# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1519640'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H21 Bi2 I9 N6 O0'
_chemical_formula_weight         1881.47

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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.485(3)
_cell_length_b                   13.080(3)
_cell_length_c                   23.566(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3848.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31620
_cell_measurement_theta_min      3.025
_cell_measurement_theta_max      27.53

_exptl_crystal_description       COLUMNAR
_exptl_crystal_colour            RED
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3256
_exptl_absorpt_coefficient_mu    16.371
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_T_max  0.140
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            37053
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8789
_reflns_number_gt                7164
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0028P)²+0.0782P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_number_reflns         8789
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0705
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.30700(3) 0.04210(3) -0.305729(16) 0.03819(10) Uani 1 1 d . . .
Bi2 Bi 0.57998(3) -0.01221(3) -0.407834(17) 0.03759(10) Uani 1 1 d . . .
I1 I 0.11459(6) 0.16282(7) -0.35470(4) 0.0706(3) Uani 1 1 d . . .
I2 I 0.16479(7) -0.11528(7) -0.25303(4) 0.0656(2) Uani 1 1 d . . .
I3 I 0.32617(7) 0.15306(7) -0.20119(3) 0.0680(2) Uani 1 1 d . . .
I4 I 0.50948(6) -0.08675(7) -0.28054(3) 0.0583(2) Uani 1 1 d . . .
I5 I 0.32977(5) -0.07871(7) -0.43164(3) 0.0546(2) Uani 1 1 d . . .
I6 I 0.47849(6) 0.19668(6) -0.35923(4) 0.0561(2) Uani 1 1 d . . .
I7 I 0.79131(6) 0.05283(7) -0.37012(4) 0.0620(2) Uani 1 1 d . . .
I8 I 0.65471(5) -0.21470(6) -0.44697(3) 0.04873(19) Uani 1 1 d . . .
I9 I 0.61012(6) 0.07560(7) -0.52378(3) 0.0558(2) Uani 1 1 d . . .
N1 N 0.7740(7) -0.0066(9) -0.1953(4) 0.063(3) Uani 1 1 d . . .
N2 N 0.5533(6) 0.2922(7) 0.0984(4) 0.046(2) Uani 1 1 d . . .
N3 N 0.1987(6) -0.1996(6) -0.0376(4) 0.042(2) Uani 1 1 d . . .
N4 N 0.6601(6) 0.0396(7) -0.1337(4) 0.048(2) Uani 1 1 d . . .
N5 N 0.5311(6) 0.1524(6) 0.0514(3) 0.0368(19) Uani 1 1 d . . .
N6 N 0.3334(6) -0.1001(6) -0.0560(4) 0.041(2) Uani 1 1 d . . .
C1 C 0.6893(13) 0.1256(11) -0.1608(6) 0.096(5) Uani 1 1 d . . .
H1A H 0.6645 0.1914 -0.1537 0.116 Uiso 1 1 calc R . .
C2 C 0.7633(12) 0.0970(11) -0.2013(6) 0.085(5) Uani 1 1 d . . .
H2A H 0.7983 0.1391 -0.2271 0.102 Uiso 1 1 calc R . .
C3 C 0.7094(7) -0.0420(9) -0.1554(4) 0.050(3) Uani 1 1 d . . .
H3A H 0.7003 -0.1098 -0.1446 0.060 Uiso 1 1 calc R . .
C4 C 0.5634(8) 0.2500(8) 0.0477(5) 0.044(3) Uani 1 1 d . . .
H4A H 0.5886 0.2822 0.0152 0.053 Uiso 1 1 calc R . .
C5 C 0.5105(8) 0.2231(9) 0.1344(5) 0.054(3) Uani 1 1 d . . .
H5A H 0.4925 0.2348 0.1722 0.065 Uiso 1 1 calc R . .
C6 C 0.4984(9) 0.1352(9) 0.1066(5) 0.055(3) Uani 1 1 d . . .
H6A H 0.4728 0.0741 0.1215 0.067 Uiso 1 1 calc R . .
C7 C 0.2740(8) -0.1131(8) -0.1051(5) 0.046(3) Uani 1 1 d . . .
H7A H 0.2890 -0.0841 -0.1403 0.056 Uiso 1 1 calc R . .
C8 C 0.2852(8) -0.1543(8) -0.0157(5) 0.047(3) Uani 1 1 d . . .
H8A H 0.3081 -0.1597 0.0217 0.057 Uiso 1 1 calc R . .
C9 C 0.1911(8) -0.1748(9) -0.0931(5) 0.052(3) Uani 1 1 d . . .
H9A H 0.1384 -0.1965 -0.1183 0.062 Uiso 1 1 calc R . .
C10 C 0.4354(7) 0.0191(8) -0.0013(4) 0.038(2) Uani 1 1 d . . .
H10A H 0.3853 0.0130 0.0278 0.046 Uiso 1 1 calc R . .
C11 C 0.5229(7) 0.0869(8) 0.0041(4) 0.036(2) Uani 1 1 d . . .
C12 C 0.6000(8) 0.0936(8) -0.0388(4) 0.043(2) Uani 1 1 d . . .
H12A H 0.6600 0.1352 -0.0351 0.051 Uiso 1 1 calc R . .
C13 C 0.5830(8) 0.0347(7) -0.0879(5) 0.046(3) Uani 1 1 d . . .
C14 C 0.4952(7) -0.0301(8) -0.0919(4) 0.042(2) Uani 1 1 d . . .
H14A H 0.4850 -0.0689 -0.1246 0.051 Uiso 1 1 calc R . .
C15 C 0.4254(7) -0.0369(8) -0.0493(4) 0.038(2) Uani 1 1 d . . .
C16 C 0.8443(11) -0.0782(13) -0.2308(6) 0.104(6) Uani 1 1 d . . .
H16A H 0.8289 -0.1479 -0.2210 0.156 Uiso 1 1 calc R . .
H16B H 0.9184 -0.0639 -0.2233 0.156 Uiso 1 1 calc R . .
H16C H 0.8297 -0.0676 -0.2703 0.156 Uiso 1 1 calc R . .
C17 C 0.5793(10) 0.4011(10) 0.1122(5) 0.068(4) Uani 1 1 d . . .
H17A H 0.6089 0.4339 0.0793 0.103 Uiso 1 1 calc R . .
H17B H 0.6304 0.4032 0.1426 0.103 Uiso 1 1 calc R . .
H17C H 0.5151 0.4361 0.1235 0.103 Uiso 1 1 calc R . .
C18 C 0.1258(8) -0.2719(10) -0.0071(5) 0.065(4) Uani 1 1 d . . .
H18A H 0.0688 -0.2923 -0.0320 0.098 Uiso 1 1 calc R . .
H18B H 0.0962 -0.2386 0.0257 0.098 Uiso 1 1 calc R . .
H18C H 0.1655 -0.3311 0.0046 0.098 Uiso 1 1 calc R . .


_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
Bi1 I3 2.8692(10) . ?
Bi1 I2 2.9887(10) . ?
Bi1 I4 3.0958(9) . ?
Bi1 I1 3.0977(9) . ?
Bi1 I6 3.2035(9) . ?
Bi1 I5 3.3736(10) . ?
Bi2 I7 2.9113(9) . ?
Bi2 I8 2.9556(10) . ?
Bi2 I9 2.9878(10) . ?
Bi2 I6 3.2222(10) . ?
Bi2 I4 3.2748(10) . ?
Bi2 I5 3.2909(9) . ?
N1 C3 1.323(12) . ?
N1 C2 1.370(16) . ?
N1 C16 1.531(15) . ?
N2 C4 1.322(13) . ?
N2 C5 1.351(13) . ?
N2 C17 1.497(14) . ?
N3 C8 1.336(12) . ?
N3 C9 1.352(13) . ?
N3 C18 1.496(13) . ?
N4 C3 1.334(14) . ?
N4 C1 1.344(15) . ?
N4 C13 1.447(12) . ?
N5 C4 1.342(12) . ?
N5 C6 1.382(12) . ?
N5 C11 1.410(12) . ?
N6 C8 1.329(12) . ?
N6 C7 1.385(12) . ?
N6 C15 1.425(12) . ?
C1 C2 1.379(17) . ?
C5 C6 1.331(15) . ?
C7 C9 1.343(13) . ?
C10 C15 1.354(13) . ?
C10 C11 1.414(13) . ?
C11 C12 1.398(13) . ?
C12 C13 1.406(14) . ?
C13 C14 1.389(13) . ?
C14 C15 1.333(13) . ?

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
I3 Bi1 I2 92.36(3) . . ?
I3 Bi1 I4 92.44(3) . . ?
I2 Bi1 I4 91.75(3) . . ?
I3 Bi1 I1 97.28(3) . . ?
I2 Bi1 I1 92.59(3) . . ?
I4 Bi1 I1 169.18(3) . . ?
I3 Bi1 I6 87.88(3) . . ?
I2 Bi1 I6 174.47(3) . . ?
I4 Bi1 I6 82.72(3) . . ?
I1 Bi1 I6 92.86(3) . . ?
I3 Bi1 I5 170.07(2) . . ?
I2 Bi1 I5 95.33(3) . . ?
I4 Bi1 I5 81.07(2) . . ?
I1 Bi1 I5 88.65(2) . . ?
I6 Bi1 I5 83.86(2) . . ?
I7 Bi2 I8 94.07(3) . . ?
I7 Bi2 I9 93.02(3) . . ?
I8 Bi2 I9 91.11(3) . . ?
I7 Bi2 I6 90.00(3) . . ?
I8 Bi2 I6 174.21(2) . . ?
I9 Bi2 I6 92.79(3) . . ?
I7 Bi2 I4 92.92(3) . . ?
I8 Bi2 I4 95.96(3) . . ?
I9 Bi2 I4 170.42(2) . . ?
I6 Bi2 I4 79.70(2) . . ?
I7 Bi2 I5 171.73(3) . . ?
I8 Bi2 I5 90.55(2) . . ?
I9 Bi2 I5 93.74(2) . . ?
I6 Bi2 I5 84.92(2) . . ?
I4 Bi2 I5 79.77(2) . . ?
Bi1 I4 Bi2 83.21(2) . . ?
Bi2 I5 Bi1 78.832(18) . . ?
Bi1 I6 Bi2 82.39(2) . . ?
C3 N1 C2 111.1(10) . . ?
C3 N1 C16 121.6(12) . . ?
C2 N1 C16 127.2(11) . . ?
C4 N2 C5 109.0(10) . . ?
C4 N2 C17 125.0(10) . . ?
C5 N2 C17 125.9(10) . . ?
C8 N3 C9 108.9(9) . . ?
C8 N3 C18 126.0(10) . . ?
C9 N3 C18 125.0(9) . . ?
C3 N4 C1 111.3(10) . . ?
C3 N4 C13 123.8(9) . . ?
C1 N4 C13 124.9(11) . . ?
C4 N5 C6 107.7(9) . . ?
C4 N5 C11 123.2(9) . . ?
C6 N5 C11 128.7(9) . . ?
C8 N6 C7 106.8(8) . . ?
C8 N6 C15 126.5(9) . . ?
C7 N6 C15 126.6(8) . . ?
N4 C1 C2 106.4(13) . . ?
N1 C2 C1 105.3(11) . . ?
N1 C3 N4 105.9(11) . . ?
N2 C4 N5 108.1(9) . . ?
C6 C5 N2 108.3(11) . . ?
C5 C6 N5 106.8(10) . . ?
C9 C7 N6 108.1(9) . . ?
N6 C8 N3 109.1(10) . . ?
C7 C9 N3 107.0(10) . . ?
C15 C10 C11 119.0(9) . . ?
C12 C11 N5 119.0(9) . . ?
C12 C11 C10 120.5(9) . . ?
N5 C11 C10 120.5(8) . . ?
C11 C12 C13 117.2(9) . . ?
C14 C13 C12 120.6(9) . . ?
C14 C13 N4 120.1(10) . . ?
C12 C13 N4 119.3(9) . . ?
C15 C14 C13 120.4(10) . . ?
C14 C15 C10 122.3(10) . . ?
C14 C15 N6 118.8(9) . . ?
C10 C15 N6 118.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.173
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1519638'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H42 Ag6 Br0 I12 N12 O0'
_chemical_formula_weight         2812.84

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.2094(3)
_cell_length_b                   13.2371(4)
_cell_length_c                   21.8384(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.965(2)
_cell_angle_gamma                90.00
_cell_volume                     3236.04(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5158
_cell_measurement_theta_min      2.3831
_cell_measurement_theta_max      24.9483

_exptl_crystal_description       columnar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2520
_exptl_absorpt_coefficient_mu    7.540
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            18068
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5716
_reflns_number_gt                4102
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0367P)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         5716
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0810
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 1.08779(7) 0.37977(6) 0.03040(3) 0.0709(2) Uani 1 1 d . . .
Ag2 Ag 1.23415(6) 0.20656(6) 0.09731(3) 0.0730(2) Uani 1 1 d . . .
Ag3 Ag 1.20583(7) 0.46207(6) 0.15094(3) 0.0682(2) Uani 1 1 d . . .
I1 I 1.01297(5) 0.18020(4) 0.02970(2) 0.05954(17) Uani 1 1 d . . .
I2 I 1.38471(5) 0.04264(4) 0.10784(3) 0.06478(18) Uani 1 1 d . . .
I3 I 1.14394(4) 0.28014(4) 0.20930(2) 0.04805(14) Uani 1 1 d . . .
I4 I 1.35254(4) 0.39945(4) 0.04888(2) 0.05088(15) Uani 1 1 d . . .
I5 I 1.29514(5) 0.59989(4) 0.23743(2) 0.05254(15) Uani 1 1 d . . .
I6 I 0.98629(4) 0.54749(4) 0.09396(2) 0.04570(14) Uani 1 1 d . . .
N1 N 0.7004(5) 0.2624(5) -0.0058(2) 0.0396(14) Uani 1 1 d . . .
N2 N 1.0509(5) 0.4272(5) 0.3506(3) 0.0423(15) Uani 1 1 d . . .
N3 N 0.5542(5) 0.7788(5) 0.2106(3) 0.0481(16) Uani 1 1 d . . .
N4 N 0.7088(5) 0.3164(4) 0.0865(2) 0.0352(13) Uani 1 1 d . . .
N5 N 0.9062(5) 0.4074(4) 0.2831(2) 0.0353(13) Uani 1 1 d . . .
N6 N 0.6356(5) 0.6416(4) 0.1793(3) 0.0375(14) Uani 1 1 d . . .
C1 C 0.7281(6) 0.3856(5) 0.1372(3) 0.0346(16) Uani 1 1 d . . .
C2 C 0.8046(6) 0.3593(5) 0.1861(3) 0.0328(16) Uani 1 1 d . . .
H2A H 0.8429 0.2970 0.1876 0.039 Uiso 1 1 calc R . .
C3 C 0.8225(5) 0.4292(5) 0.2331(3) 0.0326(15) Uani 1 1 d . . .
C4 C 0.7658(6) 0.5204(5) 0.2314(3) 0.0388(17) Uani 1 1 d . . .
H4A H 0.7775 0.5660 0.2636 0.047 Uiso 1 1 calc R . .
C5 C 0.6905(6) 0.5441(5) 0.1813(3) 0.0358(16) Uani 1 1 d . . .
C6 C 0.6687(6) 0.4772(5) 0.1341(3) 0.0360(16) Uani 1 1 d . . .
H6A H 0.6159 0.4929 0.1012 0.043 Uiso 1 1 calc R . .
C7 C 0.7311(6) 0.3398(6) 0.0289(3) 0.0396(17) Uani 1 1 d . . .
H7A H 0.7628 0.4004 0.0156 0.048 Uiso 1 1 calc R . .
C8 C 0.6639(7) 0.2205(5) 0.0875(3) 0.0446(18) Uani 1 1 d . . .
H8A H 0.6414 0.1852 0.1219 0.054 Uiso 1 1 calc R . .
C9 C 0.6584(7) 0.1868(6) 0.0296(3) 0.051(2) Uani 1 1 d . . .
H9A H 0.6311 0.1239 0.0161 0.061 Uiso 1 1 calc R . .
C10 C 0.9883(6) 0.4724(6) 0.3056(3) 0.0408(17) Uani 1 1 d . . .
H10A H 0.9994 0.5381 0.2919 0.049 Uiso 1 1 calc R . .
C11 C 1.0097(7) 0.3313(6) 0.3576(3) 0.0464(19) Uani 1 1 d . . .
H11A H 1.0388 0.2840 0.3861 0.056 Uiso 1 1 calc R . .
C12 C 0.9187(7) 0.3178(6) 0.3154(3) 0.0435(18) Uani 1 1 d . . .
H12A H 0.8733 0.2595 0.3093 0.052 Uiso 1 1 calc R . .
C13 C 0.5903(6) 0.6867(5) 0.2271(4) 0.0412(18) Uani 1 1 d . . .
H13A H 0.5846 0.6584 0.2658 0.049 Uiso 1 1 calc R . .
C14 C 0.5775(7) 0.7924(6) 0.1498(4) 0.056(2) Uani 1 1 d . . .
H14A H 0.5607 0.8500 0.1266 0.068 Uiso 1 1 calc R . .
C15 C 0.6286(7) 0.7081(6) 0.1303(4) 0.051(2) Uani 1 1 d . . .
H15A H 0.6546 0.6962 0.0912 0.061 Uiso 1 1 calc R . .
C16 C 0.7179(8) 0.2555(7) -0.0723(3) 0.067(3) Uani 1 1 d . . .
H16A H 0.7482 0.3186 -0.0867 0.100 Uiso 1 1 calc R . .
H16B H 0.6430 0.2408 -0.0937 0.100 Uiso 1 1 calc R . .
H16C H 0.7740 0.2026 -0.0798 0.100 Uiso 1 1 calc R . .
C17 C 1.1542(7) 0.4708(7) 0.3860(4) 0.061(2) Uani 1 1 d . . .
H17A H 1.1660 0.5393 0.3732 0.092 Uiso 1 1 calc R . .
H17B H 1.2244 0.4319 0.3789 0.092 Uiso 1 1 calc R . .
H17C H 1.1394 0.4696 0.4289 0.092 Uiso 1 1 calc R . .
C18 C 0.4996(7) 0.8534(6) 0.2513(4) 0.064(2) Uani 1 1 d . . .
H18A H 0.4940 0.8248 0.2914 0.096 Uiso 1 1 calc R . .
H18B H 0.4211 0.8707 0.2348 0.096 Uiso 1 1 calc R . .
H18C H 0.5483 0.9131 0.2539 0.096 Uiso 1 1 calc R . .


_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
Ag1 I1 2.7714(9) . ?
Ag1 I6 2.8833(9) . ?
Ag1 I6 2.9597(9) 3_765 ?
Ag1 I4 2.9856(9) . ?
Ag1 Ag3 3.0833(10) . ?
Ag1 Ag2 3.1361(10) . ?
Ag2 I2 2.7512(9) . ?
Ag2 I1 2.8408(9) . ?
Ag2 I3 2.8651(9) . ?
Ag2 I4 3.0893(10) . ?
Ag3 I5 2.7753(8) . ?
Ag3 I3 2.8278(9) . ?
Ag3 I6 2.9268(8) . ?
Ag3 I4 2.9562(9) . ?
I6 Ag1 2.9597(9) 3_765 ?
N1 C7 1.309(8) . ?
N1 C9 1.364(9) . ?
N1 C16 1.480(9) . ?
N2 C10 1.322(8) . ?
N2 C11 1.363(9) . ?
N2 C17 1.475(9) . ?
N3 C13 1.329(9) . ?
N3 C14 1.377(10) . ?
N3 C18 1.482(9) . ?
N4 C7 1.333(8) . ?
N4 C8 1.368(8) . ?
N4 C1 1.444(8) . ?
N5 C10 1.335(8) . ?
N5 C12 1.384(9) . ?
N5 C3 1.432(8) . ?
N6 C13 1.326(8) . ?
N6 C15 1.384(9) . ?
N6 C5 1.430(8) . ?
C1 C2 1.380(9) . ?
C1 C6 1.383(9) . ?
C2 C3 1.388(9) . ?
C3 C4 1.364(9) . ?
C4 C5 1.383(9) . ?
C5 C6 1.370(9) . ?
C8 C9 1.339(10) . ?
C11 C12 1.350(10) . ?
C14 C15 1.335(10) . ?

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 Ag1 I6 127.58(3) . . ?
I1 Ag1 I6 103.57(3) . 3_765 ?
I6 Ag1 I6 95.30(2) . 3_765 ?
I1 Ag1 I4 112.48(3) . . ?
I6 Ag1 I4 106.38(3) . . ?
I6 Ag1 I4 108.99(3) 3_765 . ?
I1 Ag1 Ag3 117.25(3) . . ?
I6 Ag1 Ag3 58.64(2) . . ?
I6 Ag1 Ag3 139.12(3) 3_765 . ?
I4 Ag1 Ag3 58.27(2) . . ?
I1 Ag1 Ag2 57.08(2) . . ?
I6 Ag1 Ag2 123.27(3) . . ?
I6 Ag1 Ag2 141.31(3) 3_765 . ?
I4 Ag1 Ag2 60.56(2) . . ?
Ag3 Ag1 Ag2 70.70(2) . . ?
I2 Ag2 I1 117.50(3) . . ?
I2 Ag2 I3 116.03(3) . . ?
I1 Ag2 I3 98.53(3) . . ?
I2 Ag2 I4 114.08(3) . . ?
I1 Ag2 I4 107.60(3) . . ?
I3 Ag2 I4 100.84(3) . . ?
I2 Ag2 Ag1 156.84(3) . . ?
I1 Ag2 Ag1 54.98(2) . . ?
I3 Ag2 Ag1 87.13(3) . . ?
I4 Ag2 Ag1 57.31(2) . . ?
I5 Ag3 I3 109.96(3) . . ?
I5 Ag3 I6 107.53(3) . . ?
I3 Ag3 I6 107.47(3) . . ?
I5 Ag3 I4 120.15(3) . . ?
I3 Ag3 I4 105.07(3) . . ?
I6 Ag3 I4 106.03(2) . . ?
I5 Ag3 Ag1 159.56(3) . . ?
I3 Ag3 Ag1 88.82(3) . . ?
I6 Ag3 Ag1 57.27(2) . . ?
I4 Ag3 Ag1 59.21(2) . . ?
Ag1 I1 Ag2 67.93(2) . . ?
Ag3 I3 Ag2 78.41(3) . . ?
Ag3 I4 Ag1 62.52(2) . . ?
Ag3 I4 Ag2 73.02(2) . . ?
Ag1 I4 Ag2 62.13(2) . . ?
Ag1 I6 Ag3 64.10(2) . . ?
Ag1 I6 Ag1 84.70(2) . 3_765 ?
Ag3 I6 Ag1 134.88(3) . 3_765 ?
C7 N1 C9 109.6(6) . . ?
C7 N1 C16 124.9(6) . . ?
C9 N1 C16 125.4(6) . . ?
C10 N2 C11 109.6(6) . . ?
C10 N2 C17 125.8(7) . . ?
C11 N2 C17 124.5(6) . . ?
C13 N3 C14 108.2(7) . . ?
C13 N3 C18 125.3(7) . . ?
C14 N3 C18 126.5(7) . . ?
C7 N4 C8 108.6(6) . . ?
C7 N4 C1 123.3(6) . . ?
C8 N4 C1 128.1(6) . . ?
C10 N5 C12 108.4(6) . . ?
C10 N5 C3 124.2(6) . . ?
C12 N5 C3 127.4(6) . . ?
C13 N6 C15 108.3(6) . . ?
C13 N6 C5 124.4(6) . . ?
C15 N6 C5 127.2(6) . . ?
C2 C1 C6 122.5(6) . . ?
C2 C1 N4 119.7(6) . . ?
C6 C1 N4 117.8(6) . . ?
C1 C2 C3 117.7(6) . . ?
C4 C3 C2 121.4(6) . . ?
C4 C3 N5 119.0(6) . . ?
C2 C3 N5 119.5(6) . . ?
C3 C4 C5 119.0(6) . . ?
C6 C5 C4 121.8(6) . . ?
C6 C5 N6 120.0(6) . . ?
C4 C5 N6 118.2(6) . . ?
C5 C6 C1 117.5(6) . . ?
N1 C7 N4 107.9(6) . . ?
C9 C8 N4 107.0(6) . . ?
C8 C9 N1 106.9(7) . . ?
N2 C10 N5 108.1(6) . . ?
C12 C11 N2 107.2(7) . . ?
C11 C12 N5 106.7(7) . . ?
N6 C13 N3 108.8(7) . . ?
C15 C14 N3 107.7(7) . . ?
C14 C15 N6 107.0(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.162
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1519639'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H46 I12 N12 O2 Pb3'
_chemical_formula_weight         2823.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.496(3)
_cell_length_b                   20.569(4)
_cell_length_c                   12.634(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.16(3)
_cell_angle_gamma                90.00
_cell_volume                     3196.3(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22282
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      27.56

_exptl_crystal_description       columnar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2488
_exptl_absorpt_coefficient_mu    13.716
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_T_max  0.254
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            30245
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7292
_reflns_number_gt                5113
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0160P)²+10.7798P] 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         7292
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.19558(3) 0.102288(18) 0.32159(3) 0.03711(10) Uani 1 1 d . . .
Pb2 Pb 0.0000 0.0000 0.5000 0.04275(15) Uani 1 2 d S . .
I1 I 0.26427(7) 0.03539(3) 0.12896(6) 0.0544(2) Uani 1 1 d . . .
I2 I 0.42976(6) 0.17308(3) 0.36829(5) 0.04693(18) Uani 1 1 d . . .
I3 I 0.09445(6) 0.22146(3) 0.18501(5) 0.04551(18) Uani 1 1 d . . .
I4 I -0.04129(6) 0.03437(4) 0.24807(5) 0.05243(19) Uani 1 1 d . . .
I5 I -0.24239(6) 0.03756(4) 0.52845(6) 0.05007(18) Uani 1 1 d . . .
I6 I 0.09225(8) 0.14542(4) 0.55035(6) 0.0619(2) Uani 1 1 d . . .
N1 N 0.3139(6) 0.2765(4) 0.8941(6) 0.0375(19) Uani 1 1 d . . .
N2 N 0.5687(7) -0.0392(4) 1.2926(6) 0.0413(19) Uani 1 1 d . . .
N3 N 0.9514(6) 0.1388(4) 0.8819(6) 0.0370(18) Uani 1 1 d . . .
N4 N 0.4322(6) 0.2105(3) 0.9806(5) 0.0314(17) Uani 1 1 d . . .
N5 N 0.6132(6) 0.0249(3) 1.1723(5) 0.0311(17) Uani 1 1 d . . .
N6 N 0.7903(6) 0.1428(3) 0.9195(6) 0.0308(16) Uani 1 1 d . . .
C1 C 0.2858(9) 0.2649(5) 0.9921(8) 0.043(3) Uani 1 1 d . . .
H1A H 0.2265 0.2826 1.0171 0.052 Uiso 1 1 calc R . .
C2 C 0.3581(8) 0.2238(5) 1.0455(8) 0.048(3) Uani 1 1 d . . .
H2A H 0.3583 0.2072 1.1141 0.057 Uiso 1 1 calc R . .
C3 C 0.4032(8) 0.2433(5) 0.8883(7) 0.038(2) Uani 1 1 d . . .
H3A H 0.4396 0.2428 0.8302 0.045 Uiso 1 1 calc R . .
C4 C 0.6360(9) -0.0735(5) 1.2390(8) 0.050(3) Uani 1 1 d . . .
H4A H 0.6577 -0.1165 1.2515 0.060 Uiso 1 1 calc R . .
C5 C 0.6648(9) -0.0337(4) 1.1651(8) 0.043(3) Uani 1 1 d . . .
H5A H 0.7112 -0.0437 1.1174 0.052 Uiso 1 1 calc R . .
C6 C 0.5553(8) 0.0203(5) 1.2522(7) 0.040(2) Uani 1 1 d . . .
H6A H 0.5133 0.0530 1.2750 0.049 Uiso 1 1 calc R . .
C7 C 0.7805(9) 0.1435(4) 0.8079(7) 0.041(2) Uani 1 1 d . . .
H7A H 0.7164 0.1455 0.7579 0.050 Uiso 1 1 calc R . .
C8 C 0.8820(9) 0.1410(5) 0.7871(8) 0.042(2) Uani 1 1 d . . .
H8A H 0.9013 0.1408 0.7193 0.050 Uiso 1 1 calc R . .
C9 C 0.8958(7) 0.1385(4) 0.9604(7) 0.034(2) Uani 1 1 d . . .
H9A H 0.9253 0.1358 1.0332 0.041 Uiso 1 1 calc R . .
C10 C 0.7028(7) 0.0878(4) 1.0515(6) 0.030(2) Uani 1 1 d . . .
H10A H 0.7626 0.0603 1.0665 0.036 Uiso 1 1 calc R . .
C11 C 0.7008(8) 0.1375(4) 0.9772(7) 0.034(2) Uani 1 1 d . . .
C12 C 0.6133(8) 0.1789(4) 0.9524(7) 0.033(2) Uani 1 1 d . . .
H12A H 0.6129 0.2122 0.9025 0.040 Uiso 1 1 calc R . .
C13 C 0.5251(7) 0.1690(4) 1.0049(6) 0.029(2) Uani 1 1 d . . .
C14 C 0.5224(8) 0.1199(4) 1.0794(7) 0.034(2) Uani 1 1 d . . .
H14A H 0.4623 0.1137 1.1125 0.040 Uiso 1 1 calc R . .
C15 C 0.6157(8) 0.0796(4) 1.1027(6) 0.030(2) Uani 1 1 d . . .
C16 C 0.2566(10) 0.3187(5) 0.8087(8) 0.055(3) Uani 1 1 d . . .
H16A H 0.1952 0.3384 0.8324 0.083 Uiso 1 1 calc R . .
H16B H 0.2320 0.2933 0.7453 0.083 Uiso 1 1 calc R . .
H16C H 0.3050 0.3521 0.7926 0.083 Uiso 1 1 calc R . .
C17 C 0.5149(10) -0.0642(6) 1.3804(8) 0.063(3) Uani 1 1 d . . .
H17A H 0.4756 -0.0296 1.4073 0.095 Uiso 1 1 calc R . .
H17B H 0.5690 -0.0808 1.4376 0.095 Uiso 1 1 calc R . .
H17C H 0.4654 -0.0984 1.3531 0.095 Uiso 1 1 calc R . .
C18 C 1.0704(9) 0.1403(6) 0.8937(9) 0.058(3) Uani 1 1 d . . .
H18A H 1.1022 0.1375 0.9685 0.087 Uiso 1 1 calc R . .
H18B H 1.0925 0.1802 0.8645 0.087 Uiso 1 1 calc R . .
H18C H 1.0945 0.1042 0.8558 0.087 Uiso 1 1 calc R . .
OW1 O 0.3331(12) 0.2190(7) 0.6346(12) 0.158(5) Uani 1 1 d . . .


_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 3.0481(9) . ?
Pb1 I3 3.1327(10) . ?
Pb1 I2 3.2282(10) . ?
Pb1 I4 3.2565(11) . ?
Pb2 I5 3.2068(9) . ?
Pb2 I5 3.2068(9) 3_556 ?
Pb2 I4 3.2121(9) 3_556 ?
Pb2 I4 3.2121(9) . ?
Pb2 I6 3.2282(10) . ?
Pb2 I6 3.2282(10) 3_556 ?
N1 C3 1.321(11) . ?
N1 C1 1.366(11) . ?
N1 C16 1.470(11) . ?
N2 C6 1.326(12) . ?
N2 C4 1.365(12) . ?
N2 C17 1.487(11) . ?
N3 C9 1.307(10) . ?
N3 C8 1.350(12) . ?
N3 C18 1.469(13) . ?
N4 C3 1.340(11) . ?
N4 C2 1.369(11) . ?
N4 C13 1.429(10) . ?
N5 C6 1.345(11) . ?
N5 C5 1.376(11) . ?
N5 C15 1.431(10) . ?
N6 C9 1.332(11) . ?
N6 C7 1.393(11) . ?
N6 C11 1.443(11) . ?
C1 C2 1.331(13) . ?
C4 C5 1.339(13) . ?
C7 C8 1.341(14) . ?
C10 C15 1.372(12) . ?
C10 C11 1.385(12) . ?
C11 C12 1.377(13) . ?
C12 C13 1.397(12) . ?
C13 C14 1.386(11) . ?
C14 C15 1.419(12) . ?

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 I3 93.24(3) . . ?
I1 Pb1 I2 88.61(3) . . ?
I3 Pb1 I2 90.70(3) . . ?
I1 Pb1 I4 87.04(3) . . ?
I3 Pb1 I4 85.44(3) . . ?
I2 Pb1 I4 174.01(2) . . ?
I5 Pb2 I5 180.0 . 3_556 ?
I5 Pb2 I4 86.08(3) . 3_556 ?
I5 Pb2 I4 93.92(3) 3_556 3_556 ?
I5 Pb2 I4 93.92(3) . . ?
I5 Pb2 I4 86.08(3) 3_556 . ?
I4 Pb2 I4 180.0 3_556 . ?
I5 Pb2 I6 93.79(2) . . ?
I5 Pb2 I6 86.21(2) 3_556 . ?
I4 Pb2 I6 91.11(2) 3_556 . ?
I4 Pb2 I6 88.89(2) . . ?
I5 Pb2 I6 86.21(2) . 3_556 ?
I5 Pb2 I6 93.79(2) 3_556 3_556 ?
I4 Pb2 I6 88.89(2) 3_556 3_556 ?
I4 Pb2 I6 91.11(2) . 3_556 ?
I6 Pb2 I6 180.0 . 3_556 ?
Pb2 I4 Pb1 80.37(3) . . ?
C3 N1 C1 108.3(8) . . ?
C3 N1 C16 124.9(8) . . ?
C1 N1 C16 126.8(8) . . ?
C6 N2 C4 109.4(8) . . ?
C6 N2 C17 124.4(9) . . ?
C4 N2 C17 126.2(9) . . ?
C9 N3 C8 109.3(8) . . ?
C9 N3 C18 126.0(9) . . ?
C8 N3 C18 124.7(8) . . ?
C3 N4 C2 108.3(8) . . ?
C3 N4 C13 124.9(7) . . ?
C2 N4 C13 126.8(7) . . ?
C6 N5 C5 108.0(7) . . ?
C6 N5 C15 126.0(8) . . ?
C5 N5 C15 125.9(7) . . ?
C9 N6 C7 107.3(8) . . ?
C9 N6 C11 127.0(8) . . ?
C7 N6 C11 125.1(8) . . ?
C2 C1 N1 108.1(9) . . ?
C1 C2 N4 107.0(8) . . ?
N1 C3 N4 108.3(7) . . ?
C5 C4 N2 107.2(9) . . ?
C4 C5 N5 107.6(8) . . ?
N2 C6 N5 107.8(9) . . ?
C8 C7 N6 106.3(9) . . ?
C7 C8 N3 107.9(8) . . ?
N3 C9 N6 109.1(8) . . ?
C15 C10 C11 119.4(8) . . ?
C12 C11 C10 121.9(8) . . ?
C12 C11 N6 119.6(8) . . ?
C10 C11 N6 118.3(8) . . ?
C11 C12 C13 117.6(8) . . ?
C14 C13 C12 123.0(8) . . ?
C14 C13 N4 117.7(8) . . ?
C12 C13 N4 119.3(7) . . ?
C13 C14 C15 116.7(8) . . ?
C10 C15 C14 121.4(8) . . ?
C10 C15 N5 119.4(8) . . ?
C14 C15 N5 118.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.216
####################################################################### 
# 
# 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 1519637'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H42 Ag8 I14 N12 O0'
_chemical_formula_weight         3282.38

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'
Ag Ag -0.8971 1.1015 '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'
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'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_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                   14.090(2)
_cell_length_b                   14.090(2)
_cell_length_c                   31.201(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5364.4(15)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14992
_cell_measurement_theta_min      22.5
_cell_measurement_theta_max      27.535

_exptl_crystal_description       columnar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4380
_exptl_absorpt_coefficient_mu    8.219
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_T_max  0.405
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17338
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.47
_reflns_number_total             2739
_reflns_number_gt                2350
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0389P)²+42.9553P] 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         2739
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.36712(6) 0.47426(6) 0.13889(2) 0.0766(2) Uani 1 1 d . . .
Ag2 Ag 0.3333 0.6667 0.06509(5) 0.0824(3) Uani 1 3 d S . .
I1 I 0.38330(3) 0.50321(4) 0.048940(13) 0.04991(13) Uani 1 1 d . . .
I2 I 0.57049(5) 0.51749(5) 0.169398(15) 0.07033(17) Uani 1 1 d . . .
I3 I 0.3333 0.6667 0.1667 0.03737(19) Uani 1 6 d S . .
I4 I 0.0000 0.0000 0.0000 0.0660(3) Uani 1 6 d S . .
N1 N 0.2887(3) 0.0352(3) 0.06243(16) 0.0409(10) Uani 1 1 d . . .
N2 N 0.4413(3) 0.1847(3) 0.07277(14) 0.0328(8) Uani 1 1 d . . .
C1 C 0.3954(4) 0.0825(4) 0.05767(16) 0.0335(10) Uani 1 1 d . . .
H1A H 0.4328 0.0501 0.0457 0.040 Uiso 1 1 calc R . .
C2 C 0.2649(5) 0.1067(5) 0.0822(3) 0.068(2) Uani 1 1 d . . .
H2A H 0.1954 0.0931 0.0897 0.081 Uiso 1 1 calc R . .
C3 C 0.3590(5) 0.1998(5) 0.0889(3) 0.068(2) Uani 1 1 d . . .
H3A H 0.3673 0.2629 0.1019 0.081 Uiso 1 1 calc R . .
C4 C 0.5565(4) 0.2601(4) 0.07281(15) 0.0303(9) Uani 1 1 d . . .
C5 C 0.6290(4) 0.2215(4) 0.07260(15) 0.0311(9) Uani 1 1 d . . .
H5A H 0.6038 0.1466 0.0723 0.037 Uiso 1 1 calc R . .
C6 C 0.2119(5) -0.0777(5) 0.0485(2) 0.0587(17) Uani 1 1 d . . .
H6A H 0.2521 -0.1085 0.0354 0.088 Uiso 1 1 calc R . .
H6B H 0.1613 -0.0770 0.0281 0.088 Uiso 1 1 calc R . .
H6C H 0.1723 -0.1211 0.0728 0.088 Uiso 1 1 calc R . .


_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
Ag1 I2 2.7711(9) 14_455 ?
Ag1 I2 2.7827(9) . ?
Ag1 I1 2.8288(10) . ?
Ag1 I3 3.1012(8) . ?
Ag1 Ag1 3.4455(10) 15 ?
Ag1 Ag1 3.4455(10) 14_455 ?
Ag2 I1 2.7704(6) 3_565 ?
Ag2 I1 2.7704(6) 2_665 ?
Ag2 I1 2.7704(6) . ?
Ag2 I3 3.1694(15) . ?
I2 Ag1 2.7711(9) 15 ?
I3 Ag1 3.1012(8) 15 ?
I3 Ag1 3.1012(8) 3_565 ?
I3 Ag1 3.1012(8) 2_665 ?
I3 Ag1 3.1012(8) 14_455 ?
I3 Ag1 3.1013(8) 13_565 ?
I3 Ag2 3.1695(15) 13_565 ?
N1 C1 1.312(6) . ?
N1 C2 1.358(8) . ?
N1 C6 1.473(7) . ?
N2 C1 1.335(6) . ?
N2 C3 1.375(7) . ?
N2 C4 1.428(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.336(9) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 C5 1.378(6) . ?
C4 C5 1.380(6) 3_665 ?
C5 C4 1.380(6) 2_655 ?
C5 H5A 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 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
I2 Ag1 I2 117.89(3) 14_455 . ?
I2 Ag1 I1 112.97(3) 14_455 . ?
I2 Ag1 I1 107.93(3) . . ?
I2 Ag1 I3 108.03(2) 14_455 . ?
I2 Ag1 I3 107.72(2) . . ?
I1 Ag1 I3 100.82(2) . . ?
I2 Ag1 Ag1 133.16(4) 14_455 15 ?
I2 Ag1 Ag1 51.51(2) . 15 ?
I1 Ag1 Ag1 113.35(3) . 15 ?
I3 Ag1 Ag1 56.254(6) . 15 ?
I2 Ag1 Ag1 51.81(2) 14_455 14_455 ?
I2 Ag1 Ag1 129.67(4) . 14_455 ?
I1 Ag1 Ag1 121.42(3) . 14_455 ?
I3 Ag1 Ag1 56.255(6) . 14_455 ?
Ag1 Ag1 Ag1 96.91(3) 15 14_455 ?
I1 Ag2 I1 116.770(18) 3_565 2_665 ?
I1 Ag2 I1 116.770(18) 3_565 . ?
I1 Ag2 I1 116.770(18) 2_665 . ?
I1 Ag2 I3 100.48(3) 3_565 . ?
I1 Ag2 I3 100.48(3) 2_665 . ?
I1 Ag2 I3 100.48(3) . . ?
Ag2 I1 Ag1 84.48(3) . . ?
Ag1 I2 Ag1 76.69(3) 15 . ?
Ag1 I3 Ag1 180.0 15 3_565 ?
Ag1 I3 Ag1 67.489(12) 15 2_665 ?
Ag1 I3 Ag1 112.511(12) 3_565 2_665 ?
Ag1 I3 Ag1 67.491(12) 15 . ?
Ag1 I3 Ag1 112.511(12) 3_565 . ?
Ag1 I3 Ag1 112.511(12) 2_665 . ?
Ag1 I3 Ag1 112.511(12) 15 14_455 ?
Ag1 I3 Ag1 67.489(12) 3_565 14_455 ?
Ag1 I3 Ag1 180.0 2_665 14_455 ?
Ag1 I3 Ag1 67.491(12) . 14_455 ?
Ag1 I3 Ag1 112.509(12) 15 13_565 ?
Ag1 I3 Ag1 67.489(12) 3_565 13_565 ?
Ag1 I3 Ag1 67.490(12) 2_665 13_565 ?
Ag1 I3 Ag1 180.0 . 13_565 ?
Ag1 I3 Ag1 112.508(12) 14_455 13_565 ?
Ag1 I3 Ag2 106.229(14) 15 . ?
Ag1 I3 Ag2 73.772(14) 3_565 . ?
Ag1 I3 Ag2 73.772(14) 2_665 . ?
Ag1 I3 Ag2 73.772(14) . . ?
Ag1 I3 Ag2 106.229(14) 14_455 . ?
Ag1 I3 Ag2 106.229(14) 13_565 . ?
Ag1 I3 Ag2 73.771(14) 15 13_565 ?
Ag1 I3 Ag2 106.227(14) 3_565 13_565 ?
Ag1 I3 Ag2 106.228(14) 2_665 13_565 ?
Ag1 I3 Ag2 106.229(14) . 13_565 ?
Ag1 I3 Ag2 73.771(14) 14_455 13_565 ?
Ag1 I3 Ag2 73.770(14) 13_565 13_565 ?
Ag2 I3 Ag2 180.0 . 13_565 ?
C1 N1 C2 108.7(4) . . ?
C1 N1 C6 123.4(5) . . ?
C2 N1 C6 127.9(5) . . ?
C1 N2 C3 107.8(4) . . ?
C1 N2 C4 124.1(4) . . ?
C3 N2 C4 128.1(4) . . ?
N1 C1 N2 108.8(4) . . ?
N1 C1 H1A 125.6 . . ?
N2 C1 H1A 125.6 . . ?
C3 C2 N1 107.9(5) . . ?
C3 C2 H2A 126.0 . . ?
N1 C2 H2A 126.0 . . ?
C2 C3 N2 106.9(5) . . ?
C2 C3 H3A 126.6 . . ?
N2 C3 H3A 126.6 . . ?
C5 C4 C5 121.5(5) . 3_665 ?
C5 C4 N2 119.8(4) . . ?
C5 C4 N2 118.7(4) 3_665 . ?
C4 C5 C4 118.5(5) . 2_655 ?
C4 C5 H5A 120.7 . . ?
C4 C5 H5A 120.7 2_655 . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.731
_refine_diff_density_min         -1.722
_refine_diff_density_rms         0.311
