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

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

data_gndu009
_database_code_depnum_ccdc_archive 'CCDC 1015086'
_audit_update_record             
;
2014-07-19 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H52 Cl3 O3'
_chemical_formula_weight         675.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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                   9.8070(4)
_cell_length_b                   13.8699(9)
_cell_length_c                   16.6745(11)
_cell_angle_alpha                109.657(6)
_cell_angle_beta                 95.088(4)
_cell_angle_gamma                107.141(4)
_cell_volume                     1996.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4115
_cell_measurement_theta_min      5.0750
_cell_measurement_theta_max      69.4040

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             722
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_min  0.8360
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       ω/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13422
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         71.31
_reflns_number_total             7557
_reflns_number_gt                5143
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97

_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)+(0.1498P)²+0.3566P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7557
_refine_ls_number_parameters     509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0734
_refine_ls_wR_factor_ref         0.2544
_refine_ls_wR_factor_gt          0.2175
_refine_ls_goodness_of_fit_ref   1.030
_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 -0.11828(19) 0.44462(16) 0.66586(11) 0.0653(5) Uani 1 1 d . . .
O2 O -0.15950(17) 0.75145(14) 0.64712(13) 0.0648(5) Uani 1 1 d . . .
O3 O 0.17123(17) 0.83678(14) 0.45556(12) 0.0620(5) Uani 1 1 d . . .
C1 C -0.0253(2) 0.48839(19) 0.74674(14) 0.0504(5) Uani 1 1 d . . .
C2 C 0.0197(3) 0.4182(2) 0.77727(16) 0.0541(5) Uani 1 1 d . . .
C3 C 0.1146(3) 0.4634(2) 0.85788(17) 0.0623(6) Uani 1 1 d . . .
H3 H 0.1467 0.4165 0.8791 0.075 Uiso 1 1 calc R . .
C4 C 0.1644(3) 0.5740(2) 0.90855(16) 0.0630(6) Uani 1 1 d . A .
C5 C 0.1089(3) 0.6394(2) 0.87784(17) 0.0609(6) Uani 1 1 d . . .
H5 H 0.1372 0.7148 0.9130 0.073 Uiso 1 1 calc R . .
C6 C 0.0137(2) 0.5989(2) 0.79778(16) 0.0533(5) Uani 1 1 d . . .
C7 C 0.2756(4) 0.6227(3) 0.9949(2) 0.0853(9) Uani 1 1 d . . .
C8 C 0.4212(8) 0.6278(17) 0.9700(8) 0.153(7) Uani 0.61(2) 1 d P A 1
H8A H 0.4968 0.6550 1.0227 0.229 Uiso 0.61(2) 1 calc PR A 1
H8B H 0.4454 0.6770 0.9387 0.229 Uiso 0.61(2) 1 calc PR A 1
H8C H 0.4159 0.5546 0.9323 0.229 Uiso 0.61(2) 1 calc PR A 1
C9 C 0.2480(13) 0.5441(9) 1.0427(6) 0.115(4) Uani 0.61(2) 1 d P A 1
H9A H 0.2504 0.4735 1.0048 0.172 Uiso 0.61(2) 1 calc PR A 1
H9B H 0.1521 0.5343 1.0582 0.172 Uiso 0.61(2) 1 calc PR A 1
H9C H 0.3237 0.5743 1.0958 0.172 Uiso 0.61(2) 1 calc PR A 1
C10 C 0.276(3) 0.7278(12) 1.0548(9) 0.210(13) Uani 0.61(2) 1 d P A 1
H10A H 0.1760 0.7220 1.0623 0.315 Uiso 0.61(2) 1 calc PR A 1
H10B H 0.3131 0.7838 1.0310 0.315 Uiso 0.61(2) 1 calc PR A 1
H10C H 0.3382 0.7481 1.1114 0.315 Uiso 0.61(2) 1 calc PR A 1
C8A C 0.392(2) 0.722(2) 0.9993(14) 0.172(14) Uani 0.39(2) 1 d P A 2
H8A1 H 0.4166 0.7780 1.0582 0.259 Uiso 0.39(2) 1 calc PR A 2
H8A2 H 0.3577 0.7494 0.9573 0.259 Uiso 0.39(2) 1 calc PR A 2
H8A3 H 0.4788 0.7041 0.9854 0.259 Uiso 0.39(2) 1 calc PR A 2
C9A C 0.346(4) 0.548(3) 1.0073(14) 0.23(2) Uani 0.39(2) 1 d P A 2
H9A1 H 0.4248 0.5863 1.0590 0.343 Uiso 0.39(2) 1 calc PR A 2
H9A2 H 0.3852 0.5188 0.9560 0.343 Uiso 0.39(2) 1 calc PR A 2
H9A3 H 0.2734 0.4870 1.0150 0.343 Uiso 0.39(2) 1 calc PR A 2
C10A C 0.198(2) 0.654(4) 1.0650(9) 0.32(3) Uani 0.39(2) 1 d P A 2
H10D H 0.1100 0.6648 1.0420 0.485 Uiso 0.39(2) 1 calc PR A 2
H10E H 0.2613 0.7225 1.1117 0.485 Uiso 0.39(2) 1 calc PR A 2
H10F H 0.1696 0.5967 1.0882 0.485 Uiso 0.39(2) 1 calc PR A 2
C11 C -0.0456(4) 0.4476(3) 0.59576(18) 0.0756(8) Uani 1 1 d . . .
H11A H -0.0016 0.5234 0.6014 0.113 Uiso 1 1 calc R . .
H11B H -0.1161 0.4057 0.5402 0.113 Uiso 1 1 calc R . .
H11C H 0.0309 0.4157 0.5976 0.113 Uiso 1 1 calc R . .
C12 C -0.0515(3) 0.6706(2) 0.76709(17) 0.0588(6) Uani 1 1 d . . .
H12 H -0.1410 0.6204 0.7213 0.071 Uiso 1 1 calc R . .
C13 C -0.0098(2) 0.77717(19) 0.66846(16) 0.0530(5) Uani 1 1 d . . .
C14 C 0.0492(2) 0.73663(19) 0.72443(16) 0.0545(6) Uani 1 1 d . . .
C15 C 0.1995(3) 0.7650(2) 0.74389(17) 0.0611(6) Uani 1 1 d . . .
H15 H 0.2404 0.7361 0.7802 0.073 Uiso 1 1 calc R . .
C16 C 0.2932(3) 0.8342(2) 0.71222(18) 0.0641(7) Uani 1 1 d . . .
C17 C 0.2298(3) 0.8761(2) 0.66030(17) 0.0606(6) Uani 1 1 d . . .
H17 H 0.2914 0.9248 0.6392 0.073 Uiso 1 1 calc R . .
C18 C 0.0797(3) 0.84932(19) 0.63805(15) 0.0529(5) Uani 1 1 d . . .
C19 C 0.4572(3) 0.8600(4) 0.7352(2) 0.0902(11) Uani 1 1 d . . .
C20 C 0.4849(6) 0.7488(6) 0.7010(6) 0.195(3) Uani 1 1 d . . .
H20A H 0.5899 0.7630 0.7062 0.292 Uiso 1 1 calc R . .
H20B H 0.4352 0.7078 0.6398 0.292 Uiso 1 1 calc R . .
H20C H 0.4468 0.7061 0.7356 0.292 Uiso 1 1 calc R . .
C21 C 0.5113(5) 0.9016(8) 0.8306(4) 0.211(4) Uani 1 1 d . . .
H21A H 0.6111 0.9019 0.8427 0.316 Uiso 1 1 calc R . .
H21B H 0.4479 0.8544 0.8549 0.316 Uiso 1 1 calc R . .
H21C H 0.5106 0.9761 0.8575 0.316 Uiso 1 1 calc R . .
C22 C 0.5412(4) 0.9295(7) 0.6923(5) 0.205(4) Uani 1 1 d . . .
H22A H 0.5401 1.0039 0.7191 0.308 Uiso 1 1 calc R . .
H22B H 0.4966 0.8993 0.6301 0.308 Uiso 1 1 calc R . .
H22C H 0.6422 0.9311 0.6994 0.308 Uiso 1 1 calc R . .
C23 C -0.2343(3) 0.6455(2) 0.5794(2) 0.0788(9) Uani 1 1 d . . .
H23A H -0.1942 0.6413 0.5270 0.118 Uiso 1 1 calc R . .
H23B H -0.3385 0.6340 0.5661 0.118 Uiso 1 1 calc R . .
H23C H -0.2209 0.5891 0.5990 0.118 Uiso 1 1 calc R . .
C24 C 0.0166(3) 0.9053(2) 0.58762(17) 0.0578(6) Uani 1 1 d . . .
H24A H -0.0546 0.9325 0.6183 0.069 Uiso 1 1 calc R . .
H24B H 0.0967 0.9696 0.5892 0.069 Uiso 1 1 calc R . .
C25 C 0.0215(2) 0.80589(18) 0.43032(16) 0.0512(5) Uani 1 1 d . . .
C26 C -0.0581(2) 0.83587(18) 0.49349(15) 0.0503(5) Uani 1 1 d . . .
C37 C -0.1008(3) 0.7473(2) 0.8393(2) 0.0756(8) Uani 1 1 d . . .
H37A H -0.0158 0.7955 0.8875 0.091 Uiso 1 1 calc R . .
H37B H -0.1371 0.7941 0.8160 0.091 Uiso 1 1 calc R . .
C27 C -0.2093(2) 0.80082(19) 0.46822(16) 0.0536(5) Uani 1 1 d . . .
H27 H -0.2640 0.8219 0.5110 0.064 Uiso 1 1 calc R . .
C28 C -0.2832(2) 0.73607(19) 0.38268(16) 0.0551(6) Uani 1 1 d . B .
C29 C -0.1989(3) 0.7068(2) 0.32232(17) 0.0572(6) Uani 1 1 d . . .
H29 H -0.2469 0.6620 0.2636 0.069 Uiso 1 1 calc R . .
C30 C -0.0480(3) 0.74015(19) 0.34383(16) 0.0541(6) Uani 1 1 d . . .
C31 C -0.4497(3) 0.6965(3) 0.35604(19) 0.0687(7) Uani 1 1 d . . .
C32 C -0.5222(5) 0.7337(6) 0.4329(4) 0.086(2) Uani 0.689(15) 1 d P B 1
H32A H -0.6280 0.7087 0.4119 0.129 Uiso 0.689(15) 1 calc PR B 1
H32B H -0.4839 0.8135 0.4606 0.129 Uiso 0.689(15) 1 calc PR B 1
H32C H -0.5012 0.7027 0.4754 0.129 Uiso 0.689(15) 1 calc PR B 1
C33 C -0.5088(7) 0.5742(6) 0.3138(9) 0.153(6) Uani 0.689(15) 1 d P B 1
H33A H -0.4831 0.5433 0.3554 0.229 Uiso 0.689(15) 1 calc PR B 1
H33B H -0.4667 0.5503 0.2627 0.229 Uiso 0.689(15) 1 calc PR B 1
H33C H -0.6152 0.5492 0.2958 0.229 Uiso 0.689(15) 1 calc PR B 1
C34 C -0.4905(7) 0.7483(12) 0.2931(6) 0.140(5) Uani 0.689(15) 1 d P B 1
H34A H -0.4591 0.7194 0.2386 0.210 Uiso 0.689(15) 1 calc PR B 1
H34B H -0.4419 0.8277 0.3198 0.210 Uiso 0.689(15) 1 calc PR B 1
H34C H -0.5965 0.7308 0.2810 0.210 Uiso 0.689(15) 1 calc PR B 1
C32A C -0.5016(17) 0.7888(17) 0.387(2) 0.160(15) Uani 0.311(15) 1 d P B 2
H32D H -0.6085 0.7620 0.3729 0.240 Uiso 0.311(15) 1 calc PR B 2
H32E H -0.4639 0.8397 0.3587 0.240 Uiso 0.311(15) 1 calc PR B 2
H32F H -0.4672 0.8265 0.4503 0.240 Uiso 0.311(15) 1 calc PR B 2
C33A C -0.5140(13) 0.612(2) 0.3939(17) 0.142(13) Uani 0.311(15) 1 d P B 2
H33D H -0.6205 0.5839 0.3755 0.213 Uiso 0.311(15) 1 calc PR B 2
H33E H -0.4867 0.6460 0.4577 0.213 Uiso 0.311(15) 1 calc PR B 2
H33F H -0.4763 0.5521 0.3731 0.213 Uiso 0.311(15) 1 calc PR B 2
C34A C -0.5023(14) 0.633(2) 0.2543(11) 0.135(9) Uani 0.311(15) 1 d P B 2
H34D H -0.4671 0.5710 0.2360 0.202 Uiso 0.311(15) 1 calc PR B 2
H34E H -0.4632 0.6819 0.2248 0.202 Uiso 0.311(15) 1 calc PR B 2
H34F H -0.6091 0.6056 0.2390 0.202 Uiso 0.311(15) 1 calc PR B 2
C35 C 0.2525(3) 0.9306(2) 0.4410(3) 0.0891(10) Uani 1 1 d . . .
H35A H 0.2280 0.9178 0.3792 0.134 Uiso 1 1 calc R . .
H35B H 0.3571 0.9451 0.4580 0.134 Uiso 1 1 calc R . .
H35C H 0.2286 0.9936 0.4759 0.134 Uiso 1 1 calc R . .
C36 C 0.0370(3) 0.7032(2) 0.27500(19) 0.0633(6) Uani 1 1 d . . .
H36A H 0.0345 0.7414 0.2347 0.076 Uiso 1 1 calc R . .
H36B H 0.1401 0.7252 0.3038 0.076 Uiso 1 1 calc R . .
C38 C -0.2198(5) 0.6861(4) 0.8745(3) 0.1121(14) Uani 1 1 d . . .
H38A H -0.3074 0.6432 0.8282 0.168 Uiso 1 1 calc R . .
H38B H -0.2428 0.7383 0.9228 0.168 Uiso 1 1 calc R . .
H38C H -0.1861 0.6372 0.8953 0.168 Uiso 1 1 calc R . .
C101 C 0.1199(6) 0.0433(4) 0.8526(3) 0.1256(15) Uani 1 1 d . . .
Cl1 Cl 0.2410(13) 0.1608(12) 0.8497(10) 0.323(10) Uani 0.371(12) 1 d P C 1
Cl2 Cl -0.0196(15) 0.0690(12) 0.8945(9) 0.258(7) Uani 0.371(12) 1 d P C 1
Cl3 Cl 0.2373(18) 0.0409(13) 0.9303(14) 0.339(10) Uani 0.371(12) 1 d P C 1
Cl1A Cl 0.2124(7) 0.1398(3) 0.8147(4) 0.171(2) Uani 0.629(12) 1 d P C 2
Cl2A Cl -0.0496(6) 0.0432(5) 0.8546(8) 0.222(4) Uani 0.629(12) 1 d P C 2
Cl3A Cl 0.2150(6) 0.0467(3) 0.9493(2) 0.170(2) Uani 0.629(12) 1 d P C 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 C1 1.387(3) . ?
O1 C11 1.428(3) . ?
O2 C13 1.387(3) . ?
O2 C23 1.440(3) . ?
O3 C25 1.383(3) . ?
O3 C35 1.422(3) . ?
C1 C6 1.393(3) . ?
C1 C2 1.395(3) . ?
C2 C3 1.391(4) . ?
C2 C36 1.509(4) 2_566 ?
C3 C4 1.385(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(4) . ?
C4 C7 1.534(4) . ?
C5 C6 1.391(3) . ?
C5 H5 0.9500 . ?
C6 C12 1.523(3) . ?
C7 C10 1.464(11) . ?
C7 C9A 1.464(18) . ?
C7 C10A 1.468(17) . ?
C7 C8A 1.481(18) . ?
C7 C8 1.511(11) . ?
C7 C9 1.532(9) . ?
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 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.533(3) . ?
C12 C37 1.536(4) . ?
C12 H12 1.0000 . ?
C13 C18 1.390(3) . ?
C13 C14 1.404(3) . ?
C14 C15 1.386(3) . ?
C15 C16 1.398(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(3) . ?
C16 C19 1.523(3) . ?
C17 C18 1.390(3) . ?
C17 H17 0.9500 . ?
C18 C24 1.525(3) . ?
C19 C21 1.483(6) . ?
C19 C22 1.491(6) . ?
C19 C20 1.568(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.514(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.391(3) . ?
C25 C30 1.397(3) . ?
C26 C27 1.393(3) . ?
C37 C38 1.518(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C27 C28 1.392(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(4) . ?
C28 C31 1.530(3) . ?
C29 C30 1.387(3) . ?
C29 H29 0.9500 . ?
C30 C36 1.517(4) . ?
C31 C32A 1.467(17) . ?
C31 C33 1.501(8) . ?
C31 C33A 1.516(13) . ?
C31 C32 1.533(6) . ?
C31 C34 1.543(8) . ?
C31 C34A 1.579(17) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
C34A H34D 0.9800 . ?
C34A H34E 0.9800 . ?
C34A H34F 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C2 1.509(4) 2_566 ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C101 Cl2A 1.665(8) . ?
C101 Cl2 1.666(14) . ?
C101 Cl3 1.67(2) . ?
C101 Cl1A 1.722(7) . ?
C101 Cl1 1.730(11) . ?
C101 Cl3A 1.769(7) . ?
Cl1 Cl3 2.46(3) . ?

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
C1 O1 C11 114.2(2) . . ?
C13 O2 C23 113.9(2) . . ?
C25 O3 C35 114.46(19) . . ?
O1 C1 C6 119.9(2) . . ?
O1 C1 C2 118.5(2) . . ?
C6 C1 C2 121.4(2) . . ?
C3 C2 C1 117.9(2) . . ?
C3 C2 C36 121.5(2) . 2_566 ?
C1 C2 C36 120.6(2) . 2_566 ?
C4 C3 C2 122.7(2) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 117.1(2) . . ?
C3 C4 C7 121.7(2) . . ?
C5 C4 C7 121.2(3) . . ?
C4 C5 C6 122.7(2) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 117.8(2) . . ?
C5 C6 C12 122.0(2) . . ?
C1 C6 C12 120.2(2) . . ?
C10 C7 C9A 131.5(9) . . ?
C10 C7 C10A 46.4(17) . . ?
C9A C7 C10A 110(2) . . ?
C10 C7 C8A 62.8(12) . . ?
C9A C7 C8A 107.7(17) . . ?
C10A C7 C8A 108.4(18) . . ?
C10 C7 C8 113.2(11) . . ?
C9A C7 C8 60.4(15) . . ?
C10A C7 C8 146.9(9) . . ?
C8A C7 C8 54.0(12) . . ?
C10 C7 C9 107.5(9) . . ?
C9A C7 C9 45.7(15) . . ?
C10A C7 C9 68(2) . . ?
C8A C7 C9 138.4(8) . . ?
C8 C7 C9 105.4(7) . . ?
C10 C7 C4 114.4(5) . . ?
C9A C7 C4 113.4(9) . . ?
C10A C7 C4 107.1(8) . . ?
C8A C7 C4 110.0(7) . . ?
C8 C7 C4 105.5(5) . . ?
C9 C7 C4 110.5(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
C7 C8A H8A1 109.5 . . ?
C7 C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7 C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7 C9A H9A1 109.5 . . ?
C7 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C7 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C7 C10A H10D 109.5 . . ?
C7 C10A H10E 109.5 . . ?
H10D C10A H10E 109.5 . . ?
C7 C10A H10F 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
O1 C11 H11A 109.5 . . ?
O1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C12 C14 113.36(19) . . ?
C6 C12 C37 113.2(2) . . ?
C14 C12 C37 109.6(2) . . ?
C6 C12 H12 106.7 . . ?
C14 C12 H12 106.7 . . ?
C37 C12 H12 106.7 . . ?
O2 C13 C18 118.5(2) . . ?
O2 C13 C14 120.2(2) . . ?
C18 C13 C14 121.2(2) . . ?
C15 C14 C13 117.9(2) . . ?
C15 C14 C12 122.2(2) . . ?
C13 C14 C12 119.8(2) . . ?
C14 C15 C16 122.7(2) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C17 C16 C15 117.2(2) . . ?
C17 C16 C19 123.3(2) . . ?
C15 C16 C19 119.6(2) . . ?
C16 C17 C18 122.5(2) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 H17 118.8 . . ?
C17 C18 C13 118.5(2) . . ?
C17 C18 C24 120.2(2) . . ?
C13 C18 C24 121.1(2) . . ?
C21 C19 C22 113.9(5) . . ?
C21 C19 C16 111.5(3) . . ?
C22 C19 C16 113.0(3) . . ?
C21 C19 C20 103.3(5) . . ?
C22 C19 C20 107.0(5) . . ?
C16 C19 C20 107.2(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 H23A 109.5 . . ?
O2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C18 116.06(19) . . ?
C26 C24 H24A 108.3 . . ?
C18 C24 H24A 108.3 . . ?
C26 C24 H24B 108.3 . . ?
C18 C24 H24B 108.3 . . ?
H24A C24 H24B 107.4 . . ?
O3 C25 C26 118.7(2) . . ?
O3 C25 C30 120.1(2) . . ?
C26 C25 C30 121.1(2) . . ?
C25 C26 C27 118.4(2) . . ?
C25 C26 C24 121.3(2) . . ?
C27 C26 C24 120.3(2) . . ?
C38 C37 C12 112.6(3) . . ?
C38 C37 H37A 109.1 . . ?
C12 C37 H37A 109.1 . . ?
C38 C37 H37B 109.1 . . ?
C12 C37 H37B 109.1 . . ?
H37A C37 H37B 107.8 . . ?
C28 C27 C26 122.5(2) . . ?
C28 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
C29 C28 C27 116.9(2) . . ?
C29 C28 C31 121.2(2) . . ?
C27 C28 C31 122.0(2) . . ?
C30 C29 C28 123.0(2) . . ?
C30 C29 H29 118.5 . . ?
C28 C29 H29 118.5 . . ?
C29 C30 C25 118.1(2) . . ?
C29 C30 C36 120.2(2) . . ?
C25 C30 C36 121.6(2) . . ?
C32A C31 C33 139.8(8) . . ?
C32A C31 C33A 111.0(16) . . ?
C33 C31 C33A 49.9(10) . . ?
C32A C31 C28 110.2(7) . . ?
C33 C31 C28 109.7(4) . . ?
C33A C31 C28 108.5(5) . . ?
C32A C31 C32 48.8(13) . . ?
C33 C31 C32 109.2(5) . . ?
C33A C31 C32 64.2(12) . . ?
C28 C31 C32 112.9(3) . . ?
C32A C31 C34 59.8(13) . . ?
C33 C31 C34 111.1(7) . . ?
C33A C31 C34 142.6(6) . . ?
C28 C31 C34 108.6(4) . . ?
C32 C31 C34 105.3(5) . . ?
C32A C31 C34A 111.6(13) . . ?
C33 C31 C34A 57.1(9) . . ?
C33A C31 C34A 104.5(12) . . ?
C28 C31 C34A 110.9(6) . . ?
C32 C31 C34A 136.1(7) . . ?
C34 C31 C34A 56.5(9) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
C31 C32A H32D 109.5 . . ?
C31 C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C31 C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
C31 C33A H33D 109.5 . . ?
C31 C33A H33E 109.5 . . ?
H33D C33A H33E 109.5 . . ?
C31 C33A H33F 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
C31 C34A H34D 109.5 . . ?
C31 C34A H34E 109.5 . . ?
H34D C34A H34E 109.5 . . ?
C31 C34A H34F 109.5 . . ?
H34D C34A H34F 109.5 . . ?
H34E C34A H34F 109.5 . . ?
O3 C35 H35A 109.5 . . ?
O3 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O3 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C2 C36 C30 114.2(2) 2_566 . ?
C2 C36 H36A 108.7 2_566 . ?
C30 C36 H36A 108.7 . . ?
C2 C36 H36B 108.7 2_566 . ?
C30 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Cl2A C101 Cl2 21.9(6) . . ?
Cl2A C101 Cl3 127.6(7) . . ?
Cl2 C101 Cl3 108.4(8) . . ?
Cl2A C101 Cl1A 110.1(5) . . ?
Cl2 C101 Cl1A 113.3(7) . . ?
Cl3 C101 Cl1A 108.1(8) . . ?
Cl2A C101 Cl1 114.8(7) . . ?
Cl2 C101 Cl1 110.4(10) . . ?
Cl3 C101 Cl1 92.7(9) . . ?
Cl1A C101 Cl1 18.6(5) . . ?
Cl2A C101 Cl3A 114.8(5) . . ?
Cl2 C101 Cl3A 95.4(6) . . ?
Cl3 C101 Cl3A 13.0(7) . . ?
Cl1A C101 Cl3A 114.9(4) . . ?
Cl1 C101 Cl3A 97.7(5) . . ?
C101 Cl1 Cl3 42.7(5) . . ?
C101 Cl3 Cl1 44.6(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
C11 O1 C1 C6 90.1(3) . . . . ?
C11 O1 C1 C2 -93.9(3) . . . . ?
O1 C1 C2 C3 179.1(2) . . . . ?
C6 C1 C2 C3 -5.0(3) . . . . ?
O1 C1 C2 C36 -2.6(3) . . . 2_566 ?
C6 C1 C2 C36 173.4(2) . . . 2_566 ?
C1 C2 C3 C4 0.6(4) . . . . ?
C36 C2 C3 C4 -177.7(2) 2_566 . . . ?
C2 C3 C4 C5 3.5(4) . . . . ?
C2 C3 C4 C7 -176.5(3) . . . . ?
C3 C4 C5 C6 -3.5(4) . . . . ?
C7 C4 C5 C6 176.6(3) . . . . ?
C4 C5 C6 C1 -0.6(4) . . . . ?
C4 C5 C6 C12 177.0(2) . . . . ?
O1 C1 C6 C5 -179.1(2) . . . . ?
C2 C1 C6 C5 5.0(3) . . . . ?
O1 C1 C6 C12 3.2(3) . . . . ?
C2 C1 C6 C12 -172.7(2) . . . . ?
C3 C4 C7 C10 -158.1(13) . . . . ?
C5 C4 C7 C10 21.8(14) . . . . ?
C3 C4 C7 C9A 13(2) . . . . ?
C5 C4 C7 C9A -167(2) . . . . ?
C3 C4 C7 C10A -109(2) . . . . ?
C5 C4 C7 C10A 71(2) . . . . ?
C3 C4 C7 C8A 133.5(17) . . . . ?
C5 C4 C7 C8A -46.5(18) . . . . ?
C3 C4 C7 C8 76.8(9) . . . . ?
C5 C4 C7 C8 -103.2(9) . . . . ?
C3 C4 C7 C9 -36.6(7) . . . . ?
C5 C4 C7 C9 143.4(6) . . . . ?
C5 C6 C12 C14 83.7(3) . . . . ?
C1 C6 C12 C14 -98.7(3) . . . . ?
C5 C6 C12 C37 -42.0(3) . . . . ?
C1 C6 C12 C37 135.7(2) . . . . ?
C23 O2 C13 C18 103.5(3) . . . . ?
C23 O2 C13 C14 -80.8(3) . . . . ?
O2 C13 C14 C15 -179.8(2) . . . . ?
C18 C13 C14 C15 -4.2(4) . . . . ?
O2 C13 C14 C12 -4.4(4) . . . . ?
C18 C13 C14 C12 171.2(2) . . . . ?
C6 C12 C14 C15 -25.7(3) . . . . ?
C37 C12 C14 C15 101.8(3) . . . . ?
C6 C12 C14 C13 159.1(2) . . . . ?
C37 C12 C14 C13 -73.4(3) . . . . ?
C13 C14 C15 C16 2.0(4) . . . . ?
C12 C14 C15 C16 -173.4(2) . . . . ?
C14 C15 C16 C17 0.9(4) . . . . ?
C14 C15 C16 C19 -178.9(3) . . . . ?
C15 C16 C17 C18 -1.6(4) . . . . ?
C19 C16 C17 C18 178.2(3) . . . . ?
C16 C17 C18 C13 -0.6(4) . . . . ?
C16 C17 C18 C24 174.6(2) . . . . ?
O2 C13 C18 C17 179.3(2) . . . . ?
C14 C13 C18 C17 3.6(4) . . . . ?
O2 C13 C18 C24 4.1(3) . . . . ?
C14 C13 C18 C24 -171.5(2) . . . . ?
C17 C16 C19 C21 126.7(5) . . . . ?
C15 C16 C19 C21 -53.5(6) . . . . ?
C17 C16 C19 C22 -3.2(6) . . . . ?
C15 C16 C19 C22 176.6(5) . . . . ?
C17 C16 C19 C20 -120.9(5) . . . . ?
C15 C16 C19 C20 58.9(5) . . . . ?
C17 C18 C24 C26 108.2(3) . . . . ?
C13 C18 C24 C26 -76.8(3) . . . . ?
C35 O3 C25 C26 -99.5(3) . . . . ?
C35 O3 C25 C30 84.5(3) . . . . ?
O3 C25 C26 C27 -177.47(19) . . . . ?
C30 C25 C26 C27 -1.4(3) . . . . ?
O3 C25 C26 C24 2.8(3) . . . . ?
C30 C25 C26 C24 178.8(2) . . . . ?
C18 C24 C26 C25 -72.1(3) . . . . ?
C18 C24 C26 C27 108.2(2) . . . . ?
C6 C12 C37 C38 -61.7(4) . . . . ?
C14 C12 C37 C38 170.6(3) . . . . ?
C25 C26 C27 C28 0.8(3) . . . . ?
C24 C26 C27 C28 -179.4(2) . . . . ?
C26 C27 C28 C29 0.2(3) . . . . ?
C26 C27 C28 C31 178.9(2) . . . . ?
C27 C28 C29 C30 -0.7(4) . . . . ?
C31 C28 C29 C30 -179.5(2) . . . . ?
C28 C29 C30 C25 0.1(4) . . . . ?
C28 C29 C30 C36 178.7(2) . . . . ?
O3 C25 C30 C29 176.95(19) . . . . ?
C26 C25 C30 C29 1.0(3) . . . . ?
O3 C25 C30 C36 -1.6(3) . . . . ?
C26 C25 C30 C36 -177.5(2) . . . . ?
C29 C28 C31 C32A -129.8(15) . . . . ?
C27 C28 C31 C32A 51.5(16) . . . . ?
C29 C28 C31 C33 55.4(7) . . . . ?
C27 C28 C31 C33 -123.2(7) . . . . ?
C29 C28 C31 C33A 108.4(13) . . . . ?
C27 C28 C31 C33A -70.2(13) . . . . ?
C29 C28 C31 C32 177.5(4) . . . . ?
C27 C28 C31 C32 -1.2(5) . . . . ?
C29 C28 C31 C34 -66.1(6) . . . . ?
C27 C28 C31 C34 115.2(6) . . . . ?
C29 C28 C31 C34A -5.8(12) . . . . ?
C27 C28 C31 C34A 175.5(12) . . . . ?
C29 C30 C36 C2 -49.8(3) . . . 2_566 ?
C25 C30 C36 C2 128.6(2) . . . 2_566 ?
Cl2A C101 Cl1 Cl3 134.0(7) . . . . ?
Cl2 C101 Cl1 Cl3 110.8(8) . . . . ?
Cl1A C101 Cl1 Cl3 -147(2) . . . . ?
Cl3A C101 Cl1 Cl3 12.0(6) . . . . ?
Cl2A C101 Cl3 Cl1 -124.5(10) . . . . ?
Cl2 C101 Cl3 Cl1 -112.5(10) . . . . ?
Cl1A C101 Cl3 Cl1 10.6(7) . . . . ?
Cl3A C101 Cl3 Cl1 -113(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.049
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_xcalibur
_database_code_depnum_ccdc_archive 'CCDC 1015087'
_audit_update_record             
;
2014-07-19 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jun 24 17:59:44 2014'
;
_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_cell_length_a                   9.8040(3)
_cell_length_b                   13.8660(9)
_cell_length_c                   16.6686(11)
_cell_angle_alpha                109.672(6)
_cell_angle_beta                 95.074(4)
_cell_angle_gamma                107.133(4)
_cell_volume                     1994.21(19)
_cell_measurement_reflns_used    4115
_cell_measurement_theta_min      5.0750
_cell_measurement_theta_max      69.4040
_cell_oxdiff_length_a            9.8040(3)
_cell_oxdiff_length_b            13.8660(9)
_cell_oxdiff_length_c            16.6686(11)
_cell_oxdiff_angle_alpha         109.672(6)
_cell_oxdiff_angle_beta          95.074(4)
_cell_oxdiff_angle_gamma         107.133(4)
_cell_oxdiff_volume              1994.21(19)
_cell_oxdiff_measurement_reflns_used 4115
_exptl_absorpt_correction_T_min  0.77174
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0309
_diffrn_reflns_number            13511
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.6078
_diffrn_reflns_theta_max         71.3457
_diffrn_measured_fraction_theta_max 0.9766
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_orient_matrix_UB_11      -0.0373631000
_diffrn_orient_matrix_UB_12      -0.1112917000
_diffrn_orient_matrix_UB_13      -0.0753358000
_diffrn_orient_matrix_UB_21      -0.0190642000
_diffrn_orient_matrix_UB_22      -0.0571515000
_diffrn_orient_matrix_UB_23      0.0652168000
_diffrn_orient_matrix_UB_31      -0.1628117000
_diffrn_orient_matrix_UB_32      -0.0126749000
_diffrn_orient_matrix_UB_33      -0.0119554000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -21.00   21.00   1.0000    1.8500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 42

#__ type_ start__ end____ width___ exp.time_
  2 omega  -15.00   30.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   90.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega   -2.00   75.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 77

#__ type_ start__ end____ width___ exp.time_
  4 omega   23.00  110.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   90.0000 87

#__ type_ start__ end____ width___ exp.time_
  5 omega   50.00  115.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 65

#__ type_ start__ end____ width___ exp.time_
  6 omega   40.00   92.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   60.0000 52

#__ type_ start__ end____ width___ exp.time_
  7 omega   59.00  143.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
  8 omega   88.00  113.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
  9 omega   43.00   92.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000 -150.0000 49

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  127.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
 11 omega   41.00   67.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 12 omega   42.00   98.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 56

#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00   89.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  -90.0000 51

#__ type_ start__ end____ width___ exp.time_
 14 omega   37.00  119.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000   37.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 15 omega   71.00  110.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 39

#__ type_ start__ end____ width___ exp.time_
 16 omega  105.00  130.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 17 omega   48.00  123.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -120.0000 75

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   90.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 50

#__ type_ start__ end____ width___ exp.time_
 19 omega   36.00  178.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000   30.0000 142

#__ type_ start__ end____ width___ exp.time_
 20 omega   38.00   84.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 46

#__ type_ start__ end____ width___ exp.time_
 21 omega   37.00   92.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 22 omega   25.00   50.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   17.00   51.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -120.0000 34

#__ type_ start__ end____ width___ exp.time_
 24 omega   36.00   87.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 51

#__ type_ start__ end____ width___ exp.time_
 25 omega   23.00   69.00   1.0000    1.8500
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 46

#__ type_ start__ end____ width___ exp.time_
 26 omega  -68.00  -30.00   1.0000    1.8500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
 27 omega  -20.00   16.00   1.0000    1.8500
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 36

;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_cell_setting           triclinic
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_gnu010
_database_code_depnum_ccdc_archive 'CCDC 1015089'
_audit_update_record             
;
2014-07-19 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H92 O6'
_chemical_formula_weight         1125.52

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           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   13.3230(14)
_cell_length_b                   16.3491(14)
_cell_length_c                   17.448(2)
_cell_angle_alpha                72.532(10)
_cell_angle_beta                 84.273(10)
_cell_angle_gamma                89.557(8)
_cell_volume                     3606.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1997
_cell_measurement_theta_min      3.3360
_cell_measurement_theta_max      19.9200

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_min  0.9793
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       ω/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30898
_diffrn_reflns_av_R_equivalents  0.2889
_diffrn_reflns_av_sigmaI/netI    0.6725
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12654
_reflns_number_gt                2835
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97

_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)+(0.1945P)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    riding
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.111(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         12654
_refine_ls_number_parameters     782
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.4219
_refine_ls_R_factor_gt           0.1584
_refine_ls_wR_factor_ref         0.4984
_refine_ls_wR_factor_gt          0.3448
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_restrained_S_all      0.948
_refine_ls_shift/su_max          1.837
_refine_ls_shift/su_mean         0.039

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 0.1959(6) 0.9863(4) 0.4093(4) 0.083(2) Uani 1 1 d . . .
O2 O 0.4830(5) 0.8126(4) 0.3024(4) 0.080(2) Uani 1 1 d . . .
O3 O 0.6496(5) 0.9155(4) 0.3707(4) 0.082(2) Uani 1 1 d . . .
O4 O 0.1560(6) 0.6641(4) 0.3690(4) 0.087(2) Uani 1 1 d . . .
O5 O -0.0187(5) 0.8080(4) 0.3037(4) 0.079(2) Uani 1 1 d . . .
O6 O -0.3076(6) 0.5707(4) 0.4124(4) 0.081(2) Uani 1 1 d . . .
C1 C 0.0904(9) 0.9671(8) 0.4098(9) 0.118(5) Uani 1 1 d . . .
H1A H 0.0824 0.9090 0.4058 0.177 Uiso 1 1 calc R . .
H1B H 0.0633 1.0085 0.3639 0.177 Uiso 1 1 calc R . .
H1C H 0.0537 0.9707 0.4603 0.177 Uiso 1 1 calc R . .
C2 C 0.2463(8) 0.9189(6) 0.4580(8) 0.068(3) Uani 1 1 d . . .
C3 C 0.2590(8) 0.9178(6) 0.5364(7) 0.066(3) Uani 1 1 d . . .
C4 C 0.3124(8) 0.8523(6) 0.5839(7) 0.075(3) Uani 1 1 d . . .
C5 C 0.3553(8) 0.7874(6) 0.5520(8) 0.080(3) Uani 1 1 d . . .
C6 C 0.3391(9) 0.7920(7) 0.4707(8) 0.080(4) Uani 1 1 d . . .
C16 C 0.3296(8) 1.0072(6) 0.2418(6) 0.072(3) Uani 1 1 d . . .
C7 C 0.2881(8) 0.8570(6) 0.4257(7) 0.066(3) Uani 1 1 d . . .
C8 C 0.4146(12) 0.7157(8) 0.6074(10) 0.111(4) Uani 1 1 d . . .
C9 C 0.399(3) 0.6314(10) 0.5935(15) 0.36(2) Uani 1 1 d . . .
H9A H 0.4239 0.6353 0.5377 0.534 Uiso 1 1 calc R . .
H9B H 0.3269 0.6160 0.6030 0.534 Uiso 1 1 calc R . .
H9C H 0.4361 0.5874 0.6308 0.534 Uiso 1 1 calc R . .
C10 C 0.384(2) 0.6983(11) 0.6992(13) 0.264(14) Uani 1 1 d . . .
H10A H 0.4373 0.6661 0.7296 0.397 Uiso 1 1 calc R . .
H10B H 0.3207 0.6649 0.7149 0.397 Uiso 1 1 calc R . .
H10C H 0.3755 0.7530 0.7110 0.397 Uiso 1 1 calc R . .
C11 C 0.5194(18) 0.7349(14) 0.594(2) 0.42(3) Uani 1 1 d . . .
H11A H 0.5509 0.7081 0.5548 0.628 Uiso 1 1 calc R . .
H11B H 0.5495 0.7128 0.6452 0.628 Uiso 1 1 calc R . .
H11C H 0.5305 0.7972 0.5734 0.628 Uiso 1 1 calc R . .
C12 C 0.2803(8) 0.8611(6) 0.3379(7) 0.082(4) Uani 1 1 d . . .
H12A H 0.2896 0.8032 0.3318 0.099 Uiso 1 1 calc R . .
H12B H 0.2122 0.8801 0.3231 0.099 Uiso 1 1 calc R . .
C13 C 0.4746(8) 0.7597(6) 0.2508(7) 0.099(4) Uani 1 1 d . . .
H13A H 0.4241 0.7832 0.2134 0.148 Uiso 1 1 calc R . .
H13B H 0.4540 0.7013 0.2838 0.148 Uiso 1 1 calc R . .
H13C H 0.5400 0.7585 0.2201 0.148 Uiso 1 1 calc R . .
C14 C 0.4559(8) 0.8975(6) 0.2650(6) 0.063(3) Uani 1 1 d . . .
C15 C 0.3592(8) 0.9227(6) 0.2813(6) 0.069(3) Uani 1 1 d . . .
C17 C 0.4043(8) 1.0670(6) 0.1922(7) 0.080(4) Uani 1 1 d . . .
C18 C 0.5010(7) 1.0423(6) 0.1804(6) 0.070(3) Uani 1 1 d . . .
C19 C 0.5307(7) 0.9572(6) 0.2176(6) 0.076(3) Uani 1 1 d . . .
C20 C 0.3647(11) 1.1574(6) 0.1445(10) 0.133(7) Uani 1 1 d . . .
C21 C 0.284(2) 1.1822(11) 0.1779(19) 0.44(3) Uani 1 1 d . . .
H21A H 0.3010 1.2284 0.1996 0.655 Uiso 1 1 calc R . .
H21B H 0.2529 1.1338 0.2219 0.655 Uiso 1 1 calc R . .
H21C H 0.2359 1.2030 0.1375 0.655 Uiso 1 1 calc R . .
C22 C 0.391(2) 1.1763(13) 0.0586(16) 0.266(13) Uani 1 1 d . . .
H22A H 0.3654 1.2324 0.0306 0.399 Uiso 1 1 calc R . .
H22B H 0.3616 1.1321 0.0397 0.399 Uiso 1 1 calc R . .
H22C H 0.4648 1.1770 0.0473 0.399 Uiso 1 1 calc R . .
C23 C 0.4508(18) 1.2251(9) 0.1463(16) 0.268(14) Uani 1 1 d . . .
H23A H 0.4390 1.2810 0.1078 0.401 Uiso 1 1 calc R . .
H23B H 0.5171 1.2048 0.1313 0.401 Uiso 1 1 calc R . .
H23C H 0.4486 1.2308 0.2007 0.401 Uiso 1 1 calc R . .
C24 C 0.6389(7) 0.9320(5) 0.2060(6) 0.071(3) Uani 1 1 d . . .
H24 H 0.6437 0.8722 0.2426 0.085 Uiso 1 1 calc R . .
C25 C 0.5635(9) 0.9483(7) 0.4105(7) 0.106(5) Uani 1 1 d . . .
H25A H 0.5833 0.9594 0.4591 0.158 Uiso 1 1 calc R . .
H25B H 0.5079 0.9057 0.4255 0.158 Uiso 1 1 calc R . .
H25C H 0.5416 1.0017 0.3735 0.158 Uiso 1 1 calc R . .
C26 C 0.7118(7) 0.9782(6) 0.3179(7) 0.067(3) Uani 1 1 d . . .
C27 C 0.7092(7) 0.9897(5) 0.2359(7) 0.063(3) Uani 1 1 d . . .
C28 C 0.7700(7) 1.0563(5) 0.1765(7) 0.078(3) Uani 1 1 d . . .
C29 C 0.8332(8) 1.1068(6) 0.2040(7) 0.074(3) Uani 1 1 d . . .
C30 C 0.8385(7) 1.0916(5) 0.2843(8) 0.070(3) Uani 1 1 d . . .
C31 C 0.7795(8) 1.0270(6) 0.3434(6) 0.066(3) Uani 1 1 d . . .
C32 C 0.8970(10) 1.1794(7) 0.1400(7) 0.091(4) Uani 1 1 d . . .
C33 C 0.8266(13) 1.2428(8) 0.0942(10) 0.152(6) Uani 1 1 d . . .
H33A H 0.7857 1.2673 0.1313 0.229 Uiso 1 1 calc R . .
H33B H 0.7824 1.2140 0.0682 0.229 Uiso 1 1 calc R . .
H33C H 0.8657 1.2887 0.0528 0.229 Uiso 1 1 calc R . .
C34 C 0.9593(11) 1.1455(8) 0.0801(9) 0.152(7) Uani 1 1 d . . .
H34A H 0.9153 1.1144 0.0561 0.228 Uiso 1 1 calc R . .
H34B H 1.0097 1.1067 0.1076 0.228 Uiso 1 1 calc R . .
H34C H 0.9934 1.1935 0.0376 0.228 Uiso 1 1 calc R . .
C35 C 0.9608(11) 1.2283(9) 0.1781(8) 0.151(7) Uani 1 1 d . . .
H35A H 0.9938 1.2773 0.1362 0.227 Uiso 1 1 calc R . .
H35B H 1.0121 1.1907 0.2057 0.227 Uiso 1 1 calc R . .
H35C H 0.9181 1.2489 0.2172 0.227 Uiso 1 1 calc R . .
C36 C 0.7866(8) 1.0128(6) 0.4306(7) 0.082(4) Uani 1 1 d . . .
H36A H 0.8586 1.0079 0.4403 0.099 Uiso 1 1 calc R . .
H36B H 0.7525 0.9574 0.4612 0.099 Uiso 1 1 calc R . .
C37 C 0.6670(7) 0.9282(6) 0.1197(6) 0.075(3) Uani 1 1 d . . .
H37A H 0.6134 0.8956 0.1053 0.089 Uiso 1 1 calc R . .
H37B H 0.6689 0.9873 0.0822 0.089 Uiso 1 1 calc R . .
C38 C 0.7673(10) 0.8874(7) 0.1074(8) 0.096(4) Uani 1 1 d . . .
H38 H 0.7774 0.8326 0.1442 0.115 Uiso 1 1 calc R . .
C39 C 0.8408(11) 0.9192(10) 0.0518(10) 0.165(7) Uani 1 1 d . . .
H39A H 0.8346 0.9737 0.0134 0.198 Uiso 1 1 calc R . .
H39B H 0.9009 0.8879 0.0495 0.198 Uiso 1 1 calc R . .
C40 C 0.0686(9) 0.6086(6) 0.4083(7) 0.103(4) Uani 1 1 d . . .
H40A H 0.0435 0.5823 0.3701 0.155 Uiso 1 1 calc R . .
H40B H 0.0155 0.6428 0.4258 0.155 Uiso 1 1 calc R . .
H40C H 0.0883 0.5636 0.4553 0.155 Uiso 1 1 calc R . .
C41 C 0.2170(7) 0.6363(6) 0.3122(7) 0.064(3) Uani 1 1 d . . .
C42 C 0.2843(8) 0.5708(5) 0.3374(7) 0.068(3) Uani 1 1 d . . .
C43 C 0.3448(7) 0.5442(6) 0.2780(8) 0.072(3) Uani 1 1 d . . .
C44 C 0.3334(9) 0.5813(6) 0.1959(8) 0.086(4) Uani 1 1 d . . .
C45 C 0.2670(8) 0.6506(5) 0.1732(7) 0.076(3) Uani 1 1 d . . .
C46 C 0.2084(7) 0.6794(6) 0.2296(8) 0.071(3) Uani 1 1 d . . .
C47 C 0.3960(12) 0.5509(8) 0.1353(9) 0.115(5) Uani 1 1 d . . .
C48 C 0.425(3) 0.4639(11) 0.1621(12) 0.32(2) Uani 1 1 d . . .
H48A H 0.3742 0.4308 0.2044 0.484 Uiso 1 1 calc R . .
H48B H 0.4904 0.4607 0.1838 0.484 Uiso 1 1 calc R . .
H48C H 0.4302 0.4401 0.1166 0.484 Uiso 1 1 calc R . .
C49 C 0.343(3) 0.550(3) 0.072(2) 0.51(4) Uani 1 1 d . . .
H49A H 0.2712 0.5547 0.0868 0.760 Uiso 1 1 calc R . .
H49B H 0.3555 0.4965 0.0588 0.760 Uiso 1 1 calc R . .
H49C H 0.3661 0.5988 0.0248 0.760 Uiso 1 1 calc R . .
C50 C 0.480(3) 0.610(2) 0.098(3) 0.47(3) Uani 1 1 d . . .
H50A H 0.5359 0.5971 0.1317 0.705 Uiso 1 1 calc R . .
H50B H 0.4586 0.6690 0.0918 0.705 Uiso 1 1 calc R . .
H50C H 0.5023 0.6042 0.0444 0.705 Uiso 1 1 calc R . .
C51 C 0.1375(7) 0.7525(5) 0.2077(6) 0.066(3) Uani 1 1 d . . .
H51 H 0.1426 0.7862 0.2465 0.080 Uiso 1 1 calc R . .
C52 C -0.0270(9) 0.8951(6) 0.2548(7) 0.095(4) Uani 1 1 d . . .
H52A H 0.0396 0.9174 0.2278 0.142 Uiso 1 1 calc R . .
H52B H -0.0527 0.9300 0.2891 0.142 Uiso 1 1 calc R . .
H52C H -0.0736 0.8974 0.2141 0.142 Uiso 1 1 calc R . .
C53 C -0.0445(8) 0.7484(5) 0.2655(6) 0.069(3) Uani 1 1 d . . .
C54 C -0.1426(7) 0.7128(5) 0.2823(6) 0.066(3) Uani 1 1 d . . .
C55 C -0.1710(8) 0.6563(6) 0.2400(7) 0.078(3) Uani 1 1 d . . .
C56 C -0.0977(8) 0.6299(5) 0.1894(7) 0.077(3) Uani 1 1 d . . .
C57 C 0.0011(8) 0.6624(5) 0.1792(6) 0.076(3) Uani 1 1 d . . .
C58 C 0.0289(7) 0.7204(5) 0.2176(6) 0.060(3) Uani 1 1 d . . .
C59 C -0.1287(11) 0.5708(8) 0.1415(9) 0.103(4) Uani 1 1 d . . .
C60 C -0.167(3) 0.6172(15) 0.0725(18) 0.41(3) Uani 1 1 d . . .
H60A H -0.2411 0.6138 0.0809 0.612 Uiso 1 1 calc R . .
H60B H -0.1439 0.5938 0.0284 0.612 Uiso 1 1 calc R . .
H60C H -0.1444 0.6772 0.0585 0.612 Uiso 1 1 calc R . .
C61 C -0.1921(17) 0.5002(12) 0.1929(13) 0.270(15) Uani 1 1 d . . .
H61A H -0.2617 0.5193 0.1980 0.406 Uiso 1 1 calc R . .
H61B H -0.1678 0.4806 0.2464 0.406 Uiso 1 1 calc R . .
H61C H -0.1899 0.4530 0.1691 0.406 Uiso 1 1 calc R . .
C62 C -0.0401(16) 0.5237(16) 0.1147(19) 0.302(18) Uani 1 1 d . . .
H62A H -0.0187 0.4796 0.1616 0.452 Uiso 1 1 calc R . .
H62B H 0.0159 0.5644 0.0896 0.452 Uiso 1 1 calc R . .
H62C H -0.0604 0.4965 0.0754 0.452 Uiso 1 1 calc R . .
C63 C -0.2202(8) 0.7385(6) 0.3386(7) 0.080(4) Uani 1 1 d . . .
H63A H -0.2117 0.8004 0.3318 0.096 Uiso 1 1 calc R . .
H63B H -0.2884 0.7288 0.3245 0.096 Uiso 1 1 calc R . .
C64 C -0.4098(10) 0.5920(8) 0.4095(9) 0.135(5) Uani 1 1 d . . .
H64A H -0.4470 0.5654 0.4626 0.203 Uiso 1 1 calc R . .
H64B H -0.4380 0.5711 0.3690 0.203 Uiso 1 1 calc R . .
H64C H -0.4157 0.6545 0.3951 0.203 Uiso 1 1 calc R . .
C65 C -0.2553(7) 0.6061(6) 0.4602(8) 0.074(3) Uani 1 1 d . . .
C66 C -0.2118(8) 0.6886(6) 0.4250(7) 0.071(3) Uani 1 1 d . . .
C67 C -0.1584(9) 0.7232(6) 0.4737(8) 0.078(3) Uani 1 1 d . . .
C68 C -0.1458(8) 0.6795(6) 0.5506(8) 0.083(4) Uani 1 1 d . . .
C69 C -0.1905(7) 0.5957(6) 0.5882(7) 0.077(3) Uani 1 1 d . . .
C70 C -0.2459(7) 0.5609(6) 0.5398(8) 0.068(3) Uani 1 1 d . . .
C71 C -0.2960(8) 0.4725(5) 0.5761(7) 0.075(3) Uani 1 1 d . . .
H71A H -0.3690 0.4779 0.5698 0.090 Uiso 1 1 calc R . .
H71B H -0.2682 0.4349 0.5444 0.090 Uiso 1 1 calc R . .
C72 C -0.0838(12) 0.7128(7) 0.6051(9) 0.107(4) Uani 1 1 d . . .
C73 C -0.119(2) 0.6761(15) 0.6958(12) 0.294(17) Uani 1 1 d . . .
H73A H -0.1098 0.6139 0.7132 0.441 Uiso 1 1 calc R . .
H73B H -0.1908 0.6880 0.7053 0.441 Uiso 1 1 calc R . .
H73C H -0.0796 0.7029 0.7266 0.441 Uiso 1 1 calc R . .
C74 C 0.0135(17) 0.700(3) 0.596(3) 0.51(4) Uani 1 1 d . . .
H74A H 0.0482 0.7256 0.6301 0.759 Uiso 1 1 calc R . .
H74B H 0.0394 0.7265 0.5391 0.759 Uiso 1 1 calc R . .
H74C H 0.0254 0.6382 0.6109 0.759 Uiso 1 1 calc R . .
C75 C -0.092(3) 0.8043(11) 0.5892(19) 0.42(3) Uani 1 1 d . . .
H75A H -0.1162 0.8168 0.6393 0.637 Uiso 1 1 calc R . .
H75B H -0.1393 0.8263 0.5488 0.637 Uiso 1 1 calc R . .
H75C H -0.0254 0.8319 0.5688 0.637 Uiso 1 1 calc R . .
C76 C 0.1642(7) 0.8155(5) 0.1203(6) 0.076(3) Uani 1 1 d . . .
H76A H 0.1677 0.7821 0.0814 0.091 Uiso 1 1 calc R . .
H76B H 0.1089 0.8566 0.1074 0.091 Uiso 1 1 calc R . .
C77 C 0.2615(10) 0.8650(7) 0.1091(8) 0.102(4) Uani 1 1 d . . .
H77 H 0.2651 0.8989 0.1445 0.122 Uiso 1 1 calc R . .
C78 C 0.3393(11) 0.8693(7) 0.0607(9) 0.131(5) Uani 1 1 d . . .
H78A H 0.3420 0.8373 0.0231 0.158 Uiso 1 1 calc R . .
H78B H 0.3953 0.9044 0.0617 0.158 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 C2 1.388(12) . ?
O1 C1 1.441(12) . ?
O2 C14 1.406(11) . ?
O2 C13 1.435(11) . ?
O3 C26 1.371(10) . ?
O3 C25 1.463(11) . ?
O4 C41 1.398(10) . ?
O4 C40 1.459(11) . ?
O5 C53 1.396(10) . ?
O5 C52 1.433(11) . ?
O6 C65 1.388(12) . ?
O6 C64 1.406(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C7 1.386(12) . ?
C2 C3 1.389(14) . ?
C3 C4 1.384(14) . ?
C3 C36 1.516(12) 2_676 ?
C4 C5 1.429(13) . ?
C5 C6 1.437(15) . ?
C5 C8 1.546(18) . ?
C6 C7 1.342(15) . ?
C16 C15 1.419(13) . ?
C16 C17 1.424(12) . ?
C7 C12 1.528(14) . ?
C8 C11 1.42(2) . ?
C8 C9 1.488(17) . ?
C8 C10 1.55(2) . ?
C9 H9A 0.9802 . ?
C9 H9B 0.9802 . ?
C9 H9C 0.9802 . ?
C10 H10A 0.9803 . ?
C10 H10B 0.9803 . ?
C10 H10C 0.9803 . ?
C11 H11A 0.9804 . ?
C11 H11B 0.9804 . ?
C11 H11C 0.9804 . ?
C12 C15 1.518(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.379(12) . ?
C14 C19 1.413(11) . ?
C17 C18 1.361(12) . ?
C17 C20 1.579(16) . ?
C18 C19 1.419(13) . ?
C19 C24 1.507(13) . ?
C20 C21 1.295(16) . ?
C20 C22 1.44(2) . ?
C20 C23 1.61(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C37 1.534(12) . ?
C24 C27 1.565(13) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.391(13) . ?
C26 C31 1.397(13) . ?
C27 C28 1.444(12) . ?
C28 C29 1.396(13) . ?
C29 C30 1.358(14) . ?
C29 C32 1.551(13) . ?
C30 C31 1.412(12) . ?
C31 C36 1.480(13) . ?
C32 C33 1.493(19) . ?
C32 C35 1.498(15) . ?
C32 C34 1.501(14) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C3 1.516(12) 2_676 ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.514(14) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.299(15) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9500 . ?
C39 H39B 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.388(13) . ?
C41 C46 1.417(13) . ?
C42 C43 1.417(13) . ?
C42 C71 1.486(13) 2_566 ?
C43 C44 1.400(15) . ?
C44 C45 1.418(14) . ?
C44 C47 1.481(14) . ?
C45 C46 1.385(12) . ?
C46 C51 1.499(13) . ?
C47 C49 1.37(3) . ?
C47 C48 1.421(18) . ?
C47 C50 1.45(2) . ?
C48 H48A 0.9810 . ?
C48 H48B 0.9810 . ?
C48 H48C 0.9810 . ?
C49 H49A 0.9810 . ?
C49 H49B 0.9810 . ?
C49 H49C 0.9809 . ?
C50 H50A 1.0347 . ?
C50 H50B 1.0398 . ?
C50 H50C 1.0330 . ?
C51 C58 1.519(12) . ?
C51 C76 1.571(12) . ?
C51 H51 1.0000 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C58 1.387(11) . ?
C53 C54 1.402(12) . ?
C54 C55 1.417(13) . ?
C54 C63 1.500(11) . ?
C55 C56 1.403(12) . ?
C56 C57 1.397(13) . ?
C56 C59 1.538(14) . ?
C57 C58 1.386(11) . ?
C59 C60 1.36(2) . ?
C59 C61 1.446(16) . ?
C59 C62 1.52(2) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C66 1.498(14) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C70 1.382(14) . ?
C65 C66 1.406(12) . ?
C66 C67 1.401(15) . ?
C67 C68 1.344(14) . ?
C68 C69 1.434(12) . ?
C68 C72 1.535(17) . ?
C69 C70 1.414(14) . ?
C70 C71 1.522(11) . ?
C71 C42 1.486(13) 2_566 ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C74 1.31(2) . ?
C72 C75 1.442(18) . ?
C72 C73 1.541(19) . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9805 . ?
C74 H74B 0.9805 . ?
C74 H74C 0.9806 . ?
C75 H75A 1.0069 . ?
C75 H75B 1.0071 . ?
C75 H75C 1.0066 . ?
C76 C77 1.498(13) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 C78 1.259(14) . ?
C77 H77 0.9500 . ?
C78 H78A 0.9500 . ?
C78 H78B 0.9500 . ?

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 O1 C1 113.0(8) . . ?
C14 O2 C13 111.5(8) . . ?
C26 O3 C25 114.0(7) . . ?
C41 O4 C40 115.2(6) . . ?
C53 O5 C52 113.0(8) . . ?
C65 O6 C64 115.2(9) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 121.5(11) . . ?
C7 C2 O1 119.2(12) . . ?
C3 C2 O1 119.2(9) . . ?
C4 C3 C2 119.2(9) . . ?
C4 C3 C36 120.6(11) . 2_676 ?
C2 C3 C36 120.2(11) . 2_676 ?
C3 C4 C5 120.2(11) . . ?
C4 C5 C6 117.8(11) . . ?
C4 C5 C8 118.3(12) . . ?
C6 C5 C8 123.9(10) . . ?
C7 C6 C5 120.6(10) . . ?
C15 C16 C17 118.6(9) . . ?
C6 C7 C2 120.7(11) . . ?
C6 C7 C12 117.6(10) . . ?
C2 C7 C12 121.7(12) . . ?
C11 C8 C9 108(2) . . ?
C11 C8 C5 111.2(14) . . ?
C9 C8 C5 111.9(14) . . ?
C11 C8 C10 106(2) . . ?
C9 C8 C10 104.4(16) . . ?
C5 C8 C10 114.7(12) . . ?
C8 C9 H9A 109.4 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.4 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.4 . . ?
C8 C10 H10A 109.7 . . ?
C8 C10 H10B 109.4 . . ?
H10A C10 H10B 109.4 . . ?
C8 C10 H10C 109.4 . . ?
H10A C10 H10C 109.4 . . ?
H10B C10 H10C 109.4 . . ?
C8 C11 H11A 109.6 . . ?
C8 C11 H11B 109.4 . . ?
H11A C11 H11B 109.4 . . ?
C8 C11 H11C 109.6 . . ?
H11A C11 H11C 109.4 . . ?
H11B C11 H11C 109.4 . . ?
C15 C12 C7 111.1(8) . . ?
C15 C12 H12A 109.4 . . ?
C7 C12 H12A 109.4 . . ?
C15 C12 H12B 109.4 . . ?
C7 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.4 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 O2 119.3(8) . . ?
C15 C14 C19 121.1(9) . . ?
O2 C14 C19 119.3(9) . . ?
C14 C15 C16 119.9(8) . . ?
C14 C15 C12 121.9(9) . . ?
C16 C15 C12 118.1(9) . . ?
C18 C17 C16 120.5(9) . . ?
C18 C17 C20 123.2(9) . . ?
C16 C17 C20 115.9(9) . . ?
C17 C18 C19 121.4(8) . . ?
C14 C19 C18 118.0(9) . . ?
C14 C19 C24 121.5(9) . . ?
C18 C19 C24 120.5(8) . . ?
C21 C20 C22 125(2) . . ?
C21 C20 C17 115.6(11) . . ?
C22 C20 C17 111.2(11) . . ?
C21 C20 C23 104.3(19) . . ?
C22 C20 C23 89.0(15) . . ?
C17 C20 C23 104.9(14) . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.6 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.4 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.6 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.4 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 C37 111.2(9) . . ?
C19 C24 C27 109.7(7) . . ?
C37 C24 C27 115.8(8) . . ?
C19 C24 H24 106.5 . . ?
C37 C24 H24 106.5 . . ?
C27 C24 H24 106.5 . . ?
O3 C25 H25A 109.5 . . ?
O3 C25 H25B 109.4 . . ?
H25A C25 H25B 109.5 . . ?
O3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 C27 117.3(9) . . ?
O3 C26 C31 122.8(10) . . ?
C27 C26 C31 119.8(9) . . ?
C26 C27 C28 120.6(9) . . ?
C26 C27 C24 120.7(8) . . ?
C28 C27 C24 118.6(9) . . ?
C29 C28 C27 118.0(11) . . ?
C30 C29 C28 120.4(10) . . ?
C30 C29 C32 121.7(10) . . ?
C28 C29 C32 118.0(11) . . ?
C29 C30 C31 122.5(10) . . ?
C26 C31 C30 118.5(10) . . ?
C26 C31 C36 120.5(9) . . ?
C30 C31 C36 120.9(10) . . ?
C33 C32 C35 105.9(11) . . ?
C33 C32 C34 107.2(13) . . ?
C35 C32 C34 111.5(12) . . ?
C33 C32 C29 108.3(10) . . ?
C35 C32 C29 112.1(11) . . ?
C34 C32 C29 111.4(9) . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.4 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.4 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C31 C36 C3 115.1(10) . 2_676 ?
C31 C36 H36A 108.5 . . ?
C3 C36 H36A 108.5 2_676 . ?
C31 C36 H36B 108.5 . . ?
C3 C36 H36B 108.5 2_676 . ?
H36A C36 H36B 107.5 . . ?
C38 C37 C24 114.5(9) . . ?
C38 C37 H37A 108.6 . . ?
C24 C37 H37A 108.6 . . ?
C38 C37 H37B 108.7 . . ?
C24 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C39 C38 C37 126.9(13) . . ?
C39 C38 H38 116.5 . . ?
C37 C38 H38 116.6 . . ?
C38 C39 H39A 120.0 . . ?
C38 C39 H39B 120.0 . . ?
H39A C39 H39B 120.0 . . ?
O4 C40 H40A 109.5 . . ?
O4 C40 H40B 109.4 . . ?
H40A C40 H40B 109.5 . . ?
O4 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 O4 120.2(11) . . ?
C42 C41 C46 122.7(9) . . ?
O4 C41 C46 117.1(9) . . ?
C41 C42 C43 118.6(11) . . ?
C41 C42 C71 122.8(10) . 2_566 ?
C43 C42 C71 118.6(10) . 2_566 ?
C44 C43 C42 120.3(10) . . ?
C43 C44 C45 118.8(9) . . ?
C43 C44 C47 119.1(12) . . ?
C45 C44 C47 121.9(13) . . ?
C46 C45 C44 122.2(11) . . ?
C45 C46 C41 117.1(10) . . ?
C45 C46 C51 123.7(11) . . ?
C41 C46 C51 119.2(9) . . ?
C49 C47 C48 101(2) . . ?
C49 C47 C50 104(3) . . ?
C48 C47 C50 113(2) . . ?
C49 C47 C44 111.6(16) . . ?
C48 C47 C44 115.4(13) . . ?
C50 C47 C44 110.8(13) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.6 . . ?
H48A C48 H48B 109.4 . . ?
C47 C48 H48C 109.7 . . ?
H48A C48 H48C 109.4 . . ?
H48B C48 H48C 109.4 . . ?
C47 C49 H49A 109.7 . . ?
C47 C49 H49B 109.8 . . ?
H49A C49 H49B 109.4 . . ?
C47 C49 H49C 109.2 . . ?
H49A C49 H49C 109.3 . . ?
H49B C49 H49C 109.4 . . ?
C47 C50 H50A 115.1 . . ?
C47 C50 H50B 116.1 . . ?
H50A C50 H50B 103.1 . . ?
C47 C50 H50C 114.7 . . ?
H50A C50 H50C 103.3 . . ?
H50B C50 H50C 102.7 . . ?
C46 C51 C58 111.3(7) . . ?
C46 C51 C76 113.5(8) . . ?
C58 C51 C76 109.9(8) . . ?
C46 C51 H51 107.3 . . ?
C58 C51 H51 107.3 . . ?
C76 C51 H51 107.3 . . ?
O5 C52 H52A 109.5 . . ?
O5 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O5 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C58 C53 O5 119.7(9) . . ?
C58 C53 C54 121.3(8) . . ?
O5 C53 C54 118.7(8) . . ?
C53 C54 C55 118.9(8) . . ?
C53 C54 C63 121.6(8) . . ?
C55 C54 C63 119.3(9) . . ?
C56 C55 C54 119.4(9) . . ?
C57 C56 C55 119.4(9) . . ?
C57 C56 C59 120.9(9) . . ?
C55 C56 C59 119.6(10) . . ?
C58 C57 C56 121.8(9) . . ?
C53 C58 C57 118.6(9) . . ?
C53 C58 C51 120.6(8) . . ?
C57 C58 C51 120.8(8) . . ?
C60 C59 C61 115(2) . . ?
C60 C59 C62 106(2) . . ?
C61 C59 C62 101.4(16) . . ?
C60 C59 C56 110.7(12) . . ?
C61 C59 C56 110.8(11) . . ?
C62 C59 C56 112.5(13) . . ?
C59 C60 H60A 109.7 . . ?
C59 C60 H60B 109.3 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.4 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.3 . . ?
C59 C61 H61B 109.6 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.6 . . ?
C59 C62 H62B 109.4 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.4 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C66 C63 C54 111.8(9) . . ?
C66 C63 H63A 109.2 . . ?
C54 C63 H63A 109.2 . . ?
C66 C63 H63B 109.3 . . ?
C54 C63 H63B 109.3 . . ?
H63A C63 H63B 107.9 . . ?
O6 C64 H64A 109.5 . . ?
O6 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O6 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C70 C65 O6 120.6(9) . . ?
C70 C65 C66 121.2(11) . . ?
O6 C65 C66 118.2(12) . . ?
C67 C66 C65 117.5(11) . . ?
C67 C66 C63 120.4(9) . . ?
C65 C66 C63 122.1(11) . . ?
C68 C67 C66 122.3(10) . . ?
C67 C68 C69 121.3(11) . . ?
C67 C68 C72 124.3(10) . . ?
C69 C68 C72 114.5(12) . . ?
C70 C69 C68 116.7(11) . . ?
C65 C70 C69 120.9(9) . . ?
C65 C70 C71 119.6(10) . . ?
C69 C70 C71 119.4(11) . . ?
C42 C71 C70 116.1(9) 2_566 . ?
C42 C71 H71A 108.2 2_566 . ?
C70 C71 H71A 108.2 . . ?
C42 C71 H71B 108.3 2_566 . ?
C70 C71 H71B 108.3 . . ?
H71A C71 H71B 107.4 . . ?
C74 C72 C75 105(2) . . ?
C74 C72 C68 114.3(13) . . ?
C75 C72 C68 111.8(14) . . ?
C74 C72 C73 107(2) . . ?
C75 C72 C73 103.9(18) . . ?
C68 C72 C73 113.8(12) . . ?
C72 C73 H73A 109.4 . . ?
C72 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72 C74 H74A 109.6 . . ?
C72 C74 H74B 109.3 . . ?
H74A C74 H74B 109.4 . . ?
C72 C74 H74C 109.7 . . ?
H74A C74 H74C 109.4 . . ?
H74B C74 H74C 109.4 . . ?
C72 C75 H75A 112.3 . . ?
C72 C75 H75B 112.4 . . ?
H75A C75 H75B 106.5 . . ?
C72 C75 H75C 112.2 . . ?
H75A C75 H75C 106.5 . . ?
H75B C75 H75C 106.5 . . ?
C77 C76 C51 114.4(9) . . ?
C77 C76 H76A 108.7 . . ?
C51 C76 H76A 108.7 . . ?
C77 C76 H76B 108.6 . . ?
C51 C76 H76B 108.7 . . ?
H76A C76 H76B 107.6 . . ?
C78 C77 C76 130.9(12) . . ?
C78 C77 H77 114.5 . . ?
C76 C77 H77 114.6 . . ?
C77 C78 H78A 120.0 . . ?
C77 C78 H78B 120.0 . . ?
H78A C78 H78B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 C2 C7 88.3(10) . . . . ?
C1 O1 C2 C3 -95.6(10) . . . . ?
C7 C2 C3 C4 -1.7(13) . . . . ?
O1 C2 C3 C4 -177.7(8) . . . . ?
C7 C2 C3 C36 179.1(8) . . . 2_676 ?
O1 C2 C3 C36 3.1(13) . . . 2_676 ?
C2 C3 C4 C5 1.1(13) . . . . ?
C36 C3 C4 C5 -179.7(8) 2_676 . . . ?
C3 C4 C5 C6 -1.3(13) . . . . ?
C3 C4 C5 C8 179.8(10) . . . . ?
C4 C5 C6 C7 2.2(14) . . . . ?
C8 C5 C6 C7 -179.0(10) . . . . ?
C5 C6 C7 C2 -2.9(15) . . . . ?
C5 C6 C7 C12 175.7(8) . . . . ?
C3 C2 C7 C6 2.6(14) . . . . ?
O1 C2 C7 C6 178.6(9) . . . . ?
C3 C2 C7 C12 -175.9(8) . . . . ?
O1 C2 C7 C12 0.0(12) . . . . ?
C4 C5 C8 C11 -96(2) . . . . ?
C6 C5 C8 C11 85(2) . . . . ?
C4 C5 C8 C9 143.7(17) . . . . ?
C6 C5 C8 C9 -35(2) . . . . ?
C4 C5 C8 C10 25.1(18) . . . . ?
C6 C5 C8 C10 -153.7(15) . . . . ?
C6 C7 C12 C15 -97.7(10) . . . . ?
C2 C7 C12 C15 80.9(11) . . . . ?
C13 O2 C14 C15 96.4(10) . . . . ?
C13 O2 C14 C19 -89.5(10) . . . . ?
O2 C14 C15 C16 -177.6(8) . . . . ?
C19 C14 C15 C16 8.4(15) . . . . ?
O2 C14 C15 C12 -0.7(14) . . . . ?
C19 C14 C15 C12 -174.7(9) . . . . ?
C17 C16 C15 C14 -6.5(15) . . . . ?
C17 C16 C15 C12 176.5(9) . . . . ?
C7 C12 C15 C14 85.3(11) . . . . ?
C7 C12 C15 C16 -97.8(12) . . . . ?
C15 C16 C17 C18 2.7(15) . . . . ?
C15 C16 C17 C20 175.3(11) . . . . ?
C16 C17 C18 C19 -0.8(16) . . . . ?
C20 C17 C18 C19 -172.8(12) . . . . ?
C15 C14 C19 C18 -6.3(15) . . . . ?
O2 C14 C19 C18 179.7(9) . . . . ?
C15 C14 C19 C24 174.1(9) . . . . ?
O2 C14 C19 C24 0.2(14) . . . . ?
C17 C18 C19 C14 2.4(16) . . . . ?
C17 C18 C19 C24 -178.0(10) . . . . ?
C18 C17 C20 C21 -160(2) . . . . ?
C16 C17 C20 C21 28(3) . . . . ?
C18 C17 C20 C22 50(2) . . . . ?
C16 C17 C20 C22 -122.7(17) . . . . ?
C18 C17 C20 C23 -45.2(19) . . . . ?
C16 C17 C20 C23 142.5(14) . . . . ?
C14 C19 C24 C37 108.4(10) . . . . ?
C18 C19 C24 C37 -71.1(11) . . . . ?
C14 C19 C24 C27 -122.1(10) . . . . ?
C18 C19 C24 C27 58.4(13) . . . . ?
C25 O3 C26 C27 -107.8(10) . . . . ?
C25 O3 C26 C31 75.3(13) . . . . ?
O3 C26 C27 C28 178.0(7) . . . . ?
C31 C26 C27 C28 -5.0(14) . . . . ?
O3 C26 C27 C24 -0.8(13) . . . . ?
C31 C26 C27 C24 176.2(8) . . . . ?
C19 C24 C27 C26 73.3(11) . . . . ?
C37 C24 C27 C26 -159.8(9) . . . . ?
C19 C24 C27 C28 -105.6(9) . . . . ?
C37 C24 C27 C28 21.3(12) . . . . ?
C26 C27 C28 C29 1.7(13) . . . . ?
C24 C27 C28 C29 -179.4(8) . . . . ?
C27 C28 C29 C30 1.8(14) . . . . ?
C27 C28 C29 C32 -178.9(9) . . . . ?
C28 C29 C30 C31 -2.0(15) . . . . ?
C32 C29 C30 C31 178.6(9) . . . . ?
O3 C26 C31 C30 -178.5(8) . . . . ?
C27 C26 C31 C30 4.7(13) . . . . ?
O3 C26 C31 C36 -0.3(14) . . . . ?
C27 C26 C31 C36 -177.2(8) . . . . ?
C29 C30 C31 C26 -1.2(14) . . . . ?
C29 C30 C31 C36 -179.4(9) . . . . ?
C30 C29 C32 C33 -117.3(12) . . . . ?
C28 C29 C32 C33 63.4(13) . . . . ?
C30 C29 C32 C35 -0.8(17) . . . . ?
C28 C29 C32 C35 179.9(11) . . . . ?
C30 C29 C32 C34 125.0(13) . . . . ?
C28 C29 C32 C34 -54.4(16) . . . . ?
C26 C31 C36 C3 -106.8(10) . . . 2_676 ?
C30 C31 C36 C3 71.3(12) . . . 2_676 ?
C19 C24 C37 C38 -169.0(8) . . . . ?
C27 C24 C37 C38 64.9(11) . . . . ?
C24 C37 C38 C39 -128.4(14) . . . . ?
C40 O4 C41 C42 -77.8(11) . . . . ?
C40 O4 C41 C46 104.0(10) . . . . ?
O4 C41 C42 C43 179.9(7) . . . . ?
C46 C41 C42 C43 -1.9(13) . . . . ?
O4 C41 C42 C71 -0.4(12) . . . 2_566 ?
C46 C41 C42 C71 177.8(8) . . . 2_566 ?
C41 C42 C43 C44 -2.6(13) . . . . ?
C71 C42 C43 C44 177.7(8) 2_566 . . . ?
C42 C43 C44 C45 5.4(14) . . . . ?
C42 C43 C44 C47 -178.6(9) . . . . ?
C43 C44 C45 C46 -4.1(15) . . . . ?
C47 C44 C45 C46 -179.9(10) . . . . ?
C44 C45 C46 C41 -0.2(14) . . . . ?
C44 C45 C46 C51 179.9(9) . . . . ?
C42 C41 C46 C45 3.3(13) . . . . ?
O4 C41 C46 C45 -178.5(7) . . . . ?
C42 C41 C46 C51 -176.9(8) . . . . ?
O4 C41 C46 C51 1.4(12) . . . . ?
C43 C44 C47 C49 144(3) . . . . ?
C45 C44 C47 C49 -40(3) . . . . ?
C43 C44 C47 C48 29(2) . . . . ?
C45 C44 C47 C48 -155(2) . . . . ?
C43 C44 C47 C50 -101(3) . . . . ?
C45 C44 C47 C50 75(3) . . . . ?
C45 C46 C51 C58 102.1(10) . . . . ?
C41 C46 C51 C58 -77.8(11) . . . . ?
C45 C46 C51 C76 -22.4(12) . . . . ?
C41 C46 C51 C76 157.7(8) . . . . ?
C52 O5 C53 C58 88.7(11) . . . . ?
C52 O5 C53 C54 -96.6(10) . . . . ?
C58 C53 C54 C55 -9.2(15) . . . . ?
O5 C53 C54 C55 176.2(9) . . . . ?
C58 C53 C54 C63 175.7(10) . . . . ?
O5 C53 C54 C63 1.2(15) . . . . ?
C53 C54 C55 C56 7.0(15) . . . . ?
C63 C54 C55 C56 -177.8(10) . . . . ?
C54 C55 C56 C57 -2.4(16) . . . . ?
C54 C55 C56 C59 -178.2(10) . . . . ?
C55 C56 C57 C58 -0.2(16) . . . . ?
C59 C56 C57 C58 175.5(11) . . . . ?
O5 C53 C58 C57 -178.9(8) . . . . ?
C54 C53 C58 C57 6.6(15) . . . . ?
O5 C53 C58 C51 1.4(14) . . . . ?
C54 C53 C58 C51 -173.1(9) . . . . ?
C56 C57 C58 C53 -1.8(16) . . . . ?
C56 C57 C58 C51 177.9(10) . . . . ?
C46 C51 C58 C53 125.2(10) . . . . ?
C76 C51 C58 C53 -108.3(10) . . . . ?
C46 C51 C58 C57 -54.6(13) . . . . ?
C76 C51 C58 C57 72.0(11) . . . . ?
C57 C56 C59 C60 -93(3) . . . . ?
C55 C56 C59 C60 82(3) . . . . ?
C57 C56 C59 C61 137.4(16) . . . . ?
C55 C56 C59 C61 -47(2) . . . . ?
C57 C56 C59 C62 25(2) . . . . ?
C55 C56 C59 C62 -159.6(16) . . . . ?
C53 C54 C63 C66 -84.4(12) . . . . ?
C55 C54 C63 C66 100.6(12) . . . . ?
C64 O6 C65 C70 93.9(11) . . . . ?
C64 O6 C65 C66 -86.6(11) . . . . ?
C70 C65 C66 C67 0.1(14) . . . . ?
O6 C65 C66 C67 -179.4(9) . . . . ?
C70 C65 C66 C63 179.4(9) . . . . ?
O6 C65 C66 C63 -0.1(13) . . . . ?
C54 C63 C66 C67 96.7(10) . . . . ?
C54 C63 C66 C65 -82.7(12) . . . . ?
C65 C66 C67 C68 1.8(16) . . . . ?
C63 C66 C67 C68 -177.5(9) . . . . ?
C66 C67 C68 C69 -2.7(17) . . . . ?
C66 C67 C68 C72 176.9(11) . . . . ?
C67 C68 C69 C70 1.6(15) . . . . ?
C72 C68 C69 C70 -178.1(10) . . . . ?
O6 C65 C70 C69 178.4(8) . . . . ?
C66 C65 C70 C69 -1.1(14) . . . . ?
O6 C65 C70 C71 -1.8(14) . . . . ?
C66 C65 C70 C71 178.7(8) . . . . ?
C68 C69 C70 C65 0.3(14) . . . . ?
C68 C69 C70 C71 -179.5(8) . . . . ?
C65 C70 C71 C42 -178.5(9) . . . 2_566 ?
C69 C70 C71 C42 1.3(14) . . . 2_566 ?
C67 C68 C72 C74 -84(3) . . . . ?
C69 C68 C72 C74 96(3) . . . . ?
C67 C68 C72 C75 35(2) . . . . ?
C69 C68 C72 C75 -145(2) . . . . ?
C67 C68 C72 C73 152.4(16) . . . . ?
C69 C68 C72 C73 -28.0(19) . . . . ?
C46 C51 C76 C77 -66.8(11) . . . . ?
C58 C51 C76 C77 168.0(8) . . . . ?
C51 C76 C77 C78 122.1(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.209
