 
data_cluster
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'I44 Pb18, (C4 H6 O2)13, (C H6 N)8' 
_chemical_formula_sum
 'C8 H48 I44 N8 Pb18' 
_chemical_formula_weight          9569.56

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'
 'I'  'I'   0.0180   3.1530
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0130   0.0070
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -9.6630   4.2420
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            87
_space_group_name_H-M_alt         'I 4/m'
_space_group_name_Hall            '-I 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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z'
 'y, -x, z'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-y+1/2, x+1/2, z+1/2'
 'y+1/2, -x+1/2, z+1/2'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z'
 '-y, x, -z'
 '-x+1/2, -y+1/2, -z+1/2'
 'x+1/2, y+1/2, -z+1/2'
 'y+1/2, -x+1/2, -z+1/2'
 '-y+1/2, x+1/2, -z+1/2'
 
_cell_length_a                    23.279(3)
_cell_length_b                    23.279(3)
_cell_length_c                    30.804(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      16693(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     600        
_cell_measurement_theta_min       3.4        
_cell_measurement_theta_max       36.0       
                                            
_exptl_crystal_description        prism      
_exptl_crystal_colour             colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.904          
_exptl_crystal_F_000              7920
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.07
_exptl_absorpt_coefficient_mu     14.548
_shelx_estimated_absorpt_T_min    0.324
_shelx_estimated_absorpt_T_max    0.429
_exptl_absorpt_correction_type    'multi-scan'           
_exptl_absorpt_correction_T_min   0.320                  
_exptl_absorpt_correction_T_max   0.420                  
_exptl_absorpt_process_details    'Scala (Evans, 2006)'  
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.96990
_diffrn_radiation_type            synchrotron        
_diffrn_source                    ?                                         
_diffrn_measurement_device_type   'Rayonix SX165 CCD' 
_diffrn_measurement_method        '/f scan'           
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             151283
_diffrn_reflns_av_unetI/netI      0.0835
_diffrn_reflns_av_R_equivalents   0.1660
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        29
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -38
_diffrn_reflns_limit_l_max        38
_diffrn_reflns_theta_min          3.378
_diffrn_reflns_theta_max          38.490
_diffrn_reflns_theta_full         35.587
_diffrn_measured_fraction_theta_max   0.990
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.990
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.990
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              9335
_reflns_number_gt                 5941
_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        'Marccd (Doyle, 2011)'         
_computing_cell_refinement        'iMosflm (Battye et al., 2011)'
_computing_data_reduction         'iMosflm'                      
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'     
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'     
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2015)'    
_computing_publication_material   'SHELXTL'                      
 
_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)+(0.1P)²+200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      difmap
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.000033(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          9335
_refine_ls_number_parameters      127
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.1693
_refine_ls_R_factor_gt            0.1265
_refine_ls_wR_factor_ref          0.3194
_refine_ls_wR_factor_gt           0.2954
_refine_ls_goodness_of_fit_ref    1.440
_refine_ls_restrained_S_all       1.440
_refine_ls_shift/su_max           0.038
_refine_ls_shift/su_mean          0.008
 
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
Pb00 Pb 0.50000(3) 0.35416(3) 0.38960(3) 0.0633(3) Uani 1 1 d . . . . .
Pb1 Pb 0.64604(5) 0.35396(5) 0.5000 0.0633(3) Uani 1 2 d S T P . .
Pb2 Pb 0.5000 0.5000 0.28321(5) 0.0711(5) Uani 1 4 d S T P . .
Pb3 Pb 0.49999(6) 0.21421(5) 0.5000 0.0735(4) Uani 1 2 d S T P . .
I005 I 0.50001(6) 0.36617(6) 0.5000 0.0581(4) Uani 1 2 d S T P . .
I006 I 0.5000 0.5000 0.39747(7) 0.0576(5) Uani 1 4 d S T P . .
I007 I 0.63975(5) 0.36023(5) 0.39427(4) 0.0668(4) Uani 1 1 d . . . . .
I008 I 0.49998(6) 0.22278(5) 0.39397(5) 0.0829(4) Uani 1 1 d . . . . .
I009 I 0.50003(6) 0.36013(6) 0.29019(5) 0.0843(4) Uani 1 1 d . . . . .
I00A I 0.64011(9) 0.22278(8) 0.5000 0.0851(6) Uani 1 2 d S T P . .
I00B I 0.35997(9) 0.22277(8) 0.5000 0.0847(6) Uani 1 2 d S T P . .
I00C I 0.5000 0.5000 0.18656(10) 0.1198(12) Uani 1 4 d S T P . .
I00D I 0.49999(13) 0.08766(9) 0.5000 0.1262(10) Uani 1 2 d S T P . .
N2AA N 0.3401(14) 0.5011(16) 0.1495(11) 0.028(4) Uani 0.25 1 d D . P . .
H2AA H 0.3662 0.4832 0.1322 0.034 Uiso 0.25 1 calc R U P . .
H2AB H 0.3391 0.4835 0.1759 0.034 Uiso 0.25 1 calc R U P . .
H2AC H 0.3502 0.5386 0.1530 0.034 Uiso 0.25 1 calc R U P . .
C0AA C 0.663(5) 0.1295(19) 0.383(3) 0.20(4) Uani 0.25 1 d D . P . .
H0AA H 0.7034 0.1194 0.3764 0.302 Uiso 0.25 1 calc R U P . .
H0AB H 0.6378 0.1093 0.3627 0.302 Uiso 0.25 1 calc R U P . .
H0AC H 0.6542 0.1181 0.4127 0.302 Uiso 0.25 1 calc R U P . .
C39 C 0.337(4) 0.1344(17) 0.380(3) 0.20(4) Uani 0.25 1 d D . P . .
H39A H 0.3601 0.1176 0.3572 0.302 Uiso 0.25 1 calc R U P . .
H39B H 0.2965 0.1228 0.3766 0.302 Uiso 0.25 1 calc R U P . .
H39C H 0.3505 0.1208 0.4086 0.302 Uiso 0.25 1 calc R U P . .
N8 N 0.3408(15) 0.1975(15) 0.3787(11) 0.028(4) Uani 0.25 1 d D . P . .
H8A H 0.3293 0.2100 0.3521 0.034 Uiso 0.25 1 calc R U P . .
H8B H 0.3779 0.2083 0.3834 0.034 Uiso 0.25 1 calc R U P . .
H8C H 0.3179 0.2131 0.3995 0.034 Uiso 0.25 1 calc R U P . .
N7 N 0.6555(15) 0.1918(15) 0.3781(11) 0.028(4) Uani 0.25 1 d D . P . .
H7A H 0.6653 0.2026 0.3507 0.034 Uiso 0.25 1 calc R U P . .
H7B H 0.6783 0.2105 0.3975 0.034 Uiso 0.25 1 calc R U P . .
H7C H 0.6181 0.2010 0.3831 0.034 Uiso 0.25 1 calc R U P . .
N1AA N 0.6535(15) 0.3445(16) 0.2603(10) 0.028(4) Uani 0.25 1 d D . P . .
H1AA H 0.6737 0.3126 0.2681 0.034 Uiso 0.25 1 calc R U P . .
H1AB H 0.6155 0.3386 0.2654 0.034 Uiso 0.25 1 calc R U P . .
H1AC H 0.6660 0.3750 0.2762 0.034 Uiso 0.25 1 calc R U P . .
C15 C 0.662(5) 0.356(4) 0.2141(14) 0.20(4) Uani 0.25 1 d D . P . .
H15A H 0.6469 0.3241 0.1970 0.302 Uiso 0.25 1 calc R U P . .
H15B H 0.7036 0.3600 0.2083 0.302 Uiso 0.25 1 calc R U P . .
H15C H 0.6426 0.3916 0.2061 0.302 Uiso 0.25 1 calc R U P . .
C25 C 0.283(3) 0.498(6) 0.129(4) 0.20(4) Uani 0.25 1 d D . P . .
H25A H 0.2603 0.5320 0.1371 0.302 Uiso 0.25 1 calc R U P . .
H25B H 0.2628 0.4634 0.1394 0.302 Uiso 0.25 1 calc R U P . .
H25C H 0.2869 0.4962 0.0975 0.302 Uiso 0.25 1 calc R U P . .
 
 
_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
Pb00 I008 3.0613(15) . ?
Pb00 I009 3.0654(17) . ?
Pb00 I007 3.2594(14) . ?
Pb00 I007 3.2599(14) 4_565 ?
Pb00 I006 3.4036(9) . ?
Pb00 I005 3.4122(11) . ?
Pb1 I00A 3.057(2) . ?
Pb1 I00B 3.057(2) 3_655 ?
Pb1 I007 3.2634(14) 10_556 ?
Pb1 I007 3.2635(14) . ?
Pb1 I005 3.4112(19) . ?
Pb1 I005 3.4115(19) 3_655 ?
Pb2 I00C 2.977(3) . ?
Pb2 I009 3.2630(14) . ?
Pb2 I009 3.2630(14) 3_655 ?
Pb2 I009 3.2630(14) 2_665 ?
Pb2 I009 3.2630(14) 4_565 ?
Pb3 I00D 2.946(2) . ?
Pb3 I00B 3.266(2) . ?
Pb3 I00A 3.268(2) . ?
Pb3 I008 3.2723(16) . ?
Pb3 I008 3.2723(16) 10_556 ?
I005 Pb1 3.4115(19) 11_566 ?
I005 Pb00 3.4122(11) 10_556 ?
I006 Pb00 3.4036(9) 4_565 ?
I006 Pb00 3.4036(9) 3_655 ?
I006 Pb00 3.4036(9) 2_665 ?
I007 Pb00 3.2598(14) 3_655 ?
I00B Pb1 3.057(2) 11_566 ?
N2AA C25 1.48(2) . ?
N2AA H2AA 0.9100 . ?
N2AA H2AB 0.9100 . ?
N2AA H2AC 0.9100 . ?
C0AA N7 1.47(2) . ?
C0AA H0AA 1.0391 . ?
C0AA H0AB 1.0361 . ?
C0AA H0AC 1.0414 . ?
C39 N8 1.47(2) . ?
C39 H39A 1.1147 . ?
C39 H39B 1.1091 . ?
C39 H39C 1.1040 . ?
N8 H8A 0.9101 . ?
N8 H8B 0.9101 . ?
N8 H8C 0.9101 . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7C 0.9100 . ?
N1AA C15 1.46(2) . ?
N1AA H1AA 0.9100 . ?
N1AA H1AB 0.9100 . ?
N1AA H1AC 0.9100 . ?
C15 H15A 1.1214 . ?
C15 H15B 1.1266 . ?
C15 H15C 1.1152 . ?
C25 H25A 0.9845 . ?
C25 H25B 0.9841 . ?
C25 H25C 0.9846 . ?
 
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
I008 Pb00 I009 95.12(4) . . ?
I008 Pb00 I007 92.38(4) . . ?
I009 Pb00 I007 92.40(4) . . ?
I008 Pb00 I007 92.37(4) . 4_565 ?
I009 Pb00 I007 92.43(4) . 4_565 ?
I007 Pb00 I007 172.90(5) . 4_565 ?
I008 Pb00 I006 173.40(5) . . ?
I009 Pb00 I006 91.48(5) . . ?
I007 Pb00 I006 87.34(3) . . ?
I007 Pb00 I006 87.33(3) 4_565 . ?
I008 Pb00 I005 92.18(4) . . ?
I009 Pb00 I005 172.70(4) . . ?
I007 Pb00 I005 87.27(4) . . ?
I007 Pb00 I005 87.28(4) 4_565 . ?
I006 Pb00 I005 81.22(5) . . ?
I00A Pb1 I00B 95.21(6) . 3_655 ?
I00A Pb1 I007 92.44(3) . 10_556 ?
I00B Pb1 I007 92.45(3) 3_655 10_556 ?
I00A Pb1 I007 92.45(3) . . ?
I00B Pb1 I007 92.45(3) 3_655 . ?
I007 Pb1 I007 172.74(5) 10_556 . ?
I00A Pb1 I005 92.19(5) . . ?
I00B Pb1 I005 172.60(6) 3_655 . ?
I007 Pb1 I005 87.23(3) 10_556 . ?
I007 Pb1 I005 87.23(3) . . ?
I00A Pb1 I005 172.63(6) . 3_655 ?
I00B Pb1 I005 92.16(5) 3_655 3_655 ?
I007 Pb1 I005 87.23(3) 10_556 3_655 ?
I007 Pb1 I005 87.23(3) . 3_655 ?
I005 Pb1 I005 80.44(6) . 3_655 ?
I00C Pb2 I009 93.78(4) . . ?
I00C Pb2 I009 93.78(4) . 3_655 ?
I009 Pb2 I009 89.751(5) . 3_655 ?
I00C Pb2 I009 93.78(4) . 2_665 ?
I009 Pb2 I009 172.44(7) . 2_665 ?
I009 Pb2 I009 89.751(5) 3_655 2_665 ?
I00C Pb2 I009 93.78(4) . 4_565 ?
I009 Pb2 I009 89.751(5) . 4_565 ?
I009 Pb2 I009 172.44(7) 3_655 4_565 ?
I009 Pb2 I009 89.751(5) 2_665 4_565 ?
I00D Pb3 I00B 93.49(7) . . ?
I00D Pb3 I00A 93.50(7) . . ?
I00B Pb3 I00A 173.01(6) . . ?
I00D Pb3 I008 93.49(3) . . ?
I00B Pb3 I008 89.78(3) . . ?
I00A Pb3 I008 89.79(3) . . ?
I00D Pb3 I008 93.49(3) . 10_556 ?
I00B Pb3 I008 89.78(3) . 10_556 ?
I00A Pb3 I008 89.79(3) . 10_556 ?
I008 Pb3 I008 173.01(6) . 10_556 ?
Pb1 I005 Pb1 170.44(6) . 11_566 ?
Pb1 I005 Pb00 89.61(3) . 10_556 ?
Pb1 I005 Pb00 89.61(3) 11_566 10_556 ?
Pb1 I005 Pb00 89.61(3) . . ?
Pb1 I005 Pb00 89.61(3) 11_566 . ?
Pb00 I005 Pb00 170.60(6) 10_556 . ?
Pb00 I006 Pb00 171.84(8) 4_565 3_655 ?
Pb00 I006 Pb00 89.710(6) 4_565 2_665 ?
Pb00 I006 Pb00 89.710(6) 3_655 2_665 ?
Pb00 I006 Pb00 89.710(6) 4_565 . ?
Pb00 I006 Pb00 89.710(6) 3_655 . ?
Pb00 I006 Pb00 171.84(8) 2_665 . ?
Pb00 I007 Pb00 94.86(4) . 3_655 ?
Pb00 I007 Pb1 94.98(4) . . ?
Pb00 I007 Pb1 94.98(4) 3_655 . ?
Pb00 I008 Pb3 96.01(4) . . ?
Pb00 I009 Pb2 96.38(5) . . ?
Pb1 I00A Pb3 96.08(6) . . ?
Pb1 I00B Pb3 96.12(6) 11_566 . ?
C25 N2AA H2AA 109.6 . . ?
C25 N2AA H2AB 109.9 . . ?
H2AA N2AA H2AB 109.5 . . ?
C25 N2AA H2AC 108.9 . . ?
H2AA N2AA H2AC 109.5 . . ?
H2AB N2AA H2AC 109.5 . . ?
N7 C0AA H0AA 115.6 . . ?
N7 C0AA H0AB 114.9 . . ?
H0AA C0AA H0AB 102.8 . . ?
N7 C0AA H0AC 116.1 . . ?
H0AA C0AA H0AC 102.6 . . ?
H0AB C0AA H0AC 103.0 . . ?
N8 C39 H39A 123.4 . . ?
N8 C39 H39B 122.8 . . ?
H39A C39 H39B 93.0 . . ?
N8 C39 H39C 122.2 . . ?
H39A C39 H39C 93.7 . . ?
H39B C39 H39C 93.5 . . ?
C39 N8 H8A 110.0 . . ?
C39 N8 H8B 109.1 . . ?
H8A N8 H8B 109.5 . . ?
C39 N8 H8C 109.4 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C0AA N7 H7A 109.9 . . ?
C0AA N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C0AA N7 H7C 109.0 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C15 N1AA H1AA 110.0 . . ?
C15 N1AA H1AB 109.3 . . ?
H1AA N1AA H1AB 109.5 . . ?
C15 N1AA H1AC 109.2 . . ?
H1AA N1AA H1AC 109.5 . . ?
H1AB N1AA H1AC 109.5 . . ?
N1AA C15 H15A 124.3 . . ?
N1AA C15 H15B 124.8 . . ?
H15A C15 H15B 91.0 . . ?
N1AA C15 H15C 123.6 . . ?
H15A C15 H15C 91.6 . . ?
H15B C15 H15C 91.8 . . ?
N2AA C25 H25A 110.2 . . ?
N2AA C25 H25B 109.3 . . ?
H25A C25 H25B 109.1 . . ?
N2AA C25 H25C 110.3 . . ?
H25A C25 H25C 109.0 . . ?
H25B C25 H25C 108.9 . . ?
 
_refine_diff_density_max    7.388
_refine_diff_density_min   -2.683
_refine_diff_density_rms    0.523

_shelxl_version_number 2013-4



