# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2007

data_global

_journal_coden_Cambridge         440

loop_
_publ_author_name
'Paris E. Georghiou'
'Julie L. Collins'
'Huu-Anh Tran'

_publ_contact_author_name        'Paris E. Georghiou'
_publ_contact_author_address     
;
Chemistry
Memorial University of Newfoundland
Elizabeth Avenue
St. John's
Newfoundland
A1B 3X7
CANADA
;

_publ_contact_author_email       PARISG@MUN.CA

_publ_requested_journal          'New Journal of Chemistry'

_publ_section_title              
;
Synthesis of "calixarene-like"
N,N-ditosyldiaza[3.3](1,4)naphthalenophanes
;

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 673893'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45.50 H45.50 Cl10.50 N2 O8 S2'
_chemical_formula_weight         1184.68

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   12.9568(11)
_cell_length_b                   14.4422(14)
_cell_length_c                   15.5453(12)
_cell_angle_alpha                92.450(2)
_cell_angle_beta                 103.0690(10)
_cell_angle_gamma                112.024(2)
_cell_volume                     2600.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    12284
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      30.7

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1214
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.7736
_exptl_absorpt_correction_T_max  0.8542
_exptl_absorpt_process_details   
;
Higashi, T. (1999). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            27650
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.50
_reflns_number_total             10658
_reflns_number_gt                9861
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalStructure 3.7.0 (Rigaku)'
_computing_publication_material  'CrystalStructure 3.7.0 (Rigaku)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0802P)^2^+4.6135P] where P=(Fo^2^+2Fc^2^)/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         10658
_refine_ls_number_parameters     632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.1813
_refine_ls_wR_factor_gt          0.1773
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Cl1 Cl 0.27597(11) 0.75623(8) 0.41348(9) 0.0692(3) Uani 1 1 d . . .
Cl2 Cl 0.11791(10) 0.59334(10) 0.27554(7) 0.0627(3) Uani 1 1 d . . .
Cl3 Cl 0.12031(10) 0.57591(8) 0.45990(7) 0.0592(3) Uani 1 1 d . . .
Cl4 Cl 0.43854(13) 0.93641(12) 0.25197(12) 0.0921(5) Uani 1 1 d . . .
Cl5 Cl 0.46626(14) 0.74883(9) 0.23210(11) 0.0873(5) Uani 1 1 d . . .
Cl6 Cl 0.56275(11) 0.87593(11) 0.39868(8) 0.0818(4) Uani 1 1 d . . .
Cl7 Cl 0.7000(2) 0.37106(15) 0.2164(3) 0.1761(14) Uani 1 1 d . . .
Cl8 Cl 0.50561(13) 0.18333(11) 0.19217(9) 0.0800(4) Uani 1 1 d . . .
Cl9 Cl 0.59673(17) 0.31246(12) 0.35830(11) 0.1044(6) Uani 1 1 d . . .
Cl10 Cl 0.4183(3) 0.5653(3) -0.0651(2) 0.1020(11) Uani 0.50 1 d P . .
Cl11 Cl 0.4908(4) 0.5850(3) 0.0419(3) 0.1224(14) Uani 0.50 1 d P . .
Cl12 Cl 0.5444(3) 0.5566(3) 0.10784(19) 0.0890(8) Uani 0.50 1 d P . .
S1 S -0.12695(6) -0.27436(5) 0.37132(5) 0.03216(18) Uani 1 1 d . . .
S2 S 0.24399(6) 0.30139(5) 0.11542(5) 0.02729(17) Uani 1 1 d . . .
O1 O -0.1150(2) -0.34163(17) 0.30691(17) 0.0398(5) Uani 1 1 d . . .
O2 O -0.0442(2) -0.24122(17) 0.45664(16) 0.0416(6) Uani 1 1 d . . .
O3 O 0.25666(19) 0.24180(16) 0.04573(15) 0.0352(5) Uani 1 1 d . . .
O4 O 0.33942(18) 0.35029(16) 0.19202(15) 0.0351(5) Uani 1 1 d . . .
O5 O -0.20563(18) 0.05838(16) 0.33828(14) 0.0329(5) Uani 1 1 d . . .
O6 O -0.31981(17) -0.08397(16) 0.14246(14) 0.0302(4) Uani 1 1 d . . .
O7 O -0.08610(19) 0.23742(16) 0.28348(14) 0.0327(5) Uani 1 1 d . . .
O8 O -0.20595(18) 0.09384(17) 0.07406(14) 0.0328(5) Uani 1 1 d . . .
N1 N -0.1209(2) -0.17272(18) 0.32533(16) 0.0282(5) Uani 1 1 d . . .
N2 N 0.1369(2) 0.22773(17) 0.15229(15) 0.0255(5) Uani 1 1 d . . .
C1 C -0.2657(3) -0.3321(2) 0.3879(2) 0.0306(6) Uani 1 1 d . . .
C2 C -0.2912(3) -0.2979(3) 0.4613(2) 0.0432(8) Uani 1 1 d . . .
H1 H -0.2327 -0.2462 0.5057 0.052 Uiso 1 1 calc R . .
C3 C -0.4037(3) -0.3402(3) 0.4696(2) 0.0458(8) Uani 1 1 d . . .
H2 H -0.4210 -0.3173 0.5206 0.055 Uiso 1 1 calc R . .
C4 C -0.4904(3) -0.4144(2) 0.4059(2) 0.0364(7) Uani 1 1 d . . .
C5 C -0.4619(3) -0.4484(3) 0.3334(3) 0.0469(9) Uani 1 1 d . . .
H3 H -0.5201 -0.5011 0.2897 0.056 Uiso 1 1 calc R . .
C6 C -0.3511(3) -0.4077(3) 0.3234(3) 0.0449(8) Uani 1 1 d . . .
H4 H -0.3335 -0.4313 0.2728 0.054 Uiso 1 1 calc R . .
C7 C -0.6132(3) -0.4567(3) 0.4126(3) 0.0507(9) Uani 1 1 d . . .
H5 H -0.6530 -0.4152 0.3851 0.061 Uiso 1 1 calc R . .
H6 H -0.6139 -0.4563 0.4756 0.061 Uiso 1 1 calc R . .
H7 H -0.6528 -0.5261 0.3816 0.061 Uiso 1 1 calc R . .
C8 C -0.1971(3) -0.1932(2) 0.23287(19) 0.0295(6) Uani 1 1 d . . .
H8 H -0.2738 -0.1960 0.2355 0.035 Uiso 1 1 calc R . .
H9 H -0.2077 -0.2596 0.2036 0.035 Uiso 1 1 calc R . .
C9 C -0.1456(2) -0.1122(2) 0.17855(18) 0.0267(6) Uani 1 1 d . . .
C10 C -0.0337(2) -0.0916(2) 0.16516(18) 0.0252(6) Uani 1 1 d . . .
C11 C 0.0233(3) -0.1582(2) 0.18616(19) 0.0294(6) Uani 1 1 d . . .
H10 H -0.0105 -0.2153 0.2138 0.035 Uiso 1 1 calc R . .
C12 C 0.1266(3) -0.1406(2) 0.1668(2) 0.0325(6) Uani 1 1 d . . .
H11 H 0.1626 -0.1867 0.1796 0.039 Uiso 1 1 calc R . .
C13 C 0.1795(3) -0.0551(2) 0.1282(2) 0.0322(6) Uani 1 1 d . . .
H12 H 0.2509 -0.0438 0.1148 0.039 Uiso 1 1 calc R . .
C14 C 0.1286(2) 0.0123(2) 0.10961(19) 0.0288(6) Uani 1 1 d . . .
H13 H 0.1661 0.0706 0.0847 0.035 Uiso 1 1 calc R . .
C15 C 0.0206(2) -0.0041(2) 0.12725(18) 0.0254(6) Uani 1 1 d . . .
C16 C -0.0354(2) 0.0643(2) 0.10669(18) 0.0255(6) Uani 1 1 d . . .
C17 C -0.1488(2) 0.0351(2) 0.10865(18) 0.0263(6) Uani 1 1 d . . .
C18 C -0.2047(2) -0.0556(2) 0.14225(18) 0.0270(6) Uani 1 1 d . . .
C19 C 0.0289(2) 0.1663(2) 0.08196(19) 0.0281(6) Uani 1 1 d . . .
H14 H 0.0487 0.1567 0.0253 0.034 Uiso 1 1 calc R . .
H15 H -0.0221 0.2037 0.0721 0.034 Uiso 1 1 calc R . .
C20 C 0.2056(2) 0.3961(2) 0.0667(2) 0.0288(6) Uani 1 1 d . . .
C21 C 0.1540(3) 0.3799(3) -0.0241(2) 0.0374(7) Uani 1 1 d . . .
H16 H 0.1388 0.3185 -0.0591 0.045 Uiso 1 1 calc R . .
C22 C 0.1247(3) 0.4540(3) -0.0633(2) 0.0442(8) Uani 1 1 d . . .
H17 H 0.0899 0.4429 -0.1256 0.053 Uiso 1 1 calc R . .
C23 C 0.1453(3) 0.5442(3) -0.0133(2) 0.0398(8) Uani 1 1 d . . .
C24 C 0.1966(3) 0.5586(3) 0.0772(2) 0.0420(8) Uani 1 1 d . . .
H18 H 0.2112 0.6198 0.1124 0.050 Uiso 1 1 calc R . .
C25 C 0.2273(3) 0.4851(2) 0.1181(2) 0.0358(7) Uani 1 1 d . . .
H19 H 0.2626 0.4962 0.1804 0.043 Uiso 1 1 calc R . .
C26 C 0.1121(4) 0.6242(3) -0.0566(3) 0.0566(11) Uani 1 1 d . . .
H20 H 0.1193 0.6224 -0.1180 0.068 Uiso 1 1 calc R . .
H21 H 0.1633 0.6908 -0.0228 0.068 Uiso 1 1 calc R . .
H22 H 0.0321 0.6115 -0.0571 0.068 Uiso 1 1 calc R . .
C27 C 0.1217(3) 0.2717(2) 0.23456(19) 0.0294(6) Uani 1 1 d . . .
H23 H 0.0679 0.3057 0.2178 0.035 Uiso 1 1 calc R . .
H24 H 0.1968 0.3230 0.2697 0.035 Uiso 1 1 calc R . .
C28 C 0.0748(3) 0.1914(2) 0.29147(18) 0.0274(6) Uani 1 1 d . . .
C29 C 0.1347(3) 0.1296(2) 0.32546(18) 0.0267(6) Uani 1 1 d . . .
C30 C 0.2510(3) 0.1535(2) 0.32457(19) 0.0309(6) Uani 1 1 d . . .
H25 H 0.2899 0.2103 0.2986 0.037 Uiso 1 1 calc R . .
C31 C 0.3081(3) 0.0953(2) 0.3608(2) 0.0346(7) Uani 1 1 d . . .
H26 H 0.3863 0.1127 0.3605 0.042 Uiso 1 1 calc R . .
C32 C 0.2511(3) 0.0105(2) 0.3984(2) 0.0350(7) Uani 1 1 d . . .
H27 H 0.2912 -0.0292 0.4236 0.042 Uiso 1 1 calc R . .
C33 C 0.1380(3) -0.0159(2) 0.3990(2) 0.0312(6) Uani 1 1 d . . .
H28 H 0.1006 -0.0741 0.4242 0.037 Uiso 1 1 calc R . .
C34 C 0.0762(2) 0.0421(2) 0.36265(18) 0.0265(6) Uani 1 1 d . . .
C35 C -0.0426(3) 0.0152(2) 0.36200(18) 0.0270(6) Uani 1 1 d . . .
C36 C -0.0912(3) 0.0838(2) 0.34021(18) 0.0277(6) Uani 1 1 d . . .
C37 C -0.0303(3) 0.1737(2) 0.30749(18) 0.0276(6) Uani 1 1 d . . .
C38 C -0.1135(3) -0.0858(2) 0.38541(19) 0.0304(6) Uani 1 1 d . . .
H29 H -0.0786 -0.0907 0.4477 0.036 Uiso 1 1 calc R . .
H30 H -0.1923 -0.0896 0.3816 0.036 Uiso 1 1 calc R . .
C39 C -0.0340(3) 0.3333(2) 0.3407(2) 0.0419(8) Uani 1 1 d . . .
H31 H -0.0694 0.3286 0.3906 0.050 Uiso 1 1 calc R . .
H32 H -0.0460 0.3855 0.3065 0.050 Uiso 1 1 calc R . .
H33 H 0.0489 0.3508 0.3637 0.050 Uiso 1 1 calc R . .
C40 C -0.2850(3) 0.1134(2) 0.1170(2) 0.0354(7) Uani 1 1 d . . .
H34 H -0.3627 0.0612 0.0925 0.042 Uiso 1 1 calc R . .
H35 H -0.2855 0.1797 0.1064 0.042 Uiso 1 1 calc R . .
H36 H -0.2604 0.1127 0.1813 0.042 Uiso 1 1 calc R . .
C41 C -0.3961(3) -0.1351(3) 0.0570(2) 0.0451(8) Uani 1 1 d . . .
H37 H -0.4013 -0.2045 0.0492 0.054 Uiso 1 1 calc R . .
H38 H -0.3662 -0.0997 0.0098 0.054 Uiso 1 1 calc R . .
H39 H -0.4729 -0.1359 0.0536 0.054 Uiso 1 1 calc R . .
C42 C -0.2313(3) 0.1266(3) 0.3910(2) 0.0376(7) Uani 1 1 d . . .
H40 H -0.1681 0.1575 0.4451 0.045 Uiso 1 1 calc R . .
H41 H -0.3030 0.0897 0.4075 0.045 Uiso 1 1 calc R . .
H42 H -0.2405 0.1795 0.3563 0.045 Uiso 1 1 calc R . .
C43 C 0.1376(3) 0.6586(3) 0.3803(3) 0.0470(8) Uani 1 1 d . . .
H44 H 0.0647 0.6748 0.3659 0.041 Uiso 1 1 d . . .
C44 C 0.5283(3) 0.8740(3) 0.2825(3) 0.0421(8) Uani 1 1 d . . .
H43 H 0.5984 0.9019 0.2677 0.041 Uiso 1 1 d . . .
C45 C 0.5708(4) 0.3079(3) 0.2443(3) 0.0591(11) Uani 1 1 d . . .
H45 H 0.5258 0.3458 0.2208 0.041 Uiso 1 1 d . . .
C46 C 0.5298(8) 0.5361(7) -0.0046(7) 0.063(2) Uani 0.50 1 d P . .
H46 H 0.5973 0.5873 -0.0250 0.041 Uiso 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0761(8) 0.0366(5) 0.0919(9) 0.0023(5) 0.0371(7) 0.0109(5)
Cl2 0.0639(6) 0.0861(8) 0.0363(5) 0.0057(5) 0.0090(4) 0.0305(6)
Cl3 0.0681(7) 0.0554(6) 0.0451(5) 0.0042(4) 0.0283(5) 0.0073(5)
Cl4 0.0801(9) 0.0986(10) 0.1271(13) 0.0497(9) 0.0262(8) 0.0648(8)
Cl5 0.0994(10) 0.0453(6) 0.1101(11) -0.0056(6) 0.0582(9) 0.0048(6)
Cl6 0.0577(7) 0.0961(9) 0.0584(7) 0.0311(6) 0.0038(5) -0.0016(6)
Cl7 0.1273(16) 0.0911(12) 0.375(4) 0.0628(18) 0.177(2) 0.0474(12)
Cl8 0.0807(9) 0.0797(8) 0.0712(8) -0.0074(6) 0.0158(6) 0.0266(7)
Cl9 0.1299(14) 0.0774(9) 0.0767(9) -0.0130(7) -0.0272(9) 0.0426(9)
Cl10 0.0726(18) 0.155(3) 0.0805(19) 0.047(2) 0.0169(15) 0.046(2)
Cl11 0.160(4) 0.078(2) 0.126(3) -0.008(2) 0.047(3) 0.040(2)
Cl12 0.097(2) 0.102(2) 0.0586(15) 0.0087(14) 0.0053(14) 0.0373(18)
S1 0.0291(4) 0.0250(3) 0.0374(4) 0.0060(3) 0.0025(3) 0.0086(3)
S2 0.0245(3) 0.0267(3) 0.0285(4) 0.0031(3) 0.0060(3) 0.0084(3)
O1 0.0395(12) 0.0302(11) 0.0528(14) 0.0052(10) 0.0129(11) 0.0168(10)
O2 0.0338(12) 0.0354(12) 0.0432(13) 0.0123(10) -0.0034(10) 0.0069(10)
O3 0.0372(12) 0.0340(11) 0.0397(12) 0.0041(9) 0.0194(10) 0.0147(9)
O4 0.0261(10) 0.0337(11) 0.0378(12) 0.0052(9) 0.0008(9) 0.0077(9)
O5 0.0296(11) 0.0319(11) 0.0351(11) 0.0006(9) 0.0081(9) 0.0106(9)
O6 0.0236(10) 0.0342(11) 0.0299(11) 0.0021(8) 0.0058(8) 0.0092(8)
O7 0.0394(12) 0.0297(11) 0.0328(11) 0.0040(8) 0.0082(9) 0.0185(9)
O8 0.0314(11) 0.0403(12) 0.0331(11) 0.0107(9) 0.0104(9) 0.0194(9)
N1 0.0290(12) 0.0226(11) 0.0270(12) 0.0021(9) 0.0025(10) 0.0065(10)
N2 0.0262(12) 0.0247(11) 0.0217(11) 0.0002(9) 0.0042(9) 0.0074(9)
C1 0.0304(15) 0.0236(13) 0.0323(15) 0.0049(11) 0.0025(12) 0.0077(12)
C2 0.0425(19) 0.0412(18) 0.0276(16) 0.0005(13) 0.0046(14) -0.0007(15)
C3 0.049(2) 0.0430(19) 0.0371(18) 0.0038(14) 0.0151(16) 0.0069(16)
C4 0.0346(16) 0.0280(15) 0.0463(19) 0.0090(13) 0.0080(14) 0.0131(13)
C5 0.0311(17) 0.0374(18) 0.056(2) -0.0141(16) 0.0000(15) 0.0052(14)
C6 0.0372(18) 0.0343(17) 0.053(2) -0.0142(15) 0.0070(16) 0.0083(14)
C7 0.0387(19) 0.047(2) 0.064(3) 0.0105(18) 0.0126(18) 0.0154(16)
C8 0.0266(14) 0.0267(14) 0.0290(15) 0.0003(11) 0.0040(11) 0.0062(11)
C9 0.0270(14) 0.0259(13) 0.0222(13) -0.0011(10) 0.0028(11) 0.0075(11)
C10 0.0247(13) 0.0259(13) 0.0202(13) -0.0030(10) 0.0013(10) 0.0081(11)
C11 0.0320(15) 0.0287(14) 0.0251(14) 0.0008(11) 0.0042(11) 0.0117(12)
C12 0.0330(15) 0.0358(16) 0.0310(15) 0.0016(12) 0.0056(12) 0.0178(13)
C13 0.0280(15) 0.0398(16) 0.0278(15) -0.0016(12) 0.0056(12) 0.0140(13)
C14 0.0283(14) 0.0304(14) 0.0240(14) -0.0009(11) 0.0057(11) 0.0086(12)
C15 0.0239(13) 0.0273(13) 0.0206(13) -0.0029(10) 0.0018(10) 0.0083(11)
C16 0.0243(13) 0.0271(13) 0.0209(13) -0.0013(10) 0.0023(10) 0.0080(11)
C17 0.0272(14) 0.0307(14) 0.0200(13) 0.0019(10) 0.0028(10) 0.0125(12)
C18 0.0226(13) 0.0305(14) 0.0239(13) -0.0006(11) 0.0040(11) 0.0079(11)
C19 0.0252(14) 0.0314(14) 0.0231(13) 0.0023(11) 0.0026(11) 0.0084(12)
C20 0.0255(14) 0.0303(14) 0.0291(14) 0.0060(11) 0.0079(11) 0.0088(11)
C21 0.0375(17) 0.0356(16) 0.0315(16) 0.0058(13) 0.0058(13) 0.0079(14)
C22 0.0403(18) 0.050(2) 0.0339(17) 0.0169(15) 0.0030(14) 0.0112(16)
C23 0.0299(16) 0.0422(18) 0.052(2) 0.0224(15) 0.0160(14) 0.0145(14)
C24 0.048(2) 0.0362(17) 0.048(2) 0.0109(15) 0.0178(16) 0.0195(15)
C25 0.0441(18) 0.0328(16) 0.0307(16) 0.0063(12) 0.0099(14) 0.0153(14)
C26 0.045(2) 0.057(2) 0.079(3) 0.042(2) 0.025(2) 0.0251(19)
C27 0.0380(16) 0.0247(13) 0.0261(14) 0.0016(11) 0.0102(12) 0.0121(12)
C28 0.0321(15) 0.0229(13) 0.0224(13) -0.0015(10) 0.0041(11) 0.0078(11)
C29 0.0322(15) 0.0247(13) 0.0190(13) -0.0015(10) 0.0033(11) 0.0092(11)
C30 0.0320(15) 0.0283(14) 0.0259(14) 0.0000(11) 0.0032(12) 0.0077(12)
C31 0.0293(15) 0.0356(16) 0.0336(16) 0.0015(13) 0.0021(12) 0.0110(13)
C32 0.0363(16) 0.0308(15) 0.0348(16) 0.0041(12) 0.0014(13) 0.0146(13)
C33 0.0339(15) 0.0257(14) 0.0293(15) 0.0043(11) 0.0021(12) 0.0099(12)
C34 0.0298(14) 0.0246(13) 0.0212(13) -0.0020(10) 0.0025(11) 0.0093(11)
C35 0.0329(15) 0.0236(13) 0.0211(13) 0.0015(10) 0.0045(11) 0.0091(11)
C36 0.0300(14) 0.0287(14) 0.0220(13) -0.0010(11) 0.0060(11) 0.0101(12)
C37 0.0343(15) 0.0245(13) 0.0223(13) -0.0010(10) 0.0055(11) 0.0112(12)
C38 0.0363(16) 0.0266(14) 0.0252(14) 0.0024(11) 0.0086(12) 0.0090(12)
C39 0.057(2) 0.0301(16) 0.0455(19) 0.0027(14) 0.0178(16) 0.0227(15)
C40 0.0329(16) 0.0376(17) 0.0405(17) 0.0061(13) 0.0115(13) 0.0181(13)
C41 0.0256(15) 0.055(2) 0.0417(19) -0.0116(16) -0.0010(14) 0.0088(15)
C42 0.0371(17) 0.0404(17) 0.0408(18) 0.0041(14) 0.0150(14) 0.0189(14)
C43 0.0413(19) 0.056(2) 0.051(2) 0.0059(17) 0.0161(16) 0.0255(17)
C44 0.0330(17) 0.0399(18) 0.054(2) 0.0101(15) 0.0135(15) 0.0132(14)
C45 0.047(2) 0.060(2) 0.087(3) 0.024(2) 0.026(2) 0.032(2)
C46 0.054(5) 0.062(5) 0.067(6) 0.009(4) 0.030(4) 0.008(4)

_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
Cl1 C43 1.758(4) . ?
Cl2 C43 1.762(4) . ?
Cl3 C43 1.750(4) . ?
Cl4 C44 1.721(4) . ?
Cl5 C44 1.741(4) . ?
Cl6 C44 1.756(4) . ?
Cl7 C45 1.744(4) . ?
Cl8 C45 1.741(5) . ?
Cl9 C45 1.721(5) . ?
Cl10 Cl11 1.668(6) . ?
Cl10 C46 1.741(11) . ?
Cl10 C46 2.077(11) 2_665 ?
Cl10 Cl12 2.112(6) 2_665 ?
Cl11 Cl12 1.277(5) . ?
Cl11 C46 1.291(10) . ?
Cl11 C46 1.720(11) 2_665 ?
Cl12 C46 1.715(10) . ?
Cl12 C46 1.856(10) 2_665 ?
Cl12 Cl10 2.112(6) 2_665 ?
S1 O2 1.434(2) . ?
S1 O1 1.439(2) . ?
S1 N1 1.644(2) . ?
S1 C1 1.760(3) . ?
S2 O3 1.431(2) . ?
S2 O4 1.433(2) . ?
S2 N2 1.641(2) . ?
S2 C20 1.766(3) . ?
O5 C36 1.380(4) . ?
O5 C42 1.433(4) . ?
O6 C18 1.391(3) . ?
O6 C41 1.436(4) . ?
O7 C37 1.384(4) . ?
O7 C39 1.444(4) . ?
O8 C17 1.374(3) . ?
O8 C40 1.444(4) . ?
N1 C38 1.492(4) . ?
N1 C8 1.494(4) . ?
N2 C27 1.488(3) . ?
N2 C19 1.494(3) . ?
C1 C2 1.378(5) . ?
C1 C6 1.386(4) . ?
C2 C3 1.392(5) . ?
C3 C4 1.376(5) . ?
C4 C5 1.386(5) . ?
C4 C7 1.507(5) . ?
C5 C6 1.382(5) . ?
C8 C9 1.510(4) . ?
C9 C18 1.374(4) . ?
C9 C10 1.432(4) . ?
C10 C15 1.422(4) . ?
C10 C11 1.425(4) . ?
C11 C12 1.370(4) . ?
C12 C13 1.404(5) . ?
C13 C14 1.372(4) . ?
C14 C15 1.422(4) . ?
C15 C16 1.436(4) . ?
C16 C17 1.377(4) . ?
C16 C19 1.512(4) . ?
C17 C18 1.425(4) . ?
C20 C25 1.382(4) . ?
C20 C21 1.387(4) . ?
C21 C22 1.384(5) . ?
C22 C23 1.391(5) . ?
C23 C24 1.384(5) . ?
C23 C26 1.510(5) . ?
C24 C25 1.395(5) . ?
C27 C28 1.515(4) . ?
C28 C37 1.371(4) . ?
C28 C29 1.433(4) . ?
C29 C30 1.418(4) . ?
C29 C34 1.431(4) . ?
C30 C31 1.374(4) . ?
C31 C32 1.402(5) . ?
C32 C33 1.371(5) . ?
C33 C34 1.416(4) . ?
C34 C35 1.436(4) . ?
C35 C36 1.376(4) . ?
C35 C38 1.515(4) . ?
C36 C37 1.427(4) . ?
C46 C46 1.078(17) 2_665 ?
C46 Cl11 1.720(11) 2_665 ?
C46 Cl12 1.856(10) 2_665 ?
C46 Cl10 2.077(11) 2_665 ?

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
Cl11 Cl10 C46 44.4(3) . . ?
Cl11 Cl10 C46 53.3(3) . 2_665 ?
C46 Cl10 C46 31.2(5) . 2_665 ?
Cl11 Cl10 Cl12 98.0(2) . 2_665 ?
C46 Cl10 Cl12 56.6(4) . 2_665 ?
C46 Cl10 Cl12 48.3(3) 2_665 2_665 ?
Cl12 Cl11 C46 83.8(6) . . ?
Cl12 Cl11 Cl10 150.3(3) . . ?
C46 Cl11 Cl10 70.8(5) . . ?
Cl12 Cl11 C46 74.9(4) . 2_665 ?
C46 Cl11 C46 38.8(6) . 2_665 ?
Cl10 Cl11 C46 75.6(4) . 2_665 ?
Cl11 Cl12 C46 48.4(4) . . ?
Cl11 Cl12 C46 63.5(4) . 2_665 ?
C46 Cl12 C46 34.9(5) . 2_665 ?
Cl11 Cl12 Cl10 111.0(3) . 2_665 ?
C46 Cl12 Cl10 64.8(4) . 2_665 ?
C46 Cl12 Cl10 51.5(4) 2_665 2_665 ?
O2 S1 O1 118.76(15) . . ?
O2 S1 N1 106.90(13) . . ?
O1 S1 N1 106.69(14) . . ?
O2 S1 C1 108.69(15) . . ?
O1 S1 C1 107.78(14) . . ?
N1 S1 C1 107.53(14) . . ?
O3 S2 O4 119.32(14) . . ?
O3 S2 N2 107.48(12) . . ?
O4 S2 N2 106.67(13) . . ?
O3 S2 C20 107.06(14) . . ?
O4 S2 C20 107.32(14) . . ?
N2 S2 C20 108.65(13) . . ?
C36 O5 C42 116.9(2) . . ?
C18 O6 C41 111.6(2) . . ?
C37 O7 C39 113.1(2) . . ?
C17 O8 C40 120.7(2) . . ?
C38 N1 C8 116.8(2) . . ?
C38 N1 S1 115.93(19) . . ?
C8 N1 S1 114.42(18) . . ?
C27 N2 C19 116.3(2) . . ?
C27 N2 S2 115.54(18) . . ?
C19 N2 S2 115.32(18) . . ?
C2 C1 C6 120.3(3) . . ?
C2 C1 S1 120.3(2) . . ?
C6 C1 S1 119.2(3) . . ?
C1 C2 C3 119.1(3) . . ?
C4 C3 C2 121.7(3) . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 C7 121.7(3) . . ?
C5 C4 C7 120.3(3) . . ?
C6 C5 C4 121.6(3) . . ?
C5 C6 C1 119.3(3) . . ?
N1 C8 C9 110.9(2) . . ?
C18 C9 C10 118.7(3) . . ?
C18 C9 C8 120.4(3) . . ?
C10 C9 C8 120.9(3) . . ?
C15 C10 C11 118.9(3) . . ?
C15 C10 C9 119.4(3) . . ?
C11 C10 C9 121.7(3) . . ?
C12 C11 C10 120.6(3) . . ?
C11 C12 C13 120.5(3) . . ?
C14 C13 C12 120.4(3) . . ?
C13 C14 C15 120.9(3) . . ?
C14 C15 C10 118.7(3) . . ?
C14 C15 C16 121.8(3) . . ?
C10 C15 C16 119.5(3) . . ?
C17 C16 C15 119.1(3) . . ?
C17 C16 C19 120.5(3) . . ?
C15 C16 C19 120.5(2) . . ?
O8 C17 C16 117.7(3) . . ?
O8 C17 C18 122.0(3) . . ?
C16 C17 C18 120.2(3) . . ?
C9 C18 O6 119.6(3) . . ?
C9 C18 C17 121.3(3) . . ?
O6 C18 C17 119.0(3) . . ?
N2 C19 C16 112.4(2) . . ?
C25 C20 C21 120.5(3) . . ?
C25 C20 S2 120.6(2) . . ?
C21 C20 S2 118.9(2) . . ?
C22 C21 C20 119.5(3) . . ?
C21 C22 C23 121.3(3) . . ?
C24 C23 C22 118.2(3) . . ?
C24 C23 C26 120.9(4) . . ?
C22 C23 C26 120.9(4) . . ?
C23 C24 C25 121.5(3) . . ?
C20 C25 C24 119.0(3) . . ?
N2 C27 C28 111.6(2) . . ?
C37 C28 C29 118.7(3) . . ?
C37 C28 C27 119.5(3) . . ?
C29 C28 C27 121.7(3) . . ?
C30 C29 C34 119.0(3) . . ?
C30 C29 C28 121.9(3) . . ?
C34 C29 C28 119.1(3) . . ?
C31 C30 C29 120.8(3) . . ?
C30 C31 C32 120.1(3) . . ?
C33 C32 C31 120.7(3) . . ?
C32 C33 C34 121.0(3) . . ?
C33 C34 C29 118.4(3) . . ?
C33 C34 C35 121.8(3) . . ?
C29 C34 C35 119.8(3) . . ?
C36 C35 C34 118.5(3) . . ?
C36 C35 C38 120.2(3) . . ?
C34 C35 C38 121.3(3) . . ?
C35 C36 O5 119.1(3) . . ?
C35 C36 C37 120.7(3) . . ?
O5 C36 C37 119.6(3) . . ?
C28 C37 O7 120.7(3) . . ?
C28 C37 C36 121.3(3) . . ?
O7 C37 C36 117.7(3) . . ?
N1 C38 C35 112.6(2) . . ?
Cl3 C43 Cl1 110.0(2) . . ?
Cl3 C43 Cl2 110.3(2) . . ?
Cl1 C43 Cl2 109.8(2) . . ?
Cl4 C44 Cl5 112.3(2) . . ?
Cl4 C44 Cl6 110.1(2) . . ?
Cl5 C44 Cl6 108.4(2) . . ?
Cl9 C45 Cl8 110.6(3) . . ?
Cl9 C45 Cl7 109.7(3) . . ?
Cl8 C45 Cl7 110.5(3) . . ?
C46 C46 Cl11 92.7(11) 2_665 . ?
C46 C46 Cl12 79.7(10) 2_665 . ?
Cl11 C46 Cl12 47.7(4) . . ?
C46 C46 Cl11 48.6(9) 2_665 2_665 ?
Cl11 C46 Cl11 141.2(6) . 2_665 ?
Cl12 C46 Cl11 113.1(6) . 2_665 ?
C46 C46 Cl10 91.9(12) 2_665 . ?
Cl11 C46 Cl10 64.8(5) . . ?
Cl12 C46 Cl10 111.0(6) . . ?
Cl11 C46 Cl10 109.9(6) 2_665 . ?
C46 C46 Cl12 65.4(10) 2_665 2_665 ?
Cl11 C46 Cl12 130.4(7) . 2_665 ?
Cl12 C46 Cl12 145.1(5) . 2_665 ?
Cl11 C46 Cl12 41.6(3) 2_665 2_665 ?
Cl10 C46 Cl12 71.8(4) . 2_665 ?
C46 C46 Cl10 56.9(10) 2_665 2_665 ?
Cl11 C46 Cl10 112.4(6) . 2_665 ?
Cl12 C46 Cl10 66.9(4) . 2_665 ?
Cl11 C46 Cl10 51.0(4) 2_665 2_665 ?
Cl10 C46 Cl10 148.8(5) . 2_665 ?
Cl12 C46 Cl10 92.6(5) 2_665 2_665 ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.077