data_roch2a-orh 


_symmetry_space_group_name_hall   'P 2ac 2ab'
#Added by publCIF




_cell_special_details   ?
#Added by publCIF

# TEXT

_publ_section_references
;
Sheldrick, G. M. (1996). <i>SADABS</i>. University of G\"ottingen, Germany.

Sheldrick, G. M. (1997). <i>SHELXL97</i>. University of G\"ottingen, Germany.

Bruker (2006). <i>SAINT</i>. Bruker Analytical X-ray Instruments Inc., Madison,
Wisconsin, USA.

Bruker (2006). <i>APEX2</i>. Bruker Analytical X-ray Instruments Inc., Madison,
Wisconsin, USA.

Dolmanov, O. V., <i>et al.</i> (2009). OLEX2: A complete structure solution,
refinement and analysis program. J. Appl. Cryst. 42, 339-341 (2009).
;

#==============================================================================



_audit_update_record
;
2011-02-01 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C28 H28 O8' 
_chemical_formula_sum 
 'C28 H28 O8' 
_chemical_formula_weight          492.50
_chemical_absolute_configuration  'ad'       
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    'P 21 21 21' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 '-x+1/2, -y, z+1/2' 
 
_cell_length_a                    6.3478(2) 
_cell_length_b                    12.4544(4) 
_cell_length_c                    30.1079(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2380.27(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     9257 
_cell_measurement_theta_min       13.744 
_cell_measurement_theta_max       131.926 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.199 
_exptl_crystal_size_mid           0.079 
_exptl_crystal_size_min           0.057 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.374 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1040 
_exptl_absorpt_coefficient_mu     0.835 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6859 
_exptl_absorpt_correction_T_max   0.7528 
_exptl_absorpt_process_details    'SADABS (Sheldrick, 1996)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker Proteum-R' 
_diffrn_measurement_method        '\f & \w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  0 
_diffrn_standards_interval_time   0 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             120163 
_diffrn_reflns_av_R_equivalents   0.0331 
_diffrn_reflns_av_sigmaI/netI     0.0099 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -35 
_diffrn_reflns_limit_l_max        35 
_diffrn_reflns_theta_min          3.84 
_diffrn_reflns_theta_max          66.23 
_reflns_number_total              4168 
_reflns_number_gt                 4141 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'APEX2 (Bruker, 2006)' 
_computing_cell_refinement        'SAINT (Bruker, 2006)' 
_computing_data_reduction         'SAINT (Bruker, 2006)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'OLEX2 (Dolmanov, et al. 2009)' 
_computing_publication_material   ? 
 
_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.

The crystallized compound was known to be a single enantiomer with >98%ee
separated by chiral chromatography. The absolute structure was determined
unambiguously from the crystal data alone, with all relevant indicators of
correctness in agreement. Upon completion of refinement with XL, OLEX2
calculates and outputs values for these parameters. This output is given
here:

Bijvoet pair analysis using Gaussian distribution Bijvoet pairs (all): 1742
Bijvoet pairs (used): 1737 Bijvoet pairs coverage: 0.99 G: 1.01(3) P2(true):
1.000 P3(true): 1.000 P3(false): 0.000 P3(racemic twin): 0.000 Hooft y:
-0.005(15) Flack x: -0.03(11)

CheckCIF alerts and response:

Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       4.52
 Ratio
PLAT230_ALERT_2_B Hirshfeld Test Diff for    O7     --  C28A    ..       8.28
 su   
PLAT413_ALERT_2_B Short Inter XH3 .. XHn     H17    ..  H28F    ..       1.92
 Ang. 
Alert level C
PLAT213_ALERT_2_C Atom C26B            has ADP max/min Ratio .....       3.20
 prola
PLAT222_ALERT_3_C Large Non-Solvent    H    Uiso(max)/Uso(min) ...       5.60
 Ratio

The structure includes three disordered OMe groups, each refined with its own
 occupancy free variable, and the diffuse electron densities associated with
 these disorders give rise to the level B and level C alerts.  Anisotropic
 refinement of the major and minor components C26A and C26B leads to somewhat
 prolate ellipsoids, and the riding H atoms have correspondingly large
 isotropic thermal parameters.  The short intermolecular H17 .. H28F contact is
 most likely due to imprecise positions for the three hydrogen atoms on C28B,
 which is part of a minor (23%) component of the C28 disorder. The relatively
 low electron density for the minor component atom C28B also likely gives rise
 to a slightly mis-oriented thermal ellipsoid for this atom, generating the
 Hirshfield test alert.  

 Despite the slight anomalies for these disordered groups, the chemical
 characteristics of interest for this research, the regio- and stereochemistry,
 are unambiguous.
; 
 
_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^)+(0.0333P)^2^+0.5417P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.03(11) 
_refine_ls_number_reflns          4168 
_refine_ls_number_parameters      367 
_refine_ls_number_restraints      13 
_refine_ls_R_factor_all           0.0238 
_refine_ls_R_factor_gt            0.0237 
_refine_ls_wR_factor_ref          0.0614 
_refine_ls_wR_factor_gt           0.0613 
_refine_ls_goodness_of_fit_ref    1.036 
_refine_ls_restrained_S_all       1.038 
_refine_ls_shift/su_max           0.002 
_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 
O2 O 0.63728(13) 0.45064(6) 0.32457(2) 0.01780(17) Uani 1 1 d . . . 
O3 O 0.13731(13) 0.52418(7) 0.37597(3) 0.02269(18) Uani 1 1 d . . . 
H3 H 0.0785 0.5843 0.3784 0.034 Uiso 1 1 calc R . . 
O1 O 1.13444(13) 0.63226(7) 0.23874(3) 0.02269(18) Uani 1 1 d . . . 
O6 O 0.60473(17) 0.83364(7) 0.31928(3) 0.0327(2) Uani 1 1 d . . . 
O4 O 0.28545(14) 0.72388(7) 0.35232(3) 0.02514(19) Uani 1 1 d . . . 
H4 H 0.3497 0.7816 0.3473 0.038 Uiso 1 1 calc R . . 
O7 O 0.28132(17) 0.00827(7) 0.37268(3) 0.0366(2) Uani 1 1 d D . . 
O8A O 0.6000(12) 0.7690(9) 0.4474(3) 0.0379(15) Uani 0.60(3) 1 d P A 1 
O5 O 0.86467(16) 0.69235(8) 0.41110(3) 0.0346(2) Uani 1 1 d . A . 
C16 C 0.4986(2) 0.35964(12) 0.53217(4) 0.0340(3) Uani 1 1 d . . . 
H16 H 0.4800 0.3289 0.5608 0.041 Uiso 1 1 calc R . . 
C17 C 0.6947(3) 0.39232(15) 0.51847(5) 0.0464(4) Uani 1 1 d . . . 
H17 H 0.8119 0.3850 0.5378 0.056 Uiso 1 1 calc R . . 
C11 C 0.59038(18) 0.50155(9) 0.40315(4) 0.0169(2) Uani 1 1 d . . . 
H11 H 0.7457 0.5023 0.3977 0.020 Uiso 1 1 calc R . . 
C18 C 0.7226(2) 0.43616(12) 0.47635(4) 0.0324(3) Uani 1 1 d . . . 
H18 H 0.8594 0.4576 0.4671 0.039 Uiso 1 1 calc R . . 
C24 C 0.56519(19) 0.26001(10) 0.38010(4) 0.0201(2) Uani 1 1 d . B . 
H24 H 0.6999 0.2841 0.3896 0.024 Uiso 1 1 calc R . . 
C1 C 1.2536(2) 0.72764(10) 0.23044(4) 0.0245(3) Uani 1 1 d . . . 
H1C H 1.2801 0.7649 0.2586 0.037 Uiso 1 1 calc R . . 
H1A H 1.1741 0.7749 0.2105 0.037 Uiso 1 1 calc R . . 
H1B H 1.3881 0.7085 0.2166 0.037 Uiso 1 1 calc R . . 
C7 C 0.87442(19) 0.54562(9) 0.28002(4) 0.0182(2) Uani 1 1 d . . . 
H7 H 0.9316 0.4789 0.2706 0.022 Uiso 1 1 calc R . . 
C9 C 0.31375(18) 0.53313(9) 0.34756(4) 0.0188(2) Uani 1 1 d . . . 
H9 H 0.2726 0.5249 0.3157 0.023 Uiso 1 1 calc R . . 
C10 C 0.48211(18) 0.45127(9) 0.36091(4) 0.0166(2) Uani 1 1 d . B . 
C12 C 0.51390(19) 0.62024(9) 0.40371(4) 0.0188(2) Uani 1 1 d . A . 
H12 H 0.3914 0.6256 0.4245 0.023 Uiso 1 1 calc R . . 
C13 C 0.55406(19) 0.44888(9) 0.44792(4) 0.0179(2) Uani 1 1 d . . . 
C15 C 0.3287(2) 0.37175(11) 0.50404(4) 0.0279(3) Uani 1 1 d . . . 
H15 H 0.1928 0.3491 0.5133 0.033 Uiso 1 1 calc R . . 
C22 C 0.3203(2) 0.11561(10) 0.36849(4) 0.0239(3) Uani 1 1 d . B . 
C21 C 0.1751(2) 0.18818(10) 0.35177(4) 0.0248(3) Uani 1 1 d . . . 
H21 H 0.0417 0.1637 0.3417 0.030 Uiso 1 1 calc R B . 
C6 C 0.70610(18) 0.54864(9) 0.30923(4) 0.0168(2) Uani 1 1 d . C . 
C23 C 0.5177(2) 0.15195(10) 0.38233(4) 0.0225(3) Uani 1 1 d . . . 
H23 H 0.6192 0.1025 0.3932 0.027 Uiso 1 1 calc R B . 
C3 C 0.8684(2) 0.73938(10) 0.27651(4) 0.0211(2) Uani 1 1 d . . . 
H3A H 0.9226 0.8048 0.2650 0.025 Uiso 1 1 calc R C . 
C5 C 0.61287(19) 0.64468(9) 0.32260(4) 0.0185(2) Uani 1 1 d . . . 
C2 C 0.95809(19) 0.64148(10) 0.26473(4) 0.0188(2) Uani 1 1 d . C . 
C19 C 0.41916(19) 0.33482(9) 0.36415(3) 0.0176(2) Uani 1 1 d . . . 
C8 C 0.43202(18) 0.63886(9) 0.35552(4) 0.0194(2) Uani 1 1 d . A . 
C25 C 0.6803(2) 0.69747(10) 0.41900(4) 0.0224(3) Uani 1 1 d . . . 
C20 C 0.2249(2) 0.29713(10) 0.34979(4) 0.0218(3) Uani 1 1 d . B . 
H20 H 0.1242 0.3464 0.3384 0.026 Uiso 1 1 calc R . . 
C4 C 0.6981(2) 0.73928(10) 0.30537(4) 0.0215(2) Uani 1 1 d . C . 
C14 C 0.3552(2) 0.41686(10) 0.46227(4) 0.0244(3) Uani 1 1 d . . . 
H14 H 0.2369 0.4260 0.4433 0.029 Uiso 1 1 calc R . . 
C28A C 0.0882(3) -0.03279(14) 0.35960(8) 0.0402(6) Uani 0.772(4) 1 d PDU B 1 
H28B H 0.0824 -0.1097 0.3665 0.060 Uiso 0.772(4) 1 calc PR B 1 
H28A H 0.0702 -0.0223 0.3276 0.060 Uiso 0.772(4) 1 calc PR B 1 
H28C H -0.0248 0.0046 0.3755 0.060 Uiso 0.772(4) 1 calc PR B 1 
C27A C 0.6151(3) 0.92590(12) 0.28969(6) 0.0284(5) Uani 0.809(4) 1 d P C 1 
H27C H 0.7575 0.9562 0.2904 0.043 Uiso 0.809(4) 1 calc PR C 1 
H27B H 0.5137 0.9803 0.2994 0.043 Uiso 0.809(4) 1 calc PR C 1 
H27A H 0.5810 0.9033 0.2594 0.043 Uiso 0.809(4) 1 calc PR C 1 
C27B C 0.7203(15) 0.9325(6) 0.3066(3) 0.0284(5) Uani 0.191(4) 1 d P C 2 
H27E H 0.8609 0.9315 0.3201 0.043 Uiso 0.191(4) 1 calc PR C 2 
H27F H 0.6429 0.9956 0.3172 0.043 Uiso 0.191(4) 1 calc PR C 2 
H27D H 0.7336 0.9359 0.2742 0.043 Uiso 0.191(4) 1 calc PR C 2 
C26A C 0.7445(11) 0.8444(10) 0.4661(4) 0.059(2) Uani 0.60(3) 1 d P A 1 
H26B H 0.8594 0.8057 0.4809 0.088 Uiso 0.60(3) 1 calc PR A 1 
H26C H 0.6710 0.8894 0.4879 0.088 Uiso 0.60(3) 1 calc PR A 1 
H26A H 0.8024 0.8897 0.4425 0.088 Uiso 0.60(3) 1 calc PR A 1 
C28B C 0.3506(12) -0.0556(5) 0.4031(2) 0.0358(18) Uani 0.228(4) 1 d PDU B 2 
H28E H 0.2468 -0.1123 0.4085 0.054 Uiso 0.228(4) 1 calc PR B 2 
H28F H 0.3740 -0.0150 0.4306 0.054 Uiso 0.228(4) 1 calc PR B 2 
H28D H 0.4835 -0.0878 0.3933 0.054 Uiso 0.228(4) 1 calc PR B 2 
O8B O 0.588(2) 0.7847(10) 0.4360(6) 0.043(2) Uani 0.40(3) 1 d P A 2 
C26B C 0.741(2) 0.8716(9) 0.4494(8) 0.074(3) Uani 0.40(3) 1 d P A 2 
H26E H 0.8468 0.8416 0.4697 0.112 Uiso 0.40(3) 1 calc PR A 2 
H26F H 0.6649 0.9296 0.4644 0.112 Uiso 0.40(3) 1 calc PR A 2 
H26D H 0.8116 0.8999 0.4229 0.112 Uiso 0.40(3) 1 calc PR A 2 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
O2 0.0202(4) 0.0168(4) 0.0164(4) 0.0016(3) 0.0037(3) 0.0000(3) 
O3 0.0162(4) 0.0276(4) 0.0244(4) 0.0038(3) 0.0039(3) 0.0026(3) 
O1 0.0223(4) 0.0221(4) 0.0237(4) 0.0037(3) 0.0093(4) 0.0013(4) 
O6 0.0459(6) 0.0176(4) 0.0344(5) 0.0044(4) 0.0212(5) 0.0052(4) 
O4 0.0232(4) 0.0229(4) 0.0294(4) 0.0056(4) 0.0053(4) 0.0084(4) 
O7 0.0516(6) 0.0207(4) 0.0376(5) 0.0013(4) -0.0002(5) -0.0083(4) 
O8A 0.0295(17) 0.044(3) 0.040(3) -0.025(2) -0.0018(16) -0.0019(17) 
O5 0.0276(5) 0.0330(5) 0.0434(6) -0.0113(4) 0.0080(4) -0.0090(4) 
C16 0.0411(8) 0.0420(8) 0.0189(6) 0.0104(6) 0.0057(6) 0.0115(7) 
C17 0.0318(8) 0.0819(12) 0.0256(7) 0.0175(8) -0.0040(6) 0.0110(8) 
C11 0.0165(5) 0.0174(5) 0.0169(5) -0.0001(4) 0.0005(4) 0.0006(5) 
C18 0.0225(6) 0.0514(9) 0.0233(6) 0.0066(6) 0.0001(5) 0.0014(6) 
C24 0.0199(6) 0.0241(6) 0.0165(5) -0.0006(5) 0.0007(4) -0.0005(5) 
C1 0.0226(6) 0.0263(6) 0.0247(6) 0.0042(5) 0.0051(5) -0.0020(5) 
C7 0.0195(6) 0.0188(5) 0.0163(5) 0.0009(4) -0.0001(5) 0.0022(5) 
C9 0.0156(5) 0.0234(6) 0.0173(5) 0.0027(5) 0.0004(4) 0.0010(5) 
C10 0.0149(5) 0.0211(6) 0.0137(5) 0.0006(4) 0.0024(4) -0.0002(5) 
C12 0.0210(6) 0.0171(6) 0.0182(5) 0.0004(4) 0.0044(5) 0.0005(5) 
C13 0.0214(6) 0.0172(5) 0.0152(5) -0.0018(4) 0.0007(5) 0.0033(5) 
C15 0.0303(7) 0.0308(6) 0.0225(6) 0.0017(5) 0.0079(5) -0.0012(6) 
C22 0.0306(7) 0.0199(6) 0.0211(6) -0.0009(5) 0.0029(5) -0.0031(5) 
C21 0.0244(6) 0.0268(6) 0.0233(6) -0.0003(5) -0.0028(5) -0.0056(5) 
C6 0.0179(5) 0.0188(5) 0.0136(5) 0.0030(4) -0.0015(4) 0.0009(5) 
C23 0.0259(6) 0.0218(6) 0.0198(6) 0.0019(5) 0.0016(5) 0.0032(5) 
C3 0.0249(6) 0.0184(5) 0.0199(5) 0.0035(4) 0.0030(5) -0.0011(5) 
C5 0.0185(5) 0.0213(6) 0.0156(5) 0.0019(4) 0.0008(5) 0.0020(5) 
C2 0.0184(6) 0.0238(6) 0.0142(5) 0.0025(5) 0.0015(4) 0.0006(5) 
C19 0.0204(6) 0.0201(6) 0.0123(5) 0.0002(4) 0.0025(4) -0.0009(5) 
C8 0.0185(6) 0.0198(6) 0.0199(6) 0.0020(5) 0.0028(5) 0.0047(5) 
C25 0.0292(7) 0.0203(6) 0.0177(5) 0.0005(5) 0.0012(5) 0.0002(5) 
C20 0.0230(6) 0.0236(6) 0.0188(6) 0.0009(5) -0.0035(5) -0.0008(5) 
C4 0.0267(6) 0.0179(6) 0.0198(5) 0.0010(5) 0.0027(5) 0.0028(5) 
C14 0.0235(6) 0.0303(6) 0.0196(6) 0.0012(5) 0.0002(5) -0.0012(5) 
C28A 0.0288(10) 0.0215(9) 0.0704(14) -0.0081(9) 0.0067(10) -0.0027(7) 
C27A 0.0347(11) 0.0179(7) 0.0325(10) 0.0067(7) 0.0084(8) 0.0052(7) 
C27B 0.0347(11) 0.0179(7) 0.0325(10) 0.0067(7) 0.0084(8) 0.0052(7) 
C26A 0.052(3) 0.055(4) 0.069(4) -0.044(3) 0.008(3) -0.018(2) 
C28B 0.054(4) 0.023(3) 0.030(3) 0.000(2) 0.002(3) -0.001(3) 
O8B 0.053(3) 0.019(2) 0.056(6) -0.020(3) -0.012(3) 0.0084(18) 
C26B 0.099(6) 0.024(3) 0.101(9) -0.021(4) -0.037(6) -0.011(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 
O2 C6 1.3762(13) . ? 
O2 C10 1.4722(13) . ? 
O3 C9 1.4138(14) . ? 
O3 H3 0.8400 . ? 
O1 C2 1.3706(14) . ? 
O1 C1 1.4303(15) . ? 
O6 C4 1.3811(15) . ? 
O6 C27A 1.4553(18) . ? 
O6 C27B 1.484(7) . ? 
O4 C8 1.4128(14) . ? 
O4 H4 0.8400 . ? 
O7 C28B 1.290(6) . ? 
O7 C22 1.3654(15) . ? 
O7 C28A 1.386(2) . ? 
O8A C25 1.336(8) . ? 
O8A C26A 1.429(11) . ? 
O5 C25 1.1958(17) . ? 
C16 C17 1.373(2) . ? 
C16 C15 1.379(2) . ? 
C16 H16 0.9500 . ? 
C17 C18 1.392(2) . ? 
C17 H17 0.9500 . ? 
C11 C13 1.5165(15) . ? 
C11 C12 1.5560(15) . ? 
C11 C10 1.5755(15) . ? 
C11 H11 1.0000 . ? 
C18 C13 1.3794(18) . ? 
C18 H18 0.9500 . ? 
C24 C23 1.3808(17) . ? 
C24 C19 1.3994(17) . ? 
C24 H24 0.9500 . ? 
C1 H1C 0.9800 . ? 
C1 H1A 0.9800 . ? 
C1 H1B 0.9800 . ? 
C7 C6 1.3843(17) . ? 
C7 C2 1.3854(17) . ? 
C7 H7 0.9500 . ? 
C9 C10 1.5307(16) . ? 
C9 C8 1.5346(16) . ? 
C9 H9 1.0000 . ? 
C10 C19 1.5075(16) . ? 
C12 C25 1.5012(17) . ? 
C12 C8 1.5583(16) . ? 
C12 H12 1.0000 . ? 
C13 C14 1.3924(18) . ? 
C15 C14 1.3877(18) . ? 
C15 H15 0.9500 . ? 
C22 C21 1.3856(18) . ? 
C22 C23 1.3961(19) . ? 
C21 C20 1.3944(17) . ? 
C21 H21 0.9500 . ? 
C6 C5 1.3939(16) . ? 
C23 H23 0.9500 . ? 
C3 C4 1.3871(17) . ? 
C3 C2 1.3917(17) . ? 
C3 H3A 0.9500 . ? 
C5 C4 1.3963(17) . ? 
C5 C8 1.5186(16) . ? 
C19 C20 1.3887(17) . ? 
C25 O8B 1.335(12) . ? 
C20 H20 0.9500 . ? 
C14 H14 0.9500 . ? 
C28A H28B 0.9800 . ? 
C28A H28A 0.9800 . ? 
C28A H28C 0.9800 . ? 
C27A H27C 0.9800 . ? 
C27A H27B 0.9800 . ? 
C27A H27A 0.9800 . ? 
C27B H27E 0.9800 . ? 
C27B H27F 0.9800 . ? 
C27B H27D 0.9800 . ? 
C26A H26B 0.9800 . ? 
C26A H26C 0.9800 . ? 
C26A H26A 0.9800 . ? 
C28B H28E 0.9800 . ? 
C28B H28F 0.9800 . ? 
C28B H28D 0.9800 . ? 
O8B C26B 1.510(18) . ? 
C26B H26E 0.9800 . ? 
C26B H26F 0.9800 . ? 
C26B H26D 0.9800 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C6 O2 C10 117.19(8) . . ? 
C9 O3 H3 109.5 . . ? 
C2 O1 C1 117.51(9) . . ? 
C4 O6 C27A 117.83(10) . . ? 
C4 O6 C27B 114.6(3) . . ? 
C27A O6 C27B 33.4(4) . . ? 
C8 O4 H4 109.5 . . ? 
C28B O7 C22 127.4(3) . . ? 
C28B O7 C28A 106.0(3) . . ? 
C22 O7 C28A 119.70(13) . . ? 
C25 O8A C26A 116.4(6) . . ? 
C17 C16 C15 119.47(12) . . ? 
C17 C16 H16 120.3 . . ? 
C15 C16 H16 120.3 . . ? 
C16 C17 C18 120.35(13) . . ? 
C16 C17 H17 119.8 . . ? 
C18 C17 H17 119.8 . . ? 
C13 C11 C12 110.73(9) . . ? 
C13 C11 C10 118.63(9) . . ? 
C12 C11 C10 104.48(9) . . ? 
C13 C11 H11 107.5 . . ? 
C12 C11 H11 107.5 . . ? 
C10 C11 H11 107.5 . . ? 
C13 C18 C17 120.77(13) . . ? 
C13 C18 H18 119.6 . . ? 
C17 C18 H18 119.6 . . ? 
C23 C24 C19 121.40(11) . . ? 
C23 C24 H24 119.3 . . ? 
C19 C24 H24 119.3 . . ? 
O1 C1 H1C 109.5 . . ? 
O1 C1 H1A 109.5 . . ? 
H1C C1 H1A 109.5 . . ? 
O1 C1 H1B 109.5 . . ? 
H1C C1 H1B 109.5 . . ? 
H1A C1 H1B 109.5 . . ? 
C6 C7 C2 118.92(11) . . ? 
C6 C7 H7 120.5 . . ? 
C2 C7 H7 120.5 . . ? 
O3 C9 C10 109.98(9) . . ? 
O3 C9 C8 111.14(9) . . ? 
C10 C9 C8 100.89(9) . . ? 
O3 C9 H9 111.5 . . ? 
C10 C9 H9 111.5 . . ? 
C8 C9 H9 111.5 . . ? 
O2 C10 C19 102.72(8) . . ? 
O2 C10 C9 105.99(8) . . ? 
C19 C10 C9 118.21(9) . . ? 
O2 C10 C11 108.08(9) . . ? 
C19 C10 C11 116.47(9) . . ? 
C9 C10 C11 104.59(9) . . ? 
C25 C12 C11 113.10(10) . . ? 
C25 C12 C8 115.15(10) . . ? 
C11 C12 C8 103.62(9) . . ? 
C25 C12 H12 108.2 . . ? 
C11 C12 H12 108.2 . . ? 
C8 C12 H12 108.2 . . ? 
C18 C13 C14 118.53(11) . . ? 
C18 C13 C11 118.90(11) . . ? 
C14 C13 C11 122.52(10) . . ? 
C16 C15 C14 120.38(12) . . ? 
C16 C15 H15 119.8 . . ? 
C14 C15 H15 119.8 . . ? 
O7 C22 C21 123.49(12) . . ? 
O7 C22 C23 116.90(12) . . ? 
C21 C22 C23 119.61(11) . . ? 
C22 C21 C20 119.97(12) . . ? 
C22 C21 H21 120.0 . . ? 
C20 C21 H21 120.0 . . ? 
O2 C6 C7 115.73(10) . . ? 
O2 C6 C5 121.96(10) . . ? 
C7 C6 C5 122.31(11) . . ? 
C24 C23 C22 119.83(12) . . ? 
C24 C23 H23 120.1 . . ? 
C22 C23 H23 120.1 . . ? 
C4 C3 C2 118.54(11) . . ? 
C4 C3 H3A 120.7 . . ? 
C2 C3 H3A 120.7 . . ? 
C6 C5 C4 116.90(10) . . ? 
C6 C5 C8 117.94(10) . . ? 
C4 C5 C8 125.14(10) . . ? 
O1 C2 C7 115.51(10) . . ? 
O1 C2 C3 123.58(11) . . ? 
C7 C2 C3 120.89(10) . . ? 
C20 C19 C24 118.04(11) . . ? 
C20 C19 C10 122.72(10) . . ? 
C24 C19 C10 119.16(10) . . ? 
O4 C8 C5 114.67(9) . . ? 
O4 C8 C9 108.07(9) . . ? 
C5 C8 C9 107.98(9) . . ? 
O4 C8 C12 113.25(9) . . ? 
C5 C8 C12 111.27(9) . . ? 
C9 C8 C12 100.43(9) . . ? 
O5 C25 O8B 123.3(6) . . ? 
O5 C25 O8A 122.5(3) . . ? 
O8B C25 O8A 17.3(7) . . ? 
O5 C25 C12 126.40(11) . . ? 
O8B C25 C12 109.3(6) . . ? 
O8A C25 C12 110.8(3) . . ? 
C19 C20 C21 121.12(12) . . ? 
C19 C20 H20 119.4 . . ? 
C21 C20 H20 119.4 . . ? 
O6 C4 C3 121.57(10) . . ? 
O6 C4 C5 116.05(10) . . ? 
C3 C4 C5 122.37(11) . . ? 
C15 C14 C13 120.48(12) . . ? 
C15 C14 H14 119.8 . . ? 
C13 C14 H14 119.8 . . ? 
O7 C28A H28B 109.5 . . ? 
O7 C28A H28A 109.5 . . ? 
O7 C28A H28C 109.5 . . ? 
O6 C27A H27C 109.5 . . ? 
O6 C27A H27B 109.5 . . ? 
O6 C27A H27A 109.5 . . ? 
O6 C27B H27E 109.5 . . ? 
O6 C27B H27F 109.5 . . ? 
H27E C27B H27F 109.5 . . ? 
O6 C27B H27D 109.5 . . ? 
H27E C27B H27D 109.5 . . ? 
H27F C27B H27D 109.5 . . ? 
O7 C28B H28E 109.5 . . ? 
O7 C28B H28F 109.5 . . ? 
H28E C28B H28F 109.5 . . ? 
O7 C28B H28D 109.5 . . ? 
H28E C28B H28D 109.5 . . ? 
H28F C28B H28D 109.5 . . ? 
C25 O8B C26B 113.8(11) . . ? 
O8B C26B H26E 109.5 . . ? 
O8B C26B H26F 109.5 . . ? 
H26E C26B H26F 109.5 . . ? 
O8B C26B H26D 109.5 . . ? 
H26E C26B H26D 109.5 . . ? 
H26F C26B H26D 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              66.23 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.220 
_refine_diff_density_min   -0.175 
_refine_diff_density_rms    0.028