# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Teresa Rodriguez-Blas'
'Andres de Blas'
'David Esteban-Gomez'
'Raquel Ferreiros-Martinez'
'Carlos Platas-Iglesias'

_publ_contact_author_name        'Teresa Rodriguez-Blas'
_publ_contact_author_email       MAYTER@UDC.ES

_publ_section_title              
;
Zn(II), Cd(II) and Pb(II) complexation with pyridinecarboxylate
containing ligands
;
_publ_requested_category         FO

# Attachment 'H2bcpe2HCl.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2006-05-05 at 12:35:37
# 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 : rfm45 struct

data_rfm45
_database_code_depnum_ccdc_archive 'CCDC 689091'

_audit_creation_date             2006-05-05T12:35:37-00:00
_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        
;
?
;
_chemical_formula_moiety         'C16 H20 N4 O4, 2(Cl)'
_chemical_formula_sum            'C16 H20 Cl2 N4 O4'
_chemical_formula_weight         403.26
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   14.2629(16)
_cell_length_b                   7.8583(9)
_cell_length_c                   8.1247(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.341(2)
_cell_angle_gamma                90
_cell_volume                     909.87(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    298.0(1)
_cell_measurement_reflns_used    3496
_cell_measurement_theta_min      2.8365
_cell_measurement_theta_max      28.2795
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   'SADABS,Bruker-AXS V2.03'
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      298.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       'omega and phi rotation with narrow frames'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.41
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_number            11928
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             2270
_reflns_number_gt                1636
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.3239P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2270
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.059
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.047

#----------------------------------------------------------------------------#
# 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'
O O 0.0106 0.006 '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'

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
C8 C 0.36034(14) 0.7483(3) 0.1085(3) 0.0446(5) Uani 1 1 d . . .
Cl1 Cl 0.10078(3) 0.90097(6) 0.37963(6) 0.04132(15) Uani 1 1 d . . .
N2 N 0.08221(9) 1.00316(18) -0.17609(17) 0.0284(3) Uani 1 1 d . . .
H2A H 0.0367 1.0061 -0.2561 0.034 Uiso 1 1 calc R . .
H2B H 0.1031 0.8953 -0.1675 0.034 Uiso 1 1 calc R . .
O2 O 0.29946(11) 0.63121(18) 0.0559(2) 0.0578(4) Uani 1 1 d . . .
H2 H 0.2631 0.6728 -0.0138 0.087 Uiso 1 1 calc R . .
O1 O 0.42681(11) 0.7114(2) 0.1964(2) 0.0696(5) Uani 1 1 d . . .
C9 C 0.04225(12) 1.0546(2) -0.0180(2) 0.0334(4) Uani 1 1 d . . .
H9A H 0.0237 1.1732 -0.0237 0.04 Uiso 1 1 calc R . .
H9B H 0.0895 1.0423 0.0705 0.04 Uiso 1 1 calc R . .
C1 C 0.16073(12) 1.1153(2) -0.2232(2) 0.0325(4) Uani 1 1 d . . .
H1A H 0.1394 1.2325 -0.2254 0.039 Uiso 1 1 calc R . .
H1B H 0.1791 1.0856 -0.3332 0.039 Uiso 1 1 calc R . .
N1 N 0.26366(9) 0.94403(18) -0.04851(18) 0.0294(3) Uani 1 1 d . . .
C2 C 0.24448(11) 1.0997(2) -0.1054(2) 0.0281(4) Uani 1 1 d . . .
C6 C 0.34030(11) 0.9256(2) 0.0510(2) 0.0321(4) Uani 1 1 d . . .
C3 C 0.29902(13) 1.2401(2) -0.0643(2) 0.0374(4) Uani 1 1 d . . .
H3 H 0.2831 1.3472 -0.1052 0.045 Uiso 1 1 calc R . .
C5 C 0.39909(13) 1.0580(3) 0.0969(2) 0.0396(5) Uani 1 1 d . . .
H5 H 0.4519 1.0395 0.1654 0.048 Uiso 1 1 calc R . .
C4 C 0.37755(14) 1.2184(3) 0.0387(3) 0.0432(5) Uani 1 1 d . . .
H4 H 0.4153 1.3108 0.0683 0.052 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C8 0.0348(10) 0.0433(12) 0.0546(13) 0.0091(10) -0.0120(9) 0.0012(9)
Cl1 0.0369(3) 0.0351(3) 0.0505(3) 0.0029(2) -0.0165(2) 0.0022(2)
N2 0.0242(7) 0.0294(8) 0.0309(8) 0.0007(6) -0.0077(6) 0.0035(6)
O2 0.0526(9) 0.0333(8) 0.0850(12) 0.0132(8) -0.0293(8) -0.0019(7)
O1 0.0454(9) 0.0665(11) 0.0939(13) 0.0248(10) -0.0339(9) 0.0041(8)
C9 0.0269(9) 0.0370(10) 0.0359(10) -0.0048(8) -0.0024(7) -0.0014(7)
C1 0.0317(9) 0.0322(9) 0.0335(9) 0.0066(8) -0.0011(7) 0.0010(8)
N1 0.0236(7) 0.0282(8) 0.0359(8) 0.0010(6) -0.0054(6) -0.0008(6)
C2 0.0247(8) 0.0293(9) 0.0306(9) -0.0014(7) 0.0029(7) 0.0006(7)
C6 0.0233(8) 0.0360(10) 0.0364(10) 0.0000(8) -0.0050(7) 0.0005(7)
C3 0.0390(10) 0.0276(9) 0.0457(11) -0.0021(8) 0.0051(9) -0.0033(8)
C5 0.0273(9) 0.0480(12) 0.0430(11) -0.0070(9) -0.0059(8) -0.0047(8)
C4 0.0367(10) 0.0390(11) 0.0536(13) -0.0112(9) -0.0007(9) -0.0133(9)

#----------------------------------------------------------------------------#
# 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
C8 O1 1.199(2) . ?
C8 O2 1.324(2) . ?
C8 C6 1.493(3) . ?
N2 C9 1.482(2) . ?
N2 C1 1.487(2) . ?
N2 H2A 0.9 . ?
N2 H2B 0.9 . ?
O2 H2 0.82 . ?
C9 C9 1.517(3) 3_575 ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C1 C2 1.505(2) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
N1 C2 1.332(2) . ?
N1 C6 1.341(2) . ?
C2 C3 1.383(2) . ?
C6 C5 1.378(2) . ?
C3 C4 1.381(3) . ?
C3 H3 0.93 . ?
C5 C4 1.376(3) . ?
C5 H5 0.93 . ?
C4 H4 0.93 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C8 O2 121.08(19) . . ?
O1 C8 C6 123.26(19) . . ?
O2 C8 C6 115.66(16) . . ?
C9 N2 C1 112.44(13) . . ?
C9 N2 H2A 109.1 . . ?
C1 N2 H2A 109.1 . . ?
C9 N2 H2B 109.1 . . ?
C1 N2 H2B 109.1 . . ?
H2A N2 H2B 107.8 . . ?
C8 O2 H2 109.5 . . ?
N2 C9 C9 110.46(18) . 3_575 ?
N2 C9 H9A 109.6 . . ?
C9 C9 H9A 109.6 3_575 . ?
N2 C9 H9B 109.6 . . ?
C9 C9 H9B 109.6 3_575 . ?
H9A C9 H9B 108.1 . . ?
N2 C1 C2 112.00(13) . . ?
N2 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N2 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C2 N1 C6 117.34(15) . . ?
N1 C2 C3 122.91(16) . . ?
N1 C2 C1 116.21(15) . . ?
C3 C2 C1 120.84(16) . . ?
N1 C6 C5 123.61(17) . . ?
N1 C6 C8 115.50(16) . . ?
C5 C6 C8 120.89(16) . . ?
C4 C3 C2 118.82(18) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C4 C5 C6 118.28(17) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C5 C4 C3 119.03(17) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?

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
C1 N2 C9 C9 175.56(17) . . . 3_575 ?
C9 N2 C1 C2 65.99(18) . . . . ?
C6 N1 C2 C3 -0.9(3) . . . . ?
C6 N1 C2 C1 177.17(15) . . . . ?
N2 C1 C2 N1 38.3(2) . . . . ?
N2 C1 C2 C3 -143.57(16) . . . . ?
C2 N1 C6 C5 0.2(3) . . . . ?
C2 N1 C6 C8 -178.59(16) . . . . ?
O1 C8 C6 N1 179.1(2) . . . . ?
O2 C8 C6 N1 -0.8(3) . . . . ?
O1 C8 C6 C5 0.3(3) . . . . ?
O2 C8 C6 C5 -179.57(19) . . . . ?
N1 C2 C3 C4 0.8(3) . . . . ?
C1 C2 C3 C4 -177.21(17) . . . . ?
N1 C6 C5 C4 0.7(3) . . . . ?
C8 C6 C5 C4 179.35(19) . . . . ?
C6 C5 C4 C3 -0.8(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?

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
N2 H2A Cl1 0.9 2.29 3.1244(14) 154.9 3_575
N2 H2B Cl1 0.9 2.36 3.2173(15) 159.2 4_575
O2 H2 N1 0.82 2.15 2.644(2) 118.7 .
O2 H2 Cl1 0.82 2.51 3.1327(15) 134.1 4_575

# Attachment '[Cd(bcpc)].cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-05-14 at 09:46:41
# 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 : uc04qf1n struct

data_uc04qf1n
_database_code_depnum_ccdc_archive 'CCDC 689092'

_audit_creation_date             2008-05-14T09:46:41-00:00
_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        
;
?
;
_chemical_formula_moiety         'C20 H22 Cd N4 O4'
_chemical_formula_sum            'C20 H22 Cd N4 O4'
_chemical_formula_weight         494.82
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'x, y, 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                   10.3652(4)
_cell_length_b                   10.4820(5)
_cell_length_c                   17.8467(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1939.01(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    1965
_cell_measurement_theta_min      2.2695
_cell_measurement_theta_max      29.0735
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_process_details   'SABADS, Bruker-AXS Version 2004/1'

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

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_standards_number         ?
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_number            3946
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             3946
_reflns_number_gt                3704
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       "'BRUKER APEX2"
_computing_cell_refinement       "'BRUKER APEX2"
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+0.9922P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3946
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0469
_refine_ls_wR_factor_gt          0.0455
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0
_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   -0.04(2)
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.064

#----------------------------------------------------------------------------#
# 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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
Cd1 Cd 0.995566(17) 0.042274(15) 0.244012(8) 0.01120(5) Uani 1 1 d . . .
O4 O 1.27201(19) -0.1937(2) 0.12719(12) 0.0228(5) Uani 1 1 d . . .
O2 O 1.14349(16) -0.11447(18) 0.21668(10) 0.0155(4) Uani 1 1 d . . .
O1 O 1.14758(17) 0.19513(17) 0.27791(11) 0.0148(4) Uani 1 1 d . . .
O3 O 1.2295(2) 0.3049(2) 0.37370(13) 0.0248(5) Uani 1 1 d . . .
N4 N 1.03309(17) 0.0456(2) 0.11944(11) 0.0115(4) Uani 1 1 d . . .
C20 C 1.1866(2) -0.1224(3) 0.14977(15) 0.0146(5) Uani 1 1 d . . .
C16 C 0.9946(3) 0.1286(2) -0.00150(12) 0.0164(5) Uani 1 1 d . . .
H16 H 0.9502 0.1846 -0.0326 0.02 Uiso 1 1 calc R . .
N1 N 0.9844(2) 0.07166(18) 0.36911(10) 0.0119(4) Uani 1 1 d . . .
C15 C 0.9684(2) 0.1247(2) 0.07471(13) 0.0116(5) Uani 1 1 d . . .
N3 N 0.8305(2) 0.1692(2) 0.18692(12) 0.0115(5) Uani 1 1 d . . .
H20 H 0.8196 0.2402 0.2156 0.014 Uiso 1 1 calc R . .
C19 C 1.1229(2) -0.0338(3) 0.09245(14) 0.0140(5) Uani 1 1 d . . .
C5 C 0.8704(2) 0.0491(3) 0.48299(14) 0.0175(6) Uani 1 1 d . . .
H5 H 0.8041 0.0112 0.5102 0.021 Uiso 1 1 calc R . .
C18 C 1.1526(2) -0.0361(3) 0.01689(15) 0.0192(6) Uani 1 1 d . . .
H18 H 1.2142 -0.0923 -0.0017 0.023 Uiso 1 1 calc R . .
C1 C 1.1553(3) 0.2268(3) 0.34656(16) 0.0151(6) Uani 1 1 d . . .
N2 N 0.80092(18) -0.0531(2) 0.28581(11) 0.0120(4) Uani 1 1 d . . .
H19 H 0.789 -0.1275 0.2604 0.014 Uiso 1 1 calc R . .
C9 C 0.5631(2) -0.0362(3) 0.27178(14) 0.0142(5) Uani 1 1 d . . .
H9A H 0.5631 -0.1046 0.2351 0.017 Uiso 1 1 calc R . .
H9B H 0.5537 -0.0744 0.321 0.017 Uiso 1 1 calc R . .
C11 C 0.4628(2) 0.1121(3) 0.17990(15) 0.0171(6) Uani 1 1 d . . .
H11A H 0.3935 0.1728 0.1721 0.021 Uiso 1 1 calc R . .
H11B H 0.4565 0.0469 0.1415 0.021 Uiso 1 1 calc R . .
C13 C 0.7091(2) 0.0945(2) 0.19040(14) 0.0112(5) Uani 1 1 d . . .
H13 H 0.7128 0.0264 0.1529 0.013 Uiso 1 1 calc R . .
C8 C 0.6928(2) 0.0344(2) 0.26802(13) 0.0118(5) Uani 1 1 d . . .
H8 H 0.6919 0.1029 0.3054 0.014 Uiso 1 1 calc R . .
C14 C 0.8692(3) 0.2113(3) 0.11190(15) 0.0143(6) Uani 1 1 d . . .
H14A H 0.9047 0.2967 0.1154 0.017 Uiso 1 1 calc R . .
H14B H 0.7932 0.2155 0.0803 0.017 Uiso 1 1 calc R . .
C12 C 0.5927(2) 0.1801(3) 0.17355(16) 0.0168(6) Uani 1 1 d . . .
H12A H 0.5935 0.2517 0.208 0.02 Uiso 1 1 calc R . .
H12B H 0.6014 0.2139 0.1232 0.02 Uiso 1 1 calc R . .
C2 C 1.0593(2) 0.1617(2) 0.39970(15) 0.0141(6) Uani 1 1 d . . .
C10 C 0.4485(2) 0.0508(3) 0.25698(15) 0.0192(6) Uani 1 1 d . . .
H10A H 0.4444 0.1166 0.2951 0.023 Uiso 1 1 calc R . .
H10B H 0.3691 0.0019 0.259 0.023 Uiso 1 1 calc R . .
C4 C 0.9499(3) 0.1387(3) 0.51633(15) 0.0196(6) Uani 1 1 d . . .
H4 H 0.9386 0.1605 0.5664 0.023 Uiso 1 1 calc R . .
C7 C 0.8112(3) -0.0819(2) 0.36665(14) 0.0159(6) Uani 1 1 d . . .
H7A H 0.8504 -0.1652 0.373 0.019 Uiso 1 1 calc R . .
H7B H 0.7254 -0.0851 0.3882 0.019 Uiso 1 1 calc R . .
C6 C 0.8907(2) 0.0165(3) 0.40843(15) 0.0141(6) Uani 1 1 d . . .
C17 C 1.0880(3) 0.0476(3) -0.03057(15) 0.0198(6) Uani 1 1 d . . .
H17 H 1.1073 0.0493 -0.0815 0.024 Uiso 1 1 calc R . .
C3 C 1.0467(3) 0.1956(3) 0.47417(15) 0.0161(6) Uani 1 1 d . . .
H3 H 1.1018 0.2553 0.4956 0.019 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.01013(8) 0.01366(8) 0.00982(8) 0.00108(6) 0.00022(10) 0.00046(9)
O4 0.0234(11) 0.0232(12) 0.0219(12) 0.0069(10) 0.0064(10) 0.0103(9)
O2 0.0153(9) 0.0166(10) 0.0146(9) 0.0043(8) 0.0028(7) 0.0026(8)
O1 0.0149(9) 0.0142(10) 0.0153(10) 0.0037(7) 0.0006(8) -0.0021(7)
O3 0.0242(11) 0.0270(13) 0.0232(12) 0.0029(10) -0.0068(10) -0.0135(10)
N4 0.0084(10) 0.0119(10) 0.0142(10) 0.0003(9) 0.0005(8) -0.0019(9)
C20 0.0115(13) 0.0148(14) 0.0176(14) 0.0027(11) 0.0009(11) -0.0033(12)
C16 0.0155(12) 0.0179(12) 0.0160(11) 0.0050(9) -0.0019(15) 0.0004(16)
N1 0.0108(11) 0.0123(10) 0.0126(9) 0.0021(7) -0.0013(10) 0.0015(9)
C15 0.0090(13) 0.0103(12) 0.0154(12) 0.0013(10) -0.0015(9) -0.0046(10)
N3 0.0130(11) 0.0107(11) 0.0109(11) -0.0020(9) -0.0002(9) -0.0006(9)
C19 0.0108(12) 0.0140(14) 0.0171(13) 0.0019(12) 0.0000(10) -0.0032(12)
C5 0.0152(12) 0.0238(15) 0.0135(13) 0.0048(13) 0.0029(10) -0.0006(13)
C18 0.0174(13) 0.0224(15) 0.0178(14) -0.0003(13) 0.0041(11) 0.0053(13)
C1 0.0133(14) 0.0144(14) 0.0176(15) 0.0047(11) -0.0034(12) 0.0029(11)
N2 0.0113(10) 0.0109(10) 0.0136(10) -0.0009(9) -0.0010(8) 0.0015(9)
C9 0.0110(11) 0.0143(13) 0.0173(13) 0.0002(12) -0.0001(10) -0.0019(11)
C11 0.0084(12) 0.0191(14) 0.0239(14) 0.0010(12) -0.0040(10) 0.0018(11)
C13 0.0102(12) 0.0114(13) 0.0119(13) -0.0014(10) -0.0017(10) -0.0011(10)
C8 0.0089(10) 0.0114(12) 0.0152(12) -0.0013(11) -0.0014(10) -0.0001(10)
C14 0.0138(14) 0.0116(13) 0.0174(15) 0.0016(11) -0.0003(12) -0.0008(11)
C12 0.0119(13) 0.0169(15) 0.0215(15) 0.0032(12) -0.0024(11) 0.0023(11)
C2 0.0119(13) 0.0121(13) 0.0183(14) 0.0035(11) -0.0033(11) 0.0023(11)
C10 0.0098(10) 0.0202(14) 0.0277(15) -0.0012(14) 0.0016(11) -0.0030(10)
C4 0.0220(14) 0.0267(16) 0.0100(13) -0.0008(12) -0.0007(11) 0.0063(12)
C7 0.0126(13) 0.0169(14) 0.0181(14) 0.0042(11) 0.0017(11) -0.0013(11)
C6 0.0111(12) 0.0149(14) 0.0163(13) 0.0048(11) -0.0025(11) 0.0040(11)
C17 0.0226(14) 0.0266(16) 0.0102(13) 0.0001(13) 0.0039(11) 0.0017(14)
C3 0.0165(13) 0.0153(14) 0.0164(14) -0.0022(11) -0.0045(11) 0.0022(11)

_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
Cd1 N1 2.2567(19) . yes
Cd1 N4 2.2572(19) . yes
Cd1 O2 2.2996(18) . yes
Cd1 O1 2.3272(17) . yes
Cd1 N2 2.3721(19) . yes
Cd1 N3 2.395(2) . yes
O4 C20 1.227(3) . ?
O2 C20 1.278(3) . ?
O1 C1 1.272(3) . ?
O3 C1 1.224(3) . ?
N4 C15 1.332(3) . ?
N4 C19 1.338(3) . ?
C20 C19 1.531(4) . ?
C16 C15 1.387(3) . ?
C16 C17 1.389(4) . ?
C16 H16 0.93 . ?
N1 C6 1.330(3) . ?
N1 C2 1.339(3) . ?
C15 C14 1.524(4) . ?
N3 C14 1.466(3) . ?
N3 C13 1.483(3) . ?
N3 H20 0.91 . ?
C19 C18 1.383(4) . ?
C5 C4 1.383(4) . ?
C5 C6 1.390(4) . ?
C5 H5 0.93 . ?
C18 C17 1.391(4) . ?
C18 H18 0.93 . ?
C1 C2 1.534(4) . ?
N2 C7 1.478(3) . ?
N2 C8 1.483(3) . ?
N2 H19 0.91 . ?
C9 C10 1.521(3) . ?
C9 C8 1.536(3) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C11 C10 1.525(4) . ?
C11 C12 1.528(4) . ?
C11 H11A 0.97 . ?
C11 H11B 0.97 . ?
C13 C8 1.531(3) . ?
C13 C12 1.533(3) . ?
C13 H13 0.98 . ?
C8 H8 0.98 . ?
C14 H14A 0.97 . ?
C14 H14B 0.97 . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C2 C3 1.382(4) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C4 C3 1.389(4) . ?
C4 H4 0.93 . ?
C7 C6 1.515(4) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C17 H17 0.93 . ?
C3 H3 0.93 . ?

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 Cd1 N4 168.86(7) . . yes
N1 Cd1 O2 109.98(7) . . yes
N4 Cd1 O2 71.77(7) . . yes
N1 Cd1 O1 71.56(7) . . yes
N4 Cd1 O1 97.40(7) . . yes
O2 Cd1 O1 95.49(7) . . yes
N1 Cd1 N2 72.70(7) . . yes
N4 Cd1 N2 117.56(7) . . yes
O2 Cd1 N2 109.43(7) . . yes
O1 Cd1 N2 141.66(7) . . yes
N1 Cd1 N3 107.96(7) . . yes
N4 Cd1 N3 72.28(7) . . yes
O2 Cd1 N3 141.54(7) . . yes
O1 Cd1 N3 102.23(7) . . yes
N2 Cd1 N3 76.13(7) . . yes
C20 O2 Cd1 118.55(16) . . ?
C1 O1 Cd1 118.19(17) . . ?
C15 N4 C19 121.4(2) . . ?
C15 N4 Cd1 120.88(16) . . ?
C19 N4 Cd1 117.71(16) . . ?
O4 C20 O2 126.8(3) . . ?
O4 C20 C19 117.5(2) . . ?
O2 C20 C19 115.7(2) . . ?
C15 C16 C17 119.0(2) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C6 N1 C2 121.0(2) . . ?
C6 N1 Cd1 120.00(17) . . ?
C2 N1 Cd1 118.01(17) . . ?
N4 C15 C16 120.5(2) . . ?
N4 C15 C14 116.7(2) . . ?
C16 C15 C14 122.8(2) . . ?
C14 N3 C13 115.44(19) . . ?
C14 N3 Cd1 111.09(15) . . ?
C13 N3 Cd1 107.16(14) . . ?
C14 N3 H20 107.6 . . ?
C13 N3 H20 107.6 . . ?
Cd1 N3 H20 107.6 . . ?
N4 C19 C18 121.1(2) . . ?
N4 C19 C20 115.9(2) . . ?
C18 C19 C20 123.0(2) . . ?
C4 C5 C6 119.3(2) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C19 C18 C17 118.4(2) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
O3 C1 O1 126.5(3) . . ?
O3 C1 C2 117.4(3) . . ?
O1 C1 C2 116.0(2) . . ?
C7 N2 C8 112.95(19) . . ?
C7 N2 Cd1 109.35(14) . . ?
C8 N2 Cd1 108.35(14) . . ?
C7 N2 H19 108.7 . . ?
C8 N2 H19 108.7 . . ?
Cd1 N2 H19 108.7 . . ?
C10 C9 C8 112.7(2) . . ?
C10 C9 H9A 109 . . ?
C8 C9 H9A 109 . . ?
C10 C9 H9B 109 . . ?
C8 C9 H9B 109 . . ?
H9A C9 H9B 107.8 . . ?
C10 C11 C12 110.4(2) . . ?
C10 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N3 C13 C8 110.42(19) . . ?
N3 C13 C12 110.5(2) . . ?
C8 C13 C12 109.4(2) . . ?
N3 C13 H13 108.8 . . ?
C8 C13 H13 108.8 . . ?
C12 C13 H13 108.8 . . ?
N2 C8 C13 111.41(19) . . ?
N2 C8 C9 110.74(19) . . ?
C13 C8 C9 109.54(19) . . ?
N2 C8 H8 108.4 . . ?
C13 C8 H8 108.4 . . ?
C9 C8 H8 108.4 . . ?
N3 C14 C15 113.8(2) . . ?
N3 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
N3 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C11 C12 C13 113.9(2) . . ?
C11 C12 H12A 108.8 . . ?
C13 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
N1 C2 C3 121.2(2) . . ?
N1 C2 C1 116.0(2) . . ?
C3 C2 C1 122.8(2) . . ?
C9 C10 C11 109.5(2) . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N2 C7 C6 112.4(2) . . ?
N2 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N1 C6 C5 120.5(2) . . ?
N1 C6 C7 115.7(2) . . ?
C5 C6 C7 123.8(2) . . ?
C16 C17 C18 119.6(2) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C2 C3 C4 118.6(3) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?

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 Cd1 O2 C20 -162.67(18) . . . . ?
N4 Cd1 O2 C20 5.68(18) . . . . ?
O1 Cd1 O2 C20 -90.32(19) . . . . ?
N2 Cd1 O2 C20 119.29(18) . . . . ?
N3 Cd1 O2 C20 27.3(2) . . . . ?
N1 Cd1 O1 C1 -0.99(18) . . . . ?
N4 Cd1 O1 C1 177.48(18) . . . . ?
O2 Cd1 O1 C1 -110.24(18) . . . . ?
N2 Cd1 O1 C1 21.1(2) . . . . ?
N3 Cd1 O1 C1 104.10(18) . . . . ?
N1 Cd1 N4 C15 -82.6(4) . . . . ?
O2 Cd1 N4 C15 176.5(2) . . . . ?
O1 Cd1 N4 C15 -90.13(18) . . . . ?
N2 Cd1 N4 C15 73.6(2) . . . . ?
N3 Cd1 N4 C15 10.40(18) . . . . ?
N1 Cd1 N4 C19 96.9(4) . . . . ?
O2 Cd1 N4 C19 -3.98(17) . . . . ?
O1 Cd1 N4 C19 89.38(18) . . . . ?
N2 Cd1 N4 C19 -106.88(18) . . . . ?
N3 Cd1 N4 C19 -170.09(19) . . . . ?
Cd1 O2 C20 O4 174.4(2) . . . . ?
Cd1 O2 C20 C19 -6.3(3) . . . . ?
N4 Cd1 N1 C6 164.7(3) . . . . ?
O2 Cd1 N1 C6 -98.26(19) . . . . ?
O1 Cd1 N1 C6 172.5(2) . . . . ?
N2 Cd1 N1 C6 6.66(18) . . . . ?
N3 Cd1 N1 C6 75.26(19) . . . . ?
N4 Cd1 N1 C2 -4.1(5) . . . . ?
O2 Cd1 N1 C2 92.93(18) . . . . ?
O1 Cd1 N1 C2 3.73(17) . . . . ?
N2 Cd1 N1 C2 -162.14(19) . . . . ?
N3 Cd1 N1 C2 -93.54(19) . . . . ?
C19 N4 C15 C16 -1.3(4) . . . . ?
Cd1 N4 C15 C16 178.23(18) . . . . ?
C19 N4 C15 C14 -179.5(2) . . . . ?
Cd1 N4 C15 C14 0.0(3) . . . . ?
C17 C16 C15 N4 0.8(4) . . . . ?
C17 C16 C15 C14 179.0(2) . . . . ?
N1 Cd1 N3 C14 149.64(15) . . . . ?
N4 Cd1 N3 C14 -18.66(15) . . . . ?
O2 Cd1 N3 C14 -40.2(2) . . . . ?
O1 Cd1 N3 C14 75.31(16) . . . . ?
N2 Cd1 N3 C14 -144.06(17) . . . . ?
N1 Cd1 N3 C13 -83.42(16) . . . . ?
N4 Cd1 N3 C13 108.28(16) . . . . ?
O2 Cd1 N3 C13 86.77(18) . . . . ?
O1 Cd1 N3 C13 -157.76(15) . . . . ?
N2 Cd1 N3 C13 -17.12(15) . . . . ?
C15 N4 C19 C18 0.4(4) . . . . ?
Cd1 N4 C19 C18 -179.1(2) . . . . ?
C15 N4 C19 C20 -178.1(2) . . . . ?
Cd1 N4 C19 C20 2.4(3) . . . . ?
O4 C20 C19 N4 -178.0(2) . . . . ?
O2 C20 C19 N4 2.7(3) . . . . ?
O4 C20 C19 C18 3.6(4) . . . . ?
O2 C20 C19 C18 -175.8(3) . . . . ?
N4 C19 C18 C17 0.9(4) . . . . ?
C20 C19 C18 C17 179.3(2) . . . . ?
Cd1 O1 C1 O3 179.9(2) . . . . ?
Cd1 O1 C1 C2 -1.5(3) . . . . ?
N1 Cd1 N2 C7 -21.91(15) . . . . ?
N4 Cd1 N2 C7 162.78(15) . . . . ?
O2 Cd1 N2 C7 83.73(16) . . . . ?
O1 Cd1 N2 C7 -43.8(2) . . . . ?
N3 Cd1 N2 C7 -136.08(17) . . . . ?
N1 Cd1 N2 C8 101.59(15) . . . . ?
N4 Cd1 N2 C8 -73.72(16) . . . . ?
O2 Cd1 N2 C8 -152.76(14) . . . . ?
O1 Cd1 N2 C8 79.69(18) . . . . ?
N3 Cd1 N2 C8 -12.58(14) . . . . ?
C14 N3 C13 C8 168.9(2) . . . . ?
Cd1 N3 C13 C8 44.6(2) . . . . ?
C14 N3 C13 C12 -69.9(3) . . . . ?
Cd1 N3 C13 C12 165.73(16) . . . . ?
C7 N2 C8 C13 162.3(2) . . . . ?
Cd1 N2 C8 C13 41.0(2) . . . . ?
C7 N2 C8 C9 -75.5(2) . . . . ?
Cd1 N2 C8 C9 163.20(16) . . . . ?
N3 C13 C8 N2 -60.2(3) . . . . ?
C12 C13 C8 N2 177.9(2) . . . . ?
N3 C13 C8 C9 176.90(19) . . . . ?
C12 C13 C8 C9 55.1(3) . . . . ?
C10 C9 C8 N2 177.7(2) . . . . ?
C10 C9 C8 C13 -59.0(3) . . . . ?
C13 N3 C14 C15 -97.2(3) . . . . ?
Cd1 N3 C14 C15 25.1(2) . . . . ?
N4 C15 C14 N3 -17.8(3) . . . . ?
C16 C15 C14 N3 164.0(2) . . . . ?
C10 C11 C12 C13 55.2(3) . . . . ?
N3 C13 C12 C11 -177.0(2) . . . . ?
C8 C13 C12 C11 -55.3(3) . . . . ?
C6 N1 C2 C3 3.5(4) . . . . ?
Cd1 N1 C2 C3 172.15(19) . . . . ?
C6 N1 C2 C1 -174.5(2) . . . . ?
Cd1 N1 C2 C1 -5.8(3) . . . . ?
O3 C1 C2 N1 -176.5(2) . . . . ?
O1 C1 C2 N1 4.8(3) . . . . ?
O3 C1 C2 C3 5.7(4) . . . . ?
O1 C1 C2 C3 -173.1(2) . . . . ?
C8 C9 C10 C11 58.4(3) . . . . ?
C12 C11 C10 C9 -54.6(3) . . . . ?
C6 C5 C4 C3 1.2(4) . . . . ?
C8 N2 C7 C6 -86.4(2) . . . . ?
Cd1 N2 C7 C6 34.3(2) . . . . ?
C2 N1 C6 C5 -1.5(4) . . . . ?
Cd1 N1 C6 C5 -169.92(19) . . . . ?
C2 N1 C6 C7 178.8(2) . . . . ?
Cd1 N1 C6 C7 10.3(3) . . . . ?
C4 C5 C6 N1 -0.9(4) . . . . ?
C4 C5 C6 C7 178.9(2) . . . . ?
N2 C7 C6 N1 -30.8(3) . . . . ?
N2 C7 C6 C5 149.4(2) . . . . ?
C15 C16 C17 C18 0.5(4) . . . . ?
C19 C18 C17 C16 -1.3(4) . . . . ?
N1 C2 C3 C4 -3.1(4) . . . . ?
C1 C2 C3 C4 174.7(2) . . . . ?
C5 C4 C3 C2 0.7(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
N3 H20 O2 0.91 1.98 2.859(3) 161.4 4_755
N2 H19 O1 0.91 2.09 2.923(3) 152 4_745
N2 H19 O3 0.91 2.5 3.228(3) 136.7 4_745

# Attachment '[Cd(bcpe)].cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2007-06-05 at 17:46:26
# 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 : 0613737s struct

data_0613737s
_database_code_depnum_ccdc_archive 'CCDC 689093'

_audit_creation_date             2007-06-05T17:46:26-00:00
_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        
;
?
;
_chemical_formula_moiety         'C16 H16 Cd1 N4 O4, 2(H2 O)'
_chemical_formula_sum            'C16 H20 Cd N4 O6'
_chemical_formula_weight         476.76
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9186(19)
_cell_length_b                   10.2199(18)
_cell_length_c                   16.454(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.284(3)
_cell_angle_gamma                90
_cell_volume                     1833.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    8744
_cell_measurement_theta_min      2.182
_cell_measurement_theta_max      28.2475
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_process_details   'SABADS, Bruker-AXS V2.03'

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

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'omega and phi rotation with narrow frames'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.033
_diffrn_reflns_number            19812
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             4532
_reflns_number_gt                3810
_reflns_threshold_expression     >2sigma(I)

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

_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+9.0644P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4532
_refine_ls_number_parameters     256
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1206
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_restrained_S_all      1.268
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.336
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.151

#----------------------------------------------------------------------------#
# 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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
Cd1 Cd 0.24219(3) 0.01037(3) 0.240998(18) 0.01522(10) Uani 1 1 d . . .
O1 O 0.3977(3) 0.1411(3) 0.29917(19) 0.0171(6) Uani 1 1 d . . .
O3 O 0.3837(3) -0.1492(3) 0.2116(2) 0.0201(7) Uani 1 1 d . . .
O4 O 0.4919(3) -0.2389(3) 0.1149(2) 0.0219(7) Uani 1 1 d . . .
N1 N 0.2319(3) 0.0088(3) 0.3790(2) 0.0155(7) Uani 1 1 d . . .
N4 N 0.2669(3) 0.0113(3) 0.1044(2) 0.0147(7) Uani 1 1 d . . .
N2 N 0.0612(4) -0.1043(4) 0.2732(2) 0.0199(8) Uani 1 1 d . . .
H2N H 0.0515 -0.1749 0.2397 0.024 Uiso 1 1 calc R . .
O2 O 0.4678(4) 0.2403(4) 0.4135(2) 0.0288(8) Uani 1 1 d . . .
C8 C -0.0392(4) -0.0099(5) 0.2536(3) 0.0240(10) Uani 1 1 d . . .
H7 H -0.0391 0.057 0.2954 0.029 Uiso 1 1 calc R . .
H8 H -0.1174 -0.055 0.2527 0.029 Uiso 1 1 calc R . .
C5 C 0.1463(5) -0.0727(5) 0.4981(3) 0.0261(11) Uani 1 1 d . . .
H3 H 0.0892 -0.1253 0.5224 0.031 Uiso 1 1 calc R . .
N3 N 0.0858(3) 0.1393(4) 0.1749(2) 0.0175(8) Uani 1 1 d . . .
H3N H 0.0711 0.2096 0.2068 0.021 Uiso 1 1 calc R . .
C16 C 0.4128(4) -0.1628(4) 0.1386(3) 0.0160(8) Uani 1 1 d . . .
C11 C 0.2056(4) 0.0938(4) 0.0551(3) 0.0160(8) Uani 1 1 d . . .
C12 C 0.2225(4) 0.0952(4) -0.0278(3) 0.0185(9) Uani 1 1 d . . .
H14 H 0.1796 0.154 -0.0619 0.022 Uiso 1 1 calc R . .
C6 C 0.1489(4) -0.0659(5) 0.4143(3) 0.0199(9) Uani 1 1 d . . .
C2 C 0.3117(4) 0.0819(4) 0.4239(3) 0.0170(9) Uani 1 1 d . . .
C4 C 0.2309(5) 0.0006(6) 0.5453(3) 0.0313(11) Uani 1 1 d . . .
H2 H 0.2321 -0.0037 0.6018 0.038 Uiso 1 1 calc R . .
O6 O 0.6417(4) 0.0728(6) 0.2536(3) 0.0529(14) Uani 1 1 d D . .
C1 C 0.3998(4) 0.1621(4) 0.3759(3) 0.0174(9) Uani 1 1 d . . .
C10 C 0.1175(4) 0.1858(4) 0.0949(3) 0.0201(9) Uani 1 1 d . . .
H13 H 0.1547 0.2717 0.1005 0.024 Uiso 1 1 calc R . .
H12 H 0.0432 0.1942 0.06 0.024 Uiso 1 1 calc R . .
C14 C 0.3676(4) -0.0809(5) -0.0070(3) 0.0183(9) Uani 1 1 d . . .
H16 H 0.4217 -0.1416 -0.027 0.022 Uiso 1 1 calc R . .
C13 C 0.3046(4) 0.0072(5) -0.0590(3) 0.0207(9) Uani 1 1 d . . .
H15 H 0.3175 0.0069 -0.1144 0.025 Uiso 1 1 calc R . .
C7 C 0.0658(5) -0.1490(5) 0.3578(3) 0.0227(10) Uani 1 1 d . . .
H4 H 0.0946 -0.2387 0.3601 0.027 Uiso 1 1 calc R . .
H5 H -0.0165 -0.1477 0.3771 0.027 Uiso 1 1 calc R . .
C15 C 0.3470(4) -0.0752(4) 0.0752(3) 0.0154(8) Uani 1 1 d . . .
C3 C 0.3140(5) 0.0806(5) 0.5074(3) 0.0264(11) Uani 1 1 d . . .
H1 H 0.3698 0.1319 0.538 0.032 Uiso 1 1 calc R . .
C9 C -0.0235(4) 0.0535(5) 0.1715(3) 0.0232(10) Uani 1 1 d . . .
H10 H -0.0147 -0.0138 0.1307 0.028 Uiso 1 1 calc R . .
H9 H -0.0959 0.1047 0.1559 0.028 Uiso 1 1 calc R . .
O5 O 0.8135(4) 0.2896(6) 0.2643(3) 0.0562(14) Uani 1 1 d D . .
H61W H 0.652(7) 0.1579(19) 0.253(5) 0.067 Uiso 1 1 d D . .
H62W H 0.566(7) 0.068(7) 0.277(5) 0.067 Uiso 1 1 d D . .
H51W H 0.774(6) 0.229(7) 0.304(4) 0.067 Uiso 1 1 d D . .
H52W H 0.885(3) 0.287(8) 0.288(4) 0.067 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.01366(15) 0.01633(16) 0.01582(16) -0.00066(12) 0.00213(10) 0.00084(12)
O1 0.0179(15) 0.0194(16) 0.0141(15) 0.0023(12) 0.0014(12) -0.0014(12)
O3 0.0231(17) 0.0188(16) 0.0190(17) 0.0048(12) 0.0057(13) 0.0054(13)
O4 0.0228(17) 0.0209(17) 0.0226(18) 0.0000(13) 0.0062(14) 0.0075(13)
N1 0.0155(16) 0.0095(16) 0.0221(18) 0.0043(14) 0.0063(14) 0.0018(14)
N4 0.0201(17) 0.0079(16) 0.0158(16) -0.0048(13) -0.0007(13) 0.0001(14)
N2 0.0214(19) 0.0149(18) 0.024(2) -0.0078(15) 0.0070(16) -0.0014(15)
O2 0.035(2) 0.030(2) 0.0215(18) -0.0005(14) -0.0023(15) -0.0157(16)
C8 0.0141(19) 0.023(2) 0.035(3) -0.010(2) 0.0035(18) -0.0002(18)
C5 0.027(3) 0.029(3) 0.023(3) 0.007(2) 0.011(2) 0.001(2)
N3 0.0173(18) 0.0163(18) 0.0186(19) -0.0059(14) -0.0005(15) 0.0015(14)
C16 0.016(2) 0.0125(19) 0.019(2) 0.0009(16) 0.0016(17) -0.0004(16)
C11 0.019(2) 0.014(2) 0.014(2) -0.0017(16) -0.0052(16) -0.0008(16)
C12 0.019(2) 0.020(2) 0.016(2) 0.0005(17) -0.0070(17) -0.0027(17)
C6 0.024(2) 0.016(2) 0.021(2) 0.0014(17) 0.0077(18) 0.0015(18)
C2 0.022(2) 0.017(2) 0.012(2) 0.0031(16) 0.0021(17) 0.0004(17)
C4 0.039(3) 0.036(3) 0.019(2) 0.005(2) 0.009(2) 0.002(2)
O6 0.027(2) 0.091(4) 0.041(3) -0.027(3) 0.0042(19) 0.006(2)
C1 0.021(2) 0.018(2) 0.013(2) 0.0051(16) 0.0018(17) 0.0017(17)
C10 0.025(2) 0.015(2) 0.019(2) -0.0015(17) -0.0055(19) 0.0047(18)
C14 0.019(2) 0.020(2) 0.017(2) -0.0033(17) 0.0022(17) -0.0018(17)
C13 0.023(2) 0.022(2) 0.016(2) -0.0008(18) 0.0002(17) -0.0051(19)
C7 0.024(2) 0.018(2) 0.026(3) -0.0019(18) 0.009(2) -0.0039(18)
C15 0.015(2) 0.013(2) 0.017(2) 0.0002(16) -0.0009(16) -0.0008(16)
C3 0.030(3) 0.032(3) 0.016(2) 0.000(2) 0.000(2) 0.000(2)
C9 0.016(2) 0.025(2) 0.028(3) -0.0102(19) -0.0014(19) 0.0018(18)
O5 0.035(2) 0.065(3) 0.067(4) -0.033(3) -0.019(2) 0.015(2)

#----------------------------------------------------------------------------#
# 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
Cd1 N1 2.280(4) . yes
Cd1 N4 2.280(4) . yes
Cd1 O3 2.317(3) . yes
Cd1 O1 2.323(3) . yes
Cd1 N3 2.370(4) . yes
Cd1 N2 2.383(4) . yes?
O1 C1 1.280(5) . ?
O3 C16 1.268(5) . ?
O4 C16 1.241(5) . ?
N1 C2 1.338(6) . ?
N1 C6 1.342(6) . ?
N4 C11 1.324(5) . ?
N4 C15 1.351(6) . ?
N2 C7 1.464(6) . ?
N2 C8 1.482(6) . ?
N2 H2N 0.91 . ?
O2 C1 1.233(6) . ?
C8 C9 1.517(7) . ?
C8 H7 0.97 . ?
C8 H8 0.97 . ?
C5 C6 1.382(7) . ?
C5 C4 1.392(8) . ?
C5 H3 0.93 . ?
N3 C10 1.460(6) . ?
N3 C9 1.479(6) . ?
N3 H3N 0.91 . ?
C16 C15 1.523(6) . ?
C11 C12 1.387(6) . ?
C11 C10 1.520(6) . ?
C12 C13 1.389(7) . ?
C12 H14 0.93 . ?
C6 C7 1.520(7) . ?
C2 C3 1.373(6) . ?
C2 C1 1.519(6) . ?
C4 C3 1.395(8) . ?
C4 H2 0.93 . ?
O6 H61W 0.877(14) . ?
O6 H62W 0.94(7) . ?
C10 H13 0.97 . ?
C10 H12 0.97 . ?
C14 C15 1.385(6) . ?
C14 C13 1.396(6) . ?
C14 H16 0.93 . ?
C13 H15 0.93 . ?
C7 H4 0.97 . ?
C7 H5 0.97 . ?
C3 H1 0.93 . ?
C9 H10 0.97 . ?
C9 H9 0.97 . ?
O5 H51W 1.01(2) . ?
O5 H52W 0.85(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N4 176.04(13) . . yes
N1 Cd1 O3 105.95(12) . . yes
N4 Cd1 O3 71.26(12) . . yes
N1 Cd1 O1 70.76(12) . . yes
N4 Cd1 O1 106.19(12) . . yes
O3 Cd1 O1 90.62(12) . . yes
N1 Cd1 N3 112.68(13) . . yes
N4 Cd1 N3 70.61(13) . . yes
O3 Cd1 N3 140.05(12) . . yes
O1 Cd1 N3 111.06(12) . . yes
N1 Cd1 N2 71.70(13) . . yes
N4 Cd1 N2 111.58(13) . . yes
O3 Cd1 N2 105.75(13) . . yes
O1 Cd1 N2 141.90(12) . . yes
N3 Cd1 N2 77.93(14) . . yes
C1 O1 Cd1 118.3(3) . . ?
C16 O3 Cd1 118.8(3) . . ?
C2 N1 C6 120.8(4) . . ?
C2 N1 Cd1 118.6(3) . . ?
C6 N1 Cd1 120.6(3) . . ?
C11 N4 C15 120.9(4) . . ?
C11 N4 Cd1 121.5(3) . . ?
C15 N4 Cd1 117.6(3) . . ?
C7 N2 C8 113.3(4) . . ?
C7 N2 Cd1 112.4(3) . . ?
C8 N2 Cd1 104.1(3) . . ?
C7 N2 H2N 109 . . ?
C8 N2 H2N 109 . . ?
Cd1 N2 H2N 109 . . ?
N2 C8 C9 110.7(4) . . ?
N2 C8 H7 109.5 . . ?
C9 C8 H7 109.5 . . ?
N2 C8 H8 109.5 . . ?
C9 C8 H8 109.5 . . ?
H7 C8 H8 108.1 . . ?
C6 C5 C4 118.6(5) . . ?
C6 C5 H3 120.7 . . ?
C4 C5 H3 120.7 . . ?
C10 N3 C9 113.0(4) . . ?
C10 N3 Cd1 113.2(3) . . ?
C9 N3 Cd1 104.3(3) . . ?
C10 N3 H3N 108.7 . . ?
C9 N3 H3N 108.7 . . ?
Cd1 N3 H3N 108.7 . . ?
O4 C16 O3 125.6(4) . . ?
O4 C16 C15 117.5(4) . . ?
O3 C16 C15 116.8(4) . . ?
N4 C11 C12 121.2(4) . . ?
N4 C11 C10 116.1(4) . . ?
C12 C11 C10 122.7(4) . . ?
C11 C12 C13 118.8(4) . . ?
C11 C12 H14 120.6 . . ?
C13 C12 H14 120.6 . . ?
N1 C6 C5 120.9(5) . . ?
N1 C6 C7 116.5(4) . . ?
C5 C6 C7 122.4(4) . . ?
N1 C2 C3 121.4(4) . . ?
N1 C2 C1 115.3(4) . . ?
C3 C2 C1 123.3(4) . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 H2 120.2 . . ?
C3 C4 H2 120.2 . . ?
H61W O6 H62W 100(5) . . ?
O2 C1 O1 125.5(4) . . ?
O2 C1 C2 118.1(4) . . ?
O1 C1 C2 116.5(4) . . ?
N3 C10 C11 112.0(4) . . ?
N3 C10 H13 109.2 . . ?
C11 C10 H13 109.2 . . ?
N3 C10 H12 109.2 . . ?
C11 C10 H12 109.2 . . ?
H13 C10 H12 107.9 . . ?
C15 C14 C13 118.1(4) . . ?
C15 C14 H16 121 . . ?
C13 C14 H16 121 . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 H15 120.1 . . ?
C14 C13 H15 120.1 . . ?
N2 C7 C6 113.2(4) . . ?
N2 C7 H4 108.9 . . ?
C6 C7 H4 108.9 . . ?
N2 C7 H5 108.9 . . ?
C6 C7 H5 108.9 . . ?
H4 C7 H5 107.7 . . ?
N4 C15 C14 121.2(4) . . ?
N4 C15 C16 115.5(4) . . ?
C14 C15 C16 123.2(4) . . ?
C2 C3 C4 118.6(5) . . ?
C2 C3 H1 120.7 . . ?
C4 C3 H1 120.7 . . ?
N3 C9 C8 110.6(4) . . ?
N3 C9 H10 109.5 . . ?
C8 C9 H10 109.5 . . ?
N3 C9 H9 109.5 . . ?
C8 C9 H9 109.5 . . ?
H10 C9 H9 108.1 . . ?
H51W O5 H52W 96(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 Cd1 O1 C1 -6.3(3) . . . . ?
N4 Cd1 O1 C1 176.3(3) . . . . ?
O3 Cd1 O1 C1 -113.0(3) . . . . ?
N3 Cd1 O1 C1 101.3(3) . . . . ?
N2 Cd1 O1 C1 4.0(4) . . . . ?
N1 Cd1 O3 C16 -175.5(3) . . . . ?
N4 Cd1 O3 C16 1.6(3) . . . . ?
O1 Cd1 O3 C16 -105.3(3) . . . . ?
N3 Cd1 O3 C16 19.6(4) . . . . ?
N2 Cd1 O3 C16 109.5(3) . . . . ?
O3 Cd1 N1 C2 87.0(3) . . . . ?
O1 Cd1 N1 C2 2.0(3) . . . . ?
N3 Cd1 N1 C2 -103.4(3) . . . . ?
N2 Cd1 N1 C2 -171.3(3) . . . . ?
O3 Cd1 N1 C6 -91.7(3) . . . . ?
O1 Cd1 N1 C6 -176.7(4) . . . . ?
N3 Cd1 N1 C6 77.8(3) . . . . ?
N2 Cd1 N1 C6 10.0(3) . . . . ?
O3 Cd1 N4 C11 179.9(4) . . . . ?
O1 Cd1 N4 C11 -95.1(3) . . . . ?
N3 Cd1 N4 C11 12.1(3) . . . . ?
N2 Cd1 N4 C11 79.9(3) . . . . ?
O3 Cd1 N4 C15 -0.4(3) . . . . ?
O1 Cd1 N4 C15 84.7(3) . . . . ?
N3 Cd1 N4 C15 -168.2(3) . . . . ?
N2 Cd1 N4 C15 -100.4(3) . . . . ?
N1 Cd1 N2 C7 -19.1(3) . . . . ?
N4 Cd1 N2 C7 158.5(3) . . . . ?
O3 Cd1 N2 C7 82.8(3) . . . . ?
O1 Cd1 N2 C7 -29.4(4) . . . . ?
N3 Cd1 N2 C7 -138.2(3) . . . . ?
N1 Cd1 N2 C8 103.8(3) . . . . ?
N4 Cd1 N2 C8 -78.5(3) . . . . ?
O3 Cd1 N2 C8 -154.2(3) . . . . ?
O1 Cd1 N2 C8 93.6(3) . . . . ?
N3 Cd1 N2 C8 -15.2(3) . . . . ?
C7 N2 C8 C9 168.3(4) . . . . ?
Cd1 N2 C8 C9 45.9(4) . . . . ?
N1 Cd1 N3 C10 156.3(3) . . . . ?
N4 Cd1 N3 C10 -21.3(3) . . . . ?
O3 Cd1 N3 C10 -39.5(4) . . . . ?
O1 Cd1 N3 C10 79.1(3) . . . . ?
N2 Cd1 N3 C10 -139.6(3) . . . . ?
N1 Cd1 N3 C9 -80.5(3) . . . . ?
N4 Cd1 N3 C9 101.9(3) . . . . ?
O3 Cd1 N3 C9 83.7(3) . . . . ?
O1 Cd1 N3 C9 -157.7(3) . . . . ?
N2 Cd1 N3 C9 -16.4(3) . . . . ?
Cd1 O3 C16 O4 175.7(4) . . . . ?
Cd1 O3 C16 C15 -2.5(5) . . . . ?
C15 N4 C11 C12 -0.7(6) . . . . ?
Cd1 N4 C11 C12 179.0(3) . . . . ?
C15 N4 C11 C10 179.6(4) . . . . ?
Cd1 N4 C11 C10 -0.6(5) . . . . ?
N4 C11 C12 C13 0.7(7) . . . . ?
C10 C11 C12 C13 -179.8(4) . . . . ?
C2 N1 C6 C5 -2.2(7) . . . . ?
Cd1 N1 C6 C5 176.5(4) . . . . ?
C2 N1 C6 C7 -177.7(4) . . . . ?
Cd1 N1 C6 C7 1.0(5) . . . . ?
C4 C5 C6 N1 0.6(7) . . . . ?
C4 C5 C6 C7 175.9(5) . . . . ?
C6 N1 C2 C3 1.8(7) . . . . ?
Cd1 N1 C2 C3 -177.0(4) . . . . ?
C6 N1 C2 C1 -179.6(4) . . . . ?
Cd1 N1 C2 C1 1.6(5) . . . . ?
C6 C5 C4 C3 1.3(8) . . . . ?
Cd1 O1 C1 O2 -171.5(4) . . . . ?
Cd1 O1 C1 C2 9.3(5) . . . . ?
N1 C2 C1 O2 173.5(4) . . . . ?
C3 C2 C1 O2 -7.9(7) . . . . ?
N1 C2 C1 O1 -7.3(6) . . . . ?
C3 C2 C1 O1 171.3(4) . . . . ?
C9 N3 C10 C11 -90.0(4) . . . . ?
Cd1 N3 C10 C11 28.3(4) . . . . ?
N4 C11 C10 N3 -19.0(6) . . . . ?
C12 C11 C10 N3 161.4(4) . . . . ?
C11 C12 C13 C14 0.4(7) . . . . ?
C15 C14 C13 C12 -1.2(7) . . . . ?
C8 N2 C7 C6 -91.5(5) . . . . ?
Cd1 N2 C7 C6 26.2(5) . . . . ?
N1 C6 C7 N2 -18.8(6) . . . . ?
C5 C6 C7 N2 165.7(4) . . . . ?
C11 N4 C15 C14 -0.2(6) . . . . ?
Cd1 N4 C15 C14 -179.9(3) . . . . ?
C11 N4 C15 C16 179.1(4) . . . . ?
Cd1 N4 C15 C16 -0.6(5) . . . . ?
C13 C14 C15 N4 1.2(6) . . . . ?
C13 C14 C15 C16 -178.1(4) . . . . ?
O4 C16 C15 N4 -176.3(4) . . . . ?
O3 C16 C15 N4 2.1(6) . . . . ?
O4 C16 C15 C14 3.0(6) . . . . ?
O3 C16 C15 C14 -178.7(4) . . . . ?
N1 C2 C3 C4 0.2(7) . . . . ?
C1 C2 C3 C4 -178.3(5) . . . . ?
C5 C4 C3 C2 -1.7(8) . . . . ?
C10 N3 C9 C8 170.4(4) . . . . ?
Cd1 N3 C9 C8 47.1(4) . . . . ?
N2 C8 C9 N3 -67.8(5) . . . . ?

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
N2 H2N O1 0.91 2.07 2.906(5) 151.9 2_545
N3 H3N O3 0.91 2.01 2.864(5) 155 2
O6 H61W O5 0.877(14) 2.22(6) 2.902(8) 135(7) .
O6 H62W O1 0.94(7) 2.03(8) 2.894(5) 152(7) .
O5 H51W O6 1.01(2) 2.28(7) 2.902(8) 119(6) .
O5 H52W O4 0.85(2) 2.04(4) 2.840(6) 155(6) 2_655

# Attachment '[Pb4(bcpe)4].cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-02-15 at 12:11:31
# 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 : uc06qf2n struct

data_uc06qf2n
_database_code_depnum_ccdc_archive 'CCDC 689094'

_audit_creation_date             2008-02-15T12:11:31-00:00
_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        
;
?
;
_chemical_formula_moiety         'C64 H64 N16 O16 Pb4'
_chemical_formula_sum            'C64 H64 N16 O16 Pb4'
_chemical_formula_weight         2142.11
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration unk

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

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_Int_Tables_number      82
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   26.9308(16)
_cell_length_b                   26.9308(16)
_cell_length_c                   11.4732(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8321.1(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    1953
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      19.26
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       needle
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.71
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4064
_exptl_special_details           
;
The crystal was of low quality, and it was a twined crystal
with many secondary domains together with the main
domain that render difficult to refine the structure and
any attempt to find the twin law. Finally to get better
results we decide to sqeeze the data to eliminate the
residual Q peaks associated with the secondary domains
of the twin.
;

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

_exptl_absorpt_coefficient_mu    8.134
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.280
_exptl_absorpt_process_details   
;
SADABS: Area-Detector Absorption Correction;
Siemens Industrial Automation, Inc.: Madison, WI, 1996.
;

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

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_reflns_av_R_equivalents  0.1295
_diffrn_reflns_av_unetI/netI     0.08
_diffrn_reflns_number            4323
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.07
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             4323
_reflns_number_gt                3267
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        XPREP
_computing_structure_solution    Dirdif99
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4323
_refine_ls_number_parameters     452
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1255
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.979
_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   0.36(2)
_refine_diff_density_max         3.324
_refine_diff_density_min         -1.037
_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'
O O 0.0106 0.006 '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
Pb1 Pb 0.08532(2) 0.45791(3) 0.13815(6) 0.0338(2) Uani 1 1 d . . .
Pb2 Pb 0.51200(3) 0.59075(2) 0.89147(5) 0.03338(19) Uani 1 1 d . . .
C1 C 0.2081(7) 0.4825(6) 0.1740(18) 0.040(4) Uani 1 1 d DU . .
C2 C 0.2028(7) 0.4962(5) 0.0500(19) 0.037(3) Uani 1 1 d DU . .
C3 C 0.2418(7) 0.5168(7) -0.014(2) 0.050(4) Uani 1 1 d DU . .
H3 H 0.2729 0.5218 0.0193 0.06 Uiso 1 1 calc R . .
C4 C 0.2327(7) 0.5294(7) -0.127(2) 0.057(5) Uani 1 1 d DU . .
H4 H 0.2569 0.5463 -0.169 0.069 Uiso 1 1 calc R . .
C5 C 0.1885(8) 0.5178(7) -0.1794(19) 0.049(5) Uani 1 1 d DU . .
H5 H 0.184 0.5228 -0.2589 0.059 Uiso 1 1 calc R . .
C6 C 0.1508(6) 0.4983(6) -0.1116(18) 0.036(3) Uani 1 1 d DU . .
C7 C 0.1011(8) 0.4863(7) -0.1519(18) 0.043(6) Uani 1 1 d . . .
H7A H 0.1021 0.4804 -0.2353 0.052 Uiso 1 1 calc R . .
H7B H 0.0796 0.5146 -0.1382 0.052 Uiso 1 1 calc R . .
C8 C 0.1039(8) 0.3978(8) -0.1249(19) 0.054(6) Uani 1 1 d . . .
H8A H 0.1396 0.4026 -0.1227 0.064 Uiso 1 1 calc R . .
H8B H 0.0948 0.3885 -0.2038 0.064 Uiso 1 1 calc R . .
C9 C 0.0896(13) 0.3565(10) -0.042(2) 0.090(11) Uani 1 1 d . . .
H9A H 0.1066 0.3261 -0.0628 0.108 Uiso 1 1 calc R . .
H9B H 0.0541 0.3506 -0.0457 0.108 Uiso 1 1 calc R . .
C10 C 0.0838(7) 0.3349(7) 0.1615(17) 0.042(5) Uani 1 1 d . . .
H10A H 0.0974 0.3026 0.1428 0.05 Uiso 1 1 calc R . .
H10B H 0.048 0.3333 0.1524 0.05 Uiso 1 1 calc R . .
C11 C 0.0967(6) 0.3484(7) 0.2901(15) 0.029(4) Uani 1 1 d . . .
C12 C 0.1145(8) 0.3179(7) 0.371(2) 0.052(6) Uani 1 1 d . . .
H12 H 0.123 0.2855 0.3506 0.062 Uiso 1 1 calc R . .
C13 C 0.1205(8) 0.3326(10) 0.481(2) 0.055(6) Uani 1 1 d . . .
H13 H 0.1309 0.3099 0.5371 0.066 Uiso 1 1 calc R . .
C14 C 0.1117(9) 0.3794(10) 0.5120(19) 0.058(7) Uani 1 1 d . . .
H14 H 0.1158 0.3904 0.5882 0.07 Uiso 1 1 calc R . .
C15 C 0.0960(7) 0.4110(7) 0.4231(16) 0.039(5) Uani 1 1 d . . .
C16 C 0.0857(9) 0.4657(9) 0.447(2) 0.058(6) Uani 1 1 d . . .
C17 C 0.6061(6) 0.6755(7) 0.9307(15) 0.031(4) Uani 1 1 d . . .
C18 C 0.6125(8) 0.6663(7) 0.8017(19) 0.043(4) Uani 1 1 d DU . .
C19 C 0.6469(8) 0.6887(8) 0.724(2) 0.057(5) Uani 1 1 d DU . .
H19 H 0.6691 0.7119 0.7535 0.068 Uiso 1 1 calc R . .
C20 C 0.6490(9) 0.6784(8) 0.610(2) 0.069(6) Uani 1 1 d DU . .
H20 H 0.6709 0.6948 0.5607 0.082 Uiso 1 1 calc R . .
C21 C 0.6211(10) 0.6465(8) 0.574(2) 0.066(6) Uani 1 1 d DU . .
H21 H 0.6243 0.6373 0.4963 0.079 Uiso 1 1 calc R . .
C22 C 0.5833(8) 0.6216(7) 0.6418(19) 0.052(4) Uani 1 1 d DU . .
C23 C 0.5465(10) 0.5836(10) 0.593(2) 0.077(11) Uani 1 1 d . . .
H23A H 0.5412 0.589 0.5108 0.092 Uiso 1 1 calc R . .
H23B H 0.5589 0.5502 0.6046 0.092 Uiso 1 1 calc R . .
C24 C 0.4704(8) 0.6356(7) 0.6239(18) 0.045(5) Uani 1 1 d . . .
H24A H 0.4933 0.663 0.6135 0.054 Uiso 1 1 calc R . .
H24B H 0.4549 0.629 0.5491 0.054 Uiso 1 1 calc R . .
C25 C 0.4341(8) 0.6497(7) 0.7019(16) 0.045(5) Uani 1 1 d . . .
H25A H 0.4089 0.624 0.705 0.054 Uiso 1 1 calc R . .
H25B H 0.4185 0.6799 0.6739 0.054 Uiso 1 1 calc R . .
C26 C 0.4146(6) 0.6694(7) 0.9049(15) 0.035(4) Uani 1 1 d . . .
H26A H 0.3888 0.6445 0.8958 0.041 Uiso 1 1 calc R . .
H26B H 0.4003 0.7013 0.8849 0.041 Uiso 1 1 calc R . .
C27 C 0.4303(7) 0.6705(7) 1.0306(16) 0.040(5) Uani 1 1 d DU . .
C28 C 0.4109(6) 0.7041(6) 1.1083(16) 0.035(4) Uani 1 1 d DU . .
H28 H 0.3882 0.7274 1.0815 0.042 Uiso 1 1 calc R . .
C29 C 0.4232(7) 0.7044(8) 1.2203(16) 0.049(5) Uani 1 1 d DU . .
H29 H 0.4098 0.7271 1.2727 0.059 Uiso 1 1 calc R . .
C30 C 0.4588(7) 0.6673(9) 1.2555(14) 0.048(4) Uani 1 1 d DU . .
H30 H 0.4689 0.6654 1.3329 0.057 Uiso 1 1 calc R . .
C31 C 0.4780(7) 0.6345(8) 1.1750(14) 0.041(4) Uani 1 1 d DU . .
C32 C 0.5148(8) 0.5925(9) 1.2050(14) 0.048(4) Uani 1 1 d DU . .
N1 N 0.1585(6) 0.4868(5) 0.0043(13) 0.037(3) Uani 1 1 d DU . .
N2 N 0.0799(7) 0.4429(8) -0.0949(15) 0.060(5) Uani 1 1 d . . .
H2 H 0.0473 0.4406 -0.1153 0.072 Uiso 1 1 calc R . .
N3 N 0.1041(6) 0.3720(6) 0.0816(13) 0.041(4) Uani 1 1 d . . .
H3A H 0.1377 0.369 0.0856 0.05 Uiso 1 1 calc R . .
N4 N 0.0886(6) 0.3961(6) 0.3133(13) 0.038(4) Uani 1 1 d . . .
N5 N 0.5808(7) 0.6327(6) 0.7555(14) 0.047(4) Uani 1 1 d DU . .
N6 N 0.4987(7) 0.5910(7) 0.6601(12) 0.051(5) Uani 1 1 d . . .
H6 H 0.4791 0.5644 0.6435 0.062 Uiso 1 1 calc R . .
N7 N 0.4537(6) 0.6587(6) 0.8248(12) 0.034(4) Uani 1 1 d . . .
H7 H 0.4724 0.6868 0.8206 0.04 Uiso 1 1 calc R . .
N8 N 0.4642(6) 0.6365(6) 1.0630(13) 0.038(4) Uani 1 1 d . . .
O1 O 0.2460(5) 0.4976(6) 0.2231(15) 0.062(4) Uani 1 1 d U . .
O2 O 0.1738(5) 0.4583(5) 0.2206(13) 0.051(4) Uani 1 1 d U . .
O3 O 0.0764(5) 0.4948(5) 0.3695(14) 0.048(4) Uani 1 1 d . . .
O4 O 0.0794(11) 0.4749(8) 0.5557(19) 0.124(9) Uani 1 1 d . . .
O5 O 0.6387(5) 0.6996(5) 0.9767(12) 0.042(3) Uani 1 1 d . . .
O6 O 0.5710(5) 0.6543(5) 0.9804(12) 0.046(4) Uani 1 1 d . . .
O7 O 0.5285(7) 0.5661(5) 1.1275(14) 0.067(5) Uani 1 1 d . . .
O8 O 0.5304(6) 0.5976(9) 1.3087(13) 0.091(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0260(4) 0.0324(4) 0.0429(4) 0.0028(3) -0.0017(3) -0.0059(3)
Pb2 0.0445(5) 0.0221(3) 0.0336(3) 0.0014(3) 0.0034(3) 0.0024(3)
C1 0.032(9) 0.025(9) 0.063(8) -0.030(7) -0.010(6) 0.005(7)
C2 0.025(7) 0.009(8) 0.078(8) 0.001(7) -0.004(6) 0.005(7)
C3 0.021(8) 0.030(11) 0.100(11) -0.014(10) 0.009(8) -0.002(8)
C4 0.026(8) 0.049(11) 0.097(12) -0.005(11) 0.039(9) -0.004(8)
C5 0.051(10) 0.026(10) 0.071(11) 0.034(9) 0.009(7) 0.011(9)
C6 0.029(8) 0.030(9) 0.050(8) -0.006(8) 0.007(7) 0.012(7)
C7 0.048(12) 0.044(13) 0.039(12) 0.012(9) 0.011(10) 0.019(10)
C8 0.066(14) 0.061(14) 0.034(11) -0.015(11) 0.004(11) -0.028(12)
C9 0.16(3) 0.061(17) 0.050(15) 0.012(13) -0.053(17) -0.041(19)
C10 0.036(11) 0.030(10) 0.060(13) 0.003(9) 0.004(9) -0.008(9)
C11 0.012(8) 0.036(11) 0.038(10) 0.001(8) 0.011(7) 0.006(8)
C12 0.058(13) 0.042(12) 0.054(14) -0.025(11) 0.003(12) 0.012(10)
C13 0.046(14) 0.067(17) 0.052(14) 0.035(13) 0.007(11) 0.009(12)
C14 0.058(15) 0.080(19) 0.036(12) 0.000(12) -0.006(10) -0.020(14)
C15 0.034(11) 0.041(11) 0.042(12) 0.009(9) -0.007(8) 0.020(9)
C16 0.064(17) 0.064(17) 0.047(13) 0.005(12) -0.035(12) 0.008(14)
C17 0.018(9) 0.040(11) 0.035(10) 0.018(8) 0.011(8) -0.006(8)
C18 0.053(12) 0.024(9) 0.053(10) 0.014(7) 0.023(8) 0.025(7)
C19 0.072(14) 0.039(12) 0.060(10) 0.015(9) 0.026(10) 0.007(9)
C20 0.086(15) 0.062(14) 0.058(10) 0.030(11) 0.022(12) 0.012(10)
C21 0.092(16) 0.050(13) 0.055(11) -0.010(9) 0.046(10) 0.030(10)
C22 0.073(12) 0.034(10) 0.049(9) 0.011(8) 0.017(9) 0.034(8)
C23 0.10(2) 0.076(19) 0.054(17) 0.053(14) 0.025(14) 0.042(17)
C24 0.068(13) 0.025(10) 0.043(12) -0.010(9) 0.002(11) 0.020(9)
C25 0.076(16) 0.018(10) 0.041(11) 0.000(8) -0.026(11) -0.008(10)
C26 0.033(10) 0.038(10) 0.033(10) -0.001(8) -0.005(8) -0.025(9)
C27 0.039(11) 0.042(12) 0.040(10) -0.035(9) 0.014(9) -0.009(10)
C28 0.038(9) 0.033(9) 0.034(8) -0.015(7) 0.017(7) -0.006(7)
C29 0.035(10) 0.077(13) 0.035(8) -0.033(9) 0.024(7) -0.024(8)
C30 0.033(10) 0.098(14) 0.011(8) -0.019(7) 0.005(6) -0.026(8)
C31 0.041(11) 0.068(12) 0.014(8) -0.012(7) -0.008(7) -0.022(8)
C32 0.055(14) 0.076(15) 0.012(8) -0.002(9) -0.010(8) -0.021(9)
N1 0.032(7) 0.026(8) 0.051(7) -0.004(7) -0.003(6) -0.011(7)
N2 0.041(10) 0.100(16) 0.039(10) -0.017(10) -0.013(9) 0.013(11)
N3 0.033(9) 0.049(10) 0.042(10) -0.010(8) 0.012(7) -0.001(8)
N4 0.023(8) 0.048(11) 0.043(9) -0.012(8) 0.009(7) 0.013(8)
N5 0.061(11) 0.033(9) 0.046(8) 0.012(7) 0.023(8) 0.018(7)
N6 0.080(13) 0.057(11) 0.017(7) 0.012(8) 0.003(8) 0.017(10)
N7 0.033(8) 0.036(9) 0.031(8) 0.006(6) -0.006(7) 0.007(7)
N8 0.041(10) 0.034(9) 0.039(9) -0.014(7) 0.023(7) -0.020(8)
O1 0.022(7) 0.085(12) 0.080(10) -0.041(9) -0.005(6) 0.008(7)
O2 0.050(8) 0.046(9) 0.057(8) 0.015(7) -0.032(7) -0.001(7)
O3 0.040(8) 0.047(8) 0.055(10) 0.003(8) -0.021(8) 0.005(7)
O4 0.23(3) 0.063(13) 0.083(16) -0.007(11) -0.010(18) 0.042(16)
O5 0.034(8) 0.025(7) 0.067(9) 0.006(7) -0.001(7) -0.006(6)
O6 0.026(7) 0.062(10) 0.050(8) -0.005(7) -0.002(6) 0.013(7)
O7 0.124(14) 0.031(8) 0.046(10) 0.001(8) -0.058(10) -0.007(9)
O8 0.048(10) 0.19(2) 0.036(9) -0.001(11) 0.015(7) 0.027(12)

#----------------------------------------------------------------------------#
# 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
Pb1 N3 2.455(15) . yes
Pb1 O2 2.564(13) . yes
Pb1 O3 2.608(13) 6_455 yes
Pb1 N4 2.612(17) . yes
Pb1 N1 2.616(15) . yes
Pb1 N2 2.708(16) . yes
Pb1 O3 2.844(16) . yes
Pb2 N7 2.530(14) . yes
Pb2 O6 2.550(14) . yes
Pb2 N8 2.654(14) . yes
Pb2 N5 2.673(17) . yes
Pb2 N6 2.679(14) . yes
Pb2 O7 2.697(15) 4_657 yes
Pb2 O7 2.824(15) . yes
C1 O1 1.24(2) . ?
C1 O2 1.25(2) . ?
C1 C2 1.48(3) . ?
C2 N1 1.33(2) . ?
C2 C3 1.40(3) . ?
C3 C4 1.36(4) . ?
C3 H3 0.93 . ?
C4 C5 1.37(3) . ?
C4 H4 0.93 . ?
C5 C6 1.38(3) . ?
C5 H5 0.93 . ?
C6 N1 1.38(2) . ?
C6 C7 1.45(3) . ?
C7 N2 1.46(3) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 N2 1.42(3) . ?
C8 C9 1.52(3) . ?
C8 H8A 0.97 . ?
C8 H8B 0.97 . ?
C9 N3 1.53(3) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 N3 1.46(2) . ?
C10 C11 1.56(3) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C11 N4 1.33(2) . ?
C11 C12 1.33(3) . ?
C12 C13 1.33(3) . ?
C12 H12 0.93 . ?
C13 C14 1.33(3) . ?
C13 H13 0.93 . ?
C14 C15 1.39(3) . ?
C14 H14 0.93 . ?
C15 N4 1.34(2) . ?
C15 C16 1.52(3) . ?
C16 O3 1.21(2) . ?
C16 O4 1.28(3) . ?
C17 O5 1.21(2) . ?
C17 O6 1.24(2) . ?
C17 C18 1.51(3) . ?
C18 N5 1.35(3) . ?
C18 C19 1.42(3) . ?
C19 C20 1.33(4) . ?
C19 H19 0.93 . ?
C20 C21 1.22(3) . ?
C20 H20 0.93 . ?
C21 C22 1.44(3) . ?
C21 H21 0.93 . ?
C22 N5 1.34(3) . ?
C22 C23 1.53(4) . ?
C23 N6 1.51(3) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C24 C25 1.38(3) . ?
C24 N6 1.48(2) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C25 N7 1.53(2) . ?
C25 H25A 0.97 . ?
C25 H25B 0.97 . ?
C26 N7 1.43(2) . ?
C26 C27 1.50(3) . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C27 N8 1.35(3) . ?
C27 C28 1.37(2) . ?
C28 C29 1.33(3) . ?
C28 H28 0.93 . ?
C29 C30 1.44(3) . ?
C29 H29 0.93 . ?
C30 C31 1.38(3) . ?
C30 H30 0.93 . ?
C31 N8 1.34(2) . ?
C31 C32 1.54(3) . ?
C32 O7 1.20(2) . ?
C32 O8 1.27(2) . ?
N2 H2 0.91 . ?
N3 H3A 0.91 . ?
N6 H6 0.91 . ?
N7 H7 0.91 . ?
O3 Pb1 2.608(13) 8 ?
O7 Pb2 2.697(15) 2_567 ?

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
N3 Pb1 O2 84.8(5) . . yes
N3 Pb1 O3 81.4(5) . 6_455 yes
O2 Pb1 O3 151.9(5) . 6_455 yes
N3 Pb1 N4 66.2(5) . . yes
O2 Pb1 N4 71.8(5) . . yes
O3 Pb1 N4 80.3(5) 6_455 . yes
N3 Pb1 N1 88.2(5) . . yes
O2 Pb1 N1 61.0(5) . . yes
O3 Pb1 N1 142.1(5) 6_455 . yes
N4 Pb1 N1 128.0(5) . . yes
N3 Pb1 N2 67.0(6) . . yes
O2 Pb1 N2 114.5(5) . . yes
O3 Pb1 N2 82.2(5) 6_455 . yes
N4 Pb1 N2 131.8(6) . . yes
N1 Pb1 N2 60.3(5) . . yes
N3 Pb1 O3 126.4(4) . . yes
O2 Pb1 O3 74.5(5) . . yes
O3 Pb1 O3 94.4(4) 6_455 . yes
N4 Pb1 O3 60.5(4) . . yes
N1 Pb1 O3 120.5(4) . . yes
N2 Pb1 O3 165.7(5) . . yes
N7 Pb2 O6 91.3(5) . . yes
N7 Pb2 N8 65.6(5) . . yes
O6 Pb2 N8 72.2(4) . . yes
N7 Pb2 N5 87.0(5) . . yes
O6 Pb2 N5 61.1(5) . . yes
N8 Pb2 N5 124.9(5) . . yes
N7 Pb2 N6 67.4(5) . . yes
O6 Pb2 N6 118.6(5) . . yes
N8 Pb2 N6 132.0(5) . . yes
N5 Pb2 N6 60.9(6) . . yes
N7 Pb2 O7 86.6(5) . 4_657 yes
O6 Pb2 O7 159.3(5) . 4_657 yes
N8 Pb2 O7 88.3(5) . 4_657 yes
N5 Pb2 O7 139.1(5) . 4_657 yes
N6 Pb2 O7 79.5(5) . 4_657 yes
N7 Pb2 O7 123.9(5) . . yes
O6 Pb2 O7 71.1(4) . . yes
N8 Pb2 O7 58.3(5) . . yes
N5 Pb2 O7 123.4(6) . . yes
N6 Pb2 O7 166.4(5) . . yes
O7 Pb2 O7 93.1(5) 4_657 . yes
O1 C1 O2 126(2) . . ?
O1 C1 C2 116(2) . . ?
O2 C1 C2 118.1(17) . . ?
N1 C2 C3 123(2) . . ?
N1 C2 C1 114.8(18) . . ?
C3 C2 C1 122(2) . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C5 121.2(19) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 118(2) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
N1 C6 C5 121.1(18) . . ?
N1 C6 C7 113.3(16) . . ?
C5 C6 C7 126(2) . . ?
C6 C7 N2 113.4(17) . . ?
C6 C7 H7A 108.9 . . ?
N2 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
N2 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
N2 C8 C9 111(2) . . ?
N2 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N2 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108 . . ?
C8 C9 N3 108.5(18) . . ?
C8 C9 H9A 110 . . ?
N3 C9 H9A 110 . . ?
C8 C9 H9B 110 . . ?
N3 C9 H9B 110 . . ?
H9A C9 H9B 108.4 . . ?
N3 C10 C11 110.6(14) . . ?
N3 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N4 C11 C12 121.0(17) . . ?
N4 C11 C10 112.2(16) . . ?
C12 C11 C10 126.8(17) . . ?
C11 C12 C13 121(2) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 121(2) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 116(2) . . ?
C13 C14 H14 122 . . ?
C15 C14 H14 122 . . ?
N4 C15 C14 123(2) . . ?
N4 C15 C16 115.8(16) . . ?
C14 C15 C16 120.7(19) . . ?
O3 C16 O4 124(2) . . ?
O3 C16 C15 122(2) . . ?
O4 C16 C15 113(2) . . ?
O5 C17 O6 126.6(18) . . ?
O5 C17 C18 115.5(17) . . ?
O6 C17 C18 117.5(19) . . ?
N5 C18 C19 117(2) . . ?
N5 C18 C17 114.9(18) . . ?
C19 C18 C17 128(2) . . ?
C20 C19 C18 124(3) . . ?
C20 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
C21 C20 C19 117(3) . . ?
C21 C20 H20 121.6 . . ?
C19 C20 H20 121.6 . . ?
C20 C21 C22 126(2) . . ?
C20 C21 H21 117.2 . . ?
C22 C21 H21 117.2 . . ?
N5 C22 C21 117(2) . . ?
N5 C22 C23 118(2) . . ?
C21 C22 C23 125(2) . . ?
N6 C23 C22 106(2) . . ?
N6 C23 H23A 110.5 . . ?
C22 C23 H23A 110.5 . . ?
N6 C23 H23B 110.5 . . ?
C22 C23 H23B 110.5 . . ?
H23A C23 H23B 108.7 . . ?
C25 C24 N6 113.9(17) . . ?
C25 C24 H24A 108.8 . . ?
N6 C24 H24A 108.8 . . ?
C25 C24 H24B 108.8 . . ?
N6 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C24 C25 N7 113.6(18) . . ?
C24 C25 H25A 108.9 . . ?
N7 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
N7 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
N7 C26 C27 114.5(15) . . ?
N7 C26 H26A 108.6 . . ?
C27 C26 H26A 108.6 . . ?
N7 C26 H26B 108.6 . . ?
C27 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
N8 C27 C28 121.8(18) . . ?
N8 C27 C26 116.2(15) . . ?
C28 C27 C26 122(2) . . ?
C29 C28 C27 123(2) . . ?
C29 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
C28 C29 C30 115.6(18) . . ?
C28 C29 H29 122.2 . . ?
C30 C29 H29 122.2 . . ?
C31 C30 C29 120.3(17) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
N8 C31 C30 121(2) . . ?
N8 C31 C32 114.9(17) . . ?
C30 C31 C32 124.0(16) . . ?
O7 C32 O8 131(2) . . ?
O7 C32 C31 117.9(15) . . ?
O8 C32 C31 110.1(19) . . ?
C2 N1 C6 118.2(16) . . ?
C2 N1 Pb1 120.1(13) . . ?
C6 N1 Pb1 121.3(11) . . ?
C8 N2 C7 113.5(17) . . ?
C8 N2 Pb1 110.1(13) . . ?
C7 N2 Pb1 107.6(13) . . ?
C8 N2 H2 108.5 . . ?
C7 N2 H2 108.5 . . ?
Pb1 N2 H2 108.5 . . ?
C10 N3 C9 107.4(16) . . ?
C10 N3 Pb1 113.6(11) . . ?
C9 N3 Pb1 116.8(14) . . ?
C10 N3 H3A 106.1 . . ?
C9 N3 H3A 106.1 . . ?
Pb1 N3 H3A 106.1 . . ?
C11 N4 C15 117.0(17) . . ?
C11 N4 Pb1 117.8(11) . . ?
C15 N4 Pb1 122.6(13) . . ?
C22 N5 C18 119.9(19) . . ?
C22 N5 Pb2 120.6(16) . . ?
C18 N5 Pb2 119.5(13) . . ?
C24 N6 C23 113.8(15) . . ?
C24 N6 Pb2 110.4(11) . . ?
C23 N6 Pb2 112.8(14) . . ?
C24 N6 H6 106.4 . . ?
C23 N6 H6 106.4 . . ?
Pb2 N6 H6 106.4 . . ?
C26 N7 C25 111.9(15) . . ?
C26 N7 Pb2 114.1(11) . . ?
C25 N7 Pb2 112.3(11) . . ?
C26 N7 H7 106 . . ?
C25 N7 H7 106 . . ?
Pb2 N7 H7 106 . . ?
C31 N8 C27 118.7(17) . . ?
C31 N8 Pb2 124.0(15) . . ?
C27 N8 Pb2 116.1(11) . . ?
C1 O2 Pb1 122.0(12) . . ?
C16 O3 Pb1 134.5(16) . 8 ?
C16 O3 Pb1 116.3(15) . . ?
Pb1 O3 Pb1 109.0(5) 8 . ?
C17 O6 Pb2 126.8(13) . . ?
C32 O7 Pb2 135.7(14) . 2_567 ?
C32 O7 Pb2 121.5(13) . . ?
Pb2 O7 Pb2 101.8(6) 2_567 . ?

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
O1 C1 C2 N1 -169.4(16) . . . . ?
O2 C1 C2 N1 8.5(16) . . . . ?
O1 C1 C2 C3 11.3(16) . . . . ?
O2 C1 C2 C3 -170.7(16) . . . . ?
N1 C2 C3 C4 3(2) . . . . ?
C1 C2 C3 C4 -178.2(14) . . . . ?
C2 C3 C4 C5 -6(3) . . . . ?
C3 C4 C5 C6 8(3) . . . . ?
C4 C5 C6 N1 -6(3) . . . . ?
C4 C5 C6 C7 176.7(18) . . . . ?
N1 C6 C7 N2 -33(2) . . . . ?
C5 C6 C7 N2 145.4(18) . . . . ?
N2 C8 C9 N3 -59(3) . . . . ?
N3 C10 C11 N4 46(2) . . . . ?
N3 C10 C11 C12 -133.3(19) . . . . ?
N4 C11 C12 C13 6(3) . . . . ?
C10 C11 C12 C13 -174.6(19) . . . . ?
C11 C12 C13 C14 -4(4) . . . . ?
C12 C13 C14 C15 0(3) . . . . ?
C13 C14 C15 N4 2(3) . . . . ?
C13 C14 C15 C16 -179(2) . . . . ?
N4 C15 C16 O3 -7(3) . . . . ?
C14 C15 C16 O3 173(2) . . . . ?
N4 C15 C16 O4 161(2) . . . . ?
C14 C15 C16 O4 -18(4) . . . . ?
O5 C17 C18 N5 169.3(16) . . . . ?
O6 C17 C18 N5 -4(2) . . . . ?
O5 C17 C18 C19 -12(3) . . . . ?
O6 C17 C18 C19 174.7(15) . . . . ?
N5 C18 C19 C20 0.1(17) . . . . ?
C17 C18 C19 C20 -179.0(19) . . . . ?
C18 C19 C20 C21 -3(2) . . . . ?
C19 C20 C21 C22 5(3) . . . . ?
C20 C21 C22 N5 -4(3) . . . . ?
C20 C21 C22 C23 176(2) . . . . ?
N5 C22 C23 N6 35(2) . . . . ?
C21 C22 C23 N6 -145.7(18) . . . . ?
N6 C24 C25 N7 56(2) . . . . ?
N7 C26 C27 N8 -38(2) . . . . ?
N7 C26 C27 C28 142.5(14) . . . . ?
N8 C27 C28 C29 -1.6(15) . . . . ?
C26 C27 C28 C29 177.7(16) . . . . ?
C27 C28 C29 C30 0.3(14) . . . . ?
C28 C29 C30 C31 0(2) . . . . ?
C29 C30 C31 N8 0(3) . . . . ?
C29 C30 C31 C32 -177.8(16) . . . . ?
N8 C31 C32 O7 1(3) . . . . ?
C30 C31 C32 O7 179(2) . . . . ?
N8 C31 C32 O8 171.5(18) . . . . ?
C30 C31 C32 O8 -10(3) . . . . ?
C3 C2 N1 C6 0(2) . . . . ?
C1 C2 N1 C6 -179.6(12) . . . . ?
C3 C2 N1 Pb1 -172.8(10) . . . . ?
C1 C2 N1 Pb1 8.0(13) . . . . ?
C5 C6 N1 C2 2(2) . . . . ?
C7 C6 N1 C2 179.9(14) . . . . ?
C5 C6 N1 Pb1 174.1(12) . . . . ?
C7 C6 N1 Pb1 -7.9(19) . . . . ?
N3 Pb1 N1 C2 -97.6(11) . . . . ?
O2 Pb1 N1 C2 -12.6(10) . . . . ?
O3 Pb1 N1 C2 -171.1(9) 6_455 . . . ?
N4 Pb1 N1 C2 -40.1(13) . . . . ?
N2 Pb1 N1 C2 -162.0(13) . . . . ?
O3 Pb1 N1 C2 34.5(12) . . . . ?
N3 Pb1 N1 C6 90.3(13) . . . . ?
O2 Pb1 N1 C6 175.3(14) . . . . ?
O3 Pb1 N1 C6 16.8(16) 6_455 . . . ?
N4 Pb1 N1 C6 147.8(12) . . . . ?
N2 Pb1 N1 C6 25.9(12) . . . . ?
O3 Pb1 N1 C6 -137.6(11) . . . . ?
C9 C8 N2 C7 165.5(18) . . . . ?
C9 C8 N2 Pb1 45(2) . . . . ?
C6 C7 N2 C8 -68(2) . . . . ?
C6 C7 N2 Pb1 53.7(19) . . . . ?
N3 Pb1 N2 C8 -16.1(13) . . . . ?
O2 Pb1 N2 C8 56.3(15) . . . . ?
O3 Pb1 N2 C8 -100.0(14) 6_455 . . . ?
N4 Pb1 N2 C8 -30.6(16) . . . . ?
N1 Pb1 N2 C8 85.6(14) . . . . ?
O3 Pb1 N2 C8 -176.8(16) . . . . ?
N3 Pb1 N2 C7 -140.3(14) . . . . ?
O2 Pb1 N2 C7 -67.8(14) . . . . ?
O3 Pb1 N2 C7 135.8(14) 6_455 . . . ?
N4 Pb1 N2 C7 -154.8(12) . . . . ?
N1 Pb1 N2 C7 -38.6(12) . . . . ?
O3 Pb1 N2 C7 59(3) . . . . ?
C11 C10 N3 C9 -179.5(19) . . . . ?
C11 C10 N3 Pb1 -48.9(17) . . . . ?
C8 C9 N3 C10 172(2) . . . . ?
C8 C9 N3 Pb1 43(3) . . . . ?
O2 Pb1 N3 C10 99.8(13) . . . . ?
O3 Pb1 N3 C10 -55.7(12) 6_455 . . . ?
N4 Pb1 N3 C10 27.4(12) . . . . ?
N1 Pb1 N3 C10 160.9(13) . . . . ?
N2 Pb1 N3 C10 -140.8(14) . . . . ?
O3 Pb1 N3 C10 33.4(14) . . . . ?
O2 Pb1 N3 C9 -134.4(17) . . . . ?
O3 Pb1 N3 C9 70.1(17) 6_455 . . . ?
N4 Pb1 N3 C9 153.2(18) . . . . ?
N1 Pb1 N3 C9 -73.3(17) . . . . ?
N2 Pb1 N3 C9 -15.0(17) . . . . ?
O3 Pb1 N3 C9 159.2(16) . . . . ?
C12 C11 N4 C15 -4(3) . . . . ?
C10 C11 N4 C15 176.6(16) . . . . ?
C12 C11 N4 Pb1 158.1(14) . . . . ?
C10 C11 N4 Pb1 -21.1(18) . . . . ?
C14 C15 N4 C11 0(3) . . . . ?
C16 C15 N4 C11 -179.3(18) . . . . ?
C14 C15 N4 Pb1 -161.2(16) . . . . ?
C16 C15 N4 Pb1 19(3) . . . . ?
N3 Pb1 N4 C11 -2.5(12) . . . . ?
O2 Pb1 N4 C11 -94.8(13) . . . . ?
O3 Pb1 N4 C11 82.4(13) 6_455 . . . ?
N1 Pb1 N4 C11 -69.6(15) . . . . ?
N2 Pb1 N4 C11 12.2(16) . . . . ?
O3 Pb1 N4 C11 -176.9(15) . . . . ?
N3 Pb1 N4 C15 158.9(16) . . . . ?
O2 Pb1 N4 C15 66.5(15) . . . . ?
O3 Pb1 N4 C15 -116.3(15) 6_455 . . . ?
N1 Pb1 N4 C15 91.7(15) . . . . ?
N2 Pb1 N4 C15 173.5(14) . . . . ?
O3 Pb1 N4 C15 -15.6(14) . . . . ?
C21 C22 N5 C18 1(3) . . . . ?
C23 C22 N5 C18 -179.6(16) . . . . ?
C21 C22 N5 Pb2 179.1(13) . . . . ?
C23 C22 N5 Pb2 -1(2) . . . . ?
C19 C18 N5 C22 1(2) . . . . ?
C17 C18 N5 C22 -179.8(16) . . . . ?
C19 C18 N5 Pb2 -177.5(9) . . . . ?
C17 C18 N5 Pb2 1.8(19) . . . . ?
N7 Pb2 N5 C22 -85.0(13) . . . . ?
O6 Pb2 N5 C22 -178.1(15) . . . . ?
N8 Pb2 N5 C22 -142.3(13) . . . . ?
N6 Pb2 N5 C22 -19.3(13) . . . . ?
O7 Pb2 N5 C22 -3.6(17) 4_657 . . . ?
O7 Pb2 N5 C22 145.6(13) . . . . ?
N7 Pb2 N5 C18 93.4(13) . . . . ?
O6 Pb2 N5 C18 0.3(12) . . . . ?
N8 Pb2 N5 C18 36.1(15) . . . . ?
N6 Pb2 N5 C18 159.1(14) . . . . ?
O7 Pb2 N5 C18 174.8(11) 4_657 . . . ?
O7 Pb2 N5 C18 -36.0(14) . . . . ?
C25 C24 N6 C23 -164(2) . . . . ?
C25 C24 N6 Pb2 -36(2) . . . . ?
C22 C23 N6 C24 76(2) . . . . ?
C22 C23 N6 Pb2 -51.3(18) . . . . ?
N7 Pb2 N6 C24 8.2(13) . . . . ?
O6 Pb2 N6 C24 -70.3(14) . . . . ?
N8 Pb2 N6 C24 20.9(17) . . . . ?
N5 Pb2 N6 C24 -91.5(14) . . . . ?
O7 Pb2 N6 C24 98.9(14) 4_657 . . . ?
O7 Pb2 N6 C24 156(2) . . . . ?
N7 Pb2 N6 C23 136.8(16) . . . . ?
O6 Pb2 N6 C23 58.3(16) . . . . ?
N8 Pb2 N6 C23 149.5(13) . . . . ?
N5 Pb2 N6 C23 37.1(14) . . . . ?
O7 Pb2 N6 C23 -132.5(16) 4_657 . . . ?
O7 Pb2 N6 C23 -75(3) . . . . ?
C27 C26 N7 C25 170.7(15) . . . . ?
C27 C26 N7 Pb2 41.8(18) . . . . ?
C24 C25 N7 C26 -175.3(16) . . . . ?
C24 C25 N7 Pb2 -45.5(19) . . . . ?
O6 Pb2 N7 C26 -93.7(11) . . . . ?
N8 Pb2 N7 C26 -23.9(10) . . . . ?
N5 Pb2 N7 C26 -154.7(12) . . . . ?
N6 Pb2 N7 C26 145.7(13) . . . . ?
O7 Pb2 N7 C26 65.7(12) 4_657 . . . ?
O7 Pb2 N7 C26 -25.7(13) . . . . ?
O6 Pb2 N7 C25 137.7(12) . . . . ?
N8 Pb2 N7 C25 -152.5(14) . . . . ?
N5 Pb2 N7 C25 76.7(13) . . . . ?
N6 Pb2 N7 C25 17.1(12) . . . . ?
O7 Pb2 N7 C25 -62.9(13) 4_657 . . . ?
O7 Pb2 N7 C25 -154.3(12) . . . . ?
C30 C31 N8 C27 -1(3) . . . . ?
C32 C31 N8 C27 176.8(16) . . . . ?
C30 C31 N8 Pb2 165.4(13) . . . . ?
C32 C31 N8 Pb2 -16(2) . . . . ?
C28 C27 N8 C31 2(2) . . . . ?
C26 C27 N8 C31 -177.2(16) . . . . ?
C28 C27 N8 Pb2 -165.8(9) . . . . ?
C26 C27 N8 Pb2 14.8(19) . . . . ?
N7 Pb2 N8 C31 -162.8(16) . . . . ?
O6 Pb2 N8 C31 -62.9(15) . . . . ?
N5 Pb2 N8 C31 -95.5(16) . . . . ?
N6 Pb2 N8 C31 -175.7(14) . . . . ?
O7 Pb2 N8 C31 110.1(15) 4_657 . . . ?
O7 Pb2 N8 C31 15.5(14) . . . . ?
N7 Pb2 N8 C27 4.4(12) . . . . ?
O6 Pb2 N8 C27 104.3(12) . . . . ?
N5 Pb2 N8 C27 71.7(14) . . . . ?
N6 Pb2 N8 C27 -8.5(15) . . . . ?
O7 Pb2 N8 C27 -82.7(12) 4_657 . . . ?
O7 Pb2 N8 C27 -177.3(14) . . . . ?
O1 C1 O2 Pb1 155.9(14) . . . . ?
C2 C1 O2 Pb1 -21.8(18) . . . . ?
N3 Pb1 O2 C1 108.9(14) . . . . ?
O3 Pb1 O2 C1 169.6(11) 6_455 . . . ?
N4 Pb1 O2 C1 175.5(15) . . . . ?
N1 Pb1 O2 C1 18.1(13) . . . . ?
N2 Pb1 O2 C1 47.1(15) . . . . ?
O3 Pb1 O2 C1 -121.0(14) . . . . ?
O4 C16 O3 Pb1 0(4) . . . 8 ?
C15 C16 O3 Pb1 167.5(14) . . . 8 ?
O4 C16 O3 Pb1 -174(2) . . . . ?
C15 C16 O3 Pb1 -7(3) . . . . ?
N3 Pb1 O3 C16 4.6(18) . . . . ?
O2 Pb1 O3 C16 -66.6(17) . . . . ?
O3 Pb1 O3 C16 87.1(18) 6_455 . . . ?
N4 Pb1 O3 C16 10.9(16) . . . . ?
N1 Pb1 O3 C16 -108.3(17) . . . . ?
N2 Pb1 O3 C16 162(2) . . . . ?
N3 Pb1 O3 Pb1 -170.9(5) . . . 8 ?
O2 Pb1 O3 Pb1 117.8(6) . . . 8 ?
O3 Pb1 O3 Pb1 -88.43(14) 6_455 . . 8 ?
N4 Pb1 O3 Pb1 -164.7(7) . . . 8 ?
N1 Pb1 O3 Pb1 76.1(6) . . . 8 ?
N2 Pb1 O3 Pb1 -13(2) . . . 8 ?
O5 C17 O6 Pb2 -167.5(14) . . . . ?
C18 C17 O6 Pb2 5(2) . . . . ?
N7 Pb2 O6 C17 -89.1(15) . . . . ?
N8 Pb2 O6 C17 -153.0(16) . . . . ?
N5 Pb2 O6 C17 -3.2(14) . . . . ?
N6 Pb2 O6 C17 -24.3(16) . . . . ?
O7 Pb2 O6 C17 -172.9(14) 4_657 . . . ?
O7 Pb2 O6 C17 145.3(15) . . . . ?
O8 C32 O7 Pb2 11(4) . . . 2_567 ?
C31 C32 O7 Pb2 179.3(13) . . . 2_567 ?
O8 C32 O7 Pb2 -155(2) . . . . ?
C31 C32 O7 Pb2 13(3) . . . . ?
N7 Pb2 O7 C32 -13(2) . . . . ?
O6 Pb2 O7 C32 65.5(17) . . . . ?
N8 Pb2 O7 C32 -14.8(16) . . . . ?
N5 Pb2 O7 C32 98.8(18) . . . . ?
N6 Pb2 O7 C32 -157(2) . . . . ?
O7 Pb2 O7 C32 -101(2) 4_657 . . . ?
N7 Pb2 O7 Pb2 177.0(5) . . . 2_567 ?
O6 Pb2 O7 Pb2 -104.7(6) . . . 2_567 ?
N8 Pb2 O7 Pb2 175.1(7) . . . 2_567 ?
N5 Pb2 O7 Pb2 -71.4(6) . . . 2_567 ?
N6 Pb2 O7 Pb2 33(3) . . . 2_567 ?
O7 Pb2 O7 Pb2 88.98(11) 4_657 . . 2_567 ?

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.004 0.192 0.889 2413.9 570.0
2 0.000 0.500 0.750 7.2 -2.2
3 0.500 0.000 0.250 7.2 -2.2
_platon_squeeze_details          
;
;

# Attachment '[Zn(bcpe)].cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2007-07-26 at 15:40:01
# 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 : rfm611129s struct

data_rfm611129s
_database_code_depnum_ccdc_archive 'CCDC 689095'

_audit_creation_date             2007-07-26T15:40:01-00:00
_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        
;
?
;
_chemical_formula_moiety         'C16 H16 N4 O4 Zn, 3(H2 O)'
_chemical_formula_sum            'C16 H22 N4 O7 Zn'
_chemical_formula_weight         447.75
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_Int_Tables_number      34
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, z'

_cell_length_a                   11.4629(5)
_cell_length_b                   15.4564(7)
_cell_length_c                   10.6802(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1892.27(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    6184
_cell_measurement_theta_min      2.212
_cell_measurement_theta_max      28.1772
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_process_details   
;
SADABS: Area-Detector Absorption Correction;
Siemens Industrial Automation, Inc.: Madison, WI, 1996.
;

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

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'omega and phi scans with narrow frames'
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_number            13474
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             3693
_reflns_number_gt                3285
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_structure_solution    'DIRDIF99 (Beurskens ET AL. 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.4071P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3693
_refine_ls_number_parameters     271
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0621
_refine_ls_wR_factor_gt          0.0602
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.056
_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   0.009(11)
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.056

#----------------------------------------------------------------------------#
# 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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
Zn1 Zn 1.00608(2) 0.776748(14) 0.99354(5) 0.01493(7) Uani 1 1 d . . .
O1 O 0.88954(16) 0.88144(11) 1.05277(17) 0.0206(4) Uani 1 1 d . . .
O3 O 0.88015(13) 0.67684(10) 0.9876(2) 0.0225(4) Uani 1 1 d . . .
O2 O 0.77932(14) 0.98941(10) 0.9763(2) 0.0202(4) Uani 1 1 d . . .
O7 O 0.69322(17) 0.96725(13) 0.3769(2) 0.0240(4) Uani 1 1 d D . .
N1 N 0.96290(17) 0.83776(13) 0.8293(2) 0.0149(4) Uani 1 1 d . . .
O4 O 0.81886(18) 0.56059(13) 1.0939(2) 0.0345(5) Uani 1 1 d . . .
O6 O 0.41671(18) 0.56599(14) 0.7984(2) 0.0273(4) Uani 1 1 d D . .
N4 N 1.02830(18) 0.71950(12) 1.1654(2) 0.0151(4) Uani 1 1 d . . .
N3 N 1.17099(17) 0.83414(13) 1.0680(2) 0.0165(4) Uani 1 1 d . . .
H3N H 1.1786 0.8914 1.0426 0.02 Uiso 1 1 calc R . .
N2 N 1.12815(17) 0.71865(13) 0.8567(2) 0.0172(4) Uani 1 1 d . . .
H2N H 1.1394 0.6604 0.8748 0.021 Uiso 1 1 calc R . .
C1 C 0.8493(2) 0.92746(15) 0.9656(2) 0.0164(5) Uani 1 1 d . . .
C9 C 1.26325(19) 0.77968(16) 1.0110(3) 0.0200(6) Uani 1 1 d . . .
H9A H 1.2657 0.7228 1.0535 0.024 Uiso 1 1 calc R . .
H9B H 1.3401 0.8079 1.0219 0.024 Uiso 1 1 calc R . .
C3 C 0.8588(2) 0.95032(16) 0.7277(3) 0.0184(5) Uani 1 1 d . . .
H3 H 0.8057 0.9975 0.7314 0.022 Uiso 1 1 calc R . .
C10 C 1.1732(2) 0.82776(16) 1.2059(3) 0.0197(5) Uani 1 1 d . . .
H10A H 1.1375 0.8802 1.2431 0.024 Uiso 1 1 calc R . .
H10B H 1.2549 0.8239 1.2354 0.024 Uiso 1 1 calc R . .
C6 C 1.0074(2) 0.81066(15) 0.7210(3) 0.0167(5) Uani 1 1 d . . .
C8 C 1.2389(2) 0.76677(16) 0.8723(3) 0.0201(6) Uani 1 1 d . . .
H8A H 1.2332 0.8237 0.8302 0.024 Uiso 1 1 calc R . .
H8B H 1.3036 0.734 0.8334 0.024 Uiso 1 1 calc R . .
C12 C 1.1217(2) 0.70670(17) 1.3621(3) 0.0206(5) Uani 1 1 d . . .
H12 H 1.1787 0.7262 1.4202 0.025 Uiso 1 1 calc R . .
C14 C 0.9686(2) 0.60751(17) 1.3021(3) 0.0214(6) Uani 1 1 d . . .
H14 H 0.9189 0.56 1.3204 0.026 Uiso 1 1 calc R . .
C4 C 0.9063(2) 0.92393(16) 0.6143(3) 0.0211(5) Uani 1 1 d . . .
H4 H 0.8871 0.954 0.5395 0.025 Uiso 1 1 calc R . .
C13 C 1.0509(2) 0.63574(17) 1.3886(3) 0.0232(6) Uani 1 1 d . . .
H13 H 1.0588 0.6065 1.4664 0.028 Uiso 1 1 calc R . .
C7 C 1.0807(2) 0.72853(16) 0.7297(3) 0.0214(6) Uani 1 1 d . . .
H7A H 1.0319 0.6777 0.7087 0.026 Uiso 1 1 calc R . .
H7B H 1.1455 0.7315 0.6685 0.026 Uiso 1 1 calc R . .
C11 C 1.1062(2) 0.74811(17) 1.2474(3) 0.0169(5) Uani 1 1 d . . .
C15 C 0.9611(2) 0.65025(15) 1.1892(3) 0.0173(5) Uani 1 1 d . . .
C2 C 0.8906(2) 0.90620(16) 0.8348(2) 0.0150(5) Uani 1 1 d . . .
C16 C 0.8793(2) 0.62712(16) 1.0815(3) 0.0216(6) Uani 1 1 d . . .
C5 C 0.9819(2) 0.85369(16) 0.6098(3) 0.0200(5) Uani 1 1 d . . .
H5 H 1.0154 0.8355 0.5328 0.024 Uiso 1 1 calc R . .
O5 O 0.89004(18) 0.53497(13) 0.6530(2) 0.0270(4) Uani 1 1 d D . .
H60 H 0.397(3) 0.5768(17) 0.729(3) 0.025 Uiso 1 1 d D . .
H50 H 0.8362(19) 0.5170(18) 0.599(3) 0.025 Uiso 1 1 d D . .
H51 H 0.9521(16) 0.5120(18) 0.631(3) 0.025 Uiso 1 1 d D . .
H70 H 0.656(2) 0.9992(17) 0.324(3) 0.025 Uiso 1 1 d D . .
H71 H 0.7644(15) 0.9684(19) 0.360(3) 0.025 Uiso 1 1 d D . .
H61 H 0.463(2) 0.5232(16) 0.805(3) 0.025 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01415(11) 0.01577(11) 0.01487(12) 0.00245(15) 0.00015(14) -0.00020(10)
O1 0.0232(9) 0.0221(9) 0.0164(10) 0.0011(7) 0.0001(7) 0.0055(8)
O3 0.0199(8) 0.0266(8) 0.0208(10) 0.0012(9) -0.0004(10) -0.0081(6)
O2 0.0194(8) 0.0189(8) 0.0222(14) -0.0043(8) -0.0002(8) 0.0041(6)
O7 0.0209(10) 0.0214(10) 0.0296(12) 0.0021(9) 0.0003(8) 0.0019(8)
N1 0.0155(10) 0.0134(10) 0.0159(11) -0.0017(8) -0.0007(8) -0.0008(8)
O4 0.0405(12) 0.0356(12) 0.0273(12) 0.0018(9) 0.0038(10) -0.0247(10)
O6 0.0250(11) 0.0386(12) 0.0182(11) 0.0035(9) -0.0010(9) 0.0026(9)
N4 0.0170(10) 0.0136(10) 0.0146(11) -0.0001(8) 0.0013(8) 0.0010(8)
N3 0.0161(10) 0.0116(10) 0.0217(12) 0.0033(8) -0.0010(8) 0.0001(8)
N2 0.0183(10) 0.0119(10) 0.0214(12) 0.0005(8) 0.0032(9) 0.0012(8)
C1 0.0152(11) 0.0156(11) 0.0182(15) -0.0040(9) -0.0012(9) -0.0032(9)
C9 0.0134(10) 0.0187(11) 0.0279(17) 0.0031(11) 0.0020(12) 0.0009(9)
C3 0.0149(12) 0.0169(12) 0.0233(15) 0.0020(10) -0.0035(11) -0.0008(9)
C10 0.0165(12) 0.0184(12) 0.0240(15) -0.0002(11) -0.0022(10) -0.0025(9)
C6 0.0168(12) 0.0145(11) 0.0187(13) -0.0013(9) -0.0010(10) -0.0050(9)
C8 0.0147(12) 0.0182(13) 0.0273(15) 0.0053(11) 0.0029(10) 0.0017(9)
C12 0.0210(12) 0.0253(13) 0.0154(13) -0.0007(11) -0.0019(10) 0.0066(10)
C14 0.0225(13) 0.0190(13) 0.0229(15) 0.0051(11) 0.0078(11) 0.0034(10)
C4 0.0241(13) 0.0224(13) 0.0168(14) 0.0033(11) -0.0067(11) -0.0058(10)
C13 0.0242(13) 0.0274(14) 0.0180(15) 0.0071(11) 0.0047(11) 0.0113(11)
C7 0.0221(14) 0.0190(14) 0.0232(16) -0.0021(11) 0.0029(12) 0.0035(11)
C11 0.0163(12) 0.0164(12) 0.0180(14) -0.0009(10) 0.0011(10) 0.0053(10)
C15 0.0168(11) 0.0143(12) 0.0208(14) -0.0015(10) 0.0047(10) 0.0008(9)
C2 0.0131(11) 0.0144(11) 0.0176(13) -0.0001(9) -0.0023(9) -0.0021(9)
C16 0.0229(13) 0.0215(13) 0.0205(14) -0.0017(11) 0.0058(11) -0.0081(10)
C5 0.0207(12) 0.0216(12) 0.0177(13) -0.0036(10) 0.0012(10) -0.0063(10)
O5 0.0192(10) 0.0320(11) 0.0298(12) 0.0003(9) -0.0046(9) 0.0014(8)

#----------------------------------------------------------------------------#
# 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
Zn1 N1 2.052(2) . yes
Zn1 N4 2.054(2) . yes
Zn1 O3 2.1148(15) . yes
Zn1 O1 2.1916(18) . yes
Zn1 N2 2.214(2) . yes
Zn1 N3 2.234(2) . yes
O1 C1 1.259(3) . ?
O3 C16 1.263(3) . ?
O2 C1 1.254(3) . ?
O7 H70 0.859(17) . ?
O7 H71 0.836(17) . ?
N1 C6 1.331(3) . ?
N1 C2 1.345(3) . ?
O4 C16 1.247(3) . ?
O6 H60 0.79(3) . ?
O6 H61 0.852(16) . ?
N4 C11 1.326(3) . ?
N4 C15 1.343(3) . ?
N3 C10 1.477(3) . ?
N3 C9 1.483(3) . ?
N3 H3N 0.93 . ?
N2 C7 1.470(4) . ?
N2 C8 1.481(3) . ?
N2 H2N 0.93 . ?
C1 C2 1.511(3) . ?
C9 C8 1.520(4) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C3 C2 1.381(4) . ?
C3 C4 1.389(4) . ?
C3 H3 0.95 . ?
C10 C11 1.517(4) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C6 C5 1.392(4) . ?
C6 C7 1.525(4) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C12 C11 1.394(4) . ?
C12 C13 1.394(4) . ?
C12 H12 0.95 . ?
C14 C15 1.378(4) . ?
C14 C13 1.390(4) . ?
C14 H14 0.95 . ?
C4 C5 1.390(4) . ?
C4 H4 0.95 . ?
C13 H13 0.95 . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C15 C16 1.526(4) . ?
C5 H5 0.95 . ?
O5 H50 0.886(17) . ?
O5 H51 0.829(16) . ?

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 Zn1 N4 172.73(8) . . yes
N1 Zn1 O3 98.36(8) . . yes
N4 Zn1 O3 78.27(8) . . yes
N1 Zn1 O1 76.14(8) . . yes
N4 Zn1 O1 97.80(8) . . yes
O3 Zn1 O1 97.57(7) . . yes
N1 Zn1 N2 76.97(8) . . yes
N4 Zn1 N2 109.69(8) . . yes
O3 Zn1 N2 96.64(7) . . yes
O1 Zn1 N2 151.09(8) . . yes
N1 Zn1 N3 109.03(8) . . yes
N4 Zn1 N3 75.40(8) . . yes
O3 Zn1 N3 151.40(8) . . yes
O1 Zn1 N3 96.88(7) . . yes
N2 Zn1 N3 82.03(8) . . yes
C1 O1 Zn1 115.28(16) . . ?
C16 O3 Zn1 115.19(17) . . ?
H70 O7 H71 109(2) . . ?
C6 N1 C2 121.4(2) . . ?
C6 N1 Zn1 120.36(17) . . ?
C2 N1 Zn1 118.18(17) . . ?
H60 O6 H61 115(3) . . ?
C11 N4 C15 121.8(2) . . ?
C11 N4 Zn1 121.99(17) . . ?
C15 N4 Zn1 116.18(18) . . ?
C10 N3 C9 111.1(2) . . ?
C10 N3 Zn1 110.07(15) . . ?
C9 N3 Zn1 103.39(14) . . ?
C10 N3 H3N 110.7 . . ?
C9 N3 H3N 110.7 . . ?
Zn1 N3 H3N 110.7 . . ?
C7 N2 C8 111.7(2) . . ?
C7 N2 Zn1 109.47(15) . . ?
C8 N2 Zn1 105.30(15) . . ?
C7 N2 H2N 110.1 . . ?
C8 N2 H2N 110.1 . . ?
Zn1 N2 H2N 110.1 . . ?
O2 C1 O1 126.7(2) . . ?
O2 C1 C2 116.8(2) . . ?
O1 C1 C2 116.5(2) . . ?
N3 C9 C8 110.1(2) . . ?
N3 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N3 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.2 . . ?
C2 C3 C4 118.3(2) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
N3 C10 C11 109.7(2) . . ?
N3 C10 H10A 109.7 . . ?
C11 C10 H10A 109.7 . . ?
N3 C10 H10B 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N1 C6 C5 120.7(2) . . ?
N1 C6 C7 114.9(2) . . ?
C5 C6 C7 124.4(2) . . ?
N2 C8 C9 109.4(2) . . ?
N2 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N2 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C11 C12 C13 117.8(3) . . ?
C11 C12 H12 121.1 . . ?
C13 C12 H12 121.1 . . ?
C15 C14 C13 118.3(2) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
N2 C7 C6 110.3(2) . . ?
N2 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
N2 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N4 C11 C12 120.9(3) . . ?
N4 C11 C10 114.8(2) . . ?
C12 C11 C10 124.3(3) . . ?
N4 C15 C14 120.8(2) . . ?
N4 C15 C16 113.4(2) . . ?
C14 C15 C16 125.9(2) . . ?
N1 C2 C3 121.0(2) . . ?
N1 C2 C1 113.9(2) . . ?
C3 C2 C1 125.1(2) . . ?
O4 C16 O3 126.1(3) . . ?
O4 C16 C15 117.0(2) . . ?
O3 C16 C15 116.8(2) . . ?
C4 C5 C6 118.3(2) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
H50 O5 H51 106(2) . . ?

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 Zn1 O1 C1 1.40(16) . . . . ?
N4 Zn1 O1 C1 -174.50(17) . . . . ?
O3 Zn1 O1 C1 -95.38(17) . . . . ?
N2 Zn1 O1 C1 23.4(3) . . . . ?
N3 Zn1 O1 C1 109.37(17) . . . . ?
N1 Zn1 O3 C16 -177.25(18) . . . . ?
N4 Zn1 O3 C16 -3.79(18) . . . . ?
O1 Zn1 O3 C16 -100.24(18) . . . . ?
N2 Zn1 O3 C16 105.01(18) . . . . ?
N3 Zn1 O3 C16 19.5(3) . . . . ?
O3 Zn1 N1 C6 -85.45(18) . . . . ?
O1 Zn1 N1 C6 178.77(19) . . . . ?
N2 Zn1 N1 C6 9.48(17) . . . . ?
N3 Zn1 N1 C6 86.16(19) . . . . ?
O3 Zn1 N1 C2 95.71(17) . . . . ?
O1 Zn1 N1 C2 -0.08(16) . . . . ?
N2 Zn1 N1 C2 -169.37(18) . . . . ?
N3 Zn1 N1 C2 -92.69(18) . . . . ?
O1 Zn1 N4 C11 -83.3(2) . . . . ?
N2 Zn1 N4 C11 87.6(2) . . . . ?
N3 Zn1 N4 C11 11.85(19) . . . . ?
O3 Zn1 N4 C15 1.88(17) . . . . ?
O1 Zn1 N4 C15 98.04(17) . . . . ?
N2 Zn1 N4 C15 -91.04(18) . . . . ?
N3 Zn1 N4 C15 -166.84(19) . . . . ?
N1 Zn1 N3 C10 150.88(15) . . . . ?
N4 Zn1 N3 C10 -23.09(15) . . . . ?
O3 Zn1 N3 C10 -46.7(2) . . . . ?
O1 Zn1 N3 C10 73.21(15) . . . . ?
N2 Zn1 N3 C10 -135.93(16) . . . . ?
N1 Zn1 N3 C9 -90.37(16) . . . . ?
N4 Zn1 N3 C9 95.66(16) . . . . ?
O3 Zn1 N3 C9 72.1(2) . . . . ?
O1 Zn1 N3 C9 -168.04(15) . . . . ?
N2 Zn1 N3 C9 -17.18(16) . . . . ?
N1 Zn1 N2 C7 -22.12(15) . . . . ?
N4 Zn1 N2 C7 154.84(15) . . . . ?
O3 Zn1 N2 C7 74.96(16) . . . . ?
O1 Zn1 N2 C7 -44.0(2) . . . . ?
N3 Zn1 N2 C7 -133.85(16) . . . . ?
N1 Zn1 N2 C8 98.05(16) . . . . ?
N4 Zn1 N2 C8 -84.99(16) . . . . ?
O3 Zn1 N2 C8 -164.87(15) . . . . ?
O1 Zn1 N2 C8 76.1(2) . . . . ?
N3 Zn1 N2 C8 -13.68(15) . . . . ?
Zn1 O1 C1 O2 178.27(18) . . . . ?
Zn1 O1 C1 C2 -2.3(3) . . . . ?
C10 N3 C9 C8 164.1(2) . . . . ?
Zn1 N3 C9 C8 46.0(2) . . . . ?
C9 N3 C10 C11 -83.4(2) . . . . ?
Zn1 N3 C10 C11 30.5(2) . . . . ?
C2 N1 C6 C5 1.2(3) . . . . ?
Zn1 N1 C6 C5 -177.59(17) . . . . ?
C2 N1 C6 C7 -175.9(2) . . . . ?
Zn1 N1 C6 C7 5.3(3) . . . . ?
C7 N2 C8 C9 161.4(2) . . . . ?
Zn1 N2 C8 C9 42.7(2) . . . . ?
N3 C9 C8 N2 -63.5(2) . . . . ?
C2 C3 C4 C5 1.4(4) . . . . ?
C15 C14 C13 C12 1.4(4) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C8 N2 C7 C6 -85.6(3) . . . . ?
Zn1 N2 C7 C6 30.6(2) . . . . ?
N1 C6 C7 N2 -24.8(3) . . . . ?
C5 C6 C7 N2 158.3(2) . . . . ?
C15 N4 C11 C12 0.3(4) . . . . ?
Zn1 N4 C11 C12 -178.27(18) . . . . ?
C15 N4 C11 C10 -179.2(2) . . . . ?
Zn1 N4 C11 C10 2.2(3) . . . . ?
C13 C12 C11 N4 -1.5(4) . . . . ?
C13 C12 C11 C10 177.9(2) . . . . ?
N3 C10 C11 N4 -22.7(3) . . . . ?
N3 C10 C11 C12 157.8(2) . . . . ?
C11 N4 C15 C14 1.8(4) . . . . ?
Zn1 N4 C15 C14 -179.53(19) . . . . ?
C11 N4 C15 C16 -178.8(2) . . . . ?
Zn1 N4 C15 C16 -0.1(3) . . . . ?
C13 C14 C15 N4 -2.6(4) . . . . ?
C13 C14 C15 C16 178.0(2) . . . . ?
C6 N1 C2 C3 0.8(3) . . . . ?
Zn1 N1 C2 C3 179.64(18) . . . . ?
C6 N1 C2 C1 -179.9(2) . . . . ?
Zn1 N1 C2 C1 -1.0(3) . . . . ?
C4 C3 C2 N1 -2.1(4) . . . . ?
C4 C3 C2 C1 178.7(2) . . . . ?
O2 C1 C2 N1 -178.3(2) . . . . ?
O1 C1 C2 N1 2.3(3) . . . . ?
O2 C1 C2 C3 1.0(3) . . . . ?
O1 C1 C2 C3 -178.4(2) . . . . ?
Zn1 O3 C16 O4 -174.4(2) . . . . ?
Zn1 O3 C16 C15 4.9(3) . . . . ?
N4 C15 C16 O4 176.1(2) . . . . ?
C14 C15 C16 O4 -4.5(4) . . . . ?
N4 C15 C16 O3 -3.3(3) . . . . ?
C14 C15 C16 O3 176.1(2) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
N1 C6 C5 C4 -1.9(3) . . . . ?
C7 C6 C5 C4 174.9(2) . . . . ?

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
N3 H3N O2 0.93 2.03 2.953(2) 170.8 4_775
N2 H2N O7 0.93 2.07 2.977(3) 165.5 3_565
O6 H60 O1 0.79(3) 1.99(3) 2.764(3) 164(3) 3_464
O5 H50 O2 0.886(17) 1.914(17) 2.798(3) 174(3) 2_644
O5 H51 O5 0.829(16) 1.964(18) 2.743(4) 156(3) 4_765
O7 H70 O5 0.859(17) 1.98(2) 2.780(3) 154(3) 2_654
O7 H71 O6 0.836(17) 1.940(19) 2.744(3) 161(3) 3_564
O6 H61 O6 0.852(16) 1.951(18) 2.794(4) 170(3) 4_665