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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex6
_database_code_depnum_ccdc_archive 'CCDC 1010479'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 Cl2 N2 O19 Pb4 S4'
_chemical_formula_sum            'C26 H20 Cl2 N2 O19 Pb4 S4'
_chemical_formula_weight         1692.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 '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           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                   10.8035(6)
_cell_length_b                   11.0281(6)
_cell_length_c                   16.5111(8)
_cell_angle_alpha                83.101(4)
_cell_angle_beta                 78.246(4)
_cell_angle_gamma                86.292(4)
_cell_volume                     1910.34(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3370
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      27.52

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    18.013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1161
_exptl_absorpt_correction_T_max  0.1399
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11460
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0788
_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       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         27.56
_reflns_number_total             8717
_reflns_number_gt                6781
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0047P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8717
_refine_ls_number_parameters     522
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0682
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.51868(3) 0.04723(3) 0.37432(2) 0.02741(10) Uani 1 1 d . . .
Pb2 Pb 0.83651(3) -0.40542(3) 0.51289(2) 0.02481(9) Uani 1 1 d . . .
Pb3 Pb 1.14864(3) -0.11680(3) 0.51503(2) 0.02284(9) Uani 1 1 d . . .
Pb4 Pb 0.46643(3) 0.40342(3) 0.27240(2) 0.02397(9) Uani 1 1 d . . .
Cl1 Cl 1.1367(3) 0.0248(3) 0.05635(17) 0.0637(10) Uani 1 1 d . . .
Cl2 Cl 0.9972(3) -0.2947(2) 0.07090(16) 0.0448(7) Uani 1 1 d . . .
S1 S 0.8082(2) -0.12021(19) 0.34146(15) 0.0222(5) Uani 1 1 d . . .
S2 S 1.2178(2) 0.13234(19) 0.35341(16) 0.0253(5) Uani 1 1 d . . .
S3 S 0.7845(2) -0.5801(2) 0.34810(16) 0.0281(6) Uani 1 1 d . . .
S4 S 1.2149(2) -0.3342(2) 0.34060(16) 0.0281(6) Uani 1 1 d . . .
O1 O 0.8371(6) -0.2346(5) 0.3886(4) 0.0382(18) Uani 1 1 d . . .
O1W O 0.4682(13) -0.0705(10) 0.2527(12) 0.138(5) Uani 1 1 d D . .
H1W1 H 0.408(10) -0.119(12) 0.259(16) 0.207 Uiso 1 1 d D . .
H1W2 H 0.538(8) -0.112(13) 0.249(17) 0.207 Uiso 1 1 d D . .
O2 O 0.7422(6) -0.0288(5) 0.3954(4) 0.0308(16) Uani 1 1 d . . .
O3 O 0.7397(6) -0.1363(6) 0.2768(4) 0.0396(18) Uani 1 1 d . . .
O4 O 1.1267(7) 0.2167(6) 0.3944(5) 0.045(2) Uani 1 1 d . . .
O5 O 1.2675(6) 0.0385(5) 0.4126(4) 0.0261(14) Uani 1 1 d . . .
O6 O 1.3221(6) 0.1900(6) 0.2950(4) 0.0419(19) Uani 1 1 d . . .
O7 O 1.0043(5) -0.0258(5) 0.4213(4) 0.0235(14) Uani 1 1 d . . .
O8 O 0.8331(7) -0.7053(5) 0.3555(5) 0.048(2) Uani 1 1 d . . .
O9 O 0.6897(6) -0.5581(6) 0.2958(5) 0.044(2) Uani 1 1 d . . .
O10 O 0.7374(6) -0.5349(6) 0.4293(4) 0.0416(18) Uani 1 1 d . . .
O11 O 1.1488(7) -0.2806(6) 0.4154(5) 0.051(2) Uani 1 1 d . . .
O12 O 1.2799(6) -0.4503(5) 0.3656(4) 0.0301(16) Uani 1 1 d . . .
O13 O 1.2970(7) -0.2549(7) 0.2794(5) 0.055(2) Uani 1 1 d . . .
O14 O 1.0002(6) -0.4962(5) 0.4159(4) 0.0261(14) Uani 1 1 d . . .
O15 O 0.5607(7) -0.2596(6) 0.5632(4) 0.0439(19) Uani 1 1 d . . .
O16 O 0.4353(6) -0.1307(5) 0.5000(5) 0.0411(18) Uani 1 1 d . . .
O17 O 0.6149(7) 0.1910(6) 0.2613(4) 0.0414(19) Uani 1 1 d . . .
O18 O 0.5865(7) 0.3161(6) 0.1532(4) 0.052(2) Uani 1 1 d . . .
N1 N 0.5170(7) 0.5915(6) 0.1678(5) 0.0293(19) Uani 1 1 d . . .
N2 N 0.3222(7) 0.4510(6) 0.1645(5) 0.0272(18) Uani 1 1 d . . .
C1 C 0.9536(8) -0.0553(7) 0.2902(5) 0.0174(18) Uani 1 1 d . . .
C2 C 1.0298(8) -0.0104(7) 0.3393(6) 0.0205(19) Uani 1 1 d . . .
C3 C 1.1362(7) 0.0536(7) 0.2948(6) 0.0178(18) Uani 1 1 d . . .
C4 C 1.1716(8) 0.0633(8) 0.2096(6) 0.028(2) Uani 1 1 d . . .
H4A H 1.2444 0.1029 0.1824 0.033 Uiso 1 1 calc R . .
C5 C 1.0956(9) 0.0122(8) 0.1652(5) 0.027(2) Uani 1 1 d . . .
C6 C 0.9851(9) -0.0438(7) 0.2049(6) 0.027(2) Uani 1 1 d . . .
H6A H 0.9327 -0.0732 0.1741 0.033 Uiso 1 1 calc R . .
C7 C 0.9113(8) -0.4865(7) 0.2942(6) 0.0210(19) Uani 1 1 d . . .
C8 C 1.0037(8) -0.4558(7) 0.3369(5) 0.0191(19) Uani 1 1 d . . .
C9 C 1.0956(8) -0.3758(7) 0.2909(6) 0.0208(19) Uani 1 1 d . . .
C10 C 1.0947(8) -0.3281(7) 0.2097(5) 0.022(2) Uani 1 1 d . . .
H10A H 1.1559 -0.2743 0.1814 0.026 Uiso 1 1 calc R . .
C11 C 1.0025(9) -0.3611(7) 0.1711(6) 0.025(2) Uani 1 1 d . . .
C12 C 0.9112(9) -0.4390(8) 0.2130(6) 0.027(2) Uani 1 1 d . . .
H12A H 0.8486 -0.4599 0.1865 0.033 Uiso 1 1 calc R . .
C13 C 0.5052(9) -0.3150(8) 0.4385(7) 0.041(3) Uani 1 1 d . . .
H13A H 0.5888 -0.3514 0.4241 0.061 Uiso 1 1 calc R . .
H13B H 0.4833 -0.2680 0.3902 0.061 Uiso 1 1 calc R . .
H13C H 0.4457 -0.3781 0.4584 0.061 Uiso 1 1 calc R . .
C14 C 0.5016(9) -0.2319(8) 0.5060(6) 0.027(2) Uani 1 1 d . . .
C15 C 0.7312(19) 0.1471(15) 0.1298(10) 0.162(11) Uani 1 1 d . . .
H15A H 0.8125 0.1437 0.1452 0.242 Uiso 1 1 calc R . .
H15B H 0.7385 0.1838 0.0733 0.242 Uiso 1 1 calc R . .
H15C H 0.7017 0.0659 0.1345 0.242 Uiso 1 1 calc R . .
C16 C 0.6393(11) 0.2220(9) 0.1863(7) 0.045(3) Uani 1 1 d . . .
C17 C 0.6053(10) 0.6661(8) 0.1758(7) 0.041(3) Uani 1 1 d . . .
H17A H 0.6437 0.6505 0.2218 0.049 Uiso 1 1 calc R . .
C18 C 0.6418(11) 0.7655(9) 0.1184(8) 0.052(3) Uani 1 1 d . . .
H18A H 0.7049 0.8147 0.1252 0.063 Uiso 1 1 calc R . .
C19 C 0.5853(12) 0.7904(10) 0.0528(8) 0.061(4) Uani 1 1 d . . .
H19A H 0.6060 0.8591 0.0150 0.073 Uiso 1 1 calc R . .
C20 C 0.4951(11) 0.7121(9) 0.0419(7) 0.050(3) Uani 1 1 d . . .
H20A H 0.4584 0.7249 -0.0048 0.060 Uiso 1 1 calc R . .
C21 C 0.4609(9) 0.6137(8) 0.1031(6) 0.030(2) Uani 1 1 d . . .
C22 C 0.3622(9) 0.5306(8) 0.0964(6) 0.030(2) Uani 1 1 d . . .
C23 C 0.3081(10) 0.5360(9) 0.0276(7) 0.041(3) Uani 1 1 d . . .
H23A H 0.3372 0.5900 -0.0192 0.049 Uiso 1 1 calc R . .
C24 C 0.2098(11) 0.4608(10) 0.0281(7) 0.048(3) Uani 1 1 d . . .
H24A H 0.1739 0.4620 -0.0186 0.057 Uiso 1 1 calc R . .
C25 C 0.1670(11) 0.3849(9) 0.0985(7) 0.047(3) Uani 1 1 d . . .
H25A H 0.0988 0.3359 0.1020 0.057 Uiso 1 1 calc R . .
C26 C 0.2272(10) 0.3831(8) 0.1637(7) 0.042(3) Uani 1 1 d . . .
H26A H 0.1988 0.3298 0.2110 0.050 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 O17 2.406(6) . ?
Pb1 O16 2.518(7) 2_656 ?
Pb1 O2 2.582(6) . ?
Pb1 O5 2.663(6) 1_455 ?
Pb1 O1W 2.679(16) . ?
Pb1 O15 2.691(7) 2_656 ?
Pb1 O16 2.731(7) . ?
Pb2 O14 2.386(6) . ?
Pb2 O14 2.441(6) 2_746 ?
Pb2 O10 2.522(7) . ?
Pb2 O12 2.570(6) 2_746 ?
Pb2 O1 2.614(6) . ?
Pb3 O7 2.379(6) 2_756 ?
Pb3 O5 2.479(6) . ?
Pb3 O7 2.498(6) . ?
Pb3 O11 2.585(7) . ?
Pb3 O8 2.752(7) 2_746 ?
Pb4 O18 2.395(7) . ?
Pb4 N1 2.547(7) . ?
Pb4 N2 2.584(7) . ?
Pb4 O9 2.589(6) 1_565 ?
Pb4 O17 2.755(7) . ?
Cl1 C5 1.752(9) . ?
Cl2 C11 1.737(9) . ?
S1 O3 1.451(7) . ?
S1 O1 1.451(6) . ?
S1 O2 1.477(6) . ?
S1 C1 1.776(8) . ?
S2 O4 1.433(7) . ?
S2 O6 1.451(7) . ?
S2 O5 1.488(6) . ?
S2 C3 1.765(9) . ?
S3 O8 1.446(6) . ?
S3 O9 1.459(6) . ?
S3 O10 1.468(7) . ?
S3 C7 1.788(9) . ?
S4 O13 1.448(7) . ?
S4 O11 1.465(7) . ?
S4 O12 1.476(6) . ?
S4 C9 1.773(9) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O5 Pb1 2.663(6) 1_655 ?
O7 C2 1.319(10) . ?
O7 Pb3 2.379(6) 2_756 ?
O8 Pb3 2.752(7) 2_746 ?
O9 Pb4 2.589(6) 1_545 ?
O12 Pb2 2.570(6) 2_746 ?
O14 C8 1.320(10) . ?
O14 Pb2 2.441(6) 2_746 ?
O15 C14 1.243(11) . ?
O15 Pb1 2.691(7) 2_656 ?
O16 C14 1.290(10) . ?
O16 Pb1 2.518(7) 2_656 ?
O17 C16 1.223(12) . ?
O18 C16 1.271(11) . ?
N1 C21 1.324(11) . ?
N1 C17 1.336(11) . ?
N2 C26 1.313(11) . ?
N2 C22 1.355(11) . ?
C1 C6 1.372(12) . ?
C1 C2 1.414(11) . ?
C2 C3 1.413(11) . ?
C3 C4 1.373(12) . ?
C4 C5 1.390(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.384(12) . ?
C6 H6A 0.9300 . ?
C7 C12 1.380(12) . ?
C7 C8 1.414(11) . ?
C8 C9 1.409(11) . ?
C9 C10 1.382(11) . ?
C10 C11 1.376(12) . ?
C10 H10A 0.9300 . ?
C11 C12 1.370(12) . ?
C12 H12A 0.9300 . ?
C13 C14 1.520(13) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 C16 1.497(16) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C17 C18 1.382(13) . ?
C17 H17A 0.9300 . ?
C18 C19 1.340(16) . ?
C18 H18A 0.9300 . ?
C19 C20 1.394(15) . ?
C19 H19A 0.9300 . ?
C20 C21 1.404(12) . ?
C20 H20A 0.9300 . ?
C21 C22 1.478(13) . ?
C22 C23 1.373(13) . ?
C23 C24 1.387(14) . ?
C23 H23A 0.9300 . ?
C24 C25 1.365(14) . ?
C24 H24A 0.9300 . ?
C25 C26 1.363(14) . ?
C25 H25A 0.9300 . ?
C26 H26A 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
O17 Pb1 O16 102.8(2) . 2_656 ?
O17 Pb1 O2 88.8(2) . . ?
O16 Pb1 O2 70.7(2) 2_656 . ?
O17 Pb1 O5 119.2(2) . 1_455 ?
O16 Pb1 O5 101.4(2) 2_656 1_455 ?
O2 Pb1 O5 151.96(18) . 1_455 ?
O17 Pb1 O1W 84.0(4) . . ?
O16 Pb1 O1W 172.4(3) 2_656 . ?
O2 Pb1 O1W 106.6(3) . . ?
O5 Pb1 O1W 77.6(3) 1_455 . ?
O17 Pb1 O15 79.5(2) . 2_656 ?
O16 Pb1 O15 50.2(2) 2_656 2_656 ?
O2 Pb1 O15 114.0(2) . 2_656 ?
O5 Pb1 O15 75.2(2) 1_455 2_656 ?
O1W Pb1 O15 135.5(3) . 2_656 ?
O17 Pb1 O16 173.5(2) . . ?
O16 Pb1 O16 77.4(2) 2_656 . ?
O2 Pb1 O16 85.1(2) . . ?
O5 Pb1 O16 66.86(18) 1_455 . ?
O1W Pb1 O16 95.4(4) . . ?
O15 Pb1 O16 105.2(2) 2_656 . ?
O14 Pb2 O14 69.9(2) . 2_746 ?
O14 Pb2 O10 71.2(2) . . ?
O14 Pb2 O10 117.3(2) 2_746 . ?
O14 Pb2 O12 116.60(19) . 2_746 ?
O14 Pb2 O12 74.23(19) 2_746 2_746 ?
O10 Pb2 O12 81.9(2) . 2_746 ?
O14 Pb2 O1 82.9(2) . . ?
O14 Pb2 O1 134.0(2) 2_746 . ?
O10 Pb2 O1 85.7(2) . . ?
O12 Pb2 O1 151.51(19) 2_746 . ?
O7 Pb3 O5 95.03(19) 2_756 . ?
O7 Pb3 O7 67.4(2) 2_756 . ?
O5 Pb3 O7 72.58(18) . . ?
O7 Pb3 O11 135.2(2) 2_756 . ?
O5 Pb3 O11 97.7(2) . . ?
O7 Pb3 O11 75.9(2) . . ?
O7 Pb3 O8 102.8(2) 2_756 2_746 ?
O5 Pb3 O8 144.2(2) . 2_746 ?
O7 Pb3 O8 143.1(2) . 2_746 ?
O11 Pb3 O8 91.1(2) . 2_746 ?
O18 Pb4 N1 77.8(2) . . ?
O18 Pb4 N2 77.4(2) . . ?
N1 Pb4 N2 63.6(2) . . ?
O18 Pb4 O9 82.3(3) . 1_565 ?
N1 Pb4 O9 80.6(2) . 1_565 ?
N2 Pb4 O9 141.7(2) . 1_565 ?
O18 Pb4 O17 49.5(2) . . ?
N1 Pb4 O17 121.6(2) . . ?
N2 Pb4 O17 116.2(2) . . ?
O9 Pb4 O17 70.3(2) 1_565 . ?
O3 S1 O1 112.9(4) . . ?
O3 S1 O2 111.1(4) . . ?
O1 S1 O2 112.5(4) . . ?
O3 S1 C1 106.4(4) . . ?
O1 S1 C1 108.0(4) . . ?
O2 S1 C1 105.5(4) . . ?
O4 S2 O6 114.1(4) . . ?
O4 S2 O5 112.9(4) . . ?
O6 S2 O5 109.9(4) . . ?
O4 S2 C3 106.1(4) . . ?
O6 S2 C3 106.7(4) . . ?
O5 S2 C3 106.7(4) . . ?
O8 S3 O9 113.7(4) . . ?
O8 S3 O10 112.5(4) . . ?
O9 S3 O10 110.8(4) . . ?
O8 S3 C7 108.0(4) . . ?
O9 S3 C7 103.7(4) . . ?
O10 S3 C7 107.5(4) . . ?
O13 S4 O11 116.4(5) . . ?
O13 S4 O12 112.5(4) . . ?
O11 S4 O12 109.1(4) . . ?
O13 S4 C9 106.5(4) . . ?
O11 S4 C9 106.2(4) . . ?
O12 S4 C9 105.4(4) . . ?
S1 O1 Pb2 160.6(4) . . ?
Pb1 O1W H1W1 124(10) . . ?
Pb1 O1W H1W2 92(10) . . ?
H1W1 O1W H1W2 109.0(18) . . ?
S1 O2 Pb1 116.8(3) . . ?
S2 O5 Pb3 128.2(3) . . ?
S2 O5 Pb1 106.5(3) . 1_655 ?
Pb3 O5 Pb1 124.9(2) . 1_655 ?
C2 O7 Pb3 114.9(5) . 2_756 ?
C2 O7 Pb3 127.1(5) . . ?
Pb3 O7 Pb3 112.6(2) 2_756 . ?
S3 O8 Pb3 135.5(5) . 2_746 ?
S3 O9 Pb4 148.7(4) . 1_545 ?
S3 O10 Pb2 131.7(4) . . ?
S4 O11 Pb3 146.7(5) . . ?
S4 O12 Pb2 118.5(3) . 2_746 ?
C8 O14 Pb2 115.3(5) . . ?
C8 O14 Pb2 131.3(5) . 2_746 ?
Pb2 O14 Pb2 110.1(2) . 2_746 ?
C14 O15 Pb1 90.4(6) . 2_656 ?
C14 O16 Pb1 97.3(6) . 2_656 ?
C14 O16 Pb1 119.0(6) . . ?
Pb1 O16 Pb1 102.6(2) 2_656 . ?
C16 O17 Pb1 148.3(7) . . ?
C16 O17 Pb4 86.1(6) . . ?
Pb1 O17 Pb4 106.3(3) . . ?
C16 O18 Pb4 102.1(7) . . ?
C21 N1 C17 119.2(8) . . ?
C21 N1 Pb4 120.8(6) . . ?
C17 N1 Pb4 119.9(6) . . ?
C26 N2 C22 117.8(9) . . ?
C26 N2 Pb4 122.2(6) . . ?
C22 N2 Pb4 118.3(6) . . ?
C6 C1 C2 122.2(8) . . ?
C6 C1 S1 119.6(7) . . ?
C2 C1 S1 118.2(7) . . ?
O7 C2 C3 121.3(8) . . ?
O7 C2 C1 123.0(8) . . ?
C3 C2 C1 115.7(8) . . ?
C4 C3 C2 123.0(8) . . ?
C4 C3 S2 120.1(6) . . ?
C2 C3 S2 116.7(7) . . ?
C3 C4 C5 118.2(8) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
C6 C5 C4 121.3(9) . . ?
C6 C5 Cl1 119.2(7) . . ?
C4 C5 Cl1 119.4(7) . . ?
C1 C6 C5 119.3(9) . . ?
C1 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
C12 C7 C8 121.5(8) . . ?
C12 C7 S3 118.6(7) . . ?
C8 C7 S3 119.7(7) . . ?
O14 C8 C9 122.7(8) . . ?
O14 C8 C7 121.6(8) . . ?
C9 C8 C7 115.7(8) . . ?
C10 C9 C8 122.6(8) . . ?
C10 C9 S4 119.4(7) . . ?
C8 C9 S4 118.0(6) . . ?
C11 C10 C9 119.3(8) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
C12 C11 C10 120.5(8) . . ?
C12 C11 Cl2 120.4(7) . . ?
C10 C11 Cl2 119.0(7) . . ?
C11 C12 C7 120.5(8) . . ?
C11 C12 H12A 119.8 . . ?
C7 C12 H12A 119.8 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O15 C14 O16 122.1(9) . . ?
O15 C14 C13 121.6(8) . . ?
O16 C14 C13 116.3(8) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O17 C16 O18 122.0(10) . . ?
O17 C16 C15 120.4(11) . . ?
O18 C16 C15 117.6(11) . . ?
N1 C17 C18 122.5(10) . . ?
N1 C17 H17A 118.8 . . ?
C18 C17 H17A 118.8 . . ?
C19 C18 C17 119.3(10) . . ?
C19 C18 H18A 120.3 . . ?
C17 C18 H18A 120.3 . . ?
C18 C19 C20 119.2(10) . . ?
C18 C19 H19A 120.4 . . ?
C20 C19 H19A 120.4 . . ?
C19 C20 C21 118.6(11) . . ?
C19 C20 H20A 120.7 . . ?
C21 C20 H20A 120.7 . . ?
N1 C21 C20 121.0(9) . . ?
N1 C21 C22 118.0(8) . . ?
C20 C21 C22 121.0(9) . . ?
N2 C22 C23 120.8(9) . . ?
N2 C22 C21 116.1(9) . . ?
C23 C22 C21 123.1(9) . . ?
C22 C23 C24 119.8(10) . . ?
C22 C23 H23A 120.1 . . ?
C24 C23 H23A 120.1 . . ?
C25 C24 C23 118.6(10) . . ?
C25 C24 H24A 120.7 . . ?
C23 C24 H24A 120.7 . . ?
C26 C25 C24 118.0(10) . . ?
C26 C25 H25A 121.0 . . ?
C24 C25 H25A 121.0 . . ?
N2 C26 C25 124.8(10) . . ?
N2 C26 H26A 117.6 . . ?
C25 C26 H26A 117.6 . . ?

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
O3 S1 O1 Pb2 -114.4(12) . . . . ?
O2 S1 O1 Pb2 12.3(14) . . . . ?
C1 S1 O1 Pb2 128.3(12) . . . . ?
O14 Pb2 O1 S1 -172.7(13) . . . . ?
O14 Pb2 O1 S1 -119.7(12) 2_746 . . . ?
O10 Pb2 O1 S1 115.8(13) . . . . ?
O12 Pb2 O1 S1 51.5(15) 2_746 . . . ?
O3 S1 O2 Pb1 8.8(5) . . . . ?
O1 S1 O2 Pb1 -118.9(4) . . . . ?
C1 S1 O2 Pb1 123.6(4) . . . . ?
O17 Pb1 O2 S1 -83.2(4) . . . . ?
O16 Pb1 O2 S1 172.7(4) 2_656 . . . ?
O5 Pb1 O2 S1 95.0(5) 1_455 . . . ?
O1W Pb1 O2 S1 0.2(5) . . . . ?
O15 Pb1 O2 S1 -161.2(3) 2_656 . . . ?
O16 Pb1 O2 S1 94.4(4) . . . . ?
O4 S2 O5 Pb3 61.4(5) . . . . ?
O6 S2 O5 Pb3 -170.0(4) . . . . ?
C3 S2 O5 Pb3 -54.7(5) . . . . ?
O4 S2 O5 Pb1 -126.2(4) . . . 1_655 ?
O6 S2 O5 Pb1 2.4(4) . . . 1_655 ?
C3 S2 O5 Pb1 117.7(3) . . . 1_655 ?
O7 Pb3 O5 S2 -52.9(5) 2_756 . . . ?
O7 Pb3 O5 S2 11.5(4) . . . . ?
O11 Pb3 O5 S2 84.1(5) . . . . ?
O8 Pb3 O5 S2 -173.1(4) 2_746 . . . ?
O7 Pb3 O5 Pb1 136.1(3) 2_756 . . 1_655 ?
O7 Pb3 O5 Pb1 -159.5(3) . . . 1_655 ?
O11 Pb3 O5 Pb1 -87.0(3) . . . 1_655 ?
O8 Pb3 O5 Pb1 15.8(5) 2_746 . . 1_655 ?
O7 Pb3 O7 C2 152.5(7) 2_756 . . . ?
O5 Pb3 O7 C2 49.2(6) . . . . ?
O11 Pb3 O7 C2 -53.8(6) . . . . ?
O8 Pb3 O7 C2 -126.3(6) 2_746 . . . ?
O7 Pb3 O7 Pb3 0.0 2_756 . . 2_756 ?
O5 Pb3 O7 Pb3 -103.3(3) . . . 2_756 ?
O11 Pb3 O7 Pb3 153.7(3) . . . 2_756 ?
O8 Pb3 O7 Pb3 81.2(4) 2_746 . . 2_756 ?
O9 S3 O8 Pb3 -124.3(5) . . . 2_746 ?
O10 S3 O8 Pb3 2.6(7) . . . 2_746 ?
C7 S3 O8 Pb3 121.1(6) . . . 2_746 ?
O8 S3 O9 Pb4 66.2(10) . . . 1_545 ?
O10 S3 O9 Pb4 -61.7(9) . . . 1_545 ?
C7 S3 O9 Pb4 -176.7(8) . . . 1_545 ?
O8 S3 O10 Pb2 99.0(6) . . . . ?
O9 S3 O10 Pb2 -132.5(5) . . . . ?
C7 S3 O10 Pb2 -19.8(6) . . . . ?
O14 Pb2 O10 S3 -21.0(5) . . . . ?
O14 Pb2 O10 S3 -75.2(6) 2_746 . . . ?
O12 Pb2 O10 S3 -142.7(6) 2_746 . . . ?
O1 Pb2 O10 S3 63.0(5) . . . . ?
O13 S4 O11 Pb3 -25.8(9) . . . . ?
O12 S4 O11 Pb3 102.8(8) . . . . ?
C9 S4 O11 Pb3 -144.0(7) . . . . ?
O7 Pb3 O11 S4 134.4(7) 2_756 . . . ?
O5 Pb3 O11 S4 29.2(8) . . . . ?
O7 Pb3 O11 S4 98.9(8) . . . . ?
O8 Pb3 O11 S4 -116.0(8) 2_746 . . . ?
O13 S4 O12 Pb2 172.2(4) . . . 2_746 ?
O11 S4 O12 Pb2 41.5(5) . . . 2_746 ?
C9 S4 O12 Pb2 -72.2(5) . . . 2_746 ?
O14 Pb2 O14 C8 -161.8(7) 2_746 . . . ?
O10 Pb2 O14 C8 68.3(6) . . . . ?
O12 Pb2 O14 C8 138.6(5) 2_746 . . . ?
O1 Pb2 O14 C8 -19.5(5) . . . . ?
O14 Pb2 O14 Pb2 0.0 2_746 . . 2_746 ?
O10 Pb2 O14 Pb2 -129.8(3) . . . 2_746 ?
O12 Pb2 O14 Pb2 -59.5(3) 2_746 . . 2_746 ?
O1 Pb2 O14 Pb2 142.3(3) . . . 2_746 ?
O16 Pb1 O16 C14 -105.8(7) 2_656 . . . ?
O2 Pb1 O16 C14 -34.6(7) . . . . ?
O5 Pb1 O16 C14 145.7(7) 1_455 . . . ?
O1W Pb1 O16 C14 71.7(7) . . . . ?
O15 Pb1 O16 C14 -148.1(6) 2_656 . . . ?
O16 Pb1 O16 Pb1 0.0 2_656 . . 2_656 ?
O2 Pb1 O16 Pb1 71.3(2) . . . 2_656 ?
O5 Pb1 O16 Pb1 -108.4(2) 1_455 . . 2_656 ?
O1W Pb1 O16 Pb1 177.5(3) . . . 2_656 ?
O15 Pb1 O16 Pb1 -42.3(3) 2_656 . . 2_656 ?
O16 Pb1 O17 C16 179.1(14) 2_656 . . . ?
O2 Pb1 O17 C16 109.2(14) . . . . ?
O5 Pb1 O17 C16 -69.8(14) 1_455 . . . ?
O1W Pb1 O17 C16 2.4(14) . . . . ?
O15 Pb1 O17 C16 -136.1(14) 2_656 . . . ?
O16 Pb1 O17 Pb4 -71.1(3) 2_656 . . . ?
O2 Pb1 O17 Pb4 -141.0(3) . . . . ?
O5 Pb1 O17 Pb4 39.9(3) 1_455 . . . ?
O1W Pb1 O17 Pb4 112.2(4) . . . . ?
O15 Pb1 O17 Pb4 -26.3(2) 2_656 . . . ?
O18 Pb4 O17 C16 2.9(7) . . . . ?
N1 Pb4 O17 C16 -28.8(7) . . . . ?
N2 Pb4 O17 C16 45.1(7) . . . . ?
O9 Pb4 O17 C16 -93.8(7) 1_565 . . . ?
O18 Pb4 O17 Pb1 -147.4(4) . . . . ?
N1 Pb4 O17 Pb1 -179.0(2) . . . . ?
N2 Pb4 O17 Pb1 -105.2(3) . . . . ?
O9 Pb4 O17 Pb1 115.9(3) 1_565 . . . ?
N1 Pb4 O18 C16 149.9(8) . . . . ?
N2 Pb4 O18 C16 -144.7(8) . . . . ?
O9 Pb4 O18 C16 67.9(7) 1_565 . . . ?
O17 Pb4 O18 C16 -2.8(7) . . . . ?
O18 Pb4 N1 C21 72.0(7) . . . . ?
N2 Pb4 N1 C21 -9.8(7) . . . . ?
O9 Pb4 N1 C21 156.0(8) 1_565 . . . ?
O17 Pb4 N1 C21 96.1(7) . . . . ?
O18 Pb4 N1 C17 -105.0(8) . . . . ?
N2 Pb4 N1 C17 173.3(8) . . . . ?
O9 Pb4 N1 C17 -20.9(7) 1_565 . . . ?
O17 Pb4 N1 C17 -80.8(8) . . . . ?
O18 Pb4 N2 C26 98.0(8) . . . . ?
N1 Pb4 N2 C26 -179.4(8) . . . . ?
O9 Pb4 N2 C26 157.6(7) 1_565 . . . ?
O17 Pb4 N2 C26 66.5(8) . . . . ?
O18 Pb4 N2 C22 -66.9(7) . . . . ?
N1 Pb4 N2 C22 15.6(6) . . . . ?
O9 Pb4 N2 C22 -7.4(9) 1_565 . . . ?
O17 Pb4 N2 C22 -98.5(7) . . . . ?
O3 S1 C1 C6 -7.0(8) . . . . ?
O1 S1 C1 C6 114.5(7) . . . . ?
O2 S1 C1 C6 -125.1(7) . . . . ?
O3 S1 C1 C2 169.3(6) . . . . ?
O1 S1 C1 C2 -69.2(7) . . . . ?
O2 S1 C1 C2 51.2(7) . . . . ?
Pb3 O7 C2 C3 97.5(8) 2_756 . . . ?
Pb3 O7 C2 C3 -54.4(10) . . . . ?
Pb3 O7 C2 C1 -82.1(8) 2_756 . . . ?
Pb3 O7 C2 C1 125.9(7) . . . . ?
C6 C1 C2 O7 -176.6(8) . . . . ?
S1 C1 C2 O7 7.2(11) . . . . ?
C6 C1 C2 C3 3.7(12) . . . . ?
S1 C1 C2 C3 -172.5(6) . . . . ?
O7 C2 C3 C4 174.7(7) . . . . ?
C1 C2 C3 C4 -5.7(12) . . . . ?
O7 C2 C3 S2 -9.9(10) . . . . ?
C1 C2 C3 S2 169.7(6) . . . . ?
O4 S2 C3 C4 117.4(7) . . . . ?
O6 S2 C3 C4 -4.6(8) . . . . ?
O5 S2 C3 C4 -122.0(7) . . . . ?
O4 S2 C3 C2 -58.1(7) . . . . ?
O6 S2 C3 C2 179.9(6) . . . . ?
O5 S2 C3 C2 62.5(7) . . . . ?
C2 C3 C4 C5 3.0(13) . . . . ?
S2 C3 C4 C5 -172.3(7) . . . . ?
C3 C4 C5 C6 2.0(13) . . . . ?
C3 C4 C5 Cl1 179.1(6) . . . . ?
C2 C1 C6 C5 0.8(13) . . . . ?
S1 C1 C6 C5 176.9(7) . . . . ?
C4 C5 C6 C1 -3.8(14) . . . . ?
Cl1 C5 C6 C1 179.1(6) . . . . ?
O8 S3 C7 C12 107.1(7) . . . . ?
O9 S3 C7 C12 -13.9(8) . . . . ?
O10 S3 C7 C12 -131.3(7) . . . . ?
O8 S3 C7 C8 -77.5(8) . . . . ?
O9 S3 C7 C8 161.5(7) . . . . ?
O10 S3 C7 C8 44.1(8) . . . . ?
Pb2 O14 C8 C9 105.3(8) . . . . ?
Pb2 O14 C8 C9 -51.8(11) 2_746 . . . ?
Pb2 O14 C8 C7 -72.0(9) . . . . ?
Pb2 O14 C8 C7 130.9(7) 2_746 . . . ?
C12 C7 C8 O14 176.4(8) . . . . ?
S3 C7 C8 O14 1.2(12) . . . . ?
C12 C7 C8 C9 -1.0(13) . . . . ?
S3 C7 C8 C9 -176.3(6) . . . . ?
O14 C8 C9 C10 -176.2(8) . . . . ?
C7 C8 C9 C10 1.2(13) . . . . ?
O14 C8 C9 S4 3.0(12) . . . . ?
C7 C8 C9 S4 -179.6(6) . . . . ?
O13 S4 C9 C10 -2.1(8) . . . . ?
O11 S4 C9 C10 122.5(7) . . . . ?
O12 S4 C9 C10 -121.8(7) . . . . ?
O13 S4 C9 C8 178.7(7) . . . . ?
O11 S4 C9 C8 -56.7(8) . . . . ?
O12 S4 C9 C8 59.0(8) . . . . ?
C8 C9 C10 C11 -1.2(13) . . . . ?
S4 C9 C10 C11 179.6(7) . . . . ?
C9 C10 C11 C12 1.0(13) . . . . ?
C9 C10 C11 Cl2 176.7(7) . . . . ?
C10 C11 C12 C7 -0.8(14) . . . . ?
Cl2 C11 C12 C7 -176.4(7) . . . . ?
C8 C7 C12 C11 0.8(14) . . . . ?
S3 C7 C12 C11 176.2(7) . . . . ?
Pb1 O15 C14 O16 -0.7(9) 2_656 . . . ?
Pb1 O15 C14 C13 178.3(8) 2_656 . . . ?
Pb1 O16 C14 O15 0.8(10) 2_656 . . . ?
Pb1 O16 C14 O15 109.6(9) . . . . ?
Pb1 O16 C14 C13 -178.3(7) 2_656 . . . ?
Pb1 O16 C14 C13 -69.5(9) . . . . ?
Pb1 O17 C16 O18 110.2(14) . . . . ?
Pb4 O17 C16 O18 -4.9(12) . . . . ?
Pb1 O17 C16 C15 -68(2) . . . . ?
Pb4 O17 C16 C15 176.8(14) . . . . ?
Pb4 O18 C16 O17 5.7(14) . . . . ?
Pb4 O18 C16 C15 -175.9(13) . . . . ?
C21 N1 C17 C18 -0.7(16) . . . . ?
Pb4 N1 C17 C18 176.2(8) . . . . ?
N1 C17 C18 C19 1.4(19) . . . . ?
C17 C18 C19 C20 -3(2) . . . . ?
C18 C19 C20 C21 3.9(19) . . . . ?
C17 N1 C21 C20 1.7(15) . . . . ?
Pb4 N1 C21 C20 -175.3(8) . . . . ?
C17 N1 C21 C22 -179.1(9) . . . . ?
Pb4 N1 C21 C22 3.9(12) . . . . ?
C19 C20 C21 N1 -3.3(17) . . . . ?
C19 C20 C21 C22 177.6(10) . . . . ?
C26 N2 C22 C23 -2.6(14) . . . . ?
Pb4 N2 C22 C23 163.1(7) . . . . ?
C26 N2 C22 C21 174.2(8) . . . . ?
Pb4 N2 C22 C21 -20.1(10) . . . . ?
N1 C21 C22 N2 11.0(13) . . . . ?
C20 C21 C22 N2 -169.9(9) . . . . ?
N1 C21 C22 C23 -172.3(10) . . . . ?
C20 C21 C22 C23 6.9(15) . . . . ?
N2 C22 C23 C24 1.1(16) . . . . ?
C21 C22 C23 C24 -175.5(9) . . . . ?
C22 C23 C24 C25 1.7(17) . . . . ?
C23 C24 C25 C26 -2.9(17) . . . . ?
C22 N2 C26 C25 1.3(16) . . . . ?
Pb4 N2 C26 C25 -163.7(9) . . . . ?
C24 C25 C26 N2 1.5(18) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O13 0.85(4) 1.93(4) 2.773(13) 168(17) 1_455
O1W H1W2 O3 0.85(4) 2.31(11) 3.069(16) 149(20) .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         2.412
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.265
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex4
_database_code_depnum_ccdc_archive 'CCDC 1010477'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H5 Cl O5 Pb S, 0.5(C10 H8 N2)'
_chemical_formula_sum            'C11 H9 Cl N O5 Pb S'
_chemical_formula_weight         509.91

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'
Cl Cl 0.1484 0.1585 '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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_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                   33.4445(16)
_cell_length_b                   10.3580(5)
_cell_length_c                   7.9750(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.332(4)
_cell_angle_gamma                90.00
_cell_volume                     2708.8(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1692
_cell_measurement_theta_min      3.92
_cell_measurement_theta_max      25.98

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1895
_exptl_absorpt_coefficient_mu    12.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1737
_exptl_absorpt_correction_T_max  0.2191
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4380
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2632
_reflns_number_gt                2129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.1206P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2632
_refine_ls_number_parameters     187
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1876
_refine_ls_wR_factor_gt          0.1739
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.023
_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 -0.231161(15) 0.07299(4) 0.03462(6) 0.0216(2) Uani 1 1 d . . .
Cl1 Cl -0.04261(14) 0.4094(5) 0.0082(8) 0.0619(14) Uani 1 1 d . . .
S1 S -0.19964(11) 0.2999(3) -0.2891(4) 0.0240(7) Uani 1 1 d . . .
O1 O -0.2159(3) 0.1705(9) -0.2706(12) 0.032(2) Uani 1 1 d . . .
O1W O -0.1825(3) 0.0873(9) 0.3515(15) 0.030(2) Uani 1 1 d D . .
H1W1 H -0.189(4) 0.162(6) 0.38(2) 0.045 Uiso 1 1 d D . .
H1W2 H -0.1568(10) 0.085(11) 0.36(2) 0.045 Uiso 1 1 d D . .
O2 O -0.1808(3) 0.3120(10) -0.4325(12) 0.032(2) Uani 1 1 d . . .
O3 O -0.2302(3) 0.4020(10) -0.2831(12) 0.030(2) Uani 1 1 d . . .
O4 O -0.2106(3) 0.2977(8) 0.0706(11) 0.027(2) Uani 1 1 d . . .
C1 C -0.1607(4) 0.3257(13) -0.1065(17) 0.024(3) Uani 1 1 d . . .
C2 C -0.1728(4) 0.3253(12) 0.0553(16) 0.028(3) Uani 1 1 d . . .
C3 C -0.1435(5) 0.3538(13) 0.1947(19) 0.032(3) Uani 1 1 d . . .
H3A H -0.1502 0.3555 0.3024 0.038 Uiso 1 1 calc R . .
C4 C -0.1040(5) 0.3802(16) 0.179(2) 0.035(3) Uani 1 1 d . . .
H4A H -0.0844 0.3999 0.2757 0.042 Uiso 1 1 calc R . .
C5 C -0.0934(5) 0.3774(17) 0.021(2) 0.041(4) Uani 1 1 d . . .
C6 C -0.1208(4) 0.3542(15) -0.1206(18) 0.032(3) Uani 1 1 d . . .
H6A H -0.1135 0.3570 -0.2272 0.038 Uiso 1 1 calc R . .
N1 N -0.1023(5) 0.0606(17) 0.512(2) 0.055(5) Uani 1 1 d . . .
C7 C -0.0829(8) -0.044(2) 0.578(4) 0.079(8) Uani 1 1 d . . .
H7A H -0.0975 -0.1213 0.5622 0.095 Uiso 1 1 calc R . .
C8 C -0.0443(8) -0.0509(18) 0.665(3) 0.063(6) Uani 1 1 d . . .
H8A H -0.0329 -0.1303 0.7016 0.075 Uiso 1 1 calc R . .
C9 C -0.0218(5) 0.0599(15) 0.698(3) 0.042(4) Uani 1 1 d . . .
C10 C -0.0405(7) 0.172(2) 0.645(3) 0.068(6) Uani 1 1 d . . .
H10A H -0.0273 0.2500 0.6703 0.081 Uiso 1 1 calc R . .
C11 C -0.0796(8) 0.167(2) 0.552(3) 0.076(7) Uani 1 1 d . . .
H11A H -0.0915 0.2454 0.5118 0.091 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 O4 2.377(9) 7_455 ?
Pb1 O4 2.429(8) . ?
Pb1 O3 2.582(9) 7_455 ?
Pb1 O1W 2.728(11) . ?
Pb1 O1 2.774(9) . ?
Pb1 O3 2.794(10) 4_444 ?
Pb1 O1W 2.912(11) 6 ?
Pb1 O1 2.954(9) 6_556 ?
Cl1 C5 1.753(16) . ?
S1 O2 1.416(9) . ?
S1 O1 1.464(10) . ?
S1 O3 1.479(10) . ?
S1 C1 1.773(14) . ?
O1 Pb1 2.954(9) 6 ?
O1W Pb1 2.912(11) 6_556 ?
O1W H1W1 0.85(9) . ?
O1W H1W2 0.85(9) . ?
O3 Pb1 2.582(9) 7_455 ?
O3 Pb1 2.794(10) 4_454 ?
O4 C2 1.323(14) . ?
O4 Pb1 2.377(9) 7_455 ?
C1 C6 1.392(18) . ?
C1 C2 1.427(17) . ?
C2 C3 1.36(2) . ?
C3 C4 1.38(2) . ?
C3 H3A 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4A 0.9300 . ?
C5 C6 1.33(2) . ?
C6 H6A 0.9300 . ?
N1 C7 1.32(3) . ?
N1 C11 1.34(3) . ?
C7 C8 1.34(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.37(3) . ?
C8 H8A 0.9300 . ?
C9 C10 1.34(2) . ?
C9 C9 1.53(4) 2_556 ?
C10 C11 1.37(3) . ?
C10 H10A 0.9300 . ?
C11 H11A 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
O4 Pb1 O4 72.2(3) 7_455 . ?
O4 Pb1 O3 73.5(3) 7_455 7_455 ?
O4 Pb1 O3 89.2(3) . 7_455 ?
O4 Pb1 O1W 126.5(3) 7_455 . ?
O4 Pb1 O1W 74.6(3) . . ?
O3 Pb1 O1W 65.2(3) 7_455 . ?
O4 Pb1 O1 76.4(3) 7_455 . ?
O4 Pb1 O1 70.0(3) . . ?
O3 Pb1 O1 147.5(3) 7_455 . ?
O1W Pb1 O1 127.8(3) . . ?
O4 Pb1 O3 82.7(3) 7_455 4_444 ?
O4 Pb1 O3 140.6(3) . 4_444 ?
O3 Pb1 O3 112.6(3) 7_455 4_444 ?
O1W Pb1 O3 143.8(3) . 4_444 ?
O1 Pb1 O3 74.9(3) . 4_444 ?
O4 Pb1 O1W 130.1(3) 7_455 6 ?
O4 Pb1 O1W 115.6(3) . 6 ?
O3 Pb1 O1W 148.8(3) 7_455 6 ?
O1W Pb1 O1W 101.8(3) . 6 ?
O1 Pb1 O1W 63.3(3) . 6 ?
O3 Pb1 O1W 60.2(3) 4_444 6 ?
O4 Pb1 O1 135.4(3) 7_455 6_556 ?
O4 Pb1 O1 137.8(3) . 6_556 ?
O3 Pb1 O1 75.1(3) 7_455 6_556 ?
O1W Pb1 O1 63.2(3) . 6_556 ?
O1 Pb1 O1 136.9(3) . 6_556 ?
O3 Pb1 O1 81.0(3) 4_444 6_556 ?
O1W Pb1 O1 73.8(3) 6 6_556 ?
O4 Pb1 Pb1 36.58(19) 7_455 7_455 ?
O4 Pb1 Pb1 35.7(2) . 7_455 ?
O3 Pb1 Pb1 79.5(2) 7_455 7_455 ?
O1W Pb1 Pb1 101.4(2) . 7_455 ?
O1 Pb1 Pb1 69.0(2) . 7_455 ?
O3 Pb1 Pb1 113.9(2) 4_444 7_455 ?
O1W Pb1 Pb1 131.7(2) 6 7_455 ?
O1 Pb1 Pb1 154.07(17) 6_556 7_455 ?
O4 Pb1 Pb1 91.2(2) 7_455 6 ?
O4 Pb1 Pb1 113.5(2) . 6 ?
O3 Pb1 Pb1 147.7(2) 7_455 6 ?
O1W Pb1 Pb1 140.9(2) . 6 ?
O1 Pb1 Pb1 43.52(19) . 6 ?
O3 Pb1 Pb1 35.82(19) 4_444 6 ?
O1W Pb1 Pb1 39.3(2) 6 6 ?
O1 Pb1 Pb1 99.05(17) 6_556 6 ?
Pb1 Pb1 Pb1 105.163(16) 7_455 6 ?
O4 Pb1 Pb1 112.3(2) 7_455 6_556 ?
O4 Pb1 Pb1 106.3(2) . 6_556 ?
O3 Pb1 Pb1 39.3(2) 7_455 6_556 ?
O1W Pb1 Pb1 42.5(2) . 6_556 ?
O1 Pb1 Pb1 169.5(2) . 6_556 ?
O3 Pb1 Pb1 111.19(19) 4_444 6_556 ?
O1W Pb1 Pb1 111.7(2) 6 6_556 ?
O1 Pb1 Pb1 40.29(17) 6_556 6_556 ?
Pb1 Pb1 Pb1 114.101(17) 7_455 6_556 ?
Pb1 Pb1 Pb1 138.47(2) 6 6_556 ?
O2 S1 O1 113.3(6) . . ?
O2 S1 O3 112.5(6) . . ?
O1 S1 O3 112.2(6) . . ?
O2 S1 C1 106.2(6) . . ?
O1 S1 C1 106.4(6) . . ?
O3 S1 C1 105.5(6) . . ?
S1 O1 Pb1 123.9(5) . . ?
S1 O1 Pb1 139.2(5) . 6 ?
Pb1 O1 Pb1 96.2(3) . 6 ?
Pb1 O1W Pb1 98.2(3) . 6_556 ?
Pb1 O1W H1W1 98(10) . . ?
Pb1 O1W H1W1 101(10) 6_556 . ?
Pb1 O1W H1W2 117(10) . . ?
Pb1 O1W H1W2 128(10) 6_556 . ?
H1W1 O1W H1W2 109.7(19) . . ?
S1 O3 Pb1 123.4(5) . 7_455 ?
S1 O3 Pb1 130.9(5) . 4_454 ?
Pb1 O3 Pb1 104.9(3) 7_455 4_454 ?
C2 O4 Pb1 125.2(8) . 7_455 ?
C2 O4 Pb1 116.7(8) . . ?
Pb1 O4 Pb1 107.8(3) 7_455 . ?
C6 C1 C2 121.4(12) . . ?
C6 C1 S1 121.7(10) . . ?
C2 C1 S1 116.7(9) . . ?
O4 C2 C3 121.3(11) . . ?
O4 C2 C1 122.0(10) . . ?
C3 C2 C1 116.7(11) . . ?
C2 C3 C4 121.3(13) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C5 C4 C3 120.1(15) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
C6 C5 C4 121.6(15) . . ?
C6 C5 Cl1 120.1(12) . . ?
C4 C5 Cl1 118.4(14) . . ?
C5 C6 C1 118.8(13) . . ?
C5 C6 H6A 120.6 . . ?
C1 C6 H6A 120.6 . . ?
C7 N1 C11 112.1(19) . . ?
N1 C7 C8 126(2) . . ?
N1 C7 H7A 116.8 . . ?
C8 C7 H7A 116.8 . . ?
C7 C8 C9 120(2) . . ?
C7 C8 H8A 120.2 . . ?
C9 C8 H8A 120.2 . . ?
C10 C9 C8 117(2) . . ?
C10 C9 C9 120.5(13) . 2_556 ?
C8 C9 C9 122.3(13) . 2_556 ?
C9 C10 C11 119(2) . . ?
C9 C10 H10A 120.7 . . ?
C11 C10 H10A 120.7 . . ?
N1 C11 C10 126(2) . . ?
N1 C11 H11A 117.0 . . ?
C10 C11 H11A 117.0 . . ?

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
O2 S1 O1 Pb1 158.3(6) . . . . ?
O3 S1 O1 Pb1 -72.8(8) . . . . ?
C1 S1 O1 Pb1 42.0(9) . . . . ?
O2 S1 O1 Pb1 -10.0(12) . . . 6 ?
O3 S1 O1 Pb1 118.9(9) . . . 6 ?
C1 S1 O1 Pb1 -126.3(9) . . . 6 ?
O4 Pb1 O1 S1 81.1(7) 7_455 . . . ?
O4 Pb1 O1 S1 5.3(7) . . . . ?
O3 Pb1 O1 S1 58.5(11) 7_455 . . . ?
O1W Pb1 O1 S1 -44.9(9) . . . . ?
O3 Pb1 O1 S1 167.0(8) 4_444 . . . ?
O1W Pb1 O1 S1 -129.1(9) 6 . . . ?
O1 Pb1 O1 S1 -134.6(3) 6_556 . . . ?
Pb1 Pb1 O1 S1 43.4(7) 7_455 . . . ?
Pb1 Pb1 O1 S1 -172.4(10) 6 . . . ?
Pb1 Pb1 O1 S1 -65.9(15) 6_556 . . . ?
O4 Pb1 O1 Pb1 -106.6(3) 7_455 . . 6 ?
O4 Pb1 O1 Pb1 177.6(4) . . . 6 ?
O3 Pb1 O1 Pb1 -129.1(5) 7_455 . . 6 ?
O1W Pb1 O1 Pb1 127.5(3) . . . 6 ?
O3 Pb1 O1 Pb1 -20.6(3) 4_444 . . 6 ?
O1W Pb1 O1 Pb1 43.3(3) 6 . . 6 ?
O1 Pb1 O1 Pb1 37.8(8) 6_556 . . 6 ?
Pb1 Pb1 O1 Pb1 -144.2(3) 7_455 . . 6 ?
Pb1 Pb1 O1 Pb1 106.5(10) 6_556 . . 6 ?
O4 Pb1 O1W Pb1 83.7(4) 7_455 . . 6_556 ?
O4 Pb1 O1W Pb1 137.1(4) . . . 6_556 ?
O3 Pb1 O1W Pb1 40.7(3) 7_455 . . 6_556 ?
O1 Pb1 O1W Pb1 -174.5(3) . . . 6_556 ?
O3 Pb1 O1W Pb1 -54.2(6) 4_444 . . 6_556 ?
O1W Pb1 O1W Pb1 -109.3(4) 6 . . 6_556 ?
O1 Pb1 O1W Pb1 -44.5(3) 6_556 . . 6_556 ?
Pb1 Pb1 O1W Pb1 113.3(2) 7_455 . . 6_556 ?
Pb1 Pb1 O1W Pb1 -114.5(3) 6 . . 6_556 ?
O2 S1 O3 Pb1 -175.9(6) . . . 7_455 ?
O1 S1 O3 Pb1 54.8(8) . . . 7_455 ?
C1 S1 O3 Pb1 -60.6(8) . . . 7_455 ?
O2 S1 O3 Pb1 16.0(10) . . . 4_454 ?
O1 S1 O3 Pb1 -113.3(7) . . . 4_454 ?
C1 S1 O3 Pb1 131.3(7) . . . 4_454 ?
O4 Pb1 O4 C2 -147.0(9) 7_455 . . . ?
O3 Pb1 O4 C2 140.1(8) 7_455 . . . ?
O1W Pb1 O4 C2 75.6(8) . . . . ?
O1 Pb1 O4 C2 -65.4(8) . . . . ?
O3 Pb1 O4 C2 -93.9(9) 4_444 . . . ?
O1W Pb1 O4 C2 -20.3(9) 6 . . . ?
O1 Pb1 O4 C2 73.6(9) 6_556 . . . ?
Pb1 Pb1 O4 C2 -147.0(9) 7_455 . . . ?
Pb1 Pb1 O4 C2 -63.7(8) 6 . . . ?
Pb1 Pb1 O4 C2 104.3(8) 6_556 . . . ?
O4 Pb1 O4 Pb1 0.0 7_455 . . 7_455 ?
O3 Pb1 O4 Pb1 -72.9(4) 7_455 . . 7_455 ?
O1W Pb1 O4 Pb1 -137.4(4) . . . 7_455 ?
O1 Pb1 O4 Pb1 81.6(4) . . . 7_455 ?
O3 Pb1 O4 Pb1 53.1(6) 4_444 . . 7_455 ?
O1W Pb1 O4 Pb1 126.7(3) 6 . . 7_455 ?
O1 Pb1 O4 Pb1 -139.4(3) 6_556 . . 7_455 ?
Pb1 Pb1 O4 Pb1 83.3(3) 6 . . 7_455 ?
Pb1 Pb1 O4 Pb1 -108.7(3) 6_556 . . 7_455 ?
O2 S1 C1 C6 1.2(15) . . . . ?
O1 S1 C1 C6 122.2(13) . . . . ?
O3 S1 C1 C6 -118.4(13) . . . . ?
O2 S1 C1 C2 176.7(10) . . . . ?
O1 S1 C1 C2 -62.3(12) . . . . ?
O3 S1 C1 C2 57.0(12) . . . . ?
Pb1 O4 C2 C3 113.2(12) 7_455 . . . ?
Pb1 O4 C2 C3 -106.2(12) . . . . ?
Pb1 O4 C2 C1 -67.3(14) 7_455 . . . ?
Pb1 O4 C2 C1 73.3(14) . . . . ?
C6 C1 C2 O4 -179.7(13) . . . . ?
S1 C1 C2 O4 4.8(17) . . . . ?
C6 C1 C2 C3 0(2) . . . . ?
S1 C1 C2 C3 -175.7(10) . . . . ?
O4 C2 C3 C4 178.8(13) . . . . ?
C1 C2 C3 C4 -1(2) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C3 C4 C5 C6 2(3) . . . . ?
C3 C4 C5 Cl1 -179.1(13) . . . . ?
C4 C5 C6 C1 -3(3) . . . . ?
Cl1 C5 C6 C1 178.3(12) . . . . ?
C2 C1 C6 C5 2(2) . . . . ?
S1 C1 C6 C5 177.4(13) . . . . ?
C11 N1 C7 C8 -4(5) . . . . ?
N1 C7 C8 C9 3(5) . . . . ?
C7 C8 C9 C10 2(4) . . . . ?
C7 C8 C9 C9 178(3) . . . 2_556 ?
C8 C9 C10 C11 -4(4) . . . . ?
C9 C9 C10 C11 180(2) 2_556 . . . ?
C7 N1 C11 C10 1(4) . . . . ?
C9 C10 C11 N1 3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O2 0.85(9) 2.14(9) 2.889(13) 146(15) 1_556
O1W H1W2 N1 0.85(9) 2.01(11) 2.750(19) 145(18) .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.430
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 1010474'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 Cl2 O9 Pb2 S2'
_chemical_formula_sum            'C12 H8 Cl2 O9 Pb2 S2'
_chemical_formula_weight         845.58

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'
Cl Cl 0.1484 0.1585 '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           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                   7.1884(5)
_cell_length_b                   10.6571(7)
_cell_length_c                   12.4644(8)
_cell_angle_alpha                92.225(5)
_cell_angle_beta                 91.080(6)
_cell_angle_gamma                109.457(6)
_cell_volume                     899.14(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2119
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.87

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    19.275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1068
_exptl_absorpt_correction_T_max  0.1381
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4793
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3522
_reflns_number_gt                2750
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0139P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3522
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.32666(5) 0.59914(4) 1.03664(3) 0.02071(12) Uani 1 1 d . . .
Pb2 Pb 0.29777(5) 0.05796(4) 1.06493(3) 0.02149(12) Uani 1 1 d . . .
Cl1 Cl 0.0891(5) 0.3652(3) 0.4662(2) 0.0460(8) Uani 1 1 d . . .
Cl2 Cl 0.2868(5) 0.0840(4) 0.4522(3) 0.0505(9) Uani 1 1 d . . .
S1 S 0.1286(3) 0.2879(3) 0.8921(2) 0.0174(6) Uani 1 1 d . . .
S2 S 0.1525(4) -0.1473(3) 0.8368(2) 0.0254(6) Uani 1 1 d . . .
O1 O 0.0753(9) 0.3839(7) 0.9635(6) 0.0226(17) Uani 1 1 d . . .
O1W O 0.1438(11) 0.5003(8) 1.2124(7) 0.042(2) Uani 1 1 d . . .
H1W1 H 0.1680 0.4328 1.2348 0.062 Uiso 1 1 d R . .
H1W2 H 0.0311 0.4720 1.1804 0.062 Uiso 1 1 d R . .
O2 O -0.0426(10) 0.1753(7) 0.8537(6) 0.0290(19) Uani 1 1 d . . .
O3 O 0.2862(9) 0.2489(6) 0.9417(6) 0.0199(16) Uani 1 1 d . . .
O4 O 0.4834(9) 0.5280(7) 0.8907(5) 0.0195(16) Uani 1 1 d . . .
O5 O -0.0174(12) -0.2277(7) 0.7729(6) 0.040(2) Uani 1 1 d . . .
O6 O 0.0907(9) -0.0797(7) 0.9289(5) 0.0228(17) Uani 1 1 d . . .
O7 O 0.2872(11) -0.2154(7) 0.8730(6) 0.035(2) Uani 1 1 d . . .
O8 O 0.5077(9) 0.0813(7) 0.9092(6) 0.0206(16) Uani 1 1 d . . .
C1 C 0.2272(13) 0.3761(9) 0.7776(8) 0.016(2) Uani 1 1 d . . .
C2 C 0.1357(14) 0.3368(11) 0.6774(8) 0.023(2) Uani 1 1 d . . .
H2A H 0.0286 0.2584 0.6683 0.027 Uiso 1 1 calc R . .
C3 C 0.2030(16) 0.4135(11) 0.5919(8) 0.024(2) Uani 1 1 d . . .
C4 C 0.3640(16) 0.5322(11) 0.6064(9) 0.030(3) Uani 1 1 d . . .
H4A H 0.4072 0.5855 0.5484 0.036 Uiso 1 1 calc R . .
C5 C 0.4592(15) 0.5709(11) 0.7056(9) 0.024(3) Uani 1 1 d . . .
H5A H 0.5679 0.6485 0.7135 0.029 Uiso 1 1 calc R . .
C6 C 0.3919(13) 0.4932(10) 0.7945(8) 0.023(3) Uani 1 1 d . . .
C7 C 0.2904(15) -0.0162(10) 0.7570(8) 0.023(2) Uani 1 1 d . . .
C8 C 0.2375(17) -0.0166(11) 0.6505(9) 0.029(3) Uani 1 1 d . . .
H8A H 0.1264 -0.0828 0.6208 0.034 Uiso 1 1 calc R . .
C9 C 0.3519(16) 0.0833(11) 0.5877(9) 0.028(3) Uani 1 1 d . . .
C10 C 0.5169(16) 0.1797(11) 0.6308(9) 0.031(3) Uani 1 1 d . . .
H10A H 0.5955 0.2450 0.5881 0.037 Uiso 1 1 calc R . .
C11 C 0.5656(15) 0.1787(10) 0.7390(9) 0.024(2) Uani 1 1 d . . .
H11A H 0.6754 0.2461 0.7686 0.028 Uiso 1 1 calc R . .
C12 C 0.4577(15) 0.0821(10) 0.8036(9) 0.020(2) 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 O4 2.386(7) . ?
Pb1 O4 2.408(6) 2_667 ?
Pb1 O1 2.524(7) . ?
Pb1 O1W 2.646(8) . ?
Pb1 O3 2.715(6) 2_667 ?
Pb2 O6 2.346(7) . ?
Pb2 O8 2.380(6) 2_657 ?
Pb2 O8 2.451(7) . ?
Pb2 O3 2.619(6) . ?
Cl1 C3 1.731(10) . ?
Cl2 C9 1.745(11) . ?
S1 O2 1.461(7) . ?
S1 O3 1.465(6) . ?
S1 O1 1.479(7) . ?
S1 C1 1.766(10) . ?
S2 O5 1.441(7) . ?
S2 O7 1.464(7) . ?
S2 O6 1.484(7) . ?
S2 C7 1.774(10) . ?
O1W H1W1 0.8500 . ?
O1W H1W2 0.8500 . ?
O3 Pb1 2.715(6) 2_667 ?
O4 C6 1.334(11) . ?
O4 Pb1 2.408(6) 2_667 ?
O8 C12 1.359(12) . ?
O8 Pb2 2.380(6) 2_657 ?
C1 C2 1.383(13) . ?
C1 C6 1.411(13) . ?
C2 C3 1.365(14) . ?
C2 H2A 0.9300 . ?
C3 C4 1.404(15) . ?
C4 C5 1.380(14) . ?
C4 H4A 0.9300 . ?
C5 C6 1.405(14) . ?
C5 H5A 0.9300 . ?
C7 C8 1.373(14) . ?
C7 C12 1.404(14) . ?
C8 C9 1.389(15) . ?
C8 H8A 0.9300 . ?
C9 C10 1.368(15) . ?
C10 C11 1.389(15) . ?
C10 H10A 0.9300 . ?
C11 C12 1.365(14) . ?
C11 H11A 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
O4 Pb1 O4 72.5(3) . 2_667 ?
O4 Pb1 O1 75.2(2) . . ?
O4 Pb1 O1 88.8(2) 2_667 . ?
O4 Pb1 O1W 138.2(2) . . ?
O4 Pb1 O1W 75.3(2) 2_667 . ?
O1 Pb1 O1W 78.2(2) . . ?
O4 Pb1 O3 74.6(2) . 2_667 ?
O4 Pb1 O3 69.7(2) 2_667 2_667 ?
O1 Pb1 O3 147.0(2) . 2_667 ?
O1W Pb1 O3 117.5(2) . 2_667 ?
O6 Pb2 O8 95.4(2) . 2_657 ?
O6 Pb2 O8 75.5(2) . . ?
O8 Pb2 O8 73.3(3) 2_657 . ?
O6 Pb2 O3 83.3(2) . . ?
O8 Pb2 O3 138.9(2) 2_657 . ?
O8 Pb2 O3 66.5(2) . . ?
O2 S1 O3 113.8(4) . . ?
O2 S1 O1 112.9(4) . . ?
O3 S1 O1 110.9(4) . . ?
O2 S1 C1 106.3(5) . . ?
O3 S1 C1 106.8(4) . . ?
O1 S1 C1 105.5(4) . . ?
O5 S2 O7 115.9(5) . . ?
O5 S2 O6 110.3(5) . . ?
O7 S2 O6 110.8(5) . . ?
O5 S2 C7 107.3(5) . . ?
O7 S2 C7 107.0(5) . . ?
O6 S2 C7 104.8(5) . . ?
S1 O1 Pb1 122.5(4) . . ?
Pb1 O1W H1W1 115.3 . . ?
Pb1 O1W H1W2 93.2 . . ?
H1W1 O1W H1W2 107.3 . . ?
S1 O3 Pb2 134.9(4) . . ?
S1 O3 Pb1 126.2(4) . 2_667 ?
Pb2 O3 Pb1 97.8(2) . 2_667 ?
C6 O4 Pb1 120.9(5) . . ?
C6 O4 Pb1 120.2(5) . 2_667 ?
Pb1 O4 Pb1 107.5(3) . 2_667 ?
S2 O6 Pb2 126.5(4) . . ?
C12 O8 Pb2 111.0(6) . 2_657 ?
C12 O8 Pb2 128.6(6) . . ?
Pb2 O8 Pb2 106.7(3) 2_657 . ?
C2 C1 C6 121.9(9) . . ?
C2 C1 S1 120.7(8) . . ?
C6 C1 S1 117.1(8) . . ?
C3 C2 C1 119.8(10) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119.7(10) . . ?
C2 C3 Cl1 120.1(9) . . ?
C4 C3 Cl1 120.2(8) . . ?
C5 C4 C3 121.0(10) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 120.1(10) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
O4 C6 C5 121.0(9) . . ?
O4 C6 C1 121.5(9) . . ?
C5 C6 C1 117.5(9) . . ?
C8 C7 C12 121.6(10) . . ?
C8 C7 S2 119.7(8) . . ?
C12 C7 S2 118.6(8) . . ?
C7 C8 C9 119.1(11) . . ?
C7 C8 H8A 120.4 . . ?
C9 C8 H8A 120.4 . . ?
C10 C9 C8 120.5(11) . . ?
C10 C9 Cl2 119.9(9) . . ?
C8 C9 Cl2 119.6(9) . . ?
C9 C10 C11 119.2(10) . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C12 C11 C10 122.2(10) . . ?
C12 C11 H11A 118.9 . . ?
C10 C11 H11A 118.9 . . ?
O8 C12 C11 121.8(9) . . ?
O8 C12 C7 120.9(9) . . ?
C11 C12 C7 117.4(10) . . ?

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
O2 S1 O1 Pb1 -175.9(4) . . . . ?
O3 S1 O1 Pb1 55.1(5) . . . . ?
C1 S1 O1 Pb1 -60.3(5) . . . . ?
O4 Pb1 O1 S1 16.8(4) . . . . ?
O4 Pb1 O1 S1 -55.4(5) 2_667 . . . ?
O1W Pb1 O1 S1 -130.6(5) . . . . ?
O3 Pb1 O1 S1 -7.6(7) 2_667 . . . ?
O2 S1 O3 Pb2 -37.6(7) . . . . ?
O1 S1 O3 Pb2 90.9(6) . . . . ?
C1 S1 O3 Pb2 -154.6(5) . . . . ?
O2 S1 O3 Pb1 157.3(4) . . . 2_667 ?
O1 S1 O3 Pb1 -74.2(5) . . . 2_667 ?
C1 S1 O3 Pb1 40.3(6) . . . 2_667 ?
O6 Pb2 O3 S1 53.6(6) . . . . ?
O8 Pb2 O3 S1 144.2(5) 2_657 . . . ?
O8 Pb2 O3 S1 130.6(6) . . . . ?
O6 Pb2 O3 Pb1 -138.5(2) . . . 2_667 ?
O8 Pb2 O3 Pb1 -47.9(4) 2_657 . . 2_667 ?
O8 Pb2 O3 Pb1 -61.5(2) . . . 2_667 ?
O4 Pb1 O4 C6 143.5(8) 2_667 . . . ?
O1 Pb1 O4 C6 50.1(7) . . . . ?
O1W Pb1 O4 C6 102.4(7) . . . . ?
O3 Pb1 O4 C6 -143.4(7) 2_667 . . . ?
O4 Pb1 O4 Pb1 0.0 2_667 . . 2_667 ?
O1 Pb1 O4 Pb1 -93.5(3) . . . 2_667 ?
O1W Pb1 O4 Pb1 -41.2(4) . . . 2_667 ?
O3 Pb1 O4 Pb1 73.1(2) 2_667 . . 2_667 ?
O5 S2 O6 Pb2 177.6(5) . . . . ?
O7 S2 O6 Pb2 47.8(6) . . . . ?
C7 S2 O6 Pb2 -67.2(6) . . . . ?
O8 Pb2 O6 S2 -43.6(5) 2_657 . . . ?
O8 Pb2 O6 S2 27.6(5) . . . . ?
O3 Pb2 O6 S2 95.0(5) . . . . ?
O6 Pb2 O8 C12 35.6(7) . . . . ?
O8 Pb2 O8 C12 135.9(8) 2_657 . . . ?
O3 Pb2 O8 C12 -53.4(7) . . . . ?
O6 Pb2 O8 Pb2 -100.3(3) . . . 2_657 ?
O8 Pb2 O8 Pb2 0.0 2_657 . . 2_657 ?
O3 Pb2 O8 Pb2 170.7(3) . . . 2_657 ?
O2 S1 C1 C2 3.0(9) . . . . ?
O3 S1 C1 C2 124.8(8) . . . . ?
O1 S1 C1 C2 -117.1(8) . . . . ?
O2 S1 C1 C6 178.0(7) . . . . ?
O3 S1 C1 C6 -60.2(8) . . . . ?
O1 S1 C1 C6 57.9(8) . . . . ?
C6 C1 C2 C3 -1.0(14) . . . . ?
S1 C1 C2 C3 173.7(8) . . . . ?
C1 C2 C3 C4 -0.4(15) . . . . ?
C1 C2 C3 Cl1 -179.9(8) . . . . ?
C2 C3 C4 C5 1.8(16) . . . . ?
Cl1 C3 C4 C5 -178.7(8) . . . . ?
C3 C4 C5 C6 -1.8(16) . . . . ?
Pb1 O4 C6 C5 112.0(8) . . . . ?
Pb1 O4 C6 C5 -109.0(9) 2_667 . . . ?
Pb1 O4 C6 C1 -69.3(10) . . . . ?
Pb1 O4 C6 C1 69.7(10) 2_667 . . . ?
C4 C5 C6 O4 179.1(9) . . . . ?
C4 C5 C6 C1 0.4(14) . . . . ?
C2 C1 C6 O4 -177.7(8) . . . . ?
S1 C1 C6 O4 7.5(12) . . . . ?
C2 C1 C6 C5 1.0(14) . . . . ?
S1 C1 C6 C5 -173.9(7) . . . . ?
O5 S2 C7 C8 -7.4(10) . . . . ?
O7 S2 C7 C8 117.6(9) . . . . ?
O6 S2 C7 C8 -124.7(9) . . . . ?
O5 S2 C7 C12 175.8(8) . . . . ?
O7 S2 C7 C12 -59.2(10) . . . . ?
O6 S2 C7 C12 58.5(9) . . . . ?
C12 C7 C8 C9 -0.3(16) . . . . ?
S2 C7 C8 C9 -177.1(8) . . . . ?
C7 C8 C9 C10 1.0(16) . . . . ?
C7 C8 C9 Cl2 179.9(8) . . . . ?
C8 C9 C10 C11 -1.8(17) . . . . ?
Cl2 C9 C10 C11 179.3(8) . . . . ?
C9 C10 C11 C12 2.1(16) . . . . ?
Pb2 O8 C12 C11 -95.1(10) 2_657 . . . ?
Pb2 O8 C12 C11 130.5(8) . . . . ?
Pb2 O8 C12 C7 85.8(10) 2_657 . . . ?
Pb2 O8 C12 C7 -48.6(12) . . . . ?
C10 C11 C12 O8 179.3(9) . . . . ?
C10 C11 C12 C7 -1.5(15) . . . . ?
C8 C7 C12 O8 179.8(9) . . . . ?
S2 C7 C12 O8 -3.5(14) . . . . ?
C8 C7 C12 C11 0.6(16) . . . . ?
S2 C7 C12 C11 177.4(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O5 0.85 2.09 2.754(11) 134.8 2_557

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.687
_refine_diff_density_rms         0.268
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 1010475'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H22 Cl2 N4 O8 Pb2 S2'
_chemical_formula_sum            'C32 H22 Cl2 N4 O8 Pb2 S2'
_chemical_formula_weight         1139.94

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   7.5895(4)
_cell_length_b                   13.3371(6)
_cell_length_c                   16.5241(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.337(4)
_cell_angle_gamma                90.00
_cell_volume                     1671.20(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1488
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    10.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2186
_exptl_absorpt_correction_T_max  0.2707
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5991
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3807
_reflns_number_gt                3025
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0340P)²+0.2516P] 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         3807
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0873
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.28666(3) 0.41501(2) 0.481913(18) 0.02944(11) Uani 1 1 d . . .
Cl1 Cl 0.2120(3) 0.90453(17) 0.24531(18) 0.0607(7) Uani 1 1 d . . .
S1 S 0.2539(2) 0.68362(14) 0.52233(12) 0.0293(4) Uani 1 1 d . . .
O1 O 0.1468(7) 0.7678(4) 0.5446(4) 0.0444(15) Uani 1 1 d . . .
O2 O 0.1562(7) 0.5886(4) 0.5220(4) 0.0374(13) Uani 1 1 d . . .
O3 O 0.4196(6) 0.6759(4) 0.5693(3) 0.0347(12) Uani 1 1 d . . .
O4 O 0.4878(6) 0.5540(3) 0.4255(3) 0.0261(11) Uani 1 1 d . . .
N1 N 0.1559(8) 0.3677(5) 0.6204(4) 0.0335(15) Uani 1 1 d . . .
N2 N 0.2758(8) 0.2242(5) 0.5212(5) 0.0404(17) Uani 1 1 d . . .
C1 C 0.3092(9) 0.7029(5) 0.4198(5) 0.0278(16) Uani 1 1 d . . .
C2 C 0.4178(9) 0.6308(5) 0.3832(5) 0.0279(16) Uani 1 1 d . . .
C3 C 0.4483(9) 0.6450(6) 0.3010(5) 0.0322(17) Uani 1 1 d . . .
H3A H 0.5127 0.5971 0.2738 0.039 Uiso 1 1 calc R . .
C4 C 0.3859(10) 0.7273(6) 0.2596(5) 0.039(2) Uani 1 1 d . . .
H4A H 0.4082 0.7351 0.2050 0.047 Uiso 1 1 calc R . .
C5 C 0.2904(10) 0.7983(6) 0.2987(6) 0.040(2) Uani 1 1 d . . .
C6 C 0.2479(9) 0.7865(5) 0.3779(5) 0.0335(18) Uani 1 1 d . . .
H6A H 0.1789 0.8339 0.4031 0.040 Uiso 1 1 calc R . .
C7 C 0.1102(10) 0.4425(6) 0.6694(5) 0.0379(19) Uani 1 1 d . . .
H7A H 0.0960 0.5065 0.6478 0.046 Uiso 1 1 calc R . .
C8 C 0.0837(11) 0.4284(7) 0.7500(6) 0.051(2) Uani 1 1 d . . .
H8A H 0.0501 0.4815 0.7824 0.062 Uiso 1 1 calc R . .
C9 C 0.1082(11) 0.3333(8) 0.7820(6) 0.052(3) Uani 1 1 d . . .
H9A H 0.0961 0.3221 0.8371 0.063 Uiso 1 1 calc R . .
C10 C 0.1504(11) 0.2558(7) 0.7321(6) 0.050(2) Uani 1 1 d . . .
H10A H 0.1648 0.1912 0.7525 0.060 Uiso 1 1 calc R . .
C11 C 0.1714(9) 0.2751(6) 0.6504(5) 0.037(2) Uani 1 1 d . . .
C12 C 0.2130(10) 0.1943(6) 0.5926(6) 0.043(2) Uani 1 1 d . . .
C13 C 0.1830(12) 0.0926(7) 0.6084(8) 0.062(3) Uani 1 1 d . . .
H13A H 0.1409 0.0723 0.6578 0.074 Uiso 1 1 calc R . .
C14 C 0.2172(14) 0.0226(7) 0.5488(9) 0.077(4) Uani 1 1 d . . .
H14A H 0.1985 -0.0452 0.5581 0.092 Uiso 1 1 calc R . .
C15 C 0.2786(13) 0.0541(8) 0.4762(9) 0.073(4) Uani 1 1 d . . .
H15A H 0.3020 0.0083 0.4355 0.088 Uiso 1 1 calc R . .
C16 C 0.3045(11) 0.1550(7) 0.4652(7) 0.054(3) Uani 1 1 d . . .
H16A H 0.3446 0.1763 0.4156 0.065 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 O4 2.287(5) 3_666 ?
Pb1 O4 2.599(4) . ?
Pb1 N1 2.609(6) . ?
Pb1 O2 2.614(5) . ?
Pb1 N2 2.628(7) . ?
Pb1 O3 2.704(5) 3_666 ?
Cl1 C5 1.760(8) . ?
S1 O1 1.442(5) . ?
S1 O3 1.454(5) . ?
S1 O2 1.468(5) . ?
S1 C1 1.781(8) . ?
O3 Pb1 2.704(5) 3_666 ?
O4 C2 1.337(8) . ?
O4 Pb1 2.287(5) 3_666 ?
N1 C11 1.334(9) . ?
N1 C7 1.339(10) . ?
N2 C16 1.331(11) . ?
N2 C12 1.351(11) . ?
C1 C6 1.384(10) . ?
C1 C2 1.417(10) . ?
C2 C3 1.401(10) . ?
C3 C4 1.369(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.369(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.367(12) . ?
C7 H7A 0.9300 . ?
C8 C9 1.384(12) . ?
C8 H8A 0.9300 . ?
C9 C10 1.369(13) . ?
C9 H9A 0.9300 . ?
C10 C11 1.389(12) . ?
C10 H10A 0.9300 . ?
C11 C12 1.483(12) . ?
C12 C13 1.402(11) . ?
C13 C14 1.389(16) . ?
C13 H13A 0.9300 . ?
C14 C15 1.370(17) . ?
C14 H14A 0.9300 . ?
C15 C16 1.374(14) . ?
C15 H15A 0.9300 . ?
C16 H16A 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
O4 Pb1 O4 71.15(18) 3_666 . ?
O4 Pb1 N1 75.97(18) 3_666 . ?
O4 Pb1 N1 137.50(18) . . ?
O4 Pb1 O2 87.23(17) 3_666 . ?
O4 Pb1 O2 72.13(14) . . ?
N1 Pb1 O2 80.23(18) . . ?
O4 Pb1 N2 92.3(2) 3_666 . ?
O4 Pb1 N2 143.53(17) . . ?
N1 Pb1 N2 62.1(2) . . ?
O2 Pb1 N2 141.16(18) . . ?
O4 Pb1 O3 71.71(16) 3_666 3_666 ?
O4 Pb1 O3 72.78(14) . 3_666 ?
N1 Pb1 O3 120.93(18) . 3_666 ?
O2 Pb1 O3 143.36(15) . 3_666 ?
N2 Pb1 O3 71.18(18) . 3_666 ?
O1 S1 O3 113.7(3) . . ?
O1 S1 O2 112.5(3) . . ?
O3 S1 O2 111.5(3) . . ?
O1 S1 C1 106.7(3) . . ?
O3 S1 C1 106.6(3) . . ?
O2 S1 C1 105.0(3) . . ?
S1 O2 Pb1 124.7(3) . . ?
S1 O3 Pb1 124.8(3) . 3_666 ?
C2 O4 Pb1 118.8(4) . 3_666 ?
C2 O4 Pb1 120.5(4) . . ?
Pb1 O4 Pb1 108.85(18) 3_666 . ?
C11 N1 C7 119.1(7) . . ?
C11 N1 Pb1 121.3(5) . . ?
C7 N1 Pb1 117.9(5) . . ?
C16 N2 C12 118.5(8) . . ?
C16 N2 Pb1 119.4(6) . . ?
C12 N2 Pb1 121.1(5) . . ?
C6 C1 C2 121.5(7) . . ?
C6 C1 S1 120.3(6) . . ?
C2 C1 S1 118.1(5) . . ?
O4 C2 C3 122.1(7) . . ?
O4 C2 C1 121.5(7) . . ?
C3 C2 C1 116.4(7) . . ?
C4 C3 C2 121.7(7) . . ?
C4 C3 H3A 119.1 . . ?
C2 C3 H3A 119.1 . . ?
C3 C4 C5 119.8(8) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C6 C5 C4 121.4(7) . . ?
C6 C5 Cl1 118.9(7) . . ?
C4 C5 Cl1 119.6(7) . . ?
C5 C6 C1 118.9(7) . . ?
C5 C6 H6A 120.5 . . ?
C1 C6 H6A 120.5 . . ?
N1 C7 C8 122.6(8) . . ?
N1 C7 H7A 118.7 . . ?
C8 C7 H7A 118.7 . . ?
C7 C8 C9 118.4(9) . . ?
C7 C8 H8A 120.8 . . ?
C9 C8 H8A 120.8 . . ?
C10 C9 C8 119.5(9) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C9 C10 C11 118.9(8) . . ?
C9 C10 H10A 120.5 . . ?
C11 C10 H10A 120.5 . . ?
N1 C11 C10 121.4(8) . . ?
N1 C11 C12 116.8(8) . . ?
C10 C11 C12 121.8(8) . . ?
N2 C12 C13 120.9(9) . . ?
N2 C12 C11 116.1(7) . . ?
C13 C12 C11 122.9(9) . . ?
C14 C13 C12 118.8(10) . . ?
C14 C13 H13A 120.6 . . ?
C12 C13 H13A 120.6 . . ?
C15 C14 C13 119.7(9) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 118.1(11) . . ?
C14 C15 H15A 120.9 . . ?
C16 C15 H15A 120.9 . . ?
N2 C16 C15 124.0(10) . . ?
N2 C16 H16A 118.0 . . ?
C15 C16 H16A 118.0 . . ?

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
O1 S1 O2 Pb1 178.2(4) . . . . ?
O3 S1 O2 Pb1 -52.6(5) . . . . ?
C1 S1 O2 Pb1 62.5(4) . . . . ?
O4 Pb1 O2 S1 52.9(4) 3_666 . . . ?
O4 Pb1 O2 S1 -18.1(4) . . . . ?
N1 Pb1 O2 S1 129.2(4) . . . . ?
N2 Pb1 O2 S1 143.1(4) . . . . ?
O3 Pb1 O2 S1 -0.8(6) 3_666 . . . ?
O1 S1 O3 Pb1 -154.7(3) . . . 3_666 ?
O2 S1 O3 Pb1 76.7(4) . . . 3_666 ?
C1 S1 O3 Pb1 -37.4(4) . . . 3_666 ?
O4 Pb1 O4 C2 -142.3(6) 3_666 . . . ?
N1 Pb1 O4 C2 -101.1(5) . . . . ?
O2 Pb1 O4 C2 -49.1(5) . . . . ?
N2 Pb1 O4 C2 150.7(5) . . . . ?
O3 Pb1 O4 C2 141.6(5) 3_666 . . . ?
O4 Pb1 O4 Pb1 0.0 3_666 . . 3_666 ?
N1 Pb1 O4 Pb1 41.2(3) . . . 3_666 ?
O2 Pb1 O4 Pb1 93.2(2) . . . 3_666 ?
N2 Pb1 O4 Pb1 -66.9(4) . . . 3_666 ?
O3 Pb1 O4 Pb1 -76.04(19) 3_666 . . 3_666 ?
O4 Pb1 N1 C11 -89.4(6) 3_666 . . . ?
O4 Pb1 N1 C11 -129.5(5) . . . . ?
O2 Pb1 N1 C11 -179.0(6) . . . . ?
N2 Pb1 N1 C11 10.8(5) . . . . ?
O3 Pb1 N1 C11 -31.2(6) 3_666 . . . ?
O4 Pb1 N1 C7 75.1(5) 3_666 . . . ?
O4 Pb1 N1 C7 35.1(6) . . . . ?
O2 Pb1 N1 C7 -14.5(5) . . . . ?
N2 Pb1 N1 C7 175.4(6) . . . . ?
O3 Pb1 N1 C7 133.3(5) 3_666 . . . ?
O4 Pb1 N2 C16 -119.7(6) 3_666 . . . ?
O4 Pb1 N2 C16 -59.1(8) . . . . ?
N1 Pb1 N2 C16 167.4(7) . . . . ?
O2 Pb1 N2 C16 151.9(6) . . . . ?
O3 Pb1 N2 C16 -49.9(6) 3_666 . . . ?
O4 Pb1 N2 C12 71.5(6) 3_666 . . . ?
O4 Pb1 N2 C12 132.2(6) . . . . ?
N1 Pb1 N2 C12 -1.3(6) . . . . ?
O2 Pb1 N2 C12 -16.8(8) . . . . ?
O3 Pb1 N2 C12 141.3(7) 3_666 . . . ?
O1 S1 C1 C6 -0.7(7) . . . . ?
O3 S1 C1 C6 -122.6(6) . . . . ?
O2 S1 C1 C6 119.0(6) . . . . ?
O1 S1 C1 C2 178.9(5) . . . . ?
O3 S1 C1 C2 57.0(6) . . . . ?
O2 S1 C1 C2 -61.5(6) . . . . ?
Pb1 O4 C2 C3 107.3(7) 3_666 . . . ?
Pb1 O4 C2 C3 -114.1(6) . . . . ?
Pb1 O4 C2 C1 -72.3(7) 3_666 . . . ?
Pb1 O4 C2 C1 66.4(8) . . . . ?
C6 C1 C2 O4 174.9(6) . . . . ?
S1 C1 C2 O4 -4.6(9) . . . . ?
C6 C1 C2 C3 -4.7(10) . . . . ?
S1 C1 C2 C3 175.8(5) . . . . ?
O4 C2 C3 C4 -175.6(6) . . . . ?
C1 C2 C3 C4 4.0(11) . . . . ?
C2 C3 C4 C5 -0.2(11) . . . . ?
C3 C4 C5 C6 -3.4(12) . . . . ?
C3 C4 C5 Cl1 179.5(6) . . . . ?
C4 C5 C6 C1 2.7(12) . . . . ?
Cl1 C5 C6 C1 179.8(5) . . . . ?
C2 C1 C6 C5 1.5(11) . . . . ?
S1 C1 C6 C5 -179.0(6) . . . . ?
C11 N1 C7 C8 2.0(12) . . . . ?
Pb1 N1 C7 C8 -162.9(7) . . . . ?
N1 C7 C8 C9 1.1(13) . . . . ?
C7 C8 C9 C10 -2.8(13) . . . . ?
C8 C9 C10 C11 1.4(13) . . . . ?
C7 N1 C11 C10 -3.5(11) . . . . ?
Pb1 N1 C11 C10 160.9(6) . . . . ?
C7 N1 C11 C12 176.9(7) . . . . ?
Pb1 N1 C11 C12 -18.8(9) . . . . ?
C9 C10 C11 N1 1.8(12) . . . . ?
C9 C10 C11 C12 -178.6(8) . . . . ?
C16 N2 C12 C13 1.6(13) . . . . ?
Pb1 N2 C12 C13 170.5(6) . . . . ?
C16 N2 C12 C11 -175.8(7) . . . . ?
Pb1 N2 C12 C11 -6.9(10) . . . . ?
N1 C11 C12 N2 16.6(10) . . . . ?
C10 C11 C12 N2 -163.0(8) . . . . ?
N1 C11 C12 C13 -160.7(8) . . . . ?
C10 C11 C12 C13 19.7(13) . . . . ?
N2 C12 C13 C14 -0.7(14) . . . . ?
C11 C12 C13 C14 176.5(8) . . . . ?
C12 C13 C14 C15 -0.2(16) . . . . ?
C13 C14 C15 C16 0.1(17) . . . . ?
C12 N2 C16 C15 -1.8(14) . . . . ?
Pb1 N2 C16 C15 -170.8(8) . . . . ?
C14 C15 C16 N2 0.9(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.220
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex5
_database_code_depnum_ccdc_archive 'CCDC 1010478'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 Cl O9 Pb S2, H2 O'
_chemical_formula_sum            'C6 H9 Cl O10 Pb S2'
_chemical_formula_weight         547.89

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   7.7120(3)
_cell_length_b                   9.8706(5)
_cell_length_c                   17.3297(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.495(4)
_cell_angle_gamma                90.00
_cell_volume                     1313.11(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1610
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    13.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1650
_exptl_absorpt_correction_T_max  0.2088
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4899
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2994
_reflns_number_gt                2385
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0417P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2994
_refine_ls_number_parameters     202
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.022
_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 0.59672(4) 0.94650(3) 0.178694(19) 0.03020(13) Uani 1 1 d . . .
Cl1 Cl 0.8973(3) 1.1377(3) 0.62809(14) 0.0462(6) Uani 1 1 d . . .
S1 S 0.6097(3) 0.7046(2) 0.47381(14) 0.0339(5) Uani 1 1 d . . .
S2 S 0.7417(3) 1.1748(2) 0.31713(13) 0.0276(5) Uani 1 1 d . . .
O1 O 0.7691(9) 0.6285(7) 0.4657(4) 0.0461(17) Uani 1 1 d . . .
O1W O 0.8477(9) 1.0094(7) 0.1034(4) 0.0434(16) Uani 1 1 d D . .
H1W1 H 0.798(13) 0.990(9) 0.059(3) 0.065 Uiso 1 1 d D . .
H1W2 H 0.890(13) 1.089(5) 0.102(5) 0.065 Uiso 1 1 d D . .
O2W O 0.8070(7) 0.7708(7) 0.2029(4) 0.0423(17) Uani 1 1 d D . .
H2W1 H 0.802(11) 0.709(8) 0.237(5) 0.063 Uiso 1 1 d D . .
H2W2 H 0.911(4) 0.797(10) 0.202(6) 0.063 Uiso 1 1 d D . .
O2 O 0.5387(8) 0.6786(7) 0.5468(4) 0.0440(17) Uani 1 1 d . . .
O3 O 0.4812(8) 0.6866(6) 0.4065(4) 0.0406(16) Uani 1 1 d . . .
O3W O 0.2275(11) 1.0678(7) 0.1947(5) 0.056(2) Uani 1 1 d D . .
H3W1 H 0.195(16) 0.995(7) 0.215(5) 0.084 Uiso 1 1 d D . .
H3W2 H 0.194(16) 1.069(11) 0.1465(17) 0.084 Uiso 1 1 d D . .
O4 O 0.8510(8) 1.2914(6) 0.3371(4) 0.0392(16) Uani 1 1 d . . .
O5 O 0.5628(7) 1.2099(6) 0.2891(4) 0.0366(15) Uani 1 1 d . . .
O6 O 0.8156(7) 1.0839(6) 0.2627(4) 0.0352(15) Uani 1 1 d . . .
O7 O 0.5857(8) 0.9023(6) 0.3356(4) 0.0347(14) Uani 1 1 d D . .
H7O H 0.525(11) 0.836(7) 0.349(6) 0.052 Uiso 1 1 d D . .
C1 C 0.6686(10) 0.8805(9) 0.4722(5) 0.0289(19) Uani 1 1 d . . .
C2 C 0.7409(11) 0.9358(10) 0.5422(5) 0.037(2) Uani 1 1 d . . .
H2A H 0.7440 0.8869 0.5882 0.044 Uiso 1 1 calc R . .
C3 C 0.8080(11) 1.0661(9) 0.5408(5) 0.032(2) Uani 1 1 d . . .
C4 C 0.8088(11) 1.1375(10) 0.4728(5) 0.035(2) Uani 1 1 d . . .
H4A H 0.8594 1.2230 0.4730 0.042 Uiso 1 1 calc R . .
C5 C 0.7353(11) 1.0831(9) 0.4044(5) 0.0274(19) Uani 1 1 d . . .
C6 C 0.6622(10) 0.9514(8) 0.4032(5) 0.0278(18) 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 O2W 2.384(6) . ?
Pb1 O1W 2.514(7) . ?
Pb1 O6 2.517(6) . ?
Pb1 O2 2.598(6) 4_575 ?
Pb1 O5 2.723(6) 2_645 ?
Cl1 C3 1.750(9) . ?
S1 O2 1.449(7) . ?
S1 O1 1.459(7) . ?
S1 O3 1.468(6) . ?
S1 C1 1.795(9) . ?
S2 O4 1.448(6) . ?
S2 O6 1.458(6) . ?
S2 O5 1.460(6) . ?
S2 C5 1.767(9) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2W H2W1 0.85(5) . ?
O2W H2W2 0.85(5) . ?
O2 Pb1 2.598(6) 4_576 ?
O3W H3W1 0.85(5) . ?
O3W H3W2 0.85(5) . ?
O5 Pb1 2.723(6) 2_655 ?
O7 C6 1.349(10) . ?
O7 H7O 0.85(5) . ?
C1 C6 1.382(12) . ?
C1 C2 1.397(12) . ?
C2 C3 1.388(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.374(12) . ?
C4 C5 1.373(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.417(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2W Pb1 O1W 74.1(2) . . ?
O2W Pb1 O6 83.3(2) . . ?
O1W Pb1 O6 70.1(2) . . ?
O2W Pb1 O2 82.3(2) . 4_575 ?
O1W Pb1 O2 74.7(2) . 4_575 ?
O6 Pb1 O2 144.5(2) . 4_575 ?
O2W Pb1 O5 69.7(2) . 2_645 ?
O1W Pb1 O5 134.7(2) . 2_645 ?
O6 Pb1 O5 129.42(19) . 2_645 ?
O2 Pb1 O5 74.3(2) 4_575 2_645 ?
O2 S1 O1 112.6(4) . . ?
O2 S1 O3 112.9(4) . . ?
O1 S1 O3 111.8(4) . . ?
O2 S1 C1 107.6(4) . . ?
O1 S1 C1 106.3(4) . . ?
O3 S1 C1 104.9(4) . . ?
O4 S2 O6 112.9(4) . . ?
O4 S2 O5 113.6(4) . . ?
O6 S2 O5 110.2(4) . . ?
O4 S2 C5 105.4(4) . . ?
O6 S2 C5 106.5(4) . . ?
O5 S2 C5 107.6(4) . . ?
Pb1 O1W H1W1 96(7) . . ?
Pb1 O1W H1W2 124(8) . . ?
H1W1 O1W H1W2 109.1(18) . . ?
Pb1 O2W H2W1 125(7) . . ?
Pb1 O2W H2W2 114(6) . . ?
H2W1 O2W H2W2 109.8(18) . . ?
S1 O2 Pb1 143.6(4) . 4_576 ?
H3W1 O3W H3W2 109.9(18) . . ?
S2 O5 Pb1 124.5(4) . 2_655 ?
S2 O6 Pb1 115.1(3) . . ?
C6 O7 H7O 104(7) . . ?
C6 C1 C2 122.1(8) . . ?
C6 C1 S1 121.0(7) . . ?
C2 C1 S1 116.4(7) . . ?
C3 C2 C1 117.7(8) . . ?
C3 C2 H2A 121.1 . . ?
C1 C2 H2A 121.1 . . ?
C4 C3 C2 121.5(8) . . ?
C4 C3 Cl1 120.1(7) . . ?
C2 C3 Cl1 118.4(7) . . ?
C5 C4 C3 120.3(8) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 120.2(8) . . ?
C4 C5 S2 119.7(7) . . ?
C6 C5 S2 120.1(6) . . ?
O7 C6 C1 123.0(8) . . ?
O7 C6 C5 118.9(7) . . ?
C1 C6 C5 118.1(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
O1 S1 O2 Pb1 5.3(8) . . . 4_576 ?
O3 S1 O2 Pb1 133.2(6) . . . 4_576 ?
C1 S1 O2 Pb1 -111.5(7) . . . 4_576 ?
O4 S2 O5 Pb1 -23.3(6) . . . 2_655 ?
O6 S2 O5 Pb1 -151.2(4) . . . 2_655 ?
C5 S2 O5 Pb1 93.1(5) . . . 2_655 ?
O4 S2 O6 Pb1 -153.0(3) . . . . ?
O5 S2 O6 Pb1 -24.7(5) . . . . ?
C5 S2 O6 Pb1 91.7(4) . . . . ?
O2W Pb1 O6 S2 -139.6(4) . . . . ?
O1W Pb1 O6 S2 144.9(4) . . . . ?
O2 Pb1 O6 S2 153.8(3) 4_575 . . . ?
O5 Pb1 O6 S2 -82.9(4) 2_645 . . . ?
O2 S1 C1 C6 -149.5(7) . . . . ?
O1 S1 C1 C6 89.6(7) . . . . ?
O3 S1 C1 C6 -29.0(8) . . . . ?
O2 S1 C1 C2 38.2(8) . . . . ?
O1 S1 C1 C2 -82.7(7) . . . . ?
O3 S1 C1 C2 158.7(7) . . . . ?
C6 C1 C2 C3 -0.1(13) . . . . ?
S1 C1 C2 C3 172.0(7) . . . . ?
C1 C2 C3 C4 -2.1(13) . . . . ?
C1 C2 C3 Cl1 179.4(7) . . . . ?
C2 C3 C4 C5 3.0(14) . . . . ?
Cl1 C3 C4 C5 -178.5(7) . . . . ?
C3 C4 C5 C6 -1.7(13) . . . . ?
C3 C4 C5 S2 -178.7(7) . . . . ?
O4 S2 C5 C4 7.1(8) . . . . ?
O6 S2 C5 C4 127.3(7) . . . . ?
O5 S2 C5 C4 -114.5(7) . . . . ?
O4 S2 C5 C6 -169.8(7) . . . . ?
O6 S2 C5 C6 -49.7(7) . . . . ?
O5 S2 C5 C6 68.6(7) . . . . ?
C2 C1 C6 O7 -176.8(8) . . . . ?
S1 C1 C6 O7 11.4(12) . . . . ?
C2 C1 C6 C5 1.3(13) . . . . ?
S1 C1 C6 C5 -170.4(6) . . . . ?
C4 C5 C6 O7 177.8(8) . . . . ?
S2 C5 C6 O7 -5.3(11) . . . . ?
C4 C5 C6 C1 -0.4(12) . . . . ?
S2 C5 C6 C1 176.5(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O1 0.85(5) 1.99(5) 2.763(9) 151(10) 4_575
O1W H1W1 O2 0.85(5) 2.59(8) 3.104(9) 120(8) 4_575
O1W H1W2 Cl1 0.85(5) 2.73(5) 3.527(8) 155(10) 4_585
O2W H2W1 O3W 0.85(5) 1.858(16) 2.706(10) 174(9) 2_645
O2W H2W2 O4 0.85(5) 2.01(5) 2.798(9) 154(11) 2_745
O3W H3W1 O4 0.85(5) 2.22(9) 2.838(9) 130(9) 2_645
O3W H3W2 O1 0.85(5) 2.08(5) 2.846(11) 150(10) 2_655
O7 H7O O3 0.85(5) 1.83(4) 2.623(9) 155(10) .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.449
_refine_diff_density_min         -2.398
_refine_diff_density_rms         0.229
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex7
_database_code_depnum_ccdc_archive 'CCDC 1010480'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Cl2 N2 O19 Pb3 S4, 2(H2 O)'
_chemical_formula_sum            'C24 H26 Cl2 N2 O21 Pb3 S4'
_chemical_formula_weight         1499.18

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'
Cl Cl 0.1484 0.1585 '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                   9.9814(5)
_cell_length_b                   14.3511(8)
_cell_length_c                   14.5242(8)
_cell_angle_alpha                70.188(5)
_cell_angle_beta                 83.453(5)
_cell_angle_gamma                87.315(5)
_cell_volume                     1944.53(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3351
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    13.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1653
_exptl_absorpt_correction_T_max  0.1966
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11565
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         27.56
_reflns_number_total             8869
_reflns_number_gt                6653
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0375P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8869
_refine_ls_number_parameters     511
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.0984
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.86860(4) 0.13034(3) 0.44746(3) 0.03234(11) Uani 1 1 d . . .
Pb2 Pb 0.47358(3) 0.17419(3) 0.49975(2) 0.02518(10) Uani 1 1 d . . .
Pb3 Pb 0.22577(4) 0.54057(3) 0.27566(3) 0.04463(13) Uani 1 1 d . . .
Cl1 Cl 0.5364(3) 0.2875(2) -0.03740(18) 0.0488(7) Uani 1 1 d . . .
Cl2 Cl 0.6750(3) -0.0408(2) 1.00062(18) 0.0537(8) Uani 1 1 d . . .
S1 S 0.7181(3) 0.02498(19) 0.2889(2) 0.0396(6) Uani 1 1 d . . .
S2 S 0.5383(3) 0.39566(18) 0.28378(18) 0.0325(6) Uani 1 1 d . . .
S3 S 0.7727(3) -0.09726(19) 0.64863(19) 0.0334(6) Uani 1 1 d . . .
S4 S 0.6310(3) 0.27096(18) 0.66764(17) 0.0330(6) Uani 1 1 d . . .
O1W O 0.9961(7) 0.1379(6) 0.5972(5) 0.0468(19) Uani 1 1 d . . .
H1W1 H 1.0096 0.1982 0.5907 0.070 Uiso 1 1 d R . .
H1W2 H 1.0719 0.1077 0.5970 0.070 Uiso 1 1 d R . .
O1 O 0.6232(10) -0.0185(8) 0.3704(9) 0.122(5) Uani 1 1 d . . .
O2W O 0.8568(7) 0.3244(6) 0.4301(6) 0.050(2) Uani 1 1 d . . .
H2W1 H 0.7981 0.3547 0.3922 0.075 Uiso 1 1 d R . .
H2W2 H 0.8274 0.3206 0.4886 0.075 Uiso 1 1 d R . .
O2 O 0.7374(13) -0.0246(7) 0.2178(8) 0.115(5) Uani 1 1 d . . .
O3 O 0.8463(8) 0.0396(6) 0.3189(6) 0.058(2) Uani 1 1 d . . .
O3W O -0.0222(12) 0.5337(10) 0.3308(15) 0.246(12) Uani 1 1 d . . .
H3W1 H -0.0572 0.4769 0.3594 0.369 Uiso 1 1 d R . .
H3W2 H -0.0649 0.5748 0.3540 0.369 Uiso 1 1 d R . .
O4 O 0.4707(8) 0.4760(5) 0.2159(5) 0.0448(19) Uani 1 1 d . . .
O4W O 0.1405(12) 0.3561(7) 0.3301(8) 0.113(4) Uani 1 1 d . . .
H4W1 H 0.1470 0.3060 0.3111 0.170 Uiso 1 1 d R . .
H4W2 H 0.1596 0.3376 0.3893 0.170 Uiso 1 1 d R . .
O5 O 0.6641(7) 0.4237(6) 0.3052(5) 0.048(2) Uani 1 1 d . . .
O5W O 0.7098(14) -0.2187(10) 0.2388(12) 0.180(8) Uani 1 1 d G . .
H5W1 H 0.6412 -0.2314 0.2813 0.271 Uiso 1 1 d R . .
H5W2 H 0.7351 -0.1597 0.2273 0.271 Uiso 1 1 d R . .
O6 O 0.4490(7) 0.3486(5) 0.3727(5) 0.0417(18) Uani 1 1 d . . .
O6W O 0.2211(10) 0.2613(9) 0.5600(10) 0.122(5) Uani 1 1 d . . .
H6W1 H 0.2555 0.2349 0.6139 0.184 Uiso 1 1 d R . .
H6W2 H 0.1719 0.3096 0.5651 0.184 Uiso 1 1 d R . .
O7 O 0.6559(6) 0.1943(5) 0.3708(4) 0.0336(16) Uani 1 1 d . . .
O7W O 0.7762(18) 0.6219(16) 0.2183(16) 0.244(10) Uani 1 1 d G . .
H7W1 H 0.7554 0.6183 0.2778 0.365 Uiso 1 1 d R . .
H7W2 H 0.7233 0.5859 0.2032 0.365 Uiso 1 1 d R . .
O8 O 0.6536(7) -0.1181(7) 0.6148(6) 0.060(2) Uani 1 1 d . . .
O9 O 0.8328(9) -0.1838(6) 0.7138(6) 0.063(2) Uani 1 1 d . . .
O10 O 0.8730(6) -0.0435(5) 0.5691(5) 0.0386(17) Uani 1 1 d . . .
O11 O 0.7616(8) 0.3116(6) 0.6202(5) 0.050(2) Uani 1 1 d . . .
O12 O 0.5840(8) 0.3090(5) 0.7456(5) 0.0469(19) Uani 1 1 d . . .
O13 O 0.5318(8) 0.2832(6) 0.5998(6) 0.053(2) Uani 1 1 d . . .
O14 O 0.6883(6) 0.1178(5) 0.5700(4) 0.0295(15) Uani 1 1 d . . .
N1 N 0.1874(9) 0.5245(8) 0.1147(8) 0.052(3) Uani 1 1 d . . .
N2 N 0.1096(9) 0.6907(8) 0.1628(8) 0.054(3) Uani 1 1 d . . .
C1 C 0.6501(9) 0.1429(7) 0.2305(7) 0.028(2) Uani 1 1 d . . .
C2 C 0.6212(9) 0.1662(7) 0.1325(7) 0.030(2) Uani 1 1 d . . .
H2A H 0.6372 0.1200 0.1003 0.055 Uiso 1 1 calc R . .
C3 C 0.5692(9) 0.2581(7) 0.0851(6) 0.030(2) Uani 1 1 d . . .
C4 C 0.5458(9) 0.3282(7) 0.1292(6) 0.027(2) Uani 1 1 d . . .
H4A H 0.5119 0.3903 0.0951 0.052 Uiso 1 1 calc R . .
C5 C 0.5735(8) 0.3053(6) 0.2257(6) 0.0235(19) Uani 1 1 d . . .
C6 C 0.6287(8) 0.2127(7) 0.2794(6) 0.026(2) Uani 1 1 d . . .
C7 C 0.7243(8) -0.0180(7) 0.7159(6) 0.0229(19) Uani 1 1 d . . .
C8 C 0.6921(8) 0.0822(7) 0.6673(6) 0.024(2) Uani 1 1 d . . .
C9 C 0.6587(9) 0.1431(7) 0.7245(7) 0.028(2) Uani 1 1 d . . .
C10 C 0.6516(9) 0.1047(7) 0.8261(6) 0.028(2) Uani 1 1 d . . .
H10A H 0.6266 0.1454 0.8633 0.054 Uiso 1 1 calc R . .
C11 C 0.6814(10) 0.0062(8) 0.8722(6) 0.033(2) Uani 1 1 d . . .
C12 C 0.7184(9) -0.0566(7) 0.8197(7) 0.029(2) Uani 1 1 d . . .
H12A H 0.7389 -0.1228 0.8517 0.055 Uiso 1 1 calc R . .
C13 C 0.2244(12) 0.4476(12) 0.0910(11) 0.067(4) Uani 1 1 d . . .
H13A H 0.2598 0.3937 0.1384 0.090 Uiso 1 1 calc R . .
C14 C 0.2145(14) 0.4405(17) -0.0020(14) 0.096(6) Uani 1 1 d . . .
H14A H 0.2395 0.3824 -0.0145 0.125 Uiso 1 1 calc R . .
C15 C 0.1688(16) 0.5183(18) -0.0723(14) 0.094(6) Uani 1 1 d . . .
H15A H 0.1652 0.5158 -0.1351 0.122 Uiso 1 1 calc R . .
C16 C 0.1271(13) 0.6022(17) -0.0511(12) 0.088(6) Uani 1 1 d . . .
C17 C 0.1394(12) 0.6053(13) 0.0448(9) 0.064(4) Uani 1 1 d . . .
C18 C 0.0731(17) 0.6881(18) -0.1214(12) 0.102(7) Uani 1 1 d . . .
H18A H 0.0620 0.6871 -0.1838 0.132 Uiso 1 1 calc R . .
C19 C 0.0389(17) 0.7689(17) -0.0987(16) 0.110(8) Uani 1 1 d . . .
H19A H 0.0091 0.8238 -0.1480 0.142 Uiso 1 1 calc R . .
C20 C 0.0448(14) 0.7777(15) -0.0003(13) 0.092(6) Uani 1 1 d . . .
C21 C 0.0999(11) 0.6899(11) 0.0713(11) 0.063(4) Uani 1 1 d . . .
C22 C 0.0044(17) 0.8573(13) 0.0303(17) 0.106(8) Uani 1 1 d . . .
H22A H -0.0283 0.9148 -0.0140 0.138 Uiso 1 1 calc R . .
C23 C 0.0127(15) 0.8512(11) 0.1257(16) 0.096(6) Uani 1 1 d . . .
H23A H -0.0204 0.9022 0.1481 0.126 Uiso 1 1 calc R . .
C24 C 0.0701(13) 0.7694(10) 0.1872(12) 0.071(4) Uani 1 1 d . . .
H24A H 0.0825 0.7686 0.2499 0.105 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 O14 2.349(6) . ?
Pb1 O7 2.500(6) . ?
Pb1 O10 2.523(7) . ?
Pb1 O3 2.646(8) . ?
Pb1 O1W 2.677(7) . ?
Pb1 O2W 2.708(8) . ?
Pb2 O7 2.411(6) . ?
Pb2 O14 2.463(6) . ?
Pb2 O1 2.532(9) 2_656 ?
Pb2 O8 2.552(7) 2_656 ?
Pb2 O6 2.578(7) . ?
Pb2 O13 2.591(7) . ?
Pb3 N1 2.498(10) . ?
Pb3 O3W 2.509(11) . ?
Pb3 N2 2.545(10) . ?
Pb3 O4W 2.645(9) . ?
Pb3 O4 2.727(7) . ?
Cl1 C3 1.749(9) . ?
Cl2 C11 1.750(9) . ?
S1 O1 1.409(9) . ?
S1 O2 1.431(9) . ?
S1 O3 1.445(8) . ?
S1 C1 1.759(10) . ?
S2 O5 1.434(7) . ?
S2 O4 1.437(7) . ?
S2 O6 1.456(7) . ?
S2 C5 1.773(9) . ?
S3 O8 1.418(7) . ?
S3 O9 1.436(8) . ?
S3 O10 1.462(7) . ?
S3 C7 1.754(9) . ?
S4 O13 1.439(7) . ?
S4 O12 1.440(7) . ?
S4 O11 1.452(7) . ?
S4 C9 1.763(10) . ?
O1W H1W1 0.8535 . ?
O1W H1W2 0.8539 . ?
O1 Pb2 2.532(9) 2_656 ?
O2W H2W1 0.8500 . ?
O2W H2W2 0.8499 . ?
O3W H3W1 0.8500 . ?
O3W H3W2 0.8499 . ?
O4W H4W1 0.8500 . ?
O4W H4W2 0.8501 . ?
O5W H5W1 0.8501 . ?
O5W H5W2 0.8501 . ?
O6W H6W1 0.8500 . ?
O6W H6W2 0.8500 . ?
O7 C6 1.320(10) . ?
O7W H7W1 0.8503 . ?
O7W H7W2 0.8501 . ?
O8 Pb2 2.552(7) 2_656 ?
O14 C8 1.334(10) . ?
N1 C13 1.289(16) . ?
N1 C17 1.365(17) . ?
N2 C24 1.325(16) . ?
N2 C21 1.348(17) . ?
C1 C2 1.408(12) . ?
C1 C6 1.408(12) . ?
C2 C3 1.373(13) . ?
C2 H2A 0.9300 . ?
C3 C4 1.363(13) . ?
C4 C5 1.385(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.415(12) . ?
C7 C8 1.410(12) . ?
C7 C12 1.413(12) . ?
C8 C9 1.402(12) . ?
C9 C10 1.384(12) . ?
C10 C11 1.378(13) . ?
C10 H10A 0.9300 . ?
C11 C12 1.379(13) . ?
C12 H12A 0.9300 . ?
C13 C14 1.40(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.33(3) . ?
C14 H14A 0.9300 . ?
C15 C16 1.37(2) . ?
C15 H15A 0.9300 . ?
C16 C17 1.43(2) . ?
C16 C18 1.43(2) . ?
C17 C21 1.42(2) . ?
C18 C19 1.33(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.49(3) . ?
C19 H19A 0.9300 . ?
C20 C22 1.39(3) . ?
C20 C21 1.47(2) . ?
C22 C23 1.37(2) . ?
C22 H22A 0.9300 . ?
C23 C24 1.359(19) . ?
C23 H23A 0.9300 . ?
C24 H24A 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
O14 Pb1 O7 69.8(2) . . ?
O14 Pb1 O10 72.8(2) . . ?
O7 Pb1 O10 118.8(2) . . ?
O14 Pb1 O3 117.9(2) . . ?
O7 Pb1 O3 73.6(2) . . ?
O10 Pb1 O3 83.9(2) . . ?
O14 Pb1 O1W 78.2(2) . . ?
O7 Pb1 O1W 138.8(2) . . ?
O10 Pb1 O1W 73.0(2) . . ?
O3 Pb1 O1W 146.7(2) . . ?
O14 Pb1 O2W 83.2(2) . . ?
O7 Pb1 O2W 75.0(2) . . ?
O10 Pb1 O2W 143.9(2) . . ?
O3 Pb1 O2W 131.8(2) . . ?
O1W Pb1 O2W 76.1(2) . . ?
O7 Pb2 O14 69.44(19) . . ?
O7 Pb2 O1 130.2(3) . 2_656 ?
O14 Pb2 O1 85.1(3) . 2_656 ?
O7 Pb2 O8 82.9(2) . 2_656 ?
O14 Pb2 O8 131.6(2) . 2_656 ?
O1 Pb2 O8 83.7(4) 2_656 2_656 ?
O7 Pb2 O6 72.8(2) . . ?
O14 Pb2 O6 121.1(2) . . ?
O1 Pb2 O6 152.2(3) 2_656 . ?
O8 Pb2 O6 84.5(3) 2_656 . ?
O7 Pb2 O13 106.2(2) . . ?
O14 Pb2 O13 70.2(2) . . ?
O1 Pb2 O13 103.9(4) 2_656 . ?
O8 Pb2 O13 158.0(3) 2_656 . ?
O6 Pb2 O13 79.4(2) . . ?
N1 Pb3 O3W 92.1(6) . . ?
N1 Pb3 N2 66.3(4) . . ?
O3W Pb3 N2 70.8(4) . . ?
N1 Pb3 O4W 78.0(4) . . ?
O3W Pb3 O4W 70.0(4) . . ?
N2 Pb3 O4W 124.9(3) . . ?
N1 Pb3 O4 77.4(3) . . ?
O3W Pb3 O4 157.3(4) . . ?
N2 Pb3 O4 121.0(3) . . ?
O4W Pb3 O4 88.0(3) . . ?
O1 S1 O2 115.4(8) . . ?
O1 S1 O3 111.8(7) . . ?
O2 S1 O3 110.1(6) . . ?
O1 S1 C1 104.4(5) . . ?
O2 S1 C1 107.3(5) . . ?
O3 S1 C1 107.3(5) . . ?
O5 S2 O4 113.3(5) . . ?
O5 S2 O6 112.2(4) . . ?
O4 S2 O6 110.8(4) . . ?
O5 S2 C5 107.7(4) . . ?
O4 S2 C5 106.2(4) . . ?
O6 S2 C5 106.2(4) . . ?
O8 S3 O9 113.1(6) . . ?
O8 S3 O10 113.3(5) . . ?
O9 S3 O10 110.2(5) . . ?
O8 S3 C7 106.3(4) . . ?
O9 S3 C7 107.3(4) . . ?
O10 S3 C7 106.1(4) . . ?
O13 S4 O12 111.9(5) . . ?
O13 S4 O11 113.4(5) . . ?
O12 S4 O11 111.1(5) . . ?
O13 S4 C9 108.0(4) . . ?
O12 S4 C9 106.2(4) . . ?
O11 S4 C9 105.7(4) . . ?
Pb1 O1W H1W1 109.5 . . ?
Pb1 O1W H1W2 109.3 . . ?
H1W1 O1W H1W2 109.3 . . ?
S1 O1 Pb2 148.4(7) . 2_656 ?
Pb1 O2W H2W1 110.5 . . ?
Pb1 O2W H2W2 100.9 . . ?
H2W1 O2W H2W2 108.4 . . ?
S1 O3 Pb1 122.6(5) . . ?
Pb3 O3W H3W1 117.6 . . ?
Pb3 O3W H3W2 124.7 . . ?
H3W1 O3W H3W2 108.5 . . ?
S2 O4 Pb3 119.7(4) . . ?
Pb3 O4W H4W1 140.6 . . ?
Pb3 O4W H4W2 97.6 . . ?
H4W1 O4W H4W2 108.2 . . ?
H5W1 O5W H5W2 109.5 . . ?
S2 O6 Pb2 127.4(4) . . ?
H6W1 O6W H6W2 107.7 . . ?
C6 O7 Pb2 119.6(5) . . ?
C6 O7 Pb1 129.6(5) . . ?
Pb2 O7 Pb1 108.7(2) . . ?
H7W1 O7W H7W2 109.5 . . ?
S3 O8 Pb2 153.2(5) . 2_656 ?
S3 O10 Pb1 130.7(4) . . ?
S4 O13 Pb2 131.4(4) . . ?
C8 O14 Pb1 127.4(5) . . ?
C8 O14 Pb2 120.5(5) . . ?
Pb1 O14 Pb2 112.0(2) . . ?
C13 N1 C17 118.5(13) . . ?
C13 N1 Pb3 122.9(10) . . ?
C17 N1 Pb3 118.1(9) . . ?
C24 N2 C21 120.5(13) . . ?
C24 N2 Pb3 123.6(10) . . ?
C21 N2 Pb3 115.7(9) . . ?
C2 C1 C6 121.0(9) . . ?
C2 C1 S1 118.0(7) . . ?
C6 C1 S1 121.0(7) . . ?
C3 C2 C1 119.0(9) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C4 C3 C2 122.3(9) . . ?
C4 C3 Cl1 118.8(7) . . ?
C2 C3 Cl1 118.8(7) . . ?
C3 C4 C5 118.8(9) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
C4 C5 C6 122.4(8) . . ?
C4 C5 S2 118.6(7) . . ?
C6 C5 S2 119.1(7) . . ?
O7 C6 C1 123.0(8) . . ?
O7 C6 C5 120.6(8) . . ?
C1 C6 C5 116.4(8) . . ?
C8 C7 C12 120.8(8) . . ?
C8 C7 S3 120.5(6) . . ?
C12 C7 S3 118.6(7) . . ?
O14 C8 C9 120.5(8) . . ?
O14 C8 C7 121.4(8) . . ?
C9 C8 C7 118.1(8) . . ?
C10 C9 C8 120.9(9) . . ?
C10 C9 S4 118.8(7) . . ?
C8 C9 S4 120.3(7) . . ?
C11 C10 C9 120.0(9) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 121.7(9) . . ?
C10 C11 Cl2 119.5(8) . . ?
C12 C11 Cl2 118.7(8) . . ?
C11 C12 C7 118.4(9) . . ?
C11 C12 H12A 120.8 . . ?
C7 C12 H12A 120.8 . . ?
N1 C13 C14 123.7(16) . . ?
N1 C13 H13A 118.1 . . ?
C14 C13 H13A 118.1 . . ?
C15 C14 C13 119(2) . . ?
C15 C14 H14A 120.4 . . ?
C13 C14 H14A 120.4 . . ?
C14 C15 C16 119.5(19) . . ?
C14 C15 H15A 120.3 . . ?
C16 C15 H15A 120.3 . . ?
C15 C16 C17 118.9(18) . . ?
C15 C16 C18 123(2) . . ?
C17 C16 C18 118(2) . . ?
N1 C17 C21 118.2(12) . . ?
N1 C17 C16 120.0(16) . . ?
C21 C17 C16 121.8(16) . . ?
C19 C18 C16 121(2) . . ?
C19 C18 H18A 119.5 . . ?
C16 C18 H18A 119.5 . . ?
C18 C19 C20 124.6(19) . . ?
C18 C19 H19A 117.7 . . ?
C20 C19 H19A 117.7 . . ?
C22 C20 C21 118.0(18) . . ?
C22 C20 C19 128.0(18) . . ?
C21 C20 C19 114(2) . . ?
N2 C21 C17 121.0(13) . . ?
N2 C21 C20 118.6(16) . . ?
C17 C21 C20 120.4(17) . . ?
C23 C22 C20 120.0(16) . . ?
C23 C22 H22A 120.0 . . ?
C20 C22 H22A 120.0 . . ?
C24 C23 C22 118.9(18) . . ?
C24 C23 H23A 120.5 . . ?
C22 C23 H23A 120.5 . . ?
N2 C24 C23 123.8(17) . . ?
N2 C24 H24A 118.1 . . ?
C23 C24 H24A 118.1 . . ?

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
O2 S1 O1 Pb2 42.1(18) . . . 2_656 ?
O3 S1 O1 Pb2 -84.8(17) . . . 2_656 ?
C1 S1 O1 Pb2 159.5(14) . . . 2_656 ?
O1 S1 O3 Pb1 -51.3(8) . . . . ?
O2 S1 O3 Pb1 179.1(6) . . . . ?
C1 S1 O3 Pb1 62.6(6) . . . . ?
O14 Pb1 O3 S1 30.4(6) . . . . ?
O7 Pb1 O3 S1 -25.3(5) . . . . ?
O10 Pb1 O3 S1 97.2(6) . . . . ?
O1W Pb1 O3 S1 143.0(4) . . . . ?
O2W Pb1 O3 S1 -76.7(6) . . . . ?
O5 S2 O4 Pb3 -116.6(5) . . . . ?
O6 S2 O4 Pb3 10.5(6) . . . . ?
C5 S2 O4 Pb3 125.4(4) . . . . ?
N1 Pb3 O4 S2 -132.5(5) . . . . ?
O3W Pb3 O4 S2 -68.4(14) . . . . ?
N2 Pb3 O4 S2 175.4(5) . . . . ?
O4W Pb3 O4 S2 -54.4(5) . . . . ?
O5 S2 O6 Pb2 -72.0(6) . . . . ?
O4 S2 O6 Pb2 160.3(5) . . . . ?
C5 S2 O6 Pb2 45.4(6) . . . . ?
O7 Pb2 O6 S2 -2.4(5) . . . . ?
O14 Pb2 O6 S2 49.5(6) . . . . ?
O1 Pb2 O6 S2 -151.8(8) 2_656 . . . ?
O8 Pb2 O6 S2 -86.7(5) 2_656 . . . ?
O13 Pb2 O6 S2 108.4(5) . . . . ?
O14 Pb2 O7 C6 166.9(7) . . . . ?
O1 Pb2 O7 C6 102.7(8) 2_656 . . . ?
O8 Pb2 O7 C6 27.3(7) 2_656 . . . ?
O6 Pb2 O7 C6 -59.1(7) . . . . ?
O13 Pb2 O7 C6 -132.2(6) . . . . ?
O14 Pb2 O7 Pb1 1.9(2) . . . . ?
O1 Pb2 O7 Pb1 -62.3(5) 2_656 . . . ?
O8 Pb2 O7 Pb1 -137.7(3) 2_656 . . . ?
O6 Pb2 O7 Pb1 135.9(3) . . . . ?
O13 Pb2 O7 Pb1 62.8(3) . . . . ?
O14 Pb1 O7 C6 -165.0(8) . . . . ?
O10 Pb1 O7 C6 -109.3(8) . . . . ?
O3 Pb1 O7 C6 -36.1(8) . . . . ?
O1W Pb1 O7 C6 153.7(7) . . . . ?
O2W Pb1 O7 C6 106.8(8) . . . . ?
O14 Pb1 O7 Pb2 -2.0(2) . . . . ?
O10 Pb1 O7 Pb2 53.7(3) . . . . ?
O3 Pb1 O7 Pb2 127.0(3) . . . . ?
O1W Pb1 O7 Pb2 -43.3(5) . . . . ?
O2W Pb1 O7 Pb2 -90.2(3) . . . . ?
O9 S3 O8 Pb2 -82.9(13) . . . 2_656 ?
O10 S3 O8 Pb2 43.4(14) . . . 2_656 ?
C7 S3 O8 Pb2 159.6(12) . . . 2_656 ?
O8 S3 O10 Pb1 67.2(7) . . . . ?
O9 S3 O10 Pb1 -164.9(5) . . . . ?
C7 S3 O10 Pb1 -49.1(6) . . . . ?
O14 Pb1 O10 S3 12.4(5) . . . . ?
O7 Pb1 O10 S3 -41.9(6) . . . . ?
O3 Pb1 O10 S3 -109.3(5) . . . . ?
O1W Pb1 O10 S3 95.0(5) . . . . ?
O2W Pb1 O10 S3 62.9(7) . . . . ?
O12 S4 O13 Pb2 -145.9(5) . . . . ?
O11 S4 O13 Pb2 87.4(7) . . . . ?
C9 S4 O13 Pb2 -29.3(7) . . . . ?
O7 Pb2 O13 S4 -72.6(7) . . . . ?
O14 Pb2 O13 S4 -12.2(6) . . . . ?
O1 Pb2 O13 S4 67.3(7) 2_656 . . . ?
O8 Pb2 O13 S4 175.4(5) 2_656 . . . ?
O6 Pb2 O13 S4 -141.0(7) . . . . ?
O7 Pb1 O14 C8 179.7(8) . . . . ?
O10 Pb1 O14 C8 49.0(7) . . . . ?
O3 Pb1 O14 C8 122.1(7) . . . . ?
O1W Pb1 O14 C8 -26.7(7) . . . . ?
O2W Pb1 O14 C8 -103.8(7) . . . . ?
O7 Pb1 O14 Pb2 2.0(2) . . . . ?
O10 Pb1 O14 Pb2 -128.7(3) . . . . ?
O3 Pb1 O14 Pb2 -55.6(3) . . . . ?
O1W Pb1 O14 Pb2 155.6(3) . . . . ?
O2W Pb1 O14 Pb2 78.5(3) . . . . ?
O7 Pb2 O14 C8 -179.9(7) . . . . ?
O1 Pb2 O14 C8 -43.6(7) 2_656 . . . ?
O8 Pb2 O14 C8 -120.6(6) 2_656 . . . ?
O6 Pb2 O14 C8 126.7(6) . . . . ?
O13 Pb2 O14 C8 63.2(6) . . . . ?
O7 Pb2 O14 Pb1 -2.1(2) . . . . ?
O1 Pb2 O14 Pb1 134.3(4) 2_656 . . . ?
O8 Pb2 O14 Pb1 57.2(4) 2_656 . . . ?
O6 Pb2 O14 Pb1 -55.5(3) . . . . ?
O13 Pb2 O14 Pb1 -119.0(3) . . . . ?
O3W Pb3 N1 C13 -112.7(10) . . . . ?
N2 Pb3 N1 C13 179.3(11) . . . . ?
O4W Pb3 N1 C13 -43.6(10) . . . . ?
O4 Pb3 N1 C13 47.0(10) . . . . ?
O3W Pb3 N1 C17 75.1(8) . . . . ?
N2 Pb3 N1 C17 7.2(8) . . . . ?
O4W Pb3 N1 C17 144.2(9) . . . . ?
O4 Pb3 N1 C17 -125.2(8) . . . . ?
N1 Pb3 N2 C24 178.7(11) . . . . ?
O3W Pb3 N2 C24 77.4(11) . . . . ?
O4W Pb3 N2 C24 124.3(10) . . . . ?
O4 Pb3 N2 C24 -124.1(10) . . . . ?
N1 Pb3 N2 C21 -6.9(7) . . . . ?
O3W Pb3 N2 C21 -108.1(9) . . . . ?
O4W Pb3 N2 C21 -61.2(9) . . . . ?
O4 Pb3 N2 C21 50.4(8) . . . . ?
O1 S1 C1 C2 -119.9(9) . . . . ?
O2 S1 C1 C2 3.0(10) . . . . ?
O3 S1 C1 C2 121.4(8) . . . . ?
O1 S1 C1 C6 61.8(10) . . . . ?
O2 S1 C1 C6 -175.3(9) . . . . ?
O3 S1 C1 C6 -57.0(9) . . . . ?
C6 C1 C2 C3 -1.1(14) . . . . ?
S1 C1 C2 C3 -179.5(7) . . . . ?
C1 C2 C3 C4 0.8(15) . . . . ?
C1 C2 C3 Cl1 178.8(7) . . . . ?
C2 C3 C4 C5 -1.1(14) . . . . ?
Cl1 C3 C4 C5 -179.2(7) . . . . ?
C3 C4 C5 C6 1.9(13) . . . . ?
C3 C4 C5 S2 -178.2(7) . . . . ?
O5 S2 C5 C4 -115.5(7) . . . . ?
O4 S2 C5 C4 6.1(8) . . . . ?
O6 S2 C5 C4 124.2(7) . . . . ?
O5 S2 C5 C6 64.5(8) . . . . ?
O4 S2 C5 C6 -173.9(7) . . . . ?
O6 S2 C5 C6 -55.9(8) . . . . ?
Pb2 O7 C6 C1 -109.1(8) . . . . ?
Pb1 O7 C6 C1 52.4(12) . . . . ?
Pb2 O7 C6 C5 69.9(10) . . . . ?
Pb1 O7 C6 C5 -128.7(7) . . . . ?
C2 C1 C6 O7 -179.2(8) . . . . ?
S1 C1 C6 O7 -0.9(13) . . . . ?
C2 C1 C6 C5 1.8(13) . . . . ?
S1 C1 C6 C5 -179.9(6) . . . . ?
C4 C5 C6 O7 178.8(8) . . . . ?
S2 C5 C6 O7 -1.1(12) . . . . ?
C4 C5 C6 C1 -2.2(13) . . . . ?
S2 C5 C6 C1 177.9(6) . . . . ?
O8 S3 C7 C8 -73.9(8) . . . . ?
O9 S3 C7 C8 164.8(7) . . . . ?
O10 S3 C7 C8 47.0(8) . . . . ?
O8 S3 C7 C12 105.9(8) . . . . ?
O9 S3 C7 C12 -15.3(9) . . . . ?
O10 S3 C7 C12 -133.1(7) . . . . ?
Pb1 O14 C8 C9 118.4(8) . . . . ?
Pb2 O14 C8 C9 -64.1(10) . . . . ?
Pb1 O14 C8 C7 -64.0(11) . . . . ?
Pb2 O14 C8 C7 113.5(8) . . . . ?
C12 C7 C8 O14 -175.3(8) . . . . ?
S3 C7 C8 O14 4.6(12) . . . . ?
C12 C7 C8 C9 2.3(13) . . . . ?
S3 C7 C8 C9 -177.8(6) . . . . ?
O14 C8 C9 C10 174.6(8) . . . . ?
C7 C8 C9 C10 -3.1(13) . . . . ?
O14 C8 C9 S4 -7.6(12) . . . . ?
C7 C8 C9 S4 174.8(7) . . . . ?
O13 S4 C9 C10 -129.0(8) . . . . ?
O12 S4 C9 C10 -8.7(9) . . . . ?
O11 S4 C9 C10 109.3(8) . . . . ?
O13 S4 C9 C8 53.1(9) . . . . ?
O12 S4 C9 C8 173.4(7) . . . . ?
O11 S4 C9 C8 -68.5(8) . . . . ?
C8 C9 C10 C11 2.1(14) . . . . ?
S4 C9 C10 C11 -175.8(7) . . . . ?
C9 C10 C11 C12 -0.2(15) . . . . ?
C9 C10 C11 Cl2 178.8(7) . . . . ?
C10 C11 C12 C7 -0.5(14) . . . . ?
Cl2 C11 C12 C7 -179.5(7) . . . . ?
C8 C7 C12 C11 -0.6(13) . . . . ?
S3 C7 C12 C11 179.5(7) . . . . ?
C17 N1 C13 C14 -2.1(19) . . . . ?
Pb3 N1 C13 C14 -174.2(10) . . . . ?
N1 C13 C14 C15 2(2) . . . . ?
C13 C14 C15 C16 -3(2) . . . . ?
C14 C15 C16 C17 3(2) . . . . ?
C14 C15 C16 C18 -178.2(14) . . . . ?
C13 N1 C17 C21 -179.5(11) . . . . ?
Pb3 N1 C17 C21 -7.0(13) . . . . ?
C13 N1 C17 C16 2.0(17) . . . . ?
Pb3 N1 C17 C16 174.6(8) . . . . ?
C15 C16 C17 N1 -2.3(18) . . . . ?
C18 C16 C17 N1 178.5(11) . . . . ?
C15 C16 C17 C21 179.4(12) . . . . ?
C18 C16 C17 C21 0.1(18) . . . . ?
C15 C16 C18 C19 -177.4(17) . . . . ?
C17 C16 C18 C19 2(2) . . . . ?
C16 C18 C19 C20 -4(3) . . . . ?
C18 C19 C20 C22 -176.3(18) . . . . ?
C18 C19 C20 C21 3(2) . . . . ?
C24 N2 C21 C17 -178.8(11) . . . . ?
Pb3 N2 C21 C17 6.5(13) . . . . ?
C24 N2 C21 C20 -0.2(17) . . . . ?
Pb3 N2 C21 C20 -174.8(8) . . . . ?
N1 C17 C21 N2 0.2(17) . . . . ?
C16 C17 C21 N2 178.6(10) . . . . ?
N1 C17 C21 C20 -178.5(10) . . . . ?
C16 C17 C21 C20 -0.1(17) . . . . ?
C22 C20 C21 N2 -0.3(19) . . . . ?
C19 C20 C21 N2 179.8(11) . . . . ?
C22 C20 C21 C17 178.4(13) . . . . ?
C19 C20 C21 C17 -1.4(17) . . . . ?
C21 C20 C22 C23 -2(2) . . . . ?
C19 C20 C22 C23 177.7(15) . . . . ?
C20 C22 C23 C24 5(3) . . . . ?
C21 N2 C24 C23 3(2) . . . . ?
Pb3 N2 C24 C23 177.4(10) . . . . ?
C22 C23 C24 N2 -6(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O6W 0.85 2.27 2.814(13) 121.4 1_655
O1W H1W2 O3 0.85 2.22 2.899(11) 136.0 2_756
O2W H2W1 O5 0.85 1.94 2.794(10) 179.8 .
O2W H2W2 O11 0.85 1.91 2.762(10) 179.8 .
O3W H3W1 O2W 0.85 2.24 3.093(15) 177.3 1_455
O4W H4W1 O9 0.85 1.90 2.749(12) 172.2 2_656
O4W H4W2 O6W 0.85 2.48 3.328(18) 172.3 .
O5W H5W1 O13 0.85 2.26 3.101(15) 173.4 2_656
O5W H5W2 O2 0.85 1.90 2.721(17) 162.7 .
O6W H6W1 O5W 0.85 2.14 2.93(2) 155.2 2_656
O6W H6W1 O13 0.85 2.84 3.268(13) 112.8 .
O7W H7W2 O5 0.85 2.36 2.91(2) 123.4 .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.960
_refine_diff_density_min         -1.779
_refine_diff_density_rms         0.224
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 1010476'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H22 Cl2 N4 O8 Pb2 S2, 2(H2 O)'
_chemical_formula_sum            'C36 H26 Cl2 N4 O10 Pb2 S2'
_chemical_formula_weight         1224.01

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'
Cl Cl 0.1484 0.1585 '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                   9.3621(6)
_cell_length_b                   9.7551(5)
_cell_length_c                   10.9477(8)
_cell_angle_alpha                80.577(5)
_cell_angle_beta                 69.059(6)
_cell_angle_gamma                88.515(5)
_cell_volume                     920.61(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2014
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.53

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    9.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2414
_exptl_absorpt_correction_T_max  0.2963
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5466
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.55
_reflns_number_total             4197
_reflns_number_gt                3573
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0109P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4197
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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 0.44109(3) 1.06872(2) 0.34842(2) 0.03124(8) Uani 1 1 d . . .
Cl1 Cl 0.2174(2) 0.37774(19) 0.38979(19) 0.0574(5) Uani 1 1 d . . .
S1 S 0.19952(18) 0.82544(17) 0.62927(15) 0.0349(4) Uani 1 1 d . . .
O1W O 0.0947(14) 0.5189(10) 0.8841(10) 0.237(6) Uani 1 1 d . . .
H1W1 H 0.0398 0.5566 0.8415 0.355 Uiso 1 1 d R . .
H1W2 H 0.1704 0.5745 0.8672 0.355 Uiso 1 1 d R . .
O1 O 0.2040(5) 0.9629(4) 0.5513(4) 0.0388(11) Uani 1 1 d . . .
O2 O 0.0460(5) 0.7667(5) 0.6943(4) 0.0547(14) Uani 1 1 d . . .
O3 O 0.2806(5) 0.8251(5) 0.7216(4) 0.0458(12) Uani 1 1 d . . .
O4 O 0.5209(4) 0.8713(4) 0.4433(3) 0.0296(9) Uani 1 1 d . . .
N1 N 0.5884(5) 0.9427(5) 0.1463(4) 0.0300(12) Uani 1 1 d . . .
N2 N 0.2764(6) 0.9198(5) 0.2595(4) 0.0317(12) Uani 1 1 d . . .
C1 C 0.4558(7) 0.7514(6) 0.4396(5) 0.0258(13) Uani 1 1 d . . .
C2 C 0.5376(7) 0.6594(6) 0.3565(5) 0.0285(13) Uani 1 1 d . . .
H2A H 0.6417 0.6768 0.3091 0.034 Uiso 1 1 calc R . .
C3 C 0.4667(7) 0.5424(6) 0.3431(5) 0.0322(14) Uani 1 1 d . . .
H3A H 0.5224 0.4818 0.2877 0.039 Uiso 1 1 calc R . .
C4 C 0.3125(7) 0.5177(6) 0.4132(6) 0.0330(14) Uani 1 1 d . . .
C5 C 0.2287(7) 0.6008(6) 0.5027(5) 0.0338(14) Uani 1 1 d . . .
H5A H 0.1258 0.5802 0.5524 0.041 Uiso 1 1 calc R . .
C6 C 0.3025(7) 0.7163(6) 0.5165(5) 0.0276(13) Uani 1 1 d . . .
C7 C 0.7408(7) 0.9491(7) 0.0941(6) 0.0374(15) Uani 1 1 d . . .
H7A H 0.7938 1.0078 0.1233 0.045 Uiso 1 1 calc R . .
C8 C 0.8245(8) 0.8710(7) -0.0033(6) 0.0453(17) Uani 1 1 d . . .
H8A H 0.9309 0.8771 -0.0366 0.054 Uiso 1 1 calc R . .
C9 C 0.7496(8) 0.7874(7) -0.0478(6) 0.0454(18) Uani 1 1 d . . .
H9A H 0.8038 0.7368 -0.1138 0.055 Uiso 1 1 calc R . .
C10 C 0.5890(7) 0.7764(6) 0.0056(5) 0.0333(14) Uani 1 1 d . . .
C11 C 0.5130(7) 0.8561(6) 0.1033(5) 0.0260(13) Uani 1 1 d . . .
C12 C 0.5049(9) 0.6861(7) -0.0369(6) 0.0494(19) Uani 1 1 d . . .
H12A H 0.5559 0.6327 -0.1014 0.059 Uiso 1 1 calc R . .
C13 C 0.3485(9) 0.6793(7) 0.0187(7) 0.0523(19) Uani 1 1 d . . .
H13A H 0.2938 0.6229 -0.0112 0.063 Uiso 1 1 calc R . .
C14 C 0.2670(8) 0.7560(7) 0.1210(6) 0.0383(16) Uani 1 1 d . . .
C15 C 0.3479(7) 0.8440(6) 0.1623(5) 0.0282(13) Uani 1 1 d . . .
C16 C 0.1077(8) 0.7488(8) 0.1798(7) 0.0515(19) Uani 1 1 d . . .
H16A H 0.0508 0.6902 0.1541 0.062 Uiso 1 1 calc R . .
C17 C 0.0358(8) 0.8269(7) 0.2742(6) 0.0464(18) Uani 1 1 d . . .
H17A H -0.0703 0.8239 0.3135 0.056 Uiso 1 1 calc R . .
C18 C 0.1259(7) 0.9116(7) 0.3102(6) 0.0402(16) Uani 1 1 d . . .
H18A H 0.0766 0.9660 0.3743 0.048 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 O4 2.274(4) . ?
Pb1 O4 2.587(3) 2_676 ?
Pb1 O1 2.602(4) . ?
Pb1 O3 2.627(4) 2_676 ?
Pb1 N1 2.632(4) . ?
Pb1 N2 2.663(5) . ?
Cl1 C4 1.750(6) . ?
S1 O2 1.442(4) . ?
S1 O1 1.459(4) . ?
S1 O3 1.465(4) . ?
S1 C6 1.765(6) . ?
O1W H1W1 0.8501 . ?
O1W H1W2 0.8500 . ?
O3 Pb1 2.627(4) 2_676 ?
O4 C1 1.346(6) . ?
O4 Pb1 2.587(3) 2_676 ?
N1 C7 1.333(7) . ?
N1 C11 1.354(7) . ?
N2 C18 1.316(7) . ?
N2 C15 1.360(7) . ?
C1 C2 1.398(7) . ?
C1 C6 1.398(8) . ?
C2 C3 1.388(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.377(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(8) . ?
C5 C6 1.392(7) . ?
C5 H5A 0.9300 . ?
C7 C8 1.403(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.341(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.405(9) . ?
C9 H9A 0.9300 . ?
C10 C11 1.398(7) . ?
C10 C12 1.429(8) . ?
C11 C15 1.446(8) . ?
C12 C13 1.369(9) . ?
C12 H12A 0.9300 . ?
C13 C14 1.425(8) . ?
C13 H13A 0.9300 . ?
C14 C15 1.386(8) . ?
C14 C16 1.395(9) . ?
C16 C17 1.355(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.389(8) . ?
C17 H17A 0.9300 . ?
C18 H18A 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
O4 Pb1 O4 73.99(14) . 2_676 ?
O4 Pb1 O1 74.10(13) . . ?
O4 Pb1 O1 73.35(12) 2_676 . ?
O4 Pb1 O3 87.81(14) . 2_676 ?
O4 Pb1 O3 71.36(12) 2_676 2_676 ?
O1 Pb1 O3 143.61(12) . 2_676 ?
O4 Pb1 N1 76.31(13) . . ?
O4 Pb1 N1 138.39(13) 2_676 . ?
O1 Pb1 N1 124.66(13) . . ?
O3 Pb1 N1 79.06(13) 2_676 . ?
O4 Pb1 N2 90.86(14) . . ?
O4 Pb1 N2 145.41(13) 2_676 . ?
O1 Pb1 N2 72.62(13) . . ?
O3 Pb1 N2 140.31(13) 2_676 . ?
N1 Pb1 N2 62.17(14) . . ?
O2 S1 O1 112.4(3) . . ?
O2 S1 O3 112.3(3) . . ?
O1 S1 O3 112.0(3) . . ?
O2 S1 C6 107.3(3) . . ?
O1 S1 C6 106.6(3) . . ?
O3 S1 C6 105.6(3) . . ?
H1W1 O1W H1W2 107.3 . . ?
S1 O1 Pb1 123.7(2) . . ?
S1 O3 Pb1 123.5(2) . 2_676 ?
C1 O4 Pb1 115.9(3) . . ?
C1 O4 Pb1 124.2(3) . 2_676 ?
Pb1 O4 Pb1 106.01(14) . 2_676 ?
C7 N1 C11 117.9(5) . . ?
C7 N1 Pb1 120.8(4) . . ?
C11 N1 Pb1 120.8(4) . . ?
C18 N2 C15 117.8(5) . . ?
C18 N2 Pb1 122.3(4) . . ?
C15 N2 Pb1 119.9(4) . . ?
O4 C1 C2 121.3(5) . . ?
O4 C1 C6 121.0(5) . . ?
C2 C1 C6 117.6(5) . . ?
C3 C2 C1 121.3(6) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
C4 C3 C2 118.9(5) . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C3 C4 C5 121.9(5) . . ?
C3 C4 Cl1 119.9(5) . . ?
C5 C4 Cl1 118.2(5) . . ?
C4 C5 C6 118.3(6) . . ?
C4 C5 H5A 120.9 . . ?
C6 C5 H5A 120.9 . . ?
C5 C6 C1 121.7(5) . . ?
C5 C6 S1 119.7(5) . . ?
C1 C6 S1 118.6(4) . . ?
N1 C7 C8 122.7(6) . . ?
N1 C7 H7A 118.6 . . ?
C8 C7 H7A 118.6 . . ?
C9 C8 C7 119.3(6) . . ?
C9 C8 H8A 120.3 . . ?
C7 C8 H8A 120.3 . . ?
C8 C9 C10 119.8(6) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
C11 C10 C9 117.8(6) . . ?
C11 C10 C12 120.6(6) . . ?
C9 C10 C12 121.6(6) . . ?
N1 C11 C10 122.4(6) . . ?
N1 C11 C15 118.7(5) . . ?
C10 C11 C15 118.9(5) . . ?
C13 C12 C10 119.2(6) . . ?
C13 C12 H12A 120.4 . . ?
C10 C12 H12A 120.4 . . ?
C12 C13 C14 121.9(6) . . ?
C12 C13 H13A 119.0 . . ?
C14 C13 H13A 119.0 . . ?
C15 C14 C16 118.3(6) . . ?
C15 C14 C13 119.1(6) . . ?
C16 C14 C13 122.6(6) . . ?
N2 C15 C14 121.7(6) . . ?
N2 C15 C11 118.0(5) . . ?
C14 C15 C11 120.3(5) . . ?
C17 C16 C14 120.1(6) . . ?
C17 C16 H16A 119.9 . . ?
C14 C16 H16A 119.9 . . ?
C16 C17 C18 117.8(6) . . ?
C16 C17 H17A 121.1 . . ?
C18 C17 H17A 121.1 . . ?
N2 C18 C17 124.3(6) . . ?
N2 C18 H18A 117.9 . . ?
C17 C18 H18A 117.9 . . ?

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
O2 S1 O1 Pb1 -154.6(2) . . . . ?
O3 S1 O1 Pb1 77.8(3) . . . . ?
C6 S1 O1 Pb1 -37.3(3) . . . . ?
O4 Pb1 O1 S1 -8.8(2) . . . . ?
O4 Pb1 O1 S1 -86.4(3) 2_676 . . . ?
O3 Pb1 O1 S1 -71.8(3) 2_676 . . . ?
N1 Pb1 O1 S1 51.5(3) . . . . ?
N2 Pb1 O1 S1 87.3(3) . . . . ?
O2 S1 O3 Pb1 -177.3(3) . . . 2_676 ?
O1 S1 O3 Pb1 -49.7(4) . . . 2_676 ?
C6 S1 O3 Pb1 66.0(3) . . . 2_676 ?
O4 Pb1 O4 C1 142.1(4) 2_676 . . . ?
O1 Pb1 O4 C1 65.3(3) . . . . ?
O3 Pb1 O4 C1 -146.6(4) 2_676 . . . ?
N1 Pb1 O4 C1 -67.4(4) . . . . ?
N2 Pb1 O4 C1 -6.3(4) . . . . ?
O4 Pb1 O4 Pb1 0.0 2_676 . . 2_676 ?
O1 Pb1 O4 Pb1 -76.81(14) . . . 2_676 ?
O3 Pb1 O4 Pb1 71.23(14) 2_676 . . 2_676 ?
N1 Pb1 O4 Pb1 150.50(17) . . . 2_676 ?
N2 Pb1 O4 Pb1 -148.46(15) . . . 2_676 ?
O4 Pb1 N1 C7 -79.0(5) . . . . ?
O4 Pb1 N1 C7 -33.6(5) 2_676 . . . ?
O1 Pb1 N1 C7 -138.3(4) . . . . ?
O3 Pb1 N1 C7 11.4(5) 2_676 . . . ?
N2 Pb1 N1 C7 -177.4(5) . . . . ?
O4 Pb1 N1 C11 92.8(4) . . . . ?
O4 Pb1 N1 C11 138.3(4) 2_676 . . . ?
O1 Pb1 N1 C11 33.6(4) . . . . ?
O3 Pb1 N1 C11 -176.8(4) 2_676 . . . ?
N2 Pb1 N1 C11 -5.6(4) . . . . ?
O4 Pb1 N2 C18 108.3(5) . . . . ?
O4 Pb1 N2 C18 45.9(6) 2_676 . . . ?
O1 Pb1 N2 C18 35.2(5) . . . . ?
O3 Pb1 N2 C18 -164.1(4) 2_676 . . . ?
N1 Pb1 N2 C18 -177.7(5) . . . . ?
O4 Pb1 N2 C15 -68.8(4) . . . . ?
O4 Pb1 N2 C15 -131.2(4) 2_676 . . . ?
O1 Pb1 N2 C15 -141.9(4) . . . . ?
O3 Pb1 N2 C15 18.8(5) 2_676 . . . ?
N1 Pb1 N2 C15 5.2(4) . . . . ?
Pb1 O4 C1 C2 107.9(5) . . . . ?
Pb1 O4 C1 C2 -117.6(5) 2_676 . . . ?
Pb1 O4 C1 C6 -70.4(6) . . . . ?
Pb1 O4 C1 C6 64.1(6) 2_676 . . . ?
O4 C1 C2 C3 -173.7(5) . . . . ?
C6 C1 C2 C3 4.6(8) . . . . ?
C1 C2 C3 C4 0.2(9) . . . . ?
C2 C3 C4 C5 -4.2(9) . . . . ?
C2 C3 C4 Cl1 175.7(4) . . . . ?
C3 C4 C5 C6 3.1(9) . . . . ?
Cl1 C4 C5 C6 -176.8(4) . . . . ?
C4 C5 C6 C1 2.1(9) . . . . ?
C4 C5 C6 S1 179.8(4) . . . . ?
O4 C1 C6 C5 172.6(5) . . . . ?
C2 C1 C6 C5 -5.8(8) . . . . ?
O4 C1 C6 S1 -5.2(8) . . . . ?
C2 C1 C6 S1 176.4(4) . . . . ?
O2 S1 C6 C5 1.8(6) . . . . ?
O1 S1 C6 C5 -118.8(5) . . . . ?
O3 S1 C6 C5 121.8(5) . . . . ?
O2 S1 C6 C1 179.6(5) . . . . ?
O1 S1 C6 C1 59.0(5) . . . . ?
O3 S1 C6 C1 -60.3(5) . . . . ?
C11 N1 C7 C8 0.4(9) . . . . ?
Pb1 N1 C7 C8 172.5(5) . . . . ?
N1 C7 C8 C9 0.9(10) . . . . ?
C7 C8 C9 C10 -1.6(10) . . . . ?
C8 C9 C10 C11 0.9(10) . . . . ?
C8 C9 C10 C12 -178.6(6) . . . . ?
C7 N1 C11 C10 -1.1(8) . . . . ?
Pb1 N1 C11 C10 -173.2(4) . . . . ?
C7 N1 C11 C15 177.8(5) . . . . ?
Pb1 N1 C11 C15 5.8(7) . . . . ?
C9 C10 C11 N1 0.5(9) . . . . ?
C12 C10 C11 N1 180.0(5) . . . . ?
C9 C10 C11 C15 -178.5(5) . . . . ?
C12 C10 C11 C15 1.0(8) . . . . ?
C11 C10 C12 C13 0.5(10) . . . . ?
C9 C10 C12 C13 179.9(7) . . . . ?
C10 C12 C13 C14 -2.2(11) . . . . ?
C12 C13 C14 C15 2.4(11) . . . . ?
C12 C13 C14 C16 -179.2(7) . . . . ?
C18 N2 C15 C14 -2.8(9) . . . . ?
Pb1 N2 C15 C14 174.5(4) . . . . ?
C18 N2 C15 C11 178.1(5) . . . . ?
Pb1 N2 C15 C11 -4.7(7) . . . . ?
C16 C14 C15 N2 1.5(9) . . . . ?
C13 C14 C15 N2 -180.0(6) . . . . ?
C16 C14 C15 C11 -179.4(6) . . . . ?
C13 C14 C15 C11 -0.8(9) . . . . ?
N1 C11 C15 N2 -0.6(8) . . . . ?
C10 C11 C15 N2 178.4(5) . . . . ?
N1 C11 C15 C14 -179.8(5) . . . . ?
C10 C11 C15 C14 -0.8(9) . . . . ?
C15 C14 C16 C17 0.3(11) . . . . ?
C13 C14 C16 C17 -178.2(7) . . . . ?
C14 C16 C17 C18 -0.7(11) . . . . ?
C15 N2 C18 C17 2.4(10) . . . . ?
Pb1 N2 C18 C17 -174.8(5) . . . . ?
C16 C17 C18 N2 -0.7(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O2 0.85 2.38 3.057(11) 137.1 .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.252
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.165
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex8
_database_code_depnum_ccdc_archive 'CCDC 1010481'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H13 Cl N2 O8 Pb S2, H2 O'
_chemical_formula_sum            'C16 H15 Cl N2 O9 Pb S2'
_chemical_formula_weight         686.06

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'
Cl Cl 0.1484 0.1585 '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           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                   8.5537(10)
_cell_length_b                   9.2608(15)
_cell_length_c                   13.8202(14)
_cell_angle_alpha                99.041(11)
_cell_angle_beta                 102.300(9)
_cell_angle_gamma                108.323(12)
_cell_volume                     985.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1841
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      27.54

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    8.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2547
_exptl_absorpt_correction_T_max  0.2952
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6434
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4493
_reflns_number_gt                3670
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0514P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4493
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1197
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.82952(4) -0.09824(4) 0.57172(3) 0.03659(14) Uani 1 1 d . . .
Cl1 Cl 0.4048(3) 0.1274(4) 0.09747(18) 0.0515(7) Uani 1 1 d . . .
S1 S 0.6905(3) 0.2219(3) 0.50067(17) 0.0384(6) Uani 1 1 d . . .
S2 S 0.8195(3) -0.1868(3) 0.21120(18) 0.0376(5) Uani 1 1 d . . .
O1 O 0.8494(10) 0.3568(10) 0.5253(6) 0.061(2) Uani 1 1 d . . .
O1W O 0.8153(11) -0.3524(10) 0.4520(7) 0.072(3) Uani 1 1 d . . .
H1W1 H 0.7508 -0.3830 0.3911 0.086 Uiso 1 1 d R . .
H1W2 H 0.8751 -0.4046 0.4739 0.086 Uiso 1 1 d R . .
O2W O 0.4570(15) -0.5012(13) 0.3448(9) 0.101(4) Uani 1 1 d . . .
H2W1 H 0.3620 -0.5730 0.3387 0.122 Uiso 1 1 d R . .
H2W2 H 0.4411 -0.4528 0.2984 0.122 Uiso 1 1 d R . .
O2 O 0.5409(9) 0.2688(10) 0.4967(5) 0.0514(19) Uani 1 1 d . . .
O3 O 0.6993(9) 0.1171(9) 0.5674(5) 0.0497(19) Uani 1 1 d . . .
O4 O 0.7413(10) -0.3265(9) 0.2421(6) 0.0543(19) Uani 1 1 d . . .
O5 O 0.7870(10) -0.2109(10) 0.1012(5) 0.056(2) Uani 1 1 d . . .
O6 O 1.0040(8) -0.1115(9) 0.2634(5) 0.0469(18) Uani 1 1 d . . .
O7 O 0.8706(7) 0.0036(8) 0.4272(4) 0.0329(14) Uani 1 1 d . . .
H7O H 0.8546 -0.0866 0.3923 0.049 Uiso 1 1 d R . .
N1 N 0.9463(11) -0.2512(11) 0.7253(7) 0.048(2) Uani 1 1 d . . .
N2 N 1.3317(11) -0.4001(11) 1.1887(7) 0.051(2) Uani 1 1 d . . .
C1 C 0.6568(11) 0.1169(11) 0.3741(6) 0.0297(19) Uani 1 1 d . . .
C2 C 0.7538(11) 0.0227(11) 0.3526(7) 0.033(2) Uani 1 1 d . . .
C3 C 0.7209(10) -0.0519(11) 0.2497(6) 0.0299(19) Uani 1 1 d . . .
C4 C 0.6109(11) -0.0217(12) 0.1701(7) 0.035(2) Uani 1 1 d . . .
H4 H 0.5931 -0.0693 0.1022 0.042 Uiso 1 1 calc R . .
C5 C 0.5304(11) 0.0812(12) 0.1961(7) 0.033(2) Uani 1 1 d . . .
C6 C 0.5514(11) 0.1503(12) 0.2966(7) 0.036(2) Uani 1 1 d . . .
H6 H 0.4955 0.2185 0.3121 0.043 Uiso 1 1 calc R . .
C7 C 0.9301(13) -0.1888(15) 0.8142(9) 0.052(3) Uani 1 1 d . . .
H7 H 0.8689 -0.1218 0.8149 0.063 Uiso 1 1 calc R . .
C8 C 1.0010(13) -0.2186(13) 0.9078(9) 0.048(3) Uani 1 1 d . . .
H8 H 0.9814 -0.1762 0.9677 0.057 Uiso 1 1 calc R . .
C9 C 1.1003(12) -0.3120(12) 0.9093(7) 0.039(2) Uani 1 1 d . . .
C10 C 1.1162(13) -0.3760(13) 0.8160(7) 0.044(2) Uani 1 1 d . . .
H10 H 1.1789 -0.4416 0.8128 0.053 Uiso 1 1 calc R . .
C11 C 1.0398(14) -0.3432(13) 0.7277(8) 0.047(3) Uani 1 1 d . . .
H11 H 1.0542 -0.3874 0.6665 0.056 Uiso 1 1 calc R . .
C12 C 1.2423(13) -0.3030(13) 1.1892(8) 0.046(2) Uani 1 1 d . . .
H12 H 1.2319 -0.2554 1.2508 0.056 Uiso 1 1 calc R . .
C13 C 1.1668(13) -0.2738(13) 1.1005(7) 0.046(2) Uani 1 1 d . . .
H13 H 1.1037 -0.2084 1.1026 0.055 Uiso 1 1 calc R . .
C14 C 1.1825(11) -0.3400(11) 1.0069(7) 0.034(2) Uani 1 1 d . . .
C15 C 1.2768(13) -0.4391(13) 1.0079(8) 0.046(3) Uani 1 1 d . . .
H15 H 1.2917 -0.4852 0.9474 0.055 Uiso 1 1 calc R . .
C16 C 1.3475(13) -0.4682(13) 1.0984(8) 0.047(3) Uani 1 1 d . . .
H16 H 1.4076 -0.5361 1.0979 0.056 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 O7 2.385(6) . ?
Pb1 O7 2.432(6) 2_756 ?
Pb1 O6 2.546(7) 2_756 ?
Pb1 O3 2.574(7) . ?
Pb1 O1W 2.608(8) . ?
Cl1 C5 1.744(9) . ?
S1 O3 1.447(7) . ?
S1 O1 1.458(8) . ?
S1 O2 1.469(6) . ?
S1 C1 1.779(9) . ?
S2 O4 1.434(8) . ?
S2 O5 1.454(7) . ?
S2 O6 1.470(7) . ?
S2 C3 1.789(8) . ?
O1W H1W1 0.8500 . ?
O1W H1W2 0.8499 . ?
O2W H2W1 0.8499 . ?
O2W H2W2 0.8500 . ?
O6 Pb1 2.546(7) 2_756 ?
O7 C2 1.349(10) . ?
O7 Pb1 2.432(6) 2_756 ?
O7 H7O 0.8500 . ?
N1 C7 1.327(14) . ?
N1 C11 1.339(13) . ?
N2 C12 1.351(14) . ?
N2 C16 1.361(13) . ?
C1 C6 1.387(11) . ?
C1 C2 1.420(12) . ?
C2 C3 1.406(12) . ?
C3 C4 1.412(11) . ?
C4 C5 1.387(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(12) . ?
C6 H6 0.9300 . ?
C7 C8 1.415(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.389(13) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(14) . ?
C9 C14 1.484(13) . ?
C10 C11 1.383(14) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.368(14) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.399(13) . ?
C15 C16 1.373(13) . ?
C15 H15 0.9300 . ?
C16 H16 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
O7 Pb1 O7 67.7(2) . 2_756 ?
O7 Pb1 O6 110.7(2) . 2_756 ?
O7 Pb1 O6 72.5(2) 2_756 2_756 ?
O7 Pb1 O3 72.1(2) . . ?
O7 Pb1 O3 112.3(2) 2_756 . ?
O6 Pb1 O3 74.1(2) 2_756 . ?
O7 Pb1 O1W 81.5(2) . . ?
O7 Pb1 O1W 83.9(2) 2_756 . ?
O6 Pb1 O1W 145.6(2) 2_756 . ?
O3 Pb1 O1W 139.5(3) . . ?
O3 S1 O1 112.7(5) . . ?
O3 S1 O2 111.8(4) . . ?
O1 S1 O2 112.0(5) . . ?
O3 S1 C1 108.1(4) . . ?
O1 S1 C1 106.8(4) . . ?
O2 S1 C1 105.1(4) . . ?
O4 S2 O5 113.2(5) . . ?
O4 S2 O6 112.4(4) . . ?
O5 S2 O6 111.2(4) . . ?
O4 S2 C3 106.5(4) . . ?
O5 S2 C3 106.3(4) . . ?
O6 S2 C3 106.8(4) . . ?
Pb1 O1W H1W1 120.0 . . ?
Pb1 O1W H1W2 120.0 . . ?
H1W1 O1W H1W2 120.0 . . ?
H2W1 O2W H2W2 107.9 . . ?
S1 O3 Pb1 133.0(4) . . ?
S2 O6 Pb1 132.2(4) . 2_756 ?
C2 O7 Pb1 128.7(5) . . ?
C2 O7 Pb1 118.9(5) . 2_756 ?
Pb1 O7 Pb1 112.3(2) . 2_756 ?
C2 O7 H7O 91.2 . . ?
Pb1 O7 H7O 91.3 . . ?
Pb1 O7 H7O 91.3 2_756 . ?
C7 N1 C11 116.5(9) . . ?
C12 N2 C16 119.1(9) . . ?
C6 C1 C2 121.5(8) . . ?
C6 C1 S1 116.6(7) . . ?
C2 C1 S1 121.2(6) . . ?
O7 C2 C3 121.3(8) . . ?
O7 C2 C1 121.9(8) . . ?
C3 C2 C1 116.8(7) . . ?
C2 C3 C4 121.9(8) . . ?
C2 C3 S2 122.2(6) . . ?
C4 C3 S2 115.9(7) . . ?
C5 C4 C3 118.0(8) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
C6 C5 C4 122.0(8) . . ?
C6 C5 Cl1 120.1(7) . . ?
C4 C5 Cl1 117.9(7) . . ?
C5 C6 C1 119.3(8) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
N1 C7 C8 123.6(10) . . ?
N1 C7 H7 118.2 . . ?
C8 C7 H7 118.2 . . ?
C9 C8 C7 119.2(10) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 116.4(9) . . ?
C10 C9 C14 123.0(9) . . ?
C8 C9 C14 120.5(9) . . ?
C11 C10 C9 120.6(10) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
N1 C11 C10 123.6(10) . . ?
N1 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
N2 C12 C13 120.9(10) . . ?
N2 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 121.3(10) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C15 117.0(9) . . ?
C13 C14 C9 122.5(9) . . ?
C15 C14 C9 120.5(8) . . ?
C16 C15 C14 119.9(10) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
N2 C16 C15 121.7(10) . . ?
N2 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?

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
O1 S1 O3 Pb1 -80.0(7) . . . . ?
O2 S1 O3 Pb1 152.9(5) . . . . ?
C1 S1 O3 Pb1 37.7(7) . . . . ?
O7 Pb1 O3 S1 -2.2(6) . . . . ?
O7 Pb1 O3 S1 53.5(7) 2_756 . . . ?
O6 Pb1 O3 S1 116.4(6) 2_756 . . . ?
O1W Pb1 O3 S1 -54.2(8) . . . . ?
O4 S2 O6 Pb1 -91.0(6) . . . 2_756 ?
O5 S2 O6 Pb1 141.0(5) . . . 2_756 ?
C3 S2 O6 Pb1 25.5(7) . . . 2_756 ?
O7 Pb1 O7 C2 -175.5(9) 2_756 . . . ?
O6 Pb1 O7 C2 -115.7(7) 2_756 . . . ?
O3 Pb1 O7 C2 -51.2(7) . . . . ?
O1W Pb1 O7 C2 97.6(7) . . . . ?
O7 Pb1 O7 Pb1 0.0 2_756 . . 2_756 ?
O6 Pb1 O7 Pb1 59.8(3) 2_756 . . 2_756 ?
O3 Pb1 O7 Pb1 124.2(3) . . . 2_756 ?
O1W Pb1 O7 Pb1 -86.9(3) . . . 2_756 ?
O3 S1 C1 C6 143.6(7) . . . . ?
O1 S1 C1 C6 -95.0(8) . . . . ?
O2 S1 C1 C6 24.1(9) . . . . ?
O3 S1 C1 C2 -46.0(9) . . . . ?
O1 S1 C1 C2 75.5(9) . . . . ?
O2 S1 C1 C2 -165.4(8) . . . . ?
Pb1 O7 C2 C3 -120.7(8) . . . . ?
Pb1 O7 C2 C3 64.1(10) 2_756 . . . ?
Pb1 O7 C2 C1 58.5(12) . . . . ?
Pb1 O7 C2 C1 -116.8(8) 2_756 . . . ?
C6 C1 C2 O7 172.6(9) . . . . ?
S1 C1 C2 O7 2.6(13) . . . . ?
C6 C1 C2 C3 -8.2(14) . . . . ?
S1 C1 C2 C3 -178.2(7) . . . . ?
O7 C2 C3 C4 -174.0(9) . . . . ?
C1 C2 C3 C4 6.8(14) . . . . ?
O7 C2 C3 S2 4.4(13) . . . . ?
C1 C2 C3 S2 -174.8(7) . . . . ?
O4 S2 C3 C2 71.8(9) . . . . ?
O5 S2 C3 C2 -167.3(8) . . . . ?
O6 S2 C3 C2 -48.5(9) . . . . ?
O4 S2 C3 C4 -109.7(8) . . . . ?
O5 S2 C3 C4 11.2(9) . . . . ?
O6 S2 C3 C4 130.0(7) . . . . ?
C2 C3 C4 C5 -2.0(14) . . . . ?
S2 C3 C4 C5 179.5(7) . . . . ?
C3 C4 C5 C6 -1.7(15) . . . . ?
C3 C4 C5 Cl1 176.2(7) . . . . ?
C4 C5 C6 C1 0.3(15) . . . . ?
Cl1 C5 C6 C1 -177.6(7) . . . . ?
C2 C1 C6 C5 4.8(15) . . . . ?
S1 C1 C6 C5 175.2(7) . . . . ?
C11 N1 C7 C8 -2.0(16) . . . . ?
N1 C7 C8 C9 3.2(17) . . . . ?
C7 C8 C9 C10 -2.9(16) . . . . ?
C7 C8 C9 C14 177.4(10) . . . . ?
C8 C9 C10 C11 1.7(16) . . . . ?
C14 C9 C10 C11 -178.6(10) . . . . ?
C7 N1 C11 C10 0.7(16) . . . . ?
C9 C10 C11 N1 -0.6(17) . . . . ?
C16 N2 C12 C13 0.6(16) . . . . ?
N2 C12 C13 C14 -1.5(17) . . . . ?
C12 C13 C14 C15 0.8(15) . . . . ?
C12 C13 C14 C9 179.2(10) . . . . ?
C10 C9 C14 C13 179.4(10) . . . . ?
C8 C9 C14 C13 -0.9(15) . . . . ?
C10 C9 C14 C15 -2.2(15) . . . . ?
C8 C9 C14 C15 177.4(10) . . . . ?
C13 C14 C15 C16 0.6(15) . . . . ?
C9 C14 C15 C16 -177.8(10) . . . . ?
C12 N2 C16 C15 0.9(17) . . . . ?
C14 C15 C16 N2 -1.5(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O4 0.85 2.19 2.899(12) 140.3 .
O1W H1W1 O2W 0.85 2.30 2.873(14) 125.0 .
O1W H1W2 O1 0.85 2.25 2.831(11) 125.3 2_756
O1W H1W2 O1 0.85 2.39 3.097(13) 141.6 1_545
O2W H2W2 N2 0.85 1.82 2.638(15) 159.8 1_454
O7 H7O O6 0.85 2.43 2.944(9) 120.0 .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.217
