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

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_c1emimac

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C32 H32 O12, 2(C6 H11 N2), O4 S, 2(C3 H6 O), 2(H2 O)'
_chemical_formula_sum            'C50 H70 N4 O20 S'
_chemical_formula_weight         1079.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0076 0.0040
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
S S 0.1431 0.1480
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.328(5)
_cell_length_b                   16.545(7)
_cell_length_c                   12.821(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.190(5)
_cell_angle_gamma                90
_cell_volume                     2469.7(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5691
_cell_measurement_theta_min      26.67
_cell_measurement_theta_max      2.34

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    0.186
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28634
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.332
_diffrn_reflns_theta_max         30.325
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5696
_reflns_number_gt                4277
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrgrogen on
 the hydroxyl groups were found in the difference map and then
 constrained and refined using a riding model, the water hydrogen
 atoms were found in the difference map and allow to refine freely.
 Extensive geometrical and displacement parameter restrains were use
 in the modelling of the disorder cation and actone 
;
_vrf_PLAT417_c1emimac            
;
PROBLEM: Short Inter D-H..H-D       H2W    ..  H5      ..       2.05 Ang.  
RESPONSE: H5 points at the H2W oxygen while H2W point at symmetry related
 version of O7. H5 and H2w do not point at each other.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1350P)²+1.2378P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5696
_refine_ls_number_parameters     419
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.2194
_refine_ls_wR_factor_gt          0.2000
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.029
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.5000 0.49024(5) 0.7500 0.0284(2) Uani 1 2 d S T P . .
O1 O 1.06476(18) 0.69771(15) 1.16564(15) 0.0502(6) Uani 1 1 d . . . . .
H1 H 1.1273 0.6904 1.1542 0.060 Uiso 1 1 calc R U . . .
N1 N 0.9295(2) 0.55511(14) 0.7823(2) 0.0445(6) Uani 1 1 d D . . . .
C1 C 0.9235(2) 0.81629(13) 0.91623(18) 0.0270(5) Uani 1 1 d . . . . .
H9 H 0.9406 0.8571 0.8718 0.032 Uiso 1 1 calc R U . . .
O2 O 0.85426(18) 0.63725(13) 1.10808(15) 0.0483(5) Uani 1 1 d . . . . .
H2 H 0.7897 0.6162 1.0766 0.058 Uiso 1 1 calc R U . . .
C2 C 1.0117(2) 0.78860(14) 1.00820(18) 0.0279(5) Uani 1 1 d . . . . .
O3 O 0.68218(16) 0.68929(12) 0.92861(15) 0.0392(5) Uani 1 1 d . . . . .
H3 H 0.6477 0.6886 0.8602 0.047 Uiso 1 1 calc R U . . .
C3 C 0.9845(2) 0.72792(15) 1.07124(18) 0.0341(6) Uani 1 1 d . . . . .
O4 O 0.59981(16) 0.67808(11) 0.69826(15) 0.0362(4) Uani 1 1 d . . . . .
H4 H 0.5670 0.6364 0.6654 0.043 Uiso 1 1 calc R U . . .
C4 C 0.8739(2) 0.69655(15) 1.0424(2) 0.0334(5) Uani 1 1 d . . . . .
O5 O 0.59858(17) 0.61255(11) 0.49662(15) 0.0388(5) Uani 1 1 d . . . . .
H5 H 0.6330 0.5694 0.5220 0.047 Uiso 1 1 calc R U . . .
C5 C 0.7884(2) 0.72500(14) 0.94985(19) 0.0293(5) Uani 1 1 d . . . . .
O6 O 0.73594(17) 0.67872(11) 0.38888(14) 0.0391(5) Uani 1 1 d . . . . .
H6 H 0.6877 0.6410 0.3710 0.047 Uiso 1 1 calc R U . . .
C6 C 0.8114(2) 0.78711(13) 0.88615(18) 0.0273(5) Uani 1 1 d . . . . .
O7 O 0.52292(16) 0.54060(10) 0.84877(15) 0.0371(4) Uani 1 1 d . . . . .
C7 C 0.7165(2) 0.82046(13) 0.78621(19) 0.0277(5) Uani 1 1 d . . . . .
H7 H 0.6416 0.8029 0.7932 0.033 Uiso 1 1 calc R U . . .
O8 O 0.60041(15) 0.43787(11) 0.75872(16) 0.0388(4) Uani 1 1 d . . . . .
C8 C 0.7901(2) 0.81701(13) 0.62215(18) 0.0257(5) Uani 1 1 d . . . . .
H8 H 0.8324 0.8648 0.6500 0.031 Uiso 1 1 calc R U . . .
O1W O 0.66177(17) 0.45533(13) 0.56785(19) 0.0402(5) Uani 1 1 d . . . . .
H1W H 0.637(6) 0.429(4) 0.607(5) 0.14(3) Uiso 1 1 d . . . . .
H2W H 0.611(4) 0.447(3) 0.499(4) 0.088(14) Uiso 1 1 d . . . . .
C9 C 0.72446(19) 0.78329(13) 0.68043(18) 0.0253(5) Uani 1 1 d . . . . .
O10 O 1.0000 0.97503(16) 0.7500 0.0437(7) Uani 1 2 d DS T P . .
C10 C 0.6639(2) 0.71222(14) 0.63991(19) 0.0288(5) Uani 1 1 d . . . . .
C11 C 0.6679(2) 0.67745(14) 0.5427(2) 0.0303(5) Uani 1 1 d . . . . .
C12 C 0.7343(2) 0.71302(14) 0.48632(19) 0.0315(5) Uani 1 1 d . . . . .
C13 C 0.7968(2) 0.78384(13) 0.52462(18) 0.0266(5) Uani 1 1 d . . . . .
C14 C 0.8668(2) 0.82290(14) 0.45995(18) 0.0295(5) Uani 1 1 d . . . . .
H14 H 0.8278 0.8091 0.3804 0.035 Uiso 1 1 calc R U . . .
C15 C 0.7158(2) 0.91306(14) 0.7833(2) 0.0355(6) Uani 1 1 d . . . . .
H15A H 0.7896 0.9326 0.7799 0.053 Uiso 1 1 calc R U . . .
H15B H 0.7036 0.9340 0.8501 0.053 Uiso 1 1 calc R U . . .
H15C H 0.6538 0.9318 0.7180 0.053 Uiso 1 1 calc R U . . .
C16 C 0.8670(2) 0.91596(15) 0.4686(2) 0.0344(5) Uani 1 1 d . . . . .
H16A H 0.7876 0.9358 0.4441 0.052 Uiso 1 1 calc R U . . .
H16B H 0.9079 0.9391 0.4218 0.052 Uiso 1 1 calc R U . . .
H16C H 0.9054 0.9321 0.5455 0.052 Uiso 1 1 calc R U . . .
C17 C 1.0000 0.5094(2) 0.7500 0.0483(10) Uani 1 2 d DS T P A .
H17 H 1.0000 0.4520 0.7500 0.058 Uiso 1 2 calc R U P . .
C18 C 0.9561(3) 0.63391(19) 0.7704(4) 0.0678(11) Uani 1 1 d D . . . .
H18 H 0.9195 0.6801 0.7877 0.081 Uiso 1 1 calc R U . . .
C19 C 0.8393(3) 0.5270(3) 0.8245(4) 0.0719(11) Uani 0.5 1 d D . P A 1
H19A H 0.7966 0.4817 0.7786 0.086 Uiso 0.5 1 calc R U P A 1
H19B H 0.7845 0.5713 0.8215 0.086 Uiso 0.5 1 calc R U P A 1
C20 C 0.8932(9) 0.4998(5) 0.9396(6) 0.075(2) Uani 0.5 1 d D . P A 1
H20A H 0.9421 0.4528 0.9411 0.112 Uiso 0.5 1 calc R U P A 1
H20B H 0.8333 0.4849 0.9708 0.112 Uiso 0.5 1 calc R U P A 1
H20C H 0.9399 0.5437 0.9833 0.112 Uiso 0.5 1 calc R U P A 1
C19A C 0.8393(3) 0.5270(3) 0.8245(4) 0.0719(11) Uani 0.5 1 d . . P A 2
H19C H 0.8577 0.5435 0.9018 0.108 Uiso 0.5 1 calc R U P A 2
H19D H 0.8342 0.4679 0.8195 0.108 Uiso 0.5 1 calc R U P A 2
H19E H 0.7656 0.5506 0.7805 0.108 Uiso 0.5 1 calc R U P A 2
C21 C 1.0000 1.0483(2) 0.7500 0.0372(8) Uani 1 2 d DS T P . .
C22 C 1.1050(3) 1.09523(19) 0.8108(3) 0.0496(8) Uani 1 1 d D . . . .
H22A H 1.1000 1.1130 0.8820 0.074 Uiso 1 1 calc R U . . .
H22B H 1.1111 1.1425 0.7670 0.074 Uiso 1 1 calc R U . . .
H22C H 1.1730 1.0610 0.8233 0.074 Uiso 1 1 calc R U . . .
N2 N 0.5320(10) 0.7947(6) 0.1828(11) 0.149(4) Uani 0.5 1 d D U P B -1
C23 C 0.5010(14) 0.7567(6) 0.2615(14) 0.150(3) Uani 0.5 1 d D U P B -1
H23 H 0.5261 0.7038 0.2867 0.181 Uiso 0.5 1 calc R U P B -1
N3 N 0.4309(11) 0.8008(8) 0.3013(12) 0.169(4) Uani 0.5 1 d D U P B -1
C25 C 0.4792(12) 0.8703(7) 0.1679(13) 0.173(4) Uani 0.5 1 d D U P B -1
H25 H 0.4842 0.9115 0.1181 0.207 Uiso 0.5 1 calc R U P B -1
C24 C 0.4176(11) 0.8726(8) 0.2411(13) 0.177(4) Uani 0.5 1 d D U P B -1
H24 H 0.3723 0.9171 0.2491 0.212 Uiso 0.5 1 calc R U P B -1
C26 C 0.6016(14) 0.7798(11) 0.1127(15) 0.158(5) Uani 0.5 1 d D U P B -1
H26A H 0.5765 0.7302 0.0680 0.190 Uiso 0.5 1 calc R U P B -1
H26B H 0.6840 0.7748 0.1569 0.190 Uiso 0.5 1 calc R U P B -1
C27 C 0.580(2) 0.8529(11) 0.0419(18) 0.191(8) Uani 0.5 1 d D U P B -1
H27A H 0.6099 0.8445 -0.0192 0.287 Uiso 0.5 1 calc R U P B -1
H27B H 0.6183 0.8995 0.0859 0.287 Uiso 0.5 1 calc R U P B -1
H27C H 0.4970 0.8631 0.0123 0.287 Uiso 0.5 1 calc R U P B -1
C28 C 0.4077(15) 0.7570(15) 0.3763(17) 0.166(6) Uani 0.5 1 d . U P B -1
H28A H 0.3619 0.7099 0.3412 0.250 Uiso 0.5 1 calc R U P B -1
H28B H 0.3642 0.7895 0.4128 0.250 Uiso 0.5 1 calc R U P B -1
H28C H 0.4795 0.7387 0.4312 0.250 Uiso 0.5 1 calc R U P B -1
C30 C 0.4660(9) 0.9138(12) 0.4696(10) 0.216(7) Uani 0.5 1 d D U P C -1
O11 O 0.4516(17) 0.8464(12) 0.4986(18) 0.259(8) Uani 0.5 1 d D U P C -1
C29 C 0.4090(17) 0.9778(12) 0.5129(18) 0.217(8) Uani 0.5 1 d D U P C -1
H29A H 0.4315 0.9729 0.5934 0.325 Uiso 0.5 1 calc R U P C -1
H29B H 0.3255 0.9720 0.4804 0.325 Uiso 0.5 1 calc R U P C -1
H29C H 0.4322 1.0309 0.4937 0.325 Uiso 0.5 1 calc R U P C -1
C31 C 0.5373(15) 0.9191(12) 0.3972(16) 0.184(7) Uani 0.5 1 d D U P C -1
H31A H 0.5385 0.8665 0.3626 0.276 Uiso 0.5 1 calc R U P C -1
H31B H 0.6157 0.9346 0.4412 0.276 Uiso 0.5 1 calc R U P C -1
H31C H 0.5049 0.9598 0.3399 0.276 Uiso 0.5 1 calc R U P C -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O7 1.4637(18) . ?
S1 O7 1.4637(18) 2_656 ?
S1 O8 1.4848(18) . ?
S1 O8 1.4848(18) 2_656 ?
O1 C3 1.381(3) . ?
O1 H1 0.8400 . ?
N1 C17 1.317(3) . ?
N1 C18 1.365(4) . ?
N1 C19 1.463(4) . ?
C1 C2 1.393(3) . ?
C1 C6 1.394(3) . ?
C1 H9 0.9500 . ?
O2 C4 1.366(3) . ?
O2 H2 0.8400 . ?
C2 C3 1.397(3) . ?
C2 C14 1.526(3) 2_756 ?
O3 C5 1.379(3) . ?
O3 H3 0.8400 . ?
C3 C4 1.390(4) . ?
O4 C10 1.375(3) . ?
O4 H4 0.8400 . ?
C4 C5 1.385(4) . ?
O5 C11 1.378(3) . ?
O5 H5 0.8400 . ?
C5 C6 1.399(3) . ?
O6 C12 1.378(3) . ?
O6 H6 0.8400 . ?
C6 C7 1.526(3) . ?
C7 C9 1.521(3) . ?
C7 C15 1.532(3) . ?
C7 H7 1.0000 . ?
C8 C9 1.387(3) . ?
C8 C13 1.392(3) . ?
C8 H8 0.9500 . ?
O1W H1W 0.80(7) . ?
O1W H2W 0.91(5) . ?
C9 C10 1.398(3) . ?
O10 C21 1.212(4) . ?
C10 C11 1.389(3) . ?
C11 C12 1.388(4) . ?
C12 C13 1.399(3) . ?
C13 C14 1.524(3) . ?
C14 C2 1.526(3) 2_756 ?
C14 C16 1.544(3) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N1 1.317(3) 2_756 ?
C17 H17 0.9500 . ?
C18 C18 1.349(7) 2_756 ?
C18 H18 0.9500 . ?
C19 C20 1.475(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.491(4) 2_756 ?
C21 C22 1.491(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N2 C23 1.346(8) . ?
N2 C25 1.394(9) . ?
N2 C26 1.453(11) . ?
C23 N3 1.352(9) . ?
C23 H23 0.9500 . ?
N3 C28 1.31(2) . ?
N3 C24 1.397(9) . ?
C25 C24 1.388(11) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C26 C27 1.483(13) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 O11 1.207(10) . ?
C30 C31 1.475(9) . ?
C30 C29 1.476(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
O7 S1 O7 110.61(15) . 2_656 ?
O7 S1 O8 110.36(10) . . ?
O7 S1 O8 108.45(11) 2_656 . ?
O7 S1 O8 108.44(11) . 2_656 ?
O7 S1 O8 110.36(10) 2_656 2_656 ?
O8 S1 O8 108.59(16) . 2_656 ?
C3 O1 H1 109.5 . . ?
C17 N1 C18 107.8(3) . . ?
C17 N1 C19 126.4(3) . . ?
C18 N1 C19 125.8(3) . . ?
C2 C1 C6 123.2(2) . . ?
C2 C1 H9 118.4 . . ?
C6 C1 H9 118.4 . . ?
C4 O2 H2 109.5 . . ?
C1 C2 C3 117.2(2) . . ?
C1 C2 C14 121.9(2) . 2_756 ?
C3 C2 C14 120.9(2) . 2_756 ?
C5 O3 H3 109.5 . . ?
O1 C3 C4 117.1(2) . . ?
O1 C3 C2 121.9(2) . . ?
C4 C3 C2 121.0(2) . . ?
C10 O4 H4 109.5 . . ?
O2 C4 C5 122.2(2) . . ?
O2 C4 C3 117.5(2) . . ?
C5 C4 C3 120.3(2) . . ?
C11 O5 H5 109.5 . . ?
O3 C5 C4 115.4(2) . . ?
O3 C5 C6 124.1(2) . . ?
C4 C5 C6 120.4(2) . . ?
C12 O6 H6 109.5 . . ?
C1 C6 C5 117.8(2) . . ?
C1 C6 C7 121.6(2) . . ?
C5 C6 C7 120.6(2) . . ?
C9 C7 C6 110.26(18) . . ?
C9 C7 C15 112.57(19) . . ?
C6 C7 C15 112.3(2) . . ?
C9 C7 H7 107.1 . . ?
C6 C7 H7 107.1 . . ?
C15 C7 H7 107.1 . . ?
C9 C8 C13 122.9(2) . . ?
C9 C8 H8 118.6 . . ?
C13 C8 H8 118.6 . . ?
H1W O1W H2W 104(5) . . ?
C8 C9 C10 118.2(2) . . ?
C8 C9 C7 122.5(2) . . ?
C10 C9 C7 119.2(2) . . ?
O4 C10 C11 121.0(2) . . ?
O4 C10 C9 118.4(2) . . ?
C11 C10 C9 120.6(2) . . ?
O5 C11 C12 119.7(2) . . ?
O5 C11 C10 120.5(2) . . ?
C12 C11 C10 119.5(2) . . ?
O6 C12 C11 118.9(2) . . ?
O6 C12 C13 119.5(2) . . ?
C11 C12 C13 121.5(2) . . ?
C8 C13 C12 117.2(2) . . ?
C8 C13 C14 122.2(2) . . ?
C12 C13 C14 120.6(2) . . ?
C13 C14 C2 112.22(18) . 2_756 ?
C13 C14 C16 111.78(19) . . ?
C2 C14 C16 112.0(2) 2_756 . ?
C13 C14 H14 106.8 . . ?
C2 C14 H14 106.8 2_756 . ?
C16 C14 H14 106.8 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 N1 109.9(3) . 2_756 ?
N1 C17 H17 125.0 . . ?
N1 C17 H17 125.0 2_756 . ?
C18 C18 N1 107.22(19) 2_756 . ?
C18 C18 H18 126.4 2_756 . ?
N1 C18 H18 126.4 . . ?
N1 C19 C20 108.7(5) . . ?
N1 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
N1 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.3 . . ?
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 . . ?
O10 C21 C22 121.40(18) . 2_756 ?
O10 C21 C22 121.40(18) . . ?
C22 C21 C22 117.2(4) 2_756 . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 N2 C25 106.6(10) . . ?
C23 N2 C26 139.0(12) . . ?
C25 N2 C26 114.4(11) . . ?
N2 C23 N3 113.9(10) . . ?
N2 C23 H23 123.0 . . ?
N3 C23 H23 123.0 . . ?
C28 N3 C23 107.5(16) . . ?
C28 N3 C24 149.6(18) . . ?
C23 N3 C24 102.9(10) . . ?
C24 C25 N2 105.5(10) . . ?
C24 C25 H25 127.3 . . ?
N2 C25 H25 127.3 . . ?
C25 C24 N3 111.0(10) . . ?
C25 C24 H24 124.5 . . ?
N3 C24 H24 124.5 . . ?
N2 C26 C27 102.4(12) . . ?
N2 C26 H26A 111.3 . . ?
C27 C26 H26A 111.3 . . ?
N2 C26 H26B 111.3 . . ?
C27 C26 H26B 111.3 . . ?
H26A C26 H26B 109.2 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O11 C30 C31 115.3(12) . . ?
O11 C30 C29 114.2(11) . . ?
C31 C30 C29 130.5(16) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.8(3) . . . . ?
C6 C1 C2 C14 -178.9(2) . . . 2_756 ?
C1 C2 C3 O1 -178.3(2) . . . . ?
C14 C2 C3 O1 1.4(4) 2_756 . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C14 C2 C3 C4 -180.0(2) 2_756 . . . ?
O1 C3 C4 O2 -1.5(4) . . . . ?
C2 C3 C4 O2 179.9(2) . . . . ?
O1 C3 C4 C5 178.8(2) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
O2 C4 C5 O3 -0.1(4) . . . . ?
C3 C4 C5 O3 179.6(2) . . . . ?
O2 C4 C5 C6 178.5(2) . . . . ?
C3 C4 C5 C6 -1.8(4) . . . . ?
C2 C1 C6 C5 -2.3(3) . . . . ?
C2 C1 C6 C7 178.6(2) . . . . ?
O3 C5 C6 C1 -178.7(2) . . . . ?
C4 C5 C6 C1 2.8(3) . . . . ?
O3 C5 C6 C7 0.4(3) . . . . ?
C4 C5 C6 C7 -178.1(2) . . . . ?
C1 C6 C7 C9 79.7(3) . . . . ?
C5 C6 C7 C9 -99.4(2) . . . . ?
C1 C6 C7 C15 -46.7(3) . . . . ?
C5 C6 C7 C15 134.2(2) . . . . ?
C13 C8 C9 C10 1.0(3) . . . . ?
C13 C8 C9 C7 -179.3(2) . . . . ?
C6 C7 C9 C8 -89.3(3) . . . . ?
C15 C7 C9 C8 36.9(3) . . . . ?
C6 C7 C9 C10 90.5(3) . . . . ?
C15 C7 C9 C10 -143.3(2) . . . . ?
C8 C9 C10 O4 179.2(2) . . . . ?
C7 C9 C10 O4 -0.6(3) . . . . ?
C8 C9 C10 C11 -1.2(3) . . . . ?
C7 C9 C10 C11 179.0(2) . . . . ?
O4 C10 C11 O5 6.6(3) . . . . ?
C9 C10 C11 O5 -172.9(2) . . . . ?
O4 C10 C11 C12 -179.4(2) . . . . ?
C9 C10 C11 C12 1.1(4) . . . . ?
O5 C11 C12 O6 -4.8(3) . . . . ?
C10 C11 C12 O6 -178.8(2) . . . . ?
O5 C11 C12 C13 173.4(2) . . . . ?
C10 C11 C12 C13 -0.6(4) . . . . ?
C9 C8 C13 C12 -0.5(3) . . . . ?
C9 C8 C13 C14 178.3(2) . . . . ?
O6 C12 C13 C8 178.6(2) . . . . ?
C11 C12 C13 C8 0.4(3) . . . . ?
O6 C12 C13 C14 -0.3(3) . . . . ?
C11 C12 C13 C14 -178.5(2) . . . . ?
C8 C13 C14 C2 93.4(3) . . . 2_756 ?
C12 C13 C14 C2 -87.7(3) . . . 2_756 ?
C8 C13 C14 C16 -33.3(3) . . . . ?
C12 C13 C14 C16 145.5(2) . . . . ?
C18 N1 C17 N1 -0.1(2) . . . 2_756 ?
C19 N1 C17 N1 -179.5(3) . . . 2_756 ?
C17 N1 C18 C18 0.4(6) . . . 2_756 ?
C19 N1 C18 C18 179.7(4) . . . 2_756 ?
C17 N1 C19 C20 76.6(5) . . . . ?
C18 N1 C19 C20 -102.7(5) . . . . ?
C25 N2 C23 N3 0.0(3) . . . . ?
C26 N2 C23 N3 180.0(4) . . . . ?
N2 C23 N3 C28 179.9(3) . . . . ?
N2 C23 N3 C24 0.1(3) . . . . ?
C23 N2 C25 C24 -0.1(5) . . . . ?
C26 N2 C25 C24 179.9(4) . . . . ?
N2 C25 C24 N3 0.2(6) . . . . ?
C28 N3 C24 C25 -179.8(6) . . . . ?
C23 N3 C24 C25 -0.2(5) . . . . ?
C23 N2 C26 C27 175.3(12) . . . . ?
C25 N2 C26 C27 -4.7(12) . . . . ?

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 O6 0.84 1.95 2.785(3) 173.5 2_756
O2 H2 O3 0.84 2.27 2.707(3) 112.4 .
O2 H2 O1W 0.84 1.95 2.727(3) 154.4 4_566
O3 H3 O4 0.84 1.97 2.796(3) 167.3 .
O4 H4 S1 0.84 2.88 3.486(2) 130.7 .
O4 H4 O5 0.84 2.35 2.799(3) 113.6 .
O4 H4 O7 0.84 1.91 2.688(3) 154.1 2_656
O5 H5 O1W 0.84 1.97 2.782(3) 161.3 .
O6 H6 O5 0.84 2.28 2.741(3) 115.1 .
O6 H6 O8 0.84 1.98 2.732(3) 148.8 4_565
O1W H1W O8 0.80(7) 2.15(7) 2.804(3) 140(6) .
O1W H2W O7 0.91(5) 1.89(5) 2.768(3) 162(4) 4_565
C17 H17 O2 0.95 2.56 3.206(4) 125.2 3_767
C17 H17 O2 0.95 2.56 3.206(4) 125.2 4_565
C19 H19A O8 0.99 2.46 3.150(4) 126.8 .

_refine_diff_density_max         0.555
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.085

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 986741'
#######################################################################
#
#                 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_F:\xtals\Completed\c2phemim.CIF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            c2phemimetso4
_chemical_melting_point          ?
_chemical_formula_moiety         
'C60 H56 O12, 3(C2 H5 O4 S), 3(C6 H11 N2), 3(H2 O)'
_chemical_formula_sum            'C84 H110 N6 O27 S3'
_chemical_formula_weight         1731.96

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   12.720(3)
_cell_length_b                   39.701(10)
_cell_length_c                   16.861(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.212(4)
_cell_angle_gamma                90.00
_cell_volume                     8480(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9918
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      24.44

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3680
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9347
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            93067
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         26.51
_reflns_number_total             17540
_reflns_number_gt                10828
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_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)+(0.0961P)²+11.4259P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17540
_refine_ls_number_parameters     1219
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.2195
_refine_ls_wR_factor_gt          0.1867
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.055
_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
S1 S 0.78527(8) 0.02789(2) 0.40658(7) 0.0439(3) Uani 1 1 d D . .
O1 O 0.25692(19) 0.10824(6) 0.32952(14) 0.0370(6) Uani 1 1 d . . .
H1 H 0.3208 0.1139 0.3320 0.044 Uiso 1 1 calc R . .
N1 N 0.8570(3) 0.16565(9) 0.15339(19) 0.0463(8) Uani 1 1 d . . .
C1 C 0.1879(2) 0.16621(7) 0.48683(17) 0.0208(6) Uani 1 1 d . . .
H13 H 0.2115 0.1865 0.5125 0.025 Uiso 1 1 calc R . .
O1W O 0.7959(2) 0.05866(7) 0.74902(19) 0.0509(7) Uani 1 1 d . . .
S2 S 0.63873(10) 0.08484(3) 0.04395(7) 0.0565(3) Uani 1 1 d DU . .
O2 O 0.0869(2) 0.07682(6) 0.38151(15) 0.0396(6) Uani 1 1 d . . .
H2 H 0.1238 0.0716 0.3446 0.047 Uiso 1 1 calc R . .
N2 N 0.8890(3) 0.11790(9) 0.2115(2) 0.0506(9) Uani 1 1 d . . .
C2 C 0.2433(2) 0.15389(8) 0.42518(18) 0.0221(6) Uani 1 1 d . . .
O2W O 0.7467(4) 0.01672(15) 0.6224(3) 0.0935(16) Uani 0.80 1 d P A 1
S3 S 0.16418(11) 0.03370(3) 0.18461(8) 0.0633(3) Uani 1 1 d . . .
O3 O -0.01932(18) 0.10407(6) 0.50023(14) 0.0340(6) Uani 1 1 d . . .
H3 H -0.0378 0.0884 0.4686 0.041 Uiso 1 1 calc R . .
N3 N 0.3884(4) 0.07482(9) 0.5608(2) 0.0642(11) Uani 1 1 d . . .
C3 C 0.2090(2) 0.12377(8) 0.39009(18) 0.0261(7) Uani 1 1 d . . .
O3W O 0.6113(5) 0.09288(16) 0.2573(3) 0.0525(14) Uani 0.55 1 d P B 1
O3W' O 0.5598(6) 0.0708(2) 0.2696(4) 0.0593(19) Uani 0.45 1 d P C 2
O4 O -0.07973(17) 0.11102(6) 0.65745(14) 0.0306(5) Uani 1 1 d . . .
H4 H -0.0784 0.1112 0.6077 0.037 Uiso 1 1 calc R . .
N4 N 0.4432(6) 0.04882(11) 0.4622(3) 0.096(2) Uani 1 1 d D . .
C4 C 0.1214(3) 0.10692(8) 0.41412(19) 0.0273(7) Uani 1 1 d . . .
O5 O -0.00920(19) 0.08534(6) 0.80186(14) 0.0372(6) Uani 1 1 d . . .
H5 H -0.0628 0.0804 0.7713 0.045 Uiso 1 1 calc R . .
N5 N 0.3820(9) 0.00984(16) 0.8644(5) 0.174(4) Uani 1 1 d DU . .
C5 C 0.0670(2) 0.12018(8) 0.47479(18) 0.0237(7) Uani 1 1 d . . .
O6 O 0.16989(19) 0.10565(6) 0.88128(13) 0.0361(6) Uani 1 1 d . . .
H6 H 0.2361 0.1052 0.8887 0.043 Uiso 1 1 calc R . .
N6 N 0.2139(6) 0.01218(13) 0.8862(4) 0.1040(19) Uani 1 1 d . . .
C6 C 0.0996(2) 0.15014(7) 0.51244(17) 0.0203(6) Uani 1 1 d . . .
O7 O 0.3981(2) 0.10239(6) 0.88517(15) 0.0396(6) Uani 1 1 d . . .
H7 H 0.4443 0.0959 0.9207 0.047 Uiso 1 1 calc R . .
C7 C 0.0394(2) 0.16440(7) 0.57889(17) 0.0217(6) Uani 1 1 d . . .
H16 H -0.0367 0.1586 0.5659 0.026 Uiso 1 1 calc R . .
O8 O 0.5870(2) 0.07884(7) 0.82656(18) 0.0501(7) Uani 1 1 d . . .
H8 H 0.5836 0.0769 0.8759 0.060 Uiso 1 1 calc R . .
C8 C 0.1671(2) 0.15829(8) 0.70214(18) 0.0228(6) Uani 1 1 d . . .
H17 H 0.2099 0.1745 0.6789 0.027 Uiso 1 1 calc R . .
O9 O 0.67678(19) 0.11381(6) 0.71411(15) 0.0376(6) Uani 1 1 d . . .
H9 H 0.6977 0.0967 0.7403 0.045 Uiso 1 1 calc R . .
C9 C 0.0748(2) 0.14783(8) 0.65887(17) 0.0215(6) Uani 1 1 d . . .
O10 O 0.72579(18) 0.12542(6) 0.56107(15) 0.0371(6) Uani 1 1 d . . .
H10 H 0.7256 0.1244 0.6108 0.045 Uiso 1 1 calc R . .
C10 C 0.0145(2) 0.12324(8) 0.69292(18) 0.0234(6) Uani 1 1 d . . .
O11 O 0.65930(19) 0.10200(6) 0.41605(15) 0.0390(6) Uani 1 1 d . . .
H11 H 0.7172 0.0994 0.4435 0.047 Uiso 1 1 calc R . .
C11 C 0.0472(2) 0.10968(8) 0.76735(19) 0.0262(7) Uani 1 1 d . . .
O12 O 0.47072(18) 0.12230(6) 0.33800(13) 0.0300(5) Uani 1 1 d . . .
H12 H 0.5219 0.1134 0.3177 0.036 Uiso 1 1 calc R . .
C12 C 0.1400(3) 0.12086(8) 0.80902(18) 0.0264(7) Uani 1 1 d . . .
O13 O 0.2542(4) 0.05058(10) 0.1418(3) 0.1038(15) Uani 1 1 d . D .
C13 C 0.2001(2) 0.14630(8) 0.77781(18) 0.0229(6) Uani 1 1 d . . .
O14 O 0.1604(5) 0.00061(11) 0.1607(3) 0.0602(13) Uani 0.70 1 d P D 1
C14 C 0.2952(2) 0.16192(8) 0.82558(18) 0.0246(7) Uani 1 1 d . . .
H14 H 0.2939 0.1539 0.8817 0.030 Uiso 1 1 calc R . .
O14A O 0.2269(14) 0.0040(4) 0.2043(17) 0.140(9) Uani 0.30 1 d P D 2
O15 O 0.1923(5) 0.03766(12) 0.2721(3) 0.0700(14) Uani 0.70 1 d P D 1
C15 C 0.4488(2) 0.16667(8) 0.73832(18) 0.0238(7) Uani 1 1 d . . .
H15 H 0.4176 0.1868 0.7166 0.029 Uiso 1 1 calc R . .
O15A O 0.1142(9) 0.0518(3) 0.2314(6) 0.057(3) Uani 0.30 1 d P D 2
O16 O 0.0731(7) 0.05403(19) 0.1642(6) 0.144(3) Uani 0.70 1 d P D 1
C16 C 0.3990(2) 0.14980(8) 0.79675(18) 0.0239(7) Uani 1 1 d . . .
O16A O 0.1071(17) 0.0265(7) 0.1030(11) 0.160(9) Uani 0.30 1 d P D 2
O17 O 0.5727(3) 0.06906(10) -0.0194(2) 0.0799(11) Uani 1 1 d U E .
C17 C 0.4458(3) 0.12041(8) 0.82770(19) 0.0292(7) Uani 1 1 d . . .
O18 O 0.6260(5) 0.07246(17) 0.1186(3) 0.146(2) Uani 1 1 d U E .
C18 C 0.5389(3) 0.10835(8) 0.8006(2) 0.0319(8) Uani 1 1 d . . .
O19 O 0.6509(6) 0.11873(16) 0.0360(5) 0.089(2) Uani 0.70 1 d P E 1
C19 C 0.5858(3) 0.12566(8) 0.7420(2) 0.0285(7) Uani 1 1 d . . .
O19A O 0.5881(17) 0.1191(4) 0.044(2) 0.157(11) Uani 0.30 1 d PDU E 2
O20 O 0.7528(4) 0.06696(15) 0.0438(3) 0.0834(16) Uani 0.70 1 d P E 1
C20 C 0.5421(2) 0.15544(8) 0.71021(18) 0.0249(7) Uani 1 1 d . . .
O20A O 0.7439(9) 0.0973(3) 0.0101(8) 0.074(3) Uani 0.30 1 d P E 2
O21 O 0.83496(19) 0.05835(6) 0.43802(16) 0.0406(6) Uani 1 1 d . F .
C21 C 0.5977(2) 0.17422(8) 0.64778(19) 0.0260(7) Uani 1 1 d . . .
H21 H 0.6749 0.1696 0.6596 0.031 Uiso 1 1 calc R . .
O22 O 0.7112(2) 0.03323(8) 0.3393(2) 0.0631(9) Uani 1 1 d . F .
C22 C 0.4720(2) 0.16995(8) 0.52232(18) 0.0236(7) Uani 1 1 d . . .
H22 H 0.4268 0.1850 0.5469 0.028 Uiso 1 1 calc R . .
O23 O 0.7564(7) 0.00437(13) 0.4609(3) 0.080(2) Uani 0.70 1 d P F 1
C23 C 0.5668(2) 0.16013(8) 0.56485(19) 0.0252(7) Uani 1 1 d . . .
O23A O 0.7200(13) 0.0186(4) 0.4769(11) 0.097(6) Uani 0.30 1 d PD F 2
O24 O 0.8631(7) -0.0013(2) 0.4195(7) 0.050(2) Uani 0.30 1 d P F 2
C24 C 0.6296(2) 0.13716(8) 0.5284(2) 0.0267(7) Uani 1 1 d . . .
O24A O 0.8723(4) 0.01046(12) 0.3532(3) 0.0550(13) Uani 0.70 1 d P F 1
C25 C 0.5984(2) 0.12472(8) 0.4529(2) 0.0269(7) Uani 1 1 d . . .
C26 C 0.5045(2) 0.13515(8) 0.41161(18) 0.0242(7) Uani 1 1 d . . .
C27 C 0.4413(2) 0.15867(8) 0.44584(18) 0.0229(6) Uani 1 1 d . . .
C28 C 0.3405(2) 0.17185(8) 0.39940(18) 0.0221(6) Uani 1 1 d . . .
H28 H 0.3455 0.1659 0.3422 0.027 Uiso 1 1 calc R . .
C29 C 0.0471(2) 0.20300(8) 0.58400(18) 0.0243(7) Uani 1 1 d . . .
H29A H 0.1218 0.2095 0.5973 0.029 Uiso 1 1 calc R . .
H29B H 0.0237 0.2127 0.5313 0.029 Uiso 1 1 calc R . .
C30 C -0.0195(3) 0.21777(8) 0.6461(2) 0.0296(7) Uani 1 1 d . . .
H30A H -0.0950 0.2134 0.6296 0.036 Uiso 1 1 calc R . .
H30B H -0.0017 0.2061 0.6975 0.036 Uiso 1 1 calc R . .
C31 C -0.0034(3) 0.25526(8) 0.6581(2) 0.0293(7) Uani 1 1 d . . .
C32 C 0.0274(3) 0.26859(10) 0.7323(2) 0.0400(9) Uani 1 1 d . . .
H32 H 0.0404 0.2539 0.7767 0.048 Uiso 1 1 calc R . .
C33 C 0.0398(3) 0.30322(11) 0.7428(3) 0.0507(11) Uani 1 1 d . . .
H33 H 0.0597 0.3121 0.7944 0.061 Uiso 1 1 calc R . .
C34 C 0.0235(3) 0.32468(10) 0.6788(3) 0.0495(10) Uani 1 1 d . . .
H34 H 0.0321 0.3483 0.6859 0.059 Uiso 1 1 calc R . .
C35 C -0.0057(3) 0.31153(10) 0.6041(3) 0.0464(10) Uani 1 1 d . . .
H35 H -0.0166 0.3262 0.5595 0.056 Uiso 1 1 calc R . .
C36 C -0.0190(3) 0.27728(9) 0.5940(2) 0.0403(9) Uani 1 1 d . . .
H36 H -0.0391 0.2686 0.5423 0.048 Uiso 1 1 calc R . .
C37 C 0.2848(3) 0.20043(8) 0.82725(19) 0.0263(7) Uani 1 1 d . . .
H37A H 0.2917 0.2094 0.7732 0.032 Uiso 1 1 calc R . .
H37B H 0.2137 0.2064 0.8422 0.032 Uiso 1 1 calc R . .
C38 C 0.3678(3) 0.21690(9) 0.8857(2) 0.0331(8) Uani 1 1 d . . .
H38A H 0.3579 0.2089 0.9401 0.040 Uiso 1 1 calc R . .
H38B H 0.4386 0.2096 0.8728 0.040 Uiso 1 1 calc R . .
C39 C 0.3639(3) 0.25466(9) 0.88510(19) 0.0315(8) Uani 1 1 d . . .
C40 C 0.4459(3) 0.27366(10) 0.8598(2) 0.0381(9) Uani 1 1 d . . .
H40 H 0.5052 0.2625 0.8416 0.046 Uiso 1 1 calc R . .
C41 C 0.4434(4) 0.30831(11) 0.8603(3) 0.0515(11) Uani 1 1 d . . .
H41 H 0.5014 0.3207 0.8435 0.062 Uiso 1 1 calc R . .
C42 C 0.3584(4) 0.32495(11) 0.8846(3) 0.0603(13) Uani 1 1 d . . .
H42 H 0.3565 0.3489 0.8848 0.072 Uiso 1 1 calc R . .
C43 C 0.2747(4) 0.30651(12) 0.9092(3) 0.0642(13) Uani 1 1 d . . .
H43 H 0.2149 0.3179 0.9261 0.077 Uiso 1 1 calc R . .
C44 C 0.2776(3) 0.27182(10) 0.9093(2) 0.0475(10) Uani 1 1 d . . .
H44 H 0.2196 0.2595 0.9262 0.057 Uiso 1 1 calc R . .
C45 C 0.5843(3) 0.21277(8) 0.6509(2) 0.0287(7) Uani 1 1 d . . .
H45A H 0.5118 0.2189 0.6293 0.034 Uiso 1 1 calc R . .
H45B H 0.5943 0.2205 0.7069 0.034 Uiso 1 1 calc R . .
C46 C 0.6641(3) 0.23032(9) 0.6025(3) 0.0429(9) Uani 1 1 d . . .
H46A H 0.7309 0.2327 0.6370 0.051 Uiso 1 1 calc R . .
H46B H 0.6785 0.2153 0.5580 0.051 Uiso 1 1 calc R . .
C47 C 0.6351(3) 0.26439(8) 0.5683(2) 0.0317(8) Uani 1 1 d . . .
C48 C 0.6984(3) 0.29206(10) 0.5845(3) 0.0521(11) Uani 1 1 d . . .
H48 H 0.7575 0.2909 0.6232 0.062 Uiso 1 1 calc R . .
C49 C 0.6737(5) 0.32279(12) 0.5421(4) 0.087(2) Uani 1 1 d . . .
H49 H 0.7172 0.3421 0.5515 0.104 Uiso 1 1 calc R . .
C50 C 0.5869(6) 0.32415(16) 0.4879(4) 0.088(2) Uani 1 1 d . . .
H50 H 0.5713 0.3444 0.4592 0.105 Uiso 1 1 calc R . .
C51 C 0.5240(5) 0.29751(16) 0.4749(3) 0.0768(17) Uani 1 1 d . . .
H51 H 0.4627 0.2990 0.4385 0.092 Uiso 1 1 calc R . .
C52 C 0.5479(3) 0.26827(11) 0.5141(2) 0.0497(10) Uani 1 1 d . . .
H52 H 0.5024 0.2495 0.5036 0.060 Uiso 1 1 calc R . .
C53 C 0.3352(2) 0.21044(8) 0.40361(19) 0.0239(7) Uani 1 1 d . . .
H53A H 0.3274 0.2172 0.4593 0.029 Uiso 1 1 calc R . .
H53B H 0.4026 0.2199 0.3886 0.029 Uiso 1 1 calc R . .
C54 C 0.2445(3) 0.22579(9) 0.3496(2) 0.0324(8) Uani 1 1 d . . .
H54A H 0.2513 0.2189 0.2938 0.039 Uiso 1 1 calc R . .
H54B H 0.1765 0.2170 0.3652 0.039 Uiso 1 1 calc R . .
C55 C 0.2439(3) 0.26368(8) 0.35473(19) 0.0296(7) Uani 1 1 d . . .
C56 C 0.3041(3) 0.28294(10) 0.3071(2) 0.0388(9) Uani 1 1 d . . .
H56 H 0.3439 0.2720 0.2697 0.047 Uiso 1 1 calc R . .
C57 C 0.3074(3) 0.31745(11) 0.3129(3) 0.0523(11) Uani 1 1 d . . .
H57 H 0.3492 0.3301 0.2797 0.063 Uiso 1 1 calc R . .
C58 C 0.2501(4) 0.33371(10) 0.3670(3) 0.0558(12) Uani 1 1 d . . .
H58 H 0.2526 0.3576 0.3714 0.067 Uiso 1 1 calc R . .
C59 C 0.1893(4) 0.31530(11) 0.4145(3) 0.0534(12) Uani 1 1 d . . .
H59 H 0.1489 0.3265 0.4512 0.064 Uiso 1 1 calc R . .
C60 C 0.1868(3) 0.28044(10) 0.4088(2) 0.0393(9) Uani 1 1 d . . .
H60 H 0.1454 0.2679 0.4425 0.047 Uiso 1 1 calc R . .
C61 C 0.8141(3) 0.13870(12) 0.1834(3) 0.0524(11) Uani 1 1 d . . .
H61 H 0.7405 0.1349 0.1844 0.063 Uiso 1 1 calc R . .
C62 C 0.9846(3) 0.13212(12) 0.1999(3) 0.0540(11) Uani 1 1 d . . .
H62 H 1.0522 0.1226 0.2144 0.065 Uiso 1 1 calc R . .
C63 C 0.9648(3) 0.16184(12) 0.1643(3) 0.0526(11) Uani 1 1 d . . .
H63 H 1.0159 0.1775 0.1494 0.063 Uiso 1 1 calc R . .
C64 C 0.7998(4) 0.19382(12) 0.1128(3) 0.0608(12) Uani 1 1 d . . .
H64A H 0.7241 0.1879 0.1034 0.073 Uiso 1 1 calc R . .
H64B H 0.8272 0.1974 0.0604 0.073 Uiso 1 1 calc R . .
C65 C 0.8106(4) 0.22561(13) 0.1596(3) 0.0732(15) Uani 1 1 d . . .
H65A H 0.7718 0.2437 0.1301 0.110 Uiso 1 1 calc R . .
H65B H 0.8854 0.2317 0.1685 0.110 Uiso 1 1 calc R . .
H65C H 0.7818 0.2224 0.2110 0.110 Uiso 1 1 calc R . .
C66 C 0.8714(4) 0.08477(13) 0.2473(3) 0.0760(16) Uani 1 1 d . . .
H66A H 0.9396 0.0742 0.2636 0.114 Uiso 1 1 calc R . .
H66B H 0.8313 0.0704 0.2082 0.114 Uiso 1 1 calc R . .
H66C H 0.8316 0.0877 0.2940 0.114 Uiso 1 1 calc R . .
C67 C 0.3595(6) 0.06402(15) 0.4891(4) 0.095(2) Uani 1 1 d . G .
H67 H 0.2916 0.0665 0.4612 0.114 Uiso 1 1 calc R . .
C68 C 0.4914(5) 0.06546(14) 0.5792(5) 0.0856(19) Uani 1 1 d . G .
H68 H 0.5331 0.0705 0.6273 0.103 Uiso 1 1 calc R . .
C69 C 0.5226(7) 0.04840(17) 0.5195(6) 0.110(3) Uani 1 1 d . G .
H69 H 0.5891 0.0377 0.5173 0.132 Uiso 1 1 calc R . .
C70 C 0.3221(4) 0.09264(13) 0.6138(3) 0.0727(15) Uani 0.70 1 d P G 1
H70A H 0.2594 0.1020 0.5822 0.087 Uiso 0.70 1 calc PR G 1
H70B H 0.3623 0.1116 0.6397 0.087 Uiso 0.70 1 calc PR G 1
C71 C 0.2875(6) 0.06968(16) 0.6755(5) 0.077(3) Uani 0.70 1 d P G 1
H71A H 0.2427 0.0820 0.7098 0.116 Uiso 0.70 1 calc PR G 1
H71B H 0.3495 0.0609 0.7077 0.116 Uiso 0.70 1 calc PR G 1
H71C H 0.2475 0.0509 0.6498 0.116 Uiso 0.70 1 calc PR G 1
C71A C 0.3527(14) 0.0230(6) 0.3682(12) 0.088(6) Uani 0.30 1 d PD G 2
H71D H 0.3551 0.0050 0.3269 0.133 Uiso 0.30 1 d P H 2
H71E H 0.3057 0.0407 0.3473 0.133 Uiso 0.30 1 d P I 2
H71F H 0.3298 0.0132 0.4161 0.133 Uiso 0.30 1 d P J 2
C72 C 0.4532(7) 0.03552(19) 0.3831(5) 0.119(3) Uani 0.70 1 d PDU G 1
H72A H 0.3862 0.0384 0.3502 0.179 Uiso 0.70 1 calc PR G 1
H72B H 0.4710 0.0115 0.3869 0.179 Uiso 0.70 1 calc PR G 1
H72C H 0.5091 0.0477 0.3588 0.179 Uiso 0.70 1 calc PR G 1
C73 C 0.2790(9) 0.00410(16) 0.8297(4) 0.121(3) Uani 1 1 d . K .
H73 H 0.2590 -0.0038 0.7773 0.145 Uiso 1 1 calc R . .
C74 C 0.2733(7) 0.02177(14) 0.9507(4) 0.0870(19) Uani 1 1 d . K .
H74 H 0.2484 0.0274 1.0005 0.104 Uiso 1 1 calc R . .
C75 C 0.3727(9) 0.0222(2) 0.9347(6) 0.134(3) Uani 1 1 d . K .
H75 H 0.4296 0.0305 0.9697 0.161 Uiso 1 1 calc R . .
C76 C 0.4670(11) 0.0082(3) 0.8000(7) 0.215(7) Uani 0.50 1 d PDU K 1
H76A H 0.4493 -0.0082 0.7566 0.258 Uiso 0.50 1 calc PR K 1
H76B H 0.4852 0.0304 0.7785 0.258 Uiso 0.50 1 calc PR K 1
C77 C 0.5328(11) -0.0026(3) 0.8545(11) 0.108(6) Uani 0.50 1 d PDU K 1
H77A H 0.6007 -0.0066 0.8329 0.162 Uiso 0.50 1 calc PR K 1
H77B H 0.5069 -0.0237 0.8758 0.162 Uiso 0.50 1 calc PR K 1
H77C H 0.5421 0.0142 0.8973 0.162 Uiso 0.50 1 calc PR K 1
C77A C 0.0797(15) 0.0284(5) 0.9448(11) 0.151(7) Uani 0.50 1 d PDU K 2
H77D H 0.0083 0.0363 0.9396 0.227 Uiso 0.50 1 d P L 2
H77E H 0.1282 0.0490 0.9511 0.227 Uiso 0.50 1 d P M 2
H77F H 0.0944 0.0154 0.9945 0.227 Uiso 0.50 1 d P N 2
C78 C 0.1059(10) 0.0079(3) 0.8700(8) 0.188(5) Uani 0.50 1 d PDU K 1
H78A H 0.0903 0.0008 0.8145 0.283 Uiso 0.50 1 calc PR K 1
H78B H 0.0699 0.0293 0.8786 0.283 Uiso 0.50 1 calc PR K 1
H78C H 0.0810 -0.0093 0.9055 0.283 Uiso 0.50 1 calc PR K 1
C79 C 0.8122(6) 0.07337(19) -0.0210(5) 0.102(2) Uani 0.70 1 d P E 1
H79A H 0.7654 0.0840 -0.0641 0.123 Uiso 0.70 1 calc PR E 1
H79B H 0.8363 0.0516 -0.0414 0.123 Uiso 0.70 1 calc PR E 1
C82 C 0.3458(5) 0.09655(16) 0.0961(5) 0.105(2) Uani 0.50 1 d P D 1
H82A H 0.3827 0.1169 0.1165 0.157 Uiso 0.50 1 calc PR D 1
H82B H 0.2883 0.1029 0.0563 0.157 Uiso 0.50 1 calc PR D 1
H82C H 0.3955 0.0818 0.0715 0.157 Uiso 0.50 1 calc PR D 1
C84 C 0.9990(7) -0.0308(2) 0.3718(6) 0.148(4) Uani 0.70 1 d P F 1
H84A H 1.0584 -0.0397 0.4067 0.222 Uiso 0.70 1 calc PR F 1
H84B H 1.0216 -0.0267 0.3186 0.222 Uiso 0.70 1 calc PR F 1
H84C H 0.9411 -0.0471 0.3682 0.222 Uiso 0.70 1 calc PR F 1
C83 C 0.9657(8) -0.0016(3) 0.4021(8) 0.089(4) Uani 0.70 1 d P F 1
H83A H 1.0225 0.0155 0.4028 0.107 Uiso 0.70 1 calc PR F 1
H83B H 0.9482 -0.0052 0.4575 0.107 Uiso 0.70 1 calc PR F 1
C83A C 0.950(2) 0.0022(4) 0.3640(8) 0.050(7) Uani 0.30 1 d P F 2
H83C H 0.9206 0.0067 0.3086 0.060 Uiso 0.30 1 calc PR F 2
H83D H 1.0000 0.0204 0.3817 0.060 Uiso 0.30 1 calc PR F 2
C80 C 0.9055(9) 0.0953(3) -0.0030(7) 0.083(3) Uani 0.70 1 d P E 1
H80A H 0.9418 0.0984 -0.0514 0.124 Uiso 0.70 1 calc PR E 1
H80B H 0.9538 0.0848 0.0383 0.124 Uiso 0.70 1 calc PR E 1
H80C H 0.8827 0.1172 0.0158 0.124 Uiso 0.70 1 calc PR E 1
C80A C 0.925(3) 0.0756(9) -0.008(2) 0.139(14) Uani 0.30 1 d PU E 2
H80D H 0.9569 0.0568 -0.0345 0.209 Uiso 0.30 1 calc PR E 2
H80E H 0.9461 0.0745 0.0496 0.209 Uiso 0.30 1 calc PR E 2
H80F H 0.9487 0.0969 -0.0291 0.209 Uiso 0.30 1 calc PR E 2
C81 C 0.3038(10) 0.0792(3) 0.1600(6) 0.066(3) Uani 0.50 1 d P D 1
H81A H 0.3625 0.0745 0.2012 0.079 Uiso 0.50 1 calc PR D 1
H81B H 0.2541 0.0945 0.1841 0.079 Uiso 0.50 1 calc PR D 1
C81A C 0.2503(9) 0.0872(2) 0.1317(6) 0.053(2) Uani 0.50 1 d P D 2
H81C H 0.1871 0.0938 0.0965 0.064 Uiso 0.50 1 calc PR D 2
H81D H 0.2475 0.0985 0.1838 0.064 Uiso 0.50 1 calc PR D 2
C84A C 0.9990(7) -0.0308(2) 0.3718(6) 0.148(4) Uani 0.30 1 d P F 2
H84D H 1.0614 -0.0313 0.3418 0.222 Uiso 0.30 1 calc PR F 2
H84E H 0.9486 -0.0480 0.3508 0.222 Uiso 0.30 1 calc PR F 2
H84F H 1.0201 -0.0354 0.4281 0.222 Uiso 0.30 1 calc PR F 2
C82A C 0.3458(5) 0.09655(16) 0.0961(5) 0.105(2) Uani 0.50 1 d P D 2
H82D H 0.3468 0.1210 0.0879 0.157 Uiso 0.50 1 calc PR D 2
H82E H 0.3477 0.0851 0.0448 0.157 Uiso 0.50 1 calc PR D 2
H82F H 0.4076 0.0899 0.1317 0.157 Uiso 0.50 1 calc PR D 2
C79A C 0.8122(6) 0.07337(19) -0.0210(5) 0.102(2) Uani 0.30 1 d P E 2
H79C H 0.7948 0.0731 -0.0794 0.123 Uiso 0.30 1 calc PR E 2
H79D H 0.7921 0.0511 -0.0010 0.123 Uiso 0.30 1 calc PR E 2
C70A C 0.3221(4) 0.09264(13) 0.6138(3) 0.0727(15) Uani 0.30 1 d P G 2
H70C H 0.3633 0.0975 0.6644 0.109 Uiso 0.30 1 calc PR G 2
H70D H 0.2613 0.0785 0.6236 0.109 Uiso 0.30 1 calc PR G 2
H70E H 0.2972 0.1138 0.5888 0.109 Uiso 0.30 1 calc PR G 2
C78A C 0.1059(10) 0.0079(3) 0.8700(8) 0.188(5) Uani 0.50 1 d P K 2
H78D H 0.0836 -0.0159 0.8718 0.226 Uiso 0.50 1 calc PR K 2
H78E H 0.0778 0.0185 0.8192 0.226 Uiso 0.50 1 calc PR K 2
C76A C 0.4670(11) 0.0082(3) 0.8000(7) 0.215(7) Uani 0.50 1 d PU K 2
H76C H 0.4352 -0.0026 0.7513 0.323 Uiso 0.50 1 calc PR K 2
H76D H 0.5284 -0.0049 0.8216 0.323 Uiso 0.50 1 calc PR K 2
H76E H 0.4893 0.0311 0.7876 0.323 Uiso 0.50 1 calc PR K 2
C72A C 0.4532(7) 0.03552(19) 0.3831(5) 0.119(3) Uani 0.30 1 d PD G 2
H72D H 0.4686 0.0534 0.3449 0.143 Uiso 0.30 1 calc PR G 2
H72E H 0.5074 0.0176 0.3834 0.143 Uiso 0.30 1 calc PR G 2
O2W' O 0.7238(16) 0.0498(5) 0.5944(13) 0.096(7) Uani 0.20 1 d P O 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
S1 O23 1.381(6) . ?
S1 O22 1.424(3) . ?
S1 O21 1.443(3) . ?
S1 O24 1.528(8) . ?
S1 O23A 1.553(14) . ?
S1 O24A 1.642(5) . ?
O1 C3 1.381(4) . ?
O1 H1 0.8400 . ?
N1 C61 1.322(5) . ?
N1 C63 1.376(5) . ?
N1 C64 1.469(6) . ?
C1 C6 1.394(4) . ?
C1 C2 1.396(4) . ?
C1 H13 0.9500 . ?
S2 O19 1.362(6) . ?
S2 O18 1.374(4) . ?
S2 O17 1.441(4) . ?
S2 O19A 1.505(15) . ?
S2 O20A 1.581(11) . ?
S2 O20 1.616(5) . ?
O2 C4 1.371(4) . ?
O2 H2 0.8400 . ?
N2 C61 1.316(5) . ?
N2 C62 1.371(5) . ?
N2 C66 1.473(6) . ?
C2 C3 1.387(4) . ?
C2 C28 1.524(4) . ?
S3 O15A 1.278(9) . ?
S3 O14 1.374(5) . ?
S3 O16 1.428(7) . ?
S3 O14A 1.445(15) . ?
S3 O15 1.494(5) . ?
S3 O16A 1.523(17) . ?
S3 O13 1.559(4) . ?
O3 C5 1.373(4) . ?
O3 H3 0.8400 . ?
N3 C67 1.304(7) . ?
N3 C68 1.369(7) . ?
N3 C70 1.465(6) . ?
C3 C4 1.391(5) . ?
O4 C10 1.379(4) . ?
O4 H4 0.8400 . ?
N4 C69 1.332(10) . ?
N4 C67 1.339(8) . ?
N4 C72 1.451(8) . ?
C4 C5 1.390(4) . ?
O5 C11 1.365(4) . ?
O5 H5 0.8400 . ?
N5 C75 1.298(11) . ?
N5 C73 1.404(13) . ?
N5 C76 1.602(12) . ?
C5 C6 1.393(4) . ?
O6 C12 1.382(4) . ?
O6 H6 0.8400 . ?
N6 C74 1.323(8) . ?
N6 C73 1.357(9) . ?
N6 C78 1.386(12) . ?
C6 C7 1.522(4) . ?
O7 C17 1.388(4) . ?
O7 H7 0.8400 . ?
C7 C9 1.531(4) . ?
C7 C29 1.537(4) . ?
C7 H16 1.0000 . ?
O8 C18 1.375(4) . ?
O8 H8 0.8400 . ?
C8 C9 1.388(4) . ?
C8 C13 1.390(4) . ?
C8 H17 0.9500 . ?
O9 C19 1.371(4) . ?
O9 H9 0.8400 . ?
C9 C10 1.397(4) . ?
O10 C24 1.376(4) . ?
O10 H10 0.8400 . ?
C10 C11 1.394(4) . ?
O11 C25 1.373(4) . ?
O11 H11 0.8400 . ?
C11 C12 1.391(4) . ?
O12 C26 1.374(4) . ?
O12 H12 0.8400 . ?
C12 C13 1.398(4) . ?
O13 C81 1.323(12) . ?
O13 C81A 1.464(10) . ?
C13 C14 1.523(4) . ?
C14 C16 1.526(4) . ?
C14 C37 1.535(4) . ?
C14 H14 1.0000 . ?
C15 C16 1.390(4) . ?
C15 C20 1.391(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(4) . ?
C17 C18 1.392(5) . ?
C18 C19 1.383(5) . ?
C19 C20 1.393(4) . ?
O20 C79 1.408(8) . ?
C20 C21 1.516(4) . ?
C21 C23 1.524(5) . ?
C21 C45 1.541(4) . ?
C21 H21 1.0000 . ?
C22 C27 1.387(4) . ?
C22 C23 1.401(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(4) . ?
O24 C83A 1.52(3) . ?
C24 C25 1.390(5) . ?
O24A C83 1.463(10) . ?
C25 C26 1.390(4) . ?
C26 C27 1.392(4) . ?
C27 C28 1.532(4) . ?
C28 C53 1.536(4) . ?
C28 H28 1.0000 . ?
C29 C30 1.524(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.513(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.383(5) . ?
C31 C36 1.390(5) . ?
C32 C33 1.394(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.525(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.500(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C44 1.385(5) . ?
C39 C40 1.386(5) . ?
C40 C41 1.376(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.362(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.386(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.378(6) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.527(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.503(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.375(5) . ?
C47 C52 1.381(5) . ?
C48 C49 1.435(8) . ?
C48 H48 0.9500 . ?
C49 C50 1.368(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.332(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.356(7) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.530(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.507(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C60 1.387(5) . ?
C55 C56 1.388(5) . ?
C56 C57 1.374(6) . ?
C56 H56 0.9500 . ?
C57 C58 1.379(7) . ?
C57 H57 0.9500 . ?
C58 C59 1.373(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.387(6) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 C63 1.337(6) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 C65 1.488(7) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67 0.9500 . ?
C68 C69 1.305(9) . ?
C68 H68 0.9500 . ?
C69 H69 0.9500 . ?
C70 C71 1.480(9) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C71A H71D 1.0001 . ?
C71A H71E 0.9682 . ?
C71A H71F 0.9640 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73 0.9500 . ?
C74 C75 1.316(11) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
C76 C77 1.261(13) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C77A H77D 0.9566 . ?
C77A H77E 1.0240 . ?
C77A H77F 0.9888 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 C80 1.481(13) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C82 C81 1.422(13) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C84 C83 1.349(12) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83A H83C 0.9900 . ?
C83A H83D 0.9900 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C80A H80D 0.9800 . ?
C80A H80E 0.9800 . ?
C80A H80F 0.9800 . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C81A H81C 0.9900 . ?
C81A H81D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O23 S1 O22 115.6(4) . . ?
O23 S1 O21 117.2(3) . . ?
O22 S1 O21 113.85(17) . . ?
O23 S1 O24 66.4(5) . . ?
O22 S1 O24 126.9(4) . . ?
O21 S1 O24 109.1(4) . . ?
O23 S1 O23A 30.6(4) . . ?
O22 S1 O23A 106.4(7) . . ?
O21 S1 O23A 99.5(7) . . ?
O24 S1 O23A 95.4(7) . . ?
O23 S1 O24A 108.2(4) . . ?
O22 S1 O24A 93.2(2) . . ?
O21 S1 O24A 105.1(2) . . ?
O24 S1 O24A 45.4(4) . . ?
O23A S1 O24A 138.8(5) . . ?
C3 O1 H1 109.5 . . ?
C61 N1 C63 107.5(4) . . ?
C61 N1 C64 126.2(4) . . ?
C63 N1 C64 126.3(4) . . ?
C6 C1 C2 123.1(3) . . ?
C6 C1 H13 118.5 . . ?
C2 C1 H13 118.5 . . ?
O19 S2 O18 117.9(5) . . ?
O19 S2 O17 114.8(3) . . ?
O18 S2 O17 114.4(3) . . ?
O19 S2 O19A 32.8(7) . . ?
O18 S2 O19A 103.9(12) . . ?
O17 S2 O19A 99.8(12) . . ?
O19 S2 O20A 63.1(6) . . ?
O18 S2 O20A 128.1(6) . . ?
O17 S2 O20A 108.9(5) . . ?
O19A S2 O20A 95.3(9) . . ?
O19 S2 O20 108.9(4) . . ?
O18 S2 O20 91.4(3) . . ?
O17 S2 O20 105.7(3) . . ?
O19A S2 O20 141.4(8) . . ?
O20A S2 O20 49.3(5) . . ?
C4 O2 H2 109.5 . . ?
C61 N2 C62 108.2(4) . . ?
C61 N2 C66 125.2(4) . . ?
C62 N2 C66 126.6(4) . . ?
C3 C2 C1 117.3(3) . . ?
C3 C2 C28 120.9(3) . . ?
C1 C2 C28 121.7(3) . . ?
O15A S3 O14 135.4(6) . . ?
O15A S3 O16 52.6(6) . . ?
O14 S3 O16 117.6(5) . . ?
O15A S3 O14A 127.7(13) . . ?
O14 S3 O14A 44.9(9) . . ?
O16 S3 O14A 159.3(8) . . ?
O15A S3 O15 54.5(6) . . ?
O14 S3 O15 112.9(3) . . ?
O16 S3 O15 107.1(5) . . ?
O14A S3 O15 77.3(12) . . ?
O15A S3 O16A 116.1(11) . . ?
O14 S3 O16A 63.6(10) . . ?
O16 S3 O16A 65.1(10) . . ?
O14A S3 O16A 105.3(15) . . ?
O15 S3 O16A 164.4(8) . . ?
O15A S3 O13 118.2(5) . . ?
O14 S3 O13 106.4(3) . . ?
O16 S3 O13 105.0(4) . . ?
O14A S3 O13 92.5(7) . . ?
O15 S3 O13 107.0(3) . . ?
O16A S3 O13 88.3(8) . . ?
C5 O3 H3 109.5 . . ?
C67 N3 C68 107.7(5) . . ?
C67 N3 C70 126.4(5) . . ?
C68 N3 C70 125.8(5) . . ?
O1 C3 C2 123.9(3) . . ?
O1 C3 C4 114.8(3) . . ?
C2 C3 C4 121.3(3) . . ?
C10 O4 H4 109.5 . . ?
C69 N4 C67 109.5(6) . . ?
C69 N4 C72 122.5(7) . . ?
C67 N4 C72 127.9(7) . . ?
O2 C4 C5 117.6(3) . . ?
O2 C4 C3 122.6(3) . . ?
C5 C4 C3 119.9(3) . . ?
C11 O5 H5 109.5 . . ?
C75 N5 C73 106.5(9) . . ?
C75 N5 C76 139.3(10) . . ?
C73 N5 C76 111.8(8) . . ?
O3 C5 C4 121.3(3) . . ?
O3 C5 C6 118.0(3) . . ?
C4 C5 C6 120.7(3) . . ?
C12 O6 H6 109.5 . . ?
C74 N6 C73 107.8(8) . . ?
C74 N6 C78 132.7(9) . . ?
C73 N6 C78 119.4(9) . . ?
C5 C6 C1 117.7(3) . . ?
C5 C6 C7 120.2(3) . . ?
C1 C6 C7 122.1(3) . . ?
C17 O7 H7 109.5 . . ?
C6 C7 C9 111.2(2) . . ?
C6 C7 C29 112.2(2) . . ?
C9 C7 C29 111.5(2) . . ?
C6 C7 H16 107.2 . . ?
C9 C7 H16 107.2 . . ?
C29 C7 H16 107.2 . . ?
C18 O8 H8 109.5 . . ?
C9 C8 C13 123.4(3) . . ?
C9 C8 H17 118.3 . . ?
C13 C8 H17 118.3 . . ?
C19 O9 H9 109.5 . . ?
C8 C9 C10 117.6(3) . . ?
C8 C9 C7 120.1(3) . . ?
C10 C9 C7 122.3(3) . . ?
C24 O10 H10 109.5 . . ?
O4 C10 C11 115.5(3) . . ?
O4 C10 C9 123.8(3) . . ?
C11 C10 C9 120.7(3) . . ?
C25 O11 H11 109.5 . . ?
O5 C11 C12 117.7(3) . . ?
O5 C11 C10 122.2(3) . . ?
C12 C11 C10 120.1(3) . . ?
C26 O12 H12 109.5 . . ?
O6 C12 C11 117.3(3) . . ?
O6 C12 C13 122.1(3) . . ?
C11 C12 C13 120.6(3) . . ?
C81 O13 C81A 35.3(5) . . ?
C81 O13 S3 128.1(6) . . ?
C81A O13 S3 117.5(5) . . ?
C8 C13 C12 117.6(3) . . ?
C8 C13 C14 120.3(3) . . ?
C12 C13 C14 122.0(3) . . ?
C13 C14 C16 111.9(2) . . ?
C13 C14 C37 110.5(3) . . ?
C16 C14 C37 113.5(3) . . ?
C13 C14 H14 106.9 . . ?
C16 C14 H14 106.9 . . ?
C37 C14 H14 106.9 . . ?
C16 C15 C20 123.0(3) . . ?
C16 C15 H15 118.5 . . ?
C20 C15 H15 118.5 . . ?
C17 C16 C15 117.6(3) . . ?
C17 C16 C14 119.9(3) . . ?
C15 C16 C14 122.4(3) . . ?
O7 C17 C16 119.7(3) . . ?
O7 C17 C18 119.4(3) . . ?
C16 C17 C18 120.9(3) . . ?
O8 C18 C19 116.3(3) . . ?
O8 C18 C17 123.7(3) . . ?
C19 C18 C17 119.9(3) . . ?
O9 C19 C18 120.4(3) . . ?
O9 C19 C20 118.6(3) . . ?
C18 C19 C20 120.9(3) . . ?
C79 O20 S2 117.9(5) . . ?
C15 C20 C19 117.6(3) . . ?
C15 C20 C21 123.1(3) . . ?
C19 C20 C21 119.3(3) . . ?
C20 C21 C23 111.0(3) . . ?
C20 C21 C45 113.9(3) . . ?
C23 C21 C45 112.0(3) . . ?
C20 C21 H21 106.5 . . ?
C23 C21 H21 106.5 . . ?
C45 C21 H21 106.5 . . ?
C27 C22 C23 122.9(3) . . ?
C27 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C24 C23 C22 117.3(3) . . ?
C24 C23 C21 122.3(3) . . ?
C22 C23 C21 120.4(3) . . ?
C83A O24 S1 109.8(10) . . ?
O10 C24 C25 114.6(3) . . ?
O10 C24 C23 124.8(3) . . ?
C25 C24 C23 120.6(3) . . ?
C83 O24A S1 112.5(6) . . ?
O11 C25 C26 117.6(3) . . ?
O11 C25 C24 121.5(3) . . ?
C26 C25 C24 120.9(3) . . ?
O12 C26 C25 121.7(3) . . ?
O12 C26 C27 118.6(3) . . ?
C25 C26 C27 119.7(3) . . ?
C22 C27 C26 118.5(3) . . ?
C22 C27 C28 121.1(3) . . ?
C26 C27 C28 120.4(3) . . ?
C2 C28 C27 110.9(2) . . ?
C2 C28 C53 114.4(2) . . ?
C27 C28 C53 110.8(2) . . ?
C2 C28 H28 106.7 . . ?
C27 C28 H28 106.7 . . ?
C53 C28 H28 106.7 . . ?
C30 C29 C7 112.7(3) . . ?
C30 C29 H29A 109.1 . . ?
C7 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
C7 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
C31 C30 C29 113.1(3) . . ?
C31 C30 H30A 109.0 . . ?
C29 C30 H30A 109.0 . . ?
C31 C30 H30B 109.0 . . ?
C29 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C32 C31 C36 118.2(3) . . ?
C32 C31 C30 121.3(3) . . ?
C36 C31 C30 120.5(3) . . ?
C31 C32 C33 120.8(4) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 120.2(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 119.3(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C36 C35 C34 120.3(4) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C31 121.1(4) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?
C38 C37 C14 112.5(3) . . ?
C38 C37 H37A 109.1 . . ?
C14 C37 H37A 109.1 . . ?
C38 C37 H37B 109.1 . . ?
C14 C37 H37B 109.1 . . ?
H37A C37 H37B 107.8 . . ?
C39 C38 C37 113.8(3) . . ?
C39 C38 H38A 108.8 . . ?
C37 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C37 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C44 C39 C40 117.5(4) . . ?
C44 C39 C38 121.1(3) . . ?
C40 C39 C38 121.4(3) . . ?
C41 C40 C39 121.6(4) . . ?
C41 C40 H40 119.2 . . ?
C39 C40 H40 119.2 . . ?
C42 C41 C40 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 119.1(4) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 H42 120.5 . . ?
C44 C43 C42 120.5(4) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C39 120.9(4) . . ?
C43 C44 H44 119.6 . . ?
C39 C44 H44 119.6 . . ?
C46 C45 C21 110.7(3) . . ?
C46 C45 H45A 109.5 . . ?
C21 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
C21 C45 H45B 109.5 . . ?
H45A C45 H45B 108.1 . . ?
C47 C46 C45 117.6(3) . . ?
C47 C46 H46A 107.9 . . ?
C45 C46 H46A 107.9 . . ?
C47 C46 H46B 107.9 . . ?
C45 C46 H46B 107.9 . . ?
H46A C46 H46B 107.2 . . ?
C48 C47 C52 117.6(4) . . ?
C48 C47 C46 121.6(4) . . ?
C52 C47 C46 120.6(3) . . ?
C47 C48 C49 118.8(5) . . ?
C47 C48 H48 120.6 . . ?
C49 C48 H48 120.6 . . ?
C50 C49 C48 119.6(5) . . ?
C50 C49 H49 120.2 . . ?
C48 C49 H49 120.2 . . ?
C51 C50 C49 121.0(5) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C50 C51 C52 119.7(6) . . ?
C50 C51 H51 120.2 . . ?
C52 C51 H51 120.2 . . ?
C51 C52 C47 123.3(5) . . ?
C51 C52 H52 118.4 . . ?
C47 C52 H52 118.4 . . ?
C54 C53 C28 113.9(3) . . ?
C54 C53 H53A 108.8 . . ?
C28 C53 H53A 108.8 . . ?
C54 C53 H53B 108.8 . . ?
C28 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C55 C54 C53 111.8(3) . . ?
C55 C54 H54A 109.3 . . ?
C53 C54 H54A 109.3 . . ?
C55 C54 H54B 109.3 . . ?
C53 C54 H54B 109.3 . . ?
H54A C54 H54B 107.9 . . ?
C60 C55 C56 117.7(3) . . ?
C60 C55 C54 121.5(3) . . ?
C56 C55 C54 120.8(3) . . ?
C57 C56 C55 121.6(4) . . ?
C57 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
C56 C57 C58 119.9(4) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C59 C58 C57 119.7(4) . . ?
C59 C58 H58 120.1 . . ?
C57 C58 H58 120.1 . . ?
C58 C59 C60 120.1(4) . . ?
C58 C59 H59 119.9 . . ?
C60 C59 H59 119.9 . . ?
C55 C60 C59 120.9(4) . . ?
C55 C60 H60 119.6 . . ?
C59 C60 H60 119.6 . . ?
N2 C61 N1 109.6(4) . . ?
N2 C61 H61 125.2 . . ?
N1 C61 H61 125.2 . . ?
C63 C62 N2 107.1(4) . . ?
C63 C62 H62 126.5 . . ?
N2 C62 H62 126.5 . . ?
C62 C63 N1 107.6(4) . . ?
C62 C63 H63 126.2 . . ?
N1 C63 H63 126.2 . . ?
N1 C64 C65 112.4(4) . . ?
N1 C64 H64A 109.1 . . ?
C65 C64 H64A 109.1 . . ?
N1 C64 H64B 109.1 . . ?
C65 C64 H64B 109.1 . . ?
H64A C64 H64B 107.9 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N2 C66 H66A 109.5 . . ?
N2 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
N2 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N3 C67 N4 107.2(6) . . ?
N3 C67 H67 126.4 . . ?
N4 C67 H67 126.4 . . ?
C69 C68 N3 108.5(7) . . ?
C69 C68 H68 125.7 . . ?
N3 C68 H68 125.7 . . ?
C68 C69 N4 106.8(7) . . ?
C68 C69 H69 126.6 . . ?
N4 C69 H69 126.6 . . ?
N3 C70 C71 110.8(4) . . ?
N3 C70 H70A 109.5 . . ?
C71 C70 H70A 109.5 . . ?
N3 C70 H70B 109.5 . . ?
C71 C70 H70B 109.5 . . ?
H70A C70 H70B 108.1 . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
H71D C71A H71E 108.8 . . ?
H71D C71A H71F 109.1 . . ?
H71E C71A H71F 111.8 . . ?
N4 C72 H72A 109.5 . . ?
N4 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
N4 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N6 C73 N5 106.0(7) . . ?
N6 C73 H73 127.0 . . ?
N5 C73 H73 127.0 . . ?
C75 C74 N6 108.8(7) . . ?
C75 C74 H74 125.6 . . ?
N6 C74 H74 125.6 . . ?
N5 C75 C74 110.5(9) . . ?
N5 C75 H75 124.7 . . ?
C74 C75 H75 124.7 . . ?
C77 C76 N5 87.9(12) . . ?
C77 C76 H76A 114.0 . . ?
N5 C76 H76A 114.0 . . ?
C77 C76 H76B 114.0 . . ?
N5 C76 H76B 114.0 . . ?
H76A C76 H76B 111.2 . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
H77D C77A H77E 107.8 . . ?
H77D C77A H77F 110.7 . . ?
H77E C77A H77F 105.3 . . ?
N6 C78 H78A 109.5 . . ?
N6 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
N6 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
O20 C79 C80 115.1(7) . . ?
O20 C79 H79A 108.5 . . ?
C80 C79 H79A 108.5 . . ?
O20 C79 H79B 108.5 . . ?
C80 C79 H79B 108.5 . . ?
H79A C79 H79B 107.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C84 C83 O24A 109.6(9) . . ?
C84 C83 H83A 109.8 . . ?
O24A C83 H83A 109.8 . . ?
C84 C83 H83B 109.8 . . ?
O24A C83 H83B 109.8 . . ?
H83A C83 H83B 108.2 . . ?
O24 C83A H83C 111.6 . . ?
O24 C83A H83D 111.6 . . ?
H83C C83A H83D 109.4 . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
H80D C80A H80E 109.5 . . ?
H80D C80A H80F 109.5 . . ?
H80E C80A H80F 109.5 . . ?
O13 C81 C82 116.4(8) . . ?
O13 C81 H81A 108.2 . . ?
C82 C81 H81A 108.2 . . ?
O13 C81 H81B 108.2 . . ?
C82 C81 H81B 108.2 . . ?
H81A C81 H81B 107.3 . . ?
O13 C81A H81C 110.5 . . ?
O13 C81A H81D 110.5 . . ?
H81C C81A H81D 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.7(4) . . . . ?
C6 C1 C2 C28 -179.2(3) . . . . ?
C1 C2 C3 O1 -178.9(3) . . . . ?
C28 C2 C3 O1 -1.4(5) . . . . ?
C1 C2 C3 C4 1.5(5) . . . . ?
C28 C2 C3 C4 178.9(3) . . . . ?
O1 C3 C4 O2 1.5(5) . . . . ?
C2 C3 C4 O2 -178.8(3) . . . . ?
O1 C3 C4 C5 179.9(3) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
O2 C4 C5 O3 -1.1(5) . . . . ?
C3 C4 C5 O3 -179.6(3) . . . . ?
O2 C4 C5 C6 178.0(3) . . . . ?
C3 C4 C5 C6 -0.5(5) . . . . ?
O3 C5 C6 C1 179.4(3) . . . . ?
C4 C5 C6 C1 0.3(4) . . . . ?
O3 C5 C6 C7 -0.8(4) . . . . ?
C4 C5 C6 C7 -179.9(3) . . . . ?
C2 C1 C6 C5 0.8(4) . . . . ?
C2 C1 C6 C7 -178.9(3) . . . . ?
C5 C6 C7 C9 83.2(3) . . . . ?
C1 C6 C7 C9 -97.1(3) . . . . ?
C5 C6 C7 C29 -151.1(3) . . . . ?
C1 C6 C7 C29 28.6(4) . . . . ?
C13 C8 C9 C10 -2.0(5) . . . . ?
C13 C8 C9 C7 174.9(3) . . . . ?
C6 C7 C9 C8 79.9(3) . . . . ?
C29 C7 C9 C8 -46.1(4) . . . . ?
C6 C7 C9 C10 -103.3(3) . . . . ?
C29 C7 C9 C10 130.6(3) . . . . ?
C8 C9 C10 O4 178.6(3) . . . . ?
C7 C9 C10 O4 1.8(5) . . . . ?
C8 C9 C10 C11 -0.5(4) . . . . ?
C7 C9 C10 C11 -177.4(3) . . . . ?
O4 C10 C11 O5 1.6(4) . . . . ?
C9 C10 C11 O5 -179.2(3) . . . . ?
O4 C10 C11 C12 -178.5(3) . . . . ?
C9 C10 C11 C12 0.7(5) . . . . ?
O5 C11 C12 O6 2.0(4) . . . . ?
C10 C11 C12 O6 -177.9(3) . . . . ?
O5 C11 C12 C13 -178.5(3) . . . . ?
C10 C11 C12 C13 1.6(5) . . . . ?
O15A S3 O13 C81 17.1(12) . . . . ?
O14 S3 O13 C81 -162.2(9) . . . . ?
O16 S3 O13 C81 72.4(10) . . . . ?
O14A S3 O13 C81 -118.8(15) . . . . ?
O15 S3 O13 C81 -41.2(9) . . . . ?
O16A S3 O13 C81 136.0(13) . . . . ?
O15A S3 O13 C81A -23.4(10) . . . . ?
O14 S3 O13 C81A 157.3(6) . . . . ?
O16 S3 O13 C81A 31.9(8) . . . . ?
O14A S3 O13 C81A -159.3(13) . . . . ?
O15 S3 O13 C81A -81.7(7) . . . . ?
O16A S3 O13 C81A 95.5(12) . . . . ?
C9 C8 C13 C12 4.2(5) . . . . ?
C9 C8 C13 C14 -172.8(3) . . . . ?
O6 C12 C13 C8 175.5(3) . . . . ?
C11 C12 C13 C8 -3.9(5) . . . . ?
O6 C12 C13 C14 -7.5(5) . . . . ?
C11 C12 C13 C14 173.0(3) . . . . ?
C8 C13 C14 C16 -77.4(4) . . . . ?
C12 C13 C14 C16 105.7(3) . . . . ?
C8 C13 C14 C37 50.0(4) . . . . ?
C12 C13 C14 C37 -126.9(3) . . . . ?
C20 C15 C16 C17 -0.1(5) . . . . ?
C20 C15 C16 C14 -178.5(3) . . . . ?
C13 C14 C16 C17 -87.4(3) . . . . ?
C37 C14 C16 C17 146.8(3) . . . . ?
C13 C14 C16 C15 90.9(3) . . . . ?
C37 C14 C16 C15 -34.9(4) . . . . ?
C15 C16 C17 O7 -178.9(3) . . . . ?
C14 C16 C17 O7 -0.5(5) . . . . ?
C15 C16 C17 C18 -0.3(5) . . . . ?
C14 C16 C17 C18 178.1(3) . . . . ?
O7 C17 C18 O8 1.0(5) . . . . ?
C16 C17 C18 O8 -177.5(3) . . . . ?
O7 C17 C18 C19 178.5(3) . . . . ?
C16 C17 C18 C19 -0.1(5) . . . . ?
O8 C18 C19 O9 -1.6(5) . . . . ?
C17 C18 C19 O9 -179.2(3) . . . . ?
O8 C18 C19 C20 178.6(3) . . . . ?
C17 C18 C19 C20 0.9(5) . . . . ?
O19 S2 O20 C79 -54.9(7) . . . . ?
O18 S2 O20 C79 -175.2(6) . . . . ?
O17 S2 O20 C79 69.0(6) . . . . ?
O19A S2 O20 C79 -60(2) . . . . ?
O20A S2 O20 C79 -32.7(8) . . . . ?
C16 C15 C20 C19 0.9(5) . . . . ?
C16 C15 C20 C21 -178.6(3) . . . . ?
O9 C19 C20 C15 178.8(3) . . . . ?
C18 C19 C20 C15 -1.3(5) . . . . ?
O9 C19 C20 C21 -1.6(4) . . . . ?
C18 C19 C20 C21 178.2(3) . . . . ?
C15 C20 C21 C23 -95.6(3) . . . . ?
C19 C20 C21 C23 84.8(3) . . . . ?
C15 C20 C21 C45 31.9(4) . . . . ?
C19 C20 C21 C45 -147.7(3) . . . . ?
C27 C22 C23 C24 -2.2(5) . . . . ?
C27 C22 C23 C21 178.2(3) . . . . ?
C20 C21 C23 C24 -98.4(3) . . . . ?
C45 C21 C23 C24 133.1(3) . . . . ?
C20 C21 C23 C22 81.2(4) . . . . ?
C45 C21 C23 C22 -47.3(4) . . . . ?
O23 S1 O24 C83A 176.4(11) . . . . ?
O22 S1 O24 C83A 71.2(10) . . . . ?
O21 S1 O24 C83A -71.5(10) . . . . ?
O23A S1 O24 C83A -173.6(12) . . . . ?
O24A S1 O24 C83A 21.0(8) . . . . ?
C22 C23 C24 O10 178.6(3) . . . . ?
C21 C23 C24 O10 -1.8(5) . . . . ?
C22 C23 C24 C25 0.0(5) . . . . ?
C21 C23 C24 C25 179.6(3) . . . . ?
O23 S1 O24A C83 -58.2(7) . . . . ?
O22 S1 O24A C83 -176.5(6) . . . . ?
O21 S1 O24A C83 67.7(6) . . . . ?
O24 S1 O24A C83 -34.5(7) . . . . ?
O23A S1 O24A C83 -56.8(14) . . . . ?
O10 C24 C25 O11 1.4(5) . . . . ?
C23 C24 C25 O11 -179.9(3) . . . . ?
O10 C24 C25 C26 -178.1(3) . . . . ?
C23 C24 C25 C26 0.7(5) . . . . ?
O11 C25 C26 O12 2.7(5) . . . . ?
C24 C25 C26 O12 -177.8(3) . . . . ?
O11 C25 C26 C27 -178.7(3) . . . . ?
C24 C25 C26 C27 0.8(5) . . . . ?
C23 C22 C27 C26 3.7(5) . . . . ?
C23 C22 C27 C28 -175.9(3) . . . . ?
O12 C26 C27 C22 175.8(3) . . . . ?
C25 C26 C27 C22 -2.9(4) . . . . ?
O12 C26 C27 C28 -4.6(4) . . . . ?
C25 C26 C27 C28 176.7(3) . . . . ?
C3 C2 C28 C27 -86.9(3) . . . . ?
C1 C2 C28 C27 90.5(3) . . . . ?
C3 C2 C28 C53 146.8(3) . . . . ?
C1 C2 C28 C53 -35.8(4) . . . . ?
C22 C27 C28 C2 -80.5(4) . . . . ?
C26 C27 C28 C2 99.9(3) . . . . ?
C22 C27 C28 C53 47.7(4) . . . . ?
C26 C27 C28 C53 -131.9(3) . . . . ?
C6 C7 C29 C30 175.7(3) . . . . ?
C9 C7 C29 C30 -58.8(3) . . . . ?
C7 C29 C30 C31 173.7(3) . . . . ?
C29 C30 C31 C32 -123.7(4) . . . . ?
C29 C30 C31 C36 56.0(4) . . . . ?
C36 C31 C32 C33 1.7(5) . . . . ?
C30 C31 C32 C33 -178.6(3) . . . . ?
C31 C32 C33 C34 -1.3(6) . . . . ?
C32 C33 C34 C35 0.2(6) . . . . ?
C33 C34 C35 C36 0.5(6) . . . . ?
C34 C35 C36 C31 -0.1(6) . . . . ?
C32 C31 C36 C35 -1.0(5) . . . . ?
C30 C31 C36 C35 179.3(3) . . . . ?
C13 C14 C37 C38 170.1(3) . . . . ?
C16 C14 C37 C38 -63.4(3) . . . . ?
C14 C37 C38 C39 176.5(3) . . . . ?
C37 C38 C39 C44 65.3(4) . . . . ?
C37 C38 C39 C40 -114.2(4) . . . . ?
C44 C39 C40 C41 1.5(5) . . . . ?
C38 C39 C40 C41 -178.9(3) . . . . ?
C39 C40 C41 C42 -1.2(6) . . . . ?
C40 C41 C42 C43 0.3(6) . . . . ?
C41 C42 C43 C44 0.3(7) . . . . ?
C42 C43 C44 C39 0.1(7) . . . . ?
C40 C39 C44 C43 -1.0(6) . . . . ?
C38 C39 C44 C43 179.5(4) . . . . ?
C20 C21 C45 C46 165.1(3) . . . . ?
C23 C21 C45 C46 -67.9(4) . . . . ?
C21 C45 C46 C47 153.3(3) . . . . ?
C45 C46 C47 C48 124.0(4) . . . . ?
C45 C46 C47 C52 -61.4(5) . . . . ?
C52 C47 C48 C49 -2.8(6) . . . . ?
C46 C47 C48 C49 172.0(4) . . . . ?
C47 C48 C49 C50 1.4(7) . . . . ?
C48 C49 C50 C51 1.1(8) . . . . ?
C49 C50 C51 C52 -2.1(8) . . . . ?
C50 C51 C52 C47 0.6(8) . . . . ?
C48 C47 C52 C51 1.9(6) . . . . ?
C46 C47 C52 C51 -172.9(4) . . . . ?
C2 C28 C53 C54 -61.5(3) . . . . ?
C27 C28 C53 C54 172.2(3) . . . . ?
C28 C53 C54 C55 -178.9(3) . . . . ?
C53 C54 C55 C60 -91.3(4) . . . . ?
C53 C54 C55 C56 86.3(4) . . . . ?
C60 C55 C56 C57 -0.1(5) . . . . ?
C54 C55 C56 C57 -177.8(3) . . . . ?
C55 C56 C57 C58 0.0(6) . . . . ?
C56 C57 C58 C59 -0.5(6) . . . . ?
C57 C58 C59 C60 0.9(6) . . . . ?
C56 C55 C60 C59 0.5(5) . . . . ?
C54 C55 C60 C59 178.2(3) . . . . ?
C58 C59 C60 C55 -1.0(6) . . . . ?
C62 N2 C61 N1 0.6(5) . . . . ?
C66 N2 C61 N1 -178.1(4) . . . . ?
C63 N1 C61 N2 -1.0(5) . . . . ?
C64 N1 C61 N2 176.7(4) . . . . ?
C61 N2 C62 C63 0.1(5) . . . . ?
C66 N2 C62 C63 178.7(5) . . . . ?
N2 C62 C63 N1 -0.6(5) . . . . ?
C61 N1 C63 C62 1.0(5) . . . . ?
C64 N1 C63 C62 -176.7(4) . . . . ?
C61 N1 C64 C65 112.1(5) . . . . ?
C63 N1 C64 C65 -70.7(6) . . . . ?
C68 N3 C67 N4 -1.4(6) . . . . ?
C70 N3 C67 N4 -179.2(5) . . . . ?
C69 N4 C67 N3 3.8(7) . . . . ?
C72 N4 C67 N3 -173.8(6) . . . . ?
C67 N3 C68 C69 -1.6(7) . . . . ?
C70 N3 C68 C69 176.2(5) . . . . ?
N3 C68 C69 N4 3.9(7) . . . . ?
C67 N4 C69 C68 -4.8(7) . . . . ?
C72 N4 C69 C68 173.0(6) . . . . ?
C67 N3 C70 C71 102.3(7) . . . . ?
C68 N3 C70 C71 -75.1(7) . . . . ?
C74 N6 C73 N5 -0.6(7) . . . . ?
C78 N6 C73 N5 -177.8(8) . . . . ?
C75 N5 C73 N6 -3.4(9) . . . . ?
C76 N5 C73 N6 -169.1(7) . . . . ?
C73 N6 C74 C75 4.4(8) . . . . ?
C78 N6 C74 C75 -179.0(9) . . . . ?
C73 N5 C75 C74 6.2(10) . . . . ?
C76 N5 C75 C74 165.7(13) . . . . ?
N6 C74 C75 N5 -6.8(10) . . . . ?
C75 N5 C76 C77 52.2(18) . . . . ?
C73 N5 C76 C77 -149.0(9) . . . . ?
S2 O20 C79 C80 107.9(8) . . . . ?
S1 O24A C83 C84 142.6(9) . . . . ?
C81A O13 C81 C82 -67.9(12) . . . . ?
S3 O13 C81 C82 -152.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.51
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 986742'
#######################################################################
#
#                 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_C:\xtals\ALS\work\2DFMJ12.CIF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            2DFMJ12
_chemical_melting_point          ?
_chemical_formula_moiety         
'C32 H32 O12, C6 H11 N2, C2 H5 O4 S, C2 H3 N, H2 O'
_chemical_formula_sum            'C42 H53 N3 O17 S'
_chemical_formula_weight         903.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020 '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 -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1206 0.1480 '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                   9.9102(15)
_cell_length_b                   14.121(2)
_cell_length_c                   14.877(2)
_cell_angle_alpha                91.328(2)
_cell_angle_beta                 96.132(2)
_cell_angle_gamma                96.436(2)
_cell_volume                     2055.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3127
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      26.33

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             956
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9250
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_process_details   'SADABS 2004 Bruker AXS, Madison, WI'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker Apex II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24409
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         29.81
_reflns_number_total             9039
_reflns_number_gt                6052
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2'
_computing_cell_refinement       'Bruker SAINTv7.34a'
_computing_data_reduction        'Bruker SAINTv7.34a'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_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)+(0.0679P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9039
_refine_ls_number_parameters     608
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1598
_refine_ls_wR_factor_gt          0.1400
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_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
S1 S 0.51517(7) 0.37514(4) 0.19259(4) 0.02030(16) Uani 1 1 d . . .
O8 O 0.4994(2) 0.60651(13) 0.09494(12) 0.0247(4) Uani 1 1 d . . .
H8 H 0.5477 0.5741 0.1291 0.030 Uiso 1 1 calc R . .
O10 O 0.19831(19) 0.81685(14) -0.10443(12) 0.0255(4) Uani 1 1 d . . .
H10 H 0.2736 0.7996 -0.0838 0.031 Uiso 1 1 calc R . .
O4 O 0.16586(18) 0.61850(12) 0.58930(12) 0.0208(4) Uani 1 1 d . . .
H4 H 0.1930 0.5668 0.6060 0.025 Uiso 1 1 calc R . .
O11 O -0.07821(19) 0.74779(14) -0.12490(12) 0.0276(4) Uani 1 1 d . . .
H11 H -0.0200 0.7419 -0.1612 0.033 Uiso 1 1 calc R . .
O12 O -0.23375(18) 0.76765(13) 0.01083(12) 0.0241(4) Uani 1 1 d . . .
H12 H -0.2526 0.7400 -0.0403 0.029 Uiso 1 1 calc R . .
O9 O 0.4062(2) 0.74403(13) -0.00562(12) 0.0255(4) Uani 1 1 d . . .
H9 H 0.4573 0.7053 -0.0230 0.031 Uiso 1 1 calc R . .
O2 O -0.17780(19) 0.53044(12) 0.29478(12) 0.0233(4) Uani 1 1 d . . .
H2 H -0.2388 0.5231 0.2507 0.028 Uiso 1 1 calc R . .
O6 O 0.59840(18) 0.64399(12) 0.46821(12) 0.0223(4) Uani 1 1 d . . .
H6 H 0.5900 0.5846 0.4733 0.027 Uiso 1 1 calc R . .
O1 O -0.21417(19) 0.65009(12) 0.15920(11) 0.0220(4) Uani 1 1 d . . .
H1 H -0.2313 0.6934 0.1233 0.026 Uiso 1 1 calc R . .
O7 O 0.55895(19) 0.62996(12) 0.27764(12) 0.0225(4) Uani 1 1 d . . .
H7 H 0.5925 0.6482 0.3303 0.027 Uiso 1 1 calc R . .
O5 O 0.41224(19) 0.54720(12) 0.57106(12) 0.0207(4) Uani 1 1 d . . .
H5 H 0.4540 0.5598 0.6229 0.025 Uiso 1 1 calc R . .
O15 O 0.41889(19) 0.34011(13) 0.11624(12) 0.0260(4) Uani 1 1 d . . .
O14 O 0.4472(2) 0.39994(13) 0.26998(12) 0.0258(4) Uani 1 1 d . . .
O16 O 0.61871(19) 0.44684(13) 0.16976(12) 0.0252(4) Uani 1 1 d . . .
O13 O 0.60118(18) 0.29060(12) 0.22231(12) 0.0241(4) Uani 1 1 d . . .
O3 O -0.0506(2) 0.58460(12) 0.45205(12) 0.0239(4) Uani 1 1 d . . .
H3 H 0.0112 0.6026 0.4940 0.029 Uiso 1 1 calc R . .
C2 C -0.1038(3) 0.78692(17) 0.25467(17) 0.0186(5) Uani 1 1 d . . .
C19 C 0.4348(3) 0.76116(18) 0.08658(17) 0.0203(5) Uani 1 1 d . . .
C25 C -0.0154(3) 0.79565(18) -0.04691(17) 0.0229(6) Uani 1 1 d . . .
C1 C -0.0302(3) 0.81381(18) 0.33807(17) 0.0195(5) Uani 1 1 d . . .
H13 H 0.0047 0.8790 0.3490 0.023 Uiso 1 1 calc R . .
C18 C 0.4846(3) 0.69078(18) 0.13915(18) 0.0209(5) Uani 1 1 d . . .
C26 C -0.0982(3) 0.80532(18) 0.02155(17) 0.0212(5) Uani 1 1 d . . .
C28 C -0.1342(3) 0.85728(18) 0.18091(17) 0.0207(5) Uani 1 1 d . . .
H28 H -0.2308 0.8389 0.1542 0.025 Uiso 1 1 calc R . .
C17 C 0.5148(3) 0.70620(17) 0.23173(17) 0.0192(5) Uani 1 1 d . . .
C22 C 0.0942(3) 0.88339(17) 0.11632(17) 0.0203(5) Uani 1 1 d . . .
H22 H 0.1323 0.9125 0.1730 0.024 Uiso 1 1 calc R . .
C21 C 0.3303(3) 0.91372(18) 0.06528(18) 0.0217(5) Uani 1 1 d . . .
H21 H 0.3676 0.9122 0.0055 0.026 Uiso 1 1 calc R . .
C24 C 0.1215(3) 0.83124(18) -0.03385(17) 0.0214(5) Uani 1 1 d . . .
C23 C 0.1785(3) 0.87659(18) 0.04824(17) 0.0203(5) Uani 1 1 d . . .
C8 C 0.3182(3) 0.79073(18) 0.44040(17) 0.0199(5) Uani 1 1 d . . .
H16 H 0.2956 0.8456 0.4090 0.024 Uiso 1 1 calc R . .
C20 C 0.4050(3) 0.84551(18) 0.12534(17) 0.0192(5) Uani 1 1 d . . .
C14 C 0.5448(3) 0.81083(17) 0.37398(17) 0.0206(5) Uani 1 1 d . . .
H14 H 0.6328 0.7825 0.3862 0.025 Uiso 1 1 calc R . .
C16 C 0.4982(3) 0.79355(18) 0.27274(17) 0.0194(5) Uani 1 1 d . . .
C15 C 0.4400(3) 0.86060(18) 0.21832(17) 0.0196(5) Uani 1 1 d . . .
H15 H 0.4234 0.9190 0.2457 0.024 Uiso 1 1 calc R . .
C11 C 0.3833(3) 0.63110(16) 0.53073(16) 0.0170(5) Uani 1 1 d . . .
C27 C -0.0447(3) 0.84900(17) 0.10468(17) 0.0199(5) Uani 1 1 d . . .
C4 C -0.1307(3) 0.62528(17) 0.30759(17) 0.0196(5) Uani 1 1 d . . .
C6 C -0.0050(3) 0.74994(18) 0.40641(17) 0.0197(5) Uani 1 1 d . . .
C7 C 0.0824(3) 0.77946(17) 0.49530(17) 0.0193(5) Uani 1 1 d . . .
H17 H 0.0381 0.7445 0.5441 0.023 Uiso 1 1 calc R . .
C3 C -0.1497(3) 0.69025(18) 0.23955(17) 0.0194(5) Uani 1 1 d . . .
C12 C 0.4756(3) 0.67772(18) 0.47765(16) 0.0187(5) Uani 1 1 d . . .
C9 C 0.2235(3) 0.74534(17) 0.49316(16) 0.0179(5) Uani 1 1 d . . .
C10 C 0.2587(3) 0.66509(17) 0.53839(16) 0.0183(5) Uani 1 1 d . . .
C5 C -0.0593(3) 0.65478(18) 0.39039(17) 0.0196(5) Uani 1 1 d . . .
C30 C 0.5749(3) 0.91622(18) 0.40331(18) 0.0243(6) Uani 1 1 d . . .
H30A H 0.6428 0.9477 0.3671 0.036 Uiso 1 1 calc R . .
H30B H 0.6107 0.9219 0.4675 0.036 Uiso 1 1 calc R . .
H30C H 0.4906 0.9466 0.3941 0.036 Uiso 1 1 calc R . .
C29 C 0.0909(3) 0.88564(18) 0.51965(18) 0.0240(6) Uani 1 1 d . . .
H29A H 0.1401 0.9223 0.4757 0.036 Uiso 1 1 calc R . .
H29B H 0.1396 0.8985 0.5803 0.036 Uiso 1 1 calc R . .
H29C H -0.0016 0.9043 0.5186 0.036 Uiso 1 1 calc R . .
C13 C 0.4447(3) 0.75860(17) 0.43202(16) 0.0185(5) Uani 1 1 d . . .
C32 C -0.1252(3) 0.96022(18) 0.21683(18) 0.0251(6) Uani 1 1 d . . .
H32A H -0.0308 0.9821 0.2413 0.038 Uiso 1 1 calc R . .
H32B H -0.1853 0.9637 0.2648 0.038 Uiso 1 1 calc R . .
H32C H -0.1538 1.0009 0.1675 0.038 Uiso 1 1 calc R . .
C40 C 0.5232(3) 0.2089(2) 0.2578(2) 0.0384(8) Uani 1 1 d . . .
H40A H 0.4468 0.1831 0.2124 0.046 Uiso 1 1 calc R . .
H40B H 0.4843 0.2287 0.3130 0.046 Uiso 1 1 calc R . .
C31 C 0.3525(3) 1.01713(18) 0.10029(19) 0.0259(6) Uani 1 1 d . . .
H31A H 0.3162 1.0218 0.1588 0.039 Uiso 1 1 calc R . .
H31B H 0.3050 1.0567 0.0570 0.039 Uiso 1 1 calc R . .
H31C H 0.4504 1.0394 0.1076 0.039 Uiso 1 1 calc R . .
C41 C 0.6143(4) 0.1353(2) 0.2794(2) 0.0452(9) Uani 1 1 d . . .
H41A H 0.6547 0.1176 0.2250 0.068 Uiso 1 1 calc R . .
H41B H 0.5618 0.0790 0.3010 0.068 Uiso 1 1 calc R . .
H41C H 0.6870 0.1602 0.3266 0.068 Uiso 1 1 calc R . .
N1 N 0.2008(2) 0.56312(17) 0.22921(16) 0.0298(6) Uani 1 1 d . . .
N2 N 0.1799(2) 0.54871(18) 0.08362(16) 0.0307(6) Uani 1 1 d . . .
C33 C 0.2153(3) 0.5058(2) 0.1594(2) 0.0356(7) Uani 1 1 d . A .
H33 H 0.2459 0.4445 0.1633 0.043 Uiso 1 1 calc R . .
C35 C 0.1550(3) 0.6443(2) 0.1974(2) 0.0321(7) Uani 1 1 d . A .
H35 H 0.1355 0.6969 0.2328 0.039 Uiso 1 1 calc R . .
C38 C 0.1912(4) 0.5106(3) -0.0073(2) 0.0473(9) Uani 0.80 1 d P A 1
H38A H 0.2871 0.5193 -0.0193 0.071 Uiso 0.80 1 calc PR A 1
H38B H 0.1365 0.5445 -0.0520 0.071 Uiso 0.80 1 calc PR A 1
H38C H 0.1575 0.4425 -0.0115 0.071 Uiso 0.80 1 calc PR A 1
C34 C 0.1426(3) 0.6366(2) 0.1069(2) 0.0347(7) Uani 1 1 d . A .
H34 H 0.1134 0.6831 0.0663 0.042 Uiso 1 1 calc R . .
C36 C 0.2342(4) 0.5444(3) 0.3240(2) 0.0448(9) Uani 0.80 1 d P B 1
H36A H 0.3339 0.5420 0.3363 0.054 Uiso 0.80 1 calc PR B 1
H36B H 0.2101 0.5975 0.3615 0.054 Uiso 0.80 1 calc PR B 1
C37 C 0.1646(4) 0.4578(3) 0.3491(3) 0.0394(10) Uani 0.80 1 d P B 1
H37A H 0.0659 0.4611 0.3400 0.059 Uiso 0.80 1 calc PR B 1
H37B H 0.1923 0.4473 0.4130 0.059 Uiso 0.80 1 calc PR B 1
H37C H 0.1875 0.4051 0.3118 0.059 Uiso 0.80 1 calc PR B 1
N3 N 0.2516(3) 0.0328(2) 0.34108(19) 0.0441(7) Uani 1 1 d . . .
C42 C 0.2306(3) 0.1088(3) 0.3498(2) 0.0384(8) Uani 1 1 d . . .
C43 C 0.2032(4) 0.2086(3) 0.3602(3) 0.0678(13) Uani 1 1 d . . .
H43A H 0.2581 0.2486 0.3215 0.102 Uiso 1 1 calc R . .
H43B H 0.2271 0.2306 0.4235 0.102 Uiso 1 1 calc R . .
H43C H 0.1060 0.2131 0.3426 0.102 Uiso 1 1 calc R . .
O17 O 0.9181(3) 0.2705(3) 0.2659(2) 0.0484(8) Uani 0.75 1 d P C 1
O17A O 0.9169(9) 0.3509(8) 0.2157(8) 0.055(3) Uani 0.25 1 d P D 2
C39 C 0.1207(15) 0.5666(9) -0.0751(9) 0.023(3) Uani 0.20 1 d P A 2
H39A H 0.0326 0.5791 -0.0558 0.035 Uiso 0.20 1 calc PR A 2
H39B H 0.1054 0.5309 -0.1333 0.035 Uiso 0.20 1 calc PR A 2
H39C H 0.1768 0.6272 -0.0815 0.035 Uiso 0.20 1 calc PR A 2
C36A C 0.2342(4) 0.5444(3) 0.3240(2) 0.0448(9) Uani 0.20 1 d P B 2
H18 H 0.2086 0.4768 0.3341 0.067 Uiso 0.20 1 calc PR B 2
H19 H 0.1839 0.5834 0.3611 0.067 Uiso 0.20 1 calc PR B 2
H36C H 0.3325 0.5606 0.3408 0.067 Uiso 0.20 1 calc PR B 2
C38A C 0.1912(4) 0.5106(3) -0.0073(2) 0.0473(9) Uani 0.20 1 d P A 2
H38D H 0.2887 0.5129 -0.0172 0.057 Uiso 0.20 1 calc PR A 2
H38E H 0.1502 0.4432 -0.0134 0.057 Uiso 0.20 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
S1 O16 1.4320(19) . ?
S1 O15 1.4429(19) . ?
S1 O14 1.4495(19) . ?
S1 O13 1.5872(19) . ?
O8 C18 1.376(3) . ?
O8 H8 0.8400 . ?
O10 C24 1.385(3) . ?
O10 H10 0.8400 . ?
O4 C10 1.375(3) . ?
O4 H4 0.8400 . ?
O11 C25 1.380(3) . ?
O11 H11 0.8400 . ?
O12 C26 1.379(3) . ?
O12 H12 0.8400 . ?
O9 C19 1.381(3) . ?
O9 H9 0.8400 . ?
O2 C4 1.370(3) . ?
O2 H2 0.8400 . ?
O6 C12 1.375(3) . ?
O6 H6 0.8400 . ?
O1 C3 1.372(3) . ?
O1 H1 0.8400 . ?
O7 C17 1.376(3) . ?
O7 H7 0.8400 . ?
O5 C11 1.385(3) . ?
O5 H5 0.8400 . ?
O13 C40 1.457(3) . ?
O3 C5 1.369(3) . ?
O3 H3 0.8400 . ?
C2 C1 1.392(4) . ?
C2 C3 1.395(3) . ?
C2 C28 1.526(3) . ?
C19 C18 1.381(4) . ?
C19 C20 1.387(4) . ?
C25 C24 1.385(4) . ?
C25 C26 1.388(4) . ?
C1 C6 1.396(3) . ?
C1 H13 0.9500 . ?
C18 C17 1.385(4) . ?
C26 C27 1.394(4) . ?
C28 C27 1.523(4) . ?
C28 C32 1.527(4) . ?
C28 H28 1.0000 . ?
C17 C16 1.398(3) . ?
C22 C23 1.388(4) . ?
C22 C27 1.398(4) . ?
C22 H22 0.9500 . ?
C21 C31 1.523(4) . ?
C21 C20 1.527(3) . ?
C21 C23 1.530(4) . ?
C21 H21 1.0000 . ?
C24 C23 1.398(4) . ?
C8 C13 1.397(4) . ?
C8 C9 1.398(4) . ?
C8 H16 0.9500 . ?
C20 C15 1.395(3) . ?
C14 C13 1.524(3) . ?
C14 C30 1.529(3) . ?
C14 C16 1.533(4) . ?
C14 H14 1.0000 . ?
C16 C15 1.394(3) . ?
C15 H15 0.9500 . ?
C11 C10 1.388(4) . ?
C11 C12 1.392(4) . ?
C4 C5 1.384(4) . ?
C4 C3 1.394(3) . ?
C6 C5 1.395(3) . ?
C6 C7 1.524(3) . ?
C7 C29 1.525(3) . ?
C7 C9 1.532(4) . ?
C7 H17 1.0000 . ?
C12 C13 1.389(3) . ?
C9 C10 1.390(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C40 C41 1.470(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
N1 C33 1.331(4) . ?
N1 C35 1.357(4) . ?
N1 C36 1.450(4) . ?
N2 C33 1.325(4) . ?
N2 C34 1.382(4) . ?
N2 C38 1.464(4) . ?
C33 H33 0.9500 . ?
C35 C34 1.339(5) . ?
C35 H35 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C34 H34 0.9500 . ?
C36 C37 1.414(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
N3 C42 1.123(4) . ?
C42 C43 1.473(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 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
O16 S1 O15 113.26(12) . . ?
O16 S1 O14 114.66(11) . . ?
O15 S1 O14 111.91(11) . . ?
O16 S1 O13 102.21(11) . . ?
O15 S1 O13 107.36(11) . . ?
O14 S1 O13 106.44(11) . . ?
C18 O8 H8 109.5 . . ?
C24 O10 H10 109.5 . . ?
C10 O4 H4 109.5 . . ?
C25 O11 H11 109.5 . . ?
C26 O12 H12 109.5 . . ?
C19 O9 H9 109.5 . . ?
C4 O2 H2 109.5 . . ?
C12 O6 H6 109.5 . . ?
C3 O1 H1 109.5 . . ?
C17 O7 H7 109.5 . . ?
C11 O5 H5 109.5 . . ?
C40 O13 S1 114.90(18) . . ?
C5 O3 H3 109.5 . . ?
C1 C2 C3 116.9(2) . . ?
C1 C2 C28 123.3(2) . . ?
C3 C2 C28 119.8(2) . . ?
C18 C19 O9 118.9(2) . . ?
C18 C19 C20 121.2(2) . . ?
O9 C19 C20 119.8(2) . . ?
O11 C25 C24 124.2(2) . . ?
O11 C25 C26 115.7(2) . . ?
C24 C25 C26 120.1(2) . . ?
C2 C1 C6 123.4(2) . . ?
C2 C1 H13 118.3 . . ?
C6 C1 H13 118.3 . . ?
O8 C18 C19 116.6(2) . . ?
O8 C18 C17 123.2(2) . . ?
C19 C18 C17 120.1(2) . . ?
O12 C26 C25 120.9(2) . . ?
O12 C26 C27 118.2(2) . . ?
C25 C26 C27 120.8(2) . . ?
C27 C28 C2 111.4(2) . . ?
C27 C28 C32 111.2(2) . . ?
C2 C28 C32 113.3(2) . . ?
C27 C28 H28 106.8 . . ?
C2 C28 H28 106.8 . . ?
C32 C28 H28 106.8 . . ?
O7 C17 C18 115.1(2) . . ?
O7 C17 C16 124.3(2) . . ?
C18 C17 C16 120.6(2) . . ?
C23 C22 C27 122.5(2) . . ?
C23 C22 H22 118.8 . . ?
C27 C22 H22 118.8 . . ?
C31 C21 C20 114.3(2) . . ?
C31 C21 C23 111.8(2) . . ?
C20 C21 C23 109.6(2) . . ?
C31 C21 H21 106.9 . . ?
C20 C21 H21 106.9 . . ?
C23 C21 H21 106.9 . . ?
C25 C24 O10 116.8(2) . . ?
C25 C24 C23 120.7(2) . . ?
O10 C24 C23 122.4(2) . . ?
C22 C23 C24 118.0(2) . . ?
C22 C23 C21 120.3(2) . . ?
C24 C23 C21 121.7(2) . . ?
C13 C8 C9 122.6(2) . . ?
C13 C8 H16 118.7 . . ?
C9 C8 H16 118.7 . . ?
C19 C20 C15 117.4(2) . . ?
C19 C20 C21 118.5(2) . . ?
C15 C20 C21 124.0(2) . . ?
C13 C14 C30 110.9(2) . . ?
C13 C14 C16 111.7(2) . . ?
C30 C14 C16 113.9(2) . . ?
C13 C14 H14 106.6 . . ?
C30 C14 H14 106.6 . . ?
C16 C14 H14 106.6 . . ?
C15 C16 C17 117.5(2) . . ?
C15 C16 C14 123.6(2) . . ?
C17 C16 C14 118.9(2) . . ?
C16 C15 C20 122.8(2) . . ?
C16 C15 H15 118.6 . . ?
C20 C15 H15 118.6 . . ?
O5 C11 C10 120.0(2) . . ?
O5 C11 C12 119.7(2) . . ?
C10 C11 C12 120.1(2) . . ?
C26 C27 C22 117.9(2) . . ?
C26 C27 C28 120.9(2) . . ?
C22 C27 C28 121.1(2) . . ?
O2 C4 C5 117.6(2) . . ?
O2 C4 C3 121.9(2) . . ?
C5 C4 C3 120.4(2) . . ?
C5 C6 C1 117.9(2) . . ?
C5 C6 C7 119.4(2) . . ?
C1 C6 C7 122.7(2) . . ?
C6 C7 C29 113.6(2) . . ?
C6 C7 C9 109.3(2) . . ?
C29 C7 C9 112.5(2) . . ?
C6 C7 H17 107.0 . . ?
C29 C7 H17 107.0 . . ?
C9 C7 H17 107.0 . . ?
O1 C3 C4 114.2(2) . . ?
O1 C3 C2 124.8(2) . . ?
C4 C3 C2 121.0(2) . . ?
O6 C12 C13 118.6(2) . . ?
O6 C12 C11 120.8(2) . . ?
C13 C12 C11 120.6(2) . . ?
C10 C9 C8 117.6(2) . . ?
C10 C9 C7 121.6(2) . . ?
C8 C9 C7 120.6(2) . . ?
O4 C10 C11 120.5(2) . . ?
O4 C10 C9 118.4(2) . . ?
C11 C10 C9 121.0(2) . . ?
O3 C5 C4 114.7(2) . . ?
O3 C5 C6 125.1(2) . . ?
C4 C5 C6 120.2(2) . . ?
C14 C30 H30A 109.5 . . ?
C14 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C14 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C7 C29 H29A 109.5 . . ?
C7 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C7 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C12 C13 C8 118.0(2) . . ?
C12 C13 C14 121.3(2) . . ?
C8 C13 C14 120.7(2) . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O13 C40 C41 108.9(3) . . ?
O13 C40 H40A 109.9 . . ?
C41 C40 H40A 109.9 . . ?
O13 C40 H40B 109.9 . . ?
C41 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
C21 C31 H31A 109.5 . . ?
C21 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C21 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C33 N1 C35 108.9(3) . . ?
C33 N1 C36 125.9(3) . . ?
C35 N1 C36 125.1(3) . . ?
C33 N2 C34 107.8(3) . . ?
C33 N2 C38 124.5(3) . . ?
C34 N2 C38 127.5(3) . . ?
N2 C33 N1 108.5(3) . . ?
N2 C33 H33 125.7 . . ?
N1 C33 H33 125.7 . . ?
C34 C35 N1 107.3(3) . . ?
C34 C35 H35 126.3 . . ?
N1 C35 H35 126.3 . . ?
N2 C38 H38A 109.5 . . ?
N2 C38 H38B 109.5 . . ?
N2 C38 H38C 109.5 . . ?
C35 C34 N2 107.4(3) . . ?
C35 C34 H34 126.3 . . ?
N2 C34 H34 126.3 . . ?
C37 C36 N1 112.3(3) . . ?
C37 C36 H36A 109.1 . . ?
N1 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
N1 C36 H36B 109.1 . . ?
H36A C36 H36B 107.9 . . ?
N3 C42 C43 179.4(4) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O16 S1 O13 C40 174.6(2) . . . . ?
O15 S1 O13 C40 -66.0(2) . . . . ?
O14 S1 O13 C40 54.0(2) . . . . ?
C3 C2 C1 C6 -2.1(4) . . . . ?
C28 C2 C1 C6 178.4(2) . . . . ?
O9 C19 C18 O8 -1.4(4) . . . . ?
C20 C19 C18 O8 174.4(2) . . . . ?
O9 C19 C18 C17 179.7(2) . . . . ?
C20 C19 C18 C17 -4.6(4) . . . . ?
O11 C25 C26 O12 0.8(4) . . . . ?
C24 C25 C26 O12 -177.9(2) . . . . ?
O11 C25 C26 C27 177.4(2) . . . . ?
C24 C25 C26 C27 -1.3(4) . . . . ?
C1 C2 C28 C27 104.8(3) . . . . ?
C3 C2 C28 C27 -74.6(3) . . . . ?
C1 C2 C28 C32 -21.4(3) . . . . ?
C3 C2 C28 C32 159.1(2) . . . . ?
O8 C18 C17 O7 -1.2(4) . . . . ?
C19 C18 C17 O7 177.7(2) . . . . ?
O8 C18 C17 C16 179.7(2) . . . . ?
C19 C18 C17 C16 -1.4(4) . . . . ?
O11 C25 C24 O10 -0.1(4) . . . . ?
C26 C25 C24 O10 178.5(2) . . . . ?
O11 C25 C24 C23 -178.2(2) . . . . ?
C26 C25 C24 C23 0.5(4) . . . . ?
C27 C22 C23 C24 -1.7(4) . . . . ?
C27 C22 C23 C21 -178.8(2) . . . . ?
C25 C24 C23 C22 1.0(4) . . . . ?
O10 C24 C23 C22 -176.9(2) . . . . ?
C25 C24 C23 C21 178.1(2) . . . . ?
O10 C24 C23 C21 0.2(4) . . . . ?
C31 C21 C23 C22 -53.8(3) . . . . ?
C20 C21 C23 C22 74.0(3) . . . . ?
C31 C21 C23 C24 129.2(3) . . . . ?
C20 C21 C23 C24 -103.0(3) . . . . ?
C18 C19 C20 C15 6.3(4) . . . . ?
O9 C19 C20 C15 -178.0(2) . . . . ?
C18 C19 C20 C21 -170.9(2) . . . . ?
O9 C19 C20 C21 4.9(4) . . . . ?
C31 C21 C20 C19 -156.2(2) . . . . ?
C23 C21 C20 C19 77.4(3) . . . . ?
C31 C21 C20 C15 26.8(4) . . . . ?
C23 C21 C20 C15 -99.6(3) . . . . ?
O7 C17 C16 C15 -173.8(2) . . . . ?
C18 C17 C16 C15 5.2(4) . . . . ?
O7 C17 C16 C14 6.4(4) . . . . ?
C18 C17 C16 C14 -174.6(2) . . . . ?
C13 C14 C16 C15 104.0(3) . . . . ?
C30 C14 C16 C15 -22.6(3) . . . . ?
C13 C14 C16 C17 -76.3(3) . . . . ?
C30 C14 C16 C17 157.1(2) . . . . ?
C17 C16 C15 C20 -3.3(4) . . . . ?
C14 C16 C15 C20 176.4(2) . . . . ?
C19 C20 C15 C16 -2.3(4) . . . . ?
C21 C20 C15 C16 174.7(2) . . . . ?
O12 C26 C27 C22 177.3(2) . . . . ?
C25 C26 C27 C22 0.6(4) . . . . ?
O12 C26 C27 C28 -1.6(3) . . . . ?
C25 C26 C27 C28 -178.3(2) . . . . ?
C23 C22 C27 C26 0.9(4) . . . . ?
C23 C22 C27 C28 179.8(2) . . . . ?
C2 C28 C27 C26 105.5(3) . . . . ?
C32 C28 C27 C26 -127.1(2) . . . . ?
C2 C28 C27 C22 -73.3(3) . . . . ?
C32 C28 C27 C22 54.1(3) . . . . ?
C2 C1 C6 C5 -1.3(4) . . . . ?
C2 C1 C6 C7 176.5(2) . . . . ?
C5 C6 C7 C29 -158.6(2) . . . . ?
C1 C6 C7 C29 23.6(3) . . . . ?
C5 C6 C7 C9 74.8(3) . . . . ?
C1 C6 C7 C9 -103.1(3) . . . . ?
O2 C4 C3 O1 -2.3(3) . . . . ?
C5 C4 C3 O1 175.8(2) . . . . ?
O2 C4 C3 C2 178.4(2) . . . . ?
C5 C4 C3 C2 -3.4(4) . . . . ?
C1 C2 C3 O1 -174.7(2) . . . . ?
C28 C2 C3 O1 4.8(4) . . . . ?
C1 C2 C3 C4 4.5(4) . . . . ?
C28 C2 C3 C4 -176.0(2) . . . . ?
O5 C11 C12 O6 -3.1(4) . . . . ?
C10 C11 C12 O6 -178.9(2) . . . . ?
O5 C11 C12 C13 175.9(2) . . . . ?
C10 C11 C12 C13 0.2(4) . . . . ?
C13 C8 C9 C10 -0.1(4) . . . . ?
C13 C8 C9 C7 -176.0(2) . . . . ?
C6 C7 C9 C10 -102.3(3) . . . . ?
C29 C7 C9 C10 130.4(2) . . . . ?
C6 C7 C9 C8 73.4(3) . . . . ?
C29 C7 C9 C8 -53.8(3) . . . . ?
O5 C11 C10 O4 3.0(4) . . . . ?
C12 C11 C10 O4 178.8(2) . . . . ?
O5 C11 C10 C9 -175.3(2) . . . . ?
C12 C11 C10 C9 0.4(4) . . . . ?
C8 C9 C10 O4 -178.8(2) . . . . ?
C7 C9 C10 O4 -3.0(3) . . . . ?
C8 C9 C10 C11 -0.4(4) . . . . ?
C7 C9 C10 C11 175.4(2) . . . . ?
O2 C4 C5 O3 -3.2(3) . . . . ?
C3 C4 C5 O3 178.5(2) . . . . ?
O2 C4 C5 C6 178.0(2) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C1 C6 C5 O3 -176.1(2) . . . . ?
C7 C6 C5 O3 6.0(4) . . . . ?
C1 C6 C5 C4 2.6(4) . . . . ?
C7 C6 C5 C4 -175.4(2) . . . . ?
O6 C12 C13 C8 178.4(2) . . . . ?
C11 C12 C13 C8 -0.6(4) . . . . ?
O6 C12 C13 C14 -1.2(4) . . . . ?
C11 C12 C13 C14 179.7(2) . . . . ?
C9 C8 C13 C12 0.6(4) . . . . ?
C9 C8 C13 C14 -179.7(2) . . . . ?
C30 C14 C13 C12 -125.3(3) . . . . ?
C16 C14 C13 C12 106.5(3) . . . . ?
C30 C14 C13 C8 55.0(3) . . . . ?
C16 C14 C13 C8 -73.2(3) . . . . ?
S1 O13 C40 C41 178.0(2) . . . . ?
C34 N2 C33 N1 0.4(4) . . . . ?
C38 N2 C33 N1 175.7(3) . . . . ?
C35 N1 C33 N2 0.1(4) . . . . ?
C36 N1 C33 N2 -177.3(3) . . . . ?
C33 N1 C35 C34 -0.5(3) . . . . ?
C36 N1 C35 C34 176.9(3) . . . . ?
N1 C35 C34 N2 0.7(3) . . . . ?
C33 N2 C34 C35 -0.7(3) . . . . ?
C38 N2 C34 C35 -175.8(3) . . . . ?
C33 N1 C36 C37 -56.6(4) . . . . ?
C35 N1 C36 C37 126.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        29.81
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 986743'
#######################################################################
#
#                 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_C:\xtals\ALS\work2\3DFMJ12.CIF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            3DFMJ12
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C36 H40 O12), 2(C6 H11 N2), O4 S, C3 H6 O, 7(H2 O)'
_chemical_formula_sum            'C87 H122 N4 O36 S'
_chemical_formula_weight         1831.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0017 '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 -0.0031 0.0035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1098 0.1311 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Cc

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'

_cell_length_a                   19.3218(16)
_cell_length_b                   14.7252(12)
_cell_length_c                   32.896(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.855(2)
_cell_angle_gamma                90.00
_cell_volume                     9046.6(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9536
_cell_measurement_theta_min      29.16
_cell_measurement_theta_max      2.88

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3904
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9843
_exptl_absorpt_correction_T_max  0.9934
_exptl_absorpt_process_details   'SADABS 2004 Bruker AXS, Madison, WI'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker Apex II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52016
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.1205
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         31.51
_reflns_number_total             26670
_reflns_number_gt                19850
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2'
_computing_cell_refinement       'Bruker SAINTv7.34a'
_computing_data_reduction        'Bruker SAINTv7.34a'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_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)+(0.1181P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(8)
_refine_ls_number_reflns         26670
_refine_ls_number_parameters     1300
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.2276
_refine_ls_wR_factor_gt          0.2043
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.011
_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 0.09472(11) 0.58195(17) 0.51738(8) 0.0369(5) Uani 1 1 d . . .
H1 H 0.0538 0.5609 0.5063 0.044 Uiso 1 1 calc R . .
C1 C 0.18487(15) 0.45409(19) 0.44995(9) 0.0276(5) Uani 1 1 d . . .
H25 H 0.1749 0.4215 0.4242 0.033 Uiso 1 1 calc R . .
O1A O 0.0944(6) 0.3852(8) 0.8196(3) 0.105(3) Uani 0.50 1 d P A 1
O1A' O -0.0810(6) 0.2978(7) 0.8095(4) 0.108(3) Uani 0.50 1 d PU B 1
N1I N 0.66582(19) 0.7773(2) 0.93701(11) 0.0460(7) Uani 1 1 d . . .
C1I C 0.6428(2) 0.7527(3) 0.96991(13) 0.0502(9) Uani 1 1 d . . .
H1I H 0.6716 0.7441 0.9978 0.060 Uiso 1 1 calc R . .
S1S S 0.64763(4) 0.27688(5) 0.60565(3) 0.03336(15) Uani 1 1 d . . .
O1S O 0.64612(13) 0.17708(14) 0.60456(7) 0.0342(4) Uani 1 1 d . . .
O1W O 0.38517(15) 0.6350(2) 0.59436(9) 0.0502(6) Uani 1 1 d . . .
O2 O 0.23155(12) 0.58794(18) 0.56340(8) 0.0413(5) Uani 1 1 d . . .
H2 H 0.1939 0.6040 0.5697 0.050 Uiso 1 1 calc R . .
C2 C 0.12816(14) 0.49281(19) 0.46261(9) 0.0267(5) Uani 1 1 d . . .
C2A C 0.0608(6) 0.2908(7) 0.7592(5) 0.078(3) Uani 0.50 1 d P A 1
H2A1 H 0.1056 0.2561 0.7670 0.117 Uiso 0.50 1 calc PR A 1
H2A2 H 0.0496 0.3058 0.7292 0.117 Uiso 0.50 1 calc PR A 1
H2A3 H 0.0219 0.2544 0.7649 0.117 Uiso 0.50 1 calc PR A 1
C2A' C -0.2025(9) 0.2896(19) 0.7990(6) 0.149(9) Uani 0.50 1 d PU B 1
H2A4 H -0.1914 0.2553 0.8254 0.224 Uiso 0.50 1 calc PR B 1
H2A5 H -0.2334 0.2531 0.7767 0.224 Uiso 0.50 1 calc PR B 1
H2A6 H -0.2272 0.3460 0.8026 0.224 Uiso 0.50 1 calc PR B 1
N2I N 0.5725(2) 0.7422(3) 0.95710(12) 0.0596(9) Uani 1 1 d . . .
C2I C 0.6079(2) 0.7831(3) 0.90248(14) 0.0492(8) Uani 1 1 d . . .
H2I H 0.6093 0.7994 0.8748 0.059 Uiso 1 1 calc R . .
O2S O 0.66654(17) 0.31193(19) 0.56913(9) 0.0525(7) Uani 1 1 d . . .
O2W O 0.53296(15) 0.5990(2) 0.60988(9) 0.0553(7) Uani 1 1 d . . .
O3 O 0.33884(11) 0.51554(17) 0.53492(8) 0.0402(5) Uani 1 1 d . . .
H3 H 0.3471 0.5695 0.5430 0.048 Uiso 1 1 calc R . .
C3 C 0.14423(14) 0.53940(19) 0.50073(9) 0.0285(5) Uani 1 1 d . . .
C3A C 0.0690(6) 0.3750(7) 0.7841(3) 0.060(2) Uani 0.50 1 d P A 1
C3A' C -0.1414(6) 0.3096(6) 0.7885(3) 0.064(2) Uani 0.50 1 d PU B 1
N3H N 0.2653(7) 0.2919(8) 0.6019(4) 0.058(3) Uani 0.30 1 d PDU C 2
N3I N 0.3032(2) 0.3291(3) 0.62711(12) 0.0347(8) Uani 0.70 1 d PU D 1
C3I C 0.5489(2) 0.7614(3) 0.91511(13) 0.0519(9) Uani 1 1 d . . .
H3I H 0.5009 0.7598 0.8983 0.062 Uiso 1 1 calc R . .
O3S O 0.70149(13) 0.30512(18) 0.64464(8) 0.0426(5) Uani 1 1 d . . .
O3W O 0.79516(15) 0.42512(19) 0.62064(9) 0.0479(6) Uani 1 1 d . . .
O4 O 0.43420(13) 0.38275(16) 0.53558(9) 0.0459(6) Uani 1 1 d . . .
H4 H 0.4106 0.4303 0.5365 0.055 Uiso 1 1 d . . .
C4 C 0.21439(15) 0.5464(2) 0.52507(9) 0.0302(5) Uani 1 1 d . . .
C4A C 0.0338(9) 0.4517(8) 0.7553(8) 0.126(8) Uani 0.50 1 d P A 1
H4A1 H -0.0056 0.4769 0.7655 0.189 Uiso 0.50 1 calc PR A 1
H4A2 H 0.0151 0.4283 0.7267 0.189 Uiso 0.50 1 calc PR A 1
H4A3 H 0.0692 0.4993 0.7552 0.189 Uiso 0.50 1 calc PR A 1
C4A' C -0.1576(11) 0.3557(15) 0.7458(7) 0.125(6) Uani 0.50 1 d PU B 1
H4A4 H -0.1950 0.4015 0.7441 0.187 Uiso 0.50 1 calc PR B 1
H4A5 H -0.1740 0.3103 0.7236 0.187 Uiso 0.50 1 calc PR B 1
H4A6 H -0.1141 0.3851 0.7420 0.187 Uiso 0.50 1 calc PR B 1
N4H N 0.3653(7) 0.3481(8) 0.6387(5) 0.071(4) Uani 0.30 1 d PDU C 2
N4I N 0.2103(3) 0.3087(4) 0.57628(14) 0.0508(12) Uani 0.70 1 d PU D 1
C4I C 0.7410(2) 0.7909(3) 0.93778(16) 0.0554(10) Uani 1 1 d . . .
H4I1 H 0.7457 0.8462 0.9216 0.067 Uiso 1 1 calc R . .
H4I2 H 0.7692 0.8001 0.9672 0.067 Uiso 1 1 calc R . .
O4S O 0.57870(15) 0.3137(2) 0.60860(12) 0.0611(8) Uani 1 1 d . . .
O4W O 0.29802(16) 0.77273(19) 0.54094(9) 0.0484(6) Uani 1 1 d . . .
O5 O 0.45749(14) 0.21884(17) 0.57261(9) 0.0451(6) Uani 1 1 d . . .
H5 H 0.4880 0.2603 0.5744 0.054 Uiso 1 1 calc R . .
C5 C 0.26970(15) 0.50826(19) 0.51102(10) 0.0307(6) Uani 1 1 d . . .
C5I C 0.7698(3) 0.7132(6) 0.9199(2) 0.095(2) Uani 1 1 d . . .
H5I1 H 0.7577 0.6571 0.9325 0.143 Uiso 1 1 calc R . .
H5I2 H 0.8220 0.7189 0.9257 0.143 Uiso 1 1 calc R . .
H5I3 H 0.7491 0.7116 0.8894 0.143 Uiso 1 1 calc R . .
O5W O 0.42324(18) 0.8451(2) 0.65424(13) 0.0673(9) Uani 1 1 d . . .
O6 O 0.38408(12) 0.07419(15) 0.54119(7) 0.0336(4) Uani 1 1 d . . .
H6 H 0.3478 0.0461 0.5441 0.040 Uiso 1 1 calc R . .
C6 C 0.25555(15) 0.46102(19) 0.47339(10) 0.0296(5) Uani 1 1 d . . .
C6I C 0.5255(3) 0.7197(7) 0.98445(18) 0.099(3) Uani 1 1 d . . .
H6I1 H 0.5037 0.6600 0.9767 0.149 Uiso 1 1 calc R . .
H6I2 H 0.4877 0.7657 0.9811 0.149 Uiso 1 1 calc R . .
H6I3 H 0.5536 0.7185 1.0138 0.149 Uiso 1 1 calc R . .
O6W O 0.50181(18) 0.8893(2) 0.59848(10) 0.0621(8) Uani 1 1 d . . .
O7 O 0.25956(13) -0.00211(16) 0.54310(8) 0.0387(5) Uani 1 1 d . . .
H7 H 0.2536 -0.0214 0.5660 0.046 Uiso 1 1 calc R . .
C7 C 0.31671(18) 0.4163(2) 0.45972(11) 0.0378(7) Uani 1 1 d . . .
H26 H 0.3598 0.4548 0.4715 0.045 Uiso 1 1 calc R . .
C7I C 0.2467(3) 0.3703(3) 0.6061(2) 0.0780(17) Uani 0.70 1 d PU D 1
H7I H 0.2326 0.4308 0.6102 0.094 Uiso 0.70 1 calc PR D 1
O7W O 0.52991(16) 0.0649(2) 0.60414(12) 0.0628(9) Uani 1 1 d . . .
O8 O 0.13823(14) -0.00437(16) 0.57315(7) 0.0397(5) Uani 1 1 d . . .
H8 H 0.1118 0.0264 0.5846 0.048 Uiso 1 1 calc R . .
C8 C 0.29316(15) 0.2473(2) 0.46579(10) 0.0323(6) Uani 1 1 d . . .
H27 H 0.2543 0.2535 0.4415 0.039 Uiso 1 1 calc R . .
C8H C 0.3342(8) 0.2772(11) 0.6158(5) 0.062(4) Uani 0.30 1 d PDU C 2
H8H H 0.3584 0.2241 0.6105 0.074 Uiso 0.30 1 calc PR C 2
C8I C 0.3052(4) 0.2417(4) 0.6130(3) 0.0586(16) Uani 0.70 1 d PU D 1
H8I H 0.3423 0.1990 0.6235 0.070 Uiso 0.70 1 calc PR D 1
O9 O 0.01224(12) 0.07143(15) 0.52543(7) 0.0344(5) Uani 1 1 d . . .
H9 H 0.0246 0.0711 0.5518 0.041 Uiso 1 1 calc R . .
C9 C 0.33318(15) 0.3238(2) 0.48109(10) 0.0320(6) Uani 1 1 d . . .
C9H C 0.3122(8) 0.4094(11) 0.6367(6) 0.069(4) Uani 0.30 1 d PDU C 2
H9H H 0.3155 0.4654 0.6515 0.082 Uiso 0.30 1 calc PR C 2
C9I C 0.2482(4) 0.2271(6) 0.5832(3) 0.070(2) Uani 0.70 1 d PU D 1
H9I H 0.2346 0.1714 0.5687 0.084 Uiso 0.70 1 calc PR D 1
O10 O -0.09336(13) 0.19975(15) 0.49965(7) 0.0348(4) Uani 1 1 d . . .
H10 H -0.0671 0.1546 0.5081 0.042 Uiso 1 1 calc R . .
C10 C 0.38873(17) 0.3147(2) 0.51734(11) 0.0367(6) Uani 1 1 d . . .
C10H C 0.2122(10) 0.2349(11) 0.5744(5) 0.058(4) Uani 0.30 1 d PDU C 2
H10A H 0.1847 0.2023 0.5914 0.069 Uiso 0.30 1 calc PR C 2
H10B H 0.2370 0.1890 0.5612 0.069 Uiso 0.30 1 calc PR C 2
C10I C 0.3582(3) 0.3697(6) 0.6616(2) 0.0619(19) Uani 0.70 1 d PU D 1
H10C H 0.3389 0.4256 0.6713 0.074 Uiso 0.70 1 calc PR D 1
H10D H 0.3701 0.3266 0.6855 0.074 Uiso 0.70 1 calc PR D 1
O11 O -0.10584(12) 0.37822(15) 0.52109(7) 0.0316(4) Uani 1 1 d . . .
H11 H -0.1307 0.3337 0.5248 0.038 Uiso 1 1 calc R . .
C11 C 0.40380(17) 0.2308(2) 0.53707(10) 0.0360(6) Uani 1 1 d . . .
C11H C 0.1602(9) 0.2888(9) 0.5397(4) 0.039(3) Uani 0.30 1 d PU C 2
H11A H 0.1317 0.3297 0.5524 0.059 Uiso 0.30 1 calc PR C 2
H11B H 0.1283 0.2466 0.5206 0.059 Uiso 0.30 1 calc PR C 2
H11C H 0.1873 0.3244 0.5239 0.059 Uiso 0.30 1 calc PR C 2
C11I C 0.4238(4) 0.3922(7) 0.6491(3) 0.062(2) Uani 0.70 1 d PU D 1
H11D H 0.4412 0.3381 0.6374 0.093 Uiso 0.70 1 calc PR D 1
H11E H 0.4605 0.4133 0.6737 0.093 Uiso 0.70 1 calc PR D 1
H11F H 0.4135 0.4402 0.6277 0.093 Uiso 0.70 1 calc PR D 1
O12 O -0.03800(11) 0.51135(14) 0.49114(7) 0.0298(4) Uani 1 1 d . . .
H12 H -0.0659 0.5131 0.5069 0.036 Uiso 1 1 calc R . .
C12 C 0.36320(16) 0.1546(2) 0.52050(10) 0.0321(6) Uani 1 1 d . . .
C12H C 0.4422(10) 0.3527(15) 0.6556(7) 0.065(5) Uani 0.30 1 d PDU C 2
H12A H 0.4639 0.2956 0.6498 0.098 Uiso 0.30 1 calc PR C 2
H12B H 0.4533 0.3624 0.6861 0.098 Uiso 0.30 1 calc PR C 2
H12C H 0.4615 0.4031 0.6424 0.098 Uiso 0.30 1 calc PR C 2
C12I C 0.1414(6) 0.3301(11) 0.5460(5) 0.131(6) Uani 0.70 1 d PU D 1
H12D H 0.1333 0.2876 0.5223 0.196 Uiso 0.70 1 calc PR D 1
H12E H 0.1428 0.3923 0.5357 0.196 Uiso 0.70 1 calc PR D 1
H12F H 0.1025 0.3245 0.5599 0.196 Uiso 0.70 1 calc PR D 1
O13 O 0.20237(12) 0.59076(18) 0.67725(8) 0.0404(5) Uani 1 1 d . . .
H13 H 0.1995 0.6200 0.6550 0.048 Uiso 1 1 calc R . .
C13 C 0.30719(15) 0.1614(2) 0.48437(9) 0.0303(6) Uani 1 1 d . . .
O14 O 0.31221(13) 0.6865(2) 0.65306(8) 0.0451(6) Uani 1 1 d . E .
H14 H 0.3062 0.6543 0.6313 0.054 Uiso 1 1 calc R . .
C14 C 0.26387(16) 0.0777(2) 0.46596(10) 0.0324(6) Uani 1 1 d . . .
H29 H 0.2934 0.0237 0.4781 0.039 Uiso 1 1 calc R . .
O15 O 0.44660(13) 0.6665(2) 0.69494(9) 0.0488(7) Uani 1 1 d . . .
H15 H 0.4323 0.7200 0.6891 0.059 Uiso 1 1 d . . .
C15 C 0.13036(16) 0.10673(19) 0.45665(9) 0.0292(5) Uani 1 1 d . . .
H30 H 0.1286 0.1320 0.4298 0.035 Uiso 1 1 calc R . .
O16 O 0.57609(13) 0.58177(17) 0.71355(7) 0.0374(5) Uani 1 1 d . . .
H16 H 0.6073 0.5842 0.6999 0.045 Uiso 1 1 calc R . .
C16 C 0.19508(16) 0.07183(19) 0.48031(9) 0.0301(5) Uani 1 1 d . . .
O17 O 0.6450(2) 0.4465(2) 0.68473(13) 0.0747(12) Uani 1 1 d . E .
H17 H 0.6564 0.3990 0.6739 0.090 Uiso 1 1 calc R . .
C17 C 0.19638(18) 0.0331(2) 0.51923(10) 0.0346(6) Uani 1 1 d . . .
O18 O 0.63998(14) 0.26835(16) 0.71369(8) 0.0399(5) Uani 1 1 d . . .
H18 H 0.6577 0.2883 0.6947 0.048 Uiso 1 1 calc R . .
C18 C 0.13578(18) 0.03120(19) 0.53415(9) 0.0329(6) Uani 1 1 d . . .
O19 O 0.54707(13) 0.12458(18) 0.69226(8) 0.0418(5) Uani 1 1 d . . .
H19 H 0.5712 0.1726 0.6970 0.050 Uiso 1 1 calc R . .
C19 C 0.07173(16) 0.06948(18) 0.51040(9) 0.0292(5) Uani 1 1 d . . .
O20 O 0.42275(16) 0.0502(3) 0.64633(10) 0.0645(10) Uani 1 1 d . E .
H20 H 0.4446 0.0814 0.6321 0.077 Uiso 1 1 d . . .
C20 C 0.06836(16) 0.10638(18) 0.47041(8) 0.0272(5) Uani 1 1 d . . .
O21 O 0.30055(16) 0.0592(3) 0.67273(12) 0.0631(9) Uani 1 1 d . . .
H21 H 0.3100 0.0122 0.6607 0.076 Uiso 1 1 calc R . .
C21 C -0.00245(15) 0.14571(18) 0.44485(8) 0.0265(5) Uani 1 1 d . . .
H31 H -0.0415 0.1094 0.4519 0.032 Uiso 1 1 calc R . .
O22 O 0.17277(13) 0.12974(16) 0.67089(8) 0.0388(5) Uani 1 1 d . . .
H22 H 0.2095 0.0973 0.6738 0.047 Uiso 1 1 calc R . .
C22 C 0.02211(14) 0.31512(18) 0.44290(8) 0.0245(5) Uani 1 1 d . . .
H32 H 0.0526 0.3016 0.4252 0.029 Uiso 1 1 calc R . .
O23 O 0.09817(18) 0.2692(2) 0.63585(10) 0.0591(8) Uani 1 1 d . E .
H23 H 0.0579 0.2706 0.6411 0.071 Uiso 1 1 calc R . .
C23 C -0.01190(14) 0.24357(18) 0.45736(8) 0.0246(5) Uani 1 1 d . . .
O24 O 0.1182(2) 0.4375(2) 0.66918(11) 0.0743(12) Uani 1 1 d . . .
H24 H 0.1406 0.4870 0.6714 0.089 Uiso 1 1 d . . .
C24 C -0.05553(15) 0.26391(19) 0.48412(8) 0.0270(5) Uani 1 1 d . . .
C25 C -0.06505(15) 0.35398(19) 0.49453(9) 0.0268(5) Uani 1 1 d . . .
C26 C -0.03052(14) 0.42336(18) 0.47945(8) 0.0261(5) Uani 1 1 d . . .
C27 C 0.01393(14) 0.40577(18) 0.45301(8) 0.0246(5) Uani 1 1 d . . .
C28 C 0.05091(14) 0.48368(19) 0.43677(9) 0.0265(5) Uani 1 1 d . . .
H28 H 0.0255 0.5407 0.4409 0.032 Uiso 1 1 calc R . .
C29 C 0.3073(2) 0.4147(3) 0.41296(13) 0.0461(8) Uani 1 1 d . . .
H29A H 0.2931 0.4760 0.4014 0.055 Uiso 1 1 calc R . .
H29B H 0.2683 0.3721 0.4000 0.055 Uiso 1 1 calc R . .
C30 C 0.3758(3) 0.3859(4) 0.40134(17) 0.0649(13) Uani 1 1 d . . .
H30A H 0.4158 0.4240 0.4165 0.097 Uiso 1 1 calc R . .
H30B H 0.3694 0.3932 0.3710 0.097 Uiso 1 1 calc R . .
H30C H 0.3862 0.3222 0.4091 0.097 Uiso 1 1 calc R . .
C31 C 0.25072(17) 0.0706(2) 0.41783(10) 0.0363(6) Uani 1 1 d . . .
H31A H 0.2182 0.0188 0.4075 0.044 Uiso 1 1 calc R . .
H31B H 0.2267 0.1266 0.4047 0.044 Uiso 1 1 calc R . .
C32 C 0.3191(2) 0.0575(3) 0.40439(12) 0.0496(9) Uani 1 1 d . . .
H32A H 0.3520 0.1077 0.4151 0.074 Uiso 1 1 calc R . .
H32B H 0.3082 0.0563 0.3736 0.074 Uiso 1 1 calc R . .
H32C H 0.3415 0.0000 0.4157 0.074 Uiso 1 1 calc R . .
C33 C -0.01117(16) 0.1355(2) 0.39728(9) 0.0310(6) Uani 1 1 d . . .
H33A H 0.0247 0.1742 0.3889 0.037 Uiso 1 1 calc R . .
H33B H -0.0015 0.0717 0.3910 0.037 Uiso 1 1 calc R . .
C34 C -0.08513(18) 0.1616(3) 0.37157(10) 0.0387(7) Uani 1 1 d . . .
H34A H -0.1208 0.1223 0.3791 0.058 Uiso 1 1 calc R . .
H34B H -0.0878 0.1545 0.3416 0.058 Uiso 1 1 calc R . .
H34C H -0.0948 0.2250 0.3773 0.058 Uiso 1 1 calc R . .
C35 C 0.04450(16) 0.4749(2) 0.38912(9) 0.0317(6) Uani 1 1 d . . .
H35A H 0.0724 0.5242 0.3803 0.038 Uiso 1 1 calc R . .
H35B H 0.0656 0.4163 0.3837 0.038 Uiso 1 1 calc R . .
C36 C -0.03211(19) 0.4797(3) 0.36300(11) 0.0415(7) Uani 1 1 d . . .
H36A H -0.0597 0.4300 0.3710 0.062 Uiso 1 1 calc R . .
H36B H -0.0333 0.4743 0.3331 0.062 Uiso 1 1 calc R . .
H36C H -0.0531 0.5380 0.3679 0.062 Uiso 1 1 calc R . .
C37 C 0.36048(16) 0.5205(2) 0.75713(10) 0.0321(6) Uani 1 1 d . E .
H37 H 0.3723 0.4821 0.7811 0.038 Uiso 1 1 calc R . .
C38 C 0.28832(16) 0.5278(2) 0.73545(9) 0.0316(6) Uani 1 1 d . . .
C39 C 0.27286(16) 0.5852(2) 0.69970(10) 0.0342(6) Uani 1 1 d . E .
C40 C 0.32590(18) 0.6311(3) 0.68809(10) 0.0379(7) Uani 1 1 d . . .
C41 C 0.39771(17) 0.6203(3) 0.71030(10) 0.0375(7) Uani 1 1 d . E .
C42 C 0.41600(16) 0.5654(2) 0.74608(9) 0.0323(6) Uani 1 1 d . . .
C43 C 0.49321(15) 0.5570(2) 0.77187(9) 0.0313(6) Uani 1 1 d . E .
H43 H 0.5180 0.6139 0.7669 0.038 Uiso 1 1 calc R . .
C44 C 0.52723(15) 0.3895(2) 0.76947(9) 0.0305(6) Uani 1 1 d . E .
H44 H 0.4987 0.3769 0.7884 0.037 Uiso 1 1 calc R . .
C45 C 0.53187(15) 0.4789(2) 0.75666(8) 0.0296(5) Uani 1 1 d . . .
C46 C 0.57210(16) 0.4946(2) 0.72781(9) 0.0327(6) Uani 1 1 d . E .
C47 C 0.6069(2) 0.4241(2) 0.71314(12) 0.0416(8) Uani 1 1 d . . .
C48 C 0.60327(16) 0.3369(2) 0.72756(10) 0.0344(6) Uani 1 1 d . E .
C49 C 0.56250(16) 0.3178(2) 0.75586(9) 0.0318(6) Uani 1 1 d . . .
C50 C 0.55678(17) 0.2207(2) 0.77011(10) 0.0337(6) Uani 1 1 d . E .
H50 H 0.5975 0.1864 0.7639 0.040 Uiso 1 1 calc R . .
C51 C 0.42459(16) 0.1801(2) 0.75704(10) 0.0320(6) Uani 1 1 d . E .
H51 H 0.4244 0.2111 0.7823 0.038 Uiso 1 1 calc R . .
C52 C 0.48841(16) 0.1768(2) 0.74458(10) 0.0329(6) Uani 1 1 d . . .
C53 C 0.48723(18) 0.1335(2) 0.70692(11) 0.0389(7) Uani 1 1 d . E .
C54 C 0.4253(2) 0.0936(3) 0.68340(13) 0.0486(9) Uani 1 1 d . . .
C55 C 0.36294(19) 0.0959(3) 0.69686(13) 0.0446(8) Uani 1 1 d . E .
C56 C 0.36150(17) 0.1403(2) 0.73421(11) 0.0361(6) Uani 1 1 d . . .
C57 C 0.29145(19) 0.1429(3) 0.74694(12) 0.0411(7) Uani 1 1 d . E .
H57 H 0.2642 0.0877 0.7342 0.049 Uiso 1 1 calc R . .
C58 C 0.25817(16) 0.3107(2) 0.74442(10) 0.0344(6) Uani 1 1 d . E .
H58 H 0.2957 0.3192 0.7692 0.041 Uiso 1 1 calc R . .
C59 C 0.24659(16) 0.2238(2) 0.72691(10) 0.0334(6) Uani 1 1 d . . .
C60 C 0.19168(17) 0.2124(2) 0.69034(10) 0.0350(6) Uani 1 1 d . E .
C61 C 0.1507(2) 0.2858(3) 0.67209(12) 0.0463(8) Uani 1 1 d . . .
C62 C 0.1631(2) 0.3709(2) 0.68996(13) 0.0485(9) Uani 1 1 d . E .
C63 C 0.21645(18) 0.3856(2) 0.72679(11) 0.0382(7) Uani 1 1 d . . .
C64 C 0.22897(17) 0.4776(2) 0.74758(11) 0.0367(6) Uani 0.50 1 d P E 1
H64 H 0.1844 0.5136 0.7360 0.044 Uiso 0.50 1 calc PR E 1
C65 C 0.49875(16) 0.5533(2) 0.81904(9) 0.0310(6) Uani 1 1 d . . .
H65A H 0.4714 0.6046 0.8267 0.037 Uiso 1 1 calc R E .
H65B H 0.4767 0.4962 0.8255 0.037 Uiso 1 1 calc R . .
C66 C 0.57592(17) 0.5580(2) 0.84566(9) 0.0354(6) Uani 1 1 d . E .
H66A H 0.6016 0.5031 0.8411 0.053 Uiso 1 1 calc R . .
H66B H 0.5763 0.5623 0.8754 0.053 Uiso 1 1 calc R . .
H66C H 0.5994 0.6115 0.8376 0.053 Uiso 1 1 calc R . .
C67 C 0.56488(19) 0.2126(2) 0.81770(10) 0.0376(7) Uani 1 1 d . . .
H67A H 0.5260 0.2471 0.8252 0.045 Uiso 1 1 calc R E .
H67B H 0.5599 0.1480 0.8249 0.045 Uiso 1 1 calc R . .
C68 C 0.6365(2) 0.2479(3) 0.84328(11) 0.0482(8) Uani 1 1 d . E .
H68A H 0.6752 0.2180 0.8341 0.072 Uiso 1 1 calc R . .
H68B H 0.6417 0.2350 0.8731 0.072 Uiso 1 1 calc R . .
H68C H 0.6390 0.3137 0.8392 0.072 Uiso 1 1 calc R . .
C69 C 0.3001(2) 0.1354(3) 0.79297(12) 0.0457(8) Uani 1 1 d . . .
H69A H 0.3204 0.1928 0.8066 0.055 Uiso 1 1 calc R E .
H69B H 0.3345 0.0861 0.8043 0.055 Uiso 1 1 calc R . .
C70 C 0.2298(2) 0.1159(4) 0.80381(13) 0.0588(12) Uani 1 1 d . E .
H70A H 0.1967 0.1666 0.7944 0.088 Uiso 1 1 calc R . .
H70B H 0.2385 0.1086 0.8343 0.088 Uiso 1 1 calc R . .
H70C H 0.2089 0.0600 0.7897 0.088 Uiso 1 1 calc R . .
C71 C 0.2395(2) 0.4745(3) 0.79554(12) 0.0477(8) Uani 0.50 1 d P E 1
H71A H 0.2030 0.4344 0.8025 0.057 Uiso 0.50 1 calc PR E 1
H71B H 0.2874 0.4500 0.8093 0.057 Uiso 0.50 1 calc PR E 1
C72 C 0.2328(7) 0.5621(9) 0.8101(4) 0.082(3) Uani 0.50 1 d P E 1
H72A H 0.2757 0.5974 0.8097 0.123 Uiso 0.50 1 calc PR E 1
H72B H 0.2275 0.5592 0.8389 0.123 Uiso 0.50 1 calc PR E 1
H72C H 0.1906 0.5914 0.7919 0.123 Uiso 0.50 1 calc PR E 1
C72A C 0.1712(5) 0.4451(7) 0.8107(3) 0.0525(19) Uani 0.50 1 d P E 2
H72D H 0.1338 0.4913 0.8023 0.079 Uiso 0.50 1 calc PR E 2
H72E H 0.1843 0.4389 0.8414 0.079 Uiso 0.50 1 calc PR E 2
H72F H 0.1533 0.3868 0.7978 0.079 Uiso 0.50 1 calc PR E 2
C7H C 0.2467(3) 0.3703(3) 0.6061(2) 0.0780(17) Uani 0.30 1 d PDU C 2
H7H H 0.2024 0.3991 0.5935 0.094 Uiso 0.30 1 calc PR C 2
C64A C 0.22897(17) 0.4776(2) 0.74758(11) 0.0367(6) Uani 0.50 1 d P E 2
H64A H 0.1844 0.5136 0.7360 0.044 Uiso 0.50 1 calc PR E 2
C71A C 0.2395(2) 0.4745(3) 0.79554(12) 0.0477(8) Uani 0.50 1 d P E 2
H71C H 0.2547 0.5355 0.8071 0.057 Uiso 0.50 1 calc PR E 2
H71D H 0.2789 0.4318 0.8076 0.057 Uiso 0.50 1 calc PR E 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 1.370(3) . ?
O1 H1 0.8400 . ?
C1 C6 1.389(4) . ?
C1 C2 1.391(4) . ?
C1 H25 0.9500 . ?
O1A C3A 1.155(13) . ?
O1A' C3A' 1.208(14) . ?
N1I C1I 1.322(6) . ?
N1I C2I 1.378(5) . ?
N1I C4I 1.461(6) . ?
C1I N2I 1.325(5) . ?
C1I H1I 0.9500 . ?
S1S O2S 1.438(3) . ?
S1S O4S 1.464(3) . ?
S1S O1S 1.470(2) . ?
S1S O3S 1.489(2) . ?
O2 C4 1.364(4) . ?
O2 H2 0.8400 . ?
C2 C3 1.393(4) . ?
C2 C28 1.523(4) . ?
C2A C3A 1.471(13) . ?
C2A H2A1 0.9800 . ?
C2A H2A2 0.9800 . ?
C2A H2A3 0.9800 . ?
C2A' C3A' 1.35(2) . ?
C2A' H2A4 0.9800 . ?
C2A' H2A5 0.9800 . ?
C2A' H2A6 0.9800 . ?
N2I C3I 1.369(6) . ?
N2I C6I 1.471(7) . ?
C2I C3I 1.348(6) . ?
C2I H2I 0.9500 . ?
O3 C5 1.369(3) . ?
O3 H3 0.8400 . ?
C3 C4 1.390(4) . ?
C3A C4A 1.516(18) . ?
C3A' C4A' 1.52(2) . ?
N3H C8H 1.309(15) . ?
N3H C10H 1.448(15) . ?
N3I C7I 1.285(6) . ?
N3I C8I 1.371(8) . ?
N3I C10I 1.468(7) . ?
C3I H3I 0.9500 . ?
O4 C10 1.366(4) . ?
O4 H4 0.8399 . ?
C4 C5 1.387(4) . ?
C4A H4A1 0.9800 . ?
C4A H4A2 0.9800 . ?
C4A H4A3 0.9800 . ?
C4A' H4A4 0.9800 . ?
C4A' H4A5 0.9800 . ?
C4A' H4A6 0.9800 . ?
N4H C8H 1.337(15) . ?
N4H C9H 1.355(16) . ?
N4H C12H 1.450(17) . ?
N4I C7I 1.389(7) . ?
N4I C9I 1.395(11) . ?
N4I C12I 1.477(10) . ?
C4I C5I 1.460(8) . ?
C4I H4I1 0.9900 . ?
C4I H4I2 0.9900 . ?
O5 C11 1.361(4) . ?
O5 H5 0.8400 . ?
C5 C6 1.385(4) . ?
C5I H5I1 0.9800 . ?
C5I H5I2 0.9800 . ?
C5I H5I3 0.9800 . ?
O6 C12 1.374(4) . ?
O6 H6 0.8400 . ?
C6 C7 1.518(4) . ?
C6I H6I1 0.9800 . ?
C6I H6I2 0.9800 . ?
C6I H6I3 0.9800 . ?
O7 C17 1.372(4) . ?
O7 H7 0.8400 . ?
C7 C29 1.502(5) . ?
C7 C9 1.528(4) . ?
C7 H26 1.0000 . ?
C7I H7I 0.9500 . ?
O8 C18 1.375(4) . ?
O8 H8 0.8400 . ?
C8 C9 1.385(5) . ?
C8 C13 1.401(4) . ?
C8 H27 0.9500 . ?
C8H H8H 0.9500 . ?
C8I C9I 1.292(11) . ?
C8I H8I 0.9500 . ?
O9 C19 1.363(4) . ?
O9 H9 0.8400 . ?
C9 C10 1.391(4) . ?
C9H H9H 0.9500 . ?
C9I H9I 0.9500 . ?
O10 C24 1.371(4) . ?
O10 H10 0.8400 . ?
C10 C11 1.392(5) . ?
C10H C11H 1.53(2) . ?
C10H H10A 0.9900 . ?
C10H H10B 0.9900 . ?
C10I C11I 1.467(10) . ?
C10I H10C 0.9900 . ?
C10I H10D 0.9900 . ?
O11 C25 1.366(3) . ?
O11 H11 0.8400 . ?
C11 C12 1.397(5) . ?
C11H H11A 0.9800 . ?
C11H H11B 0.9800 . ?
C11H H11C 0.9800 . ?
C11I H11D 0.9800 . ?
C11I H11E 0.9800 . ?
C11I H11F 0.9800 . ?
O12 C26 1.370(3) . ?
O12 H12 0.8400 . ?
C12 C13 1.391(4) . ?
C12H H12A 0.9800 . ?
C12H H12B 0.9800 . ?
C12H H12C 0.9800 . ?
C12I H12D 0.9800 . ?
C12I H12E 0.9800 . ?
C12I H12F 0.9800 . ?
O13 C39 1.375(4) . ?
O13 H13 0.8400 . ?
C13 C14 1.526(4) . ?
O14 C40 1.380(4) . ?
O14 H14 0.8400 . ?
C14 C16 1.523(4) . ?
C14 C31 1.542(4) . ?
C14 H29 1.0000 . ?
O15 C41 1.362(4) . ?
O15 H15 0.8406 . ?
C15 C20 1.385(4) . ?
C15 C16 1.391(4) . ?
C15 H30 0.9500 . ?
O16 C46 1.375(4) . ?
O16 H16 0.8400 . ?
C16 C17 1.396(4) . ?
O17 C47 1.370(4) . ?
O17 H17 0.8400 . ?
C17 C18 1.381(5) . ?
O18 C48 1.377(4) . ?
O18 H18 0.8400 . ?
C18 C19 1.401(4) . ?
O19 C53 1.368(4) . ?
O19 H19 0.8400 . ?
C19 C20 1.409(4) . ?
O20 C54 1.366(5) . ?
O20 H20 0.8412 . ?
C20 C21 1.525(4) . ?
O21 C55 1.373(4) . ?
O21 H21 0.8400 . ?
C21 C23 1.523(4) . ?
C21 C33 1.538(4) . ?
C21 H31 1.0000 . ?
O22 C60 1.380(4) . ?
O22 H22 0.8400 . ?
C22 C23 1.389(4) . ?
C22 C27 1.394(4) . ?
C22 H32 0.9500 . ?
O23 C61 1.374(5) . ?
O23 H23 0.8400 . ?
C23 C24 1.398(4) . ?
O24 C62 1.370(4) . ?
O24 H24 0.8410 . ?
C24 C25 1.394(4) . ?
C25 C26 1.380(4) . ?
C26 C27 1.394(4) . ?
C27 C28 1.519(4) . ?
C28 C35 1.546(4) . ?
C28 H28 1.0000 . ?
C29 C30 1.529(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.509(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.512(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.511(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C42 1.385(4) . ?
C37 C38 1.398(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.416(4) . ?
C38 C64 1.502(4) . ?
C39 C40 1.362(5) . ?
C40 C41 1.402(4) . ?
C41 C42 1.397(4) . ?
C42 C43 1.520(4) . ?
C43 C45 1.523(4) . ?
C43 C65 1.529(4) . ?
C43 H43 1.0000 . ?
C44 C49 1.391(5) . ?
C44 C45 1.393(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(4) . ?
C46 C47 1.389(5) . ?
C47 C48 1.376(5) . ?
C48 C49 1.394(4) . ?
C49 C50 1.517(5) . ?
C50 C52 1.517(4) . ?
C50 C67 1.537(4) . ?
C50 H50 1.0000 . ?
C51 C56 1.387(4) . ?
C51 C52 1.397(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.388(5) . ?
C53 C54 1.379(5) . ?
C54 C55 1.386(5) . ?
C55 C56 1.398(5) . ?
C56 C57 1.516(5) . ?
C57 C69 1.484(5) . ?
C57 C59 1.520(4) . ?
C57 H57 1.0000 . ?
C58 C59 1.397(5) . ?
C58 C63 1.401(4) . ?
C58 H58 0.9500 . ?
C59 C60 1.395(4) . ?
C60 C61 1.382(5) . ?
C61 C62 1.379(6) . ?
C62 C63 1.392(5) . ?
C63 C64 1.510(5) . ?
C64 C71 1.539(5) . ?
C64 H64 1.0000 . ?
C65 C66 1.525(4) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C68 1.516(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C70 1.517(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.393(12) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C72A H72D 0.9800 . ?
C72A H72E 0.9800 . ?
C72A H72F 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
C3 O1 H1 109.5 . . ?
C6 C1 C2 122.8(3) . . ?
C6 C1 H25 118.6 . . ?
C2 C1 H25 118.6 . . ?
C1I N1I C2I 108.6(4) . . ?
C1I N1I C4I 124.4(4) . . ?
C2I N1I C4I 126.9(4) . . ?
N1I C1I N2I 107.7(4) . . ?
N1I C1I H1I 126.1 . . ?
N2I C1I H1I 126.1 . . ?
O2S S1S O4S 110.6(2) . . ?
O2S S1S O1S 110.24(16) . . ?
O4S S1S O1S 111.06(17) . . ?
O2S S1S O3S 110.38(16) . . ?
O4S S1S O3S 106.64(18) . . ?
O1S S1S O3S 107.78(14) . . ?
C4 O2 H2 109.5 . . ?
C1 C2 C3 117.4(2) . . ?
C1 C2 C28 122.1(2) . . ?
C3 C2 C28 120.4(2) . . ?
C1I N2I C3I 110.3(4) . . ?
C1I N2I C6I 125.2(4) . . ?
C3I N2I C6I 124.4(4) . . ?
C3I C2I N1I 107.7(4) . . ?
C3I C2I H2I 126.2 . . ?
N1I C2I H2I 126.2 . . ?
C5 O3 H3 109.5 . . ?
O1 C3 C4 114.4(2) . . ?
O1 C3 C2 124.6(2) . . ?
C4 C3 C2 120.9(3) . . ?
O1A C3A C2A 128.9(12) . . ?
O1A C3A C4A 122.7(13) . . ?
C2A C3A C4A 108.3(12) . . ?
O1A' C3A' C2A' 127.1(13) . . ?
O1A' C3A' C4A' 122.3(13) . . ?
C2A' C3A' C4A' 110.5(13) . . ?
C8H N3H C10H 128.1(13) . . ?
C7I N3I C8I 110.8(5) . . ?
C7I N3I C10I 124.8(5) . . ?
C8I N3I C10I 124.4(6) . . ?
C2I C3I N2I 105.7(4) . . ?
C2I C3I H3I 127.2 . . ?
N2I C3I H3I 127.2 . . ?
C10 O4 H4 109.4 . . ?
O2 C4 C5 117.7(3) . . ?
O2 C4 C3 122.4(3) . . ?
C5 C4 C3 119.9(3) . . ?
C8H N4H C9H 105.6(12) . . ?
C8H N4H C12H 121.4(15) . . ?
C9H N4H C12H 132.6(14) . . ?
C7I N4I C9I 107.4(5) . . ?
C7I N4I C12I 122.9(9) . . ?
C9I N4I C12I 129.6(9) . . ?
C5I C4I N1I 111.5(4) . . ?
C5I C4I H4I1 109.3 . . ?
N1I C4I H4I1 109.3 . . ?
C5I C4I H4I2 109.3 . . ?
N1I C4I H4I2 109.3 . . ?
H4I1 C4I H4I2 108.0 . . ?
C11 O5 H5 109.5 . . ?
O3 C5 C6 119.5(3) . . ?
O3 C5 C4 119.9(3) . . ?
C6 C5 C4 120.6(3) . . ?
C4I C5I H5I1 109.5 . . ?
C4I C5I H5I2 109.5 . . ?
H5I1 C5I H5I2 109.5 . . ?
C4I C5I H5I3 109.5 . . ?
H5I1 C5I H5I3 109.5 . . ?
H5I2 C5I H5I3 109.5 . . ?
C12 O6 H6 109.5 . . ?
C5 C6 C1 118.3(3) . . ?
C5 C6 C7 119.5(3) . . ?
C1 C6 C7 122.2(3) . . ?
N2I C6I H6I1 109.5 . . ?
N2I C6I H6I2 109.5 . . ?
H6I1 C6I H6I2 109.5 . . ?
N2I C6I H6I3 109.5 . . ?
H6I1 C6I H6I3 109.5 . . ?
H6I2 C6I H6I3 109.5 . . ?
C17 O7 H7 109.5 . . ?
C29 C7 C6 114.3(3) . . ?
C29 C7 C9 114.4(3) . . ?
C6 C7 C9 109.7(3) . . ?
C29 C7 H26 105.9 . . ?
C6 C7 H26 105.9 . . ?
C9 C7 H26 105.9 . . ?
N3I C7I N4I 106.1(5) . . ?
N3I C7I H7I 126.9 . . ?
N4I C7I H7I 126.9 . . ?
C18 O8 H8 109.5 . . ?
C9 C8 C13 123.2(3) . . ?
C9 C8 H27 118.4 . . ?
C13 C8 H27 118.4 . . ?
N3H C8H N4H 109.8(13) . . ?
N3H C8H H8H 125.1 . . ?
N4H C8H H8H 125.1 . . ?
C9I C8I N3I 108.8(6) . . ?
C9I C8I H8I 125.6 . . ?
N3I C8I H8I 125.6 . . ?
C19 O9 H9 109.5 . . ?
C8 C9 C10 118.0(3) . . ?
C8 C9 C7 121.7(3) . . ?
C10 C9 C7 120.2(3) . . ?
N4H C9H H9H 127.1 . . ?
C8I C9I N4I 106.8(5) . . ?
C8I C9I H9I 126.6 . . ?
N4I C9I H9I 126.6 . . ?
C24 O10 H10 109.5 . . ?
O4 C10 C9 125.1(3) . . ?
O4 C10 C11 114.4(3) . . ?
C9 C10 C11 120.5(3) . . ?
N3H C10H C11H 112.9(12) . . ?
N3H C10H H10A 109.0 . . ?
C11H C10H H10A 109.0 . . ?
N3H C10H H10B 109.0 . . ?
C11H C10H H10B 109.0 . . ?
H10A C10H H10B 107.8 . . ?
C11I C10I N3I 112.4(6) . . ?
C11I C10I H10C 109.1 . . ?
N3I C10I H10C 109.1 . . ?
C11I C10I H10D 109.1 . . ?
N3I C10I H10D 109.1 . . ?
H10C C10I H10D 107.9 . . ?
C25 O11 H11 109.5 . . ?
O5 C11 C10 122.5(3) . . ?
O5 C11 C12 117.4(3) . . ?
C10 C11 C12 120.1(3) . . ?
C10H C11H H11A 109.5 . . ?
C10H C11H H11B 109.5 . . ?
H11A C11H H11B 109.5 . . ?
C10H C11H H11C 109.5 . . ?
H11A C11H H11C 109.5 . . ?
H11B C11H H11C 109.5 . . ?
C26 O12 H12 109.5 . . ?
O6 C12 C13 123.5(3) . . ?
O6 C12 C11 115.8(3) . . ?
C13 C12 C11 120.7(3) . . ?
N4H C12H H12A 109.5 . . ?
N4H C12H H12B 109.5 . . ?
H12A C12H H12B 109.5 . . ?
N4H C12H H12C 109.5 . . ?
H12A C12H H12C 109.5 . . ?
H12B C12H H12C 109.5 . . ?
C39 O13 H13 109.5 . . ?
C12 C13 C8 117.3(3) . . ?
C12 C13 C14 120.5(3) . . ?
C8 C13 C14 122.1(3) . . ?
C40 O14 H14 109.5 . . ?
C16 C14 C13 110.9(2) . . ?
C16 C14 C31 112.8(2) . . ?
C13 C14 C31 113.0(3) . . ?
C16 C14 H29 106.5 . . ?
C13 C14 H29 106.5 . . ?
C31 C14 H29 106.5 . . ?
C41 O15 H15 109.4 . . ?
C20 C15 C16 123.0(3) . . ?
C20 C15 H30 118.5 . . ?
C16 C15 H30 118.5 . . ?
C46 O16 H16 109.5 . . ?
C15 C16 C17 117.8(3) . . ?
C15 C16 C14 122.5(3) . . ?
C17 C16 C14 119.7(3) . . ?
C47 O17 H17 109.5 . . ?
O7 C17 C18 120.0(3) . . ?
O7 C17 C16 118.9(3) . . ?
C18 C17 C16 121.1(3) . . ?
C48 O18 H18 109.5 . . ?
O8 C18 C17 120.6(3) . . ?
O8 C18 C19 119.2(3) . . ?
C17 C18 C19 120.1(3) . . ?
C53 O19 H19 109.5 . . ?
O9 C19 C18 120.8(3) . . ?
O9 C19 C20 119.3(3) . . ?
C18 C19 C20 119.9(3) . . ?
C54 O20 H20 109.4 . . ?
C15 C20 C19 118.0(3) . . ?
C15 C20 C21 123.2(2) . . ?
C19 C20 C21 118.8(3) . . ?
C55 O21 H21 109.5 . . ?
C23 C21 C20 111.3(2) . . ?
C23 C21 C33 112.2(2) . . ?
C20 C21 C33 111.9(2) . . ?
C23 C21 H31 107.0 . . ?
C20 C21 H31 107.0 . . ?
C33 C21 H31 107.0 . . ?
C60 O22 H22 109.5 . . ?
C23 C22 C27 123.5(3) . . ?
C23 C22 H32 118.2 . . ?
C27 C22 H32 118.2 . . ?
C61 O23 H23 109.5 . . ?
C22 C23 C24 117.9(2) . . ?
C22 C23 C21 121.7(2) . . ?
C24 C23 C21 120.4(2) . . ?
C62 O24 H24 109.4 . . ?
O10 C24 C25 116.6(3) . . ?
O10 C24 C23 123.5(3) . . ?
C25 C24 C23 119.8(3) . . ?
O11 C25 C26 116.6(2) . . ?
O11 C25 C24 122.7(3) . . ?
C26 C25 C24 120.6(3) . . ?
O12 C26 C25 120.2(2) . . ?
O12 C26 C27 118.5(2) . . ?
C25 C26 C27 121.2(2) . . ?
C26 C27 C22 116.9(2) . . ?
C26 C27 C28 120.0(2) . . ?
C22 C27 C28 123.1(2) . . ?
C27 C28 C2 110.6(2) . . ?
C27 C28 C35 111.8(2) . . ?
C2 C28 C35 112.7(2) . . ?
C27 C28 H28 107.1 . . ?
C2 C28 H28 107.1 . . ?
C35 C28 H28 107.1 . . ?
C7 C29 C30 112.0(4) . . ?
C7 C29 H29A 109.2 . . ?
C30 C29 H29A 109.2 . . ?
C7 C29 H29B 109.2 . . ?
C30 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C14 112.5(3) . . ?
C32 C31 H31A 109.1 . . ?
C14 C31 H31A 109.1 . . ?
C32 C31 H31B 109.1 . . ?
C14 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C21 112.7(2) . . ?
C34 C33 H33A 109.1 . . ?
C21 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C21 C33 H33B 109.1 . . ?
H33A C33 H33B 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C28 112.6(3) . . ?
C36 C35 H35A 109.1 . . ?
C28 C35 H35A 109.1 . . ?
C36 C35 H35B 109.1 . . ?
C28 C35 H35B 109.1 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42 C37 C38 124.6(3) . . ?
C42 C37 H37 117.7 . . ?
C38 C37 H37 117.7 . . ?
C37 C38 C39 116.1(3) . . ?
C37 C38 C64 123.8(3) . . ?
C39 C38 C64 120.1(3) . . ?
C40 C39 O13 122.2(3) . . ?
C40 C39 C38 121.0(3) . . ?
O13 C39 C38 116.8(3) . . ?
C39 C40 O14 122.0(3) . . ?
C39 C40 C41 120.9(3) . . ?
O14 C40 C41 117.0(3) . . ?
O15 C41 C42 123.5(3) . . ?
O15 C41 C40 116.0(3) . . ?
C42 C41 C40 120.5(3) . . ?
C37 C42 C41 116.8(3) . . ?
C37 C42 C43 122.0(3) . . ?
C41 C42 C43 121.2(3) . . ?
C42 C43 C45 111.8(2) . . ?
C42 C43 C65 111.9(2) . . ?
C45 C43 C65 113.2(2) . . ?
C42 C43 H43 106.5 . . ?
C45 C43 H43 106.5 . . ?
C65 C43 H43 106.5 . . ?
C49 C44 C45 123.1(3) . . ?
C49 C44 H44 118.5 . . ?
C45 C44 H44 118.5 . . ?
C46 C45 C44 117.0(3) . . ?
C46 C45 C43 120.4(3) . . ?
C44 C45 C43 122.6(3) . . ?
O16 C46 C47 120.3(3) . . ?
O16 C46 C45 118.5(3) . . ?
C47 C46 C45 121.2(3) . . ?
O17 C47 C48 122.9(3) . . ?
O17 C47 C46 116.7(3) . . ?
C48 C47 C46 120.3(3) . . ?
C47 C48 O18 119.5(3) . . ?
C47 C48 C49 120.4(3) . . ?
O18 C48 C49 120.0(3) . . ?
C44 C49 C48 118.0(3) . . ?
C44 C49 C50 122.3(3) . . ?
C48 C49 C50 119.7(3) . . ?
C52 C50 C49 110.7(2) . . ?
C52 C50 C67 112.2(3) . . ?
C49 C50 C67 113.1(3) . . ?
C52 C50 H50 106.8 . . ?
C49 C50 H50 106.8 . . ?
C67 C50 H50 106.8 . . ?
C56 C51 C52 123.1(3) . . ?
C56 C51 H51 118.5 . . ?
C52 C51 H51 118.5 . . ?
C53 C52 C51 117.7(3) . . ?
C53 C52 C50 120.2(3) . . ?
C51 C52 C50 122.1(3) . . ?
O19 C53 C54 116.8(3) . . ?
O19 C53 C52 122.4(3) . . ?
C54 C53 C52 120.6(3) . . ?
O20 C54 C53 121.8(3) . . ?
O20 C54 C55 117.5(3) . . ?
C53 C54 C55 120.7(3) . . ?
O21 C55 C54 120.7(3) . . ?
O21 C55 C56 118.7(3) . . ?
C54 C55 C56 120.5(3) . . ?
C51 C56 C55 117.4(3) . . ?
C51 C56 C57 124.2(3) . . ?
C55 C56 C57 118.3(3) . . ?
C69 C57 C56 113.9(3) . . ?
C69 C57 C59 113.8(3) . . ?
C56 C57 C59 110.5(3) . . ?
C69 C57 H57 106.0 . . ?
C56 C57 H57 106.0 . . ?
C59 C57 H57 106.0 . . ?
C59 C58 C63 122.4(3) . . ?
C59 C58 H58 118.8 . . ?
C63 C58 H58 118.8 . . ?
C60 C59 C58 118.1(3) . . ?
C60 C59 C57 120.2(3) . . ?
C58 C59 C57 121.7(3) . . ?
O22 C60 C61 115.7(3) . . ?
O22 C60 C59 123.9(3) . . ?
C61 C60 C59 120.3(3) . . ?
O23 C61 C62 122.7(3) . . ?
O23 C61 C60 116.9(3) . . ?
C62 C61 C60 120.5(3) . . ?
O24 C62 C61 114.8(3) . . ?
O24 C62 C63 123.8(3) . . ?
C61 C62 C63 121.4(3) . . ?
C62 C63 C58 117.2(3) . . ?
C62 C63 C64 122.1(3) . . ?
C58 C63 C64 120.7(3) . . ?
C38 C64 C63 111.5(3) . . ?
C38 C64 C71 112.2(3) . . ?
C63 C64 C71 113.7(3) . . ?
C38 C64 H64 106.3 . . ?
C63 C64 H64 106.3 . . ?
C71 C64 H64 106.3 . . ?
C66 C65 C43 112.6(2) . . ?
C66 C65 H65A 109.1 . . ?
C43 C65 H65A 109.1 . . ?
C66 C65 H65B 109.1 . . ?
C43 C65 H65B 109.1 . . ?
H65A C65 H65B 107.8 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 C50 112.2(3) . . ?
C68 C67 H67A 109.2 . . ?
C50 C67 H67A 109.2 . . ?
C68 C67 H67B 109.2 . . ?
C50 C67 H67B 109.2 . . ?
H67A C67 H67B 107.9 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C57 C69 C70 112.3(3) . . ?
C57 C69 H69A 109.1 . . ?
C70 C69 H69A 109.1 . . ?
C57 C69 H69B 109.1 . . ?
C70 C69 H69B 109.1 . . ?
H69A C69 H69B 107.9 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 C64 109.0(6) . . ?
C72 C71 H71A 109.9 . . ?
C64 C71 H71A 109.9 . . ?
C72 C71 H71B 109.9 . . ?
C64 C71 H71B 109.9 . . ?
H71A C71 H71B 108.3 . . ?
H72D C72A H72E 109.5 . . ?
H72D C72A H72F 109.5 . . ?
H72E C72A H72F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2I N1I C1I N2I 0.5(5) . . . . ?
C4I N1I C1I N2I -176.6(4) . . . . ?
C6 C1 C2 C3 -0.6(4) . . . . ?
C6 C1 C2 C28 -179.3(3) . . . . ?
N1I C1I N2I C3I -0.8(5) . . . . ?
N1I C1I N2I C6I -176.6(6) . . . . ?
C1I N1I C2I C3I 0.0(5) . . . . ?
C4I N1I C2I C3I 177.0(4) . . . . ?
C1 C2 C3 O1 179.4(3) . . . . ?
C28 C2 C3 O1 -1.9(4) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C28 C2 C3 C4 178.5(3) . . . . ?
N1I C2I C3I N2I -0.5(5) . . . . ?
C1I N2I C3I C2I 0.8(5) . . . . ?
C6I N2I C3I C2I 176.6(6) . . . . ?
O1 C3 C4 O2 3.4(4) . . . . ?
C2 C3 C4 O2 -177.0(3) . . . . ?
O1 C3 C4 C5 -178.2(3) . . . . ?
C2 C3 C4 C5 1.4(5) . . . . ?
C1I N1I C4I C5I 101.4(6) . . . . ?
C2I N1I C4I C5I -75.2(6) . . . . ?
O2 C4 C5 O3 -1.9(5) . . . . ?
C3 C4 C5 O3 179.7(3) . . . . ?
O2 C4 C5 C6 176.7(3) . . . . ?
C3 C4 C5 C6 -1.8(5) . . . . ?
O3 C5 C6 C1 179.5(3) . . . . ?
C4 C5 C6 C1 0.9(4) . . . . ?
O3 C5 C6 C7 1.4(4) . . . . ?
C4 C5 C6 C7 -177.2(3) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
C2 C1 C6 C7 178.3(3) . . . . ?
C5 C6 C7 C29 -146.9(3) . . . . ?
C1 C6 C7 C29 35.0(4) . . . . ?
C5 C6 C7 C9 83.0(4) . . . . ?
C1 C6 C7 C9 -95.0(4) . . . . ?
C8I N3I C7I N4I -1.3(7) . . . . ?
C10I N3I C7I N4I 178.9(5) . . . . ?
C9I N4I C7I N3I 3.2(7) . . . . ?
C12I N4I C7I N3I 179.3(8) . . . . ?
C10H N3H C8H N4H 176.8(17) . . . . ?
C9H N4H C8H N3H -2(2) . . . . ?
C12H N4H C8H N3H -175.7(18) . . . . ?
C7I N3I C8I C9I -1.3(9) . . . . ?
C10I N3I C8I C9I 178.5(6) . . . . ?
C13 C8 C9 C10 -1.8(5) . . . . ?
C13 C8 C9 C7 179.4(3) . . . . ?
C29 C7 C9 C8 -48.7(4) . . . . ?
C6 C7 C9 C8 81.3(4) . . . . ?
C29 C7 C9 C10 132.6(3) . . . . ?
C6 C7 C9 C10 -97.5(4) . . . . ?
N3I C8I C9I N4I 3.2(9) . . . . ?
C7I N4I C9I C8I -4.0(9) . . . . ?
C12I N4I C9I C8I -179.7(10) . . . . ?
C8 C9 C10 O4 178.0(3) . . . . ?
C7 C9 C10 O4 -3.2(5) . . . . ?
C8 C9 C10 C11 0.9(5) . . . . ?
C7 C9 C10 C11 179.7(3) . . . . ?
C8H N3H C10H C11H -135.8(19) . . . . ?
C7I N3I C10I C11I -105.4(8) . . . . ?
C8I N3I C10I C11I 74.9(10) . . . . ?
O4 C10 C11 O5 2.7(5) . . . . ?
C9 C10 C11 O5 -179.9(3) . . . . ?
O4 C10 C11 C12 -177.3(3) . . . . ?
C9 C10 C11 C12 0.1(5) . . . . ?
O5 C11 C12 O6 -2.6(4) . . . . ?
C10 C11 C12 O6 177.4(3) . . . . ?
O5 C11 C12 C13 179.7(3) . . . . ?
C10 C11 C12 C13 -0.3(5) . . . . ?
O6 C12 C13 C8 -178.0(3) . . . . ?
C11 C12 C13 C8 -0.5(4) . . . . ?
O6 C12 C13 C14 1.4(5) . . . . ?
C11 C12 C13 C14 178.9(3) . . . . ?
C9 C8 C13 C12 1.6(4) . . . . ?
C9 C8 C13 C14 -177.8(3) . . . . ?
C12 C13 C14 C16 97.1(3) . . . . ?
C8 C13 C14 C16 -83.5(3) . . . . ?
C12 C13 C14 C31 -135.1(3) . . . . ?
C8 C13 C14 C31 44.3(4) . . . . ?
C20 C15 C16 C17 1.5(4) . . . . ?
C20 C15 C16 C14 -176.3(3) . . . . ?
C13 C14 C16 C15 94.0(3) . . . . ?
C31 C14 C16 C15 -33.9(4) . . . . ?
C13 C14 C16 C17 -83.7(3) . . . . ?
C31 C14 C16 C17 148.4(3) . . . . ?
C15 C16 C17 O7 179.8(3) . . . . ?
C14 C16 C17 O7 -2.4(4) . . . . ?
C15 C16 C17 C18 -1.4(4) . . . . ?
C14 C16 C17 C18 176.5(3) . . . . ?
O7 C17 C18 O8 1.0(4) . . . . ?
C16 C17 C18 O8 -177.8(3) . . . . ?
O7 C17 C18 C19 178.1(3) . . . . ?
C16 C17 C18 C19 -0.7(4) . . . . ?
O8 C18 C19 O9 -0.3(4) . . . . ?
C17 C18 C19 O9 -177.4(3) . . . . ?
O8 C18 C19 C20 179.9(3) . . . . ?
C17 C18 C19 C20 2.8(4) . . . . ?
C16 C15 C20 C19 0.5(4) . . . . ?
C16 C15 C20 C21 179.1(3) . . . . ?
O9 C19 C20 C15 177.5(2) . . . . ?
C18 C19 C20 C15 -2.6(4) . . . . ?
O9 C19 C20 C21 -1.2(4) . . . . ?
C18 C19 C20 C21 178.7(2) . . . . ?
C15 C20 C21 C23 -94.4(3) . . . . ?
C19 C20 C21 C23 84.2(3) . . . . ?
C15 C20 C21 C33 32.0(4) . . . . ?
C19 C20 C21 C33 -149.4(3) . . . . ?
C27 C22 C23 C24 -1.2(4) . . . . ?
C27 C22 C23 C21 178.9(2) . . . . ?
C20 C21 C23 C22 79.1(3) . . . . ?
C33 C21 C23 C22 -47.2(3) . . . . ?
C20 C21 C23 C24 -100.8(3) . . . . ?
C33 C21 C23 C24 132.9(3) . . . . ?
C22 C23 C24 O10 178.3(2) . . . . ?
C21 C23 C24 O10 -1.8(4) . . . . ?
C22 C23 C24 C25 1.6(4) . . . . ?
C21 C23 C24 C25 -178.5(2) . . . . ?
O10 C24 C25 O11 4.3(4) . . . . ?
C23 C24 C25 O11 -178.7(3) . . . . ?
O10 C24 C25 C26 -178.4(2) . . . . ?
C23 C24 C25 C26 -1.5(4) . . . . ?
O11 C25 C26 O12 -0.1(4) . . . . ?
C24 C25 C26 O12 -177.5(2) . . . . ?
O11 C25 C26 C27 178.3(2) . . . . ?
C24 C25 C26 C27 0.9(4) . . . . ?
O12 C26 C27 C22 177.9(2) . . . . ?
C25 C26 C27 C22 -0.5(4) . . . . ?
O12 C26 C27 C28 -1.9(4) . . . . ?
C25 C26 C27 C28 179.7(2) . . . . ?
C23 C22 C27 C26 0.7(4) . . . . ?
C23 C22 C27 C28 -179.5(2) . . . . ?
C26 C27 C28 C2 99.3(3) . . . . ?
C22 C27 C28 C2 -80.5(3) . . . . ?
C26 C27 C28 C35 -134.2(3) . . . . ?
C22 C27 C28 C35 46.0(3) . . . . ?
C1 C2 C28 C27 96.2(3) . . . . ?
C3 C2 C28 C27 -82.4(3) . . . . ?
C1 C2 C28 C35 -29.7(4) . . . . ?
C3 C2 C28 C35 151.6(3) . . . . ?
C6 C7 C29 C30 169.0(4) . . . . ?
C9 C7 C29 C30 -63.3(5) . . . . ?
C16 C14 C31 C32 -168.5(3) . . . . ?
C13 C14 C31 C32 64.7(4) . . . . ?
C23 C21 C33 C34 -62.3(3) . . . . ?
C20 C21 C33 C34 171.7(3) . . . . ?
C27 C28 C35 C36 63.1(3) . . . . ?
C2 C28 C35 C36 -171.6(3) . . . . ?
C42 C37 C38 C39 0.4(5) . . . . ?
C42 C37 C38 C64 179.1(3) . . . . ?
C37 C38 C39 C40 -1.1(5) . . . . ?
C64 C38 C39 C40 -179.8(3) . . . . ?
C37 C38 C39 O13 178.0(3) . . . . ?
C64 C38 C39 O13 -0.8(5) . . . . ?
O13 C39 C40 O14 0.1(6) . . . . ?
C38 C39 C40 O14 179.1(3) . . . . ?
O13 C39 C40 C41 -176.6(3) . . . . ?
C38 C39 C40 C41 2.4(6) . . . . ?
C39 C40 C41 O15 177.3(3) . . . . ?
O14 C40 C41 O15 0.5(5) . . . . ?
C39 C40 C41 C42 -3.1(6) . . . . ?
O14 C40 C41 C42 -180.0(3) . . . . ?
C38 C37 C42 C41 -1.1(5) . . . . ?
C38 C37 C42 C43 177.9(3) . . . . ?
O15 C41 C42 C37 -178.1(3) . . . . ?
C40 C41 C42 C37 2.3(5) . . . . ?
O15 C41 C42 C43 2.9(6) . . . . ?
C40 C41 C42 C43 -176.7(3) . . . . ?
C37 C42 C43 C45 90.5(4) . . . . ?
C41 C42 C43 C45 -90.5(4) . . . . ?
C37 C42 C43 C65 -37.6(4) . . . . ?
C41 C42 C43 C65 141.3(3) . . . . ?
C49 C44 C45 C46 2.2(4) . . . . ?
C49 C44 C45 C43 -179.8(3) . . . . ?
C42 C43 C45 C46 94.1(3) . . . . ?
C65 C43 C45 C46 -138.4(3) . . . . ?
C42 C43 C45 C44 -83.8(3) . . . . ?
C65 C43 C45 C44 43.7(4) . . . . ?
C44 C45 C46 O16 178.1(3) . . . . ?
C43 C45 C46 O16 0.1(4) . . . . ?
C44 C45 C46 C47 -1.1(4) . . . . ?
C43 C45 C46 C47 -179.1(3) . . . . ?
O16 C46 C47 O17 0.7(5) . . . . ?
C45 C46 C47 O17 179.8(3) . . . . ?
O16 C46 C47 C48 179.6(3) . . . . ?
C45 C46 C47 C48 -1.2(5) . . . . ?
O17 C47 C48 O18 1.0(6) . . . . ?
C46 C47 C48 O18 -177.9(3) . . . . ?
O17 C47 C48 C49 -178.7(4) . . . . ?
C46 C47 C48 C49 2.4(5) . . . . ?
C45 C44 C49 C48 -1.1(4) . . . . ?
C45 C44 C49 C50 -179.9(3) . . . . ?
C47 C48 C49 C44 -1.3(5) . . . . ?
O18 C48 C49 C44 179.1(3) . . . . ?
C47 C48 C49 C50 177.6(3) . . . . ?
O18 C48 C49 C50 -2.1(4) . . . . ?
C44 C49 C50 C52 81.6(3) . . . . ?
C48 C49 C50 C52 -97.3(3) . . . . ?
C44 C49 C50 C67 -45.2(4) . . . . ?
C48 C49 C50 C67 135.9(3) . . . . ?
C56 C51 C52 C53 1.8(5) . . . . ?
C56 C51 C52 C50 -179.9(3) . . . . ?
C49 C50 C52 C53 87.5(4) . . . . ?
C67 C50 C52 C53 -145.2(3) . . . . ?
C49 C50 C52 C51 -90.7(4) . . . . ?
C67 C50 C52 C51 36.6(4) . . . . ?
C51 C52 C53 O19 -178.5(3) . . . . ?
C50 C52 C53 O19 3.2(5) . . . . ?
C51 C52 C53 C54 -1.5(5) . . . . ?
C50 C52 C53 C54 -179.8(4) . . . . ?
O19 C53 C54 O20 -2.6(6) . . . . ?
C52 C53 C54 O20 -179.7(4) . . . . ?
O19 C53 C54 C55 177.2(4) . . . . ?
C52 C53 C54 C55 0.1(6) . . . . ?
O20 C54 C55 O21 -2.6(7) . . . . ?
C53 C54 C55 O21 177.5(4) . . . . ?
O20 C54 C55 C56 -179.1(4) . . . . ?
C53 C54 C55 C56 1.1(7) . . . . ?
C52 C51 C56 C55 -0.7(5) . . . . ?
C52 C51 C56 C57 -179.9(3) . . . . ?
O21 C55 C56 C51 -177.3(4) . . . . ?
C54 C55 C56 C51 -0.8(6) . . . . ?
O21 C55 C56 C57 2.0(5) . . . . ?
C54 C55 C56 C57 178.5(4) . . . . ?
C51 C56 C57 C69 -37.3(5) . . . . ?
C55 C56 C57 C69 143.5(4) . . . . ?
C51 C56 C57 C59 92.2(4) . . . . ?
C55 C56 C57 C59 -87.0(4) . . . . ?
C63 C58 C59 C60 0.5(5) . . . . ?
C63 C58 C59 C57 -178.8(3) . . . . ?
C69 C57 C59 C60 -132.1(3) . . . . ?
C56 C57 C59 C60 98.4(4) . . . . ?
C69 C57 C59 C58 47.2(4) . . . . ?
C56 C57 C59 C58 -82.3(4) . . . . ?
C58 C59 C60 O22 -177.2(3) . . . . ?
C57 C59 C60 O22 2.1(5) . . . . ?
C58 C59 C60 C61 0.5(5) . . . . ?
C57 C59 C60 C61 179.8(3) . . . . ?
O22 C60 C61 O23 -2.8(5) . . . . ?
C59 C60 C61 O23 179.3(4) . . . . ?
O22 C60 C61 C62 177.4(4) . . . . ?
C59 C60 C61 C62 -0.5(6) . . . . ?
O23 C61 C62 O24 1.1(7) . . . . ?
C60 C61 C62 O24 -179.2(4) . . . . ?
O23 C61 C62 C63 179.7(4) . . . . ?
C60 C61 C62 C63 -0.5(7) . . . . ?
O24 C62 C63 C58 180.0(4) . . . . ?
C61 C62 C63 C58 1.5(6) . . . . ?
O24 C62 C63 C64 0.7(7) . . . . ?
C61 C62 C63 C64 -177.8(4) . . . . ?
C59 C58 C63 C62 -1.5(5) . . . . ?
C59 C58 C63 C64 177.8(3) . . . . ?
C37 C38 C64 C63 -88.6(4) . . . . ?
C39 C38 C64 C63 90.0(4) . . . . ?
C37 C38 C64 C71 40.2(5) . . . . ?
C39 C38 C64 C71 -141.1(3) . . . . ?
C62 C63 C64 C38 -97.0(4) . . . . ?
C58 C63 C64 C38 83.7(4) . . . . ?
C62 C63 C64 C71 134.9(4) . . . . ?
C58 C63 C64 C71 -44.3(4) . . . . ?
C42 C43 C65 C66 -172.1(3) . . . . ?
C45 C43 C65 C66 60.4(3) . . . . ?
C52 C50 C67 C68 174.3(3) . . . . ?
C49 C50 C67 C68 -59.8(4) . . . . ?
C56 C57 C69 C70 -166.5(4) . . . . ?
C59 C57 C69 C70 65.7(5) . . . . ?
C38 C64 C71 C72 66.9(7) . . . . ?
C63 C64 C71 C72 -165.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        31.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 986744'
#######################################################################
#
#                 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_C:\xtals\Completed\C2emimMeCN\C2EMIMCN.CIF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            C2emimMeCN
_chemical_melting_point          ?
_chemical_formula_moiety         
'C36 H40 O12, C2 H5 O4 S, C6 H11 N2, C2 H3 N, H2 O'
_chemical_formula_sum            'C46 H61 N3 O17 S'
_chemical_formula_weight         960.04

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.0590(19)
_cell_length_b                   14.556(3)
_cell_length_c                   15.558(3)
_cell_angle_alpha                92.816(2)
_cell_angle_beta                 93.863(2)
_cell_angle_gamma                96.287(2)
_cell_volume                     2255.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7384
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.14

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9418
_exptl_absorpt_correction_T_max  0.9850
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26045
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.54
_reflns_number_total             10156
_reflns_number_gt                6839
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_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)+(0.0647P)²+1.9013P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10156
_refine_ls_number_parameters     652
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1502
_refine_ls_wR_factor_gt          0.1268
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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
S1 S 0.97788(6) 0.13532(4) 0.30593(4) 0.02942(15) Uani 1 1 d . A .
O1 O 0.70306(17) 0.29002(12) 0.41109(10) 0.0333(4) Uani 1 1 d . . .
H1 H 0.7753 0.2715 0.4294 0.040 Uiso 1 1 calc R . .
N1 N 0.7086(2) 0.05011(14) 0.73348(13) 0.0314(4) Uani 1 1 d . . .
C1 C 0.5905(3) 0.35605(15) 0.62325(15) 0.0312(5) Uani 1 1 d . . .
H13 H 0.6251 0.3847 0.6775 0.037 Uiso 1 1 calc R . .
O2 O 0.43386(18) 0.22334(13) 0.39254(11) 0.0378(4) Uani 1 1 d . . .
H2 H 0.4933 0.2177 0.3578 0.045 Uiso 1 1 calc R . .
N2 N 0.6859(2) 0.03893(14) 0.59460(13) 0.0341(5) Uani 1 1 d . . .
C2 C 0.6778(3) 0.34933(15) 0.55789(15) 0.0294(5) Uani 1 1 d . . .
O3 O 0.27289(17) 0.24228(12) 0.52264(10) 0.0335(4) Uani 1 1 d . . .
H3 H 0.2536 0.2241 0.4708 0.040 Uiso 1 1 calc R . .
N3 N 0.7129(4) 0.5155(3) 0.8260(2) 0.0718(9) Uani 1 1 d . . .
C3 C 0.6257(3) 0.30431(15) 0.47912(14) 0.0288(5) Uani 1 1 d . . .
O4 O 0.28796(17) 0.12826(11) 0.66579(10) 0.0301(4) Uani 1 1 d . . .
H4 H 0.2761 0.1694 0.6309 0.036 Uiso 1 1 calc R . .
C4 C 0.4905(3) 0.27009(16) 0.46702(14) 0.0298(5) Uani 1 1 d . . .
O5 O 0.32063(17) 0.01553(11) 0.79615(11) 0.0330(4) Uani 1 1 d . . .
H5 H 0.2621 0.0071 0.7545 0.040 Uiso 1 1 calc R . .
C5 C 0.4060(2) 0.27970(15) 0.53321(15) 0.0289(5) Uani 1 1 d . . .
O6 O 0.44626(18) 0.07318(11) 0.94487(10) 0.0333(4) Uani 1 1 d . . .
H6 H 0.4988 0.0952 0.9869 0.040 Uiso 1 1 calc R . .
C6 C 0.4545(2) 0.32258(15) 0.61272(15) 0.0289(5) Uani 1 1 d . . .
O7 O 0.65653(17) 0.11954(11) 1.08140(10) 0.0315(4) Uani 1 1 d . . .
H7 H 0.6812 0.0690 1.0962 0.038 Uiso 1 1 calc R . .
C7 C 0.3633(3) 0.33037(16) 0.68691(15) 0.0316(5) Uani 1 1 d . . .
H16 H 0.2691 0.3118 0.6624 0.038 Uiso 1 1 calc R . .
O8 O 0.90646(18) 0.05397(11) 1.06642(10) 0.0322(4) Uani 1 1 d . . .
H8 H 0.9333 0.0703 1.1178 0.039 Uiso 1 1 calc R . .
C8 C 0.4636(2) 0.29152(16) 0.83465(15) 0.0287(5) Uani 1 1 d . . .
H17 H 0.4970 0.3551 0.8442 0.034 Uiso 1 1 calc R . .
O9 O 1.08535(17) 0.13983(12) 0.95863(11) 0.0335(4) Uani 1 1 d . . .
H9 H 1.0787 0.0828 0.9662 0.040 Uiso 1 1 calc R . .
C9 C 0.3931(2) 0.26290(16) 0.75609(14) 0.0280(5) Uani 1 1 d . . .
O10 O 1.05641(17) 0.11779(11) 0.77358(10) 0.0299(4) Uani 1 1 d . . .
H10 H 1.0735 0.1347 0.8259 0.036 Uiso 1 1 calc R . .
C10 C 0.3492(2) 0.16872(16) 0.74201(14) 0.0257(5) Uani 1 1 d . . .
O11 O 1.00748(18) 0.09062(12) 0.59870(10) 0.0340(4) Uani 1 1 d . . .
H11 H 1.0522 0.0600 0.6320 0.041 Uiso 1 1 calc R . .
C11 C 0.3667(2) 0.10800(16) 0.80721(14) 0.0266(5) Uani 1 1 d . . .
O12 O 0.90668(19) 0.22003(13) 0.50370(10) 0.0369(4) Uani 1 1 d . . .
H12 H 0.9511 0.1778 0.4870 0.044 Uiso 1 1 calc R . .
C12 C 0.4353(2) 0.13921(16) 0.88556(14) 0.0263(5) Uani 1 1 d . . .
O13 O 0.8936(2) 0.22016(13) 0.29634(14) 0.0470(5) Uani 1 1 d . . .
C13 C 0.4877(2) 0.23222(15) 0.89994(14) 0.0264(5) Uani 1 1 d . . .
O14 O 0.87667(19) 0.06452(12) 0.32858(12) 0.0411(4) Uani 1 1 d . . .
C14 C 0.5694(2) 0.26558(16) 0.98424(14) 0.0286(5) Uani 1 1 d . . .
H14 H 0.5249 0.2329 1.0315 0.034 Uiso 1 1 calc R . .
O15 O 1.08189(19) 0.16080(14) 0.37385(12) 0.0468(5) Uani 1 1 d . . .
C15 C 0.8039(2) 0.27604(15) 0.92974(14) 0.0276(5) Uani 1 1 d . . .
H15 H 0.7801 0.3262 0.8974 0.033 Uiso 1 1 calc R . .
O16 O 1.03049(19) 0.11713(13) 0.22343(11) 0.0422(4) Uani 1 1 d . . .
C16 C 0.7104(2) 0.23484(15) 0.98243(14) 0.0267(5) Uani 1 1 d . . .
C17 C 0.7482(2) 0.16149(15) 1.02977(14) 0.0267(5) Uani 1 1 d . . .
C18 C 0.8736(2) 0.13057(15) 1.02355(14) 0.0271(5) Uani 1 1 d . . .
C19 C 0.9633(2) 0.17227(16) 0.96853(14) 0.0271(5) Uani 1 1 d . . .
C20 C 0.9308(2) 0.24731(15) 0.92211(14) 0.0264(5) Uani 1 1 d . . .
C21 C 1.0296(2) 0.29620(16) 0.86414(14) 0.0290(5) Uani 1 1 d . . .
H21 H 1.1168 0.2703 0.8757 0.035 Uiso 1 1 calc R . .
C22 C 0.9301(2) 0.33702(16) 0.71715(15) 0.0291(5) Uani 1 1 d . . .
H22 H 0.9109 0.3938 0.7436 0.035 Uiso 1 1 calc R . .
C23 C 0.9880(2) 0.27411(15) 0.76867(14) 0.0265(5) Uani 1 1 d . . .
C24 C 1.0106(2) 0.18915(15) 0.72984(14) 0.0257(5) Uani 1 1 d . . .
C25 C 0.9857(2) 0.17210(16) 0.64090(14) 0.0271(5) Uani 1 1 d . . .
C26 C 0.9328(2) 0.23809(16) 0.59142(14) 0.0286(5) Uani 1 1 d . . .
C27 C 0.8992(2) 0.32048(15) 0.62896(14) 0.0276(5) Uani 1 1 d . . .
C28 C 0.8273(3) 0.38638(16) 0.57384(15) 0.0320(5) Uani 1 1 d . . .
H28 H 0.8668 0.3862 0.5165 0.038 Uiso 1 1 calc R . .
C29 C 0.3694(3) 0.42994(17) 0.72558(17) 0.0412(6) Uani 1 1 d . . .
H29A H 0.3152 0.4298 0.7764 0.049 Uiso 1 1 calc R . .
H29B H 0.4634 0.4519 0.7460 0.049 Uiso 1 1 calc R . .
C30 C 0.3194(4) 0.4976(2) 0.6634(2) 0.0687(11) Uani 1 1 d . . .
H30A H 0.3739 0.4996 0.6135 0.103 Uiso 1 1 calc R . .
H30B H 0.3263 0.5593 0.6925 0.103 Uiso 1 1 calc R . .
H30C H 0.2255 0.4775 0.6440 0.103 Uiso 1 1 calc R . .
C31 C 0.5699(3) 0.36957(18) 1.00515(17) 0.0405(6) Uani 1 1 d . . .
H31A H 0.6172 0.4040 0.9608 0.049 Uiso 1 1 calc R . .
H31B H 0.4762 0.3847 1.0020 0.049 Uiso 1 1 calc R . .
C32 C 0.6358(4) 0.4015(2) 1.0927(2) 0.0568(8) Uani 1 1 d . . .
H32A H 0.5958 0.3633 1.1365 0.085 Uiso 1 1 calc R . .
H32B H 0.6227 0.4664 1.1053 0.085 Uiso 1 1 calc R . .
H32C H 0.7320 0.3956 1.0935 0.085 Uiso 1 1 calc R . .
C33 C 1.0558(3) 0.39982(17) 0.88921(16) 0.0368(6) Uani 1 1 d . . .
H33A H 1.1131 0.4305 0.8473 0.044 Uiso 1 1 calc R . .
H33B H 0.9696 0.4268 0.8865 0.044 Uiso 1 1 calc R . .
C34 C 1.1242(3) 0.4184(2) 0.97957(18) 0.0500(7) Uani 1 1 d . . .
H34A H 1.0640 0.3934 1.0218 0.075 Uiso 1 1 calc R . .
H34B H 1.1458 0.4853 0.9916 0.075 Uiso 1 1 calc R . .
H34C H 1.2070 0.3885 0.9835 0.075 Uiso 1 1 calc R . .
C35 C 0.8485(3) 0.48651(18) 0.61248(19) 0.0473(7) Uani 1 1 d . . .
H35A H 0.8057 0.4890 0.6679 0.057 Uiso 1 1 calc R . .
H35B H 0.9458 0.5049 0.6250 0.057 Uiso 1 1 calc R . .
C36 C 0.7925(5) 0.5553(2) 0.5548(3) 0.0810(14) Uani 1 1 d . . .
H36A H 0.8347 0.5537 0.4998 0.121 Uiso 1 1 calc R . .
H36B H 0.8111 0.6175 0.5829 0.121 Uiso 1 1 calc R . .
H36C H 0.6954 0.5393 0.5441 0.121 Uiso 1 1 calc R . .
C37 C 0.7257(3) -0.00232(17) 0.66416(16) 0.0339(5) Uani 1 1 d . . .
H37 H 0.7608 -0.0603 0.6643 0.041 Uiso 1 1 calc R . .
C38 C 0.6412(3) 0.12114(17) 0.62086(18) 0.0364(6) Uani 1 1 d . . .
H38 H 0.6064 0.1648 0.5845 0.044 Uiso 1 1 calc R . .
C39 C 0.6560(2) 0.12807(16) 0.70764(17) 0.0335(5) Uani 1 1 d . . .
H39 H 0.6342 0.1777 0.7441 0.040 Uiso 1 1 calc R . .
C40 C 0.7454(3) 0.03011(19) 0.82359(16) 0.0406(6) Uani 1 1 d . . .
H40A H 0.7248 0.0817 0.8625 0.049 Uiso 1 1 calc R . .
H40B H 0.8431 0.0264 0.8307 0.049 Uiso 1 1 calc R . .
C41 C 0.6733(3) -0.0574(2) 0.8489(2) 0.0548(8) Uani 1 1 d . . .
H41A H 0.5766 -0.0529 0.8448 0.082 Uiso 1 1 calc R . .
H41B H 0.7029 -0.0686 0.9084 0.082 Uiso 1 1 calc R . .
H41C H 0.6928 -0.1087 0.8102 0.082 Uiso 1 1 calc R . .
C42 C 0.6961(3) 0.0048(2) 0.50527(18) 0.0513(7) Uani 1 1 d . . .
H42A H 0.7898 -0.0027 0.4962 0.077 Uiso 1 1 calc R . .
H42B H 0.6642 0.0494 0.4657 0.077 Uiso 1 1 calc R . .
H42C H 0.6411 -0.0549 0.4942 0.077 Uiso 1 1 calc R . .
C43 C 0.9622(4) 0.3089(2) 0.2826(3) 0.0738(11) Uani 0.70 1 d P A 1
H43A H 1.0570 0.3112 0.3049 0.089 Uiso 0.70 1 calc PR A 1
H43B H 0.9211 0.3572 0.3152 0.089 Uiso 0.70 1 calc PR A 1
C45 C 0.6991(8) 0.5925(6) 0.8172(6) 0.062(2) Uani 0.80 1 d P B 1
O1W O 0.5917(3) 0.2088(3) 0.25228(18) 0.0702(9) Uani 0.80 1 d P C 1
O1W' O 0.5882(13) 0.1376(10) 0.2963(9) 0.073(3) Uiso 0.20 1 d P D 2
C44 C 0.9568(7) 0.3286(4) 0.1911(4) 0.0752(18) Uani 0.70 1 d P A 1
H44A H 1.0114 0.2879 0.1603 0.113 Uiso 0.70 1 calc PR A 1
H44B H 0.9917 0.3933 0.1852 0.113 Uiso 0.70 1 calc PR A 1
H44C H 0.8637 0.3177 0.1667 0.113 Uiso 0.70 1 calc PR A 1
C44A C 0.905(2) 0.3594(16) 0.2213(14) 0.110(8) Uiso 0.30 1 d P A 2
H44D H 0.9137 0.3309 0.1639 0.166 Uiso 0.30 1 calc PR A 2
H44E H 0.9504 0.4227 0.2255 0.166 Uiso 0.30 1 calc PR A 2
H44F H 0.8098 0.3608 0.2306 0.166 Uiso 0.30 1 calc PR A 2
C46 C 0.6901(7) 0.6915(5) 0.8150(6) 0.122(3) Uani 0.80 1 d P B 1
H46A H 0.6949 0.7188 0.8741 0.184 Uiso 0.80 1 calc PR B 1
H46B H 0.6049 0.7018 0.7848 0.184 Uiso 0.80 1 calc PR B 1
H46C H 0.7646 0.7205 0.7847 0.184 Uiso 0.80 1 calc PR B 1
C46A C 0.655(3) 0.6454(17) 0.7409(18) 0.091(7) Uani 0.20 1 d PU B 2
H46D H 0.6433 0.6210 0.6807 0.137 Uiso 0.20 1 calc PR B 2
H46E H 0.7160 0.7029 0.7454 0.137 Uiso 0.20 1 calc PR B 2
H46F H 0.5676 0.6579 0.7605 0.137 Uiso 0.20 1 calc PR B 2
C43A C 0.9622(4) 0.3089(2) 0.2826(3) 0.0738(11) Uani 0.30 1 d P A 2
H43C H 0.9716 0.3461 0.3381 0.089 Uiso 0.30 1 calc PR A 2
H43D H 1.0537 0.2999 0.2666 0.089 Uiso 0.30 1 calc PR A 2
C45A C 0.716(5) 0.570(3) 0.800(3) 0.11(2) Uani 0.20 1 d P B 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
S1 O15 1.4410(18) . ?
S1 O14 1.4411(19) . ?
S1 O16 1.4443(18) . ?
S1 O13 1.5801(19) . ?
O1 C3 1.376(3) . ?
O1 H1 0.8400 . ?
N1 C37 1.322(3) . ?
N1 C39 1.370(3) . ?
N1 C40 1.477(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.397(4) . ?
C1 H13 0.9500 . ?
O2 C4 1.371(3) . ?
O2 H2 0.8400 . ?
N2 C37 1.323(3) . ?
N2 C38 1.377(3) . ?
N2 C42 1.467(3) . ?
C2 C3 1.402(3) . ?
C2 C28 1.540(3) . ?
O3 C5 1.385(3) . ?
O3 H3 0.8400 . ?
N3 C45A 0.91(4) . ?
N3 C45 1.159(9) . ?
C3 C4 1.393(3) . ?
O4 C10 1.373(3) . ?
O4 H4 0.8400 . ?
C4 C5 1.391(3) . ?
O5 C11 1.374(3) . ?
O5 H5 0.8400 . ?
C5 C6 1.391(3) . ?
O6 C12 1.373(3) . ?
O6 H6 0.8400 . ?
C6 C7 1.529(3) . ?
O7 C17 1.376(3) . ?
O7 H7 0.8400 . ?
C7 C9 1.529(3) . ?
C7 C29 1.535(3) . ?
C7 H16 1.0000 . ?
O8 C18 1.386(3) . ?
O8 H8 0.8400 . ?
C8 C13 1.391(3) . ?
C8 C9 1.392(3) . ?
C8 H17 0.9500 . ?
O9 C19 1.378(3) . ?
O9 H9 0.8400 . ?
C9 C10 1.395(3) . ?
O10 C24 1.373(3) . ?
O10 H10 0.8400 . ?
C10 C11 1.393(3) . ?
O11 C25 1.373(3) . ?
O11 H11 0.8400 . ?
C11 C12 1.390(3) . ?
O12 C26 1.379(3) . ?
O12 H12 0.8400 . ?
C12 C13 1.400(3) . ?
O13 C43 1.429(4) . ?
C13 C14 1.528(3) . ?
C14 C31 1.532(3) . ?
C14 C16 1.535(3) . ?
C14 H14 1.0000 . ?
C15 C16 1.395(3) . ?
C15 C20 1.396(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.398(3) . ?
C17 C18 1.393(3) . ?
C18 C19 1.396(3) . ?
C19 C20 1.395(3) . ?
C20 C21 1.529(3) . ?
C21 C23 1.525(3) . ?
C21 C33 1.529(3) . ?
C21 H21 1.0000 . ?
C22 C27 1.389(3) . ?
C22 C23 1.395(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(3) . ?
C24 C25 1.395(3) . ?
C25 C26 1.389(3) . ?
C26 C27 1.393(3) . ?
C27 C28 1.526(3) . ?
C28 C35 1.536(3) . ?
C28 H28 1.0000 . ?
C29 C30 1.515(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.503(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.521(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.506(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37 0.9500 . ?
C38 C39 1.346(4) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.479(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.463(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C45 C46 1.455(11) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C44A H44D 0.9800 . ?
C44A H44E 0.9800 . ?
C44A H44F 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C46A C45A 1.62(5) . ?
C46A H46D 0.9800 . ?
C46A H46E 0.9800 . ?
C46A H46F 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
O15 S1 O14 113.28(12) . . ?
O15 S1 O16 112.67(12) . . ?
O14 S1 O16 114.08(11) . . ?
O15 S1 O13 107.48(11) . . ?
O14 S1 O13 101.11(11) . . ?
O16 S1 O13 107.13(11) . . ?
C3 O1 H1 109.5 . . ?
C37 N1 C39 108.6(2) . . ?
C37 N1 C40 125.8(2) . . ?
C39 N1 C40 125.6(2) . . ?
C2 C1 C6 123.1(2) . . ?
C2 C1 H13 118.4 . . ?
C6 C1 H13 118.4 . . ?
C4 O2 H2 109.5 . . ?
C37 N2 C38 108.2(2) . . ?
C37 N2 C42 125.3(2) . . ?
C38 N2 C42 126.4(2) . . ?
C1 C2 C3 117.6(2) . . ?
C1 C2 C28 120.7(2) . . ?
C3 C2 C28 121.7(2) . . ?
C5 O3 H3 109.5 . . ?
C45A N3 C45 22(3) . . ?
O1 C3 C4 116.6(2) . . ?
O1 C3 C2 123.0(2) . . ?
C4 C3 C2 120.4(2) . . ?
C10 O4 H4 109.5 . . ?
O2 C4 C5 116.2(2) . . ?
O2 C4 C3 123.4(2) . . ?
C5 C4 C3 120.3(2) . . ?
C11 O5 H5 109.5 . . ?
O3 C5 C6 118.6(2) . . ?
O3 C5 C4 120.4(2) . . ?
C6 C5 C4 120.9(2) . . ?
C12 O6 H6 109.5 . . ?
C5 C6 C1 117.6(2) . . ?
C5 C6 C7 121.3(2) . . ?
C1 C6 C7 121.1(2) . . ?
C17 O7 H7 109.5 . . ?
C9 C7 C6 111.21(19) . . ?
C9 C7 C29 111.6(2) . . ?
C6 C7 C29 112.4(2) . . ?
C9 C7 H16 107.1 . . ?
C6 C7 H16 107.1 . . ?
C29 C7 H16 107.1 . . ?
C18 O8 H8 109.5 . . ?
C13 C8 C9 123.6(2) . . ?
C13 C8 H17 118.2 . . ?
C9 C8 H17 118.2 . . ?
C19 O9 H9 109.5 . . ?
C8 C9 C10 117.3(2) . . ?
C8 C9 C7 122.5(2) . . ?
C10 C9 C7 120.2(2) . . ?
C24 O10 H10 109.5 . . ?
O4 C10 C11 114.90(19) . . ?
O4 C10 C9 124.6(2) . . ?
C11 C10 C9 120.5(2) . . ?
C25 O11 H11 109.5 . . ?
O5 C11 C12 117.65(19) . . ?
O5 C11 C10 121.8(2) . . ?
C12 C11 C10 120.5(2) . . ?
C26 O12 H12 109.5 . . ?
O6 C12 C11 115.34(19) . . ?
O6 C12 C13 124.3(2) . . ?
C11 C12 C13 120.4(2) . . ?
C43 O13 S1 118.8(2) . . ?
C8 C13 C12 117.4(2) . . ?
C8 C13 C14 122.2(2) . . ?
C12 C13 C14 120.4(2) . . ?
C13 C14 C31 112.7(2) . . ?
C13 C14 C16 109.47(18) . . ?
C31 C14 C16 113.5(2) . . ?
C13 C14 H14 106.9 . . ?
C31 C14 H14 106.9 . . ?
C16 C14 H14 106.9 . . ?
C16 C15 C20 123.4(2) . . ?
C16 C15 H15 118.3 . . ?
C20 C15 H15 118.3 . . ?
C15 C16 C17 117.2(2) . . ?
C15 C16 C14 121.1(2) . . ?
C17 C16 C14 121.7(2) . . ?
O7 C17 C18 121.0(2) . . ?
O7 C17 C16 117.9(2) . . ?
C18 C17 C16 121.1(2) . . ?
O8 C18 C17 120.5(2) . . ?
O8 C18 C19 119.4(2) . . ?
C17 C18 C19 119.9(2) . . ?
O9 C19 C20 118.7(2) . . ?
O9 C19 C18 120.7(2) . . ?
C20 C19 C18 120.6(2) . . ?
C19 C20 C15 117.7(2) . . ?
C19 C20 C21 121.4(2) . . ?
C15 C20 C21 120.9(2) . . ?
C23 C21 C33 113.85(19) . . ?
C23 C21 C20 112.00(18) . . ?
C33 C21 C20 111.11(19) . . ?
C23 C21 H21 106.4 . . ?
C33 C21 H21 106.4 . . ?
C20 C21 H21 106.4 . . ?
C27 C22 C23 123.1(2) . . ?
C27 C22 H22 118.5 . . ?
C23 C22 H22 118.5 . . ?
C22 C23 C24 118.0(2) . . ?
C22 C23 C21 122.3(2) . . ?
C24 C23 C21 119.7(2) . . ?
O10 C24 C25 115.5(2) . . ?
O10 C24 C23 124.4(2) . . ?
C25 C24 C23 120.1(2) . . ?
O11 C25 C26 117.1(2) . . ?
O11 C25 C24 123.0(2) . . ?
C26 C25 C24 119.9(2) . . ?
O12 C26 C25 119.5(2) . . ?
O12 C26 C27 119.0(2) . . ?
C25 C26 C27 121.4(2) . . ?
C22 C27 C26 117.2(2) . . ?
C22 C27 C28 123.0(2) . . ?
C26 C27 C28 119.8(2) . . ?
C27 C28 C35 112.5(2) . . ?
C27 C28 C2 109.61(18) . . ?
C35 C28 C2 112.5(2) . . ?
C27 C28 H28 107.3 . . ?
C35 C28 H28 107.3 . . ?
C2 C28 H28 107.3 . . ?
C30 C29 C7 114.1(2) . . ?
C30 C29 H29A 108.7 . . ?
C7 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C7 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C14 113.4(2) . . ?
C32 C31 H31A 108.9 . . ?
C14 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C14 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C21 111.8(2) . . ?
C34 C33 H33A 109.3 . . ?
C21 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C21 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C28 113.9(2) . . ?
C36 C35 H35A 108.8 . . ?
C28 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
C28 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N1 C37 N2 109.0(2) . . ?
N1 C37 H37 125.5 . . ?
N2 C37 H37 125.5 . . ?
C39 C38 N2 107.1(2) . . ?
C39 C38 H38 126.4 . . ?
N2 C38 H38 126.4 . . ?
C38 C39 N1 107.1(2) . . ?
C38 C39 H39 126.5 . . ?
N1 C39 H39 126.5 . . ?
N1 C40 C41 112.5(2) . . ?
N1 C40 H40A 109.1 . . ?
C41 C40 H40A 109.1 . . ?
N1 C40 H40B 109.1 . . ?
C41 C40 H40B 109.1 . . ?
H40A C40 H40B 107.8 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N2 C42 H42A 109.5 . . ?
N2 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N2 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O13 C43 C44 112.0(4) . . ?
O13 C43 H43A 109.2 . . ?
C44 C43 H43A 109.2 . . ?
O13 C43 H43B 109.2 . . ?
C44 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
N3 C45 C46 173.8(9) . . ?
H44D C44A H44E 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?
C45A C46A H46D 109.5 . . ?
C45A C46A H46E 109.5 . . ?
H46D C46A H46E 109.5 . . ?
C45A C46A H46F 109.5 . . ?
H46D C46A H46F 109.5 . . ?
H46E C46A H46F 109.5 . . ?
N3 C45A C46A 154(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.9(3) . . . . ?
C6 C1 C2 C28 -179.2(2) . . . . ?
C1 C2 C3 O1 -177.3(2) . . . . ?
C28 C2 C3 O1 0.0(3) . . . . ?
C1 C2 C3 C4 1.6(3) . . . . ?
C28 C2 C3 C4 178.9(2) . . . . ?
O1 C3 C4 O2 0.7(3) . . . . ?
C2 C3 C4 O2 -178.3(2) . . . . ?
O1 C3 C4 C5 178.5(2) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
O2 C4 C5 O3 0.8(3) . . . . ?
C3 C4 C5 O3 -177.2(2) . . . . ?
O2 C4 C5 C6 177.3(2) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
O3 C5 C6 C1 177.10(19) . . . . ?
C4 C5 C6 C1 0.5(3) . . . . ?
O3 C5 C6 C7 -1.2(3) . . . . ?
C4 C5 C6 C7 -177.8(2) . . . . ?
C2 C1 C6 C5 0.8(3) . . . . ?
C2 C1 C6 C7 179.1(2) . . . . ?
C5 C6 C7 C9 105.9(2) . . . . ?
C1 C6 C7 C9 -72.3(3) . . . . ?
C5 C6 C7 C29 -128.2(2) . . . . ?
C1 C6 C7 C29 53.6(3) . . . . ?
C13 C8 C9 C10 -2.4(3) . . . . ?
C13 C8 C9 C7 177.5(2) . . . . ?
C6 C7 C9 C8 104.4(3) . . . . ?
C29 C7 C9 C8 -21.9(3) . . . . ?
C6 C7 C9 C10 -75.7(3) . . . . ?
C29 C7 C9 C10 158.0(2) . . . . ?
C8 C9 C10 O4 -174.6(2) . . . . ?
C7 C9 C10 O4 5.5(3) . . . . ?
C8 C9 C10 C11 5.0(3) . . . . ?
C7 C9 C10 C11 -174.9(2) . . . . ?
O4 C10 C11 O5 -2.5(3) . . . . ?
C9 C10 C11 O5 177.8(2) . . . . ?
O4 C10 C11 C12 175.7(2) . . . . ?
C9 C10 C11 C12 -3.9(3) . . . . ?
O5 C11 C12 O6 -1.7(3) . . . . ?
C10 C11 C12 O6 180.0(2) . . . . ?
O5 C11 C12 C13 178.4(2) . . . . ?
C10 C11 C12 C13 0.0(3) . . . . ?
O15 S1 O13 C43 54.6(3) . . . . ?
O14 S1 O13 C43 173.5(2) . . . . ?
O16 S1 O13 C43 -66.8(3) . . . . ?
C9 C8 C13 C12 -1.4(4) . . . . ?
C9 C8 C13 C14 178.0(2) . . . . ?
O6 C12 C13 C8 -177.4(2) . . . . ?
C11 C12 C13 C8 2.5(3) . . . . ?
O6 C12 C13 C14 3.2(3) . . . . ?
C11 C12 C13 C14 -176.8(2) . . . . ?
C8 C13 C14 C31 23.9(3) . . . . ?
C12 C13 C14 C31 -156.7(2) . . . . ?
C8 C13 C14 C16 -103.4(2) . . . . ?
C12 C13 C14 C16 75.9(3) . . . . ?
C20 C15 C16 C17 0.4(3) . . . . ?
C20 C15 C16 C14 -176.4(2) . . . . ?
C13 C14 C16 C15 71.8(3) . . . . ?
C31 C14 C16 C15 -55.1(3) . . . . ?
C13 C14 C16 C17 -104.8(2) . . . . ?
C31 C14 C16 C17 128.3(2) . . . . ?
C15 C16 C17 O7 -179.37(19) . . . . ?
C14 C16 C17 O7 -2.6(3) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
C14 C16 C17 C18 176.1(2) . . . . ?
O7 C17 C18 O8 2.9(3) . . . . ?
C16 C17 C18 O8 -175.74(19) . . . . ?
O7 C17 C18 C19 177.9(2) . . . . ?
C16 C17 C18 C19 -0.8(3) . . . . ?
O8 C18 C19 O9 -2.0(3) . . . . ?
C17 C18 C19 O9 -177.04(19) . . . . ?
O8 C18 C19 C20 177.60(19) . . . . ?
C17 C18 C19 C20 2.6(3) . . . . ?
O9 C19 C20 C15 176.81(19) . . . . ?
C18 C19 C20 C15 -2.8(3) . . . . ?
O9 C19 C20 C21 -2.7(3) . . . . ?
C18 C19 C20 C21 177.7(2) . . . . ?
C16 C15 C20 C19 1.4(3) . . . . ?
C16 C15 C20 C21 -179.2(2) . . . . ?
C19 C20 C21 C23 107.2(2) . . . . ?
C15 C20 C21 C23 -72.3(3) . . . . ?
C19 C20 C21 C33 -124.2(2) . . . . ?
C15 C20 C21 C33 56.3(3) . . . . ?
C27 C22 C23 C24 -2.6(3) . . . . ?
C27 C22 C23 C21 175.8(2) . . . . ?
C33 C21 C23 C22 -23.2(3) . . . . ?
C20 C21 C23 C22 103.9(2) . . . . ?
C33 C21 C23 C24 155.2(2) . . . . ?
C20 C21 C23 C24 -77.6(3) . . . . ?
C22 C23 C24 O10 -174.4(2) . . . . ?
C21 C23 C24 O10 7.1(3) . . . . ?
C22 C23 C24 C25 5.1(3) . . . . ?
C21 C23 C24 C25 -173.4(2) . . . . ?
O10 C24 C25 O11 -1.3(3) . . . . ?
C23 C24 C25 O11 179.1(2) . . . . ?
O10 C24 C25 C26 176.8(2) . . . . ?
C23 C24 C25 C26 -2.8(3) . . . . ?
O11 C25 C26 O12 -0.9(3) . . . . ?
C24 C25 C26 O12 -179.1(2) . . . . ?
O11 C25 C26 C27 175.9(2) . . . . ?
C24 C25 C26 C27 -2.2(3) . . . . ?
C23 C22 C27 C26 -2.2(3) . . . . ?
C23 C22 C27 C28 175.7(2) . . . . ?
O12 C26 C27 C22 -178.5(2) . . . . ?
C25 C26 C27 C22 4.6(3) . . . . ?
O12 C26 C27 C28 3.5(3) . . . . ?
C25 C26 C27 C28 -173.3(2) . . . . ?
C22 C27 C28 C35 25.5(3) . . . . ?
C26 C27 C28 C35 -156.6(2) . . . . ?
C22 C27 C28 C2 -100.4(3) . . . . ?
C26 C27 C28 C2 77.4(3) . . . . ?
C1 C2 C28 C27 74.8(3) . . . . ?
C3 C2 C28 C27 -102.4(2) . . . . ?
C1 C2 C28 C35 -51.1(3) . . . . ?
C3 C2 C28 C35 131.7(2) . . . . ?
C9 C7 C29 C30 -170.7(3) . . . . ?
C6 C7 C29 C30 63.6(3) . . . . ?
C13 C14 C31 C32 173.2(2) . . . . ?
C16 C14 C31 C32 -61.6(3) . . . . ?
C23 C21 C33 C34 -168.2(2) . . . . ?
C20 C21 C33 C34 64.3(3) . . . . ?
C27 C28 C35 C36 173.2(3) . . . . ?
C2 C28 C35 C36 -62.4(4) . . . . ?
C39 N1 C37 N2 -0.1(3) . . . . ?
C40 N1 C37 N2 -177.7(2) . . . . ?
C38 N2 C37 N1 -0.2(3) . . . . ?
C42 N2 C37 N1 176.4(2) . . . . ?
C37 N2 C38 C39 0.4(3) . . . . ?
C42 N2 C38 C39 -176.2(3) . . . . ?
N2 C38 C39 N1 -0.4(3) . . . . ?
C37 N1 C39 C38 0.3(3) . . . . ?
C40 N1 C39 C38 177.9(2) . . . . ?
C37 N1 C40 C41 -60.8(4) . . . . ?
C39 N1 C40 C41 122.0(3) . . . . ?
S1 O13 C43 C44 97.2(5) . . . . ?
C45A N3 C45 C46 -124(14) . . . . ?
C45 N3 C45A C46A -86(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 986745'
#######################################################################
#
#                 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_F:\xtals\Completed\pgc4emimace\twin.CIF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            pgc4emimace
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H56 O12, C6 H11 N2, H O4 S, 2(H2 O)'
_chemical_formula_sum            'C50 H72 N2 O18 S'
_chemical_formula_weight         1021.16

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   21.075(9)
_cell_length_b                   12.796(6)
_cell_length_c                   18.229(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.533(6)
_cell_angle_gamma                90.00
_cell_volume                     4884(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2389
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.27

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9577
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8413
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1696
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8413
_reflns_number_gt                3996
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_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)+(0.1319P)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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8413
_refine_ls_number_parameters     662
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2169
_refine_ls_R_factor_gt           0.0934
_refine_ls_wR_factor_ref         0.2636
_refine_ls_wR_factor_gt          0.2099
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.3092(2) 0.1433(3) 0.6566(3) 0.0218(11) Uani 1 1 d . . .
H1 H 0.3481 0.1518 0.6709 0.026 Uiso 1 1 calc R . .
C1 C 0.2250(3) -0.0919(5) 0.5889(4) 0.0173(15) Uani 1 1 d . . .
H2 H 0.1832 -0.1116 0.5685 0.021 Uiso 1 1 calc R . .
N1I N 0.4728(3) -0.1639(4) 0.4517(3) 0.0278(14) Uani 1 1 d . . .
C1I C 0.4887(3) -0.0848(6) 0.4064(4) 0.0297(18) Uani 1 1 d . . .
H1I H 0.5263 -0.0809 0.3823 0.036 Uiso 1 1 calc R . .
S1S S 0.47045(8) 0.24290(13) 0.25650(9) 0.0194(4) Uani 1 1 d . . .
O1S O 0.5062(2) 0.1468(3) 0.2532(3) 0.0260(12) Uani 1 1 d . . .
O1W O 0.4918(2) -0.0009(4) 0.1337(3) 0.0244(11) Uani 1 1 d . . .
C2 C 0.2711(3) -0.1686(5) 0.6014(3) 0.0185(15) Uani 1 1 d . . .
N2I N 0.3961(3) -0.0505(4) 0.4443(3) 0.0227(13) Uani 1 1 d . . .
C2I C 0.4418(3) -0.0140(5) 0.4021(4) 0.0270(17) Uani 1 1 d . . .
H2I H 0.4402 0.0496 0.3751 0.032 Uiso 1 1 calc R . .
O2S O 0.4371(2) 0.2321(4) 0.3287(3) 0.0297(12) Uani 1 1 d . . .
O2W O 0.3536(2) 0.3904(4) 0.3337(3) 0.0302(12) Uani 1 1 d . . .
O8 O 0.3808(2) 0.0234(4) 0.2328(3) 0.0252(11) Uani 1 1 d . . .
H8 H 0.3807 0.0126 0.1873 0.030 Uiso 1 1 calc R . .
C3 C 0.3328(3) -0.1375(5) 0.6298(3) 0.0167(15) Uani 1 1 d . . .
C3I C 0.4167(3) -0.1429(5) 0.4729(4) 0.0259(17) Uani 1 1 d . . .
H3I H 0.3942 -0.1861 0.5035 0.031 Uiso 1 1 calc R . .
O3S O 0.4203(2) 0.2511(3) 0.1955(2) 0.0250(11) Uani 1 1 d . . .
O5 O 0.4206(2) -0.4743(3) 0.4641(2) 0.0210(11) Uani 1 1 d . . .
H5 H 0.4360 -0.4800 0.4237 0.025 Uiso 1 1 calc R . .
C4 C 0.3455(3) -0.0346(5) 0.6510(4) 0.0188(15) Uani 1 1 d . . .
C4I C 0.5079(3) -0.2624(6) 0.4671(4) 0.0319(18) Uani 1 1 d . . .
H4I1 H 0.5013 -0.3077 0.4229 0.038 Uiso 1 1 calc R . .
H4I2 H 0.4900 -0.2991 0.5080 0.038 Uiso 1 1 calc R . .
O4S O 0.5107(2) 0.3353(3) 0.2665(3) 0.0247(11) Uani 1 1 d . . .
O12 O 0.2508(2) 0.3080(3) 0.5766(2) 0.0231(11) Uani 1 1 d . . .
H12 H 0.2665 0.2678 0.6103 0.028 Uiso 1 1 calc R . .
C5 C 0.2979(3) 0.0398(5) 0.6387(4) 0.0182(15) Uani 1 1 d . . .
C5I C 0.5776(3) -0.2469(6) 0.4875(4) 0.0372(19) Uani 1 1 d . . .
H5I1 H 0.5955 -0.2093 0.4478 0.056 Uiso 1 1 calc R . .
H5I2 H 0.5986 -0.3151 0.4948 0.056 Uiso 1 1 calc R . .
H5I3 H 0.5847 -0.2063 0.5332 0.056 Uiso 1 1 calc R . .
O2 O 0.40352(19) -0.0038(3) 0.6835(3) 0.0228(11) Uani 1 1 d . . .
H13 H 0.4300 -0.0524 0.6811 0.027 Uiso 1 1 calc R . .
C6 C 0.2371(3) 0.0137(5) 0.6052(3) 0.0171(15) Uani 1 1 d . . .
C6I C 0.3349(3) -0.0032(6) 0.4549(4) 0.0337(19) Uani 1 1 d . . .
H6I1 H 0.3047 -0.0579 0.4654 0.050 Uiso 1 1 calc R . .
H6I2 H 0.3181 0.0344 0.4100 0.050 Uiso 1 1 calc R . .
H6I3 H 0.3407 0.0458 0.4965 0.050 Uiso 1 1 calc R . .
O6 O 0.3767(2) -0.3920(3) 0.3289(2) 0.0249(11) Uani 1 1 d . . .
H6 H 0.3797 -0.3363 0.3024 0.030 Uiso 1 1 d . . .
C7 C 0.1877(3) 0.0998(5) 0.5867(3) 0.0163(15) Uani 1 1 d . . .
H9 H 0.1937 0.1531 0.6270 0.020 Uiso 1 1 calc R . .
O4 O 0.3669(2) -0.4189(4) 0.5864(2) 0.0267(12) Uani 1 1 d . . .
H4 H 0.4004 -0.4527 0.5820 0.032 Uiso 1 1 calc R . .
C8 C 0.1816(3) 0.1074(5) 0.4465(3) 0.0161(15) Uani 1 1 d . . .
H11 H 0.1623 0.0401 0.4451 0.019 Uiso 1 1 calc R . .
C9 C 0.2004(3) 0.1534(5) 0.5148(4) 0.0201(15) Uani 1 1 d . . .
O10 O 0.2276(2) 0.3036(3) 0.3170(3) 0.0295(12) Uani 1 1 d . . .
H10 H 0.2549 0.3514 0.3252 0.035 Uiso 1 1 calc R . .
C10 C 0.2305(3) 0.2507(5) 0.5148(4) 0.0248(16) Uani 1 1 d . . .
C11 C 0.2397(3) 0.2994(5) 0.4497(4) 0.0216(16) Uani 1 1 d . . .
C12 C 0.2194(3) 0.2536(5) 0.3828(3) 0.0180(15) Uani 1 1 d . . .
O9 O 0.2869(2) 0.1582(3) 0.2413(3) 0.0259(11) Uani 1 1 d . . .
H14 H 0.2635 0.1996 0.2618 0.031 Uiso 1 1 calc R . .
C13 C 0.1900(3) 0.1566(5) 0.3804(4) 0.0184(15) Uani 1 1 d . . .
O3 O 0.38549(19) -0.2019(3) 0.6372(3) 0.0221(11) Uani 1 1 d . . .
H3 H 0.3742 -0.2631 0.6460 0.026 Uiso 1 1 calc R . .
C14 C 0.1679(3) 0.1034(5) 0.3065(3) 0.0188(15) Uani 1 1 d . . .
H15 H 0.1667 0.1592 0.2679 0.023 Uiso 1 1 calc R . .
O7 O 0.3686(2) -0.1844(3) 0.2697(3) 0.0249(11) Uani 1 1 d . . .
H7 H 0.4033 -0.1530 0.2811 0.030 Uiso 1 1 calc R . .
C15 C 0.2129(3) -0.0824(5) 0.3024(3) 0.0180(15) Uani 1 1 d . . .
H16 H 0.1743 -0.1073 0.3183 0.022 Uiso 1 1 calc R . .
C16 C 0.2184(3) 0.0247(5) 0.2885(4) 0.0180(15) Uani 1 1 d . . .
O11 O 0.2700(2) 0.3949(3) 0.4500(3) 0.0294(12) Uani 1 1 d . . .
H17 H 0.2768 0.4171 0.4935 0.035 Uiso 1 1 calc R . .
C17 C 0.2749(3) 0.0574(5) 0.2620(4) 0.0187(15) Uani 1 1 d . . .
C18 C 0.3247(3) -0.0100(5) 0.2547(3) 0.0154(14) Uani 1 1 d . . .
C19 C 0.3187(3) -0.1159(5) 0.2730(4) 0.0197(16) Uani 1 1 d . . .
C20 C 0.2613(3) -0.1543(5) 0.2942(4) 0.0194(15) Uani 1 1 d . . .
C21 C 0.2564(3) -0.2703(5) 0.3075(3) 0.0172(15) Uani 1 1 d . . .
H21 H 0.2793 -0.3053 0.2690 0.021 Uiso 1 1 calc R . .
C22 C 0.2652(3) -0.2786(5) 0.4476(4) 0.0171(15) Uani 1 1 d . . .
H22 H 0.2288 -0.2344 0.4445 0.020 Uiso 1 1 calc R . .
C23 C 0.2909(3) -0.3032(5) 0.3820(3) 0.0158(15) Uani 1 1 d . . .
C24 C 0.3448(3) -0.3649(4) 0.3891(3) 0.0128(14) Uani 1 1 d . . .
C25 C 0.3701(3) -0.4070(5) 0.4558(3) 0.0153(14) Uani 1 1 d . . .
C26 C 0.3425(3) -0.3812(5) 0.5195(4) 0.0198(16) Uani 1 1 d . . .
C27 C 0.2897(3) -0.3148(5) 0.5157(4) 0.0153(15) Uani 1 1 d . . .
C28 C 0.2592(3) -0.2843(5) 0.5851(4) 0.0168(15) Uani 1 1 d . . .
H28 H 0.2821 -0.3243 0.6273 0.020 Uiso 1 1 calc R . .
C29 C 0.1185(3) 0.0599(5) 0.5825(4) 0.0260(17) Uani 1 1 d . . .
H29A H 0.1109 0.0099 0.5409 0.031 Uiso 1 1 calc R . .
H29B H 0.1130 0.0217 0.6285 0.031 Uiso 1 1 calc R . .
C30 C 0.0689(3) 0.1468(5) 0.5717(5) 0.0330(19) Uani 1 1 d . . .
H30A H 0.0803 0.2022 0.6088 0.040 Uiso 1 1 calc R . .
H30B H 0.0699 0.1780 0.5222 0.040 Uiso 1 1 calc R . .
C31 C 0.0014(3) 0.1094(6) 0.5789(5) 0.046(2) Uani 1 1 d . . .
H31A H -0.0077 0.0479 0.5464 0.055 Uiso 1 1 calc R . .
H31B H -0.0006 0.0860 0.6303 0.055 Uiso 1 1 calc R . .
C32 C -0.0499(4) 0.1889(7) 0.5599(6) 0.061(3) Uani 1 1 d . . .
H32A H -0.0420 0.2498 0.5923 0.092 Uiso 1 1 calc R . .
H32B H -0.0915 0.1585 0.5665 0.092 Uiso 1 1 calc R . .
H32C H -0.0496 0.2107 0.5083 0.092 Uiso 1 1 calc R . .
C33 C 0.1011(3) 0.0593(5) 0.3020(4) 0.0222(16) Uani 1 1 d . . .
H33A H 0.1013 -0.0005 0.3365 0.027 Uiso 1 1 calc R . .
H33B H 0.0893 0.0319 0.2515 0.027 Uiso 1 1 calc R . .
C34 C 0.0496(3) 0.1369(6) 0.3199(4) 0.0320(19) Uani 1 1 d . . .
H34A H 0.0086 0.0991 0.3192 0.038 Uiso 1 1 calc R . .
H34B H 0.0611 0.1637 0.3706 0.038 Uiso 1 1 calc R . .
C35 C 0.0401(4) 0.2278(6) 0.2684(5) 0.053(2) Uani 1 1 d . . .
H35A H 0.0282 0.2024 0.2173 0.063 Uiso 1 1 calc R . .
H35B H 0.0805 0.2677 0.2693 0.063 Uiso 1 1 calc R . .
C36 C -0.0122(4) 0.2985(7) 0.2911(6) 0.073(3) Uani 1 1 d . . .
H36A H -0.0451 0.2559 0.3106 0.109 Uiso 1 1 calc R . .
H36B H -0.0313 0.3379 0.2480 0.109 Uiso 1 1 calc R . .
H36C H 0.0061 0.3473 0.3292 0.109 Uiso 1 1 calc R . .
C37 C 0.1880(3) -0.3129(5) 0.2976(4) 0.0221(16) Uani 1 1 d . . .
H37A H 0.1651 -0.2878 0.3388 0.027 Uiso 1 1 calc R . .
H37B H 0.1654 -0.2853 0.2510 0.027 Uiso 1 1 calc R . .
C38 C 0.1863(4) -0.4313(5) 0.2957(4) 0.0328(19) Uani 1 1 d . . .
H38A H 0.2052 -0.4556 0.2515 0.039 Uiso 1 1 calc R . .
H38B H 0.2132 -0.4584 0.3397 0.039 Uiso 1 1 calc R . .
C39 C 0.1206(4) -0.4762(6) 0.2943(5) 0.043(2) Uani 1 1 d . . .
H39A H 0.1208 -0.5486 0.2750 0.052 Uiso 1 1 calc R . .
H39B H 0.0907 -0.4347 0.2601 0.052 Uiso 1 1 calc R . .
C40 C 0.0967(6) -0.4776(8) 0.3701(6) 0.088(4) Uani 1 1 d . . .
H40A H 0.1217 -0.5281 0.4019 0.132 Uiso 1 1 calc R . .
H40B H 0.0516 -0.4978 0.3649 0.132 Uiso 1 1 calc R . .
H40C H 0.1015 -0.4079 0.3922 0.132 Uiso 1 1 calc R . .
C41 C 0.1898(3) -0.3151(5) 0.5802(4) 0.0215(16) Uani 1 1 d . . .
H41A H 0.1666 -0.2818 0.5360 0.026 Uiso 1 1 calc R . .
H41B H 0.1716 -0.2876 0.6241 0.026 Uiso 1 1 calc R . .
C42 C 0.1785(3) -0.4321(5) 0.5758(4) 0.0266(17) Uani 1 1 d . . .
H42A H 0.2047 -0.4664 0.6175 0.032 Uiso 1 1 calc R . .
H42B H 0.1928 -0.4588 0.5294 0.032 Uiso 1 1 calc R . .
C43 C 0.1090(4) -0.4616(5) 0.5781(5) 0.043(2) Uani 1 1 d . . .
H43A H 0.0828 -0.4266 0.5367 0.051 Uiso 1 1 calc R . .
H43B H 0.0949 -0.4355 0.6247 0.051 Uiso 1 1 calc R . .
C44 C 0.0968(4) -0.5808(6) 0.5727(6) 0.055(3) Uani 1 1 d . . .
H44A H 0.1051 -0.6058 0.5239 0.083 Uiso 1 1 calc R . .
H44B H 0.0523 -0.5954 0.5800 0.083 Uiso 1 1 calc R . .
H44C H 0.1253 -0.6167 0.6108 0.083 Uiso 1 1 calc R . .
H4W H 0.3757 0.4398 0.3067 0.024(19) Uiso 1 1 d R . .
H3W H 0.3495 0.4130 0.3848 0.08(3) Uiso 1 1 d R . .
H1S H 0.4067 0.2951 0.3233 0.04(2) Uiso 1 1 d R . .
H1W H 0.4828 -0.0449 0.1570 0.07(3) Uiso 1 1 d R . .
H2W H 0.4959 0.0580 0.1668 0.05(2) Uiso 1 1 d 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 1.378(7) . ?
O1 H1 0.8400 . ?
C1 C2 1.382(9) . ?
C1 C6 1.400(9) . ?
C1 H2 0.9500 . ?
N1I C3I 1.313(8) . ?
N1I C1I 1.373(9) . ?
N1I C4I 1.472(9) . ?
C1I C2I 1.337(9) . ?
C1I H1I 0.9500 . ?
S1S O1S 1.446(4) . ?
S1S O3S 1.448(4) . ?
S1S O4S 1.455(4) . ?
S1S O2S 1.567(5) . ?
O1W H1W 0.7433 . ?
O1W H2W 0.9639 . ?
C2 C3 1.401(9) . ?
C2 C28 1.525(8) . ?
N2I C3I 1.343(8) . ?
N2I C2I 1.379(8) . ?
N2I C6I 1.458(9) . ?
C2I H2I 0.9500 . ?
O2S H1S 1.0271 . ?
O2W H4W 0.9552 . ?
O2W H3W 0.9881 . ?
O8 C18 1.359(7) . ?
O8 H8 0.8400 . ?
C3 O3 1.377(7) . ?
C3 C4 1.389(9) . ?
C3I H3I 0.9500 . ?
O5 C25 1.363(7) . ?
O5 H5 0.8400 . ?
C4 O2 1.356(7) . ?
C4 C5 1.383(9) . ?
C4I C5I 1.488(10) . ?
C4I H4I1 0.9900 . ?
C4I H4I2 0.9900 . ?
O12 C10 1.371(8) . ?
O12 H12 0.8400 . ?
C5 C6 1.395(9) . ?
C5I H5I1 0.9800 . ?
C5I H5I2 0.9800 . ?
C5I H5I3 0.9800 . ?
O2 H13 0.8400 . ?
C6 C7 1.528(8) . ?
C6I H6I1 0.9800 . ?
C6I H6I2 0.9800 . ?
C6I H6I3 0.9800 . ?
O6 C24 1.393(7) . ?
O6 H6 0.8674 . ?
C7 C9 1.531(9) . ?
C7 C29 1.538(9) . ?
C7 H9 1.0000 . ?
O4 C26 1.358(7) . ?
O4 H4 0.8400 . ?
C8 C13 1.388(9) . ?
C8 C9 1.394(9) . ?
C8 H11 0.9500 . ?
C9 C10 1.396(9) . ?
O10 C12 1.387(8) . ?
O10 H10 0.8400 . ?
C10 C11 1.375(9) . ?
C11 C12 1.377(9) . ?
C11 O11 1.378(7) . ?
C12 C13 1.385(9) . ?
O9 C17 1.376(7) . ?
O9 H14 0.8400 . ?
C13 C14 1.534(9) . ?
O3 H3 0.8400 . ?
C14 C33 1.510(8) . ?
C14 C16 1.529(9) . ?
C14 H15 1.0000 . ?
O7 C19 1.375(7) . ?
O7 H7 0.8400 . ?
C15 C20 1.394(9) . ?
C15 C16 1.401(9) . ?
C15 H16 0.9500 . ?
C16 C17 1.398(9) . ?
O11 H17 0.8400 . ?
C17 C18 1.377(9) . ?
C18 C19 1.404(9) . ?
C19 C20 1.400(9) . ?
C20 C21 1.510(9) . ?
C21 C23 1.526(9) . ?
C21 C37 1.532(8) . ?
C21 H21 1.0000 . ?
C22 C27 1.371(9) . ?
C22 C23 1.403(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(8) . ?
C24 C25 1.381(8) . ?
C25 C26 1.394(9) . ?
C26 C27 1.396(9) . ?
C27 C28 1.533(9) . ?
C28 C41 1.509(9) . ?
C28 H28 1.0000 . ?
C29 C30 1.524(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.520(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.496(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.534(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.494(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.520(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.516(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.496(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.524(13) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.517(9) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.517(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.548(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
C5 O1 H1 109.5 . . ?
C2 C1 C6 122.8(6) . . ?
C2 C1 H2 118.6 . . ?
C6 C1 H2 118.6 . . ?
C3I N1I C1I 108.4(6) . . ?
C3I N1I C4I 124.7(6) . . ?
C1I N1I C4I 126.5(6) . . ?
C2I C1I N1I 107.8(6) . . ?
C2I C1I H1I 126.1 . . ?
N1I C1I H1I 126.1 . . ?
O1S S1S O3S 111.5(3) . . ?
O1S S1S O4S 113.4(3) . . ?
O3S S1S O4S 113.7(3) . . ?
O1S S1S O2S 104.2(3) . . ?
O3S S1S O2S 107.1(3) . . ?
O4S S1S O2S 106.1(3) . . ?
H1W O1W H2W 104.1 . . ?
C1 C2 C3 117.7(6) . . ?
C1 C2 C28 124.1(6) . . ?
C3 C2 C28 118.2(6) . . ?
C3I N2I C2I 107.4(6) . . ?
C3I N2I C6I 124.4(6) . . ?
C2I N2I C6I 128.1(6) . . ?
C1I C2I N2I 107.3(6) . . ?
C1I C2I H2I 126.4 . . ?
N2I C2I H2I 126.4 . . ?
S1S O2S H1S 100.7 . . ?
H4W O2W H3W 113.2 . . ?
C18 O8 H8 109.5 . . ?
O3 C3 C4 114.4(5) . . ?
O3 C3 C2 124.8(6) . . ?
C4 C3 C2 120.8(6) . . ?
N1I C3I N2I 109.2(6) . . ?
N1I C3I H3I 125.4 . . ?
N2I C3I H3I 125.4 . . ?
C25 O5 H5 109.5 . . ?
O2 C4 C5 118.2(6) . . ?
O2 C4 C3 122.2(6) . . ?
C5 C4 C3 119.7(6) . . ?
N1I C4I C5I 113.2(6) . . ?
N1I C4I H4I1 108.9 . . ?
C5I C4I H4I1 108.9 . . ?
N1I C4I H4I2 108.9 . . ?
C5I C4I H4I2 108.9 . . ?
H4I1 C4I H4I2 107.8 . . ?
C10 O12 H12 109.5 . . ?
O1 C5 C4 121.4(6) . . ?
O1 C5 C6 117.4(6) . . ?
C4 C5 C6 121.2(6) . . ?
C4I C5I H5I1 109.5 . . ?
C4I C5I H5I2 109.5 . . ?
H5I1 C5I H5I2 109.5 . . ?
C4I C5I H5I3 109.5 . . ?
H5I1 C5I H5I3 109.5 . . ?
H5I2 C5I H5I3 109.5 . . ?
C4 O2 H13 109.5 . . ?
C5 C6 C1 117.5(6) . . ?
C5 C6 C7 119.5(5) . . ?
C1 C6 C7 123.0(6) . . ?
N2I C6I H6I1 109.5 . . ?
N2I C6I H6I2 109.5 . . ?
H6I1 C6I H6I2 109.5 . . ?
N2I C6I H6I3 109.5 . . ?
H6I1 C6I H6I3 109.5 . . ?
H6I2 C6I H6I3 109.5 . . ?
C24 O6 H6 107.8 . . ?
C6 C7 C9 109.3(5) . . ?
C6 C7 C29 113.0(5) . . ?
C9 C7 C29 111.3(5) . . ?
C6 C7 H9 107.7 . . ?
C9 C7 H9 107.7 . . ?
C29 C7 H9 107.7 . . ?
C26 O4 H4 109.5 . . ?
C13 C8 C9 122.1(6) . . ?
C13 C8 H11 119.0 . . ?
C9 C8 H11 119.0 . . ?
C8 C9 C10 117.4(6) . . ?
C8 C9 C7 121.1(6) . . ?
C10 C9 C7 121.5(6) . . ?
C12 O10 H10 109.5 . . ?
O12 C10 C11 113.9(6) . . ?
O12 C10 C9 125.2(6) . . ?
C11 C10 C9 120.9(7) . . ?
C10 C11 C12 120.7(6) . . ?
C10 C11 O11 120.6(6) . . ?
C12 C11 O11 118.6(6) . . ?
C11 C12 C13 120.2(6) . . ?
C11 C12 O10 120.7(6) . . ?
C13 C12 O10 119.1(6) . . ?
C17 O9 H14 109.5 . . ?
C12 C13 C8 118.7(6) . . ?
C12 C13 C14 121.0(6) . . ?
C8 C13 C14 120.3(6) . . ?
C3 O3 H3 109.5 . . ?
C33 C14 C16 114.2(5) . . ?
C33 C14 C13 113.7(5) . . ?
C16 C14 C13 109.3(5) . . ?
C33 C14 H15 106.3 . . ?
C16 C14 H15 106.3 . . ?
C13 C14 H15 106.3 . . ?
C19 O7 H7 109.5 . . ?
C20 C15 C16 123.3(6) . . ?
C20 C15 H16 118.4 . . ?
C16 C15 H16 118.4 . . ?
C17 C16 C15 116.5(6) . . ?
C17 C16 C14 121.2(6) . . ?
C15 C16 C14 122.1(6) . . ?
C11 O11 H17 109.5 . . ?
O9 C17 C18 113.2(5) . . ?
O9 C17 C16 124.5(6) . . ?
C18 C17 C16 122.3(6) . . ?
O8 C18 C17 122.0(6) . . ?
O8 C18 C19 118.6(6) . . ?
C17 C18 C19 119.4(6) . . ?
O7 C19 C20 118.5(6) . . ?
O7 C19 C18 120.9(6) . . ?
C20 C19 C18 120.6(6) . . ?
C15 C20 C19 117.6(6) . . ?
C15 C20 C21 124.5(6) . . ?
C19 C20 C21 117.8(6) . . ?
C20 C21 C23 112.3(5) . . ?
C20 C21 C37 114.3(5) . . ?
C23 C21 C37 110.7(5) . . ?
C20 C21 H21 106.3 . . ?
C23 C21 H21 106.3 . . ?
C37 C21 H21 106.3 . . ?
C27 C22 C23 123.6(6) . . ?
C27 C22 H22 118.2 . . ?
C23 C22 H22 118.2 . . ?
C24 C23 C22 116.3(6) . . ?
C24 C23 C21 123.1(6) . . ?
C22 C23 C21 120.4(5) . . ?
C23 C24 C25 122.5(6) . . ?
C23 C24 O6 122.4(5) . . ?
C25 C24 O6 115.1(5) . . ?
O5 C25 C24 124.1(5) . . ?
O5 C25 C26 116.9(5) . . ?
C24 C25 C26 119.0(6) . . ?
O4 C26 C25 120.9(6) . . ?
O4 C26 C27 118.5(6) . . ?
C25 C26 C27 120.6(6) . . ?
C22 C27 C26 117.8(6) . . ?
C22 C27 C28 120.8(5) . . ?
C26 C27 C28 121.5(6) . . ?
C41 C28 C2 113.7(5) . . ?
C41 C28 C27 112.3(5) . . ?
C2 C28 C27 109.5(5) . . ?
C41 C28 H28 107.0 . . ?
C2 C28 H28 107.0 . . ?
C27 C28 H28 107.0 . . ?
C30 C29 C7 113.4(5) . . ?
C30 C29 H29A 108.9 . . ?
C7 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C7 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C31 C30 C29 113.3(6) . . ?
C31 C30 H30A 108.9 . . ?
C29 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C30 115.1(7) . . ?
C32 C31 H31A 108.5 . . ?
C30 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C30 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C14 C33 C34 115.1(5) . . ?
C14 C33 H33A 108.5 . . ?
C34 C33 H33A 108.5 . . ?
C14 C33 H33B 108.5 . . ?
C34 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C35 C34 C33 114.7(6) . . ?
C35 C34 H34A 108.6 . . ?
C33 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C34 C35 C36 109.9(8) . . ?
C34 C35 H35A 109.7 . . ?
C36 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
C36 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C21 112.2(6) . . ?
C38 C37 H37A 109.2 . . ?
C21 C37 H37A 109.2 . . ?
C38 C37 H37B 109.2 . . ?
C21 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C39 C38 C37 113.8(6) . . ?
C39 C38 H38A 108.8 . . ?
C37 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C37 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C38 C39 C40 112.9(8) . . ?
C38 C39 H39A 109.0 . . ?
C40 C39 H39A 109.0 . . ?
C38 C39 H39B 109.0 . . ?
C40 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C28 C41 C42 114.0(5) . . ?
C28 C41 H41A 108.8 . . ?
C42 C41 H41A 108.8 . . ?
C28 C41 H41B 108.8 . . ?
C42 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
C41 C42 C43 113.0(6) . . ?
C41 C42 H42A 109.0 . . ?
C43 C42 H42A 109.0 . . ?
C41 C42 H42B 109.0 . . ?
C43 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C42 C43 C44 113.4(6) . . ?
C42 C43 H43A 108.9 . . ?
C44 C43 H43A 108.9 . . ?
C42 C43 H43B 108.9 . . ?
C44 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3I N1I C1I C2I 1.6(8) . . . . ?
C4I N1I C1I C2I 174.5(6) . . . . ?
C6 C1 C2 C3 -1.6(9) . . . . ?
C6 C1 C2 C28 179.4(6) . . . . ?
N1I C1I C2I N2I -0.9(8) . . . . ?
C3I N2I C2I C1I -0.1(8) . . . . ?
C6I N2I C2I C1I -177.5(6) . . . . ?
C1 C2 C3 O3 -172.0(6) . . . . ?
C28 C2 C3 O3 7.0(9) . . . . ?
C1 C2 C3 C4 5.9(9) . . . . ?
C28 C2 C3 C4 -175.0(6) . . . . ?
C1I N1I C3I N2I -1.7(8) . . . . ?
C4I N1I C3I N2I -174.7(6) . . . . ?
C2I N2I C3I N1I 1.2(8) . . . . ?
C6I N2I C3I N1I 178.7(6) . . . . ?
O3 C3 C4 O2 -6.6(9) . . . . ?
C2 C3 C4 O2 175.2(6) . . . . ?
O3 C3 C4 C5 173.0(6) . . . . ?
C2 C3 C4 C5 -5.1(9) . . . . ?
C3I N1I C4I C5I -139.2(7) . . . . ?
C1I N1I C4I C5I 49.0(10) . . . . ?
O2 C4 C5 O1 1.9(9) . . . . ?
C3 C4 C5 O1 -177.7(6) . . . . ?
O2 C4 C5 C6 179.6(6) . . . . ?
C3 C4 C5 C6 -0.1(10) . . . . ?
O1 C5 C6 C1 -178.1(6) . . . . ?
C4 C5 C6 C1 4.2(9) . . . . ?
O1 C5 C6 C7 2.8(9) . . . . ?
C4 C5 C6 C7 -174.9(6) . . . . ?
C2 C1 C6 C5 -3.3(9) . . . . ?
C2 C1 C6 C7 175.7(6) . . . . ?
C5 C6 C7 C9 80.5(7) . . . . ?
C1 C6 C7 C9 -98.5(7) . . . . ?
C5 C6 C7 C29 -155.0(6) . . . . ?
C1 C6 C7 C29 25.9(9) . . . . ?
C13 C8 C9 C10 -2.1(9) . . . . ?
C13 C8 C9 C7 177.1(5) . . . . ?
C6 C7 C9 C8 78.5(7) . . . . ?
C29 C7 C9 C8 -47.0(8) . . . . ?
C6 C7 C9 C10 -102.3(7) . . . . ?
C29 C7 C9 C10 132.2(6) . . . . ?
C8 C9 C10 O12 178.5(6) . . . . ?
C7 C9 C10 O12 -0.7(10) . . . . ?
C8 C9 C10 C11 1.4(9) . . . . ?
C7 C9 C10 C11 -177.8(6) . . . . ?
O12 C10 C11 C12 -177.3(6) . . . . ?
C9 C10 C11 C12 0.1(10) . . . . ?
O12 C10 C11 O11 3.3(9) . . . . ?
C9 C10 C11 O11 -179.3(6) . . . . ?
C10 C11 C12 C13 -0.9(10) . . . . ?
O11 C11 C12 C13 178.5(6) . . . . ?
C10 C11 C12 O10 178.8(6) . . . . ?
O11 C11 C12 O10 -1.8(9) . . . . ?
C11 C12 C13 C8 0.2(9) . . . . ?
O10 C12 C13 C8 -179.6(5) . . . . ?
C11 C12 C13 C14 -179.2(6) . . . . ?
O10 C12 C13 C14 1.1(9) . . . . ?
C9 C8 C13 C12 1.4(9) . . . . ?
C9 C8 C13 C14 -179.3(6) . . . . ?
C12 C13 C14 C33 -133.4(6) . . . . ?
C8 C13 C14 C33 47.3(8) . . . . ?
C12 C13 C14 C16 97.6(7) . . . . ?
C8 C13 C14 C16 -81.7(7) . . . . ?
C20 C15 C16 C17 3.0(9) . . . . ?
C20 C15 C16 C14 -172.7(6) . . . . ?
C33 C14 C16 C17 154.7(6) . . . . ?
C13 C14 C16 C17 -76.7(8) . . . . ?
C33 C14 C16 C15 -29.9(9) . . . . ?
C13 C14 C16 C15 98.8(7) . . . . ?
C15 C16 C17 O9 176.1(6) . . . . ?
C14 C16 C17 O9 -8.2(10) . . . . ?
C15 C16 C17 C18 -4.6(9) . . . . ?
C14 C16 C17 C18 171.1(6) . . . . ?
O9 C17 C18 O8 3.1(9) . . . . ?
C16 C17 C18 O8 -176.3(6) . . . . ?
O9 C17 C18 C19 -179.2(5) . . . . ?
C16 C17 C18 C19 1.4(10) . . . . ?
O8 C18 C19 O7 0.7(9) . . . . ?
C17 C18 C19 O7 -177.1(6) . . . . ?
O8 C18 C19 C20 -178.5(6) . . . . ?
C17 C18 C19 C20 3.8(9) . . . . ?
C16 C15 C20 C19 1.9(10) . . . . ?
C16 C15 C20 C21 -178.8(6) . . . . ?
O7 C19 C20 C15 175.5(5) . . . . ?
C18 C19 C20 C15 -5.3(9) . . . . ?
O7 C19 C20 C21 -3.8(9) . . . . ?
C18 C19 C20 C21 175.4(6) . . . . ?
C15 C20 C21 C23 -101.5(7) . . . . ?
C19 C20 C21 C23 77.8(7) . . . . ?
C15 C20 C21 C37 25.6(9) . . . . ?
C19 C20 C21 C37 -155.1(6) . . . . ?
C27 C22 C23 C24 -1.9(9) . . . . ?
C27 C22 C23 C21 172.8(6) . . . . ?
C20 C21 C23 C24 -112.8(7) . . . . ?
C37 C21 C23 C24 118.1(6) . . . . ?
C20 C21 C23 C22 72.8(7) . . . . ?
C37 C21 C23 C22 -56.2(7) . . . . ?
C22 C23 C24 C25 4.5(9) . . . . ?
C21 C23 C24 C25 -170.0(6) . . . . ?
C22 C23 C24 O6 -177.5(5) . . . . ?
C21 C23 C24 O6 7.9(9) . . . . ?
C23 C24 C25 O5 175.2(6) . . . . ?
O6 C24 C25 O5 -2.9(9) . . . . ?
C23 C24 C25 C26 -4.1(9) . . . . ?
O6 C24 C25 C26 177.9(5) . . . . ?
O5 C25 C26 O4 2.3(9) . . . . ?
C24 C25 C26 O4 -178.4(6) . . . . ?
O5 C25 C26 C27 -178.5(5) . . . . ?
C24 C25 C26 C27 0.8(9) . . . . ?
C23 C22 C27 C26 -1.1(9) . . . . ?
C23 C22 C27 C28 179.8(5) . . . . ?
O4 C26 C27 C22 -179.1(5) . . . . ?
C25 C26 C27 C22 1.7(9) . . . . ?
O4 C26 C27 C28 0.0(9) . . . . ?
C25 C26 C27 C28 -179.2(6) . . . . ?
C1 C2 C28 C41 -20.8(9) . . . . ?
C3 C2 C28 C41 160.2(6) . . . . ?
C1 C2 C28 C27 105.7(7) . . . . ?
C3 C2 C28 C27 -73.3(7) . . . . ?
C22 C27 C28 C41 57.9(7) . . . . ?
C26 C27 C28 C41 -121.2(6) . . . . ?
C22 C27 C28 C2 -69.4(7) . . . . ?
C26 C27 C28 C2 111.5(6) . . . . ?
C6 C7 C29 C30 174.3(6) . . . . ?
C9 C7 C29 C30 -62.4(8) . . . . ?
C7 C29 C30 C31 -171.5(7) . . . . ?
C29 C30 C31 C32 -173.0(7) . . . . ?
C16 C14 C33 C34 180.0(6) . . . . ?
C13 C14 C33 C34 53.6(8) . . . . ?
C14 C33 C34 C35 62.7(9) . . . . ?
C33 C34 C35 C36 179.5(7) . . . . ?
C20 C21 C37 C38 168.2(6) . . . . ?
C23 C21 C37 C38 -63.9(7) . . . . ?
C21 C37 C38 C39 173.8(6) . . . . ?
C37 C38 C39 C40 -79.3(9) . . . . ?
C2 C28 C41 C42 -171.1(6) . . . . ?
C27 C28 C41 C42 63.9(7) . . . . ?
C28 C41 C42 C43 174.7(6) . . . . ?
C41 C42 C43 C44 179.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.114
_database_code_depnum_ccdc_archive 'CCDC 986746'
#######################################################################
#
#                 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_F:\xtals\Completed\pgc4emimace\twin.CIF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            pgc4emimace
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H56 O12, C6 H11 N2, H O4 S, 2(H2 O)'
_chemical_formula_sum            'C50 H72 N2 O18 S'
_chemical_formula_weight         1021.16

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   21.075(9)
_cell_length_b                   12.796(6)
_cell_length_c                   18.229(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.533(6)
_cell_angle_gamma                90.00
_cell_volume                     4884(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2389
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.27

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9577
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8413
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1696
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8413
_reflns_number_gt                3996
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'
_computing_publication_material  
'X-Seed (Atwood & Barbour, 2003; Barbour, 2001)'

_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)+(0.1319P)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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8413
_refine_ls_number_parameters     662
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2169
_refine_ls_R_factor_gt           0.0934
_refine_ls_wR_factor_ref         0.2636
_refine_ls_wR_factor_gt          0.2099
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.3092(2) 0.1433(3) 0.6566(3) 0.0218(11) Uani 1 1 d . . .
H1 H 0.3481 0.1518 0.6709 0.026 Uiso 1 1 calc R . .
C1 C 0.2250(3) -0.0919(5) 0.5889(4) 0.0173(15) Uani 1 1 d . . .
H2 H 0.1832 -0.1116 0.5685 0.021 Uiso 1 1 calc R . .
N1I N 0.4728(3) -0.1639(4) 0.4517(3) 0.0278(14) Uani 1 1 d . . .
C1I C 0.4887(3) -0.0848(6) 0.4064(4) 0.0297(18) Uani 1 1 d . . .
H1I H 0.5263 -0.0809 0.3823 0.036 Uiso 1 1 calc R . .
S1S S 0.47045(8) 0.24290(13) 0.25650(9) 0.0194(4) Uani 1 1 d . . .
O1S O 0.5062(2) 0.1468(3) 0.2532(3) 0.0260(12) Uani 1 1 d . . .
O1W O 0.4918(2) -0.0009(4) 0.1337(3) 0.0244(11) Uani 1 1 d . . .
C2 C 0.2711(3) -0.1686(5) 0.6014(3) 0.0185(15) Uani 1 1 d . . .
N2I N 0.3961(3) -0.0505(4) 0.4443(3) 0.0227(13) Uani 1 1 d . . .
C2I C 0.4418(3) -0.0140(5) 0.4021(4) 0.0270(17) Uani 1 1 d . . .
H2I H 0.4402 0.0496 0.3751 0.032 Uiso 1 1 calc R . .
O2S O 0.4371(2) 0.2321(4) 0.3287(3) 0.0297(12) Uani 1 1 d . . .
O2W O 0.3536(2) 0.3904(4) 0.3337(3) 0.0302(12) Uani 1 1 d . . .
O8 O 0.3808(2) 0.0234(4) 0.2328(3) 0.0252(11) Uani 1 1 d . . .
H8 H 0.3807 0.0126 0.1873 0.030 Uiso 1 1 calc R . .
C3 C 0.3328(3) -0.1375(5) 0.6298(3) 0.0167(15) Uani 1 1 d . . .
C3I C 0.4167(3) -0.1429(5) 0.4729(4) 0.0259(17) Uani 1 1 d . . .
H3I H 0.3942 -0.1861 0.5035 0.031 Uiso 1 1 calc R . .
O3S O 0.4203(2) 0.2511(3) 0.1955(2) 0.0250(11) Uani 1 1 d . . .
O5 O 0.4206(2) -0.4743(3) 0.4641(2) 0.0210(11) Uani 1 1 d . . .
H5 H 0.4360 -0.4800 0.4237 0.025 Uiso 1 1 calc R . .
C4 C 0.3455(3) -0.0346(5) 0.6510(4) 0.0188(15) Uani 1 1 d . . .
C4I C 0.5079(3) -0.2624(6) 0.4671(4) 0.0319(18) Uani 1 1 d . . .
H4I1 H 0.5013 -0.3077 0.4229 0.038 Uiso 1 1 calc R . .
H4I2 H 0.4900 -0.2991 0.5080 0.038 Uiso 1 1 calc R . .
O4S O 0.5107(2) 0.3353(3) 0.2665(3) 0.0247(11) Uani 1 1 d . . .
O12 O 0.2508(2) 0.3080(3) 0.5766(2) 0.0231(11) Uani 1 1 d . . .
H12 H 0.2665 0.2678 0.6103 0.028 Uiso 1 1 calc R . .
C5 C 0.2979(3) 0.0398(5) 0.6387(4) 0.0182(15) Uani 1 1 d . . .
C5I C 0.5776(3) -0.2469(6) 0.4875(4) 0.0372(19) Uani 1 1 d . . .
H5I1 H 0.5955 -0.2093 0.4478 0.056 Uiso 1 1 calc R . .
H5I2 H 0.5986 -0.3151 0.4948 0.056 Uiso 1 1 calc R . .
H5I3 H 0.5847 -0.2063 0.5332 0.056 Uiso 1 1 calc R . .
O2 O 0.40352(19) -0.0038(3) 0.6835(3) 0.0228(11) Uani 1 1 d . . .
H13 H 0.4300 -0.0524 0.6811 0.027 Uiso 1 1 calc R . .
C6 C 0.2371(3) 0.0137(5) 0.6052(3) 0.0171(15) Uani 1 1 d . . .
C6I C 0.3349(3) -0.0032(6) 0.4549(4) 0.0337(19) Uani 1 1 d . . .
H6I1 H 0.3047 -0.0579 0.4654 0.050 Uiso 1 1 calc R . .
H6I2 H 0.3181 0.0344 0.4100 0.050 Uiso 1 1 calc R . .
H6I3 H 0.3407 0.0458 0.4965 0.050 Uiso 1 1 calc R . .
O6 O 0.3767(2) -0.3920(3) 0.3289(2) 0.0249(11) Uani 1 1 d . . .
H6 H 0.3797 -0.3363 0.3024 0.030 Uiso 1 1 d . . .
C7 C 0.1877(3) 0.0998(5) 0.5867(3) 0.0163(15) Uani 1 1 d . . .
H9 H 0.1937 0.1531 0.6270 0.020 Uiso 1 1 calc R . .
O4 O 0.3669(2) -0.4189(4) 0.5864(2) 0.0267(12) Uani 1 1 d . . .
H4 H 0.4004 -0.4527 0.5820 0.032 Uiso 1 1 calc R . .
C8 C 0.1816(3) 0.1074(5) 0.4465(3) 0.0161(15) Uani 1 1 d . . .
H11 H 0.1623 0.0401 0.4451 0.019 Uiso 1 1 calc R . .
C9 C 0.2004(3) 0.1534(5) 0.5148(4) 0.0201(15) Uani 1 1 d . . .
O10 O 0.2276(2) 0.3036(3) 0.3170(3) 0.0295(12) Uani 1 1 d . . .
H10 H 0.2549 0.3514 0.3252 0.035 Uiso 1 1 calc R . .
C10 C 0.2305(3) 0.2507(5) 0.5148(4) 0.0248(16) Uani 1 1 d . . .
C11 C 0.2397(3) 0.2994(5) 0.4497(4) 0.0216(16) Uani 1 1 d . . .
C12 C 0.2194(3) 0.2536(5) 0.3828(3) 0.0180(15) Uani 1 1 d . . .
O9 O 0.2869(2) 0.1582(3) 0.2413(3) 0.0259(11) Uani 1 1 d . . .
H14 H 0.2635 0.1996 0.2618 0.031 Uiso 1 1 calc R . .
C13 C 0.1900(3) 0.1566(5) 0.3804(4) 0.0184(15) Uani 1 1 d . . .
O3 O 0.38549(19) -0.2019(3) 0.6372(3) 0.0221(11) Uani 1 1 d . . .
H3 H 0.3742 -0.2631 0.6460 0.026 Uiso 1 1 calc R . .
C14 C 0.1679(3) 0.1034(5) 0.3065(3) 0.0188(15) Uani 1 1 d . . .
H15 H 0.1667 0.1592 0.2679 0.023 Uiso 1 1 calc R . .
O7 O 0.3686(2) -0.1844(3) 0.2697(3) 0.0249(11) Uani 1 1 d . . .
H7 H 0.4033 -0.1530 0.2811 0.030 Uiso 1 1 calc R . .
C15 C 0.2129(3) -0.0824(5) 0.3024(3) 0.0180(15) Uani 1 1 d . . .
H16 H 0.1743 -0.1073 0.3183 0.022 Uiso 1 1 calc R . .
C16 C 0.2184(3) 0.0247(5) 0.2885(4) 0.0180(15) Uani 1 1 d . . .
O11 O 0.2700(2) 0.3949(3) 0.4500(3) 0.0294(12) Uani 1 1 d . . .
H17 H 0.2768 0.4171 0.4935 0.035 Uiso 1 1 calc R . .
C17 C 0.2749(3) 0.0574(5) 0.2620(4) 0.0187(15) Uani 1 1 d . . .
C18 C 0.3247(3) -0.0100(5) 0.2547(3) 0.0154(14) Uani 1 1 d . . .
C19 C 0.3187(3) -0.1159(5) 0.2730(4) 0.0197(16) Uani 1 1 d . . .
C20 C 0.2613(3) -0.1543(5) 0.2942(4) 0.0194(15) Uani 1 1 d . . .
C21 C 0.2564(3) -0.2703(5) 0.3075(3) 0.0172(15) Uani 1 1 d . . .
H21 H 0.2793 -0.3053 0.2690 0.021 Uiso 1 1 calc R . .
C22 C 0.2652(3) -0.2786(5) 0.4476(4) 0.0171(15) Uani 1 1 d . . .
H22 H 0.2288 -0.2344 0.4445 0.020 Uiso 1 1 calc R . .
C23 C 0.2909(3) -0.3032(5) 0.3820(3) 0.0158(15) Uani 1 1 d . . .
C24 C 0.3448(3) -0.3649(4) 0.3891(3) 0.0128(14) Uani 1 1 d . . .
C25 C 0.3701(3) -0.4070(5) 0.4558(3) 0.0153(14) Uani 1 1 d . . .
C26 C 0.3425(3) -0.3812(5) 0.5195(4) 0.0198(16) Uani 1 1 d . . .
C27 C 0.2897(3) -0.3148(5) 0.5157(4) 0.0153(15) Uani 1 1 d . . .
C28 C 0.2592(3) -0.2843(5) 0.5851(4) 0.0168(15) Uani 1 1 d . . .
H28 H 0.2821 -0.3243 0.6273 0.020 Uiso 1 1 calc R . .
C29 C 0.1185(3) 0.0599(5) 0.5825(4) 0.0260(17) Uani 1 1 d . . .
H29A H 0.1109 0.0099 0.5409 0.031 Uiso 1 1 calc R . .
H29B H 0.1130 0.0217 0.6285 0.031 Uiso 1 1 calc R . .
C30 C 0.0689(3) 0.1468(5) 0.5717(5) 0.0330(19) Uani 1 1 d . . .
H30A H 0.0803 0.2022 0.6088 0.040 Uiso 1 1 calc R . .
H30B H 0.0699 0.1780 0.5222 0.040 Uiso 1 1 calc R . .
C31 C 0.0014(3) 0.1094(6) 0.5789(5) 0.046(2) Uani 1 1 d . . .
H31A H -0.0077 0.0479 0.5464 0.055 Uiso 1 1 calc R . .
H31B H -0.0006 0.0860 0.6303 0.055 Uiso 1 1 calc R . .
C32 C -0.0499(4) 0.1889(7) 0.5599(6) 0.061(3) Uani 1 1 d . . .
H32A H -0.0420 0.2498 0.5923 0.092 Uiso 1 1 calc R . .
H32B H -0.0915 0.1585 0.5665 0.092 Uiso 1 1 calc R . .
H32C H -0.0496 0.2107 0.5083 0.092 Uiso 1 1 calc R . .
C33 C 0.1011(3) 0.0593(5) 0.3020(4) 0.0222(16) Uani 1 1 d . . .
H33A H 0.1013 -0.0005 0.3365 0.027 Uiso 1 1 calc R . .
H33B H 0.0893 0.0319 0.2515 0.027 Uiso 1 1 calc R . .
C34 C 0.0496(3) 0.1369(6) 0.3199(4) 0.0320(19) Uani 1 1 d . . .
H34A H 0.0086 0.0991 0.3192 0.038 Uiso 1 1 calc R . .
H34B H 0.0611 0.1637 0.3706 0.038 Uiso 1 1 calc R . .
C35 C 0.0401(4) 0.2278(6) 0.2684(5) 0.053(2) Uani 1 1 d . . .
H35A H 0.0282 0.2024 0.2173 0.063 Uiso 1 1 calc R . .
H35B H 0.0805 0.2677 0.2693 0.063 Uiso 1 1 calc R . .
C36 C -0.0122(4) 0.2985(7) 0.2911(6) 0.073(3) Uani 1 1 d . . .
H36A H -0.0451 0.2559 0.3106 0.109 Uiso 1 1 calc R . .
H36B H -0.0313 0.3379 0.2480 0.109 Uiso 1 1 calc R . .
H36C H 0.0061 0.3473 0.3292 0.109 Uiso 1 1 calc R . .
C37 C 0.1880(3) -0.3129(5) 0.2976(4) 0.0221(16) Uani 1 1 d . . .
H37A H 0.1651 -0.2878 0.3388 0.027 Uiso 1 1 calc R . .
H37B H 0.1654 -0.2853 0.2510 0.027 Uiso 1 1 calc R . .
C38 C 0.1863(4) -0.4313(5) 0.2957(4) 0.0328(19) Uani 1 1 d . . .
H38A H 0.2052 -0.4556 0.2515 0.039 Uiso 1 1 calc R . .
H38B H 0.2132 -0.4584 0.3397 0.039 Uiso 1 1 calc R . .
C39 C 0.1206(4) -0.4762(6) 0.2943(5) 0.043(2) Uani 1 1 d . . .
H39A H 0.1208 -0.5486 0.2750 0.052 Uiso 1 1 calc R . .
H39B H 0.0907 -0.4347 0.2601 0.052 Uiso 1 1 calc R . .
C40 C 0.0967(6) -0.4776(8) 0.3701(6) 0.088(4) Uani 1 1 d . . .
H40A H 0.1217 -0.5281 0.4019 0.132 Uiso 1 1 calc R . .
H40B H 0.0516 -0.4978 0.3649 0.132 Uiso 1 1 calc R . .
H40C H 0.1015 -0.4079 0.3922 0.132 Uiso 1 1 calc R . .
C41 C 0.1898(3) -0.3151(5) 0.5802(4) 0.0215(16) Uani 1 1 d . . .
H41A H 0.1666 -0.2818 0.5360 0.026 Uiso 1 1 calc R . .
H41B H 0.1716 -0.2876 0.6241 0.026 Uiso 1 1 calc R . .
C42 C 0.1785(3) -0.4321(5) 0.5758(4) 0.0266(17) Uani 1 1 d . . .
H42A H 0.2047 -0.4664 0.6175 0.032 Uiso 1 1 calc R . .
H42B H 0.1928 -0.4588 0.5294 0.032 Uiso 1 1 calc R . .
C43 C 0.1090(4) -0.4616(5) 0.5781(5) 0.043(2) Uani 1 1 d . . .
H43A H 0.0828 -0.4266 0.5367 0.051 Uiso 1 1 calc R . .
H43B H 0.0949 -0.4355 0.6247 0.051 Uiso 1 1 calc R . .
C44 C 0.0968(4) -0.5808(6) 0.5727(6) 0.055(3) Uani 1 1 d . . .
H44A H 0.1051 -0.6058 0.5239 0.083 Uiso 1 1 calc R . .
H44B H 0.0523 -0.5954 0.5800 0.083 Uiso 1 1 calc R . .
H44C H 0.1253 -0.6167 0.6108 0.083 Uiso 1 1 calc R . .
H4W H 0.3757 0.4398 0.3067 0.024(19) Uiso 1 1 d R . .
H3W H 0.3495 0.4130 0.3848 0.08(3) Uiso 1 1 d R . .
H1S H 0.4067 0.2951 0.3233 0.04(2) Uiso 1 1 d R . .
H1W H 0.4828 -0.0449 0.1570 0.07(3) Uiso 1 1 d R . .
H2W H 0.4959 0.0580 0.1668 0.05(2) Uiso 1 1 d 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 1.378(7) . ?
O1 H1 0.8400 . ?
C1 C2 1.382(9) . ?
C1 C6 1.400(9) . ?
C1 H2 0.9500 . ?
N1I C3I 1.313(8) . ?
N1I C1I 1.373(9) . ?
N1I C4I 1.472(9) . ?
C1I C2I 1.337(9) . ?
C1I H1I 0.9500 . ?
S1S O1S 1.446(4) . ?
S1S O3S 1.448(4) . ?
S1S O4S 1.455(4) . ?
S1S O2S 1.567(5) . ?
O1W H1W 0.7433 . ?
O1W H2W 0.9639 . ?
C2 C3 1.401(9) . ?
C2 C28 1.525(8) . ?
N2I C3I 1.343(8) . ?
N2I C2I 1.379(8) . ?
N2I C6I 1.458(9) . ?
C2I H2I 0.9500 . ?
O2S H1S 1.0271 . ?
O2W H4W 0.9552 . ?
O2W H3W 0.9881 . ?
O8 C18 1.359(7) . ?
O8 H8 0.8400 . ?
C3 O3 1.377(7) . ?
C3 C4 1.389(9) . ?
C3I H3I 0.9500 . ?
O5 C25 1.363(7) . ?
O5 H5 0.8400 . ?
C4 O2 1.356(7) . ?
C4 C5 1.383(9) . ?
C4I C5I 1.488(10) . ?
C4I H4I1 0.9900 . ?
C4I H4I2 0.9900 . ?
O12 C10 1.371(8) . ?
O12 H12 0.8400 . ?
C5 C6 1.395(9) . ?
C5I H5I1 0.9800 . ?
C5I H5I2 0.9800 . ?
C5I H5I3 0.9800 . ?
O2 H13 0.8400 . ?
C6 C7 1.528(8) . ?
C6I H6I1 0.9800 . ?
C6I H6I2 0.9800 . ?
C6I H6I3 0.9800 . ?
O6 C24 1.393(7) . ?
O6 H6 0.8674 . ?
C7 C9 1.531(9) . ?
C7 C29 1.538(9) . ?
C7 H9 1.0000 . ?
O4 C26 1.358(7) . ?
O4 H4 0.8400 . ?
C8 C13 1.388(9) . ?
C8 C9 1.394(9) . ?
C8 H11 0.9500 . ?
C9 C10 1.396(9) . ?
O10 C12 1.387(8) . ?
O10 H10 0.8400 . ?
C10 C11 1.375(9) . ?
C11 C12 1.377(9) . ?
C11 O11 1.378(7) . ?
C12 C13 1.385(9) . ?
O9 C17 1.376(7) . ?
O9 H14 0.8400 . ?
C13 C14 1.534(9) . ?
O3 H3 0.8400 . ?
C14 C33 1.510(8) . ?
C14 C16 1.529(9) . ?
C14 H15 1.0000 . ?
O7 C19 1.375(7) . ?
O7 H7 0.8400 . ?
C15 C20 1.394(9) . ?
C15 C16 1.401(9) . ?
C15 H16 0.9500 . ?
C16 C17 1.398(9) . ?
O11 H17 0.8400 . ?
C17 C18 1.377(9) . ?
C18 C19 1.404(9) . ?
C19 C20 1.400(9) . ?
C20 C21 1.510(9) . ?
C21 C23 1.526(9) . ?
C21 C37 1.532(8) . ?
C21 H21 1.0000 . ?
C22 C27 1.371(9) . ?
C22 C23 1.403(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(8) . ?
C24 C25 1.381(8) . ?
C25 C26 1.394(9) . ?
C26 C27 1.396(9) . ?
C27 C28 1.533(9) . ?
C28 C41 1.509(9) . ?
C28 H28 1.0000 . ?
C29 C30 1.524(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.520(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.496(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.534(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.494(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.520(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.516(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.496(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.524(13) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.517(9) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.517(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.548(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
C5 O1 H1 109.5 . . ?
C2 C1 C6 122.8(6) . . ?
C2 C1 H2 118.6 . . ?
C6 C1 H2 118.6 . . ?
C3I N1I C1I 108.4(6) . . ?
C3I N1I C4I 124.7(6) . . ?
C1I N1I C4I 126.5(6) . . ?
C2I C1I N1I 107.8(6) . . ?
C2I C1I H1I 126.1 . . ?
N1I C1I H1I 126.1 . . ?
O1S S1S O3S 111.5(3) . . ?
O1S S1S O4S 113.4(3) . . ?
O3S S1S O4S 113.7(3) . . ?
O1S S1S O2S 104.2(3) . . ?
O3S S1S O2S 107.1(3) . . ?
O4S S1S O2S 106.1(3) . . ?
H1W O1W H2W 104.1 . . ?
C1 C2 C3 117.7(6) . . ?
C1 C2 C28 124.1(6) . . ?
C3 C2 C28 118.2(6) . . ?
C3I N2I C2I 107.4(6) . . ?
C3I N2I C6I 124.4(6) . . ?
C2I N2I C6I 128.1(6) . . ?
C1I C2I N2I 107.3(6) . . ?
C1I C2I H2I 126.4 . . ?
N2I C2I H2I 126.4 . . ?
S1S O2S H1S 100.7 . . ?
H4W O2W H3W 113.2 . . ?
C18 O8 H8 109.5 . . ?
O3 C3 C4 114.4(5) . . ?
O3 C3 C2 124.8(6) . . ?
C4 C3 C2 120.8(6) . . ?
N1I C3I N2I 109.2(6) . . ?
N1I C3I H3I 125.4 . . ?
N2I C3I H3I 125.4 . . ?
C25 O5 H5 109.5 . . ?
O2 C4 C5 118.2(6) . . ?
O2 C4 C3 122.2(6) . . ?
C5 C4 C3 119.7(6) . . ?
N1I C4I C5I 113.2(6) . . ?
N1I C4I H4I1 108.9 . . ?
C5I C4I H4I1 108.9 . . ?
N1I C4I H4I2 108.9 . . ?
C5I C4I H4I2 108.9 . . ?
H4I1 C4I H4I2 107.8 . . ?
C10 O12 H12 109.5 . . ?
O1 C5 C4 121.4(6) . . ?
O1 C5 C6 117.4(6) . . ?
C4 C5 C6 121.2(6) . . ?
C4I C5I H5I1 109.5 . . ?
C4I C5I H5I2 109.5 . . ?
H5I1 C5I H5I2 109.5 . . ?
C4I C5I H5I3 109.5 . . ?
H5I1 C5I H5I3 109.5 . . ?
H5I2 C5I H5I3 109.5 . . ?
C4 O2 H13 109.5 . . ?
C5 C6 C1 117.5(6) . . ?
C5 C6 C7 119.5(5) . . ?
C1 C6 C7 123.0(6) . . ?
N2I C6I H6I1 109.5 . . ?
N2I C6I H6I2 109.5 . . ?
H6I1 C6I H6I2 109.5 . . ?
N2I C6I H6I3 109.5 . . ?
H6I1 C6I H6I3 109.5 . . ?
H6I2 C6I H6I3 109.5 . . ?
C24 O6 H6 107.8 . . ?
C6 C7 C9 109.3(5) . . ?
C6 C7 C29 113.0(5) . . ?
C9 C7 C29 111.3(5) . . ?
C6 C7 H9 107.7 . . ?
C9 C7 H9 107.7 . . ?
C29 C7 H9 107.7 . . ?
C26 O4 H4 109.5 . . ?
C13 C8 C9 122.1(6) . . ?
C13 C8 H11 119.0 . . ?
C9 C8 H11 119.0 . . ?
C8 C9 C10 117.4(6) . . ?
C8 C9 C7 121.1(6) . . ?
C10 C9 C7 121.5(6) . . ?
C12 O10 H10 109.5 . . ?
O12 C10 C11 113.9(6) . . ?
O12 C10 C9 125.2(6) . . ?
C11 C10 C9 120.9(7) . . ?
C10 C11 C12 120.7(6) . . ?
C10 C11 O11 120.6(6) . . ?
C12 C11 O11 118.6(6) . . ?
C11 C12 C13 120.2(6) . . ?
C11 C12 O10 120.7(6) . . ?
C13 C12 O10 119.1(6) . . ?
C17 O9 H14 109.5 . . ?
C12 C13 C8 118.7(6) . . ?
C12 C13 C14 121.0(6) . . ?
C8 C13 C14 120.3(6) . . ?
C3 O3 H3 109.5 . . ?
C33 C14 C16 114.2(5) . . ?
C33 C14 C13 113.7(5) . . ?
C16 C14 C13 109.3(5) . . ?
C33 C14 H15 106.3 . . ?
C16 C14 H15 106.3 . . ?
C13 C14 H15 106.3 . . ?
C19 O7 H7 109.5 . . ?
C20 C15 C16 123.3(6) . . ?
C20 C15 H16 118.4 . . ?
C16 C15 H16 118.4 . . ?
C17 C16 C15 116.5(6) . . ?
C17 C16 C14 121.2(6) . . ?
C15 C16 C14 122.1(6) . . ?
C11 O11 H17 109.5 . . ?
O9 C17 C18 113.2(5) . . ?
O9 C17 C16 124.5(6) . . ?
C18 C17 C16 122.3(6) . . ?
O8 C18 C17 122.0(6) . . ?
O8 C18 C19 118.6(6) . . ?
C17 C18 C19 119.4(6) . . ?
O7 C19 C20 118.5(6) . . ?
O7 C19 C18 120.9(6) . . ?
C20 C19 C18 120.6(6) . . ?
C15 C20 C19 117.6(6) . . ?
C15 C20 C21 124.5(6) . . ?
C19 C20 C21 117.8(6) . . ?
C20 C21 C23 112.3(5) . . ?
C20 C21 C37 114.3(5) . . ?
C23 C21 C37 110.7(5) . . ?
C20 C21 H21 106.3 . . ?
C23 C21 H21 106.3 . . ?
C37 C21 H21 106.3 . . ?
C27 C22 C23 123.6(6) . . ?
C27 C22 H22 118.2 . . ?
C23 C22 H22 118.2 . . ?
C24 C23 C22 116.3(6) . . ?
C24 C23 C21 123.1(6) . . ?
C22 C23 C21 120.4(5) . . ?
C23 C24 C25 122.5(6) . . ?
C23 C24 O6 122.4(5) . . ?
C25 C24 O6 115.1(5) . . ?
O5 C25 C24 124.1(5) . . ?
O5 C25 C26 116.9(5) . . ?
C24 C25 C26 119.0(6) . . ?
O4 C26 C25 120.9(6) . . ?
O4 C26 C27 118.5(6) . . ?
C25 C26 C27 120.6(6) . . ?
C22 C27 C26 117.8(6) . . ?
C22 C27 C28 120.8(5) . . ?
C26 C27 C28 121.5(6) . . ?
C41 C28 C2 113.7(5) . . ?
C41 C28 C27 112.3(5) . . ?
C2 C28 C27 109.5(5) . . ?
C41 C28 H28 107.0 . . ?
C2 C28 H28 107.0 . . ?
C27 C28 H28 107.0 . . ?
C30 C29 C7 113.4(5) . . ?
C30 C29 H29A 108.9 . . ?
C7 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C7 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C31 C30 C29 113.3(6) . . ?
C31 C30 H30A 108.9 . . ?
C29 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C30 115.1(7) . . ?
C32 C31 H31A 108.5 . . ?
C30 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C30 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C14 C33 C34 115.1(5) . . ?
C14 C33 H33A 108.5 . . ?
C34 C33 H33A 108.5 . . ?
C14 C33 H33B 108.5 . . ?
C34 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C35 C34 C33 114.7(6) . . ?
C35 C34 H34A 108.6 . . ?
C33 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C34 C35 C36 109.9(8) . . ?
C34 C35 H35A 109.7 . . ?
C36 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
C36 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C21 112.2(6) . . ?
C38 C37 H37A 109.2 . . ?
C21 C37 H37A 109.2 . . ?
C38 C37 H37B 109.2 . . ?
C21 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C39 C38 C37 113.8(6) . . ?
C39 C38 H38A 108.8 . . ?
C37 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C37 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C38 C39 C40 112.9(8) . . ?
C38 C39 H39A 109.0 . . ?
C40 C39 H39A 109.0 . . ?
C38 C39 H39B 109.0 . . ?
C40 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C28 C41 C42 114.0(5) . . ?
C28 C41 H41A 108.8 . . ?
C42 C41 H41A 108.8 . . ?
C28 C41 H41B 108.8 . . ?
C42 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
C41 C42 C43 113.0(6) . . ?
C41 C42 H42A 109.0 . . ?
C43 C42 H42A 109.0 . . ?
C41 C42 H42B 109.0 . . ?
C43 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C42 C43 C44 113.4(6) . . ?
C42 C43 H43A 108.9 . . ?
C44 C43 H43A 108.9 . . ?
C42 C43 H43B 108.9 . . ?
C44 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3I N1I C1I C2I 1.6(8) . . . . ?
C4I N1I C1I C2I 174.5(6) . . . . ?
C6 C1 C2 C3 -1.6(9) . . . . ?
C6 C1 C2 C28 179.4(6) . . . . ?
N1I C1I C2I N2I -0.9(8) . . . . ?
C3I N2I C2I C1I -0.1(8) . . . . ?
C6I N2I C2I C1I -177.5(6) . . . . ?
C1 C2 C3 O3 -172.0(6) . . . . ?
C28 C2 C3 O3 7.0(9) . . . . ?
C1 C2 C3 C4 5.9(9) . . . . ?
C28 C2 C3 C4 -175.0(6) . . . . ?
C1I N1I C3I N2I -1.7(8) . . . . ?
C4I N1I C3I N2I -174.7(6) . . . . ?
C2I N2I C3I N1I 1.2(8) . . . . ?
C6I N2I C3I N1I 178.7(6) . . . . ?
O3 C3 C4 O2 -6.6(9) . . . . ?
C2 C3 C4 O2 175.2(6) . . . . ?
O3 C3 C4 C5 173.0(6) . . . . ?
C2 C3 C4 C5 -5.1(9) . . . . ?
C3I N1I C4I C5I -139.2(7) . . . . ?
C1I N1I C4I C5I 49.0(10) . . . . ?
O2 C4 C5 O1 1.9(9) . . . . ?
C3 C4 C5 O1 -177.7(6) . . . . ?
O2 C4 C5 C6 179.6(6) . . . . ?
C3 C4 C5 C6 -0.1(10) . . . . ?
O1 C5 C6 C1 -178.1(6) . . . . ?
C4 C5 C6 C1 4.2(9) . . . . ?
O1 C5 C6 C7 2.8(9) . . . . ?
C4 C5 C6 C7 -174.9(6) . . . . ?
C2 C1 C6 C5 -3.3(9) . . . . ?
C2 C1 C6 C7 175.7(6) . . . . ?
C5 C6 C7 C9 80.5(7) . . . . ?
C1 C6 C7 C9 -98.5(7) . . . . ?
C5 C6 C7 C29 -155.0(6) . . . . ?
C1 C6 C7 C29 25.9(9) . . . . ?
C13 C8 C9 C10 -2.1(9) . . . . ?
C13 C8 C9 C7 177.1(5) . . . . ?
C6 C7 C9 C8 78.5(7) . . . . ?
C29 C7 C9 C8 -47.0(8) . . . . ?
C6 C7 C9 C10 -102.3(7) . . . . ?
C29 C7 C9 C10 132.2(6) . . . . ?
C8 C9 C10 O12 178.5(6) . . . . ?
C7 C9 C10 O12 -0.7(10) . . . . ?
C8 C9 C10 C11 1.4(9) . . . . ?
C7 C9 C10 C11 -177.8(6) . . . . ?
O12 C10 C11 C12 -177.3(6) . . . . ?
C9 C10 C11 C12 0.1(10) . . . . ?
O12 C10 C11 O11 3.3(9) . . . . ?
C9 C10 C11 O11 -179.3(6) . . . . ?
C10 C11 C12 C13 -0.9(10) . . . . ?
O11 C11 C12 C13 178.5(6) . . . . ?
C10 C11 C12 O10 178.8(6) . . . . ?
O11 C11 C12 O10 -1.8(9) . . . . ?
C11 C12 C13 C8 0.2(9) . . . . ?
O10 C12 C13 C8 -179.6(5) . . . . ?
C11 C12 C13 C14 -179.2(6) . . . . ?
O10 C12 C13 C14 1.1(9) . . . . ?
C9 C8 C13 C12 1.4(9) . . . . ?
C9 C8 C13 C14 -179.3(6) . . . . ?
C12 C13 C14 C33 -133.4(6) . . . . ?
C8 C13 C14 C33 47.3(8) . . . . ?
C12 C13 C14 C16 97.6(7) . . . . ?
C8 C13 C14 C16 -81.7(7) . . . . ?
C20 C15 C16 C17 3.0(9) . . . . ?
C20 C15 C16 C14 -172.7(6) . . . . ?
C33 C14 C16 C17 154.7(6) . . . . ?
C13 C14 C16 C17 -76.7(8) . . . . ?
C33 C14 C16 C15 -29.9(9) . . . . ?
C13 C14 C16 C15 98.8(7) . . . . ?
C15 C16 C17 O9 176.1(6) . . . . ?
C14 C16 C17 O9 -8.2(10) . . . . ?
C15 C16 C17 C18 -4.6(9) . . . . ?
C14 C16 C17 C18 171.1(6) . . . . ?
O9 C17 C18 O8 3.1(9) . . . . ?
C16 C17 C18 O8 -176.3(6) . . . . ?
O9 C17 C18 C19 -179.2(5) . . . . ?
C16 C17 C18 C19 1.4(10) . . . . ?
O8 C18 C19 O7 0.7(9) . . . . ?
C17 C18 C19 O7 -177.1(6) . . . . ?
O8 C18 C19 C20 -178.5(6) . . . . ?
C17 C18 C19 C20 3.8(9) . . . . ?
C16 C15 C20 C19 1.9(10) . . . . ?
C16 C15 C20 C21 -178.8(6) . . . . ?
O7 C19 C20 C15 175.5(5) . . . . ?
C18 C19 C20 C15 -5.3(9) . . . . ?
O7 C19 C20 C21 -3.8(9) . . . . ?
C18 C19 C20 C21 175.4(6) . . . . ?
C15 C20 C21 C23 -101.5(7) . . . . ?
C19 C20 C21 C23 77.8(7) . . . . ?
C15 C20 C21 C37 25.6(9) . . . . ?
C19 C20 C21 C37 -155.1(6) . . . . ?
C27 C22 C23 C24 -1.9(9) . . . . ?
C27 C22 C23 C21 172.8(6) . . . . ?
C20 C21 C23 C24 -112.8(7) . . . . ?
C37 C21 C23 C24 118.1(6) . . . . ?
C20 C21 C23 C22 72.8(7) . . . . ?
C37 C21 C23 C22 -56.2(7) . . . . ?
C22 C23 C24 C25 4.5(9) . . . . ?
C21 C23 C24 C25 -170.0(6) . . . . ?
C22 C23 C24 O6 -177.5(5) . . . . ?
C21 C23 C24 O6 7.9(9) . . . . ?
C23 C24 C25 O5 175.2(6) . . . . ?
O6 C24 C25 O5 -2.9(9) . . . . ?
C23 C24 C25 C26 -4.1(9) . . . . ?
O6 C24 C25 C26 177.9(5) . . . . ?
O5 C25 C26 O4 2.3(9) . . . . ?
C24 C25 C26 O4 -178.4(6) . . . . ?
O5 C25 C26 C27 -178.5(5) . . . . ?
C24 C25 C26 C27 0.8(9) . . . . ?
C23 C22 C27 C26 -1.1(9) . . . . ?
C23 C22 C27 C28 179.8(5) . . . . ?
O4 C26 C27 C22 -179.1(5) . . . . ?
C25 C26 C27 C22 1.7(9) . . . . ?
O4 C26 C27 C28 0.0(9) . . . . ?
C25 C26 C27 C28 -179.2(6) . . . . ?
C1 C2 C28 C41 -20.8(9) . . . . ?
C3 C2 C28 C41 160.2(6) . . . . ?
C1 C2 C28 C27 105.7(7) . . . . ?
C3 C2 C28 C27 -73.3(7) . . . . ?
C22 C27 C28 C41 57.9(7) . . . . ?
C26 C27 C28 C41 -121.2(6) . . . . ?
C22 C27 C28 C2 -69.4(7) . . . . ?
C26 C27 C28 C2 111.5(6) . . . . ?
C6 C7 C29 C30 174.3(6) . . . . ?
C9 C7 C29 C30 -62.4(8) . . . . ?
C7 C29 C30 C31 -171.5(7) . . . . ?
C29 C30 C31 C32 -173.0(7) . . . . ?
C16 C14 C33 C34 180.0(6) . . . . ?
C13 C14 C33 C34 53.6(8) . . . . ?
C14 C33 C34 C35 62.7(9) . . . . ?
C33 C34 C35 C36 179.5(7) . . . . ?
C20 C21 C37 C38 168.2(6) . . . . ?
C23 C21 C37 C38 -63.9(7) . . . . ?
C21 C37 C38 C39 173.8(6) . . . . ?
C37 C38 C39 C40 -79.3(9) . . . . ?
C2 C28 C41 C42 -171.1(6) . . . . ?
C27 C28 C41 C42 63.9(7) . . . . ?
C28 C41 C42 C43 174.7(6) . . . . ?
C41 C42 C43 C44 179.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.114
_database_code_depnum_ccdc_archive 'CCDC 986747'
