# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2010


data_global

_journal_coden_Cambridge         177

loop_
_publ_author_name
'Satu-Marjaana Ikonen'
'Raija Juvonen'
'Erkki Kolehmainen'
Nonappa
'Hannu Salo'
'Arto Valkonen'

_publ_contact_author_name        'Satu-Marjaana Ikonen'
_publ_contact_author_email       SATU.IKONEN@JYU.FI

_publ_section_title              
;
Bile acid derived mono- and diketals - synthesis, structural
characterization and self-assembling properties
;

# Attachment 'Ikonen_Crystaldata_7a_7c_10a_I_'

data_7a
_database_code_depnum_ccdc_archive 'CCDC 766948'
#TrackingRef 'Ikonen_Crystaldata_7a_7c_10a_I_'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
'Cyclic 3-ketal of methyl 3-oxo-5\b-cholan-24-oate with benzene-1,2-diol'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H44 O4'
_chemical_formula_weight         480.66
_chemical_absolute_configuration syn

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   P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   7.5708(2)
_cell_length_b                   11.1245(3)
_cell_length_c                   16.1074(5)
_cell_angle_alpha                80.080(2)
_cell_angle_beta                 85.635(2)
_cell_angle_gamma                88.002(2)
_cell_volume                     1332.10(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    11926
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Bruker Kappa APEX-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10657
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         28.27
_reflns_number_total             6565
_reflns_number_gt                4706
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker, 2004)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR-2002 (Burla, et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
'SHELXL-97; MERCURY (Macrae, <i>et al.</i>, 2006)'

_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^)+(0.0095P)^2^+1.5180P] 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         6565
_refine_ls_number_parameters     631
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.1176
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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 0.0534(4) 0.5716(3) 0.0660(2) 0.0238(7) Uani 1 1 d . . .
O2 O 0.0977(5) 0.3614(3) 0.0937(2) 0.0262(8) Uani 1 1 d . . .
O24 O -0.1282(5) -0.1284(3) 0.8723(2) 0.0344(9) Uani 1 1 d . . .
O25 O -0.1598(5) -0.0243(3) 0.9798(2) 0.0374(9) Uani 1 1 d . . .
C1 C 0.1441(6) 0.5900(4) 0.2385(3) 0.0206(10) Uani 1 1 d . . .
H1A H 0.1438 0.6667 0.1969 0.025 Uiso 1 1 calc R . .
H1B H 0.2355 0.5965 0.2782 0.025 Uiso 1 1 calc R . .
C2 C 0.1949(6) 0.4844(4) 0.1919(3) 0.0225(10) Uani 1 1 d . . .
H2A H 0.3096 0.5009 0.1587 0.027 Uiso 1 1 calc R . .
H2B H 0.2091 0.4085 0.2333 0.027 Uiso 1 1 calc R . .
C3 C 0.0540(6) 0.4679(4) 0.1336(3) 0.0221(10) Uani 1 1 d . . .
C4 C -0.1291(6) 0.4546(4) 0.1780(3) 0.0200(9) Uani 1 1 d . . .
H4A H -0.1342 0.3761 0.2178 0.024 Uiso 1 1 calc R . .
H4B H -0.2166 0.4523 0.1357 0.024 Uiso 1 1 calc R . .
C5 C -0.1801(6) 0.5594(4) 0.2270(3) 0.0203(10) Uani 1 1 d . . .
H5 H -0.1865 0.6362 0.1845 0.024 Uiso 1 1 calc R . .
C6 C -0.3666(6) 0.5385(4) 0.2718(3) 0.0226(10) Uani 1 1 d . . .
H6A H -0.4094 0.6137 0.2927 0.027 Uiso 1 1 calc R . .
H6B H -0.4493 0.5215 0.2307 0.027 Uiso 1 1 calc R . .
C7 C -0.3667(6) 0.4325(4) 0.3456(3) 0.0233(10) Uani 1 1 d . . .
H7A H -0.3395 0.3556 0.3236 0.028 Uiso 1 1 calc R . .
H7B H -0.4863 0.4261 0.3752 0.028 Uiso 1 1 calc R . .
C8 C -0.2317(6) 0.4480(4) 0.4084(3) 0.0208(10) Uani 1 1 d . . .
H8 H -0.2672 0.5218 0.4339 0.025 Uiso 1 1 calc R . .
C9 C -0.0437(6) 0.4681(4) 0.3633(3) 0.0201(10) Uani 1 1 d . . .
H9 H -0.0136 0.3935 0.3378 0.024 Uiso 1 1 calc R . .
C10 C -0.0390(6) 0.5774(4) 0.2884(3) 0.0203(10) Uani 1 1 d . . .
C11 C 0.0951(6) 0.4731(4) 0.4269(3) 0.0236(10) Uani 1 1 d . . .
H11A H 0.0753 0.5489 0.4511 0.028 Uiso 1 1 calc R . .
H11B H 0.2142 0.4768 0.3967 0.028 Uiso 1 1 calc R . .
C12 C 0.0908(6) 0.3630(4) 0.4995(3) 0.0238(11) Uani 1 1 d . . .
H12A H 0.1235 0.2877 0.4764 0.029 Uiso 1 1 calc R . .
H12B H 0.1789 0.3738 0.5398 0.029 Uiso 1 1 calc R . .
C13 C -0.0940(6) 0.3496(4) 0.5460(3) 0.0186(10) Uani 1 1 d . . .
C14 C -0.2265(6) 0.3386(4) 0.4792(3) 0.0216(10) Uani 1 1 d . . .
H14 H -0.1836 0.2677 0.4521 0.026 Uiso 1 1 calc R . .
C15 C -0.3992(6) 0.2990(4) 0.5309(3) 0.0223(10) Uani 1 1 d . . .
H15A H -0.4721 0.2521 0.4998 0.027 Uiso 1 1 calc R . .
H15B H -0.4693 0.3704 0.5451 0.027 Uiso 1 1 calc R . .
C16 C -0.3351(6) 0.2178(5) 0.6115(3) 0.0274(11) Uani 1 1 d . . .
H16A H -0.3679 0.1320 0.6133 0.033 Uiso 1 1 calc R . .
H16B H -0.3907 0.2460 0.6626 0.033 Uiso 1 1 calc R . .
C17 C -0.1299(6) 0.2277(4) 0.6086(3) 0.0206(10) Uani 1 1 d . . .
H17 H -0.0772 0.1599 0.5806 0.025 Uiso 1 1 calc R . .
C18 C -0.1379(6) 0.4581(4) 0.5916(3) 0.0226(10) Uani 1 1 d . . .
H18A H -0.2558 0.4482 0.6212 0.034 Uiso 1 1 calc R . .
H18B H -0.1365 0.5339 0.5502 0.034 Uiso 1 1 calc R . .
H18C H -0.0496 0.4618 0.6324 0.034 Uiso 1 1 calc R . .
C19 C -0.0759(6) 0.7000(4) 0.3205(3) 0.0247(10) Uani 1 1 d . . .
H19A H -0.1910 0.6974 0.3529 0.037 Uiso 1 1 calc R . .
H19B H -0.0771 0.7668 0.2722 0.037 Uiso 1 1 calc R . .
H19C H 0.0173 0.7134 0.3568 0.037 Uiso 1 1 calc R . .
C20 C -0.0570(6) 0.2128(4) 0.6966(3) 0.0224(10) Uani 1 1 d . . .
H20 H -0.1075 0.2814 0.7243 0.027 Uiso 1 1 calc R . .
C21 C 0.1452(7) 0.2218(5) 0.6907(3) 0.0289(11) Uani 1 1 d . . .
H21A H 0.1801 0.2995 0.6557 0.043 Uiso 1 1 calc R . .
H21B H 0.1988 0.1541 0.6652 0.043 Uiso 1 1 calc R . .
H21C H 0.1859 0.2175 0.7475 0.043 Uiso 1 1 calc R . .
C22 C -0.1189(6) 0.0927(4) 0.7519(3) 0.0253(11) Uani 1 1 d . . .
H22A H -0.2461 0.0827 0.7452 0.030 Uiso 1 1 calc R . .
H22B H -0.0525 0.0236 0.7320 0.030 Uiso 1 1 calc R . .
C23 C -0.0920(7) 0.0882(4) 0.8453(3) 0.0292(11) Uani 1 1 d . . .
H23A H 0.0319 0.1093 0.8511 0.035 Uiso 1 1 calc R . .
H23B H -0.1705 0.1507 0.8669 0.035 Uiso 1 1 calc R . .
C24 C -0.1296(7) -0.0338(5) 0.8983(3) 0.0275(11) Uani 1 1 d . . .
C25 C -0.1875(8) -0.1397(5) 1.0379(4) 0.0431(15) Uani 1 1 d . . .
H25A H -0.2077 -0.1237 1.0958 0.065 Uiso 1 1 calc R . .
H25B H -0.0825 -0.1930 1.0338 0.065 Uiso 1 1 calc R . .
H25C H -0.2910 -0.1798 1.0229 0.065 Uiso 1 1 calc R . .
C26 C 0.0442(6) 0.5249(4) -0.0080(3) 0.0222(10) Uani 1 1 d . . .
C27 C 0.0722(6) 0.3997(4) 0.0090(3) 0.0238(10) Uani 1 1 d . . .
C28 C 0.0751(7) 0.3290(5) -0.0531(3) 0.0286(11) Uani 1 1 d . . .
H28 H 0.0958 0.2432 -0.0417 0.034 Uiso 1 1 calc R . .
C29 C 0.0456(7) 0.3911(5) -0.1341(3) 0.0358(13) Uani 1 1 d . . .
H29 H 0.0453 0.3462 -0.1791 0.043 Uiso 1 1 calc R . .
C30 C 0.0170(7) 0.5161(5) -0.1505(3) 0.0347(13) Uani 1 1 d . . .
H30 H -0.0015 0.5547 -0.2066 0.042 Uiso 1 1 calc R . .
C31 C 0.0145(7) 0.5870(5) -0.0870(3) 0.0278(11) Uani 1 1 d . . .
H31 H -0.0064 0.6728 -0.0978 0.033 Uiso 1 1 calc R . .
O1A O 0.4203(4) -0.2308(3) 0.8453(2) 0.0270(8) Uani 1 1 d . . .
O2A O 0.4612(5) -0.0229(3) 0.7990(2) 0.0259(7) Uani 1 1 d . . .
O24A O 0.5261(5) 0.4534(3) 0.0395(2) 0.0335(9) Uani 1 1 d . . .
O25A O 0.5671(5) 0.3487(3) -0.0679(2) 0.0353(9) Uani 1 1 d . . .
C1A C 0.5684(6) -0.2772(4) 0.6743(3) 0.0201(10) Uani 1 1 d . . .
H1C H 0.5491 -0.3500 0.7186 0.024 Uiso 1 1 calc R . .
H1D H 0.6760 -0.2934 0.6386 0.024 Uiso 1 1 calc R . .
C2A C 0.6013(6) -0.1678(4) 0.7167(3) 0.0219(10) Uani 1 1 d . . .
H2C H 0.7014 -0.1872 0.7533 0.026 Uiso 1 1 calc R . .
H2D H 0.6335 -0.0965 0.6731 0.026 Uiso 1 1 calc R . .
C3A C 0.4385(7) -0.1374(4) 0.7689(3) 0.0248(11) Uani 1 1 d . . .
C4A C 0.2702(6) -0.1277(4) 0.7236(3) 0.0226(10) Uani 1 1 d . . .
H4C H 0.2707 -0.0504 0.6826 0.027 Uiso 1 1 calc R . .
H4D H 0.1684 -0.1233 0.7654 0.027 Uiso 1 1 calc R . .
C5A C 0.2421(6) -0.2330(4) 0.6765(3) 0.0210(10) Uani 1 1 d . . .
H5A H 0.2202 -0.3078 0.7199 0.025 Uiso 1 1 calc R . .
C6A C 0.0763(6) -0.2079(4) 0.6263(3) 0.0245(10) Uani 1 1 d . . .
H6C H -0.0244 -0.1860 0.6641 0.029 Uiso 1 1 calc R . .
H6D H 0.0459 -0.2832 0.6061 0.029 Uiso 1 1 calc R . .
C7A C 0.1032(6) -0.1042(4) 0.5501(3) 0.0237(10) Uani 1 1 d . . .
H7C H -0.0032 -0.0959 0.5173 0.028 Uiso 1 1 calc R . .
H7D H 0.1168 -0.0264 0.5707 0.028 Uiso 1 1 calc R . .
C8A C 0.2660(6) -0.1272(4) 0.4923(3) 0.0189(9) Uani 1 1 d . . .
H8A H 0.2451 -0.2007 0.4667 0.023 Uiso 1 1 calc R . .
C9A C 0.4332(6) -0.1521(4) 0.5434(3) 0.0164(9) Uani 1 1 d . . .
H9A H 0.4484 -0.0776 0.5689 0.020 Uiso 1 1 calc R . .
C10A C 0.4080(6) -0.2600(4) 0.6188(3) 0.0193(10) Uani 1 1 d . . .
C11A C 0.6003(6) -0.1646(4) 0.4855(3) 0.0211(10) Uani 1 1 d . . .
H11C H 0.5946 -0.2408 0.4620 0.025 Uiso 1 1 calc R . .
H11D H 0.7049 -0.1715 0.5195 0.025 Uiso 1 1 calc R . .
C12A C 0.6254(6) -0.0565(4) 0.4118(3) 0.0228(10) Uani 1 1 d . . .
H12C H 0.6460 0.0185 0.4347 0.027 Uiso 1 1 calc R . .
H12D H 0.7312 -0.0727 0.3750 0.027 Uiso 1 1 calc R . .
C13A C 0.4627(6) -0.0363(4) 0.3592(3) 0.0169(9) Uani 1 1 d . . .
C14A C 0.3012(6) -0.0182(4) 0.4208(3) 0.0195(10) Uani 1 1 d . . .
H14A H 0.3296 0.0517 0.4487 0.023 Uiso 1 1 calc R . .
C15A C 0.1522(6) 0.0272(4) 0.3641(3) 0.0236(10) Uani 1 1 d . . .
H15C H 0.0646 0.0777 0.3924 0.028 Uiso 1 1 calc R . .
H15D H 0.0909 -0.0420 0.3485 0.028 Uiso 1 1 calc R . .
C16A C 0.2485(6) 0.1047(4) 0.2849(3) 0.0257(10) Uani 1 1 d . . .
H16C H 0.2138 0.1920 0.2813 0.031 Uiso 1 1 calc R . .
H16D H 0.2170 0.0771 0.2328 0.031 Uiso 1 1 calc R . .
C17A C 0.4517(6) 0.0863(4) 0.2952(3) 0.0193(9) Uani 1 1 d . . .
H17A H 0.4886 0.1525 0.3247 0.023 Uiso 1 1 calc R . .
C18A C 0.4397(6) -0.1449(4) 0.3129(3) 0.0227(10) Uani 1 1 d . . .
H18D H 0.5445 -0.1532 0.2745 0.034 Uiso 1 1 calc R . .
H18E H 0.3344 -0.1303 0.2805 0.034 Uiso 1 1 calc R . .
H18F H 0.4257 -0.2201 0.3545 0.034 Uiso 1 1 calc R . .
C19A C 0.3859(7) -0.3824(4) 0.5875(3) 0.0261(11) Uani 1 1 d . . .
H19D H 0.4903 -0.3987 0.5509 0.039 Uiso 1 1 calc R . .
H19E H 0.2799 -0.3772 0.5555 0.039 Uiso 1 1 calc R . .
H19F H 0.3734 -0.4486 0.6361 0.039 Uiso 1 1 calc R . .
C20A C 0.5631(6) 0.0983(4) 0.2107(3) 0.0203(9) Uani 1 1 d . . .
H20A H 0.5267 0.0332 0.1801 0.024 Uiso 1 1 calc R . .
C21A C 0.7627(6) 0.0819(5) 0.2216(3) 0.0298(12) Uani 1 1 d . . .
H21D H 0.8273 0.0898 0.1659 0.045 Uiso 1 1 calc R . .
H21E H 0.7866 0.0008 0.2541 0.045 Uiso 1 1 calc R . .
H21F H 0.8014 0.1445 0.2517 0.045 Uiso 1 1 calc R . .
C22A C 0.5234(6) 0.2234(4) 0.1560(3) 0.0235(10) Uani 1 1 d . . .
H22C H 0.3942 0.2316 0.1499 0.028 Uiso 1 1 calc R . .
H22D H 0.5569 0.2887 0.1861 0.028 Uiso 1 1 calc R . .
C23A C 0.6198(6) 0.2430(4) 0.0677(3) 0.0252(10) Uani 1 1 d . . .
H23C H 0.7491 0.2433 0.0733 0.030 Uiso 1 1 calc R . .
H23D H 0.5950 0.1743 0.0390 0.030 Uiso 1 1 calc R . .
C24A C 0.5641(6) 0.3606(5) 0.0147(3) 0.0258(11) Uani 1 1 d . . .
C25A C 0.5270(9) 0.4602(6) -0.1252(4) 0.0455(15) Uani 1 1 d . . .
H25D H 0.5323 0.4436 -0.1832 0.068 Uiso 1 1 calc R . .
H25E H 0.6138 0.5220 -0.1214 0.068 Uiso 1 1 calc R . .
H25F H 0.4079 0.4903 -0.1098 0.068 Uiso 1 1 calc R . .
C26A C 0.3838(6) -0.1672(5) 0.9118(3) 0.0291(11) Uani 1 1 d . . .
C27A C 0.4072(6) -0.0438(5) 0.8834(3) 0.0267(11) Uani 1 1 d . . .
C28A C 0.3825(7) 0.0408(5) 0.9363(3) 0.0328(12) Uani 1 1 d . . .
H28A H 0.4005 0.1254 0.9168 0.039 Uiso 1 1 calc R . .
C29A C 0.3295(8) -0.0048(6) 1.0201(4) 0.0425(15) Uani 1 1 d . . .
H29A H 0.3070 0.0506 1.0586 0.051 Uiso 1 1 calc R . .
C30A C 0.3087(8) -0.1277(6) 1.0488(4) 0.0467(16) Uani 1 1 d . . .
H30A H 0.2756 -0.1557 1.1068 0.056 Uiso 1 1 calc R . .
C31A C 0.3362(7) -0.2123(5) 0.9930(3) 0.0366(13) Uani 1 1 d . . .
H31A H 0.3216 -0.2974 1.0120 0.044 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 0.0282(18) 0.0191(16) 0.0242(18) -0.0046(13) -0.0013(15) -0.0005(14)
O2 0.034(2) 0.0218(17) 0.0234(19) -0.0057(14) -0.0020(15) 0.0028(15)
O24 0.052(2) 0.0236(19) 0.027(2) 0.0000(15) -0.0072(17) -0.0029(17)
O25 0.049(2) 0.030(2) 0.031(2) -0.0014(16) 0.0003(18) 0.0025(18)
C1 0.020(2) 0.021(2) 0.022(2) -0.0065(19) 0.0000(19) -0.0033(19)
C2 0.019(2) 0.027(3) 0.022(3) -0.006(2) -0.0003(19) -0.003(2)
C3 0.026(3) 0.019(2) 0.022(3) -0.0077(19) 0.001(2) 0.0028(19)
C4 0.021(2) 0.024(2) 0.017(2) -0.0050(18) -0.0030(18) -0.0042(19)
C5 0.019(2) 0.016(2) 0.025(3) -0.0004(18) -0.0058(19) 0.0006(18)
C6 0.015(2) 0.030(3) 0.024(2) -0.008(2) -0.0019(19) 0.0024(19)
C7 0.016(2) 0.030(3) 0.025(3) -0.006(2) -0.002(2) -0.003(2)
C8 0.013(2) 0.022(2) 0.028(3) -0.0051(19) -0.0033(19) -0.0032(18)
C9 0.013(2) 0.023(2) 0.024(3) -0.0047(19) -0.0028(18) 0.0017(18)
C10 0.017(2) 0.016(2) 0.029(3) -0.0060(19) -0.0048(19) 0.0006(18)
C11 0.013(2) 0.033(3) 0.024(3) -0.004(2) -0.0019(19) -0.005(2)
C12 0.017(2) 0.027(3) 0.028(3) -0.003(2) -0.006(2) 0.001(2)
C13 0.014(2) 0.018(2) 0.025(3) -0.0071(18) -0.0011(19) 0.0006(18)
C14 0.016(2) 0.021(2) 0.030(3) -0.008(2) -0.004(2) -0.0009(19)
C15 0.016(2) 0.022(2) 0.028(3) -0.0019(19) -0.0037(19) -0.0030(18)
C16 0.024(3) 0.028(3) 0.030(3) -0.003(2) -0.002(2) -0.008(2)
C17 0.020(2) 0.019(2) 0.024(3) -0.0066(18) -0.0037(19) 0.0013(19)
C18 0.023(2) 0.018(2) 0.027(3) -0.0064(19) -0.002(2) -0.0010(19)
C19 0.029(3) 0.019(2) 0.027(3) -0.0069(19) -0.002(2) -0.002(2)
C20 0.024(2) 0.017(2) 0.027(3) -0.0050(19) -0.003(2) 0.0018(19)
C21 0.031(3) 0.027(3) 0.029(3) -0.002(2) -0.007(2) -0.002(2)
C22 0.023(3) 0.020(2) 0.032(3) -0.005(2) -0.002(2) 0.003(2)
C23 0.040(3) 0.020(2) 0.027(3) 0.000(2) -0.002(2) -0.002(2)
C24 0.022(2) 0.032(3) 0.029(3) -0.005(2) -0.002(2) 0.000(2)
C25 0.051(4) 0.041(3) 0.031(3) 0.008(3) 0.002(3) 0.006(3)
C26 0.016(2) 0.026(2) 0.027(3) -0.012(2) 0.0002(19) -0.0041(19)
C27 0.022(2) 0.028(3) 0.022(3) -0.006(2) 0.000(2) -0.004(2)
C28 0.034(3) 0.026(3) 0.028(3) -0.012(2) 0.002(2) -0.007(2)
C29 0.045(3) 0.046(3) 0.019(3) -0.011(2) 0.003(2) -0.017(3)
C30 0.041(3) 0.043(3) 0.022(3) -0.005(2) -0.002(2) -0.018(3)
C31 0.028(3) 0.029(3) 0.026(3) -0.001(2) -0.002(2) -0.004(2)
O1A 0.0305(19) 0.0273(18) 0.0218(19) -0.0006(14) 0.0009(15) -0.0037(15)
O2A 0.0332(19) 0.0212(17) 0.0236(18) -0.0064(14) 0.0036(15) -0.0033(14)
O24A 0.042(2) 0.0240(19) 0.033(2) -0.0019(16) -0.0027(17) 0.0013(16)
O25A 0.047(2) 0.036(2) 0.0207(19) 0.0011(16) -0.0046(16) 0.0025(18)
C1A 0.015(2) 0.020(2) 0.025(3) -0.0029(19) -0.0005(19) 0.0024(18)
C2A 0.021(2) 0.024(2) 0.021(2) -0.0039(19) -0.0025(19) -0.0046(19)
C3A 0.030(3) 0.021(2) 0.022(3) -0.0011(19) 0.000(2) -0.005(2)
C4A 0.022(2) 0.025(2) 0.019(2) -0.0039(19) 0.0044(19) 0.001(2)
C5A 0.014(2) 0.022(2) 0.025(3) -0.0003(19) 0.0016(19) -0.0014(18)
C6A 0.019(2) 0.026(3) 0.029(3) -0.005(2) 0.003(2) -0.002(2)
C7A 0.015(2) 0.026(2) 0.029(3) -0.006(2) 0.0018(19) 0.0014(19)
C8A 0.016(2) 0.018(2) 0.022(2) -0.0047(18) 0.0008(18) -0.0026(18)
C9A 0.014(2) 0.015(2) 0.020(2) -0.0035(17) -0.0033(17) -0.0010(17)
C10A 0.016(2) 0.021(2) 0.020(2) -0.0010(18) 0.0024(18) -0.0009(18)
C11A 0.016(2) 0.025(2) 0.020(2) 0.0028(19) -0.0009(19) 0.0006(19)
C12A 0.015(2) 0.029(3) 0.022(3) 0.002(2) -0.0012(19) 0.002(2)
C13A 0.013(2) 0.016(2) 0.022(2) -0.0008(17) -0.0034(18) -0.0010(17)
C14A 0.014(2) 0.020(2) 0.025(3) -0.0043(19) -0.0016(19) -0.0020(18)
C15A 0.017(2) 0.027(3) 0.024(3) 0.0023(19) -0.0001(19) 0.0044(19)
C16A 0.020(2) 0.026(3) 0.030(3) 0.000(2) -0.004(2) 0.004(2)
C17A 0.019(2) 0.014(2) 0.023(2) 0.0007(17) -0.0006(19) -0.0004(18)
C18A 0.025(2) 0.019(2) 0.024(3) -0.0042(19) -0.003(2) 0.002(2)
C19A 0.028(3) 0.018(2) 0.032(3) -0.002(2) -0.002(2) -0.003(2)
C20A 0.023(2) 0.019(2) 0.018(2) -0.0003(18) -0.0045(19) 0.0016(18)
C21A 0.024(3) 0.036(3) 0.025(3) 0.007(2) 0.001(2) 0.005(2)
C22A 0.025(3) 0.023(2) 0.022(3) -0.0046(19) -0.001(2) -0.004(2)
C23A 0.024(3) 0.027(3) 0.024(3) -0.003(2) -0.002(2) 0.002(2)
C24A 0.022(3) 0.029(3) 0.024(3) 0.002(2) -0.003(2) -0.005(2)
C25A 0.062(4) 0.041(3) 0.029(3) 0.009(3) -0.005(3) -0.002(3)
C26A 0.023(3) 0.040(3) 0.025(3) -0.007(2) -0.002(2) -0.006(2)
C27A 0.022(3) 0.033(3) 0.025(3) -0.005(2) 0.001(2) -0.007(2)
C28A 0.027(3) 0.042(3) 0.033(3) -0.016(2) 0.000(2) -0.004(2)
C29A 0.038(3) 0.064(4) 0.032(3) -0.024(3) -0.001(3) -0.015(3)
C30A 0.044(4) 0.075(5) 0.023(3) -0.011(3) 0.006(3) -0.030(3)
C31A 0.039(3) 0.047(3) 0.025(3) -0.004(2) 0.000(2) -0.022(3)

_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 C26 1.387(5) . ?
O1 C3 1.443(6) . ?
O2 C27 1.384(6) . ?
O2 C3 1.460(5) . ?
O24 C24 1.198(6) . ?
O25 C24 1.336(6) . ?
O25 C25 1.464(6) . ?
C1 C2 1.523(6) . ?
C1 C10 1.547(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.509(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.511(6) . ?
C4 C5 1.539(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.543(6) . ?
C5 C10 1.551(6) . ?
C5 H5 1.0000 . ?
C6 C7 1.523(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.525(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C14 1.520(7) . ?
C8 C9 1.553(6) . ?
C8 H8 1.0000 . ?
C9 C11 1.530(6) . ?
C9 C10 1.558(7) . ?
C9 H9 1.0000 . ?
C10 C19 1.549(6) . ?
C11 C12 1.540(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.536(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.532(6) . ?
C13 C14 1.548(6) . ?
C13 C17 1.563(6) . ?
C14 C15 1.531(6) . ?
C14 H14 1.0000 . ?
C15 C16 1.549(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.557(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C20 1.541(6) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.532(7) . ?
C20 C22 1.539(6) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.526(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.498(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C31 1.371(7) . ?
C26 C27 1.384(7) . ?
C27 C28 1.374(6) . ?
C28 C29 1.397(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.382(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.394(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
O1A C26A 1.387(6) . ?
O1A C3A 1.470(6) . ?
O2A C27A 1.373(6) . ?
O2A C3A 1.459(5) . ?
O24A C24A 1.189(6) . ?
O25A C24A 1.357(6) . ?
O25A C25A 1.451(7) . ?
C1A C2A 1.532(6) . ?
C1A C10A 1.549(6) . ?
C1A H1C 0.9900 . ?
C1A H1D 0.9900 . ?
C2A C3A 1.500(6) . ?
C2A H2C 0.9900 . ?
C2A H2D 0.9900 . ?
C3A C4A 1.507(7) . ?
C4A C5A 1.530(6) . ?
C4A H4C 0.9900 . ?
C4A H4D 0.9900 . ?
C5A C6A 1.536(7) . ?
C5A C10A 1.557(6) . ?
C5A H5A 1.0000 . ?
C6A C7A 1.540(7) . ?
C6A H6C 0.9900 . ?
C6A H6D 0.9900 . ?
C7A C8A 1.528(6) . ?
C7A H7C 0.9900 . ?
C7A H7D 0.9900 . ?
C8A C14A 1.537(6) . ?
C8A C9A 1.553(6) . ?
C8A H8A 1.0000 . ?
C9A C11A 1.531(6) . ?
C9A C10A 1.559(6) . ?
C9A H9A 1.0000 . ?
C10A C19A 1.549(6) . ?
C11A C12A 1.542(6) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C12A C13A 1.536(6) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C13A C14A 1.546(6) . ?
C13A C18A 1.546(6) . ?
C13A C17A 1.565(6) . ?
C14A C15A 1.523(6) . ?
C14A H14A 1.0000 . ?
C15A C16A 1.558(7) . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C16A C17A 1.563(6) . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C17A C20A 1.535(6) . ?
C17A H17A 1.0000 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C20A C21A 1.535(6) . ?
C20A C22A 1.546(6) . ?
C20A H20A 1.0000 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A C23A 1.532(7) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23A C24A 1.499(7) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26A C31A 1.345(7) . ?
C26A C27A 1.383(7) . ?
C27A C28A 1.373(7) . ?
C28A C29A 1.392(8) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.376(9) . ?
C29A H29A 0.9500 . ?
C30A C31A 1.409(8) . ?
C30A H30A 0.9500 . ?
C31A H31A 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
C26 O1 C3 106.4(3) . . ?
C27 O2 C3 105.1(3) . . ?
C24 O25 C25 115.4(4) . . ?
C2 C1 C10 114.1(4) . . ?
C2 C1 H1A 108.7 . . ?
C10 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
C10 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C1 110.3(4) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
O1 C3 O2 106.2(3) . . ?
O1 C3 C2 109.0(4) . . ?
O2 C3 C2 109.9(4) . . ?
O1 C3 C4 109.1(4) . . ?
O2 C3 C4 109.3(4) . . ?
C2 C3 C4 113.0(4) . . ?
C3 C4 C5 112.5(4) . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 109.6(4) . . ?
C4 C5 C10 112.3(4) . . ?
C6 C5 C10 112.6(4) . . ?
C4 C5 H5 107.4 . . ?
C6 C5 H5 107.4 . . ?
C10 C5 H5 107.4 . . ?
C7 C6 C5 111.7(4) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 112.2(4) . . ?
C6 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C14 C8 C7 111.7(4) . . ?
C14 C8 C9 109.5(4) . . ?
C7 C8 C9 110.9(4) . . ?
C14 C8 H8 108.2 . . ?
C7 C8 H8 108.2 . . ?
C9 C8 H8 108.2 . . ?
C11 C9 C8 111.3(4) . . ?
C11 C9 C10 114.2(4) . . ?
C8 C9 C10 112.6(4) . . ?
C11 C9 H9 106.1 . . ?
C8 C9 H9 106.1 . . ?
C10 C9 H9 106.1 . . ?
C1 C10 C19 105.8(4) . . ?
C1 C10 C5 108.5(4) . . ?
C19 C10 C5 109.6(4) . . ?
C1 C10 C9 112.5(4) . . ?
C19 C10 C9 111.1(4) . . ?
C5 C10 C9 109.3(3) . . ?
C9 C11 C12 113.4(4) . . ?
C9 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C9 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C13 C12 C11 111.0(4) . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C18 C13 C12 110.4(4) . . ?
C18 C13 C14 112.6(4) . . ?
C12 C13 C14 107.0(4) . . ?
C18 C13 C17 109.7(4) . . ?
C12 C13 C17 116.8(4) . . ?
C14 C13 C17 100.0(3) . . ?
C8 C14 C15 118.7(4) . . ?
C8 C14 C13 114.2(4) . . ?
C15 C14 C13 104.6(4) . . ?
C8 C14 H14 106.1 . . ?
C15 C14 H14 106.1 . . ?
C13 C14 H14 106.1 . . ?
C14 C15 C16 103.5(4) . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15B 111.1 . . ?
C16 C15 H15B 111.1 . . ?
H15A C15 H15B 109.0 . . ?
C15 C16 C17 107.6(4) . . ?
C15 C16 H16A 110.2 . . ?
C17 C16 H16A 110.2 . . ?
C15 C16 H16B 110.2 . . ?
C17 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C20 C17 C16 113.6(4) . . ?
C20 C17 C13 118.0(4) . . ?
C16 C17 C13 102.9(4) . . ?
C20 C17 H17 107.2 . . ?
C16 C17 H17 107.2 . . ?
C13 C17 H17 107.2 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C22 111.5(4) . . ?
C21 C20 C17 111.8(4) . . ?
C22 C20 C17 110.7(4) . . ?
C21 C20 H20 107.5 . . ?
C22 C20 H20 107.5 . . ?
C17 C20 H20 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C20 112.8(4) . . ?
C23 C22 H22A 109.0 . . ?
C20 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C20 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C22 113.4(4) . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
O24 C24 O25 123.9(5) . . ?
O24 C24 C23 125.0(5) . . ?
O25 C24 C23 111.0(4) . . ?
O25 C25 H25A 109.5 . . ?
O25 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O25 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C31 C26 C27 122.9(4) . . ?
C31 C26 O1 128.2(4) . . ?
C27 C26 O1 108.9(4) . . ?
C28 C27 O2 127.4(4) . . ?
C28 C27 C26 121.9(5) . . ?
O2 C27 C26 110.6(4) . . ?
C27 C28 C29 115.8(5) . . ?
C27 C28 H28 122.1 . . ?
C29 C28 H28 122.1 . . ?
C30 C29 C28 121.9(5) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 121.9(5) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C26 C31 C30 115.6(5) . . ?
C26 C31 H31 122.2 . . ?
C30 C31 H31 122.2 . . ?
C26A O1A C3A 105.6(4) . . ?
C27A O2A C3A 106.1(4) . . ?
C24A O25A C25A 114.8(4) . . ?
C2A C1A C10A 114.3(4) . . ?
C2A C1A H1C 108.7 . . ?
C10A C1A H1C 108.7 . . ?
C2A C1A H1D 108.7 . . ?
C10A C1A H1D 108.7 . . ?
H1C C1A H1D 107.6 . . ?
C3A C2A C1A 110.3(4) . . ?
C3A C2A H2C 109.6 . . ?
C1A C2A H2C 109.6 . . ?
C3A C2A H2D 109.6 . . ?
C1A C2A H2D 109.6 . . ?
H2C C2A H2D 108.1 . . ?
O2A C3A O1A 105.4(4) . . ?
O2A C3A C2A 110.1(4) . . ?
O1A C3A C2A 108.3(4) . . ?
O2A C3A C4A 108.5(4) . . ?
O1A C3A C4A 109.7(4) . . ?
C2A C3A C4A 114.4(4) . . ?
C3A C4A C5A 114.8(4) . . ?
C3A C4A H4C 108.6 . . ?
C5A C4A H4C 108.6 . . ?
C3A C4A H4D 108.6 . . ?
C5A C4A H4D 108.6 . . ?
H4C C4A H4D 107.5 . . ?
C4A C5A C6A 110.3(4) . . ?
C4A C5A C10A 112.5(4) . . ?
C6A C5A C10A 111.5(4) . . ?
C4A C5A H5A 107.5 . . ?
C6A C5A H5A 107.5 . . ?
C10A C5A H5A 107.5 . . ?
C5A C6A C7A 112.2(4) . . ?
C5A C6A H6C 109.2 . . ?
C7A C6A H6C 109.2 . . ?
C5A C6A H6D 109.2 . . ?
C7A C6A H6D 109.2 . . ?
H6C C6A H6D 107.9 . . ?
C8A C7A C6A 112.1(4) . . ?
C8A C7A H7C 109.2 . . ?
C6A C7A H7C 109.2 . . ?
C8A C7A H7D 109.2 . . ?
C6A C7A H7D 109.2 . . ?
H7C C7A H7D 107.9 . . ?
C7A C8A C14A 111.7(4) . . ?
C7A C8A C9A 110.7(4) . . ?
C14A C8A C9A 108.7(3) . . ?
C7A C8A H8A 108.6 . . ?
C14A C8A H8A 108.6 . . ?
C9A C8A H8A 108.6 . . ?
C11A C9A C8A 111.4(3) . . ?
C11A C9A C10A 113.9(4) . . ?
C8A C9A C10A 112.2(3) . . ?
C11A C9A H9A 106.2 . . ?
C8A C9A H9A 106.2 . . ?
C10A C9A H9A 106.2 . . ?
C19A C10A C1A 107.0(4) . . ?
C19A C10A C5A 109.8(4) . . ?
C1A C10A C5A 107.2(4) . . ?
C19A C10A C9A 111.4(4) . . ?
C1A C10A C9A 112.1(4) . . ?
C5A C10A C9A 109.2(4) . . ?
C9A C11A C12A 113.5(4) . . ?
C9A C11A H11C 108.9 . . ?
C12A C11A H11C 108.9 . . ?
C9A C11A H11D 108.9 . . ?
C12A C11A H11D 108.9 . . ?
H11C C11A H11D 107.7 . . ?
C13A C12A C11A 111.5(4) . . ?
C13A C12A H12C 109.3 . . ?
C11A C12A H12C 109.3 . . ?
C13A C12A H12D 109.3 . . ?
C11A C12A H12D 109.3 . . ?
H12C C12A H12D 108.0 . . ?
C12A C13A C14A 106.8(4) . . ?
C12A C13A C18A 111.1(4) . . ?
C14A C13A C18A 112.0(4) . . ?
C12A C13A C17A 116.8(4) . . ?
C14A C13A C17A 99.9(3) . . ?
C18A C13A C17A 109.6(4) . . ?
C15A C14A C8A 118.3(4) . . ?
C15A C14A C13A 104.8(4) . . ?
C8A C14A C13A 114.4(4) . . ?
C15A C14A H14A 106.2 . . ?
C8A C14A H14A 106.2 . . ?
C13A C14A H14A 106.2 . . ?
C14A C15A C16A 103.9(4) . . ?
C14A C15A H15C 111.0 . . ?
C16A C15A H15C 111.0 . . ?
C14A C15A H15D 111.0 . . ?
C16A C15A H15D 111.0 . . ?
H15C C15A H15D 109.0 . . ?
C15A C16A C17A 106.8(4) . . ?
C15A C16A H16C 110.4 . . ?
C17A C16A H16C 110.4 . . ?
C15A C16A H16D 110.4 . . ?
C17A C16A H16D 110.4 . . ?
H16C C16A H16D 108.6 . . ?
C20A C17A C16A 113.3(4) . . ?
C20A C17A C13A 118.7(4) . . ?
C16A C17A C13A 103.0(3) . . ?
C20A C17A H17A 107.1 . . ?
C16A C17A H17A 107.1 . . ?
C13A C17A H17A 107.1 . . ?
C13A C18A H18D 109.5 . . ?
C13A C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C13A C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C10A C19A H19D 109.5 . . ?
C10A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C10A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C17A C20A C21A 112.8(4) . . ?
C17A C20A C22A 109.7(4) . . ?
C21A C20A C22A 110.3(4) . . ?
C17A C20A H20A 108.0 . . ?
C21A C20A H20A 108.0 . . ?
C22A C20A H20A 108.0 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C23A C22A C20A 114.4(4) . . ?
C23A C22A H22C 108.7 . . ?
C20A C22A H22C 108.7 . . ?
C23A C22A H22D 108.7 . . ?
C20A C22A H22D 108.7 . . ?
H22C C22A H22D 107.6 . . ?
C24A C23A C22A 112.2(4) . . ?
C24A C23A H23C 109.2 . . ?
C22A C23A H23C 109.2 . . ?
C24A C23A H23D 109.2 . . ?
C22A C23A H23D 109.2 . . ?
H23C C23A H23D 107.9 . . ?
O24A C24A O25A 123.4(5) . . ?
O24A C24A C23A 125.9(5) . . ?
O25A C24A C23A 110.7(4) . . ?
O25A C25A H25D 109.5 . . ?
O25A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
O25A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
C31A C26A C27A 122.2(5) . . ?
C31A C26A O1A 128.1(5) . . ?
C27A C26A O1A 109.7(4) . . ?
O2A C27A C28A 127.3(5) . . ?
O2A C27A C26A 110.4(4) . . ?
C28A C27A C26A 122.2(5) . . ?
C27A C28A C29A 115.9(5) . . ?
C27A C28A H28A 122.0 . . ?
C29A C28A H28A 122.0 . . ?
C30A C29A C28A 122.0(5) . . ?
C30A C29A H29A 119.0 . . ?
C28A C29A H29A 119.0 . . ?
C29A C30A C31A 120.7(5) . . ?
C29A C30A H30A 119.7 . . ?
C31A C30A H30A 119.7 . . ?
C26A C31A C30A 116.9(5) . . ?
C26A C31A H31A 121.5 . . ?
C30A C31A H31A 121.5 . . ?

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
C10 C1 C2 C3 55.8(5) . . . . ?
C26 O1 C3 O2 16.5(4) . . . . ?
C26 O1 C3 C2 134.8(4) . . . . ?
C26 O1 C3 C4 -101.3(4) . . . . ?
C27 O2 C3 O1 -15.8(5) . . . . ?
C27 O2 C3 C2 -133.6(4) . . . . ?
C27 O2 C3 C4 101.8(4) . . . . ?
C1 C2 C3 O1 67.9(5) . . . . ?
C1 C2 C3 O2 -176.1(4) . . . . ?
C1 C2 C3 C4 -53.6(5) . . . . ?
O1 C3 C4 C5 -68.2(5) . . . . ?
O2 C3 C4 C5 176.0(4) . . . . ?
C2 C3 C4 C5 53.3(5) . . . . ?
C3 C4 C5 C6 -179.0(4) . . . . ?
C3 C4 C5 C10 -53.0(5) . . . . ?
C4 C5 C6 C7 71.0(5) . . . . ?
C10 C5 C6 C7 -54.7(5) . . . . ?
C5 C6 C7 C8 54.7(5) . . . . ?
C6 C7 C8 C14 -177.1(4) . . . . ?
C6 C7 C8 C9 -54.7(5) . . . . ?
C14 C8 C9 C11 -51.6(5) . . . . ?
C7 C8 C9 C11 -175.3(4) . . . . ?
C14 C8 C9 C10 178.8(4) . . . . ?
C7 C8 C9 C10 55.1(5) . . . . ?
C2 C1 C10 C19 -172.6(4) . . . . ?
C2 C1 C10 C5 -55.1(5) . . . . ?
C2 C1 C10 C9 65.9(5) . . . . ?
C4 C5 C10 C1 52.5(5) . . . . ?
C6 C5 C10 C1 176.7(4) . . . . ?
C4 C5 C10 C19 167.6(4) . . . . ?
C6 C5 C10 C19 -68.2(5) . . . . ?
C4 C5 C10 C9 -70.5(5) . . . . ?
C6 C5 C10 C9 53.7(5) . . . . ?
C11 C9 C10 C1 57.3(5) . . . . ?
C8 C9 C10 C1 -174.7(4) . . . . ?
C11 C9 C10 C19 -61.1(5) . . . . ?
C8 C9 C10 C19 66.9(5) . . . . ?
C11 C9 C10 C5 177.8(4) . . . . ?
C8 C9 C10 C5 -54.1(5) . . . . ?
C8 C9 C11 C12 52.4(5) . . . . ?
C10 C9 C11 C12 -178.8(4) . . . . ?
C9 C11 C12 C13 -56.1(5) . . . . ?
C11 C12 C13 C18 -66.2(5) . . . . ?
C11 C12 C13 C14 56.7(5) . . . . ?
C11 C12 C13 C17 167.7(4) . . . . ?
C7 C8 C14 C15 -54.8(5) . . . . ?
C9 C8 C14 C15 -178.1(4) . . . . ?
C7 C8 C14 C13 -179.1(4) . . . . ?
C9 C8 C14 C13 57.7(5) . . . . ?
C18 C13 C14 C8 61.4(5) . . . . ?
C12 C13 C14 C8 -60.1(5) . . . . ?
C17 C13 C14 C8 177.7(4) . . . . ?
C18 C13 C14 C15 -70.1(5) . . . . ?
C12 C13 C14 C15 168.5(4) . . . . ?
C17 C13 C14 C15 46.3(4) . . . . ?
C8 C14 C15 C16 -162.2(4) . . . . ?
C13 C14 C15 C16 -33.4(5) . . . . ?
C14 C15 C16 C17 7.3(5) . . . . ?
C15 C16 C17 C20 149.6(4) . . . . ?
C15 C16 C17 C13 20.9(5) . . . . ?
C18 C13 C17 C20 -47.6(5) . . . . ?
C12 C13 C17 C20 78.9(5) . . . . ?
C14 C13 C17 C20 -166.1(4) . . . . ?
C18 C13 C17 C16 78.4(4) . . . . ?
C12 C13 C17 C16 -155.2(4) . . . . ?
C14 C13 C17 C16 -40.2(4) . . . . ?
C16 C17 C20 C21 179.4(4) . . . . ?
C13 C17 C20 C21 -60.1(5) . . . . ?
C16 C17 C20 C22 54.4(5) . . . . ?
C13 C17 C20 C22 175.0(4) . . . . ?
C21 C20 C22 C23 69.7(5) . . . . ?
C17 C20 C22 C23 -165.1(4) . . . . ?
C20 C22 C23 C24 -172.6(4) . . . . ?
C25 O25 C24 O24 1.5(8) . . . . ?
C25 O25 C24 C23 -176.5(5) . . . . ?
C22 C23 C24 O24 21.8(8) . . . . ?
C22 C23 C24 O25 -160.2(4) . . . . ?
C3 O1 C26 C31 169.6(5) . . . . ?
C3 O1 C26 C27 -10.9(5) . . . . ?
C3 O2 C27 C28 -171.4(5) . . . . ?
C3 O2 C27 C26 9.5(5) . . . . ?
C31 C26 C27 C28 1.1(7) . . . . ?
O1 C26 C27 C28 -178.3(4) . . . . ?
C31 C26 C27 O2 -179.7(4) . . . . ?
O1 C26 C27 O2 0.8(5) . . . . ?
O2 C27 C28 C29 -179.8(5) . . . . ?
C26 C27 C28 C29 -0.8(7) . . . . ?
C27 C28 C29 C30 0.5(8) . . . . ?
C28 C29 C30 C31 -0.5(9) . . . . ?
C27 C26 C31 C30 -1.0(7) . . . . ?
O1 C26 C31 C30 178.3(5) . . . . ?
C29 C30 C31 C26 0.7(8) . . . . ?
C10A C1A C2A C3A 56.3(5) . . . . ?
C27A O2A C3A O1A -16.5(5) . . . . ?
C27A O2A C3A C2A -133.0(4) . . . . ?
C27A O2A C3A C4A 101.0(4) . . . . ?
C26A O1A C3A O2A 15.9(5) . . . . ?
C26A O1A C3A C2A 133.7(4) . . . . ?
C26A O1A C3A C4A -100.7(4) . . . . ?
C1A C2A C3A O2A -171.6(4) . . . . ?
C1A C2A C3A O1A 73.6(5) . . . . ?
C1A C2A C3A C4A -49.1(5) . . . . ?
O2A C3A C4A C5A 171.0(4) . . . . ?
O1A C3A C4A C5A -74.3(5) . . . . ?
C2A C3A C4A C5A 47.6(6) . . . . ?
C3A C4A C5A C6A -174.8(4) . . . . ?
C3A C4A C5A C10A -49.8(5) . . . . ?
C4A C5A C6A C7A 70.4(5) . . . . ?
C10A C5A C6A C7A -55.2(5) . . . . ?
C5A C6A C7A C8A 54.3(5) . . . . ?
C6A C7A C8A C14A -175.0(4) . . . . ?
C6A C7A C8A C9A -53.8(5) . . . . ?
C7A C8A C9A C11A -175.1(4) . . . . ?
C14A C8A C9A C11A -52.1(4) . . . . ?
C7A C8A C9A C10A 55.8(5) . . . . ?
C14A C8A C9A C10A 178.8(4) . . . . ?
C2A C1A C10A C19A -175.4(4) . . . . ?
C2A C1A C10A C5A -57.6(5) . . . . ?
C2A C1A C10A C9A 62.2(5) . . . . ?
C4A C5A C10A C19A 168.6(4) . . . . ?
C6A C5A C10A C19A -67.0(5) . . . . ?
C4A C5A C10A C1A 52.7(5) . . . . ?
C6A C5A C10A C1A 177.1(4) . . . . ?
C4A C5A C10A C9A -69.0(5) . . . . ?
C6A C5A C10A C9A 55.5(5) . . . . ?
C11A C9A C10A C19A -62.5(5) . . . . ?
C8A C9A C10A C19A 65.3(5) . . . . ?
C11A C9A C10A C1A 57.3(5) . . . . ?
C8A C9A C10A C1A -174.9(3) . . . . ?
C11A C9A C10A C5A 176.0(4) . . . . ?
C8A C9A C10A C5A -56.2(5) . . . . ?
C8A C9A C11A C12A 52.6(5) . . . . ?
C10A C9A C11A C12A -179.2(4) . . . . ?
C9A C11A C12A C13A -55.5(5) . . . . ?
C11A C12A C13A C14A 56.2(5) . . . . ?
C11A C12A C13A C18A -66.3(5) . . . . ?
C11A C12A C13A C17A 167.0(4) . . . . ?
C7A C8A C14A C15A -55.0(5) . . . . ?
C9A C8A C14A C15A -177.4(4) . . . . ?
C7A C8A C14A C13A -179.1(4) . . . . ?
C9A C8A C14A C13A 58.5(5) . . . . ?
C12A C13A C14A C15A 168.6(4) . . . . ?
C18A C13A C14A C15A -69.5(5) . . . . ?
C17A C13A C14A C15A 46.5(4) . . . . ?
C12A C13A C14A C8A -60.2(5) . . . . ?
C18A C13A C14A C8A 61.6(5) . . . . ?
C17A C13A C14A C8A 177.6(4) . . . . ?
C8A C14A C15A C16A -162.2(4) . . . . ?
C13A C14A C15A C16A -33.4(5) . . . . ?
C14A C15A C16A C17A 7.0(5) . . . . ?
C15A C16A C17A C20A 150.8(4) . . . . ?
C15A C16A C17A C13A 21.3(5) . . . . ?
C12A C13A C17A C20A 78.6(5) . . . . ?
C14A C13A C17A C20A -166.7(4) . . . . ?
C18A C13A C17A C20A -48.8(5) . . . . ?
C12A C13A C17A C16A -155.3(4) . . . . ?
C14A C13A C17A C16A -40.6(4) . . . . ?
C18A C13A C17A C16A 77.3(4) . . . . ?
C16A C17A C20A C21A 179.2(4) . . . . ?
C13A C17A C20A C21A -59.8(5) . . . . ?
C16A C17A C20A C22A 55.8(5) . . . . ?
C13A C17A C20A C22A 176.8(4) . . . . ?
C17A C20A C22A C23A -176.8(4) . . . . ?
C21A C20A C22A C23A 58.3(5) . . . . ?
C20A C22A C23A C24A 174.8(4) . . . . ?
C25A O25A C24A O24A 2.4(7) . . . . ?
C25A O25A C24A C23A -175.9(4) . . . . ?
C22A C23A C24A O24A 35.2(7) . . . . ?
C22A C23A C24A O25A -146.6(4) . . . . ?
C3A O1A C26A C31A 171.6(5) . . . . ?
C3A O1A C26A C27A -9.7(5) . . . . ?
C3A O2A C27A C28A -170.8(5) . . . . ?
C3A O2A C27A C26A 11.0(5) . . . . ?
C31A C26A C27A O2A 178.0(5) . . . . ?
O1A C26A C27A O2A -0.8(6) . . . . ?
C31A C26A C27A C28A -0.3(8) . . . . ?
O1A C26A C27A C28A -179.1(4) . . . . ?
O2A C27A C28A C29A -179.0(5) . . . . ?
C26A C27A C28A C29A -1.0(8) . . . . ?
C27A C28A C29A C30A 2.0(8) . . . . ?
C28A C29A C30A C31A -1.8(9) . . . . ?
C27A C26A C31A C30A 0.6(8) . . . . ?
O1A C26A C31A C30A 179.2(5) . . . . ?
C29A C30A C31A C26A 0.4(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.062

data_7c
_database_code_depnum_ccdc_archive 'CCDC 766949'
#TrackingRef 'Ikonen_Crystaldata_7a_7c_10a_I_'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
'Cyclic 3-ketal of 3,7,12-trioxo-5\b-cholan-24-oate with benzene-1,2-diol'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H40 O6'
_chemical_formula_weight         508.63
_chemical_absolute_configuration syn

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   P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   7.59160(10)
_cell_length_b                   11.4074(2)
_cell_length_c                   16.0654(3)
_cell_angle_alpha                97.4710(10)
_cell_angle_beta                 102.0690(10)
_cell_angle_gamma                95.0810(10)
_cell_volume                     1339.32(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    36306
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Bruker Kappa APEX-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10685
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         28.27
_reflns_number_total             6588
_reflns_number_gt                5921
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker, 2004)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR-2002 (Burla, et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
'SHELXL-97; MERCURY (Macrae, <i>et al.</i>, 2006)'

_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^)+(0.0270P)^2^+0.6225P] 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         6588
_refine_ls_number_parameters     704
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.6475(3) 0.62428(16) 0.88611(12) 0.0246(4) Uani 1 1 d . . .
O2 O 0.5155(3) 0.78960(16) 0.84569(12) 0.0293(4) Uani 1 1 d . . .
O7 O 0.0751(3) 0.5359(2) 0.56858(14) 0.0354(5) Uani 1 1 d . . .
O12 O 0.6320(3) 0.78890(19) 0.45947(14) 0.0408(5) Uani 1 1 d . . .
O24 O 0.1422(5) 0.7062(3) -0.06197(19) 0.0358(7) Uani 0.78 1 d P A 1
O25 O 0.1955(5) 0.8736(4) 0.0351(2) 0.0285(7) Uani 0.78 1 d P A 1
C24 C 0.2037(6) 0.7564(4) 0.0100(4) 0.0266(8) Uani 0.78 1 d P A 1
C25 C 0.1056(5) 0.9332(3) -0.0323(3) 0.0329(8) Uani 0.78 1 d P A 1
H25A H 0.1053 1.0172 -0.0096 0.049 Uiso 0.78 1 calc PR A 1
H25B H -0.0196 0.8955 -0.0540 0.049 Uiso 0.78 1 calc PR A 1
H25C H 0.1699 0.9277 -0.0794 0.049 Uiso 0.78 1 calc PR A 1
O24B O 0.233(2) 0.9166(13) 0.0700(9) 0.042(3) Uani 0.22 1 d P A 2
O25B O 0.1977(16) 0.7647(11) -0.0413(9) 0.036(3) Uani 0.22 1 d P A 2
C24B C 0.239(2) 0.817(2) 0.0408(12) 0.029(3) Uani 0.22 1 d P A 2
C25B C 0.143(2) 0.8486(15) -0.0982(10) 0.048(4) Uani 0.22 1 d P A 2
H25G H 0.1123 0.8081 -0.1579 0.072 Uiso 0.22 1 calc PR A 2
H25H H 0.2420 0.9127 -0.0911 0.072 Uiso 0.22 1 calc PR A 2
H25I H 0.0360 0.8823 -0.0843 0.072 Uiso 0.22 1 calc PR A 2
C1 C 0.7714(4) 0.5902(2) 0.72035(17) 0.0234(5) Uani 1 1 d . . .
H1A H 0.8219 0.5420 0.7647 0.028 Uiso 1 1 calc R . .
H1B H 0.8669 0.6097 0.6891 0.028 Uiso 1 1 calc R . .
C2 C 0.7232(4) 0.7058(2) 0.76503(17) 0.0257(5) Uani 1 1 d . . .
H2A H 0.8319 0.7484 0.8068 0.031 Uiso 1 1 calc R . .
H2B H 0.6831 0.7579 0.7218 0.031 Uiso 1 1 calc R . .
C3 C 0.5732(4) 0.6791(2) 0.81150(17) 0.0243(5) Uani 1 1 d . . .
C4 C 0.4096(4) 0.6004(2) 0.75635(16) 0.0238(5) Uani 1 1 d . . .
H4A H 0.3424 0.6465 0.7148 0.029 Uiso 1 1 calc R . .
H4B H 0.3283 0.5762 0.7935 0.029 Uiso 1 1 calc R . .
C5 C 0.4589(3) 0.4880(2) 0.70649(17) 0.0222(5) Uani 1 1 d . . .
H5 H 0.5059 0.4354 0.7492 0.027 Uiso 1 1 calc R . .
C6 C 0.2830(4) 0.4212(2) 0.64606(17) 0.0255(5) Uani 1 1 d . . .
H6A H 0.3070 0.3423 0.6201 0.031 Uiso 1 1 calc R . .
H6B H 0.1888 0.4086 0.6794 0.031 Uiso 1 1 calc R . .
C7 C 0.2172(3) 0.4937(2) 0.57614(17) 0.0237(5) Uani 1 1 d . . .
C8 C 0.3522(3) 0.5166(2) 0.52093(16) 0.0203(5) Uani 1 1 d . . .
H8 H 0.3788 0.4382 0.4936 0.024 Uiso 1 1 calc R . .
C9 C 0.5313(3) 0.5830(2) 0.58149(16) 0.0197(5) Uani 1 1 d . . .
H9 H 0.4984 0.6592 0.6092 0.024 Uiso 1 1 calc R . .
C10 C 0.6079(4) 0.5148(2) 0.65620(17) 0.0217(5) Uani 1 1 d . . .
C11 C 0.6729(4) 0.6186(3) 0.52990(17) 0.0262(6) Uani 1 1 d . . .
H11C H 0.7770 0.6706 0.5687 0.031 Uiso 1 1 calc R . .
H11D H 0.7185 0.5464 0.5051 0.031 Uiso 1 1 calc R . .
C12 C 0.5871(4) 0.6837(2) 0.45846(17) 0.0255(5) Uani 1 1 d . . .
C13 C 0.4279(3) 0.6106(2) 0.39384(16) 0.0209(5) Uani 1 1 d . . .
C14 C 0.2860(3) 0.5897(2) 0.44999(16) 0.0209(5) Uani 1 1 d . . .
H14 H 0.2696 0.6697 0.4790 0.025 Uiso 1 1 calc R . .
C15 C 0.1095(4) 0.5441(2) 0.38245(17) 0.0263(5) Uani 1 1 d . . .
H15C H 0.0020 0.5611 0.4058 0.032 Uiso 1 1 calc R . .
H15D H 0.1016 0.4572 0.3637 0.032 Uiso 1 1 calc R . .
C16 C 0.1224(4) 0.6135(2) 0.30698(18) 0.0257(5) Uani 1 1 d . . .
H16A H 0.0359 0.6737 0.3038 0.031 Uiso 1 1 calc R . .
H16B H 0.0928 0.5584 0.2518 0.031 Uiso 1 1 calc R . .
C17 C 0.3212(4) 0.6758(2) 0.32408(17) 0.0236(5) Uani 1 1 d . . .
H17 H 0.3228 0.7604 0.3502 0.028 Uiso 1 1 calc R . .
C18 C 0.4787(4) 0.4912(2) 0.35308(18) 0.0264(6) Uani 1 1 d . . .
H18A H 0.3724 0.4475 0.3117 0.040 Uiso 1 1 calc R . .
H18B H 0.5192 0.4434 0.3984 0.040 Uiso 1 1 calc R . .
H18C H 0.5766 0.5072 0.3234 0.040 Uiso 1 1 calc R . .
C19 C 0.6741(4) 0.3979(2) 0.62279(18) 0.0266(5) Uani 1 1 d . . .
H19A H 0.7204 0.3570 0.6714 0.040 Uiso 1 1 calc R . .
H19B H 0.7712 0.4155 0.5929 0.040 Uiso 1 1 calc R . .
H19C H 0.5730 0.3467 0.5828 0.040 Uiso 1 1 calc R . .
C20 C 0.3925(4) 0.6758(3) 0.24149(17) 0.0264(5) Uani 1 1 d . . .
H20 H 0.3849 0.5908 0.2146 0.032 Uiso 1 1 calc R . .
C21 C 0.5907(4) 0.7284(4) 0.2593(2) 0.0432(8) Uani 1 1 d . . .
H21D H 0.6300 0.7261 0.2048 0.065 Uiso 1 1 calc R . .
H21E H 0.6655 0.6818 0.2968 0.065 Uiso 1 1 calc R . .
H21F H 0.6040 0.8110 0.2878 0.065 Uiso 1 1 calc R . .
C22 C 0.2749(4) 0.7398(3) 0.1755(2) 0.0341(7) Uani 1 1 d . A .
H22C H 0.1454 0.7197 0.1755 0.041 Uiso 1 1 calc R . .
H22D H 0.3059 0.8270 0.1923 0.041 Uiso 1 1 calc R . .
C23 C 0.3045(4) 0.7036(3) 0.0853(2) 0.0361(7) Uani 1 1 d . . .
H23A H 0.4358 0.7217 0.0881 0.043 Uiso 1 1 calc R A 1
H23B H 0.2753 0.6160 0.0711 0.043 Uiso 1 1 calc R A 1
C26 C 0.6863(4) 0.7156(2) 0.95487(17) 0.0237(5) Uani 1 1 d . . .
C27 C 0.6061(4) 0.8138(2) 0.93063(17) 0.0248(5) Uani 1 1 d . . .
C28 C 0.6184(4) 0.9169(3) 0.98647(19) 0.0307(6) Uani 1 1 d . . .
H28 H 0.5620 0.9836 0.9692 0.037 Uiso 1 1 calc R . .
C29 C 0.7187(4) 0.9191(3) 1.07061(19) 0.0318(6) Uani 1 1 d . . .
H29 H 0.7299 0.9887 1.1118 0.038 Uiso 1 1 calc R . .
C30 C 0.8014(4) 0.8217(3) 1.09462(19) 0.0319(6) Uani 1 1 d . . .
H30 H 0.8701 0.8265 1.1519 0.038 Uiso 1 1 calc R . .
C31 C 0.7870(4) 0.7158(3) 1.03682(17) 0.0259(5) Uani 1 1 d . . .
H31 H 0.8432 0.6487 1.0533 0.031 Uiso 1 1 calc R . .
O1A O 0.3518(3) 0.12095(17) 0.89060(12) 0.0321(5) Uani 1 1 d . . .
O2A O 0.3414(3) 0.30612(17) 0.84460(13) 0.0377(5) Uani 1 1 d . . .
O7A O -0.2567(3) 0.13405(18) 0.59426(13) 0.0299(4) Uani 1 1 d . . .
O12A O 0.3428(3) 0.21269(17) 0.45302(12) 0.0273(4) Uani 1 1 d . . .
O24A O -0.0141(3) 0.43913(19) 0.08817(14) 0.0403(5) Uani 1 1 d . . .
O25A O -0.0571(3) 0.30497(18) -0.03156(13) 0.0341(5) Uani 1 1 d . . .
C1A C 0.4036(4) 0.0184(2) 0.71431(17) 0.0257(5) Uani 1 1 d . . .
H1A1 H 0.4250 -0.0341 0.7589 0.031 Uiso 1 1 calc R . .
H1A2 H 0.4888 0.0028 0.6763 0.031 Uiso 1 1 calc R . .
C2A C 0.4463(4) 0.1483(2) 0.75840(18) 0.0285(6) Uani 1 1 d . . .
H2A1 H 0.5711 0.1613 0.7946 0.034 Uiso 1 1 calc R . .
H2A2 H 0.4402 0.2015 0.7141 0.034 Uiso 1 1 calc R . .
C3A C 0.3136(4) 0.1790(2) 0.81386(17) 0.0279(6) Uani 1 1 d . . .
C4A C 0.1173(4) 0.1437(2) 0.76793(17) 0.0264(6) Uani 1 1 d . . .
H4A1 H 0.0833 0.1976 0.7252 0.032 Uiso 1 1 calc R . .
H4A2 H 0.0402 0.1543 0.8104 0.032 Uiso 1 1 calc R . .
C5A C 0.0785(4) 0.0138(2) 0.72146(17) 0.0231(5) Uani 1 1 d . . .
H5A H 0.0974 -0.0398 0.7663 0.028 Uiso 1 1 calc R . .
C6A C -0.1205(4) -0.0114(2) 0.67254(18) 0.0257(5) Uani 1 1 d . . .
H6A1 H -0.1509 -0.0975 0.6503 0.031 Uiso 1 1 calc R . .
H6A2 H -0.2001 0.0108 0.7121 0.031 Uiso 1 1 calc R . .
C7A C -0.1526(3) 0.0591(2) 0.59840(17) 0.0227(5) Uani 1 1 d . . .
C8A C -0.0349(3) 0.0348(2) 0.53396(16) 0.0194(5) Uani 1 1 d . . .
H8A H -0.0628 -0.0509 0.5075 0.023 Uiso 1 1 calc R . .
C9A C 0.1671(3) 0.0574(2) 0.58456(16) 0.0191(5) Uani 1 1 d . . .
H9A H 0.1880 0.1431 0.6112 0.023 Uiso 1 1 calc R . .
C10A C 0.2081(3) -0.0144(2) 0.66057(17) 0.0212(5) Uani 1 1 d . . .
C11A C 0.2998(3) 0.0439(2) 0.52307(16) 0.0229(5) Uani 1 1 d . . .
H11A H 0.4262 0.0690 0.5557 0.028 Uiso 1 1 calc R . .
H11B H 0.2905 -0.0404 0.4965 0.028 Uiso 1 1 calc R . .
C12A C 0.2493(3) 0.1214(2) 0.45386(15) 0.0196(5) Uani 1 1 d . . .
C13A C 0.0614(3) 0.0859(2) 0.39689(16) 0.0192(5) Uani 1 1 d . . .
C14A C -0.0642(3) 0.1108(2) 0.46201(16) 0.0203(5) Uani 1 1 d . . .
H14A H -0.0292 0.1956 0.4900 0.024 Uiso 1 1 calc R . .
C15A C -0.2518(4) 0.1049(3) 0.40245(18) 0.0284(6) Uani 1 1 d . . .
H15A H -0.3315 0.1529 0.4306 0.034 Uiso 1 1 calc R . .
H15B H -0.3104 0.0217 0.3857 0.034 Uiso 1 1 calc R . .
C16A C -0.2114(4) 0.1576(3) 0.32304(19) 0.0318(6) Uani 1 1 d . . .
H16C H -0.2556 0.2365 0.3213 0.038 Uiso 1 1 calc R . .
H16D H -0.2732 0.1043 0.2693 0.038 Uiso 1 1 calc R . .
C17A C -0.0019(4) 0.1697(2) 0.33180(16) 0.0224(5) Uani 1 1 d . . .
H17A H 0.0470 0.2527 0.3605 0.027 Uiso 1 1 calc R . .
C18A C 0.0291(4) -0.0453(2) 0.35330(17) 0.0254(5) Uani 1 1 d . . .
H18D H -0.0941 -0.0625 0.3171 0.038 Uiso 1 1 calc R . .
H18E H 0.0434 -0.0975 0.3976 0.038 Uiso 1 1 calc R . .
H18F H 0.1173 -0.0593 0.3175 0.038 Uiso 1 1 calc R . .
C19A C 0.1836(4) -0.1494(2) 0.62827(19) 0.0299(6) Uani 1 1 d . . .
H19D H 0.0605 -0.1735 0.5933 0.045 Uiso 1 1 calc R . .
H19E H 0.2029 -0.1926 0.6777 0.045 Uiso 1 1 calc R . .
H19F H 0.2719 -0.1679 0.5933 0.045 Uiso 1 1 calc R . .
C20A C 0.0552(4) 0.1520(2) 0.24484(17) 0.0243(5) Uani 1 1 d . . .
H20A H -0.0115 0.0755 0.2108 0.029 Uiso 1 1 calc R . .
C21A C 0.2590(4) 0.1448(3) 0.25392(18) 0.0286(6) Uani 1 1 d . . .
H21A H 0.2945 0.0800 0.2860 0.043 Uiso 1 1 calc R . .
H21B H 0.3273 0.2203 0.2850 0.043 Uiso 1 1 calc R . .
H21C H 0.2854 0.1294 0.1966 0.043 Uiso 1 1 calc R . .
C22A C -0.0029(4) 0.2539(3) 0.19426(18) 0.0292(6) Uani 1 1 d . . .
H22A H -0.1282 0.2668 0.1984 0.035 Uiso 1 1 calc R . .
H22B H 0.0772 0.3280 0.2219 0.035 Uiso 1 1 calc R . .
C23A C 0.0038(4) 0.2312(3) 0.09971(18) 0.0289(6) Uani 1 1 d . . .
H23C H 0.1227 0.2048 0.0951 0.035 Uiso 1 1 calc R . .
H23D H -0.0913 0.1654 0.0699 0.035 Uiso 1 1 calc R . .
C24A C -0.0228(4) 0.3379(3) 0.05438(18) 0.0280(6) Uani 1 1 d . . .
C25A C -0.0805(5) 0.4008(3) -0.0820(2) 0.0418(8) Uani 1 1 d . . .
H25D H -0.1055 0.3683 -0.1434 0.063 Uiso 1 1 calc R . .
H25E H 0.0305 0.4572 -0.0670 0.063 Uiso 1 1 calc R . .
H25F H -0.1823 0.4420 -0.0698 0.063 Uiso 1 1 calc R . .
C26A C 0.4074(4) 0.2105(2) 0.96014(17) 0.0253(5) Uani 1 1 d . . .
C27A C 0.4031(4) 0.3204(2) 0.93246(17) 0.0272(6) Uani 1 1 d . . .
C28A C 0.4537(4) 0.4253(3) 0.98844(19) 0.0319(6) Uani 1 1 d . . .
H28A H 0.4510 0.5004 0.9690 0.038 Uiso 1 1 calc R . .
C29A C 0.5098(4) 0.4156(3) 1.0759(2) 0.0346(7) Uani 1 1 d . . .
H29A H 0.5482 0.4859 1.1169 0.042 Uiso 1 1 calc R . .
C30A C 0.5101(4) 0.3055(3) 1.10381(18) 0.0326(6) Uani 1 1 d . . .
H30A H 0.5459 0.3019 1.1636 0.039 Uiso 1 1 calc R . .
C31A C 0.4588(4) 0.1996(3) 1.04543(18) 0.0289(6) Uani 1 1 d . . .
H31A H 0.4597 0.1239 1.0641 0.035 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 0.0347(11) 0.0207(8) 0.0193(9) 0.0052(7) 0.0058(8) 0.0052(8)
O2 0.0448(12) 0.0242(9) 0.0195(9) 0.0036(7) 0.0047(8) 0.0123(9)
O7 0.0249(10) 0.0507(13) 0.0360(11) 0.0174(10) 0.0119(9) 0.0056(9)
O12 0.0494(14) 0.0300(11) 0.0355(12) 0.0085(9) -0.0006(10) -0.0169(10)
O24 0.0415(19) 0.0379(17) 0.0235(15) 0.0043(13) -0.0005(13) 0.0002(15)
O25 0.0268(18) 0.034(2) 0.0245(18) 0.0057(16) 0.0042(15) 0.0044(16)
C24 0.025(2) 0.031(2) 0.026(2) 0.008(2) 0.0092(17) -0.0010(18)
C25 0.034(2) 0.0324(18) 0.034(2) 0.0155(16) 0.0058(16) 0.0013(16)
O24B 0.062(9) 0.035(7) 0.032(7) 0.014(5) 0.010(7) 0.000(6)
O25B 0.045(7) 0.038(7) 0.024(6) 0.014(5) 0.011(5) -0.014(5)
C24B 0.015(7) 0.035(10) 0.034(9) 0.002(9) 0.004(6) 0.001(7)
C25B 0.061(11) 0.048(9) 0.026(7) 0.018(7) -0.011(7) -0.006(8)
C1 0.0225(13) 0.0248(12) 0.0236(13) 0.0052(10) 0.0064(10) 0.0015(10)
C2 0.0320(15) 0.0215(12) 0.0229(13) 0.0042(10) 0.0064(11) -0.0031(11)
C3 0.0349(15) 0.0186(11) 0.0208(12) 0.0049(10) 0.0068(11) 0.0074(11)
C4 0.0285(14) 0.0243(12) 0.0201(12) 0.0060(10) 0.0066(10) 0.0043(11)
C5 0.0236(13) 0.0194(11) 0.0243(13) 0.0062(10) 0.0060(10) 0.0014(10)
C6 0.0258(14) 0.0218(12) 0.0283(14) 0.0062(10) 0.0061(11) -0.0035(10)
C7 0.0200(12) 0.0245(12) 0.0255(13) 0.0047(10) 0.0042(10) -0.0029(10)
C8 0.0209(12) 0.0182(11) 0.0209(12) 0.0022(9) 0.0040(10) 0.0000(9)
C9 0.0198(12) 0.0188(11) 0.0207(12) 0.0024(9) 0.0057(9) 0.0011(9)
C10 0.0231(13) 0.0171(11) 0.0254(13) 0.0036(10) 0.0062(10) 0.0032(10)
C11 0.0194(13) 0.0341(14) 0.0243(13) 0.0056(11) 0.0054(10) -0.0037(11)
C12 0.0233(13) 0.0299(13) 0.0232(13) 0.0029(10) 0.0080(10) -0.0030(11)
C13 0.0213(12) 0.0193(11) 0.0225(12) 0.0030(10) 0.0065(10) 0.0010(10)
C14 0.0230(13) 0.0195(11) 0.0210(12) 0.0035(9) 0.0064(10) 0.0026(10)
C15 0.0218(13) 0.0282(13) 0.0278(14) 0.0051(11) 0.0043(11) -0.0015(10)
C16 0.0227(13) 0.0282(13) 0.0271(13) 0.0063(11) 0.0059(10) 0.0039(11)
C17 0.0249(13) 0.0221(12) 0.0243(13) 0.0049(10) 0.0057(10) 0.0028(10)
C18 0.0308(14) 0.0255(13) 0.0245(13) 0.0025(11) 0.0085(11) 0.0085(11)
C19 0.0284(14) 0.0221(12) 0.0291(14) 0.0016(10) 0.0061(11) 0.0061(11)
C20 0.0254(13) 0.0312(14) 0.0239(13) 0.0086(11) 0.0058(11) 0.0032(11)
C21 0.0299(16) 0.066(2) 0.0332(17) 0.0160(16) 0.0064(13) -0.0074(15)
C22 0.0358(16) 0.0369(15) 0.0361(16) 0.0195(13) 0.0121(13) 0.0091(13)
C23 0.0354(16) 0.0428(17) 0.0328(15) 0.0178(13) 0.0056(13) 0.0065(14)
C26 0.0265(13) 0.0214(12) 0.0242(13) 0.0039(10) 0.0095(11) -0.0006(10)
C27 0.0263(13) 0.0295(13) 0.0198(12) 0.0053(10) 0.0068(10) 0.0030(11)
C28 0.0331(15) 0.0285(14) 0.0305(15) 0.0040(12) 0.0070(12) 0.0044(12)
C29 0.0297(15) 0.0349(15) 0.0282(14) -0.0031(12) 0.0072(12) -0.0007(12)
C30 0.0250(14) 0.0433(16) 0.0243(14) 0.0028(12) 0.0033(11) -0.0040(12)
C31 0.0216(13) 0.0333(14) 0.0220(13) 0.0081(11) 0.0026(10) -0.0009(11)
O1A 0.0515(13) 0.0245(9) 0.0191(9) 0.0071(8) 0.0055(9) -0.0015(9)
O2A 0.0655(15) 0.0222(9) 0.0211(10) 0.0044(8) 0.0041(10) -0.0058(10)
O7A 0.0266(10) 0.0332(10) 0.0338(11) 0.0061(9) 0.0115(8) 0.0109(8)
O12A 0.0243(9) 0.0294(10) 0.0253(10) 0.0036(8) 0.0027(8) -0.0047(8)
O24A 0.0592(15) 0.0294(11) 0.0307(11) 0.0048(9) 0.0074(10) 0.0030(10)
O25A 0.0482(13) 0.0325(10) 0.0236(10) 0.0094(8) 0.0067(9) 0.0102(9)
C1A 0.0227(13) 0.0326(14) 0.0237(13) 0.0100(11) 0.0045(10) 0.0058(11)
C2A 0.0261(14) 0.0324(14) 0.0239(13) 0.0100(11) -0.0008(11) -0.0061(11)
C3A 0.0411(16) 0.0209(12) 0.0194(12) 0.0055(10) 0.0027(11) -0.0022(11)
C4A 0.0353(15) 0.0221(12) 0.0254(13) 0.0057(10) 0.0121(12) 0.0077(11)
C5A 0.0239(13) 0.0228(12) 0.0246(13) 0.0067(10) 0.0081(10) 0.0015(10)
C6A 0.0228(13) 0.0264(13) 0.0311(14) 0.0078(11) 0.0115(11) 0.0019(11)
C7A 0.0178(12) 0.0239(12) 0.0257(13) 0.0022(10) 0.0058(10) -0.0014(10)
C8A 0.0185(12) 0.0185(11) 0.0220(12) 0.0032(9) 0.0060(9) 0.0023(9)
C9A 0.0182(12) 0.0185(11) 0.0208(12) 0.0036(9) 0.0043(9) 0.0030(9)
C10A 0.0212(12) 0.0201(11) 0.0248(13) 0.0081(10) 0.0069(10) 0.0049(10)
C11A 0.0194(12) 0.0294(13) 0.0216(12) 0.0087(10) 0.0045(10) 0.0051(10)
C12A 0.0189(12) 0.0235(12) 0.0170(11) 0.0013(9) 0.0061(9) 0.0030(10)
C13A 0.0183(12) 0.0186(11) 0.0197(12) 0.0024(9) 0.0026(9) 0.0019(9)
C14A 0.0189(12) 0.0196(11) 0.0223(12) 0.0030(9) 0.0041(10) 0.0039(9)
C15A 0.0213(13) 0.0376(15) 0.0264(14) 0.0078(12) 0.0029(11) 0.0062(11)
C16A 0.0238(14) 0.0450(17) 0.0274(14) 0.0088(13) 0.0036(11) 0.0091(12)
C17A 0.0234(13) 0.0237(12) 0.0196(12) 0.0034(10) 0.0033(10) 0.0039(10)
C18A 0.0304(14) 0.0199(12) 0.0243(13) -0.0014(10) 0.0069(11) -0.0002(11)
C19A 0.0379(16) 0.0191(12) 0.0346(15) 0.0067(11) 0.0092(12) 0.0075(11)
C20A 0.0270(13) 0.0251(12) 0.0191(12) 0.0032(10) 0.0017(10) 0.0024(10)
C21A 0.0270(14) 0.0356(14) 0.0258(13) 0.0097(11) 0.0074(11) 0.0062(12)
C22A 0.0319(15) 0.0324(14) 0.0244(13) 0.0064(11) 0.0056(11) 0.0087(12)
C23A 0.0355(15) 0.0285(13) 0.0229(13) 0.0066(11) 0.0052(11) 0.0038(12)
C24A 0.0263(14) 0.0338(15) 0.0250(13) 0.0094(11) 0.0055(11) 0.0026(12)
C25A 0.061(2) 0.0391(17) 0.0299(16) 0.0149(14) 0.0104(15) 0.0172(16)
C26A 0.0244(13) 0.0292(13) 0.0229(13) 0.0036(10) 0.0079(10) 0.0009(11)
C27A 0.0290(14) 0.0308(14) 0.0213(13) 0.0062(11) 0.0062(11) -0.0031(11)
C28A 0.0377(16) 0.0289(14) 0.0291(15) 0.0031(11) 0.0115(12) -0.0041(12)
C29A 0.0325(16) 0.0375(16) 0.0299(15) -0.0036(12) 0.0059(12) -0.0021(13)
C30A 0.0305(15) 0.0456(17) 0.0216(14) 0.0016(12) 0.0053(11) 0.0095(13)
C31A 0.0279(14) 0.0356(14) 0.0262(14) 0.0062(11) 0.0098(11) 0.0084(12)

_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 C26 1.379(3) . ?
O1 C3 1.456(3) . ?
O2 C27 1.374(3) . ?
O2 C3 1.450(3) . ?
O7 C7 1.210(3) . ?
O12 C12 1.215(3) . ?
O24 C24 1.200(7) . ?
O25 C24 1.356(5) . ?
O25 C25 1.438(5) . ?
C24 C23 1.514(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O24B C24B 1.18(3) . ?
O25B C24B 1.34(2) . ?
O25B C25B 1.437(18) . ?
C24B C23 1.63(2) . ?
C25B H25G 0.9800 . ?
C25B H25H 0.9800 . ?
C25B H25I 0.9800 . ?
C1 C2 1.529(4) . ?
C1 C10 1.545(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.517(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.506(4) . ?
C4 C5 1.539(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.547(4) . ?
C5 C10 1.552(3) . ?
C5 H5 1.0000 . ?
C6 C7 1.509(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.517(3) . ?
C8 C14 1.526(3) . ?
C8 C9 1.562(3) . ?
C8 H8 1.0000 . ?
C9 C11 1.547(3) . ?
C9 C10 1.554(3) . ?
C9 H9 1.0000 . ?
C10 C19 1.538(3) . ?
C11 C12 1.512(4) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C12 C13 1.519(4) . ?
C13 C18 1.548(4) . ?
C13 C17 1.552(3) . ?
C13 C14 1.565(3) . ?
C14 C15 1.538(4) . ?
C14 H14 1.0000 . ?
C15 C16 1.547(4) . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C16 C17 1.563(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C20 1.534(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.523(4) . ?
C20 C22 1.541(4) . ?
C20 H20 1.0000 . ?
C21 H21D 0.9800 . ?
C21 H21E 0.9800 . ?
C21 H21F 0.9800 . ?
C22 C23 1.523(4) . ?
C22 H22C 0.9900 . ?
C22 H22D 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C26 C31 1.377(4) . ?
C26 C27 1.383(4) . ?
C27 C28 1.367(4) . ?
C28 C29 1.402(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.405(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
O1A C26A 1.378(3) . ?
O1A C3A 1.463(3) . ?
O2A C27A 1.374(3) . ?
O2A C3A 1.451(3) . ?
O7A C7A 1.214(3) . ?
O12A C12A 1.211(3) . ?
O24A C24A 1.200(4) . ?
O25A C24A 1.346(3) . ?
O25A C25A 1.445(3) . ?
C1A C2A 1.533(4) . ?
C1A C10A 1.539(4) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2A C3A 1.513(4) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C3A C4A 1.511(4) . ?
C4A C5A 1.544(4) . ?
C4A H4A1 0.9900 . ?
C4A H4A2 0.9900 . ?
C5A C6A 1.533(4) . ?
C5A C10A 1.551(3) . ?
C5A H5A 1.0000 . ?
C6A C7A 1.512(4) . ?
C6A H6A1 0.9900 . ?
C6A H6A2 0.9900 . ?
C7A C8A 1.517(3) . ?
C8A C14A 1.525(3) . ?
C8A C9A 1.560(3) . ?
C8A H8A 1.0000 . ?
C9A C10A 1.551(3) . ?
C9A C11A 1.555(3) . ?
C9A H9A 1.0000 . ?
C10A C19A 1.541(4) . ?
C11A C12A 1.517(3) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A C13A 1.514(3) . ?
C13A C17A 1.540(3) . ?
C13A C18A 1.543(3) . ?
C13A C14A 1.572(3) . ?
C14A C15A 1.531(4) . ?
C14A H14A 1.0000 . ?
C15A C16A 1.553(4) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C16A C17A 1.559(4) . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C17A C20A 1.541(4) . ?
C17A H17A 1.0000 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C20A C21A 1.534(4) . ?
C20A C22A 1.546(4) . ?
C20A H20A 1.0000 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C22A C23A 1.520(4) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C23A C24A 1.506(4) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26A C31A 1.369(4) . ?
C26A C27A 1.384(4) . ?
C27A C28A 1.372(4) . ?
C28A C29A 1.402(4) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.388(4) . ?
C29A H29A 0.9500 . ?
C30A C31A 1.400(4) . ?
C30A H30A 0.9500 . ?
C31A H31A 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
C26 O1 C3 105.20(18) . . ?
C27 O2 C3 105.5(2) . . ?
C24 O25 C25 114.2(3) . . ?
O24 C24 O25 123.4(4) . . ?
O24 C24 C23 127.0(4) . . ?
O25 C24 C23 109.6(5) . . ?
O25 C25 H25A 109.5 . . ?
O25 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O25 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24B O25B C25B 110.8(15) . . ?
O24B C24B O25B 130(2) . . ?
O24B C24B C23 132.0(15) . . ?
O25B C24B C23 98.2(17) . . ?
O25B C25B H25G 109.5 . . ?
O25B C25B H25H 109.5 . . ?
H25G C25B H25H 109.5 . . ?
O25B C25B H25I 109.5 . . ?
H25G C25B H25I 109.5 . . ?
H25H C25B H25I 109.5 . . ?
C2 C1 C10 113.4(2) . . ?
C2 C1 H1A 108.9 . . ?
C10 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
C10 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C1 110.2(2) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
O2 C3 O1 105.70(19) . . ?
O2 C3 C4 108.7(2) . . ?
O1 C3 C4 109.8(2) . . ?
O2 C3 C2 109.6(2) . . ?
O1 C3 C2 108.5(2) . . ?
C4 C3 C2 114.2(2) . . ?
C3 C4 C5 113.0(2) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 108.1(2) . . ?
C4 C5 C10 113.3(2) . . ?
C6 C5 C10 111.6(2) . . ?
C4 C5 H5 107.9 . . ?
C6 C5 H5 107.9 . . ?
C10 C5 H5 107.9 . . ?
C7 C6 C5 109.2(2) . . ?
C7 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
C7 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
O7 C7 C6 122.9(2) . . ?
O7 C7 C8 123.2(2) . . ?
C6 C7 C8 113.7(2) . . ?
C7 C8 C14 113.8(2) . . ?
C7 C8 C9 107.8(2) . . ?
C14 C8 C9 109.49(19) . . ?
C7 C8 H8 108.5 . . ?
C14 C8 H8 108.5 . . ?
C9 C8 H8 108.5 . . ?
C11 C9 C10 113.3(2) . . ?
C11 C9 C8 111.6(2) . . ?
C10 C9 C8 112.91(19) . . ?
C11 C9 H9 106.1 . . ?
C10 C9 H9 106.1 . . ?
C8 C9 H9 106.1 . . ?
C19 C10 C1 107.1(2) . . ?
C19 C10 C5 109.8(2) . . ?
C1 C10 C5 107.7(2) . . ?
C19 C10 C9 111.7(2) . . ?
C1 C10 C9 111.1(2) . . ?
C5 C10 C9 109.4(2) . . ?
C12 C11 C9 109.8(2) . . ?
C12 C11 H11C 109.7 . . ?
C9 C11 H11C 109.7 . . ?
C12 C11 H11D 109.7 . . ?
C9 C11 H11D 109.7 . . ?
H11C C11 H11D 108.2 . . ?
O12 C12 C11 121.5(3) . . ?
O12 C12 C13 124.1(3) . . ?
C11 C12 C13 114.0(2) . . ?
C12 C13 C18 112.4(2) . . ?
C12 C13 C17 116.8(2) . . ?
C18 C13 C17 111.2(2) . . ?
C12 C13 C14 102.6(2) . . ?
C18 C13 C14 111.4(2) . . ?
C17 C13 C14 101.5(2) . . ?
C8 C14 C15 119.6(2) . . ?
C8 C14 C13 112.4(2) . . ?
C15 C14 C13 103.1(2) . . ?
C8 C14 H14 107.0 . . ?
C15 C14 H14 107.0 . . ?
C13 C14 H14 107.0 . . ?
C14 C15 C16 104.2(2) . . ?
C14 C15 H15C 110.9 . . ?
C16 C15 H15C 110.9 . . ?
C14 C15 H15D 110.9 . . ?
C16 C15 H15D 110.9 . . ?
H15C C15 H15D 108.9 . . ?
C15 C16 C17 107.5(2) . . ?
C15 C16 H16A 110.2 . . ?
C17 C16 H16A 110.2 . . ?
C15 C16 H16B 110.2 . . ?
C17 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C20 C17 C13 116.0(2) . . ?
C20 C17 C16 112.8(2) . . ?
C13 C17 C16 103.7(2) . . ?
C20 C17 H17 108.0 . . ?
C13 C17 H17 108.0 . . ?
C16 C17 H17 108.0 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C17 112.5(2) . . ?
C21 C20 C22 110.3(2) . . ?
C17 C20 C22 112.0(2) . . ?
C21 C20 H20 107.2 . . ?
C17 C20 H20 107.2 . . ?
C22 C20 H20 107.2 . . ?
C20 C21 H21D 109.5 . . ?
C20 C21 H21E 109.5 . . ?
H21D C21 H21E 109.5 . . ?
C20 C21 H21F 109.5 . . ?
H21D C21 H21F 109.5 . . ?
H21E C21 H21F 109.5 . . ?
C23 C22 C20 111.2(2) . . ?
C23 C22 H22C 109.4 . . ?
C20 C22 H22C 109.4 . . ?
C23 C22 H22D 109.4 . . ?
C20 C22 H22D 109.4 . . ?
H22C C22 H22D 108.0 . . ?
C24 C23 C22 120.3(3) . . ?
C22 C23 C24B 100.1(8) . . ?
C24 C23 H23A 107.2 . . ?
C22 C23 H23A 107.2 . . ?
C24B C23 H23A 97.1 . . ?
C24 C23 H23B 107.2 . . ?
C22 C23 H23B 107.2 . . ?
C24B C23 H23B 135.8 . . ?
H23A C23 H23B 106.9 . . ?
C31 C26 O1 128.2(2) . . ?
C31 C26 C27 122.1(3) . . ?
O1 C26 C27 109.6(2) . . ?
C28 C27 O2 127.5(2) . . ?
C28 C27 C26 122.5(2) . . ?
O2 C27 C26 110.0(2) . . ?
C27 C28 C29 116.5(3) . . ?
C27 C28 H28 121.8 . . ?
C29 C28 H28 121.8 . . ?
C30 C29 C28 121.1(3) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 122.0(3) . . ?
C29 C30 H30 119.0 . . ?
C31 C30 H30 119.0 . . ?
C26 C31 C30 115.8(3) . . ?
C26 C31 H31 122.1 . . ?
C30 C31 H31 122.1 . . ?
C26A O1A C3A 106.7(2) . . ?
C27A O2A C3A 106.9(2) . . ?
C24A O25A C25A 115.4(2) . . ?
C2A C1A C10A 114.1(2) . . ?
C2A C1A H1A1 108.7 . . ?
C10A C1A H1A1 108.7 . . ?
C2A C1A H1A2 108.7 . . ?
C10A C1A H1A2 108.7 . . ?
H1A1 C1A H1A2 107.6 . . ?
C3A C2A C1A 111.0(2) . . ?
C3A C2A H2A1 109.4 . . ?
C1A C2A H2A1 109.4 . . ?
C3A C2A H2A2 109.4 . . ?
C1A C2A H2A2 109.4 . . ?
H2A1 C2A H2A2 108.0 . . ?
O2A C3A O1A 106.1(2) . . ?
O2A C3A C4A 109.0(2) . . ?
O1A C3A C4A 109.1(2) . . ?
O2A C3A C2A 109.5(2) . . ?
O1A C3A C2A 109.3(2) . . ?
C4A C3A C2A 113.6(2) . . ?
C3A C4A C5A 113.3(2) . . ?
C3A C4A H4A1 108.9 . . ?
C5A C4A H4A1 108.9 . . ?
C3A C4A H4A2 108.9 . . ?
C5A C4A H4A2 108.9 . . ?
H4A1 C4A H4A2 107.7 . . ?
C6A C5A C4A 109.5(2) . . ?
C6A C5A C10A 111.2(2) . . ?
C4A C5A C10A 112.3(2) . . ?
C6A C5A H5A 107.9 . . ?
C4A C5A H5A 107.9 . . ?
C10A C5A H5A 107.9 . . ?
C7A C6A C5A 110.1(2) . . ?
C7A C6A H6A1 109.6 . . ?
C5A C6A H6A1 109.6 . . ?
C7A C6A H6A2 109.6 . . ?
C5A C6A H6A2 109.6 . . ?
H6A1 C6A H6A2 108.2 . . ?
O7A C7A C6A 122.0(2) . . ?
O7A C7A C8A 123.1(2) . . ?
C6A C7A C8A 114.7(2) . . ?
C7A C8A C14A 113.6(2) . . ?
C7A C8A C9A 107.7(2) . . ?
C14A C8A C9A 110.01(19) . . ?
C7A C8A H8A 108.5 . . ?
C14A C8A H8A 108.5 . . ?
C9A C8A H8A 108.5 . . ?
C10A C9A C11A 113.50(19) . . ?
C10A C9A C8A 113.48(19) . . ?
C11A C9A C8A 111.65(19) . . ?
C10A C9A H9A 105.8 . . ?
C11A C9A H9A 105.8 . . ?
C8A C9A H9A 105.8 . . ?
C1A C10A C19A 107.1(2) . . ?
C1A C10A C9A 112.3(2) . . ?
C19A C10A C9A 111.3(2) . . ?
C1A C10A C5A 107.4(2) . . ?
C19A C10A C5A 109.5(2) . . ?
C9A C10A C5A 109.04(19) . . ?
C12A C11A C9A 108.2(2) . . ?
C12A C11A H11A 110.1 . . ?
C9A C11A H11A 110.1 . . ?
C12A C11A H11B 110.1 . . ?
C9A C11A H11B 110.1 . . ?
H11A C11A H11B 108.4 . . ?
O12A C12A C13A 123.5(2) . . ?
O12A C12A C11A 121.5(2) . . ?
C13A C12A C11A 114.3(2) . . ?
C12A C13A C17A 115.8(2) . . ?
C12A C13A C18A 113.4(2) . . ?
C17A C13A C18A 111.3(2) . . ?
C12A C13A C14A 102.32(19) . . ?
C17A C13A C14A 101.09(19) . . ?
C18A C13A C14A 111.8(2) . . ?
C8A C14A C15A 120.4(2) . . ?
C8A C14A C13A 112.80(19) . . ?
C15A C14A C13A 102.8(2) . . ?
C8A C14A H14A 106.7 . . ?
C15A C14A H14A 106.7 . . ?
C13A C14A H14A 106.7 . . ?
C14A C15A C16A 103.8(2) . . ?
C14A C15A H15A 111.0 . . ?
C16A C15A H15A 111.0 . . ?
C14A C15A H15B 111.0 . . ?
C16A C15A H15B 111.0 . . ?
H15A C15A H15B 109.0 . . ?
C15A C16A C17A 107.5(2) . . ?
C15A C16A H16C 110.2 . . ?
C17A C16A H16C 110.2 . . ?
C15A C16A H16D 110.2 . . ?
C17A C16A H16D 110.2 . . ?
H16C C16A H16D 108.5 . . ?
C13A C17A C20A 118.0(2) . . ?
C13A C17A C16A 103.1(2) . . ?
C20A C17A C16A 113.8(2) . . ?
C13A C17A H17A 107.1 . . ?
C20A C17A H17A 107.1 . . ?
C16A C17A H17A 107.1 . . ?
C13A C18A H18D 109.5 . . ?
C13A C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C13A C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C10A C19A H19D 109.5 . . ?
C10A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C10A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C21A C20A C17A 113.5(2) . . ?
C21A C20A C22A 110.1(2) . . ?
C17A C20A C22A 109.4(2) . . ?
C21A C20A H20A 107.9 . . ?
C17A C20A H20A 107.9 . . ?
C22A C20A H20A 107.9 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23A C22A C20A 114.3(2) . . ?
C23A C22A H22A 108.7 . . ?
C20A C22A H22A 108.7 . . ?
C23A C22A H22B 108.7 . . ?
C20A C22A H22B 108.7 . . ?
H22A C22A H22B 107.6 . . ?
C24A C23A C22A 114.0(2) . . ?
C24A C23A H23C 108.8 . . ?
C22A C23A H23C 108.8 . . ?
C24A C23A H23D 108.8 . . ?
C22A C23A H23D 108.8 . . ?
H23C C23A H23D 107.7 . . ?
O24A C24A O25A 123.4(2) . . ?
O24A C24A C23A 126.2(3) . . ?
O25A C24A C23A 110.4(2) . . ?
O25A C25A H25D 109.5 . . ?
O25A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
O25A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
C31A C26A O1A 128.0(2) . . ?
C31A C26A C27A 122.1(3) . . ?
O1A C26A C27A 109.9(2) . . ?
C28A C27A O2A 127.5(3) . . ?
C28A C27A C26A 122.2(3) . . ?
O2A C27A C26A 110.2(2) . . ?
C27A C28A C29A 116.4(3) . . ?
C27A C28A H28A 121.8 . . ?
C29A C28A H28A 121.8 . . ?
C30A C29A C28A 121.4(3) . . ?
C30A C29A H29A 119.3 . . ?
C28A C29A H29A 119.3 . . ?
C29A C30A C31A 121.2(3) . . ?
C29A C30A H30A 119.4 . . ?
C31A C30A H30A 119.4 . . ?
C26A C31A C30A 116.7(3) . . ?
C26A C31A H31A 121.6 . . ?
C30A C31A H31A 121.6 . . ?

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
C25 O25 C24 O24 0.2(6) . . . . ?
C25 O25 C24 C23 178.7(3) . . . . ?
C25B O25B C24B O24B 2(2) . . . . ?
C25B O25B C24B C23 -176.9(11) . . . . ?
C10 C1 C2 C3 57.0(3) . . . . ?
C27 O2 C3 O1 19.0(3) . . . . ?
C27 O2 C3 C4 136.7(2) . . . . ?
C27 O2 C3 C2 -97.8(2) . . . . ?
C26 O1 C3 O2 -19.4(3) . . . . ?
C26 O1 C3 C4 -136.4(2) . . . . ?
C26 O1 C3 C2 98.1(2) . . . . ?
C1 C2 C3 O2 -173.9(2) . . . . ?
C1 C2 C3 O1 71.1(3) . . . . ?
C1 C2 C3 C4 -51.7(3) . . . . ?
O2 C3 C4 C5 171.9(2) . . . . ?
O1 C3 C4 C5 -73.0(3) . . . . ?
C2 C3 C4 C5 49.1(3) . . . . ?
C3 C4 C5 C6 -174.6(2) . . . . ?
C3 C4 C5 C10 -50.4(3) . . . . ?
C4 C5 C6 C7 68.4(3) . . . . ?
C10 C5 C6 C7 -56.9(3) . . . . ?
C5 C6 C7 O7 -115.4(3) . . . . ?
C5 C6 C7 C8 60.0(3) . . . . ?
O7 C7 C8 C14 -4.7(4) . . . . ?
C6 C7 C8 C14 179.9(2) . . . . ?
O7 C7 C8 C9 117.0(3) . . . . ?
C6 C7 C8 C9 -58.4(3) . . . . ?
C7 C8 C9 C11 -175.8(2) . . . . ?
C14 C8 C9 C11 -51.4(3) . . . . ?
C7 C8 C9 C10 55.3(3) . . . . ?
C14 C8 C9 C10 179.7(2) . . . . ?
C2 C1 C10 C19 -175.3(2) . . . . ?
C2 C1 C10 C5 -57.3(3) . . . . ?
C2 C1 C10 C9 62.5(3) . . . . ?
C4 C5 C10 C19 169.4(2) . . . . ?
C6 C5 C10 C19 -68.3(3) . . . . ?
C4 C5 C10 C1 53.1(3) . . . . ?
C6 C5 C10 C1 175.4(2) . . . . ?
C4 C5 C10 C9 -67.8(3) . . . . ?
C6 C5 C10 C9 54.6(3) . . . . ?
C11 C9 C10 C19 -60.8(3) . . . . ?
C8 C9 C10 C19 67.3(3) . . . . ?
C11 C9 C10 C1 58.7(3) . . . . ?
C8 C9 C10 C1 -173.3(2) . . . . ?
C11 C9 C10 C5 177.5(2) . . . . ?
C8 C9 C10 C5 -54.5(3) . . . . ?
C10 C9 C11 C12 179.7(2) . . . . ?
C8 C9 C11 C12 51.0(3) . . . . ?
C9 C11 C12 O12 112.0(3) . . . . ?
C9 C11 C12 C13 -60.6(3) . . . . ?
O12 C12 C13 C18 131.8(3) . . . . ?
C11 C12 C13 C18 -55.7(3) . . . . ?
O12 C12 C13 C17 1.6(4) . . . . ?
C11 C12 C13 C17 174.0(2) . . . . ?
O12 C12 C13 C14 -108.4(3) . . . . ?
C11 C12 C13 C14 64.1(3) . . . . ?
C7 C8 C14 C15 -58.3(3) . . . . ?
C9 C8 C14 C15 -179.1(2) . . . . ?
C7 C8 C14 C13 -179.5(2) . . . . ?
C9 C8 C14 C13 59.7(3) . . . . ?
C12 C13 C14 C8 -63.5(2) . . . . ?
C18 C13 C14 C8 57.0(3) . . . . ?
C17 C13 C14 C8 175.4(2) . . . . ?
C12 C13 C14 C15 166.3(2) . . . . ?
C18 C13 C14 C15 -73.2(3) . . . . ?
C17 C13 C14 C15 45.2(2) . . . . ?
C8 C14 C15 C16 -160.9(2) . . . . ?
C13 C14 C15 C16 -35.2(2) . . . . ?
C14 C15 C16 C17 12.0(3) . . . . ?
C12 C13 C17 C20 88.2(3) . . . . ?
C18 C13 C17 C20 -42.6(3) . . . . ?
C14 C13 C17 C20 -161.2(2) . . . . ?
C12 C13 C17 C16 -147.6(2) . . . . ?
C18 C13 C17 C16 81.6(3) . . . . ?
C14 C13 C17 C16 -37.0(2) . . . . ?
C15 C16 C17 C20 142.2(2) . . . . ?
C15 C16 C17 C13 15.9(3) . . . . ?
C13 C17 C20 C21 -56.5(3) . . . . ?
C16 C17 C20 C21 -175.8(3) . . . . ?
C13 C17 C20 C22 178.6(2) . . . . ?
C16 C17 C20 C22 59.2(3) . . . . ?
C21 C20 C22 C23 73.4(3) . . . . ?
C17 C20 C22 C23 -160.5(2) . . . . ?
O24 C24 C23 C22 -141.9(4) . . . . ?
O25 C24 C23 C22 39.7(5) . . . . ?
O24 C24 C23 C24B 168.1(14) . . . . ?
O25 C24 C23 C24B -10.3(11) . . . . ?
C20 C22 C23 C24 -179.5(3) . . . . ?
C20 C22 C23 C24B -157.5(6) . . . . ?
O24B C24B C23 C24 163(3) . . . . ?
O25B C24B C23 C24 -18.8(8) . . . . ?
O24B C24B C23 C22 24.9(19) . . . . ?
O25B C24B C23 C22 -156.6(8) . . . . ?
C3 O1 C26 C31 -167.6(3) . . . . ?
C3 O1 C26 C27 12.7(3) . . . . ?
C3 O2 C27 C28 169.1(3) . . . . ?
C3 O2 C27 C26 -11.6(3) . . . . ?
C31 C26 C27 C28 -1.1(4) . . . . ?
O1 C26 C27 C28 178.6(3) . . . . ?
C31 C26 C27 O2 179.5(2) . . . . ?
O1 C26 C27 O2 -0.7(3) . . . . ?
O2 C27 C28 C29 179.6(3) . . . . ?
C26 C27 C28 C29 0.4(4) . . . . ?
C27 C28 C29 C30 0.6(4) . . . . ?
C28 C29 C30 C31 -1.0(4) . . . . ?
O1 C26 C31 C30 -178.9(2) . . . . ?
C27 C26 C31 C30 0.7(4) . . . . ?
C29 C30 C31 C26 0.3(4) . . . . ?
C10A C1A C2A C3A 55.5(3) . . . . ?
C27A O2A C3A O1A 3.7(3) . . . . ?
C27A O2A C3A C4A 121.1(2) . . . . ?
C27A O2A C3A C2A -114.1(2) . . . . ?
C26A O1A C3A O2A -3.0(3) . . . . ?
C26A O1A C3A C4A -120.2(2) . . . . ?
C26A O1A C3A C2A 115.0(2) . . . . ?
C1A C2A C3A O2A -171.9(2) . . . . ?
C1A C2A C3A O1A 72.2(3) . . . . ?
C1A C2A C3A C4A -49.8(3) . . . . ?
O2A C3A C4A C5A 171.9(2) . . . . ?
O1A C3A C4A C5A -72.7(3) . . . . ?
C2A C3A C4A C5A 49.5(3) . . . . ?
C3A C4A C5A C6A -176.6(2) . . . . ?
C3A C4A C5A C10A -52.6(3) . . . . ?
C4A C5A C6A C7A 68.1(3) . . . . ?
C10A C5A C6A C7A -56.7(3) . . . . ?
C5A C6A C7A O7A -117.7(3) . . . . ?
C5A C6A C7A C8A 58.0(3) . . . . ?
O7A C7A C8A C14A -1.8(4) . . . . ?
C6A C7A C8A C14A -177.5(2) . . . . ?
O7A C7A C8A C9A 120.3(3) . . . . ?
C6A C7A C8A C9A -55.4(3) . . . . ?
C7A C8A C9A C10A 54.4(3) . . . . ?
C14A C8A C9A C10A 178.7(2) . . . . ?
C7A C8A C9A C11A -175.8(2) . . . . ?
C14A C8A C9A C11A -51.5(3) . . . . ?
C2A C1A C10A C19A -174.8(2) . . . . ?
C2A C1A C10A C9A 62.7(3) . . . . ?
C2A C1A C10A C5A -57.2(3) . . . . ?
C11A C9A C10A C1A 56.4(3) . . . . ?
C8A C9A C10A C1A -174.7(2) . . . . ?
C11A C9A C10A C19A -63.7(3) . . . . ?
C8A C9A C10A C19A 65.2(3) . . . . ?
C11A C9A C10A C5A 175.4(2) . . . . ?
C8A C9A C10A C5A -55.7(3) . . . . ?
C6A C5A C10A C1A 177.7(2) . . . . ?
C4A C5A C10A C1A 54.6(3) . . . . ?
C6A C5A C10A C19A -66.3(3) . . . . ?
C4A C5A C10A C19A 170.6(2) . . . . ?
C6A C5A C10A C9A 55.8(3) . . . . ?
C4A C5A C10A C9A -67.3(3) . . . . ?
C10A C9A C11A C12A -178.0(2) . . . . ?
C8A C9A C11A C12A 52.2(3) . . . . ?
C9A C11A C12A O12A 107.5(3) . . . . ?
C9A C11A C12A C13A -62.9(3) . . . . ?
O12A C12A C13A C17A 4.0(3) . . . . ?
C11A C12A C13A C17A 174.2(2) . . . . ?
O12A C12A C13A C18A 134.5(3) . . . . ?
C11A C12A C13A C18A -55.3(3) . . . . ?
O12A C12A C13A C14A -104.9(3) . . . . ?
C11A C12A C13A C14A 65.3(2) . . . . ?
C7A C8A C14A C15A -59.3(3) . . . . ?
C9A C8A C14A C15A 179.9(2) . . . . ?
C7A C8A C14A C13A 179.0(2) . . . . ?
C9A C8A C14A C13A 58.2(3) . . . . ?
C12A C13A C14A C8A -62.2(2) . . . . ?
C17A C13A C14A C8A 178.1(2) . . . . ?
C18A C13A C14A C8A 59.6(3) . . . . ?
C12A C13A C14A C15A 166.7(2) . . . . ?
C17A C13A C14A C15A 46.9(2) . . . . ?
C18A C13A C14A C15A -71.6(2) . . . . ?
C8A C14A C15A C16A -161.3(2) . . . . ?
C13A C14A C15A C16A -34.9(3) . . . . ?
C14A C15A C16A C17A 10.4(3) . . . . ?
C12A C13A C17A C20A 84.5(3) . . . . ?
C18A C13A C17A C20A -47.0(3) . . . . ?
C14A C13A C17A C20A -165.8(2) . . . . ?
C12A C13A C17A C16A -149.1(2) . . . . ?
C18A C13A C17A C16A 79.4(3) . . . . ?
C14A C13A C17A C16A -39.4(2) . . . . ?
C15A C16A C17A C13A 18.7(3) . . . . ?
C15A C16A C17A C20A 147.7(2) . . . . ?
C13A C17A C20A C21A -50.0(3) . . . . ?
C16A C17A C20A C21A -171.1(2) . . . . ?
C13A C17A C20A C22A -173.4(2) . . . . ?
C16A C17A C20A C22A 65.6(3) . . . . ?
C21A C20A C22A C23A 68.8(3) . . . . ?
C17A C20A C22A C23A -165.9(2) . . . . ?
C20A C22A C23A C24A -170.5(2) . . . . ?
C25A O25A C24A O24A 1.0(4) . . . . ?
C25A O25A C24A C23A -178.5(3) . . . . ?
C22A C23A C24A O24A 14.8(4) . . . . ?
C22A C23A C24A O25A -165.8(2) . . . . ?
C3A O1A C26A C31A -179.6(3) . . . . ?
C3A O1A C26A C27A 1.2(3) . . . . ?
C3A O2A C27A C28A 177.5(3) . . . . ?
C3A O2A C27A C26A -3.2(3) . . . . ?
C31A C26A C27A C28A 1.4(4) . . . . ?
O1A C26A C27A C28A -179.3(3) . . . . ?
C31A C26A C27A O2A -178.1(3) . . . . ?
O1A C26A C27A O2A 1.3(3) . . . . ?
O2A C27A C28A C29A 179.1(3) . . . . ?
C26A C27A C28A C29A -0.2(4) . . . . ?
C27A C28A C29A C30A -1.2(4) . . . . ?
C28A C29A C30A C31A 1.6(5) . . . . ?
O1A C26A C31A C30A 179.8(3) . . . . ?
C27A C26A C31A C30A -0.9(4) . . . . ?
C29A C30A C31A C26A -0.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.042

data_10a(I)
_database_code_depnum_ccdc_archive 'CCDC 766950'
#TrackingRef 'Ikonen_Crystaldata_7a_7c_10a_I_'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
'Cyclic diketal of methyl 3-oxo-5?-cholan-24-oate with pentaerythritol '
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H88 O8'
_chemical_formula_weight         877.25
_chemical_absolute_configuration syn
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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   29.4843(5)
_cell_length_b                   6.4390(10)
_cell_length_c                   12.7626(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7664(9)
_cell_angle_gamma                90.00
_cell_volume                     2400.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    25229
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      28.283

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             964
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Bruker Kappa APEX-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9619
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         28.29
_reflns_number_total             3234
_reflns_number_gt                2875
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker, 2004)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR-2002 (Burla, et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
'SHELXL-97; MERCURY (Macrae, <i>et al.</i>, 2006)'
_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^)+(0.0412P)^2^+2.6400P] 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         3234
_refine_ls_number_parameters     285
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1022
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
C1 C 0.87286(8) 0.8998(4) 0.72754(18) 0.0229(5) Uani 1 1 d . . .
H1A H 0.8981 0.8201 0.7070 0.028 Uiso 1 1 calc R . .
H1B H 0.8608 0.9858 0.6678 0.028 Uiso 1 1 calc R . .
C2 C 0.89132(7) 1.0418(4) 0.81975(17) 0.0210(5) Uani 1 1 d . . .
H2A H 0.9161 1.1255 0.7997 0.025 Uiso 1 1 calc R . .
H2B H 0.8672 1.1349 0.8352 0.025 Uiso 1 1 calc R . .
C3 C 0.90869(7) 0.9163(4) 0.91871(18) 0.0213(5) Uani 1 1 d . . .
C4 C 0.87204(8) 0.7668(4) 0.94461(18) 0.0218(5) Uani 1 1 d . . .
H4A H 0.8468 0.8460 0.9657 0.026 Uiso 1 1 calc R . .
H4B H 0.8846 0.6817 1.0043 0.026 Uiso 1 1 calc R . .
C5 C 0.85363(7) 0.6243(4) 0.85242(18) 0.0203(5) Uani 1 1 d . . .
H5 H 0.8793 0.5399 0.8356 0.024 Uiso 1 1 calc R . .
C6 C 0.81774(8) 0.4747(4) 0.88589(19) 0.0232(5) Uani 1 1 d . . .
H6A H 0.8115 0.3671 0.8327 0.028 Uiso 1 1 calc R . .
H6B H 0.8301 0.4082 0.9519 0.028 Uiso 1 1 calc R . .
C7 C 0.77314(8) 0.5837(4) 0.90023(18) 0.0219(5) Uani 1 1 d . . .
H7A H 0.7786 0.6801 0.9590 0.026 Uiso 1 1 calc R . .
H7B H 0.7509 0.4818 0.9168 0.026 Uiso 1 1 calc R . .
C8 C 0.75387(7) 0.7018(4) 0.79986(17) 0.0186(4) Uani 1 1 d . . .
H8 H 0.7472 0.6009 0.7423 0.022 Uiso 1 1 calc R . .
C9 C 0.78948(7) 0.8594(4) 0.76801(17) 0.0178(4) Uani 1 1 d . . .
H9 H 0.7971 0.9525 0.8286 0.021 Uiso 1 1 calc R . .
C10 C 0.83501(7) 0.7474(4) 0.75089(17) 0.0192(5) Uani 1 1 d . . .
C11 C 0.76879(7) 0.9965(4) 0.67460(18) 0.0217(5) Uani 1 1 d . . .
H11A H 0.7641 0.9123 0.6110 0.026 Uiso 1 1 calc R . .
H11B H 0.7905 1.1048 0.6637 0.026 Uiso 1 1 calc R . .
C12 C 0.72255(7) 1.0989(4) 0.69122(19) 0.0215(5) Uani 1 1 d . . .
H12A H 0.7276 1.1959 0.7498 0.026 Uiso 1 1 calc R . .
H12B H 0.7105 1.1758 0.6282 0.026 Uiso 1 1 calc R . .
C13 C 0.68757(7) 0.9335(4) 0.71448(17) 0.0179(4) Uani 1 1 d . . .
C14 C 0.70972(7) 0.8138(4) 0.81365(17) 0.0182(4) Uani 1 1 d . . .
H14 H 0.7174 0.9171 0.8696 0.022 Uiso 1 1 calc R . .
C15 C 0.67063(7) 0.6819(4) 0.84586(18) 0.0218(5) Uani 1 1 d . . .
H15A H 0.6760 0.6481 0.9206 0.026 Uiso 1 1 calc R . .
H15B H 0.6669 0.5543 0.8052 0.026 Uiso 1 1 calc R . .
C16 C 0.62849(8) 0.8238(4) 0.82032(18) 0.0222(5) Uani 1 1 d . . .
H16A H 0.6183 0.8725 0.8852 0.027 Uiso 1 1 calc R . .
H16B H 0.6036 0.7481 0.7799 0.027 Uiso 1 1 calc R . .
C17 C 0.64292(7) 1.0118(4) 0.75470(17) 0.0196(5) Uani 1 1 d . . .
H17 H 0.6513 1.1267 0.8039 0.024 Uiso 1 1 calc R . .
C18 C 0.67562(8) 0.7902(4) 0.61809(17) 0.0216(5) Uani 1 1 d . . .
H18A H 0.6620 0.8706 0.5587 0.032 Uiso 1 1 calc R . .
H18B H 0.6544 0.6856 0.6343 0.032 Uiso 1 1 calc R . .
H18C H 0.7030 0.7250 0.6011 0.032 Uiso 1 1 calc R . .
C19 C 0.82724(8) 0.5971(4) 0.65611(18) 0.0260(5) Uani 1 1 d . . .
H19A H 0.8154 0.6726 0.5935 0.039 Uiso 1 1 calc R . .
H19B H 0.8057 0.4918 0.6697 0.039 Uiso 1 1 calc R . .
H19C H 0.8558 0.5331 0.6461 0.039 Uiso 1 1 calc R . .
C20 C 0.60226(7) 1.0841(4) 0.67392(17) 0.0206(5) Uani 1 1 d . . .
H20 H 0.5912 0.9638 0.6308 0.025 Uiso 1 1 calc R . .
C21 C 0.61426(9) 1.2546(4) 0.5995(2) 0.0294(6) Uani 1 1 d . . .
H21A H 0.6386 1.2078 0.5624 0.044 Uiso 1 1 calc R . .
H21B H 0.6239 1.3766 0.6397 0.044 Uiso 1 1 calc R . .
H21C H 0.5878 1.2866 0.5495 0.044 Uiso 1 1 calc R . .
C22 C 0.56277(8) 1.1596(5) 0.73281(19) 0.0269(5) Uani 1 1 d . . .
H22A H 0.5623 1.0755 0.7957 0.032 Uiso 1 1 calc R . .
H22B H 0.5687 1.3020 0.7553 0.032 Uiso 1 1 calc R . .
C23 C 0.51558(8) 1.1484(5) 0.6653(2) 0.0287(6) Uani 1 1 d . . .
H23A H 0.4941 1.2325 0.6980 0.034 Uiso 1 1 calc R . .
H23B H 0.5178 1.2063 0.5960 0.034 Uiso 1 1 calc R . .
C24 C 0.49754(8) 0.9299(5) 0.6526(2) 0.0332(6) Uani 1 1 d . . .
C25 C 0.44171(11) 0.7138(6) 0.5606(2) 0.0474(9) Uani 1 1 d . . .
H25A H 0.4159 0.7208 0.5061 0.071 Uiso 1 1 calc R . .
H25B H 0.4319 0.6636 0.6247 0.071 Uiso 1 1 calc R . .
H25C H 0.4642 0.6210 0.5392 0.071 Uiso 1 1 calc R . .
C26 C 0.95817(7) 1.1756(4) 1.00922(19) 0.0245(5) Uani 1 1 d . . .
H26A H 0.9632 1.2559 1.0741 0.029 Uiso 1 1 calc R . .
H26B H 0.9534 1.2717 0.9502 0.029 Uiso 1 1 calc R . .
C27 C 0.98868(7) 0.9055(4) 0.90101(18) 0.0232(5) Uani 1 1 d . . .
H27A H 0.9853 0.9932 0.8386 0.028 Uiso 1 1 calc R . .
H27B H 1.0137 0.8099 0.8959 0.028 Uiso 1 1 calc R . .
C28 C 1.0000 1.0407(6) 1.0000 0.0200(6) Uani 1 2 d S . .
O1 O 0.51275(9) 0.7808(5) 0.6998(2) 0.0780(10) Uani 1 1 d . . .
O2 O 0.46135(7) 0.9176(4) 0.57842(17) 0.0460(6) Uani 1 1 d . . .
O3 O 0.94737(5) 0.7907(3) 0.90456(12) 0.0226(4) Uani 1 1 d . . .
O4 O 0.91842(5) 1.0467(3) 1.00939(13) 0.0247(4) Uani 1 1 d . . .

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
C1 0.0187(10) 0.0260(13) 0.0247(11) 0.0003(10) 0.0053(8) -0.0003(10)
C2 0.0150(10) 0.0202(12) 0.0284(11) -0.0007(10) 0.0046(8) -0.0006(9)
C3 0.0157(10) 0.0234(12) 0.0248(11) -0.0039(10) 0.0031(8) 0.0018(9)
C4 0.0197(10) 0.0242(13) 0.0214(10) -0.0016(10) 0.0028(8) -0.0015(10)
C5 0.0163(9) 0.0192(12) 0.0251(11) -0.0014(9) 0.0020(8) 0.0017(9)
C6 0.0234(11) 0.0196(12) 0.0256(11) 0.0022(10) -0.0003(9) 0.0008(10)
C7 0.0205(10) 0.0215(12) 0.0232(11) 0.0044(10) 0.0017(8) -0.0022(10)
C8 0.0184(10) 0.0181(11) 0.0192(10) 0.0022(9) 0.0024(8) -0.0007(9)
C9 0.0156(9) 0.0188(11) 0.0192(10) -0.0017(8) 0.0028(8) -0.0017(9)
C10 0.0166(10) 0.0217(11) 0.0197(10) -0.0038(9) 0.0034(8) -0.0004(9)
C11 0.0185(10) 0.0213(12) 0.0258(11) 0.0052(10) 0.0049(9) -0.0031(9)
C12 0.0170(10) 0.0206(12) 0.0266(11) 0.0033(10) 0.0019(8) -0.0008(9)
C13 0.0164(10) 0.0175(11) 0.0198(10) -0.0010(9) 0.0031(8) -0.0006(9)
C14 0.0167(9) 0.0193(11) 0.0187(10) 0.0000(9) 0.0022(8) -0.0026(9)
C15 0.0194(10) 0.0234(12) 0.0229(10) 0.0036(10) 0.0037(8) -0.0023(10)
C16 0.0185(10) 0.0239(12) 0.0244(11) 0.0025(10) 0.0035(8) -0.0015(10)
C17 0.0185(10) 0.0204(11) 0.0197(10) -0.0008(9) 0.0019(8) -0.0007(9)
C18 0.0207(10) 0.0227(12) 0.0208(10) -0.0008(10) 0.0010(8) -0.0010(10)
C19 0.0258(11) 0.0290(13) 0.0237(11) -0.0077(11) 0.0056(9) -0.0023(11)
C20 0.0190(10) 0.0212(11) 0.0210(10) -0.0011(9) 0.0010(8) -0.0004(9)
C21 0.0278(12) 0.0264(13) 0.0330(13) 0.0075(11) 0.0003(10) 0.0006(11)
C22 0.0216(11) 0.0331(14) 0.0256(11) -0.0069(11) 0.0015(9) 0.0031(11)
C23 0.0207(11) 0.0390(15) 0.0258(12) -0.0047(11) 0.0009(9) 0.0071(11)
C24 0.0214(12) 0.0518(18) 0.0253(12) 0.0088(13) -0.0005(10) -0.0035(13)
C25 0.0433(17) 0.053(2) 0.0412(16) 0.0175(16) -0.0105(13) -0.0260(16)
C26 0.0170(10) 0.0275(13) 0.0288(12) -0.0064(11) 0.0028(9) -0.0008(10)
C27 0.0165(10) 0.0305(13) 0.0229(11) -0.0023(10) 0.0040(8) 0.0028(10)
C28 0.0140(13) 0.0265(17) 0.0197(14) 0.000 0.0026(11) 0.000
O1 0.0638(16) 0.0645(19) 0.091(2) 0.0426(17) -0.0439(15) -0.0322(15)
O2 0.0411(11) 0.0472(13) 0.0427(12) 0.0112(11) -0.0196(9) -0.0114(11)
O3 0.0154(7) 0.0243(9) 0.0279(8) -0.0050(7) 0.0019(6) 0.0032(7)
O4 0.0163(7) 0.0301(10) 0.0281(8) -0.0111(8) 0.0048(6) -0.0022(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.531(3) . ?
C1 C10 1.545(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.528(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O4 1.427(3) . ?
C3 O3 1.429(3) . ?
C3 C4 1.517(3) . ?
C4 C5 1.532(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.534(3) . ?
C5 C10 1.554(3) . ?
C5 H5 0.9800 . ?
C6 C7 1.523(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.531(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C14 1.519(3) . ?
C8 C9 1.553(3) . ?
C8 H8 0.9800 . ?
C9 C11 1.542(3) . ?
C9 C10 1.565(3) . ?
C9 H9 0.9800 . ?
C10 C19 1.542(3) . ?
C11 C12 1.554(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.539(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C18 1.540(3) . ?
C13 C14 1.549(3) . ?
C13 C17 1.560(3) . ?
C14 C15 1.532(3) . ?
C14 H14 0.9800 . ?
C15 C16 1.541(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.563(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C20 1.544(3) . ?
C17 H17 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.524(3) . ?
C20 C22 1.547(3) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.536(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.505(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 O1 1.189(4) . ?
C24 O2 1.329(3) . ?
C25 O2 1.440(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 O4 1.436(3) . ?
C26 C28 1.526(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 O3 1.431(3) . ?
C27 C28 1.533(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C26 1.526(3) 2_757 ?
C28 C27 1.533(3) 2_757 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 114.96(19) . . ?
C2 C1 H1A 108.5 . . ?
C10 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
C10 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C3 C2 C1 111.4(2) . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O4 C3 O3 111.04(17) . . ?
O4 C3 C4 105.54(18) . . ?
O3 C3 C4 105.8(2) . . ?
O4 C3 C2 111.5(2) . . ?
O3 C3 C2 112.26(18) . . ?
C4 C3 C2 110.28(18) . . ?
C3 C4 C5 113.68(19) . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C4 C5 C6 110.39(19) . . ?
C4 C5 C10 112.5(2) . . ?
C6 C5 C10 111.92(18) . . ?
C4 C5 H5 107.2 . . ?
C6 C5 H5 107.2 . . ?
C10 C5 H5 107.2 . . ?
C7 C6 C5 112.5(2) . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 C8 110.92(19) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.0 . . ?
C14 C8 C7 111.45(18) . . ?
C14 C8 C9 109.89(18) . . ?
C7 C8 C9 110.84(17) . . ?
C14 C8 H8 108.2 . . ?
C7 C8 H8 108.2 . . ?
C9 C8 H8 108.2 . . ?
C11 C9 C8 111.45(17) . . ?
C11 C9 C10 114.41(18) . . ?
C8 C9 C10 111.01(18) . . ?
C11 C9 H9 106.5 . . ?
C8 C9 H9 106.5 . . ?
C10 C9 H9 106.5 . . ?
C19 C10 C1 106.38(18) . . ?
C19 C10 C5 109.4(2) . . ?
C1 C10 C5 107.57(17) . . ?
C19 C10 C9 111.06(18) . . ?
C1 C10 C9 113.0(2) . . ?
C5 C10 C9 109.35(17) . . ?
C9 C11 C12 113.58(18) . . ?
C9 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
C9 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C13 C12 C11 110.83(19) . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 C18 110.34(18) . . ?
C12 C13 C14 106.40(17) . . ?
C18 C13 C14 112.37(19) . . ?
C12 C13 C17 117.2(2) . . ?
C18 C13 C17 110.14(17) . . ?
C14 C13 C17 99.97(16) . . ?
C8 C14 C15 117.1(2) . . ?
C8 C14 C13 114.50(17) . . ?
C15 C14 C13 104.23(17) . . ?
C8 C14 H14 106.8 . . ?
C15 C14 H14 106.8 . . ?
C13 C14 H14 106.8 . . ?
C14 C15 C16 103.22(19) . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15B 111.1 . . ?
C16 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C15 C16 C17 107.60(18) . . ?
C15 C16 H16A 110.2 . . ?
C17 C16 H16A 110.2 . . ?
C15 C16 H16B 110.2 . . ?
C17 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C20 C17 C13 119.43(18) . . ?
C20 C17 C16 110.39(18) . . ?
C13 C17 C16 103.23(18) . . ?
C20 C17 H17 107.7 . . ?
C13 C17 H17 107.7 . . ?
C16 C17 H17 107.7 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C17 114.13(19) . . ?
C21 C20 C22 109.2(2) . . ?
C17 C20 C22 109.74(18) . . ?
C21 C20 H20 107.8 . . ?
C17 C20 H20 107.8 . . ?
C22 C20 H20 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C20 113.38(19) . . ?
C23 C22 H22A 108.9 . . ?
C20 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C20 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C24 C23 C22 112.6(2) . . ?
C24 C23 H23A 109.1 . . ?
C22 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
C22 C23 H23B 109.1 . . ?
H23A C23 H23B 107.8 . . ?
O1 C24 O2 121.7(3) . . ?
O1 C24 C23 126.6(2) . . ?
O2 C24 C23 111.7(3) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O4 C26 C28 109.8(2) . . ?
O4 C26 H26A 109.7 . . ?
C28 C26 H26A 109.7 . . ?
O4 C26 H26B 109.7 . . ?
C28 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
O3 C27 C28 111.02(17) . . ?
O3 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
O3 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C26 C28 C26 110.6(3) . 2_757 ?
C26 C28 C27 107.37(12) . . ?
C26 C28 C27 110.36(13) 2_757 . ?
C26 C28 C27 110.36(13) . 2_757 ?
C26 C28 C27 107.37(12) 2_757 2_757 ?
C27 C28 C27 110.8(3) . 2_757 ?
C24 O2 C25 115.7(2) . . ?
C3 O3 C27 114.15(19) . . ?
C3 O4 C26 114.42(17) . . ?

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
C10 C1 C2 C3 55.5(3) . . . . ?
C1 C2 C3 O4 -169.78(17) . . . . ?
C1 C2 C3 O3 64.9(2) . . . . ?
C1 C2 C3 C4 -52.9(2) . . . . ?
O4 C3 C4 C5 174.86(18) . . . . ?
O3 C3 C4 C5 -67.4(2) . . . . ?
C2 C3 C4 C5 54.3(3) . . . . ?
C3 C4 C5 C6 178.54(19) . . . . ?
C3 C4 C5 C10 -55.6(3) . . . . ?
C4 C5 C6 C7 71.2(2) . . . . ?
C10 C5 C6 C7 -55.0(3) . . . . ?
C5 C6 C7 C8 55.4(3) . . . . ?
C6 C7 C8 C14 -179.19(19) . . . . ?
C6 C7 C8 C9 -56.5(2) . . . . ?
C14 C8 C9 C11 -50.0(2) . . . . ?
C7 C8 C9 C11 -173.63(19) . . . . ?
C14 C8 C9 C10 -178.79(17) . . . . ?
C7 C8 C9 C10 57.6(2) . . . . ?
C2 C1 C10 C19 -170.8(2) . . . . ?
C2 C1 C10 C5 -53.6(3) . . . . ?
C2 C1 C10 C9 67.1(3) . . . . ?
C4 C5 C10 C19 167.49(18) . . . . ?
C6 C5 C10 C19 -67.5(2) . . . . ?
C4 C5 C10 C1 52.3(2) . . . . ?
C6 C5 C10 C1 177.34(19) . . . . ?
C4 C5 C10 C9 -70.7(2) . . . . ?
C6 C5 C10 C9 54.3(2) . . . . ?
C11 C9 C10 C19 -62.2(3) . . . . ?
C8 C9 C10 C19 65.0(2) . . . . ?
C11 C9 C10 C1 57.3(3) . . . . ?
C8 C9 C10 C1 -175.54(17) . . . . ?
C11 C9 C10 C5 177.01(19) . . . . ?
C8 C9 C10 C5 -55.8(2) . . . . ?
C8 C9 C11 C12 50.6(3) . . . . ?
C10 C9 C11 C12 177.58(19) . . . . ?
C9 C11 C12 C13 -55.7(3) . . . . ?
C11 C12 C13 C18 -64.6(2) . . . . ?
C11 C12 C13 C14 57.6(2) . . . . ?
C11 C12 C13 C17 168.34(18) . . . . ?
C7 C8 C14 C15 -56.4(3) . . . . ?
C9 C8 C14 C15 -179.66(18) . . . . ?
C7 C8 C14 C13 -178.83(19) . . . . ?
C9 C8 C14 C13 57.9(2) . . . . ?
C12 C13 C14 C8 -61.4(2) . . . . ?
C18 C13 C14 C8 59.5(2) . . . . ?
C17 C13 C14 C8 176.22(18) . . . . ?
C12 C13 C14 C15 169.42(18) . . . . ?
C18 C13 C14 C15 -69.7(2) . . . . ?
C17 C13 C14 C15 47.0(2) . . . . ?
C8 C14 C15 C16 -163.67(18) . . . . ?
C13 C14 C15 C16 -36.1(2) . . . . ?
C14 C15 C16 C17 10.9(2) . . . . ?
C12 C13 C17 C20 83.9(3) . . . . ?
C18 C13 C17 C20 -43.3(3) . . . . ?
C14 C13 C17 C20 -161.7(2) . . . . ?
C12 C13 C17 C16 -153.15(19) . . . . ?
C18 C13 C17 C16 79.7(2) . . . . ?
C14 C13 C17 C16 -38.8(2) . . . . ?
C15 C16 C17 C20 146.59(19) . . . . ?
C15 C16 C17 C13 17.8(2) . . . . ?
C13 C17 C20 C21 -55.5(3) . . . . ?
C16 C17 C20 C21 -174.8(2) . . . . ?
C13 C17 C20 C22 -178.5(2) . . . . ?
C16 C17 C20 C22 62.2(3) . . . . ?
C21 C20 C22 C23 78.2(3) . . . . ?
C17 C20 C22 C23 -156.0(2) . . . . ?
C20 C22 C23 C24 74.9(3) . . . . ?
C22 C23 C24 O1 11.1(4) . . . . ?
C22 C23 C24 O2 -168.0(2) . . . . ?
O4 C26 C28 C26 175.5(2) . . . 2_757 ?
O4 C26 C28 C27 55.0(2) . . . . ?
O4 C26 C28 C27 -65.9(2) . . . 2_757 ?
O3 C27 C28 C26 -54.6(3) . . . . ?
O3 C27 C28 C26 -175.2(2) . . . 2_757 ?
O3 C27 C28 C27 65.96(16) . . . 2_757 ?
O1 C24 O2 C25 0.8(5) . . . . ?
C23 C24 O2 C25 180.0(3) . . . . ?
O4 C3 O3 C27 -53.7(2) . . . . ?
C4 C3 O3 C27 -167.76(17) . . . . ?
C2 C3 O3 C27 71.9(2) . . . . ?
C28 C27 O3 C3 55.4(3) . . . . ?
O3 C3 O4 C26 55.0(3) . . . . ?
C4 C3 O4 C26 169.25(19) . . . . ?
C2 C3 O4 C26 -71.0(2) . . . . ?
C28 C26 O4 C3 -57.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.044