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

#######################################################################
#
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#                                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.
#
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#  fide research purposes only. It may contain copyright material
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#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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data_3b_s031

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64H80N4O4S2, CHCl3, 3 C2H5OH'
_chemical_formula_sum            'C70.50 H95.50 Cl1.50 N4 O7 S2'
_chemical_formula_weight         1228.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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   'C 1 2/c 1   '
_symmetry_space_group_name_Hall  '-C 2yc      '
_symmetry_int_tables_number      15

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

_cell_length_a                   28.3148(6)
_cell_length_b                   15.8506(3)
_cell_length_c                   18.2260(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.09(1)
_cell_angle_gamma                90.00
_cell_volume                     7216.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6112
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      33.09

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2640
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_absorpt_correction_T_min  0.9445
_exptl_absorpt_correction_T_max  0.9787

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43374
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         28.00
_reflns_number_total             8708
_reflns_number_gt                6891
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART Ver. 5.630 (Bruker-AXS, 2003)'
_computing_cell_refinement       'SAINT Ver. 6.45  (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.45'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

_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)+(0.1700P)²+20.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8708
_refine_ls_number_parameters     420
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0962
_refine_ls_wR_factor_ref         0.2888
_refine_ls_wR_factor_gt          0.2708
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.006
_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
S1 S 0.64162(3) 1.18987(6) 0.49993(5) 0.0364(2) Uani 1 1 d . . .
O1 O 0.43430(8) 0.94662(12) 0.24394(12) 0.0207(4) Uani 1 1 d . . .
O2 O 0.52980(7) 0.95602(11) 0.37774(10) 0.0183(4) Uani 1 1 d . . .
N1 N 0.57982(9) 1.10735(15) 0.35858(14) 0.0228(5) Uani 1 1 d . . .
N2 N 0.66599(10) 1.13400(18) 0.38511(16) 0.0291(5) Uani 1 1 d . . .
C1 C 0.36621(10) 0.88671(17) 0.08356(15) 0.0217(5) Uani 1 1 d . . .
H1B H 0.3294 0.8812 0.0371 0.026 Uiso 1 1 calc R . .
H1A H 0.3747 0.9476 0.0937 0.026 Uiso 1 1 calc R . .
C2 C 0.36925(10) 0.84627(17) 0.16130(16) 0.0204(5) Uani 1 1 d . . .
C3 C 0.40572(10) 0.87531(16) 0.24017(16) 0.0191(5) Uani 1 1 d . . .
C4 C 0.41120(10) 0.83412(16) 0.31189(16) 0.0197(5) Uani 1 1 d . . .
C5 C 0.37903(11) 0.76439(17) 0.30277(17) 0.0241(5) Uani 1 1 d . . .
H5 H 0.3830 0.7360 0.3512 0.029 Uiso 1 1 calc R . .
C6 C 0.34120(11) 0.73473(17) 0.22498(18) 0.0255(6) Uani 1 1 d . A .
C7 C 0.33714(10) 0.77689(18) 0.15550(17) 0.0248(5) Uani 1 1 d . . .
H7 H 0.3116 0.7579 0.1019 0.030 Uiso 1 1 calc R . .
C8 C 0.30413(13) 0.6611(2) 0.2191(2) 0.0353(7) Uani 1 1 d . . .
C9B C 0.2493(8) 0.6982(13) 0.2002(14) 0.130(6) Uiso 0.50 1 d P A 1
H9BB H 0.2378 0.7384 0.1541 0.194 Uiso 0.50 1 calc PR A 1
H9BC H 0.2522 0.7271 0.2496 0.194 Uiso 0.50 1 calc PR A 1
H9BA H 0.2230 0.6526 0.1847 0.194 Uiso 0.50 1 calc PR A 1
C10B C 0.2906(6) 0.6063(9) 0.1433(9) 0.084(3) Uiso 0.50 1 d P A 1
H10D H 0.2662 0.5611 0.1406 0.126 Uiso 0.50 1 calc PR A 1
H10E H 0.3235 0.5815 0.1476 0.126 Uiso 0.50 1 calc PR A 1
H10F H 0.2734 0.6409 0.0929 0.126 Uiso 0.50 1 calc PR A 1
C11B C 0.3259(5) 0.6068(8) 0.2930(8) 0.078(3) Uiso 0.50 1 d P A 1
H11A H 0.3027 0.5574 0.2823 0.117 Uiso 0.50 1 calc PR A 1
H11C H 0.3276 0.6384 0.3404 0.117 Uiso 0.50 1 calc PR A 1
H11B H 0.3619 0.5881 0.3057 0.117 Uiso 0.50 1 calc PR A 1
C9A C 0.2696(3) 0.6899(4) 0.2600(5) 0.0369(14) Uiso 0.50 1 d P A 2
H9AB H 0.2458 0.6438 0.2576 0.055 Uiso 0.50 1 calc PR A 2
H9AC H 0.2480 0.7390 0.2301 0.055 Uiso 0.50 1 calc PR A 2
H9AA H 0.2930 0.7051 0.3182 0.055 Uiso 0.50 1 calc PR A 2
C10A C 0.2668(2) 0.6357(4) 0.1313(4) 0.0281(11) Uiso 0.50 1 d P A 2
H10B H 0.2877 0.6198 0.1031 0.042 Uiso 0.50 1 calc PR A 2
H10C H 0.2433 0.6831 0.1020 0.042 Uiso 0.50 1 calc PR A 2
H10A H 0.2452 0.5875 0.1315 0.042 Uiso 0.50 1 calc PR A 2
C11A C 0.3394(3) 0.5855(5) 0.2667(5) 0.0404(15) Uiso 0.50 1 d P A 2
H11D H 0.3165 0.5372 0.2621 0.061 Uiso 0.50 1 calc PR A 2
H11F H 0.3611 0.6005 0.3254 0.061 Uiso 0.50 1 calc PR A 2
H11E H 0.3629 0.5706 0.2430 0.061 Uiso 0.50 1 calc PR A 2
C12 C 0.44930(10) 0.86605(17) 0.39853(16) 0.0208(5) Uani 1 1 d . . .
H12A H 0.4356 0.8488 0.4372 0.025 Uiso 1 1 calc R . .
H12B H 0.4499 0.9285 0.3975 0.025 Uiso 1 1 calc R . .
C13 C 0.50617(10) 0.83345(17) 0.43133(15) 0.0207(5) Uani 1 1 d . . .
C14 C 0.54415(10) 0.87814(16) 0.41856(14) 0.0184(5) Uani 1 1 d . . .
C15 C 0.59470(10) 0.84491(17) 0.44001(15) 0.0213(5) Uani 1 1 d . . .
C16 C 0.60724(11) 0.76623(18) 0.47962(17) 0.0254(5) Uani 1 1 d . . .
H16 H 0.6416 0.7429 0.4955 0.031 Uiso 1 1 calc R . .
C17 C 0.57178(12) 0.72097(18) 0.49659(18) 0.0287(6) Uani 1 1 d . B .
C18 C 0.52083(12) 0.75563(18) 0.47131(17) 0.0267(6) Uani 1 1 d . . .
H18 H 0.4957 0.7252 0.4817 0.032 Uiso 1 1 calc R . .
C19 C 0.58844(15) 0.6358(2) 0.5425(2) 0.0395(8) Uani 1 1 d . . .
C20B C 0.5447(4) 0.5737(6) 0.5107(6) 0.056(2) Uiso 0.50 1 d P B 2
H20C H 0.5562 0.5228 0.5453 0.084 Uiso 0.50 1 calc PR B 2
H20B H 0.5354 0.5591 0.4532 0.084 Uiso 0.50 1 calc PR B 2
H20A H 0.5134 0.5978 0.5123 0.084 Uiso 0.50 1 calc PR B 2
C21B C 0.6062(4) 0.6525(7) 0.6346(6) 0.060(2) Uiso 0.50 1 d P B 2
H21A H 0.5758 0.6741 0.6407 0.091 Uiso 0.50 1 calc PR B 2
H21C H 0.6351 0.6943 0.6559 0.091 Uiso 0.50 1 calc PR B 2
H21B H 0.6190 0.5999 0.6660 0.091 Uiso 0.50 1 calc PR B 2
C22B C 0.6416(4) 0.6006(6) 0.5463(6) 0.0538(19) Uiso 0.50 1 d P B 2
H22D H 0.6503 0.5458 0.5745 0.081 Uiso 0.50 1 calc PR B 2
H22F H 0.6710 0.6402 0.5771 0.081 Uiso 0.50 1 calc PR B 2
H22E H 0.6367 0.5940 0.4897 0.081 Uiso 0.50 1 calc PR B 2
C20A C 0.5474(8) 0.6037(13) 0.5668(13) 0.122(6) Uiso 0.50 1 d P B 1
H20D H 0.5157 0.5839 0.5171 0.183 Uiso 0.50 1 calc PR B 1
H20F H 0.5373 0.6495 0.5928 0.183 Uiso 0.50 1 calc PR B 1
H20E H 0.5628 0.5570 0.6063 0.183 Uiso 0.50 1 calc PR B 1
C21A C 0.6352(5) 0.6494(7) 0.6283(7) 0.069(3) Uiso 0.50 1 d P B 1
H21E H 0.6277 0.6978 0.6547 0.104 Uiso 0.50 1 calc PR B 1
H21F H 0.6677 0.6603 0.6235 0.104 Uiso 0.50 1 calc PR B 1
H21D H 0.6403 0.5988 0.6622 0.104 Uiso 0.50 1 calc PR B 1
C22A C 0.6124(6) 0.5798(10) 0.4998(10) 0.095(4) Uiso 0.50 1 d P B 1
H22B H 0.6301 0.5310 0.5352 0.143 Uiso 0.50 1 calc PR B 1
H22C H 0.6385 0.6123 0.4905 0.143 Uiso 0.50 1 calc PR B 1
H22A H 0.5838 0.5602 0.4462 0.143 Uiso 0.50 1 calc PR B 1
C23 C 0.53858(10) 1.02852(16) 0.43041(16) 0.0208(5) Uani 1 1 d . . .
H23B H 0.5740 1.0248 0.4805 0.025 Uiso 1 1 calc R . .
H23A H 0.5106 1.0319 0.4483 0.025 Uiso 1 1 calc R . .
C24 C 0.53609(10) 1.10524(17) 0.37893(16) 0.0215(5) Uani 1 1 d . . .
H24A H 0.5017 1.1050 0.3268 0.026 Uiso 1 1 calc R . .
H24B H 0.5372 1.1569 0.4102 0.026 Uiso 1 1 calc R . .
C25 C 0.62811(11) 1.14119(18) 0.40928(17) 0.0245(5) Uani 1 1 d . . .
C26 C 0.65847(11) 1.09962(18) 0.30785(17) 0.0242(5) Uani 1 1 d . . .
C27 C 0.68947(11) 1.03240(19) 0.30835(18) 0.0265(6) Uani 1 1 d . . .
H27 H 0.7146 1.0084 0.3599 0.032 Uiso 1 1 calc R . .
C28 C 0.68449(11) 0.99904(19) 0.23417(19) 0.0287(6) Uani 1 1 d . . .
C29 C 0.64752(12) 1.0362(2) 0.15942(19) 0.0323(6) Uani 1 1 d . . .
H29 H 0.6436 1.0144 0.1083 0.039 Uiso 1 1 calc R . .
C30 C 0.61658(12) 1.1037(2) 0.15852(19) 0.0318(6) Uani 1 1 d . . .
H30 H 0.5916 1.1278 0.1070 0.038 Uiso 1 1 calc R . .
C31 C 0.62182(12) 1.13692(19) 0.23297(18) 0.0280(6) Uani 1 1 d . . .
H31 H 0.6009 1.1839 0.2328 0.034 Uiso 1 1 calc R . .
C32 C 0.71794(14) 0.9254(2) 0.2344(2) 0.0401(8) Uani 1 1 d . . .
H32B H 0.7021 0.9002 0.1788 0.060 Uiso 1 1 calc R . .
H32A H 0.7192 0.8832 0.2746 0.060 Uiso 1 1 calc R . .
H32C H 0.7543 0.9448 0.2500 0.060 Uiso 1 1 calc R . .
O1S O 0.72404(11) 1.3428(2) 0.51762(18) 0.0522(7) Uani 1 1 d . . .
C1S C 0.6962(2) 1.3968(4) 0.4494(4) 0.0805(17) Uani 1 1 d . . .
H1SB H 0.7159 1.4508 0.4598 0.097 Uiso 1 1 calc R . .
H1SA H 0.6605 1.4090 0.4441 0.097 Uiso 1 1 calc R . .
C2S C 0.6897(3) 1.3607(4) 0.3713(4) 0.0834(18) Uani 1 1 d . . .
H2SB H 0.6728 1.4023 0.3267 0.125 Uiso 1 1 calc R . .
H2SA H 0.6670 1.3103 0.3577 0.125 Uiso 1 1 calc R . .
H2SC H 0.7248 1.3451 0.3773 0.125 Uiso 1 1 calc R . .
O3S O 0.5000 0.3066(5) 0.7500 0.0444(16) Uiso 0.50 2 d SP . 3
C5S C 0.5274(5) 0.4078(8) 0.6721(9) 0.033(2) Uiso 0.25 1 d P . 3
H5SB H 0.5154 0.3635 0.6295 0.049 Uiso 0.25 1 calc PR . 3
H5SC H 0.5596 0.4347 0.6760 0.049 Uiso 0.25 1 calc PR . 3
H5SA H 0.4990 0.4500 0.6568 0.049 Uiso 0.25 1 calc PR . 3
C4S C 0.5415(4) 0.3636(6) 0.7670(6) 0.058(2) Uiso 0.50 1 d P . .
O3SA O 0.5758(10) 0.4216(17) 0.8351(16) 0.124(7) Uiso 0.25 1 d P . 4
C5SA C 0.5409(6) 0.4151(10) 0.7134(11) 0.043(3) Uiso 0.25 1 d P . 4
H5SD H 0.5624 0.4648 0.7416 0.065 Uiso 0.25 1 calc PR . 4
H5SE H 0.5039 0.4324 0.6765 0.065 Uiso 0.25 1 calc PR . 4
H5SF H 0.5559 0.3878 0.6807 0.065 Uiso 0.25 1 calc PR . 4
Cl1 Cl 0.55032(17) 0.5432(3) 0.7497(3) 0.0520(9) Uiso 0.25 1 d P . 5
Cl2 Cl 0.54969(18) 0.6650(3) 0.8641(3) 0.0543(9) Uiso 0.25 1 d P . 5
Cl3 Cl 0.5380(3) 0.6640(4) 0.8052(4) 0.0841(16) Uiso 0.25 1 d P . 6
C6S C 0.5080(6) 0.5971(9) 0.7752(8) 0.039(3) Uiso 0.25 1 d P . .
H6SA H 0.4696 0.5960 0.7453 0.047 Uiso 0.25 1 d P . .
H1N H 0.5785(16) 1.071(3) 0.322(3) 0.040(10) Uiso 1 1 d . . .
H2N H 0.6940(16) 1.149(2) 0.419(2) 0.031(10) Uiso 1 1 d . . .
H1S H 0.706(2) 1.303(3) 0.519(3) 0.064(15) Uiso 1 1 d . . .
H1O H 0.4620(18) 0.953(3) 0.284(3) 0.038(11) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C25 1.696(3) . yes
O1 C3 1.373(3) . yes
O1 H1O 0.79(4) . ?
O2 C14 1.399(3) . yes
O2 C23 1.442(3) . yes
N1 C25 1.349(3) . yes
N1 C24 1.451(3) . yes
N1 H1N 0.86(4) . ?
N2 C25 1.343(4) . yes
N2 C26 1.429(4) . yes
N2 H2N 0.78(4) . ?
C1 C15 1.515(4) 2_655 yes
C1 C2 1.520(3) . yes
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 C3 1.395(3) . yes
C2 C7 1.399(4) . yes
C3 C4 1.403(4) . yes
C4 C5 1.391(4) . yes
C4 C12 1.520(3) . yes
C5 C6 1.396(4) . yes
C5 H5 0.9500 . ?
C6 C7 1.388(4) . yes
C6 C8 1.539(4) . yes
C7 H7 0.9500 . ?
C8 C11B 1.468(13) . yes
C8 C10A 1.498(7) . yes
C8 C10B 1.520(14) . yes
C8 C9B 1.54(2) . yes
C8 C11A 1.540(8) . yes
C8 C9A 1.553(8) . yes
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C9B H9BA 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11B H11A 0.9800 . ?
C11B H11C 0.9800 . ?
C11B H11B 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C10A H10A 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11F 0.9800 . ?
C11A H11E 0.9800 . ?
C12 C13 1.520(4) . yes
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.393(4) . yes
C13 C14 1.396(4) . yes
C14 C15 1.397(4) . yes
C15 C16 1.400(4) . yes
C15 C1 1.515(4) 2_655 yes
C16 C17 1.383(4) . yes
C16 H16 0.9500 . ?
C17 C18 1.403(4) . yes
C17 C19 1.541(4) . yes
C18 H18 0.9500 . ?
C19 C20B 1.470(10) . yes
C19 C20A 1.51(2) . yes
C19 C21A 1.514(12) . yes
C19 C21B 1.531(11) . yes
C19 C22A 1.534(16) . yes
C19 C22B 1.577(10) . yes
C20B H20C 0.9800 . ?
C20B H20B 0.9800 . ?
C20B H20A 0.9800 . ?
C21B H21A 0.9800 . ?
C21B H21C 0.9800 . ?
C21B H21B 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22F 0.9800 . ?
C22B H22E 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20F 0.9800 . ?
C20A H20E 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C21A H21D 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22A H22A 0.9800 . ?
C23 C24 1.517(4) . yes
C23 H23B 0.9900 . ?
C23 H23A 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.378(4) . yes
C26 C31 1.398(4) . yes
C27 C28 1.396(4) . yes
C27 H27 0.9500 . ?
C28 C29 1.398(4) . yes
C28 C32 1.502(5) . yes
C29 C30 1.379(5) . yes
C29 H29 0.9500 . ?
C30 C31 1.397(4) . yes
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32B 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32C 0.9800 . ?
O1S C1S 1.405(6) . yes
O1S H1S 0.82(6) . ?
C1S C2S 1.462(9) . yes
C1S H1SB 0.9900 . ?
C1S H1SA 0.9900 . ?
C2S H2SB 0.9800 . ?
C2S H2SA 0.9800 . ?
C2S H2SC 0.9800 . ?
O3S C4S 1.398(11) 2_656 ?
O3S C4S 1.398(11) . ?
C5S C4S 1.729(17) . ?
C5S H5SB 0.9800 . ?
C5S H5SC 0.9800 . ?
C5S H5SA 0.9800 . ?
C4S C5SA 1.265(19) . ?
C4S O3SA 1.48(3) . ?
C5SA H5SD 0.9800 . ?
C5SA H5SE 0.9800 . ?
C5SA H5SF 0.9800 . ?
Cl1 C6S 1.703(15) . ?
Cl1 C6S 1.721(15) 2_656 ?
Cl2 C6S 1.838(14) . ?
Cl3 C6S 1.307(15) . ?
Cl3 C6S 1.781(15) 2_656 ?
Cl3 Cl3 2.146(14) 2_656 ?
C6S C6S 0.81(2) 2_656 ?
C6S Cl1 1.721(15) 2_656 ?
C6S Cl3 1.781(15) 2_656 ?
C6S H6SA 0.9602 . ?

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
C3 O1 H1O 118(3) . . ?
C14 O2 C23 115.68(18) . . yes
C25 N1 C24 123.1(2) . . yes
C25 N1 H1N 117(3) . . ?
C24 N1 H1N 116(3) . . ?
C25 N2 C26 125.7(2) . . yes
C25 N2 H2N 113(3) . . ?
C26 N2 H2N 121(3) . . ?
C15 C1 C2 110.6(2) 2_655 . yes
C15 C1 H1B 109.5 2_655 . ?
C2 C1 H1B 109.5 . . ?
C15 C1 H1A 109.5 2_655 . ?
C2 C1 H1A 109.5 . . ?
H1B C1 H1A 108.1 . . ?
C3 C2 C7 118.5(2) . . yes
C3 C2 C1 120.7(2) . . yes
C7 C2 C1 120.8(2) . . yes
O1 C3 C2 117.1(2) . . yes
O1 C3 C4 122.2(2) . . yes
C2 C3 C4 120.7(2) . . yes
C5 C4 C3 118.7(2) . . yes
C5 C4 C12 119.5(2) . . yes
C3 C4 C12 121.7(2) . . yes
C4 C5 C6 122.3(2) . . yes
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C7 C6 C5 117.3(2) . . yes
C7 C6 C8 122.7(2) . . yes
C5 C6 C8 119.9(3) . . yes
C6 C7 C2 122.5(2) . . yes
C6 C7 H7 118.7 . . ?
C2 C7 H7 118.7 . . ?
C11B C8 C10A 127.0(6) . . yes
C11B C8 C10B 108.4(8) . . yes
C10A C8 C10B 29.2(5) . . yes
C11B C8 C9B 111.9(10) . . yes
C10A C8 C9B 74.6(9) . . yes
C10B C8 C9B 102.6(10) . . yes
C11B C8 C6 113.8(6) . . yes
C10A C8 C6 113.2(3) . . yes
C10B C8 C6 111.6(6) . . yes
C9B C8 C6 108.0(8) . . yes
C11B C8 C11A 31.3(5) . . yes
C10A C8 C11A 109.7(4) . . yes
C10B C8 C11A 83.5(6) . . yes
C9B C8 C11A 137.8(9) . . yes
C6 C8 C11A 108.1(4) . . yes
C11B C8 C9A 79.5(6) . . yes
C10A C8 C9A 107.8(4) . . yes
C10B C8 C9A 131.2(6) . . yes
C9B C8 C9A 36.7(8) . . yes
C6 C8 C9A 107.9(3) . . yes
C11A C8 C9A 110.2(4) . . yes
C8 C9B H9BB 109.5 . . ?
C8 C9B H9BC 109.5 . . ?
C8 C9B H9BA 109.5 . . ?
C8 C10B H10D 109.5 . . ?
C8 C10B H10E 109.5 . . ?
C8 C10B H10F 109.5 . . ?
C8 C11B H11A 109.5 . . ?
C8 C11B H11C 109.5 . . ?
C8 C11B H11B 109.5 . . ?
C8 C9A H9AB 109.5 . . ?
C8 C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C8 C9A H9AA 109.5 . . ?
H9AB C9A H9AA 109.5 . . ?
H9AC C9A H9AA 109.5 . . ?
C8 C10A H10B 109.5 . . ?
C8 C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C8 C10A H10A 109.5 . . ?
H10B C10A H10A 109.5 . . ?
H10C C10A H10A 109.5 . . ?
C8 C11A H11D 109.5 . . ?
C8 C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
C8 C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11F C11A H11E 109.5 . . ?
C4 C12 C13 113.4(2) . . yes
C4 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
C4 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C18 C13 C14 118.3(2) . . yes
C18 C13 C12 120.4(2) . . yes
C14 C13 C12 121.2(2) . . yes
C13 C14 C15 122.0(2) . . yes
C13 C14 O2 118.9(2) . . yes
C15 C14 O2 118.9(2) . . yes
C14 C15 C16 117.2(2) . . yes
C14 C15 C1 123.0(2) . 2_655 yes
C16 C15 C1 119.6(2) . 2_655 yes
C17 C16 C15 122.9(3) . . yes
C17 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
C16 C17 C18 117.8(3) . . yes
C16 C17 C19 120.5(3) . . yes
C18 C17 C19 121.7(3) . . yes
C13 C18 C17 121.7(3) . . yes
C13 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C20B C19 C20A 43.2(8) . . yes
C20B C19 C21A 131.8(6) . . yes
C20A C19 C21A 99.4(9) . . yes
C20B C19 C21B 109.2(6) . . yes
C20A C19 C21B 68.8(9) . . yes
C21A C19 C21B 33.6(5) . . yes
C20B C19 C22A 84.4(8) . . yes
C20A C19 C22A 122.6(10) . . yes
C21A C19 C22A 103.1(8) . . yes
C21B C19 C22A 131.4(8) . . yes
C20B C19 C17 112.7(5) . . yes
C20A C19 C17 111.9(8) . . yes
C21A C19 C17 109.4(5) . . yes
C21B C19 C17 107.6(5) . . yes
C22A C19 C17 109.0(6) . . yes
C20B C19 C22B 113.0(6) . . yes
C20A C19 C22B 135.9(9) . . yes
C21A C19 C22B 69.7(6) . . yes
C21B C19 C22B 101.5(6) . . yes
C22A C19 C22B 34.5(6) . . yes
C17 C19 C22B 112.0(4) . . yes
C19 C20B H20C 109.5 . . ?
C19 C20B H20B 109.5 . . ?
H20C C20B H20B 109.5 . . ?
C19 C20B H20A 109.5 . . ?
H20C C20B H20A 109.5 . . ?
H20B C20B H20A 109.5 . . ?
C19 C21B H21A 109.5 . . ?
C19 C21B H21C 109.5 . . ?
H21A C21B H21C 109.5 . . ?
C19 C21B H21B 109.5 . . ?
H21A C21B H21B 109.5 . . ?
H21C C21B H21B 109.5 . . ?
C19 C22B H22D 109.5 . . ?
C19 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
C19 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
H22F C22B H22E 109.5 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20F 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C22A H22B 109.5 . . ?
C19 C22A H22C 109.5 . . ?
C19 C22A H22A 109.5 . . ?
O2 C23 C24 106.5(2) . . yes
O2 C23 H23B 110.4 . . ?
C24 C23 H23B 110.4 . . ?
O2 C23 H23A 110.4 . . ?
C24 C23 H23A 110.4 . . ?
H23B C23 H23A 108.6 . . ?
N1 C24 C23 112.3(2) . . yes
N1 C24 H24A 109.1 . . ?
C23 C24 H24A 109.1 . . ?
N1 C24 H24B 109.1 . . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.9 . . ?
N2 C25 N1 116.7(2) . . yes
N2 C25 S1 120.6(2) . . yes
N1 C25 S1 122.6(2) . . yes
C27 C26 C31 120.7(3) . . yes
C27 C26 N2 119.3(3) . . yes
C31 C26 N2 119.9(3) . . yes
C26 C27 C28 120.9(3) . . yes
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C29 118.2(3) . . yes
C27 C28 C32 121.1(3) . . yes
C29 C28 C32 120.8(3) . . yes
C30 C29 C28 121.2(3) . . yes
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C31 120.3(3) . . yes
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C26 118.7(3) . . yes
C30 C31 H31 120.7 . . ?
C26 C31 H31 120.7 . . ?
C28 C32 H32B 109.5 . . ?
C28 C32 H32A 109.5 . . ?
H32B C32 H32A 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
C1S O1S H1S 113(4) . . ?
O1S C1S C2S 112.6(5) . . yes
O1S C1S H1SB 109.1 . . ?
C2S C1S H1SB 109.1 . . ?
O1S C1S H1SA 109.1 . . ?
C2S C1S H1SA 109.1 . . ?
H1SB C1S H1SA 107.8 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SA 109.5 . . ?
H2SB C2S H2SA 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
C4S O3S C4S 99.4(9) 2_656 . ?
C4S C5S H5SB 109.5 . . ?
C4S C5S H5SC 109.5 . . ?
C4S C5S H5SA 109.5 . . ?
C5SA C4S O3S 122.7(11) . . ?
C5SA C4S O3SA 90.7(14) . . ?
O3S C4S O3SA 137.6(12) . . ?
C5SA C4S C5S 19.1(9) . . ?
O3S C4S C5S 105.4(7) . . ?
O3SA C4S C5S 109.8(13) . . ?
C4S C5SA H5SD 109.5 . . ?
C4S C5SA H5SE 109.5 . . ?
H5SD C5SA H5SE 109.5 . . ?
C4S C5SA H5SF 109.5 . . ?
H5SD C5SA H5SF 109.5 . . ?
H5SE C5SA H5SF 109.5 . . ?
C6S Cl1 C6S 27.4(8) . 2_656 ?
C6S Cl3 C6S 24.8(9) . 2_656 ?
C6S Cl3 Cl3 55.9(7) . 2_656 ?
C6S Cl3 Cl3 37.4(5) 2_656 2_656 ?
C6S C6S Cl3 112.4(13) 2_656 . ?
C6S C6S Cl1 77.5(18) 2_656 . ?
Cl3 C6S Cl1 96.8(9) . . ?
C6S C6S Cl1 75.1(17) 2_656 2_656 ?
Cl3 C6S Cl1 150.2(11) . 2_656 ?
Cl1 C6S Cl1 112.9(8) . 2_656 ?
C6S C6S Cl3 42.7(9) 2_656 2_656 ?
Cl3 C6S Cl3 86.6(9) . 2_656 ?
Cl1 C6S Cl3 114.3(8) . 2_656 ?
Cl1 C6S Cl3 80.7(6) 2_656 2_656 ?
C6S C6S Cl2 141.7(9) 2_656 . ?
Cl3 C6S Cl2 30.1(4) . . ?
Cl1 C6S Cl2 107.0(8) . . ?
Cl1 C6S Cl2 131.4(9) 2_656 . ?
Cl3 C6S Cl2 107.1(8) 2_656 . ?
C6S C6S H6SA 58.3 2_656 . ?
Cl3 C6S H6SA 126.3 . . ?
Cl1 C6S H6SA 126.1 . . ?
Cl1 C6S H6SA 31.9 2_656 . ?
Cl3 C6S H6SA 49.4 2_656 . ?
Cl2 C6S H6SA 126.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O1 0.86(4) 2.25(5) 3.072(3) 159(4) 2_655
N2 H2N O1S 0.78(4) 2.05(4) 2.788(4) 158(4) 7_676
O1S H1S S1 0.82(6) 2.46(6) 3.274(3) 171(5) .
O1 H1O O2 0.79(4) 1.87(5) 2.659(3) 173(4) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.678
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.106

# File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison.
_database_code_depnum_ccdc_archive 'CCDC 1003765'
#######################################################################
#
#                 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_4b_S068

_audit_creation_method           SHELXL-97
_chemical_formula_moiety         'C70 H80 N4 O6, 2 CH3CN, 1.5 CHCl3'
_chemical_formula_sum            'C75.50 H87.50 Cl4.50 N6 O6'
_chemical_formula_weight         1334.54
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
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'
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 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_angle_alpha                90.00
_cell_angle_beta                 92.349(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6122(5)
_cell_length_b                   30.9836(12)
_cell_length_c                   18.6901(7)
_cell_measurement_reflns_used    5292
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     7297.4(5)
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  .
_exptl_absorpt_correction_T_min  .
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_F_000             2828
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_special_details           ?
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54294
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6561
_reflns_number_total             14329
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    
;
Olex2, Durham University (compiled Feb 15 2009 13:03:59)
;
_computing_publication_material  
;
Olex2, Durham University (compiled Feb 15 2009 13:03:59)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)/Bruker'
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.087
_refine_ls_R_factor_all          0.1638
_refine_ls_R_factor_gt           0.0852
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         14329
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.2683
_refine_ls_weighting_details     
;
calc w=1/[σ²(Fo²)+(0.1400P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_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.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
O1 O 0.9866(2) 0.10764(9) 0.18671(14) 0.0305(7) Uani 1 1 d . . .
H1 H 0.9472 0.0870 0.1977 0.046 Uiso 1 1 calc R . .
O2 O 0.9309(2) 0.17105(9) 0.07360(14) 0.0298(7) Uani 1 1 d . . .
O3 O 0.7332(2) 0.14341(9) 0.09619(15) 0.0315(7) Uani 1 1 d . . .
H3 H 0.7775 0.1549 0.0697 0.047 Uiso 1 1 calc R . .
O4 O 0.7906(2) 0.07594(9) 0.19870(15) 0.0290(7) Uani 1 1 d . . .
O5 O 1.1521(2) 0.08057(10) -0.05794(16) 0.0378(8) Uani 1 1 d . . .
O6 O 0.6281(2) -0.01237(9) 0.03507(17) 0.0367(8) Uani 1 1 d . . .
N1 N 1.0381(3) 0.09127(12) 0.03162(19) 0.0358(9) Uani 1 1 d . . .
H1B H 1.0220 0.0856 0.0760 0.043 Uiso 1 1 calc R . .
N2 N 1.1933(3) 0.05127(13) 0.0509(2) 0.0411(10) Uani 1 1 d . . .
H2 H 1.2615 0.0501 0.0429 0.049 Uiso 1 1 calc R . .
N3 N 0.7305(3) 0.04697(12) 0.05667(18) 0.0329(8) Uani 1 1 d . . .
H3B H 0.7440 0.0739 0.0454 0.039 Uiso 1 1 calc R . .
N4 N 0.5729(3) 0.05141(12) -0.01147(19) 0.0350(9) Uani 1 1 d . . .
H4 H 0.5116 0.0393 -0.0234 0.042 Uiso 1 1 calc R . .
C1 C 1.0923(3) 0.16283(15) 0.2407(2) 0.0337(10) Uani 1 1 d . . .
C2 C 1.0252(3) 0.12765(14) 0.2480(2) 0.0310(10) Uani 1 1 d . . .
C3 C 0.9989(3) 0.11306(15) 0.3160(2) 0.0333(10) Uani 1 1 d . . .
C4 C 1.0402(4) 0.13533(17) 0.3765(2) 0.0433(12) Uani 1 1 d . . .
H4B H 1.0218 0.1259 0.4227 0.052 Uiso 1 1 calc R . .
C5 C 1.1073(4) 0.17076(18) 0.3708(3) 0.0480(13) Uani 1 1 d . . .
C6 C 1.1328(3) 0.18309(17) 0.3018(2) 0.0424(12) Uani 1 1 d . . .
H6 H 1.1803 0.2065 0.2965 0.051 Uiso 1 1 calc R . .
C7 C 1.1532(4) 0.1950(2) 0.4355(3) 0.0640(18) Uani 1 1 d . . .
C8 C 1.2712(4) 0.1901(2) 0.4406(3) 0.0548(14) Uani 1 1 d . . .
H8A H 1.2895 0.1598 0.4489 0.082 Uiso 1 1 calc R . .
H8C H 1.3003 0.2076 0.4805 0.082 Uiso 1 1 calc R . .
H8B H 1.3013 0.1999 0.3959 0.082 Uiso 1 1 calc R . .
C9 C 1.0974(5) 0.1873(3) 0.5004(3) 0.083(2) Uani 1 1 d . . .
H9A H 1.0219 0.1939 0.4919 0.124 Uiso 1 1 calc R . .
H9C H 1.1268 0.2060 0.5387 0.124 Uiso 1 1 calc R . .
H9B H 1.1057 0.1570 0.5146 0.124 Uiso 1 1 calc R . .
C10 C 1.1358(5) 0.2465(2) 0.4215(4) 0.078(2) Uani 1 1 d . . .
H10B H 1.1806 0.2560 0.3829 0.117 Uiso 1 1 calc R . .
H10C H 1.1552 0.2625 0.4654 0.117 Uiso 1 1 calc R . .
H10A H 1.0612 0.2520 0.4079 0.117 Uiso 1 1 calc R . .
C11 C 0.9253(3) 0.07485(15) 0.3261(2) 0.0370(11) Uani 1 1 d . . .
H11A H 0.9355 0.0536 0.2874 0.044 Uiso 1 1 calc R . .
H11B H 0.9440 0.0606 0.3723 0.044 Uiso 1 1 calc R . .
C12 C 0.8098(3) 0.08852(14) 0.3250(2) 0.0299(10) Uani 1 1 d . . .
C13 C 0.7471(3) 0.09006(13) 0.2628(2) 0.0277(9) Uani 1 1 d . . .
C14 C 0.6455(3) 0.10744(13) 0.2610(2) 0.0279(9) Uani 1 1 d . . .
C15 C 0.6051(3) 0.12092(14) 0.3250(2) 0.0305(10) Uani 1 1 d . . .
H15 H 0.5349 0.1320 0.3247 0.037 Uiso 1 1 calc R . .
C16 C 0.6636(3) 0.11893(14) 0.3901(2) 0.0305(10) Uani 1 1 d . . .
C17 C 0.7668(3) 0.10332(14) 0.3891(2) 0.0325(10) Uani 1 1 d . . .
H17 H 0.8092 0.1026 0.4323 0.039 Uiso 1 1 calc R . .
C18 C 0.6140(4) 0.13436(15) 0.4588(2) 0.0382(11) Uani 1 1 d . . .
C19 C 0.6926(4) 0.13261(18) 0.5239(2) 0.0485(13) Uani 1 1 d . . .
H19B H 0.6565 0.1416 0.5669 0.073 Uiso 1 1 calc R . .
H19C H 0.7522 0.1521 0.5161 0.073 Uiso 1 1 calc R . .
H19A H 0.7190 0.1031 0.5302 0.073 Uiso 1 1 calc R . .
C20 C 0.5183(4) 0.10561(19) 0.4743(3) 0.0543(14) Uani 1 1 d . . .
H20A H 0.4662 0.1072 0.4341 0.082 Uiso 1 1 calc R . .
H20C H 0.4857 0.1157 0.5180 0.082 Uiso 1 1 calc R . .
H20B H 0.5420 0.0757 0.4808 0.082 Uiso 1 1 calc R . .
C21 C 0.5765(4) 0.18130(16) 0.4484(3) 0.0473(13) Uani 1 1 d . . .
H21A H 0.5236 0.1827 0.4086 0.071 Uiso 1 1 calc R . .
H21C H 0.6373 0.1996 0.4377 0.071 Uiso 1 1 calc R . .
H21B H 0.5448 0.1915 0.4923 0.071 Uiso 1 1 calc R . .
C22 C 0.5804(3) 0.11526(14) 0.1907(2) 0.0311(10) Uani 1 1 d . . .
H22B H 0.6065 0.0960 0.1529 0.037 Uiso 1 1 calc R . .
H22A H 0.5050 0.1081 0.1977 0.037 Uiso 1 1 calc R . .
C23 C 0.5888(3) 0.16175(14) 0.1668(2) 0.0291(10) Uani 1 1 d . . .
C24 C 0.6677(3) 0.17458(14) 0.1217(2) 0.0290(10) Uani 1 1 d . . .
C25 C 0.6785(3) 0.21818(14) 0.1029(2) 0.0295(10) Uani 1 1 d . . .
C26 C 0.6103(3) 0.24810(15) 0.1317(2) 0.0348(10) Uani 1 1 d . . .
H26 H 0.6187 0.2777 0.1198 0.042 Uiso 1 1 calc R . .
C27 C 0.5301(3) 0.23683(14) 0.1773(2) 0.0313(10) Uani 1 1 d . . .
C28 C 0.5210(3) 0.19312(14) 0.1934(2) 0.0310(10) Uani 1 1 d . . .
H28 H 0.4664 0.1842 0.2237 0.037 Uiso 1 1 calc R . .
C29 C 0.4567(4) 0.27134(15) 0.2062(2) 0.0378(11) Uani 1 1 d . . .
C30 C 0.3997(5) 0.25575(19) 0.2719(3) 0.0664(18) Uani 1 1 d . . .
H30C H 0.3552 0.2790 0.2896 0.100 Uiso 1 1 calc R . .
H30B H 0.4523 0.2474 0.3095 0.100 Uiso 1 1 calc R . .
H30A H 0.3552 0.2308 0.2589 0.100 Uiso 1 1 calc R . .
C31 C 0.5182(5) 0.31130(18) 0.2276(3) 0.0656(17) Uani 1 1 d . . .
H31A H 0.5500 0.3238 0.1853 0.098 Uiso 1 1 calc R . .
H31C H 0.5743 0.3037 0.2632 0.098 Uiso 1 1 calc R . .
H31B H 0.4702 0.3324 0.2482 0.098 Uiso 1 1 calc R . .
C32 C 0.3731(5) 0.2825(2) 0.1485(3) 0.0729(19) Uani 1 1 d . . .
H32B H 0.4078 0.2920 0.1053 0.109 Uiso 1 1 calc R . .
H32C H 0.3279 0.3058 0.1656 0.109 Uiso 1 1 calc R . .
H32A H 0.3295 0.2570 0.1374 0.109 Uiso 1 1 calc R . .
C33 C 0.7652(3) 0.23305(14) 0.0552(2) 0.0342(10) Uani 1 1 d . . .
H33B H 0.7417 0.2595 0.0295 0.041 Uiso 1 1 calc R . .
H33A H 0.7777 0.2105 0.0189 0.041 Uiso 1 1 calc R . .
C34 C 0.8682(3) 0.24224(14) 0.0969(2) 0.0320(10) Uani 1 1 d . . .
C35 C 0.9465(3) 0.21129(14) 0.1057(2) 0.0318(10) Uani 1 1 d . . .
C36 C 1.0368(3) 0.21788(14) 0.1497(2) 0.0356(11) Uani 1 1 d . . .
C37 C 1.0469(4) 0.25812(15) 0.1835(3) 0.0391(11) Uani 1 1 d . . .
H37 H 1.1087 0.2634 0.2129 0.047 Uiso 1 1 calc R . .
C38 C 0.9720(4) 0.29041(15) 0.1763(3) 0.0418(12) Uani 1 1 d . A .
C39 C 0.8817(4) 0.28169(15) 0.1318(2) 0.0392(11) Uani 1 1 d . . .
H39 H 0.8286 0.3033 0.1255 0.047 Uiso 1 1 calc R . .
C40 C 0.9824(4) 0.33434(16) 0.2142(3) 0.0518(14) Uani 1 1 d . . .
C41A C 1.0852(15) 0.3371(6) 0.2618(11) 0.099(6) Uiso 0.50 1 d P A 1
H41A H 1.0888 0.3124 0.2945 0.149 Uiso 0.50 1 calc PR A 1
H41C H 1.0851 0.3639 0.2896 0.149 Uiso 0.50 1 calc PR A 1
H41B H 1.1468 0.3368 0.2316 0.149 Uiso 0.50 1 calc PR A 1
C42A C 0.9932(10) 0.3711(4) 0.1567(6) 0.054(3) Uiso 0.50 1 d P A 1
H42B H 1.0542 0.3650 0.1274 0.081 Uiso 0.50 1 calc PR A 1
H42C H 1.0037 0.3989 0.1810 0.081 Uiso 0.50 1 calc PR A 1
H42A H 0.9285 0.3722 0.1259 0.081 Uiso 0.50 1 calc PR A 1
C43A C 0.8911(7) 0.3427(3) 0.2589(5) 0.036(2) Uiso 0.50 1 d P A 1
H43A H 0.8269 0.3462 0.2281 0.054 Uiso 0.50 1 calc PR A 1
H43C H 0.9038 0.3691 0.2867 0.054 Uiso 0.50 1 calc PR A 1
H43B H 0.8819 0.3184 0.2916 0.054 Uiso 0.50 1 calc PR A 1
C41B C 1.0583(13) 0.3304(6) 0.2854(9) 0.081(5) Uiso 0.50 1 d P A 2
H41D H 1.0346 0.3062 0.3146 0.122 Uiso 0.50 1 calc PR A 2
H41F H 1.0549 0.3572 0.3131 0.122 Uiso 0.50 1 calc PR A 2
H41E H 1.1316 0.3253 0.2720 0.122 Uiso 0.50 1 calc PR A 2
C42B C 1.0450(11) 0.3645(4) 0.1691(7) 0.061(3) Uiso 0.50 1 d P A 2
H42E H 1.1154 0.3522 0.1620 0.092 Uiso 0.50 1 calc PR A 2
H42F H 1.0526 0.3924 0.1935 0.092 Uiso 0.50 1 calc PR A 2
H42D H 1.0077 0.3686 0.1226 0.092 Uiso 0.50 1 calc PR A 2
C43B C 0.8674(13) 0.3552(5) 0.2274(9) 0.093(5) Uiso 0.50 1 d P A 2
H43E H 0.8318 0.3620 0.1812 0.139 Uiso 0.50 1 calc PR A 2
H43F H 0.8763 0.3816 0.2557 0.139 Uiso 0.50 1 calc PR A 2
H43D H 0.8244 0.3345 0.2533 0.139 Uiso 0.50 1 calc PR A 2
C44 C 1.1146(3) 0.18178(15) 0.1682(2) 0.0356(11) Uani 1 1 d . . .
H44A H 1.1083 0.1589 0.1312 0.043 Uiso 1 1 calc R . .
H44B H 1.1880 0.1932 0.1689 0.043 Uiso 1 1 calc R . .
C45 C 0.9762(4) 0.16524(15) 0.0042(2) 0.0350(11) Uani 1 1 d . . .
H45B H 1.0513 0.1747 0.0059 0.042 Uiso 1 1 calc R . .
H45A H 0.9364 0.1824 -0.0326 0.042 Uiso 1 1 calc R . .
C46 C 0.9685(3) 0.11818(14) -0.0130(2) 0.0336(10) Uani 1 1 d . . .
H46A H 0.8943 0.1087 -0.0076 0.040 Uiso 1 1 calc R . .
H46B H 0.9857 0.1139 -0.0637 0.040 Uiso 1 1 calc R . .
C47 C 1.1287(3) 0.07465(14) 0.0049(2) 0.0325(10) Uani 1 1 d . . .
C48 C 1.1533(4) 0.02757(17) 0.1141(3) 0.0496(13) Uani 1 1 d . . .
C49 C 1.0835(4) -0.00579(15) 0.1053(3) 0.0440(12) Uani 1 1 d . . .
H49 H 1.0631 -0.0142 0.0578 0.053 Uiso 1 1 calc R . .
C50 C 1.0403(4) -0.02821(15) 0.1613(3) 0.0429(12) Uani 1 1 d . . .
H50 H 0.9902 -0.0506 0.1523 0.052 Uiso 1 1 calc R . .
C51 C 1.0723(4) -0.01707(17) 0.2312(3) 0.0571(15) Uani 1 1 d . . .
H51 H 1.0450 -0.0320 0.2709 0.068 Uiso 1 1 calc R . .
C52 C 1.1807(5) 0.0294(2) 0.3135(3) 0.0609(15) Uani 1 1 d . . .
H52 H 1.1550 0.0138 0.3530 0.073 Uiso 1 1 calc R . .
C53 C 1.2496(4) 0.0632(2) 0.3236(3) 0.0616(15) Uani 1 1 d . . .
H53 H 1.2713 0.0718 0.3708 0.074 Uiso 1 1 calc R . .
C54 C 1.2895(4) 0.08581(18) 0.2624(3) 0.0568(15) Uani 1 1 d . . .
H54 H 1.3368 0.1093 0.2706 0.068 Uiso 1 1 calc R . .
C55 C 1.2627(4) 0.07514(18) 0.1958(3) 0.0571(15) Uani 1 1 d . . .
H55 H 1.2921 0.0903 0.1570 0.069 Uiso 1 1 calc R . .
C56 C 1.1858(4) 0.03916(16) 0.1815(3) 0.0431(12) Uani 1 1 d . . .
C57 C 1.1486(4) 0.01812(17) 0.2421(3) 0.0464(13) Uani 1 1 d . . .
C58 C 0.7729(3) 0.03026(14) 0.1833(2) 0.0340(10) Uani 1 1 d . . .
H58A H 0.6978 0.0225 0.1896 0.041 Uiso 1 1 calc R . .
H58B H 0.8183 0.0121 0.2156 0.041 Uiso 1 1 calc R . .
C59 C 0.8016(3) 0.02380(14) 0.1066(2) 0.0337(10) Uani 1 1 d . . .
H59B H 0.8752 0.0339 0.1007 0.040 Uiso 1 1 calc R . .
H59A H 0.7989 -0.0074 0.0952 0.040 Uiso 1 1 calc R . .
C60 C 0.6433(3) 0.02692(14) 0.0274(2) 0.0303(10) Uani 1 1 d . . .
C61 C 0.5875(4) 0.09465(16) -0.0351(2) 0.0392(11) Uani 1 1 d . . .
C62 C 0.6734(4) 0.1050(2) -0.0743(3) 0.0548(14) Uani 1 1 d . . .
H62 H 0.7237 0.0837 -0.0864 0.066 Uiso 1 1 calc R . .
C63 C 0.6853(5) 0.1498(2) -0.0969(3) 0.0579(16) Uani 1 1 d . . .
H63 H 0.7436 0.1581 -0.1245 0.069 Uiso 1 1 calc R . .
C64 C 0.6123(5) 0.1791(2) -0.0781(3) 0.0612(16) Uani 1 1 d . . .
H64 H 0.6226 0.2081 -0.0928 0.073 Uiso 1 1 calc R . .
C65 C 0.4465(5) 0.20189(16) -0.0238(3) 0.0512(14) Uani 1 1 d . . .
H65 H 0.4537 0.2307 -0.0403 0.061 Uiso 1 1 calc R . .
C66 C 0.3623(5) 0.19046(19) 0.0147(3) 0.0648(16) Uani 1 1 d . . .
H66 H 0.3121 0.2119 0.0266 0.078 Uiso 1 1 calc R . .
C67 C 0.3476(5) 0.14854(17) 0.0373(3) 0.0567(15) Uani 1 1 d . . .
H67 H 0.2866 0.1412 0.0628 0.068 Uiso 1 1 calc R . .
C68 C 0.4217(4) 0.11741(17) 0.0226(3) 0.0461(13) Uani 1 1 d . . .
H68 H 0.4121 0.0888 0.0396 0.055 Uiso 1 1 calc R . .
C69 C 0.5101(4) 0.12697(15) -0.0164(3) 0.0450(13) Uani 1 1 d . . .
C70 C 0.5235(4) 0.17039(17) -0.0391(3) 0.0520(14) Uani 1 1 d . . .
Cl1 Cl 0.52839(14) 0.48974(6) 0.32117(10) 0.0585(5) Uani 0.80 1 d P . .
Cl2 Cl 0.48319(16) 0.50563(8) 0.17314(11) 0.0795(6) Uani 0.80 1 d P . .
Cl3 Cl 0.5951(2) 0.42789(7) 0.22007(16) 0.1089(10) Uani 0.80 1 d P . .
C5S C 0.5709(5) 0.48254(19) 0.2358(4) 0.0474(16) Uani 0.80 1 d P . .
H5S H 0.6401 0.4980 0.2327 0.057 Uiso 0.80 1 calc PR . .
Cl4 Cl 1.2673(2) 0.08662(9) 0.55339(18) 0.1048(11) Uani 0.70 1 d P B 2
Cl5A Cl 1.2677(6) -0.00789(19) 0.5169(3) 0.102(2) Uiso 0.35 1 d PD B 2
Cl5B Cl 1.3150(4) 0.00531(17) 0.5137(3) 0.0728(14) Uiso 0.35 1 d PD B 2
Cl6 Cl 1.0870(3) 0.03291(13) 0.5536(2) 0.1356(14) Uani 0.70 1 d P B 2
C6S C 1.2277(7) 0.0357(3) 0.5713(5) 0.067(2) Uani 0.70 1 d PD B 2
H6S H 1.2442 0.0289 0.6218 0.081 Uiso 0.70 1 d PR B 2
N1S N 0.2419(6) 0.0646(2) 0.7353(4) 0.102(2) Uani 1 1 d . . .
C1S C 0.2857(5) 0.0817(2) 0.7830(4) 0.0658(17) Uani 1 1 d . . .
C2S C 0.3383(4) 0.10106(18) 0.8419(3) 0.0532(14) Uani 1 1 d . . .
H2SA H 0.4143 0.1030 0.8333 0.080 Uiso 1 1 calc R . .
H2SC H 0.3279 0.0837 0.8848 0.080 Uiso 1 1 calc R . .
H2SB H 0.3097 0.1301 0.8489 0.080 Uiso 1 1 calc R . .
N2S N 0.8440(4) 0.2543(2) 0.3905(3) 0.0833(18) Uani 1 1 d . . .
C3S C 0.8300(4) 0.23217(17) 0.3418(3) 0.0438(12) Uani 1 1 d . . .
C4S C 0.8115(4) 0.20582(16) 0.2799(2) 0.0437(12) Uani 1 1 d . . .
H4SB H 0.7593 0.2199 0.2473 0.066 Uiso 1 1 calc R . .
H4SA H 0.7843 0.1776 0.2944 0.066 Uiso 1 1 calc R . .
H4SC H 0.8781 0.2019 0.2555 0.066 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix. The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry. An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.374(5) . ?
O2 C35 1.394(5) . ?
O2 C45 1.449(5) . ?
O3 C24 1.369(5) . ?
O4 C13 1.408(5) . ?
O4 C58 1.460(5) . ?
O5 C47 1.236(5) . ?
O6 C60 1.242(5) . ?
N1 C47 1.366(5) . ?
N1 C46 1.450(5) . ?
N2 C47 1.368(6) . ?
N2 C48 1.496(7) . ?
N3 C60 1.358(5) . ?
N3 C59 1.457(6) . ?
N4 C60 1.357(6) . ?
N4 C61 1.425(6) . ?
C1 C6 1.382(6) . ?
C1 C2 1.390(6) . ?
C1 C44 1.513(6) . ?
C2 C3 1.402(6) . ?
C3 C4 1.406(6) . ?
C3 C11 1.520(6) . ?
C4 C5 1.393(7) . ?
C5 C6 1.395(7) . ?
C5 C7 1.518(7) . ?
C7 C9 1.447(7) . ?
C7 C8 1.495(7) . ?
C7 C10 1.631(9) . ?
C11 C12 1.517(6) . ?
C12 C13 1.380(6) . ?
C12 C17 1.411(6) . ?
C13 C14 1.389(6) . ?
C14 C15 1.384(6) . ?
C14 C22 1.540(6) . ?
C15 C16 1.398(6) . ?
C16 C17 1.390(6) . ?
C16 C18 1.527(6) . ?
C18 C20 1.538(6) . ?
C18 C19 1.539(7) . ?
C18 C21 1.539(7) . ?
C22 C23 1.513(6) . ?
C23 C24 1.387(6) . ?
C23 C28 1.399(6) . ?
C24 C25 1.404(6) . ?
C25 C26 1.388(6) . ?
C25 C33 1.512(6) . ?
C26 C27 1.393(6) . ?
C27 C28 1.393(6) . ?
C27 C29 1.527(6) . ?
C29 C31 1.506(7) . ?
C29 C32 1.516(7) . ?
C29 C30 1.527(7) . ?
C33 C34 1.513(6) . ?
C34 C35 1.381(6) . ?
C34 C39 1.393(6) . ?
C35 C36 1.393(6) . ?
C36 C37 1.400(6) . ?
C36 C44 1.519(6) . ?
C37 C38 1.378(7) . ?
C38 C39 1.409(7) . ?
C38 C40 1.537(7) . ?
C40 C43A 1.474(10) . ?
C40 C42B 1.503(13) . ?
C40 C41A 1.54(2) . ?
C40 C42A 1.576(13) . ?
C40 C41B 1.613(18) . ?
C40 C43B 1.616(17) . ?
C45 C46 1.496(6) . ?
C48 C56 1.357(7) . ?
C48 C49 1.364(7) . ?
C49 C50 1.387(7) . ?
C50 C51 1.394(7) . ?
C51 C57 1.463(8) . ?
C52 C53 1.369(8) . ?
C52 C57 1.421(7) . ?
C53 C54 1.450(8) . ?
C54 C55 1.320(8) . ?
C55 C56 1.494(7) . ?
C56 C57 1.404(7) . ?
C58 C59 1.504(6) . ?
C61 C62 1.371(7) . ?
C61 C69 1.451(7) . ?
C62 C63 1.459(8) . ?
C63 C64 1.350(8) . ?
C64 C70 1.388(8) . ?
C65 C66 1.353(8) . ?
C65 C70 1.415(7) . ?
C66 C67 1.380(8) . ?
C67 C68 1.378(7) . ?
C68 C69 1.389(7) . ?
C69 C70 1.423(7) . ?
Cl1 C5S 1.719(7) . ?
Cl2 C5S 1.732(7) . ?
Cl3 C5S 1.747(6) . ?
Cl4 C6S 1.693(8) . ?
Cl5A Cl5B 0.727(7) . ?
Cl5A C6S 1.776(10) . ?
Cl5B C6S 1.831(9) . ?
Cl6 C6S 1.794(10) . ?
N1S C1S 1.158(8) . ?
C1S C2S 1.397(8) . ?
N2S C3S 1.147(6) . ?
C3S C4S 1.428(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C35 O2 C45 116.2(3) . . ?
C13 O4 C58 114.1(3) . . ?
C47 N1 C46 120.1(4) . . ?
C47 N2 C48 123.1(4) . . ?
C60 N3 C59 120.0(4) . . ?
C60 N4 C61 127.0(4) . . ?
C6 C1 C2 118.8(4) . . ?
C6 C1 C44 119.2(4) . . ?
C2 C1 C44 121.9(4) . . ?
O1 C2 C1 118.0(4) . . ?
O1 C2 C3 121.4(4) . . ?
C1 C2 C3 120.6(4) . . ?
C2 C3 C4 118.5(4) . . ?
C2 C3 C11 122.1(4) . . ?
C4 C3 C11 119.4(4) . . ?
C5 C4 C3 122.2(4) . . ?
C4 C5 C6 116.7(4) . . ?
C4 C5 C7 122.9(5) . . ?
C6 C5 C7 120.4(5) . . ?
C1 C6 C5 123.2(5) . . ?
C9 C7 C8 116.6(5) . . ?
C9 C7 C5 113.8(5) . . ?
C8 C7 C5 110.3(4) . . ?
C9 C7 C10 103.2(5) . . ?
C8 C7 C10 103.7(5) . . ?
C5 C7 C10 108.2(5) . . ?
C12 C11 C3 111.8(4) . . ?
C13 C12 C17 118.5(4) . . ?
C13 C12 C11 122.5(4) . . ?
C17 C12 C11 118.8(4) . . ?
C12 C13 C14 122.0(4) . . ?
C12 C13 O4 118.5(4) . . ?
C14 C13 O4 119.4(4) . . ?
C15 C14 C13 117.9(4) . . ?
C15 C14 C22 119.2(4) . . ?
C13 C14 C22 122.8(4) . . ?
C14 C15 C16 122.7(4) . . ?
C17 C16 C15 117.7(4) . . ?
C17 C16 C18 122.4(4) . . ?
C15 C16 C18 119.9(4) . . ?
C16 C17 C12 121.1(4) . . ?
C16 C18 C20 109.2(4) . . ?
C16 C18 C19 112.4(4) . . ?
C20 C18 C19 108.3(4) . . ?
C16 C18 C21 109.0(4) . . ?
C20 C18 C21 109.4(4) . . ?
C19 C18 C21 108.5(4) . . ?
C23 C22 C14 111.1(3) . . ?
C24 C23 C28 118.7(4) . . ?
C24 C23 C22 120.9(4) . . ?
C28 C23 C22 120.3(4) . . ?
O3 C24 C23 117.8(4) . . ?
O3 C24 C25 121.6(4) . . ?
C23 C24 C25 120.5(4) . . ?
C26 C25 C24 118.5(4) . . ?
C26 C25 C33 120.0(4) . . ?
C24 C25 C33 121.4(4) . . ?
C25 C26 C27 123.2(4) . . ?
C28 C27 C26 116.3(4) . . ?
C28 C27 C29 123.2(4) . . ?
C26 C27 C29 120.4(4) . . ?
C27 C28 C23 122.8(4) . . ?
C31 C29 C32 109.7(5) . . ?
C31 C29 C27 110.9(4) . . ?
C32 C29 C27 108.8(4) . . ?
C31 C29 C30 107.5(5) . . ?
C32 C29 C30 107.9(5) . . ?
C27 C29 C30 112.0(4) . . ?
C25 C33 C34 112.3(3) . . ?
C35 C34 C39 118.7(4) . . ?
C35 C34 C33 121.6(4) . . ?
C39 C34 C33 119.5(4) . . ?
C34 C35 C36 122.2(4) . . ?
C34 C35 O2 118.8(4) . . ?
C36 C35 O2 118.9(4) . . ?
C35 C36 C37 117.0(4) . . ?
C35 C36 C44 122.1(4) . . ?
C37 C36 C44 120.5(4) . . ?
C38 C37 C36 123.6(5) . . ?
C37 C38 C39 116.9(4) . . ?
C37 C38 C40 123.6(5) . . ?
C39 C38 C40 119.6(5) . . ?
C34 C39 C38 121.7(4) . . ?
C43A C40 C42B 130.4(7) . . ?
C43A C40 C38 111.3(5) . . ?
C42B C40 C38 109.3(6) . . ?
C43A C40 C41A 108.7(9) . . ?
C42B C40 C41A 80.9(9) . . ?
C38 C40 C41A 111.6(8) . . ?
C43A C40 C42A 110.5(7) . . ?
C42B C40 C42A 26.7(6) . . ?
C38 C40 C42A 109.5(6) . . ?
C41A C40 C42A 105.0(9) . . ?
C43A C40 C41B 89.8(8) . . ?
C42B C40 C41B 101.7(9) . . ?
C38 C40 C41B 110.5(7) . . ?
C41A C40 C41B 21.9(9) . . ?
C42A C40 C41B 123.6(9) . . ?
C43A C40 C43B 27.8(6) . . ?
C42B C40 C43B 109.4(9) . . ?
C38 C40 C43B 111.3(7) . . ?
C41A C40 C43B 128.8(10) . . ?
C42A C40 C43B 85.3(8) . . ?
C41B C40 C43B 114.2(9) . . ?
C1 C44 C36 110.3(3) . . ?
O2 C45 C46 106.8(3) . . ?
N1 C46 C45 113.8(4) . . ?
O5 C47 N1 121.9(4) . . ?
O5 C47 N2 121.1(4) . . ?
N1 C47 N2 117.0(4) . . ?
C56 C48 C49 118.8(5) . . ?
C56 C48 N2 120.3(5) . . ?
C49 C48 N2 120.8(5) . . ?
C48 C49 C50 124.0(5) . . ?
C49 C50 C51 118.4(5) . . ?
C50 C51 C57 118.6(5) . . ?
C53 C52 C57 118.2(6) . . ?
C52 C53 C54 119.9(6) . . ?
C55 C54 C53 122.7(5) . . ?
C54 C55 C56 119.6(6) . . ?
C48 C56 C57 121.8(5) . . ?
C48 C56 C55 122.1(5) . . ?
C57 C56 C55 116.0(5) . . ?
C56 C57 C52 123.5(5) . . ?
C56 C57 C51 118.3(5) . . ?
C52 C57 C51 118.3(5) . . ?
O4 C58 C59 106.0(3) . . ?
N3 C59 C58 112.3(3) . . ?
O6 C60 N4 120.6(4) . . ?
O6 C60 N3 121.9(4) . . ?
N4 C60 N3 117.5(4) . . ?
C62 C61 N4 120.1(5) . . ?
C62 C61 C69 121.4(5) . . ?
N4 C61 C69 118.5(4) . . ?
C61 C62 C63 118.1(6) . . ?
C64 C63 C62 119.0(5) . . ?
C63 C64 C70 125.4(6) . . ?
C66 C65 C70 119.2(5) . . ?
C65 C66 C67 121.8(6) . . ?
C68 C67 C66 119.8(6) . . ?
C67 C68 C69 121.4(5) . . ?
C68 C69 C70 117.8(5) . . ?
C68 C69 C61 122.8(4) . . ?
C70 C69 C61 119.5(5) . . ?
C64 C70 C65 123.3(5) . . ?
C64 C70 C69 116.6(5) . . ?
C65 C70 C69 120.1(5) . . ?
Cl1 C5S Cl2 111.0(4) . . ?
Cl1 C5S Cl3 110.2(3) . . ?
Cl2 C5S Cl3 113.4(4) . . ?
Cl5B Cl5A C6S 82.6(4) . . ?
Cl5A Cl5B C6S 74.2(4) . . ?
Cl4 C6S Cl5A 120.1(6) . . ?
Cl4 C6S Cl6 107.8(5) . . ?
Cl5A C6S Cl6 99.2(5) . . ?
Cl4 C6S Cl5B 100.0(5) . . ?
Cl5A C6S Cl5B 23.2(3) . . ?
Cl6 C6S Cl5B 118.8(5) . . ?
N1S C1S C2S 178.0(7) . . ?
N2S C3S C4S 178.1(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O4 0.84 2.01 2.678(4) 136.4 .
O3 H3 O2 0.84 2.00 2.686(4) 138.7 .
N1 H1B O1 0.88 2.24 3.039(4) 150.8 .
N2 H2 O6 0.88 2.37 3.067(5) 136.8 3_755
N3 H3B O3 0.88 2.36 3.078(5) 139.1 .
N4 H4 O6 0.88 1.95 2.826(5) 171.7 3_655
_database_code_depnum_ccdc_archive 'CCDC 1003766'
#######################################################################
#
#                 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_4c_S049

_audit_creation_method           SHELXL-97
_chemical_formula_moiety         'C64H80N4S2O6, 0.5 CH3OH, 1.5 C3H6O'
_chemical_formula_sum            'C69 H91 N4 O8 S2'
_chemical_formula_weight         1168.58
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
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'
S S 0.1246 0.1234 '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 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_angle_alpha                90.00
_cell_angle_beta                 111.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5803(5)
_cell_length_b                   20.1679(5)
_cell_length_c                   18.2981(5)
_cell_measurement_reflns_used    4582
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.528
_cell_measurement_theta_min      2.171
_cell_volume                     6708.2(3)
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_correction_T_min  0.2082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 SADABS-2006/1 (Bruker,2006) was used for absorption correction.
 R(int) was 0.1122 before and 0.0522 after correction.
 The Ratio of minimum to maximum transmission is 0.21262254902.
 The λ/2 correction factor is 0.0015
;
_exptl_crystal_F_000             2516
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_special_details           ?
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1568
_diffrn_reflns_av_sigmaI/netI    0.1566
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55928
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.51
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6803
_reflns_number_total             14623
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    
;
Olex2, Durham University (compiled Jan 29 2009 15:17:43)
;
_computing_publication_material  
;
Olex2, Durham University (compiled Jan 29 2009 15:17:43)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)/Bruker'
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.093
_refine_ls_R_factor_all          0.1991
_refine_ls_R_factor_gt           0.0936
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         14623
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_gt          0.2441
_refine_ls_wR_factor_ref         0.2932
_refine_ls_weighting_details     
;
calc w=1/[σ²(Fo²)+(0.1400P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_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.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
S1 S -0.29705(8) 0.09417(8) -0.30572(9) 0.0531(4) Uani 1 1 d D . .
S2 S -0.08488(8) -0.05754(6) -0.13362(7) 0.0356(3) Uani 1 1 d . . .
O1 O 0.11021(18) 0.47152(16) 0.00886(19) 0.0284(7) Uani 1 1 d . . .
O2 O 0.15994(16) 0.38049(14) -0.06955(16) 0.0216(6) Uani 1 1 d . . .
O3 O 0.12909(18) 0.30577(16) 0.05491(18) 0.0306(8) Uani 1 1 d . . .
O4 O 0.05012(16) 0.38692(14) 0.11323(16) 0.0230(7) Uani 1 1 d . . .
O5 O -0.03962(18) 0.31965(17) -0.31710(17) 0.0335(8) Uani 1 1 d . . .
O6 O -0.04788(18) 0.26953(15) -0.06888(17) 0.0298(7) Uani 1 1 d . . .
N1 N 0.0135(2) 0.33308(19) -0.1842(2) 0.0261(9) Uani 1 1 d . . .
N2 N -0.0841(2) 0.2620(2) -0.2368(3) 0.0322(10) Uani 1 1 d . . .
N3 N -0.0496(2) 0.27282(19) 0.0544(2) 0.0259(9) Uani 1 1 d . . .
N4 N -0.0347(2) 0.1739(2) 0.0020(3) 0.0302(10) Uani 1 1 d . . .
C1 C 0.0872(2) 0.5288(2) 0.1346(3) 0.0257(10) Uani 1 1 d . . .
H1B H 0.0684 0.5665 0.1564 0.031 Uiso 1 1 calc R . .
H1A H 0.0458 0.5101 0.0897 0.031 Uiso 1 1 calc R . .
C2 C 0.1472(2) 0.5526(2) 0.1070(3) 0.0229(9) Uani 1 1 d . . .
C3 C 0.1587(2) 0.5205(2) 0.0450(2) 0.0227(9) Uani 1 1 d . . .
C4 C 0.2154(3) 0.5406(2) 0.0216(3) 0.0246(10) Uani 1 1 d . . .
C5 C 0.2610(2) 0.5927(2) 0.0616(3) 0.0262(10) Uani 1 1 d . . .
H5 H 0.3006 0.6054 0.0465 0.031 Uiso 1 1 calc R . .
C6 C 0.2505(3) 0.6270(2) 0.1230(3) 0.0287(10) Uani 1 1 d . . .
C7 C 0.1922(2) 0.6053(2) 0.1438(3) 0.0264(10) Uani 1 1 d . . .
H7 H 0.1831 0.6278 0.1849 0.032 Uiso 1 1 calc R . .
C8 C 0.2983(3) 0.6863(3) 0.1645(3) 0.0380(12) Uani 1 1 d . . .
C9 C 0.2531(4) 0.7496(3) 0.1363(4) 0.0502(15) Uani 1 1 d . . .
H9B H 0.2382 0.7535 0.0791 0.075 Uiso 1 1 calc R . .
H9C H 0.2830 0.7881 0.1618 0.075 Uiso 1 1 calc R . .
H9A H 0.2093 0.7477 0.1500 0.075 Uiso 1 1 calc R . .
C10 C 0.3677(3) 0.6917(3) 0.1454(4) 0.0515(15) Uani 1 1 d . . .
H10A H 0.3955 0.6502 0.1595 0.077 Uiso 1 1 calc R . .
H10C H 0.3982 0.7283 0.1756 0.077 Uiso 1 1 calc R . .
H10B H 0.3539 0.7002 0.0890 0.077 Uiso 1 1 calc R . .
C11 C 0.3205(3) 0.6805(3) 0.2544(3) 0.0529(16) Uani 1 1 d . . .
H11B H 0.2763 0.6813 0.2674 0.079 Uiso 1 1 calc R . .
H11C H 0.3526 0.7177 0.2803 0.079 Uiso 1 1 calc R . .
H11A H 0.3469 0.6387 0.2727 0.079 Uiso 1 1 calc R . .
C12 C 0.2290(3) 0.5073(2) -0.0459(3) 0.0262(10) Uani 1 1 d . . .
H12B H 0.2568 0.5379 -0.0670 0.031 Uiso 1 1 calc R . .
H12A H 0.1812 0.4978 -0.0887 0.031 Uiso 1 1 calc R . .
C13 C 0.2720(2) 0.4431(2) -0.0202(2) 0.0227(9) Uani 1 1 d . . .
C14 C 0.2364(2) 0.3819(2) -0.0289(2) 0.0205(9) Uani 1 1 d . . .
C15 C 0.2738(2) 0.3243(2) 0.0022(2) 0.0214(9) Uani 1 1 d . . .
C16 C 0.3502(2) 0.3278(2) 0.0402(2) 0.0240(10) Uani 1 1 d . . .
H16 H 0.3767 0.2883 0.0609 0.029 Uiso 1 1 calc R . .
C17 C 0.3889(2) 0.3871(2) 0.0489(2) 0.0263(10) Uani 1 1 d . . .
C18 C 0.3481(3) 0.4440(2) 0.0184(3) 0.0264(10) Uani 1 1 d . . .
H18 H 0.3731 0.4852 0.0242 0.032 Uiso 1 1 calc R . .
C19 C 0.4731(3) 0.3900(3) 0.0877(3) 0.0348(11) Uani 1 1 d . . .
C20 C 0.4983(3) 0.4545(3) 0.1363(4) 0.0627(19) Uani 1 1 d . . .
H20A H 0.4778 0.4560 0.1776 0.094 Uiso 1 1 calc R . .
H20B H 0.4809 0.4930 0.1015 0.094 Uiso 1 1 calc R . .
H20C H 0.5521 0.4554 0.1604 0.094 Uiso 1 1 calc R . .
C21 C 0.5039(3) 0.3914(4) 0.0238(4) 0.066(2) Uani 1 1 d . . .
H21C H 0.5569 0.3999 0.0470 0.099 Uiso 1 1 calc R . .
H21B H 0.4797 0.4265 -0.0139 0.099 Uiso 1 1 calc R . .
H21A H 0.4951 0.3485 -0.0033 0.099 Uiso 1 1 calc R . .
C22 C 0.5039(3) 0.3319(3) 0.1431(4) 0.0603(19) Uani 1 1 d . . .
H22B H 0.4798 0.3298 0.1814 0.090 Uiso 1 1 calc R . .
H22C H 0.5570 0.3377 0.1709 0.090 Uiso 1 1 calc R . .
H22A H 0.4946 0.2906 0.1127 0.090 Uiso 1 1 calc R . .
C23 C 0.2341(3) 0.2595(2) -0.0003(3) 0.0256(10) Uani 1 1 d . . .
H23B H 0.2581 0.2237 -0.0192 0.031 Uiso 1 1 calc R . .
H23A H 0.1825 0.2633 -0.0377 0.031 Uiso 1 1 calc R . .
C24 C 0.2354(2) 0.2420(2) 0.0814(3) 0.0237(9) Uani 1 1 d . . .
C25 C 0.1835(2) 0.2686(2) 0.1084(3) 0.0233(9) Uani 1 1 d . . .
C26 C 0.1886(2) 0.2578(2) 0.1862(3) 0.0262(10) Uani 1 1 d . . .
C27 C 0.2458(3) 0.2172(2) 0.2338(3) 0.0297(11) Uani 1 1 d . . .
H27 H 0.2498 0.2093 0.2864 0.036 Uiso 1 1 calc R . .
C28 C 0.2972(2) 0.1879(2) 0.2081(3) 0.0288(10) Uani 1 1 d . A .
C29 C 0.2910(2) 0.2015(2) 0.1313(3) 0.0254(10) Uani 1 1 d . . .
H29 H 0.3256 0.1825 0.1122 0.030 Uiso 1 1 calc R . .
C30 C 0.3595(3) 0.1441(3) 0.2627(3) 0.0416(13) Uani 1 1 d . . .
C31A C 0.4252(7) 0.1781(6) 0.3013(7) 0.042(3) Uiso 0.50 1 d P A 1
H31B H 0.4165 0.2140 0.3329 0.063 Uiso 0.50 1 calc PR A 1
H31A H 0.4432 0.1968 0.2624 0.063 Uiso 0.50 1 calc PR A 1
H31C H 0.4620 0.1475 0.3357 0.063 Uiso 0.50 1 calc PR A 1
C32A C 0.3753(6) 0.0856(5) 0.2096(6) 0.033(2) Uiso 0.50 1 d P A 1
H32C H 0.4141 0.0563 0.2435 0.050 Uiso 0.50 1 calc PR A 1
H32B H 0.3911 0.1055 0.1696 0.050 Uiso 0.50 1 calc PR A 1
H32A H 0.3303 0.0600 0.1838 0.050 Uiso 0.50 1 calc PR A 1
C31B C 0.4209(8) 0.1988(7) 0.3250(9) 0.055(3) Uiso 0.50 1 d P A 2
H31D H 0.3968 0.2233 0.3550 0.083 Uiso 0.50 1 calc PR A 2
H31E H 0.4378 0.2299 0.2942 0.083 Uiso 0.50 1 calc PR A 2
H31F H 0.4631 0.1743 0.3614 0.083 Uiso 0.50 1 calc PR A 2
C32B C 0.4042(7) 0.1096(7) 0.2238(8) 0.053(3) Uiso 0.50 1 d P A 2
H32F H 0.4445 0.0855 0.2634 0.079 Uiso 0.50 1 calc PR A 2
H32E H 0.4244 0.1423 0.1977 0.079 Uiso 0.50 1 calc PR A 2
H32D H 0.3730 0.0783 0.1847 0.079 Uiso 0.50 1 calc PR A 2
C33 C 0.3349(3) 0.1039(3) 0.3187(3) 0.0445(14) Uani 1 1 d . A .
H33A H 0.2889 0.0808 0.2888 0.067 Uiso 1 1 calc R . .
H33B H 0.3269 0.1336 0.3572 0.067 Uiso 1 1 calc R . .
H33C H 0.3729 0.0714 0.3463 0.067 Uiso 1 1 calc R . .
C34 C 0.1341(3) 0.2874(2) 0.2178(3) 0.0293(10) Uani 1 1 d . . .
H34B H 0.1376 0.2629 0.2659 0.035 Uiso 1 1 calc R . .
H34A H 0.0838 0.2807 0.1783 0.035 Uiso 1 1 calc R . .
C35 C 0.1451(2) 0.3607(2) 0.2373(3) 0.0274(10) Uani 1 1 d . . .
C36 C 0.1050(2) 0.4086(2) 0.1837(2) 0.0229(9) Uani 1 1 d . . .
C37 C 0.1187(2) 0.4762(2) 0.1975(3) 0.0254(10) Uani 1 1 d . . .
C38 C 0.1678(3) 0.4949(2) 0.2711(3) 0.0310(11) Uani 1 1 d . . .
H38 H 0.1769 0.5408 0.2818 0.037 Uiso 1 1 calc R . .
C39 C 0.2040(3) 0.4506(3) 0.3292(3) 0.0354(12) Uani 1 1 d . . .
C40 C 0.1949(3) 0.3831(3) 0.3108(3) 0.0319(11) Uani 1 1 d . . .
H40 H 0.2228 0.3516 0.3488 0.038 Uiso 1 1 calc R . .
C41 C 0.2532(3) 0.4771(3) 0.4116(3) 0.0439(14) Uani 1 1 d . . .
C42 C 0.2080(4) 0.5288(3) 0.4395(4) 0.0626(18) Uani 1 1 d . . .
H42A H 0.1625 0.5081 0.4390 0.094 Uiso 1 1 calc R . .
H42B H 0.1960 0.5670 0.4040 0.094 Uiso 1 1 calc R . .
H42C H 0.2375 0.5435 0.4931 0.094 Uiso 1 1 calc R . .
C43 C 0.3189(3) 0.5134(3) 0.4067(3) 0.0576(17) Uani 1 1 d . . .
H43C H 0.3479 0.5324 0.4582 0.086 Uiso 1 1 calc R . .
H43B H 0.3019 0.5489 0.3675 0.086 Uiso 1 1 calc R . .
H43A H 0.3495 0.4823 0.3911 0.086 Uiso 1 1 calc R . .
C44 C 0.2749(4) 0.4248(3) 0.4729(3) 0.0557(17) Uani 1 1 d . . .
H44B H 0.2308 0.4032 0.4747 0.084 Uiso 1 1 calc R . .
H44C H 0.3027 0.4448 0.5242 0.084 Uiso 1 1 calc R . .
H44A H 0.3057 0.3919 0.4603 0.084 Uiso 1 1 calc R . .
C45 C 0.1397(2) 0.3768(2) -0.1534(2) 0.0249(10) Uani 1 1 d . . .
H45A H 0.1530 0.3329 -0.1682 0.030 Uiso 1 1 calc R . .
H45B H 0.1661 0.4113 -0.1711 0.030 Uiso 1 1 calc R . .
C46 C 0.0578(2) 0.3874(2) -0.1916(3) 0.0274(10) Uani 1 1 d . . .
H46A H 0.0447 0.4274 -0.1682 0.033 Uiso 1 1 calc R . .
H46B H 0.0454 0.3965 -0.2483 0.033 Uiso 1 1 calc R . .
C47 C -0.0373(2) 0.3058(2) -0.2503(3) 0.0269(10) Uani 1 1 d . . .
C48 C -0.1504(2) 0.2379(2) -0.2938(3) 0.0308(11) Uani 1 1 d . B .
C49 C -0.1798(3) 0.1826(3) -0.2752(3) 0.0339(11) Uani 1 1 d . . .
H49 H -0.1536 0.1592 -0.2280 0.041 Uiso 1 1 calc R B .
C50 C -0.2500(3) 0.1597(3) -0.3264(3) 0.0400(13) Uani 1 1 d . B .
C51 C -0.2858(3) 0.1942(3) -0.3958(3) 0.0485(15) Uani 1 1 d . . .
H51 H -0.3327 0.1793 -0.4305 0.058 Uiso 1 1 calc R B .
C52 C -0.2555(3) 0.2487(3) -0.4153(3) 0.0495(15) Uani 1 1 d . B .
H52 H -0.2808 0.2709 -0.4636 0.059 Uiso 1 1 calc R . .
C53 C -0.1871(3) 0.2722(3) -0.3644(3) 0.0385(12) Uani 1 1 d . . .
H53 H -0.1660 0.3106 -0.3773 0.046 Uiso 1 1 calc R B .
C54A C -0.2288(9) 0.0574(10) -0.2245(9) 0.036(5) Uiso 0.30 1 d PD B 4
H54A H -0.2147 0.0879 -0.1797 0.054 Uiso 0.30 1 calc PR B 4
H54B H -0.1858 0.0474 -0.2377 0.054 Uiso 0.30 1 calc PR B 4
H54C H -0.2479 0.0163 -0.2108 0.054 Uiso 0.30 1 calc PR B 4
C54B C -0.2426(6) 0.0676(7) -0.2087(5) 0.076(4) Uiso 0.70 1 d PD B 3
H54F H -0.2653 0.0285 -0.1953 0.115 Uiso 0.70 1 calc PR B 3
H54E H -0.2394 0.1034 -0.1714 0.115 Uiso 0.70 1 calc PR B 3
H54D H -0.1931 0.0562 -0.2062 0.115 Uiso 0.70 1 calc PR B 3
C55 C -0.0213(2) 0.3811(2) 0.1189(3) 0.0240(9) Uani 1 1 d . . .
H55B H -0.0422 0.4258 0.1189 0.029 Uiso 1 1 calc R . .
H55A H -0.0162 0.3589 0.1689 0.029 Uiso 1 1 calc R . .
C56 C -0.0717(3) 0.3417(2) 0.0509(3) 0.0285(10) Uani 1 1 d . . .
H56B H -0.1223 0.3441 0.0507 0.034 Uiso 1 1 calc R . .
H56A H -0.0723 0.3615 0.0012 0.034 Uiso 1 1 calc R . .
C57 C -0.0440(2) 0.2412(2) -0.0080(2) 0.0236(9) Uani 1 1 d . . .
C58 C -0.0242(2) 0.1304(2) -0.0534(3) 0.0271(10) Uani 1 1 d . . .
C59 C -0.0567(2) 0.0681(2) -0.0627(3) 0.0263(10) Uani 1 1 d . . .
H59 H -0.0861 0.0564 -0.0335 0.032 Uiso 1 1 calc R . .
C60 C -0.0461(3) 0.0227(2) -0.1153(3) 0.0286(10) Uani 1 1 d . . .
C61 C -0.0025(3) 0.0405(3) -0.1576(3) 0.0369(12) Uani 1 1 d . . .
H61 H 0.0050 0.0100 -0.1935 0.044 Uiso 1 1 calc R . .
C62 C 0.0294(3) 0.1018(3) -0.1473(3) 0.0360(12) Uani 1 1 d . . .
H62 H 0.0591 0.1135 -0.1762 0.043 Uiso 1 1 calc R . .
C63 C 0.0190(3) 0.1471(2) -0.0953(3) 0.0330(11) Uani 1 1 d . . .
H63 H 0.0416 0.1896 -0.0886 0.040 Uiso 1 1 calc R . .
C64 C -0.1396(3) -0.0633(2) -0.0745(3) 0.0343(11) Uani 1 1 d . . .
H64A H -0.1083 -0.0570 -0.0190 0.051 Uiso 1 1 calc R . .
H64C H -0.1628 -0.1072 -0.0815 0.051 Uiso 1 1 calc R . .
H64B H -0.1778 -0.0290 -0.0907 0.051 Uiso 1 1 calc R . .
H1 H 0.009(2) 0.328(2) -0.147(3) 0.016(13) Uiso 1 1 d . . .
H1C H 0.136(4) 0.447(3) -0.006(4) 0.07(2) Uiso 1 1 d . . .
H2 H -0.078(2) 0.249(2) -0.196(3) 0.05(2) Uiso 1 1 d . . .
H3 H -0.054(3) 0.253(3) 0.090(3) 0.034(15) Uiso 1 1 d . . .
H3B H 0.094(3) 0.312(3) 0.076(3) 0.054(18) Uiso 1 1 d . . .
H4 H -0.035(3) 0.158(3) 0.038(3) 0.026(15) Uiso 1 1 d . . .
O1S O 0.4334(6) 0.3191(6) 0.5306(7) 0.093(3) Uiso 0.50 1 d P . .
C1S C 0.4871(7) 0.3499(6) 0.5346(7) 0.049(3) Uiso 0.50 1 d P . .
C2S C 0.5441(7) 0.3183(6) 0.5123(8) 0.055(3) Uiso 0.50 1 d P . .
H2SC H 0.5899 0.3152 0.5585 0.083 Uiso 0.50 1 calc PR . .
H2SB H 0.5525 0.3449 0.4716 0.083 Uiso 0.50 1 calc PR . .
H2SA H 0.5279 0.2738 0.4918 0.083 Uiso 0.50 1 calc PR . .
C3S C 0.4947(7) 0.4162(6) 0.5610(8) 0.058(3) Uiso 0.50 1 d P . .
H3SA H 0.4466 0.4333 0.5574 0.087 Uiso 0.50 1 calc PR . .
H3SB H 0.5135 0.4433 0.5281 0.087 Uiso 0.50 1 calc PR . .
H3SC H 0.5291 0.4182 0.6159 0.087 Uiso 0.50 1 calc PR . .
C4S C 0.3748(4) 0.4264(3) 0.2550(4) 0.0523(15) Uiso 1 1 d . . .
O2S O 0.4258(4) 0.4633(4) 0.2859(4) 0.075(2) Uiso 0.70 1 d P C 3
C5S C 0.3047(5) 0.4423(5) 0.1931(5) 0.051(2) Uiso 0.70 1 d P C 3
H5SA H 0.2941 0.4099 0.1503 0.076 Uiso 0.70 1 calc PR C 3
H5SC H 0.3071 0.4868 0.1727 0.076 Uiso 0.70 1 calc PR C 3
H5SB H 0.2657 0.4409 0.2144 0.076 Uiso 0.70 1 calc PR C 3
C6S C 0.3777(6) 0.3544(5) 0.2791(6) 0.070(3) Uiso 0.70 1 d P C 3
H6SB H 0.3433 0.3470 0.3059 0.105 Uiso 0.70 1 calc PR C 3
H6SC H 0.4277 0.3433 0.3149 0.105 Uiso 0.70 1 calc PR C 3
H6SA H 0.3640 0.3262 0.2323 0.105 Uiso 0.70 1 calc PR C 3
O2SA O 0.4312(11) 0.4080(11) 0.3060(12) 0.102(6) Uiso 0.30 1 d P C 4
C5SA C 0.3698(12) 0.5015(10) 0.2307(13) 0.059(6) Uiso 0.30 1 d P C 4
H5SE H 0.3649 0.5050 0.1756 0.089 Uiso 0.30 1 calc PR C 4
H5SF H 0.4145 0.5246 0.2642 0.089 Uiso 0.30 1 calc PR C 4
H5SD H 0.3268 0.5217 0.2371 0.089 Uiso 0.30 1 calc PR C 4
C6SA C 0.3138(10) 0.3914(9) 0.2024(11) 0.042(4) Uiso 0.30 1 d P C 4
H6SD H 0.3195 0.3440 0.2150 0.063 Uiso 0.30 1 calc PR C 4
H6SF H 0.3109 0.3983 0.1483 0.063 Uiso 0.30 1 calc PR C 4
H6SE H 0.2686 0.4077 0.2075 0.063 Uiso 0.30 1 calc PR C 4
O4S O 0.5691(5) 0.4403(4) 0.3930(5) 0.059(2) Uiso 0.50 1 d P . .
C7S C 0.6093(6) 0.4043(5) 0.3640(6) 0.042(3) Uiso 0.50 1 d P . .
H7SC H 0.6486 0.3822 0.4070 0.064 Uiso 0.50 1 calc PR . .
H7SB H 0.6310 0.4330 0.3351 0.064 Uiso 0.50 1 calc PR . .
H7SA H 0.5782 0.3708 0.3281 0.064 Uiso 0.50 1 calc PR . .
H4S H 0.5264 0.4359 0.3683 0.064 Uiso 0.50 1 d P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix. The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry. An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C50 1.732(6) . ?
S1 C54A 1.751(9) . ?
S1 C54B 1.779(8) . ?
S2 C60 1.766(5) . ?
S2 C64 1.787(5) . ?
O1 C3 1.359(5) . ?
O1 H1C 0.83(7) . ?
O2 C14 1.403(5) . ?
O2 C45 1.436(5) . ?
O3 C25 1.372(5) . ?
O3 H3B 0.92(6) . ?
O4 C36 1.406(5) . ?
O4 C55 1.444(5) . ?
O5 C47 1.239(5) . ?
O6 C57 1.229(5) . ?
N1 C47 1.364(6) . ?
N1 C46 1.435(6) . ?
N1 H1 0.73(5) . ?
N2 C47 1.360(6) . ?
N2 C48 1.415(6) . ?
N2 H2 0.75(4) . ?
N3 C57 1.348(6) . ?
N3 C56 1.450(6) . ?
N3 H3 0.80(5) . ?
N4 C57 1.373(6) . ?
N4 C58 1.412(6) . ?
N4 H4 0.73(5) . ?
C1 C37 1.516(6) . ?
C1 C2 1.519(6) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 C7 1.386(6) . ?
C2 C3 1.396(6) . ?
C3 C4 1.390(6) . ?
C4 C5 1.396(6) . ?
C4 C12 1.515(6) . ?
C5 C6 1.398(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.401(6) . ?
C6 C8 1.534(7) . ?
C7 H7 0.9500 . ?
C8 C10 1.526(7) . ?
C8 C9 1.529(8) . ?
C8 C11 1.542(8) . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 H9A 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10B 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 H11A 0.9800 . ?
C12 C13 1.521(6) . ?
C12 H12B 0.9900 . ?
C12 H12A 0.9900 . ?
C13 C18 1.392(6) . ?
C13 C14 1.396(6) . ?
C14 C15 1.380(6) . ?
C15 C16 1.397(6) . ?
C15 C23 1.512(6) . ?
C16 C17 1.393(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(6) . ?
C17 C19 1.535(6) . ?
C18 H18 0.9500 . ?
C19 C21 1.501(8) . ?
C19 C22 1.521(7) . ?
C19 C20 1.549(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21C 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 H22A 0.9800 . ?
C23 C24 1.527(6) . ?
C23 H23B 0.9900 . ?
C23 H23A 0.9900 . ?
C24 C25 1.391(6) . ?
C24 C29 1.396(6) . ?
C25 C26 1.407(6) . ?
C26 C27 1.400(6) . ?
C26 C34 1.511(6) . ?
C27 C28 1.392(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.393(6) . ?
C28 C30 1.536(6) . ?
C29 H29 0.9500 . ?
C30 C31A 1.395(13) . ?
C30 C32B 1.489(13) . ?
C30 C33 1.519(7) . ?
C30 C32A 1.629(12) . ?
C30 C31B 1.714(15) . ?
C31A H31B 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32C 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32A 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32F 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32D 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.518(7) . ?
C34 H34B 0.9900 . ?
C34 H34A 0.9900 . ?
C35 C36 1.394(6) . ?
C35 C40 1.410(6) . ?
C36 C37 1.394(6) . ?
C37 C38 1.386(6) . ?
C38 C39 1.368(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.398(7) . ?
C39 C41 1.551(7) . ?
C40 H40 0.9500 . ?
C41 C44 1.481(7) . ?
C41 C43 1.512(8) . ?
C41 C42 1.570(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43C 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C44 H44A 0.9800 . ?
C45 C46 1.508(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C48 C49 1.355(7) . ?
C48 C53 1.404(7) . ?
C49 C50 1.422(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.388(8) . ?
C51 C52 1.359(8) . ?
C51 H51 0.9500 . ?
C52 C53 1.399(7) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C54B H54F 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54D 0.9800 . ?
C55 C56 1.497(6) . ?
C55 H55B 0.9900 . ?
C55 H55A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 H56A 0.9900 . ?
C58 C63 1.380(6) . ?
C58 C59 1.390(6) . ?
C59 C60 1.397(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.397(7) . ?
C61 C62 1.365(7) . ?
C61 H61 0.9500 . ?
C62 C63 1.388(7) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 H64A 0.9800 . ?
C64 H64C 0.9800 . ?
C64 H64B 0.9800 . ?
O1S C1S 1.200(15) . ?
C1S C3S 1.411(17) . ?
C1S C2S 1.468(17) . ?
C2S H2SC 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SA 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
C4S O2S 1.204(9) . ?
C4S O2SA 1.21(2) . ?
C4S C6SA 1.413(18) . ?
C4S C5S 1.455(10) . ?
C4S C6S 1.513(12) . ?
C4S C5SA 1.57(2) . ?
C5S H5SA 0.9800 . ?
C5S H5SC 0.9800 . ?
C5S H5SB 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?
C6S H6SA 0.9800 . ?
C5SA H5SE 0.9800 . ?
C5SA H5SF 0.9800 . ?
C5SA H5SD 0.9800 . ?
C6SA H6SD 0.9800 . ?
C6SA H6SF 0.9800 . ?
C6SA H6SE 0.9800 . ?
O4S C7S 1.320(13) . ?
O4S H4S 0.7932 . ?
C7S H7SC 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SA 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
C50 S1 C54A 102.0(7) . . ?
C50 S1 C54B 106.1(5) . . ?
C54A S1 C54B 16.5(8) . . ?
C60 S2 C64 104.9(2) . . ?
C3 O1 H1C 101(5) . . ?
C14 O2 C45 112.5(3) . . ?
C25 O3 H3B 107(4) . . ?
C36 O4 C55 112.9(3) . . ?
C47 N1 C46 119.5(4) . . ?
C47 N1 H1 117(4) . . ?
C46 N1 H1 120(4) . . ?
C47 N2 C48 125.7(4) . . ?
C47 N2 H2 122(3) . . ?
C48 N2 H2 113(3) . . ?
C57 N3 C56 122.2(4) . . ?
C57 N3 H3 122(4) . . ?
C56 N3 H3 113(4) . . ?
C57 N4 C58 124.5(4) . . ?
C57 N4 H4 120(4) . . ?
C58 N4 H4 116(4) . . ?
C37 C1 C2 109.0(4) . . ?
C37 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
C37 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
H1B C1 H1A 108.3 . . ?
C7 C2 C3 119.0(4) . . ?
C7 C2 C1 120.7(4) . . ?
C3 C2 C1 120.2(4) . . ?
O1 C3 C4 123.8(4) . . ?
O1 C3 C2 115.9(4) . . ?
C4 C3 C2 120.2(4) . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 C12 121.6(4) . . ?
C5 C4 C12 119.3(4) . . ?
C6 C5 C4 122.5(4) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C7 116.2(4) . . ?
C5 C6 C8 122.6(4) . . ?
C7 C6 C8 121.2(4) . . ?
C2 C7 C6 122.9(4) . . ?
C2 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
C10 C8 C9 108.4(5) . . ?
C10 C8 C6 112.0(4) . . ?
C9 C8 C6 108.2(4) . . ?
C10 C8 C11 109.1(5) . . ?
C9 C8 C11 108.8(5) . . ?
C6 C8 C11 110.3(4) . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10C C10 H10B 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
H11B C11 H11A 109.5 . . ?
H11C C11 H11A 109.5 . . ?
C4 C12 C13 111.8(4) . . ?
C4 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C4 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
H12B C12 H12A 107.9 . . ?
C18 C13 C14 117.6(4) . . ?
C18 C13 C12 120.7(4) . . ?
C14 C13 C12 121.5(4) . . ?
C15 C14 C13 122.2(4) . . ?
C15 C14 O2 120.0(4) . . ?
C13 C14 O2 117.8(4) . . ?
C14 C15 C16 117.9(4) . . ?
C14 C15 C23 121.8(4) . . ?
C16 C15 C23 120.2(4) . . ?
C17 C16 C15 122.5(4) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C18 C17 C16 117.1(4) . . ?
C18 C17 C19 120.8(4) . . ?
C16 C17 C19 122.1(4) . . ?
C17 C18 C13 122.6(4) . . ?
C17 C18 H18 118.7 . . ?
C13 C18 H18 118.7 . . ?
C21 C19 C22 111.1(5) . . ?
C21 C19 C17 108.2(4) . . ?
C22 C19 C17 111.7(4) . . ?
C21 C19 C20 107.3(5) . . ?
C22 C19 C20 107.6(5) . . ?
C17 C19 C20 110.9(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21C 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21C C21 H21B 109.5 . . ?
C19 C21 H21A 109.5 . . ?
H21C C21 H21A 109.5 . . ?
H21B C21 H21A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
C15 C23 C24 110.3(3) . . ?
C15 C23 H23B 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C15 C23 H23A 109.6 . . ?
C24 C23 H23A 109.6 . . ?
H23B C23 H23A 108.1 . . ?
C25 C24 C29 119.2(4) . . ?
C25 C24 C23 120.7(4) . . ?
C29 C24 C23 120.1(4) . . ?
O3 C25 C24 115.7(4) . . ?
O3 C25 C26 123.3(4) . . ?
C24 C25 C26 121.0(4) . . ?
C27 C26 C25 117.3(4) . . ?
C27 C26 C34 120.5(4) . . ?
C25 C26 C34 122.2(4) . . ?
C28 C27 C26 123.4(4) . . ?
C28 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
C29 C28 C27 117.0(4) . . ?
C29 C28 C30 121.4(4) . . ?
C27 C28 C30 121.6(4) . . ?
C28 C29 C24 122.0(4) . . ?
C28 C29 H29 119.0 . . ?
C24 C29 H29 119.0 . . ?
C31A C30 C32B 83.0(8) . . ?
C31A C30 C33 112.6(7) . . ?
C32B C30 C33 117.6(7) . . ?
C31A C30 C28 114.0(7) . . ?
C32B C30 C28 115.0(6) . . ?
C33 C30 C28 111.8(4) . . ?
C31A C30 C32A 108.3(7) . . ?
C32B C30 C32A 26.0(5) . . ?
C33 C30 C32A 101.2(6) . . ?
C28 C30 C32A 108.0(5) . . ?
C31A C30 C31B 20.2(7) . . ?
C32B C30 C31B 103.2(8) . . ?
C33 C30 C31B 102.4(6) . . ?
C28 C30 C31B 104.7(6) . . ?
C32A C30 C31B 128.4(7) . . ?
C30 C31A H31B 109.5 . . ?
C30 C31A H31A 109.5 . . ?
C30 C31A H31C 109.5 . . ?
C30 C32A H32C 109.5 . . ?
C30 C32A H32B 109.5 . . ?
C30 C32A H32A 109.5 . . ?
C30 C31B H31D 109.5 . . ?
C30 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C30 C32B H32F 109.5 . . ?
C30 C32B H32E 109.5 . . ?
H32F C32B H32E 109.5 . . ?
C30 C32B H32D 109.5 . . ?
H32F C32B H32D 109.5 . . ?
H32E C32B H32D 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C34 C35 114.6(4) . . ?
C26 C34 H34B 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C26 C34 H34A 108.6 . . ?
C35 C34 H34A 108.6 . . ?
H34B C34 H34A 107.6 . . ?
C36 C35 C40 117.3(4) . . ?
C36 C35 C34 121.1(4) . . ?
C40 C35 C34 121.6(4) . . ?
C37 C36 C35 122.0(4) . . ?
C37 C36 O4 120.0(4) . . ?
C35 C36 O4 117.9(4) . . ?
C38 C37 C36 117.3(4) . . ?
C38 C37 C1 119.1(4) . . ?
C36 C37 C1 123.4(4) . . ?
C39 C38 C37 123.4(5) . . ?
C39 C38 H38 118.3 . . ?
C37 C38 H38 118.3 . . ?
C38 C39 C40 117.8(4) . . ?
C38 C39 C41 119.1(4) . . ?
C40 C39 C41 123.2(4) . . ?
C39 C40 C35 121.6(4) . . ?
C39 C40 H40 119.2 . . ?
C35 C40 H40 119.2 . . ?
C44 C41 C43 112.2(5) . . ?
C44 C41 C39 113.0(4) . . ?
C43 C41 C39 110.0(4) . . ?
C44 C41 C42 105.4(5) . . ?
C43 C41 C42 107.0(5) . . ?
C39 C41 C42 108.9(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43C 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43C C43 H43B 109.5 . . ?
C41 C43 H43A 109.5 . . ?
H43C C43 H43A 109.5 . . ?
H43B C43 H43A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
H44B C44 H44A 109.5 . . ?
H44C C44 H44A 109.5 . . ?
O2 C45 C46 108.2(3) . . ?
O2 C45 H45A 110.1 . . ?
C46 C45 H45A 110.1 . . ?
O2 C45 H45B 110.1 . . ?
C46 C45 H45B 110.1 . . ?
H45A C45 H45B 108.4 . . ?
N1 C46 C45 115.1(4) . . ?
N1 C46 H46A 108.5 . . ?
C45 C46 H46A 108.5 . . ?
N1 C46 H46B 108.5 . . ?
C45 C46 H46B 108.5 . . ?
H46A C46 H46B 107.5 . . ?
O5 C47 N2 123.1(4) . . ?
O5 C47 N1 122.0(4) . . ?
N2 C47 N1 114.9(4) . . ?
C49 C48 C53 121.0(5) . . ?
C49 C48 N2 117.1(4) . . ?
C53 C48 N2 121.7(5) . . ?
C48 C49 C50 119.9(5) . . ?
C48 C49 H49 120.0 . . ?
C50 C49 H49 120.0 . . ?
C51 C50 C49 118.5(5) . . ?
C51 C50 S1 116.9(4) . . ?
C49 C50 S1 124.5(4) . . ?
C52 C51 C50 121.6(5) . . ?
C52 C51 H51 119.2 . . ?
C50 C51 H51 119.2 . . ?
C51 C52 C53 120.2(5) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 H52 119.9 . . ?
C52 C53 C48 118.8(5) . . ?
C52 C53 H53 120.6 . . ?
C48 C53 H53 120.6 . . ?
S1 C54A H54A 109.5 . . ?
S1 C54A H54B 109.4 . . ?
S1 C54A H54C 109.5 . . ?
S1 C54B H54F 109.5 . . ?
S1 C54B H54E 109.5 . . ?
S1 C54B H54D 109.5 . . ?
O4 C55 C56 109.9(4) . . ?
O4 C55 H55B 109.7 . . ?
C56 C55 H55B 109.7 . . ?
O4 C55 H55A 109.7 . . ?
C56 C55 H55A 109.7 . . ?
H55B C55 H55A 108.2 . . ?
N3 C56 C55 112.2(4) . . ?
N3 C56 H56B 109.2 . . ?
C55 C56 H56B 109.2 . . ?
N3 C56 H56A 109.2 . . ?
C55 C56 H56A 109.2 . . ?
H56B C56 H56A 107.9 . . ?
O6 C57 N3 123.4(4) . . ?
O6 C57 N4 122.8(4) . . ?
N3 C57 N4 113.8(4) . . ?
C63 C58 C59 120.1(4) . . ?
C63 C58 N4 122.0(4) . . ?
C59 C58 N4 117.9(4) . . ?
C58 C59 C60 119.9(4) . . ?
C58 C59 H59 120.1 . . ?
C60 C59 H59 120.1 . . ?
C61 C60 C59 119.5(4) . . ?
C61 C60 S2 116.0(4) . . ?
C59 C60 S2 124.6(4) . . ?
C62 C61 C60 119.8(5) . . ?
C62 C61 H61 120.1 . . ?
C60 C61 H61 120.1 . . ?
C61 C62 C63 121.1(5) . . ?
C61 C62 H62 119.5 . . ?
C63 C62 H62 119.5 . . ?
C58 C63 C62 119.7(5) . . ?
C58 C63 H63 120.2 . . ?
C62 C63 H63 120.2 . . ?
S2 C64 H64A 109.5 . . ?
S2 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
S2 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64C C64 H64B 109.5 . . ?
O1S C1S C3S 119.4(12) . . ?
O1S C1S C2S 119.8(12) . . ?
C3S C1S C2S 120.8(11) . . ?
C1S C2S H2SC 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SC C2S H2SB 109.5 . . ?
C1S C2S H2SA 109.5 . . ?
H2SC C2S H2SA 109.5 . . ?
H2SB C2S H2SA 109.5 . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
O2S C4S O2SA 57.8(11) . . ?
O2S C4S C6SA 166.4(10) . . ?
O2SA C4S C6SA 132.1(14) . . ?
O2S C4S C5S 127.4(7) . . ?
O2SA C4S C5S 174.8(13) . . ?
C6SA C4S C5S 42.7(8) . . ?
O2S C4S C6S 121.4(7) . . ?
O2SA C4S C6S 63.6(11) . . ?
C6SA C4S C6S 69.5(9) . . ?
C5S C4S C6S 111.2(7) . . ?
O2S C4S C5SA 59.4(9) . . ?
O2SA C4S C5SA 117.2(14) . . ?
C6SA C4S C5SA 109.9(12) . . ?
C5S C4S C5SA 68.0(9) . . ?
C6S C4S C5SA 178.3(11) . . ?
C4S C5S H5SA 109.5 . . ?
C4S C5S H5SC 109.5 . . ?
C4S C5S H5SB 109.5 . . ?
C4S C6S H6SB 109.5 . . ?
C4S C6S H6SC 109.5 . . ?
C4S C6S H6SA 109.5 . . ?
C4S C5SA H5SE 109.5 . . ?
C4S C5SA H5SF 109.5 . . ?
C4S C5SA H5SD 109.5 . . ?
C4S C6SA H6SD 109.5 . . ?
C4S C6SA H6SF 109.5 . . ?
C4S C6SA H6SE 109.5 . . ?
C7S O4S H4S 111.6 . . ?
O4S C7S H7SC 109.5 . . ?
O4S C7S H7SB 109.5 . . ?
H7SC C7S H7SB 109.5 . . ?
O4S C7S H7SA 109.5 . . ?
H7SC C7S H7SA 109.5 . . ?
H7SB C7S H7SA 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1C O2 0.83(7) 1.93(7) 2.723(4) 158(6) .
O3 H3B O4 0.92(6) 1.97(6) 2.727(4) 138(5) .
O4S H4S O2S 0.79 2.06 2.801(11) 154.7 .
O4S H4S O2SA 0.79 1.87 2.66(2) 168.3 .
N1 H1 O6 0.73(5) 2.41(5) 3.071(5) 151(5) .
N2 H2 O6 0.75(4) 2.22(4) 2.889(5) 149(4) .
N3 H3 O5 0.80(5) 2.18(5) 2.950(5) 162(5) 4_566
N4 H4 O5 0.73(5) 2.72(5) 3.349(5) 145(5) 4_566
_database_code_depnum_ccdc_archive 'CCDC 1003767'
#######################################################################
#
#                 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_5_s458

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H88 N4 O8 S2, 4 C2 H3 N'
_chemical_formula_sum            'C80 H100 N8 O8 S2'
_chemical_formula_weight         1365.80

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1        '
_symmetry_space_group_name_Hall  '-P 1        '
_symmetry_int_tables_number      2

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

_cell_length_a                   12.1816(3)
_cell_length_b                   24.5969(7)
_cell_length_c                   26.7522(7)
_cell_angle_alpha                102.923(10)
_cell_angle_beta                 95.542(10)
_cell_angle_gamma                98.546(10)
_cell_volume                     7655.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5852
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      26.59

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2928
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_absorpt_correction_T_min  0.9491
_exptl_absorpt_correction_T_max  0.9898

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            85996
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         27.50
_reflns_number_total             35131
_reflns_number_gt                21045
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART Ver. 5.630 (Bruker-AXS, 2003)'
_computing_cell_refinement       'SAINT Ver. 6.45  (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.45'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

_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)+(0.0800P)²+2.4000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         35131
_refine_ls_number_parameters     1822
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.1766
_refine_ls_wR_factor_gt          0.1502
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.045
_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
S1 S 0.53554(6) 0.96814(3) 0.63214(2) 0.02573(14) Uani 1 1 d . . .
S2 S 0.02056(5) 0.85885(3) 0.63021(2) 0.02401(14) Uani 1 1 d . . .
O1 O 0.47111(15) 0.81454(7) 0.57227(7) 0.0240(4) Uani 1 1 d . . .
O2 O 0.25465(13) 0.76923(7) 0.54442(6) 0.0211(4) Uani 1 1 d . . .
O3 O 0.26999(16) 0.76989(7) 0.65514(7) 0.0248(4) Uani 1 1 d . . .
O4 O 0.48289(13) 0.82795(7) 0.68648(6) 0.0209(4) Uani 1 1 d . . .
O5 O 0.64921(16) 0.95818(8) 0.64029(7) 0.0339(4) Uani 1 1 d . . .
O6 O 0.51515(17) 1.02224(8) 0.65842(7) 0.0338(4) Uani 1 1 d . . .
O7 O -0.02794(15) 0.82142(8) 0.65944(7) 0.0302(4) Uani 1 1 d . . .
O8 O -0.04989(15) 0.87243(8) 0.59023(7) 0.0309(4) Uani 1 1 d . . .
N1 N 0.44628(19) 0.91973(9) 0.64729(8) 0.0272(5) Uani 1 1 d . . .
N2 N 0.11752(18) 0.83005(9) 0.60347(8) 0.0230(4) Uani 1 1 d . . .
N3 N 0.2248(2) 0.93527(10) 0.41121(9) 0.0337(5) Uani 1 1 d . . .
N4 N 0.34228(18) 1.04131(9) 0.82251(8) 0.0282(5) Uani 1 1 d . . .
C1 C 0.6799(2) 0.82239(10) 0.63184(9) 0.0229(5) Uani 1 1 d . . .
H1A H 0.7613 0.8374 0.6381 0.027 Uiso 1 1 calc R . .
H1B H 0.6398 0.8550 0.6363 0.027 Uiso 1 1 calc R . .
C2 C 0.6482(2) 0.78602(10) 0.57693(9) 0.0218(5) Uani 1 1 d . . .
C3 C 0.5431(2) 0.78249(10) 0.54880(9) 0.0219(5) Uani 1 1 d . . .
C4 C 0.5148(2) 0.74773(10) 0.49867(10) 0.0241(5) Uani 1 1 d . . .
C5 C 0.5907(2) 0.71477(11) 0.47813(10) 0.0270(6) Uani 1 1 d . . .
H5 H 0.5713 0.6910 0.4442 0.032 Uiso 1 1 calc R . .
C6 C 0.6938(2) 0.71543(11) 0.50554(10) 0.0268(6) Uani 1 1 d . . .
C7 C 0.7216(2) 0.75231(10) 0.55450(10) 0.0251(5) Uani 1 1 d . . .
H7 H 0.7931 0.7546 0.5733 0.030 Uiso 1 1 calc R . .
C8 C 0.7750(2) 0.67646(12) 0.48480(12) 0.0348(7) Uani 1 1 d . . .
C9 C 0.7942(3) 0.63905(15) 0.52255(17) 0.0593(10) Uani 1 1 d . . .
H9A H 0.7219 0.6186 0.5271 0.071 Uiso 1 1 calc R . .
H9B H 0.8316 0.6629 0.5560 0.071 Uiso 1 1 calc R . .
H9C H 0.8413 0.6118 0.5086 0.071 Uiso 1 1 calc R . .
C10 C 0.7302(3) 0.63824(17) 0.43174(15) 0.0694(13) Uani 1 1 d . . .
H10G H 0.7837 0.6134 0.4208 0.083 Uiso 1 1 calc R . .
H10F H 0.7195 0.6615 0.4069 0.083 Uiso 1 1 calc R . .
H10H H 0.6583 0.6152 0.4333 0.083 Uiso 1 1 calc R . .
C11 C 0.8884(2) 0.71162(14) 0.48303(13) 0.0431(8) Uani 1 1 d . . .
H11I H 0.9413 0.6863 0.4723 0.052 Uiso 1 1 calc R . .
H11J H 0.9172 0.7361 0.5175 0.052 Uiso 1 1 calc R . .
H11K H 0.8796 0.7350 0.4582 0.052 Uiso 1 1 calc R . .
C12 C 0.4001(2) 0.74229(11) 0.46790(9) 0.0243(5) Uani 1 1 d . . .
H12G H 0.3745 0.7793 0.4755 0.029 Uiso 1 1 calc R . .
H12H H 0.4055 0.7314 0.4304 0.029 Uiso 1 1 calc R . .
C13 C 0.3156(2) 0.69790(10) 0.48182(9) 0.0223(5) Uani 1 1 d . . .
C14 C 0.2476(2) 0.71211(10) 0.51980(9) 0.0206(5) Uani 1 1 d . . .
C15 C 0.1788(2) 0.67085(10) 0.53639(9) 0.0221(5) Uani 1 1 d . . .
C16 C 0.1768(2) 0.61415(10) 0.51162(10) 0.0254(5) Uani 1 1 d . . .
H16D H 0.1293 0.5855 0.5219 0.030 Uiso 1 1 calc R . .
C17 C 0.2416(2) 0.59796(10) 0.47261(10) 0.0263(6) Uani 1 1 d . A .
C18 C 0.3106(2) 0.64071(10) 0.45873(10) 0.0247(5) Uani 1 1 d . . .
H18 H 0.3563 0.6306 0.4325 0.030 Uiso 1 1 calc R . .
C19 C 0.2426(2) 0.53527(11) 0.44856(11) 0.0322(6) Uani 1 1 d . . .
C20A C 0.3211(6) 0.5163(3) 0.4887(3) 0.0426(16) Uiso 0.50 1 d P A 1
H20D H 0.3270 0.4765 0.4754 0.051 Uiso 0.50 1 calc PR A 1
H20E H 0.2899 0.5207 0.5215 0.051 Uiso 0.50 1 calc PR A 1
H20F H 0.3956 0.5399 0.4944 0.051 Uiso 0.50 1 calc PR A 1
C21A C 0.2951(6) 0.5272(3) 0.3975(3) 0.0418(15) Uiso 0.50 1 d P A 1
H21D H 0.2957 0.4868 0.3837 0.050 Uiso 0.50 1 calc PR A 1
H21F H 0.3720 0.5483 0.4043 0.050 Uiso 0.50 1 calc PR A 1
H21E H 0.2507 0.5413 0.3722 0.050 Uiso 0.50 1 calc PR A 1
C22A C 0.1308(5) 0.5013(3) 0.4388(3) 0.0369(16) Uiso 0.50 1 d P A 1
H22B H 0.0812 0.5171 0.4170 0.044 Uiso 0.50 1 calc PR A 1
H22A H 0.1018 0.5016 0.4718 0.044 Uiso 0.50 1 calc PR A 1
H22C H 0.1342 0.4622 0.4211 0.044 Uiso 0.50 1 calc PR A 1
C20B C 0.3459(6) 0.5176(3) 0.4705(3) 0.0362(15) Uiso 0.50 1 d P A 2
H20A H 0.3474 0.4782 0.4531 0.043 Uiso 0.50 1 calc PR A 2
H20B H 0.3454 0.5208 0.5076 0.043 Uiso 0.50 1 calc PR A 2
H20C H 0.4125 0.5421 0.4650 0.043 Uiso 0.50 1 calc PR A 2
C21B C 0.2379(6) 0.5246(3) 0.3890(3) 0.0430(15) Uiso 0.50 1 d P A 2
H21C H 0.3045 0.5467 0.3807 0.052 Uiso 0.50 1 calc PR A 2
H21A H 0.1705 0.5361 0.3746 0.052 Uiso 0.50 1 calc PR A 2
H21B H 0.2358 0.4842 0.3741 0.052 Uiso 0.50 1 calc PR A 2
C22B C 0.1359(5) 0.4946(3) 0.4578(3) 0.0340(15) Uiso 0.50 1 d P A 2
H22E H 0.0675 0.5066 0.4452 0.041 Uiso 0.50 1 calc PR A 2
H22D H 0.1380 0.4965 0.4949 0.041 Uiso 0.50 1 calc PR A 2
H22F H 0.1365 0.4555 0.4391 0.041 Uiso 0.50 1 calc PR A 2
C23 C 0.1138(2) 0.68461(10) 0.58201(9) 0.0234(5) Uani 1 1 d . . .
H23B H 0.1041 0.7247 0.5883 0.028 Uiso 1 1 calc R . .
H23A H 0.0384 0.6607 0.5737 0.028 Uiso 1 1 calc R . .
C24 C 0.1744(2) 0.67446(10) 0.63061(9) 0.0220(5) Uani 1 1 d . . .
C25 C 0.2551(2) 0.71653(10) 0.66477(9) 0.0210(5) Uani 1 1 d . . .
C26 C 0.3164(2) 0.70460(10) 0.70638(9) 0.0226(5) Uani 1 1 d . . .
C27 C 0.2953(2) 0.64966(11) 0.71395(10) 0.0250(5) Uani 1 1 d . . .
H27B H 0.3383 0.6410 0.7418 0.030 Uiso 1 1 calc R . .
C28 C 0.2136(2) 0.60734(11) 0.68211(10) 0.0257(5) Uani 1 1 d . . .
C29 C 0.1542(2) 0.62136(11) 0.64100(10) 0.0261(5) Uani 1 1 d . . .
H29 H 0.0972 0.5932 0.6191 0.031 Uiso 1 1 calc R . .
C30 C 0.1848(3) 0.54800(11) 0.69145(11) 0.0327(6) Uani 1 1 d . . .
C31 C 0.1929(3) 0.50296(12) 0.64263(12) 0.0424(7) Uani 1 1 d . . .
H31B H 0.1746 0.4652 0.6491 0.051 Uiso 1 1 calc R . .
H31A H 0.2693 0.5086 0.6338 0.051 Uiso 1 1 calc R . .
H31C H 0.1401 0.5063 0.6139 0.051 Uiso 1 1 calc R . .
C32 C 0.2642(3) 0.53985(13) 0.73605(13) 0.0473(8) Uani 1 1 d . . .
H32A H 0.2433 0.5015 0.7409 0.057 Uiso 1 1 calc R . .
H32B H 0.2589 0.5677 0.7679 0.057 Uiso 1 1 calc R . .
H32C H 0.3412 0.5452 0.7279 0.057 Uiso 1 1 calc R . .
C33 C 0.0646(3) 0.53959(13) 0.70511(13) 0.0435(8) Uani 1 1 d . . .
H33A H 0.0121 0.5422 0.6759 0.052 Uiso 1 1 calc R . .
H33B H 0.0590 0.5690 0.7357 0.052 Uiso 1 1 calc R . .
H33C H 0.0462 0.5022 0.7124 0.052 Uiso 1 1 calc R . .
C34 C 0.4068(2) 0.74835(10) 0.74367(9) 0.0230(5) Uani 1 1 d . . .
H34B H 0.3841 0.7860 0.7489 0.028 Uiso 1 1 calc R . .
H34A H 0.4140 0.7385 0.7776 0.028 Uiso 1 1 calc R . .
C35 C 0.5195(2) 0.75133(10) 0.72356(9) 0.0232(5) Uani 1 1 d . . .
C36 C 0.5528(2) 0.78941(10) 0.69418(9) 0.0210(5) Uani 1 1 d . . .
C37 C 0.6501(2) 0.78820(10) 0.67069(9) 0.0212(5) Uani 1 1 d . . .
C38 C 0.7193(2) 0.75071(11) 0.68175(10) 0.0263(5) Uani 1 1 d . . .
H38B H 0.7877 0.7506 0.6675 0.032 Uiso 1 1 calc R . .
C39 C 0.6921(2) 0.71362(11) 0.71272(10) 0.0295(6) Uani 1 1 d . . .
C40 C 0.5902(2) 0.71373(11) 0.73233(10) 0.0263(5) Uani 1 1 d . . .
H40B H 0.5683 0.6875 0.7522 0.032 Uiso 1 1 calc R . .
C41 C 0.7752(3) 0.67566(14) 0.72478(12) 0.0420(7) Uani 1 1 d . . .
C42 C 0.8827(3) 0.71401(18) 0.75567(15) 0.0642(11) Uani 1 1 d . . .
H42A H 0.9385 0.6907 0.7622 0.077 Uiso 1 1 calc R . .
H42B H 0.8657 0.7353 0.7887 0.077 Uiso 1 1 calc R . .
H42C H 0.9125 0.7405 0.7358 0.077 Uiso 1 1 calc R . .
C43 C 0.8053(3) 0.64182(15) 0.67432(14) 0.0546(9) Uani 1 1 d . . .
H43B H 0.8570 0.6169 0.6821 0.066 Uiso 1 1 calc R . .
H43A H 0.8412 0.6679 0.6555 0.066 Uiso 1 1 calc R . .
H43C H 0.7371 0.6189 0.6530 0.066 Uiso 1 1 calc R . .
C44 C 0.7287(4) 0.6348(2) 0.75569(19) 0.0805(15) Uani 1 1 d . . .
H44A H 0.6608 0.6100 0.7358 0.097 Uiso 1 1 calc R . .
H44B H 0.7105 0.6562 0.7884 0.097 Uiso 1 1 calc R . .
H44C H 0.7848 0.6118 0.7628 0.097 Uiso 1 1 calc R . .
C45 C 0.5172(2) 0.88362(10) 0.72106(9) 0.0242(5) Uani 1 1 d . . .
H45B H 0.5970 0.8982 0.7202 0.029 Uiso 1 1 calc R . .
H45A H 0.5068 0.8822 0.7570 0.029 Uiso 1 1 calc R . .
C46 C 0.4438(2) 0.92106(11) 0.70205(10) 0.0261(5) Uani 1 1 d . . .
H46B H 0.3657 0.9087 0.7076 0.031 Uiso 1 1 calc R . .
H46A H 0.4688 0.9605 0.7227 0.031 Uiso 1 1 calc R . .
C47 C 0.4916(2) 0.95099(10) 0.56461(10) 0.0266(6) Uani 1 1 d . . .
C48 C 0.5612(2) 0.92494(11) 0.53398(10) 0.0285(6) Uani 1 1 d . . .
H48B H 0.6290 0.9171 0.5491 0.034 Uiso 1 1 calc R . .
C49 C 0.5323(2) 0.90980(11) 0.48009(10) 0.0295(6) Uani 1 1 d . . .
H49 H 0.5817 0.8926 0.4587 0.035 Uiso 1 1 calc R . .
C50 C 0.4333(2) 0.91960(11) 0.45814(10) 0.0287(6) Uani 1 1 d . . .
H50B H 0.4155 0.9098 0.4215 0.034 Uiso 1 1 calc R . .
C51 C 0.2526(2) 0.95374(12) 0.46530(11) 0.0316(6) Uani 1 1 d . . .
C52 C 0.1867(2) 0.98354(12) 0.49651(12) 0.0343(6) Uani 1 1 d . . .
H52B H 0.1188 0.9913 0.4814 0.041 Uiso 1 1 calc R . .
C53 C 0.2185(2) 1.00252(12) 0.55025(12) 0.0337(6) Uani 1 1 d . . .
H53B H 0.1721 1.0236 0.5705 0.040 Uiso 1 1 calc R . .
C54 C 0.3143(2) 0.99156(11) 0.57437(11) 0.0315(6) Uani 1 1 d . . .
H54 H 0.3325 1.0033 0.6109 0.038 Uiso 1 1 calc R . .
C55 C 0.3869(2) 0.96189(10) 0.54330(10) 0.0248(5) Uani 1 1 d . . .
C56 C 0.3565(2) 0.94419(11) 0.48915(10) 0.0283(6) Uani 1 1 d . . .
C57 C 0.2022(3) 0.87383(13) 0.38997(12) 0.0446(8) Uani 1 1 d . . .
H57C H 0.1240 0.8589 0.3921 0.053 Uiso 1 1 calc R . .
H57A H 0.2519 0.8561 0.4099 0.053 Uiso 1 1 calc R . .
H57B H 0.2154 0.8653 0.3537 0.053 Uiso 1 1 calc R . .
C58 C 0.1433(3) 0.96210(14) 0.38756(12) 0.0414(7) Uani 1 1 d . . .
H58A H 0.1414 0.9517 0.3499 0.050 Uiso 1 1 calc R . .
H58B H 0.1639 1.0033 0.4002 0.050 Uiso 1 1 calc R . .
H58C H 0.0692 0.9495 0.3965 0.050 Uiso 1 1 calc R . .
C59 C 0.1808(2) 0.79981(10) 0.52052(10) 0.0239(5) Uani 1 1 d . . .
H59B H 0.1068 0.7756 0.5070 0.029 Uiso 1 1 calc R . .
H59A H 0.2130 0.8123 0.4915 0.029 Uiso 1 1 calc R . .
C60 C 0.1695(2) 0.85020(10) 0.56236(10) 0.0254(5) Uani 1 1 d . . .
H60B H 0.2442 0.8734 0.5765 0.030 Uiso 1 1 calc R . .
H60A H 0.1227 0.8741 0.5479 0.030 Uiso 1 1 calc R . .
C61 C 0.0870(2) 0.92426(10) 0.67304(9) 0.0224(5) Uani 1 1 d . . .
C62 C 0.0738(2) 0.97212(11) 0.65657(10) 0.0268(6) Uani 1 1 d . . .
H62 H 0.0290 0.9691 0.6246 0.032 Uiso 1 1 calc R . .
C63 C 0.1263(2) 1.02552(11) 0.68691(10) 0.0282(6) Uani 1 1 d . . .
H63B H 0.1149 1.0587 0.6761 0.034 Uiso 1 1 calc R . .
C64 C 0.1937(2) 1.02994(10) 0.73189(10) 0.0249(5) Uani 1 1 d . . .
H64 H 0.2296 1.0663 0.7518 0.030 Uiso 1 1 calc R . .
C65 C 0.2829(2) 0.98628(10) 0.79671(10) 0.0239(5) Uani 1 1 d . . .
C66 C 0.2902(2) 0.93886(11) 0.81528(10) 0.0268(6) Uani 1 1 d . . .
H66B H 0.3347 0.9422 0.8473 0.032 Uiso 1 1 calc R . .
C67 C 0.2316(2) 0.88548(11) 0.78681(10) 0.0272(6) Uani 1 1 d . . .
H67 H 0.2375 0.8532 0.8002 0.033 Uiso 1 1 calc R . .
C68 C 0.1668(2) 0.87866(10) 0.74067(10) 0.0242(5) Uani 1 1 d . . .
H68 H 0.1300 0.8419 0.7219 0.029 Uiso 1 1 calc R . .
C69 C 0.1542(2) 0.92677(10) 0.72050(9) 0.0215(5) Uani 1 1 d . . .
C70 C 0.2111(2) 0.98139(10) 0.74948(9) 0.0218(5) Uani 1 1 d . . .
C71 C 0.4354(2) 1.06102(12) 0.79612(12) 0.0359(7) Uani 1 1 d . . .
H71A H 0.4973 1.0408 0.8016 0.043 Uiso 1 1 calc R . .
H71B H 0.4611 1.1018 0.8102 0.043 Uiso 1 1 calc R . .
H71C H 0.4099 1.0536 0.7590 0.043 Uiso 1 1 calc R . .
C72 C 0.3806(3) 1.04905(12) 0.87759(11) 0.0400(7) Uani 1 1 d . . .
H72B H 0.3179 1.0360 0.8948 0.048 Uiso 1 1 calc R . .
H72A H 0.4094 1.0893 0.8932 0.048 Uiso 1 1 calc R . .
H72C H 0.4403 1.0270 0.8816 0.048 Uiso 1 1 calc R . .
S21 S 0.84477(6) 0.88339(3) 0.00284(3) 0.02673(14) Uani 1 1 d . . .
S22 S 1.31718(5) 0.82820(3) 0.08752(3) 0.02818(15) Uani 1 1 d . . .
O21 O 0.82031(15) 0.74506(7) 0.05614(7) 0.0244(4) Uani 1 1 d . . .
O22 O 0.89140(14) 0.83568(7) 0.15277(6) 0.0215(4) Uani 1 1 d . . .
O23 O 1.07142(16) 0.78602(7) 0.16540(7) 0.0247(4) Uani 1 1 d . . .
O24 O 1.00585(14) 0.70075(7) 0.06711(6) 0.0219(4) Uani 1 1 d . . .
O25 O 0.74266(16) 0.84806(8) -0.02479(7) 0.0352(5) Uani 1 1 d . . .
O26 O 0.84942(17) 0.94335(8) 0.01882(7) 0.0350(5) Uani 1 1 d . . .
O27 O 1.38640(16) 0.82342(9) 0.13182(8) 0.0373(5) Uani 1 1 d . . .
O28 O 1.35793(16) 0.81732(8) 0.03843(8) 0.0351(5) Uani 1 1 d . . .
N21 N 0.87175(19) 0.86143(9) 0.05408(8) 0.0266(5) Uani 1 1 d . . .
N22 N 1.20169(19) 0.78450(10) 0.08154(9) 0.0289(5) Uani 1 1 d . . .
N23 N 1.1854(2) 0.75348(11) -0.13318(9) 0.0361(6) Uani 1 1 d . . .
N24 N 1.1463(2) 1.06057(10) 0.19802(9) 0.0385(6) Uani 1 1 d . . .
C101 C 0.8053(2) 0.62405(10) 0.01398(9) 0.0227(5) Uani 1 1 d . . .
H10D H 0.7706 0.5894 -0.0128 0.027 Uiso 1 1 calc R . .
H10E H 0.8450 0.6510 -0.0035 0.027 Uiso 1 1 calc R . .
C102 C 0.7134(2) 0.65040(10) 0.04024(9) 0.0219(5) Uani 1 1 d . . .
C103 C 0.72607(19) 0.70882(10) 0.06082(9) 0.0203(5) Uani 1 1 d . . .
C104 C 0.6418(2) 0.73266(10) 0.08525(9) 0.0219(5) Uani 1 1 d . . .
C105 C 0.5448(2) 0.69673(11) 0.08803(10) 0.0255(5) Uani 1 1 d . . .
H105 H 0.4868 0.7126 0.1041 0.031 Uiso 1 1 calc R . .
C106 C 0.5285(2) 0.63781(11) 0.06818(10) 0.0267(6) Uani 1 1 d . . .
C107 C 0.6148(2) 0.61605(10) 0.04443(10) 0.0251(5) Uani 1 1 d . . .
H107 H 0.6060 0.5763 0.0306 0.030 Uiso 1 1 calc R . .
C108 C 0.4193(2) 0.60113(12) 0.07400(11) 0.0331(6) Uani 1 1 d . . .
C109 C 0.4117(3) 0.53896(12) 0.04664(14) 0.0475(9) Uani 1 1 d . . .
H10B H 0.4733 0.5239 0.0620 0.057 Uiso 1 1 calc R . .
H10A H 0.4168 0.5357 0.0098 0.057 Uiso 1 1 calc R . .
H10C H 0.3400 0.5174 0.0506 0.057 Uiso 1 1 calc R . .
C110 C 0.4120(2) 0.60549(13) 0.13175(12) 0.0384(7) Uani 1 1 d . . .
H11A H 0.3430 0.5815 0.1356 0.046 Uiso 1 1 calc R . .
H11B H 0.4115 0.6449 0.1493 0.046 Uiso 1 1 calc R . .
H11C H 0.4769 0.5928 0.1472 0.046 Uiso 1 1 calc R . .
C111 C 0.3187(2) 0.62261(13) 0.05065(13) 0.0398(7) Uani 1 1 d . . .
H11E H 0.3228 0.6202 0.0138 0.048 Uiso 1 1 calc R . .
H11D H 0.3201 0.6621 0.0687 0.048 Uiso 1 1 calc R . .
H11F H 0.2490 0.5992 0.0545 0.048 Uiso 1 1 calc R . .
C112 C 0.6564(2) 0.79541(10) 0.11077(9) 0.0226(5) Uani 1 1 d . . .
H11H H 0.7087 0.8171 0.0932 0.027 Uiso 1 1 calc R . .
H11G H 0.5833 0.8082 0.1072 0.027 Uiso 1 1 calc R . .
C113 C 0.7018(2) 0.80705(10) 0.16760(9) 0.0215(5) Uani 1 1 d . . .
C114 C 0.8146(2) 0.82414(10) 0.18661(9) 0.0216(5) Uani 1 1 d . . .
C115 C 0.8556(2) 0.82778(10) 0.23806(9) 0.0232(5) Uani 1 1 d . . .
C116 C 0.7787(2) 0.81672(11) 0.27124(10) 0.0272(6) Uani 1 1 d . . .
H116 H 0.8055 0.8193 0.3064 0.033 Uiso 1 1 calc R . .
C117 C 0.6636(2) 0.80193(11) 0.25488(10) 0.0295(6) Uani 1 1 d . B .
C118 C 0.6277(2) 0.79704(11) 0.20294(10) 0.0277(6) Uani 1 1 d . . .
H118 H 0.5498 0.7865 0.1908 0.033 Uiso 1 1 calc R . .
C119 C 0.5816(3) 0.79164(14) 0.29332(12) 0.0420(7) Uani 1 1 d . . .
C120 C 0.4618(4) 0.7730(2) 0.26833(18) 0.0547(11) Uiso 0.80 1 d P B 1
H12A H 0.4550 0.7375 0.2419 0.066 Uiso 0.80 1 calc PR B 1
H12B H 0.4388 0.8023 0.2522 0.066 Uiso 0.80 1 calc PR B 1
H12C H 0.4137 0.7671 0.2947 0.066 Uiso 0.80 1 calc PR B 1
C121 C 0.5910(3) 0.84714(17) 0.33500(15) 0.0433(9) Uiso 0.80 1 d P B 1
H12J H 0.5683 0.8765 0.3189 0.052 Uiso 0.80 1 calc PR B 1
H12I H 0.6687 0.8594 0.3518 0.052 Uiso 0.80 1 calc PR B 1
H12K H 0.5421 0.8409 0.3609 0.052 Uiso 0.80 1 calc PR B 1
C122 C 0.6192(4) 0.7467(2) 0.32085(19) 0.0559(11) Uiso 0.80 1 d P B 1
H12E H 0.5708 0.7416 0.3473 0.067 Uiso 0.80 1 calc PR B 1
H12D H 0.6970 0.7597 0.3373 0.067 Uiso 0.80 1 calc PR B 1
H12F H 0.6134 0.7106 0.2954 0.067 Uiso 0.80 1 calc PR B 1
C220 C 0.4842(18) 0.7395(9) 0.2680(8) 0.066(5) Uiso 0.20 1 d P B 2
H22G H 0.5143 0.7041 0.2640 0.099 Uiso 0.20 1 calc PR B 2
H22H H 0.4531 0.7431 0.2339 0.099 Uiso 0.20 1 calc PR B 2
H22I H 0.4251 0.7389 0.2903 0.099 Uiso 0.20 1 calc PR B 2
C221 C 0.478(3) 0.8274(13) 0.2867(12) 0.111(10) Uiso 0.20 1 d P B 2
H22J H 0.5067 0.8681 0.3000 0.167 Uiso 0.20 1 calc PR B 2
H22K H 0.4187 0.8155 0.3061 0.167 Uiso 0.20 1 calc PR B 2
H22L H 0.4484 0.8198 0.2500 0.167 Uiso 0.20 1 calc PR B 2
C222 C 0.616(3) 0.7918(17) 0.3435(14) 0.136(12) Uiso 0.20 1 d P B 2
H22M H 0.6778 0.7704 0.3446 0.205 Uiso 0.20 1 calc PR B 2
H22O H 0.5538 0.7743 0.3583 0.205 Uiso 0.20 1 calc PR B 2
H22P H 0.6424 0.8310 0.3635 0.205 Uiso 0.20 1 calc PR B 2
C123 C 0.9807(2) 0.83980(10) 0.25740(9) 0.0242(5) Uani 1 1 d . . .
H12L H 1.0203 0.8641 0.2375 0.029 Uiso 1 1 calc R . .
H12M H 0.9936 0.8606 0.2943 0.029 Uiso 1 1 calc R . .
C124 C 1.0281(2) 0.78531(10) 0.25165(9) 0.0224(5) Uani 1 1 d . . .
C125 C 1.0688(2) 0.76041(10) 0.20632(9) 0.0211(5) Uani 1 1 d . . .
C126 C 1.1100(2) 0.70995(10) 0.20185(9) 0.0222(5) Uani 1 1 d . . .
C127 C 1.1101(2) 0.68446(10) 0.24332(10) 0.0251(5) Uani 1 1 d . . .
H127 H 1.1399 0.6505 0.2406 0.030 Uiso 1 1 calc R . .
C128 C 1.0681(2) 0.70686(11) 0.28866(10) 0.0272(6) Uani 1 1 d . . .
C129 C 1.0270(2) 0.75758(11) 0.29149(9) 0.0256(5) Uani 1 1 d . . .
H129 H 0.9973 0.7736 0.3219 0.031 Uiso 1 1 calc R . .
C130 C 1.0613(3) 0.67725(12) 0.33328(11) 0.0380(7) Uani 1 1 d . . .
C131 C 0.9351(3) 0.65615(17) 0.33570(14) 0.0623(11) Uani 1 1 d . . .
H13A H 0.9016 0.6294 0.3029 0.075 Uiso 1 1 calc R . .
H13B H 0.8958 0.6886 0.3416 0.075 Uiso 1 1 calc R . .
H13C H 0.9285 0.6372 0.3641 0.075 Uiso 1 1 calc R . .
C132 C 1.1074(3) 0.71826(14) 0.38471(11) 0.0467(8) Uani 1 1 d . . .
H13J H 1.0643 0.7492 0.3905 0.056 Uiso 1 1 calc R . .
H13I H 1.1862 0.7338 0.3844 0.056 Uiso 1 1 calc R . .
H13K H 1.1017 0.6984 0.4125 0.056 Uiso 1 1 calc R . .
C133 C 1.1172(4) 0.62585(16) 0.32574(14) 0.0726(13) Uani 1 1 d . . .
H13E H 1.1083 0.6081 0.3548 0.087 Uiso 1 1 calc R . .
H13D H 1.1971 0.6373 0.3241 0.087 Uiso 1 1 calc R . .
H13F H 1.0825 0.5987 0.2934 0.087 Uiso 1 1 calc R . .
C134 C 1.1481(2) 0.68032(10) 0.15193(9) 0.0226(5) Uani 1 1 d . . .
H13G H 1.1740 0.7088 0.1327 0.027 Uiso 1 1 calc R . .
H13H H 1.2120 0.6619 0.1603 0.027 Uiso 1 1 calc R . .
C135 C 1.0541(2) 0.63601(10) 0.11792(9) 0.0216(5) Uani 1 1 d . . .
C136 C 0.9837(2) 0.64764(10) 0.07901(9) 0.0205(5) Uani 1 1 d . . .
C137 C 0.8894(2) 0.60895(10) 0.05205(9) 0.0205(5) Uani 1 1 d . . .
C138 C 0.8703(2) 0.55615(10) 0.06342(10) 0.0248(5) Uani 1 1 d . . .
H138 H 0.8069 0.5292 0.0452 0.030 Uiso 1 1 calc R . .
C139 C 0.9405(2) 0.54121(10) 0.10057(10) 0.0270(6) Uani 1 1 d . . .
C140 C 1.0307(2) 0.58229(10) 0.12763(10) 0.0254(5) Uani 1 1 d . . .
H140 H 1.0783 0.5734 0.1538 0.030 Uiso 1 1 calc R . .
C141 C 0.9196(3) 0.48147(11) 0.10977(11) 0.0389(7) Uani 1 1 d . . .
C142 C 0.9479(4) 0.44025(14) 0.06399(14) 0.0617(11) Uani 1 1 d . . .
H14D H 0.9254 0.4014 0.0674 0.074 Uiso 1 1 calc R . .
H14E H 1.0288 0.4477 0.0628 0.074 Uiso 1 1 calc R . .
H14F H 0.9080 0.4449 0.0320 0.074 Uiso 1 1 calc R . .
C143 C 0.7932(4) 0.46430(16) 0.11454(18) 0.0683(11) Uani 1 1 d . . .
H14B H 0.7476 0.4633 0.0820 0.082 Uiso 1 1 calc R . .
H14A H 0.7721 0.4921 0.1427 0.082 Uiso 1 1 calc R . .
H14C H 0.7804 0.4268 0.1219 0.082 Uiso 1 1 calc R . .
C144 C 0.9849(4) 0.47788(14) 0.15949(14) 0.0656(12) Uani 1 1 d . . .
H14H H 0.9678 0.5062 0.1884 0.079 Uiso 1 1 calc R . .
H14G H 1.0653 0.4852 0.1571 0.079 Uiso 1 1 calc R . .
H14I H 0.9640 0.4399 0.1652 0.079 Uiso 1 1 calc R . .
C145 C 0.9100(2) 0.89354(10) 0.14790(10) 0.0251(5) Uani 1 1 d . . .
H14J H 0.9644 0.9178 0.1771 0.030 Uiso 1 1 calc R . .
H14K H 0.8389 0.9085 0.1480 0.030 Uiso 1 1 calc R . .
C146 C 0.9553(2) 0.89316(11) 0.09738(10) 0.0268(6) Uani 1 1 d . . .
H14L H 0.9762 0.9326 0.0941 0.032 Uiso 1 1 calc R . .
H14M H 1.0235 0.8757 0.0968 0.032 Uiso 1 1 calc R . .
C147 C 0.9537(2) 0.87181(11) -0.03554(10) 0.0272(6) Uani 1 1 d . . .
C148 C 1.0267(2) 0.91897(12) -0.03792(11) 0.0327(6) Uani 1 1 d . . .
H148 H 1.0158 0.9555 -0.0204 0.039 Uiso 1 1 calc R . .
C149 C 1.1176(3) 0.91373(12) -0.06616(11) 0.0365(7) Uani 1 1 d . . .
H149 H 1.1662 0.9467 -0.0687 0.044 Uiso 1 1 calc R . .
C150 C 1.1358(2) 0.86157(12) -0.08978(11) 0.0330(6) Uani 1 1 d . . .
H150 H 1.1981 0.8585 -0.1084 0.040 Uiso 1 1 calc R . .
C151 C 1.0843(2) 0.75630(12) -0.11157(10) 0.0287(6) Uani 1 1 d . . .
C152 C 1.0053(2) 0.70944(12) -0.11441(10) 0.0313(6) Uani 1 1 d . . .
H152 H 1.0166 0.6732 -0.1325 0.038 Uiso 1 1 calc R . .
C153 C 0.9075(2) 0.71426(11) -0.09077(10) 0.0296(6) Uani 1 1 d . . .
H153 H 0.8530 0.6814 -0.0937 0.035 Uiso 1 1 calc R . .
C154 C 0.8899(2) 0.76559(11) -0.06370(10) 0.0261(5) Uani 1 1 d . . .
H154 H 0.8259 0.7678 -0.0462 0.031 Uiso 1 1 calc R . .
C155 C 0.9670(2) 0.81580(11) -0.06155(9) 0.0240(5) Uani 1 1 d . . .
C156 C 1.0639(2) 0.81138(11) -0.08732(9) 0.0256(5) Uani 1 1 d . . .
C157 C 1.1892(3) 0.70083(15) -0.17031(13) 0.0501(9) Uani 1 1 d . . .
H15D H 1.1858 0.6698 -0.1527 0.060 Uiso 1 1 calc R . .
H15E H 1.2590 0.7045 -0.1856 0.060 Uiso 1 1 calc R . .
H15F H 1.1252 0.6926 -0.1977 0.060 Uiso 1 1 calc R . .
C158 C 1.2868(3) 0.76924(16) -0.09445(12) 0.0471(8) Uani 1 1 d . . .
H15H H 1.2805 0.8029 -0.0680 0.056 Uiso 1 1 calc R . .
H15G H 1.3528 0.7774 -0.1115 0.056 Uiso 1 1 calc R . .
H15I H 1.2943 0.7378 -0.0781 0.056 Uiso 1 1 calc R . .
C159 C 1.0760(2) 0.70300(11) 0.02714(10) 0.0255(5) Uani 1 1 d . . .
H15B H 1.0311 0.6874 -0.0074 0.031 Uiso 1 1 calc R . .
H15A H 1.1359 0.6804 0.0306 0.031 Uiso 1 1 calc R . .
C160 C 1.1263(2) 0.76427(11) 0.03306(10) 0.0248(5) Uani 1 1 d . . .
H16F H 1.1681 0.7681 0.0037 0.030 Uiso 1 1 calc R . .
H16E H 1.0662 0.7872 0.0330 0.030 Uiso 1 1 calc R . .
C161 C 1.2822(2) 0.89745(11) 0.09825(10) 0.0285(6) Uani 1 1 d . . .
C162 C 1.2788(2) 0.92113(12) 0.05704(11) 0.0342(6) Uani 1 1 d . . .
H162 H 1.2953 0.9010 0.0248 0.041 Uiso 1 1 calc R . .
C163 C 1.2508(3) 0.97583(12) 0.06193(12) 0.0368(7) Uani 1 1 d . . .
H163 H 1.2519 0.9928 0.0333 0.044 Uiso 1 1 calc R . .
C164 C 1.2226(2) 1.00400(13) 0.10676(11) 0.0358(7) Uani 1 1 d . . .
H164 H 1.2038 1.0406 0.1094 0.043 Uiso 1 1 calc R . .
C165 C 1.1871(2) 1.00921(12) 0.19757(11) 0.0325(6) Uani 1 1 d . . .
C166 C 1.2027(3) 0.98837(13) 0.24058(11) 0.0392(7) Uani 1 1 d . . .
H166 H 1.1864 1.0089 0.2727 0.047 Uiso 1 1 calc R . .
C167 C 1.2425(3) 0.93686(14) 0.23811(11) 0.0405(7) Uani 1 1 d . . .
H167 H 1.2546 0.9241 0.2688 0.049 Uiso 1 1 calc R . .
C168 C 1.2639(2) 0.90523(13) 0.19270(11) 0.0347(6) Uani 1 1 d . . .
H168 H 1.2841 0.8691 0.1913 0.042 Uiso 1 1 calc R . .
C169 C 1.2559(2) 0.92646(11) 0.14667(10) 0.0261(6) Uani 1 1 d . . .
C170 C 1.2206(2) 0.97956(12) 0.15044(11) 0.0311(6) Uani 1 1 d . . .
C171 C 1.0349(3) 1.05222(14) 0.16749(13) 0.0463(8) Uani 1 1 d . . .
H17B H 1.0353 1.0283 0.1329 0.056 Uiso 1 1 calc R . .
H17A H 1.0173 1.0890 0.1644 0.056 Uiso 1 1 calc R . .
H17C H 0.9783 1.0338 0.1849 0.056 Uiso 1 1 calc R . .
C172 C 1.1435(3) 1.09646(14) 0.24894(12) 0.0477(8) Uani 1 1 d . . .
H17D H 1.0889 1.0772 0.2667 0.057 Uiso 1 1 calc R . .
H17E H 1.1220 1.1323 0.2452 0.057 Uiso 1 1 calc R . .
H17F H 1.2179 1.1040 0.2693 0.057 Uiso 1 1 calc R . .
N1S N 0.6141(2) 0.04496(13) 0.05163(12) 0.0521(7) Uani 1 1 d D . .
C1S C 0.5462(2) 0.06691(13) 0.03663(12) 0.0394(7) Uani 1 1 d D . .
C2S C 0.4631(3) 0.09430(14) 0.01718(13) 0.0478(8) Uani 1 1 d D . .
H2SB H 0.4036 0.0659 -0.0056 0.057 Uiso 1 1 calc R . .
H2SA H 0.4969 0.1202 -0.0024 0.057 Uiso 1 1 calc R . .
H2SC H 0.4315 0.1158 0.0461 0.057 Uiso 1 1 calc R . .
N2S N 0.4983(4) 0.3148(2) 0.14600(17) 0.1021(16) Uani 1 1 d . . .
C3S C 0.4750(4) 0.2973(2) 0.10212(19) 0.0691(12) Uani 1 1 d . . .
C4S C 0.4497(4) 0.2752(2) 0.04639(18) 0.0844(15) Uani 1 1 d . . .
H4SC H 0.4109 0.3011 0.0313 0.101 Uiso 1 1 calc R . .
H4SB H 0.4015 0.2379 0.0387 0.101 Uiso 1 1 calc R . .
H4SA H 0.5195 0.2716 0.0315 0.101 Uiso 1 1 calc R . .
N3S N 0.6734(3) 0.58280(16) 0.21067(17) 0.0817(12) Uani 1 1 d . . .
C5S C 0.7259(3) 0.61969(14) 0.20006(13) 0.0439(8) Uani 1 1 d . . .
C6S C 0.7912(3) 0.66648(13) 0.18615(13) 0.0419(7) Uani 1 1 d . . .
H6SA H 0.8098 0.6540 0.1510 0.050 Uiso 1 1 calc R . .
H6SC H 0.8604 0.6801 0.2105 0.050 Uiso 1 1 calc R . .
H6SB H 0.7478 0.6972 0.1874 0.050 Uiso 1 1 calc R . .
N4S N 0.4424(5) 0.6375(2) 0.3465(2) 0.0813(15) Uiso 0.70 1 d PD C 1
C7S C 0.4707(5) 0.5971(2) 0.3253(2) 0.0701(16) Uiso 0.70 1 d PD C 1
C8S C 0.5259(10) 0.5515(4) 0.3066(5) 0.154(4) Uiso 0.70 1 d PD C 1
H8SA H 0.4788 0.5252 0.2766 0.231 Uiso 0.70 1 calc PR C 1
H8SB H 0.5396 0.5316 0.3339 0.231 Uiso 0.70 1 calc PR C 1
H8SC H 0.5975 0.5660 0.2963 0.231 Uiso 0.70 1 calc PR C 1
N4SA N 0.2998(12) 0.5657(6) 0.2411(6) 0.110(5) Uiso 0.30 1 d PD D 2
C7SA C 0.3803(12) 0.5678(5) 0.2687(6) 0.086(5) Uiso 0.30 1 d PD D 2
C8SA C 0.4698(12) 0.5480(7) 0.2938(6) 0.076(4) Uiso 0.30 1 d PD D 2
H8SD H 0.5174 0.5799 0.3191 0.114 Uiso 0.30 1 calc PR D 2
H8SE H 0.5144 0.5309 0.2680 0.114 Uiso 0.30 1 calc PR D 2
H8SF H 0.4389 0.5196 0.3116 0.114 Uiso 0.30 1 calc PR D 2
N5S N 0.9080(3) 0.84529(19) 0.40486(14) 0.0839(12) Uani 1 1 d . . .
C9S C 0.8576(3) 0.84942(15) 0.43878(13) 0.0472(8) Uani 1 1 d . . .
C10S C 0.7944(3) 0.85394(14) 0.48175(12) 0.0403(7) Uani 1 1 d . . .
H10I H 0.7262 0.8251 0.4725 0.048 Uiso 1 1 calc R . .
H10J H 0.7740 0.8917 0.4903 0.048 Uiso 1 1 calc R . .
H10K H 0.8399 0.8481 0.5117 0.048 Uiso 1 1 calc R . .
N6S N 0.4842(4) 0.14853(18) 0.14791(14) 0.0811(11) Uani 1 1 d . . .
C11S C 0.3956(4) 0.16055(17) 0.15229(13) 0.0583(10) Uani 1 1 d . . .
C12S C 0.2865(3) 0.17443(17) 0.15834(15) 0.0614(10) Uani 1 1 d . . .
H12N H 0.2941 0.2122 0.1815 0.074 Uiso 1 1 calc R . .
H12P H 0.2435 0.1465 0.1732 0.074 Uiso 1 1 calc R . .
H12O H 0.2473 0.1741 0.1245 0.074 Uiso 1 1 calc R . .
N7S N 0.7039(5) 0.5882(4) 0.8894(3) 0.084(3) Uiso 0.50 1 d PD E 5
C13S C 0.6250(3) 0.56308(19) 0.86123(16) 0.0739(12) Uiso 0.50 1 d PD E 5
C14S C 0.5065(4) 0.5485(4) 0.8443(4) 0.087(3) Uiso 0.50 1 d PD E 5
H14N H 0.4660 0.5572 0.8743 0.130 Uiso 0.50 1 calc PR E 5
H14O H 0.4867 0.5080 0.8276 0.130 Uiso 0.50 1 calc PR E 5
H14P H 0.4858 0.5705 0.8196 0.130 Uiso 0.50 1 calc PR E 5
N7SB N 0.7192(4) 0.5658(4) 0.8763(3) 0.080(2) Uiso 0.50 1 d PD F 6
C13B C 0.6250(3) 0.56308(19) 0.86123(16) 0.0739(12) Uiso 0.50 1 d PD F 6
C14B C 0.5280(6) 0.5441(4) 0.8227(3) 0.079(3) Uiso 0.50 1 d PD F 6
H14Q H 0.5517 0.5327 0.7885 0.119 Uiso 0.50 1 calc PR F 6
H14R H 0.4852 0.5749 0.8233 0.119 Uiso 0.50 1 calc PR F 6
H14S H 0.4810 0.5116 0.8301 0.119 Uiso 0.50 1 calc PR F 6
N8S N 0.4934(3) 0.56070(17) 0.63170(16) 0.0794(11) Uani 1 1 d . . .
C15S C 0.4835(3) 0.59861(16) 0.61514(15) 0.0501(8) Uani 1 1 d . . .
C16S C 0.4710(3) 0.64700(14) 0.59461(13) 0.0461(8) Uani 1 1 d . . .
H16A H 0.4997 0.6425 0.5612 0.055 Uiso 1 1 calc R . .
H16B H 0.5131 0.6814 0.6188 0.055 Uiso 1 1 calc R . .
H16C H 0.3915 0.6501 0.5898 0.055 Uiso 1 1 calc R . .
H1O H 0.403(3) 0.7995(15) 0.5627(13) 0.052(10) Uiso 1 1 d . . .
H3O H 0.330(3) 0.7879(14) 0.6664(12) 0.041(10) Uiso 1 1 d . . .
H21O H 0.876(3) 0.7304(14) 0.0575(13) 0.045(10) Uiso 1 1 d . . .
H23O H 1.012(3) 0.8028(14) 0.1625(12) 0.045(9) Uiso 1 1 d . . .
H1N H 0.461(3) 0.8882(15) 0.6277(13) 0.051(10) Uiso 1 1 d . . .
H2N H 0.160(3) 0.8163(13) 0.6261(12) 0.038(9) Uiso 1 1 d . . .
H21N H 0.855(3) 0.8247(14) 0.0488(12) 0.042(9) Uiso 1 1 d . . .
H22N H 1.167(3) 0.7915(15) 0.1099(14) 0.055(10) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O6 1.4282(19) . yes
S1 O5 1.446(2) . yes
S1 N1 1.637(2) . yes
S1 C47 1.770(3) . yes
S2 O7 1.4343(19) . yes
S2 O8 1.4352(19) . yes
S2 N2 1.611(2) . yes
S2 C61 1.779(2) . yes
O1 C3 1.370(3) . yes
O1 H1O 0.85(4) . ?
O2 C14 1.398(3) . yes
O2 C59 1.446(3) . yes
O3 C25 1.383(3) . yes
O3 H3O 0.79(3) . ?
O4 C36 1.400(3) . yes
O4 C45 1.447(3) . yes
N1 C46 1.461(3) . yes
N1 H1N 0.89(4) . ?
N2 C60 1.463(3) . yes
N2 H2N 0.91(3) . ?
N3 C51 1.407(4) . yes
N3 C58 1.444(4) . yes
N3 C57 1.464(4) . yes
N4 C65 1.423(3) . yes
N4 C72 1.463(3) . yes
N4 C71 1.471(4) . yes
C1 C37 1.514(3) . yes
C1 C2 1.519(3) . yes
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.396(3) . yes
C2 C3 1.401(3) . yes
C3 C4 1.400(3) . yes
C4 C5 1.391(4) . yes
C4 C12 1.524(4) . yes
C5 C6 1.388(4) . yes
C5 H5 0.9500 . ?
C6 C7 1.394(4) . yes
C6 C8 1.534(4) . yes
C7 H7 0.9500 . ?
C8 C10 1.516(4) . yes
C8 C11 1.529(4) . yes
C8 C9 1.535(5) . yes
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10G 0.9800 . ?
C10 H10F 0.9800 . ?
C10 H10H 0.9800 . ?
C11 H11I 0.9800 . ?
C11 H11J 0.9800 . ?
C11 H11K 0.9800 . ?
C12 C13 1.520(3) . yes
C12 H12G 0.9900 . ?
C12 H12H 0.9900 . ?
C13 C14 1.390(3) . yes
C13 C18 1.394(3) . yes
C14 C15 1.396(3) . yes
C15 C16 1.399(3) . yes
C15 C23 1.521(3) . yes
C16 C17 1.391(4) . yes
C16 H16D 0.9500 . ?
C17 C18 1.387(4) . yes
C17 C19 1.535(3) . yes
C18 H18 0.9500 . ?
C19 C22A 1.455(7) . yes
C19 C20B 1.501(7) . yes
C19 C21A 1.549(7) . yes
C19 C21B 1.550(7) . yes
C19 C20A 1.562(7) . yes
C19 C22B 1.594(7) . yes
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21F 0.9800 . ?
C21A H21E 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22A 0.9800 . ?
C22A H22C 0.9800 . ?
C20B H20A 0.9800 . ?
C20B H20B 0.9800 . ?
C20B H20C 0.9800 . ?
C21B H21C 0.9800 . ?
C21B H21A 0.9800 . ?
C21B H21B 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C24 1.521(3) . yes
C23 H23B 0.9900 . ?
C23 H23A 0.9900 . ?
C24 C29 1.387(3) . yes
C24 C25 1.405(3) . yes
C25 C26 1.391(3) . yes
C26 C27 1.401(3) . yes
C26 C34 1.523(3) . yes
C27 C28 1.390(4) . yes
C27 H27B 0.9500 . ?
C28 C29 1.393(4) . yes
C28 C30 1.531(4) . yes
C29 H29 0.9500 . ?
C30 C32 1.530(4) . yes
C30 C31 1.534(4) . yes
C30 C33 1.538(4) . yes
C31 H31B 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.521(3) . yes
C34 H34B 0.9900 . ?
C34 H34A 0.9900 . ?
C35 C36 1.392(3) . yes
C35 C40 1.395(4) . yes
C36 C37 1.396(3) . yes
C37 C38 1.397(3) . yes
C38 C39 1.389(4) . yes
C38 H38B 0.9500 . ?
C39 C40 1.393(4) . yes
C39 C41 1.535(4) . yes
C40 H40B 0.9500 . ?
C41 C44 1.519(5) . yes
C41 C43 1.527(5) . yes
C41 C42 1.537(5) . yes
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.507(4) . yes
C45 H45B 0.9900 . ?
C45 H45A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 H46A 0.9900 . ?
C47 C48 1.364(4) . yes
C47 C55 1.432(4) . yes
C48 C49 1.402(4) . yes
C48 H48B 0.9500 . ?
C49 C50 1.368(4) . yes
C49 H49 0.9500 . ?
C50 C56 1.422(4) . yes
C50 H50B 0.9500 . ?
C51 C52 1.382(4) . yes
C51 C56 1.436(4) . yes
C52 C53 1.405(4) . yes
C52 H52B 0.9500 . ?
C53 C54 1.370(4) . yes
C53 H53B 0.9500 . ?
C54 C55 1.438(4) . yes
C54 H54 0.9500 . ?
C55 C56 1.411(4) . yes
C57 H57C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.506(3) . yes
C59 H59B 0.9900 . ?
C59 H59A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 H60A 0.9900 . ?
C61 C62 1.371(4) . yes
C61 C69 1.426(3) . yes
C62 C63 1.402(4) . yes
C62 H62 0.9500 . ?
C63 C64 1.363(4) . yes
C63 H63B 0.9500 . ?
C64 C70 1.414(3) . yes
C64 H64 0.9500 . ?
C65 C66 1.377(4) . yes
C65 C70 1.436(4) . yes
C66 C67 1.408(4) . yes
C66 H66B 0.9500 . ?
C67 C68 1.362(4) . yes
C67 H67 0.9500 . ?
C68 C69 1.428(3) . yes
C68 H68 0.9500 . ?
C69 C70 1.429(3) . yes
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72C 0.9800 . ?
S21 O26 1.4315(19) . yes
S21 O25 1.436(2) . yes
S21 N21 1.605(2) . yes
S21 C147 1.772(3) . yes
S22 O27 1.424(2) . yes
S22 O28 1.432(2) . yes
S22 N22 1.609(2) . yes
S22 C161 1.785(3) . yes
O21 C103 1.379(3) . yes
O21 H21O 0.81(3) . ?
O22 C114 1.405(3) . yes
O22 C145 1.444(3) . yes
O23 C125 1.380(3) . yes
O23 H23O 0.89(3) . ?
O24 C136 1.407(3) . yes
O24 C159 1.437(3) . yes
N21 C146 1.455(3) . yes
N21 H21N 0.87(3) . ?
N22 C160 1.455(3) . yes
N22 H22N 0.90(4) . ?
N23 C151 1.414(3) . yes
N23 C157 1.455(4) . yes
N23 C158 1.476(4) . yes
N24 C165 1.423(4) . yes
N24 C172 1.455(4) . yes
N24 C171 1.475(4) . yes
C101 C137 1.519(3) . yes
C101 C102 1.527(3) . yes
C101 H10D 0.9900 . ?
C101 H10E 0.9900 . ?
C102 C107 1.391(3) . yes
C102 C103 1.398(3) . yes
C103 C104 1.401(3) . yes
C104 C105 1.385(3) . yes
C104 C112 1.518(3) . yes
C105 C106 1.404(3) . yes
C105 H105 0.9500 . ?
C106 C107 1.392(4) . yes
C106 C108 1.534(4) . yes
C107 H107 0.9500 . ?
C108 C109 1.525(4) . yes
C108 C110 1.537(4) . yes
C108 C111 1.537(4) . yes
C109 H10B 0.9800 . ?
C109 H10A 0.9800 . ?
C109 H10C 0.9800 . ?
C110 H11A 0.9800 . ?
C110 H11B 0.9800 . ?
C110 H11C 0.9800 . ?
C111 H11E 0.9800 . ?
C111 H11D 0.9800 . ?
C111 H11F 0.9800 . ?
C112 C113 1.515(3) . yes
C112 H11H 0.9900 . ?
C112 H11G 0.9900 . ?
C113 C114 1.386(3) . yes
C113 C118 1.404(3) . yes
C114 C115 1.397(3) . yes
C115 C116 1.390(4) . yes
C115 C123 1.524(4) . yes
C116 C117 1.395(4) . yes
C116 H116 0.9500 . ?
C117 C118 1.389(4) . yes
C117 C119 1.536(4) . yes
C118 H118 0.9500 . ?
C119 C222 1.37(3) . yes
C119 C120 1.504(6) . yes
C119 C121 1.539(5) . yes
C119 C122 1.556(6) . yes
C119 C220 1.59(2) . yes
C119 C221 1.66(3) . yes
C120 H12A 0.9800 . ?
C120 H12B 0.9800 . ?
C120 H12C 0.9800 . ?
C121 H12J 0.9800 . ?
C121 H12I 0.9800 . ?
C121 H12K 0.9800 . ?
C122 H12E 0.9800 . ?
C122 H12D 0.9800 . ?
C122 H12F 0.9800 . ?
C220 H22G 0.9800 . ?
C220 H22H 0.9800 . ?
C220 H22I 0.9800 . ?
C221 H22J 0.9800 . ?
C221 H22K 0.9800 . ?
C221 H22L 0.9800 . ?
C222 H22M 0.9800 . ?
C222 H22O 0.9800 . ?
C222 H22P 0.9800 . ?
C123 C124 1.520(3) . yes
C123 H12L 0.9900 . ?
C123 H12M 0.9900 . ?
C124 C129 1.388(4) . yes
C124 C125 1.402(3) . yes
C125 C126 1.392(3) . yes
C126 C127 1.391(4) . yes
C126 C134 1.521(3) . yes
C127 C128 1.393(4) . yes
C127 H127 0.9500 . ?
C128 C129 1.401(4) . yes
C128 C130 1.534(4) . yes
C129 H129 0.9500 . ?
C130 C133 1.507(5) . yes
C130 C132 1.512(4) . yes
C130 C131 1.560(5) . yes
C131 H13A 0.9800 . ?
C131 H13B 0.9800 . ?
C131 H13C 0.9800 . ?
C132 H13J 0.9800 . ?
C132 H13I 0.9800 . ?
C132 H13K 0.9800 . ?
C133 H13E 0.9800 . ?
C133 H13D 0.9800 . ?
C133 H13F 0.9800 . ?
C134 C135 1.520(3) . yes
C134 H13G 0.9900 . ?
C134 H13H 0.9900 . ?
C135 C136 1.391(3) . yes
C135 C140 1.397(3) . yes
C136 C137 1.398(3) . yes
C137 C138 1.391(3) . yes
C138 C139 1.396(4) . yes
C138 H138 0.9500 . ?
C139 C140 1.393(4) . yes
C139 C141 1.532(4) . yes
C140 H140 0.9500 . ?
C141 C142 1.509(4) . yes
C141 C144 1.509(5) . yes
C141 C143 1.560(5) . yes
C142 H14D 0.9800 . ?
C142 H14E 0.9800 . ?
C142 H14F 0.9800 . ?
C143 H14B 0.9800 . ?
C143 H14A 0.9800 . ?
C143 H14C 0.9800 . ?
C144 H14H 0.9800 . ?
C144 H14G 0.9800 . ?
C144 H14I 0.9800 . ?
C145 C146 1.507(4) . yes
C145 H14J 0.9900 . ?
C145 H14K 0.9900 . ?
C146 H14L 0.9900 . ?
C146 H14M 0.9900 . ?
C147 C148 1.371(4) . yes
C147 C155 1.438(4) . yes
C148 C149 1.404(4) . yes
C148 H148 0.9500 . ?
C149 C150 1.358(4) . yes
C149 H149 0.9500 . ?
C150 C156 1.422(4) . yes
C150 H150 0.9500 . ?
C151 C152 1.370(4) . yes
C151 C156 1.434(4) . yes
C152 C153 1.410(4) . yes
C152 H152 0.9500 . ?
C153 C154 1.366(4) . yes
C153 H153 0.9500 . ?
C154 C155 1.422(4) . yes
C154 H154 0.9500 . ?
C155 C156 1.430(4) . yes
C157 H15D 0.9800 . ?
C157 H15E 0.9800 . ?
C157 H15F 0.9800 . ?
C158 H15H 0.9800 . ?
C158 H15G 0.9800 . ?
C158 H15I 0.9800 . ?
C159 C160 1.508(3) . yes
C159 H15B 0.9900 . ?
C159 H15A 0.9900 . ?
C160 H16F 0.9900 . ?
C160 H16E 0.9900 . ?
C161 C162 1.357(4) . yes
C161 C169 1.423(4) . yes
C162 C163 1.418(4) . yes
C162 H162 0.9500 . ?
C163 C164 1.347(4) . yes
C163 H163 0.9500 . ?
C164 C170 1.429(4) . yes
C164 H164 0.9500 . ?
C165 C166 1.368(4) . yes
C165 C170 1.437(4) . yes
C166 C167 1.413(5) . yes
C166 H166 0.9500 . ?
C167 C168 1.359(4) . yes
C167 H167 0.9500 . ?
C168 C169 1.442(4) . yes
C168 H168 0.9500 . ?
C169 C170 1.420(4) . yes
C171 H17B 0.9800 . ?
C171 H17A 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
N1S C1S 1.141(3) . yes
C1S C2S 1.416(4) . yes
C2S H2SB 0.9800 . ?
C2S H2SA 0.9800 . ?
C2S H2SC 0.9800 . ?
N2S C3S 1.148(6) . yes
C3S C4S 1.453(6) . yes
C4S H4SC 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SA 0.9800 . ?
N3S C5S 1.136(4) . yes
C5S C6S 1.439(4) . yes
C6S H6SA 0.9800 . ?
C6S H6SC 0.9800 . ?
C6S H6SB 0.9800 . ?
N4S C7S 1.146(3) . yes
C7S C8S 1.415(4) . yes
C8S H8SA 0.9800 . ?
C8S H8SB 0.9800 . ?
C8S H8SC 0.9800 . ?
N4SA C7SA 1.156(4) . yes
C7SA C8SA 1.428(4) . yes
C8SA H8SD 0.9800 . ?
C8SA H8SE 0.9800 . ?
C8SA H8SF 0.9800 . ?
N5S C9S 1.139(4) . yes
C9S C10S 1.437(5) . yes
C10S H10I 0.9800 . ?
C10S H10J 0.9800 . ?
C10S H10K 0.9800 . ?
N6S C11S 1.171(5) . yes
C11S C12S 1.435(6) . yes
C12S H12N 0.9800 . ?
C12S H12P 0.9800 . ?
C12S H12O 0.9800 . ?
N7S C13S 1.161(4) . yes
C13S C14S 1.437(4) . yes
C14S H14N 0.9800 . ?
C14S H14O 0.9800 . ?
C14S H14P 0.9800 . ?
C14B H14Q 0.9800 . ?
C14B H14R 0.9800 . ?
C14B H14S 0.9800 . ?
N8S C15S 1.135(5) . yes
C15S C16S 1.439(5) . yes
C16S H16A 0.9800 . ?
C16S H16B 0.9800 . ?
C16S H16C 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
O6 S1 O5 116.28(12) . . yes
O6 S1 N1 107.63(12) . . yes
O5 S1 N1 111.59(12) . . yes
O6 S1 C47 113.57(12) . . yes
O5 S1 C47 108.00(12) . . yes
N1 S1 C47 98.37(12) . . yes
O7 S2 O8 119.06(11) . . yes
O7 S2 N2 106.57(11) . . yes
O8 S2 N2 107.30(12) . . yes
O7 S2 C61 109.51(11) . . yes
O8 S2 C61 106.83(12) . . yes
N2 S2 C61 106.99(11) . . yes
C3 O1 H1O 113(2) . . ?
C14 O2 C59 116.10(17) . . yes
C25 O3 H3O 113(2) . . ?
C36 O4 C45 113.80(18) . . yes
C46 N1 S1 118.18(18) . . yes
C46 N1 H1N 116(2) . . ?
S1 N1 H1N 102(2) . . ?
C60 N2 S2 121.67(18) . . yes
C60 N2 H2N 119(2) . . ?
S2 N2 H2N 111.8(19) . . ?
C51 N3 C58 116.6(2) . . yes
C51 N3 C57 116.0(2) . . yes
C58 N3 C57 111.1(2) . . yes
C65 N4 C72 115.3(2) . . yes
C65 N4 C71 113.1(2) . . yes
C72 N4 C71 110.2(2) . . yes
C37 C1 C2 110.68(19) . . yes
C37 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C37 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C7 C2 C3 118.3(2) . . yes
C7 C2 C1 120.0(2) . . yes
C3 C2 C1 121.5(2) . . yes
O1 C3 C4 122.2(2) . . yes
O1 C3 C2 117.3(2) . . yes
C4 C3 C2 120.6(2) . . yes
C5 C4 C3 118.9(2) . . yes
C5 C4 C12 119.6(2) . . yes
C3 C4 C12 121.4(2) . . yes
C6 C5 C4 122.2(2) . . yes
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C7 117.5(2) . . yes
C5 C6 C8 122.8(2) . . yes
C7 C6 C8 119.7(2) . . yes
C6 C7 C2 122.4(2) . . yes
C6 C7 H7 118.8 . . ?
C2 C7 H7 118.8 . . ?
C10 C8 C11 109.8(3) . . yes
C10 C8 C6 112.6(3) . . yes
C11 C8 C6 110.2(2) . . yes
C10 C8 C9 108.4(3) . . yes
C11 C8 C9 107.4(3) . . yes
C6 C8 C9 108.3(2) . . yes
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10G 109.5 . . ?
C8 C10 H10F 109.5 . . ?
H10G C10 H10F 109.5 . . ?
C8 C10 H10H 109.5 . . ?
H10G C10 H10H 109.5 . . ?
H10F C10 H10H 109.5 . . ?
C8 C11 H11I 109.5 . . ?
C8 C11 H11J 109.5 . . ?
H11I C11 H11J 109.5 . . ?
C8 C11 H11K 109.5 . . ?
H11I C11 H11K 109.5 . . ?
H11J C11 H11K 109.5 . . ?
C13 C12 C4 110.4(2) . . yes
C13 C12 H12G 109.6 . . ?
C4 C12 H12G 109.6 . . ?
C13 C12 H12H 109.6 . . ?
C4 C12 H12H 109.6 . . ?
H12G C12 H12H 108.1 . . ?
C14 C13 C18 118.2(2) . . yes
C14 C13 C12 122.0(2) . . yes
C18 C13 C12 119.7(2) . . yes
C13 C14 C15 121.8(2) . . yes
C13 C14 O2 118.6(2) . . yes
C15 C14 O2 119.4(2) . . yes
C14 C15 C16 117.4(2) . . yes
C14 C15 C23 123.1(2) . . yes
C16 C15 C23 119.3(2) . . yes
C17 C16 C15 122.7(2) . . yes
C17 C16 H16D 118.6 . . ?
C15 C16 H16D 118.6 . . ?
C18 C17 C16 117.3(2) . . yes
C18 C17 C19 121.3(2) . . yes
C16 C17 C19 121.3(2) . . yes
C17 C18 C13 122.5(2) . . yes
C17 C18 H18 118.7 . . ?
C13 C18 H18 118.7 . . ?
C22A C19 C20B 124.6(4) . . yes
C22A C19 C17 112.0(3) . . yes
C20B C19 C17 110.8(3) . . yes
C22A C19 C21A 109.2(4) . . yes
C20B C19 C21A 85.2(4) . . yes
C17 C19 C21A 111.8(3) . . yes
C22A C19 C21B 86.7(4) . . yes
C20B C19 C21B 109.3(4) . . yes
C17 C19 C21B 110.4(3) . . yes
C21A C19 C21B 26.1(3) . . yes
C22A C19 C20A 111.4(4) . . yes
C20B C19 C20A 22.6(3) . . yes
C17 C19 C20A 105.0(3) . . yes
C21A C19 C20A 107.4(4) . . yes
C21B C19 C20A 130.1(4) . . yes
C22A C19 C22B 20.9(3) . . yes
C20B C19 C22B 108.4(4) . . yes
C17 C19 C22B 112.4(3) . . yes
C21A C19 C22B 124.4(4) . . yes
C21B C19 C22B 105.5(4) . . yes
C20A C19 C22B 91.8(4) . . yes
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21F 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C22A H22B 109.5 . . ?
C19 C22A H22A 109.5 . . ?
C19 C22A H22C 109.5 . . ?
C19 C20B H20A 109.5 . . ?
C19 C20B H20B 109.5 . . ?
H20A C20B H20B 109.5 . . ?
C19 C20B H20C 109.5 . . ?
H20A C20B H20C 109.5 . . ?
H20B C20B H20C 109.5 . . ?
C19 C21B H21C 109.5 . . ?
C19 C21B H21A 109.5 . . ?
H21C C21B H21A 109.5 . . ?
C19 C21B H21B 109.5 . . ?
H21C C21B H21B 109.5 . . ?
H21A C21B H21B 109.5 . . ?
C19 C22B H22E 109.5 . . ?
C19 C22B H22D 109.5 . . ?
H22E C22B H22D 109.5 . . ?
C19 C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
C24 C23 C15 111.1(2) . . yes
C24 C23 H23B 109.4 . . ?
C15 C23 H23B 109.4 . . ?
C24 C23 H23A 109.4 . . ?
C15 C23 H23A 109.4 . . ?
H23B C23 H23A 108.0 . . ?
C29 C24 C25 118.0(2) . . yes
C29 C24 C23 119.7(2) . . yes
C25 C24 C23 122.2(2) . . yes
O3 C25 C26 122.0(2) . . yes
O3 C25 C24 117.0(2) . . yes
C26 C25 C24 121.0(2) . . yes
C25 C26 C27 118.5(2) . . yes
C25 C26 C34 123.0(2) . . yes
C27 C26 C34 118.5(2) . . yes
C28 C27 C26 122.2(2) . . yes
C28 C27 H27B 118.9 . . ?
C26 C27 H27B 118.9 . . ?
C27 C28 C29 117.1(2) . . yes
C27 C28 C30 123.1(2) . . yes
C29 C28 C30 119.8(2) . . yes
C24 C29 C28 123.1(2) . . yes
C24 C29 H29 118.5 . . ?
C28 C29 H29 118.5 . . ?
C32 C30 C28 111.8(2) . . yes
C32 C30 C31 108.1(3) . . yes
C28 C30 C31 110.1(2) . . yes
C32 C30 C33 108.5(3) . . yes
C28 C30 C33 108.8(2) . . yes
C31 C30 C33 109.6(2) . . yes
C30 C31 H31B 109.5 . . ?
C30 C31 H31A 109.5 . . ?
H31B C31 H31A 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C26 111.8(2) . . yes
C35 C34 H34B 109.3 . . ?
C26 C34 H34B 109.3 . . ?
C35 C34 H34A 109.3 . . ?
C26 C34 H34A 109.3 . . ?
H34B C34 H34A 107.9 . . ?
C36 C35 C40 118.3(2) . . yes
C36 C35 C34 121.4(2) . . yes
C40 C35 C34 120.2(2) . . yes
C35 C36 C37 121.8(2) . . yes
C35 C36 O4 118.1(2) . . yes
C37 C36 O4 119.9(2) . . yes
C36 C37 C38 117.3(2) . . yes
C36 C37 C1 123.4(2) . . yes
C38 C37 C1 119.1(2) . . yes
C39 C38 C37 122.7(2) . . yes
C39 C38 H38B 118.6 . . ?
C37 C38 H38B 118.6 . . ?
C38 C39 C40 117.6(2) . . yes
C38 C39 C41 119.3(3) . . yes
C40 C39 C41 123.0(3) . . yes
C39 C40 C35 121.9(2) . . yes
C39 C40 H40B 119.1 . . ?
C35 C40 H40B 119.1 . . ?
C44 C41 C43 109.0(3) . . yes
C44 C41 C39 112.3(3) . . yes
C43 C41 C39 109.6(2) . . yes
C44 C41 C42 109.5(3) . . yes
C43 C41 C42 108.1(3) . . yes
C39 C41 C42 108.1(3) . . yes
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43A 109.5 . . ?
H43B C43 H43A 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O4 C45 C46 106.2(2) . . yes
O4 C45 H45B 110.5 . . ?
C46 C45 H45B 110.5 . . ?
O4 C45 H45A 110.5 . . ?
C46 C45 H45A 110.5 . . ?
H45B C45 H45A 108.7 . . ?
N1 C46 C45 112.8(2) . . yes
N1 C46 H46B 109.0 . . ?
C45 C46 H46B 109.0 . . ?
N1 C46 H46A 109.0 . . ?
C45 C46 H46A 109.0 . . ?
H46B C46 H46A 107.8 . . ?
C48 C47 C55 121.7(2) . . yes
C48 C47 S1 116.2(2) . . yes
C55 C47 S1 122.0(2) . . yes
C47 C48 C49 119.8(3) . . yes
C47 C48 H48B 120.1 . . ?
C49 C48 H48B 120.1 . . ?
C50 C49 C48 120.3(3) . . yes
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C56 121.2(3) . . yes
C49 C50 H50B 119.4 . . ?
C56 C50 H50B 119.4 . . ?
C52 C51 N3 122.7(3) . . yes
C52 C51 C56 118.1(3) . . yes
N3 C51 C56 119.1(3) . . yes
C51 C52 C53 121.1(3) . . yes
C51 C52 H52B 119.5 . . ?
C53 C52 H52B 119.5 . . ?
C54 C53 C52 122.0(3) . . yes
C54 C53 H53B 119.0 . . ?
C52 C53 H53B 119.0 . . ?
C53 C54 C55 118.8(3) . . yes
C53 C54 H54 120.6 . . ?
C55 C54 H54 120.6 . . ?
C56 C55 C47 117.9(2) . . yes
C56 C55 C54 119.1(2) . . yes
C47 C55 C54 122.9(2) . . yes
C55 C56 C50 118.9(2) . . yes
C55 C56 C51 120.7(3) . . yes
C50 C56 C51 120.3(2) . . yes
N3 C57 H57C 109.5 . . ?
N3 C57 H57A 109.5 . . ?
H57C C57 H57A 109.5 . . ?
N3 C57 H57B 109.5 . . ?
H57C C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
N3 C58 H58A 109.5 . . ?
N3 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
N3 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O2 C59 C60 105.98(19) . . yes
O2 C59 H59B 110.5 . . ?
C60 C59 H59B 110.5 . . ?
O2 C59 H59A 110.5 . . ?
C60 C59 H59A 110.5 . . ?
H59B C59 H59A 108.7 . . ?
N2 C60 C59 108.9(2) . . yes
N2 C60 H60B 109.9 . . ?
C59 C60 H60B 109.9 . . ?
N2 C60 H60A 109.9 . . ?
C59 C60 H60A 109.9 . . ?
H60B C60 H60A 108.3 . . ?
C62 C61 C69 121.9(2) . . yes
C62 C61 S2 115.89(19) . . yes
C69 C61 S2 122.15(19) . . yes
C61 C62 C63 120.0(2) . . yes
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C64 C63 C62 120.2(2) . . yes
C64 C63 H63B 119.9 . . ?
C62 C63 H63B 119.9 . . ?
C63 C64 C70 121.3(2) . . yes
C63 C64 H64 119.4 . . ?
C70 C64 H64 119.4 . . ?
C66 C65 N4 123.3(2) . . yes
C66 C65 C70 119.6(2) . . yes
N4 C65 C70 117.1(2) . . yes
C65 C66 C67 120.1(2) . . yes
C65 C66 H66B 120.0 . . ?
C67 C66 H66B 120.0 . . ?
C68 C67 C66 122.0(2) . . yes
C68 C67 H67 119.0 . . ?
C66 C67 H67 119.0 . . ?
C67 C68 C69 120.0(2) . . yes
C67 C68 H68 120.0 . . ?
C69 C68 H68 120.0 . . ?
C61 C69 C68 124.3(2) . . yes
C61 C69 C70 117.1(2) . . yes
C68 C69 C70 118.6(2) . . yes
C64 C70 C69 119.4(2) . . yes
C64 C70 C65 121.0(2) . . yes
C69 C70 C65 119.5(2) . . yes
N4 C71 H71A 109.5 . . ?
N4 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
N4 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
N4 C72 H72B 109.5 . . ?
N4 C72 H72A 109.5 . . ?
H72B C72 H72A 109.5 . . ?
N4 C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
O26 S21 O25 119.30(12) . . yes
O26 S21 N21 107.24(12) . . yes
O25 S21 N21 106.24(12) . . yes
O26 S21 C147 107.33(12) . . yes
O25 S21 C147 108.33(12) . . yes
N21 S21 C147 107.95(12) . . yes
O27 S22 O28 118.64(12) . . yes
O27 S22 N22 107.38(13) . . yes
O28 S22 N22 106.98(12) . . yes
O27 S22 C161 109.76(12) . . yes
O28 S22 C161 106.76(12) . . yes
N22 S22 C161 106.72(13) . . yes
C103 O21 H21O 111(2) . . ?
C114 O22 C145 114.89(18) . . yes
C125 O23 H23O 110(2) . . ?
C136 O24 C159 114.73(18) . . yes
C146 N21 S21 123.03(18) . . yes
C146 N21 H21N 119(2) . . ?
S21 N21 H21N 113(2) . . ?
C160 N22 S22 122.64(18) . . yes
C160 N22 H22N 115(2) . . ?
S22 N22 H22N 112(2) . . ?
C151 N23 C157 115.8(2) . . yes
C151 N23 C158 114.0(2) . . yes
C157 N23 C158 110.1(2) . . yes
C165 N24 C172 115.7(3) . . yes
C165 N24 C171 113.6(2) . . yes
C172 N24 C171 108.2(2) . . yes
C137 C101 C102 112.3(2) . . yes
C137 C101 H10D 109.1 . . ?
C102 C101 H10D 109.1 . . ?
C137 C101 H10E 109.1 . . ?
C102 C101 H10E 109.1 . . ?
H10D C101 H10E 107.9 . . ?
C107 C102 C103 118.6(2) . . yes
C107 C102 C101 120.0(2) . . yes
C103 C102 C101 121.4(2) . . yes
O21 C103 C102 121.1(2) . . yes
O21 C103 C104 117.8(2) . . yes
C102 C103 C104 121.1(2) . . yes
C105 C104 C103 118.1(2) . . yes
C105 C104 C112 119.8(2) . . yes
C103 C104 C112 122.1(2) . . yes
C104 C105 C106 122.9(2) . . yes
C104 C105 H105 118.6 . . ?
C106 C105 H105 118.6 . . ?
C107 C106 C105 117.0(2) . . yes
C107 C106 C108 123.7(2) . . yes
C105 C106 C108 119.3(2) . . yes
C102 C107 C106 122.3(2) . . yes
C102 C107 H107 118.8 . . ?
C106 C107 H107 118.8 . . ?
C109 C108 C106 112.3(2) . . yes
C109 C108 C110 108.7(3) . . yes
C106 C108 C110 109.3(2) . . yes
C109 C108 C111 108.1(2) . . yes
C106 C108 C111 109.6(2) . . yes
C110 C108 C111 108.8(2) . . yes
C108 C109 H10B 109.5 . . ?
C108 C109 H10A 109.5 . . ?
H10B C109 H10A 109.5 . . ?
C108 C109 H10C 109.5 . . ?
H10B C109 H10C 109.5 . . ?
H10A C109 H10C 109.5 . . ?
C108 C110 H11A 109.5 . . ?
C108 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C108 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
C108 C111 H11E 109.5 . . ?
C108 C111 H11D 109.5 . . ?
H11E C111 H11D 109.5 . . ?
C108 C111 H11F 109.5 . . ?
H11E C111 H11F 109.5 . . ?
H11D C111 H11F 109.5 . . ?
C113 C112 C104 110.7(2) . . yes
C113 C112 H11H 109.5 . . ?
C104 C112 H11H 109.5 . . ?
C113 C112 H11G 109.5 . . ?
C104 C112 H11G 109.5 . . ?
H11H C112 H11G 108.1 . . ?
C114 C113 C118 117.5(2) . . yes
C114 C113 C112 123.4(2) . . yes
C118 C113 C112 119.0(2) . . yes
C113 C114 C115 122.1(2) . . yes
C113 C114 O22 119.4(2) . . yes
C115 C114 O22 118.5(2) . . yes
C116 C115 C114 118.0(2) . . yes
C116 C115 C123 119.9(2) . . yes
C114 C115 C123 122.0(2) . . yes
C115 C116 C117 122.5(2) . . yes
C115 C116 H116 118.8 . . ?
C117 C116 H116 118.8 . . ?
C118 C117 C116 117.2(2) . . yes
C118 C117 C119 122.2(3) . . yes
C116 C117 C119 120.6(3) . . yes
C117 C118 C113 122.7(2) . . yes
C117 C118 H118 118.7 . . ?
C113 C118 H118 118.7 . . ?
C222 C119 C120 123.4(16) . . yes
C222 C119 C117 122.7(16) . . yes
C120 C119 C117 113.2(3) . . yes
C222 C119 C121 61.8(16) . . yes
C120 C119 C121 108.9(3) . . yes
C117 C119 C121 108.2(3) . . yes
C222 C119 C122 45.6(16) . . yes
C120 C119 C122 110.5(3) . . yes
C117 C119 C122 108.4(3) . . yes
C121 C119 C122 107.4(3) . . yes
C222 C119 C220 110.8(18) . . yes
C120 C119 C220 33.9(8) . . yes
C117 C119 C220 111.3(8) . . yes
C121 C119 C220 134.7(9) . . yes
C122 C119 C220 80.1(9) . . yes
C222 C119 C221 114(2) . . yes
C120 C119 C221 48.1(11) . . yes
C117 C119 C221 109.1(11) . . yes
C121 C119 C221 65.1(11) . . yes
C122 C119 C221 142.2(11) . . yes
C220 C119 C221 81.7(13) . . yes
C119 C120 H12A 109.5 . . ?
C119 C120 H12B 109.5 . . ?
C119 C120 H12C 109.5 . . ?
C119 C121 H12J 109.5 . . ?
C119 C121 H12I 109.5 . . ?
C119 C121 H12K 109.5 . . ?
C119 C122 H12E 109.5 . . ?
C119 C122 H12D 109.5 . . ?
C119 C122 H12F 109.5 . . ?
C119 C220 H22G 109.5 . . ?
C119 C220 H22H 109.5 . . ?
H22G C220 H22H 109.5 . . ?
C119 C220 H22I 109.5 . . ?
H22G C220 H22I 109.5 . . ?
H22H C220 H22I 109.5 . . ?
C119 C221 H22J 109.5 . . ?
C119 C221 H22K 109.5 . . ?
H22J C221 H22K 109.5 . . ?
C119 C221 H22L 109.5 . . ?
H22J C221 H22L 109.5 . . ?
H22K C221 H22L 109.5 . . ?
C119 C222 H22M 109.5 . . ?
C119 C222 H22O 109.5 . . ?
H22M C222 H22O 109.5 . . ?
C119 C222 H22P 109.5 . . ?
H22M C222 H22P 109.5 . . ?
H22O C222 H22P 109.5 . . ?
C124 C123 C115 111.3(2) . . yes
C124 C123 H12L 109.4 . . ?
C115 C123 H12L 109.4 . . ?
C124 C123 H12M 109.4 . . ?
C115 C123 H12M 109.4 . . ?
H12L C123 H12M 108.0 . . ?
C129 C124 C125 118.4(2) . . yes
C129 C124 C123 119.4(2) . . yes
C125 C124 C123 122.2(2) . . yes
O23 C125 C126 118.3(2) . . yes
O23 C125 C124 120.8(2) . . yes
C126 C125 C124 120.9(2) . . yes
C127 C126 C125 118.7(2) . . yes
C127 C126 C134 119.4(2) . . yes
C125 C126 C134 121.8(2) . . yes
C126 C127 C128 122.5(2) . . yes
C126 C127 H127 118.8 . . ?
C128 C127 H127 118.8 . . ?
C127 C128 C129 117.0(2) . . yes
C127 C128 C130 122.9(2) . . yes
C129 C128 C130 120.1(2) . . yes
C124 C129 C128 122.5(2) . . yes
C124 C129 H129 118.7 . . ?
C128 C129 H129 118.7 . . ?
C133 C130 C132 110.9(3) . . yes
C133 C130 C128 113.1(3) . . yes
C132 C130 C128 111.1(2) . . yes
C133 C130 C131 106.8(3) . . yes
C132 C130 C131 106.7(3) . . yes
C128 C130 C131 107.9(2) . . yes
C130 C131 H13A 109.5 . . ?
C130 C131 H13B 109.5 . . ?
H13A C131 H13B 109.5 . . ?
C130 C131 H13C 109.5 . . ?
H13A C131 H13C 109.5 . . ?
H13B C131 H13C 109.5 . . ?
C130 C132 H13J 109.5 . . ?
C130 C132 H13I 109.5 . . ?
H13J C132 H13I 109.5 . . ?
C130 C132 H13K 109.5 . . ?
H13J C132 H13K 109.5 . . ?
H13I C132 H13K 109.5 . . ?
C130 C133 H13E 109.5 . . ?
C130 C133 H13D 109.5 . . ?
H13E C133 H13D 109.5 . . ?
C130 C133 H13F 109.5 . . ?
H13E C133 H13F 109.5 . . ?
H13D C133 H13F 109.5 . . ?
C135 C134 C126 111.6(2) . . yes
C135 C134 H13G 109.3 . . ?
C126 C134 H13G 109.3 . . ?
C135 C134 H13H 109.3 . . ?
C126 C134 H13H 109.3 . . ?
H13G C134 H13H 108.0 . . ?
C136 C135 C140 117.3(2) . . yes
C136 C135 C134 122.7(2) . . yes
C140 C135 C134 119.9(2) . . yes
C135 C136 C137 122.4(2) . . yes
C135 C136 O24 119.2(2) . . yes
C137 C136 O24 118.4(2) . . yes
C138 C137 C136 117.7(2) . . yes
C138 C137 C101 119.9(2) . . yes
C136 C137 C101 122.3(2) . . yes
C137 C138 C139 122.5(2) . . yes
C137 C138 H138 118.7 . . ?
C139 C138 H138 118.7 . . ?
C140 C139 C138 117.2(2) . . yes
C140 C139 C141 122.1(2) . . yes
C138 C139 C141 120.7(2) . . yes
C139 C140 C135 122.8(2) . . yes
C139 C140 H140 118.6 . . ?
C135 C140 H140 118.6 . . ?
C142 C141 C144 110.9(3) . . yes
C142 C141 C139 109.0(3) . . yes
C144 C141 C139 112.4(2) . . yes
C142 C141 C143 108.4(3) . . yes
C144 C141 C143 106.6(3) . . yes
C139 C141 C143 109.5(3) . . yes
C141 C142 H14D 109.5 . . ?
C141 C142 H14E 109.5 . . ?
H14D C142 H14E 109.5 . . ?
C141 C142 H14F 109.5 . . ?
H14D C142 H14F 109.5 . . ?
H14E C142 H14F 109.5 . . ?
C141 C143 H14B 109.5 . . ?
C141 C143 H14A 109.5 . . ?
H14B C143 H14A 109.5 . . ?
C141 C143 H14C 109.5 . . ?
H14B C143 H14C 109.5 . . ?
H14A C143 H14C 109.5 . . ?
C141 C144 H14H 109.5 . . ?
C141 C144 H14G 109.5 . . ?
H14H C144 H14G 109.5 . . ?
C141 C144 H14I 109.5 . . ?
H14H C144 H14I 109.5 . . ?
H14G C144 H14I 109.5 . . ?
O22 C145 C146 107.0(2) . . yes
O22 C145 H14J 110.3 . . ?
C146 C145 H14J 110.3 . . ?
O22 C145 H14K 110.3 . . ?
C146 C145 H14K 110.3 . . ?
H14J C145 H14K 108.6 . . ?
N21 C146 C145 110.4(2) . . yes
N21 C146 H14L 109.6 . . ?
C145 C146 H14L 109.6 . . ?
N21 C146 H14M 109.6 . . ?
C145 C146 H14M 109.6 . . ?
H14L C146 H14M 108.1 . . ?
C148 C147 C155 121.6(2) . . yes
C148 C147 S21 116.5(2) . . yes
C155 C147 S21 121.9(2) . . yes
C147 C148 C149 120.4(3) . . yes
C147 C148 H148 119.8 . . ?
C149 C148 H148 119.8 . . ?
C150 C149 C148 120.0(3) . . yes
C150 C149 H149 120.0 . . ?
C148 C149 H149 120.0 . . ?
C149 C150 C156 121.6(3) . . yes
C149 C150 H150 119.2 . . ?
C156 C150 H150 119.2 . . ?
C152 C151 N23 123.0(3) . . yes
C152 C151 C156 119.7(2) . . yes
N23 C151 C156 117.3(2) . . yes
C151 C152 C153 120.8(2) . . yes
C151 C152 H152 119.6 . . ?
C153 C152 H152 119.6 . . ?
C154 C153 C152 120.9(3) . . yes
C154 C153 H153 119.6 . . ?
C152 C153 H153 119.6 . . ?
C153 C154 C155 120.4(2) . . yes
C153 C154 H154 119.8 . . ?
C155 C154 H154 119.8 . . ?
C154 C155 C156 118.8(2) . . yes
C154 C155 C147 124.4(2) . . yes
C156 C155 C147 116.8(2) . . yes
C150 C156 C155 119.4(2) . . yes
C150 C156 C151 121.5(2) . . yes
C155 C156 C151 119.0(2) . . yes
N23 C157 H15D 109.5 . . ?
N23 C157 H15E 109.5 . . ?
H15D C157 H15E 109.5 . . ?
N23 C157 H15F 109.5 . . ?
H15D C157 H15F 109.5 . . ?
H15E C157 H15F 109.5 . . ?
N23 C158 H15H 109.5 . . ?
N23 C158 H15G 109.5 . . ?
H15H C158 H15G 109.5 . . ?
N23 C158 H15I 109.5 . . ?
H15H C158 H15I 109.5 . . ?
H15G C158 H15I 109.5 . . ?
O24 C159 C160 107.5(2) . . yes
O24 C159 H15B 110.2 . . ?
C160 C159 H15B 110.2 . . ?
O24 C159 H15A 110.2 . . ?
C160 C159 H15A 110.2 . . ?
H15B C159 H15A 108.5 . . ?
N22 C160 C159 109.2(2) . . yes
N22 C160 H16F 109.8 . . ?
C159 C160 H16F 109.8 . . ?
N22 C160 H16E 109.8 . . ?
C159 C160 H16E 109.8 . . ?
H16F C160 H16E 108.3 . . ?
C162 C161 C169 120.8(3) . . yes
C162 C161 S22 116.4(2) . . yes
C169 C161 S22 122.7(2) . . yes
C161 C162 C163 120.3(3) . . yes
C161 C162 H162 119.9 . . ?
C163 C162 H162 119.9 . . ?
C164 C163 C162 120.6(3) . . yes
C164 C163 H163 119.7 . . ?
C162 C163 H163 119.7 . . ?
C163 C164 C170 120.8(3) . . yes
C163 C164 H164 119.6 . . ?
C170 C164 H164 119.6 . . ?
C166 C165 N24 123.3(3) . . yes
C166 C165 C170 118.1(3) . . yes
N24 C165 C170 118.4(3) . . yes
C165 C166 C167 121.3(3) . . yes
C165 C166 H166 119.4 . . ?
C167 C166 H166 119.4 . . ?
C168 C167 C166 121.4(3) . . yes
C168 C167 H167 119.3 . . ?
C166 C167 H167 119.3 . . ?
C167 C168 C169 120.0(3) . . yes
C167 C168 H168 120.0 . . ?
C169 C168 H168 120.0 . . ?
C170 C169 C161 118.7(2) . . yes
C170 C169 C168 117.6(2) . . yes
C161 C169 C168 123.7(3) . . yes
C169 C170 C164 118.5(2) . . yes
C169 C170 C165 121.0(3) . . yes
C164 C170 C165 120.4(3) . . yes
N24 C171 H17B 109.5 . . ?
N24 C171 H17A 109.5 . . ?
H17B C171 H17A 109.5 . . ?
N24 C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
N24 C172 H17D 109.5 . . ?
N24 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
N24 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
N1S C1S C2S 178.8(4) . . yes
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SA 109.5 . . ?
H2SB C2S H2SA 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
N2S C3S C4S 178.0(5) . . yes
C3S C4S H4SC 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SC C4S H4SB 109.5 . . ?
C3S C4S H4SA 109.5 . . ?
H4SC C4S H4SA 109.5 . . ?
H4SB C4S H4SA 109.5 . . ?
N3S C5S C6S 179.2(4) . . yes
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SC C6S H6SB 109.5 . . ?
N4S C7S C8S 168.1(8) . . yes
C7S C8S H8SA 109.5 . . ?
C7S C8S H8SB 109.5 . . ?
H8SA C8S H8SB 109.5 . . ?
C7S C8S H8SC 109.5 . . ?
H8SA C8S H8SC 109.5 . . ?
H8SB C8S H8SC 109.5 . . ?
N4SA C7SA C8SA 158.3(9) . . yes
C7SA C8SA H8SD 109.5 . . ?
C7SA C8SA H8SE 109.5 . . ?
H8SD C8SA H8SE 109.5 . . ?
C7SA C8SA H8SF 109.5 . . ?
H8SD C8SA H8SF 109.5 . . ?
H8SE C8SA H8SF 109.5 . . ?
N5S C9S C10S 179.2(4) . . yes
C9S C10S H10I 109.5 . . ?
C9S C10S H10J 109.5 . . ?
H10I C10S H10J 109.5 . . ?
C9S C10S H10K 109.5 . . ?
H10I C10S H10K 109.5 . . ?
H10J C10S H10K 109.5 . . ?
N6S C11S C12S 178.8(5) . . yes
C11S C12S H12N 109.5 . . ?
C11S C12S H12P 109.5 . . ?
H12N C12S H12P 109.5 . . ?
C11S C12S H12O 109.5 . . ?
H12N C12S H12O 109.5 . . ?
H12P C12S H12O 109.5 . . ?
N7S C13S C14S 153.7(6) . . yes
C13S C14S H14N 109.5 . . ?
C13S C14S H14O 109.5 . . ?
H14N C14S H14O 109.5 . . ?
C13S C14S H14P 109.5 . . ?
H14N C14S H14P 109.5 . . ?
H14O C14S H14P 109.5 . . ?
H14Q C14B H14R 109.5 . . ?
H14Q C14B H14S 109.5 . . ?
H14R C14B H14S 109.5 . . ?
N8S C15S C16S 179.5(4) . . yes
C15S C16S H16A 109.5 . . ?
C15S C16S H16B 109.5 . . ?
H16A C16S H16B 109.5 . . ?
C15S C16S H16C 109.5 . . ?
H16A C16S H16C 109.5 . . ?
H16B C16S H16C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O2 0.85(4) 1.82(4) 2.669(2) 178(4) .
O3 H3O O4 0.79(3) 1.94(3) 2.722(3) 173(3) .
O21 H21O O24 0.81(3) 1.86(4) 2.670(3) 175(4) .
O23 H23O O22 0.89(3) 1.81(4) 2.693(2) 177(3) .
N1 H1N O1 0.89(4) 2.10(4) 2.973(3) 169(3) .
N2 H2N O3 0.91(3) 2.08(3) 2.964(3) 161(3) .
N21 H21N O21 0.87(3) 2.00(3) 2.852(3) 166(3) .
N22 H22N O23 0.90(4) 1.99(4) 2.867(3) 165(3) .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.063

# File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison.
_database_code_depnum_ccdc_archive 'CCDC 1003768'
#######################################################################
#
#                 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_S1_s476f

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H56 N2 O4, 4 C3H6O'
_chemical_formula_sum            'C61 H84 N2 O7'
_chemical_formula_weight         957.30

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1   '
_symmetry_space_group_name_Hall  '-C 2yc      '
_symmetry_int_tables_number      15

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

_cell_length_a                   21.951(4)
_cell_length_b                   12.163(3)
_cell_length_c                   21.185(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.170(10)
_cell_angle_gamma                90.00
_cell_volume                     5654.8(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6259

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'R-AXIS SPIDER'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 10.0000
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41276
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6490
_reflns_number_gt                5278
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

_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)+(0.1000P)²+8.0000P] 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         6490
_refine_ls_number_parameters     321
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1923
_refine_ls_wR_factor_gt          0.1746
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.009
_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
O1 O 0.06551(5) 0.24911(9) 0.33220(6) 0.0221(3) Uani 1 1 d . . .
O2 O 0.05431(6) 0.22453(11) 0.19479(6) 0.0286(3) Uani 1 1 d . . .
H2O H 0.0188 0.2294 0.1796 0.043 Uiso 1 1 calc R . .
N1 N 0.19613(9) 0.47166(18) 0.23876(10) 0.0478(5) Uani 1 1 d . . .
C1 C -0.00255(7) 0.12578(14) 0.42186(8) 0.0228(3) Uani 1 1 d . . .
H1A H 0.0005 0.2070 0.4225 0.027 Uiso 1 1 calc R . .
H1B H -0.0014 0.0999 0.4662 0.027 Uiso 1 1 calc R . .
C2 C 0.05241(7) 0.07913(14) 0.38802(8) 0.0213(3) Uani 1 1 d . . .
C3 C 0.08435(7) 0.14159(13) 0.34406(8) 0.0204(3) Uani 1 1 d . . .
C4 C 0.13243(7) 0.09637(14) 0.30998(8) 0.0216(3) Uani 1 1 d . . .
C5 C 0.15090(8) -0.01044(14) 0.32460(8) 0.0244(4) Uani 1 1 d . . .
H5 H 0.1847 -0.0406 0.3032 0.029 Uiso 1 1 calc R . .
C6 C 0.12160(8) -0.07499(14) 0.36956(8) 0.0256(4) Uani 1 1 d . A .
C7 C 0.07160(8) -0.02871(14) 0.39967(8) 0.0244(4) Uani 1 1 d . . .
H7 H 0.0500 -0.0720 0.4290 0.029 Uiso 1 1 calc R . .
C8 C 0.14545(10) -0.19026(16) 0.38690(10) 0.0341(4) Uani 1 1 d . . .
C9A C 0.19087(17) -0.1765(3) 0.44179(19) 0.0369(8) Uiso 0.60 1 d P A 1
H9AA H 0.2242 -0.1284 0.4289 0.044 Uiso 0.60 1 calc PR A 1
H9AC H 0.2073 -0.2485 0.4539 0.044 Uiso 0.60 1 calc PR A 1
H9AB H 0.1703 -0.1436 0.4778 0.044 Uiso 0.60 1 calc PR A 1
C9B C 0.2110(3) -0.1779(6) 0.4179(3) 0.0486(14) Uiso 0.40 1 d P A 2
H9BA H 0.2379 -0.1411 0.3882 0.058 Uiso 0.40 1 calc PR A 2
H9BC H 0.2274 -0.2509 0.4281 0.058 Uiso 0.40 1 calc PR A 2
H9BB H 0.2085 -0.1341 0.4566 0.058 Uiso 0.40 1 calc PR A 2
C10 C 0.09551(15) -0.2613(2) 0.41679(15) 0.0601(7) Uani 1 1 d . A .
H10B H 0.0808 -0.2249 0.4548 0.072 Uiso 1 1 calc R . .
H10C H 0.1124 -0.3335 0.4281 0.072 Uiso 1 1 calc R . .
H10A H 0.0616 -0.2708 0.3865 0.072 Uiso 1 1 calc R . .
C11 C 0.16584(15) -0.2529(2) 0.32873(13) 0.0598(8) Uani 1 1 d . A .
H11A H 0.1321 -0.2564 0.2978 0.072 Uiso 1 1 calc R . .
H11C H 0.1780 -0.3276 0.3409 0.072 Uiso 1 1 calc R . .
H11B H 0.2005 -0.2149 0.3101 0.072 Uiso 1 1 calc R . .
C12 C 0.16199(7) 0.15733(15) 0.25566(8) 0.0228(3) Uani 1 1 d . . .
H12A H 0.1511 0.2363 0.2576 0.027 Uiso 1 1 calc R . .
H12B H 0.2069 0.1511 0.2598 0.027 Uiso 1 1 calc R . .
C13 C 0.14083(7) 0.10999(14) 0.19259(8) 0.0215(3) Uani 1 1 d . . .
C14 C 0.08495(7) 0.14226(14) 0.16456(8) 0.0217(3) Uani 1 1 d . . .
C15 C 0.06362(7) 0.09336(14) 0.10857(8) 0.0215(3) Uani 1 1 d . . .
C16 C 0.09990(8) 0.01338(14) 0.08016(8) 0.0232(4) Uani 1 1 d . . .
H16 H 0.0857 -0.0198 0.0420 0.028 Uiso 1 1 calc R . .
C17 C 0.15612(8) -0.01934(14) 0.10587(8) 0.0239(4) Uani 1 1 d . . .
C18 C 0.17530(7) 0.03070(14) 0.16234(8) 0.0231(4) Uani 1 1 d . . .
H18 H 0.2134 0.0097 0.1807 0.028 Uiso 1 1 calc R . .
C19 C 0.19742(8) -0.10501(15) 0.07498(8) 0.0274(4) Uani 1 1 d . . .
C20 C 0.25869(9) -0.05072(17) 0.05950(10) 0.0338(4) Uani 1 1 d . . .
H20A H 0.2516 0.0107 0.0303 0.041 Uiso 1 1 calc R . .
H20C H 0.2853 -0.1050 0.0399 0.041 Uiso 1 1 calc R . .
H20B H 0.2781 -0.0233 0.0985 0.041 Uiso 1 1 calc R . .
C21 C 0.16888(10) -0.15101(19) 0.01374(10) 0.0391(5) Uani 1 1 d . . .
H21A H 0.1302 -0.1871 0.0231 0.047 Uiso 1 1 calc R . .
H21C H 0.1967 -0.2045 -0.0048 0.047 Uiso 1 1 calc R . .
H21B H 0.1615 -0.0908 -0.0162 0.047 Uiso 1 1 calc R . .
C22 C 0.20904(10) -0.20089(17) 0.12121(10) 0.0355(4) Uani 1 1 d . . .
H22C H 0.2280 -0.1727 0.1602 0.043 Uiso 1 1 calc R . .
H22B H 0.2363 -0.2546 0.1019 0.043 Uiso 1 1 calc R . .
H22A H 0.1703 -0.2364 0.1309 0.043 Uiso 1 1 calc R . .
C23 C 0.10011(8) 0.33181(15) 0.36586(9) 0.0276(4) Uani 1 1 d . . .
H23A H 0.1440 0.3245 0.3568 0.033 Uiso 1 1 calc R . .
H23B H 0.0948 0.3236 0.4119 0.033 Uiso 1 1 calc R . .
C24 C 0.07681(9) 0.44262(16) 0.34405(10) 0.0345(4) Uani 1 1 d . . .
H24B H 0.0995 0.5007 0.3673 0.041 Uiso 1 1 calc R . .
H24A H 0.0334 0.4491 0.3551 0.041 Uiso 1 1 calc R . .
C25 C 0.08279(9) 0.46308(16) 0.27285(10) 0.0340(4) Uani 1 1 d . . .
H25A H 0.0620 0.4031 0.2493 0.041 Uiso 1 1 calc R . .
H25B H 0.0621 0.5329 0.2616 0.041 Uiso 1 1 calc R . .
C26 C 0.14646(9) 0.46874(16) 0.25358(10) 0.0335(4) Uani 1 1 d . . .
O1S O -0.03027(11) 0.3954(2) 0.44606(13) 0.0870(8) Uani 1 1 d U . .
C1S C -0.13508(18) 0.3885(3) 0.42293(16) 0.0826(10) Uani 1 1 d U . .
H1SA H -0.1279 0.3090 0.4221 0.099 Uiso 1 1 calc R . .
H1SB H -0.1526 0.4120 0.3822 0.099 Uiso 1 1 calc R . .
H1SC H -0.1634 0.4062 0.4566 0.099 Uiso 1 1 calc R . .
C2S C -0.07808(16) 0.4450(3) 0.43443(15) 0.0708(9) Uani 1 1 d U . .
C3S C -0.0765(2) 0.5668(4) 0.4321(3) 0.1191(17) Uani 1 1 d U . .
H3SA H -0.0837 0.5913 0.3885 0.143 Uiso 1 1 calc R . .
H3SB H -0.0365 0.5928 0.4471 0.143 Uiso 1 1 calc R . .
H3SC H -0.1082 0.5966 0.4590 0.143 Uiso 1 1 calc R . .
O2S O 0.00476(19) -0.3036(2) 0.23763(16) 0.0464(8) Uiso 0.50 1 d P . 2
C4S C 0.0505(2) -0.1770(4) 0.1995(2) 0.0479(11) Uiso 0.50 1 d P . 1
H4SA H 0.0665 -0.2431 0.1814 0.072 Uiso 0.50 1 d PR . 1
H4SB H 0.0323 -0.1326 0.1667 0.072 Uiso 0.50 1 d PR . 1
H4SC H 0.0828 -0.1367 0.2200 0.072 Uiso 0.50 1 d PR . 1
C5S C 0.0000 -0.2083(2) 0.2500 0.0356(6) Uiso 1 2 d S . .
C6S C 0.0280(2) -0.1140(5) 0.2242(3) 0.0544(12) Uiso 0.50 1 d P . 2
H6SA H 0.0111 -0.0492 0.2429 0.082 Uiso 0.50 1 d PR . 2
H6SB H 0.0711 -0.1163 0.2327 0.082 Uiso 0.50 1 d PR . 2
H6SC H 0.0205 -0.1123 0.1793 0.082 Uiso 0.50 1 d PR . 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
O1 C3 1.393(2) . yes
O1 C23 1.441(2) . yes
O2 C14 1.372(2) . yes
O2 H2O 0.8400 . ?
N1 C26 1.141(3) . yes
C1 C2 1.525(2) . yes
C1 C15 1.527(2) 2 yes
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.398(2) . yes
C2 C3 1.401(2) . yes
C3 C4 1.403(2) . yes
C4 C5 1.394(2) . yes
C4 C12 1.525(2) . yes
C5 C6 1.401(3) . yes
C5 H5 0.9500 . ?
C6 C7 1.399(3) . yes
C6 C8 1.538(2) . yes
C7 H7 0.9500 . ?
C8 C11 1.524(3) . yes
C8 C9A 1.525(4) . yes
C8 C10 1.542(3) . yes
C8 C9B 1.577(7) . yes
C9A H9AA 0.9800 . ?
C9A H9AC 0.9800 . ?
C9A H9AB 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BC 0.9800 . ?
C9B H9BB 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10A 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11C 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.519(2) . yes
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.390(2) . yes
C13 C14 1.408(2) . yes
C14 C15 1.399(2) . yes
C15 C16 1.401(2) . yes
C15 C1 1.527(2) 2 yes
C16 C17 1.397(2) . yes
C16 H16 0.9500 . ?
C17 C18 1.399(2) . yes
C17 C19 1.536(2) . yes
C18 H18 0.9500 . ?
C19 C21 1.535(3) . yes
C19 C20 1.540(3) . yes
C19 C22 1.541(3) . yes
C20 H20A 0.9800 . ?
C20 H20C 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21C 0.9800 . ?
C21 H21B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22A 0.9800 . ?
C23 C24 1.510(3) . yes
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.537(3) . yes
C24 H24B 0.9900 . ?
C24 H24A 0.9900 . ?
C25 C26 1.466(3) . yes
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
O1S C2S 1.231(4) . yes
C1S C2S 1.444(5) . yes
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C2S C3S 1.482(6) . yes
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
O2S O2S 0.568(6) 2 yes
O2S C5S 1.193(4) . yes
C4S C5S 1.602(5) . yes
C4S H4SA 0.9599 . ?
C4S H4SB 0.9600 . ?
C4S H4SC 0.9600 . ?
C4S H6SB 1.1092 . ?
C4S H6SC 1.1053 . ?
C5S O2S 1.193(4) 2 yes
C5S C6S 1.416(6) 2 yes
C5S C6S 1.416(6) . yes
C5S C4S 1.602(5) 2 yes
C6S C6S 1.661(11) 2 yes
C6S H4SB 1.2439 . ?
C6S H4SC 1.2405 . ?
C6S H6SA 0.9599 . ?
C6S H6SB 0.9599 . ?
C6S H6SC 0.9601 . ?

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
C3 O1 C23 114.50(13) . . yes
C14 O2 H2O 109.5 . . ?
C2 C1 C15 113.67(13) . 2 yes
C2 C1 H1A 108.8 . . ?
C15 C1 H1A 108.8 2 . ?
C2 C1 H1B 108.8 . . ?
C15 C1 H1B 108.8 2 . ?
H1A C1 H1B 107.7 . . ?
C7 C2 C3 118.22(15) . . yes
C7 C2 C1 120.29(15) . . yes
C3 C2 C1 121.48(15) . . yes
O1 C3 C2 118.57(14) . . yes
O1 C3 C4 119.92(14) . . yes
C2 C3 C4 121.44(15) . . yes
C5 C4 C3 117.99(15) . . yes
C5 C4 C12 119.64(15) . . yes
C3 C4 C12 122.27(15) . . yes
C4 C5 C6 122.54(16) . . yes
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C7 C6 C5 117.38(16) . . yes
C7 C6 C8 121.62(16) . . yes
C5 C6 C8 120.95(17) . . yes
C2 C7 C6 122.25(16) . . yes
C2 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C11 C8 C9A 118.2(2) . . yes
C11 C8 C6 111.51(17) . . yes
C9A C8 C6 107.20(19) . . yes
C11 C8 C10 105.9(2) . . yes
C9A C8 C10 102.0(2) . . yes
C6 C8 C10 111.56(18) . . yes
C11 C8 C9B 95.9(3) . . yes
C9A C8 C9B 25.2(2) . . yes
C6 C8 C9B 108.4(3) . . yes
C10 C8 C9B 122.2(3) . . yes
C8 C9A H9AA 109.5 . . ?
C8 C9A H9AC 109.5 . . ?
C8 C9A H9AB 109.5 . . ?
C8 C9B H9BA 109.5 . . ?
C8 C9B H9BC 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
C8 C9B H9BB 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BC C9B H9BB 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
H10B C10 H10A 109.5 . . ?
H10C C10 H10A 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11C C11 H11B 109.5 . . ?
C13 C12 C4 110.63(13) . . yes
C13 C12 H12A 109.5 . . ?
C4 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C4 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C18 C13 C14 118.47(15) . . yes
C18 C13 C12 120.58(15) . . yes
C14 C13 C12 120.90(15) . . yes
O2 C14 C15 123.18(15) . . yes
O2 C14 C13 115.97(15) . . yes
C15 C14 C13 120.84(15) . . yes
C14 C15 C16 118.44(15) . . yes
C14 C15 C1 121.58(15) . 2 yes
C16 C15 C1 119.98(15) . 2 yes
C17 C16 C15 122.40(16) . . yes
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C18 117.24(15) . . yes
C16 C17 C19 123.47(15) . . yes
C18 C17 C19 119.29(15) . . yes
C13 C18 C17 122.58(15) . . yes
C13 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
C21 C19 C17 111.91(15) . . yes
C21 C19 C20 108.64(16) . . yes
C17 C19 C20 109.00(15) . . yes
C21 C19 C22 108.72(17) . . yes
C17 C19 C22 109.51(15) . . yes
C20 C19 C22 109.02(15) . . yes
C19 C20 H20A 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20C C20 H20B 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21C C21 H21B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22C C22 H22B 109.5 . . ?
C19 C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
O1 C23 C24 107.45(15) . . yes
O1 C23 H23A 110.2 . . ?
C24 C23 H23A 110.2 . . ?
O1 C23 H23B 110.2 . . ?
C24 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
C23 C24 C25 114.17(16) . . yes
C23 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C23 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
H24B C24 H24A 107.6 . . ?
C26 C25 C24 112.45(17) . . yes
C26 C25 H25A 109.1 . . ?
C24 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
C24 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
N1 C26 C25 179.1(2) . . yes
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
O1S C2S C1S 122.2(3) . . yes
O1S C2S C3S 118.4(4) . . yes
C1S C2S C3S 119.4(3) . . yes
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
O2S O2S C5S 76.22(15) 2 . yes
C5S C4S H4SA 109.4 . . ?
C5S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C5S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
C5S C4S H6SB 90.7 . . ?
H4SA C4S H6SB 131.4 . . ?
H4SB C4S H6SB 104.0 . . ?
H4SC C4S H6SB 23.8 . . ?
C5S C4S H6SC 90.8 . . ?
H4SA C4S H6SC 131.5 . . ?
H4SB C4S H6SC 23.9 . . ?
H4SC C4S H6SC 103.9 . . ?
H6SB C4S H6SC 90.1 . . ?
O2S C5S O2S 27.6(3) . 2 yes
O2S C5S C6S 155.8(3) . 2 yes
O2S C5S C6S 131.4(3) 2 2 yes
O2S C5S C6S 131.4(3) . . yes
O2S C5S C6S 155.8(3) 2 . yes
C6S C5S C6S 71.9(5) 2 . yes
O2S C5S C4S 116.2(3) . 2 yes
O2S C5S C4S 91.1(3) 2 2 yes
C6S C5S C4S 40.4(3) 2 2 yes
C6S C5S C4S 112.2(4) . 2 yes
O2S C5S C4S 91.1(3) . . yes
O2S C5S C4S 116.2(3) 2 . yes
C6S C5S C4S 112.2(4) 2 . yes
C6S C5S C4S 40.4(3) . . yes
C4S C5S C4S 152.6(4) 2 . yes
C5S C6S C6S 54.1(2) . 2 yes
C5S C6S H4SB 105.9 . . ?
C6S C6S H4SB 135.8 2 . ?
C5S C6S H4SC 106.0 . . ?
C6S C6S H4SC 141.1 2 . ?
H4SB C6S H4SC 78.2 . . ?
C5S C6S H6SA 109.3 . . ?
C6S C6S H6SA 55.3 2 . ?
H4SB C6S H6SA 126.4 . . ?
H4SC C6S H6SA 126.5 . . ?
C5S C6S H6SB 109.7 . . ?
C6S C6S H6SB 127.9 2 . ?
H4SB C6S H6SB 94.8 . . ?
H4SC C6S H6SB 18.6 . . ?
H6SA C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
C6S C6S H6SC 122.6 2 . ?
H4SB C6S H6SC 18.4 . . ?
H4SC C6S H6SC 94.6 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2O O1 0.84 1.88 2.6967(17) 164.8 2

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.061

# File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison.
_database_code_depnum_ccdc_archive 'CCDC 1003769'
#######################################################################
#
#                 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_ng48sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H34 N2 O4, C H2 Cl2'
_chemical_formula_sum            'C37 H36 Cl2 N2 O4'
_chemical_formula_weight         643.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   10.0646(11)
_cell_length_b                   15.6235(17)
_cell_length_c                   20.246(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3183.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.836786
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SMART 1k'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21304
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         23.29
_reflns_number_total             4585
_reflns_number_gt                3616
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       SMART
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  X-Seed

_refine_special_details          
; 
O-H hydrogens located and refined, all other H's in calculated positions 

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)+(0.0297P)²+0.9149P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_number_reflns         4585
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_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
Cl1 Cl 0.29631(11) 0.67079(6) 0.86204(5) 0.0347(3) Uani 1 1 d . . .
Cl2 Cl 0.27749(11) 0.77298(7) 0.74173(5) 0.0343(3) Uani 1 1 d . . .
O1 O 0.3978(2) 0.43481(15) 0.65319(12) 0.0237(6) Uani 1 1 d . . .
O2 O 0.1816(3) 0.42732(18) 0.73676(13) 0.0230(7) Uani 1 1 d . . .
O3 O -0.0438(2) 0.50232(15) 0.66725(11) 0.0182(6) Uani 1 1 d . . .
O4 O 0.1901(3) 0.54750(16) 0.60551(13) 0.0223(7) Uani 1 1 d . . .
N5 N 0.1141(4) 0.2223(2) 0.51439(17) 0.0382(10) Uani 1 1 d . . .
N6 N -0.2543(5) 0.4837(3) 0.4624(2) 0.0685(15) Uani 1 1 d . . .
C1 C 0.4697(4) 0.4984(2) 0.68566(18) 0.0206(9) Uani 1 1 d . . .
C2 C 0.5002(3) 0.5733(2) 0.65174(18) 0.0196(9) Uani 1 1 d . . .
C3 C 0.5723(4) 0.6360(3) 0.68571(19) 0.0275(10) Uani 1 1 d . . .
H3 H 0.5957 0.6877 0.6639 0.033 Uiso 1 1 calc R . .
C4 C 0.6098(4) 0.6236(3) 0.7506(2) 0.0286(10) Uani 1 1 d . . .
H4 H 0.6606 0.6661 0.7728 0.034 Uiso 1 1 calc R . .
C5 C 0.5738(4) 0.5494(3) 0.7836(2) 0.0290(11) Uani 1 1 d . . .
H5 H 0.5990 0.5419 0.8284 0.035 Uiso 1 1 calc R . .
C6 C 0.5016(4) 0.4861(2) 0.75217(19) 0.0212(9) Uani 1 1 d . . .
C7 C 0.4507(4) 0.4092(2) 0.79071(19) 0.0267(10) Uani 1 1 d . . .
H7A H 0.4295 0.3625 0.7594 0.032 Uiso 1 1 calc R . .
H7B H 0.5219 0.3886 0.8205 0.032 Uiso 1 1 calc R . .
C8 C 0.3287(4) 0.4294(2) 0.83121(18) 0.0217(10) Uani 1 1 d . . .
C9 C 0.2040(4) 0.4397(2) 0.80271(16) 0.0185(9) Uani 1 1 d . . .
C10 C 0.0925(4) 0.4604(2) 0.84077(17) 0.0180(9) Uani 1 1 d . . .
C11 C 0.1081(4) 0.4716(2) 0.90782(18) 0.0221(10) Uani 1 1 d . . .
H11 H 0.0330 0.4852 0.9343 0.027 Uiso 1 1 calc R . .
C12 C 0.2330(4) 0.4633(2) 0.93757(18) 0.0270(10) Uani 1 1 d . . .
H12 H 0.2430 0.4726 0.9837 0.032 Uiso 1 1 calc R . .
C13 C 0.3414(4) 0.4414(2) 0.89935(19) 0.0252(10) Uani 1 1 d . . .
H13 H 0.4258 0.4345 0.9196 0.030 Uiso 1 1 calc R . .
C14 C -0.0430(4) 0.4713(2) 0.80808(18) 0.0209(9) Uani 1 1 d . . .
H14A H -0.0538 0.4274 0.7732 0.025 Uiso 1 1 calc R . .
H14B H -0.1136 0.4622 0.8414 0.025 Uiso 1 1 calc R . .
C15 C -0.0586(3) 0.5597(2) 0.77782(17) 0.0162(9) Uani 1 1 d . . .
C16 C -0.0691(4) 0.6314(2) 0.81791(18) 0.0198(9) Uani 1 1 d . . .
H16 H -0.0724 0.6244 0.8645 0.024 Uiso 1 1 calc R . .
C17 C -0.0749(4) 0.7129(3) 0.79124(19) 0.0235(10) Uani 1 1 d . . .
H17 H -0.0853 0.7610 0.8194 0.028 Uiso 1 1 calc R . .
C18 C -0.0655(3) 0.7244(2) 0.72359(18) 0.0211(9) Uani 1 1 d . . .
H18 H -0.0673 0.7805 0.7057 0.025 Uiso 1 1 calc R . .
C19 C -0.0533(4) 0.6540(2) 0.68150(18) 0.0169(9) Uani 1 1 d . . .
C20 C -0.0542(3) 0.5730(2) 0.70965(17) 0.0165(9) Uani 1 1 d . . .
C21 C -0.0336(4) 0.6681(2) 0.60806(18) 0.0226(9) Uani 1 1 d . . .
H21A H -0.0939 0.7142 0.5930 0.027 Uiso 1 1 calc R . .
H21B H -0.0577 0.6151 0.5841 0.027 Uiso 1 1 calc R . .
C22 C 0.1097(4) 0.6924(2) 0.59102(17) 0.0204(9) Uani 1 1 d . . .
C23 C 0.1411(4) 0.7770(3) 0.57493(18) 0.0272(10) Uani 1 1 d . . .
H23 H 0.0729 0.8190 0.5739 0.033 Uiso 1 1 calc R . .
C24 C 0.2695(4) 0.8001(2) 0.56062(18) 0.0307(11) Uani 1 1 d . . .
H24 H 0.2894 0.8579 0.5496 0.037 Uiso 1 1 calc R . .
C25 C 0.3696(4) 0.7401(3) 0.56212(18) 0.0295(11) Uani 1 1 d . . .
H25 H 0.4578 0.7570 0.5519 0.035 Uiso 1 1 calc R . .
C26 C 0.3444(4) 0.6555(2) 0.57819(17) 0.0219(10) Uani 1 1 d . . .
C27 C 0.2123(4) 0.6327(2) 0.59251(16) 0.0187(9) Uani 1 1 d . . .
C28 C 0.4545(4) 0.5896(3) 0.58134(18) 0.0257(10) Uani 1 1 d . . .
H28A H 0.5309 0.6098 0.5547 0.031 Uiso 1 1 calc R . .
H28B H 0.4226 0.5353 0.5618 0.031 Uiso 1 1 calc R . .
C29 C 0.4785(4) 0.3678(2) 0.62495(19) 0.0245(10) Uani 1 1 d . . .
H29A H 0.5402 0.3446 0.6585 0.029 Uiso 1 1 calc R . .
H29B H 0.5314 0.3904 0.5876 0.029 Uiso 1 1 calc R . .
C30 C 0.3852(4) 0.2989(2) 0.60132(19) 0.0246(10) Uani 1 1 d . . .
H30A H 0.3271 0.2805 0.6382 0.029 Uiso 1 1 calc R . .
H30B H 0.4369 0.2487 0.5863 0.029 Uiso 1 1 calc R . .
C31 C 0.3001(4) 0.3324(2) 0.54455(18) 0.0298(10) Uani 1 1 d . . .
H31A H 0.2584 0.3873 0.5575 0.036 Uiso 1 1 calc R . .
H31B H 0.3570 0.3431 0.5055 0.036 Uiso 1 1 calc R . .
C32 C 0.1951(5) 0.2697(3) 0.52710(18) 0.0260(10) Uani 1 1 d . . .
C33 C -0.1701(4) 0.4666(2) 0.64782(19) 0.0231(9) Uani 1 1 d . . .
H33A H -0.2216 0.5091 0.6222 0.028 Uiso 1 1 calc R . .
H33B H -0.2223 0.4505 0.6874 0.028 Uiso 1 1 calc R . .
C34 C -0.1426(4) 0.3886(2) 0.60615(19) 0.0250(10) Uani 1 1 d . . .
H34A H -0.2268 0.3569 0.5998 0.030 Uiso 1 1 calc R . .
H34B H -0.0808 0.3507 0.6305 0.030 Uiso 1 1 calc R . .
C35 C -0.0837(4) 0.4080(3) 0.5392(2) 0.0339(11) Uani 1 1 d . . .
H35A H -0.0038 0.4442 0.5450 0.041 Uiso 1 1 calc R . .
H35B H -0.0553 0.3538 0.5182 0.041 Uiso 1 1 calc R . .
C36 C -0.1774(5) 0.4518(3) 0.4954(2) 0.0395(12) Uani 1 1 d . . .
C1S C 0.2677(4) 0.6696(2) 0.77609(17) 0.0265(10) Uani 1 1 d . . .
H1S1 H 0.3343 0.6322 0.7546 0.032 Uiso 1 1 calc R . .
H1S2 H 0.1786 0.6454 0.7673 0.032 Uiso 1 1 calc R . .
H2O H 0.241(5) 0.422(3) 0.713(2) 0.055(18) Uiso 1 1 d . . .
H4O H 0.117(5) 0.533(3) 0.620(3) 0.08(2) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1S 1.764(4) . ?
Cl2 C1S 1.761(4) . ?
O1 C1 1.394(4) . ?
O1 C29 1.443(4) . ?
O2 C9 1.368(4) . ?
O3 C20 1.403(4) . ?
O3 C33 1.443(4) . ?
O4 C27 1.376(4) . ?
N5 C32 1.131(5) . ?
N6 C36 1.138(5) . ?
C1 C2 1.392(5) . ?
C1 C6 1.398(5) . ?
C2 C3 1.399(5) . ?
C2 C28 1.519(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.386(6) . ?
C5 C6 1.382(5) . ?
C6 C7 1.520(5) . ?
C7 C8 1.510(5) . ?
C8 C9 1.390(5) . ?
C8 C13 1.398(5) . ?
C9 C10 1.400(5) . ?
C10 C11 1.378(5) . ?
C10 C14 1.525(5) . ?
C11 C12 1.400(5) . ?
C12 C13 1.381(5) . ?
C14 C15 1.520(5) . ?
C15 C16 1.387(5) . ?
C15 C20 1.396(5) . ?
C16 C17 1.384(5) . ?
C17 C18 1.385(5) . ?
C18 C19 1.396(5) . ?
C19 C20 1.388(5) . ?
C19 C21 1.516(5) . ?
C21 C22 1.531(5) . ?
C22 C27 1.392(5) . ?
C22 C23 1.398(5) . ?
C23 C24 1.372(5) . ?
C24 C25 1.377(5) . ?
C25 C26 1.384(5) . ?
C26 C27 1.407(5) . ?
C26 C28 1.513(5) . ?
C29 C30 1.507(5) . ?
C30 C31 1.526(5) . ?
C31 C32 1.483(6) . ?
C33 C34 1.508(5) . ?
C34 C35 1.511(5) . ?
C35 C36 1.464(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C29 114.3(3) . . ?
C20 O3 C33 113.9(3) . . ?
C2 C1 O1 118.8(3) . . ?
C2 C1 C6 122.7(4) . . ?
O1 C1 C6 118.4(4) . . ?
C1 C2 C3 117.4(3) . . ?
C1 C2 C28 122.5(3) . . ?
C3 C2 C28 120.1(4) . . ?
C4 C3 C2 120.7(4) . . ?
C3 C4 C5 120.3(4) . . ?
C6 C5 C4 121.0(4) . . ?
C5 C6 C1 117.7(4) . . ?
C5 C6 C7 120.4(4) . . ?
C1 C6 C7 121.7(4) . . ?
C8 C7 C6 112.8(3) . . ?
C9 C8 C13 118.5(3) . . ?
C9 C8 C7 122.2(3) . . ?
C13 C8 C7 119.3(3) . . ?
O2 C9 C8 122.5(4) . . ?
O2 C9 C10 115.9(4) . . ?
C8 C9 C10 121.5(3) . . ?
C11 C10 C9 118.7(4) . . ?
C11 C10 C14 121.0(3) . . ?
C9 C10 C14 120.3(3) . . ?
C10 C11 C12 121.0(4) . . ?
C13 C12 C11 119.4(3) . . ?
C12 C13 C8 120.9(4) . . ?
C15 C14 C10 111.6(3) . . ?
C16 C15 C20 117.4(3) . . ?
C16 C15 C14 120.4(3) . . ?
C20 C15 C14 122.0(3) . . ?
C17 C16 C15 121.2(3) . . ?
C16 C17 C18 120.1(4) . . ?
C17 C18 C19 120.5(4) . . ?
C20 C19 C18 117.8(3) . . ?
C20 C19 C21 122.4(3) . . ?
C18 C19 C21 119.7(3) . . ?
C19 C20 C15 122.8(3) . . ?
C19 C20 O3 117.8(3) . . ?
C15 C20 O3 119.3(3) . . ?
C19 C21 C22 112.4(3) . . ?
C27 C22 C23 118.1(4) . . ?
C27 C22 C21 121.9(3) . . ?
C23 C22 C21 120.0(4) . . ?
C24 C23 C22 120.8(4) . . ?
C23 C24 C25 120.3(4) . . ?
C24 C25 C26 121.5(4) . . ?
C25 C26 C27 117.6(4) . . ?
C25 C26 C28 121.7(4) . . ?
C27 C26 C28 120.7(3) . . ?
O4 C27 C22 122.2(4) . . ?
O4 C27 C26 116.0(3) . . ?
C22 C27 C26 121.8(3) . . ?
C26 C28 C2 112.0(3) . . ?
O1 C29 C30 107.0(3) . . ?
C29 C30 C31 110.1(3) . . ?
C32 C31 C30 110.7(3) . . ?
N5 C32 C31 179.1(5) . . ?
O3 C33 C34 107.7(3) . . ?
C33 C34 C35 114.3(3) . . ?
C36 C35 C34 112.6(4) . . ?
N6 C36 C35 177.1(5) . . ?
Cl2 C1S Cl1 111.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.29
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 1003934'
#######################################################################
#
#                 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_06kma022

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            06kma022
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H82 N2 O4'
_chemical_formula_weight         895.28

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   C2/c

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

_cell_length_a                   27.48(2)
_cell_length_b                   20.311(15)
_cell_length_c                   19.585(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.34(6)
_cell_angle_gamma                90.00
_cell_volume                     10923(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3904
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9738
_exptl_absorpt_correction_T_max  0.9967
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8720
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_sigmaI/netI    0.2042
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         23.27
_reflns_number_total             5304
_reflns_number_gt                2080
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0667P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5304
_refine_ls_number_parameters     609
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1672
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_ref         0.1687
_refine_ls_wR_factor_gt          0.1364
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_restrained_S_all      0.792
_refine_ls_shift/su_max          0.034
_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
O1 O 0.32961(12) 0.0314(2) 0.3557(2) 0.0362(13) Uani 1 1 d . . .
O2 O 0.25925(12) 0.1181(2) 0.0957(2) 0.0396(13) Uani 1 1 d . . .
O3 O 0.24935(13) 0.1179(2) 0.2457(2) 0.0360(13) Uani 1 1 d . . .
O4 O 0.23581(12) -0.0925(3) 0.1876(2) 0.0380(13) Uani 1 1 d . . .
N2 N 0.1909(2) -0.1996(3) 0.0677(4) 0.083(3) Uani 1 1 d . . .
N4 N 0.3178(2) 0.2486(4) 0.1945(4) 0.055(2) Uani 1 1 d . . .
C1 C 0.4451(3) 0.1368(5) -0.0909(7) 0.130(5) Uani 1 1 d . . .
H1A H 0.4642 0.1302 -0.0481 0.196 Uiso 1 1 calc R . .
H1B H 0.4666 0.1340 -0.1295 0.196 Uiso 1 1 calc R . .
H1C H 0.4200 0.1026 -0.0956 0.196 Uiso 1 1 calc R . .
C2 C 0.4234(3) 0.1976(5) -0.0904(6) 0.099(4) Uani 1 1 d . . .
H2A H 0.4022 0.2022 -0.1322 0.118 Uiso 1 1 calc R . .
H2B H 0.4491 0.2317 -0.0919 0.118 Uiso 1 1 calc R . .
C3 C 0.2354(2) -0.1618(4) 0.1808(3) 0.039(2) Uani 1 1 d . . .
H3A H 0.2188 -0.1815 0.2198 0.047 Uiso 1 1 calc R . .
H3B H 0.2693 -0.1784 0.1818 0.047 Uiso 1 1 calc R . .
C4 C 0.29976(18) 0.1315(4) 0.2419(3) 0.039(2) Uani 1 1 d . . .
H4A H 0.3145 0.0987 0.2117 0.047 Uiso 1 1 calc R . .
H4B H 0.3154 0.1266 0.2880 0.047 Uiso 1 1 calc R . .
C5 C 0.2817(2) 0.0077(4) 0.3609(3) 0.0308(19) Uani 1 1 d . . .
C6 C 0.30816(19) -0.0961(3) 0.3000(3) 0.0316(19) Uani 1 1 d . . .
H6A H 0.3392 -0.0978 0.3275 0.038 Uiso 1 1 calc R . .
H6B H 0.2962 -0.1417 0.2937 0.038 Uiso 1 1 calc R . .
C7 C 0.1309(2) 0.1032(3) 0.1352(3) 0.036(2) Uani 1 1 d . . .
H7 H 0.1058 0.1298 0.1525 0.043 Uiso 1 1 calc R . .
C8 C 0.2713(2) -0.0567(4) 0.3380(3) 0.0319(19) Uani 1 1 d . . .
C9 C 0.21343(19) 0.0896(4) 0.1044(3) 0.033(2) Uani 1 1 d . . .
C10 C 0.2242(2) -0.0794(3) 0.3446(3) 0.0313(19) Uani 1 1 d . . .
H10 H 0.2168 -0.1234 0.3314 0.038 Uiso 1 1 calc R . .
C11 C 0.13483(19) -0.0678(3) 0.3726(4) 0.035(2) Uani 1 1 d . . .
C12 C 0.28097(19) -0.0618(3) 0.1790(4) 0.031(2) Uani 1 1 d . . .
C13 C 0.2199(2) 0.1612(3) 0.2808(4) 0.0316(19) Uani 1 1 d . . .
C14 C 0.36135(19) -0.0358(3) 0.2187(4) 0.036(2) Uani 1 1 d . . .
H14 H 0.3862 -0.0370 0.2538 0.043 Uiso 1 1 calc R . .
C15 C 0.24612(18) -0.0194(3) 0.0649(3) 0.037(2) Uani 1 1 d . . .
H15A H 0.2600 -0.0006 0.0233 0.045 Uiso 1 1 calc R . .
H15B H 0.2327 -0.0633 0.0530 0.045 Uiso 1 1 calc R . .
C16 C 0.1888(2) 0.1966(3) 0.1615(3) 0.0340(19) Uani 1 1 d . . .
H16A H 0.1653 0.2288 0.1414 0.041 Uiso 1 1 calc R . .
H16B H 0.2218 0.2098 0.1482 0.041 Uiso 1 1 calc R . .
C17 C 0.1204(2) -0.0981(3) 0.3029(3) 0.047(2) Uani 1 1 d . . .
H17A H 0.0858 -0.1097 0.3017 0.070 Uiso 1 1 calc R . .
H17B H 0.1398 -0.1378 0.2958 0.070 Uiso 1 1 calc R . .
H17C H 0.1264 -0.0662 0.2667 0.070 Uiso 1 1 calc R . .
C18 C 0.3711(2) -0.0043(3) 0.1592(4) 0.034(2) Uani 1 1 d . . .
C19 C 0.1773(2) 0.1290(3) 0.1323(3) 0.0307(19) Uani 1 1 d . . .
C20 C 0.2459(2) 0.0489(4) 0.3822(3) 0.0287(19) Uani 1 1 d . . .
C21 C 0.20498(19) 0.0248(4) 0.0872(3) 0.034(2) Uani 1 1 d . . .
C22 C 0.1198(2) 0.0393(4) 0.1136(3) 0.037(2) Uani 1 1 d . . .
C23 C 0.3564(2) 0.0339(3) 0.4197(3) 0.044(2) Uani 1 1 d . . .
H23A H 0.3617 -0.0113 0.4375 0.052 Uiso 1 1 calc R . .
H23B H 0.3378 0.0589 0.4533 0.052 Uiso 1 1 calc R . .
C24 C 0.1869(2) -0.0400(4) 0.3701(3) 0.033(2) Uani 1 1 d . . .
C25 C 0.06618(19) 0.0156(4) 0.1146(4) 0.035(2) Uani 1 1 d . . .
C26 C 0.40123(19) 0.1385(3) 0.3868(3) 0.042(2) Uani 1 1 d . . .
H26A H 0.3802 0.1627 0.4180 0.051 Uiso 1 1 calc R . .
H26B H 0.3855 0.1402 0.3404 0.051 Uiso 1 1 calc R . .
C27 C 0.3101(2) 0.1982(5) 0.2160(4) 0.034(2) Uani 1 1 d . . .
C28 C 0.1867(2) 0.1988(3) 0.2386(4) 0.036(2) Uani 1 1 d . . .
C29 C 0.1510(2) 0.2331(3) 0.2722(4) 0.037(2) Uani 1 1 d . . .
H29 H 0.1275 0.2567 0.2451 0.044 Uiso 1 1 calc R . .
C30 C 0.25370(19) 0.1216(3) 0.3957(3) 0.036(2) Uani 1 1 d . . .
H30A H 0.2878 0.1333 0.3866 0.044 Uiso 1 1 calc R . .
H30B H 0.2482 0.1311 0.4444 0.044 Uiso 1 1 calc R . .
C31 C 0.03608(19) 0.0596(3) 0.0625(3) 0.047(2) Uani 1 1 d . . .
H31A H 0.0018 0.0461 0.0616 0.071 Uiso 1 1 calc R . .
H31B H 0.0489 0.0543 0.0168 0.071 Uiso 1 1 calc R . .
H31C H 0.0387 0.1058 0.0764 0.071 Uiso 1 1 calc R . .
C32 C 0.1474(2) 0.2352(3) 0.3416(4) 0.039(2) Uani 1 1 d . . .
C33 C 0.3172(2) -0.0662(3) 0.2311(3) 0.0308(19) Uani 1 1 d . . .
C34 C 0.15762(19) 0.0001(3) 0.0919(3) 0.035(2) Uani 1 1 d . . .
H34 H 0.1512 -0.0445 0.0799 0.042 Uiso 1 1 calc R . .
C35 C 0.1068(2) 0.2681(3) 0.3790(4) 0.040(2) Uani 1 1 d . . .
C36 C 0.1836(2) 0.1996(3) 0.3820(4) 0.038(2) Uani 1 1 d . . .
H36 H 0.1831 0.2009 0.4304 0.046 Uiso 1 1 calc R . .
C37 C 0.2192(2) 0.1636(3) 0.3507(3) 0.0304(19) Uani 1 1 d . . .
C38 C 0.09821(19) -0.0145(3) 0.3898(4) 0.048(2) Uani 1 1 d . . .
H38A H 0.0981 0.0198 0.3547 0.073 Uiso 1 1 calc R . .
H38B H 0.1074 0.0048 0.4344 0.073 Uiso 1 1 calc R . .
H38C H 0.0656 -0.0340 0.3915 0.073 Uiso 1 1 calc R . .
C39 C 0.42115(19) 0.0285(3) 0.1491(3) 0.0329(19) Uani 1 1 d . . .
C40 C 0.1982(2) 0.0245(3) 0.3874(3) 0.0323(19) Uani 1 1 d . . .
H40 H 0.1734 0.0527 0.4029 0.039 Uiso 1 1 calc R . .
C41 C 0.3434(2) 0.1702(3) -0.0241(4) 0.051(2) Uani 1 1 d . . .
H41A H 0.3248 0.1793 -0.0674 0.061 Uiso 1 1 calc R . .
H41B H 0.3524 0.1230 -0.0241 0.061 Uiso 1 1 calc R . .
C42 C 0.2104(3) -0.1817(4) 0.1170(5) 0.055(3) Uani 1 1 d . . .
C43 C 0.1340(2) -0.1213(3) 0.4273(3) 0.044(2) Uani 1 1 d . . .
H43A H 0.1462 -0.1031 0.4712 0.066 Uiso 1 1 calc R . .
H43B H 0.1548 -0.1580 0.4143 0.066 Uiso 1 1 calc R . .
H43C H 0.1006 -0.1370 0.4317 0.066 Uiso 1 1 calc R . .
C44 C 0.0456(2) 0.0249(4) 0.1850(4) 0.055(2) Uani 1 1 d . . .
H44A H 0.0121 0.0082 0.1846 0.082 Uiso 1 1 calc R . .
H44B H 0.0458 0.0718 0.1968 0.082 Uiso 1 1 calc R . .
H44C H 0.0656 0.0006 0.2191 0.082 Uiso 1 1 calc R . .
C45 C 0.4508(2) 0.1732(4) 0.3855(4) 0.052(2) Uani 1 1 d . . .
H45A H 0.4656 0.1736 0.4325 0.063 Uiso 1 1 calc R . .
H45B H 0.4724 0.1473 0.3566 0.063 Uiso 1 1 calc R . .
C46 C 0.1276(2) 0.3245(4) 0.4241(4) 0.064(3) Uani 1 1 d . . .
H46A H 0.1526 0.3070 0.4562 0.096 Uiso 1 1 calc R . .
H46B H 0.1013 0.3443 0.4496 0.096 Uiso 1 1 calc R . .
H46C H 0.1420 0.3580 0.3951 0.096 Uiso 1 1 calc R . .
C47 C 0.3902(2) 0.2114(4) -0.0226(4) 0.064(3) Uani 1 1 d . . .
H47A H 0.4099 0.2009 0.0195 0.077 Uiso 1 1 calc R . .
H47B H 0.3816 0.2587 -0.0210 0.077 Uiso 1 1 calc R . .
C48 C 0.0813(2) 0.2187(4) 0.4236(4) 0.061(2) Uani 1 1 d . . .
H48A H 0.0657 0.1848 0.3947 0.092 Uiso 1 1 calc R . .
H48B H 0.0566 0.2413 0.4496 0.092 Uiso 1 1 calc R . .
H48C H 0.1052 0.1981 0.4554 0.092 Uiso 1 1 calc R . .
C49 C 0.40482(19) 0.0670(3) 0.4096(4) 0.044(2) Uani 1 1 d . . .
H49A H 0.4225 0.0419 0.3751 0.053 Uiso 1 1 calc R . .
H49B H 0.4244 0.0650 0.4532 0.053 Uiso 1 1 calc R . .
C52 C 0.2869(2) -0.0271(3) 0.1201(4) 0.033(2) Uani 1 1 d . . .
C54 C 0.0689(2) 0.2986(3) 0.3274(4) 0.059(3) Uani 1 1 d . . .
H54A H 0.0849 0.3315 0.2994 0.088 Uiso 1 1 calc R . .
H54B H 0.0429 0.3196 0.3523 0.088 Uiso 1 1 calc R . .
H54C H 0.0551 0.2638 0.2978 0.088 Uiso 1 1 calc R . .
C55 C 0.0612(2) -0.0562(3) 0.0929(4) 0.056(2) Uani 1 1 d . . .
H55A H 0.0796 -0.0841 0.1255 0.084 Uiso 1 1 calc R . .
H55B H 0.0739 -0.0617 0.0473 0.084 Uiso 1 1 calc R . .
H55C H 0.0267 -0.0688 0.0920 0.084 Uiso 1 1 calc R . .
C56 C 0.33279(19) 0.0017(3) 0.1099(4) 0.036(2) Uani 1 1 d . . .
H56 H 0.3378 0.0255 0.0690 0.043 Uiso 1 1 calc R . .
C57 C 0.4484(2) 0.2431(4) 0.3590(5) 0.070(3) Uani 1 1 d . . .
H57A H 0.4271 0.2692 0.3883 0.084 Uiso 1 1 calc R . .
H57B H 0.4333 0.2428 0.3122 0.084 Uiso 1 1 calc R . .
C58 C 0.3127(3) 0.1820(5) 0.0311(5) 0.095(3) Uani 1 1 d . . .
H58A H 0.3053 0.2297 0.0323 0.114 Uiso 1 1 calc R . .
H58B H 0.3311 0.1710 0.0741 0.114 Uiso 1 1 calc R . .
C59 C 0.4297(2) 0.0451(5) 0.0780(4) 0.112(4) Uani 1 1 d . . .
H59A H 0.4628 0.0624 0.0746 0.168 Uiso 1 1 calc R . .
H59B H 0.4062 0.0784 0.0620 0.168 Uiso 1 1 calc R . .
H59C H 0.4259 0.0055 0.0496 0.168 Uiso 1 1 calc R . .
C60 C 0.2649(3) 0.1445(4) 0.0298(4) 0.075(3) Uani 1 1 d . . .
H60A H 0.2375 0.1744 0.0175 0.090 Uiso 1 1 calc R . .
H60B H 0.2654 0.1086 -0.0044 0.090 Uiso 1 1 calc R . .
C62 C 0.4250(3) 0.0893(4) 0.1930(6) 0.129(5) Uani 1 1 d . . .
H62A H 0.4592 0.1029 0.1981 0.194 Uiso 1 1 calc R . .
H62B H 0.4126 0.0798 0.2382 0.194 Uiso 1 1 calc R . .
H62C H 0.4058 0.1249 0.1714 0.194 Uiso 1 1 calc R . .
C64 C 0.4980(2) 0.2764(4) 0.3574(5) 0.104(4) Uani 1 1 d . . .
H64A H 0.5125 0.2787 0.4039 0.156 Uiso 1 1 calc R . .
H64B H 0.4941 0.3210 0.3390 0.156 Uiso 1 1 calc R . .
H64C H 0.5193 0.2509 0.3284 0.156 Uiso 1 1 calc R . .
C66 C 0.4608(2) -0.0189(4) 0.1706(6) 0.147(6) Uani 1 1 d . . .
H66A H 0.4571 -0.0596 0.1441 0.221 Uiso 1 1 calc R . .
H66B H 0.4585 -0.0289 0.2194 0.221 Uiso 1 1 calc R . .
H66C H 0.4925 0.0008 0.1626 0.221 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
O1 C5 1.410(7) . ?
O1 C23 1.427(7) . ?
O2 C9 1.403(7) . ?
O2 C60 1.411(8) . ?
O3 C13 1.396(7) . ?
O3 C4 1.418(6) . ?
O4 C12 1.405(7) . ?
O4 C3 1.413(7) . ?
N2 C42 1.145(9) . ?
N4 C27 1.130(8) . ?
C1 C2 1.371(10) . ?
C2 C47 1.665(12) . ?
C3 C42 1.459(10) . ?
C4 C27 1.477(9) . ?
C5 C20 1.368(8) . ?
C5 C8 1.409(8) . ?
C6 C33 1.509(9) . ?
C6 C8 1.510(8) . ?
C7 C19 1.383(8) . ?
C7 C22 1.394(8) . ?
C8 C10 1.383(8) . ?
C9 C21 1.376(8) . ?
C9 C19 1.403(8) . ?
C10 C24 1.408(8) . ?
C11 C38 1.525(8) . ?
C11 C43 1.527(8) . ?
C11 C17 1.536(9) . ?
C11 C24 1.542(8) . ?
C12 C52 1.367(9) . ?
C12 C33 1.399(8) . ?
C13 C37 1.371(9) . ?
C13 C28 1.428(8) . ?
C14 C18 1.366(9) . ?
C14 C33 1.391(8) . ?
C15 C21 1.521(8) . ?
C15 C52 1.533(7) . ?
C16 C19 1.515(8) . ?
C16 C28 1.515(9) . ?
C18 C56 1.405(7) . ?
C18 C39 1.548(8) . ?
C20 C40 1.409(7) . ?
C20 C30 1.514(8) . ?
C21 C34 1.401(8) . ?
C22 C34 1.391(8) . ?
C22 C25 1.551(8) . ?
C23 C49 1.511(8) . ?
C24 C40 1.385(8) . ?
C25 C55 1.523(8) . ?
C25 C44 1.524(9) . ?
C25 C31 1.567(8) . ?
C26 C49 1.522(8) . ?
C26 C45 1.534(7) . ?
C28 C29 1.391(8) . ?
C29 C32 1.367(9) . ?
C30 C37 1.528(7) . ?
C32 C36 1.440(8) . ?
C32 C35 1.515(9) . ?
C35 C48 1.521(9) . ?
C35 C46 1.540(8) . ?
C35 C54 1.550(8) . ?
C36 C37 1.384(8) . ?
C39 C59 1.461(9) . ?
C39 C66 1.501(8) . ?
C39 C62 1.508(9) . ?
C41 C58 1.420(10) . ?
C41 C47 1.534(8) . ?
C45 C57 1.512(8) . ?
C52 C56 1.413(8) . ?
C57 C64 1.524(8) . ?
C58 C60 1.518(8) . ?

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
C5 O1 C23 113.5(5) . . ?
C9 O2 C60 113.6(5) . . ?
C13 O3 C4 119.3(5) . . ?
C12 O4 C3 115.7(5) . . ?
C1 C2 C47 114.2(9) . . ?
O4 C3 C42 110.9(6) . . ?
O3 C4 C27 113.6(5) . . ?
C20 C5 C8 121.8(6) . . ?
C20 C5 O1 119.9(6) . . ?
C8 C5 O1 118.1(6) . . ?
C33 C6 C8 111.5(5) . . ?
C19 C7 C22 122.1(6) . . ?
C10 C8 C5 117.2(6) . . ?
C10 C8 C6 121.2(6) . . ?
C5 C8 C6 121.2(6) . . ?
C21 C9 C19 121.8(6) . . ?
C21 C9 O2 120.6(6) . . ?
C19 C9 O2 117.6(6) . . ?
C8 C10 C24 122.7(6) . . ?
C38 C11 C43 108.7(6) . . ?
C38 C11 C17 109.4(5) . . ?
C43 C11 C17 109.2(5) . . ?
C38 C11 C24 111.7(5) . . ?
C43 C11 C24 108.9(5) . . ?
C17 C11 C24 108.9(6) . . ?
C52 C12 C33 122.9(6) . . ?
C52 C12 O4 117.7(5) . . ?
C33 C12 O4 119.4(7) . . ?
C37 C13 O3 123.2(6) . . ?
C37 C13 C28 121.6(6) . . ?
O3 C13 C28 114.9(6) . . ?
C18 C14 C33 124.1(6) . . ?
C21 C15 C52 112.8(6) . . ?
C19 C16 C28 112.9(5) . . ?
C14 C18 C56 117.4(6) . . ?
C14 C18 C39 121.2(5) . . ?
C56 C18 C39 121.3(7) . . ?
C7 C19 C9 117.9(6) . . ?
C7 C19 C16 120.4(6) . . ?
C9 C19 C16 121.6(5) . . ?
C5 C20 C40 119.3(6) . . ?
C5 C20 C30 123.4(6) . . ?
C40 C20 C30 117.1(6) . . ?
C9 C21 C34 118.3(6) . . ?
C9 C21 C15 120.9(6) . . ?
C34 C21 C15 120.7(6) . . ?
C34 C22 C7 118.0(6) . . ?
C34 C22 C25 123.2(6) . . ?
C7 C22 C25 118.8(6) . . ?
O1 C23 C49 109.1(6) . . ?
C40 C24 C10 117.7(6) . . ?
C40 C24 C11 122.5(6) . . ?
C10 C24 C11 119.6(6) . . ?
C55 C25 C44 109.8(6) . . ?
C55 C25 C22 111.7(5) . . ?
C44 C25 C22 111.2(5) . . ?
C55 C25 C31 108.9(5) . . ?
C44 C25 C31 108.3(5) . . ?
C22 C25 C31 106.9(6) . . ?
C49 C26 C45 113.3(5) . . ?
N4 C27 C4 178.2(8) . . ?
C29 C28 C13 116.2(7) . . ?
C29 C28 C16 122.9(6) . . ?
C13 C28 C16 120.8(6) . . ?
C32 C29 C28 124.6(6) . . ?
C20 C30 C37 111.3(5) . . ?
C29 C32 C36 116.9(6) . . ?
C29 C32 C35 125.4(6) . . ?
C36 C32 C35 117.5(7) . . ?
C14 C33 C12 116.3(7) . . ?
C14 C33 C6 120.7(5) . . ?
C12 C33 C6 122.6(6) . . ?
C22 C34 C21 121.5(6) . . ?
C32 C35 C48 110.6(6) . . ?
C32 C35 C46 110.0(5) . . ?
C48 C35 C46 109.3(7) . . ?
C32 C35 C54 110.4(6) . . ?
C48 C35 C54 109.0(6) . . ?
C46 C35 C54 107.5(5) . . ?
C37 C36 C32 120.6(7) . . ?
C13 C37 C36 120.0(6) . . ?
C13 C37 C30 121.4(6) . . ?
C36 C37 C30 118.3(6) . . ?
C59 C39 C66 105.8(7) . . ?
C59 C39 C62 110.2(7) . . ?
C66 C39 C62 109.4(7) . . ?
C59 C39 C18 113.6(5) . . ?
C66 C39 C18 109.0(6) . . ?
C62 C39 C18 108.8(6) . . ?
C24 C40 C20 121.0(6) . . ?
C58 C41 C47 114.6(6) . . ?
N2 C42 C3 177.5(8) . . ?
C57 C45 C26 114.2(5) . . ?
C41 C47 C2 112.2(6) . . ?
C23 C49 C26 114.6(5) . . ?
C12 C52 C56 118.1(5) . . ?
C12 C52 C15 122.7(6) . . ?
C56 C52 C15 119.2(7) . . ?
C18 C56 C52 121.0(7) . . ?
C45 C57 C64 113.4(6) . . ?
C41 C58 C60 116.4(7) . . ?
O2 C60 C58 107.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.674
_diffrn_reflns_theta_full        23.27
_diffrn_measured_fraction_theta_full 0.674
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 1003935'
#######################################################################
#
#                 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_07srv271

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H74 N2 O4'
_chemical_formula_sum            'C56 H74 N2 O4'
_chemical_formula_weight         839.17

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.4692(15)
_cell_length_b                   15.0701(16)
_cell_length_c                   15.3241(16)
_cell_angle_alpha                91.994(2)
_cell_angle_beta                 115.710(2)
_cell_angle_gamma                109.003(2)
_cell_volume                     2592.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       colourless
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.694057
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SMART 1k'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26960
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         29.17
_reflns_number_total             13617
_reflns_number_gt                7827
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       SMART
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  X-Seed

_refine_special_details          
; 

OH hydrogens located in difference map and refined. One tBu group is disordered over two positions 
(91:9 ration). Q-peaks and thermal parameters suggest other tBu groups may also be disordered but
this was not modelled due to the small size of the residuals.

 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)+(0.0725P)²+1.0294P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13617
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1566
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.55343(13) 0.69914(10) 0.48984(10) 0.0250(3) Uani 1 1 d . . .
O2 O 0.51927(13) 0.59430(10) 0.31773(11) 0.0263(3) Uani 1 1 d . . .
O3 O 0.26722(13) 0.52381(10) 0.15355(11) 0.0290(3) Uani 1 1 d . . .
O4 O 0.32518(14) 0.67445(11) 0.30156(12) 0.0306(4) Uani 1 1 d . . .
N1 N 0.0819(2) 0.62776(18) 0.5913(2) 0.0600(7) Uani 1 1 d . . .
N2 N -0.0991(3) 0.13613(19) 0.1019(2) 0.0689(8) Uani 1 1 d . . .
C1 C 0.60636(18) 0.78585(14) 0.46833(14) 0.0223(4) Uani 1 1 d . . .
C2 C 0.70810(17) 0.79939(14) 0.45854(14) 0.0220(4) Uani 1 1 d . . .
C3 C 0.75724(18) 0.88282(14) 0.43108(14) 0.0242(4) Uani 1 1 d . . .
H3 H 0.8266 0.8926 0.4243 0.029 Uiso 1 1 calc R . .
C4 C 0.70772(18) 0.95264(14) 0.41322(15) 0.0248(4) Uani 1 1 d . . .
C5 C 0.60480(18) 0.93489(14) 0.42226(14) 0.0241(4) Uani 1 1 d . . .
H5 H 0.5690 0.9811 0.4096 0.029 Uiso 1 1 calc R . .
C6 C 0.55218(18) 0.85198(14) 0.44910(14) 0.0222(4) Uani 1 1 d . . .
C7 C 0.43394(18) 0.83328(15) 0.44981(15) 0.0254(4) Uani 1 1 d . . .
H7A H 0.4088 0.7716 0.4700 0.030 Uiso 1 1 calc R . .
H7B H 0.4439 0.8849 0.4982 0.030 Uiso 1 1 calc R . .
C8 C 0.33992(18) 0.82983(15) 0.34776(15) 0.0251(4) Uani 1 1 d . . .
C9 C 0.3038(2) 0.90568(16) 0.32580(16) 0.0312(5) Uani 1 1 d . . .
H9 H 0.3340 0.9588 0.3777 0.037 Uiso 1 1 calc R . .
C10 C 0.2246(2) 0.90725(17) 0.23001(17) 0.0343(5) Uani 1 1 d . . .
C11 C 0.1854(2) 0.82908(17) 0.15572(16) 0.0324(5) Uani 1 1 d . . .
H11 H 0.1348 0.8297 0.0894 0.039 Uiso 1 1 calc R . .
C12 C 0.21774(18) 0.75001(16) 0.17493(15) 0.0274(5) Uani 1 1 d . . .
C13 C 0.29283(18) 0.74943(15) 0.27236(15) 0.0254(4) Uani 1 1 d . . .
C14 C 0.17140(18) 0.66735(16) 0.09061(16) 0.0296(5) Uani 1 1 d . . .
H14A H 0.1112 0.6773 0.0299 0.036 Uiso 1 1 calc R . .
H14B H 0.1312 0.6072 0.1063 0.036 Uiso 1 1 calc R . .
C15 C 0.26802(18) 0.65581(15) 0.07011(15) 0.0266(5) Uani 1 1 d . . .
C16 C 0.31765(19) 0.71921(15) 0.02248(15) 0.0283(5) Uani 1 1 d . . .
H16 H 0.2879 0.7679 0.0008 0.034 Uiso 1 1 calc R . .
C17 C 0.40909(19) 0.71357(15) 0.00577(15) 0.0274(5) Uani 1 1 d . . .
C18 C 0.45214(19) 0.64226(14) 0.04103(15) 0.0263(4) Uani 1 1 d . . .
H18 H 0.5155 0.6376 0.0314 0.032 Uiso 1 1 calc R . .
C19 C 0.40650(18) 0.57816(14) 0.08941(14) 0.0238(4) Uani 1 1 d . . .
C20 C 0.31250(18) 0.58469(14) 0.10183(15) 0.0248(4) Uani 1 1 d . . .
C21 C 0.46522(19) 0.50822(14) 0.13418(15) 0.0264(4) Uani 1 1 d . . .
H21A H 0.4205 0.4668 0.1642 0.032 Uiso 1 1 calc R . .
H21B H 0.4631 0.4666 0.0814 0.032 Uiso 1 1 calc R . .
C22 C 0.59270(18) 0.56207(14) 0.21213(15) 0.0248(4) Uani 1 1 d . . .
C23 C 0.61634(18) 0.60921(14) 0.30367(15) 0.0230(4) Uani 1 1 d . . .
C24 C 0.73293(18) 0.66701(14) 0.37338(15) 0.0236(4) Uani 1 1 d . . .
C25 C 0.82445(19) 0.67524(15) 0.35040(16) 0.0281(5) Uani 1 1 d . . .
H25 H 0.9038 0.7141 0.3978 0.034 Uiso 1 1 calc R . .
C26 C 0.8044(2) 0.62883(16) 0.26077(16) 0.0306(5) Uani 1 1 d . . .
C27 C 0.6868(2) 0.57219(15) 0.19309(16) 0.0287(5) Uani 1 1 d . . .
H27 H 0.6707 0.5393 0.1315 0.034 Uiso 1 1 calc R . .
C28 C 0.76063(18) 0.72244(14) 0.47137(15) 0.0237(4) Uani 1 1 d . . .
H28A H 0.8481 0.7529 0.5129 0.028 Uiso 1 1 calc R . .
H28B H 0.7288 0.6770 0.5066 0.028 Uiso 1 1 calc R . .
C29 C 0.7618(2) 1.04185(15) 0.37948(17) 0.0312(5) Uani 1 1 d . . .
C30 C 0.7386(3) 1.0100(2) 0.2736(2) 0.0544(10) Uani 0.911(4) 1 d P A 1
H30A H 0.7722 1.0661 0.2502 0.082 Uiso 0.911(4) 1 calc PR A 1
H30B H 0.6527 0.9794 0.2297 0.082 Uiso 0.911(4) 1 calc PR A 1
H30C H 0.7762 0.9642 0.2734 0.082 Uiso 0.911(4) 1 calc PR A 1
C31 C 0.8952(3) 1.0891(2) 0.4467(2) 0.0506(9) Uani 0.911(4) 1 d P A 1
H31A H 0.9110 1.1042 0.5153 0.076 Uiso 0.911(4) 1 calc PR A 1
H31B H 0.9273 1.1483 0.4267 0.076 Uiso 0.911(4) 1 calc PR A 1
H31C H 0.9333 1.0453 0.4414 0.076 Uiso 0.911(4) 1 calc PR A 1
C32 C 0.7064(3) 1.1162(2) 0.3773(3) 0.0591(11) Uani 0.911(4) 1 d P A 1
H32A H 0.7173 1.1359 0.4435 0.089 Uiso 0.911(4) 1 calc PR A 1
H32B H 0.6212 1.0881 0.3303 0.089 Uiso 0.911(4) 1 calc PR A 1
H32C H 0.7453 1.1723 0.3568 0.089 Uiso 0.911(4) 1 calc PR A 1
C33 C 0.1885(3) 0.9938(2) 0.20908(19) 0.0524(8) Uani 1 1 d . . .
C34 C 0.0818(5) 0.9715(3) 0.1085(2) 0.123(2) Uani 1 1 d . . .
H34A H 0.1017 0.9558 0.0571 0.185 Uiso 1 1 calc R . .
H34B H 0.0594 1.0274 0.0985 0.185 Uiso 1 1 calc R . .
H34C H 0.0150 0.9167 0.1046 0.185 Uiso 1 1 calc R . .
C35 C 0.1591(3) 1.0261(3) 0.2870(2) 0.0684(10) Uani 1 1 d . . .
H35A H 0.1358 1.0811 0.2717 0.103 Uiso 1 1 calc R . .
H35B H 0.2292 1.0446 0.3523 0.103 Uiso 1 1 calc R . .
H35C H 0.0933 0.9733 0.2871 0.103 Uiso 1 1 calc R . .
C36 C 0.2985(5) 1.0775(3) 0.2166(3) 0.0992(15) Uani 1 1 d . . .
H36A H 0.3186 1.0595 0.1661 0.149 Uiso 1 1 calc R . .
H36B H 0.3663 1.0905 0.2824 0.149 Uiso 1 1 calc R . .
H36C H 0.2798 1.1351 0.2060 0.149 Uiso 1 1 calc R . .
C37 C 0.4636(2) 0.78120(16) -0.04836(17) 0.0340(5) Uani 1 1 d . . .
C38 C 0.6002(3) 0.8233(3) 0.0117(3) 0.0756(11) Uani 1 1 d . . .
H38A H 0.6334 0.8699 -0.0211 0.113 Uiso 1 1 calc R . .
H38B H 0.6302 0.7716 0.0161 0.113 Uiso 1 1 calc R . .
H38C H 0.6241 0.8553 0.0785 0.113 Uiso 1 1 calc R . .
C39 C 0.4261(3) 0.7261(2) -0.1489(2) 0.0641(9) Uani 1 1 d . . .
H39A H 0.3392 0.7012 -0.1878 0.096 Uiso 1 1 calc R . .
H39B H 0.4533 0.6725 -0.1408 0.096 Uiso 1 1 calc R . .
H39C H 0.4616 0.7688 -0.1832 0.096 Uiso 1 1 calc R . .
C40 C 0.4248(3) 0.8664(2) -0.0623(3) 0.0701(10) Uani 1 1 d . . .
H40A H 0.3383 0.8433 -0.1037 0.105 Uiso 1 1 calc R . .
H40B H 0.4641 0.9088 -0.0945 0.105 Uiso 1 1 calc R . .
H40C H 0.4470 0.9020 0.0024 0.105 Uiso 1 1 calc R . .
C41 C 0.9038(2) 0.6429(2) 0.23256(18) 0.0411(6) Uani 1 1 d . . .
C42 C 1.0266(2) 0.7015(3) 0.3187(2) 0.0723(11) Uani 1 1 d . . .
H42A H 1.0292 0.7645 0.3403 0.108 Uiso 1 1 calc R . .
H42B H 1.0873 0.7097 0.2972 0.108 Uiso 1 1 calc R . .
H42C H 1.0423 0.6677 0.3737 0.108 Uiso 1 1 calc R . .
C43 C 0.8832(3) 0.7000(2) 0.1486(2) 0.0578(8) Uani 1 1 d . . .
H43A H 0.8045 0.6647 0.0921 0.087 Uiso 1 1 calc R . .
H43B H 0.9446 0.7086 0.1281 0.087 Uiso 1 1 calc R . .
H43C H 0.8874 0.7630 0.1726 0.087 Uiso 1 1 calc R . .
C44 C 0.9000(3) 0.5468(2) 0.1945(3) 0.0650(9) Uani 1 1 d . . .
H44A H 0.9154 0.5105 0.2475 0.098 Uiso 1 1 calc R . .
H44B H 0.9608 0.5573 0.1729 0.098 Uiso 1 1 calc R . .
H44C H 0.8212 0.5105 0.1385 0.098 Uiso 1 1 calc R . .
C45 C 0.5851(2) 0.70270(15) 0.59295(15) 0.0277(5) Uani 1 1 d . . .
H45A H 0.5573 0.7476 0.6157 0.033 Uiso 1 1 calc R . .
H45B H 0.6725 0.7249 0.6336 0.033 Uiso 1 1 calc R . .
C46 C 0.5255(2) 0.60229(16) 0.60257(17) 0.0316(5) Uani 1 1 d . . .
H46A H 0.5476 0.6023 0.6732 0.038 Uiso 1 1 calc R . .
H46B H 0.5562 0.5592 0.5811 0.038 Uiso 1 1 calc R . .
C47 C 0.3901(2) 0.56222(16) 0.54237(17) 0.0307(5) Uani 1 1 d . . .
H47A H 0.3678 0.5753 0.4749 0.037 Uiso 1 1 calc R . .
H47B H 0.3599 0.4917 0.5361 0.037 Uiso 1 1 calc R . .
C48 C 0.3296(2) 0.60397(16) 0.58726(17) 0.0332(5) Uani 1 1 d . . .
H48A H 0.3543 0.5940 0.6559 0.040 Uiso 1 1 calc R . .
H48B H 0.3548 0.6738 0.5895 0.040 Uiso 1 1 calc R . .
C49 C 0.1952(2) 0.55625(19) 0.5264(2) 0.0446(6) Uani 1 1 d . . .
H49A H 0.1719 0.5640 0.4572 0.054 Uiso 1 1 calc R . .
H49B H 0.1709 0.4867 0.5261 0.054 Uiso 1 1 calc R . .
C50 C 0.1310(2) 0.59561(19) 0.5637(2) 0.0456(6) Uani 1 1 d . . .
C51 C 0.1754(2) 0.43308(16) 0.09228(17) 0.0380(6) Uani 1 1 d . . .
H51A H 0.2032 0.4030 0.0537 0.046 Uiso 1 1 calc R . .
H51B H 0.1033 0.4430 0.0453 0.046 Uiso 1 1 calc R . .
C52 C 0.1470(2) 0.36895(17) 0.15865(19) 0.0393(6) Uani 1 1 d . . .
H52A H 0.0856 0.3058 0.1176 0.047 Uiso 1 1 calc R . .
H52B H 0.2195 0.3586 0.2042 0.047 Uiso 1 1 calc R . .
C53 C 0.1031(3) 0.4104(2) 0.2180(2) 0.0505(7) Uani 1 1 d . . .
H53A H 0.0321 0.4223 0.1719 0.061 Uiso 1 1 calc R . .
H53B H 0.1654 0.4731 0.2593 0.061 Uiso 1 1 calc R . .
C54 C 0.0703(3) 0.3481(2) 0.28549(19) 0.0517(7) Uani 1 1 d . . .
H54A H 0.0805 0.3902 0.3423 0.062 Uiso 1 1 calc R . .
H54B H 0.1261 0.3147 0.3119 0.062 Uiso 1 1 calc R . .
C55 C -0.0572(3) 0.2735(2) 0.2336(2) 0.0558(8) Uani 1 1 d . . .
H55A H -0.0769 0.2459 0.2844 0.067 Uiso 1 1 calc R . .
H55B H -0.1120 0.3063 0.2002 0.067 Uiso 1 1 calc R . .
C56 C -0.0784(2) 0.19544(19) 0.1608(2) 0.0429(6) Uani 1 1 d . . .
H2O H 0.533(2) 0.6223(18) 0.3705(19) 0.036(7) Uiso 1 1 d . . .
H4O H 0.305(3) 0.633(2) 0.255(2) 0.049(8) Uiso 1 1 d . . .
C31' C 0.874(3) 1.034(3) 0.357(3) 0.060(10) Uiso 0.089(4) 1 d P A 2
H31D H 0.8418 0.9758 0.3063 0.089 Uiso 0.089(4) 1 calc PR A 2
H31E H 0.9378 1.0298 0.4180 0.089 Uiso 0.089(4) 1 calc PR A 2
H31F H 0.9052 1.0903 0.3332 0.089 Uiso 0.089(4) 1 calc PR A 2
C32' C 0.843(4) 1.125(3) 0.478(3) 0.071(12) Uiso 0.089(4) 1 d P A 2
H32D H 0.8949 1.1796 0.4660 0.106 Uiso 0.089(4) 1 calc PR A 2
H32E H 0.8913 1.0999 0.5321 0.106 Uiso 0.089(4) 1 calc PR A 2
H32F H 0.7914 1.1451 0.4970 0.106 Uiso 0.089(4) 1 calc PR A 2
C30' C 0.686(4) 1.062(3) 0.298(3) 0.071(12) Uiso 0.089(4) 1 d P A 2
H30D H 0.7095 1.1316 0.3051 0.106 Uiso 0.089(4) 1 calc PR A 2
H30E H 0.6050 1.0335 0.2904 0.106 Uiso 0.089(4) 1 calc PR A 2
H30F H 0.6874 1.0351 0.2398 0.106 Uiso 0.089(4) 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
O1 C1 1.397(2) . ?
O1 C45 1.441(2) . ?
O2 C23 1.365(2) . ?
O3 C20 1.396(3) . ?
O3 C51 1.443(2) . ?
O4 C13 1.361(3) . ?
N1 C50 1.134(3) . ?
N2 C56 1.120(3) . ?
C1 C6 1.386(3) . ?
C1 C2 1.393(3) . ?
C2 C3 1.390(3) . ?
C2 C28 1.521(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.393(3) . ?
C4 C29 1.531(3) . ?
C5 C6 1.394(3) . ?
C6 C7 1.529(3) . ?
C7 C8 1.512(3) . ?
C8 C9 1.379(3) . ?
C8 C13 1.404(3) . ?
C9 C10 1.398(3) . ?
C10 C11 1.394(3) . ?
C10 C33 1.532(3) . ?
C11 C12 1.395(3) . ?
C12 C13 1.396(3) . ?
C12 C14 1.514(3) . ?
C14 C15 1.523(3) . ?
C15 C20 1.395(3) . ?
C15 C16 1.396(3) . ?
C16 C17 1.389(3) . ?
C17 C18 1.399(3) . ?
C17 C37 1.538(3) . ?
C18 C19 1.385(3) . ?
C19 C20 1.392(3) . ?
C19 C21 1.526(3) . ?
C21 C22 1.510(3) . ?
C22 C27 1.383(3) . ?
C22 C23 1.404(3) . ?
C23 C24 1.398(3) . ?
C24 C25 1.392(3) . ?
C24 C28 1.522(3) . ?
C25 C26 1.392(3) . ?
C26 C27 1.395(3) . ?
C26 C41 1.532(3) . ?
C29 C30' 1.35(4) . ?
C29 C31 1.518(4) . ?
C29 C32 1.530(4) . ?
C29 C30 1.539(4) . ?
C29 C32' 1.61(4) . ?
C29 C31' 1.73(3) . ?
C33 C34 1.511(4) . ?
C33 C35 1.521(4) . ?
C33 C36 1.557(5) . ?
C37 C39 1.510(4) . ?
C37 C40 1.526(4) . ?
C37 C38 1.538(4) . ?
C41 C44 1.520(4) . ?
C41 C42 1.526(4) . ?
C41 C43 1.547(4) . ?
C45 C46 1.511(3) . ?
C46 C47 1.525(3) . ?
C47 C48 1.524(3) . ?
C48 C49 1.518(3) . ?
C49 C50 1.472(3) . ?
C51 C52 1.510(3) . ?
C52 C53 1.495(3) . ?
C53 C54 1.529(4) . ?
C54 C55 1.530(4) . ?
C55 C56 1.457(4) . ?

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 C45 114.66(15) . . ?
C20 O3 C51 113.65(16) . . ?
C6 C1 C2 121.68(18) . . ?
C6 C1 O1 120.07(18) . . ?
C2 C1 O1 118.02(17) . . ?
C3 C2 C1 118.52(18) . . ?
C3 C2 C28 120.24(18) . . ?
C1 C2 C28 121.14(18) . . ?
C2 C3 C4 121.98(19) . . ?
C5 C4 C3 117.26(19) . . ?
C5 C4 C29 122.23(19) . . ?
C3 C4 C29 120.43(19) . . ?
C4 C5 C6 122.64(18) . . ?
C1 C6 C5 117.88(18) . . ?
C1 C6 C7 122.06(18) . . ?
C5 C6 C7 119.93(18) . . ?
C8 C7 C6 109.76(16) . . ?
C9 C8 C13 119.30(19) . . ?
C9 C8 C7 121.59(19) . . ?
C13 C8 C7 119.02(18) . . ?
C8 C9 C10 122.4(2) . . ?
C11 C10 C9 116.8(2) . . ?
C11 C10 C33 122.7(2) . . ?
C9 C10 C33 120.5(2) . . ?
C10 C11 C12 122.6(2) . . ?
C13 C12 C11 118.67(19) . . ?
C13 C12 C14 121.54(19) . . ?
C11 C12 C14 119.79(19) . . ?
O4 C13 C12 124.35(19) . . ?
O4 C13 C8 115.70(18) . . ?
C12 C13 C8 119.95(19) . . ?
C12 C14 C15 113.66(17) . . ?
C20 C15 C16 118.40(19) . . ?
C20 C15 C14 121.2(2) . . ?
C16 C15 C14 120.37(19) . . ?
C17 C16 C15 122.2(2) . . ?
C16 C17 C18 117.0(2) . . ?
C16 C17 C37 123.31(19) . . ?
C18 C17 C37 119.70(19) . . ?
C19 C18 C17 122.9(2) . . ?
C18 C19 C20 118.08(19) . . ?
C18 C19 C21 120.00(18) . . ?
C20 C19 C21 121.75(19) . . ?
C19 C20 C15 121.3(2) . . ?
C19 C20 O3 119.72(18) . . ?
C15 C20 O3 118.77(18) . . ?
C22 C21 C19 110.47(16) . . ?
C27 C22 C23 118.89(19) . . ?
C27 C22 C21 121.59(19) . . ?
C23 C22 C21 119.35(18) . . ?
O2 C23 C24 124.18(18) . . ?
O2 C23 C22 115.47(18) . . ?
C24 C23 C22 120.35(19) . . ?
C25 C24 C23 118.51(19) . . ?
C25 C24 C28 119.95(19) . . ?
C23 C24 C28 121.51(18) . . ?
C26 C25 C24 122.7(2) . . ?
C25 C26 C27 117.0(2) . . ?
C25 C26 C41 122.8(2) . . ?
C27 C26 C41 120.1(2) . . ?
C22 C27 C26 122.6(2) . . ?
C24 C28 C2 112.86(16) . . ?
C30' C29 C31 133.2(18) . . ?
C30' C29 C4 116.1(18) . . ?
C31 C29 C4 110.68(19) . . ?
C30' C29 C32 53.6(18) . . ?
C31 C29 C32 108.5(2) . . ?
C4 C29 C32 112.8(2) . . ?
C30' C29 C30 55.5(18) . . ?
C31 C29 C30 109.0(2) . . ?
C4 C29 C30 107.96(19) . . ?
C32 C29 C30 107.8(2) . . ?
C30' C29 C32' 118(2) . . ?
C31 C29 C32' 46.7(15) . . ?
C4 C29 C32' 104.9(15) . . ?
C32 C29 C32' 68.8(15) . . ?
C30 C29 C32' 145.1(16) . . ?
C30' C29 C31' 107(2) . . ?
C31 C29 C31' 52.5(12) . . ?
C4 C29 C31' 110.9(12) . . ?
C32 C29 C31' 136.3(12) . . ?
C30 C29 C31' 58.8(12) . . ?
C32' C29 C31' 99(2) . . ?
C34 C33 C35 108.6(3) . . ?
C34 C33 C10 111.6(2) . . ?
C35 C33 C10 111.1(2) . . ?
C34 C33 C36 111.1(3) . . ?
C35 C33 C36 107.4(3) . . ?
C10 C33 C36 107.0(3) . . ?
C39 C37 C40 108.7(2) . . ?
C39 C37 C38 109.7(3) . . ?
C40 C37 C38 106.4(2) . . ?
C39 C37 C17 109.3(2) . . ?
C40 C37 C17 112.4(2) . . ?
C38 C37 C17 110.4(2) . . ?
C44 C41 C42 110.3(2) . . ?
C44 C41 C26 110.7(2) . . ?
C42 C41 C26 112.1(2) . . ?
C44 C41 C43 108.5(2) . . ?
C42 C41 C43 107.2(3) . . ?
C26 C41 C43 107.9(2) . . ?
O1 C45 C46 107.09(17) . . ?
C45 C46 C47 113.95(18) . . ?
C48 C47 C46 113.77(19) . . ?
C49 C48 C47 110.46(19) . . ?
C50 C49 C48 113.4(2) . . ?
N1 C50 C49 178.3(3) . . ?
O3 C51 C52 108.37(19) . . ?
C53 C52 C51 112.4(2) . . ?
C52 C53 C54 115.2(2) . . ?
C53 C54 C55 113.6(2) . . ?
C56 C55 C54 114.8(2) . . ?
N2 C56 C55 176.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        29.17
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.051
_database_code_depnum_ccdc_archive 'CCDC 1003936'
