# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Maija Nissinen'
_publ_contact_author_address     
;Department of Chemistry, Nanoscience Center
University of Jyväskylä
P.O. Box 35
40014 JYU
Finland
;
_publ_contact_author_email       maija.nissinen@jyu.fi
_publ_contact_author_phone       '+358 14 260 4242'
_publ_contact_author_fax         '+358 14 260 4756'

_publ_section_title              
;
Twisting of the resorcinarene core due to solvent effects
upon crystallization
;
loop_
_publ_author_name
'Maija Nissinen'
'Kirsi Salorinne'

data_I
_database_code_depnum_ccdc_archive 'CCDC 718573'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H60 O10'
_chemical_formula_weight         772.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4/ncc

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

_cell_length_a                   16.4267(4)
_cell_length_b                   16.4267(4)
_cell_length_c                   16.1350(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4353.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_T_max  0.8788
_exptl_absorpt_process_details   
'Denzo (otwinowski, Borek, Majewski & Minor, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6315
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.81
_diffrn_reflns_theta_max         66.90
_reflns_number_total             1913
_reflns_number_gt                1634
_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)+(0.1369P)²+1.9533P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0030(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1913
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0758
_refine_ls_wR_factor_ref         0.2285
_refine_ls_wR_factor_gt          0.2184
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_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
C1 C 0.42138(13) 0.14997(13) 0.53793(12) 0.0334(6) Uani 1 1 d . . .
C2 C 0.37458(13) 0.34608(13) 0.56802(12) 0.0326(6) Uani 1 1 d . . .
H2 H 0.3447 0.3229 0.6126 0.039 Uiso 1 1 calc R . .
C3 C 0.44067(13) 0.30245(14) 0.53662(13) 0.0341(6) Uani 1 1 d . . .
C4 C 0.48235(14) 0.33681(15) 0.46968(14) 0.0408(6) Uani 1 1 d . . .
C5 C 0.41207(16) 0.04022(15) 0.43782(15) 0.0437(7) Uani 1 1 d . . .
H5 H 0.4351 0.0105 0.3931 0.052 Uiso 1 1 calc R . .
C6 C 0.45354(14) 0.10582(15) 0.47114(14) 0.0384(6) Uani 1 1 d . . .
C7 C 0.46757(13) 0.22224(13) 0.57452(13) 0.0338(6) Uani 1 1 d . . .
H7 H 0.5259 0.2148 0.5587 0.041 Uiso 1 1 calc R . .
C29 C 0.46523(14) 0.22417(14) 0.67020(13) 0.0389(6) Uani 1 1 d . . .
H29A H 0.4933 0.2739 0.6900 0.047 Uiso 1 1 calc R . .
H29B H 0.4079 0.2270 0.6888 0.047 Uiso 1 1 calc R . .
C30 C 0.50509(19) 0.15054(17) 0.70853(16) 0.0567(8) Uani 1 1 d . . .
H30A H 0.4717 0.1022 0.6977 0.085 Uiso 1 1 calc R . .
H30B H 0.5102 0.1586 0.7685 0.085 Uiso 1 1 calc R . .
H30C H 0.5593 0.1429 0.6843 0.085 Uiso 1 1 calc R . .
C37 C 0.56042(18) 0.09091(18) 0.36987(17) 0.0582(8) Uani 1 1 d . . .
H37A H 0.5682 0.0331 0.3828 0.087 Uiso 1 1 calc R . .
H37B H 0.6129 0.1153 0.3552 0.087 Uiso 1 1 calc R . .
H37C H 0.5227 0.0963 0.3232 0.087 Uiso 1 1 calc R . .
O4 O 0.54807(12) 0.30051(13) 0.43231(12) 0.0574(7) Uani 1 1 d . . .
H4 H 0.546(2) 0.249(2) 0.445(2) 0.069 Uiso 1 1 d . . .
O6 O 0.52757(10) 0.13175(11) 0.44075(11) 0.0475(6) Uani 1 1 d . . .
C42 C 0.3151(6) 0.2111(7) 0.3540(4) 0.103(3) Uani 0.50 1 d P . .
H42A H 0.3551 0.1865 0.3165 0.155 Uiso 0.50 1 calc PR . .
H42B H 0.2916 0.1687 0.3894 0.155 Uiso 0.50 1 calc PR . .
H42C H 0.3420 0.2521 0.3886 0.155 Uiso 0.50 1 calc PR . .
C41 C 0.2500 0.2500 0.3050(3) 0.0411(11) Uani 1 4 d S . .
O40 O 0.2500 0.2500 0.23074(19) 0.0475(9) Uani 1 4 d S . .
O50 O 0.7500 0.2500 0.3793(15) 0.277(10) Uiso 0.50 2 d SP . .
C51 C 0.7500 0.2500 0.4618(10) 0.123(5) Uiso 0.50 2 d SP . .
C52 C 0.6859(12) 0.2158(12) 0.5174(12) 0.202(7) Uiso 0.50 1 d P . .
H52A H 0.6423 0.1920 0.4838 0.303 Uiso 0.50 1 calc PR . .
H52B H 0.6635 0.2594 0.5521 0.303 Uiso 0.50 1 calc PR . .
H52C H 0.7098 0.1737 0.5528 0.303 Uiso 0.50 1 calc PR . .


_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
C1 C2 1.389(3) 4 ?
C1 C6 1.402(3) . ?
C1 C7 1.528(3) . ?
C2 C1 1.389(3) 3 ?
C2 C3 1.396(3) . ?
C3 C4 1.398(3) . ?
C3 C7 1.518(3) . ?
C4 O4 1.373(3) . ?
C4 C5 1.389(3) 3 ?
C5 C6 1.384(3) . ?
C5 C4 1.389(3) 4 ?
C6 O6 1.379(3) . ?
C7 C29 1.545(3) . ?
C29 C30 1.508(3) . ?
C37 O6 1.431(3) . ?
C42 C41 1.476(7) . ?
C41 O40 1.199(5) . ?
C41 C42 1.476(7) 3 ?
C41 C42 1.476(7) 4 ?
C41 C42 1.476(7) 2 ?
O50 C51 1.33(2) . ?
C51 C51 1.23(3) 11_666 ?
C51 C52 1.239(18) 11_666 ?
C51 C52 1.239(18) 12_656 ?
C51 C52 1.493(16) . ?
C51 C52 1.493(16) 2_655 ?

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
C2 C1 C6 117.0(2) 4 . ?
C2 C1 C7 122.21(18) 4 . ?
C6 C1 C7 120.8(2) . . ?
C1 C2 C3 123.80(19) 3 . ?
C2 C3 C4 117.0(2) . . ?
C2 C3 C7 121.71(19) . . ?
C4 C3 C7 121.3(2) . . ?
O4 C4 C5 115.7(2) . 3 ?
O4 C4 C3 123.3(2) . . ?
C5 C4 C3 121.0(2) 3 . ?
C6 C5 C4 120.2(2) . 4 ?
O6 C6 C5 122.5(2) . . ?
O6 C6 C1 116.5(2) . . ?
C5 C6 C1 121.1(2) . . ?
C3 C7 C1 111.97(17) . . ?
C3 C7 C29 112.18(17) . . ?
C1 C7 C29 112.95(18) . . ?
C30 C29 C7 112.50(19) . . ?
C6 O6 C37 118.15(19) . . ?
O40 C41 C42 122.4(4) . 3 ?
O40 C41 C42 122.4(4) . . ?
C42 C41 C42 73.3(3) 3 . ?
O40 C41 C42 122.4(4) . 4 ?
C42 C41 C42 115.3(7) 3 4 ?
C42 C41 C42 73.3(3) . 4 ?
O40 C41 C42 122.4(4) . 2 ?
C42 C41 C42 73.3(3) 3 2 ?
C42 C41 C42 115.3(7) . 2 ?
C42 C41 C42 73.3(3) 4 2 ?
C51 C51 C52 74.3(12) 11_666 11_666 ?
C51 C51 C52 74.3(12) 11_666 12_656 ?
C52 C51 C52 149(2) 11_666 12_656 ?
C51 C51 O50 180.000(6) 11_666 . ?
C52 C51 O50 105.7(12) 11_666 . ?
C52 C51 O50 105.7(12) 12_656 . ?
C51 C51 C52 53.1(9) 11_666 . ?
C52 C51 C52 80.7(8) 11_666 . ?
C52 C51 C52 80.7(8) 12_656 . ?
O50 C51 C52 126.9(9) . . ?
C51 C51 C52 53.1(9) 11_666 2_655 ?
C52 C51 C52 80.7(8) 11_666 2_655 ?
C52 C51 C52 80.7(8) 12_656 2_655 ?
O50 C51 C52 126.9(9) . 2_655 ?
C52 C51 C52 106.1(18) . 2_655 ?

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
C1 C2 C3 C4 -1.7(3) 3 . . . ?
C1 C2 C3 C7 176.93(19) 3 . . . ?
C2 C3 C4 O4 -179.6(2) . . . . ?
C7 C3 C4 O4 1.8(4) . . . . ?
C2 C3 C4 C5 1.7(3) . . . 3 ?
C7 C3 C4 C5 -176.9(2) . . . 3 ?
C4 C5 C6 O6 -178.7(2) 4 . . . ?
C4 C5 C6 C1 0.8(4) 4 . . . ?
C2 C1 C6 O6 178.77(19) 4 . . . ?
C7 C1 C6 O6 -0.6(3) . . . . ?
C2 C1 C6 C5 -0.8(3) 4 . . . ?
C7 C1 C6 C5 179.9(2) . . . . ?
C2 C3 C7 C1 86.8(2) . . . . ?
C4 C3 C7 C1 -94.6(2) . . . . ?
C2 C3 C7 C29 -41.4(3) . . . . ?
C4 C3 C7 C29 137.1(2) . . . . ?
C2 C1 C7 C3 -85.2(2) 4 . . . ?
C6 C1 C7 C3 94.1(2) . . . . ?
C2 C1 C7 C29 42.6(3) 4 . . . ?
C6 C1 C7 C29 -138.1(2) . . . . ?
C3 C7 C29 C30 -170.2(2) . . . . ?
C1 C7 C29 C30 62.1(3) . . . . ?
C5 C6 O6 C37 2.7(4) . . . . ?
C1 C6 O6 C37 -176.8(2) . . . . ?

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
O4 H4 O6 0.87(4) 1.96(4) 2.796(3) 163(3) .

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        66.90
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.092

#===END

data_II
_database_code_depnum_ccdc_archive 'CCDC 718574'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H66 O11'
_chemical_formula_weight         831.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   8.0141(6)
_cell_length_b                   17.3580(10)
_cell_length_c                   17.6340(11)
_cell_angle_alpha                82.173(3)
_cell_angle_beta                 78.215(4)
_cell_angle_gamma                77.500(3)
_cell_volume                     2333.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9065
_exptl_absorpt_correction_T_max  0.9362
_exptl_absorpt_process_details   
'DENZO (Otwinowski, Borek, Majewski & Minor, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10854
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         66.89
_reflns_number_total             8036
_reflns_number_gt                6182
_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)+(0.1573P)²+4.7019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0057(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8036
_refine_ls_number_parameters     562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.1005
_refine_ls_wR_factor_ref         0.3207
_refine_ls_wR_factor_gt          0.3032
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
C1 C -0.0791(5) 0.3466(2) 0.0935(2) 0.0381(9) Uani 1 1 d . . .
C2 C -0.1173(5) 0.2705(2) 0.1078(2) 0.0368(9) Uani 1 1 d . . .
H2 H -0.2243 0.2638 0.1405 0.044 Uiso 1 1 calc R . .
C3 C -0.0078(5) 0.2039(2) 0.0772(2) 0.0373(9) Uani 1 1 d . . .
C4 C 0.1506(5) 0.2148(3) 0.0320(2) 0.0408(10) Uani 1 1 d . . .
C5 C 0.1982(5) 0.2885(3) 0.0186(3) 0.0431(10) Uani 1 1 d . . .
H5 H 0.3080 0.2946 -0.0115 0.052 Uiso 1 1 calc R . .
C6 C 0.0831(5) 0.3533(3) 0.0499(3) 0.0409(10) Uani 1 1 d . . .
C7 C -0.0584(5) 0.1226(2) 0.0924(2) 0.0370(9) Uani 1 1 d . . .
H7 H 0.0057 0.0923 0.0474 0.044 Uiso 1 1 calc R . .
C8 C 0.0029(5) 0.0763(2) 0.1654(2) 0.0368(9) Uani 1 1 d . . .
C9 C -0.0919(5) 0.0905(2) 0.2392(2) 0.0365(9) Uani 1 1 d . . .
H9 H -0.1926 0.1314 0.2433 0.044 Uiso 1 1 calc R . .
C10 C -0.0472(5) 0.0480(2) 0.3073(2) 0.0367(9) Uani 1 1 d . . .
C11 C 0.1024(5) -0.0116(2) 0.2999(2) 0.0386(9) Uani 1 1 d . . .
C12 C 0.2032(5) -0.0265(2) 0.2278(3) 0.0414(10) Uani 1 1 d . . .
H12 H 0.3050 -0.0668 0.2239 0.050 Uiso 1 1 calc R . .
C13 C 0.1544(5) 0.0182(2) 0.1608(2) 0.0384(9) Uani 1 1 d . . .
C14 C -0.1553(5) 0.0671(2) 0.3868(2) 0.0380(9) Uani 1 1 d . . .
H14 H -0.1174 0.0215 0.4248 0.046 Uiso 1 1 calc R . .
C15 C -0.1160(5) 0.1405(2) 0.4134(2) 0.0382(9) Uani 1 1 d . . .
C16 C -0.2229(5) 0.2157(2) 0.4038(2) 0.0397(9) Uani 1 1 d . . .
H16 H -0.3162 0.2209 0.3766 0.048 Uiso 1 1 calc R . .
C17 C -0.1991(5) 0.2828(2) 0.4320(2) 0.0404(10) Uani 1 1 d . . .
C18 C -0.0627(6) 0.2738(3) 0.4721(3) 0.0446(10) Uani 1 1 d . . .
C19 C 0.0502(6) 0.2011(3) 0.4804(3) 0.0458(10) Uani 1 1 d . . .
H19 H 0.1440 0.1959 0.5073 0.055 Uiso 1 1 calc R . .
C20 C 0.0249(6) 0.1361(3) 0.4490(3) 0.0425(10) Uani 1 1 d . . .
C21 C -0.3151(6) 0.3641(3) 0.4176(2) 0.0420(10) Uani 1 1 d . . .
H21 H -0.3183 0.3947 0.4621 0.050 Uiso 1 1 calc R . .
C22 C -0.2337(5) 0.4098(2) 0.3442(3) 0.0402(10) Uani 1 1 d . . .
C23 C -0.2506(5) 0.3950(2) 0.2707(3) 0.0394(9) Uani 1 1 d . . .
H23 H -0.3106 0.3543 0.2675 0.047 Uiso 1 1 calc R . .
C24 C -0.1853(5) 0.4361(2) 0.2018(2) 0.0387(9) Uani 1 1 d . . .
C25 C -0.0938(5) 0.4951(3) 0.2083(3) 0.0420(10) Uani 1 1 d . . .
C26 C -0.0696(6) 0.5103(3) 0.2793(3) 0.0453(10) Uani 1 1 d . . .
H26 H -0.0069 0.5500 0.2824 0.054 Uiso 1 1 calc R . .
C27 C -0.1383(6) 0.4669(3) 0.3471(3) 0.0430(10) Uani 1 1 d . . .
C28 C -0.2102(5) 0.4189(2) 0.1227(2) 0.0391(9) Uani 1 1 d . . .
H28 H -0.1841 0.4653 0.0853 0.047 Uiso 1 1 calc R . .
C29 C -0.2518(6) 0.1271(3) 0.0946(3) 0.0430(10) Uani 1 1 d . . .
H29A H -0.3196 0.1555 0.1395 0.052 Uiso 1 1 calc R . .
H29B H -0.2849 0.1581 0.0467 0.052 Uiso 1 1 calc R . .
C30 C -0.2991(7) 0.0457(3) 0.1012(3) 0.0538(12) Uani 1 1 d . . .
H30A H -0.2263 0.0157 0.0590 0.081 Uiso 1 1 calc R . .
H30B H -0.4217 0.0520 0.0973 0.081 Uiso 1 1 calc R . .
H30C H -0.2797 0.0170 0.1514 0.081 Uiso 1 1 calc R . .
C31 C -0.3498(6) 0.0724(3) 0.3912(3) 0.0451(10) Uani 1 1 d . . .
H31A H -0.4124 0.0888 0.4427 0.054 Uiso 1 1 calc R . .
H31B H -0.3905 0.1138 0.3510 0.054 Uiso 1 1 calc R . .
C32 C -0.3953(7) -0.0048(3) 0.3795(4) 0.0615(14) Uani 1 1 d . . .
H32A H -0.3444 -0.0185 0.3265 0.092 Uiso 1 1 calc R . .
H32B H -0.5219 0.0011 0.3875 0.092 Uiso 1 1 calc R . .
H32C H -0.3490 -0.0470 0.4170 0.092 Uiso 1 1 calc R . .
C33 C -0.5033(6) 0.3594(3) 0.4167(3) 0.0478(11) Uani 1 1 d . . .
H33A H -0.5064 0.3329 0.3709 0.057 Uiso 1 1 calc R . .
H33B H -0.5476 0.3267 0.4640 0.057 Uiso 1 1 calc R . .
C34 C -0.6221(7) 0.4412(3) 0.4138(4) 0.0642(14) Uani 1 1 d . . .
H34A H -0.6156 0.4686 0.4578 0.096 Uiso 1 1 calc R . .
H34B H -0.7420 0.4351 0.4168 0.096 Uiso 1 1 calc R . .
H34C H -0.5848 0.4722 0.3649 0.096 Uiso 1 1 calc R . .
C35 C -0.3977(6) 0.4136(3) 0.1215(3) 0.0471(11) Uani 1 1 d . . .
H35A H -0.4762 0.4630 0.1383 0.057 Uiso 1 1 calc R . .
H35B H -0.4303 0.3691 0.1590 0.057 Uiso 1 1 calc R . .
C36 C -0.4226(8) 0.4009(4) 0.0405(4) 0.0717(16) Uani 1 1 d . . .
H36A H -0.3827 0.4428 0.0025 0.108 Uiso 1 1 calc R . .
H36B H -0.5460 0.4028 0.0411 0.108 Uiso 1 1 calc R . .
H36C H -0.3551 0.3492 0.0260 0.108 Uiso 1 1 calc R . .
C37 C 0.4115(6) 0.1575(3) -0.0538(3) 0.0576(13) Uani 1 1 d . . .
H37A H 0.3800 0.1960 -0.0971 0.086 Uiso 1 1 calc R . .
H37B H 0.4695 0.1065 -0.0735 0.086 Uiso 1 1 calc R . .
H37C H 0.4903 0.1769 -0.0284 0.086 Uiso 1 1 calc R . .
C38 C 0.2743(6) -0.1238(3) 0.3640(3) 0.0492(11) Uani 1 1 d . . .
H38A H 0.2486 -0.1579 0.3297 0.074 Uiso 1 1 calc R . .
H38B H 0.2750 -0.1519 0.4161 0.074 Uiso 1 1 calc R . .
H38C H 0.3883 -0.1101 0.3431 0.074 Uiso 1 1 calc R . .
C39 C 0.0614(8) 0.3295(3) 0.5603(3) 0.0600(13) Uani 1 1 d . . .
H39A H 0.0250 0.2897 0.6019 0.090 Uiso 1 1 calc R . .
H39B H 0.0497 0.3798 0.5820 0.090 Uiso 1 1 calc R . .
H39C H 0.1829 0.3112 0.5365 0.090 Uiso 1 1 calc R . .
C40 C 0.0439(8) 0.6020(3) 0.1429(3) 0.0651(15) Uani 1 1 d . . .
H40A H -0.0390 0.6385 0.1769 0.098 Uiso 1 1 calc R . .
H40B H 0.0694 0.6292 0.0906 0.098 Uiso 1 1 calc R . .
H40C H 0.1516 0.5844 0.1639 0.098 Uiso 1 1 calc R . .
O4 O 0.2579(4) 0.14758(18) 0.00138(18) 0.0479(8) Uani 1 1 d . . .
O6 O 0.1394(4) 0.42457(19) 0.0324(2) 0.0501(8) Uani 1 1 d . . .
H6 H 0.059(7) 0.463(3) 0.061(3) 0.060 Uiso 1 1 d . . .
O11 O 0.1440(4) -0.05289(18) 0.36861(18) 0.0474(8) Uani 1 1 d . . .
O13 O 0.2624(4) 0.0002(2) 0.09180(19) 0.0493(8) Uani 1 1 d . . .
H13 H 0.261(7) 0.041(4) 0.063(3) 0.059 Uiso 1 1 d . . .
O18 O -0.0454(5) 0.34054(19) 0.5027(2) 0.0558(9) Uani 1 1 d . . .
O20 O 0.1460(4) 0.0676(2) 0.4582(2) 0.0499(8) Uani 1 1 d . . .
H20 H 0.139(7) 0.025(3) 0.429(3) 0.060 Uiso 1 1 d . . .
O25 O -0.0290(4) 0.53509(19) 0.13899(18) 0.0507(8) Uani 1 1 d . . .
O27 O -0.1075(5) 0.4861(2) 0.4155(2) 0.0543(9) Uani 1 1 d . . .
H27 H -0.096(7) 0.436(4) 0.447(3) 0.065 Uiso 1 1 d . . .
C50 C 0.3549(6) 0.2417(3) 0.2541(3) 0.0479(11) Uani 1 1 d . . .
C51 C 0.2185(8) 0.3150(5) 0.2617(5) 0.099(2) Uani 1 1 d . . .
H51A H 0.2711 0.3594 0.2676 0.149 Uiso 1 1 calc R . .
H51B H 0.1293 0.3070 0.3076 0.149 Uiso 1 1 calc R . .
H51C H 0.1653 0.3270 0.2151 0.149 Uiso 1 1 calc R . .
C52 C 0.3022(10) 0.1674(5) 0.2435(4) 0.093(2) Uani 1 1 d . . .
H52A H 0.4041 0.1242 0.2392 0.139 Uiso 1 1 calc R . .
H52B H 0.2528 0.1749 0.1960 0.139 Uiso 1 1 calc R . .
H52C H 0.2151 0.1541 0.2883 0.139 Uiso 1 1 calc R . .
O50 O 0.5036(4) 0.2428(2) 0.2559(2) 0.0538(9) Uani 1 1 d . . .
C70 C 0.0410(7) 0.7982(3) 0.2096(3) 0.0592(13) Uani 1 1 d . . .
C71 C 0.0921(12) 0.8110(5) 0.1249(4) 0.096(2) Uani 1 1 d . . .
H71A H 0.1986 0.7730 0.1077 0.144 Uiso 1 1 calc R . .
H71B H 0.1129 0.8651 0.1105 0.144 Uiso 1 1 calc R . .
H71C H -0.0011 0.8035 0.1000 0.144 Uiso 1 1 calc R . .
C72 C -0.1166(8) 0.8500(4) 0.2484(5) 0.085(2) Uani 1 1 d . . .
H72A H -0.1335 0.8352 0.3047 0.127 Uiso 1 1 calc R . .
H72B H -0.2180 0.8438 0.2285 0.127 Uiso 1 1 calc R . .
H72C H -0.1026 0.9054 0.2377 0.127 Uiso 1 1 calc R . .
O70 O 0.1246(7) 0.7468(3) 0.2484(3) 0.0925(15) Uani 1 1 d . . .
C60 C 0.5427(9) 0.6783(4) 0.2689(5) 0.0825(19) Uani 1 1 d . . .
C61 C 0.5031(10) 0.6248(5) 0.2207(5) 0.097(2) Uani 1 1 d . . .
H61A H 0.5454 0.6402 0.1657 0.146 Uiso 1 1 calc R . .
H61B H 0.3771 0.6280 0.2293 0.146 Uiso 1 1 calc R . .
H61C H 0.5602 0.5703 0.2347 0.146 Uiso 1 1 calc R . .
C62 C 0.4925(11) 0.6644(5) 0.3539(5) 0.098(2) Uani 1 1 d . . .
H62A H 0.5277 0.7039 0.3788 0.147 Uiso 1 1 calc R . .
H62B H 0.5501 0.6112 0.3717 0.147 Uiso 1 1 calc R . .
H62C H 0.3662 0.6688 0.3678 0.147 Uiso 1 1 calc R . .
O60 O 0.6101(11) 0.7331(4) 0.2395(4) 0.145(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.388(6) . ?
C1 C2 1.398(6) . ?
C1 C28 1.526(6) . ?
C2 C3 1.391(6) . ?
C3 C4 1.390(6) . ?
C3 C7 1.525(6) . ?
C4 C5 1.390(6) . ?
C4 O4 1.392(5) . ?
C5 C6 1.389(6) . ?
C6 O6 1.383(5) . ?
C7 C29 1.528(6) . ?
C7 C8 1.534(6) . ?
C8 C9 1.390(6) . ?
C8 C13 1.396(6) . ?
C9 C10 1.392(6) . ?
C10 C11 1.400(6) . ?
C10 C14 1.527(6) . ?
C11 C12 1.383(6) . ?
C11 O11 1.385(5) . ?
C12 C13 1.400(6) . ?
C13 O13 1.372(5) . ?
C14 C31 1.528(6) . ?
C14 C15 1.530(6) . ?
C15 C20 1.384(6) . ?
C15 C16 1.407(6) . ?
C16 C17 1.391(6) . ?
C17 C18 1.390(6) . ?
C17 C21 1.533(6) . ?
C18 O18 1.386(5) . ?
C18 C19 1.394(6) . ?
C19 C20 1.391(6) . ?
C20 O20 1.376(5) . ?
C21 C22 1.526(6) . ?
C21 C33 1.531(6) . ?
C22 C27 1.388(6) . ?
C22 C23 1.394(6) . ?
C23 C24 1.387(6) . ?
C24 C25 1.410(6) . ?
C24 C28 1.526(6) . ?
C25 C26 1.373(7) . ?
C25 O25 1.383(5) . ?
C26 C27 1.402(6) . ?
C27 O27 1.377(6) . ?
C28 C35 1.530(6) . ?
C29 C30 1.525(6) . ?
C31 C32 1.512(6) . ?
C33 C34 1.529(7) . ?
C35 C36 1.533(8) . ?
C37 O4 1.432(5) . ?
C38 O11 1.431(5) . ?
C39 O18 1.426(6) . ?
C40 O25 1.424(6) . ?
C50 O50 1.203(5) . ?
C50 C52 1.487(8) . ?
C50 C51 1.489(8) . ?
C70 O70 1.213(7) . ?
C70 C71 1.465(9) . ?
C70 C72 1.482(9) . ?
C60 O60 1.201(8) . ?
C60 C61 1.463(11) . ?
C60 C62 1.471(10) . ?

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 C1 C2 116.6(4) . . ?
C6 C1 C28 121.6(4) . . ?
C2 C1 C28 121.8(4) . . ?
C3 C2 C1 123.9(4) . . ?
C2 C3 C4 116.9(4) . . ?
C2 C3 C7 121.8(4) . . ?
C4 C3 C7 121.3(4) . . ?
C5 C4 C3 121.6(4) . . ?
C5 C4 O4 122.4(4) . . ?
C3 C4 O4 116.0(4) . . ?
C6 C5 C4 119.2(4) . . ?
O6 C6 C1 122.8(4) . . ?
O6 C6 C5 115.3(4) . . ?
C1 C6 C5 121.8(4) . . ?
C3 C7 C29 112.8(3) . . ?
C3 C7 C8 111.2(3) . . ?
C29 C7 C8 112.3(3) . . ?
C9 C8 C13 117.4(4) . . ?
C9 C8 C7 120.9(4) . . ?
C13 C8 C7 121.7(4) . . ?
C8 C9 C10 123.5(4) . . ?
C9 C10 C11 117.2(4) . . ?
C9 C10 C14 121.1(4) . . ?
C11 C10 C14 121.7(4) . . ?
C12 C11 O11 122.7(4) . . ?
C12 C11 C10 121.3(4) . . ?
O11 C11 C10 116.0(4) . . ?
C11 C12 C13 119.6(4) . . ?
O13 C13 C8 123.2(4) . . ?
O13 C13 C12 115.9(4) . . ?
C8 C13 C12 120.9(4) . . ?
C10 C14 C31 113.3(3) . . ?
C10 C14 C15 111.6(3) . . ?
C31 C14 C15 112.3(3) . . ?
C20 C15 C16 116.7(4) . . ?
C20 C15 C14 121.7(4) . . ?
C16 C15 C14 121.6(4) . . ?
C17 C16 C15 123.4(4) . . ?
C18 C17 C16 117.3(4) . . ?
C18 C17 C21 121.2(4) . . ?
C16 C17 C21 121.5(4) . . ?
O18 C18 C17 116.5(4) . . ?
O18 C18 C19 122.4(4) . . ?
C17 C18 C19 121.0(4) . . ?
C20 C19 C18 119.6(4) . . ?
O20 C20 C15 123.2(4) . . ?
O20 C20 C19 115.2(4) . . ?
C15 C20 C19 121.6(4) . . ?
C22 C21 C33 112.4(4) . . ?
C22 C21 C17 110.4(3) . . ?
C33 C21 C17 113.3(4) . . ?
C27 C22 C23 116.9(4) . . ?
C27 C22 C21 122.1(4) . . ?
C23 C22 C21 120.9(4) . . ?
C24 C23 C22 124.0(4) . . ?
C23 C24 C25 116.7(4) . . ?
C23 C24 C28 122.1(4) . . ?
C25 C24 C28 121.2(4) . . ?
C26 C25 O25 122.8(4) . . ?
C26 C25 C24 121.5(4) . . ?
O25 C25 C24 115.8(4) . . ?
C25 C26 C27 119.5(4) . . ?
O27 C27 C22 123.1(4) . . ?
O27 C27 C26 115.5(4) . . ?
C22 C27 C26 121.3(4) . . ?
C24 C28 C1 111.5(3) . . ?
C24 C28 C35 112.8(3) . . ?
C1 C28 C35 112.7(3) . . ?
C30 C29 C7 112.8(4) . . ?
C32 C31 C14 113.4(4) . . ?
C34 C33 C21 112.4(4) . . ?
C28 C35 C36 112.1(4) . . ?
C4 O4 C37 118.1(4) . . ?
C11 O11 C38 118.3(3) . . ?
C18 O18 C39 117.8(4) . . ?
C25 O25 C40 117.8(4) . . ?
O50 C50 C52 121.1(5) . . ?
O50 C50 C51 120.9(5) . . ?
C52 C50 C51 118.1(6) . . ?
O70 C70 C71 121.8(6) . . ?
O70 C70 C72 119.6(6) . . ?
C71 C70 C72 118.6(6) . . ?
O60 C60 C61 120.5(8) . . ?
O60 C60 C62 121.3(8) . . ?
C61 C60 C62 118.1(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 -4.2(6) . . . . ?
C28 C1 C2 C3 174.6(4) . . . . ?
C1 C2 C3 C4 2.3(6) . . . . ?
C1 C2 C3 C7 -177.8(4) . . . . ?
C2 C3 C4 C5 0.6(6) . . . . ?
C7 C3 C4 C5 -179.3(4) . . . . ?
C2 C3 C4 O4 -179.5(4) . . . . ?
C7 C3 C4 O4 0.5(6) . . . . ?
C3 C4 C5 C6 -1.3(7) . . . . ?
O4 C4 C5 C6 178.8(4) . . . . ?
C2 C1 C6 O6 -178.9(4) . . . . ?
C28 C1 C6 O6 2.3(7) . . . . ?
C2 C1 C6 C5 3.3(6) . . . . ?
C28 C1 C6 C5 -175.5(4) . . . . ?
C4 C5 C6 O6 -178.7(4) . . . . ?
C4 C5 C6 C1 -0.7(7) . . . . ?
C2 C3 C7 C29 36.6(5) . . . . ?
C4 C3 C7 C29 -143.5(4) . . . . ?
C2 C3 C7 C8 -90.5(5) . . . . ?
C4 C3 C7 C8 89.4(5) . . . . ?
C3 C7 C8 C9 81.0(5) . . . . ?
C29 C7 C8 C9 -46.4(5) . . . . ?
C3 C7 C8 C13 -99.3(4) . . . . ?
C29 C7 C8 C13 133.3(4) . . . . ?
C13 C8 C9 C10 -2.6(6) . . . . ?
C7 C8 C9 C10 177.1(4) . . . . ?
C8 C9 C10 C11 0.4(6) . . . . ?
C8 C9 C10 C14 179.3(4) . . . . ?
C9 C10 C11 C12 1.3(6) . . . . ?
C14 C10 C11 C12 -177.5(4) . . . . ?
C9 C10 C11 O11 179.9(3) . . . . ?
C14 C10 C11 O11 1.0(6) . . . . ?
O11 C11 C12 C13 -179.2(4) . . . . ?
C10 C11 C12 C13 -0.7(6) . . . . ?
C9 C8 C13 O13 -177.9(4) . . . . ?
C7 C8 C13 O13 2.4(6) . . . . ?
C9 C8 C13 C12 3.2(6) . . . . ?
C7 C8 C13 C12 -176.5(4) . . . . ?
C11 C12 C13 O13 179.4(4) . . . . ?
C11 C12 C13 C8 -1.7(6) . . . . ?
C9 C10 C14 C31 49.7(5) . . . . ?
C11 C10 C14 C31 -131.5(4) . . . . ?
C9 C10 C14 C15 -78.2(5) . . . . ?
C11 C10 C14 C15 100.7(4) . . . . ?
C10 C14 C15 C20 -82.8(5) . . . . ?
C31 C14 C15 C20 148.8(4) . . . . ?
C10 C14 C15 C16 98.2(4) . . . . ?
C31 C14 C15 C16 -30.2(5) . . . . ?
C20 C15 C16 C17 -3.9(6) . . . . ?
C14 C15 C16 C17 175.2(4) . . . . ?
C15 C16 C17 C18 -0.5(6) . . . . ?
C15 C16 C17 C21 177.8(4) . . . . ?
C16 C17 C18 O18 -177.4(4) . . . . ?
C21 C17 C18 O18 4.4(6) . . . . ?
C16 C17 C18 C19 2.9(6) . . . . ?
C21 C17 C18 C19 -175.3(4) . . . . ?
O18 C18 C19 C20 179.4(4) . . . . ?
C17 C18 C19 C20 -0.9(7) . . . . ?
C16 C15 C20 O20 -176.2(4) . . . . ?
C14 C15 C20 O20 4.8(6) . . . . ?
C16 C15 C20 C19 5.9(6) . . . . ?
C14 C15 C20 C19 -173.1(4) . . . . ?
C18 C19 C20 O20 178.2(4) . . . . ?
C18 C19 C20 C15 -3.7(7) . . . . ?
C18 C17 C21 C22 85.5(5) . . . . ?
C16 C17 C21 C22 -92.6(5) . . . . ?
C18 C17 C21 C33 -147.3(4) . . . . ?
C16 C17 C21 C33 34.5(5) . . . . ?
C33 C21 C22 C27 134.2(4) . . . . ?
C17 C21 C22 C27 -98.2(5) . . . . ?
C33 C21 C22 C23 -46.5(5) . . . . ?
C17 C21 C22 C23 81.1(5) . . . . ?
C27 C22 C23 C24 -3.0(6) . . . . ?
C21 C22 C23 C24 177.7(4) . . . . ?
C22 C23 C24 C25 1.3(6) . . . . ?
C22 C23 C24 C28 -178.8(4) . . . . ?
C23 C24 C25 C26 0.5(6) . . . . ?
C28 C24 C25 C26 -179.4(4) . . . . ?
C23 C24 C25 O25 179.7(4) . . . . ?
C28 C24 C25 O25 -0.2(6) . . . . ?
O25 C25 C26 C27 -179.6(4) . . . . ?
C24 C25 C26 C27 -0.5(7) . . . . ?
C23 C22 C27 O27 -178.4(4) . . . . ?
C21 C22 C27 O27 1.0(7) . . . . ?
C23 C22 C27 C26 3.0(6) . . . . ?
C21 C22 C27 C26 -177.7(4) . . . . ?
C25 C26 C27 O27 179.9(4) . . . . ?
C25 C26 C27 C22 -1.4(7) . . . . ?
C23 C24 C28 C1 -80.7(5) . . . . ?
C25 C24 C28 C1 99.2(4) . . . . ?
C23 C24 C28 C35 47.3(5) . . . . ?
C25 C24 C28 C35 -132.8(4) . . . . ?
C6 C1 C28 C24 -88.4(5) . . . . ?
C2 C1 C28 C24 92.9(5) . . . . ?
C6 C1 C28 C35 143.6(4) . . . . ?
C2 C1 C28 C35 -35.2(5) . . . . ?
C3 C7 C29 C30 173.9(4) . . . . ?
C8 C7 C29 C30 -59.5(5) . . . . ?
C10 C14 C31 C32 62.9(5) . . . . ?
C15 C14 C31 C32 -169.6(4) . . . . ?
C22 C21 C33 C34 -62.0(5) . . . . ?
C17 C21 C33 C34 171.9(4) . . . . ?
C24 C28 C35 C36 176.7(4) . . . . ?
C1 C28 C35 C36 -55.9(5) . . . . ?
C5 C4 O4 C37 -8.3(6) . . . . ?
C3 C4 O4 C37 171.8(4) . . . . ?
C12 C11 O11 C38 -13.3(6) . . . . ?
C10 C11 O11 C38 168.1(4) . . . . ?
C17 C18 O18 C39 164.0(4) . . . . ?
C19 C18 O18 C39 -16.3(6) . . . . ?
C26 C25 O25 C40 -9.1(7) . . . . ?
C24 C25 O25 C40 171.8(4) . . . . ?

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
O6 H6 O25 0.94(6) 1.91(6) 2.803(5) 158(5) .
O13 H13 O4 0.81(6) 2.01(6) 2.821(5) 174(6) .
O20 H20 O11 0.98(6) 1.82(6) 2.793(5) 175(5) .
O27 H27 O18 0.96(6) 1.82(6) 2.775(5) 173(5) .

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        66.89
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.095

#===END

data_III
_database_code_depnum_ccdc_archive 'CCDC 718575'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H51 N O8'
_chemical_formula_weight         697.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   20.7573(5)
_cell_length_b                   8.92140(10)
_cell_length_c                   19.7132(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.1850(10)
_cell_angle_gamma                90.00
_cell_volume                     3568.33(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_T_max  0.8695
_exptl_absorpt_process_details   
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3983
_diffrn_reflns_av_R_equivalents  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.36
_diffrn_reflns_theta_max         66.64
_reflns_number_total             2889
_reflns_number_gt                2540
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.1204P)²+2.7823P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2889
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1823
_refine_ls_wR_factor_gt          0.1740
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
C1 C -0.02184(10) 0.7975(2) 0.41239(11) 0.0269(5) Uani 1 1 d . . .
C2 C 0.03474(10) 0.8127(2) 0.38478(11) 0.0266(5) Uani 1 1 d . . .
H2 H 0.0302 0.8587 0.3406 0.032 Uiso 1 1 calc R . .
C3 C 0.09709(10) 0.7644(2) 0.41822(11) 0.0264(5) Uani 1 1 d . . .
C4 C 0.10245(10) 0.6962(2) 0.48326(11) 0.0279(5) Uani 1 1 d . . .
C5 C 0.04739(11) 0.6756(2) 0.51199(11) 0.0285(5) Uani 1 1 d . . .
H5 H 0.0516 0.6273 0.5557 0.034 Uiso 1 1 calc R . .
C6 C -0.01378(11) 0.7258(2) 0.47664(11) 0.0279(5) Uani 1 1 d . . .
C7 C 0.15804(10) 0.7960(2) 0.38845(11) 0.0266(5) Uani 1 1 d . . .
H7 H 0.1958 0.7418 0.4183 0.032 Uiso 1 1 calc R . .
C8 C 0.15145(10) 0.7371(2) 0.31482(11) 0.0257(5) Uani 1 1 d . . .
C9 C 0.12383(10) 0.8204(2) 0.25650(11) 0.0261(5) Uani 1 1 d . . .
H9 H 0.1068 0.9166 0.2635 0.031 Uiso 1 1 calc R . .
C10 C 0.11937(10) 0.7722(2) 0.18791(11) 0.0249(5) Uani 1 1 d . . .
C11 C 0.14617(10) 0.6308(2) 0.17993(11) 0.0268(5) Uani 1 1 d . . .
C12 C 0.17330(10) 0.5423(2) 0.23640(11) 0.0282(5) Uani 1 1 d . . .
H12 H 0.1909 0.4466 0.2294 0.034 Uiso 1 1 calc R . .
C13 C 0.17485(10) 0.5931(2) 0.30321(11) 0.0273(5) Uani 1 1 d . . .
C14 C 0.08790(10) 0.8642(2) 0.12454(11) 0.0269(5) Uani 1 1 d . . .
H14 H 0.1181 0.8578 0.0913 0.032 Uiso 1 1 calc R . .
C29 C 0.17449(11) 0.9653(2) 0.39425(11) 0.0300(5) Uani 1 1 d . . .
H29A H 0.2134 0.9847 0.3740 0.036 Uiso 1 1 calc R . .
H29B H 0.1370 1.0225 0.3670 0.036 Uiso 1 1 calc R . .
C30 C 0.18862(12) 1.0207(3) 0.46907(12) 0.0371(6) Uani 1 1 d . . .
H30A H 0.1490 1.0094 0.4882 0.056 Uiso 1 1 calc R . .
H30B H 0.2014 1.1265 0.4704 0.056 Uiso 1 1 calc R . .
H30C H 0.2246 0.9616 0.4968 0.056 Uiso 1 1 calc R . .
C31 C 0.07935(11) 1.0320(2) 0.13879(12) 0.0318(5) Uani 1 1 d . . .
H31A H 0.0533 1.0789 0.0962 0.038 Uiso 1 1 calc R . .
H31B H 0.0537 1.0418 0.1756 0.038 Uiso 1 1 calc R . .
C32 C 0.14368(12) 1.1180(2) 0.16099(13) 0.0392(6) Uani 1 1 d . . .
H32A H 0.1690 1.0757 0.2044 0.059 Uiso 1 1 calc R . .
H32B H 0.1341 1.2237 0.1681 0.059 Uiso 1 1 calc R . .
H32C H 0.1694 1.1098 0.1248 0.059 Uiso 1 1 calc R . .
C37 C -0.06529(12) 0.6651(3) 0.57238(12) 0.0374(6) Uani 1 1 d . . .
H37A H -0.0430 0.5680 0.5810 0.056 Uiso 1 1 calc R . .
H37B H -0.1093 0.6579 0.5828 0.056 Uiso 1 1 calc R . .
H37C H -0.0396 0.7415 0.6021 0.056 Uiso 1 1 calc R . .
C38 C 0.22028(13) 0.3602(2) 0.35076(13) 0.0383(6) Uani 1 1 d . . .
H38A H 0.1837 0.3035 0.3228 0.058 Uiso 1 1 calc R . .
H38B H 0.2350 0.3108 0.3958 0.058 Uiso 1 1 calc R . .
H38C H 0.2569 0.3644 0.3265 0.058 Uiso 1 1 calc R . .
O4 O 0.16374(7) 0.65131(18) 0.51805(8) 0.0349(4) Uani 1 1 d . . .
H4 H 0.1592(14) 0.611(3) 0.5565(16) 0.042 Uiso 1 1 d . . .
O6 O -0.07109(7) 0.70558(17) 0.50136(8) 0.0335(4) Uani 1 1 d . . .
O11 O 0.14800(8) 0.57194(18) 0.11547(8) 0.0350(4) Uani 1 1 d . . .
H11 H 0.1266(14) 0.628(3) 0.0829(16) 0.042 Uiso 1 1 d . . .
O13 O 0.19884(8) 0.50869(16) 0.36134(8) 0.0334(4) Uani 1 1 d . . .
C40A C 0.0000 0.3619(11) 0.2500 0.037(3) Uiso 0.50 2 d SP A 1
N40A N 0.0000 0.2301(9) 0.2500 0.061(2) Uiso 0.50 2 d SP A 1
C40B C -0.0221(8) 0.3554(17) 0.2434(6) 0.047(3) Uiso 0.25 1 d P . 2
N40B N -0.0342(5) 0.2359(10) 0.2376(4) 0.0401(18) Uiso 0.25 1 d P . 2
C41 C 0.0000 0.5182(4) 0.2500 0.0481(9) Uiso 1 2 d S . .
H41A H 0.0273 0.5548 0.2936 0.072 Uiso 0.50 1 calc PR A 1
H41B H -0.0452 0.5548 0.2455 0.072 Uiso 0.50 1 calc PR A 1
H41C H 0.0180 0.5548 0.2109 0.072 Uiso 0.50 1 calc PR A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.397(3) . ?
C1 C2 1.401(3) . ?
C1 C14 1.531(3) 2 ?
C2 C3 1.391(3) . ?
C3 C4 1.402(3) . ?
C3 C7 1.529(3) . ?
C4 O4 1.372(3) . ?
C4 C5 1.391(3) . ?
C5 C6 1.387(3) . ?
C6 O6 1.389(3) . ?
C7 C8 1.522(3) . ?
C7 C29 1.548(3) . ?
C8 C9 1.387(3) . ?
C8 C13 1.409(3) . ?
C9 C10 1.403(3) . ?
C10 C11 1.401(3) . ?
C10 C14 1.522(3) . ?
C11 O11 1.383(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.387(3) . ?
C13 O13 1.374(3) . ?
C14 C1 1.531(3) 2 ?
C14 C31 1.540(3) . ?
C29 C30 1.524(3) . ?
C31 C32 1.522(3) . ?
C37 O6 1.426(3) . ?
C38 O13 1.427(3) . ?
C40A N40A 1.176(13) . ?
C40A C41 1.394(11) . ?
C40B C40B 0.90(3) 2 ?
C40B N40B 1.096(17) . ?
C40B C41 1.520(16) . ?
C40B N40B 1.567(18) 2 ?
N40B N40B 1.399(19) 2 ?
N40B C40B 1.567(18) 2 ?
C41 C40B 1.520(16) 2 ?

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 C1 C2 116.52(19) . . ?
C6 C1 C14 122.22(19) . 2 ?
C2 C1 C14 121.18(18) . 2 ?
C3 C2 C1 123.94(19) . . ?
C2 C3 C4 117.00(19) . . ?
C2 C3 C7 121.57(18) . . ?
C4 C3 C7 121.23(19) . . ?
O4 C4 C5 120.87(19) . . ?
O4 C4 C3 118.04(18) . . ?
C5 C4 C3 121.1(2) . . ?
C6 C5 C4 119.76(19) . . ?
C5 C6 O6 122.85(19) . . ?
C5 C6 C1 121.7(2) . . ?
O6 C6 C1 115.46(19) . . ?
C8 C7 C3 112.78(17) . . ?
C8 C7 C29 112.42(17) . . ?
C3 C7 C29 109.81(16) . . ?
C9 C8 C13 116.74(19) . . ?
C9 C8 C7 122.92(18) . . ?
C13 C8 C7 120.32(18) . . ?
C8 C9 C10 124.48(18) . . ?
C11 C10 C9 115.93(19) . . ?
C11 C10 C14 120.37(18) . . ?
C9 C10 C14 123.71(17) . . ?
O11 C11 C12 115.91(18) . . ?
O11 C11 C10 122.27(19) . . ?
C12 C11 C10 121.82(19) . . ?
C11 C12 C13 120.11(19) . . ?
O13 C13 C12 123.03(18) . . ?
O13 C13 C8 116.15(18) . . ?
C12 C13 C8 120.82(19) . . ?
C10 C14 C1 111.50(16) . 2 ?
C10 C14 C31 114.89(17) . . ?
C1 C14 C31 109.79(17) 2 . ?
C30 C29 C7 112.47(18) . . ?
C32 C31 C14 114.47(19) . . ?
C6 O6 C37 118.43(17) . . ?
C13 O13 C38 117.15(17) . . ?
N40A C40A C41 180.000(2) . . ?
C40B C40B N40B 103.1(10) 2 . ?
C40B C40B C41 72.8(6) 2 . ?
N40B C40B C41 175.4(15) . . ?
N40B C40B N40B 60.4(11) . 2 ?
C41 C40B N40B 115.7(10) . 2 ?
C40B N40B N40B 76.8(10) . 2 ?

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 -1.6(3) . . . . ?
C14 C1 C2 C3 175.09(18) 2 . . . ?
C1 C2 C3 C4 0.3(3) . . . . ?
C1 C2 C3 C7 -174.67(18) . . . . ?
C2 C3 C4 O4 -178.30(18) . . . . ?
C7 C3 C4 O4 -3.3(3) . . . . ?
C2 C3 C4 C5 1.2(3) . . . . ?
C7 C3 C4 C5 176.20(18) . . . . ?
O4 C4 C5 C6 178.19(19) . . . . ?
C3 C4 C5 C6 -1.3(3) . . . . ?
C4 C5 C6 O6 178.28(18) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C2 C1 C6 C5 1.5(3) . . . . ?
C14 C1 C6 C5 -175.16(19) 2 . . . ?
C2 C1 C6 O6 -176.99(17) . . . . ?
C14 C1 C6 O6 6.3(3) 2 . . . ?
C2 C3 C7 C8 -56.4(2) . . . . ?
C4 C3 C7 C8 128.9(2) . . . . ?
C2 C3 C7 C29 69.9(2) . . . . ?
C4 C3 C7 C29 -104.9(2) . . . . ?
C3 C7 C8 C9 88.2(2) . . . . ?
C29 C7 C8 C9 -36.6(3) . . . . ?
C3 C7 C8 C13 -92.9(2) . . . . ?
C29 C7 C8 C13 142.27(19) . . . . ?
C13 C8 C9 C10 -1.6(3) . . . . ?
C7 C8 C9 C10 177.30(19) . . . . ?
C8 C9 C10 C11 -1.1(3) . . . . ?
C8 C9 C10 C14 179.00(19) . . . . ?
C9 C10 C11 O11 -176.98(18) . . . . ?
C14 C10 C11 O11 2.9(3) . . . . ?
C9 C10 C11 C12 2.1(3) . . . . ?
C14 C10 C11 C12 -177.97(18) . . . . ?
O11 C11 C12 C13 178.81(18) . . . . ?
C10 C11 C12 C13 -0.4(3) . . . . ?
C11 C12 C13 O13 177.55(18) . . . . ?
C11 C12 C13 C8 -2.6(3) . . . . ?
C9 C8 C13 O13 -176.65(17) . . . . ?
C7 C8 C13 O13 4.4(3) . . . . ?
C9 C8 C13 C12 3.5(3) . . . . ?
C7 C8 C13 C12 -175.47(19) . . . . ?
C11 C10 C14 C1 71.7(2) . . . 2 ?
C9 C10 C14 C1 -108.4(2) . . . 2 ?
C11 C10 C14 C31 -162.56(19) . . . . ?
C9 C10 C14 C31 17.3(3) . . . . ?
C8 C7 C29 C30 -173.63(18) . . . . ?
C3 C7 C29 C30 59.9(2) . . . . ?
C10 C14 C31 C32 65.9(2) . . . . ?
C1 C14 C31 C32 -167.48(18) 2 . . . ?
C5 C6 O6 C37 15.5(3) . . . . ?
C1 C6 O6 C37 -166.02(18) . . . . ?
C12 C13 O13 C38 -2.7(3) . . . . ?
C8 C13 O13 C38 177.48(18) . . . . ?
C40B C40B N40B N40B 3.6(17) 2 . . 2 ?
N40B C40B N40B C40B -3.6(17) 2 . . 2 ?
C40B C40B C41 C40A 0.000(3) 2 . . . ?
N40B C40B C41 C40A 1.7(8) 2 . . . ?
N40B C40B C41 C40B 1.7(8) 2 . . 2 ?

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
O4 H4 O11 0.86(3) 2.04(3) 2.833(2) 152(3) 6_566
O11 H11 O6 0.86(3) 1.94(3) 2.779(2) 165(3) 2

_diffrn_measured_fraction_theta_max 0.912
_diffrn_reflns_theta_full        66.64
_diffrn_measured_fraction_theta_full 0.912
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.078

#===END

data_IV
_database_code_depnum_ccdc_archive 'CCDC 718576'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H76.50 O14.25'
_chemical_formula_weight         977.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   14.3941(3)
_cell_length_b                   21.1462(5)
_cell_length_c                   17.3931(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.6360(10)
_cell_angle_gamma                90.00
_cell_volume                     5258.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2106
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7626
_exptl_absorpt_correction_T_max  0.9002
_exptl_absorpt_process_details   
'DENZO (Otwinowski, Borek, Majewski & Minor, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17078
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         67.13
_reflns_number_total             9196
_reflns_number_gt                7278
_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)+(0.0544P)²+3.1809P] 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         9196
_refine_ls_number_parameters     687
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1411
_refine_ls_wR_factor_gt          0.1300
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.031
_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
C1 C 0.41378(13) 0.12670(9) 0.93636(11) 0.0273(4) Uani 1 1 d . . .
C2 C 0.34099(13) 0.14968(9) 0.88383(11) 0.0274(4) Uani 1 1 d . . .
H2 H 0.3372 0.1355 0.8317 0.033 Uiso 1 1 calc R . .
C3 C 0.27346(13) 0.19229(9) 0.90338(12) 0.0274(4) Uani 1 1 d . . .
C4 C 0.28130(14) 0.21184(9) 0.98039(12) 0.0305(4) Uani 1 1 d . . .
C5 C 0.35498(14) 0.19282(10) 1.03388(12) 0.0319(4) Uani 1 1 d . . .
H5 H 0.3600 0.2082 1.0855 0.038 Uiso 1 1 calc R . .
C6 C 0.42143(14) 0.15106(9) 1.01146(12) 0.0300(4) Uani 1 1 d . . .
C7 C 0.19404(14) 0.21829(9) 0.84681(12) 0.0307(4) Uani 1 1 d . . .
H7 H 0.1346 0.2084 0.8689 0.037 Uiso 1 1 calc R . .
C8 C 0.19956(14) 0.29011(10) 0.84087(12) 0.0303(4) Uani 1 1 d . . .
C9 C 0.28394(14) 0.32127(10) 0.83804(12) 0.0307(4) Uani 1 1 d . . .
H9 H 0.3391 0.2965 0.8384 0.037 Uiso 1 1 calc R . .
C10 C 0.29223(15) 0.38689(10) 0.83472(12) 0.0321(4) Uani 1 1 d . . .
C11 C 0.21057(15) 0.42205(10) 0.83482(13) 0.0343(5) Uani 1 1 d . . .
C12 C 0.12412(15) 0.39293(10) 0.83589(13) 0.0365(5) Uani 1 1 d . . .
H12 H 0.0690 0.4177 0.8350 0.044 Uiso 1 1 calc R . .
C13 C 0.11876(14) 0.32734(10) 0.83826(12) 0.0329(5) Uani 1 1 d . . .
C14 C 0.38603(14) 0.42004(9) 0.83255(13) 0.0327(5) Uani 1 1 d . . .
H14 H 0.3830 0.4601 0.8627 0.039 Uiso 1 1 calc R . .
C15 C 0.46646(14) 0.38189(9) 0.87310(12) 0.0305(4) Uani 1 1 d . . .
C16 C 0.52361(14) 0.34334(9) 0.83342(12) 0.0293(4) Uani 1 1 d . . .
H16 H 0.5109 0.3408 0.7787 0.035 Uiso 1 1 calc R . .
C17 C 0.59838(13) 0.30841(9) 0.86966(12) 0.0287(4) Uani 1 1 d . . .
C18 C 0.61411(14) 0.31204(9) 0.95020(12) 0.0310(4) Uani 1 1 d . . .
C19 C 0.55767(15) 0.34858(10) 0.99224(12) 0.0347(5) Uani 1 1 d . . .
H19 H 0.5687 0.3496 1.0471 0.042 Uiso 1 1 calc R . .
C20 C 0.48499(14) 0.38361(10) 0.95351(12) 0.0332(5) Uani 1 1 d . . .
C21 C 0.66245(14) 0.26788(9) 0.82613(12) 0.0302(4) Uani 1 1 d . . .
H21 H 0.7277 0.2821 0.8437 0.036 Uiso 1 1 calc R . .
C22 C 0.65777(14) 0.19857(9) 0.84771(11) 0.0284(4) Uani 1 1 d . . .
C23 C 0.57817(13) 0.17076(9) 0.87075(11) 0.0282(4) Uani 1 1 d . . .
H23 H 0.5241 0.1963 0.8720 0.034 Uiso 1 1 calc R . .
C24 C 0.57309(13) 0.10764(9) 0.89212(11) 0.0279(4) Uani 1 1 d . . .
C25 C 0.65453(14) 0.07134(9) 0.89109(12) 0.0296(4) Uani 1 1 d . . .
C26 C 0.73546(14) 0.09723(10) 0.86745(12) 0.0317(5) Uani 1 1 d . . .
H26 H 0.7900 0.0720 0.8668 0.038 Uiso 1 1 calc R . .
C27 C 0.73605(13) 0.16009(10) 0.84485(12) 0.0311(4) Uani 1 1 d . . .
C28 C 0.48336(13) 0.07761(9) 0.91406(12) 0.0280(4) Uani 1 1 d . . .
H28 H 0.5015 0.0512 0.9611 0.034 Uiso 1 1 calc R . .
C29 C 0.18565(15) 0.18900(10) 0.76564(13) 0.0373(5) Uani 1 1 d . . .
H29A H 0.1421 0.2151 0.7306 0.045 Uiso 1 1 calc R . .
H29B H 0.2477 0.1907 0.7463 0.045 Uiso 1 1 calc R . .
C30 C 0.15122(18) 0.12072(12) 0.76153(17) 0.0509(6) Uani 1 1 d . . .
H30A H 0.1480 0.1056 0.7080 0.076 Uiso 1 1 calc R . .
H30B H 0.0889 0.1186 0.7789 0.076 Uiso 1 1 calc R . .
H30C H 0.1946 0.0942 0.7950 0.076 Uiso 1 1 calc R . .
C31 C 0.40005(15) 0.43947(10) 0.74936(13) 0.0367(5) Uani 1 1 d . . .
H31A H 0.4047 0.4009 0.7179 0.044 Uiso 1 1 calc R . .
H31B H 0.3445 0.4635 0.7266 0.044 Uiso 1 1 calc R . .
C32 C 0.48717(16) 0.47978(11) 0.74507(14) 0.0419(5) Uani 1 1 d . . .
H32A H 0.4925 0.4906 0.6910 0.063 Uiso 1 1 calc R . .
H32B H 0.5427 0.4560 0.7664 0.063 Uiso 1 1 calc R . .
H32C H 0.4824 0.5186 0.7751 0.063 Uiso 1 1 calc R . .
C33 C 0.64915(16) 0.27484(10) 0.73784(13) 0.0374(5) Uani 1 1 d . . .
H33A H 0.6814 0.2393 0.7150 0.045 Uiso 1 1 calc R . .
H33B H 0.5816 0.2713 0.7195 0.045 Uiso 1 1 calc R . .
C34 C 0.68559(19) 0.33680(12) 0.70797(15) 0.0499(6) Uani 1 1 d . . .
H34A H 0.6745 0.3375 0.6513 0.075 Uiso 1 1 calc R . .
H34B H 0.7528 0.3404 0.7245 0.075 Uiso 1 1 calc R . .
H34C H 0.6528 0.3724 0.7289 0.075 Uiso 1 1 calc R . .
C35 C 0.44136(14) 0.03213(9) 0.84988(12) 0.0306(4) Uani 1 1 d . . .
H35A H 0.4213 0.0571 0.8027 0.037 Uiso 1 1 calc R . .
H35B H 0.4908 0.0026 0.8374 0.037 Uiso 1 1 calc R . .
C36 C 0.35839(15) -0.00623(10) 0.87072(14) 0.0370(5) Uani 1 1 d . . .
H36A H 0.3356 -0.0337 0.8272 0.055 Uiso 1 1 calc R . .
H36B H 0.3083 0.0225 0.8820 0.055 Uiso 1 1 calc R . .
H36C H 0.3778 -0.0322 0.9164 0.055 Uiso 1 1 calc R . .
C37 C 0.50536(18) 0.15193(12) 1.13849(13) 0.0468(6) Uani 1 1 d . . .
H37A H 0.5617 0.1337 1.1671 0.070 Uiso 1 1 calc R . .
H37B H 0.4503 0.1389 1.1628 0.070 Uiso 1 1 calc R . .
H37C H 0.5101 0.1982 1.1393 0.070 Uiso 1 1 calc R . .
C38 C -0.04576(15) 0.33092(12) 0.84791(16) 0.0450(6) Uani 1 1 d . . .
H38A H -0.0999 0.3026 0.8457 0.067 Uiso 1 1 calc R . .
H38B H -0.0563 0.3625 0.8066 0.067 Uiso 1 1 calc R . .
H38C H -0.0373 0.3523 0.8982 0.067 Uiso 1 1 calc R . .
C39 C 0.4506(2) 0.43271(15) 1.07067(15) 0.0590(7) Uani 1 1 d . . .
H39A H 0.4032 0.4599 1.0899 0.088 Uiso 1 1 calc R . .
H39B H 0.5117 0.4537 1.0787 0.088 Uiso 1 1 calc R . .
H39C H 0.4537 0.3925 1.0988 0.088 Uiso 1 1 calc R . .
C40 C 0.88889(18) 0.14961(13) 0.8044(2) 0.0621(8) Uani 1 1 d . . .
H40A H 0.9393 0.1758 0.7883 0.093 Uiso 1 1 calc R . .
H40B H 0.8667 0.1203 0.7626 0.093 Uiso 1 1 calc R . .
H40C H 0.9123 0.1255 0.8508 0.093 Uiso 1 1 calc R . .
C41 C 0.23312(17) 0.30156(11) 1.05027(15) 0.0426(5) Uani 1 1 d . . .
H41A H 0.2731 0.3313 1.0249 0.051 Uiso 1 1 calc R . .
H41B H 0.2673 0.2879 1.1002 0.051 Uiso 1 1 calc R . .
C42 C 0.14263(18) 0.33224(11) 1.06296(15) 0.0462(6) Uani 1 1 d . . .
H42A H 0.1118 0.3495 1.0136 0.055 Uiso 1 1 calc R . .
H42B H 0.1002 0.3008 1.0827 0.055 Uiso 1 1 calc R . .
C44 C 0.0784(2) 0.40772(14) 1.1405(2) 0.0724(9) Uani 1 1 d . . .
H44A H 0.0468 0.3761 1.1704 0.087 Uiso 1 1 calc R . .
H44B H 0.0351 0.4195 1.0943 0.087 Uiso 1 1 calc R . .
C45 C 0.1015(2) 0.46464(13) 1.18896(16) 0.0577(7) Uani 1 1 d . A .
H45A H 0.0471 0.4756 1.2163 0.069 Uiso 1 1 calc R . .
H45B H 0.1544 0.4545 1.2286 0.069 Uiso 1 1 calc R . .
C47 C 0.2207(2) 0.51933(15) 1.13412(19) 0.0627(8) Uani 1 1 d . A .
H47A H 0.2390 0.4782 1.1132 0.075 Uiso 1 1 calc R . .
H47B H 0.2599 0.5269 1.1839 0.075 Uiso 1 1 calc R . .
C48 C 0.2350(2) 0.57012(16) 1.07929(19) 0.0725(9) Uani 1 1 d D . .
H48A H 0.2207 0.6107 1.1038 0.087 Uiso 0.721(8) 1 calc PR A 1
H48B H 0.3022 0.5708 1.0722 0.087 Uiso 0.721(8) 1 calc PR A 1
H48C H 0.3009 0.5843 1.0833 0.087 Uiso 0.279(8) 1 calc PR A 2
H48D H 0.1934 0.6068 1.0845 0.087 Uiso 0.279(8) 1 calc PR A 2
O49A O 0.1824(2) 0.56821(15) 1.00345(19) 0.0541(11) Uani 0.721(8) 1 d PD A 1
C50A C 0.2290(3) 0.52411(19) 0.9575(3) 0.0538(13) Uani 0.721(8) 1 d PD A 1
H50A H 0.2300 0.4812 0.9803 0.065 Uiso 0.721(8) 1 calc PR A 1
H50B H 0.2941 0.5377 0.9534 0.065 Uiso 0.721(8) 1 calc PR A 1
O49B O 0.2072(9) 0.5333(6) 1.0079(5) 0.096(4) Uani 0.279(8) 1 d PD A 2
C50B C 0.2061(10) 0.5722(5) 0.9391(6) 0.098(6) Uani 0.279(8) 1 d PD A 2
H50C H 0.2697 0.5871 0.9316 0.118 Uiso 0.279(8) 1 calc PR A 2
H50D H 0.1641 0.6091 0.9410 0.118 Uiso 0.279(8) 1 calc PR A 2
C51 C 0.1686(2) 0.52550(12) 0.87603(17) 0.0550(7) Uani 1 1 d D . .
H51A H 0.1053 0.5082 0.8792 0.066 Uiso 0.721(8) 1 calc PR A 1
H51B H 0.1629 0.5691 0.8554 0.066 Uiso 0.721(8) 1 calc PR A 1
H51C H 0.1283 0.4961 0.9015 0.066 Uiso 0.279(8) 1 calc PR A 2
H51D H 0.1259 0.5505 0.8391 0.066 Uiso 0.279(8) 1 calc PR A 2
C52 C 0.6930(2) 0.26507(13) 1.06499(14) 0.0546(7) Uani 1 1 d . . .
H52A H 0.6309 0.2509 1.0775 0.065 Uiso 1 1 calc R . .
H52B H 0.7105 0.3038 1.0952 0.065 Uiso 1 1 calc R . .
C53 C 0.7638(2) 0.21461(16) 1.08564(18) 0.0669(8) Uani 1 1 d . B .
H53A H 0.7535 0.1962 1.1363 0.080 Uiso 1 1 calc R . .
H53B H 0.7551 0.1805 1.0465 0.080 Uiso 1 1 calc R . .
C55 C 0.8966(2) 0.23934(16) 1.01946(19) 0.0677(8) Uani 1 1 d . B .
H55A H 0.9271 0.2809 1.0146 0.081 Uiso 1 1 calc R . .
H55B H 0.8465 0.2351 0.9757 0.081 Uiso 1 1 calc R . .
C56 C 0.9676(2) 0.18773(13) 1.0143(3) 0.0802(11) Uani 1 1 d D . .
H56A H 1.0155 0.2042 0.9830 0.096 Uiso 0.483(7) 1 calc PR B 1
H56B H 0.9993 0.1807 1.0672 0.096 Uiso 0.483(7) 1 calc PR B 1
H56C H 0.9916 0.1872 0.9632 0.096 Uiso 0.517(7) 1 calc PR B 2
H56D H 1.0207 0.1914 1.0557 0.096 Uiso 0.517(7) 1 calc PR B 2
O57A O 0.9386(5) 0.1267(2) 0.9831(3) 0.0672(17) Uani 0.483(7) 1 d PD B 1
C58A C 0.9346(6) 0.0866(4) 1.0483(5) 0.048(2) Uani 0.483(7) 1 d PD B 1
H58A H 0.9305 0.1127 1.0950 0.057 Uiso 0.483(7) 1 calc PR B 1
H58B H 0.9925 0.0611 1.0568 0.057 Uiso 0.483(7) 1 calc PR B 1
C59A C 0.8522(4) 0.0437(2) 1.0363(3) 0.0393(15) Uani 0.483(7) 1 d PD B 1
H59A H 0.8498 0.0168 1.0826 0.047 Uiso 0.483(7) 1 calc PR B 1
H59B H 0.7939 0.0690 1.0285 0.047 Uiso 0.483(7) 1 calc PR B 1
O57B O 0.9090(2) 0.13158(17) 1.0255(3) 0.0487(14) Uani 0.517(7) 1 d PD B 2
C58B C 0.9654(5) 0.0763(3) 1.0367(5) 0.043(2) Uani 0.517(7) 1 d PD B 2
H58C H 1.0084 0.0805 1.0851 0.052 Uiso 0.517(7) 1 calc PR B 2
H58D H 1.0036 0.0717 0.9932 0.052 Uiso 0.517(7) 1 calc PR B 2
C59B C 0.9059(4) 0.0189(3) 1.0412(2) 0.0459(15) Uani 0.517(7) 1 d PD B 2
H59C H 0.9456 -0.0173 1.0604 0.055 Uiso 0.517(7) 1 calc PR B 2
H59D H 0.8598 0.0265 1.0783 0.055 Uiso 0.517(7) 1 calc PR B 2
C61 C 0.79335(15) -0.04570(10) 0.96386(13) 0.0369(5) Uani 1 1 d . B .
H61A H 0.7652 -0.0489 1.0130 0.044 Uiso 1 1 calc R . .
H61B H 0.8258 -0.0861 0.9560 0.044 Uiso 1 1 calc R . .
C62 C 0.71727(14) -0.03575(10) 0.89824(13) 0.0340(5) Uani 1 1 d . . .
H62A H 0.7457 -0.0214 0.8521 0.041 Uiso 1 1 calc R . .
H62B H 0.6856 -0.0766 0.8854 0.041 Uiso 1 1 calc R . .
O4 O 0.20937(10) 0.24863(7) 1.00192(9) 0.0368(3) Uani 1 1 d . . .
O6 O 0.49675(11) 0.13032(7) 1.06086(8) 0.0394(4) Uani 1 1 d . . .
O11 O 0.21893(11) 0.48711(7) 0.82984(11) 0.0467(4) Uani 1 1 d . A .
O13 O 0.03602(10) 0.29500(7) 0.83803(10) 0.0429(4) Uani 1 1 d . . .
O18 O 0.68888(10) 0.27827(7) 0.98430(8) 0.0378(3) Uani 1 1 d . . .
O20 O 0.42639(11) 0.42126(8) 0.99071(9) 0.0436(4) Uani 1 1 d . . .
O25 O 0.64913(10) 0.00977(7) 0.91590(9) 0.0370(4) Uani 1 1 d . . .
O27 O 0.81382(10) 0.18902(7) 0.82120(10) 0.0407(4) Uani 1 1 d . . .
O43 O 0.16166(13) 0.38108(8) 1.11690(11) 0.0571(5) Uani 1 1 d . . .
O46 O 0.12591(13) 0.51824(9) 1.14570(12) 0.0594(5) Uani 1 1 d . . .
O54 O 0.85643(16) 0.23755(17) 1.08968(13) 0.1005(9) Uani 1 1 d . . .
O60 O 0.85944(10) 0.00451(7) 0.96933(9) 0.0398(4) Uani 1 1 d D . .
O100 O 0.0131(7) 0.4626(5) 0.9850(6) 0.090(3) Uani 0.25 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.396(3) . ?
C1 C6 1.397(3) . ?
C1 C28 1.524(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.394(3) . ?
C3 C7 1.522(3) . ?
C4 O4 1.381(2) . ?
C4 C5 1.387(3) . ?
C5 C6 1.390(3) . ?
C6 O6 1.375(3) . ?
C7 C8 1.525(3) . ?
C7 C29 1.534(3) . ?
C8 C9 1.388(3) . ?
C8 C13 1.401(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.391(3) . ?
C10 C14 1.526(3) . ?
C11 O11 1.384(3) . ?
C11 C12 1.390(3) . ?
C12 C13 1.390(3) . ?
C13 O13 1.373(3) . ?
C14 C15 1.517(3) . ?
C14 C31 1.540(3) . ?
C15 C20 1.394(3) . ?
C15 C16 1.396(3) . ?
C16 C17 1.394(3) . ?
C17 C18 1.395(3) . ?
C17 C21 1.523(3) . ?
C18 O18 1.368(2) . ?
C18 C19 1.389(3) . ?
C19 C20 1.391(3) . ?
C20 O20 1.375(2) . ?
C21 C22 1.516(3) . ?
C21 C33 1.532(3) . ?
C22 C23 1.388(3) . ?
C22 C27 1.395(3) . ?
C23 C24 1.390(3) . ?
C24 C25 1.403(3) . ?
C24 C28 1.527(3) . ?
C25 O25 1.377(2) . ?
C25 C26 1.392(3) . ?
C26 C27 1.386(3) . ?
C27 O27 1.380(2) . ?
C28 C35 1.543(3) . ?
C29 C30 1.526(3) . ?
C31 C32 1.525(3) . ?
C33 C34 1.525(3) . ?
C35 C36 1.522(3) . ?
C37 O6 1.417(3) . ?
C38 O13 1.428(3) . ?
C39 O20 1.415(3) . ?
C40 O27 1.421(3) . ?
C41 O4 1.418(3) . ?
C41 C42 1.494(3) . ?
C42 O43 1.401(3) . ?
C44 O43 1.427(3) . ?
C44 C45 1.485(4) . ?
C45 O46 1.427(3) . ?
C47 O46 1.403(3) . ?
C47 C48 1.466(5) . ?
C48 O49A 1.444(4) . ?
C48 O49B 1.481(8) . ?
O49A C50A 1.443(4) . ?
C50A C51 1.575(5) . ?
O49B C50B 1.451(8) . ?
C50B C51 1.527(9) . ?
C51 O11 1.401(3) . ?
C52 O18 1.425(3) . ?
C52 C53 1.490(4) . ?
C53 O54 1.413(4) . ?
C55 O54 1.411(4) . ?
C55 C56 1.505(4) . ?
C56 O57A 1.442(5) . ?
C56 O57B 1.482(4) . ?
O57A C58A 1.423(6) . ?
C58A C59A 1.488(7) . ?
C59A O60 1.443(4) . ?
O57B C58B 1.423(5) . ?
C58B C59B 1.492(7) . ?
C59B O60 1.383(4) . ?
C61 O60 1.421(3) . ?
C61 C62 1.502(3) . ?
C62 O25 1.433(2) . ?
O100 O100 1.72(2) 3_567 ?

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
C2 C1 C6 117.13(17) . . ?
C2 C1 C28 122.44(18) . . ?
C6 C1 C28 120.42(18) . . ?
C1 C2 C3 123.81(19) . . ?
C4 C3 C2 116.38(18) . . ?
C4 C3 C7 119.03(17) . . ?
C2 C3 C7 124.59(18) . . ?
O4 C4 C5 121.37(18) . . ?
O4 C4 C3 116.60(18) . . ?
C5 C4 C3 121.95(18) . . ?
C4 C5 C6 119.57(19) . . ?
O6 C6 C5 123.07(18) . . ?
O6 C6 C1 115.97(17) . . ?
C5 C6 C1 120.94(19) . . ?
C3 C7 C8 111.25(17) . . ?
C3 C7 C29 114.99(17) . . ?
C8 C7 C29 109.82(17) . . ?
C9 C8 C13 117.32(19) . . ?
C9 C8 C7 121.87(18) . . ?
C13 C8 C7 120.81(18) . . ?
C8 C9 C10 123.60(19) . . ?
C11 C10 C9 117.09(19) . . ?
C11 C10 C14 120.31(18) . . ?
C9 C10 C14 122.59(18) . . ?
O11 C11 C12 121.69(19) . . ?
O11 C11 C10 116.84(19) . . ?
C12 C11 C10 121.39(19) . . ?
C13 C12 C11 119.68(19) . . ?
O13 C13 C12 123.23(18) . . ?
O13 C13 C8 115.91(18) . . ?
C12 C13 C8 120.86(19) . . ?
C15 C14 C10 111.97(16) . . ?
C15 C14 C31 113.77(17) . . ?
C10 C14 C31 110.99(18) . . ?
C20 C15 C16 117.13(19) . . ?
C20 C15 C14 120.01(18) . . ?
C16 C15 C14 122.86(19) . . ?
C17 C16 C15 123.65(19) . . ?
C16 C17 C18 116.87(18) . . ?
C16 C17 C21 123.61(18) . . ?
C18 C17 C21 119.52(18) . . ?
O18 C18 C19 122.73(19) . . ?
O18 C18 C17 115.78(18) . . ?
C19 C18 C17 121.49(19) . . ?
C18 C19 C20 119.6(2) . . ?
O20 C20 C19 123.27(19) . . ?
O20 C20 C15 115.51(18) . . ?
C19 C20 C15 121.22(19) . . ?
C22 C21 C17 111.96(16) . . ?
C22 C21 C33 109.68(17) . . ?
C17 C21 C33 115.56(17) . . ?
C23 C22 C27 117.40(18) . . ?
C23 C22 C21 122.89(17) . . ?
C27 C22 C21 119.71(17) . . ?
C22 C23 C24 123.71(18) . . ?
C23 C24 C25 116.88(18) . . ?
C23 C24 C28 122.58(17) . . ?
C25 C24 C28 120.53(17) . . ?
O25 C25 C26 122.97(17) . . ?
O25 C25 C24 115.84(17) . . ?
C26 C25 C24 121.18(18) . . ?
C27 C26 C25 119.58(18) . . ?
O27 C27 C26 122.78(18) . . ?
O27 C27 C22 116.00(18) . . ?
C26 C27 C22 121.17(18) . . ?
C1 C28 C24 112.35(16) . . ?
C1 C28 C35 113.25(16) . . ?
C24 C28 C35 110.52(16) . . ?
C30 C29 C7 114.6(2) . . ?
C32 C31 C14 113.13(19) . . ?
C34 C33 C21 114.6(2) . . ?
C36 C35 C28 114.37(17) . . ?
O4 C41 C42 106.01(19) . . ?
O43 C42 C41 108.2(2) . . ?
O43 C44 C45 110.0(3) . . ?
O46 C45 C44 113.4(2) . . ?
O46 C47 C48 108.5(3) . . ?
O49A C48 C47 118.4(3) . . ?
C47 C48 O49B 96.6(5) . . ?
C50A O49A C48 107.2(3) . . ?
O49A C50A C51 104.0(3) . . ?
C50B O49B C48 111.7(8) . . ?
O49B C50B C51 101.2(7) . . ?
O11 C51 C50B 128.5(6) . . ?
O11 C51 C50A 103.7(2) . . ?
O18 C52 C53 109.1(2) . . ?
O54 C53 C52 112.4(3) . . ?
O54 C55 C56 112.4(3) . . ?
O57A C56 C55 120.1(4) . . ?
O57B C56 C55 99.9(3) . . ?
C58A O57A C56 105.7(5) . . ?
O57A C58A C59A 110.9(6) . . ?
O60 C59A C58A 109.4(5) . . ?
C58B O57B C56 110.6(4) . . ?
O57B C58B C59B 110.7(5) . . ?
O60 C59B C58B 110.6(5) . . ?
O60 C61 C62 111.69(17) . . ?
O25 C62 C61 112.85(18) . . ?
C4 O4 C41 117.94(16) . . ?
C6 O6 C37 117.92(17) . . ?
C11 O11 C51 119.04(18) . . ?
C13 O13 C38 117.50(17) . . ?
C18 O18 C52 118.04(17) . . ?
C20 O20 C39 117.82(18) . . ?
C25 O25 C62 120.22(15) . . ?
C27 O27 C40 117.61(17) . . ?
C42 O43 C44 112.2(2) . . ?
C47 O46 C45 113.0(2) . . ?
C55 O54 C53 116.4(3) . . ?
C59B O60 C61 118.4(2) . . ?
C61 O60 C59A 111.9(2) . . ?

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 -3.8(3) . . . . ?
C28 C1 C2 C3 176.75(17) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C1 C2 C3 C7 179.49(18) . . . . ?
C2 C3 C4 O4 -173.38(16) . . . . ?
C7 C3 C4 O4 7.0(3) . . . . ?
C2 C3 C4 C5 3.4(3) . . . . ?
C7 C3 C4 C5 -176.25(18) . . . . ?
O4 C4 C5 C6 174.07(18) . . . . ?
C3 C4 C5 C6 -2.6(3) . . . . ?
C4 C5 C6 O6 179.56(18) . . . . ?
C4 C5 C6 C1 -1.7(3) . . . . ?
C2 C1 C6 O6 -176.48(17) . . . . ?
C28 C1 C6 O6 3.0(3) . . . . ?
C2 C1 C6 C5 4.7(3) . . . . ?
C28 C1 C6 C5 -175.87(18) . . . . ?
C4 C3 C7 C8 60.2(2) . . . . ?
C2 C3 C7 C8 -119.5(2) . . . . ?
C4 C3 C7 C29 -174.19(18) . . . . ?
C2 C3 C7 C29 6.2(3) . . . . ?
C3 C7 C8 C9 41.6(3) . . . . ?
C29 C7 C8 C9 -86.9(2) . . . . ?
C3 C7 C8 C13 -138.23(19) . . . . ?
C29 C7 C8 C13 93.3(2) . . . . ?
C13 C8 C9 C10 1.6(3) . . . . ?
C7 C8 C9 C10 -178.2(2) . . . . ?
C8 C9 C10 C11 0.4(3) . . . . ?
C8 C9 C10 C14 179.29(19) . . . . ?
C9 C10 C11 O11 -178.65(19) . . . . ?
C14 C10 C11 O11 2.5(3) . . . . ?
C9 C10 C11 C12 -1.8(3) . . . . ?
C14 C10 C11 C12 179.3(2) . . . . ?
O11 C11 C12 C13 177.8(2) . . . . ?
C10 C11 C12 C13 1.1(3) . . . . ?
C11 C12 C13 O13 -178.8(2) . . . . ?
C11 C12 C13 C8 1.1(3) . . . . ?
C9 C8 C13 O13 177.48(19) . . . . ?
C7 C8 C13 O13 -2.7(3) . . . . ?
C9 C8 C13 C12 -2.4(3) . . . . ?
C7 C8 C13 C12 177.5(2) . . . . ?
C11 C10 C14 C15 150.2(2) . . . . ?
C9 C10 C14 C15 -28.6(3) . . . . ?
C11 C10 C14 C31 -81.5(2) . . . . ?
C9 C10 C14 C31 99.7(2) . . . . ?
C10 C14 C15 C20 -80.5(2) . . . . ?
C31 C14 C15 C20 152.65(19) . . . . ?
C10 C14 C15 C16 98.5(2) . . . . ?
C31 C14 C15 C16 -28.4(3) . . . . ?
C20 C15 C16 C17 -1.6(3) . . . . ?
C14 C15 C16 C17 179.37(18) . . . . ?
C15 C16 C17 C18 1.4(3) . . . . ?
C15 C16 C17 C21 -178.13(18) . . . . ?
C16 C17 C18 O18 -178.85(17) . . . . ?
C21 C17 C18 O18 0.7(3) . . . . ?
C16 C17 C18 C19 0.2(3) . . . . ?
C21 C17 C18 C19 179.76(18) . . . . ?
O18 C18 C19 C20 177.54(19) . . . . ?
C17 C18 C19 C20 -1.5(3) . . . . ?
C18 C19 C20 O20 -179.55(19) . . . . ?
C18 C19 C20 C15 1.2(3) . . . . ?
C16 C15 C20 O20 -179.00(17) . . . . ?
C14 C15 C20 O20 0.0(3) . . . . ?
C16 C15 C20 C19 0.3(3) . . . . ?
C14 C15 C20 C19 179.32(19) . . . . ?
C16 C17 C21 C22 -118.0(2) . . . . ?
C18 C17 C21 C22 62.5(2) . . . . ?
C16 C17 C21 C33 8.5(3) . . . . ?
C18 C17 C21 C33 -170.98(18) . . . . ?
C17 C21 C22 C23 29.8(3) . . . . ?
C33 C21 C22 C23 -99.9(2) . . . . ?
C17 C21 C22 C27 -150.11(19) . . . . ?
C33 C21 C22 C27 80.2(2) . . . . ?
C27 C22 C23 C24 1.2(3) . . . . ?
C21 C22 C23 C24 -178.75(19) . . . . ?
C22 C23 C24 C25 1.1(3) . . . . ?
C22 C23 C24 C28 -177.43(19) . . . . ?
C23 C24 C25 O25 177.11(18) . . . . ?
C28 C24 C25 O25 -4.3(3) . . . . ?
C23 C24 C25 C26 -1.9(3) . . . . ?
C28 C24 C25 C26 176.71(19) . . . . ?
O25 C25 C26 C27 -178.57(19) . . . . ?
C24 C25 C26 C27 0.3(3) . . . . ?
C25 C26 C27 O27 179.59(19) . . . . ?
C25 C26 C27 C22 2.1(3) . . . . ?
C23 C22 C27 O27 179.55(18) . . . . ?
C21 C22 C27 O27 -0.5(3) . . . . ?
C23 C22 C27 C26 -2.8(3) . . . . ?
C21 C22 C27 C26 177.13(19) . . . . ?
C2 C1 C28 C24 95.9(2) . . . . ?
C6 C1 C28 C24 -83.5(2) . . . . ?
C2 C1 C28 C35 -30.2(3) . . . . ?
C6 C1 C28 C35 150.37(18) . . . . ?
C23 C24 C28 C1 -19.5(3) . . . . ?
C25 C24 C28 C1 162.00(18) . . . . ?
C23 C24 C28 C35 108.1(2) . . . . ?
C25 C24 C28 C35 -70.4(2) . . . . ?
C3 C7 C29 C30 70.8(2) . . . . ?
C8 C7 C29 C30 -162.88(19) . . . . ?
C15 C14 C31 C32 -59.6(2) . . . . ?
C10 C14 C31 C32 173.04(17) . . . . ?
C22 C21 C33 C34 -159.44(19) . . . . ?
C17 C21 C33 C34 72.9(2) . . . . ?
C1 C28 C35 C36 -60.1(2) . . . . ?
C24 C28 C35 C36 172.86(17) . . . . ?
O4 C41 C42 O43 174.01(19) . . . . ?
O43 C44 C45 O46 73.8(3) . . . . ?
O46 C47 C48 O49A -58.5(4) . . . . ?
O46 C47 C48 O49B -84.1(6) . . . . ?
C47 C48 O49A C50A -80.1(4) . . . . ?
O49B C48 O49A C50A -27.2(8) . . . . ?
C48 O49A C50A C51 -179.2(3) . . . . ?
O49A C48 O49B C50B 40.4(8) . . . . ?
C47 C48 O49B C50B 175.4(11) . . . . ?
C48 O49B C50B C51 -175.6(8) . . . . ?
O49B C50B C51 O11 -94.9(10) . . . . ?
O49B C50B C51 C50A -30.9(7) . . . . ?
O49A C50A C51 O11 174.8(3) . . . . ?
O49A C50A C51 C50B 41.2(7) . . . . ?
O18 C52 C53 O54 76.0(3) . . . . ?
O54 C55 C56 O57A 88.6(5) . . . . ?
O54 C55 C56 O57B 56.9(4) . . . . ?
O57B C56 O57A C58A -38.7(5) . . . . ?
C55 C56 O57A C58A -101.0(7) . . . . ?
C56 O57A C58A C59A 140.3(5) . . . . ?
O57A C58A C59A O60 60.6(8) . . . . ?
O57A C56 O57B C58B 61.4(6) . . . . ?
C55 C56 O57B C58B -169.6(6) . . . . ?
C56 O57B C58B C59B -175.2(5) . . . . ?
O57B C58B C59B O60 71.6(7) . . . . ?
O60 C61 C62 O25 -77.2(2) . . . . ?
C5 C4 O4 C41 45.8(3) . . . . ?
C3 C4 O4 C41 -137.4(2) . . . . ?
C42 C41 O4 C4 179.38(18) . . . . ?
C5 C6 O6 C37 1.2(3) . . . . ?
C1 C6 O6 C37 -177.65(19) . . . . ?
C12 C11 O11 C51 44.7(3) . . . . ?
C10 C11 O11 C51 -138.5(2) . . . . ?
C50B C51 O11 C11 118.0(6) . . . . ?
C50A C51 O11 C11 80.0(3) . . . . ?
C12 C13 O13 C38 -10.0(3) . . . . ?
C8 C13 O13 C38 170.2(2) . . . . ?
C19 C18 O18 C52 18.7(3) . . . . ?
C17 C18 O18 C52 -162.2(2) . . . . ?
C53 C52 O18 C18 165.1(2) . . . . ?
C19 C20 O20 C39 10.5(3) . . . . ?
C15 C20 O20 C39 -170.2(2) . . . . ?
C26 C25 O25 C62 -17.8(3) . . . . ?
C24 C25 O25 C62 163.24(18) . . . . ?
C61 C62 O25 C25 98.1(2) . . . . ?
C26 C27 O27 C40 13.2(3) . . . . ?
C22 C27 O27 C40 -169.2(2) . . . . ?
C41 C42 O43 C44 -172.2(2) . . . . ?
C45 C44 O43 C42 -172.3(2) . . . . ?
C48 C47 O46 C45 171.1(2) . . . . ?
C44 C45 O46 C47 -85.6(3) . . . . ?
C56 C55 O54 C53 -105.6(3) . . . . ?
C52 C53 O54 C55 -85.8(4) . . . . ?
C58B C59B O60 C61 -174.8(3) . . . . ?
C58B C59B O60 C59A -84.8(6) . . . . ?
C62 C61 O60 C59B 150.9(3) . . . . ?
C62 C61 O60 C59A 109.0(3) . . . . ?
C58A C59A O60 C59B 59.7(5) . . . . ?
C58A C59A O60 C61 168.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        67.13
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.044

#===END

data_V
_database_code_depnum_ccdc_archive 'CCDC 718577'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H76.50 D6 O15.50 S'
_chemical_formula_weight         1065.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   14.5962(3)
_cell_length_b                   15.3340(4)
_cell_length_c                   26.2678(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.548(2)
_cell_angle_gamma                90.00
_cell_volume                     5828.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2282
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8211
_exptl_absorpt_correction_T_max  0.9043
_exptl_absorpt_process_details   
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10188
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         66.85
_reflns_number_total             10188
_reflns_number_gt                7385
_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)+(0.1708P)²+10.8426P] 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         10188
_refine_ls_number_parameters     741
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0973
_refine_ls_wR_factor_ref         0.3140
_refine_ls_wR_factor_gt          0.2822
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.080
_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
C1 C -0.0450(3) 0.7941(3) 0.09523(14) 0.0308(8) Uani 1 1 d . . .
C2 C -0.1005(3) 0.8266(3) 0.13016(14) 0.0314(8) Uani 1 1 d . . .
H2 H -0.0884 0.8838 0.1433 0.038 Uiso 1 1 calc R . .
C3 C -0.1733(3) 0.7797(3) 0.14696(15) 0.0321(9) Uani 1 1 d . . .
C4 C -0.1865(3) 0.6949(3) 0.12844(16) 0.0353(9) Uani 1 1 d . . .
C5 C -0.1328(3) 0.6595(3) 0.09378(17) 0.0428(10) Uani 1 1 d . . .
H5 H -0.1437 0.6016 0.0817 0.051 Uiso 1 1 calc R . .
C6 C -0.0631(3) 0.7090(3) 0.07680(16) 0.0372(9) Uani 1 1 d . . .
C7 C -0.2367(3) 0.8141(3) 0.18384(15) 0.0344(9) Uani 1 1 d . . .
H7 H -0.3008 0.7973 0.1690 0.041 Uiso 1 1 calc R . .
C8 C -0.2181(3) 0.7686(3) 0.23561(15) 0.0316(8) Uani 1 1 d . . .
C9 C -0.1309(3) 0.7407(3) 0.25674(15) 0.0311(8) Uani 1 1 d . . .
H9 H -0.0799 0.7543 0.2391 0.037 Uiso 1 1 calc R . .
C10 C -0.1141(3) 0.6940(3) 0.30252(15) 0.0334(9) Uani 1 1 d . . .
C11 C -0.1898(3) 0.6745(3) 0.32768(16) 0.0359(9) Uani 1 1 d . . .
C12 C -0.2779(3) 0.7031(3) 0.30869(17) 0.0406(10) Uani 1 1 d . . .
H12 H -0.3287 0.6901 0.3266 0.049 Uiso 1 1 calc R . .
C13 C -0.2913(3) 0.7506(3) 0.26354(16) 0.0357(9) Uani 1 1 d . . .
C14 C -0.0163(3) 0.6657(3) 0.32382(15) 0.0341(9) Uani 1 1 d . . .
H14 H -0.0222 0.6168 0.3484 0.041 Uiso 1 1 calc R . .
C15 C 0.0352(3) 0.6305(3) 0.28194(15) 0.0319(9) Uani 1 1 d . . .
C16 C 0.1114(3) 0.6724(3) 0.26579(15) 0.0320(8) Uani 1 1 d . . .
H16 H 0.1293 0.7273 0.2806 0.038 Uiso 1 1 calc R . .
C17 C 0.1626(3) 0.6383(3) 0.22939(15) 0.0313(8) Uani 1 1 d . . .
C18 C 0.1345(3) 0.5588(3) 0.20749(15) 0.0340(9) Uani 1 1 d . . .
C19 C 0.0573(3) 0.5143(3) 0.22140(16) 0.0363(9) Uani 1 1 d . . .
H19 H 0.0383 0.4604 0.2056 0.044 Uiso 1 1 calc R . .
C20 C 0.0094(3) 0.5501(3) 0.25858(15) 0.0333(9) Uani 1 1 d . . .
C21 C 0.2480(3) 0.6843(3) 0.21454(15) 0.0328(9) Uani 1 1 d . . .
H21 H 0.2950 0.6379 0.2111 0.039 Uiso 1 1 calc R . .
C22 C 0.2297(3) 0.7297(3) 0.16282(15) 0.0310(8) Uani 1 1 d . . .
C23 C 0.1445(3) 0.7633(3) 0.14265(15) 0.0316(8) Uani 1 1 d . . .
H23 H 0.0942 0.7553 0.1618 0.038 Uiso 1 1 calc R . .
C24 C 0.1277(3) 0.8079(3) 0.09632(15) 0.0318(8) Uani 1 1 d . . .
C25 C 0.2023(3) 0.8182(3) 0.06847(15) 0.0359(9) Uani 1 1 d . . .
C26 C 0.2894(3) 0.7845(3) 0.08681(16) 0.0368(9) Uani 1 1 d . . .
H26 H 0.3394 0.7910 0.0674 0.044 Uiso 1 1 calc R . .
C27 C 0.3021(3) 0.7415(3) 0.13340(16) 0.0339(9) Uani 1 1 d . . .
C28 C 0.0328(3) 0.8447(3) 0.07570(15) 0.0335(9) Uani 1 1 d . . .
H28 H 0.0253 0.8366 0.0376 0.040 Uiso 1 1 calc R . .
C29 C -0.2372(3) 0.9134(3) 0.18945(17) 0.0402(10) Uani 1 1 d . . .
H29A H -0.2712 0.9292 0.2184 0.048 Uiso 1 1 calc R . .
H29B H -0.1728 0.9343 0.1979 0.048 Uiso 1 1 calc R . .
C30 C -0.2819(4) 0.9595(4) 0.1408(2) 0.0557(13) Uani 1 1 d . . .
H30A H -0.2481 0.9448 0.1121 0.084 Uiso 1 1 calc R . .
H30B H -0.2800 1.0227 0.1463 0.084 Uiso 1 1 calc R . .
H30C H -0.3463 0.9405 0.1329 0.084 Uiso 1 1 calc R . .
C31 C 0.0348(3) 0.7403(3) 0.35465(17) 0.0421(10) Uani 1 1 d . . .
H31A H 0.1008 0.7242 0.3629 0.051 Uiso 1 1 calc R . .
H31B H 0.0315 0.7931 0.3328 0.051 Uiso 1 1 calc R . .
C32 C -0.0032(4) 0.7623(4) 0.4046(2) 0.0567(13) Uani 1 1 d . . .
H32A H -0.0681 0.7799 0.3968 0.085 Uiso 1 1 calc R . .
H32B H 0.0327 0.8101 0.4220 0.085 Uiso 1 1 calc R . .
H32C H 0.0012 0.7108 0.4269 0.085 Uiso 1 1 calc R . .
C33 C 0.2925(3) 0.7488(3) 0.25524(16) 0.0373(9) Uani 1 1 d . . .
H33A H 0.3428 0.7805 0.2412 0.045 Uiso 1 1 calc R . .
H33B H 0.2456 0.7923 0.2622 0.045 Uiso 1 1 calc R . .
C34 C 0.3319(3) 0.7056(4) 0.30564(18) 0.0489(12) Uani 1 1 d . . .
H34A H 0.2813 0.6818 0.3225 0.073 Uiso 1 1 calc R . .
H34B H 0.3660 0.7489 0.3282 0.073 Uiso 1 1 calc R . .
H34C H 0.3738 0.6584 0.2987 0.073 Uiso 1 1 calc R . .
C35 C 0.0300(3) 0.9436(3) 0.08533(17) 0.0390(10) Uani 1 1 d . . .
H35A H 0.0324 0.9539 0.1227 0.047 Uiso 1 1 calc R . .
H35B H 0.0855 0.9706 0.0741 0.047 Uiso 1 1 calc R . .
C36 C -0.0561(3) 0.9882(3) 0.0574(2) 0.0510(12) Uani 1 1 d . . .
H36A H -0.0639 0.9718 0.0211 0.077 Uiso 1 1 calc R . .
H36B H -0.0491 1.0517 0.0605 0.077 Uiso 1 1 calc R . .
H36C H -0.1106 0.9699 0.0728 0.077 Uiso 1 1 calc R . .
C37 C -0.0269(5) 0.5964(4) 0.0211(3) 0.0750(19) Uani 1 1 d . . .
H37A H -0.0138 0.5531 0.0485 0.113 Uiso 1 1 calc R . .
H37B H 0.0130 0.5858 -0.0055 0.113 Uiso 1 1 calc R . .
H37C H -0.0918 0.5918 0.0060 0.113 Uiso 1 1 calc R . .
C38 C -0.4545(3) 0.7485(4) 0.2644(2) 0.0654(16) Uani 1 1 d . . .
H38A H -0.4550 0.6846 0.2637 0.098 Uiso 1 1 calc R . .
H38B H -0.5115 0.7707 0.2448 0.098 Uiso 1 1 calc R . .
H38C H -0.4504 0.7688 0.3000 0.098 Uiso 1 1 calc R . .
C39 C -0.0874(3) 0.4245(3) 0.25874(19) 0.0460(11) Uani 1 1 d . . .
H39A H -0.1062 0.4246 0.2215 0.069 Uiso 1 1 calc R . .
H39B H -0.1382 0.4024 0.2761 0.069 Uiso 1 1 calc R . .
H39C H -0.0332 0.3869 0.2670 0.069 Uiso 1 1 calc R . .
C40 C 0.4611(3) 0.7114(4) 0.1230(2) 0.0528(13) Uani 1 1 d . . .
H40A H 0.4435 0.6796 0.0909 0.079 Uiso 1 1 calc R . .
H40B H 0.5166 0.6849 0.1418 0.079 Uiso 1 1 calc R . .
H40C H 0.4739 0.7724 0.1153 0.079 Uiso 1 1 calc R . .
C41 C -0.2426(4) 0.5595(4) 0.1555(3) 0.0633(15) Uani 1 1 d . . .
H41A H -0.1825 0.5522 0.1773 0.076 Uiso 1 1 calc R . .
H41B H -0.2406 0.5266 0.1232 0.076 Uiso 1 1 calc R . .
C42 C -0.3199(3) 0.5255(4) 0.1831(2) 0.0609(15) Uani 1 1 d . . .
H42A H -0.3053 0.4659 0.1962 0.073 Uiso 1 1 calc R . .
H42B H -0.3281 0.5637 0.2126 0.073 Uiso 1 1 calc R . .
C44 C -0.4696(4) 0.4646(4) 0.1588(2) 0.0667(16) Uani 1 1 d . . .
H44A H -0.4406 0.4064 0.1646 0.080 Uiso 1 1 calc R . .
H44B H -0.5175 0.4600 0.1286 0.080 Uiso 1 1 calc R . .
C45 C -0.5163(4) 0.4882(4) 0.2055(2) 0.0607(14) Uani 1 1 d . A .
H45A H -0.5337 0.5506 0.2042 0.073 Uiso 1 1 calc R . .
H45B H -0.5730 0.4530 0.2059 0.073 Uiso 1 1 calc R . .
C47 C -0.4958(4) 0.4728(4) 0.2949(2) 0.0551(13) Uani 1 1 d . A .
H47A H -0.5436 0.4267 0.2937 0.066 Uiso 1 1 calc R . .
H47B H -0.5256 0.5300 0.2986 0.066 Uiso 1 1 calc R . .
C48 C -0.4206(5) 0.4572(4) 0.3394(3) 0.088(2) Uani 1 1 d D . .
H48A H -0.4485 0.4408 0.3704 0.105 Uiso 0.814(7) 1 calc PR A 1
H48B H -0.3800 0.4089 0.3311 0.105 Uiso 0.814(7) 1 calc PR A 1
H48C H -0.4449 0.4063 0.3566 0.105 Uiso 0.186(7) 1 calc PR A 2
H48D H -0.3699 0.4334 0.3219 0.105 Uiso 0.186(7) 1 calc PR A 2
O49A O -0.3672(3) 0.5370(3) 0.34872(19) 0.0630(13) Uani 0.814(7) 1 d PD A 1
C50A C -0.2916(5) 0.5208(5) 0.3871(4) 0.095(4) Uani 0.814(7) 1 d PD A 1
H50A H -0.2492 0.4779 0.3744 0.114 Uiso 0.814(7) 1 calc PR A 1
H50B H -0.3142 0.4962 0.4180 0.114 Uiso 0.814(7) 1 calc PR A 1
O49B O -0.3725(13) 0.5025(13) 0.3807(6) 0.0630(13) Uani 0.186(7) 1 d PD A 2
C50B C -0.288(2) 0.535(2) 0.3655(12) 0.088(2) Uani 0.186(7) 1 d PD A 2
H50C H -0.3012 0.5592 0.3304 0.105 Uiso 0.186(7) 1 calc PR A 2
H50D H -0.2449 0.4853 0.3642 0.105 Uiso 0.186(7) 1 calc PR A 2
C51 C -0.2424(4) 0.6028(5) 0.4002(2) 0.0701(18) Uani 1 1 d D . .
H51A H -0.2882 0.6507 0.3967 0.084 Uiso 0.814(7) 1 calc PR A 1
H51B H -0.2158 0.6001 0.4369 0.084 Uiso 0.814(7) 1 calc PR A 1
H51C H -0.2838 0.6527 0.4042 0.084 Uiso 0.186(7) 1 calc PR A 2
H51D H -0.2183 0.5790 0.4344 0.084 Uiso 0.186(7) 1 calc PR A 2
C52 C 0.1651(3) 0.4424(3) 0.15016(18) 0.0432(10) Uani 1 1 d . . .
H52A H 0.1020 0.4435 0.1310 0.052 Uiso 1 1 calc R . .
H52B H 0.1671 0.3975 0.1773 0.052 Uiso 1 1 calc R . .
C53 C 0.2346(4) 0.4212(3) 0.11413(18) 0.0507(12) Uani 1 1 d . B .
H53A H 0.2970 0.4374 0.1310 0.061 Uiso 1 1 calc R . .
H53B H 0.2343 0.3574 0.1084 0.061 Uiso 1 1 calc R . .
C55 C 0.2349(5) 0.5552(4) 0.0658(2) 0.0719(17) Uani 1 1 d . B .
H55A H 0.2964 0.5677 0.0851 0.086 Uiso 1 1 calc R . .
H55B H 0.1879 0.5845 0.0837 0.086 Uiso 1 1 calc R . .
C56 C 0.2309(5) 0.5911(4) 0.0141(3) 0.083(2) Uani 1 1 d D . .
H56A H 0.2068 0.6515 0.0123 0.099 Uiso 0.572(10) 1 calc PR B 1
H56B H 0.1925 0.5545 -0.0115 0.099 Uiso 0.572(10) 1 calc PR B 1
H56C H 0.1652 0.5965 0.0008 0.099 Uiso 0.428(10) 1 d PR B 5
H56D H 0.2557 0.6519 0.0177 0.099 Uiso 0.428(10) 1 d PR B 5
C58 C 0.3412(7) 0.6128(6) -0.0432(3) 0.111(3) Uani 1 1 d D . .
H58A H 0.2903 0.5883 -0.0677 0.133 Uiso 0.572(10) 1 calc PR B 1
H58B H 0.3998 0.5875 -0.0515 0.133 Uiso 0.572(10) 1 calc PR B 1
H58C H 0.3737 0.5811 -0.0698 0.133 Uiso 0.428(10) 1 d PR B 2
H58D H 0.3852 0.6283 -0.0149 0.133 Uiso 0.428(10) 1 d PR B 2
O57A O 0.3285(5) 0.5883(5) 0.0065(3) 0.069(3) Uani 0.572(10) 1 d PD B 1
C59A C 0.3437(7) 0.7098(8) -0.0500(5) 0.094(6) Uani 0.572(10) 1 d PD B 1
H59A H 0.3870 0.7352 -0.0218 0.113 Uiso 0.572(10) 1 calc PR B 1
H59B H 0.3678 0.7230 -0.0827 0.113 Uiso 0.572(10) 1 calc PR B 1
O60A O 0.2543(8) 0.7505(5) -0.0507(4) 0.091(3) Uani 0.572(10) 1 d PD B 1
C61A C 0.2463(10) 0.8403(7) -0.0551(4) 0.054(3) Uani 0.572(10) 1 d PD B 1
H61A H 0.1850 0.8542 -0.0742 0.065 Uiso 0.572(10) 1 calc PR B 1
H61B H 0.2937 0.8617 -0.0757 0.065 Uiso 0.572(10) 1 calc PR B 1
O57B O 0.2721(9) 0.5527(6) -0.0268(4) 0.097(5) Uani 0.428(10) 1 d PD B 2
C59B C 0.2965(15) 0.6922(9) -0.0675(5) 0.111(3) Uani 0.428(10) 1 d PD B 2
H59C H 0.3250 0.7111 -0.0979 0.133 Uiso 0.428(10) 1 calc PR B 2
H59D H 0.2290 0.6848 -0.0770 0.133 Uiso 0.428(10) 1 calc PR B 2
O60B O 0.3188(9) 0.7495(7) -0.0243(3) 0.065(3) Uani 0.428(10) 1 d PD B 2
C61B C 0.2826(14) 0.8274(9) -0.0452(5) 0.072(7) Uani 0.428(10) 1 d PD B 2
H61C H 0.2274 0.8148 -0.0702 0.087 Uiso 0.428(10) 1 calc PR B 2
H61D H 0.3290 0.8559 -0.0640 0.087 Uiso 0.428(10) 1 calc PR B 2
C62 C 0.2565(3) 0.8885(4) -0.00537(18) 0.0512(12) Uani 1 1 d D . .
H62A H 0.3171 0.8750 0.0146 0.061 Uiso 0.572(10) 1 calc PR B 1
H62B H 0.2535 0.9521 -0.0119 0.061 Uiso 0.572(10) 1 calc PR B 1
H62C H 0.3127 0.8999 0.0195 0.061 Uiso 0.428(10) 1 d PR B 5
H62D H 0.2387 0.9445 -0.0226 0.061 Uiso 0.428(10) 1 d PR B 5
O4 O -0.2589(2) 0.64856(19) 0.14455(12) 0.0429(7) Uani 1 1 d . . .
O6 O -0.0098(2) 0.6809(2) 0.04162(12) 0.0480(8) Uani 1 1 d . . .
O11 O -0.1716(2) 0.6245(2) 0.37157(12) 0.0482(8) Uani 1 1 d . A .
O13 O -0.37683(19) 0.7798(2) 0.24208(12) 0.0475(8) Uani 1 1 d . . .
O18 O 0.1877(2) 0.52593(19) 0.17261(11) 0.0407(7) Uani 1 1 d . . .
O20 O -0.0652(2) 0.5105(2) 0.27560(12) 0.0424(7) Uani 1 1 d . . .
O25 O 0.1840(2) 0.8632(2) 0.02295(12) 0.0494(8) Uani 1 1 d . B .
O27 O 0.38668(19) 0.7076(2) 0.15399(11) 0.0411(7) Uani 1 1 d . . .
O43 O -0.4012(2) 0.5247(2) 0.14746(14) 0.0555(9) Uani 1 1 d . . .
O46 O -0.4538(2) 0.4712(3) 0.24983(15) 0.0604(10) Uani 1 1 d . . .
O54 O 0.2191(3) 0.4634(2) 0.06570(13) 0.0586(9) Uani 1 1 d . . .
S10A S -0.3351(3) 0.7931(3) 0.48490(13) 0.0547(9) Uani 0.35 1 d PD C 1
S10B S -0.4156(7) 0.7832(6) 0.4911(3) 0.079(4) Uani 0.15 1 d PD C 2
O11A O -0.4014(6) 0.7812(6) 0.4356(3) 0.081(3) Uani 0.50 1 d PD . .
C12A C -0.3780(9) 0.8755(8) 0.5189(5) 0.097(4) Uani 0.50 1 d PD . .
D12A H -0.3744 0.9307 0.5005 0.145 Uiso 0.35 1 calc PR C 1
D12B H -0.3415 0.8799 0.5529 0.145 Uiso 0.35 1 calc PR C 1
D12C H -0.4426 0.8631 0.5228 0.145 Uiso 0.35 1 calc PR C 1
D12D H -0.3807 0.9218 0.4930 0.145 Uiso 0.15 1 calc PR C 2
D12E H -0.3140 0.8680 0.5350 0.145 Uiso 0.15 1 calc PR C 2
D12F H -0.4169 0.8914 0.5451 0.145 Uiso 0.15 1 calc PR C 2
C13A C -0.3489(10) 0.7096(9) 0.5254(5) 0.097(4) Uani 0.50 1 d PD . .
D13A H -0.3271 0.6553 0.5113 0.145 Uiso 0.35 1 calc PR C 1
D13B H -0.4144 0.7038 0.5293 0.145 Uiso 0.35 1 calc PR C 1
D13C H -0.3131 0.7212 0.5589 0.145 Uiso 0.35 1 calc PR C 1
D13D H -0.3362 0.6610 0.5031 0.145 Uiso 0.15 1 calc PR C 2
D13E H -0.3809 0.6876 0.5533 0.145 Uiso 0.15 1 calc PR C 2
D13F H -0.2905 0.7370 0.5398 0.145 Uiso 0.15 1 calc PR C 2
S20A S 0.5291(4) 0.9930(5) 0.0293(2) 0.1331(18) Uiso 0.50 1 d PD . .
O21A O 0.4797(10) 0.9148(10) 0.0461(5) 0.131(4) Uiso 0.50 1 d PD . .
C22A C 0.5105(16) 1.0841(12) 0.0662(8) 0.120(8) Uiso 0.50 1 d PD . .
D22A H 0.4944 1.1341 0.0436 0.180 Uiso 0.50 1 calc PR . .
D22B H 0.5669 1.0971 0.0896 0.180 Uiso 0.50 1 calc PR . .
D22C H 0.4598 1.0721 0.0863 0.180 Uiso 0.50 1 calc PR . .
C23A C 0.4564(14) 1.0652(13) -0.0065(9) 0.140(8) Uiso 0.50 1 d PD . .
D23A H 0.4499 1.1180 0.0137 0.210 Uiso 0.50 1 calc PR . .
D23B H 0.3957 1.0381 -0.0156 0.210 Uiso 0.50 1 calc PR . .
D23C H 0.4824 1.0805 -0.0378 0.210 Uiso 0.50 1 calc PR . .
O30A O 0.5022(8) 0.8683(10) -0.0907(5) 0.118(5) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.394(5) . ?
C1 C6 1.404(6) . ?
C1 C28 1.520(5) . ?
C2 C3 1.401(5) . ?
C3 C4 1.393(6) . ?
C3 C7 1.520(5) . ?
C4 O4 1.386(5) . ?
C4 C5 1.388(6) . ?
C5 C6 1.389(6) . ?
C6 O6 1.354(5) . ?
C7 C8 1.521(6) . ?
C7 C29 1.530(6) . ?
C8 C9 1.388(6) . ?
C8 C13 1.400(5) . ?
C9 C10 1.394(6) . ?
C10 C11 1.393(6) . ?
C10 C14 1.526(5) . ?
C11 O11 1.380(5) . ?
C11 C12 1.388(6) . ?
C12 C13 1.384(6) . ?
C13 O13 1.376(5) . ?
C14 C15 1.512(5) . ?
C14 C31 1.538(6) . ?
C15 C16 1.398(5) . ?
C15 C20 1.406(6) . ?
C16 C17 1.390(6) . ?
C17 C18 1.388(6) . ?
C17 C21 1.526(5) . ?
C18 O18 1.372(5) . ?
C18 C19 1.405(6) . ?
C19 C20 1.387(6) . ?
C20 O20 1.372(5) . ?
C21 C22 1.519(5) . ?
C21 C33 1.537(6) . ?
C22 C23 1.385(6) . ?
C22 C27 1.400(5) . ?
C23 C24 1.390(6) . ?
C24 C25 1.398(6) . ?
C24 C28 1.526(6) . ?
C25 O25 1.376(5) . ?
C25 C26 1.398(6) . ?
C26 C27 1.381(6) . ?
C27 O27 1.383(5) . ?
C28 C35 1.538(6) . ?
C29 C30 1.529(6) . ?
C31 C32 1.527(6) . ?
C33 C34 1.524(6) . ?
C35 C36 1.531(6) . ?
C37 O6 1.413(6) . ?
C38 O13 1.426(5) . ?
C39 O20 1.416(5) . ?
C40 O27 1.441(5) . ?
C41 O4 1.409(6) . ?
C41 C42 1.513(7) . ?
C42 O43 1.413(6) . ?
C44 O43 1.418(6) . ?
C44 C45 1.522(8) . ?
C45 O46 1.407(7) . ?
C47 O46 1.402(6) . ?
C47 C48 1.514(9) . ?
C48 O49B 1.398(10) . ?
C48 O49A 1.455(7) . ?
O49A C50A 1.416(7) . ?
C50A C51 1.467(10) . ?
O49B C50B 1.431(10) . ?
C50B C51 1.485(14) . ?
C51 O11 1.397(6) . ?
C52 O18 1.430(5) . ?
C52 C53 1.511(6) . ?
C53 O54 1.418(6) . ?
C55 O54 1.427(7) . ?
C55 C56 1.459(9) . ?
C56 O57B 1.423(8) . ?
C56 O57A 1.464(7) . ?
C58 O57A 1.393(7) . ?
C58 O57B 1.471(8) . ?
C58 C59B 1.485(11) . ?
C58 C59A 1.499(10) . ?
C59A O60A 1.444(8) . ?
O60A C61A 1.386(12) . ?
C61A C62 1.491(9) . ?
C59B O60B 1.439(9) . ?
O60B C61B 1.390(13) . ?
C61B C62 1.491(10) . ?
C62 O25 1.426(5) . ?
S10A O11A 1.523(9) . ?
S10A C13A 1.694(11) . ?
S10A C12A 1.712(12) . ?
S10B O11A 1.501(10) . ?
S10B C12A 1.653(11) . ?
S10B C13A 1.675(12) . ?
S20A C23A 1.11(2) 3_675 ?
S20A O21A 1.495(16) . ?
S20A S20A 1.670(12) 3_675 ?
S20A C23A 1.723(17) . ?
S20A C22A 1.742(17) . ?
O21A C23A 1.52(2) 3_675 ?
O30A C22A 1.006(19) 3_675 ?

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
C2 C1 C6 117.4(4) . . ?
C2 C1 C28 124.4(4) . . ?
C6 C1 C28 118.2(3) . . ?
C1 C2 C3 123.6(4) . . ?
C4 C3 C2 116.5(4) . . ?
C4 C3 C7 118.6(4) . . ?
C2 C3 C7 124.9(4) . . ?
O4 C4 C5 121.3(4) . . ?
O4 C4 C3 116.6(4) . . ?
C5 C4 C3 122.0(4) . . ?
C4 C5 C6 119.8(4) . . ?
O6 C6 C5 123.8(4) . . ?
O6 C6 C1 115.6(4) . . ?
C5 C6 C1 120.6(4) . . ?
C3 C7 C8 111.0(3) . . ?
C3 C7 C29 114.7(3) . . ?
C8 C7 C29 112.0(3) . . ?
C9 C8 C13 116.9(4) . . ?
C9 C8 C7 123.0(3) . . ?
C13 C8 C7 120.0(3) . . ?
C8 C9 C10 123.4(4) . . ?
C11 C10 C9 117.3(4) . . ?
C11 C10 C14 121.8(4) . . ?
C9 C10 C14 120.8(4) . . ?
O11 C11 C12 122.9(4) . . ?
O11 C11 C10 116.0(4) . . ?
C12 C11 C10 121.1(4) . . ?
C13 C12 C11 119.6(4) . . ?
O13 C13 C12 122.8(4) . . ?
O13 C13 C8 115.8(4) . . ?
C12 C13 C8 121.4(4) . . ?
C15 C14 C10 111.4(3) . . ?
C15 C14 C31 113.3(3) . . ?
C10 C14 C31 110.3(3) . . ?
C16 C15 C20 116.7(4) . . ?
C16 C15 C14 123.3(4) . . ?
C20 C15 C14 120.0(3) . . ?
C17 C16 C15 123.9(4) . . ?
C18 C17 C16 117.3(4) . . ?
C18 C17 C21 120.5(4) . . ?
C16 C17 C21 122.2(4) . . ?
O18 C18 C17 115.9(4) . . ?
O18 C18 C19 122.6(4) . . ?
C17 C18 C19 121.5(4) . . ?
C20 C19 C18 119.1(4) . . ?
O20 C20 C19 123.3(4) . . ?
O20 C20 C15 115.1(4) . . ?
C19 C20 C15 121.6(4) . . ?
C22 C21 C17 112.7(3) . . ?
C22 C21 C33 109.6(3) . . ?
C17 C21 C33 113.8(3) . . ?
C23 C22 C27 116.5(4) . . ?
C23 C22 C21 123.8(3) . . ?
C27 C22 C21 119.7(3) . . ?
C22 C23 C24 124.4(4) . . ?
C23 C24 C25 117.0(4) . . ?
C23 C24 C28 122.7(3) . . ?
C25 C24 C28 120.3(3) . . ?
O25 C25 C24 115.8(4) . . ?
O25 C25 C26 123.3(4) . . ?
C24 C25 C26 120.9(4) . . ?
C27 C26 C25 119.5(4) . . ?
C26 C27 O27 122.3(4) . . ?
C26 C27 C22 121.8(4) . . ?
O27 C27 C22 115.8(4) . . ?
C1 C28 C24 112.0(3) . . ?
C1 C28 C35 114.2(3) . . ?
C24 C28 C35 110.4(3) . . ?
C30 C29 C7 112.7(4) . . ?
C32 C31 C14 114.2(4) . . ?
C34 C33 C21 113.6(4) . . ?
C36 C35 C28 113.6(4) . . ?
O4 C41 C42 108.4(4) . . ?
O43 C42 C41 107.4(5) . . ?
O43 C44 C45 114.6(5) . . ?
O46 C45 C44 108.3(5) . . ?
O46 C47 C48 107.2(5) . . ?
O49B C48 C47 139.5(10) . . ?
O49A C48 C47 108.4(5) . . ?
C50A O49A C48 108.8(5) . . ?
O49A C50A C51 109.2(5) . . ?
C48 O49B C50B 108.6(13) . . ?
O49B C50B C51 113.9(14) . . ?
O11 C51 C50A 116.9(7) . . ?
O11 C51 C50B 98.1(10) . . ?
O18 C52 C53 108.3(4) . . ?
O54 C53 C52 115.0(4) . . ?
O54 C55 C56 112.6(5) . . ?
O57B C56 C55 125.2(7) . . ?
O57B C56 O57A 51.1(6) . . ?
C55 C56 O57A 101.3(6) . . ?
O57A C58 O57B 51.4(6) . . ?
O57A C58 C59B 121.3(10) . . ?
O57B C58 C59B 111.1(13) . . ?
O57A C58 C59A 112.8(8) . . ?
O57B C58 C59A 133.2(8) . . ?
C58 O57A C56 111.8(6) . . ?
O60A C59A C58 113.2(8) . . ?
C61A O60A C59A 119.8(10) . . ?
O60A C61A C62 115.0(9) . . ?
C56 O57B C58 109.6(7) . . ?
O60B C59B C58 96.9(9) . . ?
C61B O60B C59B 100.3(10) . . ?
O60B C61B C62 112.4(10) . . ?
O25 C62 C61B 118.1(8) . . ?
O25 C62 C61A 109.0(6) . . ?
C4 O4 C41 116.3(3) . . ?
C6 O6 C37 117.6(4) . . ?
C11 O11 C51 120.6(4) . . ?
C13 O13 C38 116.7(3) . . ?
C18 O18 C52 118.9(3) . . ?
C20 O20 C39 118.0(3) . . ?
C25 O25 C62 121.2(3) . . ?
C27 O27 C40 117.7(3) . . ?
C42 O43 C44 114.8(4) . . ?
C47 O46 C45 112.8(4) . . ?
C53 O54 C55 116.2(4) . . ?
O11A S10A C13A 109.2(6) . . ?
O11A S10A C12A 107.3(6) . . ?
C13A S10A C12A 98.6(7) . . ?
O11A S10B C12A 111.5(7) . . ?
O11A S10B C13A 111.3(8) . . ?
C12A S10B C13A 101.7(8) . . ?
S10B O11A S10A 47.5(5) . . ?
C23A S20A O21A 69.4(13) 3_675 . ?
C23A S20A S20A 73.5(11) 3_675 3_675 ?
O21A S20A S20A 99.7(7) . 3_675 ?
C23A S20A C23A 111.7(11) 3_675 . ?
O21A S20A C23A 112.9(8) . . ?
C23A S20A C22A 177.9(15) 3_675 . ?
O21A S20A C22A 111.2(8) . . ?
S20A S20A C22A 108.2(10) 3_675 . ?
C23A S20A C22A 70.1(12) . . ?

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 -0.9(6) . . . . ?
C28 C1 C2 C3 178.6(4) . . . . ?
C1 C2 C3 C4 2.5(6) . . . . ?
C1 C2 C3 C7 -178.3(4) . . . . ?
C2 C3 C4 O4 -179.4(3) . . . . ?
C7 C3 C4 O4 1.4(5) . . . . ?
C2 C3 C4 C5 -2.2(6) . . . . ?
C7 C3 C4 C5 178.5(4) . . . . ?
O4 C4 C5 C6 177.4(4) . . . . ?
C3 C4 C5 C6 0.4(7) . . . . ?
C4 C5 C6 O6 -177.4(4) . . . . ?
C4 C5 C6 C1 1.4(7) . . . . ?
C2 C1 C6 O6 177.8(4) . . . . ?
C28 C1 C6 O6 -1.8(5) . . . . ?
C2 C1 C6 C5 -1.1(6) . . . . ?
C28 C1 C6 C5 179.3(4) . . . . ?
C4 C3 C7 C8 69.4(5) . . . . ?
C2 C3 C7 C8 -109.8(4) . . . . ?
C4 C3 C7 C29 -162.5(4) . . . . ?
C2 C3 C7 C29 18.4(6) . . . . ?
C3 C7 C8 C9 33.8(5) . . . . ?
C29 C7 C8 C9 -95.9(5) . . . . ?
C3 C7 C8 C13 -144.3(4) . . . . ?
C29 C7 C8 C13 86.0(5) . . . . ?
C13 C8 C9 C10 2.4(6) . . . . ?
C7 C8 C9 C10 -175.7(4) . . . . ?
C8 C9 C10 C11 0.3(6) . . . . ?
C8 C9 C10 C14 -179.7(4) . . . . ?
C9 C10 C11 O11 177.0(4) . . . . ?
C14 C10 C11 O11 -3.0(6) . . . . ?
C9 C10 C11 C12 -2.1(6) . . . . ?
C14 C10 C11 C12 177.9(4) . . . . ?
O11 C11 C12 C13 -178.0(4) . . . . ?
C10 C11 C12 C13 1.1(7) . . . . ?
C11 C12 C13 O13 178.9(4) . . . . ?
C11 C12 C13 C8 1.8(7) . . . . ?
C9 C8 C13 O13 179.2(4) . . . . ?
C7 C8 C13 O13 -2.6(6) . . . . ?
C9 C8 C13 C12 -3.5(6) . . . . ?
C7 C8 C13 C12 174.7(4) . . . . ?
C11 C10 C14 C15 136.9(4) . . . . ?
C9 C10 C14 C15 -43.1(5) . . . . ?
C11 C10 C14 C31 -96.3(5) . . . . ?
C9 C10 C14 C31 83.7(5) . . . . ?
C10 C14 C15 C16 112.7(4) . . . . ?
C31 C14 C15 C16 -12.4(5) . . . . ?
C10 C14 C15 C20 -69.9(5) . . . . ?
C31 C14 C15 C20 165.0(4) . . . . ?
C20 C15 C16 C17 -1.3(6) . . . . ?
C14 C15 C16 C17 176.2(4) . . . . ?
C15 C16 C17 C18 1.2(6) . . . . ?
C15 C16 C17 C21 -177.2(4) . . . . ?
C16 C17 C18 O18 -178.5(3) . . . . ?
C21 C17 C18 O18 0.0(5) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
C21 C17 C18 C19 178.5(4) . . . . ?
O18 C18 C19 C20 177.3(4) . . . . ?
C17 C18 C19 C20 -1.2(6) . . . . ?
C18 C19 C20 O20 -178.3(4) . . . . ?
C18 C19 C20 C15 1.1(6) . . . . ?
C16 C15 C20 O20 179.6(3) . . . . ?
C14 C15 C20 O20 2.0(5) . . . . ?
C16 C15 C20 C19 0.0(6) . . . . ?
C14 C15 C20 C19 -177.5(4) . . . . ?
C18 C17 C21 C22 77.6(5) . . . . ?
C16 C17 C21 C22 -104.1(4) . . . . ?
C18 C17 C21 C33 -156.8(4) . . . . ?
C16 C17 C21 C33 21.6(5) . . . . ?
C17 C21 C22 C23 29.4(5) . . . . ?
C33 C21 C22 C23 -98.5(4) . . . . ?
C17 C21 C22 C27 -152.4(4) . . . . ?
C33 C21 C22 C27 79.7(4) . . . . ?
C27 C22 C23 C24 -0.8(6) . . . . ?
C21 C22 C23 C24 177.4(4) . . . . ?
C22 C23 C24 C25 0.7(6) . . . . ?
C22 C23 C24 C28 -179.4(4) . . . . ?
C23 C24 C25 O25 -179.5(4) . . . . ?
C28 C24 C25 O25 0.6(6) . . . . ?
C23 C24 C25 C26 0.2(6) . . . . ?
C28 C24 C25 C26 -179.7(4) . . . . ?
O25 C25 C26 C27 178.8(4) . . . . ?
C24 C25 C26 C27 -0.9(7) . . . . ?
C25 C26 C27 O27 -179.2(4) . . . . ?
C25 C26 C27 C22 0.7(7) . . . . ?
C23 C22 C27 C26 0.1(6) . . . . ?
C21 C22 C27 C26 -178.3(4) . . . . ?
C23 C22 C27 O27 -180.0(4) . . . . ?
C21 C22 C27 O27 1.7(6) . . . . ?
C2 C1 C28 C24 110.3(4) . . . . ?
C6 C1 C28 C24 -70.1(5) . . . . ?
C2 C1 C28 C35 -16.1(5) . . . . ?
C6 C1 C28 C35 163.4(4) . . . . ?
C23 C24 C28 C1 -26.9(5) . . . . ?
C25 C24 C28 C1 153.0(4) . . . . ?
C23 C24 C28 C35 101.6(4) . . . . ?
C25 C24 C28 C35 -78.5(5) . . . . ?
C3 C7 C29 C30 68.7(5) . . . . ?
C8 C7 C29 C30 -163.7(4) . . . . ?
C15 C14 C31 C32 -166.2(4) . . . . ?
C10 C14 C31 C32 68.1(5) . . . . ?
C22 C21 C33 C34 -167.9(3) . . . . ?
C17 C21 C33 C34 64.8(5) . . . . ?
C1 C28 C35 C36 -63.2(5) . . . . ?
C24 C28 C35 C36 169.6(3) . . . . ?
O4 C41 C42 O43 68.9(6) . . . . ?
O43 C44 C45 O46 -74.3(6) . . . . ?
O46 C47 C48 O49B 109.5(16) . . . . ?
O46 C47 C48 O49A 75.9(6) . . . . ?
O49B C48 O49A C50A 38.4(14) . . . . ?
C47 C48 O49A C50A -174.7(7) . . . . ?
C48 O49A C50A C51 -174.8(7) . . . . ?
O49A C48 O49B C50B -42(2) . . . . ?
C47 C48 O49B C50B -95(3) . . . . ?
C48 O49B C50B C51 165(2) . . . . ?
O49A C50A C51 O11 -89.1(8) . . . . ?
O49A C50A C51 C50B -48(4) . . . . ?
O49B C50B C51 O11 -174(3) . . . . ?
O49B C50B C51 C50A 42.8(18) . . . . ?
O18 C52 C53 O54 -78.6(5) . . . . ?
O54 C55 C56 O57B -43.7(10) . . . . ?
O54 C55 C56 O57A -93.6(7) . . . . ?
O57B C58 O57A C56 -45.7(7) . . . . ?
C59B C58 O57A C56 47.4(14) . . . . ?
C59A C58 O57A C56 82.2(9) . . . . ?
O57B C56 O57A C58 48.0(7) . . . . ?
C55 C56 O57A C58 174.5(6) . . . . ?
O57A C58 C59A O60A -72.4(14) . . . . ?
O57B C58 C59A O60A -14.6(19) . . . . ?
C59B C58 C59A O60A 40.5(14) . . . . ?
C58 C59A O60A C61A 177.9(9) . . . . ?
C59A O60A C61A C62 -90.6(14) . . . . ?
C55 C56 O57B C58 -118.7(9) . . . . ?
O57A C56 O57B C58 -44.0(7) . . . . ?
O57A C58 O57B C56 46.5(7) . . . . ?
C59B C58 O57B C56 -67.3(11) . . . . ?
C59A C58 O57B C56 -39.5(17) . . . . ?
O57A C58 C59B O60B 45.7(18) . . . . ?
O57B C58 C59B O60B 102.5(13) . . . . ?
C59A C58 C59B O60B -37.7(10) . . . . ?
C58 C59B O60B C61B 177.2(13) . . . . ?
C59B O60B C61B C62 154.0(16) . . . . ?
O60B C61B C62 O25 -64.5(16) . . . . ?
O60B C61B C62 C61A -136(3) . . . . ?
O60A C61A C62 O25 -62.8(12) . . . . ?
O60A C61A C62 C61B 55(2) . . . . ?
C5 C4 O4 C41 41.8(6) . . . . ?
C3 C4 O4 C41 -141.0(5) . . . . ?
C42 C41 O4 C4 167.7(4) . . . . ?
C5 C6 O6 C37 0.2(7) . . . . ?
C1 C6 O6 C37 -178.6(5) . . . . ?
C12 C11 O11 C51 -2.2(7) . . . . ?
C10 C11 O11 C51 178.7(5) . . . . ?
C50A C51 O11 C11 91.1(6) . . . . ?
C50B C51 O11 C11 75(2) . . . . ?
C12 C13 O13 C38 -8.7(7) . . . . ?
C8 C13 O13 C38 168.5(5) . . . . ?
C17 C18 O18 C52 177.3(4) . . . . ?
C19 C18 O18 C52 -1.2(6) . . . . ?
C53 C52 O18 C18 -179.1(4) . . . . ?
C19 C20 O20 C39 7.6(6) . . . . ?
C15 C20 O20 C39 -171.9(4) . . . . ?
C24 C25 O25 C62 171.2(4) . . . . ?
C26 C25 O25 C62 -8.5(7) . . . . ?
C61B C62 O25 C25 91.0(9) . . . . ?
C61A C62 O25 C25 114.0(7) . . . . ?
C26 C27 O27 C40 -5.4(6) . . . . ?
C22 C27 O27 C40 174.7(4) . . . . ?
C41 C42 O43 C44 155.7(5) . . . . ?
C45 C44 O43 C42 69.9(7) . . . . ?
C48 C47 O46 C45 -177.9(5) . . . . ?
C44 C45 O46 C47 -167.2(4) . . . . ?
C52 C53 O54 C55 70.0(6) . . . . ?
C56 C55 O54 C53 171.3(5) . . . . ?
C12A S10B O11A S10A 57.5(7) . . . . ?
C13A S10B O11A S10A -55.3(6) . . . . ?
C13A S10A O11A S10B 53.4(6) . . . . ?
C12A S10A O11A S10B -52.5(6) . . . . ?
O11A S10B C12A S10A -55.2(6) . . . . ?
C13A S10B C12A S10A 63.6(6) . . . . ?
O11A S10A C12A S10B 52.0(6) . . . . ?
C13A S10A C12A S10B -61.3(5) . . . . ?
O11A S10B C13A S10A 54.0(6) . . . . ?
C12A S10B C13A S10A -64.9(6) . . . . ?
O11A S10A C13A S10B -51.8(6) . . . . ?
C12A S10A C13A S10B 59.9(5) . . . . ?
S20A S20A O21A C23A 68.2(12) 3_675 . . 3_675 ?
C23A S20A O21A C23A 105.6(14) . . . 3_675 ?
C22A S20A O21A C23A -177.9(15) . . . 3_675 ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        66.85
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.097

#===END


