# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_148
_database_code_depnum_ccdc_archive 'CCDC 1577216'
_audit_update_record             
;
2017-09-29 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_148                 
;
PROBLEM: Check Calcd Positive Residual Density on    Pb22       6.98 eA-3
RESPONSE: Because of huge electron-number disparity between inorganic bromoplumbate and organic component and anisotropic feature of crystal sample, it resulted in residual density maximum on metal atom location. Both powder X-ray diffraction patterns and elemental analysis data indicate that the space group, structure and formula of compund {(EV)12[Pb18Br54][Pb6.5Br19]}n are right.
;
_vrf_PLAT973_148_2               
;
PROBLEM: Check Calcd Positive Residual Density on    Pb11       3.20 eA-3
RESPONSE: Ibid.
;
_vrf_PLAT973_148_3               
;
PROBLEM: Check Calcd Positive Residual Density on    Pb12       2.42 eA-3
RESPONSE: Ibid.
;
#===================================================================== 

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        {(EV)12[Pb18Br54][Pb6.5Br19]}n
_chemical_name_common            {(EV)12[Pb18Br54][Pb6.5Br19]}n
_chemical_melting_point          ?
_chemical_formula_moiety         '6(Br9 Pb3), Br19 Pb6.50, 12(C14 H18 N2)'
_chemical_formula_sum            'C168 H216 Br73 N24 Pb24.50'
_chemical_formula_weight         13481.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   47.1755(5)
_cell_length_b                   47.1755(5)
_cell_length_c                   11.6900(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     22530.9(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9838
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      Fiber
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.981
_exptl_crystal_F_000             17868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    37.760
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
SuperNova, Dual, Cu at zero, Atlas
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49280
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.748
_diffrn_reflns_theta_max         74.682
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10136
_reflns_number_gt                8145
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0521P)²+558.7437P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10136
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1385
_refine_ls_wR_factor_gt          0.1287
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.004
_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
Pb11 Pb 0.80524(2) 0.66484(2) 0.33297(3) 0.03724(11) Uani 1 1 d . . . . .
Pb12 Pb 0.85368(2) 0.72175(2) 0.67304(3) 0.04113(11) Uani 1 1 d . . . . .
Pb13 Pb 0.79318(2) 0.70973(2) 0.99729(4) 0.04829(12) Uani 1 1 d . . . . .
Br11 Br 0.75161(3) 0.66143(3) 0.19491(10) 0.0513(3) Uani 1 1 d . . . . .
Br12 Br 0.76431(3) 0.60570(3) 0.47567(11) 0.0564(3) Uani 1 1 d . . . . .
Br13 Br 0.85521(3) 0.71662(3) 0.16296(10) 0.0483(3) Uani 1 1 d . . . . .
Br14 Br 0.86106(2) 0.67364(2) 0.49823(9) 0.0445(3) Uani 1 1 d . . . . .
Br15 Br 0.79908(3) 0.71031(3) 0.50055(10) 0.0478(2) Uani 1 1 d . . . . .
Br16 Br 0.90389(3) 0.77746(3) 0.56721(14) 0.0713(4) Uani 1 1 d . . . . .
Br17 Br 0.83200(3) 0.75883(3) 0.80832(10) 0.0540(3) Uani 1 1 d . . . . .
Br18 Br 0.79619(4) 0.76433(3) 1.10315(14) 0.0750(4) Uani 1 1 d . . . . .
Br19 Br 0.73524(3) 0.69100(3) 0.88227(13) 0.0672(3) Uani 1 1 d . . . . .
Pb21 Pb 1.01165(2) 0.95063(2) 0.33537(4) 0.04817(13) Uani 1 1 d . . . . .
Pb22 Pb 1.0000 1.0000 0.0000 0.0269(3) Uani 0.5 6 d S T P . .
Br21 Br 1.01787(4) 0.90192(4) 0.22264(15) 0.0801(4) Uani 1 1 d . . . . .
Br22 Br 1.07011(3) 0.97157(3) 0.47742(12) 0.0588(3) Uani 1 1 d . . . . .
Br23 Br 1.05568(3) 1.00774(3) 0.17417(12) 0.0600(3) Uani 1 1 d . . . . .
Br24 Br 1.0000 1.0000 0.5000 0.0437(5) Uani 1 6 d S T P . .
N11 N 0.7571(2) 0.7936(3) 0.7804(9) 0.059(2) Uani 1 1 d . . . . .
N12 N 0.7111(3) 0.7323(3) 0.2275(9) 0.060(2) Uani 1 1 d . . . . .
N21 N 0.9391(2) 0.8430(2) -0.1054(8) 0.054(2) Uani 1 1 d . . . . .
N22 N 0.8679(2) 0.8190(2) 0.4380(8) 0.055(2) Uani 1 1 d . . . . .
C1 C 0.7487(4) 0.7540(3) 0.6441(13) 0.071(4) Uani 1 1 d . . . . .
H1A H 0.7492 0.7351 0.6256 0.085 Uiso 1 1 calc R U . . .
C2 C 0.7575(4) 0.7668(3) 0.7513(13) 0.072(4) Uani 1 1 d . . . . .
H2A H 0.7640 0.7565 0.8047 0.086 Uiso 1 1 calc R U . . .
C3 C 0.7471(3) 0.8082(3) 0.7047(13) 0.071(4) Uani 1 1 d . . . . .
H3A H 0.7460 0.8265 0.7276 0.085 Uiso 1 1 calc R U . . .
C4 C 0.7386(3) 0.7971(3) 0.5958(11) 0.059(3) Uani 1 1 d . . . . .
H4A H 0.7326 0.8083 0.5444 0.071 Uiso 1 1 calc R U . . .
C5 C 0.7388(3) 0.7686(2) 0.5612(10) 0.048(2) Uani 1 1 d . . . . .
C6 C 0.7298(2) 0.7565(2) 0.4444(10) 0.047(2) Uani 1 1 d . . . . .
C7 C 0.7424(3) 0.7389(3) 0.3923(12) 0.060(3) Uani 1 1 d . . . . .
H7A H 0.7573 0.7351 0.4312 0.072 Uiso 1 1 calc R U . . .
C8 C 0.7330(3) 0.7271(3) 0.2833(12) 0.066(3) Uani 1 1 d . . . . .
H8A H 0.7417 0.7155 0.2481 0.080 Uiso 1 1 calc R U . . .
C9 C 0.6985(3) 0.7495(3) 0.2760(11) 0.061(3) Uani 1 1 d . . . . .
H9A H 0.6834 0.7529 0.2359 0.074 Uiso 1 1 calc R U . . .
C10 C 0.7077(3) 0.7618(3) 0.3822(11) 0.057(3) Uani 1 1 d . . . . .
H10A H 0.6991 0.7739 0.4144 0.068 Uiso 1 1 calc R U . . .
C11 C 0.7682(4) 0.8079(5) 0.8944(13) 0.091(5) Uani 1 1 d . . . . .
H11A H 0.7627 0.7906 0.9495 0.109 Uiso 1 1 calc R U . . .
H11B H 0.7568 0.8194 0.9167 0.109 Uiso 1 1 calc R U . . .
C12 C 0.8036(5) 0.8308(5) 0.8967(17) 0.120(7) Uani 1 1 d . . . . .
H12A H 0.8101 0.8397 0.9722 0.180 Uiso 1 1 calc R U . . .
H12B H 0.8150 0.8194 0.8760 0.180 Uiso 1 1 calc R U . . .
H12C H 0.8090 0.8482 0.8432 0.180 Uiso 1 1 calc R U . . .
C13 C 0.6999(4) 0.7182(4) 0.1097(12) 0.082(4) Uani 1 1 d . . . . .
H13A H 0.6891 0.7288 0.0733 0.098 Uiso 1 1 calc R U . . .
H13B H 0.7187 0.7225 0.0636 0.098 Uiso 1 1 calc R U . . .
C14 C 0.6770(4) 0.6826(4) 0.1157(13) 0.094(5) Uani 1 1 d . . . . .
H14A H 0.6702 0.6741 0.0399 0.141 Uiso 1 1 calc R U . . .
H14B H 0.6878 0.6721 0.1508 0.141 Uiso 1 1 calc R U . . .
H14C H 0.6582 0.6785 0.1604 0.141 Uiso 1 1 calc R U . . .
C21 C 0.8972(3) 0.8104(3) 0.0226(12) 0.080(5) Uani 1 1 d . . . . .
H21A H 0.8779 0.7909 0.0372 0.096 Uiso 1 1 calc R U . . .
C22 C 0.9117(3) 0.8153(4) -0.0824(12) 0.076(4) Uani 1 1 d . . . . .
H22A H 0.9022 0.7991 -0.1381 0.091 Uiso 1 1 calc R U . . .
C23 C 0.9522(3) 0.8664(3) -0.0264(12) 0.071(4) Uani 1 1 d . . . . .
H23A H 0.9709 0.8861 -0.0446 0.085 Uiso 1 1 calc R U . . .
C24 C 0.9391(3) 0.8623(2) 0.0812(11) 0.063(3) Uani 1 1 d . . . . .
H24A H 0.9493 0.8786 0.1361 0.075 Uiso 1 1 calc R U . . .
C25 C 0.9106(2) 0.8337(2) 0.1070(9) 0.044(2) Uani 1 1 d . . . . .
C26 C 0.8965(2) 0.8291(2) 0.2247(10) 0.047(2) Uani 1 1 d . . . . .
C27 C 0.9068(3) 0.8542(3) 0.3030(13) 0.074(4) Uani 1 1 d . . . . .
H27A H 0.9235 0.8751 0.2834 0.089 Uiso 1 1 calc R U . . .
C28 C 0.8927(3) 0.8487(3) 0.4099(12) 0.072(4) Uani 1 1 d . . . . .
H28A H 0.9005 0.8656 0.4629 0.087 Uiso 1 1 calc R U . . .
C29 C 0.8573(4) 0.7944(3) 0.3658(11) 0.073(4) Uani 1 1 d . . . . .
H29A H 0.8405 0.7739 0.3875 0.088 Uiso 1 1 calc R U . . .
C30 C 0.8708(3) 0.7987(2) 0.2593(10) 0.060(3) Uani 1 1 d . . . . .
H30A H 0.8627 0.7811 0.2090 0.072 Uiso 1 1 calc R U . . .
C31 C 0.8521(4) 0.8152(4) 0.5522(12) 0.075(4) Uani 1 1 d . . . . .
H31A H 0.8401 0.7921 0.5724 0.090 Uiso 1 1 calc R U . . .
H31B H 0.8690 0.8265 0.6095 0.090 Uiso 1 1 calc R U . . .
C32 C 0.8293(4) 0.8285(5) 0.5521(14) 0.095(5) Uani 1 1 d . . . . .
H32A H 0.8196 0.8257 0.6265 0.142 Uiso 1 1 calc R U . . .
H32B H 0.8412 0.8514 0.5334 0.142 Uiso 1 1 calc R U . . .
H32C H 0.8123 0.8171 0.4964 0.142 Uiso 1 1 calc R U . . .
C33 C 0.9546(4) 0.8466(4) -0.2189(11) 0.077(4) Uani 1 1 d . . . . .
H33A H 0.9683 0.8697 -0.2362 0.093 Uiso 1 1 calc R U . . .
H33B H 0.9377 0.8371 -0.2770 0.093 Uiso 1 1 calc R U . . .
C34 C 0.9753(4) 0.8300(5) -0.2234(15) 0.104(6) Uani 1 1 d . . . . .
H34A H 0.9849 0.8329 -0.2980 0.156 Uiso 1 1 calc R U . . .
H34B H 0.9924 0.8396 -0.1671 0.156 Uiso 1 1 calc R U . . .
H34C H 0.9617 0.8070 -0.2078 0.156 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
Pb11 Br11 2.9368(11) . ?
Pb11 Br12 2.9845(12) . ?
Pb11 Br15 3.0243(11) . ?
Pb11 Br13 3.0854(11) 13_665 ?
Pb11 Br13 3.1170(12) . ?
Pb11 Br14 3.1219(10) . ?
Pb12 Br16 2.7969(13) . ?
Pb12 Br17 2.8978(12) . ?
Pb12 Br12 3.0609(12) 13_666 ?
Pb12 Br15 3.0989(11) . ?
Pb12 Br14 3.1995(11) . ?
Pb13 Br19 2.7652(13) . ?
Pb13 Br18 2.7966(14) . ?
Pb13 Br17 3.0590(12) . ?
Pb13 Br11 3.1473(13) 1_556 ?
Br11 Pb13 3.1473(13) 1_554 ?
Br12 Pb12 3.0609(12) 13_666 ?
Br13 Pb11 3.0854(11) 13_665 ?
Pb21 Br21 2.7893(14) . ?
Pb21 Br22 2.9351(13) . ?
Pb21 Br22 3.0593(13) 11_566 ?
Pb21 Br23 3.0867(13) . ?
Pb22 Br23 3.1967(13) . ?
Pb22 Br23 3.1967(13) 10_775 ?
Pb22 Br23 3.1967(13) 11_565 ?
Pb22 Br23 3.1967(13) 2_765 ?
Pb22 Br23 3.1967(13) 12_655 ?
Pb22 Br23 3.1967(13) 3_675 ?
Br22 Pb21 3.0593(13) 12_656 ?
N11 C2 1.321(16) . ?
N11 C3 1.342(17) . ?
N11 C11 1.468(18) . ?
N12 C8 1.343(16) . ?
N12 C9 1.345(15) . ?
N12 C13 1.505(18) . ?
N21 C23 1.329(16) . ?
N21 C22 1.329(16) . ?
N21 C33 1.483(16) . ?
N22 C29 1.314(16) . ?
N22 C28 1.343(16) . ?
N22 C31 1.493(16) . ?
C1 C2 1.36(2) . ?
C1 C5 1.397(16) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C4 1.358(19) . ?
C3 H3A 0.9300 . ?
C4 C5 1.409(15) . ?
C4 H4A 0.9300 . ?
C5 C6 1.459(16) . ?
C6 C7 1.379(14) . ?
C6 C10 1.393(15) . ?
C7 C8 1.373(18) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.347(18) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.47(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.48(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C21 C22 1.367(18) . ?
C21 C25 1.374(15) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.372(18) . ?
C23 H23A 0.9300 . ?
C24 C25 1.379(14) . ?
C24 H24A 0.9300 . ?
C25 C26 1.497(16) . ?
C26 C27 1.379(16) . ?
C26 C30 1.397(14) . ?
C27 C28 1.378(19) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
C29 C30 1.366(17) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
C31 C32 1.50(2) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.53(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 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
Br11 Pb11 Br12 96.84(3) . . ?
Br11 Pb11 Br15 90.52(3) . . ?
Br12 Pb11 Br15 93.11(4) . . ?
Br11 Pb11 Br13 91.00(3) . 13_665 ?
Br12 Pb11 Br13 84.93(3) . 13_665 ?
Br15 Pb11 Br13 177.65(3) . 13_665 ?
Br11 Pb11 Br13 89.18(3) . . ?
Br12 Pb11 Br13 166.23(4) . . ?
Br15 Pb11 Br13 99.23(3) . . ?
Br13 Pb11 Br13 82.59(3) 13_665 . ?
Br11 Pb11 Br14 173.55(3) . . ?
Br12 Pb11 Br14 83.50(3) . . ?
Br15 Pb11 Br14 83.03(3) . . ?
Br13 Pb11 Br14 95.44(3) 13_665 . ?
Br13 Pb11 Br14 91.91(3) . . ?
Br16 Pb12 Br17 93.60(4) . . ?
Br16 Pb12 Br12 88.98(4) . 13_666 ?
Br17 Pb12 Br12 92.04(4) . 13_666 ?
Br16 Pb12 Br15 96.63(4) . . ?
Br17 Pb12 Br15 86.94(3) . . ?
Br12 Pb12 Br15 174.35(3) 13_666 . ?
Br16 Pb12 Br14 92.44(4) . . ?
Br17 Pb12 Br14 166.70(3) . . ?
Br12 Pb12 Br14 99.91(3) 13_666 . ?
Br15 Pb12 Br14 80.60(3) . . ?
Br19 Pb13 Br18 95.53(5) . . ?
Br19 Pb13 Br17 90.72(4) . . ?
Br18 Pb13 Br17 83.49(4) . . ?
Br19 Pb13 Br11 88.11(4) . 1_556 ?
Br18 Pb13 Br11 93.92(4) . 1_556 ?
Br17 Pb13 Br11 177.04(3) . 1_556 ?
Pb11 Br11 Pb13 98.97(3) . 1_554 ?
Pb11 Br12 Pb12 101.77(3) . 13_666 ?
Pb11 Br13 Pb11 97.41(3) 13_665 . ?
Pb11 Br14 Pb12 96.08(3) . . ?
Pb11 Br15 Pb12 100.29(3) . . ?
Pb12 Br17 Pb13 101.26(3) . . ?
Br21 Pb21 Br22 94.37(4) . . ?
Br21 Pb21 Br22 89.59(5) . 11_566 ?
Br22 Pb21 Br22 88.331(13) . 11_566 ?
Br21 Pb21 Br23 97.39(5) . . ?
Br22 Pb21 Br23 86.71(4) . . ?
Br22 Pb21 Br23 171.72(4) 11_566 . ?
Br23 Pb22 Br23 180.0 . 10_775 ?
Br23 Pb22 Br23 96.23(3) . 11_565 ?
Br23 Pb22 Br23 83.77(3) 10_775 11_565 ?
Br23 Pb22 Br23 83.77(3) . 2_765 ?
Br23 Pb22 Br23 96.23(3) 10_775 2_765 ?
Br23 Pb22 Br23 180.00(3) 11_565 2_765 ?
Br23 Pb22 Br23 96.23(3) . 12_655 ?
Br23 Pb22 Br23 83.77(3) 10_775 12_655 ?
Br23 Pb22 Br23 83.77(3) 11_565 12_655 ?
Br23 Pb22 Br23 96.23(3) 2_765 12_655 ?
Br23 Pb22 Br23 83.77(3) . 3_675 ?
Br23 Pb22 Br23 96.23(3) 10_775 3_675 ?
Br23 Pb22 Br23 96.23(3) 11_565 3_675 ?
Br23 Pb22 Br23 83.77(3) 2_765 3_675 ?
Br23 Pb22 Br23 180.0 12_655 3_675 ?
Pb21 Br22 Pb21 102.36(4) . 12_656 ?
Pb21 Br23 Pb22 97.66(3) . . ?
C2 N11 C3 120.0(12) . . ?
C2 N11 C11 120.1(12) . . ?
C3 N11 C11 119.9(12) . . ?
C8 N12 C9 121.0(11) . . ?
C8 N12 C13 119.8(11) . . ?
C9 N12 C13 119.2(11) . . ?
C23 N21 C22 119.8(11) . . ?
C23 N21 C33 121.9(11) . . ?
C22 N21 C33 118.3(11) . . ?
C29 N22 C28 120.8(11) . . ?
C29 N22 C31 121.4(11) . . ?
C28 N22 C31 117.8(11) . . ?
C2 C1 C5 121.6(12) . . ?
C2 C1 H1A 119.2 . . ?
C5 C1 H1A 119.2 . . ?
N11 C2 C1 120.8(12) . . ?
N11 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
N11 C3 C4 122.2(11) . . ?
N11 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
C3 C4 C5 119.6(11) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C1 C5 C4 115.8(11) . . ?
C1 C5 C6 124.0(10) . . ?
C4 C5 C6 120.2(10) . . ?
C7 C6 C10 117.6(11) . . ?
C7 C6 C5 121.4(10) . . ?
C10 C6 C5 121.1(9) . . ?
C8 C7 C6 120.4(11) . . ?
C8 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
N12 C8 C7 119.9(11) . . ?
N12 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
N12 C9 C10 120.3(11) . . ?
N12 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C9 C10 C6 120.8(10) . . ?
C9 C10 H10A 119.6 . . ?
C6 C10 H10A 119.6 . . ?
N11 C11 C12 111.6(14) . . ?
N11 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N11 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N12 110.7(11) . . ?
C14 C13 H13A 109.5 . . ?
N12 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
N12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C22 C21 C25 121.2(11) . . ?
C22 C21 H21A 119.4 . . ?
C25 C21 H21A 119.4 . . ?
N21 C22 C21 120.4(12) . . ?
N21 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
N21 C23 C24 122.0(10) . . ?
N21 C23 H23A 119.0 . . ?
C24 C23 H23A 119.0 . . ?
C23 C24 C25 119.3(11) . . ?
C23 C24 H24A 120.4 . . ?
C25 C24 H24A 120.4 . . ?
C21 C25 C24 117.3(11) . . ?
C21 C25 C26 123.4(10) . . ?
C24 C25 C26 119.3(10) . . ?
C27 C26 C30 116.3(11) . . ?
C27 C26 C25 122.9(10) . . ?
C30 C26 C25 120.7(9) . . ?
C28 C27 C26 120.5(11) . . ?
C28 C27 H27A 119.7 . . ?
C26 C27 H27A 119.7 . . ?
N22 C28 C27 120.4(11) . . ?
N22 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?
N22 C29 C30 120.8(11) . . ?
N22 C29 H29A 119.6 . . ?
C30 C29 H29A 119.6 . . ?
C29 C30 C26 121.1(11) . . ?
C29 C30 H30A 119.5 . . ?
C26 C30 H30A 119.5 . . ?
C32 C31 N22 111.6(12) . . ?
C32 C31 H31A 109.3 . . ?
N22 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
N22 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N21 C33 C34 112.2(11) . . ?
N21 C33 H33A 109.2 . . ?
C34 C33 H33A 109.2 . . ?
N21 C33 H33B 109.2 . . ?
C34 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

_refine_diff_density_max         6.754
_refine_diff_density_min         -2.227
_refine_diff_density_rms         0.217

_shelxl_version_number           2014/6

