# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_l1pb
_database_code_depnum_ccdc_archive 'CCDC 776590'
_audit_update_record             
;
2010-05-10 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
#TrackingRef 'l1pb.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H31 N7 O6.50 Pb S2'
_chemical_formula_weight         924.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.572(3)
_cell_length_b                   16.149(4)
_cell_length_c                   19.077(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.520(5)
_cell_angle_gamma                90.00
_cell_volume                     3808.0(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    996
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      26.1

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    4.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4602
_exptl_absorpt_correction_T_max  0.6566
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G ttingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35682
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_sigmaI/netI    0.1294
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         28.28
_reflns_number_total             9178
_reflns_number_gt                4978
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0231P)²+57.7901P] 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         9178
_refine_ls_number_parameters     483
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.022
_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 0.16803(3) 0.30771(3) 0.189774(19) 0.02823(11) Uani 1 1 d . . .
S1 S -0.2415(2) 0.2038(2) -0.00737(16) 0.0447(7) Uani 1 1 d . . .
S2 S 0.5106(2) 0.38119(19) 0.06406(14) 0.0355(6) Uani 1 1 d . . .
O1 O 0.3435(5) 0.3714(5) 0.1694(3) 0.0350(17) Uani 1 1 d . . .
O2 O 0.0338(5) 0.3575(5) 0.0863(3) 0.0351(17) Uani 1 1 d . . .
O3 O 0.5759(6) 0.4092(5) 0.0145(4) 0.048(2) Uani 1 1 d . . .
O4 O 0.4942(6) 0.2940(5) 0.0692(4) 0.048(2) Uani 1 1 d . . .
O5 O -0.1401(7) 0.1625(5) 0.0089(4) 0.053(2) Uani 1 1 d . . .
O6 O -0.3224(7) 0.1726(5) -0.0633(5) 0.068(3) Uani 1 1 d . . .
N1 N 0.3949(8) 0.4251(7) 0.0419(5) 0.039(2) Uani 1 1 d D . .
N2 N 0.4342(6) 0.2981(6) 0.2662(4) 0.037(2) Uani 1 1 d . . .
N3 N 0.3335(7) 0.2732(6) 0.2759(4) 0.034(2) Uani 1 1 d . . .
N4 N 0.1344(7) 0.2310(6) 0.2943(4) 0.034(2) Uani 1 1 d . . .
N5 N -0.0249(6) 0.2742(5) 0.1899(4) 0.032(2) Uani 1 1 d . . .
N6 N -0.1051(7) 0.2949(6) 0.1326(4) 0.036(2) Uani 1 1 d . . .
N7 N -0.2936(8) 0.2038(7) 0.0639(5) 0.047(3) Uani 1 1 d D . .
C1 C 0.5729(8) 0.4164(7) 0.1496(5) 0.034(2) Uani 1 1 d . . .
C2 C 0.6665(9) 0.4603(8) 0.1530(7) 0.054(4) Uani 1 1 d . . .
H2 H 0.6915 0.4729 0.1112 0.065 Uiso 1 1 calc R . .
C3 C 0.7246(11) 0.4862(11) 0.2178(8) 0.077(5) Uani 1 1 d . . .
H3 H 0.7864 0.5185 0.2201 0.092 Uiso 1 1 calc R . .
C4 C 0.6888(12) 0.4629(10) 0.2794(8) 0.078(5) Uani 1 1 d . . .
H4 H 0.7286 0.4777 0.3236 0.094 Uiso 1 1 calc R . .
C5 C 0.5955(10) 0.4185(9) 0.2757(6) 0.057(4) Uani 1 1 d . . .
H5 H 0.5728 0.4040 0.3178 0.068 Uiso 1 1 calc R . .
C6 C 0.5338(8) 0.3943(7) 0.2115(5) 0.035(3) Uani 1 1 d . . .
C7 C 0.4266(8) 0.3523(7) 0.2135(6) 0.038(3) Uani 1 1 d . . .
C8 C 0.3291(9) 0.2294(8) 0.3315(6) 0.044(3) Uani 1 1 d . . .
C9 C 0.4252(9) 0.2023(12) 0.3831(8) 0.093(6) Uani 1 1 d . . .
H9A H 0.4467 0.1482 0.3701 0.139 Uiso 1 1 calc R . .
H9B H 0.4079 0.2004 0.4300 0.139 Uiso 1 1 calc R . .
H9C H 0.4833 0.2407 0.3825 0.139 Uiso 1 1 calc R . .
C10 C 0.2181(9) 0.2104(7) 0.3438(6) 0.041(3) Uani 1 1 d . . .
C11 C 0.2011(10) 0.1761(8) 0.4091(6) 0.053(4) Uani 1 1 d . . .
H11 H 0.2595 0.1587 0.4431 0.064 Uiso 1 1 calc R . .
C12 C 0.0981(10) 0.1688(9) 0.4214(6) 0.058(4) Uani 1 1 d . . .
H12 H 0.0860 0.1492 0.4651 0.070 Uiso 1 1 calc R . .
C13 C 0.0116(10) 0.1904(9) 0.3691(6) 0.052(3) Uani 1 1 d . . .
H13 H -0.0592 0.1838 0.3762 0.062 Uiso 1 1 calc R . .
C14 C 0.0329(8) 0.2225(7) 0.3052(6) 0.035(3) Uani 1 1 d . . .
C15 C -0.0561(9) 0.2485(7) 0.2466(5) 0.036(3) Uani 1 1 d . . .
C16 C -0.1706(9) 0.2479(10) 0.2582(7) 0.069(4) Uani 1 1 d . . .
H16A H -0.2125 0.2867 0.2265 0.103 Uiso 1 1 calc R . .
H16B H -0.1724 0.2631 0.3066 0.103 Uiso 1 1 calc R . .
H16C H -0.2004 0.1934 0.2490 0.103 Uiso 1 1 calc R . .
C17 C -0.0636(8) 0.3348(6) 0.0840(5) 0.029(2) Uani 1 1 d . . .
C18 C -0.1393(8) 0.3592(6) 0.0159(5) 0.029(2) Uani 1 1 d . . .
C19 C -0.1259(9) 0.4380(8) -0.0082(6) 0.042(3) Uani 1 1 d . . .
H19 H -0.0756 0.4725 0.0193 0.050 Uiso 1 1 calc R . .
C20 C -0.1842(9) 0.4683(7) -0.0718(6) 0.043(3) Uani 1 1 d . . .
H20 H -0.1729 0.5220 -0.0864 0.052 Uiso 1 1 calc R . .
C21 C -0.2580(9) 0.4185(8) -0.1128(6) 0.048(3) Uani 1 1 d . . .
H21 H -0.2971 0.4388 -0.1554 0.058 Uiso 1 1 calc R . .
C22 C -0.2758(8) 0.3390(8) -0.0923(6) 0.042(3) Uani 1 1 d . . .
H22 H -0.3268 0.3056 -0.1203 0.050 Uiso 1 1 calc R . .
C23 C -0.2156(8) 0.3096(7) -0.0286(5) 0.033(2) Uani 1 1 d . . .
C24 C 0.1480(9) 0.4215(6) 0.2466(5) 0.032(2) Uani 1 1 d . . .
C25 C 0.0498(10) 0.4594(8) 0.2389(7) 0.055(4) Uani 1 1 d . . .
H25 H -0.0074 0.4415 0.2042 0.066 Uiso 1 1 calc R . .
C26 C 0.0354(10) 0.5253(9) 0.2834(8) 0.068(4) Uani 1 1 d . . .
H26 H -0.0325 0.5495 0.2793 0.081 Uiso 1 1 calc R . .
C27 C 0.1184(11) 0.5548(9) 0.3324(8) 0.067(4) Uani 1 1 d . . .
H27 H 0.1079 0.5986 0.3621 0.080 Uiso 1 1 calc R . .
C28 C 0.2181(11) 0.5189(9) 0.3373(7) 0.060(4) Uani 1 1 d . . .
H28 H 0.2766 0.5396 0.3696 0.072 Uiso 1 1 calc R . .
C29 C 0.2328(10) 0.4518(8) 0.2944(7) 0.056(4) Uani 1 1 d . . .
H29 H 0.3007 0.4276 0.2983 0.067 Uiso 1 1 calc R . .
C30 C 0.1934(10) 0.2063(8) 0.1210(6) 0.045(3) Uani 1 1 d . . .
C31 C 0.2924(12) 0.1877(10) 0.1077(9) 0.086(5) Uani 1 1 d . . .
H31 H 0.3519 0.2182 0.1297 0.103 Uiso 1 1 calc R . .
C32 C 0.3072(18) 0.1237(12) 0.0617(12) 0.121(8) Uani 1 1 d . . .
H32 H 0.3748 0.1120 0.0508 0.145 Uiso 1 1 calc R . .
C33 C 0.2156(17) 0.0779(12) 0.0326(10) 0.101(6) Uani 1 1 d . . .
H33 H 0.2238 0.0325 0.0041 0.121 Uiso 1 1 calc R . .
C34 C 0.1205(15) 0.0957(11) 0.0435(11) 0.108(7) Uani 1 1 d . . .
H34 H 0.0607 0.0656 0.0211 0.130 Uiso 1 1 calc R . .
C35 C 0.1080(12) 0.1613(9) 0.0899(8) 0.073(5) Uani 1 1 d . . .
H35 H 0.0396 0.1736 0.0992 0.087 Uiso 1 1 calc R . .
H1A H 0.358(11) 0.425(10) 0.078(6) 0.109 Uiso 1 1 d D . .
H1B H 0.405(13) 0.478(3) 0.031(8) 0.109 Uiso 1 1 d D . .
H7A H -0.361(6) 0.225(9) 0.060(9) 0.109 Uiso 1 1 d D . .
H7B H -0.250(11) 0.236(8) 0.095(7) 0.109 Uiso 1 1 d D . .
O1S O 0.573(2) 0.158(2) 0.2383(15) 0.170(16) Uani 0.50 1 d P . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 C30 2.158(11) . ?
Pb1 C24 2.171(10) . ?
Pb1 N4 2.449(8) . ?
Pb1 N3 2.468(8) . ?
Pb1 O2 2.485(7) . ?
Pb1 N5 2.485(8) . ?
Pb1 O1 2.528(7) . ?
S1 O5 1.422(8) . ?
S1 O6 1.425(8) . ?
S1 N7 1.614(11) . ?
S1 C23 1.800(12) . ?
S2 O4 1.429(8) . ?
S2 O3 1.434(8) . ?
S2 N1 1.603(10) . ?
S2 C1 1.771(11) . ?
O1 C7 1.254(12) . ?
O2 C17 1.271(11) . ?
N2 C7 1.322(14) . ?
N2 N3 1.374(11) . ?
N3 C8 1.285(13) . ?
N4 C10 1.322(13) . ?
N4 C14 1.337(13) . ?
N5 C15 1.283(12) . ?
N5 N6 1.387(11) . ?
N6 C17 1.313(12) . ?
C1 C2 1.365(14) . ?
C1 C6 1.404(14) . ?
C2 C3 1.381(18) . ?
C3 C4 1.384(19) . ?
C4 C5 1.366(18) . ?
C5 C6 1.382(15) . ?
C6 C7 1.516(14) . ?
C8 C9 1.478(15) . ?
C8 C10 1.489(15) . ?
C10 C11 1.413(15) . ?
C11 C12 1.364(16) . ?
C12 C13 1.380(16) . ?
C13 C14 1.394(14) . ?
C14 C15 1.491(14) . ?
C15 C16 1.497(15) . ?
C17 C18 1.516(13) . ?
C18 C19 1.373(15) . ?
C18 C23 1.409(14) . ?
C19 C20 1.387(15) . ?
C20 C21 1.361(16) . ?
C21 C22 1.372(16) . ?
C22 C23 1.392(14) . ?
C24 C29 1.361(15) . ?
C24 C25 1.362(16) . ?
C25 C26 1.393(16) . ?
C26 C27 1.354(17) . ?
C27 C28 1.369(18) . ?
C28 C29 1.391(17) . ?
C30 C35 1.342(17) . ?
C30 C31 1.350(17) . ?
C31 C32 1.390(19) . ?
C32 C33 1.40(2) . ?
C33 C34 1.28(2) . ?
C34 C35 1.41(2) . ?

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
C30 Pb1 C24 171.6(4) . . ?
C30 Pb1 N4 100.2(4) . . ?
C24 Pb1 N4 88.2(3) . . ?
C30 Pb1 N3 91.9(4) . . ?
C24 Pb1 N3 91.1(4) . . ?
N4 Pb1 N3 66.0(3) . . ?
C30 Pb1 O2 85.2(4) . . ?
C24 Pb1 O2 89.9(3) . . ?
N4 Pb1 O2 128.1(2) . . ?
N3 Pb1 O2 165.8(2) . . ?
C30 Pb1 N5 95.0(4) . . ?
C24 Pb1 N5 88.9(3) . . ?
N4 Pb1 N5 64.9(3) . . ?
N3 Pb1 N5 130.8(3) . . ?
O2 Pb1 N5 63.3(2) . . ?
C30 Pb1 O1 89.2(4) . . ?
C24 Pb1 O1 85.2(3) . . ?
N4 Pb1 O1 128.1(2) . . ?
N3 Pb1 O1 62.7(3) . . ?
O2 Pb1 O1 103.4(2) . . ?
N5 Pb1 O1 165.5(2) . . ?
O5 S1 O6 119.2(6) . . ?
O5 S1 N7 107.6(5) . . ?
O6 S1 N7 106.6(6) . . ?
O5 S1 C23 107.6(5) . . ?
O6 S1 C23 107.5(5) . . ?
N7 S1 C23 107.9(5) . . ?
O4 S2 O3 117.6(5) . . ?
O4 S2 N1 108.6(5) . . ?
O3 S2 N1 106.7(5) . . ?
O4 S2 C1 107.3(5) . . ?
O3 S2 C1 107.2(5) . . ?
N1 S2 C1 109.2(5) . . ?
C7 O1 Pb1 116.1(7) . . ?
C17 O2 Pb1 116.3(6) . . ?
C7 N2 N3 110.8(8) . . ?
C8 N3 N2 116.9(9) . . ?
C8 N3 Pb1 121.1(7) . . ?
N2 N3 Pb1 122.0(6) . . ?
C10 N4 C14 121.4(9) . . ?
C10 N4 Pb1 118.4(7) . . ?
C14 N4 Pb1 119.4(7) . . ?
C15 N5 N6 116.9(8) . . ?
C15 N5 Pb1 121.3(7) . . ?
N6 N5 Pb1 121.1(6) . . ?
C17 N6 N5 110.4(8) . . ?
C2 C1 C6 121.6(10) . . ?
C2 C1 S2 116.3(8) . . ?
C6 C1 S2 121.9(8) . . ?
C1 C2 C3 120.6(12) . . ?
C2 C3 C4 118.5(13) . . ?
C5 C4 C3 120.5(13) . . ?
C4 C5 C6 122.1(12) . . ?
C5 C6 C1 116.6(10) . . ?
C5 C6 C7 117.5(10) . . ?
C1 C6 C7 125.8(9) . . ?
O1 C7 N2 127.5(10) . . ?
O1 C7 C6 120.5(10) . . ?
N2 C7 C6 112.0(9) . . ?
N3 C8 C9 124.0(11) . . ?
N3 C8 C10 115.3(10) . . ?
C9 C8 C10 120.7(10) . . ?
N4 C10 C11 120.0(10) . . ?
N4 C10 C8 118.8(9) . . ?
C11 C10 C8 121.1(10) . . ?
C12 C11 C10 119.1(10) . . ?
C11 C12 C13 120.1(10) . . ?
C12 C13 C14 118.3(10) . . ?
N4 C14 C13 121.0(10) . . ?
N4 C14 C15 117.4(9) . . ?
C13 C14 C15 121.6(10) . . ?
N5 C15 C14 114.9(9) . . ?
N5 C15 C16 125.3(10) . . ?
C14 C15 C16 119.7(9) . . ?
O2 C17 N6 128.5(9) . . ?
O2 C17 C18 113.8(9) . . ?
N6 C17 C18 117.6(9) . . ?
C19 C18 C23 115.9(10) . . ?
C19 C18 C17 115.6(10) . . ?
C23 C18 C17 128.4(9) . . ?
C18 C19 C20 122.8(11) . . ?
C21 C20 C19 119.3(11) . . ?
C20 C21 C22 121.3(10) . . ?
C21 C22 C23 118.5(11) . . ?
C22 C23 C18 122.3(11) . . ?
C22 C23 S1 115.4(8) . . ?
C18 C23 S1 122.4(8) . . ?
C29 C24 C25 119.6(11) . . ?
C29 C24 Pb1 119.4(9) . . ?
C25 C24 Pb1 120.8(8) . . ?
C24 C25 C26 119.6(11) . . ?
C27 C26 C25 121.4(12) . . ?
C26 C27 C28 118.6(13) . . ?
C27 C28 C29 120.5(12) . . ?
C24 C29 C28 120.2(12) . . ?
C35 C30 C31 119.1(12) . . ?
C35 C30 Pb1 119.0(9) . . ?
C31 C30 Pb1 121.8(10) . . ?
C30 C31 C32 121.3(15) . . ?
C31 C32 C33 116.6(17) . . ?
C34 C33 C32 123.0(17) . . ?
C33 C34 C35 118.9(16) . . ?
C30 C35 C34 120.9(14) . . ?

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
N1 H1A O1 0.90(2) 1.98(9) 2.767(11) 145(14) .
N1 H1B O3 0.90(2) 2.04(4) 2.932(13) 169(15) 3_665
N7 H7A O4 0.90(2) 2.17(4) 3.056(13) 168(15) 1_455
N7 H7A S2 0.90(2) 3.00(10) 3.777(11) 145(13) 1_455
N7 H7B N6 0.90(2) 2.07(8) 2.892(13) 152(15) .

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.206
####################################################################### 
# 
# 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_me2snl
_database_code_depnum_ccdc_archive 'CCDC 776591'
_audit_update_record             
;
2010-05-10 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
#TrackingRef 'me2snl.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H29 N7 O7 S2 Sn'
_chemical_formula_weight         722.36

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   14.5188(4)
_cell_length_b                   7.6162(2)
_cell_length_c                   27.7076(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.505(2)
_cell_angle_gamma                90.00
_cell_volume                     2991.17(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9683
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      26.03

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G ttingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53774
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         26.38
_reflns_number_total             6131
_reflns_number_gt                4888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0142P)²+9.8219P] 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         6131
_refine_ls_number_parameters     407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0780
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_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
Sn1 Sn 0.784250(18) 0.04070(4) 0.829446(9) 0.01109(7) Uani 1 1 d . . .
S1 S 0.44244(7) 0.23332(13) 0.88828(4) 0.0172(2) Uani 1 1 d . . .
S2 S 1.00714(7) -0.37972(14) 0.92768(4) 0.0181(2) Uani 1 1 d . . .
O1 O 0.69289(17) -0.0368(4) 0.88185(9) 0.0169(6) Uani 1 1 d . . .
O2 O 0.90779(17) -0.0219(4) 0.89191(9) 0.0161(6) Uani 1 1 d . . .
O3 O 0.53088(19) 0.3239(4) 0.89276(10) 0.0209(6) Uani 1 1 d . . .
O4 O 0.3725(2) 0.3044(4) 0.91228(11) 0.0262(7) Uani 1 1 d . . .
O5 O 0.98881(19) -0.3777(4) 0.87489(9) 0.0189(6) Uani 1 1 d . . .
O6 O 1.0490(2) -0.5350(4) 0.95317(10) 0.0281(7) Uani 1 1 d . . .
N1 N 0.3943(3) 0.2179(5) 0.83009(12) 0.0197(8) Uani 1 1 d . . .
N2 N 0.5595(2) 0.0195(4) 0.81952(11) 0.0134(7) Uani 1 1 d . . .
N3 N 0.6248(2) 0.0609(4) 0.79140(11) 0.0127(7) Uani 1 1 d . . .
N4 N 0.7621(2) 0.1265(4) 0.74732(11) 0.0160(7) Uani 1 1 d . . .
N5 N 0.9277(2) 0.0879(4) 0.80687(11) 0.0144(7) Uani 1 1 d . . .
N6 N 1.0108(2) 0.0590(4) 0.84198(11) 0.0168(7) Uani 1 1 d . . .
N7 N 0.9090(3) -0.3468(5) 0.94448(14) 0.0213(8) Uani 1 1 d . . .
C1 C 0.4700(3) 0.0174(5) 0.91177(13) 0.0152(8) Uani 1 1 d . . .
C2 C 0.4187(3) -0.0482(6) 0.94475(14) 0.0203(8) Uani 1 1 d . . .
H2 H 0.3688 0.0190 0.9525 0.024 Uiso 1 1 calc R . .
C3 C 0.4403(3) -0.2117(6) 0.96625(14) 0.0213(9) Uani 1 1 d . . .
H3 H 0.4047 -0.2567 0.9885 0.026 Uiso 1 1 calc R . .
C4 C 0.5131(3) -0.3089(6) 0.95545(14) 0.0209(9) Uani 1 1 d . . .
H4 H 0.5279 -0.4207 0.9703 0.025 Uiso 1 1 calc R . .
C5 C 0.5652(3) -0.2428(5) 0.92266(14) 0.0168(8) Uani 1 1 d . . .
H5 H 0.6160 -0.3099 0.9157 0.020 Uiso 1 1 calc R . .
C6 C 0.5442(3) -0.0805(5) 0.89997(13) 0.0134(8) Uani 1 1 d . . .
C7 C 0.6041(2) -0.0236(5) 0.86513(13) 0.0129(8) Uani 1 1 d . . .
C8 C 0.5972(3) 0.0912(5) 0.74451(13) 0.0130(8) Uani 1 1 d . . .
C9 C 0.4964(3) 0.0846(5) 0.71682(14) 0.0172(9) Uani 1 1 d . . .
H9A H 0.4587 0.0209 0.7365 0.026 Uiso 1 1 calc R . .
H9B H 0.4926 0.0242 0.6852 0.026 Uiso 1 1 calc R . .
H9C H 0.4720 0.2044 0.7107 0.026 Uiso 1 1 calc R . .
C10 C 0.6744(3) 0.1352(5) 0.71913(14) 0.0159(8) Uani 1 1 d . . .
C11 C 0.6604(3) 0.1756(6) 0.66921(15) 0.0214(9) Uani 1 1 d . . .
H11 H 0.5984 0.1812 0.6492 0.026 Uiso 1 1 calc R . .
C12 C 0.7378(3) 0.2077(7) 0.64892(16) 0.0303(11) Uani 1 1 d . . .
H12 H 0.7293 0.2355 0.6148 0.036 Uiso 1 1 calc R . .
C13 C 0.8278(3) 0.1991(6) 0.67852(15) 0.0255(10) Uani 1 1 d . . .
H13 H 0.8815 0.2223 0.6651 0.031 Uiso 1 1 calc R . .
C14 C 0.8383(3) 0.1558(5) 0.72823(14) 0.0179(9) Uani 1 1 d . . .
C15 C 0.9317(3) 0.1332(5) 0.76239(14) 0.0185(9) Uani 1 1 d . . .
C16 C 1.0211(3) 0.1548(8) 0.74436(16) 0.0377(13) Uani 1 1 d . . .
H16A H 1.0689 0.2110 0.7701 0.057 Uiso 1 1 calc R . .
H16B H 1.0090 0.2283 0.7146 0.057 Uiso 1 1 calc R . .
H16C H 1.0439 0.0394 0.7365 0.057 Uiso 1 1 calc R . .
C17 C 0.9895(3) 0.0008(4) 0.88330(14) 0.0139(8) Uani 1 1 d . . .
C18 C 1.0721(3) -0.0377(6) 0.92522(13) 0.0177(8) Uani 1 1 d . . .
C19 C 1.1352(3) 0.0959(6) 0.94323(15) 0.0193(9) Uani 1 1 d . . .
H19 H 1.1292 0.2064 0.9269 0.023 Uiso 1 1 calc R . .
C20 C 1.2076(3) 0.0697(6) 0.98521(15) 0.0255(11) Uani 1 1 d . . .
H20 H 1.2494 0.1630 0.9977 0.031 Uiso 1 1 calc R . .
C21 C 1.2179(3) -0.0926(6) 1.00831(15) 0.0274(11) Uani 1 1 d . . .
H21 H 1.2671 -0.1105 1.0367 0.033 Uiso 1 1 calc R . .
C22 C 1.1573(3) -0.2283(6) 0.99042(15) 0.0250(10) Uani 1 1 d . . .
H22 H 1.1652 -0.3398 1.0061 0.030 Uiso 1 1 calc R . .
C23 C 1.0842(3) -0.2016(6) 0.94923(14) 0.0177(9) Uani 1 1 d . . .
C24 C 0.7794(3) -0.2265(5) 0.80588(14) 0.0155(8) Uani 1 1 d . . .
H24A H 0.8347 -0.2891 0.8246 0.023 Uiso 1 1 calc R . .
H24B H 0.7793 -0.2311 0.7705 0.023 Uiso 1 1 calc R . .
H24C H 0.7218 -0.2819 0.8117 0.023 Uiso 1 1 calc R . .
C25 C 0.7835(3) 0.3018(5) 0.85587(15) 0.0216(9) Uani 1 1 d . . .
H25A H 0.7199 0.3317 0.8599 0.032 Uiso 1 1 calc R . .
H25B H 0.8020 0.3825 0.8321 0.032 Uiso 1 1 calc R . .
H25C H 0.8281 0.3119 0.8878 0.032 Uiso 1 1 calc R . .
H1A H 0.429(3) 0.157(6) 0.8132(16) 0.027(13) Uiso 1 1 d . . .
H1B H 0.329(4) 0.176(6) 0.8254(17) 0.038(14) Uiso 1 1 d . . .
H7A H 0.882(4) -0.248(9) 0.935(2) 0.07(2) Uiso 1 1 d . . .
H7B H 0.916(3) -0.358(6) 0.9747(17) 0.020(12) Uiso 1 1 d . . .
O1S O 0.2004(3) 0.1958(7) 0.83797(15) 0.0501(12) Uani 1 1 d . . .
H1S H 0.225(5) 0.223(9) 0.860(2) 0.06(2) Uiso 1 1 d . . .
H2S H 0.137(4) 0.164(7) 0.8402(19) 0.050(16) Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C25 2.120(4) . ?
Sn1 C24 2.133(4) . ?
Sn1 O1 2.247(3) . ?
Sn1 O2 2.257(2) . ?
Sn1 N4 2.322(3) . ?
Sn1 N5 2.328(3) . ?
Sn1 N3 2.332(3) . ?
S1 O4 1.435(3) . ?
S1 O3 1.439(3) . ?
S1 N1 1.617(3) . ?
S1 C1 1.782(4) . ?
S2 O5 1.429(3) . ?
S2 O6 1.442(3) . ?
S2 N7 1.612(4) . ?
S2 C23 1.777(4) . ?
O1 C7 1.275(4) . ?
O2 C17 1.272(4) . ?
N2 C7 1.330(5) . ?
N2 N3 1.387(4) . ?
N3 C8 1.295(5) . ?
N4 C14 1.344(5) . ?
N4 C10 1.344(5) . ?
N5 C15 1.294(5) . ?
N5 N6 1.394(4) . ?
N6 C17 1.325(5) . ?
C1 C2 1.391(5) . ?
C1 C6 1.405(5) . ?
C2 C3 1.387(6) . ?
C3 C4 1.375(6) . ?
C4 C5 1.396(6) . ?
C5 C6 1.390(5) . ?
C6 C7 1.497(5) . ?
C8 C10 1.484(5) . ?
C8 C9 1.499(5) . ?
C10 C11 1.389(5) . ?
C11 C12 1.382(6) . ?
C12 C13 1.386(6) . ?
C13 C14 1.392(5) . ?
C14 C15 1.487(5) . ?
C15 C16 1.497(6) . ?
C17 C18 1.507(5) . ?
C18 C19 1.388(6) . ?
C18 C23 1.408(6) . ?
C19 C20 1.403(6) . ?
C20 C21 1.385(6) . ?
C21 C22 1.379(6) . ?
C22 C23 1.394(5) . ?

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
C25 Sn1 C24 176.40(16) . . ?
C25 Sn1 O1 88.57(14) . . ?
C24 Sn1 O1 87.83(13) . . ?
C25 Sn1 O2 89.77(13) . . ?
C24 Sn1 O2 90.09(12) . . ?
O1 Sn1 O2 86.06(9) . . ?
C25 Sn1 N4 93.70(14) . . ?
C24 Sn1 N4 88.86(13) . . ?
O1 Sn1 N4 136.99(10) . . ?
O2 Sn1 N4 136.83(10) . . ?
C25 Sn1 N5 91.14(14) . . ?
C24 Sn1 N5 92.15(13) . . ?
O1 Sn1 N5 154.35(10) . . ?
O2 Sn1 N5 68.29(10) . . ?
N4 Sn1 N5 68.62(11) . . ?
C25 Sn1 N3 90.87(14) . . ?
C24 Sn1 N3 87.73(13) . . ?
O1 Sn1 N3 69.04(9) . . ?
O2 Sn1 N3 155.07(10) . . ?
N4 Sn1 N3 67.98(11) . . ?
N5 Sn1 N3 136.60(10) . . ?
O4 S1 O3 119.16(18) . . ?
O4 S1 N1 107.02(19) . . ?
O3 S1 N1 107.83(18) . . ?
O4 S1 C1 107.73(18) . . ?
O3 S1 C1 106.55(17) . . ?
N1 S1 C1 108.15(18) . . ?
O5 S2 O6 118.37(17) . . ?
O5 S2 N7 108.28(19) . . ?
O6 S2 N7 107.0(2) . . ?
O5 S2 C23 107.45(18) . . ?
O6 S2 C23 107.03(19) . . ?
N7 S2 C23 108.42(19) . . ?
C7 O1 Sn1 115.8(2) . . ?
C17 O2 Sn1 116.5(2) . . ?
C7 N2 N3 109.8(3) . . ?
C8 N3 N2 120.2(3) . . ?
C8 N3 Sn1 121.8(2) . . ?
N2 N3 Sn1 117.6(2) . . ?
C14 N4 C10 121.4(3) . . ?
C14 N4 Sn1 118.8(2) . . ?
C10 N4 Sn1 119.7(3) . . ?
C15 N5 N6 119.7(3) . . ?
C15 N5 Sn1 121.7(3) . . ?
N6 N5 Sn1 118.5(2) . . ?
C17 N6 N5 109.1(3) . . ?
C2 C1 C6 120.6(4) . . ?
C2 C1 S1 117.5(3) . . ?
C6 C1 S1 121.9(3) . . ?
C3 C2 C1 120.1(4) . . ?
C4 C3 C2 120.2(4) . . ?
C3 C4 C5 119.9(4) . . ?
C6 C5 C4 121.2(4) . . ?
C5 C6 C1 118.1(4) . . ?
C5 C6 C7 116.6(3) . . ?
C1 C6 C7 125.3(3) . . ?
O1 C7 N2 127.6(3) . . ?
O1 C7 C6 115.2(3) . . ?
N2 C7 C6 116.9(3) . . ?
N3 C8 C10 114.5(3) . . ?
N3 C8 C9 124.3(3) . . ?
C10 C8 C9 121.2(3) . . ?
N4 C10 C11 120.3(4) . . ?
N4 C10 C8 115.5(3) . . ?
C11 C10 C8 124.1(3) . . ?
C12 C11 C10 119.2(4) . . ?
C11 C12 C13 119.7(4) . . ?
C12 C13 C14 118.9(4) . . ?
N4 C14 C13 120.4(4) . . ?
N4 C14 C15 116.5(3) . . ?
C13 C14 C15 123.1(4) . . ?
N5 C15 C14 114.4(3) . . ?
N5 C15 C16 124.7(4) . . ?
C14 C15 C16 120.8(3) . . ?
O2 C17 N6 127.5(3) . . ?
O2 C17 C18 116.6(3) . . ?
N6 C17 C18 115.8(3) . . ?
C19 C18 C23 118.4(3) . . ?
C19 C18 C17 119.2(4) . . ?
C23 C18 C17 122.3(3) . . ?
C18 C19 C20 120.8(4) . . ?
C21 C20 C19 119.8(4) . . ?
C22 C21 C20 120.4(4) . . ?
C21 C22 C23 119.9(4) . . ?
C22 C23 C18 120.7(4) . . ?
C22 C23 S2 118.4(3) . . ?
C18 C23 S2 120.8(3) . . ?

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
N1 H1A N2 0.89(5) 2.13(5) 2.903(5) 144(4) .
N1 H1B O1S 0.99(5) 1.97(5) 2.874(5) 151(4) .
N7 H7A O2 0.86(6) 2.18(6) 2.870(5) 137(5) .
N7 H7B O6 0.83(4) 2.12(5) 2.911(5) 162(4) 3_747
O1S H1S O4 0.68(6) 2.39(6) 2.989(5) 150(7) .
O1S H2S N6 0.97(6) 2.00(6) 2.969(5) 171(5) 1_455

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.600
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.105
####################################################################### 
# 
# 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_ph2snl1
_database_code_depnum_ccdc_archive 'CCDC 776592'
_audit_update_record             
;
2010-05-10 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
#TrackingRef 'ph2snl1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H37 N9 O6 S2 Sn'
_chemical_formula_weight         910.59

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'I 2/a'

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

_cell_length_a                   10.0349(3)
_cell_length_b                   15.1394(5)
_cell_length_c                   26.2883(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.571(2)
_cell_angle_gamma                90.00
_cell_volume                     3959.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1957
_cell_measurement_theta_min      2.705
_cell_measurement_theta_max      30.485

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8050
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G ttingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            99635
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         30.63
_reflns_number_total             6094
_reflns_number_gt                5754
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0203P)²+4.3158P] 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         6094
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0464
_refine_ls_wR_factor_gt          0.0455
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Sn1 Sn 0.2500 0.226084(6) 0.5000 0.00695(3) Uani 1 2 d S . .
S1 S 0.56332(3) 0.303100(19) 0.698408(10) 0.01254(5) Uani 1 1 d . . .
O1 O 0.37353(7) 0.33283(5) 0.54336(3) 0.01018(14) Uani 1 1 d . . .
O3 O 0.41934(8) 0.30359(6) 0.68678(3) 0.01736(17) Uani 1 1 d . . .
O4 O 0.62281(9) 0.33186(6) 0.74858(3) 0.01910(17) Uani 1 1 d . . .
N1 N 0.61556(11) 0.20386(7) 0.69143(4) 0.01569(19) Uani 1 1 d . . .
N2 N 0.51036(9) 0.22375(6) 0.58544(4) 0.01005(16) Uani 1 1 d . . .
N3 N 0.42419(9) 0.16622(6) 0.55707(3) 0.00909(16) Uani 1 1 d . . .
N4 N 0.2500 0.07029(8) 0.5000 0.0091(2) Uani 1 2 d S . .
C1 C 0.62324(11) 0.37452(7) 0.65259(4) 0.01203(19) Uani 1 1 d . . .
C2 C 0.72044(12) 0.43650(8) 0.67089(5) 0.0184(2) Uani 1 1 d . . .
H2 H 0.7599 0.4348 0.7058 0.022 Uiso 1 1 calc R . .
C3 C 0.75981(13) 0.50085(9) 0.63816(5) 0.0230(3) Uani 1 1 d . . .
H3 H 0.8281 0.5420 0.6505 0.028 Uiso 1 1 calc R . .
C4 C 0.69969(13) 0.50511(8) 0.58766(5) 0.0211(2) Uani 1 1 d . . .
H4 H 0.7244 0.5503 0.5656 0.025 Uiso 1 1 calc R . .
C5 C 0.60296(12) 0.44294(8) 0.56936(5) 0.0154(2) Uani 1 1 d . . .
H5 H 0.5617 0.4464 0.5347 0.018 Uiso 1 1 calc R . .
C6 C 0.56531(10) 0.37558(7) 0.60083(4) 0.01047(18) Uani 1 1 d . . .
C7 C 0.47243(10) 0.30684(7) 0.57539(4) 0.00908(18) Uani 1 1 d . . .
C8 C 0.44640(10) 0.08214(7) 0.56182(4) 0.00949(18) Uani 1 1 d . . .
C9 C 0.56016(11) 0.04167(7) 0.59637(4) 0.0135(2) Uani 1 1 d . . .
H9A H 0.6347 0.0838 0.6021 0.020 Uiso 1 1 calc R . .
H9B H 0.5902 -0.0120 0.5804 0.020 Uiso 1 1 calc R . .
H9C H 0.5301 0.0266 0.6293 0.020 Uiso 1 1 calc R . .
C10 C 0.34633(10) 0.02636(7) 0.53032(4) 0.00999(18) Uani 1 1 d . . .
C11 C 0.34883(11) -0.06587(7) 0.53148(4) 0.0130(2) Uani 1 1 d . . .
H11 H 0.4165 -0.0966 0.5533 0.016 Uiso 1 1 calc R . .
C12 C 0.2500 -0.11163(10) 0.5000 0.0147(3) Uani 1 2 d S . .
H12 H 0.2500 -0.1744 0.5000 0.018 Uiso 1 2 calc SR . .
C13 C 0.11944(10) 0.23280(7) 0.55860(4) 0.01000(18) Uani 1 1 d . . .
C14 C 0.15449(12) 0.19216(8) 0.60609(4) 0.0153(2) Uani 1 1 d . . .
H14 H 0.2375 0.1614 0.6128 0.018 Uiso 1 1 calc R . .
C15 C 0.06917(13) 0.19606(9) 0.64396(5) 0.0206(2) Uani 1 1 d . . .
H15 H 0.0938 0.1671 0.6759 0.025 Uiso 1 1 calc R . .
C16 C -0.05145(13) 0.24206(9) 0.63513(5) 0.0199(2) Uani 1 1 d . . .
H16 H -0.1091 0.2450 0.6610 0.024 Uiso 1 1 calc R . .
C17 C -0.08714(12) 0.28358(8) 0.58832(5) 0.0181(2) Uani 1 1 d . . .
H17 H -0.1691 0.3155 0.5821 0.022 Uiso 1 1 calc R . .
C18 C -0.00274(11) 0.27844(8) 0.55036(4) 0.0144(2) Uani 1 1 d . . .
H18 H -0.0287 0.3065 0.5182 0.017 Uiso 1 1 calc R . .
H1A H 0.5959(18) 0.1881(13) 0.6605(7) 0.032(5) Uiso 1 1 d . . .
H1B H 0.6933(18) 0.1935(12) 0.7068(7) 0.027(4) Uiso 1 1 d . . .
N1S N 0.32077(16) 0.02044(11) 0.68103(6) 0.0434(4) Uani 1 1 d . . .
C1S C 0.33819(15) 0.06550(11) 0.71594(6) 0.0320(3) Uani 1 1 d . . .
C2S C 0.3594(2) 0.12441(12) 0.75999(7) 0.0437(4) Uani 1 1 d . . .
H2S1 H 0.3871 0.1826 0.7490 0.066 Uiso 1 1 calc R . .
H2S2 H 0.4297 0.1002 0.7856 0.066 Uiso 1 1 calc R . .
H2S3 H 0.2755 0.1301 0.7751 0.066 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
Sn1 C13 2.1523(10) . ?
Sn1 C13 2.1523(10) 2_556 ?
Sn1 O1 2.2528(8) . ?
Sn1 O1 2.2528(8) 2_556 ?
Sn1 N3 2.3316(9) 2_556 ?
Sn1 N3 2.3316(9) . ?
Sn1 N4 2.3587(13) . ?
S1 O3 1.4369(9) . ?
S1 O4 1.4416(9) . ?
S1 N1 1.6096(11) . ?
S1 C1 1.7810(11) . ?
O1 C7 1.2762(13) . ?
N2 C7 1.3306(14) . ?
N2 N3 1.3757(12) . ?
N3 C8 1.2955(14) . ?
N4 C10 1.3450(12) 2_556 ?
N4 C10 1.3450(12) . ?
C1 C2 1.3926(16) . ?
C1 C6 1.4076(15) . ?
C2 C3 1.3910(18) . ?
C3 C4 1.3854(19) . ?
C4 C5 1.3916(16) . ?
C5 C6 1.3962(15) . ?
C6 C7 1.4950(14) . ?
C8 C10 1.4793(15) . ?
C8 C9 1.4933(15) . ?
C10 C11 1.3968(15) . ?
C11 C12 1.3901(14) . ?
C12 C11 1.3901(13) 2_556 ?
C13 C14 1.3946(15) . ?
C13 C18 1.3992(15) . ?
C14 C15 1.3971(16) . ?
C15 C16 1.3893(18) . ?
C16 C17 1.3862(18) . ?
C17 C18 1.3935(16) . ?
N1S C1S 1.138(2) . ?
C1S C2S 1.455(3) . ?

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
C13 Sn1 C13 174.59(6) . 2_556 ?
C13 Sn1 O1 87.15(3) . . ?
C13 Sn1 O1 88.97(3) 2_556 . ?
C13 Sn1 O1 88.97(3) . 2_556 ?
C13 Sn1 O1 87.15(3) 2_556 2_556 ?
O1 Sn1 O1 88.32(4) . 2_556 ?
C13 Sn1 N3 90.20(4) . 2_556 ?
C13 Sn1 N3 91.91(4) 2_556 2_556 ?
O1 Sn1 N3 156.96(3) . 2_556 ?
O1 Sn1 N3 68.74(3) 2_556 2_556 ?
C13 Sn1 N3 91.91(4) . . ?
C13 Sn1 N3 90.20(4) 2_556 . ?
O1 Sn1 N3 68.74(3) . . ?
O1 Sn1 N3 156.96(3) 2_556 . ?
N3 Sn1 N3 134.26(4) 2_556 . ?
C13 Sn1 N4 92.71(3) . . ?
C13 Sn1 N4 92.71(3) 2_556 . ?
O1 Sn1 N4 135.838(19) . . ?
O1 Sn1 N4 135.84(2) 2_556 . ?
N3 Sn1 N4 67.13(2) 2_556 . ?
N3 Sn1 N4 67.13(2) . . ?
O3 S1 O4 118.46(5) . . ?
O3 S1 N1 108.30(6) . . ?
O4 S1 N1 106.53(5) . . ?
O3 S1 C1 105.82(5) . . ?
O4 S1 C1 107.42(5) . . ?
N1 S1 C1 110.22(5) . . ?
C7 O1 Sn1 116.16(7) . . ?
C7 N2 N3 110.36(9) . . ?
C8 N3 N2 118.81(9) . . ?
C8 N3 Sn1 123.29(7) . . ?
N2 N3 Sn1 117.85(6) . . ?
C10 N4 C10 120.73(13) 2_556 . ?
C10 N4 Sn1 119.63(7) 2_556 . ?
C10 N4 Sn1 119.63(7) . . ?
C2 C1 C6 120.49(10) . . ?
C2 C1 S1 117.33(9) . . ?
C6 C1 S1 121.83(8) . . ?
C3 C2 C1 120.10(11) . . ?
C4 C3 C2 120.13(11) . . ?
C3 C4 C5 119.71(11) . . ?
C4 C5 C6 121.33(11) . . ?
C5 C6 C1 118.14(10) . . ?
C5 C6 C7 116.41(10) . . ?
C1 C6 C7 125.33(10) . . ?
O1 C7 N2 126.85(10) . . ?
O1 C7 C6 117.74(9) . . ?
N2 C7 C6 115.09(9) . . ?
N3 C8 C10 114.30(9) . . ?
N3 C8 C9 124.74(10) . . ?
C10 C8 C9 120.95(9) . . ?
N4 C10 C11 121.11(10) . . ?
N4 C10 C8 115.55(9) . . ?
C11 C10 C8 123.33(10) . . ?
C12 C11 C10 118.41(11) . . ?
C11 C12 C11 120.21(14) . 2_556 ?
C14 C13 C18 117.98(10) . . ?
C14 C13 Sn1 120.95(8) . . ?
C18 C13 Sn1 121.07(8) . . ?
C13 C14 C15 120.88(11) . . ?
C16 C15 C14 120.29(11) . . ?
C17 C16 C15 119.55(11) . . ?
C16 C17 C18 120.00(11) . . ?
C17 C18 C13 121.30(11) . . ?
N1S C1S C2S 178.96(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
N1 H1A N2 0.846(19) 2.114(19) 2.8624(14) 147.1(17) .
N1 H1B O4 0.845(18) 2.088(19) 2.9294(14) 174.3(17) 7_656

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.63
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_ph2snl1b
_database_code_depnum_ccdc_archive 'CCDC 776593'
_audit_update_record             
;
2010-05-10 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
#TrackingRef 'ph2snl1b.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H31 N7 O6 S2 Sn'
_chemical_formula_weight         828.48

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n m a'

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

_cell_length_a                   14.6879(3)
_cell_length_b                   18.3871(4)
_cell_length_c                   12.6439(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3414.71(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9773
_cell_measurement_theta_min      2.215
_cell_measurement_theta_max      32.75

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7192
_exptl_absorpt_correction_T_max  0.8581
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G ttingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            109478
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         31.50
_reflns_number_total             5835
_reflns_number_gt                5153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0246P)²+2.4202P] 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         5835
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0586
_refine_ls_wR_factor_gt          0.0566
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Sn1 Sn 0.464250(8) 0.2500 0.366748(10) 0.00993(4) Uani 1 2 d S . .
S1 S 0.40682(2) -0.05392(2) 0.22854(3) 0.01956(8) Uani 1 1 d . . .
O1 O 0.35783(6) 0.16595(5) 0.33475(8) 0.01307(18) Uani 1 1 d . . .
O2 O 0.43173(8) 0.00584(7) 0.16175(9) 0.0268(3) Uani 1 1 d . . .
O3 O 0.38399(8) -0.12253(7) 0.18152(10) 0.0294(3) Uani 1 1 d . . .
N1 N 0.48997(9) -0.06915(8) 0.30914(12) 0.0224(3) Uani 1 1 d . . .
N2 N 0.46218(7) 0.07591(6) 0.38231(9) 0.0125(2) Uani 1 1 d . . .
N3 N 0.52236(7) 0.13346(6) 0.38891(9) 0.0119(2) Uani 1 1 d . . .
N4 N 0.62050(10) 0.2500 0.40782(14) 0.0131(3) Uani 1 2 d S . .
C1 C 0.31182(9) -0.02519(8) 0.30500(11) 0.0144(2) Uani 1 1 d . . .
C2 C 0.24032(9) -0.07440(8) 0.31363(12) 0.0164(3) Uani 1 1 d . . .
H2 H 0.2454 -0.1212 0.2823 0.020 Uiso 1 1 calc R . .
C3 C 0.16163(9) -0.05546(8) 0.36781(12) 0.0171(3) Uani 1 1 d . . .
H3 H 0.1136 -0.0897 0.3752 0.021 Uiso 1 1 calc R . .
C4 C 0.15336(9) 0.01333(8) 0.41093(13) 0.0183(3) Uani 1 1 d . . .
H4 H 0.0992 0.0267 0.4471 0.022 Uiso 1 1 calc R . .
C5 C 0.22459(9) 0.06323(8) 0.40144(12) 0.0159(3) Uani 1 1 d . . .
H5 H 0.2178 0.1107 0.4301 0.019 Uiso 1 1 calc R . .
C6 C 0.30555(9) 0.04450(7) 0.35047(11) 0.0125(2) Uani 1 1 d . . .
C7 C 0.37999(8) 0.10026(7) 0.35382(10) 0.0114(2) Uani 1 1 d . . .
C8 C 0.60801(8) 0.12052(7) 0.40482(11) 0.0122(2) Uani 1 1 d . . .
C9 C 0.64703(9) 0.04557(8) 0.41266(13) 0.0176(3) Uani 1 1 d . . .
H9A H 0.6088 0.0159 0.4593 0.026 Uiso 1 1 calc R . .
H9B H 0.7088 0.0482 0.4417 0.026 Uiso 1 1 calc R . .
H9C H 0.6491 0.0235 0.3422 0.026 Uiso 1 1 calc R . .
C10 C 0.66526(8) 0.18617(7) 0.41266(11) 0.0127(2) Uani 1 1 d . . .
C11 C 0.75998(9) 0.18462(8) 0.42454(12) 0.0159(3) Uani 1 1 d . . .
H11 H 0.7918 0.1397 0.4273 0.019 Uiso 1 1 calc R . .
C12 C 0.80622(13) 0.2500 0.43214(17) 0.0184(4) Uani 1 2 d S . .
H12 H 0.8703 0.2500 0.4427 0.022 Uiso 1 2 calc SR . .
C13 C 0.42190(12) 0.2500 0.52888(15) 0.0125(3) Uani 1 2 d S . .
C14 C 0.48445(14) 0.2500 0.61183(16) 0.0172(4) Uani 1 2 d S . .
H14 H 0.5478 0.2500 0.5966 0.021 Uiso 1 2 calc SR . .
C15 C 0.45536(15) 0.2500 0.71682(17) 0.0211(4) Uani 1 2 d S . .
H15 H 0.4988 0.2500 0.7725 0.025 Uiso 1 2 calc SR . .
C16 C 0.36343(16) 0.2500 0.74003(17) 0.0213(4) Uani 1 2 d S . .
H16 H 0.3437 0.2500 0.8116 0.026 Uiso 1 2 calc SR . .
C17 C 0.30017(15) 0.2500 0.65882(18) 0.0210(4) Uani 1 2 d S . .
H17 H 0.2369 0.2500 0.6746 0.025 Uiso 1 2 calc SR . .
C18 C 0.32929(13) 0.2500 0.55368(17) 0.0179(4) Uani 1 2 d S . .
H18 H 0.2855 0.2500 0.4984 0.021 Uiso 1 2 calc SR . .
C19 C 0.50303(12) 0.2500 0.20430(15) 0.0127(3) Uani 1 2 d S . .
C20 C 0.51561(9) 0.18448(8) 0.14970(11) 0.0159(3) Uani 1 1 d . . .
H20 H 0.5059 0.1395 0.1850 0.019 Uiso 1 1 calc R . .
C21 C 0.54221(9) 0.18475(9) 0.04396(12) 0.0183(3) Uani 1 1 d . . .
H21 H 0.5502 0.1401 0.0074 0.022 Uiso 1 1 calc R . .
C22 C 0.55703(13) 0.2500 -0.00803(16) 0.0185(4) Uani 1 2 d S . .
H22 H 0.5774 0.2500 -0.0794 0.022 Uiso 1 2 calc SR . .
H1A H 0.4990(15) -0.0333(13) 0.3483(17) 0.029(5) Uiso 1 1 d . . .
H1B H 0.4879(16) -0.1086(14) 0.3377(19) 0.040(7) Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C19 2.1315(19) . ?
Sn1 C13 2.1423(19) . ?
Sn1 O1 2.2349(9) 8_565 ?
Sn1 O1 2.2349(9) . ?
Sn1 N3 2.3236(12) 8_565 ?
Sn1 N3 2.3236(12) . ?
Sn1 N4 2.3530(15) . ?
S1 O2 1.4331(13) . ?
S1 O3 1.4343(12) . ?
S1 N1 1.6151(15) . ?
S1 C1 1.7779(14) . ?
O1 C7 1.2740(16) . ?
N2 C7 1.3370(16) . ?
N2 N3 1.3813(16) . ?
N3 C8 1.2960(16) . ?
N4 C10 1.3468(15) 8_565 ?
N4 C10 1.3468(15) . ?
C1 C2 1.3905(19) . ?
C1 C6 1.4074(19) . ?
C2 C3 1.388(2) . ?
C3 C4 1.383(2) . ?
C4 C5 1.3967(19) . ?
C5 C6 1.3957(18) . ?
C6 C7 1.4994(18) . ?
C8 C10 1.4745(19) . ?
C8 C9 1.4958(19) . ?
C10 C11 1.3995(17) . ?
C11 C12 1.3841(17) . ?
C12 C11 1.3841(17) 8_565 ?
C13 C14 1.394(3) . ?
C13 C18 1.396(3) . ?
C14 C15 1.395(3) . ?
C15 C16 1.382(3) . ?
C16 C17 1.385(3) . ?
C17 C18 1.396(3) . ?
C19 C20 1.4008(17) 8_565 ?
C19 C20 1.4008(17) . ?
C20 C21 1.393(2) . ?
C21 C22 1.3852(19) . ?
C22 C21 1.3852(19) 8_565 ?

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
C19 Sn1 C13 178.62(7) . . ?
C19 Sn1 O1 90.72(4) . 8_565 ?
C13 Sn1 O1 88.29(4) . 8_565 ?
C19 Sn1 O1 90.72(4) . . ?
C13 Sn1 O1 88.29(4) . . ?
O1 Sn1 O1 87.49(5) 8_565 . ?
C19 Sn1 N3 91.03(3) . 8_565 ?
C13 Sn1 N3 89.50(3) . 8_565 ?
O1 Sn1 N3 68.96(4) 8_565 8_565 ?
O1 Sn1 N3 156.41(4) . 8_565 ?
C19 Sn1 N3 91.03(3) . . ?
C13 Sn1 N3 89.50(3) . . ?
O1 Sn1 N3 156.41(4) 8_565 . ?
O1 Sn1 N3 68.96(4) . . ?
N3 Sn1 N3 134.51(5) 8_565 . ?
C19 Sn1 N4 87.25(6) . . ?
C13 Sn1 N4 94.13(6) . . ?
O1 Sn1 N4 136.23(2) 8_565 . ?
O1 Sn1 N4 136.23(2) . . ?
N3 Sn1 N4 67.36(3) 8_565 . ?
N3 Sn1 N4 67.36(3) . . ?
O2 S1 O3 119.32(8) . . ?
O2 S1 N1 108.16(8) . . ?
O3 S1 N1 106.61(8) . . ?
O2 S1 C1 107.04(7) . . ?
O3 S1 C1 107.65(7) . . ?
N1 S1 C1 107.57(7) . . ?
C7 O1 Sn1 116.27(8) . . ?
C7 N2 N3 109.72(11) . . ?
C8 N3 N2 119.33(12) . . ?
C8 N3 Sn1 123.00(9) . . ?
N2 N3 Sn1 117.66(8) . . ?
C10 N4 C10 121.27(16) 8_565 . ?
C10 N4 Sn1 119.09(8) 8_565 . ?
C10 N4 Sn1 119.09(8) . . ?
C2 C1 C6 120.73(12) . . ?
C2 C1 S1 116.24(11) . . ?
C6 C1 S1 122.95(10) . . ?
C3 C2 C1 120.29(13) . . ?
C4 C3 C2 119.82(13) . . ?
C3 C4 C5 120.08(13) . . ?
C6 C5 C4 121.05(13) . . ?
C5 C6 C1 117.97(12) . . ?
C5 C6 C7 116.07(12) . . ?
C1 C6 C7 125.90(12) . . ?
O1 C7 N2 126.81(12) . . ?
O1 C7 C6 117.17(11) . . ?
N2 C7 C6 115.91(12) . . ?
N3 C8 C10 114.44(12) . . ?
N3 C8 C9 123.46(12) . . ?
C10 C8 C9 122.09(11) . . ?
N4 C10 C11 120.52(13) . . ?
N4 C10 C8 115.59(11) . . ?
C11 C10 C8 123.88(12) . . ?
C12 C11 C10 118.53(13) . . ?
C11 C12 C11 120.58(17) 8_565 . ?
C14 C13 C18 118.24(19) . . ?
C14 C13 Sn1 121.90(14) . . ?
C18 C13 Sn1 119.86(14) . . ?
C13 C14 C15 120.94(19) . . ?
C16 C15 C14 120.1(2) . . ?
C15 C16 C17 119.9(2) . . ?
C16 C17 C18 120.0(2) . . ?
C13 C18 C17 120.81(19) . . ?
C20 C19 C20 118.65(18) 8_565 . ?
C20 C19 Sn1 120.67(9) 8_565 . ?
C20 C19 Sn1 120.67(9) . . ?
C21 C20 C19 120.46(14) . . ?
C22 C21 C20 120.18(15) . . ?
C21 C22 C21 120.02(19) 8_565 . ?

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
N1 H1A N2 0.84(2) 2.12(2) 2.8524(19) 146(2) .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        31.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.077


