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

#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36.50 H31 Cl O2'
_chemical_formula_weight         537.06

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'
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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.1923(18)
_cell_length_b                   9.5033(19)
_cell_length_c                   17.017(3)
_cell_angle_alpha                75.35(3)
_cell_angle_beta                 77.27(3)
_cell_angle_gamma                84.99(3)
_cell_volume                     1402.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3706
_cell_measurement_theta_min      2.2164
_cell_measurement_theta_max      27.8601

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             566
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9671
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_process_details   crystalclear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13386
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.89
_reflns_number_total             6519
_reflns_number_gt                3602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       crystalclear
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0995P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6519
_refine_ls_number_parameters     369
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.1890
_refine_ls_wR_factor_gt          0.1685
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.030
_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 0.86265(17) 0.8379(2) 0.36598(11) 0.0415(4) Uani 1 1 d . . .
O2 O 0.27688(17) 0.67652(19) 0.48300(10) 0.0380(4) Uani 1 1 d . . .
C1 C 0.4092(2) 0.7699(3) 0.59232(14) 0.0337(5) Uani 1 1 d . . .
H1A H 0.3455 0.8599 0.5872 0.040 Uiso 1 1 calc R . .
H1B H 0.3432 0.6862 0.6166 0.040 Uiso 1 1 calc R . .
C2 C 0.4945(2) 0.7591(2) 0.50590(13) 0.0263(5) Uani 1 1 d . . .
C3 C 0.6419(2) 0.8011(2) 0.47620(14) 0.0295(5) Uani 1 1 d . . .
H3 H 0.6922 0.8331 0.5114 0.035 Uiso 1 1 calc R . .
C4 C 0.7171(2) 0.7972(2) 0.39642(14) 0.0290(5) Uani 1 1 d . . .
C5 C 0.6479(2) 0.7500(2) 0.34334(13) 0.0267(5) Uani 1 1 d . . .
C6 C 0.5001(2) 0.7076(2) 0.37304(13) 0.0274(5) Uani 1 1 d . . .
H6 H 0.4502 0.6749 0.3380 0.033 Uiso 1 1 calc R . .
C7 C 0.4244(2) 0.7121(2) 0.45284(13) 0.0264(5) Uani 1 1 d . . .
C8 C 0.9321(3) 0.8990(4) 0.41624(19) 0.0532(8) Uani 1 1 d . . .
H8A H 0.8744 0.9857 0.4280 0.080 Uiso 1 1 calc R . .
H8B H 1.0337 0.9261 0.3867 0.080 Uiso 1 1 calc R . .
H8C H 0.9360 0.8272 0.4685 0.080 Uiso 1 1 calc R . .
C9 C 0.2109(3) 0.6014(3) 0.43741(17) 0.0466(7) Uani 1 1 d . . .
H9A H 0.2061 0.6651 0.3828 0.070 Uiso 1 1 calc R . .
H9B H 0.1098 0.5740 0.4678 0.070 Uiso 1 1 calc R . .
H9C H 0.2714 0.5136 0.4304 0.070 Uiso 1 1 calc R . .
C10 C 0.7273(3) 0.7469(2) 0.25622(13) 0.0302(5) Uani 1 1 d . . .
H10A H 0.7838 0.8371 0.2317 0.036 Uiso 1 1 calc R . .
H10B H 0.6512 0.7481 0.2229 0.036 Uiso 1 1 calc R . .
C11 C 0.8349(2) 0.6171(2) 0.24801(13) 0.0253(5) Uani 1 1 d . . .
C12 C 0.8777(2) 0.5197(2) 0.31532(13) 0.0285(5) Uani 1 1 d . . .
H12 H 0.8398 0.5333 0.3696 0.034 Uiso 1 1 calc R . .
C13 C 0.9748(2) 0.4027(2) 0.30475(13) 0.0279(5) Uani 1 1 d . . .
H13 H 1.0030 0.3383 0.3519 0.033 Uiso 1 1 calc R . .
C14 C 1.0320(2) 0.3775(2) 0.22615(13) 0.0248(5) Uani 1 1 d . . .
C15 C 0.9909(2) 0.4773(2) 0.15839(14) 0.0302(5) Uani 1 1 d . . .
H15 H 1.0299 0.4649 0.1039 0.036 Uiso 1 1 calc R . .
C16 C 0.8945(3) 0.5939(2) 0.16936(13) 0.0305(5) Uani 1 1 d . . .
H16 H 0.8681 0.6600 0.1221 0.037 Uiso 1 1 calc R . .
C17 C 1.1330(2) 0.2470(2) 0.21819(13) 0.0255(5) Uani 1 1 d . . .
C18 C 1.2627(2) 0.2340(2) 0.25926(13) 0.0252(5) Uani 1 1 d . . .
C19 C 1.3373(2) 0.3590(2) 0.25418(14) 0.0296(5) Uani 1 1 d . . .
H19 H 1.3110 0.4484 0.2195 0.035 Uiso 1 1 calc R . .
C20 C 1.4477(2) 0.3572(2) 0.29774(14) 0.0302(5) Uani 1 1 d . . .
H20 H 1.4964 0.4444 0.2921 0.036 Uiso 1 1 calc R . .
C21 C 1.4883(2) 0.2284(2) 0.35010(13) 0.0276(5) Uani 1 1 d . . .
C22 C 1.4218(2) 0.1016(2) 0.35176(13) 0.0298(5) Uani 1 1 d . . .
H22 H 1.4529 0.0114 0.3838 0.036 Uiso 1 1 calc R . .
C23 C 1.3112(2) 0.1037(2) 0.30779(13) 0.0278(5) Uani 1 1 d . . .
H23 H 1.2674 0.0152 0.3106 0.033 Uiso 1 1 calc R . .
C24 C 1.1037(2) 0.1500(2) 0.17805(13) 0.0246(5) Uani 1 1 d . . .
C25 C 1.2039(2) 0.0194(2) 0.16725(13) 0.0248(5) Uani 1 1 d . . .
C26 C 1.1451(2) -0.1180(2) 0.20051(14) 0.0290(5) Uani 1 1 d . . .
H26 H 1.0436 -0.1268 0.2285 0.035 Uiso 1 1 calc R . .
C27 C 1.2323(3) -0.2418(2) 0.19339(15) 0.0337(5) Uani 1 1 d . . .
H27 H 1.1913 -0.3351 0.2175 0.040 Uiso 1 1 calc R . .
C28 C 1.3782(3) -0.2301(2) 0.15140(15) 0.0342(6) Uani 1 1 d . . .
H28 H 1.4384 -0.3153 0.1465 0.041 Uiso 1 1 calc R . .
C29 C 1.4373(3) -0.0943(3) 0.11630(15) 0.0357(6) Uani 1 1 d . . .
H29 H 1.5377 -0.0861 0.0863 0.043 Uiso 1 1 calc R . .
C30 C 1.3506(2) 0.0301(2) 0.12469(14) 0.0303(5) Uani 1 1 d . . .
H30 H 1.3923 0.1232 0.1011 0.036 Uiso 1 1 calc R . .
C31 C 0.9700(2) 0.1600(2) 0.14071(13) 0.0264(5) Uani 1 1 d . . .
C32 C 0.8257(2) 0.1673(2) 0.18693(14) 0.0311(5) Uani 1 1 d . . .
H32 H 0.8097 0.1685 0.2438 0.037 Uiso 1 1 calc R . .
C33 C 0.7039(3) 0.1729(3) 0.14895(16) 0.0371(6) Uani 1 1 d . . .
H33 H 0.6050 0.1781 0.1801 0.045 Uiso 1 1 calc R . .
C34 C 0.7281(3) 0.1707(3) 0.06505(15) 0.0366(6) Uani 1 1 d . . .
H34 H 0.6456 0.1747 0.0393 0.044 Uiso 1 1 calc R . .
C35 C 0.8687(3) 0.1628(3) 0.02076(15) 0.0396(6) Uani 1 1 d . . .
H35 H 0.8844 0.1629 -0.0363 0.047 Uiso 1 1 calc R . .
C36 C 0.9898(3) 0.1546(3) 0.05770(14) 0.0332(5) Uani 1 1 d . . .
H36 H 1.0877 0.1453 0.0263 0.040 Uiso 1 1 calc R . .
Cl1 Cl 0.3162(7) 0.4405(9) -0.0400(5) 0.0737(7) Uani 0.25 1 d PDU A -1
Cl2 Cl 0.5882(12) 0.5456(14) -0.0249(7) 0.0737(7) Uani 0.25 1 d PDU A -1
C37 C 0.3982(14) 0.509(2) 0.0285(9) 0.0737(7) Uani 0.25 1 d PDU A -1
H37A H 0.3950 0.4365 0.0819 0.088 Uiso 0.25 1 calc PR A -1
H37B H 0.3447 0.5995 0.0396 0.088 Uiso 0.25 1 calc PR A -1
Cl1' Cl 0.3334(7) 0.4116(8) -0.0221(5) 0.0737(7) Uani 0.25 1 d PDU B -2
Cl2' Cl 0.5862(11) 0.5627(13) -0.0117(7) 0.0737(7) Uani 0.25 1 d PDU B -2
C37' C 0.4247(17) 0.470(2) 0.0452(9) 0.0737(7) Uani 0.25 1 d PDU B -2
H37C H 0.3564 0.5356 0.0746 0.088 Uiso 0.25 1 calc PR B -2
H37D H 0.4518 0.3851 0.0873 0.088 Uiso 0.25 1 calc PR B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C4 1.375(3) . ?
O1 C8 1.426(3) . ?
O2 C7 1.379(3) . ?
O2 C9 1.429(3) . ?
C1 C21 1.505(3) 2_766 ?
C1 C2 1.531(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.393(3) . ?
C2 C7 1.393(3) . ?
C3 C4 1.389(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C5 C6 1.398(3) . ?
C5 C10 1.508(3) . ?
C6 C7 1.392(3) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.527(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.387(3) . ?
C11 C16 1.395(3) . ?
C12 C13 1.387(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.397(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.395(3) . ?
C14 C17 1.499(3) . ?
C15 C16 1.382(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C24 1.353(3) . ?
C17 C18 1.491(3) . ?
C18 C19 1.397(3) . ?
C18 C23 1.401(3) . ?
C19 C20 1.379(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.396(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.389(3) . ?
C21 C1 1.505(3) 2_766 ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C31 1.489(3) . ?
C24 C25 1.505(3) . ?
C25 C30 1.382(3) . ?
C25 C26 1.389(3) . ?
C26 C27 1.381(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.374(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.391(3) . ?
C31 C36 1.397(3) . ?
C32 C33 1.401(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.401(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.352(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.381(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
Cl1 C37 1.792(9) . ?
Cl2 C37 1.800(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
Cl1' C37' 1.776(9) . ?
Cl2' C37' 1.754(9) . ?
C37' H37C 0.9900 . ?
C37' H37D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 O1 C8 117.71(19) . . ?
C7 O2 C9 117.34(18) . . ?
C21 C1 C2 112.43(18) 2_766 . ?
C21 C1 H1A 109.1 2_766 . ?
C2 C1 H1A 109.1 . . ?
C21 C1 H1B 109.1 2_766 . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C7 117.71(19) . . ?
C3 C2 C1 121.6(2) . . ?
C7 C2 C1 120.6(2) . . ?
C4 C3 C2 121.6(2) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
O1 C4 C3 122.5(2) . . ?
O1 C4 C5 116.5(2) . . ?
C3 C4 C5 121.0(2) . . ?
C4 C5 C6 117.57(19) . . ?
C4 C5 C10 121.6(2) . . ?
C6 C5 C10 120.8(2) . . ?
C7 C6 C5 121.5(2) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
O2 C7 C6 123.0(2) . . ?
O2 C7 C2 116.26(19) . . ?
C6 C7 C2 120.7(2) . . ?
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 C9 H9A 109.5 . . ?
O2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 C11 115.80(18) . . ?
C5 C10 H10A 108.3 . . ?
C11 C10 H10A 108.3 . . ?
C5 C10 H10B 108.3 . . ?
C11 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C12 C11 C16 117.52(18) . . ?
C12 C11 C10 123.28(18) . . ?
C16 C11 C10 119.20(19) . . ?
C13 C12 C11 121.14(19) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 121.4(2) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 117.34(18) . . ?
C15 C14 C17 123.28(18) . . ?
C13 C14 C17 119.38(19) . . ?
C16 C15 C14 120.94(19) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C11 121.6(2) . . ?
C15 C16 H16 119.2 . . ?
C11 C16 H16 119.2 . . ?
C24 C17 C18 124.41(18) . . ?
C24 C17 C14 121.30(19) . . ?
C18 C17 C14 114.28(17) . . ?
C19 C18 C23 116.5(2) . . ?
C19 C18 C17 119.37(19) . . ?
C23 C18 C17 124.0(2) . . ?
C20 C19 C18 122.4(2) . . ?
C20 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C19 C20 C21 120.5(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 117.7(2) . . ?
C22 C21 C1 121.5(2) . 2_766 ?
C20 C21 C1 120.7(2) . 2_766 ?
C23 C22 C21 121.5(2) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C18 121.2(2) . . ?
C22 C23 H23 119.4 . . ?
C18 C23 H23 119.4 . . ?
C17 C24 C31 124.08(18) . . ?
C17 C24 C25 122.93(19) . . ?
C31 C24 C25 112.99(17) . . ?
C30 C25 C26 118.69(19) . . ?
C30 C25 C24 123.0(2) . . ?
C26 C25 C24 118.35(19) . . ?
C27 C26 C25 120.9(2) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C28 C27 C26 120.0(2) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.8(2) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 120.2(2) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C25 C30 C29 120.4(2) . . ?
C25 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C32 C31 C36 118.9(2) . . ?
C32 C31 C24 122.06(19) . . ?
C36 C31 C24 118.97(19) . . ?
C31 C32 C33 119.5(2) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C34 C33 C32 120.0(2) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.1(2) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.7(2) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.8(2) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
Cl1 C37 Cl2 105.4(6) . . ?
Cl1 C37 H37A 110.7 . . ?
Cl2 C37 H37A 110.7 . . ?
Cl1 C37 H37B 110.7 . . ?
Cl2 C37 H37B 110.7 . . ?
H37A C37 H37B 108.8 . . ?
Cl2' C37' Cl1' 110.2(7) . . ?
Cl2' C37' H37C 109.6 . . ?
Cl1' C37' H37C 109.6 . . ?
Cl2' C37' H37D 109.6 . . ?
Cl1' C37' H37D 109.6 . . ?
H37C C37' H37D 108.1 . . ?

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
C21 C1 C2 C3 -22.4(3) 2_766 . . . ?
C21 C1 C2 C7 160.3(2) 2_766 . . . ?
C7 C2 C3 C4 0.3(3) . . . . ?
C1 C2 C3 C4 -177.1(2) . . . . ?
C8 O1 C4 C3 -6.1(3) . . . . ?
C8 O1 C4 C5 174.5(2) . . . . ?
C2 C3 C4 O1 -179.8(2) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
O1 C4 C5 C6 179.75(18) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
O1 C4 C5 C10 -1.4(3) . . . . ?
C3 C4 C5 C10 179.23(19) . . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C10 C5 C6 C7 -178.90(19) . . . . ?
C9 O2 C7 C6 14.4(3) . . . . ?
C9 O2 C7 C2 -167.9(2) . . . . ?
C5 C6 C7 O2 177.40(19) . . . . ?
C5 C6 C7 C2 -0.2(3) . . . . ?
C3 C2 C7 O2 -177.67(18) . . . . ?
C1 C2 C7 O2 -0.2(3) . . . . ?
C3 C2 C7 C6 0.1(3) . . . . ?
C1 C2 C7 C6 177.5(2) . . . . ?
C4 C5 C10 C11 80.0(3) . . . . ?
C6 C5 C10 C11 -101.2(2) . . . . ?
C5 C10 C11 C12 -10.2(3) . . . . ?
C5 C10 C11 C16 170.0(2) . . . . ?
C16 C11 C12 C13 -0.7(3) . . . . ?
C10 C11 C12 C13 179.5(2) . . . . ?
C11 C12 C13 C14 -0.7(3) . . . . ?
C12 C13 C14 C15 1.8(3) . . . . ?
C12 C13 C14 C17 -178.2(2) . . . . ?
C13 C14 C15 C16 -1.6(3) . . . . ?
C17 C14 C15 C16 178.4(2) . . . . ?
C14 C15 C16 C11 0.2(4) . . . . ?
C12 C11 C16 C15 0.9(3) . . . . ?
C10 C11 C16 C15 -179.2(2) . . . . ?
C15 C14 C17 C24 -54.0(3) . . . . ?
C13 C14 C17 C24 126.0(2) . . . . ?
C15 C14 C17 C18 127.2(2) . . . . ?
C13 C14 C17 C18 -52.8(3) . . . . ?
C24 C17 C18 C19 141.4(2) . . . . ?
C14 C17 C18 C19 -39.9(3) . . . . ?
C24 C17 C18 C23 -42.6(3) . . . . ?
C14 C17 C18 C23 136.2(2) . . . . ?
C23 C18 C19 C20 -3.3(3) . . . . ?
C17 C18 C19 C20 173.05(19) . . . . ?
C18 C19 C20 C21 -0.7(3) . . . . ?
C19 C20 C21 C22 4.6(3) . . . . ?
C19 C20 C21 C1 -170.37(19) . . . 2_766 ?
C20 C21 C22 C23 -4.5(3) . . . . ?
C1 C21 C22 C23 170.42(19) 2_766 . . . ?
C21 C22 C23 C18 0.5(3) . . . . ?
C19 C18 C23 C22 3.4(3) . . . . ?
C17 C18 C23 C22 -172.76(19) . . . . ?
C18 C17 C24 C31 176.9(2) . . . . ?
C14 C17 C24 C31 -1.7(3) . . . . ?
C18 C17 C24 C25 -2.6(3) . . . . ?
C14 C17 C24 C25 178.75(19) . . . . ?
C17 C24 C25 C30 -61.2(3) . . . . ?
C31 C24 C25 C30 119.3(2) . . . . ?
C17 C24 C25 C26 119.9(2) . . . . ?
C31 C24 C25 C26 -59.7(3) . . . . ?
C30 C25 C26 C27 1.8(3) . . . . ?
C24 C25 C26 C27 -179.2(2) . . . . ?
C25 C26 C27 C28 -1.4(3) . . . . ?
C26 C27 C28 C29 -0.1(4) . . . . ?
C27 C28 C29 C30 1.3(4) . . . . ?
C26 C25 C30 C29 -0.6(3) . . . . ?
C24 C25 C30 C29 -179.6(2) . . . . ?
C28 C29 C30 C25 -0.9(4) . . . . ?
C17 C24 C31 C32 -55.9(3) . . . . ?
C25 C24 C31 C32 123.7(2) . . . . ?
C17 C24 C31 C36 127.3(2) . . . . ?
C25 C24 C31 C36 -53.1(3) . . . . ?
C36 C31 C32 C33 -1.6(3) . . . . ?
C24 C31 C32 C33 -178.4(2) . . . . ?
C31 C32 C33 C34 0.2(4) . . . . ?
C32 C33 C34 C35 0.2(4) . . . . ?
C33 C34 C35 C36 1.0(4) . . . . ?
C34 C35 C36 C31 -2.5(4) . . . . ?
C32 C31 C36 C35 2.8(3) . . . . ?
C24 C31 C36 C35 179.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.89
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 1012065'
#######################################################################
#
#                 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_mo_dm13619_0m

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H92 O4'
_chemical_formula_weight         1213.61

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.871(5)
_cell_length_b                   11.053(5)
_cell_length_c                   15.840(7)
_cell_angle_alpha                81.772(8)
_cell_angle_beta                 77.584(8)
_cell_angle_gamma                68.140(8)
_cell_volume                     1720.9(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    1886
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      24.04

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_F_000             652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.070
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5864
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11569
_diffrn_reflns_av_unetI/netI     0.1293
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.319
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6328
_reflns_number_gt                3314
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1683P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6328
_refine_ls_number_parameters     461
_refine_ls_number_restraints     207
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.0821
_refine_ls_wR_factor_ref         0.2957
_refine_ls_wR_factor_gt          0.2314
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.029
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.6109(3) 0.1769(3) 0.59602(18) 0.0408(7) Uani 1 1 d . . . . .
O2 O 1.0919(3) 0.1755(4) 0.6577(2) 0.0724(12) Uani 1 1 d . . . . .
C1 C 0.6351(4) 0.4896(4) 0.2501(2) 0.0315(9) Uani 1 1 d . . . . .
H1 H 0.6502 0.4132 0.2885 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5155(4) 0.5968(4) 0.2684(2) 0.0329(9) Uani 1 1 d . . . . .
H2 H 0.4496 0.5911 0.3175 0.040 Uiso 1 1 calc R U . . .
C3 C 0.4933(4) 0.7109(4) 0.2150(2) 0.0359(10) Uani 1 1 d . . . . .
C4 C 0.5921(4) 0.7138(4) 0.1428(2) 0.0366(10) Uani 1 1 d . . . . .
H4 H 0.5791 0.7915 0.1057 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7074(4) 0.6077(4) 0.1239(2) 0.0307(9) Uani 1 1 d . . . . .
H5 H 0.7717 0.6129 0.0737 0.037 Uiso 1 1 calc R U . . .
C6 C 0.7321(4) 0.4920(4) 0.1772(2) 0.0294(9) Uani 1 1 d . . . . .
C7 C 0.8631(4) 0.3792(4) 0.1621(3) 0.0299(9) Uani 1 1 d . . . . .
C8 C 0.9162(4) 0.3281(4) 0.0845(3) 0.0309(9) Uani 1 1 d . . . . .
C9 C 0.8387(4) 0.3671(4) 0.0116(3) 0.0311(9) Uani 1 1 d . . . . .
C10 C 0.7121(4) 0.3551(4) 0.0209(3) 0.0422(11) Uani 1 1 d . . . . .
H10 H 0.6727 0.3251 0.0754 0.051 Uiso 1 1 calc R U . . .
C11 C 0.6449(5) 0.3862(5) -0.0479(3) 0.0518(13) Uani 1 1 d . . . . .
H11 H 0.5606 0.3750 -0.0410 0.062 Uiso 1 1 calc R U . . .
C12 C 0.6985(5) 0.4335(4) -0.1269(3) 0.0501(13) Uani 1 1 d . . . . .
H12 H 0.6504 0.4574 -0.1738 0.060 Uiso 1 1 calc R U . . .
C13 C 0.8219(5) 0.4457(4) -0.1371(3) 0.0445(11) Uani 1 1 d . . . . .
H13 H 0.8590 0.4781 -0.1914 0.053 Uiso 1 1 calc R U . . .
C14 C 0.8933(4) 0.4116(4) -0.0694(3) 0.0354(10) Uani 1 1 d . . . . .
H14 H 0.9797 0.4184 -0.0781 0.042 Uiso 1 1 calc R U . . .
C15 C 1.0533(4) 0.2252(4) 0.0658(2) 0.0295(9) Uani 1 1 d . . . . .
C16 C 1.1662(4) 0.2329(4) 0.0899(2) 0.0337(9) Uani 1 1 d . . . . .
H16 H 1.1569 0.3053 0.1198 0.040 Uiso 1 1 calc R U . . .
C17 C 1.2912(4) 0.1368(4) 0.0710(2) 0.0379(10) Uani 1 1 d . . . . .
H17 H 1.3668 0.1442 0.0878 0.046 Uiso 1 1 calc R U . . .
C18 C 1.3074(4) 0.0317(4) 0.0285(3) 0.0421(11) Uani 1 1 d . . . . .
H18 H 1.3935 -0.0348 0.0164 0.051 Uiso 1 1 calc R U . . .
C19 C 1.1972(5) 0.0229(4) 0.0030(3) 0.0467(11) Uani 1 1 d . . . . .
H19 H 1.2074 -0.0499 -0.0268 0.056 Uiso 1 1 calc R U . . .
C20 C 1.0715(4) 0.1204(4) 0.0211(3) 0.0423(11) Uani 1 1 d . . . . .
H20 H 0.9968 0.1144 0.0022 0.051 Uiso 1 1 calc R U . . .
C21 C 0.9261(4) 0.3267(4) 0.2414(2) 0.0304(9) Uani 1 1 d . . . . .
C22 C 0.9297(4) 0.4137(4) 0.2962(2) 0.0330(9) Uani 1 1 d . . . . .
H22 H 0.8967 0.5049 0.2808 0.040 Uiso 1 1 calc R U . . .
C23 C 0.9802(4) 0.3695(4) 0.3722(3) 0.0361(10) Uani 1 1 d . . . . .
H23 H 0.9818 0.4310 0.4078 0.043 Uiso 1 1 calc R U . . .
C24 C 1.0287(4) 0.2373(4) 0.3976(3) 0.0372(10) Uani 1 1 d . . . . .
C25 C 1.0262(4) 0.1516(4) 0.3436(3) 0.0380(10) Uani 1 1 d . . . . .
H25 H 1.0600 0.0604 0.3591 0.046 Uiso 1 1 calc R U . . .
C26 C 0.9756(4) 0.1945(4) 0.2671(3) 0.0345(10) Uani 1 1 d . . . . .
H26 H 0.9748 0.1324 0.2317 0.041 Uiso 1 1 calc R U . . .
C27 C 1.0723(4) 0.1903(5) 0.4847(3) 0.0476(12) Uani 1 1 d . . . . .
H27A H 1.1141 0.2488 0.4990 0.057 Uiso 1 1 calc R U . . .
H27B H 1.1416 0.1016 0.4806 0.057 Uiso 1 1 calc R U . . .
C28 C 0.9557(4) 0.1863(4) 0.5584(3) 0.0362(10) Uani 1 1 d . . . . .
C29 C 0.8357(4) 0.1853(4) 0.5416(2) 0.0302(9) Uani 1 1 d . . . . .
H29 H 0.8252 0.1873 0.4834 0.036 Uiso 1 1 calc R U . . .
C30 C 0.7306(4) 0.1815(4) 0.6087(2) 0.0350(10) Uani 1 1 d . . . . .
C31 C 0.7435(4) 0.1787(4) 0.6950(3) 0.0425(11) Uani 1 1 d . . . . .
C32 C 0.8621(5) 0.1808(4) 0.7110(3) 0.0483(13) Uani 1 1 d . . . . .
H32 H 0.8719 0.1814 0.7691 0.058 Uiso 1 1 calc R U . . .
C33 C 0.9688(4) 0.1822(5) 0.6435(3) 0.0468(12) Uani 1 1 d . . . . .
C34 C 0.6320(5) 0.1678(5) 0.7689(3) 0.0551(14) Uani 1 1 d . . . . .
H34A H 0.6041 0.0968 0.7577 0.066 Uiso 1 1 calc R U . . .
H34B H 0.6703 0.1407 0.8229 0.066 Uiso 1 1 calc R U . . .
C35 C 1.1189(9) 0.1990(11) 0.7348(7) 0.060(3) Uani 0.5 1 d D U P A 1
H35A H 1.0579 0.1739 0.7842 0.072 Uiso 0.5 1 calc R U P A 1
H35B H 1.0999 0.2937 0.7356 0.072 Uiso 0.5 1 calc R U P A 1
C36 C 1.2588(9) 0.1266(8) 0.7458(7) 0.053(2) Uani 0.5 1 d D U P A 1
H36A H 1.2705 0.1507 0.8006 0.064 Uiso 0.5 1 calc R U P A 1
H36B H 1.3175 0.1581 0.6982 0.064 Uiso 0.5 1 calc R U P A 1
C37 C 1.3105(10) -0.0204(8) 0.7476(8) 0.054(2) Uani 0.5 1 d D U P A 1
H37A H 1.2272 -0.0387 0.7505 0.065 Uiso 0.5 1 calc R U P A 1
H37B H 1.3594 -0.0367 0.6876 0.065 Uiso 0.5 1 calc R U P A 1
C38 C 1.3757(11) -0.1141(10) 0.7885(7) 0.076(3) Uani 0.5 1 d D U P A 1
H38A H 1.3154 -0.1651 0.8077 0.091 Uiso 0.5 1 calc R U P A 1
H38B H 1.3774 -0.0772 0.8415 0.091 Uiso 0.5 1 calc R U P A 1
C39 C 1.5158(14) -0.2193(16) 0.7698(13) 0.095(5) Uani 0.5 1 d D U P A 1
H39A H 1.5311 -0.2814 0.8206 0.142 Uiso 0.5 1 calc R U P A 1
H39B H 1.5842 -0.1781 0.7571 0.142 Uiso 0.5 1 calc R U P A 1
H39C H 1.5219 -0.2655 0.7199 0.142 Uiso 0.5 1 calc R U P A 1
C35' C 1.0957(8) 0.1464(10) 0.7560(6) 0.044(2) Uani 0.5 1 d D U P A 2
H35C H 1.0414 0.2268 0.7864 0.052 Uiso 0.5 1 calc R U P A 2
H35D H 1.0547 0.0793 0.7792 0.052 Uiso 0.5 1 calc R U P A 2
C36' C 1.2270(9) 0.1022(12) 0.7725(7) 0.071(3) Uani 0.5 1 d D U P A 2
H36C H 1.2212 0.0732 0.8349 0.085 Uiso 0.5 1 calc R U P A 2
H36D H 1.2534 0.1802 0.7650 0.085 Uiso 0.5 1 calc R U P A 2
C37' C 1.3428(10) -0.0018(12) 0.7263(9) 0.069(3) Uani 0.5 1 d D U P A 2
H37C H 1.3082 -0.0709 0.7207 0.083 Uiso 0.5 1 calc R U P A 2
H37D H 1.3626 0.0367 0.6669 0.083 Uiso 0.5 1 calc R U P A 2
C38' C 1.4672(9) -0.0667(9) 0.7522(7) 0.059(2) Uani 0.5 1 d D U P A 2
H38C H 1.4556 -0.0491 0.8135 0.070 Uiso 0.5 1 calc R U P A 2
H38D H 1.5297 -0.0241 0.7183 0.070 Uiso 0.5 1 calc R U P A 2
C39' C 1.5388(17) -0.2127(12) 0.7460(10) 0.091(5) Uani 0.5 1 d D U P A 2
H39D H 1.6239 -0.2402 0.7674 0.137 Uiso 0.5 1 calc R U P A 2
H39E H 1.5571 -0.2336 0.6854 0.137 Uiso 0.5 1 calc R U P A 2
H39F H 1.4817 -0.2588 0.7811 0.137 Uiso 0.5 1 calc R U P A 2
C40 C 0.5894(4) 0.1857(4) 0.5093(3) 0.0408(11) Uani 1 1 d . . . . .
H40A H 0.6478 0.1045 0.4808 0.049 Uiso 1 1 calc R U . . .
H40B H 0.6106 0.2601 0.4754 0.049 Uiso 1 1 calc R U . . .
C41 C 0.4422(4) 0.2056(4) 0.5147(3) 0.0436(11) Uani 1 1 d . . . . .
H41A H 0.4221 0.1333 0.5524 0.052 Uiso 1 1 calc R U . . .
H41B H 0.4267 0.2008 0.4561 0.052 Uiso 1 1 calc R U . . .
C42 C 0.3452(4) 0.3343(5) 0.5495(3) 0.0464(12) Uani 1 1 d . . . . .
H42A H 0.3728 0.3477 0.6021 0.056 Uiso 1 1 calc R U . . .
H42B H 0.2542 0.3290 0.5670 0.056 Uiso 1 1 calc R U . . .
C43 C 0.3376(5) 0.4524(5) 0.4852(3) 0.0531(13) Uani 1 1 d . . . . .
H43A H 0.2993 0.5323 0.5176 0.064 Uiso 1 1 calc R U . . .
H43B H 0.4301 0.4450 0.4561 0.064 Uiso 1 1 calc R U . . .
C44 C 0.2542(5) 0.4675(5) 0.4171(4) 0.0631(15) Uani 1 1 d . . . . .
H44A H 0.2925 0.3897 0.3837 0.095 Uiso 1 1 calc R U . . .
H44B H 0.2543 0.5448 0.3782 0.095 Uiso 1 1 calc R U . . .
H44C H 0.1616 0.4777 0.4451 0.095 Uiso 1 1 calc R U . . .


_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 C30 1.379(5) . ?
O1 C40 1.426(5) . ?
O2 C33 1.377(5) . ?
O2 C35 1.396(11) . ?
O2 C35' 1.551(10) . ?
C1 C6 1.391(5) . ?
C1 C2 1.402(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.386(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.397(6) . ?
C3 C34 1.519(6) 2_666 ?
C4 C5 1.372(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.502(5) . ?
C7 C8 1.347(5) . ?
C7 C21 1.499(5) . ?
C8 C9 1.494(5) . ?
C8 C15 1.499(5) . ?
C9 C14 1.396(6) . ?
C9 C10 1.406(5) . ?
C10 C11 1.374(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.370(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.374(6) . ?
C15 C16 1.395(5) . ?
C16 C17 1.380(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.362(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(6) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.389(5) . ?
C21 C22 1.400(6) . ?
C22 C23 1.380(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.376(6) . ?
C24 C27 1.513(6) . ?
C25 C26 1.387(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.537(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C33 1.378(6) . ?
C28 C29 1.391(5) . ?
C29 C30 1.392(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.399(6) . ?
C31 C32 1.375(7) . ?
C31 C34 1.520(6) . ?
C32 C33 1.401(7) . ?
C32 H32 0.9500 . ?
C34 C3 1.519(6) 2_666 ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.467(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.506(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.206(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.532(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C35' C36' 1.396(8) . ?
C35' H35C 0.9900 . ?
C35' H35D 0.9900 . ?
C36' C37' 1.486(8) . ?
C36' H36C 0.9900 . ?
C36' H36D 0.9900 . ?
C37' C38' 1.395(13) . ?
C37' H37C 0.9900 . ?
C37' H37D 0.9900 . ?
C38' C39' 1.516(9) . ?
C38' H38C 0.9900 . ?
C38' H38D 0.9900 . ?
C39' H39D 0.9800 . ?
C39' H39E 0.9800 . ?
C39' H39F 0.9800 . ?
C40 C41 1.518(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.516(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.524(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.507(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C30 O1 C40 118.4(3) . . ?
C33 O2 C35 126.0(5) . . ?
C33 O2 C35' 108.8(4) . . ?
C6 C1 C2 121.8(4) . . ?
C6 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 117.8(4) . . ?
C2 C3 C34 123.6(4) . 2_666 ?
C4 C3 C34 118.6(4) . 2_666 ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 117.1(4) . . ?
C1 C6 C7 120.7(3) . . ?
C5 C6 C7 121.9(3) . . ?
C8 C7 C21 123.5(4) . . ?
C8 C7 C6 122.4(4) . . ?
C21 C7 C6 114.1(3) . . ?
C7 C8 C9 121.7(4) . . ?
C7 C8 C15 123.1(4) . . ?
C9 C8 C15 115.2(3) . . ?
C14 C9 C10 117.9(4) . . ?
C14 C9 C8 120.5(3) . . ?
C10 C9 C8 121.5(4) . . ?
C11 C10 C9 120.7(4) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.6(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.3(4) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 121.1(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C9 120.2(4) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
C20 C15 C16 117.7(4) . . ?
C20 C15 C8 119.6(4) . . ?
C16 C15 C8 122.6(4) . . ?
C17 C16 C15 121.0(4) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 119.2(4) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C18 C19 C20 120.1(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C15 C20 C19 121.2(4) . . ?
C15 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C26 C21 C22 116.9(4) . . ?
C26 C21 C7 123.4(3) . . ?
C22 C21 C7 119.6(3) . . ?
C23 C22 C21 121.3(4) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 121.4(4) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C25 C24 C23 117.4(4) . . ?
C25 C24 C27 121.3(4) . . ?
C23 C24 C27 121.1(4) . . ?
C24 C25 C26 121.8(4) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C21 C26 C25 121.1(4) . . ?
C21 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C24 C27 C28 113.3(3) . . ?
C24 C27 H27A 108.9 . . ?
C28 C27 H27A 108.9 . . ?
C24 C27 H27B 108.9 . . ?
C28 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C33 C28 C29 118.3(4) . . ?
C33 C28 C27 120.3(4) . . ?
C29 C28 C27 121.4(3) . . ?
C28 C29 C30 121.1(3) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
O1 C30 C31 115.9(4) . . ?
O1 C30 C29 123.6(3) . . ?
C31 C30 C29 120.5(4) . . ?
C32 C31 C30 118.0(4) . . ?
C32 C31 C34 121.1(4) . . ?
C30 C31 C34 120.8(4) . . ?
C31 C32 C33 121.5(4) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 H32 119.3 . . ?
O2 C33 C28 116.5(4) . . ?
O2 C33 C32 122.9(4) . . ?
C28 C33 C32 120.6(4) . . ?
C3 C34 C31 117.2(4) 2_666 . ?
C3 C34 H34A 108.0 2_666 . ?
C31 C34 H34A 108.0 . . ?
C3 C34 H34B 108.0 2_666 . ?
C31 C34 H34B 108.0 . . ?
H34A C34 H34B 107.3 . . ?
O2 C35 C36 112.6(8) . . ?
O2 C35 H35A 109.1 . . ?
C36 C35 H35A 109.1 . . ?
O2 C35 H35B 109.1 . . ?
C36 C35 H35B 109.1 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 C37 118.7(8) . . ?
C35 C36 H36A 107.6 . . ?
C37 C36 H36A 107.6 . . ?
C35 C36 H36B 107.6 . . ?
C37 C36 H36B 107.6 . . ?
H36A C36 H36B 107.1 . . ?
C38 C37 C36 139.6(12) . . ?
C38 C37 H37A 102.2 . . ?
C36 C37 H37A 102.2 . . ?
C38 C37 H37B 102.2 . . ?
C36 C37 H37B 102.2 . . ?
H37A C37 H37B 104.8 . . ?
C37 C38 C39 134.8(11) . . ?
C37 C38 H38A 103.5 . . ?
C39 C38 H38A 103.5 . . ?
C37 C38 H38B 103.5 . . ?
C39 C38 H38B 103.5 . . ?
H38A C38 H38B 105.3 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36' C35' O2 111.8(7) . . ?
C36' C35' H35C 109.3 . . ?
O2 C35' H35C 109.3 . . ?
C36' C35' H35D 109.3 . . ?
O2 C35' H35D 109.3 . . ?
H35C C35' H35D 107.9 . . ?
C35' C36' C37' 124.7(10) . . ?
C35' C36' H36C 106.1 . . ?
C37' C36' H36C 106.1 . . ?
C35' C36' H36D 106.1 . . ?
C37' C36' H36D 106.1 . . ?
H36C C36' H36D 106.3 . . ?
C38' C37' C36' 126.0(12) . . ?
C38' C37' H37C 105.8 . . ?
C36' C37' H37C 105.8 . . ?
C38' C37' H37D 105.8 . . ?
C36' C37' H37D 105.8 . . ?
H37C C37' H37D 106.2 . . ?
C37' C38' C39' 121.5(11) . . ?
C37' C38' H38C 107.0 . . ?
C39' C38' H38C 107.0 . . ?
C37' C38' H38D 107.0 . . ?
C39' C38' H38D 107.0 . . ?
H38C C38' H38D 106.7 . . ?
C38' C39' H39D 109.5 . . ?
C38' C39' H39E 109.5 . . ?
H39D C39' H39E 109.5 . . ?
C38' C39' H39F 109.5 . . ?
H39D C39' H39F 109.5 . . ?
H39E C39' H39F 109.5 . . ?
O1 C40 C41 106.9(3) . . ?
O1 C40 H40A 110.3 . . ?
C41 C40 H40A 110.3 . . ?
O1 C40 H40B 110.3 . . ?
C41 C40 H40B 110.3 . . ?
H40A C40 H40B 108.6 . . ?
C40 C41 C42 114.1(4) . . ?
C40 C41 H41A 108.7 . . ?
C42 C41 H41A 108.7 . . ?
C40 C41 H41B 108.7 . . ?
C42 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
C41 C42 C43 114.1(4) . . ?
C41 C42 H42A 108.7 . . ?
C43 C42 H42A 108.7 . . ?
C41 C42 H42B 108.7 . . ?
C43 C42 H42B 108.7 . . ?
H42A C42 H42B 107.6 . . ?
C44 C43 C42 114.1(4) . . ?
C44 C43 H43A 108.7 . . ?
C42 C43 H43A 108.7 . . ?
C44 C43 H43B 108.7 . . ?
C42 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.3(6) . . . . ?
C1 C2 C3 C4 1.0(6) . . . . ?
C1 C2 C3 C34 -178.8(4) . . . 2_666 ?
C2 C3 C4 C5 0.5(6) . . . . ?
C34 C3 C4 C5 -179.6(4) 2_666 . . . ?
C3 C4 C5 C6 -1.0(6) . . . . ?
C2 C1 C6 C5 1.9(6) . . . . ?
C2 C1 C6 C7 176.1(3) . . . . ?
C4 C5 C6 C1 -0.3(6) . . . . ?
C4 C5 C6 C7 -174.4(4) . . . . ?
C1 C6 C7 C8 134.3(4) . . . . ?
C5 C6 C7 C8 -51.7(5) . . . . ?
C1 C6 C7 C21 -43.8(5) . . . . ?
C5 C6 C7 C21 130.1(4) . . . . ?
C21 C7 C8 C9 168.8(3) . . . . ?
C6 C7 C8 C9 -9.2(6) . . . . ?
C21 C7 C8 C15 -8.7(6) . . . . ?
C6 C7 C8 C15 173.3(3) . . . . ?
C7 C8 C9 C14 126.6(4) . . . . ?
C15 C8 C9 C14 -55.7(5) . . . . ?
C7 C8 C9 C10 -56.2(5) . . . . ?
C15 C8 C9 C10 121.5(4) . . . . ?
C14 C9 C10 C11 0.1(6) . . . . ?
C8 C9 C10 C11 -177.2(4) . . . . ?
C9 C10 C11 C12 -1.9(7) . . . . ?
C10 C11 C12 C13 1.9(7) . . . . ?
C11 C12 C13 C14 -0.1(7) . . . . ?
C12 C13 C14 C9 -1.7(6) . . . . ?
C10 C9 C14 C13 1.7(6) . . . . ?
C8 C9 C14 C13 179.0(4) . . . . ?
C7 C8 C15 C20 136.0(4) . . . . ?
C9 C8 C15 C20 -41.6(5) . . . . ?
C7 C8 C15 C16 -45.9(5) . . . . ?
C9 C8 C15 C16 136.5(4) . . . . ?
C20 C15 C16 C17 -1.3(6) . . . . ?
C8 C15 C16 C17 -179.5(4) . . . . ?
C15 C16 C17 C18 -0.2(6) . . . . ?
C16 C17 C18 C19 1.0(6) . . . . ?
C17 C18 C19 C20 -0.2(6) . . . . ?
C16 C15 C20 C19 2.1(6) . . . . ?
C8 C15 C20 C19 -179.7(4) . . . . ?
C18 C19 C20 C15 -1.4(7) . . . . ?
C8 C7 C21 C26 -45.7(5) . . . . ?
C6 C7 C21 C26 132.4(4) . . . . ?
C8 C7 C21 C22 138.1(4) . . . . ?
C6 C7 C21 C22 -43.8(5) . . . . ?
C26 C21 C22 C23 0.0(5) . . . . ?
C7 C21 C22 C23 176.4(3) . . . . ?
C21 C22 C23 C24 -0.4(6) . . . . ?
C22 C23 C24 C25 0.9(6) . . . . ?
C22 C23 C24 C27 -174.5(4) . . . . ?
C23 C24 C25 C26 -0.9(6) . . . . ?
C27 C24 C25 C26 174.4(4) . . . . ?
C22 C21 C26 C25 -0.1(6) . . . . ?
C7 C21 C26 C25 -176.3(4) . . . . ?
C24 C25 C26 C21 0.6(6) . . . . ?
C25 C24 C27 C28 -88.9(5) . . . . ?
C23 C24 C27 C28 86.2(5) . . . . ?
C24 C27 C28 C33 -161.6(4) . . . . ?
C24 C27 C28 C29 19.1(6) . . . . ?
C33 C28 C29 C30 0.6(6) . . . . ?
C27 C28 C29 C30 179.9(4) . . . . ?
C40 O1 C30 C31 177.1(4) . . . . ?
C40 O1 C30 C29 -4.5(6) . . . . ?
C28 C29 C30 O1 -178.2(4) . . . . ?
C28 C29 C30 C31 0.1(6) . . . . ?
O1 C30 C31 C32 178.9(4) . . . . ?
C29 C30 C31 C32 0.5(6) . . . . ?
O1 C30 C31 C34 1.5(6) . . . . ?
C29 C30 C31 C34 -177.0(4) . . . . ?
C30 C31 C32 C33 -1.7(6) . . . . ?
C34 C31 C32 C33 175.7(4) . . . . ?
C35 O2 C33 C28 165.0(7) . . . . ?
C35' O2 C33 C28 -169.8(5) . . . . ?
C35 O2 C33 C32 -17.0(9) . . . . ?
C35' O2 C33 C32 8.2(7) . . . . ?
C29 C28 C33 O2 176.3(4) . . . . ?
C27 C28 C33 O2 -3.1(6) . . . . ?
C29 C28 C33 C32 -1.8(6) . . . . ?
C27 C28 C33 C32 178.9(4) . . . . ?
C31 C32 C33 O2 -175.5(4) . . . . ?
C31 C32 C33 C28 2.4(7) . . . . ?
C32 C31 C34 C3 107.9(5) . . . 2_666 ?
C30 C31 C34 C3 -74.7(6) . . . 2_666 ?
C33 O2 C35 C36 152.0(7) . . . . ?
C35' O2 C35 C36 93.0(13) . . . . ?
O2 C35 C36 C37 -59.4(14) . . . . ?
C35 C36 C37 C38 -135.2(15) . . . . ?
C36 C37 C38 C39 -111(2) . . . . ?
C33 O2 C35' C36' 163.2(8) . . . . ?
C35 O2 C35' C36' -63.9(11) . . . . ?
O2 C35' C36' C37' -47.8(16) . . . . ?
C35' C36' C37' C38' -166.0(13) . . . . ?
C36' C37' C38' C39' 138.4(15) . . . . ?
C30 O1 C40 C41 -168.9(3) . . . . ?
O1 C40 C41 C42 65.6(5) . . . . ?
C40 C41 C42 C43 74.8(5) . . . . ?
C41 C42 C43 C44 77.9(5) . . . . ?

_refine_diff_density_max         1.042
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1012066'
#######################################################################
#
#                 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_r140319g1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H40 O4'
_chemical_formula_weight         632.76

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   9.6016(19)
_cell_length_b                   14.338(3)
_cell_length_c                   24.574(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3383.0(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    8636
_cell_measurement_theta_min      1.6574
_cell_measurement_theta_max      26.0023

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9845
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_process_details   crystalclear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            34474
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5968
_reflns_number_gt                5192
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1117P)²+0.1203P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_number_reflns         5968
_refine_ls_number_parameters     438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0743
_refine_ls_wR_factor_ref         0.2004
_refine_ls_wR_factor_gt          0.1935
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_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 0.8500(3) 0.5027(2) -0.05201(12) 0.0632(8) Uani 1 1 d . . .
O2 O 0.2968(3) 0.57207(17) -0.00255(11) 0.0569(7) Uani 1 1 d . . .
O3 O 0.1911(3) -0.27486(19) 0.16205(12) 0.0570(7) Uani 1 1 d . . .
O4 O 0.7649(3) -0.30022(17) 0.14077(12) 0.0546(7) Uani 1 1 d . . .
C1 C 0.9477(4) 0.2119(2) 0.16024(15) 0.0438(8) Uani 1 1 d . . .
C2 C 0.9935(4) 0.3034(2) 0.13683(15) 0.0444(8) Uani 1 1 d . . .
C3 C 0.9676(5) 0.3254(3) 0.08248(17) 0.0559(10) Uani 1 1 d . . .
H3 H 0.9185 0.2822 0.0603 0.067 Uiso 1 1 calc R . .
C4 C 1.0122(5) 0.4094(3) 0.06007(17) 0.0580(10) Uani 1 1 d . . .
H4 H 0.9944 0.4232 0.0229 0.070 Uiso 1 1 calc R . .
C5 C 1.0826(4) 0.4727(3) 0.09245(18) 0.0545(10) Uani 1 1 d . . .
H5 H 1.1126 0.5304 0.0775 0.065 Uiso 1 1 calc R . .
C6 C 1.1093(4) 0.4524(2) 0.14618(18) 0.0499(9) Uani 1 1 d . . .
H6 H 1.1575 0.4964 0.1681 0.060 Uiso 1 1 calc R . .
C7 C 1.0664(4) 0.3677(2) 0.16874(16) 0.0447(9) Uani 1 1 d . . .
H7 H 1.0867 0.3538 0.2057 0.054 Uiso 1 1 calc R . .
C8 C 1.0622(4) 0.1561(2) 0.18584(16) 0.0451(9) Uani 1 1 d . . .
C9 C 1.1942(4) 0.1530(3) 0.16146(18) 0.0527(9) Uani 1 1 d . . .
H9 H 1.2102 0.1866 0.1287 0.063 Uiso 1 1 calc R . .
C10 C 1.3009(5) 0.1020(3) 0.18423(18) 0.0561(10) Uani 1 1 d . . .
H10 H 1.3890 0.0995 0.1667 0.067 Uiso 1 1 calc R . .
C11 C 1.2804(5) 0.0549(3) 0.2320(2) 0.0620(11) Uani 1 1 d . . .
H11 H 1.3550 0.0206 0.2476 0.074 Uiso 1 1 calc R . .
C12 C 1.1526(4) 0.0567(3) 0.25774(18) 0.0515(10) Uani 1 1 d . . .
H12 H 1.1387 0.0231 0.2906 0.062 Uiso 1 1 calc R . .
C13 C 1.0436(4) 0.1086(2) 0.23495(16) 0.0468(9) Uani 1 1 d . . .
H13 H 0.9563 0.1116 0.2530 0.056 Uiso 1 1 calc R . .
C14 C 0.8139(4) 0.1821(2) 0.15741(14) 0.0427(8) Uani 1 1 d . . .
C15 C 0.7010(4) 0.2395(2) 0.13292(15) 0.0424(8) Uani 1 1 d . . .
C16 C 0.6174(5) 0.2029(3) 0.09127(17) 0.0536(10) Uani 1 1 d . . .
H16 H 0.6250 0.1387 0.0823 0.064 Uiso 1 1 calc R . .
C17 C 0.5238(5) 0.2584(3) 0.06292(17) 0.0568(10) Uani 1 1 d . . .
H17 H 0.4705 0.2323 0.0341 0.068 Uiso 1 1 calc R . .
C18 C 0.5077(4) 0.3520(3) 0.07645(16) 0.0489(9) Uani 1 1 d . . .
C19 C 0.5811(4) 0.3869(3) 0.12104(16) 0.0504(10) Uani 1 1 d . . .
H19 H 0.5644 0.4490 0.1329 0.060 Uiso 1 1 calc R . .
C20 C 0.6779(4) 0.3328(2) 0.14834(15) 0.0466(9) Uani 1 1 d . . .
H20 H 0.7292 0.3588 0.1777 0.056 Uiso 1 1 calc R . .
C21 C 0.4183(5) 0.4159(3) 0.04209(17) 0.0559(10) Uani 1 1 d . . .
H21A H 0.3591 0.4538 0.0666 0.067 Uiso 1 1 calc R . .
H21B H 0.3557 0.3772 0.0194 0.067 Uiso 1 1 calc R . .
C22 C 0.4995(4) 0.4812(2) 0.00504(15) 0.0485(9) Uani 1 1 d . . .
C23 C 0.6384(4) 0.4650(3) -0.00852(16) 0.0528(10) Uani 1 1 d . . .
H23 H 0.6836 0.4107 0.0049 0.063 Uiso 1 1 calc R . .
C24 C 0.7124(4) 0.5272(3) -0.04161(16) 0.0513(9) Uani 1 1 d . . .
C25 C 0.6497(5) 0.6083(3) -0.06009(16) 0.0547(10) Uani 1 1 d . . .
H25 H 0.7008 0.6523 -0.0810 0.066 Uiso 1 1 calc R . .
C26 C 0.5093(4) 0.6241(3) -0.04738(16) 0.0520(10) Uani 1 1 d . . .
H26 H 0.4645 0.6786 -0.0607 0.062 Uiso 1 1 calc R . .
C27 C 0.4355(4) 0.5623(3) -0.01602(15) 0.0479(9) Uani 1 1 d . . .
C28 C 0.9276(5) 0.5626(3) -0.0879(2) 0.0656(12) Uani 1 1 d . . .
H28A H 0.8779 0.5687 -0.1225 0.098 Uiso 1 1 calc R . .
H28B H 1.0199 0.5356 -0.0944 0.098 Uiso 1 1 calc R . .
H28C H 0.9380 0.6242 -0.0711 0.098 Uiso 1 1 calc R . .
C29 C 0.2321(5) 0.6593(3) -0.01625(19) 0.0682(12) Uani 1 1 d . . .
H29A H 0.2819 0.7103 0.0018 0.102 Uiso 1 1 calc R . .
H29B H 0.1349 0.6587 -0.0041 0.102 Uiso 1 1 calc R . .
H29C H 0.2354 0.6683 -0.0558 0.102 Uiso 1 1 calc R . .
C30 C 0.7732(4) 0.0858(2) 0.17432(14) 0.0408(8) Uani 1 1 d . . .
C31 C 0.8347(4) 0.0067(2) 0.14972(14) 0.0424(8) Uani 1 1 d . . .
H31 H 0.9007 0.0148 0.1213 0.051 Uiso 1 1 calc R . .
C32 C 0.7997(4) -0.0819(2) 0.16657(15) 0.0448(8) Uani 1 1 d . . .
H32 H 0.8406 -0.1342 0.1490 0.054 Uiso 1 1 calc R . .
C33 C 0.7048(4) -0.0964(2) 0.20918(14) 0.0423(8) Uani 1 1 d . . .
C34 C 0.6439(4) -0.0178(2) 0.23311(15) 0.0436(8) Uani 1 1 d . . .
H34 H 0.5798 -0.0256 0.2622 0.052 Uiso 1 1 calc R . .
C35 C 0.6753(4) 0.0705(2) 0.21518(15) 0.0438(8) Uani 1 1 d . . .
H35 H 0.6291 0.1224 0.2310 0.053 Uiso 1 1 calc R . .
C36 C 0.6671(4) -0.1938(2) 0.22808(16) 0.0455(9) Uani 1 1 d . . .
H36A H 0.6216 -0.1900 0.2642 0.055 Uiso 1 1 calc R . .
H36B H 0.7533 -0.2310 0.2322 0.055 Uiso 1 1 calc R . .
C37 C 0.5700(4) -0.2431(2) 0.18851(15) 0.0422(8) Uani 1 1 d . . .
C38 C 0.4256(4) -0.2338(2) 0.19459(15) 0.0454(9) Uani 1 1 d . . .
H38 H 0.3891 -0.1960 0.2230 0.054 Uiso 1 1 calc R . .
C39 C 0.3351(4) -0.2797(2) 0.15929(15) 0.0487(9) Uani 1 1 d . . .
C40 C 0.3887(5) -0.3356(3) 0.11808(17) 0.0549(10) Uani 1 1 d . . .
H40 H 0.3274 -0.3688 0.0947 0.066 Uiso 1 1 calc R . .
C41 C 0.5307(5) -0.3430(3) 0.11113(16) 0.0536(10) Uani 1 1 d . . .
H41 H 0.5667 -0.3800 0.0823 0.064 Uiso 1 1 calc R . .
C42 C 0.6212(4) -0.2973(2) 0.14564(16) 0.0468(9) Uani 1 1 d . . .
C43 C 0.1333(5) -0.2088(3) 0.19919(18) 0.0601(11) Uani 1 1 d . . .
H43A H 0.1617 -0.2247 0.2364 0.090 Uiso 1 1 calc R . .
H43B H 0.0315 -0.2101 0.1966 0.090 Uiso 1 1 calc R . .
H43C H 0.1671 -0.1462 0.1901 0.090 Uiso 1 1 calc R . .
C44 C 0.8224(5) -0.3658(3) 0.1035(2) 0.0631(11) Uani 1 1 d . . .
H44A H 0.7879 -0.4283 0.1121 0.095 Uiso 1 1 calc R . .
H44B H 0.9242 -0.3649 0.1062 0.095 Uiso 1 1 calc R . .
H44C H 0.7946 -0.3491 0.0663 0.095 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
O1 C24 1.391(5) . ?
O1 C28 1.438(5) . ?
O2 C27 1.379(5) . ?
O2 C29 1.437(4) . ?
O3 C39 1.386(5) . ?
O3 C43 1.428(5) . ?
O4 C42 1.386(5) . ?
O4 C44 1.424(5) . ?
C1 C14 1.357(5) . ?
C1 C8 1.498(5) . ?
C1 C2 1.499(5) . ?
C2 C3 1.395(6) . ?
C2 C7 1.398(5) . ?
C3 C4 1.393(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.376(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.397(5) . ?
C8 C9 1.402(6) . ?
C9 C10 1.378(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.368(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.401(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.489(5) . ?
C14 C30 1.494(5) . ?
C15 C16 1.403(5) . ?
C15 C20 1.407(5) . ?
C16 C17 1.388(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(6) . ?
C18 C21 1.513(5) . ?
C19 C20 1.384(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.522(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.394(6) . ?
C22 C27 1.413(5) . ?
C23 C24 1.401(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.386(6) . ?
C25 C26 1.402(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.372(5) . ?
C26 H26 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C35 1.393(5) . ?
C30 C31 1.413(5) . ?
C31 C32 1.379(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.404(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(5) . ?
C33 C36 1.515(5) . ?
C34 C35 1.375(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.521(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C42 1.398(5) . ?
C37 C38 1.401(5) . ?
C38 C39 1.393(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.391(6) . ?
C40 C41 1.378(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.380(6) . ?
C41 H41 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C24 O1 C28 117.0(3) . . ?
C27 O2 C29 116.7(3) . . ?
C39 O3 C43 116.9(3) . . ?
C42 O4 C44 117.5(3) . . ?
C14 C1 C8 123.2(3) . . ?
C14 C1 C2 122.3(3) . . ?
C8 C1 C2 114.4(3) . . ?
C3 C2 C7 118.6(3) . . ?
C3 C2 C1 120.8(3) . . ?
C7 C2 C1 120.6(3) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C2 C7 C6 119.9(4) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C13 C8 C9 118.0(4) . . ?
C13 C8 C1 121.9(3) . . ?
C9 C8 C1 120.1(3) . . ?
C10 C9 C8 121.0(4) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.8(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C13 119.4(4) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C8 C13 C12 120.6(4) . . ?
C8 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C1 C14 C15 122.4(3) . . ?
C1 C14 C30 121.7(3) . . ?
C15 C14 C30 115.7(3) . . ?
C16 C15 C20 117.6(3) . . ?
C16 C15 C14 120.3(3) . . ?
C20 C15 C14 122.1(3) . . ?
C17 C16 C15 121.5(3) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C19 118.5(4) . . ?
C17 C18 C21 120.9(4) . . ?
C19 C18 C21 120.5(3) . . ?
C20 C19 C18 121.2(3) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C19 C20 C15 120.5(4) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C18 C21 C22 114.6(3) . . ?
C18 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
C18 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C23 C22 C27 117.8(3) . . ?
C23 C22 C21 122.0(3) . . ?
C27 C22 C21 120.2(3) . . ?
C22 C23 C24 121.1(4) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C25 C24 O1 124.4(4) . . ?
C25 C24 C23 120.3(4) . . ?
O1 C24 C23 115.3(3) . . ?
C24 C25 C26 118.7(4) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C27 C26 C25 121.1(4) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C26 C27 O2 124.6(3) . . ?
C26 C27 C22 120.9(4) . . ?
O2 C27 C22 114.5(3) . . ?
O1 C28 H28A 109.5 . . ?
O1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 C29 H29A 109.5 . . ?
O2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 117.7(3) . . ?
C35 C30 C14 121.4(3) . . ?
C31 C30 C14 120.9(3) . . ?
C32 C31 C30 120.6(3) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C33 121.3(3) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.4 . . ?
C34 C33 C32 117.7(3) . . ?
C34 C33 C36 120.9(3) . . ?
C32 C33 C36 121.3(3) . . ?
C35 C34 C33 121.1(3) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C30 121.6(3) . . ?
C34 C35 H35 119.2 . . ?
C30 C35 H35 119.2 . . ?
C33 C36 C37 112.2(3) . . ?
C33 C36 H36A 109.2 . . ?
C37 C36 H36A 109.2 . . ?
C33 C36 H36B 109.2 . . ?
C37 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
C42 C37 C38 118.8(3) . . ?
C42 C37 C36 121.6(3) . . ?
C38 C37 C36 119.7(3) . . ?
C39 C38 C37 120.4(4) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
O3 C39 C40 115.7(3) . . ?
O3 C39 C38 124.6(4) . . ?
C40 C39 C38 119.7(4) . . ?
C41 C40 C39 120.0(4) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.7(4) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C41 C42 O4 124.0(4) . . ?
C41 C42 C37 120.4(4) . . ?
O4 C42 C37 115.6(3) . . ?
O3 C43 H43A 109.5 . . ?
O3 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O3 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O4 C44 H44A 109.5 . . ?
O4 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O4 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C3 -54.5(5) . . . . ?
C8 C1 C2 C3 124.4(4) . . . . ?
C14 C1 C2 C7 127.1(4) . . . . ?
C8 C1 C2 C7 -54.0(5) . . . . ?
C7 C2 C3 C4 -0.3(6) . . . . ?
C1 C2 C3 C4 -178.7(4) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
C3 C4 C5 C6 0.6(6) . . . . ?
C4 C5 C6 C7 0.2(6) . . . . ?
C3 C2 C7 C6 1.0(5) . . . . ?
C1 C2 C7 C6 179.5(3) . . . . ?
C5 C6 C7 C2 -1.1(6) . . . . ?
C14 C1 C8 C13 -42.8(5) . . . . ?
C2 C1 C8 C13 138.3(3) . . . . ?
C14 C1 C8 C9 139.4(4) . . . . ?
C2 C1 C8 C9 -39.5(5) . . . . ?
C13 C8 C9 C10 2.2(6) . . . . ?
C1 C8 C9 C10 -179.9(3) . . . . ?
C8 C9 C10 C11 -1.4(6) . . . . ?
C9 C10 C11 C12 0.8(6) . . . . ?
C10 C11 C12 C13 -1.0(6) . . . . ?
C9 C8 C13 C12 -2.4(5) . . . . ?
C1 C8 C13 C12 179.7(3) . . . . ?
C11 C12 C13 C8 1.8(6) . . . . ?
C8 C1 C14 C15 178.6(3) . . . . ?
C2 C1 C14 C15 -2.6(6) . . . . ?
C8 C1 C14 C30 -7.0(5) . . . . ?
C2 C1 C14 C30 171.9(3) . . . . ?
C1 C14 C15 C16 125.9(4) . . . . ?
C30 C14 C15 C16 -48.9(5) . . . . ?
C1 C14 C15 C20 -51.1(5) . . . . ?
C30 C14 C15 C20 134.1(4) . . . . ?
C20 C15 C16 C17 5.5(6) . . . . ?
C14 C15 C16 C17 -171.5(4) . . . . ?
C15 C16 C17 C18 -2.0(7) . . . . ?
C16 C17 C18 C19 -3.9(6) . . . . ?
C16 C17 C18 C21 173.2(4) . . . . ?
C17 C18 C19 C20 6.0(6) . . . . ?
C21 C18 C19 C20 -171.0(4) . . . . ?
C18 C19 C20 C15 -2.4(6) . . . . ?
C16 C15 C20 C19 -3.4(5) . . . . ?
C14 C15 C20 C19 173.7(3) . . . . ?
C17 C18 C21 C22 -103.4(4) . . . . ?
C19 C18 C21 C22 73.6(5) . . . . ?
C18 C21 C22 C23 18.5(5) . . . . ?
C18 C21 C22 C27 -160.3(3) . . . . ?
C27 C22 C23 C24 0.4(6) . . . . ?
C21 C22 C23 C24 -178.4(3) . . . . ?
C28 O1 C24 C25 -5.1(6) . . . . ?
C28 O1 C24 C23 177.2(3) . . . . ?
C22 C23 C24 C25 2.2(6) . . . . ?
C22 C23 C24 O1 -180.0(4) . . . . ?
O1 C24 C25 C26 179.1(4) . . . . ?
C23 C24 C25 C26 -3.3(6) . . . . ?
C24 C25 C26 C27 1.8(6) . . . . ?
C25 C26 C27 O2 -178.8(4) . . . . ?
C25 C26 C27 C22 0.8(6) . . . . ?
C29 O2 C27 C26 -8.9(5) . . . . ?
C29 O2 C27 C22 171.4(3) . . . . ?
C23 C22 C27 C26 -1.9(5) . . . . ?
C21 C22 C27 C26 176.9(4) . . . . ?
C23 C22 C27 O2 177.7(3) . . . . ?
C21 C22 C27 O2 -3.4(5) . . . . ?
C1 C14 C30 C35 121.4(4) . . . . ?
C15 C14 C30 C35 -63.7(5) . . . . ?
C1 C14 C30 C31 -57.7(5) . . . . ?
C15 C14 C30 C31 117.1(4) . . . . ?
C35 C30 C31 C32 -1.1(5) . . . . ?
C14 C30 C31 C32 178.1(3) . . . . ?
C30 C31 C32 C33 -1.3(5) . . . . ?
C31 C32 C33 C34 1.7(5) . . . . ?
C31 C32 C33 C36 -179.5(3) . . . . ?
C32 C33 C34 C35 0.5(5) . . . . ?
C36 C33 C34 C35 -178.4(3) . . . . ?
C33 C34 C35 C30 -2.9(5) . . . . ?
C31 C30 C35 C34 3.2(5) . . . . ?
C14 C30 C35 C34 -176.0(3) . . . . ?
C34 C33 C36 C37 104.0(4) . . . . ?
C32 C33 C36 C37 -74.8(4) . . . . ?
C33 C36 C37 C42 89.9(4) . . . . ?
C33 C36 C37 C38 -89.6(4) . . . . ?
C42 C37 C38 C39 1.5(5) . . . . ?
C36 C37 C38 C39 -178.9(3) . . . . ?
C43 O3 C39 C40 -172.1(3) . . . . ?
C43 O3 C39 C38 8.5(5) . . . . ?
C37 C38 C39 O3 180.0(3) . . . . ?
C37 C38 C39 C40 0.6(5) . . . . ?
O3 C39 C40 C41 178.4(3) . . . . ?
C38 C39 C40 C41 -2.2(5) . . . . ?
C39 C40 C41 C42 1.7(6) . . . . ?
C40 C41 C42 O4 -179.0(3) . . . . ?
C40 C41 C42 C37 0.4(5) . . . . ?
C44 O4 C42 C41 -10.2(5) . . . . ?
C44 O4 C42 C37 170.3(3) . . . . ?
C38 C37 C42 C41 -2.0(5) . . . . ?
C36 C37 C42 C41 178.4(3) . . . . ?
C38 C37 C42 O4 177.5(3) . . . . ?
C36 C37 C42 O4 -2.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 1012067'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H56 O'
_chemical_formula_sum            'C60 H56 O'
_chemical_formula_weight         793.04

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6111(13)
_cell_length_b                   9.8047(14)
_cell_length_c                   12.6063(15)
_cell_angle_alpha                75.516(8)
_cell_angle_beta                 79.934(9)
_cell_angle_gamma                88.667(10)
_cell_volume                     1132.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3884
_cell_measurement_theta_min      1.69
_cell_measurement_theta_max      32.58

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_F_000             424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.067
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            18132
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_theta_min         1.694
_diffrn_reflns_theta_max         32.559
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8098
_reflns_number_gt                4445
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'

_refine_special_details          
; 
    ENTER TEXT OF LETTER 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0684P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.073(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8098
_refine_ls_number_parameters     301
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1419
_refine_ls_wR_factor_gt          0.1258
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.978
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.91688(11) 0.74945(11) 0.20192(9) 0.0248(2) Uani 1 1 d . . . . .
C2 C 0.94577(11) 0.85611(10) 0.24603(9) 0.0246(2) Uani 1 1 d . . . . .
C3 C 0.79621(11) 0.75056(11) 0.14173(9) 0.0253(2) Uani 1 1 d . . . . .
C4 C 0.76554(12) 0.86701(12) 0.06045(9) 0.0304(2) Uani 1 1 d . . . . .
H4 H 0.8248 0.9489 0.0401 0.037 Uiso 1 1 calc R U . . .
C5 C 0.64947(12) 0.86487(12) 0.00881(9) 0.0316(3) Uani 1 1 d . . . . .
H5 H 0.6312 0.9454 -0.0465 0.038 Uiso 1 1 calc R U . . .
C6 C 0.55931(12) 0.74751(12) 0.03623(9) 0.0297(2) Uani 1 1 d . . . . .
C7 C 0.59123(12) 0.63089(12) 0.11587(10) 0.0322(3) Uani 1 1 d . . . . .
H7 H 0.5318 0.5491 0.1362 0.039 Uiso 1 1 calc R U . . .
C8 C 0.70823(12) 0.63149(11) 0.16636(9) 0.0298(2) Uani 1 1 d . . . . .
H8 H 0.7290 0.5490 0.2189 0.036 Uiso 1 1 calc R U . . .
C9 C 0.43402(13) 0.74578(14) -0.02037(11) 0.0417(3) Uani 1 1 d . . . . .
H9A H 0.4541 0.6866 -0.0732 0.063 Uiso 1 1 calc R U . . .
H9B H 0.4155 0.8420 -0.0602 0.063 Uiso 1 1 calc R U . . .
H9C H 0.3509 0.7076 0.0355 0.063 Uiso 1 1 calc R U . . .
C10 C 1.00154(11) 0.61802(10) 0.21683(9) 0.0243(2) Uani 1 1 d . . . . .
C11 C 1.06574(12) 0.56789(11) 0.12653(9) 0.0289(2) Uani 1 1 d . . . . .
H11 H 1.0535 0.6166 0.0536 0.035 Uiso 1 1 calc R U . . .
C12 C 1.14726(12) 0.44807(12) 0.14098(10) 0.0321(3) Uani 1 1 d . . . . .
H12 H 1.1916 0.4175 0.0777 0.038 Uiso 1 1 calc R U . . .
C13 C 1.16510(12) 0.37221(11) 0.24650(10) 0.0296(2) Uani 1 1 d . . . . .
C14 C 1.09713(12) 0.41958(11) 0.33688(10) 0.0306(2) Uani 1 1 d . . . . .
H14 H 1.1057 0.3681 0.4100 0.037 Uiso 1 1 calc R U . . .
C15 C 1.01727(12) 0.54008(11) 0.32291(9) 0.0292(2) Uani 1 1 d . . . . .
H15 H 0.9726 0.5701 0.3863 0.035 Uiso 1 1 calc R U . . .
C16 C 1.25354(14) 0.24155(13) 0.26407(12) 0.0430(3) Uani 1 1 d . . . . .
H16A H 1.3455 0.2648 0.2794 0.065 Uiso 1 1 calc R U . . .
H16B H 1.2676 0.2061 0.1969 0.065 Uiso 1 1 calc R U . . .
H16C H 1.2048 0.1691 0.3273 0.065 Uiso 1 1 calc R U . . .
C17 C 0.85218(11) 0.97933(11) 0.25093(9) 0.0245(2) Uani 1 1 d . . . . .
C18 C 0.71136(12) 0.96164(11) 0.30397(10) 0.0305(2) Uani 1 1 d . . . . .
H18 H 0.6712 0.8694 0.3332 0.037 Uiso 1 1 calc R U . . .
C19 C 0.62938(12) 1.07720(12) 0.31446(10) 0.0342(3) Uani 1 1 d . . . . .
H19 H 0.5337 1.0635 0.3510 0.041 Uiso 1 1 calc R U . . .
C20 C 0.68590(12) 1.21245(12) 0.27213(10) 0.0316(3) Uani 1 1 d . . . . .
H20 H 0.6295 1.2914 0.2798 0.038 Uiso 1 1 calc R U . . .
C21 C 0.82470(12) 1.23167(12) 0.21879(10) 0.0325(3) Uani 1 1 d . . . . .
H21 H 0.8636 1.3243 0.1888 0.039 Uiso 1 1 calc R U . . .
C22 C 0.90770(12) 1.11651(11) 0.20870(9) 0.0292(2) Uani 1 1 d . . . . .
H22 H 1.0035 1.1310 0.1726 0.035 Uiso 1 1 calc R U . . .
C23 C 1.07260(11) 0.85661(10) 0.29960(9) 0.0248(2) Uani 1 1 d . . . . .
C24 C 1.20846(12) 0.84119(12) 0.24432(9) 0.0304(2) Uani 1 1 d . . . . .
H24 H 1.2217 0.8316 0.1701 0.037 Uiso 1 1 calc R U . . .
C25 C 1.32485(12) 0.83968(13) 0.29616(11) 0.0366(3) Uani 1 1 d . . . . .
H25 H 1.4171 0.8310 0.2569 0.044 Uiso 1 1 calc R U . . .
C26 C 1.30662(13) 0.85078(13) 0.40472(11) 0.0370(3) Uani 1 1 d . . . . .
H26 H 1.3860 0.8472 0.4408 0.044 Uiso 1 1 calc R U . . .
C27 C 1.17255(13) 0.86715(12) 0.46101(10) 0.0347(3) Uani 1 1 d . . . . .
H27 H 1.1598 0.8747 0.5357 0.042 Uiso 1 1 calc R U . . .
C28 C 1.05668(12) 0.87244(11) 0.40798(9) 0.0292(2) Uani 1 1 d . . . . .
H28 H 0.9654 0.8870 0.4460 0.035 Uiso 1 1 calc R U . . .
O1 O 0.4240(3) 0.5683(2) 0.57890(18) 0.0585(6) Uani 0.5 1 d D . P A -1
C29 C 0.3541(6) 0.4848(7) 0.5224(4) 0.0538(12) Uani 0.5 1 d D . P A -1
H29A H 0.2773 0.5389 0.4892 0.065 Uiso 0.5 1 calc R U P A -1
H29B H 0.3128 0.3972 0.5756 0.065 Uiso 0.5 1 calc R U P A -1
C30 C 0.4645(6) 0.4502(7) 0.4326(5) 0.0507(14) Uani 0.5 1 d D . P A -1
H30A H 0.4447 0.4975 0.3579 0.061 Uiso 0.5 1 calc R U P A -1
H30B H 0.4676 0.3473 0.4401 0.061 Uiso 0.5 1 calc R U P A -1
C31 C 0.6052(6) 0.5061(7) 0.4512(5) 0.0533(12) Uani 0.5 1 d D . P A -1
H31A H 0.6821 0.4383 0.4440 0.064 Uiso 0.5 1 calc R U P A -1
H31B H 0.6340 0.5981 0.3984 0.064 Uiso 0.5 1 calc R U P A -1
C32 C 0.5660(7) 0.5204(9) 0.5705(6) 0.0640(19) Uani 0.5 1 d D . P A -1
H32A H 0.5718 0.4286 0.6245 0.077 Uiso 0.5 1 calc R U P A -1
H32B H 0.6294 0.5895 0.5846 0.077 Uiso 0.5 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3559(14) . ?
C1 C3 1.4912(15) . ?
C1 C10 1.4972(14) . ?
C2 C23 1.4939(14) . ?
C2 C17 1.4967(14) . ?
C3 C4 1.3947(15) . ?
C3 C8 1.3954(15) . ?
C4 C5 1.3894(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.3918(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.3880(16) . ?
C6 C9 1.5056(16) . ?
C7 C8 1.3863(16) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.3923(15) . ?
C10 C15 1.3961(14) . ?
C11 C12 1.3882(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.3896(16) . ?
C12 H12 0.9500 . ?
C13 C14 1.3896(16) . ?
C13 C16 1.5119(15) . ?
C14 C15 1.3845(15) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.3948(15) . ?
C17 C22 1.3975(15) . ?
C18 C19 1.3852(16) . ?
C18 H18 0.9500 . ?
C19 C20 1.3844(16) . ?
C19 H19 0.9500 . ?
C20 C21 1.3791(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.3864(15) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.3925(15) . ?
C23 C28 1.3949(15) . ?
C24 C25 1.3887(16) . ?
C24 H24 0.9500 . ?
C25 C26 1.3802(18) . ?
C25 H25 0.9500 . ?
C26 C27 1.3847(17) . ?
C26 H26 0.9500 . ?
C27 C28 1.3893(16) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
O1 C32 1.427(6) . ?
O1 C29 1.454(4) . ?
C29 C30 1.509(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.547(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.527(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C3 123.20(9) . . ?
C2 C1 C10 121.07(9) . . ?
C3 C1 C10 115.65(9) . . ?
C1 C2 C23 122.14(9) . . ?
C1 C2 C17 123.97(9) . . ?
C23 C2 C17 113.84(8) . . ?
C4 C3 C8 117.31(10) . . ?
C4 C3 C1 122.85(9) . . ?
C8 C3 C1 119.84(9) . . ?
C5 C4 C3 120.90(10) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.58(10) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 117.45(10) . . ?
C7 C6 C9 121.25(11) . . ?
C5 C6 C9 121.29(11) . . ?
C8 C7 C6 121.25(10) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C3 121.45(10) . . ?
C7 C8 H8 119.3 . . ?
C3 C8 H8 119.3 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 117.54(10) . . ?
C11 C10 C1 121.71(9) . . ?
C15 C10 C1 120.74(9) . . ?
C12 C11 C10 121.28(10) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 121.05(10) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 117.65(10) . . ?
C12 C13 C16 121.90(11) . . ?
C14 C13 C16 120.45(11) . . ?
C15 C14 C13 121.55(10) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C10 120.87(10) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 118.15(10) . . ?
C18 C17 C2 121.62(9) . . ?
C22 C17 C2 120.08(9) . . ?
C19 C18 C17 120.69(10) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 120.48(11) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 119.51(10) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 120.34(10) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C17 120.82(11) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
C24 C23 C28 118.22(10) . . ?
C24 C23 C2 121.78(9) . . ?
C28 C23 C2 120.01(9) . . ?
C25 C24 C23 120.93(11) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C26 C25 C24 120.05(11) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 119.97(11) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 119.87(11) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C23 120.90(11) . . ?
C27 C28 H28 119.5 . . ?
C23 C28 H28 119.5 . . ?
C32 O1 C29 104.8(4) . . ?
O1 C29 C30 107.2(4) . . ?
O1 C29 H29A 110.3 . . ?
C30 C29 H29A 110.3 . . ?
O1 C29 H29B 110.3 . . ?
C30 C29 H29B 110.3 . . ?
H29A C29 H29B 108.5 . . ?
C29 C30 C31 104.6(4) . . ?
C29 C30 H30A 110.8 . . ?
C31 C30 H30A 110.8 . . ?
C29 C30 H30B 110.8 . . ?
C31 C30 H30B 110.8 . . ?
H30A C30 H30B 108.9 . . ?
C32 C31 C30 101.6(4) . . ?
C32 C31 H31A 111.5 . . ?
C30 C31 H31A 111.5 . . ?
C32 C31 H31B 111.5 . . ?
C30 C31 H31B 111.5 . . ?
H31A C31 H31B 109.3 . . ?
O1 C32 C31 104.5(5) . . ?
O1 C32 H32A 110.9 . . ?
C31 C32 H32A 110.9 . . ?
O1 C32 H32B 110.9 . . ?
C31 C32 H32B 110.9 . . ?
H32A C32 H32B 108.9 . . ?

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
C3 C1 C2 C23 -176.03(9) . . . . ?
C10 C1 C2 C23 7.44(16) . . . . ?
C3 C1 C2 C17 7.03(17) . . . . ?
C10 C1 C2 C17 -169.50(9) . . . . ?
C2 C1 C3 C4 46.40(16) . . . . ?
C10 C1 C3 C4 -136.89(11) . . . . ?
C2 C1 C3 C8 -133.43(11) . . . . ?
C10 C1 C3 C8 43.28(14) . . . . ?
C8 C3 C4 C5 1.76(16) . . . . ?
C1 C3 C4 C5 -178.07(10) . . . . ?
C3 C4 C5 C6 0.29(18) . . . . ?
C4 C5 C6 C7 -1.27(17) . . . . ?
C4 C5 C6 C9 -179.79(11) . . . . ?
C5 C6 C7 C8 0.17(17) . . . . ?
C9 C6 C7 C8 178.69(10) . . . . ?
C6 C7 C8 C3 1.95(18) . . . . ?
C4 C3 C8 C7 -2.87(16) . . . . ?
C1 C3 C8 C7 176.97(10) . . . . ?
C2 C1 C10 C11 -126.24(12) . . . . ?
C3 C1 C10 C11 56.98(13) . . . . ?
C2 C1 C10 C15 54.59(15) . . . . ?
C3 C1 C10 C15 -122.19(11) . . . . ?
C15 C10 C11 C12 -2.60(16) . . . . ?
C1 C10 C11 C12 178.20(10) . . . . ?
C10 C11 C12 C13 1.40(17) . . . . ?
C11 C12 C13 C14 0.76(16) . . . . ?
C11 C12 C13 C16 -179.94(11) . . . . ?
C12 C13 C14 C15 -1.66(17) . . . . ?
C16 C13 C14 C15 179.03(11) . . . . ?
C13 C14 C15 C10 0.42(17) . . . . ?
C11 C10 C15 C14 1.70(16) . . . . ?
C1 C10 C15 C14 -179.09(10) . . . . ?
C1 C2 C17 C18 57.29(15) . . . . ?
C23 C2 C17 C18 -119.88(11) . . . . ?
C1 C2 C17 C22 -127.27(12) . . . . ?
C23 C2 C17 C22 55.56(13) . . . . ?
C22 C17 C18 C19 -0.13(16) . . . . ?
C2 C17 C18 C19 175.39(10) . . . . ?
C17 C18 C19 C20 0.16(17) . . . . ?
C18 C19 C20 C21 0.29(17) . . . . ?
C19 C20 C21 C22 -0.76(17) . . . . ?
C20 C21 C22 C17 0.80(17) . . . . ?
C18 C17 C22 C21 -0.34(16) . . . . ?
C2 C17 C22 C21 -175.94(10) . . . . ?
C1 C2 C23 C24 54.39(15) . . . . ?
C17 C2 C23 C24 -128.38(11) . . . . ?
C1 C2 C23 C28 -125.43(11) . . . . ?
C17 C2 C23 C28 51.79(13) . . . . ?
C28 C23 C24 C25 0.87(16) . . . . ?
C2 C23 C24 C25 -178.96(10) . . . . ?
C23 C24 C25 C26 1.27(17) . . . . ?
C24 C25 C26 C27 -1.69(18) . . . . ?
C25 C26 C27 C28 -0.04(18) . . . . ?
C26 C27 C28 C23 2.23(17) . . . . ?
C24 C23 C28 C27 -2.61(15) . . . . ?
C2 C23 C28 C27 177.22(10) . . . . ?
C32 O1 C29 C30 -30.3(5) . . . . ?
O1 C29 C30 C31 6.1(8) . . . . ?
C29 C30 C31 C32 18.3(9) . . . . ?
C29 O1 C32 C31 42.5(6) . . . . ?
C30 C31 C32 O1 -37.3(8) . . . . ?

_refine_diff_density_max         0.306
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.043

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 1012068'
