# Electronic Supplementary Material (ESI) for ChemComm.
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#                                CCDC 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_MeO3-111-1_5DCE

_vrf_PLAT410_MeO3-111-1_5DCE     
;
RESPONSE:
H22A is a calculated hydrogen on a disordered methylene bridge 
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H48 Cl3 O9'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         911.24

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'
Cl Cl 0.1484 0.1585 '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_int_tables_number      14
_chemical_absolute_configuration ?

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                   19.8657(19)
_cell_length_b                   10.6594(10)
_cell_length_c                   21.676(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.9410(10)
_cell_angle_gamma                90.00
_cell_volume                     4314.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    37575
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      25.86
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1908
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6547
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART, Bruker APEXII CCD'
_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            26613
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.09
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7599
_reflns_number_gt                5453
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, L.Barbour (1999); http://x-seed.net/'
_computing_publication_material  'X-SEED, L.Barbour (1999); http://x-seed.net/'

_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)+(0.0612P)²+2.1526P] 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         7599
_refine_ls_number_parameters     627
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1135
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
C22B C -0.0050(9) 0.6841(15) 0.0458(7) 0.0249(13) Uani 0.35 1 d P A 2
H22A H 0.0232 0.6149 0.0363 0.030 Uiso 0.35 1 calc PR A 2
H22B H -0.0535 0.6525 0.0407 0.030 Uiso 0.35 1 calc PR A 2
Cl3S Cl 0.40473(4) 1.11341(6) -0.03216(4) 0.03123(18) Uani 1 1 d . . .
O1A O 0.35299(9) 0.86063(15) 0.32050(8) 0.0208(4) Uani 1 1 d . . .
O2A O 0.45494(9) 0.75258(15) 0.31139(8) 0.0198(4) Uani 1 1 d . . .
O3A O 0.33542(9) 0.38363(17) -0.01378(8) 0.0253(4) Uani 1 1 d . . .
O4A O 0.40832(10) 0.54857(15) -0.02243(8) 0.0227(4) Uani 1 1 d . . .
O8A O 0.50241(10) 0.62157(17) 0.09516(9) 0.0278(4) Uani 1 1 d . . .
O9 O 0.21915(10) 0.93962(18) 0.29120(9) 0.0323(5) Uani 1 1 d . . .
C8A C 0.36681(13) 0.8748(2) 0.06596(12) 0.0164(5) Uani 1 1 d . . .
C40A C 0.42447(13) 0.6350(2) 0.29428(12) 0.0174(5) Uani 1 1 d . . .
C13A C 0.31999(13) 0.8374(2) 0.00459(12) 0.0171(5) Uani 1 1 d . . .
O5A O 0.03491(10) 0.7389(2) 0.12070(10) 0.0433(6) Uani 0.65 1 d P A 1
C6A C 0.31585(13) 0.9728(2) 0.14862(12) 0.0173(5) Uani 1 1 d . . .
C42A C 0.33283(13) 0.4764(2) 0.27871(12) 0.0178(5) Uani 1 1 d . . .
C33A C 0.29915(14) 0.3753(2) 0.03047(12) 0.0229(6) Uani 1 1 d . . .
C1A C 0.35436(13) 0.9261(2) 0.21134(12) 0.0168(5) Uani 1 1 d . . .
H1A H 0.4034 0.9043 0.2217 0.020 Uiso 1 1 calc R . .
C12A C 0.33480(13) 0.7259(2) -0.02269(12) 0.0184(5) Uani 1 1 d . . .
H12A H 0.3031 0.6995 -0.0643 0.022 Uiso 1 1 calc R . .
C10A C 0.44238(13) 0.6933(2) 0.06922(12) 0.0175(5) Uani 1 1 d . . .
C2A C 0.32225(13) 0.9111(2) 0.25845(12) 0.0179(5) Uani 1 1 d . . .
C35A C 0.29075(14) 0.3197(2) 0.13579(12) 0.0217(6) Uani 1 1 d . . .
C38A C 0.42999(13) 0.4437(2) 0.23882(12) 0.0206(6) Uani 1 1 d . . .
H38A H 0.4545 0.3911 0.2181 0.025 Uiso 1 1 calc R . .
C34A C 0.32985(14) 0.3290(2) 0.09305(13) 0.0216(6) Uani 1 1 d . . .
H34A H 0.3785 0.3028 0.1076 0.026 Uiso 1 1 calc R . .
C5A C 0.24282(13) 1.0014(2) 0.13267(12) 0.0201(6) Uani 1 1 d . . .
C43A C 0.26265(13) 0.4421(2) 0.28837(12) 0.0206(6) Uani 1 1 d . . .
H43A H 0.2544 0.3508 0.2814 0.025 Uiso 1 1 calc R . .
H43B H 0.2665 0.4610 0.3342 0.025 Uiso 1 1 calc R . .
C41A C 0.36343(13) 0.5919(2) 0.30440(12) 0.0188(5) Uani 1 1 d . . .
H41A H 0.3419 0.6413 0.3291 0.023 Uiso 1 1 calc R . .
C7A C 0.35613(13) 0.9927(2) 0.10094(12) 0.0179(5) Uani 1 1 d . . .
H7A1 H 0.3297 1.0548 0.0675 0.021 Uiso 1 1 calc R A .
H7A2 H 0.4037 1.0289 0.1253 0.021 Uiso 1 1 calc R . .
C37A C 0.36539(13) 0.4017(2) 0.24415(12) 0.0191(5) Uani 1 1 d . . .
C21B C 0.198(3) 1.051(5) 0.062(3) 0.021(2) Uani 0.35 1 d P A 2
H21A H 0.1637 1.1163 0.0652 0.025 Uiso 0.35 1 calc PR A 2
H21B H 0.2299 1.0873 0.0406 0.025 Uiso 0.35 1 calc PR A 2
C14B C 0.250(3) 0.903(6) -0.031(3) 0.015(2) Uani 0.35 1 d P A 2
H14A H 0.2599 0.9946 -0.0249 0.018 Uiso 0.35 1 calc PR A 2
H14B H 0.2382 0.8856 -0.0780 0.018 Uiso 0.35 1 calc PR A 2
C15A C 0.1891(10) 0.8618(17) -0.0244(8) 0.012(2) Uani 0.65 1 d P A 1
C11A C 0.39389(13) 0.6538(2) 0.00902(12) 0.0187(5) Uani 1 1 d . . .
C39A C 0.45932(13) 0.5588(2) 0.26254(12) 0.0195(6) Uani 1 1 d . . .
H39A H 0.5027 0.5856 0.2573 0.023 Uiso 1 1 calc R . .
C26A C 0.19902(13) 0.5125(2) 0.24186(12) 0.0217(6) Uani 1 1 d . . .
C4A C 0.21266(13) 0.9903(2) 0.18191(13) 0.0215(6) Uani 1 1 d . A .
H4A H 0.1639 1.0131 0.1723 0.026 Uiso 1 1 calc R . .
C9A C 0.42797(13) 0.8024(2) 0.09706(12) 0.0182(5) Uani 1 1 d . . .
H9A H 0.4604 0.8289 0.1384 0.022 Uiso 1 1 calc R A .
C16A C 0.1529(7) 0.7538(12) -0.0575(6) 0.0172(19) Uani 0.65 1 d P A 1
H16A H 0.1680 0.7200 -0.0912 0.021 Uiso 0.65 1 calc PR A 1
C27A C 0.15616(13) 0.4646(3) 0.18078(13) 0.0237(6) Uani 1 1 d . . .
C24A C 0.12842(14) 0.7042(3) 0.21876(14) 0.0291(7) Uani 1 1 d . A .
H24A H 0.1193 0.7856 0.2320 0.035 Uiso 1 1 calc R . .
C25A C 0.18257(14) 0.6323(2) 0.25928(14) 0.0256(6) Uani 1 1 d . . .
H25A H 0.2102 0.6649 0.3010 0.031 Uiso 1 1 calc R . .
C3A C 0.25085(13) 0.9478(2) 0.24362(12) 0.0186(5) Uani 1 1 d . . .
C45A C 0.40661(14) 0.4318(2) 0.00857(13) 0.0220(6) Uani 1 1 d . . .
H45A H 0.4232 0.4433 0.0568 0.026 Uiso 1 1 calc R A .
H45B H 0.4391 0.3716 -0.0018 0.026 Uiso 1 1 calc R . .
C36A C 0.33204(14) 0.2838(2) 0.20654(12) 0.0225(6) Uani 1 1 d . . .
H36A H 0.3699 0.2224 0.2080 0.027 Uiso 1 1 calc R . .
H36B H 0.2993 0.2448 0.2267 0.027 Uiso 1 1 calc R . .
C14A C 0.2555(18) 0.915(3) -0.0359(14) 0.015(2) Uani 0.65 1 d P A 1
H14C H 0.2497 0.9107 -0.0831 0.018 Uiso 0.65 1 calc PR A 1
H14D H 0.2624 1.0044 -0.0221 0.018 Uiso 0.65 1 calc PR A 1
C44A C 0.42715(13) 0.8358(2) 0.34762(13) 0.0222(6) Uani 1 1 d . . .
H44A H 0.4373 0.8005 0.3921 0.027 Uiso 1 1 calc R . .
H44B H 0.4532 0.9164 0.3525 0.027 Uiso 1 1 calc R . .
C30A C 0.21794(14) 0.3506(3) 0.11310(13) 0.0266(6) Uani 1 1 d . . .
O7B O 0.0394(4) 0.6427(8) -0.0764(5) 0.042(2) Uani 0.35 1 d P A 2
C21A C 0.1926(16) 1.032(2) 0.0653(16) 0.021(2) Uani 0.65 1 d P A 1
H21C H 0.2184 1.0841 0.0427 0.025 Uiso 0.65 1 calc PR A 1
H21D H 0.1528 1.0833 0.0694 0.025 Uiso 0.65 1 calc PR A 1
C20A C 0.1600(5) 0.9136(5) 0.0210(4) 0.0152(13) Uani 0.65 1 d PU A 1
O6A O 0.02213(14) 0.6734(3) 0.01520(13) 0.0199(6) Uani 0.65 1 d P A 1
C46A C 0.55992(15) 0.6748(3) 0.14811(14) 0.0303(7) Uani 1 1 d . . .
H46A H 0.5735 0.7558 0.1344 0.045 Uiso 1 1 calc R . .
H46B H 0.6011 0.6179 0.1601 0.045 Uiso 1 1 calc R . .
H46C H 0.5445 0.6872 0.1860 0.045 Uiso 1 1 calc R . .
C3S C 0.46691(14) 0.9895(2) -0.02915(13) 0.0256(6) Uani 1 1 d . . .
H3S1 H 0.4454 0.9074 -0.0253 0.031 Uiso 1 1 calc R . .
H3S2 H 0.4790 0.9893 -0.0698 0.031 Uiso 1 1 calc R . .
C28A C 0.09975(14) 0.5368(3) 0.14016(14) 0.0302(7) Uani 1 1 d . A .
H28A H 0.0696 0.5031 0.0996 0.036 Uiso 1 1 calc R . .
C29A C 0.16984(15) 0.3391(3) 0.15449(14) 0.0293(7) Uani 1 1 d . . .
H29A H 0.1235 0.3017 0.1275 0.035 Uiso 1 1 calc R . .
H29B H 0.1925 0.2818 0.1918 0.035 Uiso 1 1 calc R . .
C23A C 0.08708(14) 0.6568(3) 0.15815(14) 0.0292(7) Uani 1 1 d . . .
C31A C 0.18789(16) 0.3956(3) 0.04913(14) 0.0392(8) Uani 1 1 d . . .
H31A H 0.1386 0.4177 0.0332 0.047 Uiso 1 1 calc R . .
C32A C 0.22762(16) 0.4091(3) 0.00813(14) 0.0379(8) Uani 1 1 d . . .
H32A H 0.2060 0.4413 -0.0350 0.046 Uiso 1 1 calc R . .
C18A C 0.0743(2) 0.7439(4) 0.0028(2) 0.0186(9) Uani 0.65 1 d P A 1
C17A C 0.0995(3) 0.6958(4) -0.0453(3) 0.0175(11) Uani 0.65 1 d P A 1
C19A C 0.1045(3) 0.8537(4) 0.0348(3) 0.0201(11) Uani 0.65 1 d P A 1
H19A H 0.0869 0.8887 0.0667 0.024 Uiso 0.65 1 calc PR A 1
C48B C 0.0585(11) 0.588(2) -0.1271(10) 0.0329(15) Uani 0.35 1 d P A 2
H48A H 0.0635 0.6540 -0.1568 0.049 Uiso 0.35 1 calc PR A 2
H48B H 0.0211 0.5290 -0.1515 0.049 Uiso 0.35 1 calc PR A 2
H48C H 0.1040 0.5435 -0.1083 0.049 Uiso 0.35 1 calc PR A 2
C22A C -0.0113(4) 0.7145(7) 0.0618(3) 0.0249(13) Uani 0.65 1 d P A 1
H22C H -0.0398 0.7909 0.0445 0.030 Uiso 0.65 1 calc PR A 1
H22D H -0.0446 0.6484 0.0657 0.030 Uiso 0.65 1 calc PR A 1
C47A C 0.2382(2) 1.0426(3) 0.33626(17) 0.0550(10) Uani 1 1 d . . .
H47A H 0.2903 1.0441 0.3582 0.083 Uiso 1 1 calc R A .
H47B H 0.2148 1.0328 0.3691 0.083 Uiso 1 1 calc R . .
H47C H 0.2226 1.1214 0.3123 0.083 Uiso 1 1 calc R . .
Cl1S Cl -0.13539(4) 0.82285(9) 0.13210(5) 0.0522(2) Uani 1 1 d . B 2
Cl2S Cl 0.03519(5) 1.09007(10) 0.21134(5) 0.0617(3) Uani 1 1 d . . .
C1S C -0.06115(17) 0.9033(4) 0.18998(17) 0.0484(9) Uani 1 1 d . . .
H1S1 H -0.0757 0.9396 0.2256 0.058 Uiso 1 1 calc R B 2
H1S2 H -0.0213 0.8440 0.2098 0.058 Uiso 1 1 calc R B 2
C2S C -0.0378(2) 1.0044(4) 0.1548(2) 0.0620(11) Uani 1 1 d . B .
H2S1 H -0.0783 1.0620 0.1340 0.074 Uiso 1 1 calc R . .
H2S2 H -0.0225 0.9675 0.1198 0.074 Uiso 1 1 calc R . .
O6B O -0.0088(3) 0.7814(6) 0.0058(3) 0.0388(15) Uani 0.35 1 d P A 2
C17B C 0.0821(6) 0.7378(10) -0.0442(7) 0.0175(11) Uani 0.35 1 d P A 2
C18B C 0.0583(5) 0.8064(8) -0.0004(4) 0.0186(9) Uani 0.35 1 d P A 2
C19B C 0.0942(7) 0.9051(9) 0.0318(6) 0.0201(11) Uani 0.35 1 d P A 2
H19B H 0.0741 0.9509 0.0589 0.024 Uiso 0.35 1 calc PR A 2
C20B C 0.1619(11) 0.9472(12) 0.0281(9) 0.0152(13) Uani 0.35 1 d PU A 2
C15B C 0.183(2) 0.879(4) -0.0146(18) 0.012(2) Uani 0.35 1 d P A 2
C16B C 0.1516(18) 0.780(2) -0.0521(14) 0.031(7) Uani 0.35 1 d PU A 2
H16B H 0.1714 0.7396 -0.0811 0.037 Uiso 0.35 1 calc PR A 2
O7A O 0.0646(2) 0.5924(4) -0.0774(2) 0.0287(9) Uani 0.65 1 d P A 1
C48A C 0.0673(5) 0.5702(10) -0.1427(4) 0.0329(15) Uani 0.65 1 d P A 1
H48D H 0.0509 0.6454 -0.1696 0.049 Uiso 0.65 1 calc PR A 1
H48E H 0.0361 0.4994 -0.1629 0.049 Uiso 0.65 1 calc PR A 1
H48F H 0.1166 0.5510 -0.1395 0.049 Uiso 0.65 1 calc PR A 1
O5B O 0.03491(10) 0.7389(2) 0.12070(10) 0.0433(6) Uani 0.35 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C22B O6B 1.337(18) . ?
C22B H22A 0.9900 . ?
C22B H22B 0.9900 . ?
Cl3S C3S 1.795(3) . ?
O1A C2A 1.383(3) . ?
O1A C44A 1.413(3) . ?
O2A C40A 1.386(3) . ?
O2A C44A 1.415(3) . ?
O3A C33A 1.385(3) . ?
O3A C45A 1.425(3) . ?
O4A C11A 1.393(3) . ?
O4A C45A 1.420(3) . ?
O8A C10A 1.366(3) . ?
O8A C46A 1.432(3) . ?
O9 C3A 1.382(3) . ?
O9 C47A 1.432(4) . ?
C8A C13A 1.396(3) . ?
C8A C9A 1.403(3) . ?
C8A C7A 1.519(3) . ?
C40A C41A 1.382(3) . ?
C40A C39A 1.392(3) . ?
C13A C12A 1.403(3) . ?
C13A C14B 1.51(7) . ?
C13A C14A 1.53(4) . ?
O5A C22A 1.319(7) . ?
O5A C23A 1.387(3) . ?
C6A C1A 1.404(3) . ?
C6A C5A 1.406(3) . ?
C6A C7A 1.522(3) . ?
C42A C37A 1.394(3) . ?
C42A C41A 1.401(3) . ?
C42A C43A 1.523(3) . ?
C33A C34A 1.375(4) . ?
C33A C32A 1.384(4) . ?
C1A C2A 1.385(3) . ?
C1A H1A 0.9500 . ?
C12A C11A 1.375(3) . ?
C12A H12A 0.9500 . ?
C10A C9A 1.384(3) . ?
C10A C11A 1.397(3) . ?
C2A C3A 1.399(3) . ?
C35A C30A 1.399(4) . ?
C35A C34A 1.401(4) . ?
C35A C36A 1.521(4) . ?
C38A C39A 1.380(4) . ?
C38A C37A 1.401(3) . ?
C38A H38A 0.9500 . ?
C34A H34A 0.9500 . ?
C5A C4A 1.396(4) . ?
C5A C21A 1.50(3) . ?
C5A C21B 1.57(6) . ?
C43A C26A 1.519(4) . ?
C43A H43A 0.9900 . ?
C43A H43B 0.9900 . ?
C41A H41A 0.9500 . ?
C7A H7A1 0.9900 . ?
C7A H7A2 0.9900 . ?
C37A C36A 1.522(3) . ?
C21B C20B 1.39(6) . ?
C21B H21A 0.9900 . ?
C21B H21B 0.9900 . ?
C14B C15B 1.51(6) . ?
C14B H14A 0.9900 . ?
C14B H14B 0.9900 . ?
C15A C20A 1.412(13) . ?
C15A C16A 1.42(2) . ?
C15A C14A 1.53(3) . ?
C39A H39A 0.9500 . ?
C26A C25A 1.401(4) . ?
C26A C27A 1.403(4) . ?
C4A C3A 1.371(4) . ?
C4A H4A 0.9500 . ?
C9A H9A 0.9500 . ?
C16A C17A 1.328(16) . ?
C16A H16A 0.9500 . ?
C27A C28A 1.396(4) . ?
C27A C29A 1.515(4) . ?
C24A C25A 1.369(4) . ?
C24A C23A 1.385(4) . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C44A H44A 0.9900 . ?
C44A H44B 0.9900 . ?
C30A C31A 1.395(4) . ?
C30A C29A 1.523(4) . ?
O7B C17B 1.353(16) . ?
O7B C48B 1.403(15) . ?
C21A C20A 1.59(3) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C20A C19A 1.393(12) . ?
O6A C18A 1.379(5) . ?
O6A C22A 1.452(5) . ?
C46A H46A 0.9800 . ?
C46A H46B 0.9800 . ?
C46A H46C 0.9800 . ?
C3S C3S 1.497(5) 3_675 ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C28A C23A 1.386(4) . ?
C28A H28A 0.9500 . ?
C29A H29A 0.9900 . ?
C29A H29B 0.9900 . ?
C31A C32A 1.383(4) . ?
C31A H31A 0.9500 . ?
C32A H32A 0.9500 . ?
C18A C19A 1.388(7) . ?
C18A C17A 1.400(7) . ?
C17A O7A 1.361(7) . ?
C19A H19A 0.9500 . ?
C48B H48A 0.9800 . ?
C48B H48B 0.9800 . ?
C48B H48C 0.9800 . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C47A H47A 0.9800 . ?
C47A H47B 0.9800 . ?
C47A H47C 0.9800 . ?
Cl1S C1S 1.795(4) . ?
Cl2S C2S 1.796(4) . ?
C1S C2S 1.483(5) . ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
O6B C18B 1.410(10) . ?
C17B C18B 1.402(15) . ?
C17B C16B 1.52(4) . ?
C18B C19B 1.328(15) . ?
C19B C20B 1.45(3) . ?
C19B H19B 0.9500 . ?
C20B C15B 1.35(3) . ?
C15B C16B 1.35(4) . ?
C16B H16B 0.9500 . ?
O7A C48A 1.453(7) . ?
C48A H48D 0.9800 . ?
C48A H48E 0.9800 . ?
C48A H48F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6B C22B H22A 110.7 . . ?
O6B C22B H22B 110.7 . . ?
H22A C22B H22B 108.8 . . ?
C2A O1A C44A 121.99(19) . . ?
C40A O2A C44A 119.83(19) . . ?
C33A O3A C45A 118.56(19) . . ?
C11A O4A C45A 115.61(18) . . ?
C10A O8A C46A 117.0(2) . . ?
C3A O9 C47A 112.3(2) . . ?
C13A C8A C9A 119.1(2) . . ?
C13A C8A C7A 123.4(2) . . ?
C9A C8A C7A 117.4(2) . . ?
C41A C40A O2A 125.8(2) . . ?
C41A C40A C39A 119.7(2) . . ?
O2A C40A C39A 114.5(2) . . ?
C8A C13A C12A 118.4(2) . . ?
C8A C13A C14B 123(2) . . ?
C12A C13A C14B 118(2) . . ?
C8A C13A C14A 123.2(12) . . ?
C12A C13A C14A 118.3(12) . . ?
C14B C13A C14A 8(2) . . ?
C22A O5A C23A 125.2(4) . . ?
C1A C6A C5A 119.4(2) . . ?
C1A C6A C7A 117.9(2) . . ?
C5A C6A C7A 122.7(2) . . ?
C37A C42A C41A 119.8(2) . . ?
C37A C42A C43A 123.4(2) . . ?
C41A C42A C43A 116.7(2) . . ?
C34A C33A C32A 119.7(2) . . ?
C34A C33A O3A 123.1(2) . . ?
C32A C33A O3A 117.1(2) . . ?
C2A C1A C6A 121.2(2) . . ?
C2A C1A H1A 119.4 . . ?
C6A C1A H1A 119.4 . . ?
C11A C12A C13A 121.9(2) . . ?
C11A C12A H12A 119.0 . . ?
C13A C12A H12A 119.0 . . ?
O8A C10A C9A 124.9(2) . . ?
O8A C10A C11A 116.3(2) . . ?
C9A C10A C11A 118.8(2) . . ?
O1A C2A C1A 126.9(2) . . ?
O1A C2A C3A 114.1(2) . . ?
C1A C2A C3A 119.0(2) . . ?
C30A C35A C34A 119.4(2) . . ?
C30A C35A C36A 123.4(2) . . ?
C34A C35A C36A 117.0(2) . . ?
C39A C38A C37A 122.4(2) . . ?
C39A C38A H38A 118.8 . . ?
C37A C38A H38A 118.8 . . ?
C33A C34A C35A 121.2(2) . . ?
C33A C34A H34A 119.4 . . ?
C35A C34A H34A 119.4 . . ?
C4A C5A C6A 118.0(2) . . ?
C4A C5A C21A 116.6(11) . . ?
C6A C5A C21A 125.1(12) . . ?
C4A C5A C21B 121(2) . . ?
C6A C5A C21B 121(2) . . ?
C21A C5A C21B 9(2) . . ?
C26A C43A C42A 112.5(2) . . ?
C26A C43A H43A 109.1 . . ?
C42A C43A H43A 109.1 . . ?
C26A C43A H43B 109.1 . . ?
C42A C43A H43B 109.1 . . ?
H43A C43A H43B 107.8 . . ?
C40A C41A C42A 120.9(2) . . ?
C40A C41A H41A 119.5 . . ?
C42A C41A H41A 119.5 . . ?
C8A C7A C6A 114.75(19) . . ?
C8A C7A H7A1 108.6 . . ?
C6A C7A H7A1 108.6 . . ?
C8A C7A H7A2 108.6 . . ?
C6A C7A H7A2 108.6 . . ?
H7A1 C7A H7A2 107.6 . . ?
C42A C37A C38A 117.9(2) . . ?
C42A C37A C36A 124.2(2) . . ?
C38A C37A C36A 117.6(2) . . ?
C20B C21B C5A 106(3) . . ?
C20B C21B H21A 110.6 . . ?
C5A C21B H21A 110.6 . . ?
C20B C21B H21B 110.6 . . ?
C5A C21B H21B 110.6 . . ?
H21A C21B H21B 108.8 . . ?
C15B C14B C13A 122(4) . . ?
C15B C14B H14A 106.8 . . ?
C13A C14B H14A 106.8 . . ?
C15B C14B H14B 106.8 . . ?
C13A C14B H14B 106.8 . . ?
H14A C14B H14B 106.6 . . ?
C20A C15A C16A 114.4(14) . . ?
C20A C15A C14A 123.1(18) . . ?
C16A C15A C14A 122.5(15) . . ?
C12A C11A O4A 119.3(2) . . ?
C12A C11A C10A 119.9(2) . . ?
O4A C11A C10A 120.6(2) . . ?
C38A C39A C40A 119.0(2) . . ?
C38A C39A H39A 120.5 . . ?
C40A C39A H39A 120.5 . . ?
C25A C26A C27A 117.6(2) . . ?
C25A C26A C43A 119.3(2) . . ?
C27A C26A C43A 123.1(2) . . ?
C3A C4A C5A 122.4(2) . . ?
C3A C4A H4A 118.8 . . ?
C5A C4A H4A 118.8 . . ?
C10A C9A C8A 121.8(2) . . ?
C10A C9A H9A 119.1 . . ?
C8A C9A H9A 119.1 . . ?
C17A C16A C15A 125.4(13) . . ?
C17A C16A H16A 117.3 . . ?
C15A C16A H16A 117.3 . . ?
C28A C27A C26A 119.5(3) . . ?
C28A C27A C29A 117.3(2) . . ?
C26A C27A C29A 123.2(2) . . ?
C25A C24A C23A 119.1(3) . . ?
C25A C24A H24A 120.5 . . ?
C23A C24A H24A 120.5 . . ?
C24A C25A C26A 122.8(3) . . ?
C24A C25A H25A 118.6 . . ?
C26A C25A H25A 118.6 . . ?
C4A C3A O9 120.5(2) . . ?
C4A C3A C2A 119.8(2) . . ?
O9 C3A C2A 119.7(2) . . ?
O4A C45A O3A 109.6(2) . . ?
O4A C45A H45A 109.7 . . ?
O3A C45A H45A 109.7 . . ?
O4A C45A H45B 109.7 . . ?
O3A C45A H45B 109.7 . . ?
H45A C45A H45B 108.2 . . ?
C35A C36A C37A 108.6(2) . . ?
C35A C36A H36A 110.0 . . ?
C37A C36A H36A 110.0 . . ?
C35A C36A H36B 110.0 . . ?
C37A C36A H36B 110.0 . . ?
H36A C36A H36B 108.4 . . ?
C13A C14A C15A 107.6(16) . . ?
C13A C14A H14C 110.2 . . ?
C15A C14A H14C 110.2 . . ?
C13A C14A H14D 110.2 . . ?
C15A C14A H14D 110.2 . . ?
H14C C14A H14D 108.5 . . ?
O1A C44A O2A 115.8(2) . . ?
O1A C44A H44A 108.3 . . ?
O2A C44A H44A 108.3 . . ?
O1A C44A H44B 108.3 . . ?
O2A C44A H44B 108.3 . . ?
H44A C44A H44B 107.4 . . ?
C31A C30A C35A 118.1(3) . . ?
C31A C30A C29A 118.1(2) . . ?
C35A C30A C29A 123.7(2) . . ?
C17B O7B C48B 115.2(12) . . ?
C5A C21A C20A 114.5(16) . . ?
C5A C21A H21C 108.6 . . ?
C20A C21A H21C 108.6 . . ?
C5A C21A H21D 108.6 . . ?
C20A C21A H21D 108.6 . . ?
H21C C21A H21D 107.6 . . ?
C19A C20A C15A 120.8(10) . . ?
C19A C20A C21A 115.1(12) . . ?
C15A C20A C21A 123.7(15) . . ?
C18A O6A C22A 121.6(4) . . ?
O8A C46A H46A 109.5 . . ?
O8A C46A H46B 109.5 . . ?
H46A C46A H46B 109.5 . . ?
O8A C46A H46C 109.5 . . ?
H46A C46A H46C 109.5 . . ?
H46B C46A H46C 109.5 . . ?
C3S C3S Cl3S 108.4(2) 3_675 . ?
C3S C3S H3S1 110.0 3_675 . ?
Cl3S C3S H3S1 110.0 . . ?
C3S C3S H3S2 110.0 3_675 . ?
Cl3S C3S H3S2 110.0 . . ?
H3S1 C3S H3S2 108.4 . . ?
C23A C28A C27A 121.0(3) . . ?
C23A C28A H28A 119.5 . . ?
C27A C28A H28A 119.5 . . ?
C27A C29A C30A 112.3(2) . . ?
C27A C29A H29A 109.1 . . ?
C30A C29A H29A 109.1 . . ?
C27A C29A H29B 109.1 . . ?
C30A C29A H29B 109.1 . . ?
H29A C29A H29B 107.9 . . ?
C24A C23A C28A 119.9(3) . . ?
C24A C23A O5A 114.1(3) . . ?
C28A C23A O5A 126.1(3) . . ?
C32A C31A C30A 122.0(3) . . ?
C32A C31A H31A 119.0 . . ?
C30A C31A H31A 119.0 . . ?
C31A C32A C33A 119.4(3) . . ?
C31A C32A H32A 120.3 . . ?
C33A C32A H32A 120.3 . . ?
O6A C18A C19A 125.9(4) . . ?
O6A C18A C17A 115.5(4) . . ?
C19A C18A C17A 118.6(5) . . ?
C16A C17A O7A 125.3(8) . . ?
C16A C17A C18A 119.4(8) . . ?
O7A C17A C18A 115.3(5) . . ?
C18A C19A C20A 121.1(5) . . ?
C18A C19A H19A 119.4 . . ?
C20A C19A H19A 119.4 . . ?
O7B C48B H48A 109.5 . . ?
O7B C48B H48B 109.5 . . ?
H48A C48B H48B 109.5 . . ?
O7B C48B H48C 109.5 . . ?
H48A C48B H48C 109.5 . . ?
H48B C48B H48C 109.5 . . ?
O5A C22A O6A 113.6(5) . . ?
O5A C22A H22C 108.8 . . ?
O6A C22A H22C 108.8 . . ?
O5A C22A H22D 108.8 . . ?
O6A C22A H22D 108.8 . . ?
H22C C22A H22D 107.7 . . ?
O9 C47A H47A 109.5 . . ?
O9 C47A H47B 109.5 . . ?
H47A C47A H47B 109.5 . . ?
O9 C47A H47C 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C2S C1S Cl1S 108.3(3) . . ?
C2S C1S H1S1 110.0 . . ?
Cl1S C1S H1S1 110.0 . . ?
C2S C1S H1S2 110.0 . . ?
Cl1S C1S H1S2 110.0 . . ?
H1S1 C1S H1S2 108.4 . . ?
C1S C2S Cl2S 109.9(3) . . ?
C1S C2S H2S1 109.7 . . ?
Cl2S C2S H2S1 109.7 . . ?
C1S C2S H2S2 109.7 . . ?
Cl2S C2S H2S2 109.7 . . ?
H2S1 C2S H2S2 108.2 . . ?
C22B O6B C18B 111.2(9) . . ?
O7B C17B C18B 116.3(10) . . ?
O7B C17B C16B 126.7(14) . . ?
C18B C17B C16B 116.9(13) . . ?
C19B C18B C17B 121.6(10) . . ?
C19B C18B O6B 117.1(9) . . ?
C17B C18B O6B 120.9(9) . . ?
C18B C19B C20B 124.0(11) . . ?
C18B C19B H19B 118.0 . . ?
C20B C19B H19B 118.0 . . ?
C15B C20B C21B 125(3) . . ?
C15B C20B C19B 113(2) . . ?
C21B C20B C19B 123(3) . . ?
C20B C15B C16B 130(3) . . ?
C20B C15B C14B 125(4) . . ?
C16B C15B C14B 105(3) . . ?
C15B C16B C17B 115(3) . . ?
C15B C16B H16B 122.7 . . ?
C17B C16B H16B 122.7 . . ?
C17A O7A C48A 116.5(5) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 935199'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1.5-MeOs-111-NO2Me

_vrf_PLAT097_1.5-MeOs-111-NO2Me  
;
RESPONSE:
This electron density is in close proximity to a molecule of 57 non-hydrogen atoms 
that is disordered in two positions. The small residual electron density may correspond to
small unaccounted disorder which would be diffcult to model.
;
_vrf_DIFMX01_1.5-MeOs-111-NO2Me  
;
RESPONSE:
This electron density is in close proximity to a molecule of 57 non-hydrogen atoms 
that is disordered in two positions. The small residual electron density may correspond to
small unaccounted disorder which would be diffcult to model. 
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '1.5(C48 H42 O9), N1 O2 C1 H3'
_chemical_formula_sum            'C73 H66 N O15.50'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane'
_chemical_melting_point          ?

_exptl_crystal_description       cube
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1205.27

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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                   10.5024(14)
_cell_length_b                   29.658(4)
_cell_length_c                   19.900(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.954(2)
_cell_angle_gamma                90.00
_cell_volume                     6040.7(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    71733
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      27.42
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2540
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6393
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART, Bruker APEXII CCD'
_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            53038
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         28.00
_reflns_number_total             14414
_reflns_number_gt                9931
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, L.Barbour (1999); http://x-seed.net/'
_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)+(0.0650P)²+1.3982P] 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         14414
_refine_ls_number_parameters     1107
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1402
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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
O4S O 0.3676(17) 0.1995(4) 0.2345(6) 0.109(7) Uani 0.35 1 d PD A 2
O1A O 0.63211(13) -0.25496(4) 0.03902(7) 0.0362(3) Uani 1 1 d . . .
O2A O 0.67186(12) -0.20383(4) 0.14751(6) 0.0332(3) Uani 1 1 d . . .
O3A O 0.35898(12) -0.00110(4) 0.19392(6) 0.0312(3) Uani 1 1 d . . .
O4A O 0.12107(11) 0.00905(4) 0.10623(6) 0.0250(3) Uani 1 1 d . . .
O5A O -0.09672(12) -0.15160(5) -0.15369(8) 0.0454(4) Uani 1 1 d . . .
O6A O 0.05401(13) -0.21786(5) -0.18666(7) 0.0428(4) Uani 1 1 d . . .
O7A O 0.63682(12) -0.14686(5) 0.22670(6) 0.0373(3) Uani 1 1 d . . .
O8A O 0.11456(14) -0.26853(5) -0.09770(8) 0.0472(4) Uani 1 1 d . . .
O9A O -0.03954(11) -0.03687(4) 0.13293(6) 0.0303(3) Uani 1 1 d . . .
O1B O -0.3742(13) 0.0808(2) 0.5567(7) 0.0294(13) Uani 0.50 1 d P B -1
O2B O -0.2156(3) 0.11467(12) 0.3376(3) 0.0607(10) Uani 0.50 1 d P B -1
O3B O -0.1790(2) -0.06216(9) 0.65464(12) 0.0284(5) Uani 0.50 1 d P B -1
O4B O 0.2951(3) -0.10220(9) 0.63945(13) 0.0414(7) Uani 0.50 1 d P B -1
O5B O 0.4508(2) -0.06958(8) 0.55764(13) 0.0331(6) Uani 0.50 1 d P B -1
O6B O 0.1727(3) 0.09780(12) 0.33135(14) 0.0512(8) Uani 0.50 1 d P B -1
O7B O -0.0267(3) 0.15601(11) 0.34635(16) 0.0537(8) Uani 0.50 1 d P B -1
O8B O 0.3703(13) -0.0950(2) 0.4471(6) 0.0384(19) Uani 0.50 1 d P B -1
O9B O -0.3044(2) 0.00444(8) 0.61831(12) 0.0267(5) Uani 0.50 1 d P B -1
O1S O 0.4239(5) 0.17645(17) 0.2633(3) 0.0735(13) Uani 0.65 1 d PD C 1
O2S O 0.3057(3) 0.22802(12) 0.20066(16) 0.0635(8) Uani 0.65 1 d PD C 1
O3S O 0.4116(7) 0.1362(3) 0.2875(4) 0.108(2) Uani 0.35 1 d PD A 2
N1S N 0.3284(5) 0.20172(19) 0.2490(3) 0.0504(14) Uani 0.65 1 d PD C 1
N2S N 0.3554(8) 0.1721(3) 0.2781(4) 0.063(2) Uani 0.35 1 d PD A 2
C1A C 0.55776(15) -0.11720(5) 0.01229(8) 0.0214(3) Uani 1 1 d . . .
C2A C 0.52456(15) -0.14529(6) -0.04508(8) 0.0220(3) Uani 1 1 d . . .
C3A C 0.55065(15) -0.19150(6) -0.03658(9) 0.0247(3) Uani 1 1 d . . .
H3A H 0.5324 -0.2106 -0.0759 0.030 Uiso 1 1 calc R . .
C4A C 0.60213(16) -0.21006(5) 0.02727(9) 0.0257(4) Uani 1 1 d . . .
C5A C 0.62684(16) -0.18212(6) 0.08512(8) 0.0244(3) Uani 1 1 d . . .
C6A C 0.60766(15) -0.13658(6) 0.07703(8) 0.0239(3) Uani 1 1 d . . .
H6A H 0.6288 -0.1176 0.1164 0.029 Uiso 1 1 calc R . .
C7A C 0.54618(16) -0.06627(5) 0.00904(9) 0.0247(3) Uani 1 1 d . . .
H7A1 H 0.5412 -0.0565 -0.0391 0.030 Uiso 1 1 calc R . .
H7A2 H 0.6266 -0.0531 0.0380 0.030 Uiso 1 1 calc R . .
C8A C 0.6407(2) -0.28152(7) -0.01939(13) 0.0479(6) Uani 1 1 d . . .
H8A1 H 0.5534 -0.2853 -0.0490 0.072 Uiso 1 1 calc R . .
H8A2 H 0.6773 -0.3111 -0.0040 0.072 Uiso 1 1 calc R . .
H8A3 H 0.6974 -0.2664 -0.0453 0.072 Uiso 1 1 calc R . .
C9A C 0.30688(15) -0.04081(5) -0.01179(8) 0.0209(3) Uani 1 1 d . . .
C10A C 0.42900(15) -0.04735(5) 0.03255(8) 0.0217(3) Uani 1 1 d . . .
C11A C 0.44643(16) -0.03498(5) 0.10173(9) 0.0244(3) Uani 1 1 d . . .
H11A H 0.5295 -0.0392 0.1319 0.029 Uiso 1 1 calc R . .
C12A C 0.34601(16) -0.01668(5) 0.12764(8) 0.0235(3) Uani 1 1 d . . .
C13A C 0.22277(16) -0.01214(5) 0.08375(8) 0.0220(3) Uani 1 1 d . . .
C14A C 0.20476(16) -0.02378(5) 0.01525(8) 0.0219(3) Uani 1 1 d . . .
H14A H 0.1208 -0.0201 -0.0144 0.026 Uiso 1 1 calc R . .
C15A C 0.28153(16) -0.04956(6) -0.08907(8) 0.0245(3) Uani 1 1 d . . .
H15A H 0.2186 -0.0268 -0.1131 0.029 Uiso 1 1 calc R . .
H15B H 0.3643 -0.0452 -0.1042 0.029 Uiso 1 1 calc R . .
C16A C 0.48959(19) 0.00292(8) 0.23396(10) 0.0436(5) Uani 1 1 d . . .
H16A H 0.5306 -0.0269 0.2399 0.065 Uiso 1 1 calc R . .
H16B H 0.4881 0.0156 0.2793 0.065 Uiso 1 1 calc R . .
H16C H 0.5397 0.0228 0.2102 0.065 Uiso 1 1 calc R . .
C17A C 0.30633(16) -0.13158(6) -0.12535(8) 0.0248(4) Uani 1 1 d . . .
C18A C 0.22868(16) -0.09603(6) -0.11163(8) 0.0244(3) Uani 1 1 d . . .
C19A C 0.09327(16) -0.10226(6) -0.12008(8) 0.0279(4) Uani 1 1 d . . .
H19A H 0.0413 -0.0781 -0.1098 0.033 Uiso 1 1 calc R . .
C20A C 0.03432(17) -0.14264(7) -0.14301(9) 0.0349(4) Uani 1 1 d . . .
C21A C 0.11261(18) -0.17796(7) -0.15775(10) 0.0364(4) Uani 1 1 d . . .
C22A C 0.24499(17) -0.17245(6) -0.14829(8) 0.0302(4) Uani 1 1 d . . .
H22A H 0.2965 -0.1970 -0.1575 0.036 Uiso 1 1 calc R . .
C23A C 0.45431(16) -0.12896(6) -0.11587(8) 0.0258(4) Uani 1 1 d . . .
H23A H 0.4813 -0.1476 -0.1516 0.031 Uiso 1 1 calc R . .
H23B H 0.4799 -0.0974 -0.1222 0.031 Uiso 1 1 calc R . .
C24A C -0.17863(19) -0.11693(8) -0.13650(12) 0.0499(6) Uani 1 1 d . . .
H24A H -0.1458 -0.1078 -0.0884 0.075 Uiso 1 1 calc R . .
H24B H -0.2681 -0.1283 -0.1426 0.075 Uiso 1 1 calc R . .
H24C H -0.1781 -0.0909 -0.1667 0.075 Uiso 1 1 calc R . .
C25A C 0.32713(17) -0.20885(6) 0.22234(9) 0.0272(4) Uani 1 1 d . . .
C26A C 0.26015(17) -0.17537(6) 0.24998(8) 0.0256(4) Uani 1 1 d . . .
C27A C 0.32550(17) -0.13539(6) 0.27223(8) 0.0291(4) Uani 1 1 d . . .
H27A H 0.2824 -0.1131 0.2933 0.035 Uiso 1 1 calc R . .
C28A C 0.45045(17) -0.12706(7) 0.26473(9) 0.0312(4) Uani 1 1 d . . .
H28A H 0.4918 -0.0991 0.2791 0.037 Uiso 1 1 calc R . .
C29A C 0.51512(17) -0.15993(7) 0.23599(8) 0.0304(4) Uani 1 1 d . . .
C30A C 0.45571(17) -0.20082(6) 0.21675(9) 0.0298(4) Uani 1 1 d . . .
H30A H 0.5026 -0.2238 0.1995 0.036 Uiso 1 1 calc R . .
C31A C 0.26583(19) -0.25348(6) 0.19508(10) 0.0332(4) Uani 1 1 d . . .
H31A H 0.1906 -0.2596 0.2161 0.040 Uiso 1 1 calc R . .
H31B H 0.3306 -0.2778 0.2097 0.040 Uiso 1 1 calc R . .
C32A C 0.09137(18) -0.24469(6) 0.08227(10) 0.0319(4) Uani 1 1 d . . .
C33A C 0.21926(18) -0.25499(6) 0.11712(10) 0.0306(4) Uani 1 1 d . . .
C34A C 0.30741(19) -0.26789(6) 0.07722(10) 0.0342(4) Uani 1 1 d . . .
H34A H 0.3945 -0.2752 0.0999 0.041 Uiso 1 1 calc R . .
C35A C 0.27251(19) -0.27042(6) 0.00638(11) 0.0364(4) Uani 1 1 d . . .
H35A H 0.3354 -0.2784 -0.0192 0.044 Uiso 1 1 calc R . .
C36A C 0.14531(19) -0.26121(6) -0.02720(11) 0.0373(5) Uani 1 1 d . . .
C37A C 0.05525(18) -0.24898(7) 0.01079(11) 0.0374(5) Uani 1 1 d . . .
H37A H -0.0328 -0.2434 -0.0123 0.045 Uiso 1 1 calc R . .
C38A C -0.01364(18) -0.22853(6) 0.11852(10) 0.0333(4) Uani 1 1 d . . .
H38A H -0.1001 -0.2390 0.0924 0.040 Uiso 1 1 calc R . .
H38B H 0.0023 -0.2420 0.1652 0.040 Uiso 1 1 calc R . .
C39A C 0.03945(16) -0.15477(6) 0.18608(8) 0.0243(3) Uani 1 1 d . . .
C40A C -0.01561(16) -0.17749(6) 0.12469(9) 0.0275(4) Uani 1 1 d . . .
C41A C -0.07530(16) -0.15180(6) 0.06722(9) 0.0313(4) Uani 1 1 d . . .
H41A H -0.1137 -0.1668 0.0254 0.038 Uiso 1 1 calc R . .
C42A C -0.08019(17) -0.10533(6) 0.06928(9) 0.0306(4) Uani 1 1 d . . .
H42A H -0.1195 -0.0887 0.0292 0.037 Uiso 1 1 calc R . .
C43A C -0.02717(15) -0.08342(6) 0.13030(9) 0.0251(3) Uani 1 1 d . . .
C44A C 0.02950(16) -0.10796(6) 0.18824(8) 0.0244(3) Uani 1 1 d . . .
H44A H 0.0624 -0.0926 0.2305 0.029 Uiso 1 1 calc R . .
C45A C 0.11613(17) -0.17813(6) 0.25002(9) 0.0280(4) Uani 1 1 d . . .
H45A H 0.0888 -0.2101 0.2502 0.034 Uiso 1 1 calc R . .
H45B H 0.0994 -0.1633 0.2918 0.034 Uiso 1 1 calc R . .
C46A C 0.72211(18) -0.17866(8) 0.20774(9) 0.0426(5) Uani 1 1 d . . .
H46A H 0.7498 -0.2000 0.2465 0.051 Uiso 1 1 calc R . .
H46B H 0.8012 -0.1626 0.2014 0.051 Uiso 1 1 calc R . .
C47A C 0.0083(2) -0.24546(8) -0.13958(11) 0.0454(5) Uani 1 1 d . . .
H47A H -0.0557 -0.2674 -0.1649 0.054 Uiso 1 1 calc R . .
H47B H -0.0359 -0.2267 -0.1105 0.054 Uiso 1 1 calc R . .
C48A C 0.07526(17) -0.01203(6) 0.16006(8) 0.0266(4) Uani 1 1 d . . .
H48A H 0.1434 -0.0325 0.1859 0.032 Uiso 1 1 calc R . .
H48B H 0.0568 0.0111 0.1924 0.032 Uiso 1 1 calc R . .
C1B C 0.022(2) 0.0622(5) 0.6490(11) 0.019(2) Uani 0.50 1 d P B -1
C2B C -0.019(3) 0.1035(10) 0.6113(10) 0.018(2) Uani 0.50 1 d PU B -1
C3B C -0.1504(14) 0.1098(6) 0.5787(7) 0.025(3) Uani 0.50 1 d P B -1
H3B H -0.1747 0.1368 0.5534 0.030 Uiso 0.50 1 calc PR B -1
C4B C -0.255(2) 0.0759(9) 0.5818(15) 0.021(2) Uani 0.50 1 d PU B -1
C5B C -0.1999(18) 0.0372(4) 0.6212(8) 0.020(2) Uani 0.50 1 d P B -1
C6B C -0.077(2) 0.0303(6) 0.6540(7) 0.023(3) Uani 0.50 1 d P B -1
H6B H -0.0547 0.0039 0.6812 0.028 Uiso 0.50 1 calc PR B -1
C7B C -0.0905(18) -0.1332(5) 0.3981(11) 0.044(4) Uani 0.50 1 d P B -1
H7B1 H -0.0489 -0.1632 0.4065 0.052 Uiso 0.50 1 calc PR B -1
H7B2 H -0.1646 -0.1348 0.3575 0.052 Uiso 0.50 1 calc PR B -1
C8B C 0.3974(4) -0.10682(12) 0.51691(18) 0.0311(8) Uani 0.50 1 d P B -1
H8B1 H 0.4600 -0.1322 0.5252 0.037 Uiso 0.50 1 calc PR B -1
H8B2 H 0.3160 -0.1167 0.5299 0.037 Uiso 0.50 1 calc PR B -1
C11B C -0.1384(12) -0.1149(4) 0.4667(8) 0.029(2) Uani 0.50 1 d P B -1
C12B C -0.2393(6) -0.08463(18) 0.4658(3) 0.0264(12) Uani 0.50 1 d P B -1
C13B C -0.2578(4) -0.06795(15) 0.5295(2) 0.0274(8) Uani 0.50 1 d P B -1
H13B H -0.3285 -0.0480 0.5297 0.033 Uiso 0.50 1 calc PR B -1
C14B C -0.1762(4) -0.07983(14) 0.5909(2) 0.0245(8) Uani 0.50 1 d P B -1
C15B C -0.0754(5) -0.10981(13) 0.5938(2) 0.0269(10) Uani 0.50 1 d P B -1
H15C H -0.0207 -0.1185 0.6366 0.032 Uiso 0.50 1 calc PR B -1
C16B C -0.0563(7) -0.12683(18) 0.5321(5) 0.0365(16) Uani 0.50 1 d P B -1
H16D H 0.0139 -0.1472 0.5331 0.044 Uiso 0.50 1 calc PR B -1
C17B C -0.3258(6) -0.0660(3) 0.4015(3) 0.0309(13) Uani 0.50 1 d P B -1
H17A H -0.3226 -0.0864 0.3627 0.037 Uiso 0.50 1 calc PR B -1
H17B H -0.4169 -0.0656 0.4074 0.037 Uiso 0.50 1 calc PR B -1
C18B C -0.2831(4) -0.03414(12) 0.66110(18) 0.0290(8) Uani 0.50 1 d P B -1
H18A H -0.2680 -0.0240 0.7097 0.035 Uiso 0.50 1 calc PR B -1
H18B H -0.3641 -0.0524 0.6514 0.035 Uiso 0.50 1 calc PR B -1
C21B C -0.2904(6) -0.0195(2) 0.3830(3) 0.0271(11) Uani 0.50 1 d P B -1
C22B C -0.2100(8) -0.0104(3) 0.3380(4) 0.0275(16) Uani 0.50 1 d P B -1
C23B C -0.1866(5) 0.03389(18) 0.3210(3) 0.0366(11) Uani 0.50 1 d P B -1
H23C H -0.1360 0.0395 0.2879 0.044 Uiso 0.50 1 calc PR B -1
C24B C -0.2353(4) 0.06953(16) 0.3510(2) 0.0379(10) Uani 0.50 1 d P B -1
C25B C -0.3147(7) 0.0603(2) 0.3968(3) 0.0371(13) Uani 0.50 1 d P B -1
H25B H -0.3504 0.0846 0.4178 0.044 Uiso 0.50 1 calc PR B -1
C26B C -0.3422(5) 0.0173(2) 0.4120(2) 0.0376(11) Uani 0.50 1 d P B -1
H26B H -0.3977 0.0120 0.4430 0.045 Uiso 0.50 1 calc PR B -1
C27B C 0.1620(15) 0.0528(5) 0.6886(8) 0.0234(19) Uani 0.50 1 d P B -1
H27B H 0.1604 0.0387 0.7334 0.028 Uiso 0.50 1 calc PR B -1
H27C H 0.2106 0.0816 0.6977 0.028 Uiso 0.50 1 calc PR B -1
C28B C -0.1144(5) 0.12757(17) 0.3050(2) 0.0588(13) Uani 0.50 1 d P B -1
H28B H -0.0681 0.1003 0.2945 0.071 Uiso 0.50 1 calc PR B -1
H28C H -0.1528 0.1429 0.2610 0.071 Uiso 0.50 1 calc PR B -1
C31B C 0.2331(7) 0.0208(3) 0.6465(4) 0.0222(15) Uani 0.50 1 d P B -1
C32B C 0.3073(5) 0.0360(2) 0.6017(3) 0.0195(10) Uani 0.50 1 d P B -1
C33B C 0.3736(4) 0.00422(15) 0.5703(2) 0.0264(8) Uani 0.50 1 d P B -1
H33B H 0.4248 0.0143 0.5395 0.032 Uiso 0.50 1 calc PR B -1
C34B C 0.3670(4) -0.0414(2) 0.5828(2) 0.0249(8) Uani 0.50 1 d P B -1
C35B C 0.2907(6) -0.05745(19) 0.6279(3) 0.0253(10) Uani 0.50 1 d P B -1
C36B C 0.2250(5) -0.02542(17) 0.6583(2) 0.0265(9) Uani 0.50 1 d P B -1
H36B H 0.1723 -0.0354 0.6885 0.032 Uiso 0.50 1 calc PR B -1
C37B C 0.3222(6) 0.08517(19) 0.5846(3) 0.0241(11) Uani 0.50 1 d P B -1
H37B H 0.4110 0.0899 0.5767 0.029 Uiso 0.50 1 calc PR B -1
H37C H 0.3145 0.1037 0.6249 0.029 Uiso 0.50 1 calc PR B -1
C38B C 0.2757(5) -0.11614(14) 0.7049(2) 0.0382(9) Uani 0.50 1 d P B -1
H38C H 0.3365 -0.0999 0.7414 0.057 Uiso 0.50 1 calc PR B -1
H38D H 0.2916 -0.1486 0.7105 0.057 Uiso 0.50 1 calc PR B -1
H38E H 0.1857 -0.1095 0.7078 0.057 Uiso 0.50 1 calc PR B -1
C41B C 0.2234(7) 0.10183(18) 0.5220(3) 0.0243(12) Uani 0.50 1 d P B -1
C42B C 0.1119(13) 0.1263(4) 0.5269(8) 0.0271(19) Uani 0.50 1 d P B -1
C43B C 0.0325(6) 0.1427(2) 0.4680(3) 0.0287(11) Uani 0.50 1 d P B -1
H43B H -0.0395 0.1613 0.4713 0.034 Uiso 0.50 1 calc PR B -1
C44B C 0.0546(5) 0.1328(2) 0.4043(2) 0.0382(10) Uani 0.50 1 d P B -1
C45B C 0.1601(5) 0.1062(2) 0.3978(2) 0.0372(10) Uani 0.50 1 d P B -1
C46B C 0.2460(4) 0.09156(16) 0.4567(2) 0.0316(9) Uani 0.50 1 d P B -1
H46C H 0.3207 0.0745 0.4531 0.038 Uiso 0.50 1 calc PR B -1
C47B C 0.0827(15) 0.1343(4) 0.5913(10) 0.029(3) Uani 0.50 1 d P B -1
H47C H 0.0519 0.1658 0.5920 0.035 Uiso 0.50 1 calc PR B -1
H47D H 0.1647 0.1318 0.6272 0.035 Uiso 0.50 1 calc PR B -1
C48B C 0.2911(6) 0.07741(16) 0.3243(2) 0.0570(13) Uani 0.50 1 d P B -1
H48C H 0.3646 0.0971 0.3444 0.086 Uiso 0.50 1 calc PR B -1
H48D H 0.2887 0.0727 0.2753 0.086 Uiso 0.50 1 calc PR B -1
H48E H 0.3017 0.0483 0.3483 0.086 Uiso 0.50 1 calc PR B -1
C51B C 0.008(3) -0.0972(10) 0.3884(13) 0.030(5) Uani 0.50 1 d P B -1
C52B C -0.008(2) -0.0608(7) 0.3476(11) 0.035(5) Uani 0.50 1 d P B -1
C53B C 0.094(2) -0.0331(6) 0.3467(8) 0.039(5) Uani 0.50 1 d P B -1
H53B H 0.0757 -0.0057 0.3216 0.047 Uiso 0.50 1 calc PR B -1
C54B C 0.225(2) -0.0420(6) 0.3805(10) 0.037(4) Uani 0.50 1 d P B -1
H54B H 0.2973 -0.0230 0.3797 0.045 Uiso 0.50 1 calc PR B -1
C55B C 0.2307(19) -0.0828(8) 0.4152(14) 0.023(3) Uani 0.50 1 d P B -1
C56B C 0.1369(15) -0.1087(5) 0.4194(7) 0.035(4) Uani 0.50 1 d P B -1
H56B H 0.1544 -0.1362 0.4440 0.041 Uiso 0.50 1 calc PR B -1
C57B C -0.1425(17) -0.0470(6) 0.3071(9) 0.039(3) Uani 0.50 1 d P B -1
H57A H -0.1346 -0.0370 0.2608 0.046 Uiso 0.50 1 calc PR B -1
H57B H -0.1992 -0.0740 0.3008 0.046 Uiso 0.50 1 calc PR B -1
C58B C -0.4196(4) 0.12560(14) 0.5360(2) 0.0339(8) Uani 0.50 1 d P B -1
H58A H -0.3943 0.1462 0.5752 0.051 Uiso 0.50 1 calc PR B -1
H58B H -0.5150 0.1254 0.5203 0.051 Uiso 0.50 1 calc PR B -1
H58C H -0.3804 0.1357 0.4983 0.051 Uiso 0.50 1 calc PR B -1
C1S C 0.2353(4) 0.19901(16) 0.2953(2) 0.0510(11) Uani 0.65 1 d PD C 1
H1S1 H 0.2720 0.2149 0.3385 0.077 Uiso 0.65 1 calc PR C 1
H1S2 H 0.2203 0.1673 0.3052 0.077 Uiso 0.65 1 calc PR C 1
H1S3 H 0.1522 0.2131 0.2727 0.077 Uiso 0.65 1 calc PR C 1
C2S C 0.2589(8) 0.1812(3) 0.3199(4) 0.0407(19) Uani 0.35 1 d PD A 2
H2S1 H 0.2783 0.2103 0.3433 0.061 Uiso 0.35 1 calc PR A 2
H2S2 H 0.2631 0.1573 0.3543 0.061 Uiso 0.35 1 calc PR A 2
H2S3 H 0.1711 0.1821 0.2899 0.061 Uiso 0.35 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4S N2S 1.215(9) . ?
O1A C4A 1.376(2) . ?
O1A C8A 1.424(2) . ?
O2A C5A 1.3845(19) . ?
O2A C46A 1.410(2) . ?
O3A C12A 1.3753(19) . ?
O3A C16A 1.428(2) . ?
O4A C13A 1.3964(19) . ?
O4A C48A 1.4145(19) . ?
O5A C20A 1.371(2) . ?
O5A C24A 1.430(2) . ?
O6A C21A 1.397(2) . ?
O6A C47A 1.407(3) . ?
O7A C29A 1.387(2) . ?
O7A C46A 1.409(2) . ?
O8A C36A 1.384(2) . ?
O8A C47A 1.411(3) . ?
O9A C43A 1.389(2) . ?
O9A C48A 1.413(2) . ?
O1B C4B 1.25(3) . ?
O1B C58B 1.440(8) . ?
O2B C24B 1.390(6) . ?
O2B C28B 1.416(6) . ?
O3B C14B 1.379(4) . ?
O3B C18B 1.401(4) . ?
O4B C35B 1.346(6) . ?
O4B C38B 1.424(5) . ?
O5B C34B 1.386(5) . ?
O5B C8B 1.410(4) . ?
O6B C45B 1.380(5) . ?
O6B C48B 1.417(6) . ?
O7B C28B 1.377(5) . ?
O7B C44B 1.447(6) . ?
O8B C8B 1.399(11) . ?
O8B C55B 1.50(3) . ?
O9B C18B 1.414(4) . ?
O9B C5B 1.456(14) . ?
O1S N1S 1.234(6) . ?
O2S N1S 1.220(6) . ?
O3S N2S 1.213(8) . ?
N1S C1S 1.488(5) . ?
N2S C2S 1.473(8) . ?
C1A C2A 1.393(2) . ?
C1A C6A 1.401(2) . ?
C1A C7A 1.516(2) . ?
C2A C3A 1.400(2) . ?
C2A C23A 1.516(2) . ?
C3A C4A 1.379(2) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.395(2) . ?
C5A C6A 1.369(2) . ?
C6A H6A 0.9500 . ?
C7A C10A 1.519(2) . ?
C7A H7A1 0.9900 . ?
C7A H7A2 0.9900 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A C10A 1.398(2) . ?
C9A C14A 1.398(2) . ?
C9A C15A 1.523(2) . ?
C10A C11A 1.397(2) . ?
C11A C12A 1.384(2) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.396(2) . ?
C13A C14A 1.377(2) . ?
C14A H14A 0.9500 . ?
C15A C18A 1.516(2) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C17A C18A 1.397(2) . ?
C17A C22A 1.400(2) . ?
C17A C23A 1.525(2) . ?
C18A C19A 1.406(2) . ?
C19A C20A 1.378(3) . ?
C19A H19A 0.9500 . ?
C20A C21A 1.403(3) . ?
C21A C22A 1.370(3) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A C26A 1.399(2) . ?
C25A C30A 1.400(2) . ?
C25A C31A 1.518(3) . ?
C26A C27A 1.392(3) . ?
C26A C45A 1.515(2) . ?
C27A C28A 1.376(3) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.383(3) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.378(3) . ?
C30A H30A 0.9500 . ?
C31A C33A 1.519(3) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C32A C37A 1.393(3) . ?
C32A C33A 1.400(3) . ?
C32A C38A 1.524(2) . ?
C33A C34A 1.401(2) . ?
C34A C35A 1.377(3) . ?
C34A H34A 0.9500 . ?
C35A C36A 1.380(3) . ?
C35A H35A 0.9500 . ?
C36A C37A 1.385(3) . ?
C37A H37A 0.9500 . ?
C38A C40A 1.519(2) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C39A C44A 1.394(2) . ?
C39A C40A 1.402(2) . ?
C39A C45A 1.513(2) . ?
C40A C41A 1.400(3) . ?
C41A C42A 1.380(3) . ?
C41A H41A 0.9500 . ?
C42A C43A 1.380(2) . ?
C42A H42A 0.9500 . ?
C43A C44A 1.380(2) . ?
C44A H44A 0.9500 . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C48A H48A 0.9900 . ?
C48A H48B 0.9900 . ?
C1B C6B 1.43(3) . ?
C1B C2B 1.45(3) . ?
C1B C27B 1.53(3) . ?
C2B C3B 1.40(3) . ?
C2B C47B 1.52(3) . ?
C3B C4B 1.50(2) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.44(3) . ?
C5B C6B 1.33(3) . ?
C6B H6B 0.9500 . ?
C7B C51B 1.53(4) . ?
C7B C11B 1.65(2) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
C11B C12B 1.386(9) . ?
C11B C16B 1.435(15) . ?
C12B C13B 1.414(7) . ?
C12B C17B 1.499(8) . ?
C13B C14B 1.373(6) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.374(5) . ?
C15B C16B 1.383(9) . ?
C15B H15C 0.9500 . ?
C16B H16D 0.9500 . ?
C17B C21B 1.494(7) . ?
C17B H17A 0.9900 . ?
C17B H17B 0.9900 . ?
C18B H18A 0.9900 . ?
C18B H18B 0.9900 . ?
C21B C22B 1.389(7) . ?
C21B C26B 1.401(9) . ?
C22B C23B 1.393(8) . ?
C22B C57B 1.50(2) . ?
C23B C24B 1.368(7) . ?
C23B H23C 0.9500 . ?
C24B C25B 1.393(7) . ?
C25B C26B 1.356(9) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C27B C31B 1.562(19) . ?
C27B H27B 0.9900 . ?
C27B H27C 0.9900 . ?
C28B H28B 0.9900 . ?
C28B H28C 0.9900 . ?
C31B C32B 1.384(7) . ?
C31B C36B 1.398(8) . ?
C32B C33B 1.401(7) . ?
C32B C37B 1.512(6) . ?
C33B C34B 1.379(7) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.414(6) . ?
C35B C36B 1.390(7) . ?
C36B H36B 0.9500 . ?
C37B C41B 1.514(7) . ?
C37B H37B 0.9900 . ?
C37B H37C 0.9900 . ?
C38B H38C 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C41B C42B 1.399(10) . ?
C41B C46B 1.406(8) . ?
C42B C43B 1.366(13) . ?
C42B C47B 1.40(2) . ?
C43B C44B 1.372(9) . ?
C43B H43B 0.9500 . ?
C44B C45B 1.389(7) . ?
C45B C46B 1.380(7) . ?
C46B H46C 0.9500 . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C48B H48C 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C51B C52B 1.34(3) . ?
C51B C56B 1.40(3) . ?
C52B C53B 1.35(3) . ?
C52B C57B 1.52(3) . ?
C53B C54B 1.42(3) . ?
C53B H53B 0.9500 . ?
C54B C55B 1.39(3) . ?
C54B H54B 0.9500 . ?
C55B C56B 1.27(2) . ?
C56B H56B 0.9500 . ?
C57B H57A 0.9900 . ?
C57B H57B 0.9900 . ?
C58B H58A 0.9800 . ?
C58B H58B 0.9800 . ?
C58B H58C 0.9800 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4A O1A C8A 116.78(15) . . ?
C5A O2A C46A 120.22(15) . . ?
C12A O3A C16A 116.05(14) . . ?
C13A O4A C48A 117.27(12) . . ?
C20A O5A C24A 117.41(15) . . ?
C21A O6A C47A 113.78(14) . . ?
C29A O7A C46A 120.58(16) . . ?
C36A O8A C47A 119.77(15) . . ?
C43A O9A C48A 116.98(13) . . ?
C4B O1B C58B 117.3(13) . . ?
C24B O2B C28B 120.5(4) . . ?
C14B O3B C18B 119.2(3) . . ?
C35B O4B C38B 115.8(3) . . ?
C34B O5B C8B 118.5(3) . . ?
C45B O6B C48B 116.5(4) . . ?
C28B O7B C44B 112.3(4) . . ?
C8B O8B C55B 116.2(13) . . ?
C18B O9B C5B 119.9(7) . . ?
O2S N1S O1S 125.1(5) . . ?
O2S N1S C1S 118.9(4) . . ?
O1S N1S C1S 116.0(6) . . ?
O3S N2S O4S 124.8(12) . . ?
O3S N2S C2S 116.5(8) . . ?
O4S N2S C2S 118.5(11) . . ?
C2A C1A C6A 118.80(15) . . ?
C2A C1A C7A 123.91(15) . . ?
C6A C1A C7A 117.27(14) . . ?
C1A C2A C3A 118.68(15) . . ?
C1A C2A C23A 123.44(15) . . ?
C3A C2A C23A 117.79(14) . . ?
C4A C3A C2A 121.84(15) . . ?
C4A C3A H3A 119.1 . . ?
C2A C3A H3A 119.1 . . ?
O1A C4A C3A 124.77(15) . . ?
O1A C4A C5A 116.20(15) . . ?
C3A C4A C5A 119.03(15) . . ?
C6A C5A O2A 125.16(15) . . ?
C6A C5A C4A 119.58(15) . . ?
O2A C5A C4A 115.26(15) . . ?
C5A C6A C1A 121.85(15) . . ?
C5A C6A H6A 119.1 . . ?
C1A C6A H6A 119.1 . . ?
C1A C7A C10A 114.70(13) . . ?
C1A C7A H7A1 108.6 . . ?
C10A C7A H7A1 108.6 . . ?
C1A C7A H7A2 108.6 . . ?
C10A C7A H7A2 108.6 . . ?
H7A1 C7A H7A2 107.6 . . ?
O1A C8A H8A1 109.5 . . ?
O1A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
O1A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A C14A 118.80(14) . . ?
C10A C9A C15A 122.81(14) . . ?
C14A C9A C15A 118.34(14) . . ?
C11A C10A C9A 119.00(15) . . ?
C11A C10A C7A 117.68(14) . . ?
C9A C10A C7A 123.30(14) . . ?
C12A C11A C10A 121.85(15) . . ?
C12A C11A H11A 119.1 . . ?
C10A C11A H11A 119.1 . . ?
O3A C12A C11A 124.68(15) . . ?
O3A C12A C13A 116.50(14) . . ?
C11A C12A C13A 118.79(15) . . ?
C14A C13A O4A 118.99(14) . . ?
C14A C13A C12A 119.82(15) . . ?
O4A C13A C12A 120.75(14) . . ?
C13A C14A C9A 121.64(15) . . ?
C13A C14A H14A 119.2 . . ?
C9A C14A H14A 119.2 . . ?
C18A C15A C9A 115.05(13) . . ?
C18A C15A H15A 108.5 . . ?
C9A C15A H15A 108.5 . . ?
C18A C15A H15B 108.5 . . ?
C9A C15A H15B 108.5 . . ?
H15A C15A H15B 107.5 . . ?
O3A C16A H16A 109.5 . . ?
O3A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
O3A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C18A C17A C22A 118.10(15) . . ?
C18A C17A C23A 124.12(15) . . ?
C22A C17A C23A 117.77(15) . . ?
C17A C18A C19A 119.77(16) . . ?
C17A C18A C15A 123.59(15) . . ?
C19A C18A C15A 116.63(15) . . ?
C20A C19A C18A 121.40(16) . . ?
C20A C19A H19A 119.3 . . ?
C18A C19A H19A 119.3 . . ?
O5A C20A C19A 125.50(16) . . ?
O5A C20A C21A 115.98(16) . . ?
C19A C20A C21A 118.51(16) . . ?
C22A C21A O6A 119.83(16) . . ?
C22A C21A C20A 120.43(17) . . ?
O6A C21A C20A 119.60(16) . . ?
C21A C22A C17A 121.77(16) . . ?
C21A C22A H22A 119.1 . . ?
C17A C22A H22A 119.1 . . ?
C2A C23A C17A 111.65(13) . . ?
C2A C23A H23A 109.3 . . ?
C17A C23A H23A 109.3 . . ?
C2A C23A H23B 109.3 . . ?
C17A C23A H23B 109.3 . . ?
H23A C23A H23B 108.0 . . ?
O5A C24A H24A 109.5 . . ?
O5A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
O5A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C26A C25A C30A 119.31(17) . . ?
C26A C25A C31A 123.31(16) . . ?
C30A C25A C31A 117.34(15) . . ?
C27A C26A C25A 118.31(16) . . ?
C27A C26A C45A 117.85(15) . . ?
C25A C26A C45A 123.50(16) . . ?
C28A C27A C26A 122.19(16) . . ?
C28A C27A H27A 118.9 . . ?
C26A C27A H27A 118.9 . . ?
C27A C28A C29A 119.15(17) . . ?
C27A C28A H28A 120.4 . . ?
C29A C28A H28A 120.4 . . ?
C30A C29A C28A 120.09(16) . . ?
C30A C29A O7A 125.60(16) . . ?
C28A C29A O7A 114.25(17) . . ?
C29A C30A C25A 120.81(16) . . ?
C29A C30A H30A 119.6 . . ?
C25A C30A H30A 119.6 . . ?
C25A C31A C33A 113.85(14) . . ?
C25A C31A H31A 108.8 . . ?
C33A C31A H31A 108.8 . . ?
C25A C31A H31B 108.8 . . ?
C33A C31A H31B 108.8 . . ?
H31A C31A H31B 107.7 . . ?
C37A C32A C33A 119.81(16) . . ?
C37A C32A C38A 116.84(17) . . ?
C33A C32A C38A 123.35(17) . . ?
C32A C33A C34A 117.46(18) . . ?
C32A C33A C31A 123.56(16) . . ?
C34A C33A C31A 118.97(17) . . ?
C35A C34A C33A 122.49(19) . . ?
C35A C34A H34A 118.8 . . ?
C33A C34A H34A 118.8 . . ?
C34A C35A C36A 119.43(17) . . ?
C34A C35A H35A 120.3 . . ?
C36A C35A H35A 120.3 . . ?
C35A C36A O8A 116.11(16) . . ?
C35A C36A C37A 119.53(19) . . ?
O8A C36A C37A 124.16(18) . . ?
C36A C37A C32A 121.21(18) . . ?
C36A C37A H37A 119.4 . . ?
C32A C37A H37A 119.4 . . ?
C40A C38A C32A 112.09(14) . . ?
C40A C38A H38A 109.2 . . ?
C32A C38A H38A 109.2 . . ?
C40A C38A H38B 109.2 . . ?
C32A C38A H38B 109.2 . . ?
H38A C38A H38B 107.9 . . ?
C44A C39A C40A 119.12(16) . . ?
C44A C39A C45A 117.38(15) . . ?
C40A C39A C45A 123.43(15) . . ?
C41A C40A C39A 118.18(16) . . ?
C41A C40A C38A 119.21(16) . . ?
C39A C40A C38A 122.62(17) . . ?
C42A C41A C40A 122.15(16) . . ?
C42A C41A H41A 118.9 . . ?
C40A C41A H41A 118.9 . . ?
C43A C42A C41A 119.07(17) . . ?
C43A C42A H42A 120.5 . . ?
C41A C42A H42A 120.5 . . ?
C42A C43A C44A 120.01(16) . . ?
C42A C43A O9A 118.59(15) . . ?
C44A C43A O9A 121.27(15) . . ?
C43A C44A C39A 121.39(15) . . ?
C43A C44A H44A 119.3 . . ?
C39A C44A H44A 119.3 . . ?
C39A C45A C26A 108.54(13) . . ?
C39A C45A H45A 110.0 . . ?
C26A C45A H45A 110.0 . . ?
C39A C45A H45B 110.0 . . ?
C26A C45A H45B 110.0 . . ?
H45A C45A H45B 108.4 . . ?
O7A C46A O2A 116.27(14) . . ?
O7A C46A H46A 108.2 . . ?
O2A C46A H46A 108.2 . . ?
O7A C46A H46B 108.2 . . ?
O2A C46A H46B 108.2 . . ?
H46A C46A H46B 107.4 . . ?
O6A C47A O8A 109.46(16) . . ?
O6A C47A H47A 109.8 . . ?
O8A C47A H47A 109.8 . . ?
O6A C47A H47B 109.8 . . ?
O8A C47A H47B 109.8 . . ?
H47A C47A H47B 108.2 . . ?
O9A C48A O4A 110.31(13) . . ?
O9A C48A H48A 109.6 . . ?
O4A C48A H48A 109.6 . . ?
O9A C48A H48B 109.6 . . ?
O4A C48A H48B 109.6 . . ?
H48A C48A H48B 108.1 . . ?
C6B C1B C2B 117(2) . . ?
C6B C1B C27B 118.4(17) . . ?
C2B C1B C27B 124.1(18) . . ?
C3B C2B C1B 120(2) . . ?
C3B C2B C47B 118.3(19) . . ?
C1B C2B C47B 120(2) . . ?
C2B C3B C4B 123(2) . . ?
C2B C3B H3B 118.5 . . ?
C4B C3B H3B 118.5 . . ?
O1B C4B C5B 123.6(17) . . ?
O1B C4B C3B 126(2) . . ?
C5B C4B C3B 110.7(18) . . ?
C6B C5B C4B 128.2(14) . . ?
C6B C5B O9B 124.0(13) . . ?
C4B C5B O9B 107.8(14) . . ?
C5B C6B C1B 120.6(17) . . ?
C5B C6B H6B 119.7 . . ?
C1B C6B H6B 119.7 . . ?
C51B C7B C11B 102.6(15) . . ?
C51B C7B H7B1 111.2 . . ?
C11B C7B H7B1 111.3 . . ?
C51B C7B H7B2 111.3 . . ?
C11B C7B H7B2 111.3 . . ?
H7B1 C7B H7B2 109.2 . . ?
O8B C8B O5B 109.9(5) . . ?
O8B C8B H8B1 109.7 . . ?
O5B C8B H8B1 109.7 . . ?
O8B C8B H8B2 109.7 . . ?
O5B C8B H8B2 109.7 . . ?
H8B1 C8B H8B2 108.2 . . ?
C12B C11B C16B 118.3(11) . . ?
C12B C11B C7B 125.2(12) . . ?
C16B C11B C7B 115.9(10) . . ?
C11B C12B C13B 118.2(8) . . ?
C11B C12B C17B 124.5(8) . . ?
C13B C12B C17B 117.2(5) . . ?
C14B C13B C12B 121.7(4) . . ?
C14B C13B H13B 119.2 . . ?
C12B C13B H13B 119.2 . . ?
C13B C14B C15B 121.6(4) . . ?
C13B C14B O3B 125.7(3) . . ?
C15B C14B O3B 112.5(4) . . ?
C14B C15B C16B 117.6(5) . . ?
C14B C15B H15C 121.2 . . ?
C16B C15B H15C 121.2 . . ?
C15B C16B C11B 122.5(7) . . ?
C15B C16B H16D 118.7 . . ?
C11B C16B H16D 118.7 . . ?
C21B C17B C12B 114.4(5) . . ?
C21B C17B H17A 108.6 . . ?
C12B C17B H17A 108.6 . . ?
C21B C17B H17B 108.6 . . ?
C12B C17B H17B 108.6 . . ?
H17A C17B H17B 107.6 . . ?
O3B C18B O9B 116.5(3) . . ?
O3B C18B H18A 108.2 . . ?
O9B C18B H18A 108.2 . . ?
O3B C18B H18B 108.2 . . ?
O9B C18B H18B 108.2 . . ?
H18A C18B H18B 107.3 . . ?
C22B C21B C26B 117.6(7) . . ?
C22B C21B C17B 124.0(6) . . ?
C26B C21B C17B 118.4(6) . . ?
C21B C22B C23B 120.4(8) . . ?
C21B C22B C57B 122.4(8) . . ?
C23B C22B C57B 117.2(8) . . ?
C24B C23B C22B 121.3(6) . . ?
C24B C23B H23C 119.4 . . ?
C22B C23B H23C 119.4 . . ?
C23B C24B O2B 125.0(5) . . ?
C23B C24B C25B 118.1(5) . . ?
O2B C24B C25B 116.9(5) . . ?
C26B C25B C24B 121.3(6) . . ?
C26B C25B H25B 119.3 . . ?
C24B C25B H25B 119.3 . . ?
C25B C26B C21B 121.2(6) . . ?
C25B C26B H26B 119.4 . . ?
C21B C26B H26B 119.4 . . ?
C1B C27B C31B 110.7(13) . . ?
C1B C27B H27B 109.5 . . ?
C31B C27B H27B 109.5 . . ?
C1B C27B H27C 109.5 . . ?
C31B C27B H27C 109.5 . . ?
H27B C27B H27C 108.1 . . ?
O7B C28B O2B 111.2(4) . . ?
O7B C28B H28B 109.4 . . ?
O2B C28B H28B 109.4 . . ?
O7B C28B H28C 109.4 . . ?
O2B C28B H28C 109.4 . . ?
H28B C28B H28C 108.0 . . ?
C32B C31B C36B 119.5(6) . . ?
C32B C31B C27B 123.6(8) . . ?
C36B C31B C27B 116.8(7) . . ?
C31B C32B C33B 118.4(6) . . ?
C31B C32B C37B 124.1(6) . . ?
C33B C32B C37B 117.5(6) . . ?
C34B C33B C32B 122.0(5) . . ?
C34B C33B H33B 119.0 . . ?
C32B C33B H33B 119.0 . . ?
C33B C34B O5B 117.7(4) . . ?
C33B C34B C35B 120.2(4) . . ?
O5B C34B C35B 121.5(5) . . ?
O4B C35B C36B 126.9(5) . . ?
O4B C35B C34B 116.0(5) . . ?
C36B C35B C34B 117.0(4) . . ?
C35B C36B C31B 122.8(5) . . ?
C35B C36B H36B 118.6 . . ?
C31B C36B H36B 118.6 . . ?
C32B C37B C41B 114.4(5) . . ?
C32B C37B H37B 108.7 . . ?
C41B C37B H37B 108.7 . . ?
C32B C37B H37C 108.7 . . ?
C41B C37B H37C 108.7 . . ?
H37B C37B H37C 107.6 . . ?
C42B C41B C46B 119.6(8) . . ?
C42B C41B C37B 122.8(8) . . ?
C46B C41B C37B 117.6(6) . . ?
C43B C42B C41B 119.0(11) . . ?
C43B C42B C47B 120.4(11) . . ?
C41B C42B C47B 120.6(12) . . ?
C42B C43B C44B 121.3(8) . . ?
C42B C43B H43B 119.4 . . ?
C44B C43B H43B 119.4 . . ?
C43B C44B C45B 120.8(5) . . ?
C43B C44B O7B 116.2(5) . . ?
C45B C44B O7B 122.5(4) . . ?
O6B C45B C46B 124.9(5) . . ?
O6B C45B C44B 116.2(4) . . ?
C46B C45B C44B 118.8(4) . . ?
C45B C46B C41B 120.3(5) . . ?
C45B C46B H46C 119.9 . . ?
C41B C46B H46C 119.9 . . ?
C42B C47B C2B 116.4(14) . . ?
C42B C47B H47C 108.2 . . ?
C2B C47B H47C 108.2 . . ?
C42B C47B H47D 108.2 . . ?
C2B C47B H47D 108.2 . . ?
H47C C47B H47D 107.3 . . ?
C52B C51B C56B 116(3) . . ?
C52B C51B C7B 130(3) . . ?
C56B C51B C7B 113(2) . . ?
C51B C52B C53B 121(2) . . ?
C51B C52B C57B 121(2) . . ?
C53B C52B C57B 118.2(19) . . ?
C52B C53B C54B 124.6(19) . . ?
C52B C53B H53B 117.7 . . ?
C54B C53B H53B 117.7 . . ?
C55B C54B C53B 109.2(17) . . ?
C55B C54B H54B 125.4 . . ?
C53B C54B H54B 125.4 . . ?
C56B C55B C54B 128(2) . . ?
C56B C55B O8B 122(2) . . ?
C54B C55B O8B 110.5(14) . . ?
C55B C56B C51B 121(2) . . ?
C55B C56B H56B 119.5 . . ?
C51B C56B H56B 119.5 . . ?
C22B C57B C52B 116.5(14) . . ?
C22B C57B H57A 108.2 . . ?
C52B C57B H57A 108.2 . . ?
C22B C57B H57B 108.2 . . ?
C52B C57B H57B 108.2 . . ?
H57A C57B H57B 107.3 . . ?
N2S C2S H2S1 109.5 . . ?
N2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
N2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.049
_database_code_depnum_ccdc_archive 'CCDC 1027976'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_13005d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C48 H42 O9, 1.5(C2 H4 Cl2), 0.92(Xe)'
_chemical_formula_sum            'C51 H48 Cl3 O9 Xe0.92'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1032.04

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Xe Xe -0.4205 1.9578 '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_int_tables_number      14
_chemical_absolute_configuration ?

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                   19.9358(2)
_cell_length_b                   10.94100(10)
_cell_length_c                   21.0740(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.3330(10)
_cell_angle_gamma                90.00
_cell_volume                     4387.87(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    58919
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      30.18
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2107
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'


_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker, APEX Duo'
_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            49839
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.00
_reflns_number_total             10591
_reflns_number_gt                7927
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, L.Barbour (1999); http://x-seed.net/'
_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)+(0.0574P)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         10591
_refine_ls_number_parameters     580
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.979
_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
Xe1 Xe 0.266709(8) 0.641783(15) 0.123933(8) 0.01833(6) Uani 0.92 1 d P . .
Cl3 Cl 0.40946(3) 1.11806(6) -0.02659(3) 0.02744(14) Uani 1 1 d . . .
Cl2 Cl 0.02955(4) 1.06454(9) 0.19051(6) 0.0570(3) Uani 1 1 d . . .
Cl1 Cl -0.13416(5) 0.79648(10) 0.13337(6) 0.0636(3) Uani 1 1 d . . .
O1M O 0.04885(9) 0.63684(16) -0.07975(9) 0.0230(4) Uani 1 1 d . . .
O6 O 0.35737(8) 0.84414(15) 0.32789(8) 0.0169(3) Uani 1 1 d . . .
O5 O 0.45490(8) 0.73721(15) 0.31122(8) 0.0171(3) Uani 1 1 d . . .
O2M O 0.49639(8) 0.61279(15) 0.08973(8) 0.0191(4) Uani 1 1 d . . .
O3 O 0.33461(9) 0.37549(16) -0.01067(8) 0.0210(4) Uani 1 1 d . . .
C10A C 0.18973(12) 0.8688(2) -0.01669(11) 0.0160(5) Uani 1 1 d . . .
O3M O 0.22412(8) 0.91058(16) 0.30335(8) 0.0196(4) Uani 1 1 d . . .
C11A C 0.16489(12) 0.9245(2) 0.03133(11) 0.0169(5) Uani 1 1 d . . .
O1 O 0.03705(9) 0.67855(17) 0.12235(8) 0.0219(4) Uani 1 1 d . . .
C24A C 0.35877(12) 0.9164(2) 0.21712(11) 0.0155(5) Uani 1 1 d . . .
H24A H 0.4074 0.8988 0.2260 0.019 Uiso 1 1 calc R . .
C16A C 0.36871(12) 0.8693(2) 0.06663(11) 0.0151(5) Uani 1 1 d . . .
C13A C 0.38920(12) 0.6485(2) 0.00744(11) 0.0157(5) Uani 1 1 d . . .
C1S C -0.05997(16) 0.8793(3) 0.18297(16) 0.0367(7) Uani 1 1 d . . .
H1S1 H -0.0712 0.9184 0.2209 0.044 Uiso 1 1 calc R . .
H1S2 H -0.0196 0.8234 0.2006 0.044 Uiso 1 1 calc R . .
O2 O 0.00247(8) 0.74766(16) 0.01424(8) 0.0208(4) Uani 1 1 d . . .
C6A C 0.10549(12) 0.4912(2) 0.15240(12) 0.0177(5) Uani 1 1 d . . .
H6A H 0.0759 0.4495 0.1150 0.021 Uiso 1 1 calc R . .
C8B C 0.35991(12) 0.9842(2) 0.10363(11) 0.0161(5) Uani 1 1 d . . .
H8B1 H 0.3340 1.0457 0.0710 0.019 Uiso 1 1 calc R . .
H8B2 H 0.4069 1.0182 0.1264 0.019 Uiso 1 1 calc R . .
O4 O 0.40014(9) 0.54246(15) -0.02432(8) 0.0185(3) Uani 1 1 d . . .
C35A C 0.29954(12) 0.3523(2) 0.03586(12) 0.0178(5) Uani 1 1 d . . .
C14A C 0.43911(12) 0.6875(2) 0.06594(11) 0.0158(5) Uani 1 1 d . . .
C19A C 0.32097(12) 0.9631(2) 0.15481(12) 0.0153(5) Uani 1 1 d . . .
C17A C 0.32105(12) 0.8335(2) 0.00554(11) 0.0153(5) Uani 1 1 d . . .
C33A C 0.18978(12) 0.3392(2) 0.05965(12) 0.0180(5) Uani 1 1 d . . .
H33A H 0.1399 0.3432 0.0447 0.022 Uiso 1 1 calc R . .
C34A C 0.22697(13) 0.3599(2) 0.01473(12) 0.0192(5) Uani 1 1 d . . .
H34A H 0.2029 0.3792 -0.0302 0.023 Uiso 1 1 calc R . .
C1B C 0.00996(13) 0.6434(2) 0.05466(12) 0.0207(5) Uani 1 1 d . . .
H1B1 H 0.0423 0.5847 0.0433 0.025 Uiso 1 1 calc R . .
H1B2 H -0.0362 0.6030 0.0471 0.025 Uiso 1 1 calc R . .
C20A C 0.24906(12) 0.9883(2) 0.14171(12) 0.0164(5) Uani 1 1 d . . .
C30A C 0.46110(12) 0.5454(2) 0.26494(11) 0.0163(5) Uani 1 1 d . . .
H30A H 0.5038 0.5714 0.2579 0.020 Uiso 1 1 calc R . .
C12A C 0.10251(12) 0.8811(2) 0.04120(12) 0.0182(5) Uani 1 1 d . . .
H12A H 0.0854 0.9186 0.0740 0.022 Uiso 1 1 calc R . .
C27A C 0.33739(11) 0.4652(2) 0.28768(11) 0.0154(5) Uani 1 1 d . . .
C25A C 0.42589(12) 0.6219(2) 0.29688(11) 0.0150(5) Uani 1 1 d . . .
C15A C 0.42783(11) 0.7962(2) 0.09483(11) 0.0155(5) Uani 1 1 d . . .
H15A H 0.4612 0.8220 0.1350 0.019 Uiso 1 1 calc R . .
C26A C 0.36590(12) 0.5805(2) 0.31045(11) 0.0160(5) Uani 1 1 d . . .
H26A H 0.3438 0.6303 0.3353 0.019 Uiso 1 1 calc R . .
C7A C 0.06545(12) 0.7854(2) 0.00450(12) 0.0184(5) Uani 1 1 d . . .
C18A C 0.33261(12) 0.7226(2) -0.02261(11) 0.0163(5) Uani 1 1 d . . .
H18A H 0.3005 0.6976 -0.0637 0.020 Uiso 1 1 calc R . .
C4A C 0.20444(12) 0.4885(2) 0.25249(11) 0.0162(5) Uani 1 1 d . . .
C3B C 0.42968(12) 0.8191(2) 0.35084(12) 0.0176(5) Uani 1 1 d . . .
H3B1 H 0.4407 0.7850 0.3963 0.021 Uiso 1 1 calc R . .
H3B2 H 0.4556 0.8972 0.3540 0.021 Uiso 1 1 calc R . .
C5B C 0.17879(12) 0.3030(2) 0.17381(12) 0.0169(5) Uani 1 1 d . . .
H5B1 H 0.1342 0.2606 0.1512 0.020 Uiso 1 1 calc R . .
H5B2 H 0.2040 0.2543 0.2133 0.020 Uiso 1 1 calc R . .
C6B C 0.33956(12) 0.2726(2) 0.21802(11) 0.0173(5) Uani 1 1 d . . .
H6B1 H 0.3779 0.2148 0.2183 0.021 Uiso 1 1 calc R . .
H6B2 H 0.3094 0.2342 0.2422 0.021 Uiso 1 1 calc R . .
C7B C 0.25692(12) 0.9078(2) -0.03118(12) 0.0167(5) Uani 1 1 d . . .
H7B1 H 0.2499 0.9008 -0.0796 0.020 Uiso 1 1 calc R . .
H7B2 H 0.2660 0.9949 -0.0189 0.020 Uiso 1 1 calc R . .
C23A C 0.32677(12) 0.8952(2) 0.26601(11) 0.0154(5) Uani 1 1 d . . .
C4B C 0.26881(12) 0.4302(2) 0.30092(11) 0.0164(5) Uani 1 1 d . . .
H4B1 H 0.2636 0.3402 0.2981 0.020 Uiso 1 1 calc R . .
H4B2 H 0.2712 0.4551 0.3467 0.020 Uiso 1 1 calc R . .
C3S C 0.46781(13) 0.9951(2) -0.02952(13) 0.0224(5) Uani 1 1 d . . .
H3S1 H 0.4442 0.9158 -0.0287 0.027 Uiso 1 1 calc R . .
H3S2 H 0.4812 0.9997 -0.0711 0.027 Uiso 1 1 calc R . .
C21A C 0.21838(12) 0.9706(2) 0.19260(12) 0.0168(5) Uani 1 1 d . . .
H21A H 0.1701 0.9902 0.1846 0.020 Uiso 1 1 calc R . .
C28A C 0.37054(12) 0.3910(2) 0.25255(11) 0.0160(5) Uani 1 1 d . . .
C3A C 0.18689(12) 0.6084(2) 0.26425(12) 0.0189(5) Uani 1 1 d . . .
H3A H 0.2139 0.6484 0.3036 0.023 Uiso 1 1 calc R . .
C2M C 0.55345(12) 0.6608(2) 0.14178(12) 0.0209(5) Uani 1 1 d . . .
H2M1 H 0.5687 0.7386 0.1275 0.031 Uiso 1 1 calc R . .
H2M2 H 0.5926 0.6027 0.1522 0.031 Uiso 1 1 calc R . .
H2M3 H 0.5383 0.6742 0.1814 0.031 Uiso 1 1 calc R . .
C32A C 0.22367(12) 0.3126(2) 0.12658(12) 0.0164(5) Uani 1 1 d . . .
C36A C 0.33375(12) 0.3164(2) 0.10048(12) 0.0170(5) Uani 1 1 d . . .
H36A H 0.3831 0.3033 0.1137 0.020 Uiso 1 1 calc R . .
C2B C 0.40208(12) 0.4321(2) 0.01149(12) 0.0184(5) Uani 1 1 d . . .
H2B1 H 0.4144 0.4495 0.0597 0.022 Uiso 1 1 calc R . .
H2B2 H 0.4382 0.3766 0.0039 0.022 Uiso 1 1 calc R . .
C31A C 0.29636(12) 0.2993(2) 0.14673(12) 0.0161(5) Uani 1 1 d . . .
C9B C 0.20164(12) 1.0302(2) 0.07442(12) 0.0175(5) Uani 1 1 d . . .
H9B1 H 0.1659 1.0871 0.0813 0.021 Uiso 1 1 calc R . .
H9B2 H 0.2301 1.0753 0.0509 0.021 Uiso 1 1 calc R . .
C5A C 0.16315(12) 0.4296(2) 0.19546(12) 0.0171(5) Uani 1 1 d . . .
C2A C 0.13184(12) 0.6708(2) 0.22088(12) 0.0192(5) Uani 1 1 d . . .
H2A H 0.1218 0.7528 0.2298 0.023 Uiso 1 1 calc R . .
C29A C 0.43394(12) 0.4318(2) 0.24356(11) 0.0175(5) Uani 1 1 d . . .
H29A H 0.4587 0.3797 0.2222 0.021 Uiso 1 1 calc R . .
C22A C 0.25566(12) 0.9260(2) 0.25384(12) 0.0165(5) Uani 1 1 d . . .
C9A C 0.15124(12) 0.7719(2) -0.05436(12) 0.0177(5) Uani 1 1 d . . .
H9A H 0.1679 0.7345 -0.0874 0.021 Uiso 1 1 calc R . .
C1A C 0.09121(12) 0.6116(2) 0.16370(12) 0.0183(5) Uani 1 1 d . . .
C8A C 0.08933(12) 0.7293(2) -0.04440(12) 0.0187(5) Uani 1 1 d . . .
C3M C 0.24168(13) 1.0094(2) 0.35040(13) 0.0243(5) Uani 1 1 d . . .
H3M1 H 0.2926 1.0223 0.3644 0.036 Uiso 1 1 calc R . .
H3M2 H 0.2264 0.9891 0.3893 0.036 Uiso 1 1 calc R . .
H3M3 H 0.2180 1.0841 0.3296 0.036 Uiso 1 1 calc R . .
C1M C 0.06680(14) 0.5927(3) -0.13620(14) 0.0309(6) Uani 1 1 d . . .
H1M1 H 0.0669 0.6608 -0.1664 0.046 Uiso 1 1 calc R . .
H1M2 H 0.0323 0.5315 -0.1594 0.046 Uiso 1 1 calc R . .
H1M3 H 0.1136 0.5554 -0.1217 0.046 Uiso 1 1 calc R . .
C2S C -0.04260(17) 0.9722(3) 0.14048(18) 0.0505(9) Uani 1 1 d . . .
H2S1 H -0.0841 1.0245 0.1206 0.061 Uiso 1 1 calc R . .
H2S2 H -0.0289 0.9324 0.1040 0.061 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
Cl3 C3S 1.792(3) . ?
Cl2 C2S 1.816(4) . ?
Cl1 C1S 1.783(3) . ?
O1M C8A 1.368(3) . ?
O1M C1M 1.425(3) . ?
O6 C23A 1.382(3) . ?
O6 C3B 1.404(3) . ?
O5 C25A 1.384(3) . ?
O5 C3B 1.415(3) . ?
O2M C14A 1.372(3) . ?
O2M C2M 1.425(3) . ?
O3 C35A 1.387(3) . ?
O3 C2B 1.427(3) . ?
C10A C11A 1.393(3) . ?
C10A C9A 1.407(3) . ?
C10A C7B 1.521(3) . ?
O3M C22A 1.380(3) . ?
O3M C3M 1.438(3) . ?
C11A C12A 1.403(3) . ?
C11A C9B 1.517(3) . ?
O1 C1A 1.379(3) . ?
O1 C1B 1.420(3) . ?
C24A C23A 1.383(3) . ?
C24A C19A 1.401(3) . ?
C24A H24A 0.9500 . ?
C16A C15A 1.402(3) . ?
C16A C17A 1.409(3) . ?
C16A C8B 1.517(3) . ?
C13A C18A 1.380(3) . ?
C13A O4 1.389(3) . ?
C13A C14A 1.400(3) . ?
C1S C2S 1.463(4) . ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
O2 C7A 1.394(3) . ?
O2 C1B 1.405(3) . ?
C6A C1A 1.383(3) . ?
C6A C5A 1.406(3) . ?
C6A H6A 0.9500 . ?
C8B C19A 1.523(3) . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
O4 C2B 1.419(3) . ?
C35A C34A 1.384(3) . ?
C35A C36A 1.386(3) . ?
C14A C15A 1.385(3) . ?
C19A C20A 1.404(3) . ?
C17A C18A 1.399(3) . ?
C17A C7B 1.519(3) . ?
C33A C34A 1.384(3) . ?
C33A C32A 1.401(3) . ?
C33A H33A 0.9500 . ?
C34A H34A 0.9500 . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C20A C21A 1.397(3) . ?
C20A C9B 1.522(3) . ?
C30A C29A 1.377(3) . ?
C30A C25A 1.388(3) . ?
C30A H30A 0.9500 . ?
C12A C7A 1.378(3) . ?
C12A H12A 0.9500 . ?
C27A C28A 1.391(3) . ?
C27A C26A 1.407(3) . ?
C27A C4B 1.524(3) . ?
C25A C26A 1.386(3) . ?
C15A H15A 0.9500 . ?
C26A H26A 0.9500 . ?
C7A C8A 1.399(3) . ?
C18A H18A 0.9500 . ?
C4A C5A 1.396(3) . ?
C4A C3A 1.398(3) . ?
C4A C4B 1.521(3) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C5B C5A 1.519(3) . ?
C5B C32A 1.527(3) . ?
C5B H5B1 0.9900 . ?
C5B H5B2 0.9900 . ?
C6B C31A 1.521(3) . ?
C6B C28A 1.524(3) . ?
C6B H6B1 0.9900 . ?
C6B H6B2 0.9900 . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C23A C22A 1.404(3) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C3S C3S 1.502(5) 3_675 ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C21A C22A 1.373(3) . ?
C21A H21A 0.9500 . ?
C28A C29A 1.405(3) . ?
C3A C2A 1.382(3) . ?
C3A H3A 0.9500 . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?
C32A C31A 1.391(3) . ?
C36A C31A 1.405(3) . ?
C36A H36A 0.9500 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C9B H9B1 0.9900 . ?
C9B H9B2 0.9900 . ?
C2A C1A 1.395(3) . ?
C2A H2A 0.9500 . ?
C29A H29A 0.9500 . ?
C9A C8A 1.392(3) . ?
C9A H9A 0.9500 . ?
C3M H3M1 0.9800 . ?
C3M H3M2 0.9800 . ?
C3M H3M3 0.9800 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8A O1M C1M 116.82(19) . . ?
C23A O6 C3B 121.53(18) . . ?
C25A O5 C3B 120.50(18) . . ?
C14A O2M C2M 116.65(18) . . ?
C35A O3 C2B 118.21(18) . . ?
C11A C10A C9A 119.2(2) . . ?
C11A C10A C7B 123.2(2) . . ?
C9A C10A C7B 117.6(2) . . ?
C22A O3M C3M 110.94(18) . . ?
C10A C11A C12A 118.8(2) . . ?
C10A C11A C9B 123.8(2) . . ?
C12A C11A C9B 117.4(2) . . ?
C1A O1 C1B 118.88(19) . . ?
C23A C24A C19A 121.4(2) . . ?
C23A C24A H24A 119.3 . . ?
C19A C24A H24A 119.3 . . ?
C15A C16A C17A 118.8(2) . . ?
C15A C16A C8B 117.8(2) . . ?
C17A C16A C8B 123.4(2) . . ?
C18A C13A O4 119.6(2) . . ?
C18A C13A C14A 119.6(2) . . ?
O4 C13A C14A 120.4(2) . . ?
C2S C1S Cl1 107.5(2) . . ?
C2S C1S H1S1 110.2 . . ?
Cl1 C1S H1S1 110.2 . . ?
C2S C1S H1S2 110.2 . . ?
Cl1 C1S H1S2 110.2 . . ?
H1S1 C1S H1S2 108.5 . . ?
C7A O2 C1B 113.10(18) . . ?
C1A C6A C5A 121.1(2) . . ?
C1A C6A H6A 119.5 . . ?
C5A C6A H6A 119.5 . . ?
C16A C8B C19A 113.57(19) . . ?
C16A C8B H8B1 108.9 . . ?
C19A C8B H8B1 108.9 . . ?
C16A C8B H8B2 108.9 . . ?
C19A C8B H8B2 108.9 . . ?
H8B1 C8B H8B2 107.7 . . ?
C13A O4 C2B 115.99(18) . . ?
C34A C35A C36A 119.7(2) . . ?
C34A C35A O3 117.4(2) . . ?
C36A C35A O3 122.9(2) . . ?
O2M C14A C15A 125.3(2) . . ?
O2M C14A C13A 115.9(2) . . ?
C15A C14A C13A 118.9(2) . . ?
C24A C19A C20A 119.2(2) . . ?
C24A C19A C8B 118.3(2) . . ?
C20A C19A C8B 122.5(2) . . ?
C18A C17A C16A 118.5(2) . . ?
C18A C17A C7B 117.9(2) . . ?
C16A C17A C7B 123.5(2) . . ?
C34A C33A C32A 121.8(2) . . ?
C34A C33A H33A 119.1 . . ?
C32A C33A H33A 119.1 . . ?
C35A C34A C33A 119.5(2) . . ?
C35A C34A H34A 120.3 . . ?
C33A C34A H34A 120.3 . . ?
O2 C1B O1 109.24(19) . . ?
O2 C1B H1B1 109.8 . . ?
O1 C1B H1B1 109.8 . . ?
O2 C1B H1B2 109.8 . . ?
O1 C1B H1B2 109.8 . . ?
H1B1 C1B H1B2 108.3 . . ?
C21A C20A C19A 118.5(2) . . ?
C21A C20A C9B 117.7(2) . . ?
C19A C20A C9B 123.8(2) . . ?
C29A C30A C25A 119.8(2) . . ?
C29A C30A H30A 120.1 . . ?
C25A C30A H30A 120.1 . . ?
C7A C12A C11A 121.6(2) . . ?
C7A C12A H12A 119.2 . . ?
C11A C12A H12A 119.2 . . ?
C28A C27A C26A 119.8(2) . . ?
C28A C27A C4B 123.0(2) . . ?
C26A C27A C4B 117.1(2) . . ?
O5 C25A C26A 125.7(2) . . ?
O5 C25A C30A 114.6(2) . . ?
C26A C25A C30A 119.7(2) . . ?
C14A C15A C16A 122.0(2) . . ?
C14A C15A H15A 119.0 . . ?
C16A C15A H15A 119.0 . . ?
C25A C26A C27A 120.5(2) . . ?
C25A C26A H26A 119.7 . . ?
C27A C26A H26A 119.7 . . ?
C12A C7A O2 119.9(2) . . ?
C12A C7A C8A 120.2(2) . . ?
O2 C7A C8A 119.8(2) . . ?
C13A C18A C17A 122.0(2) . . ?
C13A C18A H18A 119.0 . . ?
C17A C18A H18A 119.0 . . ?
C5A C4A C3A 118.1(2) . . ?
C5A C4A C4B 123.2(2) . . ?
C3A C4A C4B 118.7(2) . . ?
O6 C3B O5 115.40(18) . . ?
O6 C3B H3B1 108.4 . . ?
O5 C3B H3B1 108.4 . . ?
O6 C3B H3B2 108.4 . . ?
O5 C3B H3B2 108.4 . . ?
H3B1 C3B H3B2 107.5 . . ?
C5A C5B C32A 110.21(19) . . ?
C5A C5B H5B1 109.6 . . ?
C32A C5B H5B1 109.6 . . ?
C5A C5B H5B2 109.6 . . ?
C32A C5B H5B2 109.6 . . ?
H5B1 C5B H5B2 108.1 . . ?
C31A C6B C28A 109.74(19) . . ?
C31A C6B H6B1 109.7 . . ?
C28A C6B H6B1 109.7 . . ?
C31A C6B H6B2 109.7 . . ?
C28A C6B H6B2 109.7 . . ?
H6B1 C6B H6B2 108.2 . . ?
C17A C7B C10A 113.90(19) . . ?
C17A C7B H7B1 108.8 . . ?
C10A C7B H7B1 108.8 . . ?
C17A C7B H7B2 108.8 . . ?
C10A C7B H7B2 108.8 . . ?
H7B1 C7B H7B2 107.7 . . ?
O6 C23A C24A 126.8(2) . . ?
O6 C23A C22A 114.0(2) . . ?
C24A C23A C22A 119.2(2) . . ?
C4A C4B C27A 113.28(18) . . ?
C4A C4B H4B1 108.9 . . ?
C27A C4B H4B1 108.9 . . ?
C4A C4B H4B2 108.9 . . ?
C27A C4B H4B2 108.9 . . ?
H4B1 C4B H4B2 107.7 . . ?
C3S C3S Cl3 108.7(2) 3_675 . ?
C3S C3S H3S1 109.9 3_675 . ?
Cl3 C3S H3S1 109.9 . . ?
C3S C3S H3S2 109.9 3_675 . ?
Cl3 C3S H3S2 109.9 . . ?
H3S1 C3S H3S2 108.3 . . ?
C22A C21A C20A 122.2(2) . . ?
C22A C21A H21A 118.9 . . ?
C20A C21A H21A 118.9 . . ?
C27A C28A C29A 118.4(2) . . ?
C27A C28A C6B 124.1(2) . . ?
C29A C28A C6B 117.3(2) . . ?
C2A C3A C4A 122.6(2) . . ?
C2A C3A H3A 118.7 . . ?
C4A C3A H3A 118.7 . . ?
O2M C2M H2M1 109.5 . . ?
O2M C2M H2M2 109.5 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.5 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?
C31A C32A C33A 118.4(2) . . ?
C31A C32A C5B 123.6(2) . . ?
C33A C32A C5B 118.0(2) . . ?
C35A C36A C31A 120.8(2) . . ?
C35A C36A H36A 119.6 . . ?
C31A C36A H36A 119.6 . . ?
O4 C2B O3 108.75(18) . . ?
O4 C2B H2B1 109.9 . . ?
O3 C2B H2B1 109.9 . . ?
O4 C2B H2B2 109.9 . . ?
O3 C2B H2B2 109.9 . . ?
H2B1 C2B H2B2 108.3 . . ?
C32A C31A C36A 119.6(2) . . ?
C32A C31A C6B 123.6(2) . . ?
C36A C31A C6B 116.7(2) . . ?
C11A C9B C20A 112.53(19) . . ?
C11A C9B H9B1 109.1 . . ?
C20A C9B H9B1 109.1 . . ?
C11A C9B H9B2 109.1 . . ?
C20A C9B H9B2 109.1 . . ?
H9B1 C9B H9B2 107.8 . . ?
C4A C5A C6A 119.5(2) . . ?
C4A C5A C5B 124.0(2) . . ?
C6A C5A C5B 116.4(2) . . ?
C3A C2A C1A 118.9(2) . . ?
C3A C2A H2A 120.5 . . ?
C1A C2A H2A 120.5 . . ?
C30A C29A C28A 121.6(2) . . ?
C30A C29A H29A 119.2 . . ?
C28A C29A H29A 119.2 . . ?
C21A C22A O3M 120.9(2) . . ?
C21A C22A C23A 119.4(2) . . ?
O3M C22A C23A 119.7(2) . . ?
C8A C9A C10A 121.7(2) . . ?
C8A C9A H9A 119.1 . . ?
C10A C9A H9A 119.1 . . ?
O1 C1A C6A 124.0(2) . . ?
O1 C1A C2A 116.3(2) . . ?
C6A C1A C2A 119.7(2) . . ?
O1M C8A C9A 124.8(2) . . ?
O1M C8A C7A 116.8(2) . . ?
C9A C8A C7A 118.4(2) . . ?
O3M C3M H3M1 109.5 . . ?
O3M C3M H3M2 109.5 . . ?
H3M1 C3M H3M2 109.5 . . ?
O3M C3M H3M3 109.5 . . ?
H3M1 C3M H3M3 109.5 . . ?
H3M2 C3M H3M3 109.5 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C1S C2S Cl2 108.8(2) . . ?
C1S C2S H2S1 109.9 . . ?
Cl2 C2S H2S1 109.9 . . ?
C1S C2S H2S2 109.9 . . ?
Cl2 C2S H2S2 109.9 . . ?
H2S1 C2S H2S2 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 1027977'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_13037

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            trisbromo-cryptophane-111
_chemical_formula_moiety         
'0.018 (C45 H30 Br6 O6), 0.982 (C45 H33 Br3 O6)'
_chemical_formula_sum            'C45 H32.94 Br3.06 O6'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Nitrobenzene'
_chemical_melting_point          ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         913.78

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'
Br Br -0.2901 2.4595 '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_int_tables_number      14
_chemical_absolute_configuration ?

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                   10.6375(10)
_cell_length_b                   30.647(3)
_cell_length_c                   11.2147(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.9160(10)
_cell_angle_gamma                90.00
_cell_volume                     3636.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6910
_cell_measurement_theta_min      2.259
_cell_measurement_theta_max      27.079
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1831
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART, Bruker APEXII CCD'
_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            28012
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.99
_reflns_number_total             8291
_reflns_number_gt                6427
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-97, G. Sheldrick (1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, L. Barbour (1999); http://x-seed.net/'
_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. 

 Electron densities greater 1e-/A3 were found at the rim of the CTB cups that
 were modeled as being associated with 1.8% occupancy of hexabromo-cryptophane-
 111 impurities.
 This result was consistent in multiple crystals and also observed by NMR
 Spectroscopy. The atoms from trisbromo-cryptophane-111 corresponding to 
 these positions were modeled with a 98.2% occupancy.
;
_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)+(0.0538P)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         8291
_refine_ls_number_parameters     504
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Br1 Br 0.04901(3) 0.055434(10) 0.62747(3) 0.02143(9) Uani 0.98 1 d P A 1
Br2 Br 0.24837(3) 0.288626(10) 0.21218(3) 0.02681(9) Uani 1 1 d . A 1
Br3 Br 0.34655(3) 0.038935(10) -0.13752(3) 0.02321(9) Uani 1 1 d . A 1
Br4 Br 0.118(3) 0.0639(10) 0.640(3) 0.058(8) Uiso 0.02 1 d P B 2
Br5 Br 0.202(3) 0.2659(10) 0.526(3) 0.065(7) Uiso 0.02 1 d P C 2
Br6 Br 0.5526(18) 0.1360(6) -0.1385(17) 0.030(4) Uiso 0.02 1 d P D 2
Br7 Br 0.206(2) -0.0321(8) 0.460(2) 0.053(6) Uiso 0.02 1 d P E 2
O1 O 0.0099(2) 0.15166(7) 0.62151(17) 0.0215(5) Uani 1 1 d . A 1
O2 O 0.3013(2) 0.24086(7) -0.0160(2) 0.0276(5) Uani 1 1 d . A 1
O3 O 0.27821(19) -0.00962(7) 0.07174(18) 0.0217(5) Uani 1 1 d . A 1
O4 O 0.19166(19) 0.18990(7) 0.68747(18) 0.0233(5) Uani 1 1 d . A 1
O5 O 0.4981(2) 0.21036(7) -0.02383(19) 0.0244(5) Uani 1 1 d . A 1
O6 O 0.23907(19) -0.02738(7) 0.27171(19) 0.0228(5) Uani 1 1 d . A 1
C1 C -0.0134(3) 0.13504(10) 0.5069(3) 0.0179(6) Uani 1 1 d . A 1
C2 C -0.0576(3) 0.15981(10) 0.4079(3) 0.0184(6) Uani 1 1 d . A 1
H2 H -0.0702 0.1902 0.4179 0.022 Uiso 1 1 calc R A 1
C3 C -0.0843(2) 0.14171(9) 0.2943(2) 0.0150(6) Uani 1 1 d . A 1
C4 C -0.0707(3) 0.09654(9) 0.2789(3) 0.0158(6) Uani 1 1 d . A 1
C5 C -0.0296(3) 0.07155(9) 0.3800(3) 0.0171(6) Uani 1 1 d . A 1
H5 H -0.0209 0.0409 0.3719 0.021 Uiso 1 1 calc R A 1
C6 C -0.0014(3) 0.09043(9) 0.4912(3) 0.0170(6) Uani 1 1 d . A 1
C7 C 0.1959(3) 0.22369(9) 0.0305(3) 0.0190(6) Uani 1 1 d . A 1
C8 C 0.1217(3) 0.19161(9) -0.0275(3) 0.0187(6) Uani 1 1 d . A 1
H8 H 0.1424 0.1812 -0.1029 0.022 Uiso 1 1 calc R A 1
C9 C 0.0172(3) 0.17407(9) 0.0213(3) 0.0167(6) Uani 1 1 d . A 1
C10 C -0.0161(3) 0.19017(9) 0.1304(3) 0.0164(6) Uani 1 1 d . A 1
C11 C 0.0563(3) 0.22400(9) 0.1854(3) 0.0171(6) Uani 1 1 d . A 1
H11 H 0.0335 0.2359 0.2584 0.021 Uiso 1 1 calc R A 1
C12 C 0.1597(3) 0.24059(9) 0.1366(3) 0.0183(6) Uani 1 1 d . A 1
C13 C 0.1890(3) 0.02261(10) 0.0489(3) 0.0184(6) Uani 1 1 d . A 1
C14 C 0.0855(3) 0.03057(9) 0.1118(3) 0.0183(6) Uani 1 1 d . A 1
H14 H 0.0689 0.0115 0.1751 0.022 Uiso 1 1 calc R A 1
C15 C 0.0050(3) 0.06606(9) 0.0843(2) 0.0162(6) Uani 1 1 d . A 1
C16 C 0.0275(3) 0.09391(9) -0.0110(2) 0.0166(6) Uani 1 1 d . A 1
C17 C 0.1296(3) 0.08502(10) -0.0760(3) 0.0186(6) Uani 1 1 d . A 1
H17 H 0.1446 0.1032 -0.1417 0.022 Uiso 1 1 calc R A 1
C18 C 0.2094(3) 0.05004(9) -0.0462(3) 0.0179(6) Uani 1 1 d . A 1
C19 C 0.2829(3) 0.18342(10) 0.6072(2) 0.0195(6) Uani 1 1 d . A 1
C20 C 0.3559(3) 0.14624(10) 0.6208(3) 0.0198(6) Uani 1 1 d . A 1
H20 H 0.3378 0.1250 0.6784 0.024 Uiso 1 1 calc R A 1
C21 C 0.4562(3) 0.13910(10) 0.5515(3) 0.0193(6) Uani 1 1 d . A 1
C22 C 0.4832(3) 0.17138(10) 0.4684(3) 0.0184(6) Uani 1 1 d . A 1
C23 C 0.4061(3) 0.20823(10) 0.4546(3) 0.0231(7) Uani 1 1 d . A 1
H23 H 0.4230 0.2297 0.3972 0.028 Uiso 1 1 calc R A 1
C24 C 0.3049(3) 0.21448(10) 0.5225(3) 0.0223(7) Uani 1 1 d . A 1
H24 H 0.2523 0.2395 0.5109 0.027 Uiso 0.98 1 calc PR A 1
C25 C 0.5183(3) 0.17656(10) 0.0605(3) 0.0225(7) Uani 1 1 d . A 1
C26 C 0.5398(3) 0.18663(10) 0.1811(3) 0.0207(6) Uani 1 1 d . A 1
H26 H 0.5348 0.2162 0.2060 0.025 Uiso 1 1 calc R A 1
C27 C 0.5686(3) 0.15431(10) 0.2667(3) 0.0182(6) Uani 1 1 d . A 1
C28 C 0.5750(3) 0.11074(10) 0.2301(3) 0.0184(6) Uani 1 1 d . A 1
C29 C 0.5521(3) 0.10108(10) 0.1071(3) 0.0220(7) Uani 1 1 d . A 1
H29 H 0.5560 0.0716 0.0814 0.026 Uiso 1 1 calc R A 1
C30 C 0.5241(3) 0.13362(10) 0.0225(3) 0.0247(7) Uani 1 1 d . A 1
H30 H 0.5091 0.1266 -0.0602 0.030 Uiso 0.98 1 calc PR A 1
C31 C 0.3195(3) 0.00214(9) 0.3354(3) 0.0189(6) Uani 1 1 d . A 1
C32 C 0.4227(3) 0.02267(9) 0.2939(3) 0.0174(6) Uani 1 1 d . A 1
H32 H 0.4447 0.0164 0.2158 0.021 Uiso 1 1 calc R A 1
C33 C 0.4949(3) 0.05260(9) 0.3663(3) 0.0179(6) Uani 1 1 d . A 1
C34 C 0.4603(3) 0.06206(9) 0.4806(3) 0.0181(6) Uani 1 1 d . A 1
C35 C 0.3561(3) 0.04080(10) 0.5184(3) 0.0216(6) Uani 1 1 d . A 1
H35 H 0.3325 0.0469 0.5961 0.026 Uiso 1 1 calc R A 1
C36 C 0.2860(3) 0.01140(10) 0.4480(3) 0.0228(7) Uani 1 1 d . A 1
H36 H 0.2151 -0.0025 0.4765 0.027 Uiso 0.98 1 calc PR A 1
C37 C -0.1269(3) 0.17273(9) 0.1917(3) 0.0179(6) Uani 1 1 d . A 1
H37A H -0.1858 0.1572 0.1321 0.021 Uiso 1 1 calc R A 1
H37B H -0.1731 0.1975 0.2233 0.021 Uiso 1 1 calc R A 1
C38 C -0.0474(3) 0.13536(9) -0.0437(3) 0.0182(6) Uani 1 1 d . A 1
H38A H -0.0527 0.1402 -0.1314 0.022 Uiso 1 1 calc R A 1
H38B H -0.1344 0.1323 -0.0208 0.022 Uiso 1 1 calc R A 1
C39 C -0.1041(3) 0.07269(9) 0.1602(3) 0.0181(6) Uani 1 1 d . A 1
H39A H -0.1393 0.0437 0.1775 0.022 Uiso 1 1 calc R A 1
H39B H -0.1714 0.0893 0.1123 0.022 Uiso 1 1 calc R A 1
C40 C 0.5973(3) 0.16889(10) 0.3966(3) 0.0211(6) Uani 1 1 d . A 1
H40A H 0.6375 0.1980 0.3973 0.025 Uiso 1 1 calc R A 1
H40B H 0.6595 0.1484 0.4376 0.025 Uiso 1 1 calc R A 1
C41 C 0.6084(3) 0.07326(10) 0.3165(3) 0.0192(6) Uani 1 1 d . A 1
H41A H 0.6533 0.0505 0.2747 0.023 Uiso 1 1 calc R A 1
H41B H 0.6672 0.0842 0.3842 0.023 Uiso 1 1 calc R A 1
C42 C 0.5262(3) 0.09602(10) 0.5650(3) 0.0206(6) Uani 1 1 d . A 1
H42A H 0.5286 0.0857 0.6489 0.025 Uiso 1 1 calc R A 1
H42B H 0.6143 0.1001 0.5461 0.025 Uiso 1 1 calc R A 1
C43 C 0.0655(3) 0.19350(10) 0.6373(3) 0.0219(6) Uani 1 1 d . A 1
H43A H 0.0624 0.2085 0.5590 0.026 Uiso 1 1 calc R A 1
H43B H 0.0172 0.2112 0.6908 0.026 Uiso 1 1 calc R A 1
C44 C 0.3746(3) 0.21314(10) -0.0813(3) 0.0231(7) Uani 1 1 d . A 1
H44A H 0.3361 0.1837 -0.0873 0.028 Uiso 1 1 calc R A 1
H44B H 0.3769 0.2247 -0.1635 0.028 Uiso 1 1 calc R A 1
C45 C 0.2634(3) -0.04217(9) 0.1585(3) 0.0203(6) Uani 1 1 d . A 1
H45A H 0.1931 -0.0615 0.1273 0.024 Uiso 1 1 calc R A 1
H45B H 0.3413 -0.0601 0.1680 0.024 Uiso 1 1 calc R A 1


_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
Br1 C6 1.898(3) . ?
Br2 C12 1.900(3) . ?
Br3 C18 1.897(3) . ?
O1 C1 1.381(3) . ?
O1 C43 1.416(4) . ?
O2 C7 1.388(3) . ?
O2 C44 1.409(4) . ?
O3 C13 1.375(3) . ?
O3 C45 1.414(3) . ?
O4 C19 1.404(3) . ?
O4 C43 1.405(3) . ?
O5 C25 1.404(4) . ?
O5 C44 1.405(4) . ?
O6 C31 1.391(4) . ?
O6 C45 1.397(4) . ?
C1 C6 1.386(4) . ?
C1 C2 1.387(4) . ?
C2 C3 1.391(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(4) . ?
C3 C37 1.524(4) . ?
C4 C5 1.401(4) . ?
C4 C39 1.529(4) . ?
C5 C6 1.379(4) . ?
C5 H5 0.9500 . ?
C7 C8 1.381(4) . ?
C7 C12 1.388(4) . ?
C8 C9 1.398(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(4) . ?
C9 C38 1.519(4) . ?
C10 C11 1.396(4) . ?
C10 C37 1.522(4) . ?
C11 C12 1.375(4) . ?
C11 H11 0.9500 . ?
C13 C14 1.389(4) . ?
C13 C18 1.392(4) . ?
C14 C15 1.399(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.407(4) . ?
C15 C39 1.521(4) . ?
C16 C17 1.396(4) . ?
C16 C38 1.524(4) . ?
C17 C18 1.387(4) . ?
C17 H17 0.9500 . ?
C19 C20 1.378(4) . ?
C19 C24 1.382(4) . ?
C20 C21 1.400(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.409(4) . ?
C21 C42 1.516(4) . ?
C22 C23 1.395(4) . ?
C22 C40 1.526(4) . ?
C23 C24 1.395(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.383(4) . ?
C25 C30 1.387(4) . ?
C26 C27 1.391(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.401(4) . ?
C27 C40 1.525(4) . ?
C28 C29 1.407(4) . ?
C28 C41 1.521(4) . ?
C29 C30 1.387(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.377(4) . ?
C31 C32 1.387(4) . ?
C32 C33 1.400(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(4) . ?
C33 C41 1.520(4) . ?
C34 C35 1.390(4) . ?
C34 C42 1.527(4) . ?
C35 C36 1.367(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C43 118.9(2) . . ?
C7 O2 C44 118.6(2) . . ?
C13 O3 C45 120.7(2) . . ?
C19 O4 C43 116.7(2) . . ?
C25 O5 C44 115.1(2) . . ?
C31 O6 C45 121.1(2) . . ?
O1 C1 C6 118.1(3) . . ?
O1 C1 C2 123.9(3) . . ?
C6 C1 C2 117.8(3) . . ?
C1 C2 C3 122.4(3) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 C37 117.3(3) . . ?
C4 C3 C37 123.3(3) . . ?
C5 C4 C3 117.8(3) . . ?
C5 C4 C39 118.0(2) . . ?
C3 C4 C39 124.1(3) . . ?
C6 C5 C4 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 120.9(3) . . ?
C5 C6 Br1 120.5(2) . . ?
C1 C6 Br1 118.5(2) . . ?
C8 C7 O2 122.5(3) . . ?
C8 C7 C12 118.3(3) . . ?
O2 C7 C12 119.1(3) . . ?
C7 C8 C9 121.9(3) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 C38 123.6(3) . . ?
C8 C9 C38 116.8(3) . . ?
C11 C10 C9 118.1(3) . . ?
C11 C10 C37 118.6(3) . . ?
C9 C10 C37 123.3(3) . . ?
C12 C11 C10 121.7(3) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C7 120.5(3) . . ?
C11 C12 Br2 119.3(2) . . ?
C7 C12 Br2 120.2(2) . . ?
O3 C13 C14 126.8(3) . . ?
O3 C13 C18 114.6(3) . . ?
C14 C13 C18 118.5(3) . . ?
C13 C14 C15 121.6(3) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C16 119.4(3) . . ?
C14 C15 C39 117.7(3) . . ?
C16 C15 C39 122.9(3) . . ?
C17 C16 C15 118.7(3) . . ?
C17 C16 C38 116.9(3) . . ?
C15 C16 C38 124.3(3) . . ?
C18 C17 C16 121.0(3) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C13 120.7(3) . . ?
C17 C18 Br3 119.6(2) . . ?
C13 C18 Br3 119.6(2) . . ?
C20 C19 C24 120.8(3) . . ?
C20 C19 O4 117.7(3) . . ?
C24 C19 O4 121.4(3) . . ?
C19 C20 C21 121.4(3) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C22 118.5(3) . . ?
C20 C21 C42 118.4(3) . . ?
C22 C21 C42 123.1(3) . . ?
C23 C22 C21 118.9(3) . . ?
C23 C22 C40 118.2(3) . . ?
C21 C22 C40 122.8(3) . . ?
C24 C23 C22 121.9(3) . . ?
C24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C19 C24 C23 118.4(3) . . ?
C19 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C26 C25 C30 120.3(3) . . ?
C26 C25 O5 119.5(3) . . ?
C30 C25 O5 120.1(3) . . ?
C25 C26 C27 121.2(3) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C26 C27 C28 119.4(3) . . ?
C26 C27 C40 117.3(3) . . ?
C28 C27 C40 123.3(3) . . ?
C27 C28 C29 118.6(3) . . ?
C27 C28 C41 123.2(3) . . ?
C29 C28 C41 118.1(3) . . ?
C30 C29 C28 121.5(3) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C25 C30 C29 119.1(3) . . ?
C25 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C36 C31 C32 120.2(3) . . ?
C36 C31 O6 113.7(3) . . ?
C32 C31 O6 126.1(3) . . ?
C31 C32 C33 120.6(3) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C34 119.1(3) . . ?
C32 C33 C41 118.0(3) . . ?
C34 C33 C41 122.9(3) . . ?
C35 C34 C33 118.4(3) . . ?
C35 C34 C42 117.4(3) . . ?
C33 C34 C42 124.2(3) . . ?
C36 C35 C34 122.5(3) . . ?
C36 C35 H35 118.7 . . ?
C34 C35 H35 118.7 . . ?
C35 C36 C31 119.3(3) . . ?
C35 C36 H36 120.4 . . ?
C31 C36 H36 120.4 . . ?
C10 C37 C3 112.1(2) . . ?
C10 C37 H37A 109.2 . . ?
C3 C37 H37A 109.2 . . ?
C10 C37 H37B 109.2 . . ?
C3 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C9 C38 C16 109.6(2) . . ?
C9 C38 H38A 109.7 . . ?
C16 C38 H38A 109.7 . . ?
C9 C38 H38B 109.7 . . ?
C16 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C15 C39 C4 115.4(2) . . ?
C15 C39 H39A 108.4 . . ?
C4 C39 H39A 108.4 . . ?
C15 C39 H39B 108.4 . . ?
C4 C39 H39B 108.4 . . ?
H39A C39 H39B 107.5 . . ?
C27 C40 C22 115.3(2) . . ?
C27 C40 H40A 108.5 . . ?
C22 C40 H40A 108.5 . . ?
C27 C40 H40B 108.5 . . ?
C22 C40 H40B 108.5 . . ?
H40A C40 H40B 107.5 . . ?
C33 C41 C28 114.0(2) . . ?
C33 C41 H41A 108.8 . . ?
C28 C41 H41A 108.8 . . ?
C33 C41 H41B 108.8 . . ?
C28 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
C21 C42 C34 110.0(2) . . ?
C21 C42 H42A 109.7 . . ?
C34 C42 H42A 109.7 . . ?
C21 C42 H42B 109.7 . . ?
C34 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
O4 C43 O1 110.4(2) . . ?
O4 C43 H43A 109.6 . . ?
O1 C43 H43A 109.6 . . ?
O4 C43 H43B 109.6 . . ?
O1 C43 H43B 109.6 . . ?
H43A C43 H43B 108.1 . . ?
O5 C44 O2 109.8(2) . . ?
O5 C44 H44A 109.7 . . ?
O2 C44 H44A 109.7 . . ?
O5 C44 H44B 109.7 . . ?
O2 C44 H44B 109.7 . . ?
H44A C44 H44B 108.2 . . ?
O6 C45 O3 116.2(2) . . ?
O6 C45 H45A 108.2 . . ?
O3 C45 H45A 108.2 . . ?
O6 C45 H45B 108.2 . . ?
O3 C45 H45B 108.2 . . ?
H45A C45 H45B 107.4 . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.098
_database_code_depnum_ccdc_archive 'CCDC 1027974'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_13004

_vrf_PLAT434_13004               
;
RESPONSE:
Caused by the presence of hexabromo-cryptophane-111 impurities
Explained further under _refine_special_details  
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            Xe@trisbromo-cryptophane-111
_chemical_formula_moiety         
'0.96 (Xe), 0.018 (C45 H30 Br6 O6), 0.982 (C45 H33 Br3 O6)'
_chemical_formula_sum            'C45 H32.94 Br3.06 O6 Xe0.96'
_chemical_melting_point          ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1039.83

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Xe Xe -0.4205 1.9578 '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_int_tables_number      14
_chemical_absolute_configuration ?

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                   10.85910(10)
_cell_length_b                   30.5071(4)
_cell_length_c                   11.08070(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.2160(10)
_cell_angle_gamma                90.00
_cell_volume                     3660.88(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10725
_cell_measurement_theta_min      2.276
_cell_measurement_theta_max      29.653
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2039
_exptl_absorpt_coefficient_mu    4.293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6654
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker, APEX Duo'
_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            26976
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         28.00
_reflns_number_total             8852
_reflns_number_gt                6629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-97, G. Sheldrick (1990)'
_computing_structure_refinement  'SHELXL-97-2, G. Sheldrick (1997)'
_computing_molecular_graphics    'X-SEED, L. Barbour (1999); http://x-seed.net/'
_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. 

 Electron densities greater 1e-/A3 were found at the rim of the CTB cups that
 were modeled as being associated with 1.8% occupancy of hexabromo-cryptophane-
 111 impurities. This caused a level A alert in the CheckCIF.
 This result was consistent in multiple crystals and also observed by NMR
 Spectroscopy. The atoms from trisbromo-cryptophane-111 corresponding to 
 these positions were modeled with a 98.2% occupancy. 
;
_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)+(0.0366P)²+2.7475P] 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         8852
_refine_ls_number_parameters     513
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Xe1 Xe 0.24860(2) 0.126734(7) 0.26020(2) 0.01880(6) Uani 0.96 1 d P A 1
Br1 Br 0.25120(3) 0.286818(12) 0.21681(3) 0.02507(9) Uani 0.98 1 d P B 1
Br2 Br 0.04420(4) 0.056055(11) 0.62575(3) 0.02359(9) Uani 1 1 d . B 1
Br3 Br 0.34608(4) 0.040733(12) -0.13688(3) 0.02544(9) Uani 1 1 d . B 1
Br4 Br 0.2110(16) 0.3179(6) 0.2504(15) 0.015(3) Uiso 0.02 1 d P . 2
Br5 Br 0.563(2) 0.1318(7) -0.138(2) 0.034(5) Uiso 0.02 1 d P . 2
Br6 Br 0.229(3) 0.2639(9) 0.510(2) 0.046(6) Uiso 0.02 1 d P C 2
Br7 Br 0.203(3) -0.0319(9) 0.469(2) 0.048(6) Uiso 0.02 1 d P D 2
O1 O 0.3064(2) 0.23860(8) -0.0128(2) 0.0258(6) Uani 1 1 d . B 1
O2 O 0.0186(2) 0.15302(7) 0.6185(2) 0.0206(5) Uani 1 1 d . B 1
O3 O 0.2738(2) -0.00814(8) 0.0725(2) 0.0255(6) Uani 1 1 d . B 1
O4 O 0.4992(2) 0.20851(7) -0.0202(2) 0.0215(5) Uani 1 1 d . B 1
O5 O 0.1944(2) 0.19099(8) 0.6839(2) 0.0231(5) Uani 1 1 d . B 1
O6 O 0.2374(2) -0.02587(8) 0.2744(2) 0.0253(6) Uani 1 1 d . B 1
C1 C 0.1989(3) 0.22312(11) 0.0303(3) 0.0187(7) Uani 1 1 d . B 1
C2 C 0.1247(3) 0.19182(11) -0.0295(3) 0.0187(7) Uani 1 1 d . B 1
H2 H 0.1462 0.1814 -0.1060 0.022 Uiso 1 1 calc R B 1
C3 C 0.0193(3) 0.17502(10) 0.0189(3) 0.0169(7) Uani 1 1 d . B 1
C4 C -0.0165(3) 0.19180(10) 0.1289(3) 0.0158(7) Uani 1 1 d . B 1
C5 C 0.0549(3) 0.22540(10) 0.1850(3) 0.0173(7) Uani 1 1 d . B 1
H5 H 0.0299 0.2379 0.2578 0.021 Uiso 1 1 calc R B 1
C6 C 0.1603(3) 0.24078(10) 0.1372(3) 0.0189(7) Uani 1 1 d . B 1
C7 C -0.0127(3) 0.13604(11) 0.5049(3) 0.0173(7) Uani 1 1 d . B 1
C8 C -0.0571(3) 0.16133(11) 0.4072(3) 0.0162(7) Uani 1 1 d . B 1
H8 H -0.0671 0.1920 0.4181 0.019 Uiso 1 1 calc R B 1
C9 C -0.0874(3) 0.14299(11) 0.2931(3) 0.0158(7) Uani 1 1 d . B 1
C10 C -0.0770(3) 0.09727(11) 0.2781(3) 0.0173(7) Uani 1 1 d . B 1
C11 C -0.0381(3) 0.07198(11) 0.3784(3) 0.0186(7) Uani 1 1 d . B 1
H11 H -0.0334 0.0410 0.3700 0.022 Uiso 1 1 calc R B 1
C12 C -0.0059(3) 0.09086(11) 0.4905(3) 0.0170(7) Uani 1 1 d . B 1
C13 C 0.1851(3) 0.02372(11) 0.0481(3) 0.0218(7) Uani 1 1 d . B 1
C14 C 0.0812(3) 0.03100(11) 0.1108(3) 0.0195(7) Uani 1 1 d . B 1
H14 H 0.0631 0.0116 0.1741 0.023 Uiso 1 1 calc R B 1
C15 C 0.0016(3) 0.06681(11) 0.0821(3) 0.0185(7) Uani 1 1 d . B 1
C16 C 0.0273(3) 0.09479(11) -0.0130(3) 0.0175(7) Uani 1 1 d . B 1
C17 C 0.1294(3) 0.08586(11) -0.0777(3) 0.0189(7) Uani 1 1 d . B 1
H17 H 0.1458 0.1040 -0.1444 0.023 Uiso 1 1 calc R B 1
C18 C 0.2070(3) 0.05144(11) -0.0471(3) 0.0189(7) Uani 1 1 d . B 1
C19 C 0.5226(3) 0.17468(11) 0.0635(3) 0.0198(7) Uani 1 1 d . B 1
C20 C 0.5489(3) 0.18457(11) 0.1844(3) 0.0195(7) Uani 1 1 d . B 1
H20 H 0.5465 0.2143 0.2096 0.023 Uiso 1 1 calc R B 1
C21 C 0.5790(3) 0.15216(11) 0.2709(3) 0.0169(7) Uani 1 1 d . B 1
C22 C 0.5826(3) 0.10827(11) 0.2329(3) 0.0187(7) Uani 1 1 d . B 1
C23 C 0.5571(3) 0.09892(11) 0.1095(3) 0.0230(8) Uani 1 1 d . B 1
H23 H 0.5601 0.0694 0.0828 0.028 Uiso 1 1 calc R B 1
C24 C 0.5275(3) 0.13170(11) 0.0252(3) 0.0242(8) Uani 1 1 d . B 1
H24 H 0.5108 0.1246 -0.0579 0.029 Uiso 0.98 1 calc PR B 1
C25 C 0.2888(3) 0.18374(11) 0.6061(3) 0.0179(7) Uani 1 1 d . B 1
C26 C 0.3574(3) 0.14588(11) 0.6217(3) 0.0194(7) Uani 1 1 d . B 1
H26 H 0.3348 0.1246 0.6786 0.023 Uiso 1 1 calc R B 1
C27 C 0.4598(3) 0.13831(11) 0.5548(3) 0.0172(7) Uani 1 1 d . B 1
C28 C 0.4938(3) 0.17064(11) 0.4733(3) 0.0169(7) Uani 1 1 d . B 1
C29 C 0.4221(3) 0.20814(11) 0.4595(3) 0.0194(7) Uani 1 1 d . B 1
H29 H 0.4441 0.2298 0.4034 0.023 Uiso 1 1 calc R B 1
C30 C 0.3192(3) 0.21519(11) 0.5245(3) 0.0198(7) Uani 1 1 d . B 1
H30 H 0.2711 0.2411 0.5129 0.024 Uiso 0.98 1 calc PR B 1
C31 C 0.3190(3) 0.00251(11) 0.3373(3) 0.0225(8) Uani 1 1 d . B 1
C32 C 0.4240(3) 0.02091(11) 0.2955(3) 0.0207(7) Uani 1 1 d . B 1
H32 H 0.4476 0.0138 0.2170 0.025 Uiso 1 1 calc R B 1
C33 C 0.4967(3) 0.05033(11) 0.3692(3) 0.0187(7) Uani 1 1 d . B 1
C34 C 0.4599(3) 0.06085(11) 0.4836(3) 0.0188(7) Uani 1 1 d . B 1
C35 C 0.3530(3) 0.04096(11) 0.5220(3) 0.0239(8) Uani 1 1 d . B 1
H35 H 0.3281 0.0476 0.6004 0.029 Uiso 1 1 calc R B 1
C36 C 0.2834(3) 0.01248(11) 0.4510(3) 0.0228(8) Uani 1 1 d . B 1
H36 H 0.2113 -0.0003 0.4795 0.027 Uiso 0.98 1 calc PR B 1
C37 C -0.1266(3) 0.17433(11) 0.1912(3) 0.0174(7) Uani 1 1 d . B 1
H37A H -0.1722 0.1992 0.2241 0.021 Uiso 1 1 calc R B 1
H37B H -0.1831 0.1590 0.1310 0.021 Uiso 1 1 calc R B 1
C38 C -0.1074(3) 0.07342(11) 0.1590(3) 0.0210(7) Uani 1 1 d . B 1
H38A H -0.1720 0.0902 0.1111 0.025 Uiso 1 1 calc R B 1
H38B H -0.1423 0.0444 0.1768 0.025 Uiso 1 1 calc R B 1
C39 C -0.0448(3) 0.13667(11) -0.0466(3) 0.0197(7) Uani 1 1 d . B 1
H39A H -0.0477 0.1414 -0.1352 0.024 Uiso 1 1 calc R B 1
H39B H -0.1305 0.1340 -0.0227 0.024 Uiso 1 1 calc R B 1
C40 C 0.6077(3) 0.16636(11) 0.4014(3) 0.0204(7) Uani 1 1 d . B 1
H40A H 0.6509 0.1950 0.4021 0.024 Uiso 1 1 calc R B 1
H40B H 0.6647 0.1448 0.4422 0.024 Uiso 1 1 calc R B 1
C41 C 0.5240(3) 0.09415(11) 0.5686(3) 0.0208(7) Uani 1 1 d . B 1
H41A H 0.6114 0.0972 0.5500 0.025 Uiso 1 1 calc R B 1
H41B H 0.5223 0.0839 0.6532 0.025 Uiso 1 1 calc R B 1
C42 C 0.6109(3) 0.07005(11) 0.3185(3) 0.0203(7) Uani 1 1 d . B 1
H42A H 0.6679 0.0802 0.3866 0.024 Uiso 1 1 calc R B 1
H42B H 0.6537 0.0469 0.2749 0.024 Uiso 1 1 calc R B 1
C43 C 0.3790(3) 0.20922(11) -0.0760(3) 0.0212(8) Uani 1 1 d . B 1
H43A H 0.3427 0.1795 -0.0752 0.025 Uiso 1 1 calc R B 1
H43B H 0.3810 0.2187 -0.1613 0.025 Uiso 1 1 calc R B 1
C44 C 0.0720(3) 0.19472(11) 0.6292(3) 0.0196(7) Uani 1 1 d . B 1
H44A H 0.0222 0.2137 0.6792 0.024 Uiso 1 1 calc R B 1
H44B H 0.0739 0.2083 0.5481 0.024 Uiso 1 1 calc R B 1
C45 C 0.2597(3) -0.04077(10) 0.1596(3) 0.0188(7) Uani 1 1 d . B 1
H45A H 0.1906 -0.0601 0.1304 0.023 Uiso 1 1 calc R B 1
H45B H 0.3356 -0.0589 0.1663 0.023 Uiso 1 1 calc R B 1


_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
Br1 C6 1.897(3) . ?
Br2 C12 1.884(3) . ?
Br3 C18 1.897(3) . ?
Br4 Br5 2.60(3) 4_566 ?
Br5 Br4 2.60(3) 4_665 ?
O1 C1 1.376(4) . ?
O1 C43 1.413(4) . ?
O2 C7 1.381(4) . ?
O2 C44 1.399(4) . ?
O3 C13 1.381(4) . ?
O3 C45 1.403(4) . ?
O4 C19 1.398(4) . ?
O4 C43 1.403(4) . ?
O5 C25 1.405(4) . ?
O5 C44 1.425(4) . ?
O6 C45 1.388(4) . ?
O6 C31 1.390(4) . ?
C1 C2 1.387(5) . ?
C1 C6 1.394(5) . ?
C2 C3 1.397(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.403(4) . ?
C3 C39 1.518(5) . ?
C4 C5 1.402(5) . ?
C4 C37 1.520(4) . ?
C5 C6 1.378(5) . ?
C5 H5 0.9500 . ?
C7 C8 1.386(5) . ?
C7 C12 1.390(5) . ?
C8 C9 1.400(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.410(5) . ?
C9 C37 1.516(4) . ?
C10 C11 1.393(5) . ?
C10 C38 1.522(4) . ?
C11 C12 1.390(5) . ?
C11 H11 0.9500 . ?
C13 C18 1.386(5) . ?
C13 C14 1.386(5) . ?
C14 C15 1.415(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(5) . ?
C15 C38 1.522(5) . ?
C16 C17 1.391(5) . ?
C16 C39 1.530(5) . ?
C17 C18 1.373(5) . ?
C17 H17 0.9500 . ?
C19 C24 1.381(5) . ?
C19 C20 1.383(5) . ?
C20 C21 1.399(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.405(5) . ?
C21 C40 1.520(5) . ?
C22 C23 1.404(5) . ?
C22 C42 1.520(5) . ?
C23 C24 1.390(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.375(5) . ?
C25 C26 1.378(5) . ?
C26 C27 1.400(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.405(5) . ?
C27 C41 1.519(5) . ?
C28 C29 1.386(5) . ?
C28 C40 1.525(4) . ?
C29 C30 1.390(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.379(5) . ?
C31 C32 1.381(5) . ?
C32 C33 1.414(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.394(5) . ?
C33 C42 1.523(5) . ?
C34 C35 1.404(5) . ?
C34 C41 1.519(5) . ?
C35 C36 1.362(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C43 118.2(3) . . ?
C7 O2 C44 119.4(3) . . ?
C13 O3 C45 121.6(3) . . ?
C19 O4 C43 114.9(3) . . ?
C25 O5 C44 116.8(2) . . ?
C45 O6 C31 121.0(3) . . ?
O1 C1 C2 123.3(3) . . ?
O1 C1 C6 118.6(3) . . ?
C2 C1 C6 118.1(3) . . ?
C1 C2 C3 122.2(3) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 C39 117.3(3) . . ?
C4 C3 C39 123.4(3) . . ?
C5 C4 C3 118.2(3) . . ?
C5 C4 C37 118.9(3) . . ?
C3 C4 C37 122.9(3) . . ?
C6 C5 C4 121.8(3) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 Br1 119.5(3) . . ?
C1 C6 Br1 120.2(3) . . ?
O2 C7 C8 123.5(3) . . ?
O2 C7 C12 117.7(3) . . ?
C8 C7 C12 118.7(3) . . ?
C7 C8 C9 121.9(3) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C10 119.1(3) . . ?
C8 C9 C37 117.1(3) . . ?
C10 C9 C37 123.8(3) . . ?
C11 C10 C9 118.4(3) . . ?
C11 C10 C38 117.4(3) . . ?
C9 C10 C38 124.1(3) . . ?
C12 C11 C10 121.7(3) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C7 C12 C11 120.1(3) . . ?
C7 C12 Br2 118.8(2) . . ?
C11 C12 Br2 121.1(2) . . ?
O3 C13 C18 115.0(3) . . ?
O3 C13 C14 126.6(3) . . ?
C18 C13 C14 118.4(3) . . ?
C13 C14 C15 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 C14 119.2(3) . . ?
C16 C15 C38 123.2(3) . . ?
C14 C15 C38 117.7(3) . . ?
C17 C16 C15 118.6(3) . . ?
C17 C16 C39 116.8(3) . . ?
C15 C16 C39 124.4(3) . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C13 121.2(3) . . ?
C17 C18 Br3 120.0(3) . . ?
C13 C18 Br3 118.8(3) . . ?
C24 C19 C20 119.7(3) . . ?
C24 C19 O4 120.4(3) . . ?
C20 C19 O4 119.8(3) . . ?
C19 C20 C21 122.1(3) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C22 118.6(3) . . ?
C20 C21 C40 118.1(3) . . ?
C22 C21 C40 123.3(3) . . ?
C23 C22 C21 118.5(3) . . ?
C23 C22 C42 117.9(3) . . ?
C21 C22 C42 123.5(3) . . ?
C24 C23 C22 121.8(3) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C19 C24 C23 119.3(3) . . ?
C19 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C30 C25 C26 120.9(3) . . ?
C30 C25 O5 121.0(3) . . ?
C26 C25 O5 117.8(3) . . ?
C25 C26 C27 121.0(3) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C28 118.7(3) . . ?
C26 C27 C41 118.0(3) . . ?
C28 C27 C41 123.1(3) . . ?
C29 C28 C27 118.6(3) . . ?
C29 C28 C40 118.9(3) . . ?
C27 C28 C40 122.5(3) . . ?
C28 C29 C30 122.5(3) . . ?
C28 C29 H29 118.8 . . ?
C30 C29 H29 118.8 . . ?
C25 C30 C29 118.3(3) . . ?
C25 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C36 C31 C32 120.7(3) . . ?
C36 C31 O6 112.6(3) . . ?
C32 C31 O6 126.6(3) . . ?
C31 C32 C33 120.2(3) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 119.1(3) . . ?
C34 C33 C42 122.7(3) . . ?
C32 C33 C42 118.2(3) . . ?
C33 C34 C35 118.3(3) . . ?
C33 C34 C41 124.7(3) . . ?
C35 C34 C41 116.9(3) . . ?
C36 C35 C34 122.4(3) . . ?
C36 C35 H35 118.8 . . ?
C34 C35 H35 118.8 . . ?
C35 C36 C31 119.2(3) . . ?
C35 C36 H36 120.4 . . ?
C31 C36 H36 120.4 . . ?
C9 C37 C4 111.9(3) . . ?
C9 C37 H37A 109.2 . . ?
C4 C37 H37A 109.2 . . ?
C9 C37 H37B 109.2 . . ?
C4 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C10 C38 C15 114.9(3) . . ?
C10 C38 H38A 108.5 . . ?
C15 C38 H38A 108.5 . . ?
C10 C38 H38B 108.5 . . ?
C15 C38 H38B 108.5 . . ?
H38A C38 H38B 107.5 . . ?
C3 C39 C16 108.6(3) . . ?
C3 C39 H39A 110.0 . . ?
C16 C39 H39A 110.0 . . ?
C3 C39 H39B 110.0 . . ?
C16 C39 H39B 110.0 . . ?
H39A C39 H39B 108.4 . . ?
C21 C40 C28 113.8(3) . . ?
C21 C40 H40A 108.8 . . ?
C28 C40 H40A 108.8 . . ?
C21 C40 H40B 108.8 . . ?
C28 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C34 C41 C27 110.2(3) . . ?
C34 C41 H41A 109.6 . . ?
C27 C41 H41A 109.6 . . ?
C34 C41 H41B 109.6 . . ?
C27 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
C22 C42 C33 113.6(3) . . ?
C22 C42 H42A 108.8 . . ?
C33 C42 H42A 108.8 . . ?
C22 C42 H42B 108.8 . . ?
C33 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
O4 C43 O1 109.1(3) . . ?
O4 C43 H43A 109.9 . . ?
O1 C43 H43A 109.9 . . ?
O4 C43 H43B 109.9 . . ?
O1 C43 H43B 109.9 . . ?
H43A C43 H43B 108.3 . . ?
O2 C44 O5 109.3(3) . . ?
O2 C44 H44A 109.8 . . ?
O5 C44 H44A 109.8 . . ?
O2 C44 H44B 109.8 . . ?
O5 C44 H44B 109.8 . . ?
H44A C44 H44B 108.3 . . ?
O6 C45 O3 115.7(3) . . ?
O6 C45 H45A 108.4 . . ?
O3 C45 H45A 108.4 . . ?
O6 C45 H45B 108.4 . . ?
O3 C45 H45B 108.4 . . ?
H45A C45 H45B 107.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.114

#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Nitrobenzene'
_database_code_depnum_ccdc_archive 'CCDC 1027975'
