# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_150513d
_database_code_depnum_ccdc_archive 'CCDC 1472920'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-07-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H28 Br4 N8 O12 Pb4 Pd'
_chemical_formula_weight         2115.54

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'
Pd Pd -0.9988 1.0072 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.634(5)
_cell_length_b                   13.084(8)
_cell_length_c                   14.166(10)
_cell_angle_alpha                105.216(13)
_cell_angle_beta                 105.376(9)
_cell_angle_gamma                94.884(9)
_cell_volume                     1298.2(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1470
_cell_measurement_theta_min      3.066
_cell_measurement_theta_max      23.590

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             958
_exptl_absorpt_coefficient_mu    16.409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1050
_exptl_absorpt_correction_T_max  0.5598
_exptl_absorpt_process_details   sadabs

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6690
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4563
_reflns_number_gt                2924
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0798P)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_number_reflns         4563
_refine_ls_number_parameters     319
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.1723
_refine_ls_wR_factor_gt          0.1639
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.005
_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
Br1 Br 0.8570(3) 0.83928(18) 0.97362(19) 0.0432(6) Uani 1 1 d . . .
Br2 Br 0.5406(3) 0.6025(2) 0.7383(2) 0.0524(7) Uani 1 1 d . . .
C1 C 0.043(2) 0.6184(14) 0.7280(14) 0.015(4) Uani 1 1 d U . .
C2 C 0.023(3) 0.6469(14) 0.6316(15) 0.025(5) Uani 1 1 d . . .
C3 C -0.115(2) 0.5943(14) 0.5456(15) 0.021(4) Uani 1 1 d . . .
H3 H -0.1940 0.5356 0.5448 0.026 Uiso 1 1 calc R . .
C4 C -0.139(3) 0.6283(14) 0.4571(14) 0.024(3) Uani 1 1 d . . .
H4 H -0.2301 0.5897 0.3968 0.029 Uiso 1 1 calc R . .
C5 C -0.030(3) 0.7182(14) 0.4595(14) 0.024(3) Uani 1 1 d . . .
C6 C 0.109(2) 0.7714(14) 0.5464(14) 0.021(4) Uani 1 1 d . . .
H6 H 0.1860 0.8315 0.5483 0.025 Uiso 1 1 calc R . .
C7 C 0.135(2) 0.7346(16) 0.6337(16) 0.029(5) Uani 1 1 d . . .
H7 H 0.2301 0.7706 0.6931 0.034 Uiso 1 1 calc R . .
C8 C -0.109(2) 0.6973(16) 0.2728(16) 0.031(5) Uani 1 1 d . . .
H8 H -0.1217 0.6229 0.2487 0.037 Uiso 1 1 calc R . .
C9 C -0.128(2) 0.7636(16) 0.2150(15) 0.026(5) Uani 1 1 d . . .
H9 H -0.1602 0.7451 0.1439 0.031 Uiso 1 1 calc R . .
C10 C -0.052(2) 0.8658(13) 0.3800(14) 0.017(4) Uani 1 1 d . . .
C11 C -0.076(3) 0.9688(15) 0.2568(16) 0.029(5) Uani 1 1 d . . .
H11A H -0.0805 0.9537 0.1853 0.035 Uiso 1 1 calc R . .
H11B H -0.1802 1.0036 0.2661 0.035 Uiso 1 1 calc R . .
C12 C 0.151(2) 1.0584(14) 0.4219(14) 0.020(4) Uani 1 1 d U . .
C13 C 0.211(3) 1.0944(17) 0.2830(18) 0.040(6) Uani 1 1 d . . .
H13 H 0.1958 1.0923 0.2152 0.048 Uiso 1 1 calc R . .
C14 C 0.346(3) 1.1496(17) 0.3653(17) 0.034(5) Uani 1 1 d . . .
H14 H 0.4463 1.1952 0.3648 0.041 Uiso 1 1 calc R . .
C15 C 0.441(2) 1.1731(17) 0.5546(15) 0.027(5) Uani 1 1 d . . .
C16 C 0.463(2) 1.1105(15) 0.6223(14) 0.022(4) Uani 1 1 d U . .
H16 H 0.4065 1.0390 0.6000 0.026 Uiso 1 1 calc R . .
C17 C 0.567(2) 1.1564(15) 0.7203(15) 0.025(3) Uani 1 1 d . . .
H17 H 0.5782 1.1155 0.7656 0.030 Uiso 1 1 calc R . .
C18 C 0.658(2) 1.2594(15) 0.7562(15) 0.025(3) Uani 1 1 d . . .
C19 C 0.646(3) 1.3159(16) 0.6855(16) 0.027(5) Uani 1 1 d . . .
H19 H 0.7143 1.3845 0.7059 0.033 Uiso 1 1 calc R . .
C20 C 0.538(3) 1.2740(16) 0.5873(17) 0.036(5) Uani 1 1 d . . .
H20 H 0.5311 1.3146 0.5419 0.043 Uiso 1 1 calc R . .
C21 C 0.768(2) 1.3113(15) 0.8672(15) 0.023(4) Uani 1 1 d U . .
C22 C 0.387(3) 0.4867(17) 0.9815(16) 0.030(5) Uani 1 1 d U . .
N1 N 0.095(2) 1.0399(12) 0.3214(12) 0.024(4) Uani 1 1 d . . .
N2 N 0.3189(19) 1.1302(12) 0.4529(12) 0.023(4) Uani 1 1 d . . .
N3 N -0.088(2) 0.8669(12) 0.2841(12) 0.023(4) Uani 1 1 d . . .
N4 N -0.067(2) 0.7570(12) 0.3736(11) 0.022(4) Uani 1 1 d . . .
O1 O 0.8676(18) 1.4009(10) 0.8948(10) 0.031(3) Uani 1 1 d . . .
O2 O 0.760(2) 1.2650(12) 0.9319(11) 0.043(4) Uani 1 1 d . . .
O3 O 0.1293(17) 0.6843(10) 0.8108(10) 0.026(3) Uani 1 1 d . . .
O4 O -0.0291(19) 0.5279(10) 0.7245(11) 0.034(3) Uani 1 1 d . . .
O5 O 0.3044(18) 0.5364(11) 0.9281(11) 0.036(4) Uani 1 1 d . . .
O6 O 0.3249(17) 0.4040(11) 1.0017(12) 0.041(4) Uani 1 1 d . . .
Pb1 Pb -0.02825(10) 0.60473(6) 0.91647(6) 0.0279(2) Uani 1 1 d . . .
Pb2 Pb 0.46887(10) 0.70922(6) 0.91501(7) 0.0337(3) Uani 1 1 d . . .
Pd1 Pd 0.0000 1.0000 0.5000 0.0202(5) Uani 1 2 d S . .


_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
Br1 Pb2 3.076(3) . ?
Br1 Pb1 3.220(3) 1_655 ?
Br2 Pb2 2.745(3) . ?
C1 O3 1.23(2) . ?
C1 O4 1.25(2) . ?
C1 C2 1.48(2) . ?
C2 C7 1.36(3) . ?
C2 C3 1.35(2) . ?
C3 C4 1.41(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.37(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.36(2) . ?
C5 N4 1.41(2) . ?
C6 C7 1.41(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.33(3) . ?
C8 N4 1.37(2) . ?
C8 H8 0.9300 . ?
C9 N3 1.40(2) . ?
C9 H9 0.9300 . ?
C10 N3 1.32(2) . ?
C10 N4 1.39(2) . ?
C10 Pd1 2.022(17) . ?
C11 N1 1.46(2) . ?
C11 N3 1.49(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N1 1.32(2) . ?
C12 N2 1.42(2) . ?
C12 Pd1 2.025(18) . ?
C13 C14 1.32(3) . ?
C13 N1 1.39(3) . ?
C13 H13 0.9300 . ?
C14 N2 1.39(3) . ?
C14 H14 0.9300 . ?
C15 C20 1.36(3) . ?
C15 C16 1.40(2) . ?
C15 N2 1.43(2) . ?
C16 C17 1.35(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.36(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.38(3) . ?
C18 C21 1.51(3) . ?
C19 C20 1.35(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O2 1.24(2) . ?
C21 O1 1.25(2) . ?
C22 O5 1.21(2) . ?
C22 O6 1.27(2) . ?
C22 C22 1.65(4) 2_667 ?
O1 Pb1 2.630(12) 1_665 ?
O1 Pb1 2.653(13) 2_677 ?
O2 Pb1 2.622(14) 2_677 ?
O3 Pb1 2.516(13) . ?
O3 Pb2 2.565(12) . ?
O4 Pb1 2.639(14) . ?
O5 Pb2 2.566(14) . ?
O5 Pb1 2.742(13) . ?
O6 Pb2 2.528(13) 2_667 ?
Pb1 O2 2.622(15) 2_677 ?
Pb1 O1 2.630(12) 1_445 ?
Pb1 O1 2.653(13) 2_677 ?
Pb1 Br1 3.220(3) 1_455 ?
Pb2 O6 2.528(13) 2_667 ?
Pd1 C10 2.022(17) 2_576 ?
Pd1 C12 2.025(18) 2_576 ?

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
Pb2 Br1 Pb1 83.17(7) . 1_655 ?
O3 C1 O4 120.5(16) . . ?
O3 C1 C2 120.0(16) . . ?
O4 C1 C2 119.5(16) . . ?
C7 C2 C3 120.0(18) . . ?
C7 C2 C1 118.5(18) . . ?
C3 C2 C1 121.1(17) . . ?
C2 C3 C4 119.9(17) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.3(17) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 119.6(17) . . ?
C6 C5 N4 120.8(16) . . ?
C4 C5 N4 119.6(16) . . ?
C5 C6 C7 119.5(17) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C2 C7 C6 120.6(18) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C9 C8 N4 108.7(17) . . ?
C9 C8 H8 125.7 . . ?
N4 C8 H8 125.7 . . ?
C8 C9 N3 105.4(17) . . ?
C8 C9 H9 127.3 . . ?
N3 C9 H9 127.3 . . ?
N3 C10 N4 104.4(15) . . ?
N3 C10 Pd1 123.4(12) . . ?
N4 C10 Pd1 132.2(13) . . ?
N1 C11 N3 109.9(14) . . ?
N1 C11 H11A 109.7 . . ?
N3 C11 H11A 109.7 . . ?
N1 C11 H11B 109.7 . . ?
N3 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
N1 C12 N2 103.2(15) . . ?
N1 C12 Pd1 123.5(13) . . ?
N2 C12 Pd1 133.2(13) . . ?
C14 C13 N1 104(2) . . ?
C14 C13 H13 128.0 . . ?
N1 C13 H13 128.0 . . ?
C13 C14 N2 111(2) . . ?
C13 C14 H14 124.7 . . ?
N2 C14 H14 124.7 . . ?
C20 C15 C16 119.0(19) . . ?
C20 C15 N2 121.0(18) . . ?
C16 C15 N2 120.1(18) . . ?
C17 C16 C15 118.5(18) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C18 123.3(19) . . ?
C16 C17 H17 118.4 . . ?
C18 C17 H17 118.4 . . ?
C17 C18 C19 116.6(19) . . ?
C17 C18 C21 122.8(18) . . ?
C19 C18 C21 120.6(17) . . ?
C20 C19 C18 121.8(19) . . ?
C20 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C19 C20 C15 120.4(19) . . ?
C19 C20 H20 119.8 . . ?
C15 C20 H20 119.8 . . ?
O2 C21 O1 119.3(19) . . ?
O2 C21 C18 119.9(17) . . ?
O1 C21 C18 120.8(17) . . ?
O5 C22 O6 128.8(18) . . ?
O5 C22 C22 117(2) . 2_667 ?
O6 C22 C22 113(2) . 2_667 ?
C12 N1 C13 114.8(17) . . ?
C12 N1 C11 122.1(16) . . ?
C13 N1 C11 123.1(17) . . ?
C14 N2 C12 107.5(16) . . ?
C14 N2 C15 126.0(16) . . ?
C12 N2 C15 126.5(16) . . ?
C10 N3 C9 112.4(15) . . ?
C10 N3 C11 121.9(16) . . ?
C9 N3 C11 125.6(16) . . ?
C8 N4 C10 109.1(15) . . ?
C8 N4 C5 126.8(15) . . ?
C10 N4 C5 123.9(16) . . ?
C21 O1 Pb1 160.3(12) . 1_665 ?
C21 O1 Pb1 95.1(11) . 2_677 ?
Pb1 O1 Pb1 99.9(4) 1_665 2_677 ?
C21 O2 Pb1 96.8(12) . 2_677 ?
C1 O3 Pb1 95.8(11) . . ?
C1 O3 Pb2 129.5(11) . . ?
Pb1 O3 Pb2 101.3(4) . . ?
C1 O4 Pb1 89.6(11) . . ?
C22 O5 Pb2 120.5(13) . . ?
C22 O5 Pb1 130.6(13) . . ?
Pb2 O5 Pb1 95.5(4) . . ?
C22 O6 Pb2 123.1(12) . 2_667 ?
O3 Pb1 O2 82.3(5) . 2_677 ?
O3 Pb1 O1 128.4(4) . 1_445 ?
O2 Pb1 O1 125.4(4) 2_677 1_445 ?
O3 Pb1 O4 49.2(4) . . ?
O2 Pb1 O4 126.6(5) 2_677 . ?
O1 Pb1 O4 82.6(4) 1_445 . ?
O3 Pb1 O1 125.0(4) . 2_677 ?
O2 Pb1 O1 47.9(4) 2_677 2_677 ?
O1 Pb1 O1 80.1(4) 1_445 2_677 ?
O4 Pb1 O1 142.6(4) . 2_677 ?
O3 Pb1 O5 70.5(4) . . ?
O2 Pb1 O5 67.7(5) 2_677 . ?
O1 Pb1 O5 81.1(4) 1_445 . ?
O4 Pb1 O5 74.9(4) . . ?
O1 Pb1 O5 69.8(4) 2_677 . ?
O3 Pb1 Br1 82.4(3) . 1_455 ?
O2 Pb1 Br1 71.1(3) 2_677 1_455 ?
O1 Pb1 Br1 143.5(3) 1_445 1_455 ?
O4 Pb1 Br1 114.9(3) . 1_455 ?
O1 Pb1 Br1 98.4(3) 2_677 1_455 ?
O5 Pb1 Br1 132.9(3) . 1_455 ?
O6 Pb2 O3 136.0(4) 2_667 . ?
O6 Pb2 O5 64.2(4) 2_667 . ?
O3 Pb2 O5 72.7(4) . . ?
O6 Pb2 Br2 85.3(4) 2_667 . ?
O3 Pb2 Br2 88.6(3) . . ?
O5 Pb2 Br2 92.6(3) . . ?
O6 Pb2 Br1 76.7(3) 2_667 . ?
O3 Pb2 Br1 146.0(3) . . ?
O5 Pb2 Br1 140.9(3) . . ?
Br2 Pb2 Br1 85.18(8) . . ?
C10 Pd1 C10 180.000(4) 2_576 . ?
C10 Pd1 C12 97.2(7) 2_576 . ?
C10 Pd1 C12 82.8(7) . . ?
C10 Pd1 C12 82.8(7) 2_576 2_576 ?
C10 Pd1 C12 97.2(7) . 2_576 ?
C12 Pd1 C12 180.0(9) . 2_576 ?

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 C1 C2 C7 16(3) . . . . ?
O4 C1 C2 C7 -165.3(17) . . . . ?
O3 C1 C2 C3 -157.9(17) . . . . ?
O4 C1 C2 C3 21(3) . . . . ?
C7 C2 C3 C4 2(3) . . . . ?
C1 C2 C3 C4 175.2(17) . . . . ?
C2 C3 C4 C5 -4(3) . . . . ?
C3 C4 C5 C6 3(3) . . . . ?
C3 C4 C5 N4 -173.9(18) . . . . ?
C4 C5 C6 C7 -1(3) . . . . ?
N4 C5 C6 C7 175.7(18) . . . . ?
C3 C2 C7 C6 0(3) . . . . ?
C1 C2 C7 C6 -173.6(18) . . . . ?
C5 C6 C7 C2 0(3) . . . . ?
N4 C8 C9 N3 3(2) . . . . ?
N1 C13 C14 N2 1(2) . . . . ?
C20 C15 C16 C17 6(3) . . . . ?
N2 C15 C16 C17 -174.6(16) . . . . ?
C15 C16 C17 C18 -2(3) . . . . ?
C16 C17 C18 C19 -3(3) . . . . ?
C16 C17 C18 C21 177.4(18) . . . . ?
C17 C18 C19 C20 5(3) . . . . ?
C21 C18 C19 C20 -175.4(18) . . . . ?
C18 C19 C20 C15 -2(3) . . . . ?
C16 C15 C20 C19 -4(3) . . . . ?
N2 C15 C20 C19 176.4(18) . . . . ?
C17 C18 C21 O2 -9(3) . . . . ?
C19 C18 C21 O2 171.2(19) . . . . ?
C17 C18 C21 O1 171.1(18) . . . . ?
C19 C18 C21 O1 -8(3) . . . . ?
N2 C12 N1 C13 -1(2) . . . . ?
Pd1 C12 N1 C13 174.8(13) . . . . ?
N2 C12 N1 C11 180.0(15) . . . . ?
Pd1 C12 N1 C11 -4(2) . . . . ?
C14 C13 N1 C12 0(2) . . . . ?
C14 C13 N1 C11 179.4(17) . . . . ?
N3 C11 N1 C12 -47(2) . . . . ?
N3 C11 N1 C13 133.3(18) . . . . ?
C13 C14 N2 C12 -1(2) . . . . ?
C13 C14 N2 C15 177.5(18) . . . . ?
N1 C12 N2 C14 1.0(18) . . . . ?
Pd1 C12 N2 C14 -173.9(14) . . . . ?
N1 C12 N2 C15 -177.5(16) . . . . ?
Pd1 C12 N2 C15 8(3) . . . . ?
C20 C15 N2 C14 36(3) . . . . ?
C16 C15 N2 C14 -143.8(18) . . . . ?
C20 C15 N2 C12 -146.0(18) . . . . ?
C16 C15 N2 C12 34(3) . . . . ?
N4 C10 N3 C9 0(2) . . . . ?
Pd1 C10 N3 C9 -177.1(12) . . . . ?
N4 C10 N3 C11 -176.5(15) . . . . ?
Pd1 C10 N3 C11 6(2) . . . . ?
C8 C9 N3 C10 -2(2) . . . . ?
C8 C9 N3 C11 174.9(17) . . . . ?
N1 C11 N3 C10 47(2) . . . . ?
N1 C11 N3 C9 -129.8(18) . . . . ?
C9 C8 N4 C10 -2(2) . . . . ?
C9 C8 N4 C5 -177.6(18) . . . . ?
N3 C10 N4 C8 1(2) . . . . ?
Pd1 C10 N4 C8 178.4(13) . . . . ?
N3 C10 N4 C5 176.5(16) . . . . ?
Pd1 C10 N4 C5 -6(3) . . . . ?
C6 C5 N4 C8 138.3(19) . . . . ?
C4 C5 N4 C8 -45(3) . . . . ?
C6 C5 N4 C10 -36(3) . . . . ?
C4 C5 N4 C10 141.0(18) . . . . ?
O2 C21 O1 Pb1 -130(3) . . . 1_665 ?
C18 C21 O1 Pb1 49(5) . . . 1_665 ?
O2 C21 O1 Pb1 9.6(19) . . . 2_677 ?
C18 C21 O1 Pb1 -170.9(15) . . . 2_677 ?
O1 C21 O2 Pb1 -9.7(19) . . . 2_677 ?
C18 C21 O2 Pb1 170.8(14) . . . 2_677 ?
O4 C1 O3 Pb1 -23.3(17) . . . . ?
C2 C1 O3 Pb1 155.8(14) . . . . ?
O4 C1 O3 Pb2 86.5(19) . . . . ?
C2 C1 O3 Pb2 -94.3(17) . . . . ?
O3 C1 O4 Pb1 22.1(16) . . . . ?
C2 C1 O4 Pb1 -157.1(14) . . . . ?
O6 C22 O5 Pb2 175.3(17) . . . . ?
C22 C22 O5 Pb2 -16(3) 2_667 . . . ?
O6 C22 O5 Pb1 45(3) . . . . ?
C22 C22 O5 Pb1 -146.9(17) 2_667 . . . ?
O5 C22 O6 Pb2 167.0(17) . . . 2_667 ?
C22 C22 O6 Pb2 -2(3) 2_667 . . 2_667 ?
C1 O3 Pb1 O2 167.9(10) . . . 2_677 ?
Pb2 O3 Pb1 O2 35.6(5) . . . 2_677 ?
C1 O3 Pb1 O1 38.2(11) . . . 1_445 ?
Pb2 O3 Pb1 O1 -94.1(5) . . . 1_445 ?
C1 O3 Pb1 O4 12.3(9) . . . . ?
Pb2 O3 Pb1 O4 -120.0(6) . . . . ?
C1 O3 Pb1 O1 144.8(9) . . . 2_677 ?
Pb2 O3 Pb1 O1 12.5(7) . . . 2_677 ?
C1 O3 Pb1 O5 98.8(10) . . . . ?
Pb2 O3 Pb1 O5 -33.4(4) . . . . ?
C1 O3 Pb1 Br1 -120.2(9) . . . 1_455 ?
Pb2 O3 Pb1 Br1 107.5(4) . . . 1_455 ?
C1 O4 Pb1 O3 -12.1(9) . . . . ?
C1 O4 Pb1 O2 -42.7(11) . . . 2_677 ?
C1 O4 Pb1 O1 -171.9(10) . . . 1_445 ?
C1 O4 Pb1 O1 -109.0(10) . . . 2_677 ?
C1 O4 Pb1 O5 -89.1(10) . . . . ?
C1 O4 Pb1 Br1 41.6(10) . . . 1_455 ?
C22 O5 Pb1 O3 171.7(18) . . . . ?
Pb2 O5 Pb1 O3 32.9(4) . . . . ?
C22 O5 Pb1 O2 82.2(18) . . . 2_677 ?
Pb2 O5 Pb1 O2 -56.7(5) . . . 2_677 ?
C22 O5 Pb1 O1 -52.0(17) . . . 1_445 ?
Pb2 O5 Pb1 O1 169.1(5) . . . 1_445 ?
C22 O5 Pb1 O4 -136.7(18) . . . . ?
Pb2 O5 Pb1 O4 84.4(5) . . . . ?
C22 O5 Pb1 O1 30.6(17) . . . 2_677 ?
Pb2 O5 Pb1 O1 -108.3(5) . . . 2_677 ?
C22 O5 Pb1 Br1 113.1(17) . . . 1_455 ?
Pb2 O5 Pb1 Br1 -25.8(6) . . . 1_455 ?
C1 O3 Pb2 O6 -60.4(16) . . . 2_667 ?
Pb1 O3 Pb2 O6 47.0(8) . . . 2_667 ?
C1 O3 Pb2 O5 -71.8(14) . . . . ?
Pb1 O3 Pb2 O5 35.5(5) . . . . ?
C1 O3 Pb2 Br2 21.3(14) . . . . ?
Pb1 O3 Pb2 Br2 128.7(4) . . . . ?
C1 O3 Pb2 Br1 100.5(14) . . . . ?
Pb1 O3 Pb2 Br1 -152.1(2) . . . . ?
C22 O5 Pb2 O6 12.5(15) . . . 2_667 ?
Pb1 O5 Pb2 O6 157.1(7) . . . 2_667 ?
C22 O5 Pb2 O3 -176.3(16) . . . . ?
Pb1 O5 Pb2 O3 -31.7(4) . . . . ?
C22 O5 Pb2 Br2 96.0(15) . . . . ?
Pb1 O5 Pb2 Br2 -119.4(3) . . . . ?
C22 O5 Pb2 Br1 10.5(18) . . . . ?
Pb1 O5 Pb2 Br1 155.09(18) . . . . ?
Pb1 Br1 Pb2 O6 35.4(4) 1_655 . . 2_667 ?
Pb1 Br1 Pb2 O3 -131.1(5) 1_655 . . . ?
Pb1 Br1 Pb2 O5 37.2(5) 1_655 . . . ?
Pb1 Br1 Pb2 Br2 -50.93(7) 1_655 . . . ?
N3 C10 Pd1 C10 18(100) . . . 2_576 ?
N4 C10 Pd1 C10 -159(100) . . . 2_576 ?
N3 C10 Pd1 C12 -42.1(15) . . . . ?
N4 C10 Pd1 C12 141.1(17) . . . . ?
N3 C10 Pd1 C12 137.9(15) . . . 2_576 ?
N4 C10 Pd1 C12 -38.9(17) . . . 2_576 ?
N1 C12 Pd1 C10 -138.3(15) . . . 2_576 ?
N2 C12 Pd1 C10 35.8(17) . . . 2_576 ?
N1 C12 Pd1 C10 41.7(15) . . . . ?
N2 C12 Pd1 C10 -144.2(17) . . . . ?
N1 C12 Pd1 C12 -50(100) . . . 2_576 ?
N2 C12 Pd1 C12 125(100) . . . 2_576 ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 1.000 1.000 98 44 ' '

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         4.474
_refine_diff_density_min         -3.457
_refine_diff_density_rms         0.446
