# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_morsa1408_0ma
_database_code_depnum_ccdc_archive 'CCDC 1063325'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[Pb(INO)Cl]n'
_chemical_name_common            ?
_chemical_melting_point          'dp> 300'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H4 Cl N O3 Pb'
_chemical_formula_weight         380.74

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'
Pb Pb -3.3944 10.1111 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbcn '
_symmetry_space_group_name_Hall  '-P 2n 2ab '


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

_cell_length_a                   13.0104(5)
_cell_length_b                   7.1278(3)
_cell_length_c                   17.3503(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1608.99(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9872
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      33.82

_exptl_crystal_description       ?
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    21.264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3459
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57348
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1749
_reflns_number_gt                1604
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0408P)²+7.6277P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0046(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1749
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_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 0.658063(15) 0.20892(3) 0.727395(10) 0.01863(13) Uani 1 1 d . . .
Cl1 Cl 0.84518(12) 0.3550(3) 0.80240(10) 0.0372(4) Uani 1 1 d . . .
O2 O 0.5855(4) 0.1608(7) 0.5897(3) 0.0349(10) Uani 1 1 d . . .
O3 O 0.7855(3) 0.0104(6) 0.6559(2) 0.0270(9) Uani 1 1 d . . .
N1 N 0.8340(3) 0.0814(7) 0.5953(3) 0.0212(10) Uani 1 1 d . . .
O1 O 0.4725(4) 0.2999(7) 0.6651(2) 0.0314(10) Uani 1 1 d . . .
C2 C 0.8487(4) 0.1035(9) 0.4602(3) 0.0235(12) Uani 1 1 d . . .
H2 H 0.8234 0.0761 0.4113 0.028 Uiso 1 1 calc R . .
C4 C 0.9733(5) 0.2466(8) 0.5421(3) 0.0217(11) Uani 1 1 d . . .
H4 H 1.0324 0.3183 0.5489 0.026 Uiso 1 1 calc R . .
C6 C 0.5031(5) 0.2453(8) 0.6002(3) 0.0235(12) Uani 1 1 d . . .
C1 C 0.7962(5) 0.0443(9) 0.5250(3) 0.0259(12) Uani 1 1 d . . .
H1 H 0.7348 -0.0213 0.5199 0.031 Uiso 1 1 calc R . .
C5 C 0.9197(5) 0.1827(8) 0.6055(3) 0.0232(12) Uani 1 1 d . . .
H5 H 0.9428 0.2097 0.6549 0.028 Uiso 1 1 calc R . .
C3 C 0.9394(5) 0.2043(7) 0.4685(3) 0.0196(11) 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 0.02000(17) 0.02695(19) 0.00893(16) 0.00283(7) 0.00005(6) 0.00125(7)
Cl1 0.0391(9) 0.0429(10) 0.0295(9) 0.0092(8) -0.0123(6) 0.0027(7)
O2 0.038(2) 0.039(2) 0.028(2) -0.004(2) -0.0129(19) 0.012(2)
O3 0.033(2) 0.034(2) 0.0141(18) 0.0111(16) 0.0126(16) 0.0062(19)
N1 0.027(2) 0.021(2) 0.016(2) 0.0056(19) 0.0078(18) 0.0059(18)
O1 0.034(2) 0.049(3) 0.0114(19) 0.0052(18) -0.0027(17) -0.001(2)
C2 0.030(3) 0.032(3) 0.009(2) 0.002(2) -0.002(2) 0.001(2)
C4 0.029(3) 0.022(3) 0.014(3) -0.002(2) -0.001(2) -0.001(2)
C6 0.029(3) 0.022(2) 0.019(3) 0.005(2) -0.005(3) -0.008(2)
C1 0.025(3) 0.032(3) 0.020(3) 0.003(2) 0.000(2) -0.003(3)
C5 0.029(3) 0.029(3) 0.011(3) -0.002(2) 0.001(2) 0.004(2)
C3 0.024(3) 0.021(3) 0.013(3) 0.002(2) 0.003(2) 0.004(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O3 2.508(4) . ?
Pb1 O3 2.587(4) 6_765 ?
Pb1 O2 2.592(4) . ?
Pb1 O1 2.604(4) 3_656 ?
Pb1 O1 2.724(5) . ?
Pb1 Cl1 2.8388(19) 6_755 ?
Pb1 Cl1 2.9503(17) . ?
Cl1 Pb1 2.8388(18) 6_765 ?
O2 C6 1.243(8) . ?
O3 N1 1.327(6) . ?
O3 Pb1 2.587(4) 6_755 ?
N1 C5 1.339(8) . ?
N1 C1 1.341(7) . ?
O1 C6 1.257(8) . ?
O1 Pb1 2.604(4) 3_656 ?
C2 C1 1.381(8) . ?
C2 C3 1.389(8) . ?
C2 H2 0.9300 . ?
C4 C5 1.380(8) . ?
C4 C3 1.386(8) . ?
C4 H4 0.9300 . ?
C6 C3 1.496(8) 2_456 ?
C1 H1 0.9300 . ?
C5 H5 0.9300 . ?
C3 C6 1.496(8) 2_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Pb1 O3 92.53(9) . 6_765 ?
O3 Pb1 O2 73.17(14) . . ?
O3 Pb1 O2 76.79(14) 6_765 . ?
O3 Pb1 O1 157.77(13) . 3_656 ?
O3 Pb1 O1 108.75(14) 6_765 3_656 ?
O2 Pb1 O1 117.10(14) . 3_656 ?
O3 Pb1 O1 121.62(13) . . ?
O3 Pb1 O1 82.16(13) 6_765 . ?
O2 Pb1 O1 48.91(14) . . ?
O1 Pb1 O1 69.32(15) 3_656 . ?
O3 Pb1 Cl1 74.63(10) . 6_755 ?
O3 Pb1 Cl1 164.14(10) 6_765 6_755 ?
O2 Pb1 Cl1 107.43(12) . 6_755 ?
O1 Pb1 Cl1 83.30(11) 3_656 6_755 ?
O1 Pb1 Cl1 112.35(10) . 6_755 ?
O3 Pb1 Cl1 82.63(11) . . ?
O3 Pb1 Cl1 71.59(9) 6_765 . ?
O2 Pb1 Cl1 138.94(12) . . ?
O1 Pb1 Cl1 97.71(10) 3_656 . ?
O1 Pb1 Cl1 145.33(11) . . ?
Cl1 Pb1 Cl1 97.11(5) 6_755 . ?
Pb1 Cl1 Pb1 95.69(5) 6_765 . ?
C6 O2 Pb1 96.6(4) . . ?
N1 O3 Pb1 119.4(3) . . ?
N1 O3 Pb1 124.2(3) . 6_755 ?
Pb1 O3 Pb1 114.79(13) . 6_755 ?
O3 N1 C5 119.8(5) . . ?
O3 N1 C1 118.1(5) . . ?
C5 N1 C1 122.1(5) . . ?
C6 O1 Pb1 140.5(4) . 3_656 ?
C6 O1 Pb1 90.0(4) . . ?
Pb1 O1 Pb1 103.57(14) 3_656 . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
O2 C6 O1 123.8(5) . . ?
O2 C6 C3 118.6(5) . 2_456 ?
O1 C6 C3 117.6(5) . 2_456 ?
N1 C1 C2 119.9(5) . . ?
N1 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
N1 C5 C4 119.6(5) . . ?
N1 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C2 C3 C4 118.6(5) . . ?
C2 C3 C6 120.9(5) . 2_556 ?
C4 C3 C6 120.3(5) . 2_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Pb1 Cl1 Pb1 107.54(10) . . . 6_765 ?
O3 Pb1 Cl1 Pb1 12.38(11) 6_765 . . 6_765 ?
O2 Pb1 Cl1 Pb1 53.90(17) . . . 6_765 ?
O1 Pb1 Cl1 Pb1 -94.89(11) 3_656 . . 6_765 ?
O1 Pb1 Cl1 Pb1 -30.40(18) . . . 6_765 ?
Cl1 Pb1 Cl1 Pb1 -179.05(4) 6_755 . . 6_765 ?
O3 Pb1 O2 C6 176.9(4) . . . . ?
O3 Pb1 O2 C6 -86.3(4) 6_765 . . . ?
O1 Pb1 O2 C6 18.2(4) 3_656 . . . ?
O1 Pb1 O2 C6 4.7(3) . . . . ?
Cl1 Pb1 O2 C6 109.5(4) 6_755 . . . ?
Cl1 Pb1 O2 C6 -126.6(3) . . . . ?
O3 Pb1 O3 N1 -11.3(4) 6_765 . . . ?
O2 Pb1 O3 N1 64.1(4) . . . . ?
O1 Pb1 O3 N1 -174.7(4) 3_656 . . . ?
O1 Pb1 O3 N1 71.0(4) . . . . ?
Cl1 Pb1 O3 N1 178.1(4) 6_755 . . . ?
Cl1 Pb1 O3 N1 -82.4(4) . . . . ?
O3 Pb1 O3 Pb1 154.78(18) 6_765 . . 6_755 ?
O2 Pb1 O3 Pb1 -129.8(2) . . . 6_755 ?
O1 Pb1 O3 Pb1 -8.6(5) 3_656 . . 6_755 ?
O1 Pb1 O3 Pb1 -122.87(17) . . . 6_755 ?
Cl1 Pb1 O3 Pb1 -15.78(14) 6_755 . . 6_755 ?
Cl1 Pb1 O3 Pb1 83.71(16) . . . 6_755 ?
Pb1 O3 N1 C5 85.2(5) . . . . ?
Pb1 O3 N1 C5 -79.5(6) 6_755 . . . ?
Pb1 O3 N1 C1 -96.5(5) . . . . ?
Pb1 O3 N1 C1 98.8(5) 6_755 . . . ?
O3 Pb1 O1 C6 -13.5(4) . . . . ?
O3 Pb1 O1 C6 74.6(3) 6_765 . . . ?
O2 Pb1 O1 C6 -4.7(3) . . . . ?
O1 Pb1 O1 C6 -171.9(3) 3_656 . . . ?
Cl1 Pb1 O1 C6 -98.7(3) 6_755 . . . ?
Cl1 Pb1 O1 C6 115.2(3) . . . . ?
O3 Pb1 O1 Pb1 129.06(15) . . . 3_656 ?
O3 Pb1 O1 Pb1 -142.80(17) 6_765 . . 3_656 ?
O2 Pb1 O1 Pb1 137.9(3) . . . 3_656 ?
O1 Pb1 O1 Pb1 -29.3(2) 3_656 . . 3_656 ?
Cl1 Pb1 O1 Pb1 43.84(17) 6_755 . . 3_656 ?
Cl1 Pb1 O1 Pb1 -102.22(17) . . . 3_656 ?
Pb1 O2 C6 O1 -9.3(7) . . . . ?
Pb1 O2 C6 C3 166.9(4) . . . 2_456 ?
Pb1 O1 C6 O2 -102.8(7) 3_656 . . . ?
Pb1 O1 C6 O2 8.8(6) . . . . ?
Pb1 O1 C6 C3 80.9(7) 3_656 . . 2_456 ?
Pb1 O1 C6 C3 -167.4(4) . . . 2_456 ?
O3 N1 C1 C2 -175.1(5) . . . . ?
C5 N1 C1 C2 3.1(9) . . . . ?
C3 C2 C1 N1 -1.2(9) . . . . ?
O3 N1 C5 C4 176.1(5) . . . . ?
C1 N1 C5 C4 -2.2(9) . . . . ?
C3 C4 C5 N1 -0.7(8) . . . . ?
C1 C2 C3 C4 -1.6(9) . . . . ?
C1 C2 C3 C6 174.1(6) . . . 2_556 ?
C5 C4 C3 C2 2.6(8) . . . . ?
C5 C4 C3 C6 -173.2(5) . . . 2_556 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.205
_refine_diff_density_min         -2.407
_refine_diff_density_rms         0.217
_exptl_crystal_recrystallization_method 'Brunch tube '
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_morsa1407_0ma
_database_code_depnum_ccdc_archive 'CCDC 1063326'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[Pb(INO)I]n'
_chemical_name_common            ?
_chemical_melting_point          dp>280
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H4 I N O3 Pb'
_chemical_formula_weight         472.19

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   'Pbcn '
_symmetry_space_group_name_Hall  '-P 2n 2ab '

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

_cell_length_a                   13.7536(4)
_cell_length_b                   6.8778(2)
_cell_length_c                   17.8671(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1690.13(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9985
_cell_measurement_theta_min      2.72

_exptl_crystal_description       ?
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    23.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4621
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32465
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1847
_reflns_number_gt                1686
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0246P)²+4.2861P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1847
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0503
_refine_ls_wR_factor_gt          0.0490
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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 1.151187(11) 0.25675(2) 0.719341(9) 0.02108(8) Uani 1 1 d . . .
I1 I 1.13991(2) -0.14700(5) 0.803936(17) 0.02992(10) Uani 1 1 d . . .
O1 O 0.7692(2) 0.4573(5) 0.35531(16) 0.0259(7) Uani 1 1 d . . .
O2 O 1.0759(2) 0.1962(6) 0.59246(19) 0.0338(8) Uani 1 1 d . . .
O3 O 0.9698(2) 0.3389(5) 0.66688(17) 0.0303(7) Uani 1 1 d . . .
N1 N 0.8184(3) 0.3967(5) 0.41552(18) 0.0182(7) Uani 1 1 d . . .
C1 C 0.9956(3) 0.2756(6) 0.6047(2) 0.0200(9) Uani 1 1 d . . .
C2 C 0.9293(3) 0.3065(6) 0.5384(2) 0.0187(8) Uani 1 1 d . . .
C3 C 0.8414(3) 0.4006(7) 0.5463(2) 0.0239(9) Uani 1 1 d . . .
H3 H 0.8198 0.4363 0.5937 0.029 Uiso 1 1 calc R . .
C4 C 0.7853(3) 0.4419(7) 0.4842(2) 0.0237(9) Uani 1 1 d . . .
H4 H 0.7249 0.5007 0.4898 0.028 Uiso 1 1 calc R . .
C5 C 0.9027(3) 0.2975(7) 0.4058(2) 0.0216(9) Uani 1 1 d . . .
H5 H 0.9227 0.2609 0.3581 0.026 Uiso 1 1 calc R . .
C6 C 0.9580(3) 0.2519(6) 0.4672(2) 0.0211(9) Uani 1 1 d . . .
H6 H 1.0157 0.1833 0.4609 0.025 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
Pb1 0.01741(11) 0.03043(13) 0.01540(11) 0.00389(6) -0.00104(5) -0.00034(6)
I1 0.02574(16) 0.0397(2) 0.02427(16) 0.00581(13) 0.00580(11) -0.00219(13)
O1 0.0271(15) 0.0311(17) 0.0195(14) 0.0082(13) -0.0086(12) -0.0022(14)
O2 0.0278(17) 0.049(2) 0.0247(17) -0.0069(16) -0.0098(14) 0.0096(16)
O3 0.0332(18) 0.041(2) 0.0171(15) 0.0003(14) -0.0033(13) -0.0002(16)
N1 0.0208(16) 0.0178(19) 0.0159(16) 0.0033(13) -0.0045(13) -0.0020(14)
C1 0.022(2) 0.021(2) 0.018(2) 0.0032(16) -0.0052(17) -0.0029(17)
C2 0.021(2) 0.020(2) 0.0153(19) 0.0002(16) -0.0022(15) -0.0017(17)
C3 0.024(2) 0.032(3) 0.0159(19) -0.0022(18) 0.0017(16) 0.0015(19)
C4 0.021(2) 0.030(2) 0.020(2) 0.0038(18) 0.0008(17) 0.0010(18)
C5 0.024(2) 0.023(2) 0.017(2) -0.0002(17) -0.0010(17) 0.0010(18)
C6 0.020(2) 0.024(2) 0.019(2) -0.0028(16) -0.0001(17) 0.0025(17)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.527(3) . ?
Pb1 O1 2.565(3) 2_556 ?
Pb1 O1 2.617(3) 5_766 ?
Pb1 O3 2.687(3) 3_756 ?
Pb1 O3 2.724(3) . ?
Pb1 I1 3.1654(4) . ?
Pb1 I1 3.3132(3) 6_865 ?
I1 Pb1 3.3132(3) 6_855 ?
O1 N1 1.338(4) . ?
O1 Pb1 2.565(3) 2_456 ?
O1 Pb1 2.617(3) 5_766 ?
O2 C1 1.251(6) . ?
O3 C1 1.245(5) . ?
O3 Pb1 2.687(3) 3_756 ?
N1 C4 1.345(5) . ?
N1 C5 1.356(6) . ?
C1 C2 1.511(6) . ?
C2 C3 1.378(6) . ?
C2 C6 1.384(6) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.372(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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 O1 72.43(11) . 2_556 ?
O2 Pb1 O1 80.68(11) . 5_766 ?
O1 Pb1 O1 84.35(6) 2_556 5_766 ?
O2 Pb1 O3 117.35(10) . 3_756 ?
O1 Pb1 O3 154.93(10) 2_556 3_756 ?
O1 Pb1 O3 119.14(11) 5_766 3_756 ?
O2 Pb1 O3 49.47(10) . . ?
O1 Pb1 O3 121.29(10) 2_556 . ?
O1 Pb1 O3 92.99(10) 5_766 . ?
O3 Pb1 O3 69.48(11) 3_756 . ?
O2 Pb1 I1 105.30(9) . . ?
O1 Pb1 I1 77.04(7) 2_556 . ?
O1 Pb1 I1 157.40(7) 5_766 . ?
O3 Pb1 I1 78.05(8) 3_756 . ?
O3 Pb1 I1 107.54(7) . . ?
O2 Pb1 I1 142.90(8) . 6_865 ?
O1 Pb1 I1 78.66(7) 2_556 6_865 ?
O1 Pb1 I1 73.70(6) 5_766 6_865 ?
O3 Pb1 I1 98.63(7) 3_756 6_865 ?
O3 Pb1 I1 155.45(8) . 6_865 ?
I1 Pb1 I1 89.996(9) . 6_865 ?
Pb1 I1 Pb1 85.123(8) . 6_855 ?
N1 O1 Pb1 124.0(2) . 2_456 ?
N1 O1 Pb1 115.6(2) . 5_766 ?
Pb1 O1 Pb1 115.54(11) 2_456 5_766 ?
C1 O2 Pb1 97.6(3) . . ?
C1 O3 Pb1 141.1(3) . 3_756 ?
C1 O3 Pb1 88.5(3) . . ?
Pb1 O3 Pb1 105.26(10) 3_756 . ?
O1 N1 C4 119.3(4) . . ?
O1 N1 C5 119.1(3) . . ?
C4 N1 C5 121.5(4) . . ?
O3 C1 O2 124.1(4) . . ?
O3 C1 C2 118.6(4) . . ?
O2 C1 C2 117.2(4) . . ?
C3 C2 C6 118.2(4) . . ?
C3 C2 C1 121.0(4) . . ?
C6 C2 C1 120.7(4) . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N1 C4 C3 119.8(4) . . ?
N1 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C6 119.1(4) . . ?
N1 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C2 120.9(4) . . ?
C5 C6 H6 119.5 . . ?
C2 C6 H6 119.5 . . ?

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
O2 Pb1 I1 Pb1 86.16(8) . . . 6_855 ?
O1 Pb1 I1 Pb1 18.74(7) 2_556 . . 6_855 ?
O1 Pb1 I1 Pb1 -16.56(18) 5_766 . . 6_855 ?
O3 Pb1 I1 Pb1 -158.44(7) 3_756 . . 6_855 ?
O3 Pb1 I1 Pb1 137.83(7) . . . 6_855 ?
I1 Pb1 I1 Pb1 -59.617(12) 6_865 . . 6_855 ?
O1 Pb1 O2 C1 174.1(3) 2_556 . . . ?
O1 Pb1 O2 C1 -99.0(3) 5_766 . . . ?
O3 Pb1 O2 C1 19.1(3) 3_756 . . . ?
O3 Pb1 O2 C1 3.1(3) . . . . ?
I1 Pb1 O2 C1 103.4(3) . . . . ?
I1 Pb1 O2 C1 -145.5(2) 6_865 . . . ?
O2 Pb1 O3 C1 -3.1(3) . . . . ?
O1 Pb1 O3 C1 -13.3(3) 2_556 . . . ?
O1 Pb1 O3 C1 71.9(3) 5_766 . . . ?
O3 Pb1 O3 C1 -168.0(2) 3_756 . . . ?
I1 Pb1 O3 C1 -98.5(2) . . . . ?
I1 Pb1 O3 C1 127.7(2) 6_865 . . . ?
O2 Pb1 O3 Pb1 140.0(2) . . . 3_756 ?
O1 Pb1 O3 Pb1 129.80(11) 2_556 . . 3_756 ?
O1 Pb1 O3 Pb1 -145.00(12) 5_766 . . 3_756 ?
O3 Pb1 O3 Pb1 -24.93(15) 3_756 . . 3_756 ?
I1 Pb1 O3 Pb1 44.57(12) . . . 3_756 ?
I1 Pb1 O3 Pb1 -89.22(18) 6_865 . . 3_756 ?
Pb1 O1 N1 C4 -99.5(4) 2_456 . . . ?
Pb1 O1 N1 C4 106.4(4) 5_766 . . . ?
Pb1 O1 N1 C5 83.1(4) 2_456 . . . ?
Pb1 O1 N1 C5 -71.1(4) 5_766 . . . ?
Pb1 O3 C1 O2 -106.9(5) 3_756 . . . ?
Pb1 O3 C1 O2 5.8(5) . . . . ?
Pb1 O3 C1 C2 77.1(6) 3_756 . . . ?
Pb1 O3 C1 C2 -170.2(4) . . . . ?
Pb1 O2 C1 O3 -6.3(5) . . . . ?
Pb1 O2 C1 C2 169.7(3) . . . . ?
O3 C1 C2 C3 -0.8(7) . . . . ?
O2 C1 C2 C3 -177.1(4) . . . . ?
O3 C1 C2 C6 175.1(4) . . . . ?
O2 C1 C2 C6 -1.2(6) . . . . ?
C6 C2 C3 C4 -1.4(7) . . . . ?
C1 C2 C3 C4 174.6(4) . . . . ?
O1 N1 C4 C3 -172.2(4) . . . . ?
C5 N1 C4 C3 5.1(7) . . . . ?
C2 C3 C4 N1 -2.5(7) . . . . ?
O1 N1 C5 C6 173.7(4) . . . . ?
C4 N1 C5 C6 -3.7(7) . . . . ?
N1 C5 C6 C2 -0.3(7) . . . . ?
C3 C2 C6 C5 2.8(7) . . . . ?
C1 C2 C6 C5 -173.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.146
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_morsa1411_0ma
_database_code_depnum_ccdc_archive 'CCDC 1063338'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[Pb(INO)Br)n'
_chemical_name_common            ?
_chemical_melting_point          dp>300
_chemical_formula_moiety         'C6 H4 Br N O3 Pb'
_chemical_formula_sum            'C6 H4 Br N O3 Pb'
_chemical_formula_weight         425.20

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n '


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

_cell_length_a                   13.2594(7)
_cell_length_b                   7.0293(4)
_cell_length_c                   17.5526(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1635.98(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9991
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      31.63

_exptl_crystal_description       irregular
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    25.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3713
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28723
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         28.00
_reflns_number_total             1974
_reflns_number_gt                1785
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0230P)²+3.4109P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00320(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1974
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0197
_refine_ls_wR_factor_ref         0.0510
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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 0.845109(10) 0.22560(2) 0.224092(8) 0.01914(8) Uani 1 1 d . . .
Br1 Br 0.85302(3) -0.14789(8) 0.30383(3) 0.03350(13) Uani 1 1 d . . .
O2 O 0.9718(2) 0.3170(5) 0.33347(16) 0.0307(7) Uani 1 1 d . . .
C1 C 1.0008(3) 0.2574(5) 0.1018(2) 0.0198(8) Uani 1 1 d . . .
O1 O 0.9197(2) 0.1731(5) 0.09087(17) 0.0328(7) Uani 1 1 d . . .
C2 C 0.9343(3) 0.6988(5) -0.0345(2) 0.0176(7) Uani 1 1 d . . .
O3 O 0.7775(2) 0.5200(4) 0.15180(15) 0.0259(6) Uani 1 1 d . . .
N1 N 0.8269(2) 0.5878(5) 0.09042(18) 0.0200(7) Uani 1 1 d . . .
C4 C 0.9111(3) 0.6894(6) 0.1007(2) 0.0231(8) Uani 1 1 d . . .
H4 H 0.9322 0.7212 0.1496 0.028 Uiso 1 1 calc R . .
C3 C 0.9665(3) 0.7465(5) 0.0383(2) 0.0201(8) Uani 1 1 d . . .
H3 H 1.0252 0.8169 0.0449 0.024 Uiso 1 1 calc R . .
C6 C 0.8445(3) 0.5978(7) -0.0426(2) 0.0241(9) Uani 1 1 d . . .
H6 H 0.8208 0.5661 -0.0908 0.029 Uiso 1 1 calc R . .
C5 C 0.7914(3) 0.5457(6) 0.0211(2) 0.0243(8) Uani 1 1 d . . .
H5 H 0.7306 0.4810 0.0161 0.029 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
Pb1 0.01823(11) 0.02799(12) 0.01120(10) 0.00329(5) 0.00014(5) -0.00068(5)
Br1 0.0327(2) 0.0422(3) 0.0257(2) 0.0081(2) -0.00962(17) 0.00313(19)
O2 0.0323(16) 0.0471(19) 0.0127(14) -0.0015(13) 0.0010(12) -0.0011(14)
C1 0.024(2) 0.0201(19) 0.0156(19) 0.0042(13) 0.0043(16) 0.0065(15)
O1 0.0308(16) 0.0425(19) 0.0252(16) -0.0043(14) 0.0076(13) -0.0115(15)
C2 0.0215(19) 0.0187(18) 0.0126(17) 0.0016(14) 0.0027(14) 0.0043(14)
O3 0.0303(15) 0.0301(15) 0.0173(14) 0.0105(12) 0.0128(12) 0.0034(12)
N1 0.0242(16) 0.0216(17) 0.0142(15) 0.0069(13) 0.0061(12) 0.0041(13)
C4 0.027(2) 0.030(2) 0.0126(18) -0.0026(16) 0.0010(15) -0.0001(17)
C3 0.024(2) 0.0203(19) 0.0165(19) -0.0014(14) 0.0025(15) -0.0011(15)
C6 0.027(2) 0.031(2) 0.0142(19) 0.0029(16) -0.0007(15) -0.0011(16)
C5 0.022(2) 0.029(2) 0.022(2) 0.0025(16) 0.0005(15) -0.0056(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O3 2.518(3) 6_755 ?
Pb1 O1 2.566(3) . ?
Pb1 O3 2.588(3) . ?
Pb1 O2 2.631(3) . ?
Pb1 O2 2.706(3) 3_755 ?
Pb1 Br1 2.9771(5) . ?
Pb1 Br1 3.1067(5) 6_765 ?
Br1 Pb1 3.1067(5) 6_755 ?
O2 C1 1.263(5) 3_755 ?
O2 Pb1 2.706(3) 3_755 ?
C1 O1 1.243(5) . ?
C1 O2 1.263(5) 3_755 ?
C1 C2 1.495(5) 5_765 ?
C2 C3 1.387(5) . ?
C2 C6 1.393(6) . ?
C2 C1 1.495(5) 5_765 ?
O3 N1 1.348(4) . ?
O3 Pb1 2.518(3) 6_765 ?
N1 C5 1.337(5) . ?
N1 C4 1.338(5) . ?
C4 C3 1.379(5) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C6 C5 1.370(5) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Pb1 O1 72.95(9) 6_755 . ?
O3 Pb1 O3 89.32(6) 6_755 . ?
O1 Pb1 O3 78.56(10) . . ?
O3 Pb1 O2 156.94(9) 6_755 . ?
O1 Pb1 O2 117.01(10) . . ?
O3 Pb1 O2 112.57(10) . . ?
O3 Pb1 O2 121.80(9) 6_755 3_755 ?
O1 Pb1 O2 49.33(9) . 3_755 ?
O3 Pb1 O2 86.43(9) . 3_755 ?
O2 Pb1 O2 69.00(10) . 3_755 ?
O3 Pb1 Br1 75.73(6) 6_755 . ?
O1 Pb1 Br1 106.74(8) . . ?
O3 Pb1 Br1 161.44(6) . . ?
O2 Pb1 Br1 81.36(7) . . ?
O2 Pb1 Br1 110.69(7) 3_755 . ?
O3 Pb1 Br1 81.11(7) 6_755 6_765 ?
O1 Pb1 Br1 141.05(8) . 6_765 ?
O3 Pb1 Br1 72.48(6) . 6_765 ?
O2 Pb1 Br1 98.13(7) . 6_765 ?
O2 Pb1 Br1 149.16(7) 3_755 6_765 ?
Br1 Pb1 Br1 94.037(14) . 6_765 ?
Pb1 Br1 Pb1 90.619(12) . 6_755 ?
C1 O2 Pb1 139.3(3) 3_755 . ?
C1 O2 Pb1 90.0(2) 3_755 3_755 ?
Pb1 O2 Pb1 104.03(10) . 3_755 ?
O1 C1 O2 123.1(4) . 3_755 ?
O1 C1 C2 118.3(4) . 5_765 ?
O2 C1 C2 118.5(4) 3_755 5_765 ?
C1 O1 Pb1 97.1(2) . . ?
C3 C2 C6 118.7(4) . . ?
C3 C2 C1 120.1(4) . 5_765 ?
C6 C2 C1 121.1(3) . 5_765 ?
N1 O3 Pb1 120.9(2) . 6_765 ?
N1 O3 Pb1 120.4(2) . . ?
Pb1 O3 Pb1 115.82(9) 6_765 . ?
C5 N1 C4 122.3(3) . . ?
C5 N1 O3 118.6(3) . . ?
C4 N1 O3 119.1(3) . . ?
N1 C4 C3 119.5(4) . . ?
N1 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C6 C2 119.5(4) . . ?
C5 C6 H6 120.3 . . ?
C2 C6 H6 120.3 . . ?
N1 C5 C6 120.1(4) . . ?
N1 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?

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
O3 Pb1 Br1 Pb1 -15.35(7) 6_755 . . 6_755 ?
O1 Pb1 Br1 Pb1 -82.25(7) . . . 6_755 ?
O3 Pb1 Br1 Pb1 21.9(2) . . . 6_755 ?
O2 Pb1 Br1 Pb1 162.03(7) . . . 6_755 ?
O2 Pb1 Br1 Pb1 -134.38(7) 3_755 . . 6_755 ?
Br1 Pb1 Br1 Pb1 64.40(2) 6_765 . . 6_755 ?
O3 Pb1 O2 C1 -12.1(5) 6_755 . . 3_755 ?
O1 Pb1 O2 C1 -123.0(4) . . . 3_755 ?
O3 Pb1 O2 C1 148.7(4) . . . 3_755 ?
O2 Pb1 O2 C1 -134.7(4) 3_755 . . 3_755 ?
Br1 Pb1 O2 C1 -18.6(4) . . . 3_755 ?
Br1 Pb1 O2 C1 74.3(4) 6_765 . . 3_755 ?
O3 Pb1 O2 Pb1 94.7(2) 6_755 . . 3_755 ?
O1 Pb1 O2 Pb1 -16.19(16) . . . 3_755 ?
O3 Pb1 O2 Pb1 -104.51(11) . . . 3_755 ?
O2 Pb1 O2 Pb1 -27.91(14) 3_755 . . 3_755 ?
Br1 Pb1 O2 Pb1 88.26(9) . . . 3_755 ?
Br1 Pb1 O2 Pb1 -178.86(8) 6_765 . . 3_755 ?
O2 C1 O1 Pb1 7.8(4) 3_755 . . . ?
C2 C1 O1 Pb1 -168.0(3) 5_765 . . . ?
O3 Pb1 O1 C1 -176.0(3) 6_755 . . . ?
O3 Pb1 O1 C1 91.2(3) . . . . ?
O2 Pb1 O1 C1 -18.5(3) . . . . ?
O2 Pb1 O1 C1 -4.0(2) 3_755 . . . ?
Br1 Pb1 O1 C1 -107.2(2) . . . . ?
Br1 Pb1 O1 C1 133.5(2) 6_765 . . . ?
O3 Pb1 O3 N1 -98.0(2) 6_755 . . . ?
O1 Pb1 O3 N1 -25.2(3) . . . . ?
O2 Pb1 O3 N1 89.4(3) . . . . ?
O2 Pb1 O3 N1 24.0(3) 3_755 . . . ?
Br1 Pb1 O3 N1 -133.9(2) . . . . ?
Br1 Pb1 O3 N1 -178.9(3) 6_765 . . . ?
O3 Pb1 O3 Pb1 101.01(17) 6_755 . . 6_765 ?
O1 Pb1 O3 Pb1 173.75(14) . . . 6_765 ?
O2 Pb1 O3 Pb1 -71.57(14) . . . 6_765 ?
O2 Pb1 O3 Pb1 -137.07(13) 3_755 . . 6_765 ?
Br1 Pb1 O3 Pb1 65.1(3) . . . 6_765 ?
Br1 Pb1 O3 Pb1 20.12(9) 6_765 . . 6_765 ?
Pb1 O3 N1 C5 -98.6(4) 6_765 . . . ?
Pb1 O3 N1 C5 101.3(3) . . . . ?
Pb1 O3 N1 C4 83.5(4) 6_765 . . . ?
Pb1 O3 N1 C4 -76.6(4) . . . . ?
C5 N1 C4 C3 -2.9(6) . . . . ?
O3 N1 C4 C3 174.9(3) . . . . ?
N1 C4 C3 C2 0.2(6) . . . . ?
C6 C2 C3 C4 1.7(6) . . . . ?
C1 C2 C3 C4 -173.7(4) 5_765 . . . ?
C3 C2 C6 C5 -1.1(6) . . . . ?
C1 C2 C6 C5 174.3(4) 5_765 . . . ?
C4 N1 C5 C6 3.6(6) . . . . ?
O3 N1 C5 C6 -174.2(4) . . . . ?
C2 C6 C5 N1 -1.5(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.516
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.173
_exptl_crystal_recrystallization_method 'brunch tube'
