21 H21B 107 . . ?
C22 C21 H21B 107 . . ?
H21A C21 H21B 106.7 . . ?
C23 C22 C21 126.5(17) . . ?
C23 C22 H22A 105.7 . . ?
C21 C22 H22A 105.7 . . ?
C23 C22 H22B 105.7 . . ?
C21 C22 H22B 105.7 . . ?
H22A C22 H22B 106.1 . . ?
C22 C23 C24 127.9(18) . . ?
C22 C23 H23A 105.3 . . ?
C24 C23 H23A 105.3 . . ?
C22 C23 H23B 105.3 . . ?
C24 C23 H23B 105.3 . . ?
H23A C23 H23B 106 . . ?
C17 C24 C23 126.8(16) . . ?
C17 C24 H24A 105.6 . . ?
C23 C24 H24A 105.6 . . ?
C17 C24 H24B 105.6 . . ?
C23 C24 H24B 105.6 . . ?
H24A C24 H24B 106.1 . . ?
C17 N3 H3A 109.5 . . ?
C17 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C17 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C32 C25 C26 119.6(14) . . ?
C32 C25 N4 106.9(13) . . ?
C26 C25 N4 107.1(12) . . ?
C32 C25 H25 107.5 . . ?
C26 C25 H25 107.5 . . ?
N4 C25 H25 107.5 . . ?
C25 C26 C27 115.0(14) . . ?
C25 C26 H26A 108.5 . . ?
C27 C26 H26A 108.5 . . ?
C25 C26 H26B 108.5 . . ?
C27 C26 H26B 108.5 . . ?
H26A C26 H26B 107.5 . . ?
C28 C27 C26 115.0(15) . . ?
C28 C27 H27A 108.5 . . ?
C26 C27 H27A 108.5 . . ?
C28 C27 H27B 108.5 . . ?
C26 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C29 C28 C27 117.8(15) . . ?
C29 C28 H28A 107.9 . . ?
C27 C28 H28A 107.9 . . ?
C29 C28 H28B 107.9 . . ?
C27 C28 H28B 107.9 . . ?
H28A C28 H28B 107.2 . . ?
C28 C29 C30 116.9(17) . . ?
C28 C29 H29A 108.1 . . ?
C30 C29 H29A 108.1 . . ?
C28 C29 H29B 108.1 . . ?
C30 C29 H29B 108.1 . . ?
H29A C29 H29B 107.3 . . ?
C31 C30 C29 119.6(15) . . ?
C31 C30 H30A 107.4 . . ?
C29 C30 H30A 107.4 . . ?
C31 C30 H30B 107.4 . . ?
C29 C30 H30B 107.4 . . ?
H30A C30 H30B 106.9 . . ?
C30 C31 C32 116.4(15) . . ?
C30 C31 H31A 108.2 . . ?
C32 C31 H31A 108.2 . . ?
C30 C31 H31B 108.2 . . ?
C32 C31 H31B 108.2 . . ?
H31A C31 H31B 107.4 . . ?
C25 C32 C31 115.1(14) . . ?
C25 C32 H32A 108.5 . . ?
C31 C32 H32A 108.5 . . ?
C25 C32 H32B 108.5 . . ?
C31 C32 H32B 108.5 . . ?
H32A C32 H32B 107.5 . . ?
C25 N4 H4A 109.5 . . ?
C25 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C25 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
N5 C33 C34 110.3(15) . . ?
N5 C33 C40 107.4(14) . . ?
C34 C33 C40 118.3(15) . . ?
N5 C33 H33 106.7 . . ?
C34 C33 H33 106.7 . . ?
C40 C33 H33 106.7 . . ?
C33 C34 C35 116.2(15) . . ?
C33 C34 H34A 108.2 . . ?
C35 C34 H34A 108.2 . . ?
C33 C34 H34B 108.2 . . ?
C35 C34 H34B 108.2 . . ?
H34A C34 H34B 107.4 . . ?
C36 C35 C34 118.9(16) . . ?
C36 C35 H35A 107.6 . . ?
C34 C35 H35A 107.6 . . ?
C36 C35 H35B 107.6 . . ?
C34 C35 H35B 107.6 . . ?
H35A C35 H35B 107 . . ?
C37 C36 C35 125.7(19) . . ?
C37 C36 H36A 105.9 . . ?
C35 C36 H36A 105.9 . . ?
C37 C36 H36B 105.9 . . ?
C35 C36 H36B 105.9 . . ?
H36A C36 H36B 106.2 . . ?
C36 C37 C38 122.0(17) . . ?
C36 C37 H37A 106.8 . . ?
C38 C37 H37A 106.8 . . ?
C36 C37 H37B 106.8 . . ?
C38 C37 H37B 106.8 . . ?
H37A C37 H37B 106.7 . . ?
C39 C38 C37 117.2(17) . . ?
C39 C38 H38A 108 . . ?
C37 C38 H38A 108 . . ?
C39 C38 H38B 108 . . ?
C37 C38 H38B 108 . . ?
H38A C38 H38B 107.2 . . ?
C38 C39 C40 115.8(16) . . ?
C38 C39 H39A 108.3 . . ?
C40 C39 H39A 108.3 . . ?
C38 C39 H39B 108.3 . . ?
C40 C39 H39B 108.3 . . ?
H39A C39 H39B 107.4 . . ?
C33 C40 C39 118.2(15) . . ?
C33 C40 H40A 107.8 . . ?
C39 C40 H40A 107.8 . . ?
C33 C40 H40B 107.8 . . ?
C39 C40 H40B 107.8 . . ?
H40A C40 H40B 107.1 . . ?
C33 N5 H5A 109.5 . . ?
C33 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C33 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
N6 C41 C42 104.4(17) . . ?
N6 C41 C48 110.5(16) . . ?
C42 C41 C48 117.5(17) . . ?
N6 C41 H41 108.1 . . ?
C42 C41 H41 108.1 . . ?
C48 C41 H41 108.1 . . ?
C43 C42 C41 116.9(18) . . ?
C43 C42 H42A 108.1 . . ?
C41 C42 H42A 108.1 . . ?
C43 C42 H42B 108.1 . . ?
C41 C42 H42B 108.1 . . ?
H42A C42 H42B 107.3 . . ?
C44 C43 C42 116.7(17) . . ?
C44 C43 H43A 108.1 . . ?
C42 C43 H43A 108.1 . . ?
C44 C43 H43B 108.1 . . ?
C42 C43 H43B 108.1 . . ?
H43A C43 H43B 107.3 . . ?
C45 C44 C43 128(2) . . ?
C45 C44 H44A 105.2 . . ?
C43 C44 H44A 105.2 . . ?
C45 C44 H44B 105.2 . . ?
C43 C44 H44B 105.2 . . ?
H44A C44 H44B 105.9 . . ?
C44 C45 C46 125(2) . . ?
C44 C45 H45A 106 . . ?
C46 C45 H45A 106 . . ?
C44 C45 H45B 106 . . ?
C46 C45 H45B 106 . . ?
H45A C45 H45B 106.3 . . ?
C47 C46 C45 123.3(18) . . ?
C47 C46 H46A 106.5 . . ?
C45 C46 H46A 106.5 . . ?
C47 C46 H46B 106.5 . . ?
C45 C46 H46B 106.5 . . ?
H46A C46 H46B 106.5 . . ?
C46 C47 C48 115.7(18) . . ?
C46 C47 H47A 108.4 . . ?
C48 C47 H47A 108.4 . . ?
C46 C47 H47B 108.4 . . ?
C48 C47 H47B 108.4 . . ?
H47A C47 H47B 107.4 . . ?
C41 C48 C47 119.6(15) . . ?
C41 C48 H48A 107.4 . . ?
C47 C48 H48A 107.4 . . ?
C41 C48 H48B 107.4 . . ?
C47 C48 H48B 107.4 . . ?
H48A C48 H48B 106.9 . . ?
C41 N6 H6A 109.5 . . ?
C41 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C41 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
N7 C49 C56 116.0(18) . . ?
N7 C49 C50 108.9(16) . . ?
C56 C49 C50 120.4(18) . . ?
N7 C49 H49 102.9 . . ?
C56 C49 H49 102.9 . . ?
C50 C49 H49 102.9 . . ?
C49 C50 C51 117.4(18) . . ?
C49 C50 H50A 107.9 . . ?
C51 C50 H50A 107.9 . . ?
C49 C50 H50B 107.9 . . ?
C51 C50 H50B 107.9 . . ?
H50A C50 H50B 107.2 . . ?
C52 C51 C50 116.6(16) . . ?
C52 C51 H51A 108.1 . . ?
C50 C51 H51A 108.1 . . ?
C52 C51 H51B 108.1 . . ?
C50 C51 H51B 108.1 . . ?
H51A C51 H51B 107.3 . . ?
C51 C52 C53 121.9(16) . . ?
C51 C52 H52A 106.9 . . ?
C53 C52 H52A 106.8 . . ?
C51 C52 H52B 106.8 . . ?
C53 C52 H52B 106.8 . . ?
H52A C52 H52B 106.7 . . ?
C54 C53 C52 114.1(19) . . ?
C54 C53 H53A 108.7 . . ?
C52 C53 H53A 108.7 . . ?
C54 C53 H53B 108.7 . . ?
C52 C53 H53B 108.7 . . ?
H53A C53 H53B 107.6 . . ?
C55 C54 C53 121.0(17) . . ?
C55 C54 H54A 107.1 . . ?
C53 C54 H54A 107.1 . . ?
C55 C54 H54B 107.1 . . ?
C53 C54 H54B 107.1 . . ?
H54A C54 H54B 106.8 . . ?
C54 C55 C56 115.9(18) . . ?
C54 C55 H55A 108.3 . . ?
C56 C55 H55A 108.3 . . ?
C54 C55 H55B 108.3 . . ?
C56 C55 H55B 108.3 . . ?
H55A C55 H55B 107.4 . . ?
C49 C56 C55 116.0(18) . . ?
C49 C56 H56A 108.3 . . ?
C55 C56 H56A 108.3 . . ?
C49 C56 H56B 108.3 . . ?
C55 C56 H56B 108.3 . . ?
H56A C56 H56B 107.4 . . ?
C49 N7 H7A 109.5 . . ?
C49 N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C49 N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C58 C57 C64 131.7(16) . . ?
C58 C57 N8 111.9(13) . . ?
C64 C57 N8 115.8(14) . . ?
C58 C57 H57 92.3 . . ?
C64 C57 H57 92.3 . . ?
N8 C57 H57 92.3 . . ?
C57 C58 C59 131.1(15) . . ?
C57 C58 H58A 104.5 . . ?
C59 C58 H58A 104.5 . . ?
C57 C58 H58B 104.5 . . ?
C59 C58 H58B 104.5 . . ?
H58A C58 H58B 105.6 . . ?
C58 C59 C60 121.8(15) . . ?
C58 C59 H59A 106.9 . . ?
C60 C59 H59A 106.9 . . ?
C58 C59 H59B 106.9 . . ?
C60 C59 H59B 106.9 . . ?
H59A C59 H59B 106.7 . . ?
C61 C60 C59 119.6(17) . . ?
C61 C60 H60A 107.4 . . ?
C59 C60 H60A 107.4 . . ?
C61 C60 H60B 107.4 . . ?
C59 C60 H60B 107.4 . . ?
H60A C60 H60B 107 . . ?
C60 C61 C62 117.9(15) . . ?
C60 C61 H61A 107.8 . . ?
C62 C61 H61A 107.8 . . ?
C60 C61 H61B 107.8 . . ?
C62 C61 H61B 107.8 . . ?
H61A C61 H61B 107.2 . . ?
C63 C62 C61 118.8(17) . . ?
C63 C62 H62A 107.6 . . ?
C61 C62 H62A 107.6 . . ?
C63 C62 H62B 107.6 . . ?
C61 C62 H62B 107.6 . . ?
H62A C62 H62B 107 . . ?
C62 C63 C64 122.6(15) . . ?
C62 C63 H63A 106.7 . . ?
C64 C63 H63A 106.7 . . ?
C62 C63 H63B 106.7 . . ?
C64 C63 H63B 106.7 . . ?
H63A C63 H63B 106.6 . . ?
C57 C64 C63 127.6(16) . . ?
C57 C64 H64A 105.4 . . ?
C63 C64 H64A 105.4 . . ?
C57 C64 H64B 105.4 . . ?
C63 C64 H64B 105.4 . . ?
H64A C64 H64B 106 . . ?
C57 N8 H8A 109.5 . . ?
C57 N8 H8B 109.5 . . ?
H8A N8 H8B 109.5 . . ?
C57 N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C66 C65 C72 119.3(14) . . ?
C66 C65 N9 107.7(13) . . ?
C72 C65 N9 107.4(13) . . ?
C66 C65 H65 107.3 . . ?
C72 C65 H65 107.3 . . ?
N9 C65 H65 107.3 . . ?
C65 C66 C67 117.0(15) . . ?
C65 C66 H66A 108.1 . . ?
C67 C66 H66A 108.1 . . ?
C65 C66 H66B 108.1 . . ?
C67 C66 H66B 108.1 . . ?
H66A C66 H66B 107.3 . . ?
C68 C67 C66 117.4(14) . . ?
C68 C67 H67A 108 . . ?
C66 C67 H67A 108 . . ?
C68 C67 H67B 108 . . ?
C66 C67 H67B 108 . . ?
H67A C67 H67B 107.2 . . ?
C69 C68 C67 118.7(14) . . ?
C69 C68 H68A 107.6 . . ?
C67 C68 H68A 107.6 . . ?
C69 C68 H68B 107.6 . . ?
C67 C68 H68B 107.6 . . ?
H68A C68 H68B 107.1 . . ?
C68 C69 C70 116.0(16) . . ?
C68 C69 H69A 108.3 . . ?
C70 C69 H69A 108.3 . . ?
C68 C69 H69B 108.3 . . ?
C70 C69 H69B 108.3 . . ?
H69A C69 H69B 107.4 . . ?
C71 C70 C69 121.0(15) . . ?
C71 C70 H70A 107.1 . . ?
C69 C70 H70A 107.1 . . ?
C71 C70 H70B 107.1 . . ?
C69 C70 H70B 107.1 . . ?
H70A C70 H70B 106.8 . . ?
C70 C71 C72 117.0(15) . . ?
C70 C71 H71A 108.1 . . ?
C72 C71 H71A 108.1 . . ?
C70 C71 H71B 108.1 . . ?
C72 C71 H71B 108.1 . . ?
H71A C71 H71B 107.3 . . ?
C65 C72 C71 118.0(15) . . ?
C65 C72 H72A 107.8 . . ?
C71 C72 H72A 107.8 . . ?
C65 C72 H72B 107.8 . . ?
C71 C72 H72B 107.8 . . ?
H72A C72 H72B 107.1 . . ?
C65 N9 H9A 109.5 . . ?
C65 N9 H9B 109.5 . . ?
H9A N9 H9B 109.5 . . ?
C65 N9 H9C 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
Cl3 Pb1 Cl2 83.66(12) . . ?
Cl3 Pb1 Cl18 100.12(11) . 2_755 ?
Cl2 Pb1 Cl18 104.31(12) . 2_755 ?
Cl3 Pb1 Cl19 78.17(10) . 1_556 ?
Cl2 Pb1 Cl19 76.72(11) . 1_556 ?
Cl18 Pb1 Cl19 177.95(11) 2_755 1_556 ?
Cl3 Pb1 Cl1 90.32(12) . . ?
Cl2 Pb1 Cl1 159.61(12) . . ?
Cl18 Pb1 Cl1 95.92(12) 2_755 . ?
Cl19 Pb1 Cl1 82.99(12) 1_556 . ?
Cl3 Pb1 Cl1 159.21(11) . 2_756 ?
Cl2 Pb1 Cl1 88.16(11) . 2_756 ?
Cl18 Pb1 Cl1 100.42(12) 2_755 2_756 ?
Cl19 Pb1 Cl1 81.35(11) 1_556 2_756 ?
Cl1 Pb1 Cl1 90.78(12) . 2_756 ?
Cl6 Pb2 Cl5 91.65(11) 2_656 2_656 ?
Cl6 Pb2 Cl19 76.33(10) 2_656 1_556 ?
Cl5 Pb2 Cl19 76.77(10) 2_656 1_556 ?
Cl6 Pb2 Cl4 74.27(7) 2_656 . ?
Cl5 Pb2 Cl4 75.18(7) 2_656 . ?
Cl19 Pb2 Cl4 138.27(7) 1_556 . ?
Cl6 Pb2 Cl3 89.68(11) 2_656 . ?
Cl5 Pb2 Cl3 146.90(10) 2_656 . ?
Cl19 Pb2 Cl3 71.44(9) 1_556 . ?
Cl4 Pb2 Cl3 136.44(7) . . ?
Cl6 Pb2 Cl2 145.11(10) 2_656 . ?
Cl5 Pb2 Cl2 88.25(11) 2_656 . ?
Cl19 Pb2 Cl2 69.70(9) 1_556 . ?
Cl4 Pb2 Cl2 138.59(7) . . ?
Cl3 Pb2 Cl2 72.44(11) . . ?
Cl6 Pb2 Cl8 140.74(10) 2_656 . ?
Cl5 Pb2 Cl8 88.89(10) 2_656 . ?
Cl19 Pb2 Cl8 141.28(9) 1_556 . ?
Cl4 Pb2 Cl8 67.97(7) . . ?
Cl3 Pb2 Cl8 110.32(10) . . ?
Cl2 Pb2 Cl8 74.15(9) . . ?
Cl7 Pb3 Cl8 88.53(13) . . ?
Cl7 Pb3 Cl9 84.57(12) . . ?
Cl8 Pb3 Cl9 82.53(11) . . ?
Cl7 Pb3 Cl4 74.58(9) . . ?
Cl8 Pb3 Cl4 73.98(7) . . ?
Cl9 Pb3 Cl4 148.69(8) . . ?
Cl7 Pb3 Cl17 127.00(13) . 2_655 ?
Cl8 Pb3 Cl17 132.70(10) . 2_655 ?
Cl9 Pb3 Cl17 72.65(10) . 2_655 ?
Cl4 Pb3 Cl17 138.66(7) . 2_655 ?
Cl7 Pb3 Cl5 85.21(11) . . ?
Cl8 Pb3 Cl5 142.92(10) . . ?
Cl9 Pb3 Cl5 132.88(11) . . ?
Cl4 Pb3 Cl5 69.12(6) . . ?
Cl17 Pb3 Cl5 77.54(9) 2_655 . ?
Cl13 Pb4 Cl11 82.61(11) . . ?
Cl13 Pb4 Cl14 161.68(11) . . ?
Cl11 Pb4 Cl14 80.95(11) . . ?
Cl13 Pb4 Cl12 95.91(12) . . ?
Cl11 Pb4 Cl12 81.80(10) . . ?
Cl14 Pb4 Cl12 89.71(12) . . ?
Cl13 Pb4 Cl10 80.78(8) . . ?
Cl11 Pb4 Cl10 87.54(7) . . ?
Cl14 Pb4 Cl10 90.47(8) . . ?
Cl12 Pb4 Cl10 169.17(7) . . ?
Cl13 Pb4 Cl9 95.11(12) . . ?
Cl11 Pb4 Cl9 160.65(10) . . ?
Cl14 Pb4 Cl9 103.08(12) . . ?
Cl12 Pb4 Cl9 79.32(10) . . ?
Cl10 Pb4 Cl9 111.15(8) . . ?
Cl16 Pb5 Cl16 180.0(2) 2_755 . ?
Cl16 Pb5 Cl15 90.31(15) 2_755 2_755 ?
Cl16 Pb5 Cl15 89.69(15) . 2_755 ?
Cl16 Pb5 Cl15 89.69(15) 2_755 . ?
Cl16 Pb5 Cl15 90.31(15) . . ?
Cl15 Pb5 Cl15 180.0(4) 2_755 . ?
Cl16 Pb5 Cl12 93.35(11) 2_755 2_755 ?
Cl16 Pb5 Cl12 86.65(11) . 2_755 ?
Cl15 Pb5 Cl12 90.16(12) 2_755 2_755 ?
Cl15 Pb5 Cl12 89.84(12) . 2_755 ?
Cl16 Pb5 Cl12 86.65(11) 2_755 . ?
Cl16 Pb5 Cl12 93.35(11) . . ?
Cl15 Pb5 Cl12 89.84(12) 2_755 . ?
Cl15 Pb5 Cl12 90.16(12) . . ?
Cl12 Pb5 Cl12 180.00(18) 2_755 . ?
Cl20 Pb6 Cl17 90.60(11) . . ?
Cl20 Pb6 Cl11 88.84(11) . . ?
Cl17 Pb6 Cl11 83.27(10) . . ?
Cl20 Pb6 Cl21 172.25(10) . . ?
Cl17 Pb6 Cl21 89.01(10) . . ?
Cl11 Pb6 Cl21 83.43(10) . . ?
Cl20 Pb6 Cl19 94.78(10) . . ?
Cl17 Pb6 Cl19 105.80(10) . . ?
Cl11 Pb6 Cl19 170.16(10) . . ?
Cl21 Pb6 Cl19 92.78(10) . . ?
Cl20 Pb6 Cl18 85.62(11) . . ?
Cl17 Pb6 Cl18 161.56(10) . . ?
Cl11 Pb6 Cl18 78.61(10) . . ?
Cl21 Pb6 Cl18 92.31(11) . . ?
Cl19 Pb6 Cl18 92.51(10) . . ?
Pb1 Cl1 Pb1 89.22(12) . 2_756 ?
Pb1 Cl2 Pb2 87.76(10) . . ?
Pb1 Cl3 Pb2 91.78(11) . . ?
Pb2 Cl4 Pb2 180 . 2_656 ?
Pb2 Cl4 Pb3 88.467(15) . 2_656 ?
Pb2 Cl4 Pb3 91.533(15) 2_656 2_656 ?
Pb2 Cl4 Pb3 91.533(15) . . ?
Pb2 Cl4 Pb3 88.467(15) 2_656 . ?
Pb3 Cl4 Pb3 180 2_656 . ?
Pb2 Cl5 Pb3 89.85(10) 2_656 . ?
Pb3 Cl8 Pb2 93.43(11) . . ?
Pb3 Cl9 Pb4 147.36(15) . . ?
Pb4 Cl10 Pb4 180.00(2) . 2_655 ?
Pb4 Cl11 Pb6 158.07(14) . . ?
Pb4 Cl12 Pb5 175.43(17) . . ?
Pb6 Cl17 Pb3 123.60(12) . 2_655 ?
Pb1 Cl18 Pb6 122.52(13) 2_755 . ?
Pb1 Cl19 Pb6 144.37(14) 1_554 . ?
Pb1 Cl19 Pb2 90.74(9) 1_554 1_554 ?
Pb6 Cl19 Pb2 124.90(12) . 1_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

N1 C1 C2 C3 -169.7(11) . . . . ?
C8 C1 C2 C3 -43.3(18) . . . . ?
C1 C2 C3 C4 101.4(16) . . . . ?
C2 C3 C4 C5 -67.8(19) . . . . ?
C3 C4 C5 C6 65.1(19) . . . . ?
C4 C5 C6 C7 -98.0(17) . . . . ?
C5 C6 C7 C8 43.3(19) . . . . ?
N1 C1 C8 C7 62.7(16) . . . . ?
C2 C1 C8 C7 -62.4(18) . . . . ?
C6 C7 C8 C1 62.6(19) . . . . ?
N2 C9 C10 C11 135.9(17) . . . . ?
C16 C9 C10 C11 -101(2) . . . . ?
C9 C10 C11 C12 59(3) . . . . ?
C10 C11 C12 C13 -58(3) . . . . ?
C11 C12 C13 C14 97(2) . . . . ?
C12 C13 C14 C15 -54(3) . . . . ?
C13 C14 C15 C16 -45(3) . . . . ?
C10 C9 C16 C15 52(2) . . . . ?
N2 C9 C16 C15 175.8(16) . . . . ?
C14 C15 C16 C9 48(3) . . . . ?
N3 C17 C18 C19 171(2) . . . . ?
C24 C17 C18 C19 4(5) . . . . ?
C17 C18 C19 C20 79(3) . . . . ?
C18 C19 C20 C21 -55(3) . . . . ?
C19 C20 C21 C22 -46(4) . . . . ?
C20 C21 C22 C23 52(4) . . . . ?
C21 C22 C23 C24 34(5) . . . . ?
N3 C17 C24 C23 168(3) . . . . ?
C18 C17 C24 C23 -25(5) . . . . ?
C22 C23 C24 C17 -40(5) . . . . ?
C32 C25 C26 C27 -69(2) . . . . ?
N4 C25 C26 C27 169.7(14) . . . . ?
C25 C26 C27 C28 100(2) . . . . ?
C26 C27 C28 C29 -45(3) . . . . ?
C27 C28 C29 C30 -63(3) . . . . ?
C28 C29 C30 C31 69(3) . . . . ?
C29 C30 C31 C32 36(3) . . . . ?
C26 C25 C32 C31 69(2) . . . . ?
N4 C25 C32 C31 -169.0(14) . . . . ?
C30 C31 C32 C25 -96(2) . . . . ?
N5 C33 C34 C35 166.9(18) . . . . ?
C40 C33 C34 C35 -69(3) . . . . ?
C33 C34 C35 C36 -33(3) . . . . ?
C34 C35 C36 C37 89(3) . . . . ?
C35 C36 C37 C38 -55(4) . . . . ?
C36 C37 C38 C39 56(3) . . . . ?
C37 C38 C39 C40 -96(2) . . . . ?
N5 C33 C40 C39 -167.4(19) . . . . ?
C34 C33 C40 C39 67(3) . . . . ?
C38 C39 C40 C33 44(3) . . . . ?
N6 C41 C42 C43 134(2) . . . . ?
C48 C41 C42 C43 -104(3) . . . . ?
C41 C42 C43 C44 64(3) . . . . ?
C42 C43 C44 C45 -47(4) . . . . ?
C43 C44 C45 C46 79(4) . . . . ?
C44 C45 C46 C47 -39(4) . . . . ?
C45 C46 C47 C48 -57(4) . . . . ?
N6 C41 C48 C47 155(2) . . . . ?
C42 C41 C48 C47 35(3) . . . . ?
C46 C47 C48 C41 64(3) . . . . ?
N7 C49 C50 C51 149(2) . . . . ?
C56 C49 C50 C51 -74(3) . . . . ?
C49 C50 C51 C52 90(3) . . . . ?
C50 C51 C52 C53 -22(4) . . . . ?
C51 C52 C53 C54 -76(3) . . . . ?
C52 C53 C54 C55 62(3) . . . . ?
C53 C54 C55 C56 42(4) . . . . ?
N7 C49 C56 C55 -156(2) . . . . ?
C50 C49 C56 C55 69(3) . . . . ?
C54 C55 C56 C49 -95(3) . . . . ?
C64 C57 C58 C59 -6(5) . . . . ?
N8 C57 C58 C59 166(3) . . . . ?
C57 C58 C59 C60 -10(5) . . . . ?
C58 C59 C60 C61 82(3) . . . . ?
C59 C60 C61 C62 -51(3) . . . . ?
C60 C61 C62 C63 -57(3) . . . . ?
C61 C62 C63 C64 73(3) . . . . ?
C58 C57 C64 C63 -41(5) . . . . ?
N8 C57 C64 C63 148(2) . . . . ?
C62 C63 C64 C57 14(4) . . . . ?
C72 C65 C66 C67 68(2) . . . . ?
N9 C65 C66 C67 -169.1(15) . . . . ?
C65 C66 C67 C68 -98(2) . . . . ?
C66 C67 C68 C69 35(3) . . . . ?
C67 C68 C69 C70 68(3) . . . . ?
C68 C69 C70 C71 -64(3) . . . . ?
C69 C70 C71 C72 -41(3) . . . . ?
C66 C65 C72 C71 -64(2) . . . . ?
N9 C65 C72 C71 173.2(15) . . . . ?
C70 C71 C72 C65 93(2) . . . . ?
Cl3 Pb1 Cl1 Pb1 -159.23(11) . . . 2_756 ?
Cl2 Pb1 Cl1 Pb1 -86.8(3) . . . 2_756 ?
Cl18 Pb1 Cl1 Pb1 100.55(12) 2_755 . . 2_756 ?
Cl19 Pb1 Cl1 Pb1 -81.19(11) 1_556 . . 2_756 ?
Cl1 Pb1 Cl1 Pb1 0 2_756 . . 2_756 ?
Cl3 Pb1 Cl2 Pb2 37.03(10) . . . . ?
Cl18 Pb1 Cl2 Pb2 135.90(10) 2_755 . . . ?
Cl19 Pb1 Cl2 Pb2 -42.27(9) 1_556 . . . ?
Cl1 Pb1 Cl2 Pb2 -36.5(4) . . . . ?
Cl1 Pb1 Cl2 Pb2 -123.82(11) 2_756 . . . ?
Cl6 Pb2 Cl2 Pb1 28.4(2) 2_656 . . . ?
Cl5 Pb2 Cl2 Pb1 118.77(11) 2_656 . . . ?
Cl19 Pb2 Cl2 Pb1 42.23(9) 1_556 . . . ?
Cl4 Pb2 Cl2 Pb1 -176.17(3) . . . . ?
Cl3 Pb2 Cl2 Pb1 -33.95(10) . . . . ?
Cl8 Pb2 Cl2 Pb1 -151.89(12) . . . . ?
Cl2 Pb1 Cl3 Pb2 -38.72(11) . . . . ?
Cl18 Pb1 Cl3 Pb2 -142.18(11) 2_755 . . . ?
Cl19 Pb1 Cl3 Pb2 38.99(10) 1_556 . . . ?
Cl1 Pb1 Cl3 Pb2 121.76(12) . . . . ?
Cl1 Pb1 Cl3 Pb2 28.7(4) 2_756 . . . ?
Cl6 Pb2 Cl3 Pb1 -114.40(11) 2_656 . . . ?
Cl5 Pb2 Cl3 Pb1 -21.9(2) 2_656 . . . ?
Cl19 Pb2 Cl3 Pb1 -38.72(10) 1_556 . . . ?
Cl4 Pb2 Cl3 Pb1 179.15(3) . . . . ?
Cl2 Pb2 Cl3 Pb1 35.16(10) . . . . ?
Cl8 Pb2 Cl3 Pb1 100.15(11) . . . . ?
Cl6 Pb2 Cl4 Pb3 49.32(8) 2_656 . . 2_656 ?
Cl5 Pb2 Cl4 Pb3 -46.73(8) 2_656 . . 2_656 ?
Cl19 Pb2 Cl4 Pb3 2.54(10) 1_556 . . 2_656 ?
Cl3 Pb2 Cl4 Pb3 121.58(11) . . . 2_656 ?
Cl2 Pb2 Cl4 Pb3 -116.37(11) . . . 2_656 ?
Cl8 Pb2 Cl4 Pb3 -141.64(7) . . . 2_656 ?
Cl6 Pb2 Cl4 Pb3 -130.68(8) 2_656 . . . ?
Cl5 Pb2 Cl4 Pb3 133.27(8) 2_656 . . . ?
Cl19 Pb2 Cl4 Pb3 -177.46(10) 1_556 . . . ?
Cl3 Pb2 Cl4 Pb3 -58.42(11) . . . . ?
Cl2 Pb2 Cl4 Pb3 63.63(11) . . . . ?
Cl8 Pb2 Cl4 Pb3 38.36(7) . . . . ?
Cl7 Pb3 Cl4 Pb2 48.49(10) . . . . ?
Cl8 Pb3 Cl4 Pb2 -44.47(9) . . . . ?
Cl9 Pb3 Cl4 Pb2 -1.55(18) . . . . ?
Cl17 Pb3 Cl4 Pb2 177.65(11) 2_655 . . . ?
Cl5 Pb3 Cl4 Pb2 139.20(7) . . . . ?
Cl7 Pb3 Cl4 Pb2 -131.51(10) . . . 2_656 ?
Cl8 Pb3 Cl4 Pb2 135.53(9) . . . 2_656 ?
Cl9 Pb3 Cl4 Pb2 178.45(18) . . . 2_656 ?
Cl17 Pb3 Cl4 Pb2 -2.35(11) 2_655 . . 2_656 ?
Cl5 Pb3 Cl4 Pb2 -40.80(7) . . . 2_656 ?
Cl7 Pb3 Cl5 Pb2 120.67(13) . . . 2_656 ?
Cl8 Pb3 Cl5 Pb2 39.5(2) . . . 2_656 ?
Cl9 Pb3 Cl5 Pb2 -161.30(11) . . . 2_656 ?
Cl4 Pb3 Cl5 Pb2 45.36(6) . . . 2_656 ?
Cl17 Pb3 Cl5 Pb2 -109.76(11) 2_655 . . 2_656 ?
Cl7 Pb3 Cl8 Pb2 -33.01(11) . . . . ?
Cl9 Pb3 Cl8 Pb2 -117.73(11) . . . . ?
Cl4 Pb3 Cl8 Pb2 41.36(6) . . . . ?
Cl17 Pb3 Cl8 Pb2 -175.71(9) 2_655 . . . ?
Cl5 Pb3 Cl8 Pb2 47.1(2) . . . . ?
Cl6 Pb2 Cl8 Pb3 -26.8(2) 2_656 . . . ?
Cl5 Pb2 Cl8 Pb3 -118.00(11) 2_656 . . . ?
Cl19 Pb2 Cl8 Pb3 174.97(11) 1_556 . . . ?
Cl4 Pb2 Cl8 Pb3 -43.55(7) . . . . ?
Cl3 Pb2 Cl8 Pb3 89.59(12) . . . . ?
Cl2 Pb2 Cl8 Pb3 153.51(13) . . . . ?
Cl7 Pb3 Cl9 Pb4 127.0(3) . . . . ?
Cl8 Pb3 Cl9 Pb4 -143.8(3) . . . . ?
Cl4 Pb3 Cl9 Pb4 174.89(16) . . . . ?
Cl17 Pb3 Cl9 Pb4 -4.6(3) 2_655 . . . ?
Cl5 Pb3 Cl9 Pb4 48.7(4) . . . . ?
Cl13 Pb4 Cl9 Pb3 -75.0(3) . . . . ?
Cl11 Pb4 Cl9 Pb3 -157.2(3) . . . . ?
Cl14 Pb4 Cl9 Pb3 102.8(3) . . . . ?
Cl12 Pb4 Cl9 Pb3 -170.1(3) . . . . ?
Cl10 Pb4 Cl9 Pb3 7.1(3) . . . . ?
Cl13 Pb4 Cl11 Pb6 114.9(4) . . . . ?
Cl14 Pb4 Cl11 Pb6 -57.0(4) . . . . ?
Cl12 Pb4 Cl11 Pb6 -148.0(4) . . . . ?
Cl10 Pb4 Cl11 Pb6 33.9(4) . . . . ?
Cl9 Pb4 Cl11 Pb6 -160.8(3) . . . . ?
Cl20 Pb6 Cl11 Pb4 59.8(4) . . . . ?
Cl17 Pb6 Cl11 Pb4 -30.9(4) . . . . ?
Cl21 Pb6 Cl11 Pb4 -120.7(4) . . . . ?
Cl18 Pb6 Cl11 Pb4 145.6(4) . . . . ?
Cl20 Pb6 Cl17 Pb3 100.29(15) . . . 2_655 ?
Cl11 Pb6 Cl17 Pb3 -170.95(16) . . . 2_655 ?
Cl21 Pb6 Cl17 Pb3 -87.46(15) . . . 2_655 ?
Cl19 Pb6 Cl17 Pb3 5.15(17) . . . 2_655 ?
Cl18 Pb6 Cl17 Pb3 178.2(3) . . . 2_655 ?
Cl20 Pb6 Cl18 Pb1 -97.29(17) . . . 2_755 ?
Cl17 Pb6 Cl18 Pb1 -176.0(3) . . . 2_755 ?
Cl11 Pb6 Cl18 Pb1 173.01(19) . . . 2_755 ?
Cl21 Pb6 Cl18 Pb1 90.20(17) . . . 2_755 ?
Cl19 Pb6 Cl18 Pb1 -2.69(17) . . . 2_755 ?
Cl20 Pb6 Cl19 Pb1 86.3(2) . . . 1_554 ?
Cl17 Pb6 Cl19 Pb1 178.3(2) . . . 1_554 ?
Cl21 Pb6 Cl19 Pb1 -91.9(2) . . . 1_554 ?
Cl18 Pb6 Cl19 Pb1 0.5(2) . . . 1_554 ?
Cl20 Pb6 Cl19 Pb2 -93.52(15) . . . 1_554 ?
Cl17 Pb6 Cl19 Pb2 -1.54(17) . . . 1_554 ?
Cl21 Pb6 Cl19 Pb2 88.22(15) . . . 1_554 ?
Cl18 Pb6 Cl19 Pb2 -179.33(15) . . . 1_554 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl13 0.91 2.42 3.272(13) 155.8 .
N1 H1C Cl21 0.91 2.35 3.228(13) 161.2 .
N1 H1B Cl17 0.91 2.66 3.252(13) 123.6 .
N2 H2A Cl14 0.91 2.38 3.283(14) 174.7 .
N2 H2C Cl13 0.91 2.43 3.297(14) 160.1 2_655
N2 H2B Cl17 0.91 2.35 3.235(14) 163.1 .
N3 H3A Cl1 0.91 2.57 3.327(17) 141.2 2_755
N3 H3C Cl20 0.91 2.56 3.170(15) 124.5 .
N3 H3B Cl2 0.91 2.35 3.241(15) 164.7 1_554
N4 H4A Cl11 0.91 2.64 3.316(14) 132.1 .
N4 H4C Cl15 0.91 2.31 3.205(14) 167.7 2_755
N4 H4B Cl18 0.91 2.41 3.238(15) 150.8 .
N4 H4A Cl12 0.91 2.75 3.425(14) 132.0 .
N5 H5A Cl14 0.91 2.55 3.344(16) 146.0 .
N5 H5C Cl20 0.91 2.62 3.376(15) 141.2 .
N5 H5B Cl16 0.91 2.36 3.268(17) 172.5 2_755
N6 H6A Cl21 0.91 2.27 3.154(16) 165.0 1_556
N6 H6C Cl1 0.91 2.38 3.26(2) 162.3 .
N6 H6B Cl6 0.91 2.52 3.29(2) 143.1 2_656
N7 H7A Cl7 0.91 2.63 3.28(2) 128.3 .
N7 H7C Cl16 0.91 2.41 3.28(2) 159.1 .
N7 H7B Cl9 0.91 2.40 3.26(2) 158.2 .
N8 H8A Cl8 0.91 2.38 3.252(15) 161.0 .
N8 H8B Cl6 0.91 2.34 3.206(14) 158.4 .
N8 H8C Cl5 0.91 2.55 3.222(15) 130.8 2_656
N8 H8C Cl7 0.91 2.71 3.276(16) 121.7 2_656
N9 H9A Cl12 0.91 2.66 3.340(15) 131.7 .
N9 H9C Cl15 0.91 2.31 3.209(18) 167.9 .

### END

_chemical_name_common            
;octadecakis(cyclooctylammonium)tetracontachloroundecaplumbate(
ii)
;

