# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_togr_19_0m
#TrackingRef 'togr_19_0m.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N2 O8'
_chemical_formula_sum            'C32 H30 N2 O8'
_chemical_formula_weight         570.58

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

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   39.4134(4)
_cell_length_b                   39.4134(4)
_cell_length_c                   10.4024(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13994.3(5)
_cell_formula_units_Z            18
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    7709
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.91

_exptl_crystal_description       irregular
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5400
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1%
_diffrn_reflns_number            114418
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         29.05
_reflns_number_total             8290
_reflns_number_gt                6448
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kappa APEX 2 (Bruker-AXS)'
_computing_cell_refinement       'SAINT-NT (Sheldrick, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0877P)^2^+17.1128P] where P=(Fo^2^+2Fc^2^)/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         8290
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1517
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.52834(3) 0.17718(3) -0.12673(9) 0.0283(2) Uani 1 1 d . . .
O2 O 0.55804(5) 0.17669(5) 0.46393(12) 0.0542(4) Uani 1 1 d . . .
O3 O 0.52246(5) 0.20393(5) 0.46377(12) 0.0488(4) Uani 1 1 d . . .
O4 O 0.43889(3) 0.12517(3) -0.03823(9) 0.0238(2) Uani 1 1 d . . .
O5 O 0.43157(4) 0.10087(4) 0.51573(11) 0.0343(3) Uani 1 1 d . . .
O6 O 0.46404(4) 0.07021(4) 0.52093(11) 0.0405(3) Uani 1 1 d . . .
O7 O 0.39816(3) 0.03024(3) -0.03944(10) 0.0261(2) Uani 1 1 d . . .
O8 O 0.49475(3) 0.08805(3) -0.04423(9) 0.0245(2) Uani 1 1 d . . .
N1 N 0.53856(4) 0.18849(4) 0.40782(12) 0.0325(3) Uani 1 1 d . . .
N2 N 0.44346(3) 0.08078(4) 0.46516(11) 0.0226(2) Uani 1 1 d . . .
C1 C 0.57232(4) 0.14675(4) 0.00027(14) 0.0252(3) Uani 1 1 d . . .
H1A H 0.5671 0.1461 -0.0931 0.030 Uiso 1 1 calc R . .
H1B H 0.6010 0.1621 0.0135 0.030 Uiso 1 1 calc R . .
C2 C 0.55287(4) 0.16626(4) 0.07051(13) 0.0223(3) Uani 1 1 d . . .
C3 C 0.55507(4) 0.16905(4) 0.20378(14) 0.0241(3) Uani 1 1 d . . .
H3 H 0.5699 0.1602 0.2505 0.029 Uiso 1 1 calc R . .
C4 C 0.53534(4) 0.18502(4) 0.26766(13) 0.0245(3) Uani 1 1 d . . .
C5 C 0.51273(4) 0.19756(4) 0.20421(13) 0.0234(3) Uani 1 1 d . . .
H5 H 0.4992 0.2078 0.2511 0.028 Uiso 1 1 calc R . .
C6 C 0.51007(4) 0.19497(4) 0.07104(13) 0.0217(3) Uani 1 1 d . . .
C7 C 0.53094(4) 0.18003(4) 0.00549(13) 0.0222(3) Uani 1 1 d . . .
C8 C 0.55834(5) 0.21099(5) -0.19069(15) 0.0349(4) Uani 1 1 d . . .
H8A H 0.5570 0.2342 -0.1642 0.052 Uiso 1 1 calc R . .
H8B H 0.5546 0.2075 -0.2839 0.052 Uiso 1 1 calc R . .
H8C H 0.5840 0.2145 -0.1679 0.052 Uiso 1 1 calc R . .
C9 C 0.48373(4) 0.20657(4) 0.00062(14) 0.0245(3) Uani 1 1 d . . .
H9A H 0.4934 0.2348 0.0145 0.029 Uiso 1 1 calc R . .
H9B H 0.4847 0.2023 -0.0928 0.029 Uiso 1 1 calc R . .
C10 C 0.44176(4) 0.18297(4) 0.04715(13) 0.0227(3) Uani 1 1 d . . .
C11 C 0.42331(5) 0.19990(4) 0.11410(14) 0.0264(3) Uani 1 1 d . . .
H11 H 0.4366 0.2275 0.1270 0.032 Uiso 1 1 calc R . .
C12 C 0.38568(5) 0.17687(5) 0.16206(15) 0.0278(3) Uani 1 1 d . . .
H12 H 0.3729 0.1888 0.2040 0.033 Uiso 1 1 calc R . .
C13 C 0.36655(4) 0.13624(5) 0.14886(14) 0.0258(3) Uani 1 1 d . . .
H13 H 0.3413 0.1206 0.1852 0.031 Uiso 1 1 calc R . .
C14 C 0.38426(4) 0.11852(4) 0.08293(13) 0.0228(3) Uani 1 1 d . . .
C15 C 0.42123(4) 0.14247(4) 0.02898(13) 0.0210(3) Uani 1 1 d . . .
C16 C 0.43019(6) 0.12133(6) -0.17271(15) 0.0379(4) Uani 1 1 d . . .
H16A H 0.4018 0.1087 -0.1849 0.057 Uiso 1 1 calc R . .
H16B H 0.4399 0.1053 -0.2127 0.057 Uiso 1 1 calc R . .
H16C H 0.4429 0.1473 -0.2126 0.057 Uiso 1 1 calc R . .
C17 C 0.36679(4) 0.07453(4) 0.07855(15) 0.0249(3) Uani 1 1 d . . .
H17A H 0.3634 0.0657 -0.0120 0.030 Uiso 1 1 calc R . .
H17B H 0.3407 0.0616 0.1199 0.030 Uiso 1 1 calc R . .
C18 C 0.39330(4) 0.06282(4) 0.14781(13) 0.0201(3) Uani 1 1 d . . .
C19 C 0.40505(4) 0.07578(4) 0.27267(13) 0.0198(3) Uani 1 1 d . . .
H19 H 0.3951 0.0901 0.3165 0.024 Uiso 1 1 calc R . .
C20 C 0.43153(4) 0.06754(4) 0.33270(12) 0.0182(2) Uani 1 1 d . . .
C21 C 0.44736(4) 0.04742(4) 0.27151(13) 0.0189(2) Uani 1 1 d . . .
H21 H 0.4659 0.0428 0.3146 0.023 Uiso 1 1 calc R . .
C22 C 0.43594(4) 0.03409(4) 0.14679(13) 0.0192(3) Uani 1 1 d . . .
C23 C 0.40854(4) 0.04162(4) 0.08648(13) 0.0196(3) Uani 1 1 d . . .
C24 C 0.36609(6) -0.00837(5) -0.05404(18) 0.0423(4) Uani 1 1 d . . .
H24A H 0.3728 -0.0271 -0.0168 0.063 Uiso 1 1 calc R . .
H24B H 0.3602 -0.0141 -0.1456 0.063 Uiso 1 1 calc R . .
H24C H 0.3431 -0.0106 -0.0098 0.063 Uiso 1 1 calc R . .
C25 C 0.45568(4) 0.01483(4) 0.07725(14) 0.0235(3) Uani 1 1 d . . .
H25A H 0.4476 -0.0110 0.1163 0.028 Uiso 1 1 calc R . .
H25B H 0.4476 0.0107 -0.0142 0.028 Uiso 1 1 calc R . .
C26 C 0.49964(4) 0.04071(4) 0.08661(13) 0.0230(3) Uani 1 1 d . . .
C27 C 0.52283(5) 0.03093(5) 0.16156(14) 0.0269(3) Uani 1 1 d . . .
H27 H 0.5114 0.0060 0.2023 0.032 Uiso 1 1 calc R . .
C28 C 0.56263(5) 0.05742(5) 0.17705(15) 0.0294(3) Uani 1 1 d . . .
H28 H 0.5785 0.0500 0.2248 0.035 Uiso 1 1 calc R . .
C29 C 0.57924(4) 0.09442(5) 0.12323(14) 0.0278(3) Uani 1 1 d . . .
H29 H 0.6062 0.1126 0.1367 0.033 Uiso 1 1 calc R . .
C30 C 0.55676(4) 0.10538(4) 0.04939(13) 0.0238(3) Uani 1 1 d . . .
C31 C 0.51732(4) 0.07757(4) 0.02849(13) 0.0212(3) Uani 1 1 d . . .
C32 C 0.49523(5) 0.08060(5) -0.17894(15) 0.0346(4) Uani 1 1 d . . .
H32A H 0.5201 0.0820 -0.2011 0.052 Uiso 1 1 calc R . .
H32B H 0.4925 0.1003 -0.2284 0.052 Uiso 1 1 calc R . .
H32C H 0.4734 0.0544 -0.1994 0.052 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0349(6) 0.0354(6) 0.0136(5) 0.0010(4) 0.0012(4) 0.0169(5)
O2 0.0880(11) 0.0959(12) 0.0207(6) -0.0070(6) -0.0107(6) 0.0776(10)
O3 0.0732(10) 0.0863(11) 0.0211(6) -0.0101(6) -0.0044(6) 0.0655(9)
O4 0.0301(5) 0.0283(5) 0.0192(5) -0.0049(4) -0.0034(4) 0.0193(4)
O5 0.0473(7) 0.0444(7) 0.0240(6) -0.0105(5) -0.0039(5) 0.0326(6)
O6 0.0539(8) 0.0618(8) 0.0253(6) -0.0131(5) -0.0159(5) 0.0435(7)
O7 0.0324(5) 0.0264(5) 0.0187(5) -0.0060(4) -0.0070(4) 0.0142(4)
O8 0.0265(5) 0.0334(5) 0.0188(5) -0.0026(4) -0.0029(4) 0.0189(4)
N1 0.0446(8) 0.0488(8) 0.0178(6) -0.0044(5) -0.0035(5) 0.0336(7)
N2 0.0238(6) 0.0264(6) 0.0185(6) -0.0030(4) -0.0010(4) 0.0133(5)
C1 0.0209(6) 0.0320(7) 0.0214(7) -0.0016(5) 0.0038(5) 0.0123(6)
C2 0.0210(6) 0.0250(6) 0.0187(6) -0.0019(5) 0.0016(5) 0.0099(5)
C3 0.0256(7) 0.0312(7) 0.0191(6) -0.0022(5) -0.0018(5) 0.0169(6)
C4 0.0303(7) 0.0322(7) 0.0141(6) -0.0024(5) -0.0021(5) 0.0180(6)
C5 0.0288(7) 0.0264(7) 0.0186(6) -0.0021(5) -0.0008(5) 0.0165(6)
C6 0.0251(6) 0.0213(6) 0.0178(6) 0.0015(5) -0.0005(5) 0.0108(5)
C7 0.0240(6) 0.0240(6) 0.0147(6) 0.0005(5) 0.0009(5) 0.0090(5)
C8 0.0416(9) 0.0426(9) 0.0231(7) 0.0115(6) 0.0101(6) 0.0230(8)
C9 0.0318(7) 0.0237(6) 0.0196(6) 0.0021(5) -0.0020(5) 0.0151(6)
C10 0.0303(7) 0.0252(6) 0.0174(6) 0.0002(5) -0.0049(5) 0.0175(6)
C11 0.0366(8) 0.0254(7) 0.0235(7) -0.0024(5) -0.0050(6) 0.0202(6)
C12 0.0364(8) 0.0325(7) 0.0248(7) -0.0041(6) -0.0031(6) 0.0248(7)
C13 0.0278(7) 0.0327(7) 0.0234(7) -0.0010(6) -0.0027(5) 0.0200(6)
C14 0.0271(7) 0.0261(7) 0.0208(6) -0.0025(5) -0.0072(5) 0.0175(6)
C15 0.0283(7) 0.0260(6) 0.0160(6) -0.0021(5) -0.0050(5) 0.0191(6)
C16 0.0503(10) 0.0499(10) 0.0212(8) -0.0113(7) -0.0079(7) 0.0309(9)
C17 0.0229(6) 0.0255(7) 0.0282(7) -0.0033(5) -0.0079(5) 0.0136(6)
C18 0.0187(6) 0.0190(6) 0.0225(6) -0.0005(5) -0.0025(5) 0.0094(5)
C19 0.0195(6) 0.0189(6) 0.0217(6) -0.0013(5) 0.0006(5) 0.0103(5)
C20 0.0185(6) 0.0193(6) 0.0154(6) -0.0011(4) -0.0001(4) 0.0084(5)
C21 0.0188(6) 0.0198(6) 0.0195(6) 0.0001(5) -0.0004(5) 0.0108(5)
C22 0.0204(6) 0.0184(6) 0.0190(6) -0.0012(5) 0.0006(5) 0.0098(5)
C23 0.0214(6) 0.0181(6) 0.0170(6) -0.0022(5) -0.0028(5) 0.0082(5)
C24 0.0516(11) 0.0269(8) 0.0332(9) -0.0093(7) -0.0174(8) 0.0083(7)
C25 0.0270(7) 0.0243(6) 0.0233(7) -0.0062(5) -0.0011(5) 0.0159(6)
C26 0.0268(7) 0.0291(7) 0.0187(6) -0.0062(5) -0.0002(5) 0.0182(6)
C27 0.0356(8) 0.0325(7) 0.0217(7) -0.0038(6) -0.0002(6) 0.0239(7)
C28 0.0332(8) 0.0438(9) 0.0234(7) -0.0062(6) -0.0049(6) 0.0282(7)
C29 0.0249(7) 0.0395(8) 0.0241(7) -0.0081(6) -0.0023(5) 0.0199(6)
C30 0.0241(6) 0.0330(7) 0.0177(6) -0.0043(5) 0.0025(5) 0.0168(6)
C31 0.0236(6) 0.0299(7) 0.0159(6) -0.0053(5) -0.0011(5) 0.0177(6)
C32 0.0442(9) 0.0452(9) 0.0197(7) -0.0042(6) -0.0052(6) 0.0264(8)

_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 C7 1.3796(16) . ?
O1 C8 1.4284(19) . ?
O2 N1 1.2262(18) . ?
O3 N1 1.2238(17) . ?
O4 C15 1.3832(16) . ?
O4 C16 1.4302(18) . ?
O5 N2 1.2227(16) . ?
O6 N2 1.2272(16) . ?
O7 C23 1.3786(16) . ?
O7 C24 1.4189(19) . ?
O8 C31 1.3788(16) . ?
O8 C32 1.4337(18) . ?
N1 C4 1.4640(18) . ?
N2 C20 1.4653(17) . ?
C1 C30 1.515(2) . ?
C1 C2 1.5175(19) . ?
C2 C3 1.3900(19) . ?
C2 C7 1.403(2) . ?
C3 C4 1.3899(19) . ?
C4 C5 1.384(2) . ?
C5 C6 1.3891(19) . ?
C6 C7 1.4045(19) . ?
C6 C9 1.5158(19) . ?
C9 C10 1.516(2) . ?
C10 C11 1.394(2) . ?
C10 C15 1.3954(19) . ?
C11 C12 1.388(2) . ?
C12 C13 1.395(2) . ?
C13 C14 1.3901(19) . ?
C14 C15 1.398(2) . ?
C14 C17 1.5127(19) . ?
C17 C18 1.5187(18) . ?
C18 C19 1.3877(19) . ?
C18 C23 1.4028(18) . ?
C19 C20 1.3870(18) . ?
C20 C21 1.3852(17) . ?
C21 C22 1.3875(18) . ?
C22 C23 1.4031(18) . ?
C22 C25 1.5152(18) . ?
C25 C26 1.512(2) . ?
C26 C27 1.395(2) . ?
C26 C31 1.396(2) . ?
C27 C28 1.392(2) . ?
C28 C29 1.384(2) . ?
C29 C30 1.394(2) . ?
C30 C31 1.400(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
C7 O1 C8 113.28(12) . . ?
C15 O4 C16 113.16(11) . . ?
C23 O7 C24 114.26(12) . . ?
C31 O8 C32 113.49(11) . . ?
O3 N1 O2 122.74(13) . . ?
O3 N1 C4 118.55(12) . . ?
O2 N1 C4 118.69(13) . . ?
O5 N2 O6 123.31(12) . . ?
O5 N2 C20 118.46(11) . . ?
O6 N2 C20 118.20(11) . . ?
C30 C1 C2 110.35(11) . . ?
C3 C2 C7 118.46(12) . . ?
C3 C2 C1 119.52(13) . . ?
C7 C2 C1 121.95(12) . . ?
C4 C3 C2 119.05(13) . . ?
C5 C4 C3 122.68(13) . . ?
C5 C4 N1 118.86(12) . . ?
C3 C4 N1 118.46(12) . . ?
C4 C5 C6 119.18(13) . . ?
C5 C6 C7 118.47(12) . . ?
C5 C6 C9 119.83(12) . . ?
C7 C6 C9 121.65(12) . . ?
O1 C7 C2 118.96(12) . . ?
O1 C7 C6 118.88(12) . . ?
C2 C7 C6 122.10(12) . . ?
C10 C9 C6 111.26(11) . . ?
C11 C10 C15 118.18(13) . . ?
C11 C10 C9 122.43(13) . . ?
C15 C10 C9 119.31(12) . . ?
C12 C11 C10 120.60(13) . . ?
C11 C12 C13 120.19(13) . . ?
C14 C13 C12 120.45(14) . . ?
C13 C14 C15 118.32(13) . . ?
C13 C14 C17 122.38(13) . . ?
C15 C14 C17 119.04(12) . . ?
O4 C15 C10 119.05(13) . . ?
O4 C15 C14 118.79(12) . . ?
C10 C15 C14 122.05(13) . . ?
C14 C17 C18 110.24(11) . . ?
C19 C18 C23 118.78(12) . . ?
C19 C18 C17 119.07(12) . . ?
C23 C18 C17 121.99(12) . . ?
C20 C19 C18 119.13(12) . . ?
C21 C20 C19 122.31(12) . . ?
C21 C20 N2 118.67(11) . . ?
C19 C20 N2 119.02(11) . . ?
C20 C21 C22 119.50(12) . . ?
C21 C22 C23 118.46(12) . . ?
C21 C22 C25 119.03(12) . . ?
C23 C22 C25 122.33(12) . . ?
O7 C23 C18 118.69(12) . . ?
O7 C23 C22 119.39(12) . . ?
C18 C23 C22 121.78(12) . . ?
C26 C25 C22 109.48(11) . . ?
C27 C26 C31 118.34(13) . . ?
C27 C26 C25 122.55(14) . . ?
C31 C26 C25 118.80(12) . . ?
C28 C27 C26 120.39(14) . . ?
C29 C28 C27 120.35(14) . . ?
C28 C29 C30 120.69(14) . . ?
C29 C30 C31 118.15(14) . . ?
C29 C30 C1 122.75(13) . . ?
C31 C30 C1 118.92(13) . . ?
O8 C31 C26 119.22(12) . . ?
O8 C31 C30 118.72(13) . . ?
C26 C31 C30 121.89(13) . . ?

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
C30 C1 C2 C3 56.78(17) . . . . ?
C30 C1 C2 C7 -120.08(14) . . . . ?
C7 C2 C3 C4 0.5(2) . . . . ?
C1 C2 C3 C4 -176.48(13) . . . . ?
C2 C3 C4 C5 1.5(2) . . . . ?
C2 C3 C4 N1 -178.80(14) . . . . ?
O3 N1 C4 C5 -3.1(2) . . . . ?
O2 N1 C4 C5 178.70(17) . . . . ?
O3 N1 C4 C3 177.21(16) . . . . ?
O2 N1 C4 C3 -1.0(2) . . . . ?
C3 C4 C5 C6 -1.3(2) . . . . ?
N1 C4 C5 C6 178.93(14) . . . . ?
C4 C5 C6 C7 -0.7(2) . . . . ?
C4 C5 C6 C9 176.77(13) . . . . ?
C8 O1 C7 C2 -90.82(16) . . . . ?
C8 O1 C7 C6 92.10(16) . . . . ?
C3 C2 C7 O1 -179.58(13) . . . . ?
C1 C2 C7 O1 -2.7(2) . . . . ?
C3 C2 C7 C6 -2.6(2) . . . . ?
C1 C2 C7 C6 174.29(13) . . . . ?
C5 C6 C7 O1 179.71(12) . . . . ?
C9 C6 C7 O1 2.3(2) . . . . ?
C5 C6 C7 C2 2.7(2) . . . . ?
C9 C6 C7 C2 -174.73(13) . . . . ?
C5 C6 C9 C10 -57.48(17) . . . . ?
C7 C6 C9 C10 119.95(14) . . . . ?
C6 C9 C10 C11 113.07(15) . . . . ?
C6 C9 C10 C15 -63.39(16) . . . . ?
C15 C10 C11 C12 0.6(2) . . . . ?
C9 C10 C11 C12 -175.93(13) . . . . ?
C10 C11 C12 C13 3.0(2) . . . . ?
C11 C12 C13 C14 -2.7(2) . . . . ?
C12 C13 C14 C15 -1.0(2) . . . . ?
C12 C13 C14 C17 173.08(13) . . . . ?
C16 O4 C15 C10 -92.41(16) . . . . ?
C16 O4 C15 C14 91.28(16) . . . . ?
C11 C10 C15 O4 179.41(12) . . . . ?
C9 C10 C15 O4 -3.99(18) . . . . ?
C11 C10 C15 C14 -4.4(2) . . . . ?
C9 C10 C15 C14 172.19(12) . . . . ?
C13 C14 C15 O4 -179.19(12) . . . . ?
C17 C14 C15 O4 6.56(18) . . . . ?
C13 C14 C15 C10 4.6(2) . . . . ?
C17 C14 C15 C10 -169.63(12) . . . . ?
C13 C14 C17 C18 -114.44(15) . . . . ?
C15 C14 C17 C18 59.57(17) . . . . ?
C14 C17 C18 C19 52.87(17) . . . . ?
C14 C17 C18 C23 -122.53(14) . . . . ?
C23 C18 C19 C20 0.2(2) . . . . ?
C17 C18 C19 C20 -175.31(12) . . . . ?
C18 C19 C20 C21 1.3(2) . . . . ?
C18 C19 C20 N2 -179.16(12) . . . . ?
O5 N2 C20 C21 174.97(13) . . . . ?
O6 N2 C20 C21 -7.02(19) . . . . ?
O5 N2 C20 C19 -4.59(19) . . . . ?
O6 N2 C20 C19 173.42(13) . . . . ?
C19 C20 C21 C22 -1.5(2) . . . . ?
N2 C20 C21 C22 178.97(12) . . . . ?
C20 C21 C22 C23 0.1(2) . . . . ?
C20 C21 C22 C25 175.44(12) . . . . ?
C24 O7 C23 C18 -95.27(16) . . . . ?
C24 O7 C23 C22 89.01(17) . . . . ?
C19 C18 C23 O7 -177.22(12) . . . . ?
C17 C18 C23 O7 -1.80(19) . . . . ?
C19 C18 C23 C22 -1.6(2) . . . . ?
C17 C18 C23 C22 173.82(12) . . . . ?
C21 C22 C23 O7 177.01(12) . . . . ?
C25 C22 C23 O7 1.8(2) . . . . ?
C21 C22 C23 C18 1.4(2) . . . . ?
C25 C22 C23 C18 -173.74(12) . . . . ?
C21 C22 C25 C26 -50.61(17) . . . . ?
C23 C22 C25 C26 124.52(14) . . . . ?
C22 C25 C26 C27 109.41(14) . . . . ?
C22 C25 C26 C31 -64.08(16) . . . . ?
C31 C26 C27 C28 -0.2(2) . . . . ?
C25 C26 C27 C28 -173.74(13) . . . . ?
C26 C27 C28 C29 3.0(2) . . . . ?
C27 C28 C29 C30 -2.0(2) . . . . ?
C28 C29 C30 C31 -1.7(2) . . . . ?
C28 C29 C30 C1 173.29(13) . . . . ?
C2 C1 C30 C29 -109.56(15) . . . . ?
C2 C1 C30 C31 65.43(16) . . . . ?
C32 O8 C31 C26 -94.77(15) . . . . ?
C32 O8 C31 C30 89.82(15) . . . . ?
C27 C26 C31 O8 -178.92(12) . . . . ?
C25 C26 C31 O8 -5.16(18) . . . . ?
C27 C26 C31 C30 -3.7(2) . . . . ?
C25 C26 C31 C30 170.10(12) . . . . ?
C29 C30 C31 O8 179.92(12) . . . . ?
C1 C30 C31 O8 4.70(18) . . . . ?
C29 C30 C31 C26 4.6(2) . . . . ?
C1 C30 C31 C26 -170.59(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        29.05
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.060


_database_code_depnum_ccdc_archive 'CCDC 787340'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_togr4ax
#TrackingRef 'togr4ax.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N2 O8, 0.34(C3 H6 O)'
_chemical_formula_sum            'C33 H32 N2 O8.34'
_chemical_formula_weight         589.94

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

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   39.3244(3)
_cell_length_b                   39.3244(3)
_cell_length_c                   10.4186(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13952.9(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    7220
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      23.61

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5592
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1%
_diffrn_reflns_number            105784
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.61
_reflns_number_total             7896
_reflns_number_gt                5211
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kappa APEX 2 (Bruker-AXS)'
_computing_cell_refinement       'SAINT-NT (Sheldrick, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0600P)^2^+22.8232P] where P=(Fo^2^+2Fc^2^)/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         7896
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1462
_refine_ls_wR_factor_gt          0.1258
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.85705(5) -0.01512(4) 1.12948(13) 0.0510(5) Uani 1 1 d . A 1
O2 O 0.89286(6) 0.04780(4) 1.12952(14) 0.0546(5) Uani 1 1 d . A 1
O3 O 0.86255(4) 0.01771(4) 0.54005(11) 0.0300(3) Uani 1 1 d . A 1
O4 O 0.82858(4) 0.07331(4) 0.62272(12) 0.0289(3) Uani 1 1 d . A 1
O5 O 0.79695(5) 0.06046(4) 1.18772(14) 0.0464(4) Uani 1 1 d . A 1
O6 O 0.76463(5) -0.00274(4) 1.18200(13) 0.0382(4) Uani 1 1 d . A 1
O7 O 0.73193(4) 0.03470(4) 0.62710(12) 0.0294(3) Uani 1 1 d . A 1
O8 O 0.77274(4) -0.01984(4) 0.62827(11) 0.0266(3) Uani 1 1 d . A 1
N1 N 0.87341(5) 0.01648(5) 1.07360(15) 0.0354(4) Uani 1 1 d . A 1
N2 N 0.77659(5) 0.02937(5) 1.13163(14) 0.0263(3) Uani 1 1 d . A 1
C1 C 0.81761(6) -0.05649(5) 0.66753(17) 0.0271(4) Uani 1 1 d . A 1
H1A H 0.8185 -0.0513 0.5743 0.032 Uiso 1 1 calc R A 1
H1B H 0.8272 -0.0752 0.6812 0.032 Uiso 1 1 calc R A 1
C2 C 0.84429(5) -0.01842(5) 0.73757(17) 0.0245(4) Uani 1 1 d . A 1
C3 C 0.84724(6) -0.01840(5) 0.87026(17) 0.0262(4) Uani 1 1 d . A 1
H3 H 0.8338 -0.0423 0.9171 0.031 Uiso 1 1 calc R A 1
C4 C 0.87004(6) 0.01685(6) 0.93350(16) 0.0268(4) Uani 1 1 d . A 1
C5 C 0.88947(5) 0.05250(5) 0.87003(17) 0.0260(4) Uani 1 1 d . A 1
H5 H 0.9042 0.0762 0.9167 0.031 Uiso 1 1 calc R A 1
C6 C 0.88709(5) 0.05308(5) 0.73693(17) 0.0244(4) Uani 1 1 d . A 1
C7 C 0.86516(5) 0.01741(5) 0.67235(16) 0.0243(4) Uani 1 1 d . A 1
C8 C 0.89268(7) 0.01384(7) 0.47636(19) 0.0365(5) Uani 1 1 d . A 1
H8A H 0.9184 0.0357 0.5009 0.055 Uiso 1 1 calc R A 1
H8B H 0.8893 0.0142 0.3832 0.055 Uiso 1 1 calc R A 1
H8C H 0.8909 -0.0110 0.5013 0.055 Uiso 1 1 calc R A 1
C9 C 0.90633(6) 0.09223(6) 0.66706(17) 0.0281(4) Uani 1 1 d . A 1
H9A H 0.9351 0.1057 0.6801 0.034 Uiso 1 1 calc R A 1
H9B H 0.9011 0.0877 0.5739 0.034 Uiso 1 1 calc R A 1
C10 C 0.89061(6) 0.11793(6) 0.71626(17) 0.0283(4) Uani 1 1 d . A 1
C11 C 0.91316(6) 0.15145(6) 0.79044(18) 0.0318(4) Uani 1 1 d . A 1
H11 H 0.9402 0.1604 0.8041 0.038 Uiso 1 1 calc R A 1
C12 C 0.89641(6) 0.17168(6) 0.84386(19) 0.0336(5) Uani 1 1 d . A 1
H12 H 0.9122 0.1949 0.8920 0.040 Uiso 1 1 calc R A 1
C13 C 0.85683(6) 0.15859(6) 0.82822(18) 0.0310(4) Uani 1 1 d . A 1
H13 H 0.8455 0.1722 0.8687 0.037 Uiso 1 1 calc R A 1
C14 C 0.83351(6) 0.12554(5) 0.75335(17) 0.0266(4) Uani 1 1 d . A 1
C15 C 0.85113(5) 0.10642(5) 0.69554(16) 0.0235(4) Uani 1 1 d . A 1
C16 C 0.82906(7) 0.08149(7) 0.48799(19) 0.0392(5) Uani 1 1 d . A 1
H16A H 0.8079 0.0869 0.4685 0.059 Uiso 1 1 calc R A 1
H16B H 0.8253 0.0587 0.4382 0.059 Uiso 1 1 calc R A 1
H16C H 0.8544 0.1044 0.4654 0.059 Uiso 1 1 calc R A 1
C17 C 0.78947(5) 0.10771(5) 0.74382(18) 0.0263(4) Uani 1 1 d . A 1
H17A H 0.7814 0.1038 0.6525 0.032 Uiso 1 1 calc R A 1
H17B H 0.7815 0.1256 0.7830 0.032 Uiso 1 1 calc R A 1
C18 C 0.76956(5) 0.06852(5) 0.81329(16) 0.0217(4) Uani 1 1 d . A 1
C19 C 0.78077(5) 0.06655(5) 0.93819(16) 0.0214(3) Uani 1 1 d . A 1
H19 H 0.7993 0.0898 0.9815 0.026 Uiso 1 1 calc R A 1
C20 C 0.76484(5) 0.03066(5) 0.99900(16) 0.0208(3) Uani 1 1 d . A 1
C21 C 0.73851(5) -0.00405(5) 0.93898(16) 0.0220(4) Uani 1 1 d . A 1
H21 H 0.7285 -0.0284 0.9827 0.026 Uiso 1 1 calc R A 1
C22 C 0.72686(5) -0.00287(5) 0.81396(17) 0.0221(4) Uani 1 1 d . A 1
C23 C 0.74226(5) 0.03361(5) 0.75305(16) 0.0223(4) Uani 1 1 d . A 1
C24 C 0.69967(7) 0.04117(8) 0.6126(2) 0.0462(6) Uani 1 1 d . A 1
H24A H 0.6766 0.0202 0.6563 0.069 Uiso 1 1 calc R A 1
H24B H 0.6938 0.0412 0.5211 0.069 Uiso 1 1 calc R A 1
H24C H 0.7063 0.0666 0.6503 0.069 Uiso 1 1 calc R A 1
C25 C 0.70051(5) -0.04115(5) 0.74460(18) 0.0274(4) Uani 1 1 d . A 1
H25A H 0.6743 -0.0545 0.7855 0.033 Uiso 1 1 calc R A 1
H25B H 0.6973 -0.0356 0.6541 0.033 Uiso 1 1 calc R A 1
C26 C 0.71810(5) -0.06766(5) 0.74923(17) 0.0253(4) Uani 1 1 d . A 1
C27 C 0.70032(6) -0.10315(5) 0.81560(18) 0.0287(4) Uani 1 1 d . A 1
H27 H 0.6750 -0.1128 0.8517 0.034 Uiso 1 1 calc R A 1
C28 C 0.71949(6) -0.12454(6) 0.82924(18) 0.0318(4) Uani 1 1 d . A 1
H28 H 0.7067 -0.1493 0.8715 0.038 Uiso 1 1 calc R A 1
C29 C 0.75710(6) -0.11003(6) 0.78167(17) 0.0294(4) Uani 1 1 d . A 1
H29 H 0.7704 -0.1243 0.7949 0.035 Uiso 1 1 calc R A 1
C30 C 0.77568(6) -0.07463(5) 0.71451(16) 0.0252(4) Uani 1 1 d . A 1
C31 C 0.75506(5) -0.05474(5) 0.69562(16) 0.0235(4) Uani 1 1 d . A 1
C32 C 0.76392(7) -0.02493(7) 0.49362(19) 0.0414(5) Uani 1 1 d . A 1
H32A H 0.7772 -0.0377 0.4537 0.062 Uiso 1 1 calc R A 1
H32B H 0.7731 0.0008 0.4536 0.062 Uiso 1 1 calc R A 1
H32C H 0.7355 -0.0413 0.4816 0.062 Uiso 1 1 calc R A 1
C1G C 0.9956(3) 0.9560(3) 0.7996(9) 0.108(3) Uiso 0.50 1 d P B 1
O1G O 0.9396(4) 0.9669(4) 0.7982(13) 0.075(3) Uiso 0.17 1 d P . 1
C1GA C 0.9755(3) 0.9793(3) 0.8131(10) 0.127(3) Uiso 0.50 1 d P . 1
O1GA O 0.9578(4) 0.9419(4) 0.7957(14) 0.082(4) Uiso 0.17 1 d P B 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0790(12) 0.0312(8) 0.0206(7) 0.0065(6) -0.0020(7) 0.0109(8)
O2 0.0847(13) 0.0315(8) 0.0216(7) -0.0033(6) -0.0092(8) 0.0095(8)
O3 0.0357(7) 0.0402(8) 0.0149(6) 0.0011(5) 0.0015(5) 0.0197(6)
O4 0.0309(7) 0.0270(7) 0.0219(6) -0.0007(5) -0.0029(5) 0.0094(6)
O5 0.0603(10) 0.0327(8) 0.0299(8) -0.0033(6) -0.0181(7) 0.0110(8)
O6 0.0521(9) 0.0307(8) 0.0261(7) 0.0077(6) -0.0039(6) 0.0165(7)
O7 0.0359(7) 0.0340(7) 0.0212(6) -0.0010(5) -0.0076(5) 0.0196(6)
O8 0.0350(7) 0.0226(6) 0.0203(6) 0.0022(5) -0.0034(5) 0.0130(6)
N1 0.0478(11) 0.0299(9) 0.0194(8) 0.0011(7) -0.0021(7) 0.0126(8)
N2 0.0268(8) 0.0272(8) 0.0217(7) 0.0021(6) -0.0019(6) 0.0111(7)
C1 0.0357(10) 0.0283(10) 0.0209(9) -0.0041(7) -0.0027(7) 0.0187(9)
C2 0.0281(9) 0.0292(10) 0.0201(8) -0.0025(7) -0.0002(7) 0.0173(8)
C3 0.0333(10) 0.0250(9) 0.0212(9) 0.0023(7) 0.0013(7) 0.0154(8)
C4 0.0337(10) 0.0308(10) 0.0146(8) 0.0012(7) 0.0000(7) 0.0152(8)
C5 0.0272(9) 0.0267(9) 0.0203(8) -0.0004(7) -0.0012(7) 0.0106(8)
C6 0.0228(9) 0.0300(10) 0.0200(8) 0.0038(7) 0.0024(7) 0.0130(8)
C7 0.0263(9) 0.0338(10) 0.0161(8) 0.0003(7) 0.0008(7) 0.0175(8)
C8 0.0440(12) 0.0414(12) 0.0236(9) -0.0003(8) 0.0099(9) 0.0209(10)
C9 0.0249(9) 0.0316(10) 0.0220(9) 0.0066(7) 0.0034(7) 0.0099(8)
C10 0.0296(10) 0.0277(10) 0.0197(9) 0.0084(7) 0.0022(7) 0.0085(8)
C11 0.0299(10) 0.0296(10) 0.0250(9) 0.0056(8) -0.0024(8) 0.0067(8)
C12 0.0381(11) 0.0267(10) 0.0253(10) 0.0008(8) -0.0052(8) 0.0081(9)
C13 0.0409(11) 0.0244(9) 0.0243(9) 0.0043(7) 0.0006(8) 0.0138(9)
C14 0.0309(10) 0.0233(9) 0.0209(8) 0.0067(7) 0.0003(7) 0.0102(8)
C15 0.0263(9) 0.0197(8) 0.0174(8) 0.0055(6) -0.0003(7) 0.0062(7)
C16 0.0503(13) 0.0414(12) 0.0224(9) -0.0035(8) -0.0060(9) 0.0203(11)
C17 0.0310(10) 0.0231(9) 0.0253(9) 0.0052(7) -0.0002(7) 0.0139(8)
C18 0.0232(9) 0.0232(9) 0.0214(8) 0.0018(7) 0.0009(7) 0.0137(7)
C19 0.0213(8) 0.0205(8) 0.0213(8) -0.0019(7) -0.0006(7) 0.0095(7)
C20 0.0218(8) 0.0253(9) 0.0164(8) 0.0008(6) -0.0007(6) 0.0126(7)
C21 0.0207(8) 0.0202(8) 0.0241(9) 0.0025(7) 0.0022(7) 0.0096(7)
C22 0.0200(8) 0.0221(9) 0.0252(9) -0.0024(7) -0.0021(7) 0.0113(7)
C23 0.0246(9) 0.0268(9) 0.0184(8) -0.0007(7) -0.0029(7) 0.0151(8)
C24 0.0553(15) 0.0666(16) 0.0372(12) -0.0080(11) -0.0187(10) 0.0459(13)
C25 0.0255(9) 0.0237(9) 0.0298(10) -0.0030(7) -0.0062(7) 0.0098(8)
C26 0.0293(10) 0.0220(9) 0.0222(9) -0.0056(7) -0.0075(7) 0.0111(8)
C27 0.0303(10) 0.0239(9) 0.0257(9) -0.0022(7) -0.0031(8) 0.0088(8)
C28 0.0418(12) 0.0212(9) 0.0276(10) 0.0020(7) -0.0020(8) 0.0122(9)
C29 0.0419(11) 0.0261(10) 0.0246(9) -0.0032(7) -0.0056(8) 0.0203(9)
C30 0.0343(10) 0.0232(9) 0.0177(8) -0.0062(7) -0.0059(7) 0.0140(8)
C31 0.0319(10) 0.0191(8) 0.0165(8) -0.0031(6) -0.0051(7) 0.0104(8)
C32 0.0530(14) 0.0432(13) 0.0233(10) 0.0045(9) -0.0069(9) 0.0205(11)

_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 N1 1.224(2) . ?
O2 N1 1.225(2) . ?
O3 C7 1.383(2) . ?
O3 C8 1.431(2) . ?
O4 C15 1.379(2) . ?
O4 C16 1.438(2) . ?
O5 N2 1.224(2) . ?
O6 N2 1.223(2) . ?
O7 C23 1.381(2) . ?
O7 C24 1.421(2) . ?
O8 C31 1.380(2) . ?
O8 C32 1.435(2) . ?
N1 C4 1.466(2) . ?
N2 C20 1.466(2) . ?
C1 C30 1.514(3) . ?
C1 C2 1.518(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.387(2) . ?
C2 C7 1.401(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(3) . ?
C5 C6 1.391(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.398(3) . ?
C6 C9 1.519(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.514(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.397(3) . ?
C10 C15 1.400(3) . ?
C11 C12 1.379(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C14 C17 1.512(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.518(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.389(2) . ?
C18 C23 1.399(2) . ?
C19 C20 1.379(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(2) . ?
C21 C22 1.389(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.399(2) . ?
C22 C25 1.517(2) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.513(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.392(3) . ?
C26 C31 1.395(3) . ?
C27 C28 1.389(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.394(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.394(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C1G O1G 1.280(15) 2_765 ?
C1G O1GA 1.299(16) . ?
C1G C1GA 1.391(14) 2_765 ?
C1G C1GA 1.482(15) . ?
O1G C1GA 1.253(15) . ?
O1G C1G 1.280(15) 3_675 ?
O1G O1GA 1.481(19) . ?
C1GA O1GA 1.288(16) . ?
C1GA C1G 1.391(14) 3_675 ?
C1GA C1GA 1.554(17) 3_675 ?
C1GA C1GA 1.554(17) 2_765 ?

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
C7 O3 C8 113.11(14) . . ?
C15 O4 C16 113.29(14) . . ?
C23 O7 C24 114.18(15) . . ?
C31 O8 C32 113.08(14) . . ?
O1 N1 O2 122.81(16) . . ?
O1 N1 C4 118.65(16) . . ?
O2 N1 C4 118.53(16) . . ?
O6 N2 O5 123.22(15) . . ?
O6 N2 C20 118.35(15) . . ?
O5 N2 C20 118.40(15) . . ?
C30 C1 C2 111.25(14) . . ?
C30 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
C30 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C3 C2 C7 118.42(17) . . ?
C3 C2 C1 119.73(16) . . ?
C7 C2 C1 121.80(16) . . ?
C4 C3 C2 119.13(17) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 122.69(16) . . ?
C5 C4 N1 118.61(16) . . ?
C3 C4 N1 118.70(16) . . ?
C4 C5 C6 119.03(17) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C7 118.44(16) . . ?
C5 C6 C9 119.39(16) . . ?
C7 C6 C9 122.08(16) . . ?
O3 C7 C6 118.84(16) . . ?
O3 C7 C2 118.90(16) . . ?
C6 C7 C2 122.19(15) . . ?
C10 C9 C6 110.59(15) . . ?
C10 C9 H9A 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C15 117.94(18) . . ?
C11 C10 C9 122.61(18) . . ?
C15 C10 C9 119.27(17) . . ?
C12 C11 C10 120.44(19) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.75(19) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C14 120.36(19) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 118.26(18) . . ?
C15 C14 C17 119.09(16) . . ?
C13 C14 C17 122.37(18) . . ?
O4 C15 C14 119.35(16) . . ?
O4 C15 C10 118.42(16) . . ?
C14 C15 C10 122.06(17) . . ?
C14 C17 C18 109.23(14) . . ?
C14 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C14 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C23 118.34(16) . . ?
C19 C18 C17 119.11(16) . . ?
C23 C18 C17 122.38(15) . . ?
C20 C19 C18 119.56(16) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 122.36(16) . . ?
C19 C20 N2 118.60(15) . . ?
C21 C20 N2 119.04(15) . . ?
C20 C21 C22 119.18(16) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C23 118.59(16) . . ?
C21 C22 C25 119.11(16) . . ?
C23 C22 C25 122.13(16) . . ?
O7 C23 C18 119.28(15) . . ?
O7 C23 C22 118.66(15) . . ?
C18 C23 C22 121.94(15) . . ?
C26 C25 C22 110.36(15) . . ?
C26 C25 H25A 109.6 . . ?
C22 C25 H25A 109.6 . . ?
C26 C25 H25B 109.6 . . ?
C22 C25 H25B 109.6 . . ?
H25A C25 H25B 108.1 . . ?
C27 C26 C31 118.27(17) . . ?
C27 C26 C25 122.22(17) . . ?
C31 C26 C25 119.24(16) . . ?
C28 C27 C26 120.34(18) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 120.35(17) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.67(18) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C31 C30 C29 118.02(18) . . ?
C31 C30 C1 119.48(16) . . ?
C29 C30 C1 122.44(17) . . ?
O8 C31 C30 119.01(16) . . ?
O8 C31 C26 118.74(16) . . ?
C30 C31 C26 122.13(16) . . ?
O1G C1G O1GA 174.9(13) 2_765 . ?
O1G C1G C1GA 55.7(8) 2_765 2_765 ?
O1GA C1G C1GA 120.1(11) . 2_765 ?
O1G C1G C1GA 121.1(11) 2_765 . ?
O1GA C1G C1GA 54.7(8) . . ?
C1GA C1G C1GA 65.4(9) 2_765 . ?
C1GA O1G C1G 66.7(10) . 3_675 ?
C1GA O1G O1GA 55.5(9) . . ?
C1G O1G O1GA 121.6(12) 3_675 . ?
O1G C1GA O1GA 71.3(10) . . ?
O1G C1GA C1G 57.6(9) . 3_675 ?
O1GA C1GA C1G 128.2(11) . 3_675 ?
O1G C1GA C1G 126.4(11) . . ?
O1GA C1GA C1G 55.4(9) . . ?
C1G C1GA C1G 167.4(11) 3_675 . ?
O1G C1GA C1GA 117.7(14) . 3_675 ?
O1GA C1GA C1GA 167.2(12) . 3_675 ?
C1G C1GA C1GA 60.1(9) 3_675 3_675 ?
C1G C1GA C1GA 114.2(8) . 3_675 ?
O1G C1GA C1GA 172.6(9) . 2_765 ?
O1GA C1GA C1GA 109.8(14) . 2_765 ?
C1G C1GA C1GA 119.8(9) 3_675 2_765 ?
C1G C1GA C1GA 54.5(8) . 2_765 ?
C1GA C1GA C1GA 60.000(13) 3_675 2_765 ?
C1GA O1GA C1G 69.9(10) . . ?
C1GA O1GA O1G 53.2(8) . . ?
C1G O1GA O1G 122.9(13) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.61
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 787341'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_lure_1a_0m
#TrackingRef 'LuRe1Afin.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N2 O8, C H Cl3'
_chemical_formula_sum            'C33 H31 Cl3 N2 O8'
_chemical_formula_weight         689.95

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   16.1514(5)
_cell_length_b                   16.4165(5)
_cell_length_c                   24.4814(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6491.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7592
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      29.58

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2864
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.8497
_exptl_absorpt_correction_T_max  0.9575
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1%
_diffrn_reflns_number            45746
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.10
_reflns_number_total             6445
_reflns_number_gt                5278
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kappa APEX 2 (Bruker-AXS)'
_computing_cell_refinement       'SAINT-NT (Sheldrick, 2008)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0957P)^2^+9.2233P] where P=(Fo^2^+2Fc^2^)/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         6445
_refine_ls_number_parameters     444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.2150
_refine_ls_wR_factor_gt          0.1960
_refine_ls_goodness_of_fit_ref   1.284
_refine_ls_restrained_S_all      1.286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.76596(15) 0.10487(15) 0.42732(10) 0.0277(6) Uani 1 1 d . A 2
O2 O 0.96430(14) 0.10793(13) 0.40254(9) 0.0204(5) Uani 1 1 d . A 2
O3 O 1.09048(14) -0.06368(14) 0.39657(10) 0.0270(5) Uani 1 1 d . A 2
O4 O 0.84667(17) -0.08790(17) 0.28512(10) 0.0343(6) Uani 1 1 d . A 2
O5 O 0.82854(18) 0.0995(2) 0.17599(11) 0.0446(8) Uani 1 1 d . A 2
O6 O 0.8401(2) 0.2294(2) 0.19121(12) 0.0512(8) Uani 1 1 d . A 2
O7 O 1.0372(2) 0.14373(16) 0.18506(12) 0.0447(8) Uani 1 1 d . A 2
O8 O 1.00789(17) 0.02468(16) 0.15391(10) 0.0340(6) Uani 1 1 d . A 2
N1 N 0.82826(18) 0.1586(2) 0.20682(13) 0.0354(8) Uani 1 1 d . A 2
N2 N 1.02950(18) 0.07015(17) 0.19102(12) 0.0261(6) Uani 1 1 d . A 2
C1 C 0.7202(2) -0.0212(2) 0.35384(14) 0.0283(8) Uani 1 1 d . A 2
H1A H 0.6788 -0.0116 0.3830 0.034 Uiso 1 1 calc R A 2
H1B H 0.6919 -0.0483 0.3229 0.034 Uiso 1 1 calc R A 2
C2 C 0.75578(19) 0.0602(2) 0.33486(13) 0.0247(7) Uani 1 1 d . A 2
C3 C 0.7717(2) 0.0738(2) 0.27983(14) 0.0281(8) Uani 1 1 d . A 2
H3 H 0.7550 0.0352 0.2531 0.034 Uiso 1 1 calc R A 2
C4 C 0.8122(2) 0.1445(2) 0.26466(14) 0.0285(8) Uani 1 1 d . A 2
C5 C 0.8401(2) 0.2018(2) 0.30181(14) 0.0277(8) Uani 1 1 d . A 2
H5 H 0.8690 0.2489 0.2898 0.033 Uiso 1 1 calc R A 2
C6 C 0.8250(2) 0.1892(2) 0.35695(14) 0.0257(7) Uani 1 1 d . A 2
C7 C 0.7808(2) 0.1193(2) 0.37257(14) 0.0242(7) Uani 1 1 d . A 2
C8 C 0.6901(3) 0.1427(3) 0.44543(17) 0.0414(10) Uani 1 1 d . A 2
H8A H 0.6934 0.2016 0.4395 0.062 Uiso 1 1 calc R A 2
H8B H 0.6820 0.1317 0.4844 0.062 Uiso 1 1 calc R A 2
H8C H 0.6434 0.1205 0.4247 0.062 Uiso 1 1 calc R A 2
C9 C 0.8625(2) 0.2468(2) 0.39887(15) 0.0288(8) Uani 1 1 d . A 2
H9A H 0.8377 0.3016 0.3947 0.035 Uiso 1 1 calc R A 2
H9B H 0.8496 0.2270 0.4361 0.035 Uiso 1 1 calc R A 2
C10 C 0.9551(2) 0.2525(2) 0.39185(13) 0.0234(7) Uani 1 1 d . A 2
C11 C 0.9955(3) 0.3260(2) 0.38206(14) 0.0299(8) Uani 1 1 d . A 2
H11 H 0.9641 0.3749 0.3806 0.036 Uiso 1 1 calc R A 2
C12 C 1.0800(3) 0.3293(2) 0.37446(14) 0.0306(8) Uani 1 1 d . A 2
H12 H 1.1064 0.3804 0.3687 0.037 Uiso 1 1 calc R A 2
C13 C 1.1266(2) 0.2585(2) 0.37512(14) 0.0268(7) Uani 1 1 d . A 2
H13 H 1.1846 0.2610 0.3690 0.032 Uiso 1 1 calc R A 2
C14 C 1.0887(2) 0.18357(19) 0.38470(13) 0.0211(7) Uani 1 1 d . A 2
C15 C 1.0034(2) 0.18203(18) 0.39463(12) 0.0189(6) Uani 1 1 d . A 2
C16 C 0.9595(2) 0.0838(2) 0.45881(15) 0.0320(8) Uani 1 1 d . A 2
H16A H 1.0152 0.0718 0.4725 0.048 Uiso 1 1 calc R A 2
H16B H 0.9248 0.0351 0.4620 0.048 Uiso 1 1 calc R A 2
H16C H 0.9353 0.1281 0.4804 0.048 Uiso 1 1 calc R A 2
C17 C 1.13547(19) 0.1033(2) 0.38068(14) 0.0230(7) Uani 1 1 d . A 2
H17A H 1.1946 0.1142 0.3730 0.028 Uiso 1 1 calc R A 2
H17B H 1.1318 0.0740 0.4159 0.028 Uiso 1 1 calc R A 2
C18 C 1.09953(18) 0.05047(19) 0.33551(13) 0.0200(6) Uani 1 1 d . A 2
C19 C 1.08359(18) 0.08312(19) 0.28445(14) 0.0208(6) Uani 1 1 d . A 2
H19 H 1.0982 0.1379 0.2765 0.025 Uiso 1 1 calc R A 2
C20 C 1.04597(19) 0.03488(19) 0.24504(13) 0.0210(7) Uani 1 1 d . A 2
C21 C 1.0195(2) -0.04439(19) 0.25550(14) 0.0236(7) Uani 1 1 d . A 2
H21 H 0.9929 -0.0754 0.2279 0.028 Uiso 1 1 calc R A 2
C22 C 1.0328(2) -0.07729(19) 0.30686(14) 0.0225(7) Uani 1 1 d . A 2
C23 C 1.07565(19) -0.03051(19) 0.34582(14) 0.0217(7) Uani 1 1 d . A 2
C24 C 1.1724(3) -0.0950(3) 0.40226(18) 0.0409(10) Uani 1 1 d . A 2
H24A H 1.1795 -0.1419 0.3779 0.061 Uiso 1 1 calc R A 2
H24B H 1.1814 -0.1121 0.4402 0.061 Uiso 1 1 calc R A 2
H24C H 1.2125 -0.0526 0.3926 0.061 Uiso 1 1 calc R A 2
C25 C 0.9945(2) -0.1585(2) 0.32307(15) 0.0278(8) Uani 1 1 d . A 2
H25A H 0.9757 -0.1879 0.2900 0.033 Uiso 1 1 calc R A 2
H25B H 1.0363 -0.1925 0.3419 0.033 Uiso 1 1 calc R A 2
C26 C 0.9220(2) -0.1432(2) 0.36059(16) 0.0324(8) Uani 1 1 d . A 2
C27 C 0.9255(3) -0.1613(2) 0.41625(17) 0.0351(9) Uani 1 1 d . A 2
H27 H 0.9720 -0.1894 0.4307 0.042 Uiso 1 1 calc R A 2
C28 C 0.8614(2) -0.1380(2) 0.45033(16) 0.0347(9) Uani 1 1 d . A 2
H28 H 0.8634 -0.1522 0.4879 0.042 Uiso 1 1 calc R A 2
C29 C 0.7953(2) -0.0952(2) 0.43096(15) 0.0323(8) Uani 1 1 d . A 2
H29 H 0.7531 -0.0783 0.4555 0.039 Uiso 1 1 calc R A 2
C30 C 0.7888(2) -0.0759(2) 0.37545(15) 0.0310(8) Uani 1 1 d . A 2
C31 C 0.8510(2) -0.10325(19) 0.34104(13) 0.0226(7) Uani 1 1 d . A 2
C32 C 0.7998(3) -0.1502(3) 0.25540(18) 0.0526(12) Uani 1 1 d . A 2
H32A H 0.8261 -0.2035 0.2607 0.079 Uiso 1 1 calc R A 2
H32B H 0.7991 -0.1369 0.2164 0.079 Uiso 1 1 calc R A 2
H32C H 0.7429 -0.1520 0.2692 0.079 Uiso 1 1 calc R A 2
C1G C 0.3980(2) 0.1210(2) 0.44144(17) 0.0255(8) Uani 0.860(3) 1 d PD B 1
H1G H 0.4175 0.1253 0.4028 0.031 Uiso 0.860(3) 1 calc PR B 1
Cl1G Cl 0.32071(11) 0.19542(9) 0.45235(12) 0.0385(4) Uani 0.860(3) 1 d PD B 1
Cl2G Cl 0.35765(10) 0.02379(7) 0.45160(6) 0.0553(4) Uani 0.860(3) 1 d PD B 1
Cl3G Cl 0.48211(8) 0.13999(11) 0.48470(5) 0.0562(5) Uani 0.860(3) 1 d PD B 1
C1H C 0.4171(8) 0.1415(7) 0.4450(8) 0.0255(8) Uani 0.140(3) 1 d PD B 2
H1H H 0.4234 0.1309 0.4050 0.031 Uiso 0.140(3) 1 calc PR B 2
Cl1H Cl 0.3167(6) 0.1758(8) 0.4546(9) 0.0385(4) Uani 0.140(3) 1 d PD B 2
Cl2H Cl 0.4891(4) 0.2157(4) 0.4617(3) 0.039(2) Uani 0.140(3) 1 d PD B 2
Cl3H Cl 0.4341(7) 0.0500(4) 0.4777(4) 0.072(4) Uani 0.140(3) 1 d PD B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0252(12) 0.0346(14) 0.0233(12) 0.0056(10) 0.0074(10) 0.0108(10)
O2 0.0214(11) 0.0169(11) 0.0229(11) 0.0060(9) -0.0017(9) -0.0014(9)
O3 0.0244(12) 0.0234(12) 0.0332(13) 0.0058(10) -0.0001(10) 0.0025(9)
O4 0.0365(14) 0.0384(14) 0.0281(13) -0.0041(11) 0.0021(11) -0.0113(12)
O5 0.0383(16) 0.070(2) 0.0254(14) 0.0077(14) 0.0037(12) 0.0016(15)
O6 0.0520(18) 0.068(2) 0.0338(16) 0.0260(15) -0.0051(13) -0.0182(16)
O7 0.076(2) 0.0220(14) 0.0365(15) 0.0055(11) -0.0083(14) -0.0047(13)
O8 0.0447(16) 0.0309(14) 0.0265(13) -0.0049(11) -0.0034(11) -0.0002(12)
N1 0.0205(15) 0.062(2) 0.0237(16) 0.0110(16) -0.0023(12) -0.0043(15)
N2 0.0262(15) 0.0252(15) 0.0268(15) -0.0010(12) 0.0037(12) 0.0018(12)
C1 0.0172(15) 0.044(2) 0.0238(17) 0.0004(15) 0.0016(13) -0.0061(15)
C2 0.0116(14) 0.0391(19) 0.0235(16) 0.0074(14) 0.0019(12) 0.0015(13)
C3 0.0143(15) 0.046(2) 0.0240(17) 0.0054(15) -0.0024(12) 0.0022(14)
C4 0.0177(16) 0.048(2) 0.0199(16) 0.0155(15) 0.0013(13) 0.0051(15)
C5 0.0198(16) 0.0368(19) 0.0264(18) 0.0134(15) -0.0007(13) 0.0067(14)
C6 0.0201(16) 0.0310(18) 0.0260(17) 0.0048(14) 0.0011(13) 0.0129(14)
C7 0.0173(15) 0.0321(18) 0.0232(17) 0.0089(14) 0.0036(12) 0.0107(13)
C8 0.036(2) 0.048(2) 0.040(2) 0.0077(19) 0.0201(18) 0.0179(18)
C9 0.0338(19) 0.0240(17) 0.0286(18) 0.0015(14) 0.0059(15) 0.0117(15)
C10 0.0361(18) 0.0171(15) 0.0169(15) -0.0020(12) 0.0013(13) 0.0051(14)
C11 0.049(2) 0.0170(16) 0.0235(17) -0.0005(13) 0.0019(15) 0.0043(15)
C12 0.051(2) 0.0165(15) 0.0247(17) 0.0017(13) 0.0005(16) -0.0116(15)
C13 0.0287(17) 0.0275(17) 0.0241(17) -0.0013(14) -0.0013(14) -0.0097(14)
C14 0.0254(16) 0.0200(16) 0.0179(15) -0.0009(12) -0.0038(12) -0.0023(13)
C15 0.0275(16) 0.0137(14) 0.0156(14) 0.0013(11) -0.0021(12) -0.0021(12)
C16 0.0307(19) 0.035(2) 0.0299(19) 0.0172(15) -0.0056(15) -0.0079(15)
C17 0.0162(15) 0.0219(16) 0.0310(17) 0.0005(13) -0.0036(13) -0.0013(12)
C18 0.0135(14) 0.0180(15) 0.0285(17) -0.0005(12) 0.0006(12) 0.0019(12)
C19 0.0155(14) 0.0157(14) 0.0311(17) -0.0010(13) 0.0037(12) -0.0012(11)
C20 0.0186(15) 0.0201(15) 0.0244(16) 0.0005(13) 0.0056(12) 0.0018(12)
C21 0.0227(16) 0.0179(15) 0.0300(17) -0.0053(13) 0.0051(13) 0.0004(12)
C22 0.0218(15) 0.0140(15) 0.0317(18) -0.0027(13) 0.0071(13) 0.0025(12)
C23 0.0174(15) 0.0184(15) 0.0293(17) 0.0032(13) 0.0044(12) 0.0037(12)
C24 0.038(2) 0.038(2) 0.046(2) 0.0101(18) -0.0021(18) 0.0150(18)
C25 0.0317(19) 0.0142(15) 0.038(2) -0.0006(14) 0.0051(15) -0.0015(13)
C26 0.036(2) 0.0226(17) 0.038(2) -0.0008(15) 0.0042(16) -0.0081(15)
C27 0.040(2) 0.0236(18) 0.042(2) 0.0051(16) -0.0012(17) -0.0064(16)
C28 0.033(2) 0.038(2) 0.0329(19) -0.0057(16) 0.0005(16) -0.0140(16)
C29 0.034(2) 0.035(2) 0.0284(19) -0.0014(15) 0.0050(15) -0.0113(16)
C30 0.0294(18) 0.0324(19) 0.0312(19) 0.0015(15) 0.0034(15) -0.0125(15)
C31 0.0273(17) 0.0184(15) 0.0221(16) 0.0004(12) 0.0041(13) -0.0102(13)
C32 0.070(3) 0.059(3) 0.029(2) -0.008(2) 0.008(2) -0.019(2)
C1G 0.025(2) 0.032(2) 0.0197(17) -0.0045(16) -0.0048(15) -0.0053(16)
Cl1G 0.0513(6) 0.0347(10) 0.0294(6) -0.0034(9) -0.0034(5) 0.0135(6)
Cl2G 0.0739(10) 0.0271(6) 0.0650(9) 0.0000(6) 0.0171(7) -0.0068(6)
Cl3G 0.0318(6) 0.1002(12) 0.0365(7) -0.0154(7) -0.0104(5) 0.0003(7)
C1H 0.025(2) 0.032(2) 0.0197(17) -0.0045(16) -0.0048(15) -0.0053(16)
Cl1H 0.0513(6) 0.0347(10) 0.0294(6) -0.0034(9) -0.0034(5) 0.0135(6)
Cl2H 0.031(3) 0.040(4) 0.045(4) 0.002(3) 0.005(3) -0.005(3)
Cl3H 0.125(10) 0.041(5) 0.049(5) 0.017(4) 0.007(5) 0.026(5)

_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 C7 1.382(4) . ?
O1 C8 1.443(4) . ?
O2 C15 1.385(4) . ?
O2 C16 1.435(4) . ?
O3 C23 1.378(4) . ?
O3 C24 1.426(5) . ?
O4 C31 1.394(4) . ?
O4 C32 1.466(5) . ?
O5 N1 1.229(5) . ?
O6 N1 1.238(5) . ?
O7 N2 1.223(4) . ?
O8 N2 1.227(4) . ?
N1 C4 1.458(4) . ?
N2 C20 1.468(4) . ?
C1 C2 1.526(5) . ?
C1 C30 1.522(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.390(5) . ?
C2 C7 1.400(5) . ?
C3 C4 1.383(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C9 1.521(5) . ?
C7 C6 1.404(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.509(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.397(4) . ?
C10 C11 1.392(5) . ?
C11 C12 1.379(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(5) . ?
C13 H13 0.9500 . ?
C14 C17 1.522(4) . ?
C15 C14 1.399(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.520(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.384(5) . ?
C19 C20 1.388(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.393(5) . ?
C21 C22 1.385(5) . ?
C21 H21 0.9500 . ?
C22 C25 1.522(4) . ?
C23 C22 1.406(5) . ?
C23 C18 1.407(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.509(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.396(6) . ?
C27 C28 1.384(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.363(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.399(5) . ?
C29 H29 0.9500 . ?
C31 C30 1.386(5) . ?
C31 C26 1.405(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C1G Cl2G 1.742(4) . ?
C1G Cl3G 1.750(4) . ?
C1G Cl1G 1.767(4) . ?
C1G H1G 1.0000 . ?
C1H Cl3H 1.725(10) . ?
C1H Cl2H 1.732(10) . ?
C1H Cl1H 1.733(10) . ?
C1H H1H 1.0000 . ?

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
C7 O1 C8 111.8(3) . . ?
C15 O2 C16 113.7(2) . . ?
C23 O3 C24 113.1(3) . . ?
C31 O4 C32 112.8(3) . . ?
O5 N1 O6 123.4(3) . . ?
O5 N1 C4 118.1(3) . . ?
O6 N1 C4 118.5(4) . . ?
O7 N2 O8 122.8(3) . . ?
O7 N2 C20 118.6(3) . . ?
O8 N2 C20 118.6(3) . . ?
O1 C7 C2 118.1(3) . . ?
O1 C7 C6 119.5(3) . . ?
C2 C7 C6 122.3(3) . . ?
C3 C2 C7 118.3(3) . . ?
C3 C2 C1 120.4(3) . . ?
C7 C2 C1 121.0(3) . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 123.2(3) . . ?
C3 C4 N1 118.6(3) . . ?
C5 C4 N1 118.2(3) . . ?
C4 C5 C6 118.7(3) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C5 C6 C7 118.5(3) . . ?
C5 C6 C9 119.5(3) . . ?
C7 C6 C9 121.8(3) . . ?
C10 C9 C6 110.9(3) . . ?
C10 C9 H9A 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 108.0 . . ?
O2 C15 C10 118.6(3) . . ?
O2 C15 C14 119.3(3) . . ?
C10 C15 C14 121.8(3) . . ?
C11 C10 C15 117.7(3) . . ?
C11 C10 C9 122.5(3) . . ?
C15 C10 C9 119.8(3) . . ?
C12 C11 C10 121.4(3) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C14 120.3(3) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C15 118.5(3) . . ?
C13 C14 C17 122.4(3) . . ?
C15 C14 C17 118.9(3) . . ?
C18 C17 C14 110.6(3) . . ?
C18 C17 H17A 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
O3 C23 C22 118.8(3) . . ?
O3 C23 C18 119.2(3) . . ?
C22 C23 C18 122.0(3) . . ?
C19 C18 C23 118.5(3) . . ?
C19 C18 C17 120.5(3) . . ?
C23 C18 C17 120.9(3) . . ?
C18 C19 C20 119.2(3) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C19 C20 C21 122.6(3) . . ?
C19 C20 N2 118.7(3) . . ?
C21 C20 N2 118.6(3) . . ?
C22 C21 C20 118.9(3) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C21 C22 C23 118.6(3) . . ?
C21 C22 C25 121.0(3) . . ?
C23 C22 C25 120.1(3) . . ?
C26 C25 C22 109.2(3) . . ?
C26 C25 H25A 109.8 . . ?
C22 C25 H25A 109.8 . . ?
C26 C25 H25B 109.8 . . ?
C22 C25 H25B 109.8 . . ?
H25A C25 H25B 108.3 . . ?
C30 C31 O4 120.2(3) . . ?
C30 C31 C26 122.4(3) . . ?
O4 C31 C26 117.4(3) . . ?
C27 C26 C31 117.7(3) . . ?
C27 C26 C25 121.8(4) . . ?
C31 C26 C25 120.2(3) . . ?
C28 C27 C26 120.0(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 121.2(4) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 120.9(4) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C31 C30 C29 117.6(4) . . ?
C31 C30 C1 120.5(3) . . ?
C29 C30 C1 121.7(3) . . ?
C30 C1 C2 110.4(3) . . ?
C30 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
C30 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C32 H32A 109.5 . . ?
O4 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O4 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Cl2G C1G Cl3G 111.5(2) . . ?
Cl2G C1G Cl1G 110.3(2) . . ?
Cl3G C1G Cl1G 109.5(2) . . ?
Cl2G C1G H1G 108.5 . . ?
Cl3G C1G H1G 108.5 . . ?
Cl1G C1G H1G 108.5 . . ?
Cl3H C1H Cl2H 113.3(8) . . ?
Cl3H C1H Cl1H 111.6(8) . . ?
Cl2H C1H Cl1H 111.6(8) . . ?
Cl3H C1H H1H 106.6 . . ?
Cl2H C1H H1H 106.6 . . ?
Cl1H C1H H1H 106.6 . . ?

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
C8 O1 C7 C2 -95.7(4) . . . . ?
C8 O1 C7 C6 88.7(4) . . . . ?
O1 C7 C2 C3 -179.0(3) . . . . ?
C6 C7 C2 C3 -3.5(5) . . . . ?
O1 C7 C2 C1 -5.3(4) . . . . ?
C6 C7 C2 C1 170.2(3) . . . . ?
C7 C2 C3 C4 0.7(5) . . . . ?
C1 C2 C3 C4 -173.0(3) . . . . ?
C2 C3 C4 C5 1.9(5) . . . . ?
C2 C3 C4 N1 -179.6(3) . . . . ?
O5 N1 C4 C3 -21.4(5) . . . . ?
O6 N1 C4 C3 158.0(3) . . . . ?
O5 N1 C4 C5 157.1(3) . . . . ?
O6 N1 C4 C5 -23.5(5) . . . . ?
C3 C4 C5 C6 -1.7(5) . . . . ?
N1 C4 C5 C6 179.8(3) . . . . ?
C4 C5 C6 C7 -1.1(5) . . . . ?
C4 C5 C6 C9 173.9(3) . . . . ?
O1 C7 C6 C5 179.1(3) . . . . ?
C2 C7 C6 C5 3.7(5) . . . . ?
O1 C7 C6 C9 4.3(5) . . . . ?
C2 C7 C6 C9 -171.1(3) . . . . ?
C5 C6 C9 C10 -54.6(4) . . . . ?
C7 C6 C9 C10 120.1(3) . . . . ?
C16 O2 C15 C10 -93.8(3) . . . . ?
C16 O2 C15 C14 92.0(3) . . . . ?
O2 C15 C10 C11 -177.9(3) . . . . ?
C14 C15 C10 C11 -3.9(5) . . . . ?
O2 C15 C10 C9 1.5(4) . . . . ?
C14 C15 C10 C9 175.6(3) . . . . ?
C6 C9 C10 C11 122.0(3) . . . . ?
C6 C9 C10 C15 -57.4(4) . . . . ?
C15 C10 C11 C12 1.0(5) . . . . ?
C9 C10 C11 C12 -178.4(3) . . . . ?
C10 C11 C12 C13 1.6(5) . . . . ?
C11 C12 C13 C14 -1.5(5) . . . . ?
C12 C13 C14 C15 -1.3(5) . . . . ?
C12 C13 C14 C17 174.2(3) . . . . ?
O2 C15 C14 C13 178.0(3) . . . . ?
C10 C15 C14 C13 4.0(5) . . . . ?
O2 C15 C14 C17 2.4(4) . . . . ?
C10 C15 C14 C17 -171.6(3) . . . . ?
C13 C14 C17 C18 -117.1(3) . . . . ?
C15 C14 C17 C18 58.3(4) . . . . ?
C24 O3 C23 C22 99.8(4) . . . . ?
C24 O3 C23 C18 -83.8(4) . . . . ?
O3 C23 C18 C19 -179.5(3) . . . . ?
C22 C23 C18 C19 -3.1(5) . . . . ?
O3 C23 C18 C17 -4.5(4) . . . . ?
C22 C23 C18 C17 171.8(3) . . . . ?
C14 C17 C18 C19 47.3(4) . . . . ?
C14 C17 C18 C23 -127.6(3) . . . . ?
C23 C18 C19 C20 -1.0(4) . . . . ?
C17 C18 C19 C20 -176.0(3) . . . . ?
C18 C19 C20 C21 3.3(5) . . . . ?
C18 C19 C20 N2 -179.9(3) . . . . ?
O7 N2 C20 C19 -11.4(5) . . . . ?
O8 N2 C20 C19 169.3(3) . . . . ?
O7 N2 C20 C21 165.5(3) . . . . ?
O8 N2 C20 C21 -13.8(4) . . . . ?
C19 C20 C21 C22 -1.4(5) . . . . ?
N2 C20 C21 C22 -178.2(3) . . . . ?
C20 C21 C22 C23 -2.6(5) . . . . ?
C20 C21 C22 C25 171.1(3) . . . . ?
O3 C23 C22 C21 -178.7(3) . . . . ?
C18 C23 C22 C21 5.0(5) . . . . ?
O3 C23 C22 C25 7.5(4) . . . . ?
C18 C23 C22 C25 -168.8(3) . . . . ?
C21 C22 C25 C26 -104.2(4) . . . . ?
C23 C22 C25 C26 69.5(4) . . . . ?
C32 O4 C31 C30 -87.0(4) . . . . ?
C32 O4 C31 C26 96.1(4) . . . . ?
C30 C31 C26 C27 5.3(5) . . . . ?
O4 C31 C26 C27 -177.9(3) . . . . ?
C30 C31 C26 C25 -169.2(3) . . . . ?
O4 C31 C26 C25 7.7(5) . . . . ?
C22 C25 C26 C27 -108.2(4) . . . . ?
C22 C25 C26 C31 66.0(4) . . . . ?
C31 C26 C27 C28 -1.6(5) . . . . ?
C25 C26 C27 C28 172.8(3) . . . . ?
C26 C27 C28 C29 -2.1(6) . . . . ?
C27 C28 C29 C30 2.4(6) . . . . ?
O4 C31 C30 C29 178.2(3) . . . . ?
C26 C31 C30 C29 -5.1(5) . . . . ?
O4 C31 C30 C1 -6.7(5) . . . . ?
C26 C31 C30 C1 170.0(3) . . . . ?
C28 C29 C30 C31 1.2(5) . . . . ?
C28 C29 C30 C1 -173.8(3) . . . . ?
C31 C30 C1 C2 -64.1(4) . . . . ?
C29 C30 C1 C2 110.7(4) . . . . ?
C3 C2 C1 C30 98.6(4) . . . . ?
C7 C2 C1 C30 -74.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.10
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 870204'