
#=======================================================================
data_global
#=======================================================================

_audit_creation_method                   'Jana2006 Version : 10/03/2017'



# 2. SUBMISSION DETAILS

_publ_contact_author_name                'Alla Arakcheeva'
_publ_contact_author_address
; EPFL SB IPHYS LPMC
PH L1 490 (Bâtiment PH)
 Station 3
 CH-1015 Lausanne Switzerland
;
_publ_contact_author_email               alla.arakcheeva@epfl.ch
_publ_contact_author_fax                 ?
_publ_contact_author_phone               +41216933371

_publ_contact_letter
; The used crystal of EDPbI4 has been taken after the thermal treatment: 
heating at 423 K for one hour in air followed by cooling.
;

#=======================================================================
data_I
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic
; ?
;
_chemical_name_common                    ?
_chemical_formula_moiety                 'I4 Pb, C2 H10 N2, 0.042(O)'
_chemical_formula_structural             ?
_chemical_formula_analytical             ?
_chemical_formula_iupac                  ?
_chemical_formula_sum                    'C2 H10 I4 N2 O0.042 Pb1'
_chemical_formula_weight                 777.6
_chemical_melting_point                  ?
_chemical_compound_source                ?
_chemical_absolute_configuration         .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting                   trigonal
_symmetry_space_group_name_H-M           'R -3'
_symmetry_space_group_name_Hall          '-R 3'
_symmetry_Int_Tables_number              148

loop_
 _space_group_symop_id
 _space_group_symop_operation_xyz
 1   x,y,z
 2   -y,x-y,z
 3   -x+y,-x,z
 4   -x,-y,-z
 5   y,-x+y,-z
 6   x-y,x,-z
 7   x+2/3,y+1/3,z+1/3
 8   -y+2/3,x-y+1/3,z+1/3
 9   -x+y+2/3,-x+1/3,z+1/3
 10  -x+2/3,-y+1/3,-z+1/3
 11  y+2/3,-x+y+1/3,-z+1/3
 12  x-y+2/3,x+1/3,-z+1/3
 13  x+1/3,y+2/3,z+2/3
 14  -y+1/3,x-y+2/3,z+2/3
 15  -x+y+1/3,-x+2/3,z+2/3
 16  -x+1/3,-y+2/3,-z+2/3
 17  y+1/3,-x+y+2/3,-z+2/3
 18  x-y+1/3,x+2/3,-z+2/3

_cell_length_a                           14.56450(10)
_cell_length_b                           14.56450(10)
_cell_length_c                           32.7195(4)
_cell_angle_alpha                        90
_cell_angle_beta                         90
_cell_angle_gamma                        120
_cell_volume                             6010.75(13)

loop_
 _twin_individual_id
 _twin_individual_mass_fraction_refined
 _twin_individual_twin_matrix_11
 _twin_individual_twin_matrix_12
 _twin_individual_twin_matrix_13
 _twin_individual_twin_matrix_21
 _twin_individual_twin_matrix_22
 _twin_individual_twin_matrix_23
 _twin_individual_twin_matrix_31
 _twin_individual_twin_matrix_32
 _twin_individual_twin_matrix_33
1 0.385(5)
1 0 0
0 1 0
0 0 1
2 0.362(4)
1 -1 0
0 -1 0
0 0 -1
3 0.253(2)
1 -1 0
1 0 0
0 0 1

_cell_formula_units_Z                    18

_cell_measurement_reflns_used            12312
_cell_measurement_theta_min              0.88
_cell_measurement_theta_max              28.83
_cell_measurement_temperature            293
_cell_special_details
; ?
;

_exptl_crystal_density_diffrn            3.8668
_exptl_crystal_F_000                     5946.2

_exptl_absorpt_coefficient_mu            21.793
_exptl_crystal_description               plate
_exptl_crystal_size_max                  0.03
_exptl_crystal_size_mid                  0.02
_exptl_crystal_size_min                  0.003
_exptl_crystal_colour                    'yellow'
_exptl_absorpt_correction_type           'multi-scan'
_exptl_absorpt_correction_T_min          0.619
_exptl_absorpt_correction_T_max          0.936
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

;

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details                   ?

_diffrn_ambient_temperature              293
_diffrn_source                           synchrotron
_diffrn_radiation_type                   synchrotron
_diffrn_radiation_source                 synchrotron
_diffrn_radiation_wavelength             0.7129
_diffrn_radiation_monochromator          synchrotron
_diffrn_measurement_device               'abstract diffractometer'
_diffrn_measurement_device_type          'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_detector                         'PILATUSatSNBL'
_diffrn_detector_area_resol_mean         ?
_diffrn_measurement_method               'ω scans'
_diffrn_measurement_specimen_support     ?

_diffrn_reflns_number                    12312
_diffrn_reflns_theta_min                 1.74
_diffrn_reflns_theta_max                 28.88
_diffrn_reflns_theta_full                28.29
_diffrn_measured_fraction_theta_max      0.86
_diffrn_measured_fraction_theta_full     0.98
_diffrn_reflns_av_R_equivalents          0.0379
_diffrn_reflns_av_unetI/netI             0.0328
_diffrn_reflns_limit_h_min               -18
_diffrn_reflns_limit_h_max               18
_diffrn_reflns_limit_k_min               -16
_diffrn_reflns_limit_k_max               16
_diffrn_reflns_limit_l_min               -43
_diffrn_reflns_limit_l_max               43
_diffrn_reflns_reduction_process         ?

_diffrn_radiation_probe                  X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details
;For the ethylenediammonium cation, a split cation model is used.
Two cation positions with 0.5 occupancy are refined along with
the atomic parameters of N1, N2, C1 and C2 constituting the cation.
;

_reflns_number_total                     2999
_reflns_number_gt                        2450
_reflns_threshold_expression             'I>3σ(I)'

_refine_ls_structure_factor_coef         F
_refine_ls_R_factor_gt                   0.0389
_refine_ls_wR_factor_gt                  0.0467
_refine_ls_R_factor_all                  0.0448
_refine_ls_wR_factor_ref                 0.0480
_refine_ls_goodness_of_fit_ref           1.85
_refine_ls_goodness_of_fit_gt            2.00
_refine_ls_number_reflns                 2999
_refine_ls_number_parameters             222
_refine_ls_number_restraints             0
_refine_ls_number_constraints            0
_refine_ls_weighting_scheme              sigma
_refine_ls_weighting_details             'w=1/(σ²(F)+0.0001F²)'
_refine_ls_hydrogen_treatment            'constr'
_refine_ls_shift/su_max                  0.0482
_refine_ls_shift/su_mean                 0.0069
_refine_diff_density_max                 1.46
_refine_diff_density_min                 -2.44
_refine_ls_extinction_method
 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef               1750(140)

loop_
 _atom_type_symbol
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 C    0.0034  0.0017
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 H    0.0000  0.0000
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 I   -0.4322  1.8508
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 N    0.0067  0.0034
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 O    0.0115  0.0063
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 Pb  -3.4785 10.2492
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection               
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

;
_computing_cell_refinement               
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

;
_computing_data_reduction                ?
_computing_structure_solution            
; 
Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790

;
_computing_structure_refinement          
;
 Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352

;
_computing_molecular_graphics
;
Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3.
Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany.
;

#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_adp_type
 _atom_site_U_iso_or_equiv
 _atom_site_site_symmetry_multiplicity
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
  Pb1 Pb 0 0 0.5 Uani 0.112(2) 3 1 d . . .
  Pb2 Pb 0 0 0 Uani 0.0876(17) 3 1 d . . .
  Pb3 Pb 0 0 0.37529(9) Uani 0.1104(16) 6 1 d . . .
  Pb4 Pb 0 0 0.12547(7) Uani 0.0869(13) 6 1 d . . .
  I1 I 0.3167(3) 0.4846(3) 0.84583(8) Uani 0.110(2) 18 1 d . . .
  I2 I 0.1654(4) 0.1875(4) 0.3214(9) Uani 0.117(2) 18 1 d . . .
  I3 I 0.1882(3) 0.0269(3) 0.44122(9) Uani 0.107(2) 18 1 d . . .
  I4 I 0.1671(4) -0.0168(5) 0.05834(9) Uani 0.128(3) 18 1 d . . .
  N1a N 0.612(2) 0.603(2) 0.6332(5) Uani 0.110(16) 18 0.5 d . . .
  N2a N 0.720(4) 0.635(4) 0.5277(8) Uani 0.095(7) 18 0.5 d . . .
  C1a C 0.622(3) 0.570(3) 0.5938(8) Uani 0.082(9) 18 0.5 d . . .
  C2a C 0.708(3) 0.655(4) 0.5726(8) Uani 0.13(2) 18 0.5 d . . .
  H3n1a H 0.539922 0.586764 0.637352 Uiso 0.1326 18 0.5 d . . .
  H2n1a H 0.630223 0.56717 0.653266 Uiso 0.1326 18 0.5 d . . .
  H1n1a H 0.658378 0.678361 0.635684 Uiso 0.1326 18 0.5 d . . .
  H1n2a H 0.776774 0.698724 0.515886 Uiso 0.1143 18 0.5 d . . .
  H3n2a H 0.6552 0.61624 0.513457 Uiso 0.1143 18 0.5 d . . .
  H1c1a H 0.635012 0.511893 0.596018 Uiso 0.0989 18 0.5 d . . .
  H2c1a H 0.557448 0.547197 0.578798 Uiso 0.0989 18 0.5 d . . .
  H2n2a H 0.735528 0.578949 0.525623 Uiso 0.1143 18 0.5 d . . .
  H1c2a H 0.772836 0.675803 0.586744 Uiso 0.1598 18 0.5 d . . .
  H2c2a H 0.701924 0.718012 0.574935 Uiso 0.1598 18 0.5 d . . .
  N1b N 0.610(4) 0.588(5) 0.6373(9) Uani 0.11(3) 18 0.5 d . . .
  N2b N 0.729(5) 0.658(6) 0.5334(10) Uani 0.095(13) 18 0.5 d . . .
  C1b C 0.629(5) 0.634(5) 0.5982(12) Uani 0.082(14) 18 0.5 d . . .
  C2b C 0.709(4) 0.624(5) 0.5779(10) Uani 0.13(3) 18 0.5 d . . .
  H3n1b H 0.535479 0.53888 0.640595 Uiso 0.1326 18 0.5 d . . .
  H2n1b H 0.632963 0.642054 0.657809 Uiso 0.1326 18 0.5 d . . .
  H1n1b H 0.648483 0.550574 0.640249 Uiso 0.1326 18 0.5 d . . .
  H1n2b H 0.7814 0.643855 0.522073 Uiso 0.1143 18 0.5 d . . .
  H3n2b H 0.66412 0.619801 0.518251 Uiso 0.1143 18 0.5 d . . .
  H1c1b H 0.650699 0.708106 0.600844 Uiso 0.0989 18 0.5 d . . .
  H2c1b H 0.564623 0.60001 0.582446 Uiso 0.0989 18 0.5 d . . .
  H2n2b H 0.753838 0.732806 0.531642 Uiso 0.1143 18 0.5 d . . .
  H1c2b H 0.774602 0.661088 0.592917 Uiso 0.1598 18 0.5 d . . .
  H2c2b H 0.694163 0.551503 0.579996 Uiso 0.1598 18 0.5 d . . .
  O1 O 0.666666 0.333333 0.6236(18) Uiso 0.033(12) 6 0.127(2) d . . .


loop_
 _jana_atom_site_ADP_C_label
 _jana_atom_site_ADP_C_type_symbol
 _jana_atom_site_ADP_C_111
 _jana_atom_site_ADP_C_112
 _jana_atom_site_ADP_C_113
 _jana_atom_site_ADP_C_122
 _jana_atom_site_ADP_C_123
 _jana_atom_site_ADP_C_133
 _jana_atom_site_ADP_C_222
 _jana_atom_site_ADP_C_223
 _jana_atom_site_ADP_C_233
 _jana_atom_site_ADP_C_333
 Pb1 Pb 0 0 0 0 0 0 0 0 0 0
 Pb2 Pb 0 0 0 0 0 0 0 0 0 0
 Pb3 Pb -0.0003(3) -0.0005(4) -0.00059(12) -0.0002(5) -0.00029(6) 0
 0.0003(3) -0.00059(12) 0 0.00022(4)
 Pb4 Pb 0.00029(19) 0.0001(3) -0.00015(6) -0.0002(3) -0.00008(3) 0
 -0.00029(19) -0.00015(6) 0 0.00018(2)
 I1 I 0.0124(11) 0.0051(7) -0.00100(15) 0.0038(7) -0.00001(11) 0.00031(6)
 0.0063(11) 0.00060(14) 0.00040(6) 0.00011(4)
 I2 I 0.0021(14) 0.0064(9) -0.00010(16) 0.0058(9) 0.00053(13) 0.00015(6)
 0.0080(13) 0.00088(16) 0.00029(6) 0.00015(4)
 I3 I 0.0036(7) 0.0038(5) -0.00040(12) 0.0047(5) -0.00021(10) 0.00017(5)
 0.0123(8) -0.00017(14) 0.00020(5) 0.00002(4)
 I4 I 0.0090(15) 0.0073(11) -0.00034(17) 0.0064(12) 0.00003(15) 0.00023(6)
 0.0128(19) -0.0004(2) 0.00031(7) 0.00002(4)

loop_
 _jana_atom_site_ADP_D_label
 _jana_atom_site_ADP_D_type_symbol
 _jana_atom_site_ADP_D_1111
 _jana_atom_site_ADP_D_1112
 _jana_atom_site_ADP_D_1113
 _jana_atom_site_ADP_D_1122
 _jana_atom_site_ADP_D_1123
 _jana_atom_site_ADP_D_1133
 _jana_atom_site_ADP_D_1222
 _jana_atom_site_ADP_D_1223
 _jana_atom_site_ADP_D_1233
 _jana_atom_site_ADP_D_1333
 _jana_atom_site_ADP_D_2222
 _jana_atom_site_ADP_D_2223
 _jana_atom_site_ADP_D_2233
 _jana_atom_site_ADP_D_2333
 _jana_atom_site_ADP_D_3333
 Pb1 Pb 0.0144(10) 0.0072(5) 0.00010(6) 0.0072(5) 0.00028(10) 0.00075(5)
 0.0072(5) 0.00018(12) 0.00037(3) 0 0.0144(10) -0.00010(6) 0.00075(5)
 0 0.00013(2)
 Pb2 Pb 0.0056(6) 0.0028(3) -0.00027(4) 0.0028(3) 0.00001(6) 0.00022(2)
 0.0028(3) 0.00027(8) 0.000110(11) 0 0.0056(6) 0.00027(4) 0.00022(2)
 0 0.000044(10)
 Pb3 Pb 0.0134(8) 0.0067(4) -0.00010(5) 0.0067(4) -0.00011(8) 0.00061(3)
 0.0067(4) -0.00002(9) 0.000303(16) 0 0.0134(8) 0.00010(5) 0.00061(3)
 0 0.000080(12)
 Pb4 Pb 0.0053(4) 0.0027(2) -0.00010(3) 0.0027(2) -0.00006(5) 0.000215(16)
 0.0027(2) 0.00004(6) 0.000108(8) 0 0.0053(4) 0.00010(3) 0.000215(16)
 0 0.000044(7)
 I1 I 0.0065(7) 0.0034(5) -0.00029(14) 0.0040(4) -0.00031(10) 0.00045(4)
 0.0048(5) -0.00043(10) 0.00028(3) -0.000116(18) 0.0098(9) -0.00071(14)
 0.00041(4) -0.000109(17) 0.000072(13)
 I2 I 0.0152(13) 0.0092(8) 0.0004(2) 0.0081(7) 0.00035(14) 0.00060(4)
 0.0077(8) 0.00057(14) 0.00037(3) 0.000032(18) 0.0128(11) 0.00079(20)
 0.00053(4) 0.000071(17) 0.000045(12)
 I3 I 0.0054(7) 0.0017(4) -0.00021(12) 0.0013(3) -0.00011(7) 0.00046(4)
 0.0011(3) -0.00011(7) 0.00013(3) -0.000075(19) 0.0022(5) 0.00003(10)
 0.00026(3) 0.000014(18) 0.000107(16)
 I4 I 0.0159(15) 0.0076(10) -0.0007(2) 0.0069(9) -0.00051(16) 0.00053(4)
 0.0065(11) -0.00039(17) 0.00033(4) -0.000080(19) 0.0143(19) -0.0001(3)
 0.00062(5) 0.00000(2) 0.000079(14)

#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_1
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
  Pb1 I3 . . 3.208(4) ?
  Pb1 I3 . 2_555 3.208(5) ?
  Pb1 I3 . 3_555 3.208(3) ?
  Pb1 I3 . 4_556 3.208(4) ?
  Pb1 I3 . 5_556 3.208(5) ?
  Pb1 I3 . 6_556 3.208(3) ?
  Pb2 I4 . . 3.197(6) ?
  Pb2 I4 . 2_555 3.197(8) ?
  Pb2 I4 . 3_555 3.197(5) ?
  Pb2 I4 . 4_555 3.197(6) ?
  Pb2 I4 . 5_555 3.197(8) ?
  Pb2 I4 . 6_555 3.197(5) ?
  Pb3 I2 . . 3.130(4) ?
  Pb3 I2 . 2_555 3.130(6) ?
  Pb3 I2 . 3_555 3.130(6) ?
  Pb3 I3 . . 3.353(4) ?
  Pb3 I3 . 2_555 3.353(5) ?
  Pb3 I3 . 3_555 3.353(4) ?
  Pb4 I1 . 7_444 3.087(5) ?
  Pb4 I1 . 8_554 3.087(4) ?
  Pb4 I1 . 9_454 3.087(6) ?
  Pb4 I4 . . 3.376(6) ?
  Pb4 I4 . 2_555 3.376(8) ?
  Pb4 I4 . 3_555 3.376(5) ?
  N1a C1a . . 1.41(4) ?
  N1a H3n1a . . 0.96 ?
  N1a H2n1a . . 0.96 ?
  N1a H1n1a . . 0.96 ?
  N2a C2a . . 1.52(4) ?
  N2a H1n2a . . 0.96 ?
  N2a H3n2a . . 0.96 ?
  N2a H2n2a . . 0.96 ?
  C1a C2a . . 1.43(5) ?
  C1a H1c1a . . 0.96 ?
  C1a H2c1a . . 0.96 ?
  C2a H1c2a . . 0.96 ?
  C2a H2c2a . . 0.96 ?
  N1b C1b . . 1.41(6) ?
  N1b H3n1b . . 0.96 ?
  N1b H2n1b . . 0.96 ?
  N1b H1n1b . . 0.96 ?
  N2b C2b . . 1.52(5) ?
  N2b H1n2b . . 0.96 ?
  N2b H3n2b . . 0.96 ?
  N2b H2n2b . . 0.96 ?
  C1b C2b . . 1.43(10) ?
  C1b H1c1b . . 0.96 ?
  C1b H2c1b . . 0.96 ?
  C2b H1c2b . . 0.96 ?
  C2b H2c2b . . 0.96 ?

loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_2
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
  I3 Pb1 I3 . . 2_555 87.76(11) ?
  I3 Pb1 I3 . . 3_555 87.76(10) ?
  I3 Pb1 I3 . . 4_556 180.0(5) ?
  I3 Pb1 I3 . . 5_556 92.25(11) ?
  I3 Pb1 I3 . . 6_556 92.25(10) ?
  I3 Pb1 I3 2_555 . 3_555 87.76(10) ?
  I3 Pb1 I3 2_555 . 4_556 92.24(11) ?
  I3 Pb1 I3 2_555 . 5_556 180.0(5) ?
  I3 Pb1 I3 2_555 . 6_556 92.24(10) ?
  I3 Pb1 I3 3_555 . 4_556 92.24(10) ?
  I3 Pb1 I3 3_555 . 5_556 92.25(10) ?
  I3 Pb1 I3 3_555 . 6_556 180.0(5) ?
  I3 Pb1 I3 4_556 . 5_556 87.75(11) ?
  I3 Pb1 I3 4_556 . 6_556 87.75(10) ?
  I3 Pb1 I3 5_556 . 6_556 87.75(10) ?
  I4 Pb2 I4 . . 2_555 88.00(18) ?
  I4 Pb2 I4 . . 3_555 88.00(16) ?
  I4 Pb2 I4 . . 4_555 180.0(5) ?
  I4 Pb2 I4 . . 5_555 92.00(18) ?
  I4 Pb2 I4 . . 6_555 92.00(16) ?
  I4 Pb2 I4 2_555 . 3_555 88.00(14) ?
  I4 Pb2 I4 2_555 . 4_555 92.00(18) ?
  I4 Pb2 I4 2_555 . 5_555 180.0(5) ?
  I4 Pb2 I4 2_555 . 6_555 92.00(14) ?
  I4 Pb2 I4 3_555 . 4_555 92.00(16) ?
  I4 Pb2 I4 3_555 . 5_555 92.00(14) ?
  I4 Pb2 I4 3_555 . 6_555 180.0(5) ?
  I4 Pb2 I4 4_555 . 5_555 88.00(18) ?
  I4 Pb2 I4 4_555 . 6_555 88.00(16) ?
  I4 Pb2 I4 5_555 . 6_555 88.00(14) ?
  I2 Pb3 I2 . . 2_555 91.32(14) ?
  I2 Pb3 I2 . . 3_555 91.32(14) ?
  I2 Pb3 I3 . . . 91.91(10) ?
  I2 Pb3 I3 . . 2_555 93.44(11) ?
  I2 Pb3 I3 . . 3_555 174.18(12) ?
  I2 Pb3 I2 2_555 . 3_555 91.32(19) ?
  I2 Pb3 I3 2_555 . . 174.18(14) ?
  I2 Pb3 I3 2_555 . 2_555 91.91(14) ?
  I2 Pb3 I3 2_555 . 3_555 93.44(12) ?
  I2 Pb3 I3 3_555 . . 93.44(14) ?
  I2 Pb3 I3 3_555 . 2_555 174.18(14) ?
  I2 Pb3 I3 3_555 . 3_555 91.91(11) ?
  I3 Pb3 I3 . . 2_555 83.07(12) ?
  I3 Pb3 I3 . . 3_555 83.07(11) ?
  I3 Pb3 I3 2_555 . 3_555 83.07(11) ?
  I1 Pb4 I1 7_444 . 8_554 90.82(14) ?
  I1 Pb4 I1 7_444 . 9_454 90.82(14) ?
  I1 Pb4 I4 7_444 . . 93.32(14) ?
  I1 Pb4 I4 7_444 . 2_555 174.11(15) ?
  I1 Pb4 I4 7_444 . 3_555 93.32(12) ?
  I1 Pb4 I1 8_554 . 9_454 90.82(13) ?
  I1 Pb4 I4 8_554 . . 93.32(12) ?
  I1 Pb4 I4 8_554 . 2_555 93.32(14) ?
  I1 Pb4 I4 8_554 . 3_555 174.11(11) ?
  I1 Pb4 I4 9_454 . . 174.11(14) ?
  I1 Pb4 I4 9_454 . 2_555 93.32(16) ?
  I1 Pb4 I4 9_454 . 3_555 93.32(16) ?
  I4 Pb4 I4 . . 2_555 82.26(18) ?
  I4 Pb4 I4 . . 3_555 82.26(16) ?
  I4 Pb4 I4 2_555 . 3_555 82.26(13) ?
  C1a N1a H3n1a . . . 109.47 ?
  C1a N1a H2n1a . . . 109.47 ?
  C1a N1a H1n1a . . . 109.47 ?
  H3n1a N1a H2n1a . . . 109.47 ?
  H3n1a N1a H1n1a . . . 109.47 ?
  H2n1a N1a H1n1a . . . 109.47 ?
  N1a C1a C2a . . . 110(3) ?
  N2a C2a H1c2a . . . 109.47 ?
  N2a C2a H2c2a . . . 109.47 ?
  C1a C2a H1c2a . . . 109.47 ?
  C1a C2a H2c2a . . . 109.47 ?

loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_D
 _geom_hbond_site_symmetry_H
 _geom_hbond_site_symmetry_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_publ_flag
  N1a H3n1a I4 . . 17_555   0.96   2.98   3.83(3)   149.34 ?
  N1a H1n1a I2 . . 4_666   0.96   2.71   3.48(2)   137.65 ?
  N2a H1n2a I3 . . 3_665   0.96   2.83   3.63(3)   141.09 ?
  N2a H3n2a I1 . . 12_556   0.96   2.70   3.58(6)   153.58 ?
  N2a H2n2a I1 . . 14_654   0.96   2.49   3.39(7)   155.73 ?
  N1b H2n1b I2 . . 4_666   0.96   2.82   3.54(4)   132.44 ?
  N1b H2n1b I4 . . 13_555   0.96   2.97   3.61(5)   125.65 ?
  N1b H1n1b I2 . . 7_555   0.96   2.95   3.86(7)   157.92 ?
  N2b H1n2b I1 . . 14_654   0.96   2.76   3.60(10)   146.79 ?
  N2b H3n2b I1 . . 12_556   0.96   2.84   3.62(8)   139.12 ?

#=======================================================================

