# Electronic Supplementary Material (ESI) for Organdic and Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
#TrackingRef 'Methylester.cif'

_journal_coden_Cambridge         177

# SUBMISSION DETAILS

_publ_contact_author_name        'Prof. Dr. Edwin Weber'
_publ_contact_author_address     
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
_publ_contact_author_email       Edwin.Weber@chemie.tu-freiberg.de
_publ_contact_author_fax         '49(03731) 393170'
_publ_contact_author_phone       '49(03731) 392386'

_publ_requested_journal          'Organic & Biomolecular Chemistry'

# TITLE AND AUTHOR LIST

_publ_section_title              
; New Laterally Modified Calix[4]arenes - Synthesis,
Conformational Behaviour and Sensor Application
;

loop_
_publ_author_name
_publ_author_address

'Fischer, Conrad'
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
'Gruber, Tobias'
; University of Oxford
Department of Chemistry
Chemistry Research Laboratory
Mansfield Road
Oxford OXI 3TA
United Kingdom
;
'Seichter, Wilhelm'
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
'Weber, Edwin'
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;

# TEXT

_publ_section_abstract           
; Application of derivatization reactions to
5,11,17,23-tetra-tert-butyl-25,26,27,28-tetramethoxy-
calix[4]arene-2-carboxylic acid (1), i.e. esterification,
amidation and reduction yielded a series of seven new
laterally monofunctionalized calixarenes (2-8). All
isolated products have been characterized with respect
to their conformational behaviour both in solution and
solid state. Unexpectedly, the presented X-ray structures
of the methyl ester (2) and propyl ester derivative (4)
differ in the conformation of the calixarene molecule
indicating a distinct influence of the length of the
lateral substituent. Using this mutual interaction
between the chalice conformation and the peripheric
substituent, a calixarene with a laterally attached
dansyl group (7) was prepared and photophysically
investigated, showing selective sensing property
towards Cu2+ ions.
;

data_guish_1_0m
_database_code_depnum_ccdc_archive 'CCDC 806418'
#TrackingRef 'Methylester.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H66 O6'
_chemical_formula_sum            'C50 H66 O6'
_chemical_formula_weight         763.03

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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.6769(2)
_cell_length_b                   12.8446(2)
_cell_length_c                   14.6153(3)
_cell_angle_alpha                91.3430(10)
_cell_angle_beta                 94.0610(10)
_cell_angle_gamma                106.2170(10)
_cell_volume                     2277.05(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      32.81

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1%
_diffrn_reflns_number            55737
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         30.40
_reflns_number_total             13742
_reflns_number_gt                11351
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.5386P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13742
_refine_ls_number_parameters     522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.27328(6) 0.47740(6) 0.20624(5) 0.01697(14) Uani 1 1 d . . .
O2 O 0.43716(5) 0.36061(5) 0.16761(4) 0.01407(13) Uani 1 1 d . . .
O3 O 0.38408(6) 0.18310(6) -0.00769(5) 0.01729(14) Uani 1 1 d . . .
O4 O 0.10762(6) 0.11610(6) 0.19058(5) 0.01821(14) Uani 1 1 d . . .
O5 O 0.71026(7) 0.13409(6) 0.12383(5) 0.02320(16) Uani 1 1 d . . .
O6 O 0.72216(6) 0.26778(6) 0.02524(5) 0.01869(14) Uani 1 1 d . . .
C1 C 0.25913(7) 0.41151(8) 0.28093(6) 0.01415(16) Uani 1 1 d . . .
C2 C 0.15625(7) 0.33697(8) 0.28799(6) 0.01477(17) Uani 1 1 d . . .
C3 C 0.14116(8) 0.27386(8) 0.36446(6) 0.01602(17) Uani 1 1 d . . .
H3 H 0.0705 0.2252 0.3708 0.019 Uiso 1 1 calc R . .
C4 C 0.22624(8) 0.27934(8) 0.43248(6) 0.01533(17) Uani 1 1 d . . .
C5 C 0.32949(8) 0.34982(8) 0.41977(6) 0.01519(17) Uani 1 1 d . . .
H5 H 0.3895 0.3526 0.4634 0.018 Uiso 1 1 calc R . .
C6 C 0.34748(7) 0.41650(7) 0.34486(6) 0.01401(16) Uani 1 1 d . . .
C7 C 0.46196(7) 0.48986(8) 0.33314(6) 0.01506(17) Uani 1 1 d . . .
H7A H 0.4901 0.5345 0.3905 0.018 Uiso 1 1 calc R . .
H7B H 0.4572 0.5397 0.2834 0.018 Uiso 1 1 calc R . .
C8 C 0.52870(7) 0.36786(7) 0.22697(6) 0.01203(15) Uani 1 1 d . . .
C9 C 0.54266(7) 0.42712(7) 0.31042(6) 0.01295(16) Uani 1 1 d . . .
C10 C 0.63037(7) 0.42500(7) 0.37340(6) 0.01405(16) Uani 1 1 d . . .
H10 H 0.6399 0.4649 0.4304 0.017 Uiso 1 1 calc R . .
C11 C 0.70422(7) 0.36598(7) 0.35495(6) 0.01336(16) Uani 1 1 d . . .
C12 C 0.68850(7) 0.30866(7) 0.27006(6) 0.01383(16) Uani 1 1 d . . .
H12 H 0.7389 0.2693 0.2556 0.017 Uiso 1 1 calc R . .
C13 C 0.60135(7) 0.30762(7) 0.20626(6) 0.01260(16) Uani 1 1 d . . .
C14 C 0.57438(7) 0.23559(7) 0.11827(6) 0.01339(16) Uani 1 1 d . . .
H14 H 0.5527 0.2790 0.0681 0.016 Uiso 1 1 calc R . .
C15 C 0.38196(8) 0.12070(7) 0.06859(6) 0.01410(16) Uani 1 1 d . . .
C16 C 0.47568(7) 0.13902(7) 0.12995(6) 0.01364(16) Uani 1 1 d . . .
C17 C 0.47171(8) 0.07612(8) 0.20638(6) 0.01519(17) Uani 1 1 d . . .
H17 H 0.5361 0.0868 0.2470 0.018 Uiso 1 1 calc R . .
C18 C 0.37545(8) -0.00245(7) 0.22506(6) 0.01531(17) Uani 1 1 d . . .
C19 C 0.28205(8) -0.01443(7) 0.16489(7) 0.01563(17) Uani 1 1 d . . .
H19 H 0.2151 -0.0656 0.1776 0.019 Uiso 1 1 calc R . .
C20 C 0.28336(8) 0.04600(7) 0.08682(6) 0.01455(16) Uani 1 1 d . . .
C21 C 0.17836(8) 0.03689(7) 0.02685(7) 0.01624(17) Uani 1 1 d . . .
H21A H 0.1185 -0.0237 0.0469 0.019 Uiso 1 1 calc R . .
H21B H 0.1898 0.0202 -0.0376 0.019 Uiso 1 1 calc R . .
C22 C 0.11355(7) 0.17825(7) 0.11371(6) 0.01433(16) Uani 1 1 d . . .
C23 C 0.14434(7) 0.14090(7) 0.03182(6) 0.01387(16) Uani 1 1 d . . .
C24 C 0.14920(7) 0.20489(7) -0.04416(6) 0.01402(16) Uani 1 1 d . . .
H24 H 0.1681 0.1791 -0.1004 0.017 Uiso 1 1 calc R . .
C25 C 0.12730(7) 0.30579(7) -0.04076(6) 0.01328(16) Uani 1 1 d . . .
C26 C 0.10252(7) 0.34222(7) 0.04345(6) 0.01405(16) Uani 1 1 d . . .
H26 H 0.0907 0.4119 0.0483 0.017 Uiso 1 1 calc R . .
C27 C 0.09439(7) 0.27966(8) 0.12106(6) 0.01382(16) Uani 1 1 d . . .
C28 C 0.06569(8) 0.32197(8) 0.21111(6) 0.01625(17) Uani 1 1 d . . .
H28A H 0.0502 0.3925 0.2014 0.019 Uiso 1 1 calc R . .
H28B H -0.0023 0.2706 0.2300 0.019 Uiso 1 1 calc R . .
C29 C 0.20300(8) 0.21056(9) 0.51695(7) 0.01970(19) Uani 1 1 d . . .
C30 C 0.14566(12) 0.09140(11) 0.48751(9) 0.0358(3) Uani 1 1 d . . .
H30A H 0.0743 0.0860 0.4543 0.054 Uiso 1 1 calc R . .
H30B H 0.1343 0.0479 0.5420 0.054 Uiso 1 1 calc R . .
H30C H 0.1919 0.0643 0.4474 0.054 Uiso 1 1 calc R . .
C31 C 0.12719(12) 0.25412(14) 0.57490(8) 0.0389(3) Uani 1 1 d . . .
H31A H 0.1643 0.3294 0.5957 0.058 Uiso 1 1 calc R . .
H31B H 0.1098 0.2096 0.6283 0.058 Uiso 1 1 calc R . .
H31C H 0.0589 0.2513 0.5378 0.058 Uiso 1 1 calc R . .
C32 C 0.30794(10) 0.21450(11) 0.57698(8) 0.0295(2) Uani 1 1 d . . .
H32A H 0.3589 0.1898 0.5403 0.044 Uiso 1 1 calc R . .
H32B H 0.2892 0.1671 0.6285 0.044 Uiso 1 1 calc R . .
H32C H 0.3430 0.2891 0.6006 0.044 Uiso 1 1 calc R . .
C33 C 0.25131(10) 0.57851(9) 0.22429(8) 0.0263(2) Uani 1 1 d . . .
H33A H 0.1745 0.5654 0.2386 0.039 Uiso 1 1 calc R . .
H33B H 0.2640 0.6224 0.1701 0.039 Uiso 1 1 calc R . .
H33C H 0.3003 0.6173 0.2766 0.039 Uiso 1 1 calc R . .
C34 C 0.79976(8) 0.36055(8) 0.42338(6) 0.01520(17) Uani 1 1 d . . .
C35 C 0.80193(10) 0.24170(9) 0.43099(8) 0.0246(2) Uani 1 1 d . . .
H35A H 0.7301 0.1974 0.4477 0.037 Uiso 1 1 calc R . .
H35B H 0.8593 0.2377 0.4783 0.037 Uiso 1 1 calc R . .
H35C H 0.8178 0.2144 0.3718 0.037 Uiso 1 1 calc R . .
C36 C 0.90908(8) 0.42680(9) 0.38888(7) 0.02095(19) Uani 1 1 d . . .
H36A H 0.9162 0.3995 0.3271 0.031 Uiso 1 1 calc R . .
H36B H 0.9706 0.4198 0.4305 0.031 Uiso 1 1 calc R . .
H36C H 0.9102 0.5033 0.3870 0.031 Uiso 1 1 calc R . .
C37 C 0.78909(9) 0.40531(9) 0.51940(7) 0.02096(19) Uani 1 1 d . . .
H37A H 0.7930 0.4824 0.5167 0.031 Uiso 1 1 calc R . .
H37B H 0.8492 0.3967 0.5618 0.031 Uiso 1 1 calc R . .
H37C H 0.7183 0.3654 0.5411 0.031 Uiso 1 1 calc R . .
C38 C 0.45338(8) 0.43707(8) 0.09694(7) 0.01888(18) Uani 1 1 d . . .
H38A H 0.4731 0.5109 0.1247 0.028 Uiso 1 1 calc R . .
H38B H 0.3853 0.4242 0.0569 0.028 Uiso 1 1 calc R . .
H38C H 0.5129 0.4286 0.0608 0.028 Uiso 1 1 calc R . .
C39 C 0.37381(9) -0.06552(9) 0.31242(7) 0.0226(2) Uani 1 1 d . . .
C40 C 0.45643(11) -0.13223(13) 0.31020(11) 0.0428(4) Uani 1 1 d . . .
H40A H 0.4350 -0.1853 0.2582 0.064 Uiso 1 1 calc R . .
H40B H 0.4571 -0.1703 0.3675 0.064 Uiso 1 1 calc R . .
H40C H 0.5302 -0.0839 0.3035 0.064 Uiso 1 1 calc R . .
C41 C 0.40572(13) 0.01650(14) 0.39541(9) 0.0447(4) Uani 1 1 d . . .
H41A H 0.3991 -0.0227 0.4524 0.067 Uiso 1 1 calc R . .
H41B H 0.3564 0.0632 0.3937 0.067 Uiso 1 1 calc R . .
H41C H 0.4819 0.0612 0.3929 0.067 Uiso 1 1 calc R . .
C42 C 0.25978(9) -0.14289(10) 0.32369(8) 0.0274(2) Uani 1 1 d . . .
H42A H 0.2368 -0.1934 0.2700 0.041 Uiso 1 1 calc R . .
H42B H 0.2065 -0.1010 0.3293 0.041 Uiso 1 1 calc R . .
H42C H 0.2630 -0.1838 0.3791 0.041 Uiso 1 1 calc R . .
C43 C 0.42650(10) 0.14216(10) -0.08470(7) 0.0261(2) Uani 1 1 d . . .
H43A H 0.5025 0.1412 -0.0683 0.039 Uiso 1 1 calc R . .
H43B H 0.4251 0.1889 -0.1365 0.039 Uiso 1 1 calc R . .
H43C H 0.3810 0.0683 -0.1021 0.039 Uiso 1 1 calc R . .
C44 C 0.13091(8) 0.37010(8) -0.12786(6) 0.01555(17) Uani 1 1 d . . .
C45 C 0.03523(9) 0.30866(9) -0.19690(7) 0.0219(2) Uani 1 1 d . . .
H45A H 0.0431 0.2366 -0.2119 0.033 Uiso 1 1 calc R . .
H45B H 0.0366 0.3493 -0.2529 0.033 Uiso 1 1 calc R . .
H45C H -0.0349 0.3010 -0.1698 0.033 Uiso 1 1 calc R . .
C46 C 0.24062(9) 0.38263(10) -0.17115(8) 0.0248(2) Uani 1 1 d . . .
H46A H 0.3020 0.4173 -0.1259 0.037 Uiso 1 1 calc R . .
H46B H 0.2435 0.4277 -0.2246 0.037 Uiso 1 1 calc R . .
H46C H 0.2462 0.3109 -0.1905 0.037 Uiso 1 1 calc R . .
C47 C 0.11892(12) 0.48360(9) -0.10858(8) 0.0284(2) Uani 1 1 d . . .
H47A H 0.0481 0.4775 -0.0832 0.043 Uiso 1 1 calc R . .
H47B H 0.1220 0.5221 -0.1659 0.043 Uiso 1 1 calc R . .
H47C H 0.1790 0.5239 -0.0643 0.043 Uiso 1 1 calc R . .
C48 C 0.00189(10) 0.04169(10) 0.19746(8) 0.0286(2) Uani 1 1 d . . .
H48A H -0.0542 0.0811 0.1952 0.043 Uiso 1 1 calc R . .
H48B H 0.0014 0.0053 0.2557 0.043 Uiso 1 1 calc R . .
H48C H -0.0143 -0.0125 0.1463 0.043 Uiso 1 1 calc R . .
C49 C 0.67473(8) 0.20384(8) 0.09098(6) 0.01524(17) Uani 1 1 d . . .
C50 C 0.82468(9) 0.25239(9) -0.00078(8) 0.0247(2) Uani 1 1 d . . .
H50A H 0.8719 0.2492 0.0545 0.037 Uiso 1 1 calc R . .
H50B H 0.8621 0.3131 -0.0369 0.037 Uiso 1 1 calc R . .
H50C H 0.8097 0.1844 -0.0376 0.037 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0185(3) 0.0192(3) 0.0142(3) 0.0021(2) 0.0014(2) 0.0069(3)
O2 0.0118(3) 0.0170(3) 0.0126(3) 0.0014(2) -0.0017(2) 0.0034(2)
O3 0.0207(3) 0.0174(3) 0.0131(3) 0.0029(2) -0.0015(2) 0.0047(3)
O4 0.0190(3) 0.0186(3) 0.0141(3) 0.0042(2) -0.0026(2) 0.0012(3)
O5 0.0251(4) 0.0247(4) 0.0247(4) 0.0035(3) 0.0049(3) 0.0142(3)
O6 0.0147(3) 0.0198(3) 0.0223(3) 0.0017(3) 0.0060(3) 0.0049(3)
C1 0.0144(4) 0.0176(4) 0.0115(4) -0.0007(3) 0.0013(3) 0.0063(3)
C2 0.0118(4) 0.0210(4) 0.0123(4) -0.0019(3) 0.0002(3) 0.0064(3)
C3 0.0129(4) 0.0214(4) 0.0135(4) -0.0006(3) 0.0009(3) 0.0045(3)
C4 0.0153(4) 0.0199(4) 0.0118(4) -0.0005(3) 0.0012(3) 0.0066(3)
C5 0.0134(4) 0.0196(4) 0.0131(4) -0.0022(3) -0.0013(3) 0.0063(3)
C6 0.0120(4) 0.0170(4) 0.0133(4) -0.0030(3) 0.0007(3) 0.0050(3)
C7 0.0129(4) 0.0157(4) 0.0164(4) -0.0030(3) 0.0004(3) 0.0042(3)
C8 0.0098(4) 0.0128(4) 0.0124(4) 0.0010(3) 0.0003(3) 0.0015(3)
C9 0.0109(4) 0.0133(4) 0.0137(4) -0.0003(3) 0.0014(3) 0.0018(3)
C10 0.0126(4) 0.0156(4) 0.0127(4) -0.0013(3) 0.0002(3) 0.0022(3)
C11 0.0109(4) 0.0155(4) 0.0127(4) 0.0010(3) 0.0005(3) 0.0020(3)
C12 0.0121(4) 0.0155(4) 0.0139(4) -0.0001(3) 0.0010(3) 0.0038(3)
C13 0.0124(4) 0.0130(4) 0.0118(4) 0.0000(3) 0.0015(3) 0.0023(3)
C14 0.0136(4) 0.0143(4) 0.0121(4) -0.0007(3) 0.0002(3) 0.0041(3)
C15 0.0172(4) 0.0124(4) 0.0123(4) 0.0001(3) -0.0015(3) 0.0042(3)
C16 0.0136(4) 0.0133(4) 0.0134(4) -0.0012(3) -0.0005(3) 0.0034(3)
C17 0.0145(4) 0.0173(4) 0.0134(4) 0.0001(3) -0.0020(3) 0.0047(3)
C18 0.0166(4) 0.0151(4) 0.0145(4) 0.0020(3) 0.0001(3) 0.0053(3)
C19 0.0157(4) 0.0126(4) 0.0177(4) 0.0003(3) -0.0013(3) 0.0032(3)
C20 0.0160(4) 0.0121(4) 0.0147(4) -0.0014(3) -0.0034(3) 0.0039(3)
C21 0.0167(4) 0.0125(4) 0.0177(4) -0.0011(3) -0.0050(3) 0.0029(3)
C22 0.0122(4) 0.0161(4) 0.0128(4) 0.0016(3) -0.0027(3) 0.0018(3)
C23 0.0125(4) 0.0127(4) 0.0148(4) -0.0005(3) -0.0034(3) 0.0021(3)
C24 0.0136(4) 0.0145(4) 0.0129(4) -0.0014(3) -0.0014(3) 0.0030(3)
C25 0.0115(4) 0.0140(4) 0.0133(4) 0.0007(3) -0.0012(3) 0.0023(3)
C26 0.0121(4) 0.0155(4) 0.0145(4) -0.0003(3) -0.0011(3) 0.0046(3)
C27 0.0101(4) 0.0180(4) 0.0126(4) -0.0008(3) -0.0015(3) 0.0035(3)
C28 0.0119(4) 0.0242(5) 0.0132(4) -0.0003(3) -0.0005(3) 0.0064(3)
C29 0.0187(4) 0.0257(5) 0.0148(4) 0.0041(4) 0.0008(3) 0.0063(4)
C30 0.0370(7) 0.0288(6) 0.0332(6) 0.0092(5) -0.0028(5) -0.0036(5)
C31 0.0439(7) 0.0651(9) 0.0196(5) 0.0141(6) 0.0145(5) 0.0311(7)
C32 0.0257(5) 0.0347(6) 0.0255(5) 0.0120(5) -0.0055(4) 0.0053(4)
C33 0.0332(6) 0.0235(5) 0.0267(5) 0.0045(4) 0.0015(4) 0.0153(4)
C34 0.0133(4) 0.0191(4) 0.0129(4) 0.0001(3) -0.0010(3) 0.0046(3)
C35 0.0292(5) 0.0229(5) 0.0224(5) 0.0025(4) -0.0063(4) 0.0106(4)
C36 0.0125(4) 0.0300(5) 0.0189(4) 0.0002(4) -0.0002(3) 0.0041(4)
C37 0.0187(4) 0.0316(5) 0.0128(4) -0.0007(4) -0.0012(3) 0.0081(4)
C38 0.0207(4) 0.0220(5) 0.0159(4) 0.0051(3) 0.0014(3) 0.0089(4)
C39 0.0185(4) 0.0293(5) 0.0192(5) 0.0107(4) 0.0001(4) 0.0051(4)
C40 0.0275(6) 0.0499(8) 0.0590(9) 0.0389(7) 0.0104(6) 0.0194(6)
C41 0.0451(8) 0.0588(9) 0.0157(5) 0.0038(5) 0.0005(5) -0.0089(7)
C42 0.0219(5) 0.0327(6) 0.0263(5) 0.0145(4) 0.0033(4) 0.0042(4)
C43 0.0338(6) 0.0293(5) 0.0138(4) -0.0003(4) 0.0022(4) 0.0065(4)
C44 0.0178(4) 0.0154(4) 0.0138(4) 0.0025(3) 0.0018(3) 0.0050(3)
C45 0.0200(5) 0.0296(5) 0.0151(4) 0.0037(4) -0.0009(3) 0.0057(4)
C46 0.0188(5) 0.0296(5) 0.0251(5) 0.0094(4) 0.0067(4) 0.0035(4)
C47 0.0489(7) 0.0196(5) 0.0211(5) 0.0059(4) 0.0062(5) 0.0158(5)
C48 0.0275(5) 0.0264(5) 0.0239(5) 0.0072(4) 0.0009(4) -0.0059(4)
C49 0.0149(4) 0.0156(4) 0.0140(4) -0.0037(3) 0.0000(3) 0.0030(3)
C50 0.0167(5) 0.0251(5) 0.0331(6) -0.0011(4) 0.0095(4) 0.0058(4)

_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 1.3879(11) . ?
O1 C33 1.4248(12) . ?
O2 C8 1.3788(10) . ?
O2 C38 1.4278(11) . ?
O3 C15 1.3857(11) . ?
O3 C43 1.4311(13) . ?
O4 C22 1.3876(11) . ?
O4 C48 1.4242(13) . ?
O5 C49 1.2047(12) . ?
O6 C49 1.3423(12) . ?
O6 C50 1.4432(12) . ?
C1 C6 1.3931(12) . ?
C1 C2 1.3980(13) . ?
C2 C3 1.3889(13) . ?
C2 C28 1.5170(12) . ?
C3 C4 1.3996(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.3955(13) . ?
C4 C29 1.5326(13) . ?
C5 C6 1.3980(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.5172(13) . ?
C7 C9 1.5174(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.3961(12) . ?
C8 C13 1.4019(12) . ?
C9 C10 1.3991(12) . ?
C10 C11 1.3952(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.4005(12) . ?
C11 C34 1.5332(12) . ?
C12 C13 1.3912(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.5271(12) . ?
C14 C49 1.5159(13) . ?
C14 C16 1.5188(13) . ?
C14 H14 1.0000 . ?
C15 C20 1.3940(13) . ?
C15 C16 1.3980(12) . ?
C16 C17 1.3894(13) . ?
C17 C18 1.3980(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.3940(13) . ?
C18 C39 1.5263(13) . ?
C19 C20 1.3935(13) . ?
C19 H19 0.9500 . ?
C20 C21 1.5155(12) . ?
C21 C23 1.5157(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.3932(13) . ?
C22 C23 1.3996(13) . ?
C23 C24 1.3917(12) . ?
C24 C25 1.3996(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.3937(12) . ?
C25 C44 1.5301(12) . ?
C26 C27 1.3986(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.5181(13) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C32 1.5288(15) . ?
C29 C31 1.5321(16) . ?
C29 C30 1.5360(17) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
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 C37 1.5332(13) . ?
C34 C36 1.5360(14) . ?
C34 C35 1.5410(14) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.5289(17) . ?
C39 C42 1.5308(15) . ?
C39 C41 1.5419(18) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C47 1.5292(14) . ?
C44 C46 1.5379(14) . ?
C44 C45 1.5385(14) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 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
C1 O1 C33 112.76(8) . . ?
C8 O2 C38 115.10(7) . . ?
C15 O3 C43 113.27(8) . . ?
C22 O4 C48 113.63(8) . . ?
C49 O6 C50 115.27(8) . . ?
O1 C1 C6 120.28(8) . . ?
O1 C1 C2 118.62(8) . . ?
C6 C1 C2 121.03(8) . . ?
C3 C2 C1 118.49(8) . . ?
C3 C2 C28 121.18(8) . . ?
C1 C2 C28 120.25(8) . . ?
C2 C3 C4 122.37(9) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C5 C4 C3 117.23(9) . . ?
C5 C4 C29 123.02(8) . . ?
C3 C4 C29 119.74(8) . . ?
C4 C5 C6 122.14(8) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 118.52(8) . . ?
C1 C6 C7 121.43(8) . . ?
C5 C6 C7 120.03(8) . . ?
C6 C7 C9 112.75(7) . . ?
C6 C7 H7A 109.0 . . ?
C9 C7 H7A 109.0 . . ?
C6 C7 H7B 109.0 . . ?
C9 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
O2 C8 C9 119.71(8) . . ?
O2 C8 C13 119.29(8) . . ?
C9 C8 C13 120.76(8) . . ?
C8 C9 C10 118.79(8) . . ?
C8 C9 C7 120.34(8) . . ?
C10 C9 C7 120.85(8) . . ?
C11 C10 C9 121.93(8) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 117.70(8) . . ?
C10 C11 C34 123.03(8) . . ?
C12 C11 C34 119.27(8) . . ?
C13 C12 C11 121.99(8) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C8 118.82(8) . . ?
C12 C13 C14 123.06(8) . . ?
C8 C13 C14 117.87(8) . . ?
C49 C14 C16 113.46(7) . . ?
C49 C14 C13 111.02(7) . . ?
C16 C14 C13 109.41(7) . . ?
C49 C14 H14 107.6 . . ?
C16 C14 H14 107.6 . . ?
C13 C14 H14 107.6 . . ?
O3 C15 C20 119.19(8) . . ?
O3 C15 C16 119.90(8) . . ?
C20 C15 C16 120.73(8) . . ?
C17 C16 C15 119.05(8) . . ?
C17 C16 C14 121.15(8) . . ?
C15 C16 C14 119.37(8) . . ?
C16 C17 C18 121.72(8) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C19 C18 C17 117.54(8) . . ?
C19 C18 C39 122.67(8) . . ?
C17 C18 C39 119.65(8) . . ?
C20 C19 C18 122.33(9) . . ?
C20 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C19 C20 C15 118.47(8) . . ?
C19 C20 C21 120.84(8) . . ?
C15 C20 C21 120.54(8) . . ?
C20 C21 C23 111.56(7) . . ?
C20 C21 H21A 109.3 . . ?
C23 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C23 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
O4 C22 C27 119.10(8) . . ?
O4 C22 C23 119.67(8) . . ?
C27 C22 C23 121.15(8) . . ?
C24 C23 C22 118.31(8) . . ?
C24 C23 C21 120.35(8) . . ?
C22 C23 C21 121.23(8) . . ?
C23 C24 C25 122.46(8) . . ?
C23 C24 H24 118.8 . . ?
C25 C24 H24 118.8 . . ?
C26 C25 C24 117.22(8) . . ?
C26 C25 C44 123.28(8) . . ?
C24 C25 C44 119.50(8) . . ?
C25 C26 C27 122.26(8) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C22 C27 C26 118.48(8) . . ?
C22 C27 C28 121.04(8) . . ?
C26 C27 C28 120.48(8) . . ?
C2 C28 C27 113.35(7) . . ?
C2 C28 H28A 108.9 . . ?
C27 C28 H28A 108.9 . . ?
C2 C28 H28B 108.9 . . ?
C27 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
C32 C29 C31 108.27(10) . . ?
C32 C29 C4 112.53(9) . . ?
C31 C29 C4 108.53(9) . . ?
C32 C29 C30 107.99(10) . . ?
C31 C29 C30 109.07(11) . . ?
C4 C29 C30 110.38(9) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 C33 H33A 109.5 . . ?
O1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C11 C34 C37 111.99(8) . . ?
C11 C34 C36 109.30(8) . . ?
C37 C34 C36 108.83(8) . . ?
C11 C34 C35 109.60(8) . . ?
C37 C34 C35 108.26(8) . . ?
C36 C34 C35 108.81(8) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 H38A 109.5 . . ?
O2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C18 C39 C40 109.87(9) . . ?
C18 C39 C42 112.03(8) . . ?
C40 C39 C42 108.33(10) . . ?
C18 C39 C41 108.36(10) . . ?
C40 C39 C41 109.67(12) . . ?
C42 C39 C41 108.55(10) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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 . . ?
C47 C44 C25 112.05(8) . . ?
C47 C44 C46 108.04(9) . . ?
C25 C44 C46 110.49(8) . . ?
C47 C44 C45 108.26(9) . . ?
C25 C44 C45 108.76(8) . . ?
C46 C44 C45 109.18(8) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O4 C48 H48A 109.5 . . ?
O4 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O4 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O5 C49 O6 123.75(9) . . ?
O5 C49 C14 126.34(9) . . ?
O6 C49 C14 109.88(8) . . ?
O6 C50 H50A 109.5 . . ?
O6 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
O6 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 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
C33 O1 C1 C6 -90.99(10) . . . . ?
C33 O1 C1 C2 92.00(10) . . . . ?
O1 C1 C2 C3 -177.73(8) . . . . ?
C6 C1 C2 C3 5.29(13) . . . . ?
O1 C1 C2 C28 5.37(13) . . . . ?
C6 C1 C2 C28 -171.61(8) . . . . ?
C1 C2 C3 C4 -2.56(14) . . . . ?
C28 C2 C3 C4 174.31(9) . . . . ?
C2 C3 C4 C5 -1.46(14) . . . . ?
C2 C3 C4 C29 177.73(9) . . . . ?
C3 C4 C5 C6 2.93(13) . . . . ?
C29 C4 C5 C6 -176.23(9) . . . . ?
O1 C1 C6 C5 179.18(8) . . . . ?
C2 C1 C6 C5 -3.89(13) . . . . ?
O1 C1 C6 C7 -2.53(13) . . . . ?
C2 C1 C6 C7 174.40(8) . . . . ?
C4 C5 C6 C1 -0.32(13) . . . . ?
C4 C5 C6 C7 -178.64(8) . . . . ?
C1 C6 C7 C9 -109.98(10) . . . . ?
C5 C6 C7 C9 68.29(11) . . . . ?
C38 O2 C8 C9 95.99(10) . . . . ?
C38 O2 C8 C13 -89.66(10) . . . . ?
O2 C8 C9 C10 173.99(8) . . . . ?
C13 C8 C9 C10 -0.27(13) . . . . ?
O2 C8 C9 C7 -4.25(13) . . . . ?
C13 C8 C9 C7 -178.51(8) . . . . ?
C6 C7 C9 C8 66.33(11) . . . . ?
C6 C7 C9 C10 -111.87(9) . . . . ?
C8 C9 C10 C11 0.32(13) . . . . ?
C7 C9 C10 C11 178.56(8) . . . . ?
C9 C10 C11 C12 0.49(13) . . . . ?
C9 C10 C11 C34 -178.86(8) . . . . ?
C10 C11 C12 C13 -1.41(13) . . . . ?
C34 C11 C12 C13 177.96(8) . . . . ?
C11 C12 C13 C8 1.47(13) . . . . ?
C11 C12 C13 C14 -172.65(8) . . . . ?
O2 C8 C13 C12 -174.89(8) . . . . ?
C9 C8 C13 C12 -0.60(13) . . . . ?
O2 C8 C13 C14 -0.46(12) . . . . ?
C9 C8 C13 C14 173.83(8) . . . . ?
C12 C13 C14 C49 -23.07(12) . . . . ?
C8 C13 C14 C49 162.75(8) . . . . ?
C12 C13 C14 C16 102.91(10) . . . . ?
C8 C13 C14 C16 -71.28(10) . . . . ?
C43 O3 C15 C20 -99.15(10) . . . . ?
C43 O3 C15 C16 85.80(11) . . . . ?
O3 C15 C16 C17 179.56(8) . . . . ?
C20 C15 C16 C17 4.59(13) . . . . ?
O3 C15 C16 C14 7.02(13) . . . . ?
C20 C15 C16 C14 -167.95(8) . . . . ?
C49 C14 C16 C17 74.72(11) . . . . ?
C13 C14 C16 C17 -49.85(11) . . . . ?
C49 C14 C16 C15 -112.90(9) . . . . ?
C13 C14 C16 C15 122.53(9) . . . . ?
C15 C16 C17 C18 -2.14(14) . . . . ?
C14 C16 C17 C18 170.26(8) . . . . ?
C16 C17 C18 C19 -1.17(14) . . . . ?
C16 C17 C18 C39 -177.01(9) . . . . ?
C17 C18 C19 C20 2.18(14) . . . . ?
C39 C18 C19 C20 177.87(9) . . . . ?
C18 C19 C20 C15 0.18(14) . . . . ?
C18 C19 C20 C21 -175.39(8) . . . . ?
O3 C15 C20 C19 -178.63(8) . . . . ?
C16 C15 C20 C19 -3.62(13) . . . . ?
O3 C15 C20 C21 -3.04(13) . . . . ?
C16 C15 C20 C21 171.96(8) . . . . ?
C19 C20 C21 C23 112.14(10) . . . . ?
C15 C20 C21 C23 -63.34(11) . . . . ?
C48 O4 C22 C27 93.18(11) . . . . ?
C48 O4 C22 C23 -90.26(11) . . . . ?
O4 C22 C23 C24 179.80(8) . . . . ?
C27 C22 C23 C24 -3.70(13) . . . . ?
O4 C22 C23 C21 -3.85(13) . . . . ?
C27 C22 C23 C21 172.65(8) . . . . ?
C20 C21 C23 C24 111.64(9) . . . . ?
C20 C21 C23 C22 -64.64(11) . . . . ?
C22 C23 C24 C25 1.70(13) . . . . ?
C21 C23 C24 C25 -174.69(8) . . . . ?
C23 C24 C25 C26 1.53(13) . . . . ?
C23 C24 C25 C44 -178.19(8) . . . . ?
C24 C25 C26 C27 -2.92(13) . . . . ?
C44 C25 C26 C27 176.79(8) . . . . ?
O4 C22 C27 C26 178.91(8) . . . . ?
C23 C22 C27 C26 2.39(13) . . . . ?
O4 C22 C27 C28 -0.90(13) . . . . ?
C23 C22 C27 C28 -177.41(8) . . . . ?
C25 C26 C27 C22 1.02(13) . . . . ?
C25 C26 C27 C28 -179.17(8) . . . . ?
C3 C2 C28 C27 -113.92(10) . . . . ?
C1 C2 C28 C27 62.89(12) . . . . ?
C22 C27 C28 C2 62.49(12) . . . . ?
C26 C27 C28 C2 -117.31(9) . . . . ?
C5 C4 C29 C32 -8.89(14) . . . . ?
C3 C4 C29 C32 171.97(9) . . . . ?
C5 C4 C29 C31 110.91(11) . . . . ?
C3 C4 C29 C31 -68.23(12) . . . . ?
C5 C4 C29 C30 -129.61(11) . . . . ?
C3 C4 C29 C30 51.25(13) . . . . ?
C10 C11 C34 C37 12.48(13) . . . . ?
C12 C11 C34 C37 -166.86(9) . . . . ?
C10 C11 C34 C36 -108.20(10) . . . . ?
C12 C11 C34 C36 72.47(11) . . . . ?
C10 C11 C34 C35 132.64(10) . . . . ?
C12 C11 C34 C35 -46.69(11) . . . . ?
C19 C18 C39 C40 121.53(11) . . . . ?
C17 C18 C39 C40 -62.86(13) . . . . ?
C19 C18 C39 C42 1.06(14) . . . . ?
C17 C18 C39 C42 176.67(9) . . . . ?
C19 C18 C39 C41 -118.66(11) . . . . ?
C17 C18 C39 C41 56.95(13) . . . . ?
C26 C25 C44 C47 7.29(13) . . . . ?
C24 C25 C44 C47 -173.01(9) . . . . ?
C26 C25 C44 C46 127.83(10) . . . . ?
C24 C25 C44 C46 -52.47(11) . . . . ?
C26 C25 C44 C45 -112.35(10) . . . . ?
C24 C25 C44 C45 67.35(11) . . . . ?
C50 O6 C49 O5 -3.69(14) . . . . ?
C50 O6 C49 C14 174.50(8) . . . . ?
C16 C14 C49 O5 -44.82(13) . . . . ?
C13 C14 C49 O5 78.88(12) . . . . ?
C16 C14 C49 O6 137.06(8) . . . . ?
C13 C14 C49 O6 -99.25(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.40
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.080

# Attachment 'Propylester.cif'

data_guish_22_0m
_database_code_depnum_ccdc_archive 'CCDC 806419'
#TrackingRef 'Propylester.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H70 O6'
_chemical_formula_sum            'C52 H70 O6'
_chemical_formula_weight         791.08

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.5457(2)
_cell_length_b                   24.1928(5)
_cell_length_c                   17.0958(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0980(10)
_cell_angle_gamma                90.00
_cell_volume                     4748.23(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    8876
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.97

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.9344
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1%?
_diffrn_reflns_number            43813
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         27.10
_reflns_number_total             10457
_reflns_number_gt                6925
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kappa APEX 2 (Bruker-AXS)'
_computing_cell_refinement       'SAINT-NT (Sheldrick, 2009)'
_computing_data_reduction        SAINT-NT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia)'
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+3.5282P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10457
_refine_ls_number_parameters     540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1520
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_restrained_S_all      0.941
_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 0.25168(12) 0.11777(6) 0.67390(8) 0.0289(3) Uani 1 1 d . . .
O2 O 0.19837(11) 0.21707(6) 0.56399(8) 0.0260(3) Uani 1 1 d . . .
O3 O 0.29678(11) 0.23884(5) 0.74414(8) 0.0260(3) Uani 1 1 d . . .
O4 O 0.42564(12) 0.14227(6) 0.83209(8) 0.0306(3) Uani 1 1 d . . .
O5 O 0.18982(16) 0.39993(8) 0.59272(13) 0.0603(5) Uani 1 1 d . . .
O6 O 0.00696(14) 0.37795(7) 0.61118(10) 0.0432(4) Uani 1 1 d . . .
C1 C 0.17470(17) 0.07405(8) 0.67440(12) 0.0260(4) Uani 1 1 d . . .
C2 C 0.19088(18) 0.03467(8) 0.73486(12) 0.0286(4) Uani 1 1 d . . .
C3 C 0.11075(19) -0.00800(9) 0.73533(12) 0.0297(4) Uani 1 1 d . . .
H3 H 0.1220 -0.0354 0.7752 0.036 Uiso 1 1 calc R . .
C4 C 0.01364(18) -0.01212(8) 0.67896(12) 0.0285(4) Uani 1 1 d . . .
C5 C -0.00038(18) 0.02868(8) 0.62129(12) 0.0269(4) Uani 1 1 d . . .
H5 H -0.0659 0.0269 0.5828 0.032 Uiso 1 1 calc R . .
C6 C 0.07856(17) 0.07211(8) 0.61818(11) 0.0260(4) Uani 1 1 d . . .
C7 C 0.05765(18) 0.11832(8) 0.55828(11) 0.0270(4) Uani 1 1 d . . .
H7A H -0.0050 0.1071 0.5173 0.032 Uiso 1 1 calc R . .
H7B H 0.1294 0.1243 0.5324 0.032 Uiso 1 1 calc R . .
C8 C 0.09513(16) 0.21837(8) 0.59933(11) 0.0224(4) Uani 1 1 d . . .
C9 C 0.02355(17) 0.17210(8) 0.59554(11) 0.0239(4) Uani 1 1 d . . .
C10 C -0.08134(17) 0.17501(9) 0.62947(11) 0.0262(4) Uani 1 1 d . . .
H10 H -0.1314 0.1437 0.6263 0.031 Uiso 1 1 calc R . .
C11 C -0.11469(16) 0.22222(9) 0.66762(11) 0.0259(4) Uani 1 1 d . . .
C12 C -0.03734(17) 0.26651(8) 0.67393(11) 0.0264(4) Uani 1 1 d . . .
H12 H -0.0568 0.2985 0.7020 0.032 Uiso 1 1 calc R . .
C13 C 0.06751(16) 0.26574(8) 0.64060(11) 0.0231(4) Uani 1 1 d . . .
C14 C 0.15464(17) 0.31303(8) 0.65439(11) 0.0251(4) Uani 1 1 d . . .
H14 H 0.2278 0.3007 0.6331 0.030 Uiso 1 1 calc R . .
C15 C 0.25464(16) 0.28250(8) 0.78460(12) 0.0233(4) Uani 1 1 d . . .
C16 C 0.18463(16) 0.32152(8) 0.74286(11) 0.0233(4) Uani 1 1 d . . .
C17 C 0.13916(17) 0.36489(8) 0.78461(12) 0.0252(4) Uani 1 1 d . . .
H17 H 0.0926 0.3923 0.7566 0.030 Uiso 1 1 calc R . .
C18 C 0.16049(17) 0.36889(8) 0.86613(12) 0.0261(4) Uani 1 1 d . . .
C19 C 0.22955(17) 0.32823(8) 0.90567(12) 0.0264(4) Uani 1 1 d . . .
H19 H 0.2446 0.3303 0.9613 0.032 Uiso 1 1 calc R . .
C20 C 0.27721(16) 0.28469(8) 0.86631(12) 0.0245(4) Uani 1 1 d . . .
C21 C 0.34603(18) 0.23883(8) 0.91018(12) 0.0278(4) Uani 1 1 d . . .
H21A H 0.3619 0.2490 0.9664 0.033 Uiso 1 1 calc R . .
H21B H 0.4217 0.2344 0.8886 0.033 Uiso 1 1 calc R . .
C22 C 0.31960(17) 0.13880(8) 0.86392(11) 0.0259(4) Uani 1 1 d . . .
C23 C 0.28008(17) 0.18446(8) 0.90307(11) 0.0250(4) Uani 1 1 d . . .
C24 C 0.17244(17) 0.18063(8) 0.93321(11) 0.0265(4) Uani 1 1 d . . .
H24 H 0.1446 0.2117 0.9596 0.032 Uiso 1 1 calc R . .
C25 C 0.10457(17) 0.13303(9) 0.92598(11) 0.0269(4) Uani 1 1 d . . .
C26 C 0.14735(18) 0.08878(8) 0.88549(12) 0.0277(4) Uani 1 1 d . . .
H26 H 0.1027 0.0558 0.8797 0.033 Uiso 1 1 calc R . .
C27 C 0.25281(17) 0.09104(8) 0.85330(11) 0.0269(4) Uani 1 1 d . . .
C28 C 0.28674(19) 0.04315(9) 0.80179(13) 0.0322(5) Uani 1 1 d . . .
H28A H 0.3611 0.0517 0.7804 0.039 Uiso 1 1 calc R . .
H28B H 0.2975 0.0090 0.8336 0.039 Uiso 1 1 calc R . .
C29 C -0.0736(2) -0.05921(9) 0.68445(13) 0.0352(5) Uani 1 1 d . . .
C30 C -0.1265(3) -0.05450(14) 0.76317(16) 0.0657(9) Uani 1 1 d . . .
H30A H -0.0645 -0.0580 0.8067 0.099 Uiso 1 1 calc R . .
H30B H -0.1839 -0.0840 0.7667 0.099 Uiso 1 1 calc R . .
H30C H -0.1646 -0.0185 0.7662 0.099 Uiso 1 1 calc R . .
C31 C -0.0121(2) -0.11467(10) 0.67918(18) 0.0530(7) Uani 1 1 d . . .
H31A H 0.0237 -0.1165 0.6298 0.079 Uiso 1 1 calc R . .
H31B H -0.0687 -0.1447 0.6808 0.079 Uiso 1 1 calc R . .
H31C H 0.0484 -0.1184 0.7236 0.079 Uiso 1 1 calc R . .
C32 C -0.1752(2) -0.05654(10) 0.61919(15) 0.0403(5) Uani 1 1 d . . .
H32A H -0.2194 -0.0224 0.6246 0.061 Uiso 1 1 calc R . .
H32B H -0.2264 -0.0885 0.6235 0.061 Uiso 1 1 calc R . .
H32C H -0.1449 -0.0570 0.5678 0.061 Uiso 1 1 calc R . .
C33 C 0.3450(2) 0.10783(10) 0.62713(15) 0.0407(6) Uani 1 1 d . . .
H33A H 0.4060 0.0863 0.6576 0.061 Uiso 1 1 calc R . .
H33B H 0.3773 0.1432 0.6118 0.061 Uiso 1 1 calc R . .
H33C H 0.3157 0.0872 0.5798 0.061 Uiso 1 1 calc R . .
C34 C -0.23376(17) 0.22793(10) 0.69912(12) 0.0316(5) Uani 1 1 d . . .
C35 C -0.2215(2) 0.25162(11) 0.78241(14) 0.0439(6) Uani 1 1 d . . .
H35A H -0.1705 0.2277 0.8172 0.066 Uiso 1 1 calc R . .
H35B H -0.2984 0.2536 0.8016 0.066 Uiso 1 1 calc R . .
H35C H -0.1877 0.2888 0.7819 0.066 Uiso 1 1 calc R . .
C36 C -0.2977(2) 0.17256(11) 0.70049(15) 0.0424(6) Uani 1 1 d . . .
H36A H -0.3147 0.1587 0.6466 0.064 Uiso 1 1 calc R . .
H36B H -0.3707 0.1777 0.7240 0.064 Uiso 1 1 calc R . .
H36C H -0.2485 0.1458 0.7317 0.064 Uiso 1 1 calc R . .
C37 C -0.3072(2) 0.26759(13) 0.64428(16) 0.0565(8) Uani 1 1 d . . .
H37A H -0.2660 0.3028 0.6416 0.085 Uiso 1 1 calc R . .
H37B H -0.3823 0.2739 0.6646 0.085 Uiso 1 1 calc R . .
H37C H -0.3203 0.2514 0.5915 0.085 Uiso 1 1 calc R . .
C38 C 0.1815(2) 0.23133(10) 0.48260(12) 0.0356(5) Uani 1 1 d . . .
H38A H 0.1201 0.2081 0.4558 0.053 Uiso 1 1 calc R . .
H38B H 0.2542 0.2255 0.4590 0.053 Uiso 1 1 calc R . .
H38C H 0.1587 0.2703 0.4771 0.053 Uiso 1 1 calc R . .
C39 C 0.10892(19) 0.41555(9) 0.91263(13) 0.0327(5) Uani 1 1 d . . .
C40 C 0.0364(2) 0.45590(10) 0.85951(15) 0.0421(6) Uani 1 1 d . . .
H40A H 0.0856 0.4731 0.8230 0.063 Uiso 1 1 calc R . .
H40B H 0.0048 0.4846 0.8917 0.063 Uiso 1 1 calc R . .
H40C H -0.0277 0.4360 0.8296 0.063 Uiso 1 1 calc R . .
C41 C 0.0301(2) 0.39009(11) 0.97017(16) 0.0507(7) Uani 1 1 d . . .
H41A H -0.0012 0.4195 1.0013 0.076 Uiso 1 1 calc R . .
H41B H 0.0755 0.3643 1.0054 0.076 Uiso 1 1 calc R . .
H41C H -0.0343 0.3703 0.9405 0.076 Uiso 1 1 calc R . .
C42 C 0.2084(2) 0.44780(11) 0.95879(16) 0.0476(6) Uani 1 1 d . . .
H42A H 0.2588 0.4637 0.9220 0.071 Uiso 1 1 calc R . .
H42B H 0.2540 0.4227 0.9951 0.071 Uiso 1 1 calc R . .
H42C H 0.1758 0.4775 0.9887 0.071 Uiso 1 1 calc R . .
C43 C 0.40857(18) 0.24938(10) 0.71857(14) 0.0360(5) Uani 1 1 d . . .
H43A H 0.4041 0.2821 0.6846 0.054 Uiso 1 1 calc R . .
H43B H 0.4329 0.2174 0.6892 0.054 Uiso 1 1 calc R . .
H43C H 0.4654 0.2559 0.7644 0.054 Uiso 1 1 calc R . .
C44 C -0.01375(18) 0.12820(10) 0.95857(14) 0.0352(5) Uani 1 1 d . . .
C45 C -0.0535(2) 0.18335(12) 0.99068(16) 0.0486(6) Uani 1 1 d . . .
H45A H 0.0009 0.1946 1.0358 0.073 Uiso 1 1 calc R . .
H45B H -0.1316 0.1791 1.0073 0.073 Uiso 1 1 calc R . .
H45C H -0.0551 0.2116 0.9495 0.073 Uiso 1 1 calc R . .
C46 C -0.1063(2) 0.11043(12) 0.89266(19) 0.0558(7) Uani 1 1 d . . .
H46A H -0.1069 0.1364 0.8486 0.084 Uiso 1 1 calc R . .
H46B H -0.1829 0.1103 0.9124 0.084 Uiso 1 1 calc R . .
H46C H -0.0882 0.0732 0.8747 0.084 Uiso 1 1 calc R . .
C47 C -0.0052(2) 0.08595(15) 1.0246(2) 0.0691(10) Uani 1 1 d . . .
H47A H 0.0177 0.0501 1.0045 0.104 Uiso 1 1 calc R . .
H47B H -0.0810 0.0824 1.0451 0.104 Uiso 1 1 calc R . .
H47C H 0.0533 0.0980 1.0669 0.104 Uiso 1 1 calc R . .
C48 C 0.5202(2) 0.12162(12) 0.88358(16) 0.0473(6) Uani 1 1 d . . .
H48A H 0.5254 0.1420 0.9333 0.071 Uiso 1 1 calc R . .
H48B H 0.5928 0.1263 0.8593 0.071 Uiso 1 1 calc R . .
H48C H 0.5077 0.0823 0.8936 0.071 Uiso 1 1 calc R . .
C49 C 0.12082(19) 0.36783(10) 0.61539(13) 0.0350(5) Uani 1 1 d . . .
C50 C -0.0302(2) 0.43352(10) 0.58408(15) 0.0420(6) Uani 1 1 d . . .
H50A H -0.0012 0.4418 0.5329 0.050 Uiso 1 1 calc R . .
H50B H 0.0004 0.4618 0.6228 0.050 Uiso 1 1 calc R . .
C51 C -0.1589(2) 0.43324(11) 0.57598(17) 0.0480(6) Uani 1 1 d . . .
H51A H -0.1863 0.4209 0.6261 0.058 Uiso 1 1 calc R . .
H51B H -0.1880 0.4066 0.5345 0.058 Uiso 1 1 calc R . .
C52 C -0.2081(2) 0.48950(11) 0.5553(2) 0.0620(8) Uani 1 1 d . . .
H52A H -0.1855 0.5152 0.5985 0.093 Uiso 1 1 calc R . .
H52B H -0.2932 0.4873 0.5465 0.093 Uiso 1 1 calc R . .
H52C H -0.1776 0.5027 0.5073 0.093 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0312(7) 0.0242(7) 0.0319(8) -0.0030(6) 0.0064(6) -0.0010(6)
O2 0.0257(7) 0.0311(8) 0.0222(7) -0.0005(6) 0.0078(5) 0.0021(6)
O3 0.0253(7) 0.0235(7) 0.0299(7) -0.0029(6) 0.0059(6) 0.0026(6)
O4 0.0266(7) 0.0335(8) 0.0319(8) 0.0045(6) 0.0030(6) 0.0055(6)
O5 0.0484(11) 0.0502(12) 0.0852(15) 0.0268(10) 0.0201(10) 0.0016(9)
O6 0.0389(9) 0.0371(9) 0.0540(11) 0.0095(8) 0.0066(8) 0.0067(7)
C1 0.0303(10) 0.0217(10) 0.0272(10) -0.0053(8) 0.0083(8) 0.0004(8)
C2 0.0335(11) 0.0245(10) 0.0282(10) -0.0059(8) 0.0054(8) 0.0051(8)
C3 0.0402(12) 0.0236(10) 0.0262(10) 0.0004(8) 0.0073(9) 0.0031(9)
C4 0.0363(11) 0.0235(10) 0.0271(10) -0.0050(8) 0.0100(8) 0.0002(8)
C5 0.0311(10) 0.0260(10) 0.0243(10) -0.0051(8) 0.0065(8) 0.0011(8)
C6 0.0316(10) 0.0245(10) 0.0233(10) -0.0042(8) 0.0095(8) 0.0024(8)
C7 0.0346(11) 0.0260(11) 0.0210(10) -0.0035(8) 0.0056(8) -0.0023(8)
C8 0.0216(9) 0.0276(10) 0.0184(9) 0.0029(7) 0.0039(7) 0.0026(8)
C9 0.0277(10) 0.0269(10) 0.0172(9) 0.0018(7) 0.0019(7) 0.0025(8)
C10 0.0244(9) 0.0321(11) 0.0219(9) 0.0039(8) 0.0020(7) -0.0018(8)
C11 0.0228(9) 0.0340(11) 0.0208(9) 0.0046(8) 0.0026(7) 0.0056(8)
C12 0.0266(10) 0.0289(11) 0.0244(10) 0.0006(8) 0.0052(8) 0.0065(8)
C13 0.0251(9) 0.0241(10) 0.0203(9) 0.0039(7) 0.0031(7) 0.0035(8)
C14 0.0275(10) 0.0237(10) 0.0252(10) -0.0002(8) 0.0073(8) 0.0017(8)
C15 0.0196(9) 0.0205(10) 0.0304(10) -0.0027(8) 0.0058(7) -0.0029(7)
C16 0.0215(9) 0.0228(10) 0.0264(10) -0.0001(8) 0.0066(7) -0.0019(7)
C17 0.0253(10) 0.0221(10) 0.0289(10) 0.0017(8) 0.0056(8) 0.0019(8)
C18 0.0259(10) 0.0240(10) 0.0296(10) -0.0026(8) 0.0089(8) -0.0036(8)
C19 0.0300(10) 0.0255(10) 0.0241(10) -0.0024(8) 0.0054(8) -0.0053(8)
C20 0.0211(9) 0.0220(10) 0.0299(10) 0.0009(8) 0.0011(8) -0.0039(7)
C21 0.0291(10) 0.0251(11) 0.0279(10) -0.0010(8) -0.0026(8) -0.0011(8)
C22 0.0274(10) 0.0281(11) 0.0216(10) 0.0036(8) -0.0007(8) 0.0026(8)
C23 0.0279(10) 0.0240(10) 0.0218(9) 0.0029(8) -0.0030(8) 0.0007(8)
C24 0.0306(10) 0.0277(10) 0.0202(9) -0.0018(8) -0.0021(8) 0.0030(8)
C25 0.0274(10) 0.0300(11) 0.0222(10) 0.0035(8) -0.0029(8) 0.0008(8)
C26 0.0315(10) 0.0229(10) 0.0276(10) 0.0023(8) -0.0020(8) -0.0017(8)
C27 0.0334(11) 0.0241(10) 0.0221(10) 0.0017(8) -0.0028(8) 0.0046(8)
C28 0.0385(12) 0.0255(11) 0.0315(11) -0.0017(9) -0.0003(9) 0.0084(9)
C29 0.0450(13) 0.0298(12) 0.0322(11) -0.0026(9) 0.0098(10) -0.0078(10)
C30 0.077(2) 0.083(2) 0.0408(15) -0.0031(15) 0.0235(14) -0.0385(18)
C31 0.0619(17) 0.0289(13) 0.0643(18) 0.0041(12) -0.0109(14) -0.0060(12)
C32 0.0396(12) 0.0347(13) 0.0473(14) -0.0049(11) 0.0075(10) -0.0091(10)
C33 0.0327(11) 0.0368(13) 0.0550(15) -0.0035(11) 0.0151(11) -0.0012(10)
C34 0.0250(10) 0.0425(13) 0.0284(11) 0.0078(9) 0.0080(8) 0.0077(9)
C35 0.0434(13) 0.0564(16) 0.0347(13) -0.0013(11) 0.0175(10) 0.0032(12)
C36 0.0297(11) 0.0555(15) 0.0437(14) 0.0020(12) 0.0119(10) -0.0027(11)
C37 0.0315(12) 0.088(2) 0.0527(16) 0.0350(15) 0.0158(11) 0.0226(13)
C38 0.0411(12) 0.0412(13) 0.0261(11) 0.0059(9) 0.0111(9) -0.0047(10)
C39 0.0384(12) 0.0292(11) 0.0326(11) -0.0037(9) 0.0137(9) 0.0022(9)
C40 0.0517(14) 0.0325(13) 0.0440(14) -0.0061(10) 0.0134(11) 0.0116(11)
C41 0.0582(16) 0.0485(15) 0.0509(16) 0.0000(12) 0.0317(13) 0.0058(13)
C42 0.0537(15) 0.0378(14) 0.0508(15) -0.0175(11) 0.0035(12) 0.0008(11)
C43 0.0274(11) 0.0397(13) 0.0424(13) -0.0060(10) 0.0118(9) 0.0055(9)
C44 0.0267(10) 0.0395(13) 0.0388(12) 0.0046(10) 0.0014(9) 0.0002(9)
C45 0.0309(12) 0.0615(17) 0.0542(16) -0.0125(13) 0.0083(11) 0.0019(11)
C46 0.0315(12) 0.0530(17) 0.080(2) -0.0152(15) -0.0074(13) -0.0021(12)
C47 0.0407(15) 0.091(2) 0.079(2) 0.0471(19) 0.0245(14) 0.0142(15)
C48 0.0325(12) 0.0546(16) 0.0540(16) 0.0132(12) 0.0004(11) 0.0114(11)
C49 0.0348(12) 0.0362(12) 0.0350(12) 0.0006(10) 0.0085(9) 0.0011(10)
C50 0.0500(14) 0.0340(13) 0.0415(13) 0.0038(10) 0.0028(11) 0.0102(11)
C51 0.0473(14) 0.0367(14) 0.0601(17) 0.0055(12) 0.0059(12) 0.0051(11)
C52 0.0342(13) 0.0337(14) 0.116(3) 0.0063(15) -0.0035(15) 0.0015(11)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.382(2) . ?
O1 C33 1.428(3) . ?
O2 C8 1.393(2) . ?
O2 C38 1.427(2) . ?
O3 C15 1.379(2) . ?
O3 C43 1.429(2) . ?
O4 C22 1.394(2) . ?
O4 C48 1.418(3) . ?
O5 C49 1.206(3) . ?
O6 C49 1.332(3) . ?
O6 C50 1.471(3) . ?
C1 C6 1.390(3) . ?
C1 C2 1.404(3) . ?
C2 C3 1.387(3) . ?
C2 C28 1.519(3) . ?
C3 C4 1.402(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(3) . ?
C4 C29 1.531(3) . ?
C5 C6 1.396(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.518(3) . ?
C7 C9 1.519(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.389(3) . ?
C8 C13 1.400(3) . ?
C9 C10 1.399(3) . ?
C10 C11 1.390(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(3) . ?
C11 C34 1.535(3) . ?
C12 C13 1.392(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.525(3) . ?
C14 C49 1.516(3) . ?
C14 C16 1.529(3) . ?
C14 H14 1.0000 . ?
C15 C16 1.390(3) . ?
C15 C20 1.395(3) . ?
C16 C17 1.402(3) . ?
C17 C18 1.393(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(3) . ?
C18 C39 1.537(3) . ?
C19 C20 1.394(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.516(3) . ?
C21 C23 1.518(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.390(3) . ?
C22 C23 1.393(3) . ?
C23 C24 1.398(3) . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(3) . ?
C25 C44 1.534(3) . ?
C26 C27 1.390(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.531(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C31 1.526(3) . ?
C29 C32 1.532(3) . ?
C29 C30 1.540(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
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 C35 1.528(3) . ?
C34 C36 1.531(3) . ?
C34 C37 1.533(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.522(3) . ?
C39 C42 1.535(3) . ?
C39 C41 1.538(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C47 1.519(3) . ?
C44 C46 1.529(3) . ?
C44 C45 1.532(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C50 C51 1.478(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.502(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 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
C1 O1 C33 113.47(15) . . ?
C8 O2 C38 112.54(15) . . ?
C15 O3 C43 113.26(15) . . ?
C22 O4 C48 112.73(16) . . ?
C49 O6 C50 116.00(18) . . ?
O1 C1 C6 119.23(18) . . ?
O1 C1 C2 119.25(18) . . ?
C6 C1 C2 121.37(19) . . ?
C3 C2 C1 118.22(19) . . ?
C3 C2 C28 121.96(19) . . ?
C1 C2 C28 119.50(19) . . ?
C2 C3 C4 122.28(19) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 117.43(19) . . ?
C5 C4 C29 122.91(19) . . ?
C3 C4 C29 119.62(19) . . ?
C4 C5 C6 122.24(19) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 118.41(18) . . ?
C1 C6 C7 120.00(18) . . ?
C5 C6 C7 121.49(18) . . ?
C6 C7 C9 112.18(15) . . ?
C6 C7 H7A 109.2 . . ?
C9 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C9 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 O2 119.60(17) . . ?
C9 C8 C13 121.13(17) . . ?
O2 C8 C13 119.23(16) . . ?
C8 C9 C10 118.50(18) . . ?
C8 C9 C7 122.04(17) . . ?
C10 C9 C7 119.43(18) . . ?
C11 C10 C9 122.08(19) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 117.49(17) . . ?
C10 C11 C34 122.80(19) . . ?
C12 C11 C34 119.66(18) . . ?
C11 C12 C13 122.47(18) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C12 C13 C8 118.15(18) . . ?
C12 C13 C14 120.98(17) . . ?
C8 C13 C14 120.67(16) . . ?
C49 C14 C13 116.94(17) . . ?
C49 C14 C16 109.76(16) . . ?
C13 C14 C16 109.27(15) . . ?
C49 C14 H14 106.8 . . ?
C13 C14 H14 106.8 . . ?
C16 C14 H14 106.8 . . ?
O3 C15 C16 118.67(17) . . ?
O3 C15 C20 119.55(17) . . ?
C16 C15 C20 121.67(18) . . ?
C15 C16 C17 118.42(18) . . ?
C15 C16 C14 118.34(17) . . ?
C17 C16 C14 123.12(17) . . ?
C18 C17 C16 121.70(18) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 117.85(18) . . ?
C17 C18 C39 122.12(18) . . ?
C19 C18 C39 120.02(18) . . ?
C20 C19 C18 122.24(18) . . ?
C20 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
C19 C20 C15 118.09(18) . . ?
C19 C20 C21 121.81(18) . . ?
C15 C20 C21 120.01(17) . . ?
C20 C21 C23 111.25(16) . . ?
C20 C21 H21A 109.4 . . ?
C23 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C23 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C27 C22 C23 121.08(18) . . ?
C27 C22 O4 119.81(18) . . ?
C23 C22 O4 119.05(18) . . ?
C22 C23 C24 118.27(18) . . ?
C22 C23 C21 122.57(18) . . ?
C24 C23 C21 119.07(18) . . ?
C25 C24 C23 122.46(19) . . ?
C25 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C24 C25 C26 117.00(18) . . ?
C24 C25 C44 123.09(19) . . ?
C26 C25 C44 119.89(19) . . ?
C27 C26 C25 122.57(19) . . ?
C27 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C26 C27 C22 118.57(18) . . ?
C26 C27 C28 119.11(18) . . ?
C22 C27 C28 122.12(18) . . ?
C2 C28 C27 108.97(16) . . ?
C2 C28 H28A 109.9 . . ?
C27 C28 H28A 109.9 . . ?
C2 C28 H28B 109.9 . . ?
C27 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
C31 C29 C4 109.69(19) . . ?
C31 C29 C32 108.65(19) . . ?
C4 C29 C32 112.46(18) . . ?
C31 C29 C30 110.3(2) . . ?
C4 C29 C30 108.85(19) . . ?
C32 C29 C30 106.8(2) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 C33 H33A 109.5 . . ?
O1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C36 108.13(18) . . ?
C35 C34 C37 109.0(2) . . ?
C36 C34 C37 108.7(2) . . ?
C35 C34 C11 111.29(18) . . ?
C36 C34 C11 112.21(18) . . ?
C37 C34 C11 107.44(17) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 H38A 109.5 . . ?
O2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C42 108.3(2) . . ?
C40 C39 C18 112.40(18) . . ?
C42 C39 C18 109.23(18) . . ?
C40 C39 C41 108.3(2) . . ?
C42 C39 C41 109.6(2) . . ?
C18 C39 C41 108.96(18) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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 . . ?
C47 C44 C46 110.1(2) . . ?
C47 C44 C45 108.5(2) . . ?
C46 C44 C45 107.25(19) . . ?
C47 C44 C25 109.34(18) . . ?
C46 C44 C25 109.5(2) . . ?
C45 C44 C25 112.09(19) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O4 C48 H48A 109.5 . . ?
O4 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O4 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O5 C49 O6 123.1(2) . . ?
O5 C49 C14 123.8(2) . . ?
O6 C49 C14 113.03(18) . . ?
O6 C50 C51 106.4(2) . . ?
O6 C50 H50A 110.5 . . ?
C51 C50 H50A 110.5 . . ?
O6 C50 H50B 110.5 . . ?
C51 C50 H50B 110.5 . . ?
H50A C50 H50B 108.6 . . ?
C50 C51 C52 111.6(2) . . ?
C50 C51 H51A 109.3 . . ?
C52 C51 H51A 109.3 . . ?
C50 C51 H51B 109.3 . . ?
C52 C51 H51B 109.3 . . ?
H51A C51 H51B 108.0 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 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
C33 O1 C1 C6 -90.5(2) . . . . ?
C33 O1 C1 C2 93.9(2) . . . . ?
O1 C1 C2 C3 178.28(17) . . . . ?
C6 C1 C2 C3 2.8(3) . . . . ?
O1 C1 C2 C28 4.7(3) . . . . ?
C6 C1 C2 C28 -170.86(18) . . . . ?
C1 C2 C3 C4 -1.6(3) . . . . ?
C28 C2 C3 C4 171.86(19) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C2 C3 C4 C29 -177.99(18) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C29 C4 C5 C6 178.43(18) . . . . ?
O1 C1 C6 C5 -177.80(16) . . . . ?
C2 C1 C6 C5 -2.3(3) . . . . ?
O1 C1 C6 C7 -1.3(3) . . . . ?
C2 C1 C6 C7 174.20(17) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C4 C5 C6 C7 -175.82(18) . . . . ?
C1 C6 C7 C9 -69.3(2) . . . . ?
C5 C6 C7 C9 107.1(2) . . . . ?
C38 O2 C8 C9 85.8(2) . . . . ?
C38 O2 C8 C13 -96.5(2) . . . . ?
O2 C8 C9 C10 -178.12(16) . . . . ?
C13 C8 C9 C10 4.3(3) . . . . ?
O2 C8 C9 C7 3.9(3) . . . . ?
C13 C8 C9 C7 -173.70(17) . . . . ?
C6 C7 C9 C8 113.3(2) . . . . ?
C6 C7 C9 C10 -64.6(2) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C7 C9 C10 C11 176.97(18) . . . . ?
C9 C10 C11 C12 -2.5(3) . . . . ?
C9 C10 C11 C34 174.76(18) . . . . ?
C10 C11 C12 C13 3.1(3) . . . . ?
C34 C11 C12 C13 -174.31(18) . . . . ?
C11 C12 C13 C8 0.0(3) . . . . ?
C11 C12 C13 C14 -174.92(18) . . . . ?
C9 C8 C13 C12 -3.8(3) . . . . ?
O2 C8 C13 C12 178.61(16) . . . . ?
C9 C8 C13 C14 171.18(17) . . . . ?
O2 C8 C13 C14 -6.4(3) . . . . ?
C12 C13 C14 C49 -70.2(2) . . . . ?
C8 C13 C14 C49 115.0(2) . . . . ?
C12 C13 C14 C16 55.3(2) . . . . ?
C8 C13 C14 C16 -119.54(19) . . . . ?
C43 O3 C15 C16 91.9(2) . . . . ?
C43 O3 C15 C20 -91.9(2) . . . . ?
O3 C15 C16 C17 178.10(16) . . . . ?
C20 C15 C16 C17 2.0(3) . . . . ?
O3 C15 C16 C14 1.9(2) . . . . ?
C20 C15 C16 C14 -174.18(17) . . . . ?
C49 C14 C16 C15 -157.97(17) . . . . ?
C13 C14 C16 C15 72.6(2) . . . . ?
C49 C14 C16 C17 26.1(3) . . . . ?
C13 C14 C16 C17 -103.4(2) . . . . ?
C15 C16 C17 C18 -1.4(3) . . . . ?
C14 C16 C17 C18 174.60(18) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C16 C17 C18 C39 -178.66(18) . . . . ?
C17 C18 C19 C20 0.3(3) . . . . ?
C39 C18 C19 C20 179.22(18) . . . . ?
C18 C19 C20 C15 0.3(3) . . . . ?
C18 C19 C20 C21 -176.23(18) . . . . ?
O3 C15 C20 C19 -177.55(16) . . . . ?
C16 C15 C20 C19 -1.5(3) . . . . ?
O3 C15 C20 C21 -1.0(3) . . . . ?
C16 C15 C20 C21 175.13(17) . . . . ?
C19 C20 C21 C23 110.8(2) . . . . ?
C15 C20 C21 C23 -65.6(2) . . . . ?
C48 O4 C22 C27 -88.3(2) . . . . ?
C48 O4 C22 C23 94.5(2) . . . . ?
C27 C22 C23 C24 1.5(3) . . . . ?
O4 C22 C23 C24 178.71(17) . . . . ?
C27 C22 C23 C21 -175.05(18) . . . . ?
O4 C22 C23 C21 2.1(3) . . . . ?
C20 C21 C23 C22 114.7(2) . . . . ?
C20 C21 C23 C24 -61.8(2) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C21 C23 C24 C25 177.19(18) . . . . ?
C23 C24 C25 C26 -1.3(3) . . . . ?
C23 C24 C25 C44 -179.89(18) . . . . ?
C24 C25 C26 C27 0.0(3) . . . . ?
C44 C25 C26 C27 178.72(18) . . . . ?
C25 C26 C27 C22 1.9(3) . . . . ?
C25 C26 C27 C28 -173.08(18) . . . . ?
C23 C22 C27 C26 -2.7(3) . . . . ?
O4 C22 C27 C26 -179.83(17) . . . . ?
C23 C22 C27 C28 172.14(18) . . . . ?
O4 C22 C27 C28 -5.0(3) . . . . ?
C3 C2 C28 C27 -102.7(2) . . . . ?
C1 C2 C28 C27 70.7(2) . . . . ?
C26 C27 C28 C2 55.8(2) . . . . ?
C22 C27 C28 C2 -118.9(2) . . . . ?
C5 C4 C29 C31 122.0(2) . . . . ?
C3 C4 C29 C31 -60.2(3) . . . . ?
C5 C4 C29 C32 0.9(3) . . . . ?
C3 C4 C29 C32 178.80(19) . . . . ?
C5 C4 C29 C30 -117.3(2) . . . . ?
C3 C4 C29 C30 60.6(3) . . . . ?
C10 C11 C34 C35 134.2(2) . . . . ?
C12 C11 C34 C35 -48.6(3) . . . . ?
C10 C11 C34 C36 12.9(3) . . . . ?
C12 C11 C34 C36 -169.87(19) . . . . ?
C10 C11 C34 C37 -106.5(2) . . . . ?
C12 C11 C34 C37 70.7(3) . . . . ?
C17 C18 C39 C40 -1.2(3) . . . . ?
C19 C18 C39 C40 179.91(19) . . . . ?
C17 C18 C39 C42 -121.5(2) . . . . ?
C19 C18 C39 C42 59.6(2) . . . . ?
C17 C18 C39 C41 118.8(2) . . . . ?
C19 C18 C39 C41 -60.1(3) . . . . ?
C24 C25 C44 C47 -113.8(3) . . . . ?
C26 C25 C44 C47 67.6(3) . . . . ?
C24 C25 C44 C46 125.5(2) . . . . ?
C26 C25 C44 C46 -53.1(3) . . . . ?
C24 C25 C44 C45 6.6(3) . . . . ?
C26 C25 C44 C45 -171.9(2) . . . . ?
C50 O6 C49 O5 -5.8(3) . . . . ?
C50 O6 C49 C14 171.90(18) . . . . ?
C13 C14 C49 O5 -148.1(2) . . . . ?
C16 C14 C49 O5 86.7(3) . . . . ?
C13 C14 C49 O6 34.2(3) . . . . ?
C16 C14 C49 O6 -91.0(2) . . . . ?
C49 O6 C50 C51 174.1(2) . . . . ?
O6 C50 C51 C52 175.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.054