
data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Kou-Lin Zhang'
_publ_contact_author_address     
;
College of Chemistry and Chemical Engineering
Yangzhou University
Yangzhou City
225002
CHINA
;

_publ_contact_author_email       KLZHANG@YZU.EDU.CN

_publ_section_title              
;
Effect of N-donor auxiliary ligands on the
engineering of crystalline architectures of a series of lead(II)
complexes with 5-amino-2,4,6-triiodoisophthalic acid
;
loop_
_publ_author_name
'Kou-Lin Zhang.'
'Yan Chang.'
'Chuan-Tao Hou.'
'Seik-Weng Ng'

# Attachment 'PB1.cif'

data_pb
_database_code_depnum_ccdc_archive 'CCDC 730069'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18H12 I3 N3 O5 Pb,3(H2O)'
_chemical_formula_sum            'C18 H18 I3 N3 O8 Pb'
_chemical_formula_weight         992.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   17.1458(9)
_cell_length_b                   9.6805(5)
_cell_length_c                   15.0694(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2501.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.416
_cell_measurement_theta_max      27.554

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    10.495
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20739
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5697
_reflns_number_gt                5441
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0531P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_number_reflns         5697
_refine_ls_number_parameters     298
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.870585(12) 0.22359(2) 0.500128(18) 0.02867(7) Uani 1 1 d . . .
I1 I 0.73781(2) 0.42419(5) 0.69608(3) 0.03444(10) Uani 1 1 d . . .
I2 I 0.85700(3) 0.60719(5) 1.05347(3) 0.04039(11) Uani 1 1 d . . .
I3 I 1.05356(3) 0.22826(5) 0.82170(4) 0.04134(12) Uani 1 1 d . . .
O1 O 0.9414(3) 0.3403(6) 0.6334(3) 0.0390(11) Uani 1 1 d . . .
O2 O 0.8748(3) 0.1566(5) 0.6799(4) 0.0396(11) Uani 1 1 d . . .
O3 O 0.7301(3) 0.6818(5) 0.8616(4) 0.0408(11) Uani 1 1 d . . .
O4 O 0.6867(3) 0.5030(5) 0.9381(4) 0.0392(11) Uani 1 1 d . . .
O1W O 0.8144(4) 0.4858(7) 0.4518(4) 0.0595(16) Uani 1 1 d D . .
H1W1 H 0.7939 0.5037 0.4016 0.089 Uiso 1 1 d RD . .
H1W2 H 0.8068 0.5534 0.4869 0.089 Uiso 1 1 d RD . .
O2W O 0.7505(3) 0.5594(6) 0.2753(4) 0.0523(14) Uani 1 1 d DU . .
H2W1 H 0.7389 0.6447 0.2682 0.078 Uiso 1 1 d RD . .
H2W2 H 0.7255 0.5098 0.2381 0.078 Uiso 1 1 d RD . .
O3W O 0.8169(5) 0.7431(7) 0.5322(5) 0.0685(19) Uani 1 1 d DU . .
H3W1 H 0.7856 0.7558 0.5753 0.103 Uiso 1 1 d RD . .
H3W2 H 0.8123 0.8089 0.4951 0.103 Uiso 1 1 d RD . .
O4W O 0.7697(5) 0.2991(7) 0.1853(5) 0.0689(18) Uani 1 1 d DU . .
H4W2 H 0.8153 0.2803 0.1667 0.103 Uiso 1 1 d RD . .
H4W1 H 0.7615 0.2558 0.2339 0.103 Uiso 1 1 d RD . .
N1 N 1.0020(3) 0.4222(7) 0.9875(4) 0.0426(14) Uani 1 1 d D . .
H1N1 H 0.9955 0.4675 1.0360 0.051 Uiso 1 1 calc RD . .
H1N2 H 1.0450 0.3789 0.9780 0.051 Uiso 1 1 calc RD . .
N2 N 0.9891(3) 0.0739(5) 0.5046(4) 0.0340(11) Uani 1 1 d . . .
N3 N 0.9611(4) 0.2555(6) 0.3743(4) 0.0352(13) Uani 1 1 d . . .
C1 C 0.9061(4) 0.2728(6) 0.6912(4) 0.0285(12) Uani 1 1 d . . .
C2 C 0.8939(4) 0.3440(7) 0.7808(4) 0.0275(12) Uani 1 1 d . . .
C3 C 0.8243(3) 0.4157(6) 0.7952(4) 0.0239(11) Uani 1 1 d . . .
C4 C 0.8134(3) 0.4877(6) 0.8744(4) 0.0241(11) Uani 1 1 d . . .
C5 C 0.8720(3) 0.4883(7) 0.9377(4) 0.0263(12) Uani 1 1 d . . .
C6 C 0.9436(4) 0.4188(7) 0.9249(4) 0.0284(13) Uani 1 1 d . . .
C7 C 0.9517(3) 0.3426(7) 0.8448(4) 0.0301(13) Uani 1 1 d . . .
C8 C 0.7372(3) 0.5644(7) 0.8916(4) 0.0270(12) Uani 1 1 d . . .
C9 C 1.0020(5) -0.0153(8) 0.5733(5) 0.0450(17) Uani 1 1 d . . .
H9 H 0.9659 -0.0185 0.6193 0.054 Uiso 1 1 calc R . .
C10 C 1.0657(5) -0.1001(9) 0.5772(7) 0.055(2) Uani 1 1 d . . .
H10 H 1.0724 -0.1599 0.6248 0.066 Uiso 1 1 calc R . .
C11 C 1.1188(4) -0.0960(8) 0.5110(7) 0.051(2) Uani 1 1 d . . .
H11 H 1.1623 -0.1533 0.5124 0.061 Uiso 1 1 calc R . .
C12 C 1.1077(4) -0.0052(10) 0.4411(6) 0.0487(19) Uani 1 1 d . . .
H12 H 1.1438 -0.0004 0.3951 0.058 Uiso 1 1 calc R . .
C13 C 1.0421(4) 0.0786(7) 0.4404(5) 0.0343(14) Uani 1 1 d . . .
C14 C 1.0274(4) 0.1793(8) 0.3666(5) 0.0356(14) Uani 1 1 d . . .
C15 C 1.0779(5) 0.1999(9) 0.2963(6) 0.051(2) Uani 1 1 d . . .
H15 H 1.1237 0.1488 0.2924 0.062 Uiso 1 1 calc R . .
C16 C 1.0606(5) 0.2947(10) 0.2330(6) 0.052(2) Uani 1 1 d . . .
H16 H 1.0936 0.3066 0.1847 0.063 Uiso 1 1 calc R . .
C17 C 0.9939(6) 0.3732(9) 0.2407(5) 0.0503(19) Uani 1 1 d . . .
H17 H 0.9822 0.4412 0.1992 0.060 Uiso 1 1 calc R . .
C18 C 0.9455(5) 0.3486(9) 0.3109(6) 0.0464(18) Uani 1 1 d . . .
H18 H 0.8994 0.3988 0.3148 0.056 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N3 2.470(6) . ?
Pb1 N2 2.498(5) . ?
Pb1 O4 2.530(5) 4_644 ?
Pb1 O1 2.604(5) . ?
Pb1 O3 2.739(5) 4_644 ?
Pb1 O1W 2.811(7) . ?
I1 C3 2.106(6) . ?
I2 C5 2.106(6) . ?
I3 C7 2.097(6) . ?
O1 C1 1.246(8) . ?
O2 C1 1.257(8) . ?
O3 C8 1.230(8) . ?
O3 Pb1 2.739(5) 4_655 ?
O4 C8 1.262(8) . ?
O4 Pb1 2.530(5) 4_655 ?
N1 C6 1.376(8) . ?
N2 C13 1.327(9) . ?
N2 C9 1.366(10) . ?
N3 C18 1.341(10) . ?
N3 C14 1.359(10) . ?
C1 C2 1.531(8) . ?
C2 C7 1.383(8) . ?
C2 C3 1.398(8) . ?
C3 C4 1.396(8) . ?
C4 C5 1.385(8) . ?
C4 C8 1.524(8) . ?
C5 C6 1.412(8) . ?
C6 C7 1.422(9) . ?
C9 C10 1.368(11) . ?
C10 C11 1.351(14) . ?
C11 C12 1.385(13) . ?
C12 C13 1.387(10) . ?
C13 C14 1.501(11) . ?
C14 C15 1.383(10) . ?
C15 C16 1.356(13) . ?
C16 C17 1.378(13) . ?
C17 C18 1.365(12) . ?

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 N2 65.3(2) . . ?
N3 Pb1 O4 93.77(19) . 4_644 ?
N2 Pb1 O4 80.56(16) . 4_644 ?
N3 Pb1 O1 104.14(18) . . ?
N2 Pb1 O1 81.46(18) . . ?
O4 Pb1 O1 146.34(17) 4_644 . ?
N3 Pb1 O3 80.2(2) . 4_644 ?
N2 Pb1 O3 116.59(18) . 4_644 ?
O4 Pb1 O3 49.36(15) 4_644 4_644 ?
O1 Pb1 O3 161.02(17) . 4_644 ?
N3 Pb1 O1W 84.5(2) . . ?
N2 Pb1 O1W 144.09(19) . . ?
O4 Pb1 O1W 122.23(19) 4_644 . ?
O1 Pb1 O1W 88.16(18) . . ?
O3 Pb1 O1W 73.74(18) 4_644 . ?
C1 O1 Pb1 94.9(4) . . ?
C8 O3 Pb1 85.3(4) . 4_655 ?
C8 O4 Pb1 94.3(4) . 4_655 ?
C13 N2 C9 117.6(6) . . ?
C13 N2 Pb1 121.2(5) . . ?
C9 N2 Pb1 121.2(5) . . ?
C18 N3 C14 118.1(6) . . ?
C18 N3 Pb1 120.4(5) . . ?
C14 N3 Pb1 121.5(5) . . ?
O1 C1 O2 125.6(6) . . ?
O1 C1 C2 116.5(5) . . ?
O2 C1 C2 117.7(6) . . ?
C7 C2 C3 120.5(5) . . ?
C7 C2 C1 120.9(5) . . ?
C3 C2 C1 118.5(5) . . ?
C4 C3 C2 119.7(5) . . ?
C4 C3 I1 119.5(4) . . ?
C2 C3 I1 120.7(4) . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 C8 120.2(5) . . ?
C3 C4 C8 120.2(5) . . ?
C4 C5 C6 122.3(6) . . ?
C4 C5 I2 118.9(4) . . ?
C6 C5 I2 118.6(4) . . ?
N1 C6 C5 121.9(6) . . ?
N1 C6 C7 121.5(6) . . ?
C5 C6 C7 116.6(5) . . ?
C2 C7 C6 121.2(6) . . ?
C2 C7 I3 119.0(4) . . ?
C6 C7 I3 119.8(4) . . ?
O3 C8 O4 124.8(5) . . ?
O3 C8 C4 118.2(5) . . ?
O4 C8 C4 117.0(6) . . ?
N2 C9 C10 122.7(8) . . ?
C11 C10 C9 119.3(9) . . ?
C10 C11 C12 119.2(7) . . ?
C11 C12 C13 119.2(8) . . ?
N2 C13 C12 122.0(7) . . ?
N2 C13 C14 116.6(6) . . ?
C12 C13 C14 121.4(7) . . ?
N3 C14 C15 120.7(7) . . ?
N3 C14 C13 115.4(6) . . ?
C15 C14 C13 123.8(7) . . ?
C16 C15 C14 119.9(8) . . ?
C15 C16 C17 119.7(8) . . ?
C18 C17 C16 118.2(8) . . ?
N3 C18 C17 123.3(7) . . ?

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
O4W H4W1 O3 0.85 2.06 2.888(9) 163.6 4_644
O3W H3W2 O4 0.85 2.07 2.890(9) 162.3 4_654
O3W H3W1 O4W 0.85 1.96 2.797(11) 169.5 4_655
O2W H2W2 O4W 0.85 2.32 2.880(10) 123.8 .
O2W H2W1 O2 0.86 2.36 2.751(8) 108.0 4_654
O1W H1W2 O3W 0.85 1.97 2.770(10) 156.9 .
O1W H1W1 O2W 0.85 2.11 2.963(9) 175.4 .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.499
_refine_diff_density_min         -2.067
_refine_diff_density_rms         0.171

# Attachment 'PB3.cif'

data_pb3
_database_code_depnum_ccdc_archive 'CCDC 730206'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_absolute_configuration RM
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H2 I3 N O4 Pb'
_chemical_formula_sum            'C8 H2 I3 N O4 Pb'
_chemical_formula_weight         764.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P31

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

_cell_length_a                   9.3959(9)
_cell_length_b                   9.3959(9)
_cell_length_c                   12.2406(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     935.86(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3356
_cell_measurement_theta_min      2.503
_cell_measurement_theta_max      27.114

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             990
_exptl_absorpt_coefficient_mu    20.943
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3663
_exptl_absorpt_correction_T_max  0.3921
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7965
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         27.57
_reflns_number_total             2760
_reflns_number_gt                2533
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0246P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_number_reflns         2760
_refine_ls_number_parameters     148
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0541
_refine_ls_wR_factor_gt          0.0527
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.03714(4) 0.13912(4) 0.50002(3) 0.024 Uani 1 1 d . . .
I1 I 0.25808(7) 0.42151(8) 0.71659(6) 0.02836(14) Uani 1 1 d . . .
I2 I 0.41006(8) -0.13169(8) 0.71701(6) 0.03405(16) Uani 1 1 d . . .
I3 I 0.96071(7) 0.57229(8) 0.68325(6) 0.03120(16) Uani 1 1 d . . .
O1 O 0.0877(9) 0.0193(9) 0.6647(6) 0.0318(16) Uani 1 1 d . . .
O2 O 0.1549(8) 0.0049(8) 0.8339(5) 0.0295(16) Uani 1 1 d . . .
O3 O 0.8279(10) 0.1537(11) 0.6074(7) 0.054(2) Uani 1 1 d . . .
O4 O 0.8247(10) 0.1451(10) 0.7886(7) 0.046(2) Uani 1 1 d . . .
C1 C 0.1959(10) 0.0561(10) 0.7367(7) 0.0186(18) Uani 1 1 d . . .
C2 C 0.3753(10) 0.1738(10) 0.7165(6) 0.0161(17) Uani 1 1 d . . .
C3 C 0.4904(10) 0.1213(9) 0.7123(7) 0.0176(17) Uani 1 1 d . . .
C4 C 0.6586(11) 0.2318(11) 0.6997(6) 0.0203(19) Uani 1 1 d . . .
C5 C 0.7090(10) 0.3994(11) 0.6906(7) 0.0187(17) Uani 1 1 d . . .
C6 C 0.5991(11) 0.4578(10) 0.6896(6) 0.0186(18) Uani 1 1 d . . .
C7 C 0.4300(11) 0.3414(10) 0.7059(7) 0.0208(18) Uani 1 1 d . . .
C8 C 0.7802(11) 0.1721(11) 0.6980(8) 0.024(2) Uani 1 1 d . . .
N1 N 0.6510(10) 0.6228(9) 0.6745(6) 0.0268(19) Uani 1 1 d . . .
H1A H 0.7537 0.6922 0.6655 0.032 Uiso 1 1 calc R . .
H1B H 0.5806 0.6558 0.6742 0.032 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.422(6) 3_554 ?
Pb1 O3 2.425(8) 1_455 ?
Pb1 O1 2.468(6) . ?
Pb1 O4 2.568(7) 3_664 ?
I1 C7 2.100(8) . ?
I2 C3 2.105(8) . ?
I3 C5 2.097(8) . ?
O1 C1 1.256(10) . ?
O2 C1 1.269(10) . ?
O2 Pb1 2.422(6) 2 ?
O3 C8 1.240(12) . ?
O3 Pb1 2.425(7) 1_655 ?
O4 C8 1.255(12) . ?
O4 Pb1 2.568(7) 2_655 ?
C1 C2 1.504(11) . ?
C2 C3 1.396(11) . ?
C2 C7 1.397(11) . ?
C3 C4 1.400(12) . ?
C4 C5 1.404(12) . ?
C4 C8 1.503(12) . ?
C5 C6 1.391(12) . ?
C6 N1 1.385(11) . ?
C6 C7 1.422(12) . ?

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
O2 Pb1 O3 85.2(3) 3_554 1_455 ?
O2 Pb1 O1 70.9(2) 3_554 . ?
O3 Pb1 O1 86.0(3) 1_455 . ?
O2 Pb1 O4 105.4(2) 3_554 3_664 ?
O3 Pb1 O4 157.5(3) 1_455 3_664 ?
O1 Pb1 O4 79.1(2) . 3_664 ?
C1 O1 Pb1 139.6(6) . . ?
C1 O2 Pb1 102.8(5) . 2 ?
C8 O3 Pb1 148.5(7) . 1_655 ?
C8 O4 Pb1 125.4(7) . 2_655 ?
O1 C1 O2 120.2(8) . . ?
O1 C1 C2 122.8(8) . . ?
O2 C1 C2 116.7(7) . . ?
C3 C2 C7 118.8(7) . . ?
C3 C2 C1 121.9(7) . . ?
C7 C2 C1 119.3(7) . . ?
C2 C3 C4 122.0(7) . . ?
C2 C3 I2 119.6(6) . . ?
C4 C3 I2 118.4(6) . . ?
C3 C4 C5 117.6(7) . . ?
C3 C4 C8 120.8(8) . . ?
C5 C4 C8 121.6(8) . . ?
C6 C5 C4 122.9(8) . . ?
C6 C5 I3 117.8(6) . . ?
C4 C5 I3 119.3(6) . . ?
N1 C6 C5 121.8(8) . . ?
N1 C6 C7 120.8(8) . . ?
C5 C6 C7 117.3(7) . . ?
C2 C7 C6 121.4(7) . . ?
C2 C7 I1 118.9(6) . . ?
C6 C7 I1 119.8(6) . . ?
O3 C8 O4 125.6(10) . . ?
O3 C8 C4 117.3(9) . . ?
O4 C8 C4 117.1(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.913
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.181


# Attachment 'PB2.CIF'

data_pb2
_database_code_depnum_ccdc_archive 'CCDC 736508'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Pb (C6 H6 N4) (C8 H2 I3 N O4), H2 O'
_chemical_formula_sum            'C14 H10 I3 N5 O5 Pb'
_chemical_formula_weight         916.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'

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

_cell_length_a                   28.218(2)
_cell_length_b                   28.218(2)
_cell_length_c                   17.741(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12233.8(14)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4461
_cell_measurement_theta_min      2.486
_cell_measurement_theta_max      22.555

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7380
_exptl_absorpt_coefficient_mu    9.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_T_max  0.462
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            25809
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6225
_reflns_number_gt                4032
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0796P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6225
_refine_ls_number_parameters     253
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1574
_refine_ls_wR_factor_gt          0.1375
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.185288(16) 0.918598(16) 0.31869(2) 0.04942(15) Uani 1 1 d . . .
I1 I 0.08100(4) 0.87108(4) 0.51556(4) 0.0729(3) Uani 1 1 d . . .
I2 I 0.10139(3) 0.76261(3) 0.79575(4) 0.0617(2) Uani 1 1 d . . .
I3 I 0.27618(4) 0.84096(5) 0.55700(5) 0.0898(3) Uani 1 1 d . . .
O1 O 0.2192(3) 0.9220(3) 0.4641(3) 0.0502(17) Uani 1 1 d . . .
O2 O 0.1756(3) 0.8373(3) 0.4215(4) 0.064(2) Uani 1 1 d . . .
O3 O 0.0106(3) 0.7613(4) 0.6517(4) 0.064(2) Uani 1 1 d . . .
O4 O 0.0414(4) 0.8407(4) 0.7115(5) 0.084(3) Uani 1 1 d . . .
O1W O 0.1156(8) 0.9363(8) 0.7998(11) 0.219(8) Uani 1 1 d U . .
H1W1 H 0.1103 0.9150 0.7652 0.328 Uiso 1 1 d R . .
H1W2 H 0.1484 0.9589 0.8019 0.328 Uiso 1 1 d R . .
N1 N 0.2134(4) 0.7923(4) 0.7117(5) 0.077(3) Uani 1 1 d . . .
H11 H 0.2007 0.7760 0.7540 0.093 Uiso 1 1 calc R . .
H12 H 0.2442 0.7974 0.6952 0.093 Uiso 1 1 calc R . .
N2 N 0.2690(4) 0.9191(4) 0.3091(4) 0.053(2) Uani 1 1 d . . .
N3 N 0.3429(4) 0.9348(4) 0.2473(5) 0.072(3) Uani 1 1 d . . .
H3 H 0.3659 0.9437 0.2109 0.086 Uiso 1 1 calc R . .
N4 N 0.2929(5) 0.9659(4) 0.1124(5) 0.080(3) Uani 1 1 d . . .
H4 H 0.3216 0.9668 0.0942 0.096 Uiso 1 1 calc R . .
N5 N 0.2292(4) 0.9545(4) 0.1930(5) 0.059(2) Uani 1 1 d . . .
C1 C 0.1915(4) 0.8714(4) 0.4745(5) 0.044(2) Uani 1 1 d . . .
C2 C 0.1737(4) 0.8500(4) 0.5536(5) 0.041(2) Uani 1 1 d . . .
C3 C 0.1252(4) 0.8433(4) 0.5820(5) 0.043(2) Uani 1 1 d . . .
C4 C 0.1043(4) 0.8194(4) 0.6505(5) 0.042(2) Uani 1 1 d . . .
C5 C 0.1348(4) 0.8031(4) 0.6946(5) 0.044(2) Uani 1 1 d . . .
C6 C 0.1843(4) 0.8103(4) 0.6704(5) 0.049(2) Uani 1 1 d . . .
C7 C 0.2029(4) 0.8332(4) 0.5981(6) 0.056(3) Uani 1 1 d . . .
C8 C 0.0480(5) 0.8061(5) 0.6735(5) 0.055(3) Uani 1 1 d . . .
C9 C 0.3012(5) 0.9072(5) 0.3539(7) 0.075(4) Uani 1 1 d . . .
H9 H 0.2924 0.8938 0.4029 0.090 Uiso 1 1 calc R . .
C10 C 0.3486(5) 0.9178(6) 0.3164(7) 0.080(4) Uani 1 1 d . . .
H10 H 0.3775 0.9140 0.3345 0.095 Uiso 1 1 calc R . .
C11 C 0.2968(5) 0.9356(4) 0.2443(5) 0.052(3) Uani 1 1 d . . .
C12 C 0.2732(5) 0.9509(4) 0.1837(6) 0.064(3) Uani 1 1 d . . .
C13 C 0.2597(7) 0.9792(5) 0.0756(7) 0.088(5) Uani 1 1 d . . .
H13 H 0.2628 0.9908 0.0259 0.105 Uiso 1 1 calc R . .
C14 C 0.2217(6) 0.9722(5) 0.1248(7) 0.077(4) Uani 1 1 d . . .
H14 H 0.1931 0.9786 0.1143 0.093 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N2 2.362(9) . ?
Pb1 O3 2.363(7) 12_666 ?
Pb1 N5 2.505(9) . ?
Pb1 O2 2.587(6) 16_565 ?
Pb1 O1 2.737(6) . ?
Pb1 O2 2.833(7) . ?
I1 C3 2.131(10) . ?
I2 C5 2.082(9) . ?
I3 C7 2.099(10) . ?
O1 C1 1.251(11) . ?
O2 C1 1.257(10) . ?
O2 Pb1 2.587(6) 16_565 ?
O3 C8 1.236(13) . ?
O3 Pb1 2.363(7) 11_456 ?
O4 C8 1.272(13) . ?
N1 C6 1.372(13) . ?
N2 C11 1.337(11) . ?
N2 C9 1.368(15) . ?
N3 C11 1.313(14) . ?
N3 C10 1.357(16) . ?
N4 C13 1.341(18) . ?
N4 C12 1.360(12) . ?
N5 C12 1.307(15) . ?
N5 C14 1.366(14) . ?
C1 C2 1.511(11) . ?
C2 C3 1.379(13) . ?
C2 C7 1.383(14) . ?
C3 C4 1.372(12) . ?
C4 C5 1.398(14) . ?
C4 C8 1.497(14) . ?
C5 C6 1.376(13) . ?
C6 C7 1.415(13) . ?
C9 C10 1.386(16) . ?
C11 C12 1.440(17) . ?
C13 C14 1.319(19) . ?

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
N2 Pb1 O3 78.3(3) . 12_666 ?
N2 Pb1 N5 69.1(3) . . ?
O3 Pb1 N5 78.6(3) 12_666 . ?
N2 Pb1 O2 77.4(3) . 16_565 ?
O3 Pb1 O2 150.9(3) 12_666 16_565 ?
N5 Pb1 O2 78.0(2) . 16_565 ?
N2 Pb1 O1 74.7(2) . . ?
O3 Pb1 O1 72.0(2) 12_666 . ?
N5 Pb1 O1 137.0(3) . . ?
O2 Pb1 O1 116.0(2) 16_565 . ?
N2 Pb1 O2 75.1(3) . . ?
O3 Pb1 O2 117.2(2) 12_666 . ?
N5 Pb1 O2 136.7(3) . . ?
O2 Pb1 O2 71.1(2) 16_565 . ?
O1 Pb1 O2 46.55(18) . . ?
C1 O1 Pb1 95.2(5) . . ?
C1 O2 Pb1 160.1(7) . 16_565 ?
C1 O2 Pb1 90.6(6) . . ?
Pb1 O2 Pb1 108.9(2) 16_565 . ?
C8 O3 Pb1 120.4(7) . 11_456 ?
C11 N2 C9 103.9(9) . . ?
C11 N2 Pb1 118.3(7) . . ?
C9 N2 Pb1 137.8(7) . . ?
C11 N3 C10 109.6(9) . . ?
C13 N4 C12 107.8(12) . . ?
C12 N5 C14 104.1(10) . . ?
C12 N5 Pb1 112.3(7) . . ?
C14 N5 Pb1 143.2(9) . . ?
O1 C1 O2 122.9(8) . . ?
O1 C1 C2 119.1(7) . . ?
O2 C1 C2 118.0(8) . . ?
C3 C2 C7 117.6(8) . . ?
C3 C2 C1 120.1(9) . . ?
C7 C2 C1 122.1(9) . . ?
C4 C3 C2 122.9(9) . . ?
C4 C3 I1 119.0(7) . . ?
C2 C3 I1 118.1(6) . . ?
C3 C4 C5 118.3(9) . . ?
C3 C4 C8 120.4(9) . . ?
C5 C4 C8 121.1(8) . . ?
C6 C5 C4 121.5(8) . . ?
C6 C5 I2 119.8(7) . . ?
C4 C5 I2 118.6(7) . . ?
N1 C6 C5 122.0(9) . . ?
N1 C6 C7 119.9(9) . . ?
C5 C6 C7 117.9(9) . . ?
C2 C7 C6 121.7(9) . . ?
C2 C7 I3 119.4(7) . . ?
C6 C7 I3 118.9(8) . . ?
O3 C8 O4 124.9(11) . . ?
O3 C8 C4 115.3(10) . . ?
O4 C8 C4 119.8(11) . . ?
N2 C9 C10 110.8(11) . . ?
N3 C10 C9 103.7(11) . . ?
N3 C11 N2 111.9(9) . . ?
N3 C11 C12 130.1(9) . . ?
N2 C11 C12 118.0(10) . . ?
N5 C12 N4 110.5(12) . . ?
N5 C12 C11 121.8(9) . . ?
N4 C12 C11 127.6(13) . . ?
C14 C13 N4 105.5(12) . . ?
C13 C14 N5 112.1(14) . . ?

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 H3 O1 0.86 1.80 2.66(1) 176 8_664
N4 H4 O3 0.86 2.25 2.84(1) 126 16_565
O1w H1w1 O4 0.82 2.24 2.91(2) 140 .
O1w H1w2 I3 0.82 3.02 3.71(2) 142 6_465

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.235

# Attachment 'H2ATIBDC.H2O.cif'

data_cy33_0m
_database_code_depnum_ccdc_archive 'CCDC 740896'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H6 I3 N O5'
_chemical_formula_weight         576.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   9.3044(9)
_cell_length_b                   15.8623(15)
_cell_length_c                   18.9924(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2803.1(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    6.698
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.131
_exptl_absorpt_correction_T_max  0.245
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22616
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         27.63
_reflns_number_total             3246
_reflns_number_gt                2938
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0202P)²+14.1592P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3246
_refine_ls_number_parameters     156
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.004

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
I1 I 0.21818(4) 0.82462(2) 0.76697(2) 0.04697(12) Uani 1 1 d . . .
I2 I 0.54054(4) 0.52077(2) 0.87620(2) 0.05084(12) Uani 1 1 d . . .
I3 I 0.68537(4) 0.86811(2) 0.98562(2) 0.04569(11) Uani 1 1 d . . .
C8 C 0.4961(5) 0.6505(3) 0.8803(2) 0.0259(9) Uani 1 1 d . . .
C5 C 0.4560(5) 0.8243(3) 0.8767(2) 0.0242(8) Uani 1 1 d . . .
C3 C 0.5829(4) 0.7028(3) 0.9214(2) 0.0246(8) Uani 1 1 d . . .
C7 C 0.3821(4) 0.6830(3) 0.8400(2) 0.0249(8) Uani 1 1 d . . .
C4 C 0.5620(4) 0.7895(3) 0.9204(2) 0.0238(8) Uani 1 1 d . . .
C6 C 0.3677(4) 0.7713(3) 0.8369(2) 0.0247(8) Uani 1 1 d . . .
O1 O 0.6491(4) 0.6365(3) 1.0263(2) 0.0429(9) Uani 1 1 d . . .
H1 H 0.7093 0.6063 1.0453 0.064 Uiso 1 1 calc R . .
O3 O 0.3402(4) 0.9557(2) 0.90018(19) 0.0365(8) Uani 1 1 d . . .
O2 O 0.8231(4) 0.6590(3) 0.9478(2) 0.0521(11) Uani 1 1 d . . .
O4 O 0.5369(4) 0.9538(2) 0.8328(2) 0.0401(9) Uani 1 1 d . . .
H4 H 0.5205 1.0044 0.8295 0.060 Uiso 1 1 calc R . .
N1 N 0.2919(4) 0.6301(3) 0.8012(2) 0.0365(9) Uani 1 1 d . . .
H1A H 0.3057 0.5764 0.8017 0.044 Uiso 1 1 calc R . .
H1B H 0.2227 0.6511 0.7769 0.044 Uiso 1 1 calc R . .
C1 C 0.6990(5) 0.6635(3) 0.9665(3) 0.0310(10) Uani 1 1 d . . .
C2 C 0.4382(5) 0.9184(3) 0.8717(2) 0.0265(9) Uani 1 1 d . . .
O1W O 0.5363(4) 0.1151(2) 0.8245(2) 0.0425(9) Uani 1 1 d D . .
H1WA H 0.5977 0.1194 0.7912 0.051 Uiso 1 1 d RD . .
H1WB H 0.5755 0.1315 0.8627 0.051 Uiso 1 1 d RD . .


_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
I1 C6 2.101(4) . ?
I2 C8 2.100(4) . ?
I3 C4 2.100(4) . ?
C8 C3 1.397(6) . ?
C8 C7 1.406(6) . ?
C5 C6 1.398(6) . ?
C5 C4 1.402(6) . ?
C5 C2 1.504(6) . ?
C3 C4 1.389(6) . ?
C3 C1 1.513(6) . ?
C7 N1 1.397(6) . ?
C7 C6 1.408(6) . ?
O1 C1 1.300(6) . ?
O1 H1 0.8200 . ?
O3 C2 1.214(5) . ?
O2 C1 1.210(6) . ?
O4 C2 1.305(5) . ?
O4 H4 0.8200 . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
O1W H1WA 0.8545 . ?
O1W H1WB 0.8534 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C8 C7 121.5(4) . . ?
C3 C8 I2 119.3(3) . . ?
C7 C8 I2 119.2(3) . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 C2 119.8(4) . . ?
C4 C5 C2 120.5(4) . . ?
C4 C3 C8 120.0(4) . . ?
C4 C3 C1 121.1(4) . . ?
C8 C3 C1 119.0(4) . . ?
N1 C7 C8 121.3(4) . . ?
N1 C7 C6 121.2(4) . . ?
C8 C7 C6 117.4(4) . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 I3 120.2(3) . . ?
C5 C4 I3 119.9(3) . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 I1 119.3(3) . . ?
C7 C6 I1 119.3(3) . . ?
C1 O1 H1 109.5 . . ?
C2 O4 H4 109.5 . . ?
C7 N1 H1A 120.0 . . ?
C7 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
O2 C1 O1 125.3(5) . . ?
O2 C1 C3 122.7(5) . . ?
O1 C1 C3 112.1(4) . . ?
O3 C2 O4 124.8(4) . . ?
O3 C2 C5 122.5(4) . . ?
O4 C2 C5 112.7(4) . . ?
H1WA O1W H1WB 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.147

