# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  data retrieval see:
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data_compound1a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H14 B N9 O Pb S8'
_chemical_formula_sum            'C13 H14 B N9 O Pb S8'
_chemical_formula_weight         786.81

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'
B B 0.0013 0.0007 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.1258(9)
_cell_length_b                   11.5049(11)
_cell_length_c                   12.7990(19)
_cell_angle_alpha                111.827(6)
_cell_angle_beta                 108.210(6)
_cell_angle_gamma                95.805(5)
_cell_volume                     1274.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9141
_cell_measurement_theta_min      3.150
_cell_measurement_theta_max      43.998

_exptl_crystal_description       column
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             756
_exptl_absorpt_coefficient_mu    7.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1664
_exptl_absorpt_correction_T_max  0.4279
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       'Bruker KAPPA APEX II   '
_diffrn_radiation_source         'fine focus sealed tube  '
_diffrn_radiation_monochromator  'graphite monochromator  '
_diffrn_measurement_device_type  'four three circle diffractometer'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            87623
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7414
_reflns_number_gt                7306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Disorder of N-methylpyrrolidone on two positions (69:31). Bondlength and angles
 of this disorder were restrained with SAME.
 Hydrogen bonded to the boron atom was refined isotropically.

 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)+(0.0123P)²+1.9951P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7414
_refine_ls_number_parameters     293
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0150
_refine_ls_wR_factor_ref         0.0356
_refine_ls_wR_factor_gt          0.0354
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_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 0.102614(7) 0.448860(6) 0.320915(6) 0.01509(2) Uani 1 1 d . . .
S1 S 0.28211(5) 0.38624(4) 0.15974(4) 0.01926(8) Uani 1 1 d . . .
S2 S 0.14691(5) 0.12257(5) -0.04730(4) 0.02280(9) Uani 1 1 d . . .
S3 S 0.62187(5) 0.36106(5) 0.56276(4) 0.01918(8) Uani 1 1 d . . .
S4 S 0.78093(4) 0.21580(4) 0.41361(4) 0.01775(8) Uani 1 1 d . . .
S5 S 0.03892(5) 0.16679(4) 0.31599(5) 0.02120(9) Uani 1 1 d . . .
S6 S 0.14045(7) -0.02585(7) 0.40647(8) 0.04140(16) Uani 1 1 d . . .
S7 S 0.02291(6) 0.36638(5) 0.74585(5) 0.02642(10) Uani 1 1 d . . .
S8 S 0.30320(6) 0.38024(7) 0.69992(6) 0.03425(13) Uani 1 1 d . . .
N1 N 0.26907(16) 0.15176(15) 0.16842(14) 0.0165(3) Uani 1 1 d . . .
N2 N 0.22158(18) 0.01940(16) 0.10070(16) 0.0223(3) Uani 1 1 d . . .
N3 N 0.51418(16) 0.19456(14) 0.32454(14) 0.0154(3) Uani 1 1 d . . .
N4 N 0.54260(17) 0.11053(16) 0.22924(15) 0.0213(3) Uani 1 1 d . . .
N5 N 0.29650(16) 0.10709(16) 0.35158(15) 0.0185(3) Uani 1 1 d . . .
N6 N 0.3784(2) 0.0286(2) 0.3843(2) 0.0356(5) Uani 1 1 d . . .
N7 N 0.09150(16) 0.45503(15) 0.60014(14) 0.0163(3) Uani 1 1 d . . .
N8 N 0.19500(17) 0.48199(16) 0.55825(14) 0.0180(3) Uani 1 1 d . . .
B1 B 0.3563(2) 0.20158(19) 0.30669(18) 0.0157(3) Uani 1 1 d . . .
H1B H 0.350(2) 0.298(2) 0.355(2) 0.013(5) Uiso 1 1 d . . .
C1 C 0.23997(18) 0.22386(17) 0.10621(16) 0.0165(3) Uani 1 1 d . . .
C2 C 0.1563(2) -0.0080(2) -0.01241(19) 0.0250(4) Uani 1 1 d . . .
H2 H 0.1160 -0.0945 -0.0727 0.030 Uiso 1 1 calc R . .
C3 C 0.62669(18) 0.25767(16) 0.43019(16) 0.0149(3) Uani 1 1 d . . .
C4 C 0.6779(2) 0.11353(19) 0.26423(18) 0.0211(4) Uani 1 1 d . . .
H4 H 0.7179 0.0624 0.2107 0.025 Uiso 1 1 calc R . .
C5 C 0.16574(19) 0.09189(18) 0.35681(18) 0.0192(3) Uani 1 1 d . . .
C6 C 0.3093(3) -0.0457(3) 0.4143(4) 0.0512(9) Uani 1 1 d . . .
H6 H 0.3486 -0.1071 0.4391 0.061 Uiso 1 1 calc R . .
C7 C 0.1304(2) 0.40209(18) 0.67650(17) 0.0184(3) Uani 1 1 d . . .
C8 C 0.3105(2) 0.4485(2) 0.6023(2) 0.0257(4) Uani 1 1 d . . .
H8 H 0.3922 0.4605 0.5824 0.031 Uiso 1 1 calc R . .
O1 O -0.15023(19) 0.29818(17) 0.14895(16) 0.0339(3) Uiso 1 1 d . . .
N9A N -0.2577(3) 0.3082(2) -0.0316(2) 0.0223(6) Uiso 0.686(5) 1 d PD A 1
C9A C -0.2612(3) 0.2912(3) 0.0652(3) 0.0205(6) Uiso 0.686(5) 1 d PD A 1
C10A C -0.3966(4) 0.2942(4) -0.1175(4) 0.0298(8) Uiso 0.686(5) 1 d PD A 1
H10A H -0.4263 0.2114 -0.1909 0.036 Uiso 0.686(5) 1 calc PR A 1
H10B H -0.3961 0.3661 -0.1423 0.036 Uiso 0.686(5) 1 calc PR A 1
C11A C -0.4960(5) 0.2969(4) -0.0493(4) 0.0417(9) Uiso 0.686(5) 1 d PD A 1
H11A H -0.5876 0.2309 -0.1028 0.050 Uiso 0.686(5) 1 calc PR A 1
H11B H -0.5169 0.3829 -0.0196 0.050 Uiso 0.686(5) 1 calc PR A 1
C12A C -0.4160(5) 0.2678(5) 0.0575(4) 0.0342(9) Uiso 0.686(5) 1 d PD A 1
H12A H -0.4535 0.1773 0.0412 0.041 Uiso 0.686(5) 1 calc PR A 1
H12B H -0.4238 0.3266 0.1336 0.041 Uiso 0.686(5) 1 calc PR A 1
C13A C -0.1323(4) 0.3179(5) -0.0587(4) 0.0320(9) Uiso 0.686(5) 1 d PD A 1
H13A H -0.0477 0.3367 0.0140 0.048 Uiso 0.686(5) 1 calc PR A 1
H13B H -0.1240 0.3876 -0.0845 0.048 Uiso 0.686(5) 1 calc PR A 1
H13C H -0.1387 0.2361 -0.1242 0.048 Uiso 0.686(5) 1 calc PR A 1
N9B N -0.3343(7) 0.2726(6) -0.0115(6) 0.0330(16) Uiso 0.314(5) 1 d PD A 2
C9B C -0.1944(7) 0.3066(6) 0.0467(6) 0.0231(14) Uiso 0.314(5) 1 d PD A 2
C10B C -0.3897(7) 0.2591(8) -0.1388(6) 0.0223(15) Uiso 0.314(5) 1 d PD A 2
H10C H -0.4444 0.3240 -0.1470 0.027 Uiso 0.314(5) 1 calc PR A 2
H10D H -0.4505 0.1714 -0.1967 0.027 Uiso 0.314(5) 1 calc PR A 2
C11B C -0.2431(11) 0.2854(11) -0.1568(9) 0.056(3) Uiso 0.314(5) 1 d PD A 2
H11C H -0.2248 0.2028 -0.2037 0.068 Uiso 0.314(5) 1 calc PR A 2
H11D H -0.2479 0.3394 -0.2020 0.068 Uiso 0.314(5) 1 calc PR A 2
C12B C -0.1274(8) 0.3528(9) -0.0355(8) 0.0266(18) Uiso 0.314(5) 1 d PD A 2
H12C H -0.1081 0.4477 -0.0070 0.032 Uiso 0.314(5) 1 calc PR A 2
H12D H -0.0378 0.3252 -0.0350 0.032 Uiso 0.314(5) 1 calc PR A 2
C13B C -0.4323(8) 0.2301(9) 0.0302(8) 0.0261(16) Uiso 0.314(5) 1 d PD A 2
H13D H -0.5299 0.2091 -0.0295 0.039 Uiso 0.314(5) 1 calc PR A 2
H13E H -0.4230 0.2984 0.1079 0.039 Uiso 0.314(5) 1 calc PR A 2
H13F H -0.4131 0.1530 0.0415 0.039 Uiso 0.314(5) 1 calc PR A 2


_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 N7 2.6376(15) 2_566 ?
Pb1 O1 2.6735(18) . ?
Pb1 N8 2.7456(16) . ?
Pb1 S7 2.8430(6) 2_566 ?
Pb1 S3 2.9208(6) 2_666 ?
Pb1 S1 3.0953(5) . ?
S1 C1 1.6869(19) . ?
S2 C2 1.723(2) . ?
S2 C1 1.7391(18) . ?
S3 C3 1.6909(18) . ?
S3 Pb1 2.9208(6) 2_666 ?
S4 C4 1.721(2) . ?
S4 C3 1.7319(17) . ?
S5 C5 1.6744(19) . ?
S6 C6 1.725(3) . ?
S6 C5 1.725(2) . ?
S7 C7 1.711(2) . ?
S7 Pb1 2.8430(6) 2_566 ?
S8 C8 1.720(2) . ?
S8 C7 1.7409(19) . ?
N1 C1 1.343(2) . ?
N1 N2 1.382(2) . ?
N1 B1 1.551(3) . ?
N2 C2 1.285(3) . ?
N3 C3 1.339(2) . ?
N3 N4 1.380(2) . ?
N3 B1 1.558(2) . ?
N4 C4 1.294(2) . ?
N5 C5 1.344(2) . ?
N5 N6 1.377(2) . ?
N5 B1 1.558(3) . ?
N6 C6 1.287(3) . ?
N7 C7 1.316(2) . ?
N7 N8 1.375(2) . ?
N7 Pb1 2.6377(15) 2_566 ?
N8 C8 1.295(2) . ?
B1 H1B 1.06(2) . ?
C2 H2 0.9500 . ?
C4 H4 0.9500 . ?
C6 H6 0.9500 . ?
C8 H8 0.9500 . ?
O1 C9A 1.259(3) . ?
O1 C9B 1.289(6) . ?
N9A C9A 1.334(4) . ?
N9A C13A 1.422(5) . ?
N9A C10A 1.438(4) . ?
C9A C12A 1.529(5) . ?
C10A C11A 1.521(6) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C11A C12A 1.529(6) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
N9B C9B 1.314(8) . ?
N9B C13B 1.391(9) . ?
N9B C10B 1.488(9) . ?
C9B C12B 1.623(9) . ?
C10B C11B 1.588(11) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11B C12B 1.472(12) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?

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
N7 Pb1 O1 74.82(5) 2_566 . ?
N7 Pb1 N8 75.60(5) 2_566 . ?
O1 Pb1 N8 124.29(5) . . ?
N7 Pb1 S7 57.95(4) 2_566 2_566 ?
O1 Pb1 S7 79.32(4) . 2_566 ?
N8 Pb1 S7 120.40(4) . 2_566 ?
N7 Pb1 S3 111.62(4) 2_566 2_666 ?
O1 Pb1 S3 159.12(4) . 2_666 ?
N8 Pb1 S3 76.39(4) . 2_666 ?
S7 Pb1 S3 87.473(16) 2_566 2_666 ?
N7 Pb1 S1 157.12(3) 2_566 . ?
O1 Pb1 S1 97.30(4) . . ?
N8 Pb1 S1 124.87(3) . . ?
S7 Pb1 S1 99.781(16) 2_566 . ?
S3 Pb1 S1 68.903(15) 2_666 . ?
C1 S1 Pb1 98.74(6) . . ?
C2 S2 C1 88.81(10) . . ?
C3 S3 Pb1 103.72(6) . 2_666 ?
C4 S4 C3 88.21(9) . . ?
C6 S6 C5 88.77(11) . . ?
C7 S7 Pb1 80.09(6) . 2_566 ?
C8 S8 C7 87.95(9) . . ?
C1 N1 N2 116.19(15) . . ?
C1 N1 B1 126.68(15) . . ?
N2 N1 B1 117.06(15) . . ?
C2 N2 N1 110.37(17) . . ?
C3 N3 N4 115.83(14) . . ?
C3 N3 B1 124.64(14) . . ?
N4 N3 B1 119.32(14) . . ?
C4 N4 N3 109.85(16) . . ?
C5 N5 N6 116.05(16) . . ?
C5 N5 B1 124.59(15) . . ?
N6 N5 B1 119.30(15) . . ?
C6 N6 N5 110.28(18) . . ?
C7 N7 N8 113.99(15) . . ?
C7 N7 Pb1 95.34(11) . 2_566 ?
N8 N7 Pb1 142.32(12) . 2_566 ?
C8 N8 N7 112.37(16) . . ?
C8 N8 Pb1 119.16(13) . . ?
N7 N8 Pb1 116.97(11) . . ?
N1 B1 N5 108.34(14) . . ?
N1 B1 N3 107.87(14) . . ?
N5 B1 N3 107.06(14) . . ?
N1 B1 H1B 110.6(13) . . ?
N5 B1 H1B 111.4(13) . . ?
N3 B1 H1B 111.4(13) . . ?
N1 C1 S1 128.48(14) . . ?
N1 C1 S2 109.13(13) . . ?
S1 C1 S2 122.39(11) . . ?
N2 C2 S2 115.50(15) . . ?
N2 C2 H2 122.3 . . ?
S2 C2 H2 122.3 . . ?
N3 C3 S3 125.95(13) . . ?
N3 C3 S4 110.14(12) . . ?
S3 C3 S4 123.90(11) . . ?
N4 C4 S4 115.95(14) . . ?
N4 C4 H4 122.0 . . ?
S4 C4 H4 122.0 . . ?
N5 C5 S5 127.27(15) . . ?
N5 C5 S6 109.55(14) . . ?
S5 C5 S6 123.11(11) . . ?
N6 C6 S6 115.34(18) . . ?
N6 C6 H6 122.3 . . ?
S6 C6 H6 122.3 . . ?
N7 C7 S7 122.55(14) . . ?
N7 C7 S8 111.55(14) . . ?
S7 C7 S8 125.87(11) . . ?
N8 C8 S8 114.14(15) . . ?
N8 C8 H8 122.9 . . ?
S8 C8 H8 122.9 . . ?
C9A O1 C9B 37.0(3) . . ?
C9A O1 Pb1 145.43(17) . . ?
C9B O1 Pb1 119.3(3) . . ?
C9A N9A C13A 123.4(3) . . ?
C9A N9A C10A 114.1(3) . . ?
C13A N9A C10A 121.8(3) . . ?
O1 C9A N9A 122.9(3) . . ?
O1 C9A C12A 127.7(3) . . ?
N9A C9A C12A 109.4(3) . . ?
N9A C10A C11A 104.3(3) . . ?
N9A C10A H10A 110.9 . . ?
C11A C10A H10A 110.9 . . ?
N9A C10A H10B 110.9 . . ?
C11A C10A H10B 110.9 . . ?
H10A C10A H10B 108.9 . . ?
C10A C11A C12A 105.8(3) . . ?
C10A C11A H11A 110.6 . . ?
C12A C11A H11A 110.6 . . ?
C10A C11A H11B 110.6 . . ?
C12A C11A H11B 110.6 . . ?
H11A C11A H11B 108.7 . . ?
C11A C12A C9A 103.0(3) . . ?
C11A C12A H12A 111.2 . . ?
C9A C12A H12A 111.2 . . ?
C11A C12A H12B 111.2 . . ?
C9A C12A H12B 111.2 . . ?
H12A C12A H12B 109.1 . . ?
C9B N9B C13B 124.6(7) . . ?
C9B N9B C10B 117.1(6) . . ?
C13B N9B C10B 117.5(6) . . ?
O1 C9B N9B 115.2(5) . . ?
O1 C9B C12B 138.6(5) . . ?
N9B C9B C12B 106.2(6) . . ?
N9B C10B C11B 100.3(6) . . ?
N9B C10B H10C 111.7 . . ?
C11B C10B H10C 111.7 . . ?
N9B C10B H10D 111.7 . . ?
C11B C10B H10D 111.7 . . ?
H10C C10B H10D 109.5 . . ?
C12B C11B C10B 107.9(7) . . ?
C12B C11B H11C 110.1 . . ?
C10B C11B H11C 110.1 . . ?
C12B C11B H11D 110.1 . . ?
C10B C11B H11D 110.1 . . ?
H11C C11B H11D 108.4 . . ?
C11B C12B C9B 101.8(6) . . ?
C11B C12B H12C 111.4 . . ?
C9B C12B H12C 111.4 . . ?
C11B C12B H12D 111.4 . . ?
C9B C12B H12D 111.4 . . ?
H12C C12B H12D 109.3 . . ?
N9B C13B H13D 109.5 . . ?
N9B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
N9B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.333
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.078
_database_code_depnum_ccdc_archive 'CCDC 992111'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound2

_audit_creation_date             2013-06-27
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H20 B2 N4 Pb S8'
_chemical_formula_sum            'C16 H20 B2 N4 Pb S8'
_chemical_formula_weight         753.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C8 H24 B N O3 Pb S4'
_chemical_oxdiff_usercomment     'V.Nr 315 vom 15.4.13'
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'
B B 0.0013 0.0007 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.93379(19)
_cell_length_b                   12.2627(3)
_cell_length_c                   12.4372(3)
_cell_angle_alpha                65.316(2)
_cell_angle_beta                 83.1389(17)
_cell_angle_gamma                66.8959(19)
_cell_volume                     1264.40(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    43855
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.8410
_cell_measurement_theta_min      3.1840
_exptl_absorpt_coefficient_mu    7.346
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.3512
_exptl_crystal_size_mid          0.2091
_exptl_crystal_size_min          0.1473
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            74818
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_min         2.795
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.6228
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9516
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -8.00   85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   77.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega   -4.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   77.0000   60.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega   -4.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   57.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
  4 omega  -27.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -57.0000  -60.0000 70

#__ type_ start__ end____ width___ exp.time_
  5 omega  -51.00   18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -57.0000 -180.0000 69

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -99.0000   60.0000 76

#__ type_ start__ end____ width___ exp.time_
  7 omega   11.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   38.0000 -180.0000 35

#__ type_ start__ end____ width___ exp.time_
  8 omega   60.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   38.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
  9 omega   37.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  178.0000 -150.0000 33

#__ type_ start__ end____ width___ exp.time_
 10 omega  -15.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -99.0000  -90.0000 71

#__ type_ start__ end____ width___ exp.time_
 11 omega   55.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -153.0000 -134.0374 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -86.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  148.0000   14.7631 51

#__ type_ start__ end____ width___ exp.time_
 13 omega  -88.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -38.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
 14 omega  -88.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -38.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
 15 omega  -75.00  -27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  131.0000  -82.7173 48

#__ type_ start__ end____ width___ exp.time_
 16 omega  -88.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -38.0000    0.0000 92

#__ type_ start__ end____ width___ exp.time_
 17 omega  -94.00   16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -19.0000  150.0000 110

#__ type_ start__ end____ width___ exp.time_
 18 omega   35.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  178.0000   30.0000 66

#__ type_ start__ end____ width___ exp.time_
 19 omega    7.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -133.0000  -93.7391 70

#__ type_ start__ end____ width___ exp.time_
 20 omega  -20.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -99.0000   90.0000 76

#__ type_ start__ end____ width___ exp.time_
 21 omega  -90.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  153.0000 -157.0994 52

#__ type_ start__ end____ width___ exp.time_
 22 omega  -94.00   16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -19.0000 -120.0000 110

#__ type_ start__ end____ width___ exp.time_
 23 omega  -85.00    8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -57.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
 24 omega  -90.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  153.0000  -36.0747 52

#__ type_ start__ end____ width___ exp.time_
 25 omega  -68.00    9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854    0.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
 26 omega  -54.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -38.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
 27 omega   16.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -153.0000 -134.0374 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0261927000
_diffrn_orient_matrix_UB_12      0.0206612000
_diffrn_orient_matrix_UB_13      0.0357534000
_diffrn_orient_matrix_UB_21      -0.0714087000
_diffrn_orient_matrix_UB_22      0.0464531000
_diffrn_orient_matrix_UB_23      -0.0021418000
_diffrn_orient_matrix_UB_31      -0.0160652000
_diffrn_orient_matrix_UB_32      -0.0463710000
_diffrn_orient_matrix_UB_33      0.0516506000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7025
_reflns_number_total             7372
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0146
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0124P)²+0.3336P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0327
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.88990(2) 0.15588(2) 0.82237(2) 0.00996(2) Uani 1 1 d . . . . .
S1 S 0.73564(5) 0.20073(4) 0.60987(4) 0.01222(8) Uani 1 1 d . . . . .
S2 S 0.84008(5) 0.12257(4) 0.40870(4) 0.01519(9) Uani 1 1 d . . . . .
S3 S 0.82610(5) 0.41438(4) 0.73934(4) 0.01364(8) Uani 1 1 d . . . . .
S4 S 0.60361(5) 0.59876(4) 0.54326(4) 0.01580(9) Uani 1 1 d . . . . .
S5 S 0.59610(5) 0.25397(4) 0.87847(4) 0.01289(8) Uani 1 1 d . . . . .
S6 S 0.36875(5) 0.15140(4) 1.00185(4) 0.01484(8) Uani 1 1 d . . . . .
S7 S 1.02398(5) 0.16951(4) 1.01500(4) 0.01299(8) Uani 1 1 d . . . . .
S8 S 0.83219(5) 0.41785(4) 1.03211(4) 0.01654(9) Uani 1 1 d . . . . .
N1 N 0.96561(16) 0.23334(14) 0.47156(12) 0.0115(3) Uani 1 1 d . . . . .
N2 N 0.84236(15) 0.43994(13) 0.50685(12) 0.0101(3) Uani 1 1 d . . . . .
N3 N 0.60337(15) 0.09157(13) 1.11279(12) 0.0104(3) Uani 1 1 d . . . . .
N4 N 0.75131(15) 0.22715(14) 1.10650(12) 0.0107(3) Uani 1 1 d . . . . .
B1 B 0.9905(2) 0.31886(18) 0.52730(17) 0.0118(4) Uani 1 1 d . . . . .
H1A H 1.018(2) 0.260(2) 0.6277(18) 0.017(5) Uiso 1 1 d . . . . .
H1B H 1.079(2) 0.3497(19) 0.4804(17) 0.010(5) Uiso 1 1 d . . . . .
B2 B 0.7561(2) 0.08624(19) 1.13968(18) 0.0120(4) Uani 1 1 d . . . . .
H2A H 0.834(2) 0.0457(18) 1.0833(17) 0.008(5) Uiso 1 1 d . . . . .
H2B H 0.787(2) 0.0250(19) 1.2361(18) 0.012(5) Uiso 1 1 d . . . . .
C1 C 0.85478(19) 0.19094(16) 0.50031(15) 0.0115(3) Uani 1 1 d . . . . .
C2 C 0.9911(2) 0.14657(17) 0.33513(15) 0.0164(4) Uani 1 1 d . . . . .
H2 H 1.0296 0.1226 0.2728 0.020 Uiso 1 1 calc R U . . .
C3 C 1.0461(2) 0.20438(17) 0.37929(15) 0.0149(3) Uani 1 1 d . . . . .
C4 C 1.1807(2) 0.2336(2) 0.34009(18) 0.0228(4) Uani 1 1 d . . . . .
H4A H 1.1555 0.3255 0.3101 0.034 Uiso 1 1 calc R U . . .
H4B H 1.2224 0.2040 0.2789 0.034 Uiso 1 1 calc R U . . .
H4C H 1.2506 0.1902 0.4061 0.034 Uiso 1 1 calc R U . . .
C5 C 0.77009(19) 0.47339(16) 0.59364(15) 0.0116(3) Uani 1 1 d . . . . .
C6 C 0.6359(2) 0.61032(18) 0.40127(16) 0.0160(4) Uani 1 1 d . . . . .
H6 H 0.5717 0.6707 0.3360 0.019 Uiso 1 1 calc R U . . .
C7 C 0.76645(19) 0.52054(16) 0.39660(15) 0.0120(3) Uani 1 1 d . . . . .
C8 C 0.8294(2) 0.50886(18) 0.28476(15) 0.0172(4) Uani 1 1 d . . . . .
H8A H 0.9266 0.5089 0.2795 0.026 Uiso 1 1 calc R U . . .
H8B H 0.7689 0.5809 0.2180 0.026 Uiso 1 1 calc R U . . .
H8C H 0.8332 0.4293 0.2850 0.026 Uiso 1 1 calc R U . . .
C9 C 0.53791(18) 0.15836(16) 1.00410(15) 0.0117(3) Uani 1 1 d . . . . .
C10 C 0.3911(2) 0.05292(17) 1.15071(16) 0.0154(3) Uani 1 1 d . . . . .
H10 H 0.3223 0.0202 1.1940 0.019 Uiso 1 1 calc R U . . .
C11 C 0.52077(19) 0.02903(16) 1.19689(15) 0.0135(3) Uani 1 1 d . . . . .
C12 C 0.5752(2) -0.05323(19) 1.32338(16) 0.0199(4) Uani 1 1 d . . . . .
H12A H 0.6664 -0.1229 1.3272 0.030 Uiso 1 1 calc R U . . .
H12B H 0.5045 -0.0883 1.3665 0.030 Uiso 1 1 calc R U . . .
H12C H 0.5898 -0.0013 1.3577 0.030 Uiso 1 1 calc R U . . .
C13 C 0.86364(19) 0.26143(16) 1.05473(15) 0.0117(3) Uani 1 1 d . . . . .
C14 C 0.6656(2) 0.43568(17) 1.09450(16) 0.0169(4) Uani 1 1 d . . . . .
H14 H 0.6021 0.5109 1.1027 0.020 Uiso 1 1 calc R U . . .
C15 C 0.63846(19) 0.32662(17) 1.13011(15) 0.0130(3) Uani 1 1 d . . . . .
C16 C 0.5042(2) 0.31002(18) 1.19016(17) 0.0181(4) Uani 1 1 d . . . . .
H16A H 0.4468 0.3018 1.1391 0.027 Uiso 1 1 calc R U . . .
H16B H 0.4473 0.3842 1.2073 0.027 Uiso 1 1 calc R U . . .
H16C H 0.5320 0.2333 1.2627 0.027 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
Pb1 S1 2.9543(4) . ?
Pb1 S3 2.7132(4) . ?
Pb1 S5 2.8126(4) . ?
Pb1 S7 2.9686(4) . ?
Pb1 H1A 2.66(2) . ?
Pb1 B1 3.6092(19) . ?
S1 C1 1.7064(18) . ?
S2 C1 1.7193(18) . ?
S2 C2 1.7226(19) . ?
S3 C5 1.7166(18) . ?
S4 C5 1.7143(18) . ?
S4 C6 1.7125(18) . ?
S5 C9 1.7136(17) . ?
S6 C9 1.7196(17) . ?
S6 C10 1.7192(19) . ?
S7 C13 1.7088(18) . ?
S8 C13 1.7193(18) . ?
S8 C14 1.715(2) . ?
N1 B1 1.579(2) . ?
N1 C1 1.345(2) . ?
N1 C3 1.407(2) . ?
N2 B1 1.579(2) . ?
N2 C5 1.343(2) . ?
N2 C7 1.398(2) . ?
N3 B2 1.563(2) . ?
N3 C9 1.337(2) . ?
N3 C11 1.405(2) . ?
N4 B2 1.582(2) . ?
N4 C13 1.344(2) . ?
N4 C15 1.406(2) . ?
B1 H1A 1.15(2) . ?
B1 H1B 1.098(19) . ?
B2 H2A 1.095(19) . ?
B2 H2B 1.12(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.343(3) . ?
C3 C4 1.493(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C6 H6 0.9300 . ?
C6 C7 1.346(2) . ?
C7 C8 1.495(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10 0.9300 . ?
C10 C11 1.347(3) . ?
C11 C12 1.495(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C15 1.348(3) . ?
C15 C16 1.492(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 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
S1 Pb1 S7 168.273(12) . . ?
S3 Pb1 S1 89.612(13) . . ?
S3 Pb1 S5 76.938(13) . . ?
S3 Pb1 S7 78.687(13) . . ?
S5 Pb1 S1 79.156(12) . . ?
S5 Pb1 S7 97.222(12) . . ?
H1A Pb1 S5 128.2(5) . . ?
C1 S1 Pb1 110.25(6) . . ?
C1 S2 C2 91.13(9) . . ?
C5 S3 Pb1 104.18(6) . . ?
C6 S4 C5 90.96(9) . . ?
C9 S5 Pb1 118.33(6) . . ?
C10 S6 C9 90.82(9) . . ?
C13 S7 Pb1 95.89(6) . . ?
C14 S8 C13 91.33(9) . . ?
C1 N1 B1 122.70(14) . . ?
C1 N1 C3 112.81(15) . . ?
C3 N1 B1 124.20(14) . . ?
C5 N2 B1 124.26(14) . . ?
C5 N2 C7 111.95(14) . . ?
C7 N2 B1 123.68(14) . . ?
C9 N3 B2 122.00(14) . . ?
C9 N3 C11 113.01(14) . . ?
C11 N3 B2 124.99(14) . . ?
C13 N4 B2 121.12(14) . . ?
C13 N4 C15 112.68(14) . . ?
C15 N4 B2 126.15(14) . . ?
N1 B1 N2 107.36(14) . . ?
N1 B1 H1A 109.5(11) . . ?
N1 B1 H1B 107.3(11) . . ?
N2 B1 H1A 109.0(11) . . ?
N2 B1 H1B 110.7(10) . . ?
H1A B1 H1B 112.8(15) . . ?
N3 B2 N4 110.90(14) . . ?
N3 B2 H2A 107.4(10) . . ?
N3 B2 H2B 108.6(10) . . ?
N4 B2 H2A 107.7(10) . . ?
N4 B2 H2B 110.2(11) . . ?
H2A B2 H2B 112.0(14) . . ?
S1 C1 S2 120.63(10) . . ?
N1 C1 S1 127.88(14) . . ?
N1 C1 S2 111.48(12) . . ?
S2 C2 H2 124.3 . . ?
C3 C2 S2 111.32(14) . . ?
C3 C2 H2 124.3 . . ?
N1 C3 C4 121.49(17) . . ?
C2 C3 N1 113.15(16) . . ?
C2 C3 C4 125.33(17) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
S4 C5 S3 118.63(10) . . ?
N2 C5 S3 129.11(13) . . ?
N2 C5 S4 112.17(12) . . ?
S4 C6 H6 124.5 . . ?
C7 C6 S4 111.07(13) . . ?
C7 C6 H6 124.5 . . ?
N2 C7 C8 122.06(15) . . ?
C6 C7 N2 113.76(15) . . ?
C6 C7 C8 124.15(16) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
S5 C9 S6 119.85(10) . . ?
N3 C9 S5 128.12(13) . . ?
N3 C9 S6 111.82(12) . . ?
S6 C10 H10 124.2 . . ?
C11 C10 S6 111.58(13) . . ?
C11 C10 H10 124.2 . . ?
N3 C11 C12 121.77(16) . . ?
C10 C11 N3 112.74(16) . . ?
C10 C11 C12 125.48(16) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
S7 C13 S8 120.30(10) . . ?
N4 C13 S7 128.15(13) . . ?
N4 C13 S8 111.54(13) . . ?
S8 C14 H14 124.4 . . ?
C15 C14 S8 111.23(14) . . ?
C15 C14 H14 124.4 . . ?
N4 C15 C16 122.45(15) . . ?
C14 C15 N4 113.21(16) . . ?
C14 C15 C16 124.33(16) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 1 1 0.0751 -0.0000 1.0000 1.0000 0.0564 0.0443 0.0053
0 -1 -1 0.0721 0.0000 -1.0000 -1.0000 -0.0564 -0.0443 -0.0053
-1 -1 1 0.1415 -1.0000 -1.0000 1.0000 -0.0111 0.0228 0.1141
-1 0 0 0.0892 -1.0000 0.0000 -0.0000 -0.0262 0.0714 0.0161
1 1 0 0.0649 1.0000 1.0000 0.0000 0.0469 -0.0250 -0.0624
1 0 0 0.1018 1.0000 -0.0000 0.0000 0.0262 -0.0714 -0.0161
0 -1 1 0.1383 -0.0000 -1.0000 1.0000 0.0151 -0.0486 0.0980
-1 -1 0 0.1240 -1.0000 -1.0000 -0.0000 -0.0469 0.0250 0.0624
0 1 0 0.1467 -0.0000 1.0000 -0.0000 0.0207 0.0465 -0.0464
0 1 -1 0.1686 0.0000 1.0000 -1.0000 -0.0151 0.0486 -0.0980

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?



_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.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 992112'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound3

_vrf_PLAT772_compound3           
;
PROBLEM: Suspect O-H Bond in CIF:   O1     --  H1      ..       1.95 Ang.  
RESPONSE: no bond, hydrogen bridging distance
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N6 O6 Pb S2'
_chemical_formula_sum            'C14 H12 N6 O6 Pb S2'
_chemical_formula_weight         631.61

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'
S S 0.1246 0.1234 '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           Orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'

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

_cell_length_a                   12.354(5)
_cell_length_b                   16.814(6)
_cell_length_c                   9.0073(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1870.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      5.032
_cell_measurement_theta_max      19.488

_exptl_crystal_description       needle
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    9.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1671
_exptl_absorpt_correction_T_max  0.7680
_exptl_absorpt_process_details   
'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10'

_exptl_special_details           
; 
  
;

_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19912
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2139
_reflns_number_gt                1520
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        
'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_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)+(0.0093P)²+10.8802P] 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         2139
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0515
_refine_ls_wR_factor_gt          0.0450
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.2500 0.2500 0.02246(2) 0.01214(7) Uani 1 2 d S . .
S1 S 0.09982(9) 0.31279(7) 0.23814(13) 0.0133(2) Uani 1 1 d . . .
N1 N 0.1164(3) 0.4639(2) 0.3453(4) 0.0118(8) Uani 1 1 d . . .
H1 H 0.1159 0.4486 0.4387 0.014 Uiso 1 1 calc R . .
N2 N 0.1136(3) 0.4597(2) 0.1039(4) 0.0126(9) Uani 1 1 d . . .
H2 H 0.1105 0.4414 0.0125 0.015 Uiso 1 1 calc R . .
C1 C 0.1111(4) 0.4145(3) 0.2261(6) 0.0112(10) Uani 1 1 d . . .
C2 C 0.1227(4) 0.5429(3) 0.2973(5) 0.0112(9) Uani 1 1 d . . .
C3 C 0.1273(4) 0.6145(3) 0.3747(6) 0.0156(10) Uani 1 1 d . . .
H3 H 0.1273 0.6163 0.4801 0.019 Uiso 1 1 calc R . .
C4 C 0.1319(4) 0.6828(3) 0.2895(6) 0.0193(11) Uani 1 1 d . . .
H4 H 0.1355 0.7330 0.3376 0.023 Uiso 1 1 calc R . .
C5 C 0.1313(4) 0.6798(3) 0.1329(6) 0.0193(11) Uani 1 1 d . . .
H5 H 0.1344 0.7283 0.0787 0.023 Uiso 1 1 calc R . .
C6 C 0.1263(4) 0.6089(3) 0.0558(5) 0.0148(10) Uani 1 1 d . . .
H6 H 0.1259 0.6071 -0.0496 0.018 Uiso 1 1 calc R . .
C7 C 0.1219(4) 0.5399(3) 0.1419(5) 0.0131(10) Uani 1 1 d . . .
O1 O 0.1463(3) 0.1242(2) 0.1015(3) 0.0155(7) Uani 1 1 d . . .
O2 O 0.1376(3) 0.1303(2) 0.3442(3) 0.0170(8) Uani 1 1 d . . .
O3 O 0.1276(3) 0.01595(19) 0.2326(4) 0.0186(7) Uani 1 1 d . . .
N3 N 0.1373(3) 0.0892(2) 0.2289(5) 0.0127(9) 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 O1 2.574(3) . ?
Pb1 O1 2.574(3) 2 ?
Pb1 O2 3.792(3) . ?
Pb1 O2 2.925(3) 7_655 ?
Pb1 O2 2.925(3) 8_565 ?
Pb1 S1 2.8863(13) 2 ?
Pb1 S1 2.8863(13) . ?
S1 C1 1.719(5) . ?
N1 C1 1.360(6) . ?
N1 C2 1.399(6) . ?
N1 H1 0.8800 . ?
N2 C1 1.337(6) . ?
N2 C7 1.396(6) . ?
N2 H2 0.8800 . ?
C2 C3 1.391(7) . ?
C2 C7 1.401(6) . ?
C3 C4 1.383(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.412(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(7) . ?
C6 H6 0.9500 . ?
O1 N3 1.294(5) . ?
O2 N3 1.248(5) . ?
O3 N3 1.238(5) . ?
O1 H1 1.9464 8_565 ?
O1 N1 2.767(5) 8_565 ?
O2 H2 1.9654 8_566 ?
O2 N2 2.802(5) 8_566 ?

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
O1 Pb1 O1 147.87(14) . 2 ?
O1 Pb1 S1 80.40(8) . 2 ?
O1 Pb1 S1 78.13(8) 2 2 ?
O1 Pb1 S1 78.13(8) . . ?
O1 Pb1 S1 80.40(8) 2 . ?
S1 Pb1 S1 95.39(5) 2 . ?
C1 S1 Pb1 105.62(18) . . ?
C1 N1 C2 109.8(4) . . ?
C1 N1 H1 125.1 . . ?
C2 N1 H1 125.1 . . ?
C1 N2 C7 110.4(4) . . ?
C1 N2 H2 124.8 . . ?
C7 N2 H2 124.8 . . ?
N2 C1 N1 107.5(4) . . ?
N2 C1 S1 128.2(4) . . ?
N1 C1 S1 124.2(4) . . ?
C3 C2 N1 131.9(4) . . ?
C3 C2 C7 122.1(5) . . ?
N1 C2 C7 105.9(4) . . ?
C4 C3 C2 116.3(5) . . ?
C4 C3 H3 121.9 . . ?
C2 C3 H3 121.9 . . ?
C3 C4 C5 121.6(5) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C6 C5 C4 122.2(5) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C7 116.1(4) . . ?
C5 C6 H6 122.0 . . ?
C7 C6 H6 122.0 . . ?
N2 C7 C6 132.0(4) . . ?
N2 C7 C2 106.3(4) . . ?
C6 C7 C2 121.7(5) . . ?
N3 O1 Pb1 131.4(3) . . ?
O3 N3 O2 121.9(4) . . ?
O3 N3 O1 119.0(4) . . ?
O2 N3 O1 119.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.454
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.152
_database_code_depnum_ccdc_archive 'CCDC 992113'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound4

_audit_creation_date             2014-06-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C64 H60 N20 O12 Pb2 S8, 2(C4 H8 O), 2(H2 O)'
_chemical_formula_sum            'C72 H80 N20 O16 Pb2 S8'
_chemical_formula_weight         2152.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3940 10.1110 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.8252(2)
_cell_length_b                   20.7570(2)
_cell_length_c                   15.8960(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.0600(6)
_cell_angle_gamma                90
_cell_volume                     8521.10(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    94289
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      30.034
_cell_measurement_temperature    100(2)
_shelx_estimated_absorpt_T_max   0.678
_shelx_estimated_absorpt_T_min   0.407
_exptl_absorpt_coefficient_mu    4.218
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.690436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24540
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.155
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9591
_reflns_number_total             12428
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.774
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         12428
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0359P)²+22.5869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0823
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O8A, O8B}
{C34A, C34B}
3. Restrained distances
 C33A-C34A \\sim C34A-C35A
 with sigma of 0.02
 C33B-C34B \\sim C34B-C35B
 with sigma of 0.02
 C16-C13 \\sim C16B-C14
 with sigma of 0.02
 C24B-C21 \\sim C24-C22
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O8A) = Uanis(O8B)
Uanis(C34A) = Uanis(C34B)
5. Same fragment restrains
{O8A, C36A, C35A, C34A, C33A}
as
{O8A, C33A, C34A, C35A, C36A}
{O8B, C36B, C35B, C34B, C33B}
as
{O8B, C33B, C34B, C35B, C36B}
6. Others
 Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(O8B)=Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=
 Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=1-FVAR(3)
 Sof(O8A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C33A(H33A,H33B), C34A(H34A,H34B), C35A(H35A,H35B), C36A(H36A,H36B), C33B(H33C,
 H33D), C34B(H34C,H34D), C35B(H35C,H35D), C36B(H36C,H36D)
7.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), C4(H4A),
 C5(H5A), C7(H7A), C12(H12), C15(H15), C20(H20), C23(H23), C28(H28), C29(H29),
 C31(H31)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C24(H24A,H24B,
 H24C), C24B(H24D,H24E,H24F), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.19451(2) 0.16886(2) 0.95821(2) 0.03023(4) Uani 1 1 d . . . . .
S1 S 0.28631(3) 0.25341(4) 0.89885(5) 0.03148(16) Uani 1 1 d . . . . .
S2 S 0.13228(4) 0.28822(5) 0.95664(6) 0.0495(2) Uani 1 1 d . . . . .
S3 S 0.14362(3) 0.10114(4) 1.09116(5) 0.03342(17) Uani 1 1 d . . . . .
S4 S 0.27874(4) 0.07585(4) 1.00066(5) 0.03623(18) Uani 1 1 d . . . . .
N1 N 0.24514(11) 0.26511(14) 0.74315(16) 0.0334(6) Uani 1 1 d . . . . .
H1 H 0.2528 0.2252 0.7292 0.040 Uiso 1 1 calc R . . . .
N2 N 0.23760(11) 0.35334(14) 0.81649(16) 0.0318(6) Uani 1 1 d . . . . .
H2 H 0.2398 0.3811 0.8582 0.038 Uiso 1 1 calc R . . . .
N3 N 0.10057(13) 0.26035(17) 0.7962(2) 0.0466(8) Uani 1 1 d . . . . .
H3 H 0.1078 0.2189 0.7980 0.056 Uiso 1 1 calc R . . . .
N4 N 0.09290(12) 0.36135(17) 0.8311(2) 0.0484(8) Uani 1 1 d . . . . .
H4 H 0.0945 0.3973 0.8603 0.058 Uiso 1 1 calc R . . . .
N5 N 0.09242(11) 0.02757(15) 0.97416(17) 0.0364(6) Uani 1 1 d . . . . .
H5 H 0.1002 0.0519 0.9306 0.044 Uiso 1 1 calc R . . . .
N6 N 0.08896(11) -0.00938(14) 1.10192(19) 0.0395(7) Uani 1 1 d . . . . .
H6 H 0.0943 -0.0137 1.1563 0.047 Uiso 1 1 calc R . . . .
N7 N 0.21914(11) -0.00082(14) 0.90049(17) 0.0357(6) Uani 1 1 d . . . . .
H7 H 0.2227 0.0237 0.8557 0.043 Uiso 1 1 calc R . . . .
N8 N 0.22423(12) -0.03503(13) 1.02917(18) 0.0375(6) Uani 1 1 d . . . . .
H8 H 0.2319 -0.0370 1.0831 0.045 Uiso 1 1 calc R . . . .
C1 C 0.25522(13) 0.29272(16) 0.81848(19) 0.0308(6) Uani 1 1 d . . . . .
C2 C 0.22079(13) 0.30954(18) 0.6915(2) 0.0349(7) Uani 1 1 d . . . . .
C3 C 0.21513(13) 0.36580(17) 0.7382(2) 0.0343(7) Uani 1 1 d . . . . .
C4 C 0.19222(14) 0.4203(2) 0.7045(2) 0.0424(8) Uani 1 1 d . . . . .
H4A H 0.1882 0.4588 0.7361 0.051 Uiso 1 1 calc R . . . .
C5 C 0.17548(14) 0.4151(2) 0.6216(2) 0.0465(10) Uani 1 1 d . . . . .
H5A H 0.1592 0.4513 0.5966 0.056 Uiso 1 1 calc R . . . .
C6 C 0.18126(15) 0.3601(2) 0.5736(2) 0.0486(10) Uani 1 1 d . . . . .
C7 C 0.20405(15) 0.3057(2) 0.6081(2) 0.0436(9) Uani 1 1 d . . . . .
H7A H 0.2081 0.2673 0.5763 0.052 Uiso 1 1 calc R . . . .
C8 C 0.16308(19) 0.3586(3) 0.4830(3) 0.0647(14) Uani 1 1 d . . . . .
H8A H 0.1778 0.3209 0.4547 0.097 Uiso 1 1 calc GR . . . .
H8B H 0.1744 0.3979 0.4543 0.097 Uiso 1 1 calc GR . . . .
H8C H 0.1252 0.3560 0.4815 0.097 Uiso 1 1 calc GR . . . .
C9 C 0.10847(15) 0.30244(19) 0.8590(2) 0.0435(8) Uani 1 1 d . . . . .
C10 C 0.07903(16) 0.2928(2) 0.7274(3) 0.0549(11) Uani 1 1 d . . . . .
C11 C 0.07432(14) 0.3559(2) 0.7503(3) 0.0536(11) Uani 1 1 d . . . . .
C12 C 0.05390(16) 0.4025(3) 0.6960(4) 0.0736(17) Uani 1 1 d . . . . .
H12 H 0.0509 0.4462 0.7127 0.088 Uiso 1 1 calc R . . . .
C13 C 0.03848(19) 0.3826(4) 0.6181(4) 0.087(2) Uani 1 1 d . . . . .
C14 C 0.0427(2) 0.3182(4) 0.5946(3) 0.091(2) Uani 1 1 d . . . . .
C15 C 0.0639(2) 0.2709(3) 0.6486(3) 0.0768(17) Uani 1 1 d . . . . .
H15 H 0.0675 0.2272 0.6321 0.092 Uiso 1 1 calc R . . . .
C16 C 0.0168(3) 0.4269(6) 0.5544(6) 0.131(5) Uani 0.737(10) 1 d . . P A 1
H16A H -0.0067 0.4030 0.5172 0.196 Uiso 0.737(10) 1 calc GR . P A 1
H16B H 0.0450 0.4455 0.5212 0.196 Uiso 0.737(10) 1 calc GR . P A 1
H16C H -0.0024 0.4614 0.5826 0.196 Uiso 0.737(10) 1 calc GR . P A 1
C16B C 0.0253(8) 0.3035(11) 0.5092(10) 0.072(6) Uiso 0.263(10) 1 d . . P A 2
H16D H -0.0120 0.2948 0.5096 0.109 Uiso 0.263(10) 1 calc GR . P A 2
H16E H 0.0438 0.2655 0.4883 0.109 Uiso 0.263(10) 1 calc GR . P A 2
H16F H 0.0324 0.3404 0.4725 0.109 Uiso 0.263(10) 1 calc GR . P A 2
C17 C 0.10821(13) 0.03829(16) 1.0536(2) 0.0328(7) Uani 1 1 d . . . . .
C18 C 0.06215(14) -0.02740(19) 0.9711(2) 0.0425(9) Uani 1 1 d . . . . .
C19 C 0.05938(14) -0.05079(18) 1.0524(3) 0.0457(9) Uani 1 1 d . . . . .
C20 C 0.02997(17) -0.1048(2) 1.0723(4) 0.0622(12) Uani 1 1 d . . . . .
H20 H 0.0276 -0.1204 1.1283 0.075 Uiso 1 1 calc R . . . .
C21 C 0.00413(17) -0.1349(2) 1.0062(4) 0.0709(16) Uani 1 1 d . . . . .
C22 C 0.00846(16) -0.1121(3) 0.9233(4) 0.0732(18) Uani 1 1 d . . . . .
C23 C 0.03706(15) -0.0578(3) 0.9052(3) 0.0597(13) Uani 1 1 d . . . . .
H23 H 0.0395 -0.0418 0.8494 0.072 Uiso 1 1 calc R . . . .
C24 C -0.0177(3) -0.1551(5) 0.8629(6) 0.081(3) Uani 0.643(10) 1 d . . P B 1
H24A H 0.0080 -0.1828 0.8357 0.121 Uiso 0.643(10) 1 calc GR . P B 1
H24B H -0.0355 -0.1292 0.8202 0.121 Uiso 0.643(10) 1 calc GR . P B 1
H24C H -0.0430 -0.1818 0.8928 0.121 Uiso 0.643(10) 1 calc GR . P B 1
C24B C -0.0257(5) -0.1922(6) 1.0027(8) 0.054(4) Uiso 0.357(10) 1 d . . P B 2
H24D H -0.0270 -0.2118 1.0587 0.080 Uiso 0.357(10) 1 calc GR . P B 2
H24E H -0.0097 -0.2224 0.9631 0.080 Uiso 0.357(10) 1 calc GR . P B 2
H24F H -0.0609 -0.1820 0.9839 0.080 Uiso 0.357(10) 1 calc GR . P B 2
C25 C 0.23889(14) 0.01209(16) 0.9769(2) 0.0342(7) Uani 1 1 d . . . . .
C26 C 0.19219(13) -0.05867(17) 0.9029(2) 0.0363(7) Uani 1 1 d . . . . .
C27 C 0.19521(15) -0.08023(16) 0.9861(2) 0.0385(8) Uani 1 1 d . . . . .
C28 C 0.17089(16) -0.13700(18) 1.0119(3) 0.0457(9) Uani 1 1 d . . . . .
H28 H 0.1715 -0.1507 1.0689 0.055 Uiso 1 1 calc R . . . .
C29 C 0.14602(16) -0.17206(18) 0.9508(3) 0.0453(9) Uani 1 1 d . . . . .
H29 H 0.1292 -0.2110 0.9663 0.054 Uiso 1 1 calc R . . . .
C30 C 0.14452(14) -0.15265(19) 0.8662(3) 0.0441(9) Uani 1 1 d . . . . .
C31 C 0.16700(14) -0.09509(19) 0.8414(2) 0.0405(8) Uani 1 1 d . . . . .
H31 H 0.1653 -0.0809 0.7847 0.049 Uiso 1 1 calc R . . . .
C32 C 0.11796(18) -0.1957(2) 0.8031(3) 0.0545(10) Uani 1 1 d . . . . .
H32A H 0.1074 -0.1701 0.7541 0.082 Uiso 1 1 calc GR . . . .
H32B H 0.0873 -0.2152 0.8289 0.082 Uiso 1 1 calc GR . . . .
H32C H 0.1419 -0.2297 0.7852 0.082 Uiso 1 1 calc GR . . . .
O1 O 0.23219(12) 0.11369(13) 0.79946(15) 0.0501(7) Uani 1 1 d . . . . .
O2 O 0.23902(13) 0.03996(13) 0.70507(17) 0.0548(8) Uani 1 1 d . . . . .
O3 O 0.25218(12) 0.14019(13) 0.67269(15) 0.0495(7) Uani 1 1 d . . . . .
N9 N 0.24091(12) 0.09816(15) 0.72542(18) 0.0392(7) Uani 1 1 d . . . . .
O4 O 0.11138(11) 0.12512(13) 0.85098(15) 0.0446(6) Uani 1 1 d . . . . .
O5 O 0.10773(13) 0.03748(14) 0.77692(17) 0.0537(7) Uani 1 1 d . . . . .
O6 O 0.11920(13) 0.12959(15) 0.71554(16) 0.0560(8) Uani 1 1 d . . . . .
N10 N 0.11269(12) 0.09668(16) 0.77923(18) 0.0422(7) Uani 1 1 d . . . . .
O7 O 0.11490(17) 0.4825(2) 0.9065(3) 0.0962(13) Uani 1 1 d . . . . .
O8A O 0.1090(3) 0.5713(3) 0.7743(4) 0.141(2) Uani 0.491(12) 1 d . . P C 1
C33A C 0.1182(9) 0.5647(8) 0.6848(8) 0.117(7) Uani 0.491(12) 1 d . . P C 1
H33A H 0.1551 0.5738 0.6725 0.141 Uiso 0.491(12) 1 calc R . P C 1
H33B H 0.1107 0.5200 0.6672 0.141 Uiso 0.491(12) 1 calc R . P C 1
C34A C 0.0876(4) 0.6063(6) 0.6408(5) 0.170(5) Uani 0.491(12) 1 d . . P C 1
H34A H 0.0527 0.5877 0.6326 0.204 Uiso 0.491(12) 1 calc R . P C 1
H34B H 0.1029 0.6154 0.5849 0.204 Uiso 0.491(12) 1 calc R . P C 1
C35A C 0.0847(5) 0.6646(5) 0.6903(7) 0.072(4) Uani 0.491(12) 1 d . . P C 1
H35A H 0.0486 0.6795 0.6978 0.086 Uiso 0.491(12) 1 calc R . P C 1
H35B H 0.1059 0.6997 0.6661 0.086 Uiso 0.491(12) 1 calc R . P C 1
C36A C 0.1067(8) 0.6397(6) 0.7679(12) 0.146(10) Uani 0.491(12) 1 d . . P C 1
H36A H 0.1422 0.6570 0.7740 0.175 Uiso 0.491(12) 1 calc R . P C 1
H36B H 0.0860 0.6563 0.8156 0.175 Uiso 0.491(12) 1 calc R . P C 1
O8B O 0.1090(3) 0.5713(3) 0.7743(4) 0.141(2) Uani 0.509(12) 1 d . . P C 2
C33B C 0.1343(4) 0.6034(7) 0.7063(10) 0.093(5) Uani 0.509(12) 1 d . . P C 2
H33C H 0.1638 0.5781 0.6843 0.112 Uiso 0.509(12) 1 calc R . P C 2
H33D H 0.1463 0.6470 0.7225 0.112 Uiso 0.509(12) 1 calc R . P C 2
C34B C 0.0876(4) 0.6063(6) 0.6408(5) 0.170(5) Uani 0.509(12) 1 d . . P C 2
H34C H 0.0944 0.6369 0.5944 0.204 Uiso 0.509(12) 1 calc R . P C 2
H34D H 0.0792 0.5633 0.6175 0.204 Uiso 0.509(12) 1 calc R . P C 2
C35B C 0.0464(6) 0.6303(14) 0.6999(10) 0.191(13) Uani 0.509(12) 1 d . . P C 2
H35C H 0.0117 0.6157 0.6816 0.229 Uiso 0.509(12) 1 calc R . P C 2
H35D H 0.0465 0.6780 0.7026 0.229 Uiso 0.509(12) 1 calc R . P C 2
C36B C 0.0605(6) 0.6011(9) 0.7860(11) 0.128(7) Uani 0.509(12) 1 d . . P C 2
H36C H 0.0628 0.6352 0.8295 0.154 Uiso 0.509(12) 1 calc R . P C 2
H36D H 0.0342 0.5691 0.8036 0.154 Uiso 0.509(12) 1 calc R . P C 2


_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 S1 2.8300(8) 7_557 ?
Pb1 S1 3.0977(9) . ?
Pb1 S2 2.9532(10) . ?
Pb1 S3 2.8592(8) . ?
Pb1 S4 2.9852(9) . ?
S1 Pb1 2.8300(8) 7_557 ?
S1 C1 1.715(3) . ?
S2 C9 1.695(4) . ?
S3 C17 1.701(4) . ?
S4 C25 1.718(4) . ?
N1 H1 0.8800 . ?
N1 C1 1.353(4) . ?
N1 C2 1.385(4) . ?
N2 H2 0.8800 . ?
N2 C1 1.338(4) . ?
N2 C3 1.397(4) . ?
N3 H3 0.8800 . ?
N3 C9 1.342(5) . ?
N3 C10 1.398(5) . ?
N4 H4 0.8800 . ?
N4 C9 1.361(5) . ?
N4 C11 1.377(6) . ?
N5 H5 0.8800 . ?
N5 C17 1.345(4) . ?
N5 C18 1.384(5) . ?
N6 H6 0.8800 . ?
N6 C17 1.348(4) . ?
N6 C19 1.393(5) . ?
N7 H7 0.8800 . ?
N7 C25 1.344(4) . ?
N7 C26 1.388(5) . ?
N8 H8 0.8800 . ?
N8 C25 1.338(4) . ?
N8 C27 1.382(5) . ?
C2 C3 1.391(5) . ?
C2 C7 1.396(5) . ?
C3 C4 1.384(5) . ?
C4 H4A 0.9500 . ?
C4 C5 1.391(5) . ?
C5 H5A 0.9500 . ?
C5 C6 1.380(6) . ?
C6 C7 1.386(6) . ?
C6 C8 1.515(5) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 C11 1.365(7) . ?
C10 C15 1.388(7) . ?
C11 C12 1.399(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.364(9) . ?
C13 C14 1.393(10) . ?
C13 C16 1.477(8) . ?
C14 C15 1.413(8) . ?
C14 C16B 1.461(15) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C18 C19 1.383(6) . ?
C18 C23 1.383(5) . ?
C19 C20 1.390(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.392(7) . ?
C21 C22 1.404(8) . ?
C21 C24B 1.419(11) . ?
C22 C23 1.378(8) . ?
C22 C24 1.474(8) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C26 C27 1.398(5) . ?
C26 C31 1.396(5) . ?
C27 C28 1.397(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.372(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.404(6) . ?
C30 C31 1.386(6) . ?
C30 C32 1.508(6) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O1 N9 1.241(3) . ?
O2 N9 1.251(4) . ?
O3 N9 1.245(4) . ?
O4 N10 1.285(4) . ?
O5 N10 1.236(4) . ?
O6 N10 1.233(4) . ?
O8A C33A 1.448(13) . ?
O8A C36A 1.425(13) . ?
C33A H33A 0.9900 . ?
C33A H33B 0.9900 . ?
C33A C34A 1.363(13) . ?
C34A H34A 0.9900 . ?
C34A H34B 0.9900 . ?
C34A C35A 1.445(12) . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C35A C36A 1.453(14) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C33B H33C 0.9900 . ?
C33B H33D 0.9900 . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C35B C36B 1.541(15) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?

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
S1 Pb1 S1 77.77(2) 7_557 . ?
S1 Pb1 S2 67.87(3) 7_557 . ?
S1 Pb1 S3 76.53(2) 7_557 . ?
S1 Pb1 S4 93.46(2) 7_557 . ?
S2 Pb1 S1 86.49(3) . . ?
S2 Pb1 S4 160.20(3) . . ?
S3 Pb1 S1 148.89(2) . . ?
S3 Pb1 S2 99.68(3) . . ?
S3 Pb1 S4 81.39(2) . . ?
S4 Pb1 S1 82.96(2) . . ?
Pb1 S1 Pb1 102.23(2) 7_557 . ?
C1 S1 Pb1 114.10(11) . 7_557 ?
C1 S1 Pb1 97.97(11) . . ?
C9 S2 Pb1 110.53(14) . . ?
C17 S3 Pb1 111.38(12) . . ?
C25 S4 Pb1 90.71(11) . . ?
C1 N1 H1 125.4 . . ?
C1 N1 C2 109.2(3) . . ?
C2 N1 H1 125.4 . . ?
C1 N2 H2 125.2 . . ?
C1 N2 C3 109.6(3) . . ?
C3 N2 H2 125.2 . . ?
C9 N3 H3 125.4 . . ?
C9 N3 C10 109.1(4) . . ?
C10 N3 H3 125.4 . . ?
C9 N4 H4 125.3 . . ?
C9 N4 C11 109.4(4) . . ?
C11 N4 H4 125.3 . . ?
C17 N5 H5 125.0 . . ?
C17 N5 C18 109.9(3) . . ?
C18 N5 H5 125.0 . . ?
C17 N6 H6 125.3 . . ?
C17 N6 C19 109.4(3) . . ?
C19 N6 H6 125.3 . . ?
C25 N7 H7 125.2 . . ?
C25 N7 C26 109.7(3) . . ?
C26 N7 H7 125.2 . . ?
C25 N8 H8 125.0 . . ?
C25 N8 C27 110.0(3) . . ?
C27 N8 H8 125.0 . . ?
N1 C1 S1 123.2(3) . . ?
N2 C1 S1 128.6(2) . . ?
N2 C1 N1 108.2(3) . . ?
N1 C2 C3 106.9(3) . . ?
N1 C2 C7 131.7(4) . . ?
C3 C2 C7 121.4(4) . . ?
C2 C3 N2 106.0(3) . . ?
C4 C3 N2 132.3(3) . . ?
C4 C3 C2 121.7(3) . . ?
C3 C4 H4A 122.1 . . ?
C3 C4 C5 115.8(4) . . ?
C5 C4 H4A 122.1 . . ?
C4 C5 H5A 118.2 . . ?
C6 C5 C4 123.7(4) . . ?
C6 C5 H5A 118.2 . . ?
C5 C6 C7 120.1(3) . . ?
C5 C6 C8 120.6(4) . . ?
C7 C6 C8 119.3(4) . . ?
C2 C7 H7A 121.3 . . ?
C6 C7 C2 117.4(4) . . ?
C6 C7 H7A 121.3 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 S2 128.5(3) . . ?
N3 C9 N4 107.4(3) . . ?
N4 C9 S2 124.1(3) . . ?
C11 C10 N3 106.8(4) . . ?
C11 C10 C15 121.9(4) . . ?
C15 C10 N3 131.3(5) . . ?
N4 C11 C12 130.5(5) . . ?
C10 C11 N4 107.3(3) . . ?
C10 C11 C12 122.2(5) . . ?
C11 C12 H12 121.3 . . ?
C13 C12 C11 117.4(6) . . ?
C13 C12 H12 121.3 . . ?
C12 C13 C14 120.7(5) . . ?
C12 C13 C16 123.0(9) . . ?
C14 C13 C16 116.3(8) . . ?
C13 C14 C15 122.2(5) . . ?
C13 C14 C16B 115.1(10) . . ?
C15 C14 C16B 122.6(11) . . ?
C10 C15 C14 115.5(6) . . ?
C10 C15 H15 122.2 . . ?
C14 C15 H15 122.2 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C16B H16D 109.5 . . ?
C14 C16B H16E 109.5 . . ?
C14 C16B H16F 109.5 . . ?
H16D C16B H16E 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
N5 C17 S3 128.3(3) . . ?
N5 C17 N6 107.6(3) . . ?
N6 C17 S3 124.1(2) . . ?
C19 C18 N5 106.6(3) . . ?
C23 C18 N5 131.9(4) . . ?
C23 C18 C19 121.5(4) . . ?
C18 C19 N6 106.4(3) . . ?
C18 C19 C20 121.6(4) . . ?
C20 C19 N6 131.9(4) . . ?
C19 C20 H20 121.6 . . ?
C19 C20 C21 116.8(5) . . ?
C21 C20 H20 121.6 . . ?
C20 C21 C22 121.2(5) . . ?
C20 C21 C24B 131.7(8) . . ?
C22 C21 C24B 106.8(7) . . ?
C21 C22 C24 111.7(7) . . ?
C23 C22 C21 120.9(4) . . ?
C23 C22 C24 127.2(7) . . ?
C18 C23 H23 121.1 . . ?
C22 C23 C18 117.8(5) . . ?
C22 C23 H23 121.1 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C24B H24D 109.5 . . ?
C21 C24B H24E 109.5 . . ?
C21 C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N7 C25 S4 125.3(3) . . ?
N8 C25 S4 126.6(3) . . ?
N8 C25 N7 107.9(3) . . ?
N7 C26 C27 106.0(3) . . ?
N7 C26 C31 133.0(3) . . ?
C31 C26 C27 120.9(3) . . ?
N8 C27 C26 106.3(3) . . ?
N8 C27 C28 132.1(3) . . ?
C28 C27 C26 121.5(4) . . ?
C27 C28 H28 121.6 . . ?
C29 C28 C27 116.7(4) . . ?
C29 C28 H28 121.6 . . ?
C28 C29 H29 118.7 . . ?
C28 C29 C30 122.5(4) . . ?
C30 C29 H29 118.7 . . ?
C29 C30 C32 118.6(4) . . ?
C31 C30 C29 120.5(4) . . ?
C31 C30 C32 120.8(4) . . ?
C26 C31 H31 121.2 . . ?
C30 C31 C26 117.6(3) . . ?
C30 C31 H31 121.2 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 N9 O2 119.3(3) . . ?
O1 N9 O3 120.0(3) . . ?
O3 N9 O2 120.8(3) . . ?
O5 N10 O4 118.7(3) . . ?
O6 N10 O4 118.6(3) . . ?
O6 N10 O5 122.7(3) . . ?
C36A O8A C33A 91.8(12) . . ?
O8A C33A H33A 109.6 . . ?
O8A C33A H33B 109.6 . . ?
H33A C33A H33B 108.1 . . ?
C34A C33A O8A 110.4(11) . . ?
C34A C33A H33A 109.6 . . ?
C34A C33A H33B 109.6 . . ?
C33A C34A H34A 110.5 . . ?
C33A C34A H34B 110.5 . . ?
C33A C34A C35A 106.3(10) . . ?
H34A C34A H34B 108.7 . . ?
C35A C34A H34A 110.5 . . ?
C35A C34A H34B 110.5 . . ?
C34A C35A H35A 112.1 . . ?
C34A C35A H35B 112.1 . . ?
C34A C35A C36A 98.3(9) . . ?
H35A C35A H35B 109.7 . . ?
C36A C35A H35A 112.1 . . ?
C36A C35A H35B 112.1 . . ?
O8A C36A C35A 115.5(11) . . ?
O8A C36A H36A 108.4 . . ?
O8A C36A H36B 108.4 . . ?
C35A C36A H36A 108.4 . . ?
C35A C36A H36B 108.4 . . ?
H36A C36A H36B 107.5 . . ?
H33C C33B H33D 109.6 . . ?
H35C C35B H35D 108.8 . . ?
C36B C35B H35C 110.8 . . ?
C36B C35B H35D 110.8 . . ?
C35B C36B H36C 110.7 . . ?
C35B C36B H36D 110.7 . . ?
H36C C36B H36D 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 S1 C1 N1 176.2(2) 7_557 . . . ?
Pb1 S1 C1 N1 -76.5(3) . . . . ?
Pb1 S1 C1 N2 -2.8(3) 7_557 . . . ?
Pb1 S1 C1 N2 104.4(3) . . . . ?
Pb1 S2 C9 N3 22.7(4) . . . . ?
Pb1 S2 C9 N4 -158.3(3) . . . . ?
Pb1 S3 C17 N5 -17.1(3) . . . . ?
Pb1 S3 C17 N6 165.9(3) . . . . ?
Pb1 S4 C25 N7 63.9(3) . . . . ?
Pb1 S4 C25 N8 -119.8(3) . . . . ?
N1 C2 C3 N2 1.3(4) . . . . ?
N1 C2 C3 C4 179.7(3) . . . . ?
N1 C2 C7 C6 -179.1(3) . . . . ?
N2 C3 C4 C5 177.8(3) . . . . ?
N3 C10 C11 N4 0.3(4) . . . . ?
N3 C10 C11 C12 -180.0(4) . . . . ?
N3 C10 C15 C14 179.2(4) . . . . ?
N4 C11 C12 C13 179.8(4) . . . . ?
N5 C18 C19 N6 -0.9(4) . . . . ?
N5 C18 C19 C20 177.5(4) . . . . ?
N5 C18 C23 C22 -178.6(4) . . . . ?
N6 C19 C20 C21 179.0(4) . . . . ?
N7 C26 C27 N8 -0.8(4) . . . . ?
N7 C26 C27 C28 178.3(3) . . . . ?
N7 C26 C31 C30 178.6(3) . . . . ?
N8 C27 C28 C29 -178.1(4) . . . . ?
C1 N1 C2 C3 -1.1(4) . . . . ?
C1 N1 C2 C7 177.8(4) . . . . ?
C1 N2 C3 C2 -1.0(4) . . . . ?
C1 N2 C3 C4 -179.2(4) . . . . ?
C2 N1 C1 S1 -178.7(2) . . . . ?
C2 N1 C1 N2 0.5(4) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C3 N2 C1 S1 179.5(3) . . . . ?
C3 N2 C1 N1 0.3(4) . . . . ?
C3 C2 C7 C6 -0.3(5) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C4 C5 C6 C7 1.1(6) . . . . ?
C4 C5 C6 C8 -178.6(4) . . . . ?
C5 C6 C7 C2 -0.5(5) . . . . ?
C7 C2 C3 N2 -177.7(3) . . . . ?
C7 C2 C3 C4 0.7(5) . . . . ?
C8 C6 C7 C2 179.2(3) . . . . ?
C9 N3 C10 C11 0.3(5) . . . . ?
C9 N3 C10 C15 -179.8(5) . . . . ?
C9 N4 C11 C10 -0.7(4) . . . . ?
C9 N4 C11 C12 179.6(4) . . . . ?
C10 N3 C9 S2 178.4(3) . . . . ?
C10 N3 C9 N4 -0.7(4) . . . . ?
C10 C11 C12 C13 0.1(6) . . . . ?
C11 N4 C9 S2 -178.3(3) . . . . ?
C11 N4 C9 N3 0.8(4) . . . . ?
C11 C10 C15 C14 -0.8(7) . . . . ?
C11 C12 C13 C14 0.5(7) . . . . ?
C11 C12 C13 C16 -179.4(5) . . . . ?
C12 C13 C14 C15 -1.3(8) . . . . ?
C12 C13 C14 C16B -179.4(10) . . . . ?
C13 C14 C15 C10 1.4(8) . . . . ?
C15 C10 C11 N4 -179.7(4) . . . . ?
C15 C10 C11 C12 0.1(7) . . . . ?
C16 C13 C14 C15 178.6(5) . . . . ?
C16 C13 C14 C16B 0.5(12) . . . . ?
C16B C14 C15 C10 179.4(11) . . . . ?
C17 N5 C18 C19 0.2(4) . . . . ?
C17 N5 C18 C23 179.6(4) . . . . ?
C17 N6 C19 C18 1.3(4) . . . . ?
C17 N6 C19 C20 -176.8(4) . . . . ?
C18 N5 C17 S3 -176.8(3) . . . . ?
C18 N5 C17 N6 0.6(4) . . . . ?
C18 C19 C20 C21 1.1(6) . . . . ?
C19 N6 C17 S3 176.4(3) . . . . ?
C19 N6 C17 N5 -1.1(4) . . . . ?
C19 C18 C23 C22 0.8(6) . . . . ?
C19 C20 C21 C22 1.0(7) . . . . ?
C19 C20 C21 C24B 175.0(8) . . . . ?
C20 C21 C22 C23 -2.3(7) . . . . ?
C20 C21 C22 C24 174.2(5) . . . . ?
C21 C22 C23 C18 1.3(6) . . . . ?
C23 C18 C19 N6 179.6(3) . . . . ?
C23 C18 C19 C20 -2.0(6) . . . . ?
C24 C22 C23 C18 -174.5(5) . . . . ?
C24B C21 C22 C23 -177.6(6) . . . . ?
C24B C21 C22 C24 -1.2(8) . . . . ?
C25 N7 C26 C27 1.5(4) . . . . ?
C25 N7 C26 C31 -176.3(4) . . . . ?
C25 N8 C27 C26 -0.2(4) . . . . ?
C25 N8 C27 C28 -179.2(4) . . . . ?
C26 N7 C25 S4 175.2(2) . . . . ?
C26 N7 C25 N8 -1.6(4) . . . . ?
C26 C27 C28 C29 3.0(5) . . . . ?
C27 N8 C25 S4 -175.6(3) . . . . ?
C27 N8 C25 N7 1.1(4) . . . . ?
C27 C26 C31 C30 1.0(5) . . . . ?
C27 C28 C29 C30 -0.1(6) . . . . ?
C28 C29 C30 C31 -2.3(6) . . . . ?
C28 C29 C30 C32 177.7(4) . . . . ?
C29 C30 C31 C26 1.8(5) . . . . ?
C31 C26 C27 N8 177.4(3) . . . . ?
C31 C26 C27 C28 -3.5(5) . . . . ?
C32 C30 C31 C26 -178.2(4) . . . . ?
O8A C33A C34A C35A 36.8(19) . . . . ?
C33A O8A C36A C35A 33.8(19) . . . . ?
C33A C34A C35A C36A -12.4(17) . . . . ?
C34A C35A C36A O8A -16(2) . . . . ?
C36A O8A C33A C34A -41.4(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_database_code_depnum_ccdc_archive 'CCDC 1008780'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound5

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H4 N4 O4 Pb S'
_chemical_formula_sum            'C2 H4 N4 O4 Pb S'
_chemical_formula_weight         387.34

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'
O O 0.0492 0.0322 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

_cell_length_a                   17.9942(7)
_cell_length_b                   6.3605(2)
_cell_length_c                   13.1333(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1503.13(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9816
_cell_measurement_theta_min      4.169
_cell_measurement_theta_max      71.466

_exptl_crystal_description       needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.423
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    46.229
_shelx_estimated_absorpt_T_min   0.023
_shelx_estimated_absorpt_T_max   0.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0231
_exptl_absorpt_correction_T_max  0.3377
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'I\mS Incoatec Microfocus'
_diffrn_radiation_monochromator  'Quazar Montel multilayer optic Montel200'
_diffrn_measurement_device_type  'Bruker AXS X8 Prospector Ultra with APEX II'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27266
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.915
_diffrn_reflns_theta_max         69.973
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1418
_reflns_number_gt                1393
_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       'APEX 2, Bruker AXS'
_computing_cell_refinement       'APEX 2, Bruker AXS'
_computing_data_reduction        'APEX 2, Bruker AXS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0287P)²+5.8247P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000059(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1418
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0553
_refine_ls_wR_factor_gt          0.0550
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.195
_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_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
Pb1 Pb 0.34677(2) 0.18855(3) 0.48212(2) 0.01250(12) Uani 1 1 d . . . . .
S1 S 0.32482(7) 0.6241(2) 0.50658(8) 0.0147(2) Uani 1 1 d . . . . .
N1 N 0.2199(2) 0.6706(5) 0.6524(3) 0.0118(7) Uani 1 1 d . . . . .
N2 N 0.3311(2) 0.6691(6) 0.7157(3) 0.0135(8) Uani 1 1 d . . . . .
H2 H 0.373(4) 0.679(8) 0.725(5) 0.016 Uiso 1 1 d . U . . .
N3 N 0.2852(2) 0.6989(6) 0.7972(3) 0.0130(8) Uani 1 1 d . . . . .
C1 C 0.2925(2) 0.6522(7) 0.6303(4) 0.0138(9) Uani 1 1 d . . . . .
C2 C 0.2189(3) 0.7005(7) 0.7551(4) 0.0137(9) Uani 1 1 d . . . . .
H2A H 0.177(4) 0.729(9) 0.788(5) 0.016 Uiso 1 1 d . U . . .
O1 O 0.45722(19) 0.3048(5) 0.6009(3) 0.0219(8) Uani 1 1 d . . . . .
O2 O 0.55153(17) 0.1258(6) 0.6578(3) 0.0219(7) Uani 1 1 d . . . . .
O3 O 0.45288(17) -0.0358(5) 0.6019(3) 0.0218(7) Uani 1 1 d . . . . .
N4 N 0.4879(2) 0.1306(7) 0.6212(3) 0.0164(8) Uani 1 1 d . . . . .
O4 O 0.44780(19) 0.3576(7) 0.3520(3) 0.0177(7) Uani 1 1 d . . . . .
H4A H 0.478(4) 0.283(10) 0.361(5) 0.021 Uiso 1 1 d . U . . .
H4B H 0.465(3) 0.458(10) 0.365(5) 0.021 Uiso 1 1 d . 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
Pb1 N1 2.540(4) 7_655 ?
Pb1 O1 2.632(3) . ?
Pb1 O3 2.856(3) . ?
Pb1 O4 2.716(3) . ?
Pb1 N3 2.764(4) 8_565 ?
Pb1 S1 2.8167(13) . ?
Pb1 S1 3.1314(12) 7_655 ?
S1 C1 1.735(5) . ?
N1 C1 1.344(6) . ?
N1 C2 1.362(6) . ?
N1 Pb1 2.540(4) 7_665 ?
N2 C1 1.324(6) . ?
N2 N3 1.365(5) . ?
N2 H2 0.76(6) . ?
N3 C2 1.316(6) . ?
N3 Pb1 2.764(4) 8_566 ?
C2 H2A 0.90(6) . ?
O1 N4 1.267(5) . ?
O2 N4 1.241(5) . ?
O3 N4 1.258(5) . ?
O4 H4A 0.73(6) . ?
O4 H4B 0.73(6) . ?

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
S1 Pb1 O3 121.49(7) . . ?
O4 Pb1 O3 95.56(10) . . ?
N1 Pb1 O1 81.22(12) 7_655 . ?
N1 Pb1 O4 152.54(11) 7_655 . ?
O1 Pb1 O4 75.88(12) . . ?
N1 Pb1 N3 126.58(12) 7_655 8_565 ?
O1 Pb1 N3 138.65(11) . 8_565 ?
O4 Pb1 N3 67.25(11) . 8_565 ?
N1 Pb1 S1 82.97(8) 7_655 . ?
O1 Pb1 S1 76.24(7) . . ?
O4 Pb1 S1 77.07(9) . . ?
N3 Pb1 S1 77.84(8) 8_565 . ?
C1 S1 Pb1 104.79(16) . . ?
C1 N1 C2 103.8(4) . . ?
C1 N1 Pb1 105.8(3) . 7_665 ?
C2 N1 Pb1 149.2(3) . 7_665 ?
C1 N2 N3 111.0(4) . . ?
C1 N2 H2 131(5) . . ?
N3 N2 H2 117(5) . . ?
C2 N3 N2 102.7(4) . . ?
C2 N3 Pb1 137.0(3) . 8_566 ?
N2 N3 Pb1 118.8(3) . 8_566 ?
N2 C1 N1 108.6(4) . . ?
N2 C1 S1 128.8(4) . . ?
N1 C1 S1 122.5(3) . . ?
N3 C2 N1 113.8(4) . . ?
N3 C2 H2A 125(4) . . ?
N1 C2 H2A 121(4) . . ?
N4 O1 Pb1 102.1(3) . . ?
O2 N4 O3 121.3(4) . . ?
O2 N4 O1 120.4(4) . . ?
O3 N4 O1 118.4(3) . . ?
Pb1 O4 H4A 98(5) . . ?
Pb1 O4 H4B 119(5) . . ?
H4A O4 H4B 102(6) . . ?

_refine_diff_density_max         1.357
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.169

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 992115'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound6

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H20 N14 O6 Pb S4'
_chemical_formula_sum            'C12 H20 N14 O6 Pb S4'
_chemical_formula_weight         791.85

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_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'

_cell_length_a                   10.5430(11)
_cell_length_b                   10.5430(11)
_cell_length_c                   11.7670(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1308.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    165
_cell_measurement_theta_min      5.626
_cell_measurement_theta_max      21.552

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    6.827
_shelx_estimated_absorpt_T_min   0.234
_shelx_estimated_absorpt_T_max   0.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.690436
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   
'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13152
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.865
_diffrn_reflns_theta_max         29.966
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             1804
_reflns_number_gt                1804
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_max     0.911
_reflns_Friedel_fraction_full    0.914

_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       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        
'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Hydrogens were refined isotropically.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 819 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.066(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1804
_refine_ls_number_parameters     105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0130
_refine_ls_R_factor_gt           0.0130
_refine_ls_wR_factor_ref         0.0284
_refine_ls_wR_factor_gt          0.0284
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_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_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
Pb1 Pb 0.0000 0.0000 0.0000 0.00883(5) Uani 1 4 d S T P . .
S1 S -0.08438(7) 0.26568(7) 0.05907(6) 0.01394(14) Uani 1 1 d . . . . .
N1 N 0.0417(2) 0.3505(2) -0.1289(2) 0.0118(5) Uani 1 1 d . . . . .
H1 H -0.013(4) 0.329(4) -0.182(4) 0.020(10) Uiso 1 1 d . . . . .
N2 N 0.1542(3) 0.4032(3) -0.1626(3) 0.0133(6) Uani 1 1 d . . . . .
N3 N 0.1495(2) 0.3757(2) 0.02297(18) 0.0115(6) Uani 1 1 d . . . . .
N4 N 0.0000 0.0000 0.2671(2) 0.0115(5) Uani 1 2 d S T P . .
O1 O 0.1014(2) 0.0159(2) 0.21261(19) 0.0195(5) Uani 1 1 d . . . . .
O2 O 0.0000 0.0000 0.37305(19) 0.0192(5) Uani 1 2 d S T P . .
C1 C 0.0357(3) 0.3313(3) -0.0164(3) 0.0107(7) Uani 1 1 d . . . . .
C2 C 0.2176(3) 0.4181(3) -0.0681(3) 0.0139(6) Uani 1 1 d . . . . .
H2 H 0.300(4) 0.450(4) -0.068(4) 0.021(10) Uiso 1 1 d . . . . .
C3 C 0.1904(4) 0.3725(5) 0.1412(4) 0.0229(9) Uani 1 1 d . . . . .
H3A H 0.151(6) 0.430(6) 0.190(5) 0.045(18) Uiso 1 1 d . . . . .
H3B H 0.179(5) 0.292(6) 0.172(4) 0.044(15) Uiso 1 1 d . . . . .
H3C H 0.275(7) 0.385(6) 0.147(5) 0.054(17) Uiso 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 O1 2.726(2) 3 ?
Pb1 O1 2.726(2) 4 ?
Pb1 O1 2.726(2) 2 ?
Pb1 O1 2.726(2) . ?
Pb1 S1 3.0200(8) . ?
Pb1 S1 3.0200(8) 4 ?
Pb1 S1 3.0200(8) 3 ?
Pb1 S1 3.0200(8) 2 ?
S1 C1 1.694(3) . ?
N1 C1 1.340(4) . ?
N1 N2 1.368(4) . ?
N1 H1 0.88(5) . ?
N2 C2 1.307(5) . ?
N3 C2 1.365(4) . ?
N3 C1 1.369(4) . ?
N3 C3 1.457(5) . ?
N4 O2 1.246(4) . ?
N4 O1 1.258(2) 2 ?
N4 O1 1.258(2) . ?
C2 H2 0.93(5) . ?
C3 H3A 0.93(6) . ?
C3 H3B 0.93(6) . ?
C3 H3C 0.91(7) . ?

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
O1 Pb1 O1 46.77(9) 3 4 ?
O1 Pb1 O1 147.40(6) 3 2 ?
O1 Pb1 O1 147.40(6) 4 2 ?
O1 Pb1 O1 147.40(6) 3 . ?
O1 Pb1 O1 147.40(6) 4 . ?
O1 Pb1 O1 46.77(9) 2 . ?
O1 Pb1 S1 126.38(5) 3 . ?
O1 Pb1 S1 80.18(5) 4 . ?
O1 Pb1 S1 74.36(6) 2 . ?
O1 Pb1 S1 81.20(6) . . ?
O1 Pb1 S1 74.36(6) 3 4 ?
O1 Pb1 S1 81.20(6) 4 4 ?
O1 Pb1 S1 80.18(5) 2 4 ?
O1 Pb1 S1 126.38(5) . 4 ?
S1 Pb1 S1 93.037(6) . 4 ?
O1 Pb1 S1 81.20(6) 3 3 ?
O1 Pb1 S1 74.36(6) 4 3 ?
O1 Pb1 S1 126.38(5) 2 3 ?
O1 Pb1 S1 80.18(5) . 3 ?
S1 Pb1 S1 93.036(6) . 3 ?
S1 Pb1 S1 153.39(3) 4 3 ?
O1 Pb1 S1 80.18(5) 3 2 ?
O1 Pb1 S1 126.38(5) 4 2 ?
O1 Pb1 S1 81.20(6) 2 2 ?
O1 Pb1 S1 74.36(6) . 2 ?
S1 Pb1 S1 153.39(3) . 2 ?
S1 Pb1 S1 93.037(6) 4 2 ?
S1 Pb1 S1 93.037(6) 3 2 ?
C1 S1 Pb1 92.17(10) . . ?
C1 N1 N2 112.9(3) . . ?
C1 N1 H1 129(3) . . ?
N2 N1 H1 118(3) . . ?
C2 N2 N1 104.2(3) . . ?
C2 N3 C1 107.9(2) . . ?
C2 N3 C3 127.0(3) . . ?
C1 N3 C3 125.1(3) . . ?
O2 N4 O1 120.67(14) . 2 ?
O2 N4 O1 120.67(14) . . ?
O1 N4 O1 118.7(3) 2 . ?
N4 O1 Pb1 97.28(16) . . ?
N1 C1 N3 103.9(3) . . ?
N1 C1 S1 128.0(2) . . ?
N3 C1 S1 128.1(3) . . ?
N2 C2 N3 111.1(3) . . ?
N2 C2 H2 122(3) . . ?
N3 C2 H2 127(3) . . ?
N3 C3 H3A 116(4) . . ?
N3 C3 H3B 111(3) . . ?
H3A C3 H3B 107(5) . . ?
N3 C3 H3C 111(4) . . ?
H3A C3 H3C 107(6) . . ?
H3B C3 H3C 103(5) . . ?

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 992116'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H7 N8 O Pb2 S8'
_chemical_formula_sum            'C9 H7 N8 O Pb2 S8'
_chemical_formula_weight         914.09

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   4.05170(10)
_cell_length_b                   24.3412(7)
_cell_length_c                   10.7681(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.9769(17)
_cell_angle_gamma                90.00
_cell_volume                     1059.43(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    55177
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       needle
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             834
_exptl_absorpt_coefficient_mu    16.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1352
_exptl_absorpt_correction_T_max  0.6616
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
; 
  
;

_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22633
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4808
_reflns_number_gt                4442
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_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)+(0.0652P)²+2.8433P] 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   0.030(8)
_refine_ls_number_reflns         4808
_refine_ls_number_parameters     254
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_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 0.36716(9) 0.144657(16) 0.86558(4) 0.01623(11) Uani 1 1 d . . .
Pb2 Pb 1.39233(10) 0.311957(15) 0.62122(4) 0.01712(11) Uani 1 1 d . . .
S1 S -0.1081(6) 0.13925(12) 1.0871(3) 0.0187(5) Uani 1 1 d . . .
S2 S 0.0392(7) 0.02185(12) 1.1840(3) 0.0207(6) Uani 1 1 d . . .
S3 S 0.8132(7) 0.08057(11) 0.7319(3) 0.0171(5) Uani 1 1 d . . .
S4 S 0.6530(7) 0.08682(13) 0.4496(3) 0.0233(6) Uani 1 1 d . . .
S5 S 0.8894(6) 0.24029(11) 0.7742(2) 0.0155(5) Uani 1 1 d . . .
S6 S 1.0068(8) 0.28747(13) 1.0385(3) 0.0243(6) Uani 1 1 d . . .
S7 S 1.8799(7) 0.39599(11) 0.6524(3) 0.0189(5) Uani 1 1 d . . .
S8 S 1.8643(7) 0.47324(13) 0.4294(3) 0.0237(6) Uani 1 1 d . . .
N1 N 0.208(2) 0.0579(4) 0.9768(9) 0.0180(19) Uani 1 1 d . . .
N2 N 0.320(2) 0.0046(4) 0.9836(9) 0.0183(18) Uani 1 1 d . . .
N3 N 0.452(2) 0.1566(4) 0.6052(8) 0.021(2) Uani 1 1 d . . .
N4 N 0.322(2) 0.1736(4) 0.4878(9) 0.021(2) Uani 1 1 d . . .
N5 N 1.254(2) 0.3280(3) 0.8502(8) 0.0159(18) Uani 1 1 d . . .
N6 N 1.349(2) 0.3634(4) 0.9437(9) 0.021(2) Uani 1 1 d . . .
N7 N 1.550(2) 0.3826(4) 0.4299(9) 0.021(2) Uani 1 1 d . . .
N8 N 1.487(2) 0.4040(4) 0.3109(9) 0.022(2) Uani 1 1 d . . .
C1 C 0.052(2) 0.0735(4) 1.0719(11) 0.017(2) Uani 1 1 d . . .
C2 C 0.248(3) -0.0194(5) 1.0860(9) 0.020(2) Uani 1 1 d . . .
H2 H 0.3065 -0.0564 1.1051 0.024 Uiso 1 1 calc R . .
C3 C 0.634(3) 0.1126(4) 0.6009(10) 0.016(2) Uani 1 1 d . . .
C4 C 0.415(2) 0.1415(5) 0.3973(10) 0.017(2) Uani 1 1 d . . .
H4 H 0.3548 0.1481 0.3117 0.020 Uiso 1 1 calc R . .
C5 C 1.063(3) 0.2877(5) 0.8816(9) 0.016(2) Uani 1 1 d . . .
C6 C 1.234(3) 0.3465(5) 1.0481(11) 0.025(3) Uani 1 1 d . . .
H6 H 1.2748 0.3659 1.1241 0.030 Uiso 1 1 calc R . .
C7 C 1.747(2) 0.4144(5) 0.5025(10) 0.017(2) Uani 1 1 d . . .
C8 C 1.641(3) 0.4499(5) 0.2958(11) 0.021(2) Uani 1 1 d . . .
H8 H 1.6319 0.4691 0.2189 0.025 Uiso 1 1 calc R . .
O1 O 0.877(2) 0.2630(3) 0.4624(7) 0.0228(17) Uani 1 1 d . . .
C9 C 0.887(3) 0.2689(5) 0.3328(12) 0.025(2) Uani 1 1 d . . .
H9A H 0.7676 0.3023 0.3056 0.037 Uiso 1 1 calc R . .
H9B H 0.7830 0.2369 0.2909 0.037 Uiso 1 1 calc R . .
H9C H 1.1178 0.2716 0.3115 0.037 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
Pb1 N3 2.864(13) . ?
Pb2 O1 2.865(12) . ?
Pb2 O1 2.943(12) 1_655 ?
Pb1 N1 2.534(9) . ?
Pb1 S3 2.852(3) . ?
Pb1 S3 3.016(3) 1_455 ?
Pb1 S1 3.086(3) 1_655 ?
Pb2 N5 2.595(9) . ?
Pb2 N7 2.791(9) . ?
Pb2 S7 2.847(3) . ?
Pb2 S7 2.950(3) 1_455 ?
Pb2 S5 3.058(3) 1_655 ?
S1 C1 1.739(11) . ?
S1 Pb1 3.086(3) 1_455 ?
S2 C2 1.722(11) . ?
S2 C1 1.746(11) . ?
S3 C3 1.728(11) . ?
S3 Pb1 3.016(3) 1_655 ?
S4 C4 1.716(12) . ?
S4 C3 1.752(11) . ?
S5 C5 1.748(11) . ?
S5 Pb2 3.058(3) 1_455 ?
S6 C6 1.706(13) . ?
S6 C5 1.720(10) . ?
S7 C7 1.726(12) . ?
S7 Pb2 2.950(3) 1_655 ?
S8 C7 1.718(12) . ?
S8 C8 1.741(12) . ?
N1 C1 1.298(14) . ?
N1 N2 1.373(13) . ?
N2 C2 1.297(14) . ?
N3 C3 1.303(14) . ?
N3 N4 1.397(13) . ?
N4 C4 1.323(15) . ?
N5 C5 1.308(14) . ?
N5 N6 1.360(13) . ?
N6 C6 1.312(16) . ?
N7 C7 1.326(15) . ?
N7 N8 1.390(13) . ?
N8 C8 1.297(15) . ?
C2 H2 0.9500 . ?
C4 H4 0.9500 . ?
C6 H6 0.9500 . ?
C8 H8 0.9500 . ?
O1 C9 1.407(14) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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
N1 Pb1 S3 88.5(2) . . ?
N1 Pb1 S3 65.7(2) . 1_455 ?
S3 Pb1 S3 87.30(7) . 1_455 ?
N1 Pb1 S1 77.5(2) . 1_655 ?
S3 Pb1 S1 86.56(8) . 1_655 ?
S3 Pb1 S1 142.83(8) 1_455 1_655 ?
N1 Pb1 N3 126.8(4) . . ?
N5 Pb2 N7 133.2(3) . . ?
N5 Pb2 S7 88.5(2) . . ?
N7 Pb2 S7 56.8(2) . . ?
N5 Pb2 S7 65.7(2) . 1_455 ?
N7 Pb2 S7 81.7(2) . 1_455 ?
S7 Pb2 S7 88.65(8) . 1_455 ?
N5 Pb2 S5 75.6(2) . 1_655 ?
N7 Pb2 S5 125.0(2) . 1_655 ?
S7 Pb2 S5 85.45(7) . 1_655 ?
S7 Pb2 S5 140.96(8) 1_455 1_655 ?
C1 S1 Pb1 102.0(4) . 1_455 ?
C2 S2 C1 87.5(5) . . ?
C3 S3 Pb1 85.4(4) . . ?
C3 S3 Pb1 114.4(4) . 1_655 ?
Pb1 S3 Pb1 87.30(7) . 1_655 ?
C4 S4 C3 88.1(5) . . ?
C5 S5 Pb2 101.5(4) . 1_455 ?
C6 S6 C5 87.0(6) . . ?
C7 S7 Pb2 84.6(4) . . ?
C7 S7 Pb2 104.5(4) . 1_655 ?
Pb2 O1 Pb2 88.4(3) . 1_455 ?
Pb2 S7 Pb2 88.65(11) . 1_655 ?
C7 S8 C8 87.8(5) . . ?
C1 N1 N2 114.3(9) . . ?
C1 N1 Pb1 106.4(7) . . ?
N2 N1 Pb1 136.0(7) . . ?
C2 N2 N1 112.2(9) . . ?
C3 N3 N4 112.9(9) . . ?
C4 N4 N3 112.6(9) . . ?
C5 N5 N6 115.1(9) . . ?
C5 N5 Pb2 107.7(6) . . ?
N6 N5 Pb2 136.9(7) . . ?
C6 N6 N5 109.7(9) . . ?
C7 N7 N8 112.9(9) . . ?
C7 N7 Pb2 94.8(7) . . ?
N8 N7 Pb2 150.9(7) . . ?
C8 N8 N7 112.3(10) . . ?
N1 C1 S1 123.3(8) . . ?
N1 C1 S2 112.0(8) . . ?
S1 C1 S2 124.6(7) . . ?
N2 C2 S2 114.1(9) . . ?
N2 C2 H2 123.0 . . ?
S2 C2 H2 123.0 . . ?
N3 C3 S3 123.3(8) . . ?
N3 C3 S4 112.9(8) . . ?
S3 C3 S4 123.7(6) . . ?
N4 C4 S4 113.4(8) . . ?
N4 C4 H4 123.3 . . ?
S4 C4 H4 123.3 . . ?
N5 C5 S6 112.2(8) . . ?
N5 C5 S5 122.8(8) . . ?
S6 C5 S5 125.0(7) . . ?
N6 C6 S6 115.7(9) . . ?
N6 C6 H6 122.1 . . ?
S6 C6 H6 122.1 . . ?
N7 C7 S8 113.1(8) . . ?
N7 C7 S7 122.4(9) . . ?
S8 C7 S7 124.5(6) . . ?
N8 C8 S8 113.9(9) . . ?
N8 C8 H8 123.0 . . ?
S8 C8 H8 123.0 . . ?
O1 C9 H9A 109.5 . . ?
O1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.178
_refine_diff_density_min         -2.082
_refine_diff_density_rms         0.260
_database_code_depnum_ccdc_archive 'CCDC 992117'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound8

_audit_creation_date             2013-07-03
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C6 H6 N4 Pb S4'
_chemical_formula_sum            'C6 H6 N4 Pb S4'
_chemical_formula_weight         469.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 H6 N4 Pb S4'
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'
S S 0.3331 0.5567 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3192(4)
_cell_length_b                   11.7420(4)
_cell_length_c                   7.72600(19)
_cell_angle_alpha                90
_cell_angle_beta                 93.931(2)
_cell_angle_gamma                90
_cell_volume                     1205.46(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11084
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      4.9660
_exptl_absorpt_coefficient_mu    33.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25323
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.2026
_exptl_crystal_size_mid          0.0587
_exptl_crystal_size_min          0.022
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            44530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.996
_diffrn_reflns_theta_min         3.326
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -37.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 70

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00   35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000   90.0000 81

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega  -63.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
  5 omega   55.00  104.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -60.0000 49

#__ type_ start__ end____ width___ exp.time_
  6 omega   80.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega   13.00   93.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -150.0000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega   24.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  150.0000 60

#__ type_ start__ end____ width___ exp.time_
  9 omega   43.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988 -110.0000   42.0000 44

#__ type_ start__ end____ width___ exp.time_
 10 omega   13.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
 11 omega   16.00   80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -60.0000 64

#__ type_ start__ end____ width___ exp.time_
 12 omega   11.00   38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   83.0000  107.2156 27

#__ type_ start__ end____ width___ exp.time_
 13 omega   19.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 14 omega   18.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -180.0000 35

#__ type_ start__ end____ width___ exp.time_
 15 omega   81.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 16 omega  142.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 36

#__ type_ start__ end____ width___ exp.time_
 17 omega   32.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 77

#__ type_ start__ end____ width___ exp.time_
 18 omega   85.00  118.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 33

#__ type_ start__ end____ width___ exp.time_
 19 omega   54.00  101.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 47

#__ type_ start__ end____ width___ exp.time_
 20 omega   40.00  140.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   60.0000 100

#__ type_ start__ end____ width___ exp.time_
 21 omega   86.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   60.0000  -86.1190 26

#__ type_ start__ end____ width___ exp.time_
 22 omega   82.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   81.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 33

#__ type_ start__ end____ width___ exp.time_
 24 omega   86.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 30

#__ type_ start__ end____ width___ exp.time_
 25 omega   81.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 26 omega   81.00  137.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 56

#__ type_ start__ end____ width___ exp.time_
 27 omega   86.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 28 omega   81.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
 29 omega   85.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 30 omega   86.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 31 omega   86.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   56.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 43

#__ type_ start__ end____ width___ exp.time_
 33 omega  121.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000 -178.4082 31

#__ type_ start__ end____ width___ exp.time_
 34 omega   81.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 30

#__ type_ start__ end____ width___ exp.time_
 35 omega   61.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 60

#__ type_ start__ end____ width___ exp.time_
 36 omega   85.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 37 omega   96.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega  122.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 56

#__ type_ start__ end____ width___ exp.time_
 39 omega   86.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
 40 omega   81.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 96

#__ type_ start__ end____ width___ exp.time_
 41 omega   81.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
 42 omega   85.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
 43 omega   43.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
 44 omega   85.00  162.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 77

#__ type_ start__ end____ width___ exp.time_
 45 omega  125.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
 46 omega   82.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 47 omega  119.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 58

#__ type_ start__ end____ width___ exp.time_
 48 omega   85.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
 49 omega   81.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 33

#__ type_ start__ end____ width___ exp.time_
 50 omega  125.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 51

#__ type_ start__ end____ width___ exp.time_
 51 omega   81.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 34

#__ type_ start__ end____ width___ exp.time_
 52 omega   84.00  117.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000 -178.4082 33

#__ type_ start__ end____ width___ exp.time_
 53 omega   84.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000 -116.2067 28

#__ type_ start__ end____ width___ exp.time_
 54 omega  -56.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   45.0000 -150.0000 87

#__ type_ start__ end____ width___ exp.time_
 55 omega -107.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -61.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 56 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -150.0000 94

#__ type_ start__ end____ width___ exp.time_
 57 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  -30.0000 70

#__ type_ start__ end____ width___ exp.time_
 58 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
 59 omega  -34.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  -19.0000 -120.0000 110

#__ type_ start__ end____ width___ exp.time_
 60 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  -60.0000 70

#__ type_ start__ end____ width___ exp.time_
 61 omega   11.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   83.0000  107.2156 29

#__ type_ start__ end____ width___ exp.time_
 62 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
 63 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 102

#__ type_ start__ end____ width___ exp.time_
 64 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 102

#__ type_ start__ end____ width___ exp.time_
 65 omega   23.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
 66 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  150.0000 70

#__ type_ start__ end____ width___ exp.time_
 67 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000 -150.0000 70

#__ type_ start__ end____ width___ exp.time_
 68 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
 69 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

#__ type_ start__ end____ width___ exp.time_
 70 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
 71 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
 72 omega   82.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000  147.7038 96

#__ type_ start__ end____ width___ exp.time_
 73 omega   71.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  120.0000 107

#__ type_ start__ end____ width___ exp.time_
 74 omega   41.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 81

#__ type_ start__ end____ width___ exp.time_
 75 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 89

#__ type_ start__ end____ width___ exp.time_
 76 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
 77 omega   31.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 78

#__ type_ start__ end____ width___ exp.time_
 78 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
 79 omega   31.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
 80 omega   31.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 78

#__ type_ start__ end____ width___ exp.time_
 81 omega   41.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   60.0000 58

#__ type_ start__ end____ width___ exp.time_
 82 omega   81.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

#__ type_ start__ end____ width___ exp.time_
 83 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 93

#__ type_ start__ end____ width___ exp.time_
 84 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
 85 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -30.0000 89

#__ type_ start__ end____ width___ exp.time_
 86 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
 87 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
 88 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -90.0000 89

#__ type_ start__ end____ width___ exp.time_
 89 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 89

#__ type_ start__ end____ width___ exp.time_
 90 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   90.0000 89

#__ type_ start__ end____ width___ exp.time_
 91 omega   90.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0007375000
_diffrn_orient_matrix_UB_12      0.0215967000
_diffrn_orient_matrix_UB_13      -0.1967856000
_diffrn_orient_matrix_UB_21      0.1134064000
_diffrn_orient_matrix_UB_22      -0.0267290000
_diffrn_orient_matrix_UB_23      0.0052664000
_diffrn_orient_matrix_UB_31      -0.0240637000
_diffrn_orient_matrix_UB_32      -0.1266807000
_diffrn_orient_matrix_UB_33      -0.0345730000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.7543 26262 17761
2 0.2457 26280 17761

_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4189
_reflns_number_total             4649
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         4649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0552P)²+18.2097P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1131
_refine_special_details          
;
 Refined as a 2-component twin.
   Rot(UB1,UB2)=-179.9775 deg 
   around 0.99 -0.00 -0.12 (rec) 1.00 -0.00 -0.00 (dir)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.8495(7) 0.5940(9) 0.4241(13) 0.016(2) Uani 1 1 d . . . . .
C2 C 0.8869(8) 0.4059(9) 0.3288(14) 0.018(2) Uani 1 1 d . . . . .
C3 C 0.9232(9) 0.2999(10) 0.2476(16) 0.024(2) Uani 1 1 d . . . . .
H3A H 0.9907 0.2840 0.2926 0.035 Uiso 1 1 calc R U . . .
H3B H 0.9221 0.3098 0.1242 0.035 Uiso 1 1 calc R U . . .
H3C H 0.8802 0.2375 0.2738 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5921(8) 0.5806(9) 0.2511(14) 0.017(2) Uani 1 1 d . . . . .
C5 C 0.6525(7) 0.4417(9) 0.0528(13) 0.015(2) Uani 1 1 d . . . . .
C6 C 0.6773(9) 0.3413(9) -0.0552(15) 0.020(2) Uani 1 1 d . . . . .
H6A H 0.6186 0.3187 -0.1259 0.030 Uiso 1 1 calc R U . . .
H6B H 0.6992 0.2793 0.0192 0.030 Uiso 1 1 calc R U . . .
H6C H 0.7301 0.3613 -0.1282 0.030 Uiso 1 1 calc R U . . .
N1 N 0.7982(7) 0.5148(8) 0.4991(12) 0.0192(18) Uani 1 1 d . . . . .
N2 N 0.8193(7) 0.4052(8) 0.4427(13) 0.023(2) Uani 1 1 d . . . . .
N3 N 0.6577(7) 0.6216(7) 0.1457(11) 0.0157(17) Uani 1 1 d . . . . .
N4 N 0.6928(7) 0.5418(7) 0.0338(11) 0.0157(17) Uani 1 1 d . . . . .
S1 S 0.83490(19) 0.7374(2) 0.4685(3) 0.0151(5) Uani 1 1 d . . . . .
S2 S 0.93045(19) 0.5389(2) 0.2782(3) 0.0177(5) Uani 1 1 d . . . . .
S3 S 0.53642(19) 0.6646(2) 0.3996(3) 0.0171(5) Uani 1 1 d . . . . .
S4 S 0.56988(19) 0.4370(2) 0.2153(3) 0.0161(5) Uani 1 1 d . . . . .
Pb1 Pb 0.68921(3) 0.67244(3) 0.68948(5) 0.01291(16) 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
C1 N1 1.312(14) . ?
C1 S1 1.732(11) . ?
C1 S2 1.737(10) . ?
C2 C3 1.489(15) . ?
C2 N2 1.302(15) . ?
C2 S2 1.720(12) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N3 1.326(14) . ?
C4 S3 1.720(11) . ?
C4 S4 1.731(11) . ?
C5 C6 1.495(14) . ?
C5 N4 1.305(13) . ?
C5 S4 1.726(10) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N1 N2 1.393(13) . ?
N1 Pb1 2.827(9) . ?
N3 N4 1.378(12) . ?
N3 Pb1 2.473(8) 4_575 ?
S1 Pb1 2.778(3) . ?
S1 Pb1 2.993(3) 4_575 ?
S3 Pb1 2.922(3) . ?
Pb1 N3 2.473(8) 4_576 ?
Pb1 S1 2.993(3) 4_576 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 S1 122.2(8) . . ?
N1 C1 S2 112.8(8) . . ?
S1 C1 S2 125.0(6) . . ?
C3 C2 S2 122.6(8) . . ?
N2 C2 C3 122.6(10) . . ?
N2 C2 S2 114.8(8) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 C4 S3 122.3(8) . . ?
N3 C4 S4 111.6(8) . . ?
S3 C4 S4 126.1(6) . . ?
C6 C5 S4 123.8(8) . . ?
N4 C5 C6 122.7(9) . . ?
N4 C5 S4 113.5(8) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 N1 N2 113.2(9) . . ?
C2 N2 N1 111.7(9) . . ?
C4 N3 N4 113.9(8) . . ?
C4 N3 Pb1 112.6(7) . 4_575 ?
N4 N3 Pb1 133.5(6) . 4_575 ?
C5 N4 N3 112.5(8) . . ?
C1 S1 Pb1 87.0(4) . . ?
C1 S1 Pb1 106.1(3) . 4_575 ?
Pb1 S1 Pb1 95.40(8) . 4_575 ?
C2 S2 C1 87.5(5) . . ?
C4 S3 Pb1 102.7(4) . . ?
C5 S4 C4 88.5(5) . . ?
N3 Pb1 N1 131.1(3) 4_576 . ?
N1 Pb1 S3 86.4(2) . . ?
N3 Pb1 S1 76.5(2) 4_576 . ?
N3 Pb1 S1 81.3(2) 4_576 4_576 ?
N3 Pb1 S3 79.8(2) 4_576 . ?
S1 Pb1 S1 84.25(6) . 4_576 ?
S1 Pb1 S3 90.96(7) . . ?
S3 Pb1 S1 161.08(7) . 4_576 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8 2 0 0.0110 7.9986 1.9990 -0.0015 0.0376 0.8537 -0.4457
2 7 0 0.0199 1.9982 6.9978 -0.0003 0.1497 0.0396 -0.9346
-2 -7 0 0.0199 -1.9982 -6.9978 0.0003 -0.1497 -0.0396 0.9346
1 0 5 0.0962 1.0064 -0.0014 4.9973 -0.9842 0.1405 -0.1968
-1 0 -5 0.0962 -1.0064 0.0014 -4.9973 0.9842 -0.1405 0.1968
-8 -2 0 0.0110 -7.9986 -1.9990 0.0015 -0.0376 -0.8537 0.4457

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?

_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.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 992118'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound9

_audit_creation_date             2013-06-26
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C4 H6 N8 Pb S2'
_chemical_formula_sum            'C4 H6 N8 Pb S2'
_chemical_formula_weight         437.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C4 H6 N8 Pb S2'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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                   8.94447(19)
_cell_length_b                   4.92209(8)
_cell_length_c                   23.5863(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.5552(18)
_cell_angle_gamma                90
_cell_volume                     1037.36(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    41146
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.6460
_cell_measurement_theta_min      3.3300
_exptl_absorpt_coefficient_mu    16.646
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.026
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.801
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.4898
_exptl_crystal_size_mid          0.0895
_exptl_crystal_size_min          0.0297
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77856
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.376
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.6228
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9732
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -90.00  -59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000  -25.3815 31

#__ type_ start__ end____ width___ exp.time_
  2 omega  -90.00  -63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -127.3463 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -36.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   38.0000  -30.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega   14.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922 -130.0000 -133.8619 61

#__ type_ start__ end____ width___ exp.time_
  5 omega   -8.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   57.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega   37.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  178.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
  7 omega  -13.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   77.0000  -60.0000 102

#__ type_ start__ end____ width___ exp.time_
  8 omega  -48.00    7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -38.0000  150.0000 55

#__ type_ start__ end____ width___ exp.time_
  9 omega  -51.00   24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -38.0000   30.0000 75

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  178.0000  -30.0000 42

#__ type_ start__ end____ width___ exp.time_
 11 omega   -3.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   38.0000 -150.0000 91

#__ type_ start__ end____ width___ exp.time_
 12 omega  -37.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   38.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
 13 omega  -42.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   57.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
 14 omega  -88.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -38.0000  150.0000 92

#__ type_ start__ end____ width___ exp.time_
 15 omega  -85.00    8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -57.0000   90.0000 93

#__ type_ start__ end____ width___ exp.time_
 16 omega  -88.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -38.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
 17 omega  -72.00  -26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  128.0000   56.0000 46

#__ type_ start__ end____ width___ exp.time_
 18 omega    6.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922 -130.0000 -133.8619 69

#__ type_ start__ end____ width___ exp.time_
 19 omega   34.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922 -178.0000   90.0000 68

#__ type_ start__ end____ width___ exp.time_
 20 omega  -54.00   38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -38.0000   90.0000 92

#__ type_ start__ end____ width___ exp.time_
 21 omega  -90.00  -38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -176.0073 52

#__ type_ start__ end____ width___ exp.time_
 22 omega -101.00  -55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  178.0000   30.0000 46

#__ type_ start__ end____ width___ exp.time_
 23 omega  -90.00  -38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -127.3463 52

#__ type_ start__ end____ width___ exp.time_
 24 omega  -88.00   13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -77.0000  -30.0000 101

#__ type_ start__ end____ width___ exp.time_
 25 omega  -68.00   51.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -150.0000 119

#__ type_ start__ end____ width___ exp.time_
 26 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -180.0000 171

#__ type_ start__ end____ width___ exp.time_
 27 omega  -90.00  -38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000  -63.9193 52

#__ type_ start__ end____ width___ exp.time_
 28 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -150.0000 171

#__ type_ start__ end____ width___ exp.time_
 29 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000    0.0000 171

#__ type_ start__ end____ width___ exp.time_
 30 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  -90.0000 171

#__ type_ start__ end____ width___ exp.time_
 31 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  -60.0000 171

#__ type_ start__ end____ width___ exp.time_
 32 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  -30.0000 171

#__ type_ start__ end____ width___ exp.time_
 33 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -120.0000 171

#__ type_ start__ end____ width___ exp.time_
 34 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000   30.0000 171

#__ type_ start__ end____ width___ exp.time_
 35 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000   60.0000 171

#__ type_ start__ end____ width___ exp.time_
 36 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000   90.0000 171

#__ type_ start__ end____ width___ exp.time_
 37 omega  -68.00   23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  120.0000 91

#__ type_ start__ end____ width___ exp.time_
 38 omega  -68.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -180.0000 150
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0071239000
_diffrn_orient_matrix_UB_12      0.0468669000
_diffrn_orient_matrix_UB_13      0.0284510000
_diffrn_orient_matrix_UB_21      0.0014875000
_diffrn_orient_matrix_UB_22      -0.1362075000
_diffrn_orient_matrix_UB_23      0.0097623000
_diffrn_orient_matrix_UB_31      0.0790491000
_diffrn_orient_matrix_UB_32      -0.0017261000
_diffrn_orient_matrix_UB_33      -0.0013960000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1740
_reflns_number_total             1819
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         3.320
_refine_diff_density_min         -3.082
_refine_diff_density_rms         0.287
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1819
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0540P)²+17.8915P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0943
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.51423(3) 0.46983(7) 0.25847(2) 0.01250(16) Uani 1 1 d . . . . .
S1 S 0.3165(3) 0.0776(5) 0.29849(10) 0.0183(5) Uani 1 1 d . . . . .
S2 S 0.7316(2) 0.1740(4) 0.31647(9) 0.0158(5) Uani 1 1 d . . . . .
N1 N 0.3760(9) -0.0315(14) 0.4112(3) 0.0147(16) Uani 1 1 d . . . . .
N5 N 0.8799(9) 0.4208(16) 0.4051(3) 0.0167(16) Uani 1 1 d . . . . .
C3 C 0.8504(9) 0.4087(19) 0.3477(4) 0.0126(17) Uani 1 1 d . . . . .
N6 N 0.9832(8) 0.6139(16) 0.4167(3) 0.0198(16) Uani 1 1 d . . . . .
N7 N 1.0171(8) 0.7197(15) 0.3687(3) 0.0181(16) Uani 1 1 d . . . . .
N8 N 0.9388(9) 0.5953(15) 0.3254(3) 0.0178(16) Uani 1 1 d . . . . .
C1 C 0.3954(10) -0.0867(19) 0.3567(4) 0.0164(18) Uani 1 1 d . . . . .
N3 N 0.5272(8) -0.3622(16) 0.4108(3) 0.0199(16) Uani 1 1 d . . . . .
N2 N 0.4571(8) -0.2049(16) 0.4447(3) 0.0196(16) Uani 1 1 d . . . . .
C4 C 0.8176(10) 0.2558(18) 0.4497(4) 0.0190(19) Uani 1 1 d . . . . .
H4A H 0.7123 0.2915 0.4513 0.028 Uiso 1 1 calc R U . . .
H4B H 0.8666 0.3005 0.4856 0.028 Uiso 1 1 calc R U . . .
H4C H 0.8328 0.0670 0.4416 0.028 Uiso 1 1 calc R U . . .
C2 C 0.2769(10) 0.1696(18) 0.4354(4) 0.0193(19) Uani 1 1 d . . . . .
H2A H 0.2676 0.3237 0.4106 0.029 Uiso 1 1 calc R U . . .
H2B H 0.3179 0.2267 0.4718 0.029 Uiso 1 1 calc R U . . .
H2C H 0.1800 0.0904 0.4399 0.029 Uiso 1 1 calc R U . . .
N4 N 0.4916(8) -0.2969(15) 0.3561(3) 0.0191(16) 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 S1 2.810(2) . ?
Pb1 S2 3.108(2) 2_655 ?
Pb1 S2 2.745(2) . ?
Pb1 N8 2.749(7) 2_645 ?
Pb1 N4 2.589(8) 1_565 ?
S1 C1 1.717(10) . ?
S2 Pb1 3.108(2) 2_645 ?
S2 C3 1.713(9) . ?
N1 C1 1.333(12) . ?
N1 N2 1.352(11) . ?
N1 C2 1.462(11) . ?
N5 C3 1.369(12) . ?
N5 N6 1.345(11) . ?
N5 C4 1.459(11) . ?
C3 N8 1.336(12) . ?
N6 N7 1.295(11) . ?
N7 N8 1.359(11) . ?
N8 Pb1 2.749(7) 2_655 ?
C1 N4 1.346(12) . ?
N3 N2 1.294(11) . ?
N3 N4 1.354(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
N4 Pb1 2.589(8) 1_545 ?

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
S1 Pb1 S2 154.23(6) . 2_655 ?
S2 Pb1 S1 84.88(7) . . ?
S2 Pb1 S2 86.28(5) . 2_655 ?
S2 Pb1 N8 82.83(17) . 2_645 ?
N8 Pb1 S1 84.24(17) 2_645 . ?
N8 Pb1 S2 70.66(17) 2_645 2_655 ?
N4 Pb1 S1 86.02(17) 1_565 . ?
N4 Pb1 S2 116.78(17) 1_565 2_655 ?
N4 Pb1 S2 82.75(18) 1_565 . ?
N4 Pb1 N8 163.2(2) 1_565 2_645 ?
C1 S1 Pb1 110.4(3) . . ?
Pb1 S2 Pb1 114.07(7) . 2_645 ?
C3 S2 Pb1 90.4(3) . 2_645 ?
C3 S2 Pb1 105.6(3) . . ?
C1 N1 N2 110.2(7) . . ?
C1 N1 C2 128.5(8) . . ?
N2 N1 C2 121.2(8) . . ?
C3 N5 C4 128.7(8) . . ?
N6 N5 C3 109.4(7) . . ?
N6 N5 C4 121.9(8) . . ?
N5 C3 S2 122.9(7) . . ?
N8 C3 S2 131.3(7) . . ?
N8 C3 N5 105.6(8) . . ?
N7 N6 N5 107.0(7) . . ?
N6 N7 N8 110.1(7) . . ?
C3 N8 Pb1 149.0(6) . 2_655 ?
C3 N8 N7 107.9(7) . . ?
N7 N8 Pb1 98.5(5) . 2_655 ?
N1 C1 S1 127.4(7) . . ?
N1 C1 N4 106.1(8) . . ?
N4 C1 S1 126.5(7) . . ?
N2 N3 N4 110.3(7) . . ?
N3 N2 N1 106.2(7) . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 N4 Pb1 115.2(6) . 1_545 ?
C1 N4 N3 107.2(7) . . ?
N3 N4 Pb1 135.9(6) . 1_545 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 0 33 0.0148 -1.0363 -0.0219 32.9761 0.9298 0.3234 -0.1279
1 0 -33 0.0148 1.0363 0.0219 -32.9761 -0.9298 -0.3234 0.1279
-1 7 2 0.2397 -1.0171 6.9911 2.0945 0.3800 -0.9333 -0.0954
1 -7 -2 0.2397 1.0171 -6.9911 -2.0945 -0.3800 0.9333 0.0954
-13 0 3 0.0426 -12.9890 -0.0096 2.8738 -0.0112 0.0100 -1.0308
13 0 -3 0.0426 12.9890 0.0096 -2.8738 0.0112 -0.0100 1.0308

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 992119'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound10

_audit_creation_date             2013-06-26
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H12 N2 Pb S4'
_chemical_formula_sum            'C18 H12 N2 Pb S4'
_chemical_formula_weight         591.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C18 H10 N2 Pb S4'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.9345(3)
_cell_length_b                   7.34785(13)
_cell_length_c                   24.3982(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3573.75(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19790
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.7920
_cell_measurement_theta_min      3.3770
_exptl_absorpt_coefficient_mu    9.913
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.1802
_exptl_crystal_size_mid          0.0538
_exptl_crystal_size_min          0.0374
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31790
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.070
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.6228
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9358
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -75.00  -40.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  131.0000  -90.3124 35

#__ type_ start__ end____ width___ exp.time_
  2 omega  -75.00   13.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -77.0000 -180.0000 88

#__ type_ start__ end____ width___ exp.time_
  3 omega    6.00   75.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -130.0000  133.0860 69

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   86.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -       17.4854   38.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
  5 omega  -51.00   43.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -57.0000  -30.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00   89.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -       17.4854   38.0000  -60.0000 88

#__ type_ start__ end____ width___ exp.time_
  7 omega  -48.00   38.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -38.0000 -150.0000 86

#__ type_ start__ end____ width___ exp.time_
  8 omega   -8.00   17.00   1.0000  186.6100
omega____ theta____ kappa____ phi______ frames
    -       17.4854   57.0000  120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0089768000
_diffrn_orient_matrix_UB_12      0.0923089000
_diffrn_orient_matrix_UB_13      -0.0042557000
_diffrn_orient_matrix_UB_21      0.0304535000
_diffrn_orient_matrix_UB_22      0.0144957000
_diffrn_orient_matrix_UB_23      -0.0144116000
_diffrn_orient_matrix_UB_31      -0.0160847000
_diffrn_orient_matrix_UB_32      -0.0241794000
_diffrn_orient_matrix_UB_33      -0.0248836000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2972
_reflns_number_total             3150
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0111P)²+14.8325P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0444
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.19551(2) 0.64375(2) 0.58470(2) 0.00953(6) Uani 1 1 d . . . . .
S1 S 0.29159(5) 0.79338(13) 0.65447(4) 0.0109(2) Uani 1 1 d . . . . .
S2 S 0.22577(5) 0.82379(14) 0.76733(4) 0.0142(2) Uani 1 1 d . . . . .
S3 S 0.30316(5) 0.49642(13) 0.52439(4) 0.0100(2) Uani 1 1 d . . . . .
S4 S 0.25911(5) 0.37676(13) 0.40949(4) 0.0112(2) Uani 1 1 d . . . . .
N1 N 0.16038(17) 0.8326(4) 0.67731(13) 0.0114(7) Uani 1 1 d . . . . .
N2 N 0.18100(16) 0.5271(4) 0.47910(13) 0.0107(7) Uani 1 1 d . . . . .
C1 C 0.2216(2) 0.8212(5) 0.69601(15) 0.0105(8) Uani 1 1 d . . . . .
C2 C 0.1403(2) 0.8400(5) 0.77011(16) 0.0137(9) Uani 1 1 d . . . . .
H2 H 0.1154 0.8459 0.8023 0.016 Uiso 1 1 calc R U . . .
C3 C 0.1134(2) 0.8431(5) 0.71879(16) 0.0109(8) Uani 1 1 d . . . . .
C4 C 0.0418(2) 0.8631(5) 0.70479(16) 0.0123(8) Uani 1 1 d . . . . .
C5 C 0.0233(2) 0.9393(5) 0.65482(16) 0.0132(8) Uani 1 1 d . . . . .
H5 H 0.0561 0.9696 0.6293 0.016 Uiso 1 1 calc R U . . .
C6 C -0.0434(2) 0.9702(5) 0.64280(17) 0.0162(9) Uani 1 1 d . . . . .
H6 H -0.0554 1.0216 0.6094 0.019 Uiso 1 1 calc R U . . .
C7 C -0.0929(2) 0.9243(6) 0.68084(17) 0.0163(9) Uani 1 1 d . . . . .
H7 H -0.1378 0.9472 0.6731 0.020 Uiso 1 1 calc R U . . .
C8 C -0.0750(2) 0.8449(6) 0.72991(17) 0.0165(9) Uani 1 1 d . . . . .
H8 H -0.1080 0.8115 0.7549 0.020 Uiso 1 1 calc R U . . .
C9 C -0.0081(2) 0.8148(5) 0.74202(16) 0.0141(8) Uani 1 1 d . . . . .
H9 H 0.0036 0.7618 0.7753 0.017 Uiso 1 1 calc R U . . .
C10 C 0.2426(2) 0.4704(5) 0.47304(15) 0.0109(8) Uani 1 1 d . . . . .
C11 C 0.1777(2) 0.4176(5) 0.39101(16) 0.0121(8) Uani 1 1 d . . . . .
H11 H 0.1595 0.3883 0.3570 0.015 Uiso 1 1 calc R U . . .
C12 C 0.1429(2) 0.4984(5) 0.43232(15) 0.0100(8) Uani 1 1 d . . . . .
C13 C 0.0728(2) 0.5624(5) 0.43102(15) 0.0106(8) Uani 1 1 d . . . . .
C14 C 0.0291(2) 0.5086(6) 0.38946(16) 0.0131(8) Uani 1 1 d . . . . .
H14 H 0.0442 0.4298 0.3623 0.016 Uiso 1 1 calc R U . . .
C15 C -0.0362(2) 0.5705(6) 0.38804(17) 0.0135(8) Uani 1 1 d . . . . .
H15 H -0.0645 0.5352 0.3596 0.016 Uiso 1 1 calc R U . . .
C16 C -0.0597(2) 0.6854(5) 0.42898(16) 0.0135(9) Uani 1 1 d . . . . .
H16 H -0.1039 0.7261 0.4283 0.016 Uiso 1 1 calc R U . . .
C17 C -0.0170(2) 0.7390(6) 0.47081(16) 0.0134(8) Uani 1 1 d . . . . .
H17 H -0.0325 0.8157 0.4983 0.016 Uiso 1 1 calc R U . . .
C18 C 0.0486(2) 0.6788(5) 0.47176(16) 0.0125(8) Uani 1 1 d . . . . .
H18 H 0.0770 0.7162 0.4998 0.015 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
Pb1 S1 2.7883(10) . ?
Pb1 S1 3.0971(10) 7_655 ?
Pb1 S3 2.8182(10) . ?
Pb1 S3 2.9802(10) 7_665 ?
Pb1 N1 2.742(3) . ?
Pb1 N2 2.731(3) . ?
S1 Pb1 3.0971(10) 7_665 ?
S1 C1 1.737(4) . ?
S2 C1 1.742(4) . ?
S2 C2 1.710(4) . ?
S3 Pb1 2.9802(10) 7_655 ?
S3 C10 1.750(4) . ?
S4 C10 1.728(4) . ?
S4 C11 1.712(4) . ?
N1 C1 1.305(5) . ?
N1 C3 1.382(5) . ?
N2 C10 1.305(5) . ?
N2 C12 1.387(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.363(6) . ?
C3 C4 1.473(6) . ?
C4 C5 1.391(6) . ?
C4 C9 1.394(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.380(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.396(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.379(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(6) . ?
C9 H9 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.359(6) . ?
C12 C13 1.474(6) . ?
C13 C14 1.394(6) . ?
C13 C18 1.398(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.379(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.387(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.380(6) . ?
C18 H18 0.9300 . ?

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
S1 Pb1 S1 86.28(3) . 7_655 ?
S1 Pb1 S3 86.97(3) . . ?
S1 Pb1 S3 87.28(3) . 7_665 ?
S3 Pb1 S1 84.52(3) . 7_655 ?
S3 Pb1 S1 173.45(3) 7_665 7_655 ?
S3 Pb1 S3 93.98(3) . 7_665 ?
N1 Pb1 S1 89.36(7) . 7_655 ?
N1 Pb1 S1 58.19(7) . . ?
N1 Pb1 S3 88.23(7) . 7_665 ?
N1 Pb1 S3 144.99(7) . . ?
N2 Pb1 S1 105.45(7) . 7_655 ?
N2 Pb1 S1 140.59(7) . . ?
N2 Pb1 S3 78.93(7) . 7_665 ?
N2 Pb1 S3 57.82(7) . . ?
N2 Pb1 N1 155.38(10) . . ?
Pb1 S1 Pb1 92.82(3) . 7_665 ?
C1 S1 Pb1 106.84(13) . 7_665 ?
C1 S1 Pb1 81.40(13) . . ?
C2 S2 C1 89.56(19) . . ?
Pb1 S3 Pb1 94.76(3) . 7_655 ?
C10 S3 Pb1 83.71(13) . . ?
C10 S3 Pb1 105.35(13) . 7_655 ?
C11 S4 C10 89.2(2) . . ?
C1 N1 Pb1 91.0(2) . . ?
C1 N1 C3 112.4(3) . . ?
C3 N1 Pb1 143.6(3) . . ?
C10 N2 Pb1 96.2(2) . . ?
C10 N2 C12 111.9(3) . . ?
C12 N2 Pb1 151.9(3) . . ?
S1 C1 S2 123.0(2) . . ?
N1 C1 S1 123.7(3) . . ?
N1 C1 S2 113.2(3) . . ?
S2 C2 H2 124.5 . . ?
C3 C2 S2 110.9(3) . . ?
C3 C2 H2 124.5 . . ?
N1 C3 C4 119.5(3) . . ?
C2 C3 N1 113.9(4) . . ?
C2 C3 C4 126.6(4) . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 C9 118.9(4) . . ?
C9 C4 C3 121.0(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(4) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0(4) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.8(4) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C4 C9 H9 119.7 . . ?
C8 C9 C4 120.6(4) . . ?
C8 C9 H9 119.7 . . ?
S4 C10 S3 123.7(2) . . ?
N2 C10 S3 122.2(3) . . ?
N2 C10 S4 114.1(3) . . ?
S4 C11 H11 124.3 . . ?
C12 C11 S4 111.4(3) . . ?
C12 C11 H11 124.3 . . ?
N2 C12 C13 119.2(3) . . ?
C11 C12 N2 113.4(4) . . ?
C11 C12 C13 127.3(4) . . ?
C14 C13 C12 121.2(4) . . ?
C14 C13 C18 118.3(4) . . ?
C18 C13 C12 120.5(4) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.1(4) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.6(4) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C13 C18 H18 119.6 . . ?
C17 C18 C13 120.8(4) . . ?
C17 C18 H18 119.6 . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 -10 4 0.0894 -5.0635 -9.9629 4.0267 -0.8913 -0.3567 0.2221
5 10 -4 0.0894 5.0635 9.9629 -4.0267 0.8913 0.3567 -0.2221
-12 0 -31 0.0187 -11.9308 0.0080 -30.9278 0.2395 0.0825 0.9613
12 0 31 0.0187 11.9308 -0.0080 30.9278 -0.2395 -0.0825 -0.9613
16 -3 -26 0.0205 15.9568 -3.0189 -25.9096 -0.3117 0.8156 0.4611
-16 3 26 0.0205 -15.9568 3.0189 25.9096 0.3117 -0.8156 -0.4611
28 0 6 0.0259 27.9089 -0.0355 6.0035 -0.2794 0.7629 -0.5974
-28 0 -6 0.0259 -27.9089 0.0355 -6.0035 0.2794 -0.7629 0.5974

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2


#===END 
_database_code_depnum_ccdc_archive 'CCDC 992120'
