# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

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

data_yx_321
_database_code_depnum_ccdc_archive 'CCDC 998483'
_audit_update_record             
;
2014-04-20 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_audit_creation_date             2013-12-13
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C33 H34 Cl N O8'
_chemical_formula_sum            'C33 H34 Cl N O8'
_chemical_formula_weight         608.06
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'

_cell_length_a                   10.1917(6)
_cell_length_b                   13.1711(8)
_cell_length_c                   21.6852(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2910.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2190
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5400
_cell_measurement_theta_min      3.4500
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7886
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.09
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.7749
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -18.00   20.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5262  -99.0000    0.0000 38

#__ type_ start__ end____ width___ exp.time_
  2 omega  -10.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8075   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega   57.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8075   77.0000    0.0000 35

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8075  -99.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0080750000
_diffrn_orient_matrix_UB_12      -0.0403245000
_diffrn_orient_matrix_UB_13      0.0213446000
_diffrn_orient_matrix_UB_21      -0.0314922000
_diffrn_orient_matrix_UB_22      -0.0336202000
_diffrn_orient_matrix_UB_23      -0.0208402000
_diffrn_orient_matrix_UB_31      0.0615924000
_diffrn_orient_matrix_UB_32      -0.0119206000
_diffrn_orient_matrix_UB_33      -0.0133799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3512
_reflns_number_total             5091
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(13)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0582
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0567P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1535
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H20 of C20, H19 of C19, H17 of C17, H15 of C15, H14 of C14, H13 of C13, H10
  of C10, {H9A,H9B} of C9, H32 of C32, H31 of C31, H30 of C30, H29 of C29, H1A
  of C1A, H2 of C2, {H3A,H3B} of C3, {H4A,H4B} of C4
 At 1.5 times of:
  {H23A,H23B,H23C} of C23, {H22A,H22B,H22C} of C22, {H21A,H21B,H21C} of C21,
  {H24A,H24B,H24C} of C24, {H25A,H25B,H25C} of C25
2.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10), C15(H15), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C13(H13), C14(H14), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.44212(14) 0.55446(12) 0.57030(6) 0.0876(5) Uani 1 1 d . . .
O1 O 1.1402(2) 0.2149(2) 0.69441(12) 0.0483(7) Uani 1 1 d . . .
O2 O 0.9295(3) 0.0898(2) 0.74660(11) 0.0532(7) Uani 1 1 d . . .
O3 O 0.9291(3) 0.1987(2) 0.82346(12) 0.0600(8) Uani 1 1 d . . .
O4 O 0.8231(5) -0.1685(2) 0.62182(17) 0.0849(11) Uani 1 1 d . . .
O5 O 0.9332(3) 0.57803(19) 0.43006(11) 0.0518(7) Uani 1 1 d . . .
O6 O 0.7922(5) 0.5450(3) 0.35548(19) 0.1137(16) Uani 1 1 d . . .
O7 O 0.7663(3) 0.4991(2) 0.69531(13) 0.0545(7) Uani 1 1 d . . .
O8 O 0.6174(4) 0.4129(3) 0.6379(2) 0.1157(16) Uani 1 1 d . . .
N1 N 0.8539(3) 0.4121(2) 0.68711(14) 0.0471(8) Uani 1 1 d . . .
C1 C 1.0034(4) 0.4071(3) 0.50960(16) 0.0383(8) Uani 1 1 d . . .
C1A C 0.9220(6) -0.1000(3) 0.6301(2) 0.0686(13) Uani 1 1 d . . .
H1A H 1.0057 -0.1061 0.6135 0.082 Uiso 1 1 calc R . .
C2 C 0.9992(4) 0.3203(3) 0.55870(15) 0.0366(8) Uani 1 1 d . . .
H2 H 0.9064 0.3011 0.5603 0.044 Uiso 1 1 calc R . .
C3 C 1.0696(4) 0.2211(3) 0.54419(17) 0.0449(9) Uani 1 1 d . . .
H3A H 1.1593 0.2242 0.5591 0.054 Uiso 1 1 calc R . .
H3B H 1.0718 0.2105 0.4999 0.054 Uiso 1 1 calc R . .
C4 C 0.9969(4) 0.1327(3) 0.57550(17) 0.0448(9) Uani 1 1 d . . .
H4A H 1.0569 0.0760 0.5801 0.054 Uiso 1 1 calc R . .
H4B H 0.9256 0.1109 0.5490 0.054 Uiso 1 1 calc R . .
C5 C 0.9400(4) 0.1609(2) 0.64034(16) 0.0380(8) Uani 1 1 d . . .
C6 C 1.0194(3) 0.2493(3) 0.66543(16) 0.0378(8) Uani 1 1 d . . .
C7 C 1.0332(4) 0.3478(3) 0.62673(16) 0.0372(8) Uani 1 1 d . . .
C8 C 0.9339(4) 0.4299(2) 0.64309(16) 0.0380(8) Uani 1 1 d . . .
C9 C 0.9389(4) 0.5210(3) 0.60200(15) 0.0442(9) Uani 1 1 d . . .
H9A H 1.0241 0.5532 0.6061 0.053 Uiso 1 1 calc R . .
H9B H 0.8730 0.5694 0.6152 0.053 Uiso 1 1 calc R . .
C10 C 0.9152(4) 0.4939(3) 0.53330(15) 0.0405(9) Uani 1 1 d . . .
H10 H 0.8258 0.4667 0.5319 0.049 Uiso 1 1 calc R . .
C11 C 0.9092(4) 0.5948(3) 0.49635(18) 0.0455(9) Uani 1 1 d . . .
C12 C 0.8581(5) 0.5135(3) 0.3968(2) 0.0583(11) Uani 1 1 d . . .
C13 C 0.8758(4) 0.4048(3) 0.40743(17) 0.0493(10) Uani 1 1 d . . .
H13 H 0.8372 0.3613 0.3789 0.059 Uiso 1 1 calc R . .
C14 C 0.9404(4) 0.3617(3) 0.45288(17) 0.0456(9) Uani 1 1 d . . .
H14 H 0.9487 0.2916 0.4496 0.055 Uiso 1 1 calc R . .
C15 C 0.9636(4) 0.0672(3) 0.68269(17) 0.0445(9) Uani 1 1 d . . .
H15 H 1.0566 0.0486 0.6807 0.053 Uiso 1 1 calc R . .
C16 C 0.9633(4) 0.1791(3) 0.77126(18) 0.0489(10) Uani 1 1 d . . .
C17 C 1.0363(4) 0.2525(3) 0.73279(17) 0.0471(10) Uani 1 1 d . . .
H17 H 1.0501 0.3199 0.7508 0.056 Uiso 1 1 calc R . .
C18 C 0.8824(4) -0.0235(3) 0.66522(18) 0.0489(10) Uani 1 1 d . . .
C19 C 0.7508(5) -0.0454(4) 0.6820(2) 0.0647(12) Uani 1 1 d . . .
H19 H 0.6965 -0.0063 0.7070 0.078 Uiso 1 1 calc R . .
C20 C 0.7204(6) -0.1332(4) 0.6548(2) 0.0755(15) Uani 1 1 d . . .
H20 H 0.6396 -0.1656 0.6581 0.091 Uiso 1 1 calc R . .
C21 C 1.1734(4) 0.3911(3) 0.63735(19) 0.0500(10) Uani 1 1 d . . .
H21A H 1.1925 0.3914 0.6807 0.075 Uiso 1 1 calc R . .
H21B H 1.1778 0.4591 0.6217 0.075 Uiso 1 1 calc R . .
H21C H 1.2363 0.3494 0.6162 0.075 Uiso 1 1 calc R . .
C22 C 1.1455(4) 0.4397(3) 0.49329(19) 0.0528(10) Uani 1 1 d . . .
H22A H 1.1808 0.4801 0.5262 0.079 Uiso 1 1 calc R . .
H22B H 1.1447 0.4789 0.4559 0.079 Uiso 1 1 calc R . .
H22C H 1.1989 0.3804 0.4876 0.079 Uiso 1 1 calc R . .
C23 C 1.0140(5) 0.6711(3) 0.5122(2) 0.0606(12) Uani 1 1 d . . .
H23A H 1.0989 0.6410 0.5063 0.091 Uiso 1 1 calc R . .
H23B H 1.0045 0.6916 0.5544 0.091 Uiso 1 1 calc R . .
H23C H 1.0054 0.7294 0.4858 0.091 Uiso 1 1 calc R . .
C24 C 0.7736(5) 0.6423(4) 0.5025(2) 0.0708(14) Uani 1 1 d . . .
H24A H 0.7702 0.7038 0.4788 0.106 Uiso 1 1 calc R . .
H24B H 0.7566 0.6574 0.5450 0.106 Uiso 1 1 calc R . .
H24C H 0.7086 0.5956 0.4875 0.106 Uiso 1 1 calc R . .
C25 C 0.7936(4) 0.1865(3) 0.64030(18) 0.0432(9) Uani 1 1 d . . .
H25A H 0.7641 0.1959 0.6820 0.065 Uiso 1 1 calc R . .
H25B H 0.7455 0.1319 0.6216 0.065 Uiso 1 1 calc R . .
H25C H 0.7793 0.2478 0.6173 0.065 Uiso 1 1 calc R . .
C26 C 0.6464(5) 0.4846(4) 0.6690(2) 0.0614(12) Uani 1 1 d . . .
C27 C 0.5613(4) 0.5734(3) 0.6839(2) 0.0592(11) Uani 1 1 d . . .
C28 C 0.4641(4) 0.6083(4) 0.6424(2) 0.0647(13) Uani 1 1 d . . .
C29 C 0.3860(5) 0.6901(4) 0.6579(3) 0.0800(16) Uani 1 1 d . . .
H29 H 0.3222 0.7128 0.6305 0.096 Uiso 1 1 calc R . .
C30 C 0.4023(6) 0.7373(4) 0.7130(3) 0.0837(17) Uani 1 1 d . . .
H30 H 0.3485 0.7918 0.7233 0.100 Uiso 1 1 calc R . .
C31 C 0.4966(6) 0.7062(4) 0.7536(2) 0.0772(14) Uani 1 1 d . . .
H31 H 0.5075 0.7402 0.7908 0.093 Uiso 1 1 calc R . .
C32 C 0.5760(5) 0.6239(4) 0.7393(2) 0.0675(13) Uani 1 1 d . . .
H32 H 0.6396 0.6027 0.7673 0.081 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C28 1.731(5) . ?
O1 C6 1.455(4) . ?
O1 C17 1.435(4) . ?
O2 C15 1.460(4) . ?
O2 C16 1.337(5) . ?
O3 C16 1.212(5) . ?
O4 C1A 1.366(6) . ?
O4 C20 1.350(6) . ?
O5 C11 1.475(5) . ?
O5 C12 1.353(5) . ?
O6 C12 1.194(5) . ?
O7 N1 1.463(4) . ?
O7 C26 1.362(5) . ?
O8 C26 1.197(5) . ?
N1 C8 1.277(4) . ?
C1 C2 1.563(5) . ?
C1 C10 1.542(5) . ?
C1 C14 1.511(5) . ?
C1 C22 1.551(5) . ?
C1A H1A 0.9300 . ?
C1A C18 1.325(6) . ?
C2 H2 0.9800 . ?
C2 C3 1.524(5) . ?
C2 C7 1.558(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.538(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.566(5) . ?
C5 C6 1.518(5) . ?
C5 C15 1.557(5) . ?
C5 C25 1.530(5) . ?
C6 C7 1.551(5) . ?
C6 C17 1.472(5) . ?
C7 C8 1.523(5) . ?
C7 C21 1.555(5) . ?
C8 C9 1.496(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.551(5) . ?
C10 H10 0.9800 . ?
C10 C11 1.552(5) . ?
C11 C23 1.507(6) . ?
C11 C24 1.523(6) . ?
C12 C13 1.461(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.314(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9800 . ?
C15 C18 1.503(5) . ?
C16 C17 1.478(5) . ?
C17 H17 0.9800 . ?
C18 C19 1.419(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.335(6) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.492(6) . ?
C27 C28 1.415(6) . ?
C27 C32 1.382(6) . ?
C28 C29 1.380(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.358(8) . ?
C30 H30 0.9300 . ?
C30 C31 1.366(7) . ?
C31 H31 0.9300 . ?
C31 C32 1.387(6) . ?
C32 H32 0.9300 . ?

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
C17 O1 C6 61.2(2) . . ?
C16 O2 C15 119.8(3) . . ?
C20 O4 C1A 105.9(4) . . ?
C12 O5 C11 121.3(3) . . ?
C26 O7 N1 112.7(3) . . ?
C8 N1 O7 109.7(3) . . ?
C10 C1 C2 107.4(3) . . ?
C10 C1 C22 114.5(3) . . ?
C14 C1 C2 104.7(3) . . ?
C14 C1 C10 108.5(3) . . ?
C14 C1 C22 108.7(3) . . ?
C22 C1 C2 112.6(3) . . ?
O4 C1A H1A 124.7 . . ?
C18 C1A O4 110.7(5) . . ?
C18 C1A H1A 124.7 . . ?
C1 C2 H2 103.9 . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 H2 103.9 . . ?
C3 C2 C7 106.9(3) . . ?
C7 C2 C1 118.0(3) . . ?
C7 C2 H2 103.9 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 C4 109.3(3) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C3 C4 C5 113.3(3) . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C6 C5 C4 107.9(3) . . ?
C6 C5 C15 108.3(3) . . ?
C6 C5 C25 110.5(3) . . ?
C15 C5 C4 106.5(3) . . ?
C25 C5 C4 114.4(3) . . ?
C25 C5 C15 109.0(3) . . ?
O1 C6 C5 111.5(3) . . ?
O1 C6 C7 114.7(3) . . ?
O1 C6 C17 58.7(2) . . ?
C5 C6 C7 119.7(3) . . ?
C17 C6 C5 116.1(3) . . ?
C17 C6 C7 120.2(3) . . ?
C6 C7 C2 107.3(3) . . ?
C6 C7 C21 108.0(3) . . ?
C8 C7 C2 103.7(3) . . ?
C8 C7 C6 114.0(3) . . ?
C8 C7 C21 108.4(3) . . ?
C21 C7 C2 115.5(3) . . ?
N1 C8 C7 118.0(3) . . ?
N1 C8 C9 127.9(3) . . ?
C9 C8 C7 114.1(3) . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
C8 C9 C10 112.5(3) . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C1 C10 C9 113.5(3) . . ?
C1 C10 H10 105.1 . . ?
C1 C10 C11 119.0(3) . . ?
C9 C10 H10 105.1 . . ?
C9 C10 C11 107.8(3) . . ?
C11 C10 H10 105.1 . . ?
O5 C11 C10 111.6(3) . . ?
O5 C11 C23 101.7(3) . . ?
O5 C11 C24 107.3(4) . . ?
C23 C11 C10 115.2(3) . . ?
C23 C11 C24 110.4(3) . . ?
C24 C11 C10 110.0(3) . . ?
O5 C12 C13 117.5(4) . . ?
O6 C12 O5 120.0(4) . . ?
O6 C12 C13 121.9(4) . . ?
C12 C13 H13 116.4 . . ?
C14 C13 C12 127.1(4) . . ?
C14 C13 H13 116.4 . . ?
C1 C14 H14 114.6 . . ?
C13 C14 C1 130.7(3) . . ?
C13 C14 H14 114.6 . . ?
O2 C15 C5 111.2(3) . . ?
O2 C15 H15 108.8 . . ?
O2 C15 C18 105.7(3) . . ?
C5 C15 H15 108.8 . . ?
C18 C15 C5 113.4(3) . . ?
C18 C15 H15 108.8 . . ?
O2 C16 C17 118.7(4) . . ?
O3 C16 O2 119.2(4) . . ?
O3 C16 C17 122.1(4) . . ?
O1 C17 C6 60.1(2) . . ?
O1 C17 C16 118.2(3) . . ?
O1 C17 H17 116.0 . . ?
C6 C17 C16 118.9(3) . . ?
C6 C17 H17 116.0 . . ?
C16 C17 H17 116.0 . . ?
C1A C18 C15 125.5(4) . . ?
C1A C18 C19 106.3(4) . . ?
C19 C18 C15 128.1(4) . . ?
C18 C19 H19 126.8 . . ?
C20 C19 C18 106.3(5) . . ?
C20 C19 H19 126.8 . . ?
O4 C20 H20 124.7 . . ?
C19 C20 O4 110.7(5) . . ?
C19 C20 H20 124.7 . . ?
C7 C21 H21A 109.5 . . ?
C7 C21 H21B 109.5 . . ?
C7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C1 C22 H22A 109.5 . . ?
C1 C22 H22B 109.5 . . ?
C1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C11 C23 H23A 109.5 . . ?
C11 C23 H23B 109.5 . . ?
C11 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C11 C24 H24A 109.5 . . ?
C11 C24 H24B 109.5 . . ?
C11 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C5 C25 H25A 109.5 . . ?
C5 C25 H25B 109.5 . . ?
C5 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O7 C26 C27 108.7(4) . . ?
O8 C26 O7 124.7(5) . . ?
O8 C26 C27 126.6(5) . . ?
C28 C27 C26 121.6(4) . . ?
C32 C27 C26 120.2(4) . . ?
C32 C27 C28 118.2(4) . . ?
C27 C28 Cl1 122.1(4) . . ?
C29 C28 Cl1 117.7(4) . . ?
C29 C28 C27 120.2(5) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 120.1(5) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 119.5 . . ?
C29 C30 C31 121.0(5) . . ?
C31 C30 H30 119.5 . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C32 120.1(5) . . ?
C32 C31 H31 119.9 . . ?
C27 C32 C31 120.4(5) . . ?
C27 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?

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
Cl1 C28 C29 C30 -177.7(4) . . . . ?
O1 C6 C7 C2 117.5(3) . . . . ?
O1 C6 C7 C8 -128.2(3) . . . . ?
O1 C6 C7 C21 -7.6(4) . . . . ?
O1 C6 C17 C16 -107.8(4) . . . . ?
O2 C15 C18 C1A -141.8(4) . . . . ?
O2 C15 C18 C19 38.3(5) . . . . ?
O2 C16 C17 O1 -42.3(5) . . . . ?
O2 C16 C17 C6 27.2(5) . . . . ?
O3 C16 C17 O1 140.5(4) . . . . ?
O3 C16 C17 C6 -150.0(4) . . . . ?
O4 C1A C18 C15 -178.3(4) . . . . ?
O4 C1A C18 C19 1.6(5) . . . . ?
O5 C12 C13 C14 12.5(7) . . . . ?
O6 C12 C13 C14 -176.4(5) . . . . ?
O7 N1 C8 C7 -179.5(3) . . . . ?
O7 N1 C8 C9 -3.1(5) . . . . ?
O7 C26 C27 C28 147.6(4) . . . . ?
O7 C26 C27 C32 -32.5(6) . . . . ?
O8 C26 C27 C28 -30.6(8) . . . . ?
O8 C26 C27 C32 149.3(6) . . . . ?
N1 O7 C26 O8 -6.1(7) . . . . ?
N1 O7 C26 C27 175.7(3) . . . . ?
N1 C8 C9 C10 -117.9(4) . . . . ?
C1 C2 C3 C4 -148.8(3) . . . . ?
C1 C2 C7 C6 179.1(3) . . . . ?
C1 C2 C7 C8 58.1(4) . . . . ?
C1 C2 C7 C21 -60.4(4) . . . . ?
C1 C10 C11 O5 29.0(5) . . . . ?
C1 C10 C11 C23 -86.4(4) . . . . ?
C1 C10 C11 C24 148.0(4) . . . . ?
C1A O4 C20 C19 1.1(6) . . . . ?
C1A C18 C19 C20 -0.9(5) . . . . ?
C2 C1 C10 C9 46.6(4) . . . . ?
C2 C1 C10 C11 175.1(3) . . . . ?
C2 C1 C14 C13 152.1(4) . . . . ?
C2 C3 C4 C5 -36.8(4) . . . . ?
C2 C7 C8 N1 118.7(3) . . . . ?
C2 C7 C8 C9 -58.2(4) . . . . ?
C3 C2 C7 C6 -44.8(4) . . . . ?
C3 C2 C7 C8 -165.8(3) . . . . ?
C3 C2 C7 C21 75.8(4) . . . . ?
C3 C4 C5 C6 -23.8(4) . . . . ?
C3 C4 C5 C15 -139.9(3) . . . . ?
C3 C4 C5 C25 99.6(4) . . . . ?
C4 C5 C6 O1 -82.7(3) . . . . ?
C4 C5 C6 C7 55.1(4) . . . . ?
C4 C5 C6 C17 -147.4(3) . . . . ?
C4 C5 C15 O2 172.7(3) . . . . ?
C4 C5 C15 C18 -68.4(4) . . . . ?
C5 C6 C7 C2 -19.1(4) . . . . ?
C5 C6 C7 C8 95.2(4) . . . . ?
C5 C6 C7 C21 -144.2(3) . . . . ?
C5 C6 C17 O1 100.3(3) . . . . ?
C5 C6 C17 C16 -7.4(5) . . . . ?
C5 C15 C18 C1A 96.2(5) . . . . ?
C5 C15 C18 C19 -83.7(5) . . . . ?
C6 O1 C17 C16 108.9(4) . . . . ?
C6 C5 C15 O2 56.9(4) . . . . ?
C6 C5 C15 C18 175.8(3) . . . . ?
C6 C7 C8 N1 2.3(5) . . . . ?
C6 C7 C8 C9 -174.6(3) . . . . ?
C7 C2 C3 C4 75.2(4) . . . . ?
C7 C6 C17 O1 -102.2(3) . . . . ?
C7 C6 C17 C16 150.0(3) . . . . ?
C7 C8 C9 C10 58.6(4) . . . . ?
C8 C9 C10 C1 -51.4(4) . . . . ?
C8 C9 C10 C11 174.6(3) . . . . ?
C9 C10 C11 O5 160.1(3) . . . . ?
C9 C10 C11 C23 44.7(5) . . . . ?
C9 C10 C11 C24 -80.9(4) . . . . ?
C10 C1 C2 C3 175.1(3) . . . . ?
C10 C1 C2 C7 -53.8(4) . . . . ?
C10 C1 C14 C13 37.7(6) . . . . ?
C11 O5 C12 O6 116.2(5) . . . . ?
C11 O5 C12 C13 -72.6(5) . . . . ?
C12 O5 C11 C10 57.1(5) . . . . ?
C12 O5 C11 C23 -179.6(4) . . . . ?
C12 O5 C11 C24 -63.6(4) . . . . ?
C12 C13 C14 C1 6.4(8) . . . . ?
C14 C1 C2 C3 59.9(4) . . . . ?
C14 C1 C2 C7 -168.9(3) . . . . ?
C14 C1 C10 C9 159.2(3) . . . . ?
C14 C1 C10 C11 -72.3(4) . . . . ?
C15 O2 C16 O3 176.7(3) . . . . ?
C15 O2 C16 C17 -0.6(5) . . . . ?
C15 C5 C6 O1 32.2(4) . . . . ?
C15 C5 C6 C7 170.0(3) . . . . ?
C15 C5 C6 C17 -32.5(4) . . . . ?
C15 C18 C19 C20 179.0(4) . . . . ?
C16 O2 C15 C5 -42.0(5) . . . . ?
C16 O2 C15 C18 -165.4(3) . . . . ?
C17 O1 C6 C5 -108.3(3) . . . . ?
C17 O1 C6 C7 111.6(4) . . . . ?
C17 C6 C7 C2 -175.7(3) . . . . ?
C17 C6 C7 C8 -61.4(4) . . . . ?
C17 C6 C7 C21 59.2(4) . . . . ?
C18 C19 C20 O4 -0.1(6) . . . . ?
C20 O4 C1A C18 -1.7(6) . . . . ?
C21 C7 C8 N1 -118.1(4) . . . . ?
C21 C7 C8 C9 65.0(4) . . . . ?
C22 C1 C2 C3 -58.0(4) . . . . ?
C22 C1 C2 C7 73.2(4) . . . . ?
C22 C1 C10 C9 -79.2(4) . . . . ?
C22 C1 C10 C11 49.3(4) . . . . ?
C22 C1 C14 C13 -87.4(5) . . . . ?
C25 C5 C6 O1 151.5(3) . . . . ?
C25 C5 C6 C7 -70.6(4) . . . . ?
C25 C5 C6 C17 86.9(4) . . . . ?
C25 C5 C15 O2 -63.4(4) . . . . ?
C25 C5 C15 C18 55.5(4) . . . . ?
C26 O7 N1 C8 100.3(4) . . . . ?
C26 C27 C28 Cl1 -3.1(6) . . . . ?
C26 C27 C28 C29 179.3(4) . . . . ?
C26 C27 C32 C31 -179.6(5) . . . . ?
C27 C28 C29 C30 0.0(7) . . . . ?
C28 C27 C32 C31 0.3(7) . . . . ?
C28 C29 C30 C31 0.9(8) . . . . ?
C29 C30 C31 C32 -1.2(8) . . . . ?
C30 C31 C32 C27 0.5(8) . . . . ?
C32 C27 C28 Cl1 177.0(4) . . . . ?
C32 C27 C28 C29 -0.6(7) . . . . ?

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

data_yx_322
_database_code_depnum_ccdc_archive 'CCDC 998484'
_audit_update_record             
;
2014-04-20 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_audit_creation_date             2013-12-14
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C33 H34 Cl N O8'
_chemical_formula_sum            'C33 H34 Cl N O8'
_chemical_formula_weight         608.06
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'

_cell_length_a                   10.9438(4)
_cell_length_b                   14.3642(5)
_cell_length_c                   19.1003(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3002.52(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.4490
_cell_measurement_theta_min      3.6950
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.34
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8939
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.03
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.8366
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -17.00   49.00   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6512  -77.0000   90.0000 44

#__ type_ start__ end____ width___ exp.time_
  2 omega  -37.00   71.00   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6512    0.0000   30.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0254327000
_diffrn_orient_matrix_UB_12      -0.0453158000
_diffrn_orient_matrix_UB_13      -0.0022453000
_diffrn_orient_matrix_UB_21      0.0325101000
_diffrn_orient_matrix_UB_22      0.0133129000
_diffrn_orient_matrix_UB_23      -0.0305158000
_diffrn_orient_matrix_UB_31      0.0499657000
_diffrn_orient_matrix_UB_32      0.0144513000
_diffrn_orient_matrix_UB_33      0.0210297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3370
_reflns_number_total             5650
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(12)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0571
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0267P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1233
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H20 of C20, H20B of C20B, H14 of C14, {H9A,H9B} of C9, H17 of C17, H2 of C2,
   H15 of C15, H13 of C13, H19B of C19B, H19 of C19, {H4A,H4B} of C4, {H3A,H3B}
  of C3, H10 of C10, H32 of C32, H31 of C31, H29 of C29, H21 of C21, H21B of
  C21B, H33 of C33
 At 1.5 times of:
  {H26A,H26B,H26C} of C26, {H22A,H22B,H22C} of C22, {H23A,H23B,H23C} of C23,
  {H24A,H24B,H24C} of C24, {H25A,H25B,H25C} of C25
2. Uiso/Uaniso restraints and constraints
Uanis(C19) ~ Ueq, Uanis(C21B) ~ Ueq, Uanis(O4B) ~ Ueq, Uanis(C20) ~ Ueq, Uanis(C20B) ~ Ueq, Uanis(O4) ~ Ueq, Uanis(C21) ~ Ueq, Uanis(C19B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O4(0.5) O4B(0.5) C19(0.5) H19(0.5) C19B(0.5) H19B(0.5) C20(0.5)
 H20(0.5) C20B(0.5) H20B(0.5) C21(0.5) H21(0.5) C21B(0.5) H21B(0.5)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10), C15(H15), C17(H17)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C19(H19), C19B(H19B), C20(H20), C20B(H20B), C21(H21),
 C21B(H21B), C29(H29), C31(H31), C32(H32), C33(H33)
4.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.33904(16) 0.96025(9) 0.72036(7) 0.1137(5) Uani 1 1 d . . .
O1 O 0.0893(2) 0.37529(18) 0.47821(13) 0.0576(7) Uani 1 1 d . . .
O2 O 0.1969(2) 0.26159(18) 0.58868(15) 0.0643(8) Uani 1 1 d . . .
O3 O 0.3570(2) 0.3529(2) 0.57739(16) 0.0792(9) Uani 1 1 d . . .
O4 O -0.0440(8) 0.0182(6) 0.6248(5) 0.097(3) Uani 0.50 1 d PU A 1
O4B O 0.0603(10) 0.0526(10) 0.7041(7) 0.109(4) Uani 0.50 1 d PU B 2
O5 O -0.5819(3) 0.7216(2) 0.58792(18) 0.0872(10) Uani 1 1 d . . .
O6 O -0.3854(2) 0.74472(18) 0.57512(15) 0.0684(8) Uani 1 1 d . . .
O7 O 0.1497(2) 0.63617(18) 0.66488(14) 0.0620(7) Uani 1 1 d . . .
O8 O 0.2657(3) 0.5269(2) 0.71953(19) 0.0915(11) Uani 1 1 d . . .
N1 N 0.1121(3) 0.5596(2) 0.62105(16) 0.0516(8) Uani 1 1 d . . .
C1 C -0.2522(3) 0.5726(2) 0.5564(2) 0.0495(9) Uani 1 1 d . . .
C2 C -0.1641(3) 0.4870(2) 0.5609(2) 0.0472(9) Uani 1 1 d . . .
H2 H -0.1572 0.4739 0.6111 0.057 Uiso 1 1 calc R . .
C3 C -0.2059(3) 0.3953(2) 0.5288(2) 0.0559(10) Uani 1 1 d . . .
H3A H -0.1839 0.3934 0.4796 0.067 Uiso 1 1 calc R . .
H3B H -0.2940 0.3899 0.5324 0.067 Uiso 1 1 calc R . .
C4 C -0.1443(3) 0.3140(2) 0.5679(2) 0.0592(11) Uani 1 1 d . . .
H4A H -0.1454 0.2594 0.5380 0.071 Uiso 1 1 calc R . .
H4B H -0.1918 0.2998 0.6094 0.071 Uiso 1 1 calc R . .
C5 C -0.0100(3) 0.3341(2) 0.59006(19) 0.0465(9) Uani 1 1 d . . .
C6 C 0.0404(3) 0.4118(2) 0.54421(18) 0.0455(9) Uani 1 1 d . . .
C7 C -0.0296(3) 0.5047(2) 0.53644(19) 0.0448(9) Uani 1 1 d . . .
C8 C 0.0174(3) 0.5799(2) 0.5853(2) 0.0485(9) Uani 1 1 d . . .
C9 C -0.0562(3) 0.6686(2) 0.5860(2) 0.0580(11) Uani 1 1 d . . .
H9A H -0.0492 0.6989 0.5408 0.070 Uiso 1 1 calc R . .
H9B H -0.0231 0.7103 0.6212 0.070 Uiso 1 1 calc R . .
C10 C -0.1932(3) 0.6500(2) 0.6021(2) 0.0521(10) Uani 1 1 d . . .
H10 H -0.1938 0.6247 0.6497 0.063 Uiso 1 1 calc R . .
C11 C -0.2635(4) 0.7450(3) 0.6080(3) 0.0713(13) Uani 1 1 d . . .
C12 C -0.4803(4) 0.6896(3) 0.5945(2) 0.0683(12) Uani 1 1 d . . .
C13 C -0.4599(3) 0.5935(3) 0.6156(2) 0.0744(13) Uani 1 1 d . . .
H13 H -0.5176 0.5659 0.6446 0.089 Uiso 1 1 calc R . .
C14 C -0.3647(3) 0.5427(3) 0.5962(2) 0.0680(12) Uani 1 1 d . . .
H14 H -0.3677 0.4802 0.6087 0.082 Uiso 1 1 calc R . .
C15 C 0.0669(3) 0.2454(3) 0.5743(2) 0.0547(10) Uani 1 1 d . . .
H15 H 0.0580 0.2305 0.5245 0.066 Uiso 1 1 calc R . .
C16 C 0.2494(4) 0.3407(3) 0.5665(2) 0.0587(11) Uani 1 1 d . . .
C17 C 0.1730(3) 0.4096(3) 0.5297(2) 0.0546(10) Uani 1 1 d . . .
H17 H 0.2115 0.4696 0.5195 0.066 Uiso 1 1 calc R . .
C18 C 0.0355(4) 0.1604(3) 0.6156(3) 0.0724(13) Uani 1 1 d . . .
C19 C 0.0485(12) 0.1321(12) 0.6773(10) 0.089(4) Uani 0.50 1 d PU A 1
H19 H 0.0840 0.1681 0.7123 0.107 Uiso 0.50 1 calc PR A 1
C19B C -0.0645(12) 0.1011(9) 0.6218(7) 0.098(4) Uani 0.50 1 d PU B 2
H19B H -0.1339 0.1064 0.5939 0.117 Uiso 0.50 1 calc PR B 2
C20 C 0.0062(15) 0.0445(14) 0.6887(11) 0.086(6) Uani 0.50 1 d PU A 1
H20 H 0.0100 0.0099 0.7298 0.104 Uiso 0.50 1 calc PR A 1
C20B C -0.0519(14) 0.0364(11) 0.6709(8) 0.079(4) Uani 0.50 1 d PU B 2
H20B H -0.1071 -0.0109 0.6813 0.095 Uiso 0.50 1 calc PR B 2
C21 C -0.0268(9) 0.0870(7) 0.5783(6) 0.069(3) Uani 0.50 1 d PU A 1
H21 H -0.0502 0.0873 0.5315 0.082 Uiso 0.50 1 calc PR A 1
C21B C 0.1110(11) 0.1275(11) 0.6733(8) 0.080(4) Uani 0.50 1 d PU B 2
H21B H 0.1844 0.1546 0.6870 0.096 Uiso 0.50 1 calc PR B 2
C22 C -0.0170(3) 0.5388(3) 0.46015(19) 0.0575(10) Uani 1 1 d . . .
H22A H 0.0670 0.5345 0.4459 0.086 Uiso 1 1 calc R . .
H22B H -0.0435 0.6023 0.4570 0.086 Uiso 1 1 calc R . .
H22C H -0.0664 0.5007 0.4301 0.086 Uiso 1 1 calc R . .
C23 C 0.0023(4) 0.3586(3) 0.66823(19) 0.0578(10) Uani 1 1 d . . .
H23A H 0.0863 0.3721 0.6788 0.087 Uiso 1 1 calc R . .
H23B H -0.0245 0.3068 0.6961 0.087 Uiso 1 1 calc R . .
H23C H -0.0470 0.4121 0.6786 0.087 Uiso 1 1 calc R . .
C24 C -0.2865(3) 0.5998(3) 0.4814(2) 0.0599(11) Uani 1 1 d . . .
H24A H -0.2233 0.6383 0.4619 0.090 Uiso 1 1 calc R . .
H24B H -0.3621 0.6336 0.4818 0.090 Uiso 1 1 calc R . .
H24C H -0.2955 0.5447 0.4535 0.090 Uiso 1 1 calc R . .
C25 C -0.2812(5) 0.7716(4) 0.6842(3) 0.116(2) Uani 1 1 d . . .
H25A H -0.3238 0.8299 0.6869 0.174 Uiso 1 1 calc R . .
H25B H -0.2029 0.7774 0.7065 0.174 Uiso 1 1 calc R . .
H25C H -0.3280 0.7243 0.7074 0.174 Uiso 1 1 calc R . .
C26 C -0.2052(4) 0.8251(3) 0.5670(3) 0.110(2) Uani 1 1 d . . .
H26A H -0.2031 0.8097 0.5181 0.165 Uiso 1 1 calc R . .
H26B H -0.1235 0.8352 0.5836 0.165 Uiso 1 1 calc R . .
H26C H -0.2525 0.8807 0.5736 0.165 Uiso 1 1 calc R . .
C27 C 0.2389(4) 0.6068(3) 0.7108(2) 0.0646(11) Uani 1 1 d . . .
C28 C 0.3015(4) 0.6857(3) 0.7445(2) 0.0609(11) Uani 1 1 d . . .
C29 C 0.2856(4) 0.7770(3) 0.7213(2) 0.0640(11) Uani 1 1 d . . .
H29 H 0.2288 0.7908 0.6866 0.077 Uiso 1 1 calc R . .
C30 C 0.3562(4) 0.8465(3) 0.7508(2) 0.0679(12) Uani 1 1 d . . .
C31 C 0.4408(4) 0.8277(3) 0.8016(2) 0.0693(13) Uani 1 1 d . . .
H31 H 0.4892 0.8751 0.8198 0.083 Uiso 1 1 calc R . .
C32 C 0.4535(4) 0.7377(4) 0.8255(3) 0.0816(14) Uani 1 1 d . . .
H32 H 0.5092 0.7245 0.8609 0.098 Uiso 1 1 calc R . .
C33 C 0.3836(4) 0.6672(3) 0.7971(2) 0.0755(13) Uani 1 1 d . . .
H33 H 0.3922 0.6067 0.8138 0.091 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C30 1.744(4) . ?
O1 C6 1.466(4) . ?
O1 C17 1.431(4) . ?
O2 C15 1.468(4) . ?
O2 C16 1.342(5) . ?
O3 C16 1.209(5) . ?
O4 C20 1.39(2) . ?
O4 C21 1.342(13) . ?
O4B C20B 1.401(19) . ?
O4B C21B 1.35(2) . ?
O5 C12 1.210(5) . ?
O6 C11 1.474(5) . ?
O6 C12 1.357(5) . ?
O7 N1 1.443(3) . ?
O7 C27 1.379(5) . ?
O8 C27 1.195(4) . ?
N1 C8 1.275(4) . ?
C1 C2 1.565(4) . ?
C1 C10 1.554(5) . ?
C1 C14 1.510(5) . ?
C1 C24 1.531(5) . ?
C2 H2 0.9800 . ?
C2 C3 1.523(4) . ?
C2 C7 1.564(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.542(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.557(5) . ?
C5 C6 1.521(5) . ?
C5 C15 1.557(5) . ?
C5 C23 1.540(5) . ?
C6 C7 1.546(5) . ?
C6 C17 1.477(5) . ?
C7 C8 1.517(5) . ?
C7 C22 1.544(5) . ?
C8 C9 1.508(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.553(5) . ?
C10 H10 0.9800 . ?
C10 C11 1.571(5) . ?
C11 C25 1.517(7) . ?
C11 C26 1.531(6) . ?
C12 C13 1.455(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.324(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9800 . ?
C15 C18 1.494(6) . ?
C16 C17 1.474(5) . ?
C17 H17 0.9800 . ?
C18 C19 1.254(18) . ?
C18 C19B 1.391(13) . ?
C18 C21 1.444(11) . ?
C18 C21B 1.455(16) . ?
C19 H19 0.9300 . ?
C19 C20 1.36(3) . ?
C19B H19B 0.9300 . ?
C19B C20B 1.329(19) . ?
C20 H20 0.9300 . ?
C20B H20B 0.9300 . ?
C21 H21 0.9300 . ?
C21B H21B 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.472(5) . ?
C28 C29 1.395(5) . ?
C28 C33 1.375(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.382(5) . ?
C30 C31 1.369(6) . ?
C31 H31 0.9300 . ?
C31 C32 1.378(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.380(6) . ?
C33 H33 0.9300 . ?

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
C17 O1 C6 61.3(2) . . ?
C16 O2 C15 119.4(3) . . ?
C21 O4 C20 109.0(11) . . ?
C21B O4B C20B 107.3(13) . . ?
C12 O6 C11 125.3(3) . . ?
C27 O7 N1 109.7(3) . . ?
C8 N1 O7 111.6(3) . . ?
C10 C1 C2 106.0(3) . . ?
C14 C1 C2 104.5(3) . . ?
C14 C1 C10 105.0(3) . . ?
C14 C1 C24 110.1(3) . . ?
C24 C1 C2 113.8(3) . . ?
C24 C1 C10 116.4(3) . . ?
C1 C2 H2 104.6 . . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 H2 104.6 . . ?
C3 C2 C7 107.7(3) . . ?
C7 C2 C1 115.8(3) . . ?
C7 C2 H2 104.6 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 C4 109.2(3) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C3 C4 C5 113.8(3) . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C6 C5 C4 108.7(3) . . ?
C6 C5 C15 107.0(3) . . ?
C6 C5 C23 111.1(3) . . ?
C15 C5 C4 107.8(3) . . ?
C23 C5 C4 112.9(3) . . ?
C23 C5 C15 109.1(3) . . ?
O1 C6 C5 111.4(3) . . ?
O1 C6 C7 114.0(3) . . ?
O1 C6 C17 58.2(2) . . ?
C5 C6 C7 120.6(3) . . ?
C17 C6 C5 116.6(3) . . ?
C17 C6 C7 119.1(3) . . ?
C6 C7 C2 107.3(3) . . ?
C8 C7 C2 104.6(3) . . ?
C8 C7 C6 112.8(3) . . ?
C8 C7 C22 108.9(3) . . ?
C22 C7 C2 114.7(3) . . ?
C22 C7 C6 108.7(3) . . ?
N1 C8 C7 116.3(3) . . ?
N1 C8 C9 128.5(3) . . ?
C9 C8 C7 115.2(3) . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C8 C9 C10 111.9(3) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C1 C10 H10 104.7 . . ?
C1 C10 C11 117.3(3) . . ?
C9 C10 C1 114.3(3) . . ?
C9 C10 H10 104.7 . . ?
C9 C10 C11 109.8(3) . . ?
C11 C10 H10 104.7 . . ?
O6 C11 C10 114.2(3) . . ?
O6 C11 C25 107.1(4) . . ?
O6 C11 C26 99.3(3) . . ?
C25 C11 C10 110.5(4) . . ?
C25 C11 C26 110.8(4) . . ?
C26 C11 C10 114.3(3) . . ?
O5 C12 O6 116.9(4) . . ?
O5 C12 C13 122.1(4) . . ?
O6 C12 C13 120.7(4) . . ?
C12 C13 H13 117.7 . . ?
C14 C13 C12 124.5(4) . . ?
C14 C13 H13 117.7 . . ?
C1 C14 H14 115.6 . . ?
C13 C14 C1 128.7(4) . . ?
C13 C14 H14 115.6 . . ?
O2 C15 C5 110.9(3) . . ?
O2 C15 H15 108.2 . . ?
O2 C15 C18 104.7(3) . . ?
C5 C15 H15 108.2 . . ?
C18 C15 C5 116.3(3) . . ?
C18 C15 H15 108.2 . . ?
O2 C16 C17 118.4(3) . . ?
O3 C16 O2 119.1(4) . . ?
O3 C16 C17 122.5(4) . . ?
O1 C17 C6 60.5(2) . . ?
O1 C17 C16 117.3(3) . . ?
O1 C17 H17 116.2 . . ?
C6 C17 H17 116.2 . . ?
C16 C17 C6 118.8(3) . . ?
C16 C17 H17 116.2 . . ?
C19 C18 C15 137.3(9) . . ?
C19 C18 C19B 79.2(9) . . ?
C19 C18 C21 106.4(10) . . ?
C19 C18 C21B 28.3(7) . . ?
C19B C18 C15 136.4(7) . . ?
C19B C18 C21 39.1(6) . . ?
C19B C18 C21B 100.7(8) . . ?
C21 C18 C15 116.3(6) . . ?
C21 C18 C21B 113.9(8) . . ?
C21B C18 C15 122.3(7) . . ?
C18 C19 H19 122.9 . . ?
C18 C19 C20 114.3(16) . . ?
C20 C19 H19 122.9 . . ?
C18 C19B H19B 123.0 . . ?
C20B C19B C18 113.9(11) . . ?
C20B C19B H19B 123.0 . . ?
O4 C20 H20 127.9 . . ?
C19 C20 O4 104.3(16) . . ?
C19 C20 H20 127.9 . . ?
O4B C20B H20B 126.5 . . ?
C19B C20B O4B 107.1(14) . . ?
C19B C20B H20B 126.5 . . ?
O4 C21 C18 106.0(8) . . ?
O4 C21 H21 127.0 . . ?
C18 C21 H21 127.0 . . ?
O4B C21B C18 110.8(10) . . ?
O4B C21B H21B 124.6 . . ?
C18 C21B H21B 124.6 . . ?
C7 C22 H22A 109.5 . . ?
C7 C22 H22B 109.5 . . ?
C7 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C5 C23 H23A 109.5 . . ?
C5 C23 H23B 109.5 . . ?
C5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1 C24 H24A 109.5 . . ?
C1 C24 H24B 109.5 . . ?
C1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C11 C25 H25A 109.5 . . ?
C11 C25 H25B 109.5 . . ?
C11 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C11 C26 H26A 109.5 . . ?
C11 C26 H26B 109.5 . . ?
C11 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O7 C27 C28 111.8(4) . . ?
O8 C27 O7 123.8(4) . . ?
O8 C27 C28 124.4(4) . . ?
C29 C28 C27 121.8(4) . . ?
C33 C28 C27 118.3(4) . . ?
C33 C28 C29 119.7(4) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 C28 118.7(4) . . ?
C30 C29 H29 120.7 . . ?
C29 C30 Cl1 118.7(4) . . ?
C31 C30 Cl1 119.6(3) . . ?
C31 C30 C29 121.6(4) . . ?
C30 C31 H31 120.4 . . ?
C30 C31 C32 119.2(4) . . ?
C32 C31 H31 120.4 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.2(4) . . ?
C33 C32 H32 119.9 . . ?
C28 C33 C32 120.5(4) . . ?
C28 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?

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
Cl1 C30 C31 C32 179.8(4) . . . . ?
O1 C6 C7 C2 118.8(3) . . . . ?
O1 C6 C7 C8 -126.6(3) . . . . ?
O1 C6 C7 C22 -5.7(4) . . . . ?
O1 C6 C17 C16 -106.9(4) . . . . ?
O2 C15 C18 C19 50.1(12) . . . . ?
O2 C15 C18 C19B -172.2(9) . . . . ?
O2 C15 C18 C21 -129.7(6) . . . . ?
O2 C15 C18 C21B 18.3(8) . . . . ?
O2 C16 C17 O1 -43.5(5) . . . . ?
O2 C16 C17 C6 26.2(5) . . . . ?
O3 C16 C17 O1 136.7(4) . . . . ?
O3 C16 C17 C6 -153.7(4) . . . . ?
O5 C12 C13 C14 149.6(5) . . . . ?
O6 C12 C13 C14 -24.2(7) . . . . ?
O7 N1 C8 C7 179.3(3) . . . . ?
O7 N1 C8 C9 -2.0(5) . . . . ?
O7 C27 C28 C29 -11.3(6) . . . . ?
O7 C27 C28 C33 173.1(4) . . . . ?
O8 C27 C28 C29 165.5(5) . . . . ?
O8 C27 C28 C33 -10.1(7) . . . . ?
N1 O7 C27 O8 -10.7(6) . . . . ?
N1 O7 C27 C28 166.0(3) . . . . ?
N1 C8 C9 C10 -124.1(4) . . . . ?
C1 C2 C3 C4 -152.2(3) . . . . ?
C1 C2 C7 C6 -179.3(3) . . . . ?
C1 C2 C7 C8 60.7(4) . . . . ?
C1 C2 C7 C22 -58.5(4) . . . . ?
C1 C10 C11 O6 6.6(5) . . . . ?
C1 C10 C11 C25 127.4(4) . . . . ?
C1 C10 C11 C26 -106.9(4) . . . . ?
C2 C1 C10 C9 50.0(4) . . . . ?
C2 C1 C10 C11 -179.3(3) . . . . ?
C2 C1 C14 C13 170.4(5) . . . . ?
C2 C3 C4 C5 -37.4(4) . . . . ?
C2 C7 C8 N1 121.7(3) . . . . ?
C2 C7 C8 C9 -57.2(4) . . . . ?
C3 C2 C7 C6 -44.5(4) . . . . ?
C3 C2 C7 C8 -164.5(3) . . . . ?
C3 C2 C7 C22 76.3(4) . . . . ?
C3 C4 C5 C6 -21.5(4) . . . . ?
C3 C4 C5 C15 -137.2(3) . . . . ?
C3 C4 C5 C23 102.2(4) . . . . ?
C4 C5 C6 O1 -85.2(3) . . . . ?
C4 C5 C6 C7 52.4(4) . . . . ?
C4 C5 C6 C17 -149.4(3) . . . . ?
C4 C5 C15 O2 175.5(3) . . . . ?
C4 C5 C15 C18 -65.1(4) . . . . ?
C5 C6 C7 C2 -17.8(4) . . . . ?
C5 C6 C7 C8 96.8(4) . . . . ?
C5 C6 C7 C22 -142.3(3) . . . . ?
C5 C6 C17 O1 99.8(3) . . . . ?
C5 C6 C17 C16 -7.1(5) . . . . ?
C5 C15 C18 C19 -72.7(12) . . . . ?
C5 C15 C18 C19B 65.0(11) . . . . ?
C5 C15 C18 C21 107.5(6) . . . . ?
C5 C15 C18 C21B -104.5(8) . . . . ?
C6 O1 C17 C16 109.3(4) . . . . ?
C6 C5 C15 O2 58.6(4) . . . . ?
C6 C5 C15 C18 178.1(3) . . . . ?
C6 C7 C8 N1 5.5(5) . . . . ?
C6 C7 C8 C9 -173.4(3) . . . . ?
C7 C2 C3 C4 74.3(4) . . . . ?
C7 C6 C17 O1 -101.7(3) . . . . ?
C7 C6 C17 C16 151.4(3) . . . . ?
C7 C8 C9 C10 54.6(5) . . . . ?
C8 C9 C10 C1 -50.2(4) . . . . ?
C8 C9 C10 C11 175.6(3) . . . . ?
C9 C10 C11 O6 139.3(4) . . . . ?
C9 C10 C11 C25 -99.9(5) . . . . ?
C9 C10 C11 C26 25.9(5) . . . . ?
C10 C1 C2 C3 172.2(3) . . . . ?
C10 C1 C2 C7 -58.0(4) . . . . ?
C10 C1 C14 C13 59.1(6) . . . . ?
C11 O6 C12 O5 147.4(4) . . . . ?
C11 O6 C12 C13 -38.5(6) . . . . ?
C12 O6 C11 C10 62.0(5) . . . . ?
C12 O6 C11 C25 -60.6(5) . . . . ?
C12 O6 C11 C26 -175.9(4) . . . . ?
C12 C13 C14 C1 7.3(8) . . . . ?
C14 C1 C2 C3 61.5(4) . . . . ?
C14 C1 C2 C7 -168.6(3) . . . . ?
C14 C1 C10 C9 160.4(3) . . . . ?
C14 C1 C10 C11 -69.0(4) . . . . ?
C15 O2 C16 O3 -178.7(4) . . . . ?
C15 O2 C16 C17 1.5(5) . . . . ?
C15 C5 C6 O1 30.9(4) . . . . ?
C15 C5 C6 C7 168.6(3) . . . . ?
C15 C5 C6 C17 -33.2(4) . . . . ?
C15 C18 C19 C20 -177.6(10) . . . . ?
C15 C18 C19B C20B -175.4(9) . . . . ?
C15 C18 C21 O4 179.2(6) . . . . ?
C15 C18 C21B O4B 177.1(9) . . . . ?
C16 O2 C15 C5 -45.0(5) . . . . ?
C16 O2 C15 C18 -171.1(3) . . . . ?
C17 O1 C6 C5 -108.9(3) . . . . ?
C17 O1 C6 C7 110.5(3) . . . . ?
C17 C6 C7 C2 -175.5(3) . . . . ?
C17 C6 C7 C8 -60.9(4) . . . . ?
C17 C6 C7 C22 60.0(4) . . . . ?
C18 C19 C20 O4 -2.8(19) . . . . ?
C18 C19B C20B O4B 2.9(17) . . . . ?
C19 C18 C19B C20B -23.1(14) . . . . ?
C19 C18 C21 O4 -0.7(11) . . . . ?
C19 C18 C21B O4B 46(2) . . . . ?
C19B C18 C19 C20 30.6(13) . . . . ?
C19B C18 C21 O4 -48.5(10) . . . . ?
C19B C18 C21B O4B 4.4(14) . . . . ?
C20 O4 C21 C18 -1.0(13) . . . . ?
C20B O4B C21B C18 -3.0(16) . . . . ?
C21 O4 C20 C19 2.2(17) . . . . ?
C21 C18 C19 C20 2.2(15) . . . . ?
C21 C18 C19B C20B 110.5(17) . . . . ?
C21 C18 C21B O4B -34.2(14) . . . . ?
C21B O4B C20B C19B 0.2(17) . . . . ?
C21B C18 C19 C20 -108(3) . . . . ?
C21B C18 C19B C20B -4.5(15) . . . . ?
C21B C18 C21 O4 28.5(11) . . . . ?
C22 C7 C8 N1 -115.3(4) . . . . ?
C22 C7 C8 C9 65.9(4) . . . . ?
C23 C5 C6 O1 150.0(3) . . . . ?
C23 C5 C6 C7 -72.4(4) . . . . ?
C23 C5 C6 C17 85.8(4) . . . . ?
C23 C5 C15 O2 -61.6(4) . . . . ?
C23 C5 C15 C18 57.8(4) . . . . ?
C24 C1 C2 C3 -58.6(4) . . . . ?
C24 C1 C2 C7 71.2(4) . . . . ?
C24 C1 C10 C9 -77.6(4) . . . . ?
C24 C1 C10 C11 53.0(5) . . . . ?
C24 C1 C14 C13 -67.0(6) . . . . ?
C27 O7 N1 C8 170.1(3) . . . . ?
C27 C28 C29 C30 -173.8(4) . . . . ?
C27 C28 C33 C32 173.5(4) . . . . ?
C28 C29 C30 Cl1 178.5(3) . . . . ?
C28 C29 C30 C31 0.3(6) . . . . ?
C29 C28 C33 C32 -2.2(7) . . . . ?
C29 C30 C31 C32 -2.1(6) . . . . ?
C30 C31 C32 C33 1.7(7) . . . . ?
C31 C32 C33 C28 0.5(7) . . . . ?
C33 C28 C29 C30 1.8(6) . . . . ?

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

data_yx_324
_database_code_depnum_ccdc_archive 'CCDC 998485'
_audit_update_record             
;
2014-04-20 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_audit_creation_date             2013-12-14
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C34 H37 N O8'
_chemical_formula_sum            'C34 H37 N O8'
_chemical_formula_weight         587.65
_chemical_absolute_configuration unk
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'

_cell_length_a                   10.7476(9)
_cell_length_b                   14.2825(12)
_cell_length_c                   19.7165(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3026.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.0190
_cell_measurement_theta_min      3.4230
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12084
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.03
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.8221
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -38.00  -11.00   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5262   57.0000  -30.0000 18

#__ type_ start__ end____ width___ exp.time_
  2 omega   27.00   54.00   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5262   38.0000 -180.0000 18

#__ type_ start__ end____ width___ exp.time_
  3 omega  -18.00   12.00   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5262  -99.0000  120.0000 20

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   11.50   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5262   38.0000 -180.0000 41

#__ type_ start__ end____ width___ exp.time_
  5 omega   24.00   96.00   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8075   77.0000   30.0000 48

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00   17.50   1.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8075  -99.0000  -90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0638008000
_diffrn_orient_matrix_UB_12      0.0025093000
_diffrn_orient_matrix_UB_13      0.0091255000
_diffrn_orient_matrix_UB_21      -0.0155859000
_diffrn_orient_matrix_UB_22      -0.0287682000
_diffrn_orient_matrix_UB_23      -0.0281227000
_diffrn_orient_matrix_UB_31      0.0070854000
_diffrn_orient_matrix_UB_32      -0.0404918000
_diffrn_orient_matrix_UB_33      0.0205297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3176
_reflns_number_total             5521
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max         0.154
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.5(17)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5521
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0603
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0358P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1435
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H29 of C29, H32 of C32, H31 of C31, H33 of C33, {H13A,H13B} of C13, H15 of
  C15, H3 of C3, H4 of C4, H2 of C2, H1A of C1A, {H11A,H11B} of C11, H10 of C10,
   {H9A,H9B} of C9, H20 of C20, H19B of C19B, H19 of C19, H20B of C20B, H21B of
  C21B, H21 of C21
 At 1.5 times of:
  {H34A,H34B,H34C} of C34, {H25A,H25B,H25C} of C25, {H24A,H24B,H24C} of C24,
  {H23A,H23B,H23C} of C23, {H22A,H22B,H22C} of C22
2. Restrained distances
 C20B-C19B
 1.4 with sigma of 0.02
 H26A-C26
 0.94 with sigma of 0.01
 H26B-C26
 0.94 with sigma of 0.01
 H26C-C26
 0.94 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C21) ~ Ueq, Uanis(C19B) ~ Ueq, Uanis(O4) ~ Ueq, Uanis(C20B) ~ Ueq, Uanis(C20) ~ Ueq, Uanis(O20B) ~ Ueq, Uanis(C19) ~ Ueq, Uanis(C21B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O4(0.6) O20B(0.4) C19(0.6) H19(0.6) C19B(0.4) H19B(0.4) C20(0.6)
 H20(0.6) C20B(0.4) H20B(0.4) C21(0.6) H21(0.6) C21B(0.4) H21B(0.4)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C10(H10), C15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C3(H3), C19(H19), C19B(H19B), C20(H20), C20B(H20B), C21(H21),
 C21B(H21B), C29(H29), C31(H31), C32(H32), C33(H33)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.4118(3) -0.62665(18) -0.51758(13) 0.0560(8) Uani 1 1 d . . .
O2 O -0.2916(3) -0.7394(2) -0.41402(15) 0.0618(8) Uani 1 1 d . . .
O3 O -0.1303(3) -0.6478(2) -0.43177(17) 0.0764(10) Uani 1 1 d . . .
O4 O -0.4121(8) -0.9504(6) -0.2979(5) 0.093(3) Uani 0.60 1 d PU A 1
O5 O -1.0886(3) -0.2791(2) -0.41915(18) 0.0824(10) Uani 1 1 d . . .
O6 O -0.8883(3) -0.25373(19) -0.42280(16) 0.0670(9) Uani 1 1 d . . .
O7 O -0.3463(3) -0.36628(18) -0.33272(15) 0.0596(8) Uani 1 1 d . . .
O8 O -0.2383(3) -0.4779(2) -0.27611(18) 0.0818(10) Uani 1 1 d . . .
O20B O -0.5385(15) -0.9826(10) -0.3655(8) 0.126(5) Uani 0.40 1 d PU B 2
N1 N -0.3839(3) -0.4423(2) -0.37604(17) 0.0512(9) Uani 1 1 d . . .
C1 C -0.7545(4) -0.4283(3) -0.4380(2) 0.0481(10) Uani 1 1 d . . .
C1A C -0.9666(4) -0.4047(3) -0.3829(2) 0.0701(14) Uani 1 1 d . . .
H1A H -1.0267 -0.4303 -0.3544 0.084 Uiso 1 1 calc R . .
C2 C -0.6643(3) -0.5143(2) -0.4339(2) 0.0458(10) Uani 1 1 d . . .
H2 H -0.6558 -0.5268 -0.3852 0.055 Uiso 1 1 calc R . .
C3 C -0.8699(4) -0.4575(3) -0.3989(2) 0.0656(13) Uani 1 1 d . . .
H3 H -0.8729 -0.5195 -0.3846 0.079 Uiso 1 1 calc R . .
C4 C -0.3224(4) -0.5902(3) -0.4699(2) 0.0522(11) Uani 1 1 d . . .
H4 H -0.2846 -0.5297 -0.4809 0.063 Uiso 1 1 calc R . .
C5 C -0.5032(4) -0.6682(2) -0.40714(19) 0.0457(10) Uani 1 1 d . . .
C6 C -0.4557(4) -0.5897(3) -0.45288(18) 0.0459(10) Uani 1 1 d . . .
C7 C -0.5283(4) -0.4961(3) -0.45882(19) 0.0441(9) Uani 1 1 d . . .
C8 C -0.4794(4) -0.4212(3) -0.4112(2) 0.0466(10) Uani 1 1 d . . .
C9 C -0.5538(4) -0.3311(3) -0.4101(2) 0.0563(11) Uani 1 1 d . . .
H9A H -0.5469 -0.3005 -0.4539 0.068 Uiso 1 1 calc R . .
H9B H -0.5194 -0.2894 -0.3761 0.068 Uiso 1 1 calc R . .
C10 C -0.6935(4) -0.3496(3) -0.3941(2) 0.0509(11) Uani 1 1 d . . .
H10 H -0.6935 -0.3747 -0.3478 0.061 Uiso 1 1 calc R . .
C11 C -0.6420(4) -0.6885(3) -0.4256(2) 0.0578(12) Uani 1 1 d . . .
H11A H -0.6456 -0.7446 -0.4532 0.069 Uiso 1 1 calc R . .
H11B H -0.6878 -0.7008 -0.3842 0.069 Uiso 1 1 calc R . .
C12 C -0.9857(5) -0.3082(3) -0.4070(2) 0.0657(13) Uani 1 1 d . . .
C13 C -0.7069(4) -0.6078(3) -0.4643(2) 0.0562(11) Uani 1 1 d . . .
H13A H -0.6853 -0.6104 -0.5120 0.067 Uiso 1 1 calc R . .
H13B H -0.7965 -0.6137 -0.4602 0.067 Uiso 1 1 calc R . .
C14 C -0.7653(4) -0.2547(3) -0.3885(3) 0.0664(13) Uani 1 1 d . . .
C15 C -0.4253(4) -0.7566(3) -0.4234(2) 0.0540(11) Uani 1 1 d . . .
H15 H -0.4395 -0.7735 -0.4709 0.065 Uiso 1 1 calc R . .
C16 C -0.2411(4) -0.6605(3) -0.4374(2) 0.0579(11) Uani 1 1 d . . .
C18 C -0.4521(5) -0.8412(3) -0.3802(3) 0.0702(14) Uani 1 1 d . . .
C19 C -0.5552(12) -0.8980(8) -0.3709(6) 0.086(3) Uani 0.60 1 d PU A 1
H19 H -0.6310 -0.8908 -0.3931 0.103 Uiso 0.60 1 calc PR A 1
C19B C -0.4261(18) -0.8688(13) -0.3212(11) 0.089(6) Uani 0.40 1 d PDU B 2
H19B H -0.3796 -0.8337 -0.2906 0.106 Uiso 0.40 1 calc PR B 2
C20 C -0.5293(15) -0.9657(10) -0.3245(6) 0.077(4) Uani 0.60 1 d PU A 1
H20 H -0.5821 -1.0145 -0.3125 0.093 Uiso 0.60 1 calc PR A 1
C20B C -0.473(2) -0.9560(15) -0.3065(15) 0.080(7) Uani 0.40 1 d PDU B 2
H20B H -0.4643 -0.9899 -0.2665 0.096 Uiso 0.40 1 calc PR B 2
C21 C -0.3627(10) -0.8766(8) -0.3316(7) 0.079(3) Uani 0.60 1 d PU A 1
H21 H -0.2834 -0.8523 -0.3246 0.094 Uiso 0.60 1 calc PR A 1
C21B C -0.5279(15) -0.9136(10) -0.4107(9) 0.080(4) Uani 0.40 1 d PU B 2
H21B H -0.5628 -0.9123 -0.4539 0.096 Uiso 0.40 1 calc PR B 2
C22 C -0.7903(4) -0.4014(3) -0.5113(2) 0.0591(11) Uani 1 1 d . . .
H22A H -0.7333 -0.3551 -0.5280 0.089 Uiso 1 1 calc R . .
H22B H -0.8733 -0.3765 -0.5118 0.089 Uiso 1 1 calc R . .
H22C H -0.7866 -0.4560 -0.5397 0.089 Uiso 1 1 calc R . .
C23 C -0.5176(4) -0.4609(3) -0.5324(2) 0.0594(12) Uani 1 1 d . . .
H23A H -0.5481 -0.3978 -0.5351 0.089 Uiso 1 1 calc R . .
H23B H -0.5661 -0.5004 -0.5616 0.089 Uiso 1 1 calc R . .
H23C H -0.4321 -0.4626 -0.5464 0.089 Uiso 1 1 calc R . .
C24 C -0.4884(4) -0.6427(3) -0.33096(19) 0.0584(11) Uani 1 1 d . . .
H24A H -0.4021 -0.6321 -0.3210 0.088 Uiso 1 1 calc R . .
H24B H -0.5189 -0.6933 -0.3035 0.088 Uiso 1 1 calc R . .
H24C H -0.5351 -0.5870 -0.3212 0.088 Uiso 1 1 calc R . .
C25 C -0.7887(6) -0.2307(4) -0.3136(3) 0.103(2) Uani 1 1 d . . .
H25A H -0.8308 -0.1716 -0.3106 0.154 Uiso 1 1 calc R . .
H25B H -0.7106 -0.2270 -0.2901 0.154 Uiso 1 1 calc R . .
H25C H -0.8392 -0.2786 -0.2934 0.154 Uiso 1 1 calc R . .
C26 C -0.7034(6) -0.1729(4) -0.4250(5) 0.094(2) Uani 1 1 d D . .
C27 C -0.2596(4) -0.3972(3) -0.2861(2) 0.0585(11) Uani 1 1 d . . .
C28 C -0.1963(4) -0.3177(3) -0.2524(2) 0.0535(11) Uani 1 1 d . . .
C29 C -0.2003(4) -0.2273(3) -0.2784(2) 0.0573(11) Uani 1 1 d . . .
H29 H -0.2523 -0.2142 -0.3149 0.069 Uiso 1 1 calc R . .
C30 C -0.1278(4) -0.1561(3) -0.2509(2) 0.0576(11) Uani 1 1 d . . .
C31 C -0.0523(4) -0.1783(3) -0.1966(2) 0.0641(12) Uani 1 1 d . . .
H31 H -0.0013 -0.1322 -0.1784 0.077 Uiso 1 1 calc R . .
C32 C -0.0499(5) -0.2673(3) -0.1684(2) 0.0673(13) Uani 1 1 d . . .
H32 H -0.0001 -0.2799 -0.1309 0.081 Uiso 1 1 calc R . .
C33 C -0.1225(4) -0.3372(3) -0.1966(2) 0.0662(13) Uani 1 1 d . . .
H33 H -0.1218 -0.3971 -0.1781 0.079 Uiso 1 1 calc R . .
C34 C -0.1263(6) -0.0590(3) -0.2818(2) 0.0942(19) Uani 1 1 d . . .
H34A H -0.1402 -0.0636 -0.3298 0.141 Uiso 1 1 calc R . .
H34B H -0.0470 -0.0302 -0.2736 0.141 Uiso 1 1 calc R . .
H34C H -0.1907 -0.0217 -0.2617 0.141 Uiso 1 1 calc R . .
H26A H -0.624(2) -0.158(4) -0.408(3) 0.11(2) Uiso 1 1 d D . .
H26B H -0.754(4) -0.120(2) -0.418(3) 0.12(2) Uiso 1 1 d D . .
H26C H -0.693(7) -0.191(4) -0.4705(12) 0.15(3) Uiso 1 1 d 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
O1 C4 1.442(5) . ?
O1 C6 1.459(4) . ?
O2 C15 1.469(5) . ?
O2 C16 1.333(5) . ?
O3 C16 1.210(5) . ?
O4 C20 1.382(17) . ?
O4 C21 1.356(13) . ?
O5 C12 1.206(5) . ?
O6 C12 1.341(5) . ?
O6 C14 1.485(5) . ?
O7 N1 1.439(4) . ?
O7 C27 1.382(5) . ?
O8 C27 1.192(5) . ?
O20B C20B 1.41(3) . ?
O20B C21B 1.33(2) . ?
N1 C8 1.275(5) . ?
C1 C2 1.566(5) . ?
C1 C3 1.518(5) . ?
C1 C10 1.564(5) . ?
C1 C22 1.545(5) . ?
C1A H1A 0.9300 . ?
C1A C3 1.323(5) . ?
C1A C12 1.473(6) . ?
C2 H2 0.9800 . ?
C2 C7 1.564(5) . ?
C2 C13 1.534(5) . ?
C3 H3 0.9300 . ?
C4 H4 0.9800 . ?
C4 C6 1.471(5) . ?
C4 C16 1.477(6) . ?
C5 C6 1.527(5) . ?
C5 C11 1.563(5) . ?
C5 C15 1.549(5) . ?
C5 C24 1.554(5) . ?
C6 C7 1.552(5) . ?
C7 C8 1.516(5) . ?
C7 C23 1.540(5) . ?
C8 C9 1.516(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.557(5) . ?
C10 H10 0.9800 . ?
C10 C14 1.563(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C13 1.548(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C25 1.535(7) . ?
C14 C26 1.525(8) . ?
C15 H15 0.9800 . ?
C15 C18 1.505(6) . ?
C18 C19 1.385(13) . ?
C18 C19B 1.26(2) . ?
C18 C21 1.448(12) . ?
C18 C21B 1.447(17) . ?
C19 H19 0.9300 . ?
C19 C20 1.360(16) . ?
C19B H19B 0.9300 . ?
C19B C20B 1.377(18) . ?
C20 H20 0.9300 . ?
C20B H20B 0.9300 . ?
C21 H21 0.9300 . ?
C21B H21B 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.941(10) . ?
C26 H26B 0.944(10) . ?
C26 H26C 0.943(10) . ?
C27 C28 1.481(6) . ?
C28 C29 1.389(6) . ?
C28 C33 1.384(6) . ?
C29 H29 0.9300 . ?
C29 C30 1.392(5) . ?
C30 C31 1.380(6) . ?
C30 C34 1.515(6) . ?
C31 H31 0.9300 . ?
C31 C32 1.388(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.384(6) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 O1 C6 61.0(2) . . ?
C16 O2 C15 119.8(3) . . ?
C21 O4 C20 107.1(10) . . ?
C12 O6 C14 125.7(3) . . ?
C27 O7 N1 110.1(3) . . ?
C21B O20B C20B 108.1(16) . . ?
C8 N1 O7 111.8(3) . . ?
C3 C1 C2 105.3(3) . . ?
C3 C1 C10 105.0(3) . . ?
C3 C1 C22 109.9(3) . . ?
C10 C1 C2 106.0(3) . . ?
C22 C1 C2 113.4(3) . . ?
C22 C1 C10 116.3(3) . . ?
C3 C1A H1A 117.8 . . ?
C3 C1A C12 124.4(4) . . ?
C12 C1A H1A 117.8 . . ?
C1 C2 H2 104.6 . . ?
C7 C2 C1 115.6(3) . . ?
C7 C2 H2 104.6 . . ?
C13 C2 C1 118.5(3) . . ?
C13 C2 H2 104.6 . . ?
C13 C2 C7 107.5(3) . . ?
C1 C3 H3 116.3 . . ?
C1A C3 C1 127.4(4) . . ?
C1A C3 H3 116.3 . . ?
O1 C4 H4 116.8 . . ?
O1 C4 C6 60.1(2) . . ?
O1 C4 C16 115.6(3) . . ?
C6 C4 H4 116.8 . . ?
C6 C4 C16 118.8(4) . . ?
C16 C4 H4 116.8 . . ?
C6 C5 C11 108.5(3) . . ?
C6 C5 C15 107.2(3) . . ?
C6 C5 C24 111.4(3) . . ?
C15 C5 C11 108.5(3) . . ?
C15 C5 C24 109.6(3) . . ?
C24 C5 C11 111.5(4) . . ?
O1 C6 C4 58.9(2) . . ?
O1 C6 C5 111.0(3) . . ?
O1 C6 C7 114.1(3) . . ?
C4 C6 C5 117.1(4) . . ?
C4 C6 C7 118.5(4) . . ?
C5 C6 C7 120.6(3) . . ?
C6 C7 C2 107.6(3) . . ?
C8 C7 C2 104.3(3) . . ?
C8 C7 C6 112.7(3) . . ?
C8 C7 C23 109.1(3) . . ?
C23 C7 C2 114.8(3) . . ?
C23 C7 C6 108.3(3) . . ?
N1 C8 C7 116.7(3) . . ?
N1 C8 C9 128.1(4) . . ?
C9 C8 C7 115.1(3) . . ?
C8 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C8 C9 C10 111.6(3) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
C1 C10 H10 104.6 . . ?
C9 C10 C1 114.4(3) . . ?
C9 C10 H10 104.6 . . ?
C9 C10 C14 110.1(3) . . ?
C14 C10 C1 117.1(3) . . ?
C14 C10 H10 104.6 . . ?
C5 C11 H11A 108.8 . . ?
C5 C11 H11B 108.8 . . ?
H11A C11 H11B 107.6 . . ?
C13 C11 C5 114.0(3) . . ?
C13 C11 H11A 108.8 . . ?
C13 C11 H11B 108.8 . . ?
O5 C12 O6 118.0(4) . . ?
O5 C12 C1A 121.0(5) . . ?
O6 C12 C1A 120.6(4) . . ?
C2 C13 C11 108.8(3) . . ?
C2 C13 H13A 109.9 . . ?
C2 C13 H13B 109.9 . . ?
C11 C13 H13A 109.9 . . ?
C11 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
O6 C14 C10 114.5(4) . . ?
O6 C14 C25 106.9(4) . . ?
O6 C14 C26 99.5(4) . . ?
C25 C14 C10 110.0(4) . . ?
C26 C14 C10 114.6(4) . . ?
C26 C14 C25 110.8(5) . . ?
O2 C15 C5 111.5(3) . . ?
O2 C15 H15 108.3 . . ?
O2 C15 C18 104.6(4) . . ?
C5 C15 H15 108.3 . . ?
C18 C15 C5 115.8(4) . . ?
C18 C15 H15 108.3 . . ?
O2 C16 C4 118.9(4) . . ?
O3 C16 O2 119.7(4) . . ?
O3 C16 C4 121.4(5) . . ?
C19 C18 C15 134.3(6) . . ?
C19 C18 C21 103.8(7) . . ?
C19 C18 C21B 35.6(6) . . ?
C19B C18 C15 136.9(10) . . ?
C19B C18 C19 82.6(10) . . ?
C19B C18 C21 29.8(9) . . ?
C19B C18 C21B 106.6(12) . . ?
C21 C18 C15 121.7(6) . . ?
C21B C18 C15 116.5(8) . . ?
C21B C18 C21 113.6(8) . . ?
C18 C19 H19 125.0 . . ?
C20 C19 C18 110.0(11) . . ?
C20 C19 H19 125.0 . . ?
C18 C19B H19B 123.4 . . ?
C18 C19B C20B 113(2) . . ?
C20B C19B H19B 123.4 . . ?
O4 C20 H20 125.4 . . ?
C19 C20 O4 109.3(12) . . ?
C19 C20 H20 125.4 . . ?
O20B C20B H20B 127.7 . . ?
C19B C20B O20B 105(2) . . ?
C19B C20B H20B 127.7 . . ?
O4 C21 C18 109.6(9) . . ?
O4 C21 H21 125.2 . . ?
C18 C21 H21 125.2 . . ?
O20B C21B C18 107.3(14) . . ?
O20B C21B H21B 126.3 . . ?
C18 C21B H21B 126.3 . . ?
C1 C22 H22A 109.5 . . ?
C1 C22 H22B 109.5 . . ?
C1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C7 C23 H23A 109.5 . . ?
C7 C23 H23B 109.5 . . ?
C7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C5 C24 H24A 109.5 . . ?
C5 C24 H24B 109.5 . . ?
C5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C14 C25 H25A 109.5 . . ?
C14 C25 H25B 109.5 . . ?
C14 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C14 C26 H26A 114(4) . . ?
C14 C26 H26B 107(4) . . ?
C14 C26 H26C 107(4) . . ?
H26A C26 H26B 106(4) . . ?
H26A C26 H26C 107(6) . . ?
H26B C26 H26C 116(5) . . ?
O7 C27 C28 111.3(4) . . ?
O8 C27 O7 123.3(4) . . ?
O8 C27 C28 125.4(4) . . ?
C29 C28 C27 122.2(4) . . ?
C33 C28 C27 117.7(4) . . ?
C33 C28 C29 119.9(4) . . ?
C28 C29 H29 119.4 . . ?
C28 C29 C30 121.2(4) . . ?
C30 C29 H29 119.4 . . ?
C29 C30 C34 121.2(4) . . ?
C31 C30 C29 117.6(4) . . ?
C31 C30 C34 121.1(4) . . ?
C30 C31 H31 118.9 . . ?
C30 C31 C32 122.2(4) . . ?
C32 C31 H31 118.9 . . ?
C31 C32 H32 120.4 . . ?
C33 C32 C31 119.2(4) . . ?
C33 C32 H32 120.4 . . ?
C28 C33 H33 120.1 . . ?
C32 C33 C28 119.8(4) . . ?
C32 C33 H33 120.1 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C4 C6 C5 99.3(4) . . . . ?
O1 C4 C6 C7 -102.5(3) . . . . ?
O1 C4 C16 O2 -44.9(5) . . . . ?
O1 C4 C16 O3 135.0(4) . . . . ?
O1 C6 C7 C2 116.9(3) . . . . ?
O1 C6 C7 C8 -128.7(3) . . . . ?
O1 C6 C7 C23 -7.8(5) . . . . ?
O2 C15 C18 C19 -173.3(8) . . . . ?
O2 C15 C18 C19B 45.5(15) . . . . ?
O2 C15 C18 C21 11.8(8) . . . . ?
O2 C15 C18 C21B -134.8(8) . . . . ?
O7 N1 C8 C7 -179.8(3) . . . . ?
O7 N1 C8 C9 -1.9(6) . . . . ?
O7 C27 C28 C29 -16.3(6) . . . . ?
O7 C27 C28 C33 169.3(4) . . . . ?
O8 C27 C28 C29 162.2(5) . . . . ?
O8 C27 C28 C33 -12.1(7) . . . . ?
N1 O7 C27 O8 -12.7(6) . . . . ?
N1 O7 C27 C28 165.9(3) . . . . ?
N1 C8 C9 C10 -123.0(5) . . . . ?
C1 C2 C7 C6 -178.2(3) . . . . ?
C1 C2 C7 C8 61.9(4) . . . . ?
C1 C2 C7 C23 -57.5(5) . . . . ?
C1 C2 C13 C11 -152.0(4) . . . . ?
C1 C10 C14 O6 3.6(6) . . . . ?
C1 C10 C14 C25 124.0(5) . . . . ?
C1 C10 C14 C26 -110.5(6) . . . . ?
C2 C1 C3 C1A 172.8(5) . . . . ?
C2 C1 C10 C9 49.5(4) . . . . ?
C2 C1 C10 C14 -179.4(3) . . . . ?
C2 C7 C8 N1 119.9(4) . . . . ?
C2 C7 C8 C9 -58.3(4) . . . . ?
C3 C1 C2 C7 -169.2(3) . . . . ?
C3 C1 C2 C13 61.0(5) . . . . ?
C3 C1 C10 C9 160.8(3) . . . . ?
C3 C1 C10 C14 -68.2(4) . . . . ?
C3 C1A C12 O5 145.0(5) . . . . ?
C3 C1A C12 O6 -28.0(8) . . . . ?
C4 O1 C6 C5 -109.8(4) . . . . ?
C4 O1 C6 C7 109.9(4) . . . . ?
C4 C6 C7 C2 -176.7(3) . . . . ?
C4 C6 C7 C8 -62.3(4) . . . . ?
C4 C6 C7 C23 58.6(5) . . . . ?
C5 C6 C7 C2 -19.3(5) . . . . ?
C5 C6 C7 C8 95.2(4) . . . . ?
C5 C6 C7 C23 -144.0(4) . . . . ?
C5 C11 C13 C2 -39.4(5) . . . . ?
C5 C15 C18 C19 63.6(10) . . . . ?
C5 C15 C18 C19B -77.5(15) . . . . ?
C5 C15 C18 C21 -111.3(7) . . . . ?
C5 C15 C18 C21B 102.2(9) . . . . ?
C6 O1 C4 C16 109.9(4) . . . . ?
C6 C4 C16 O2 23.5(6) . . . . ?
C6 C4 C16 O3 -156.5(4) . . . . ?
C6 C5 C11 C13 -19.5(5) . . . . ?
C6 C5 C15 O2 57.0(4) . . . . ?
C6 C5 C15 C18 176.3(4) . . . . ?
C6 C7 C8 N1 3.4(5) . . . . ?
C6 C7 C8 C9 -174.7(3) . . . . ?
C7 C2 C13 C11 74.6(4) . . . . ?
C7 C8 C9 C10 54.9(5) . . . . ?
C8 C9 C10 C1 -49.5(5) . . . . ?
C8 C9 C10 C14 176.1(3) . . . . ?
C9 C10 C14 O6 136.7(4) . . . . ?
C9 C10 C14 C25 -103.0(5) . . . . ?
C9 C10 C14 C26 22.5(6) . . . . ?
C10 C1 C2 C7 -58.2(4) . . . . ?
C10 C1 C2 C13 172.0(3) . . . . ?
C10 C1 C3 C1A 61.2(6) . . . . ?
C11 C5 C6 O1 -85.1(4) . . . . ?
C11 C5 C6 C4 -150.0(3) . . . . ?
C11 C5 C6 C7 52.3(5) . . . . ?
C11 C5 C15 O2 174.0(3) . . . . ?
C11 C5 C15 C18 -66.7(5) . . . . ?
C12 O6 C14 C10 62.3(6) . . . . ?
C12 O6 C14 C25 -59.8(6) . . . . ?
C12 O6 C14 C26 -175.0(5) . . . . ?
C12 C1A C3 C1 6.9(8) . . . . ?
C13 C2 C7 C6 -43.3(4) . . . . ?
C13 C2 C7 C8 -163.2(3) . . . . ?
C13 C2 C7 C23 77.4(4) . . . . ?
C14 O6 C12 O5 152.5(4) . . . . ?
C14 O6 C12 C1A -34.3(7) . . . . ?
C15 O2 C16 O3 -177.4(4) . . . . ?
C15 O2 C16 C4 2.5(6) . . . . ?
C15 C5 C6 O1 31.9(4) . . . . ?
C15 C5 C6 C4 -33.0(5) . . . . ?
C15 C5 C6 C7 169.3(3) . . . . ?
C15 C5 C11 C13 -135.7(4) . . . . ?
C15 C18 C19 C20 -179.3(8) . . . . ?
C15 C18 C19B C20B -178.6(13) . . . . ?
C15 C18 C21 O4 177.5(7) . . . . ?
C15 C18 C21B O20B 178.7(10) . . . . ?
C16 O2 C15 C5 -44.2(5) . . . . ?
C16 O2 C15 C18 -169.9(4) . . . . ?
C16 C4 C6 O1 -104.6(4) . . . . ?
C16 C4 C6 C5 -5.3(6) . . . . ?
C16 C4 C6 C7 152.9(3) . . . . ?
C18 C19 C20 O4 5.1(14) . . . . ?
C18 C19B C20B O20B -1(2) . . . . ?
C19 C18 C19B C20B 28.3(17) . . . . ?
C19 C18 C21 O4 1.3(11) . . . . ?
C19 C18 C21B O20B -51.3(14) . . . . ?
C19B C18 C19 C20 -25.0(13) . . . . ?
C19B C18 C21 O4 47(2) . . . . ?
C19B C18 C21B O20B -1.6(17) . . . . ?
C20 O4 C21 C18 1.7(13) . . . . ?
C20B O20B C21B C18 1(2) . . . . ?
C21 O4 C20 C19 -4.1(14) . . . . ?
C21 C18 C19 C20 -3.8(12) . . . . ?
C21 C18 C19B C20B -107(3) . . . . ?
C21 C18 C21B O20B 29.4(16) . . . . ?
C21B O20B C20B C19B 0(2) . . . . ?
C21B C18 C19 C20 107.5(19) . . . . ?
C21B C18 C19B C20B 2(2) . . . . ?
C21B C18 C21 O4 -35.0(13) . . . . ?
C22 C1 C2 C7 70.6(4) . . . . ?
C22 C1 C2 C13 -59.2(5) . . . . ?
C22 C1 C3 C1A -64.6(6) . . . . ?
C22 C1 C10 C9 -77.5(4) . . . . ?
C22 C1 C10 C14 53.5(5) . . . . ?
C23 C7 C8 N1 -117.0(4) . . . . ?
C23 C7 C8 C9 64.9(4) . . . . ?
C24 C5 C6 O1 151.8(3) . . . . ?
C24 C5 C6 C4 86.9(4) . . . . ?
C24 C5 C6 C7 -70.8(5) . . . . ?
C24 C5 C11 C13 103.5(4) . . . . ?
C24 C5 C15 O2 -64.1(4) . . . . ?
C24 C5 C15 C18 55.2(5) . . . . ?
C27 O7 N1 C8 168.0(3) . . . . ?
C27 C28 C29 C30 -171.9(4) . . . . ?
C27 C28 C33 C32 172.3(4) . . . . ?
C28 C29 C30 C31 -0.3(7) . . . . ?
C28 C29 C30 C34 176.2(5) . . . . ?
C29 C28 C33 C32 -2.2(7) . . . . ?
C29 C30 C31 C32 -2.0(7) . . . . ?
C30 C31 C32 C33 2.1(7) . . . . ?
C31 C32 C33 C28 0.0(7) . . . . ?
C33 C28 C29 C30 2.3(7) . . . . ?
C34 C30 C31 C32 -178.5(5) . . . . ?

