# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100422_wanggp_2_2
_database_code_depnum_ccdc_archive 'CCDC 790566'
_audit_update_record             
;
2010-08-25 deposited with the CCDC.
2015-02-05 downloaded from the CCDC.
;
#TrackingRef 'Chao Shen Department of Chemical and Biological Engineering, Zhejiang University.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H48 N2 O9 S'
_chemical_formula_weight         648.79

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   13.6507(6)
_cell_length_b                   10.3032(3)
_cell_length_c                   13.9805(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.803(5)
_cell_angle_gamma                90.00
_cell_volume                     1850.03(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2511
_cell_measurement_theta_min      3.5556
_cell_measurement_theta_max      29.2463

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   multi-scan'
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.53 (release 17-11-2009 CrysAlis171 .NET)
(compiled Nov 17 2009,16:58:22)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3592
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7299
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5121
_reflns_number_gt                2811
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1222P)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   0.0(2)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         5121
_refine_ls_number_parameters     411
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1906
_refine_ls_wR_factor_gt          0.1717
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_restrained_S_all      0.947
_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
S S 0.21254(19) 0.5539(3) 1.17983(16) 0.1177(7) Uani 1 1 d . . .
O1 O 0.2477(2) 0.5691(3) 0.8535(2) 0.0592(8) Uani 1 1 d . . .
O2 O 0.0817(3) 0.6332(5) 0.6689(3) 0.0929(14) Uani 1 1 d . A .
O3 O 0.3892(3) 0.6863(3) 0.6911(3) 0.0670(10) Uani 1 1 d . . .
O4 O 0.3902(5) 0.5117(5) 0.5974(4) 0.1181(18) Uani 1 1 d . . .
O5 O 0.5509(3) 0.5937(3) 0.8702(3) 0.0624(9) Uani 1 1 d . . .
O6 O 0.6233(4) 0.7893(4) 0.8903(4) 0.0994(14) Uani 1 1 d . . .
O7 O 0.4967(3) 0.6364(3) 1.0497(2) 0.0604(9) Uani 1 1 d . . .
O8 O 0.5855(3) 0.4496(4) 1.0862(3) 0.0810(12) Uani 1 1 d . . .
N1 N 0.1424(4) 0.7162(5) 1.0036(4) 0.0813(13) Uiso 1 1 d . . .
N2 N 0.2887(3) 0.5577(4) 1.0285(3) 0.0643(11) Uani 1 1 d . . .
H2 H 0.3185 0.4870 1.0560 0.077 Uiso 1 1 calc R . .
C1 C 0.0719(7) 0.6953(10) 1.2395(7) 0.123(3) Uani 1 1 d . . .
H1 H 0.0893 0.6459 1.2986 0.148 Uiso 1 1 calc R . .
C2 C -0.0007(8) 0.7928(12) 1.2229(10) 0.132(3) Uani 1 1 d . . .
H2A H -0.0326 0.8098 1.2707 0.158 Uiso 1 1 calc R . .
C3 C -0.0258(6) 0.8651(10) 1.1350(11) 0.126(3) Uani 1 1 d . . .
H3 H -0.0748 0.9314 1.1233 0.151 Uiso 1 1 calc R . .
C4 C 0.0205(6) 0.8396(9) 1.0660(7) 0.112(3) Uani 1 1 d . . .
H4 H 0.0029 0.8880 1.0064 0.135 Uiso 1 1 calc R . .
C5 C 0.0937(5) 0.7427(7) 1.0827(5) 0.0794(17) Uani 1 1 d . . .
C6 C 0.1181(5) 0.6715(6) 1.1693(5) 0.0814(17) Uani 1 1 d . . .
C7 C 0.2127(4) 0.6155(6) 1.0624(4) 0.0782(18) Uani 1 1 d . . .
C8 C 0.3163(4) 0.6157(4) 0.9491(3) 0.0540(12) Uani 1 1 d . . .
H8 H 0.3089 0.7101 0.9519 0.065 Uiso 1 1 calc R . .
C9 C 0.2626(4) 0.6375(5) 0.7703(3) 0.0594(13) Uani 1 1 d . . .
H9 H 0.2533 0.7310 0.7769 0.071 Uiso 1 1 calc R . .
C10 C 0.3713(4) 0.6089(4) 0.7694(3) 0.0541(12) Uani 1 1 d . . .
H10 H 0.3773 0.5166 0.7555 0.065 Uiso 1 1 calc R . .
C11 C 0.4518(4) 0.6446(4) 0.8688(4) 0.0518(11) Uani 1 1 d . . .
H11 H 0.4559 0.7392 0.8764 0.062 Uiso 1 1 calc R . .
C12 C 0.4275(3) 0.5836(4) 0.9573(3) 0.0500(11) Uani 1 1 d . . .
H12 H 0.4365 0.4893 0.9567 0.060 Uiso 1 1 calc R . .
C13 C 0.1799(4) 0.5853(8) 0.6747(4) 0.0862(18) Uani 1 1 d . . .
H13A H 0.1959 0.6120 0.6150 0.103 Uiso 1 1 calc R . .
H13B H 0.1795 0.4912 0.6766 0.103 Uiso 1 1 calc R . .
C14 C 0.0312(7) 0.7090(9) 0.5987(6) 0.117(3) Uani 1 1 d D . .
C15 C -0.0711(7) 0.7549(10) 0.5993(7) 0.120(3) Uani 1 1 d U A .
C16 C -0.1409(8) 0.6308(12) 0.5949(9) 0.165(4) Uani 1 1 d U . .
H16A H -0.1210 0.5629 0.5582 0.248 Uiso 1 1 calc R A .
H16B H -0.2128 0.6524 0.5612 0.248 Uiso 1 1 calc R . .
H16C H -0.1311 0.6018 0.6628 0.248 Uiso 1 1 calc R . .
C17 C -0.1247(10) 0.8340(14) 0.5071(10) 0.194(4) Uani 1 1 d U . .
H17A H -0.1184 0.7919 0.4482 0.292 Uiso 1 1 calc R A .
H17C H -0.0933 0.9185 0.5143 0.292 Uiso 1 1 calc R . .
H17B H -0.1970 0.8427 0.4993 0.292 Uiso 1 1 calc R . .
C18 C -0.0553(9) 0.8211(11) 0.6966(8) 0.151(3) Uani 1 1 d U . .
H18C H -0.1173 0.8678 0.6930 0.227 Uiso 1 1 calc R A .
H18B H 0.0019 0.8807 0.7102 0.227 Uiso 1 1 calc R . .
H18A H -0.0402 0.7580 0.7502 0.227 Uiso 1 1 calc R . .
C19 C 0.3987(5) 0.6241(6) 0.6093(4) 0.0791(16) Uani 1 1 d . . .
C20 C 0.4159(8) 0.7205(8) 0.5324(6) 0.114(2) Uani 1 1 d U . .
C21 C 0.3365(11) 0.8266(11) 0.5097(8) 0.165(3) Uani 1 1 d U . .
H21A H 0.2704 0.7935 0.4670 0.248 Uiso 1 1 calc R . .
H21B H 0.3576 0.8962 0.4754 0.248 Uiso 1 1 calc R . .
H21C H 0.3305 0.8581 0.5721 0.248 Uiso 1 1 calc R . .
C22 C 0.4030(12) 0.6502(13) 0.4347(8) 0.186(4) Uani 1 1 d U . .
H22B H 0.4625 0.5958 0.4434 0.279 Uiso 1 1 calc R . .
H22C H 0.3969 0.7122 0.3818 0.279 Uiso 1 1 calc R . .
H22A H 0.3413 0.5977 0.4167 0.279 Uiso 1 1 calc R . .
C23 C 0.5210(11) 0.7744(13) 0.5763(10) 0.194(4) Uani 1 1 d U . .
H23C H 0.5344 0.7952 0.6465 0.290 Uiso 1 1 calc R . .
H23B H 0.5265 0.8517 0.5400 0.290 Uiso 1 1 calc R . .
H23A H 0.5709 0.7117 0.5711 0.290 Uiso 1 1 calc R . .
C24 C 0.6308(5) 0.6736(6) 0.8802(4) 0.0708(15) Uani 1 1 d . . .
C25 C 0.7268(5) 0.6015(7) 0.8815(5) 0.0867(19) Uani 1 1 d . . .
C26 C 0.6999(7) 0.4882(10) 0.8060(7) 0.141(4) Uani 1 1 d . . .
H26B H 0.6667 0.4206 0.8312 0.211 Uiso 1 1 calc R . .
H26C H 0.7625 0.4552 0.7982 0.211 Uiso 1 1 calc R . .
H26A H 0.6536 0.5178 0.7414 0.211 Uiso 1 1 calc R . .
C27 C 0.7986(7) 0.6967(13) 0.8534(10) 0.172(5) Uani 1 1 d . . .
H27A H 0.7647 0.7282 0.7856 0.257 Uiso 1 1 calc R . .
H27B H 0.8621 0.6534 0.8570 0.257 Uiso 1 1 calc R . .
H27C H 0.8143 0.7684 0.9001 0.257 Uiso 1 1 calc R . .
C28 C 0.7830(7) 0.5520(12) 0.9871(6) 0.142(3) Uani 1 1 d . . .
H28C H 0.7832 0.6179 1.0357 0.214 Uiso 1 1 calc R . .
H28B H 0.8533 0.5303 0.9936 0.214 Uiso 1 1 calc R . .
H28A H 0.7482 0.4761 0.9993 0.214 Uiso 1 1 calc R . .
C29 C 0.5723(4) 0.5588(5) 1.1101(4) 0.0562(12) Uani 1 1 d . . .
C30 C 0.6347(5) 0.6227(6) 1.2078(4) 0.0812(17) Uani 1 1 d . . .
C31 C 0.5667(9) 0.6446(16) 1.2703(7) 0.195(6) Uani 1 1 d . . .
H31B H 0.5263 0.7220 1.2476 0.293 Uiso 1 1 calc R . .
H31C H 0.6091 0.6541 1.3404 0.293 Uiso 1 1 calc R . .
H31A H 0.5208 0.5718 1.2631 0.293 Uiso 1 1 calc R . .
C32 C 0.7257(8) 0.5380(9) 1.2661(6) 0.143(4) Uani 1 1 d . . .
H32B H 0.7010 0.4529 1.2742 0.214 Uiso 1 1 calc R . .
H32C H 0.7604 0.5754 1.3318 0.214 Uiso 1 1 calc R . .
H32A H 0.7735 0.5319 1.2294 0.214 Uiso 1 1 calc R . .
C33 C 0.6799(7) 0.7475(7) 1.1861(6) 0.118(3) Uani 1 1 d . . .
H33A H 0.7132 0.7322 1.1366 0.178 Uiso 1 1 calc R . .
H33C H 0.7302 0.7797 1.2476 0.178 Uiso 1 1 calc R . .
H33B H 0.6253 0.8102 1.1601 0.178 Uiso 1 1 calc R . .
O9 O 0.0442(9) 0.7004(12) 0.5136(8) 0.121(3) Uiso 0.50 1 d PD A 1
O9A O 0.0899(9) 0.7725(11) 0.5591(9) 0.121(3) Uiso 0.50 1 d PD 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
S C6 1.739(7) . ?
S C7 1.760(6) . ?
O1 C8 1.430(6) . ?
O1 C9 1.433(6) . ?
O2 C14 1.261(8) . ?
O2 C13 1.405(7) . ?
O3 C19 1.355(6) . ?
O3 C10 1.442(6) . ?
O4 C19 1.171(6) . ?
O5 C24 1.336(6) . ?
O5 C11 1.444(6) . ?
O6 C24 1.209(7) . ?
O7 C29 1.353(6) . ?
O7 C12 1.425(5) . ?
O8 C29 1.204(6) . ?
N1 C7 1.462(8) . ?
N1 C5 1.497(8) . ?
N2 C7 1.411(7) . ?
N2 C8 1.419(6) . ?
N2 H2 0.8600 . ?
C1 C6 1.357(10) . ?
C1 C2 1.374(13) . ?
C1 H1 0.9300 . ?
C2 C3 1.378(13) . ?
C2 H2A 0.9300 . ?
C3 C4 1.347(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.357(9) . ?
C8 C12 1.519(7) . ?
C8 H8 0.9800 . ?
C9 C10 1.517(7) . ?
C9 C13 1.526(8) . ?
C9 H9 0.9800 . ?
C10 C11 1.496(7) . ?
C10 H10 0.9800 . ?
C11 C12 1.521(6) . ?
C11 H11 0.9800 . ?
C12 H12 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O9 1.264(11) . ?
C14 O9A 1.295(12) . ?
C14 C15 1.476(11) . ?
C15 C18 1.471(13) . ?
C15 C17 1.491(12) . ?
C15 C16 1.584(14) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17C 0.9600 . ?
C17 H17B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18A 0.9600 . ?
C19 C20 1.538(9) . ?
C20 C23 1.465(14) . ?
C20 C21 1.495(13) . ?
C20 C22 1.503(12) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 H22A 0.9600 . ?
C23 H23C 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23A 0.9600 . ?
C24 C25 1.502(8) . ?
C25 C28 1.503(10) . ?
C25 C27 1.530(11) . ?
C25 C26 1.533(10) . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26 H26A 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28C 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28A 0.9600 . ?
C29 C30 1.495(8) . ?
C30 C31 1.491(11) . ?
C30 C33 1.501(9) . ?
C30 C32 1.511(10) . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 H31A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 H32A 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33C 0.9600 . ?
C33 H33B 0.9600 . ?

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
C6 S C7 84.5(3) . . ?
C8 O1 C9 111.4(3) . . ?
C14 O2 C13 121.5(5) . . ?
C19 O3 C10 118.0(4) . . ?
C24 O5 C11 120.3(4) . . ?
C29 O7 C12 118.2(4) . . ?
C7 N1 C5 94.8(5) . . ?
C7 N2 C8 120.4(4) . . ?
C7 N2 H2 119.8 . . ?
C8 N2 H2 119.8 . . ?
C6 C1 C2 119.6(9) . . ?
C6 C1 H1 120.2 . . ?
C2 C1 H1 120.2 . . ?
C1 C2 C3 119.6(8) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
C4 C3 C2 119.8(9) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.7(9) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.3(7) . . ?
C6 C5 N1 121.7(6) . . ?
C4 C5 N1 119.1(7) . . ?
C5 C6 C1 121.0(7) . . ?
C5 C6 S 113.8(5) . . ?
C1 C6 S 125.3(7) . . ?
N2 C7 N1 121.8(5) . . ?
N2 C7 S 113.2(5) . . ?
N1 C7 S 125.0(4) . . ?
N2 C8 O1 109.0(4) . . ?
N2 C8 C12 111.9(4) . . ?
O1 C8 C12 108.6(3) . . ?
N2 C8 H8 109.1 . . ?
O1 C8 H8 109.1 . . ?
C12 C8 H8 109.1 . . ?
O1 C9 C10 108.6(4) . . ?
O1 C9 C13 105.8(4) . . ?
C10 C9 C13 111.1(4) . . ?
O1 C9 H9 110.4 . . ?
C10 C9 H9 110.4 . . ?
C13 C9 H9 110.4 . . ?
O3 C10 C11 108.0(4) . . ?
O3 C10 C9 108.5(4) . . ?
C11 C10 C9 111.0(4) . . ?
O3 C10 H10 109.8 . . ?
C11 C10 H10 109.8 . . ?
C9 C10 H10 109.8 . . ?
O5 C11 C10 108.3(3) . . ?
O5 C11 C12 107.5(4) . . ?
C10 C11 C12 111.1(4) . . ?
O5 C11 H11 110.0 . . ?
C10 C11 H11 110.0 . . ?
C12 C11 H11 110.0 . . ?
O7 C12 C8 108.9(3) . . ?
O7 C12 C11 108.6(4) . . ?
C8 C12 C11 109.7(4) . . ?
O7 C12 H12 109.9 . . ?
C8 C12 H12 109.9 . . ?
C11 C12 H12 109.9 . . ?
O2 C13 C9 109.5(5) . . ?
O2 C13 H13A 109.8 . . ?
C9 C13 H13A 109.8 . . ?
O2 C13 H13B 109.8 . . ?
C9 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
O2 C14 O9 118.3(8) . . ?
O2 C14 O9A 113.0(9) . . ?
O9 C14 O9A 47.8(6) . . ?
O2 C14 C15 117.6(6) . . ?
O9 C14 C15 117.6(9) . . ?
O9A C14 C15 124.3(9) . . ?
C18 C15 C14 108.2(8) . . ?
C18 C15 C17 114.9(10) . . ?
C14 C15 C17 111.0(8) . . ?
C18 C15 C16 107.9(8) . . ?
C14 C15 C16 107.4(8) . . ?
C17 C15 C16 107.2(9) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17C C17 H17B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18C C18 H18B 109.5 . . ?
C15 C18 H18A 109.5 . . ?
H18C C18 H18A 109.5 . . ?
H18B C18 H18A 109.5 . . ?
O4 C19 O3 123.7(5) . . ?
O4 C19 C20 124.9(6) . . ?
O3 C19 C20 111.4(5) . . ?
C23 C20 C21 110.4(10) . . ?
C23 C20 C22 111.1(9) . . ?
C21 C20 C22 107.8(9) . . ?
C23 C20 C19 108.1(7) . . ?
C21 C20 C19 110.5(7) . . ?
C22 C20 C19 108.9(8) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
C20 C23 H23C 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
C20 C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?
O6 C24 O5 121.5(5) . . ?
O6 C24 C25 126.5(5) . . ?
O5 C24 C25 112.0(5) . . ?
C24 C25 C28 109.4(5) . . ?
C24 C25 C27 108.2(6) . . ?
C28 C25 C27 108.2(7) . . ?
C24 C25 C26 111.3(5) . . ?
C28 C25 C26 110.0(7) . . ?
C27 C25 C26 109.7(7) . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
H26C C26 H26A 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28C 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C25 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
O8 C29 O7 122.2(5) . . ?
O8 C29 C30 125.0(5) . . ?
O7 C29 C30 112.8(4) . . ?
C31 C30 C29 109.1(6) . . ?
C31 C30 C33 111.7(8) . . ?
C29 C30 C33 109.8(5) . . ?
C31 C30 C32 109.4(8) . . ?
C29 C30 C32 110.4(6) . . ?
C33 C30 C32 106.5(7) . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
H31B C31 H31A 109.5 . . ?
H31C C31 H31A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
H32B C32 H32A 109.5 . . ?
H32C C32 H32A 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33C C33 H33B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.045


