# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_pbbrbdc-1
_database_code_depnum_ccdc_archive 'CCDC 1836046'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date             2017-11-07
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C32 H16 Br6 O16 Pb4), 3(C2 H8 N)'
_chemical_formula_sum            'C22 H32 Br3 N3 O8 Pb2'
_chemical_formula_weight         1120.61
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Br Br -0.2900 2.4600 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3940 10.1110 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'

_cell_length_a                   13.8177(5)
_cell_length_b                   13.8177(5)
_cell_length_c                   16.3601(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3123.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      26.473
_cell_measurement_theta_min      2.894
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.649
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1777 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.4663.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2071
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23339
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.894
_diffrn_ambient_temperature      295.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   ?
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2510
_reflns_number_total             2760
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.794
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 
;
 Flack x determined using 942 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2760
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0204P)²+3.0832P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0517
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.12932(3) -0.07846(3) 0.42366(2) 0.02983(11) Uani 1 1 d . . . . .
Br1 Br 0.17007(10) -0.17007(10) 0.250000 0.0577(5) Uani 1 2 d S T P . .
Br2 Br 0.12325(11) -0.01828(10) 0.59320(7) 0.0632(4) Uani 1 1 d . . . . .
O1 O 0.2756(5) 0.0511(5) 0.4187(4) 0.0424(17) Uani 1 1 d . . . . .
O2 O 0.3002(5) -0.1029(4) 0.4438(4) 0.0415(18) Uani 1 1 d . . . . .
O3 O 0.7542(5) 0.1460(5) 0.5265(4) 0.0393(18) Uani 1 1 d . . . . .
O4 O 0.7750(5) -0.0053(5) 0.5613(4) 0.0407(17) Uani 1 1 d . . . . .
C1 C 0.3283(7) -0.0182(7) 0.4391(6) 0.031(2) Uani 1 1 d . . . . .
C2 C 0.4343(7) 0.0012(6) 0.4585(5) 0.028(2) Uani 1 1 d . . . . .
C3 C 0.4734(7) 0.0923(7) 0.4461(6) 0.038(3) Uani 1 1 d . . . . .
H3 H 0.436596 0.140673 0.421787 0.046 Uiso 1 1 calc R . . . .
C4 C 0.5666(7) 0.1108(7) 0.4699(6) 0.042(3) Uani 1 1 d . . . . .
H4 H 0.592342 0.172272 0.462134 0.050 Uiso 1 1 calc R . . . .
C5 C 0.4913(7) -0.0710(8) 0.4909(6) 0.039(3) Uani 1 1 d . . . . .
H5 H 0.466772 -0.133321 0.496547 0.047 Uiso 1 1 calc R . . . .
C6 C 0.5844(8) -0.0511(7) 0.5150(6) 0.038(2) Uani 1 1 d . . . . .
H6 H 0.622083 -0.099618 0.538233 0.045 Uiso 1 1 calc R . . . .
C7 C 0.7259(7) 0.0624(7) 0.5339(5) 0.025(2) Uani 1 1 d . . . . .
C8 C 0.6225(7) 0.0403(7) 0.5048(5) 0.029(2) Uani 1 1 d . . . . .
N1 N 0.7225(7) 0.2775(7) 0.250000 0.051(4) Uani 1 2 d S T P . .
H1A H 0.662459 0.271016 0.231078 0.061 Uiso 0.5 1 calc R . . . .
H1B H 0.728982 0.337541 0.268923 0.061 Uiso 0.5 1 calc R . . . .
C9 C 0.7377(14) 0.2103(12) 0.3152(9) 0.122(7) Uani 1 1 d . . . . .
H9A H 0.709740 0.148960 0.300979 0.182 Uiso 1 1 calc GR . . . .
H9B H 0.707743 0.234312 0.364086 0.182 Uiso 1 1 calc GR . . . .
H9C H 0.805911 0.202447 0.324296 0.182 Uiso 1 1 calc GR . . . .
N2 N 0.8109(6) -0.1652(6) 0.6624(5) 0.044(2) Uani 1 1 d . . . . .
H2A H 0.772593 -0.214105 0.676692 0.052 Uiso 1 1 calc R . . . .
H2B H 0.775704 -0.124327 0.632653 0.052 Uiso 1 1 calc R . . . .
C10 C 0.8872(10) -0.2025(10) 0.6119(7) 0.073(4) Uani 1 1 d . . . . .
H10A H 0.860337 -0.244360 0.570956 0.110 Uiso 1 1 calc GR . . . .
H10B H 0.931952 -0.238369 0.645105 0.110 Uiso 1 1 calc GR . . . .
H10C H 0.920488 -0.149823 0.585983 0.110 Uiso 1 1 calc GR . . . .
C11 C 0.8419(10) -0.1159(8) 0.7356(7) 0.067(4) Uani 1 1 d . . . . .
H11A H 0.879988 -0.060421 0.720996 0.101 Uiso 1 1 calc GR . . . .
H11B H 0.880196 -0.159087 0.768299 0.101 Uiso 1 1 calc GR . . . .
H11C H 0.786270 -0.095500 0.766150 0.101 Uiso 1 1 calc GR . . . .


_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 Br1 3.1609(9) . ?
Pb1 Br2 3.4647(14) 8_556 ?
Pb1 Br2 2.8969(12) . ?
Pb1 O1 2.702(6) . ?
Pb1 O2 2.408(6) . ?
Pb1 O3 2.463(6) 8_546 ?
Pb1 O4 2.760(6) 8_546 ?
Pb1 C1 2.883(9) . ?
Pb1 C7 2.940(9) 8_546 ?
O1 C1 1.249(11) . ?
O2 C1 1.235(11) . ?
O3 C7 1.225(11) . ?
O4 C7 1.239(10) . ?
C1 C2 1.523(13) . ?
C2 C3 1.385(13) . ?
C2 C5 1.378(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.369(13) . ?
C4 H4 0.9300 . ?
C4 C8 1.367(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.373(13) . ?
C6 H6 0.9300 . ?
C6 C8 1.378(12) . ?
C7 C8 1.537(13) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C9 1.430(15) 7_665 ?
N1 C9 1.430(15) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C10 1.435(14) . ?
N2 C11 1.443(13) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

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
Br1 Pb1 Br2 110.83(4) . 8_556 ?
Br2 Pb1 Br1 168.73(4) . . ?
Br2 Pb1 Br2 80.11(4) . 8_556 ?
Br2 Pb1 C7 91.64(16) . 8_546 ?
O1 Pb1 Br1 96.03(15) . . ?
O1 Pb1 Br2 84.54(15) . 8_556 ?
O1 Pb1 Br2 81.97(16) . . ?
O1 Pb1 O4 173.21(19) . 8_546 ?
O1 Pb1 C1 25.6(2) . . ?
O1 Pb1 C7 148.4(2) . 8_546 ?
O2 Pb1 Br1 83.81(17) . . ?
O2 Pb1 Br2 86.42(17) . . ?
O2 Pb1 Br2 134.52(15) . 8_556 ?
O2 Pb1 O1 50.5(2) . . ?
O2 Pb1 O3 74.4(2) . 8_546 ?
O2 Pb1 O4 123.1(2) . 8_546 ?
O2 Pb1 C1 25.0(2) . . ?
O2 Pb1 C7 98.5(2) . 8_546 ?
O3 Pb1 Br1 84.54(16) 8_546 . ?
O3 Pb1 Br2 146.79(16) 8_546 8_556 ?
O3 Pb1 Br2 87.43(16) 8_546 . ?
O3 Pb1 O1 124.2(2) 8_546 . ?
O3 Pb1 O4 49.1(2) 8_546 8_546 ?
O3 Pb1 C1 98.8(3) 8_546 . ?
O3 Pb1 C7 24.2(2) 8_546 8_546 ?
O4 Pb1 Br1 84.64(15) 8_546 . ?
O4 Pb1 Br2 96.06(15) 8_546 . ?
O4 Pb1 Br2 101.57(14) 8_546 8_556 ?
O4 Pb1 C1 147.8(2) 8_546 . ?
O4 Pb1 C7 24.8(2) 8_546 8_546 ?
C1 Pb1 Br1 91.41(19) . . ?
C1 Pb1 Br2 109.64(19) . 8_556 ?
C1 Pb1 Br2 82.00(19) . . ?
C1 Pb1 C7 123.0(3) . 8_546 ?
C7 Pb1 Br1 84.27(16) 8_546 . ?
C7 Pb1 Br2 124.97(18) 8_546 8_556 ?
Pb1 Br1 Pb1 131.70(7) . 7 ?
Pb1 Br2 Pb1 96.67(4) . 8_556 ?
C1 O1 Pb1 85.4(5) . . ?
C1 O2 Pb1 99.6(6) . . ?
C7 O3 Pb1 100.3(6) . 8_656 ?
C7 O4 Pb1 85.7(5) . 8_656 ?
O1 C1 Pb1 69.1(5) . . ?
O1 C1 C2 118.7(8) . . ?
O2 C1 Pb1 55.4(5) . . ?
O2 C1 O1 124.1(9) . . ?
O2 C1 C2 117.2(9) . . ?
C2 C1 Pb1 170.5(7) . . ?
C3 C2 C1 120.4(9) . . ?
C5 C2 C1 120.2(8) . . ?
C5 C2 C3 119.4(9) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.7(9) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 119.4 . . ?
C8 C4 C3 121.1(10) . . ?
C8 C4 H4 119.4 . . ?
C2 C5 H5 120.0 . . ?
C6 C5 C2 120.1(9) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C8 120.4(10) . . ?
C8 C6 H6 119.8 . . ?
O3 C7 Pb1 55.5(5) . 8_656 ?
O3 C7 O4 125.0(9) . . ?
O3 C7 C8 116.9(8) . . ?
O4 C7 Pb1 69.4(5) . 8_656 ?
O4 C7 C8 118.1(8) . . ?
C8 C7 Pb1 172.1(6) . 8_656 ?
C4 C8 C6 119.2(9) . . ?
C4 C8 C7 120.9(9) . . ?
C6 C8 C7 119.9(9) . . ?
H1A N1 H1B 108.0 . . ?
C9 N1 H1A 109.3 7_665 . ?
C9 N1 H1A 109.3 . . ?
C9 N1 H1B 109.3 . . ?
C9 N1 H1B 109.3 7_665 . ?
C9 N1 C9 111.4(19) 7_665 . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H2A N2 H2B 107.5 . . ?
C10 N2 H2A 108.4 . . ?
C10 N2 H2B 108.4 . . ?
C10 N2 C11 115.4(10) . . ?
C11 N2 H2A 108.4 . . ?
C11 N2 H2B 108.4 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
Pb1 O1 C1 O2 6.8(10) . . . . ?
Pb1 O1 C1 C2 -174.1(8) . . . . ?
Pb1 O2 C1 O1 -7.7(12) . . . . ?
Pb1 O2 C1 C2 173.1(7) . . . . ?
Pb1 O3 C7 O4 1.1(10) 8_656 . . . ?
Pb1 O3 C7 C8 -177.4(6) 8_656 . . . ?
Pb1 O4 C7 O3 -1.0(9) 8_656 . . . ?
Pb1 O4 C7 C8 177.5(7) 8_656 . . . ?
O1 C1 C2 C3 -6.1(14) . . . . ?
O1 C1 C2 C5 171.9(10) . . . . ?
O2 C1 C2 C3 173.1(10) . . . . ?
O2 C1 C2 C5 -8.9(14) . . . . ?
O3 C7 C8 C4 2.2(13) . . . . ?
O3 C7 C8 C6 -176.9(9) . . . . ?
O4 C7 C8 C4 -176.4(9) . . . . ?
O4 C7 C8 C6 4.5(13) . . . . ?
C1 C2 C3 C4 174.8(9) . . . . ?
C1 C2 C5 C6 -174.4(9) . . . . ?
C2 C3 C4 C8 0.8(17) . . . . ?
C2 C5 C6 C8 -1.8(16) . . . . ?
C3 C2 C5 C6 3.7(16) . . . . ?
C3 C4 C8 C6 1.0(16) . . . . ?
C3 C4 C8 C7 -178.0(9) . . . . ?
C5 C2 C3 C4 -3.2(16) . . . . ?
C5 C6 C8 C4 -0.6(16) . . . . ?
C5 C6 C8 C7 178.5(9) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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. 
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#######################################################################

data_pbibdc-5
_database_code_depnum_ccdc_archive 'CCDC 1836048'
_audit_update_record             
;
2018-05-05 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date             2017-11-03
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C32 H16 I6 O16 Pb4), 3(C2 H8 N)'
_chemical_formula_sum            'C22 H32 I3 N3 O8 Pb2'
_chemical_formula_weight         1261.60
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
I I -0.4740 1.8120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3940 10.1110 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'

_cell_length_a                   13.9190(10)
_cell_length_b                   13.9190(10)
_cell_length_c                   17.003(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3294.1(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    278.15
_cell_measurement_theta_max      27.456
_cell_measurement_theta_min      2.808
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.063
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44508
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         2.927
_diffrn_ambient_temperature      278.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3616
_reflns_number_total             3771
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.022(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3771
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0171
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0113P)²+0.1790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0369
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.978(5)
 0.022(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.63055(2) 0.58305(2) 0.32248(2) 0.02488(5) Uani 1 1 d . . . . .
I1 I 0.62326(3) 0.52048(3) 0.14659(2) 0.04524(11) Uani 1 1 d . . . . .
I2 I 0.67039(3) 0.67039(3) 0.500000 0.04658(15) Uani 1 2 d S T P . .
O1 O 0.4959(3) 0.7276(3) 0.3106(2) 0.0383(9) Uani 1 1 d . . . . .
O2 O 0.6478(2) 0.7494(2) 0.2781(2) 0.0334(9) Uani 1 1 d . . . . .
O3 O 0.5470(3) 1.2250(3) 0.1726(2) 0.0383(9) Uani 1 1 d . . . . .
O4 O 0.3937(2) 1.1990(2) 0.1953(2) 0.0333(9) Uani 1 1 d . . . . .
C1 C 0.5619(4) 0.7788(3) 0.2849(3) 0.0256(10) Uani 1 1 d . . . . .
C2 C 0.5401(3) 0.8806(3) 0.2581(3) 0.0254(10) Uani 1 1 d . . . . .
C3 C 0.4508(4) 0.9185(4) 0.2700(3) 0.0345(13) Uani 1 1 d . . . . .
H3 H 0.403145 0.881121 0.293183 0.041 Uiso 1 1 calc R . . . .
C4 C 0.4304(4) 1.0124(4) 0.2477(4) 0.0356(13) Uani 1 1 d . . . . .
H4 H 0.369525 1.037622 0.256517 0.043 Uiso 1 1 calc R . . . .
C5 C 0.4996(4) 1.0679(4) 0.2127(3) 0.0266(11) Uani 1 1 d . . . . .
C6 C 0.4797(4) 1.1704(4) 0.1917(3) 0.0282(11) Uani 1 1 d . . . . .
C7 C 0.5900(4) 1.0285(4) 0.1982(3) 0.0337(12) Uani 1 1 d . . . . .
H7 H 0.636967 1.064845 0.173046 0.040 Uiso 1 1 calc R . . . .
C8 C 0.6096(4) 0.9353(4) 0.2213(3) 0.0335(13) Uani 1 1 d . . . . .
H8 H 0.669996 0.909178 0.211923 0.040 Uiso 1 1 calc R . . . .
N1 N 0.1913(3) 1.1655(4) 0.1554(3) 0.0430(12) Uani 1 1 d . . . . .
H1A H 0.233189 1.212133 0.166005 0.052 Uiso 1 1 calc R . . . .
H1B H 0.221215 1.122381 0.125554 0.052 Uiso 1 1 calc R . . . .
C9 C 0.1639(6) 1.1198(5) 0.2289(4) 0.066(2) Uani 1 1 d . . . . .
H9A H 0.121983 1.066622 0.218109 0.099 Uiso 1 1 calc GR . . . .
H9B H 0.131162 1.165470 0.261656 0.099 Uiso 1 1 calc GR . . . .
H9C H 0.220339 1.097093 0.255467 0.099 Uiso 1 1 calc GR . . . .
C10 C 0.1126(5) 1.2060(6) 0.1110(4) 0.062(2) Uani 1 1 d . . . . .
H10A H 0.137400 1.238628 0.065541 0.093 Uiso 1 1 calc GR . . . .
H10B H 0.078024 1.250689 0.143263 0.093 Uiso 1 1 calc GR . . . .
H10C H 0.070235 1.155424 0.094495 0.093 Uiso 1 1 calc GR . . . .
N2 N 0.7168(3) 1.2832(3) 0.250000 0.0410(17) Uani 1 2 d S T P . .
H2A H 0.722305 1.342188 0.269675 0.049 Uiso 0.5 1 calc R . . . .
H2B H 0.657811 1.277695 0.230327 0.049 Uiso 0.5 1 calc R . . . .
C11 C 0.7271(6) 1.2144(6) 0.3143(5) 0.084(3) Uani 1 1 d . . . . .
H11A H 0.736285 1.151143 0.293046 0.126 Uiso 1 1 calc GR . . . .
H11B H 0.670167 1.215245 0.346127 0.126 Uiso 1 1 calc GR . . . .
H11C H 0.781608 1.231558 0.345873 0.126 Uiso 1 1 calc GR . . . .


_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 I1 3.5974(5) 7_665 ?
Pb1 I1 3.1166(7) . ?
Pb1 I2 3.3009(6) . ?
Pb1 O1 2.758(4) . ?
Pb1 O2 2.447(3) . ?
Pb1 O3 2.707(4) 7_765 ?
Pb1 O4 2.414(3) 7_765 ?
Pb1 C1 2.957(5) . ?
Pb1 C6 2.915(5) 7_765 ?
O1 C1 1.242(6) . ?
O2 C1 1.269(6) . ?
O3 C6 1.249(6) . ?
O4 C6 1.262(6) . ?
C1 C2 1.519(7) . ?
C2 C3 1.366(7) . ?
C2 C8 1.380(7) . ?
C3 C4 1.390(7) . ?
C4 C5 1.370(8) . ?
C5 C6 1.497(7) . ?
C5 C7 1.395(7) . ?
C7 C8 1.383(7) . ?
N1 C9 1.453(8) . ?
N1 C10 1.445(8) . ?
N2 C11 1.460(8) . ?
N2 C11 1.460(8) 7_775 ?

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
I1 Pb1 I1 84.154(12) . 7_665 ?
I1 Pb1 I2 170.355(14) . . ?
I2 Pb1 I1 104.981(14) . 7_665 ?
O1 Pb1 I1 96.39(8) . . ?
O1 Pb1 I1 101.31(8) . 7_665 ?
O1 Pb1 I2 84.99(8) . . ?
O1 Pb1 C1 24.78(12) . . ?
O1 Pb1 C6 149.17(13) . 7_765 ?
O2 Pb1 I1 88.36(9) . . ?
O2 Pb1 I1 149.04(8) . 7_665 ?
O2 Pb1 I2 85.26(9) . . ?
O2 Pb1 O1 49.72(11) . . ?
O2 Pb1 O3 124.73(11) . 7_765 ?
O2 Pb1 C1 24.94(13) . . ?
O2 Pb1 C6 99.49(13) . 7_765 ?
O3 Pb1 I1 84.00(8) 7_765 7_665 ?
O3 Pb1 I1 82.35(9) 7_765 . ?
O3 Pb1 I2 95.35(9) 7_765 . ?
O3 Pb1 O1 174.42(11) 7_765 . ?
O3 Pb1 C1 149.66(13) 7_765 . ?
O3 Pb1 C6 25.34(12) 7_765 7_765 ?
O4 Pb1 I1 87.08(9) 7_765 . ?
O4 Pb1 I1 134.39(8) 7_765 7_665 ?
O4 Pb1 I2 84.27(9) 7_765 . ?
O4 Pb1 O1 124.15(11) 7_765 . ?
O4 Pb1 O2 74.84(11) 7_765 . ?
O4 Pb1 O3 50.45(11) 7_765 7_765 ?
O4 Pb1 C1 99.63(13) 7_765 . ?
O4 Pb1 C6 25.23(13) 7_765 7_765 ?
C1 Pb1 I1 125.33(10) . 7_665 ?
C1 Pb1 I1 92.28(10) . . ?
C1 Pb1 I2 84.98(9) . . ?
C6 Pb1 I1 109.16(10) 7_765 7_665 ?
C6 Pb1 I1 82.40(10) 7_765 . ?
C6 Pb1 I2 91.51(10) 7_765 . ?
C6 Pb1 C1 124.43(14) 7_765 . ?
Pb1 I1 Pb1 92.810(11) . 7_665 ?
Pb1 I2 Pb1 135.43(2) . 8_556 ?
C1 O1 Pb1 86.6(3) . . ?
C1 O2 Pb1 100.6(3) . . ?
C6 O3 Pb1 86.7(3) . 7_675 ?
C6 O4 Pb1 100.2(3) . 7_675 ?
O1 C1 Pb1 68.6(3) . . ?
O1 C1 O2 123.0(5) . . ?
O1 C1 C2 119.5(5) . . ?
O2 C1 Pb1 54.4(2) . . ?
O2 C1 C2 117.5(4) . . ?
C2 C1 Pb1 171.4(3) . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 C8 119.5(5) . . ?
C8 C2 C1 120.7(4) . . ?
C2 C3 C4 120.5(5) . . ?
C5 C4 C3 120.4(5) . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 C7 119.3(5) . . ?
C7 C5 C6 119.9(5) . . ?
O3 C6 Pb1 68.0(3) . 7_675 ?
O3 C6 O4 122.1(5) . . ?
O3 C6 C5 120.2(5) . . ?
O4 C6 Pb1 54.6(2) . 7_675 ?
O4 C6 C5 117.6(5) . . ?
C5 C6 Pb1 168.9(4) . 7_675 ?
C8 C7 C5 119.7(5) . . ?
C2 C8 C7 120.6(5) . . ?
C10 N1 C9 114.9(5) . . ?
C11 N2 C11 115.6(9) . 7_775 ?

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
Pb1 O1 C1 O2 -1.5(5) . . . . ?
Pb1 O1 C1 C2 176.8(4) . . . . ?
Pb1 O2 C1 O1 1.7(6) . . . . ?
Pb1 O2 C1 C2 -176.6(3) . . . . ?
Pb1 O3 C6 O4 7.2(5) 7_675 . . . ?
Pb1 O3 C6 C5 -171.6(5) 7_675 . . . ?
Pb1 O4 C6 O3 -8.2(6) 7_675 . . . ?
Pb1 O4 C6 C5 170.7(4) 7_675 . . . ?
O1 C1 C2 C3 6.9(7) . . . . ?
O1 C1 C2 C8 -172.7(5) . . . . ?
O2 C1 C2 C3 -174.7(5) . . . . ?
O2 C1 C2 C8 5.6(7) . . . . ?
C1 C2 C3 C4 178.3(5) . . . . ?
C1 C2 C8 C7 -178.8(5) . . . . ?
C2 C3 C4 C5 0.6(9) . . . . ?
C3 C2 C8 C7 1.6(8) . . . . ?
C3 C4 C5 C6 -177.3(5) . . . . ?
C3 C4 C5 C7 1.4(9) . . . . ?
C4 C5 C6 Pb1 32(2) . . . 7_675 ?
C4 C5 C6 O3 167.7(5) . . . . ?
C4 C5 C6 O4 -11.2(8) . . . . ?
C4 C5 C7 C8 -2.0(9) . . . . ?
C5 C7 C8 C2 0.5(9) . . . . ?
C6 C5 C7 C8 176.8(5) . . . . ?
C7 C5 C6 Pb1 -146.6(17) . . . 7_675 ?
C7 C5 C6 O3 -11.0(8) . . . . ?
C7 C5 C6 O4 170.0(5) . . . . ?
C8 C2 C3 C4 -2.1(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.978(5)
2 0.022(5)

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1836047'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H32 I3 N3 O8 Pb2'
_chemical_formula_weight         1261.58

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.9257(16)
_cell_length_b                   13.9257(16)
_cell_length_c                   17.035(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3303.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9862
_cell_measurement_theta_min      2.9256
_cell_measurement_theta_max      27.3881

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_F_000             2288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    13.026
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.036
_exptl_absorpt_correction_T_max  0.057
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39638
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.803
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3071
_reflns_number_gt                2952
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.698
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SAINT'
_computing_publication_material  'Bruker SAINT'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.020(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3071
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0165
_refine_ls_wR_factor_ref         0.0403
_refine_ls_wR_factor_gt          0.0400
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.86948(2) 0.08309(2) 1.07251(2) 0.02568(7) Uani 1 1 d . . . . .
I1 I 0.82955(4) 0.17045(4) 1.2500 0.04716(19) Uani 1 2 d S T P . .
I2 I 0.87673(4) 0.02048(4) 0.89657(3) 0.04614(14) Uani 1 1 d . . . . .
O1 O 1.0044(3) 0.2276(3) 1.0608(3) 0.0380(11) Uani 1 1 d . . . . .
O2 O 0.8524(3) 0.2496(3) 1.0282(3) 0.0349(11) Uani 1 1 d . . . . .
O3 O 1.1063(3) 0.6989(3) 0.9452(3) 0.0342(11) Uani 1 1 d . . . . .
O4 O 0.9534(3) 0.7250(3) 0.9228(3) 0.0403(12) Uani 1 1 d . . . . .
N1 N 0.6650(5) 0.3083(4) 0.0947(3) 0.0426(15) Uani 1 1 d . . . . .
H1A H 0.6210 0.2780 0.1243 0.051 Uiso 1 1 d R U . . .
H1B H 0.7121 0.2661 0.0838 0.051 Uiso 1 1 d R U . . .
N2 N 0.7166(4) 0.2834(4) 0.7500 0.042(2) Uani 1 2 d S T P . .
H2A H 0.6576 0.2779 0.7696 0.050 Uiso 0.5 1 calc R U P . .
H2B H 0.7221 0.3424 0.7304 0.050 Uiso 0.5 1 calc R U P . .
C1 C 0.9379(5) 0.2783(5) 1.0352(3) 0.0274(14) Uani 1 1 d . . . . .
C2 C 0.9599(4) 0.3806(4) 1.0079(3) 0.0252(14) Uani 1 1 d . . . . .
C3 C 1.0496(5) 0.4185(5) 1.0202(4) 0.0339(16) Uani 1 1 d . . . . .
H3 H 1.0970 0.3815 1.0438 0.041 Uiso 1 1 calc R U . . .
C4 C 1.0695(5) 0.5121(5) 0.9974(4) 0.0350(16) Uani 1 1 d . . . . .
H4 H 1.1306 0.5372 1.0055 0.042 Uiso 1 1 calc R U . . .
C5 C 1.0001(4) 0.5680(4) 0.9629(4) 0.0252(14) Uani 1 1 d . . . . .
C6 C 0.9099(5) 0.5282(5) 0.9483(4) 0.0346(16) Uani 1 1 d . . . . .
H6 H 0.8629 0.5642 0.9231 0.042 Uiso 1 1 calc R U . . .
C7 C 0.8908(5) 0.4360(5) 0.9714(4) 0.0350(17) Uani 1 1 d . . . . .
H7 H 0.8303 0.4101 0.9623 0.042 Uiso 1 1 calc R U . . .
C8 C 1.0206(5) 0.6696(5) 0.9421(4) 0.0289(15) Uani 1 1 d . . . . .
C9 C 0.7054(7) 0.3866(6) 0.1384(5) 0.061(2) Uani 1 1 d . . . . .
H9A H 0.7508 0.4204 0.1062 0.092 Uiso 1 1 calc R U . . .
H9B H 0.7373 0.3621 0.1842 0.092 Uiso 1 1 calc R U . . .
H9C H 0.6551 0.4296 0.1542 0.092 Uiso 1 1 calc R U . . .
C10 C 0.6196(6) 0.3370(7) 0.0212(5) 0.066(3) Uani 1 1 d . . . . .
H10A H 0.5668 0.3793 0.0322 0.099 Uiso 1 1 calc R U . . .
H10B H 0.5964 0.2811 -0.0057 0.099 Uiso 1 1 calc R U . . .
H10C H 0.6656 0.3696 -0.0112 0.099 Uiso 1 1 calc R U . . .
C11 C 0.7856(8) 0.2729(8) 0.8142(6) 0.088(3) Uani 1 1 d . . . . .
H11A H 0.7883 0.3315 0.8438 0.132 Uiso 1 1 calc R U . . .
H11B H 0.8480 0.2589 0.7931 0.132 Uiso 1 1 calc R U . . .
H11C H 0.7658 0.2213 0.8479 0.132 Uiso 1 1 calc R U . . .


_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 O3 2.416(4) 7_547 ?
Pb1 O2 2.450(4) . ?
Pb1 O4 2.704(5) 7_547 ?
Pb1 I2 3.1231(8) . ?
Pb1 I1 3.3062(7) . ?
I1 Pb1 3.3062(7) 8_667 ?
O1 C1 1.245(7) . ?
O2 C1 1.262(8) . ?
O3 C8 1.263(8) . ?
O3 Pb1 2.416(4) 7_657 ?
O4 C8 1.256(8) . ?
O4 Pb1 2.705(5) 7_657 ?
N1 C9 1.435(9) . ?
N1 C10 1.458(9) . ?
N2 C11 1.464(10) 8_666 ?
N2 C11 1.464(10) . ?
C1 C2 1.530(9) . ?
C2 C3 1.372(9) . ?
C2 C7 1.381(8) . ?
C3 C4 1.387(10) . ?
C4 C5 1.373(9) . ?
C5 C6 1.396(9) . ?
C5 C8 1.486(9) . ?
C6 C7 1.369(9) . ?

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 O2 74.88(14) 7_547 . ?
O3 Pb1 O4 50.35(14) 7_547 7_547 ?
O2 Pb1 O4 124.66(14) . 7_547 ?
O3 Pb1 I2 87.08(11) 7_547 . ?
O2 Pb1 I2 88.38(11) . . ?
O4 Pb1 I2 82.28(10) 7_547 . ?
O3 Pb1 I1 84.25(11) 7_547 . ?
O2 Pb1 I1 85.25(11) . . ?
O4 Pb1 I1 95.39(10) 7_547 . ?
I2 Pb1 I1 170.338(18) . . ?
Pb1 I1 Pb1 135.45(3) . 8_667 ?
C1 O2 Pb1 100.3(4) . . ?
C8 O3 Pb1 100.7(4) . 7_657 ?
C8 O4 Pb1 87.2(4) . 7_657 ?
C9 N1 C10 114.1(6) . . ?
C11 N2 C11 115.3(11) 8_666 . ?
O1 C1 O2 123.8(6) . . ?
O1 C1 C2 119.0(6) . . ?
O2 C1 C2 117.2(6) . . ?
C3 C2 C7 119.2(6) . . ?
C3 C2 C1 119.7(6) . . ?
C7 C2 C1 121.1(6) . . ?
C2 C3 C4 120.0(6) . . ?
C5 C4 C3 120.8(6) . . ?
C4 C5 C6 119.0(6) . . ?
C4 C5 C8 120.5(6) . . ?
C6 C5 C8 120.5(6) . . ?
C7 C6 C5 119.7(6) . . ?
C6 C7 C2 121.2(6) . . ?
O4 C8 O3 121.1(6) . . ?
O4 C8 C5 120.3(6) . . ?
O3 C8 C5 118.6(6) . . ?

_refine_diff_density_max         0.515
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.155

