 
data_03hur337
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C56 H40 O16'
_chemical_formula_weight          968.88
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    7.520(5)
_cell_length_b                    13.984(4)
_cell_length_c                    21.530(2)
_cell_angle_alpha                 102.71(3)
_cell_angle_beta                  93.44(8)
_cell_angle_gamma                 94.76(2)
_cell_volume                      2193.8(16)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        colourless
_exptl_crystal_colour             block
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.467
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1008
_exptl_absorpt_coefficient_mu     0.108
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   0.9808
_exptl_absorpt_correction_T_max   0.9850

 

 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             5033
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.3666
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          24.78
_reflns_number_total              5033
_reflns_number_gt                 1412
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        0
_refine_ls_number_reflns          5033
_refine_ls_number_parameters      655
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1410
_refine_ls_R_factor_gt            0.0485
_refine_ls_wR_factor_ref          0.1039
_refine_ls_wR_factor_gt           0.0723
_refine_ls_goodness_of_fit_ref    0.523
_refine_ls_restrained_S_all       0.523
_refine_ls_shift/su_max           0.027
_refine_ls_shift/su_mean          0.005
 
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 1.0354(5) 0.1220(3) 0.1787(2) 0.0301(11) Uani 1 1 d . . .
O2 O 0.4470(5) 0.3893(3) 0.2108(2) 0.0290(11) Uani 1 1 d . . .
O3 O 0.6319(5) 0.0918(3) 0.4079(2) 0.0279(11) Uani 1 1 d . . .
O4 O 0.2363(5) 0.3978(3) 0.3510(2) 0.0323(12) Uani 1 1 d . . .
O5 O 0.9320(4) 0.0117(3) 0.3051(2) 0.0269(11) Uani 1 1 d . . .
O6 O 0.2800(5) 0.4606(3) 0.0826(2) 0.0321(12) Uani 1 1 d . . .
O7 O 0.6623(5) 0.1683(3) 0.1931(2) 0.0362(12) Uani 1 1 d . . .
O8 O 0.4187(5) -0.0438(4) 0.2636(2) 0.0359(12) Uani 1 1 d . . .
O9 O 0.8252(6) 0.4415(3) 0.1063(2) 0.0434(14) Uani 1 1 d . . .
O10 O 0.4784(5) 0.6614(3) 0.1991(2) 0.0404(13) Uani 1 1 d . . .
O11 O 0.7449(5) -0.1975(4) 0.3823(2) 0.0415(13) Uani 1 1 d . . .
O12 O 0.7902(6) 0.4167(4) 0.3873(2) 0.0468(14) Uani 1 1 d . . .
O13 O 0.5747(5) 0.0164(3) 0.1345(2) 0.0422(13) Uani 1 1 d . . .
C1 C 0.3930(8) 0.5178(5) 0.1301(3) 0.0230(16) Uani 1 1 d . . .
O17 O 0.3444(5) 0.6847(4) 0.3362(2) 0.0571(17) Uani 1 1 d . . .
O14 O 0.1029(5) 0.5732(4) 0.3078(2) 0.0411(14) Uani 1 1 d . . .
C3 C 0.6994(8) -0.0722(5) 0.2326(3) 0.0291(17) Uani 1 1 d . . .
H3 H 0.6713 -0.1042 0.1863 0.035 Uiso 1 1 calc R . .
C4 C 0.3005(7) 0.4324(4) 0.2441(3) 0.0259(17) Uani 1 1 d . . .
C5 C 0.5887(7) 0.0237(5) 0.3530(3) 0.0222(16) Uani 1 1 d . . .
O15 O 1.0727(5) -0.1776(3) 0.1265(2) 0.0434(13) Uani 1 1 d . . .
C6 C 0.4948(8) 0.3887(5) 0.4221(3) 0.0297(18) Uani 1 1 d . . .
C7 C 0.6814(8) 0.0396(4) 0.2442(3) 0.0214(16) Uani 1 1 d . . .
C8 C 1.1284(7) -0.0188(5) 0.1041(3) 0.0277(18) Uani 1 1 d . . .
C9 C 0.5465(8) 0.3953(5) 0.0412(3) 0.0236(16) Uani 1 1 d . . .
C10 C 0.3548(9) 0.4133(5) 0.3090(3) 0.0349(19) Uani 1 1 d . . .
C11 C 1.0012(7) -0.0396(5) 0.2003(3) 0.0265(17) Uani 1 1 d . . .
C12 C 0.6308(8) 0.0710(6) 0.1846(3) 0.0310(18) Uani 1 1 d . . .
C13 C 0.3514(7) 0.5415(5) 0.2487(3) 0.0317(18) Uani 1 1 d . . .
C14 C 0.3230(8) 0.5861(5) 0.1861(4) 0.0352(19) Uani 1 1 d . . .
C15 C 0.6102(8) -0.0710(5) 0.3434(3) 0.0264(16) Uani 1 1 d . . .
C16 C 0.6258(9) 0.4112(5) 0.3753(3) 0.0312(18) Uani 1 1 d . . .
C17 C 1.2034(7) -0.0534(5) 0.0470(3) 0.0318(18) Uani 1 1 d . . .
H17 H 1.2183 -0.1213 0.0330 0.038 Uiso 1 1 calc R . .
C18 C 0.5349(8) 0.4202(5) 0.3174(3) 0.0293(17) Uani 1 1 d . . .
C19 C 0.9023(7) -0.0736(5) 0.2521(3) 0.0274(17) Uani 1 1 d . . .
H19 H 0.9365 -0.1367 0.2618 0.033 Uiso 1 1 calc R . .
C20 C 0.5562(8) 0.3709(5) 0.4803(3) 0.0346(19) Uani 1 1 d . . .
H20 H 0.6816 0.3752 0.4906 0.042 Uiso 1 1 calc R . .
C21 C 0.6934(8) 0.0554(5) 0.4595(3) 0.0280(17) Uani 1 1 d . . .
C22 C 0.2555(8) 0.3486(6) -0.0175(3) 0.043(2) Uani 1 1 d . . .
H22 H 0.1304 0.3543 -0.0199 0.052 Uiso 1 1 calc R . .
C23 C 0.6631(9) 0.4520(5) 0.0960(3) 0.0309(18) Uani 1 1 d . . .
C24 C 0.7801(7) 0.0920(6) 0.5714(3) 0.038(2) Uani 1 1 d . . .
H24 H 0.7973 0.1375 0.6116 0.045 Uiso 1 1 calc R . .
C25 C 0.5677(8) 0.5186(5) 0.1369(3) 0.0241(16) Uani 1 1 d . . .
C26 C 0.5237(8) 0.0487(5) 0.2916(3) 0.0310(17) Uani 1 1 d . . .
C27 C 0.3632(8) 0.4026(5) 0.0347(3) 0.0256(17) Uani 1 1 d . . .
C28 C 0.7235(7) -0.0432(5) 0.4519(3) 0.0278(17) Uani 1 1 d . . .
C29 C 1.0706(8) -0.0868(5) 0.1433(3) 0.0291(17) Uani 1 1 d . . .
C30 C 0.3092(8) 0.3823(5) 0.4082(3) 0.0322(18) Uani 1 1 d . . .
C31 C 0.1885(9) 0.3614(5) 0.4511(3) 0.036(2) Uani 1 1 d . . .
H31 H 0.0628 0.3584 0.4417 0.044 Uiso 1 1 calc R . .
C32 C 0.9869(8) 0.0579(5) 0.2137(3) 0.0270(17) Uani 1 1 d . . .
C33 C 0.6186(8) 0.3306(5) -0.0098(3) 0.0354(19) Uani 1 1 d . . .
H33 H 0.7437 0.3249 -0.0079 0.042 Uiso 1 1 calc R . .
C34 C 0.7197(7) 0.1224(5) 0.5167(3) 0.0335(18) Uani 1 1 d . . .
H34 H 0.6972 0.1890 0.5194 0.040 Uiso 1 1 calc R . .
C35 C 0.8766(7) 0.0834(5) 0.2716(3) 0.0244(16) Uani 1 1 d . . .
C36 C 0.6982(8) -0.1108(6) 0.3916(4) 0.037(2) Uani 1 1 d . . .
C37 C 0.5540(7) -0.1095(5) 0.2735(3) 0.0335(18) Uani 1 1 d . . .
H37 H 0.5130 -0.1815 0.2605 0.040 Uiso 1 1 calc R . .
C38 C 0.5113(9) 0.2763(5) -0.0616(3) 0.040(2) Uani 1 1 d . . .
H38 H 0.5616 0.2318 -0.0943 0.048 Uiso 1 1 calc R . .
C39 C 0.2681(9) 0.6083(5) 0.3023(3) 0.0333(18) Uani 1 1 d . . .
C40 C 0.2610(10) 0.3453(5) 0.5079(3) 0.045(2) Uani 1 1 d . . .
H40 H 0.1818 0.3320 0.5384 0.054 Uiso 1 1 calc R . .
C41 C 0.4437(9) 0.3475(5) 0.5228(3) 0.044(2) Uani 1 1 d . . .
H41 H 0.4885 0.3331 0.5615 0.053 Uiso 1 1 calc R . .
C42 C 1.1138(8) 0.0803(6) 0.1220(3) 0.037(2) Uani 1 1 d . . .
C43 C 0.7874(7) -0.0687(5) 0.5067(3) 0.0324(18) Uani 1 1 d . . .
H43 H 0.8145 -0.1348 0.5032 0.039 Uiso 1 1 calc R . .
C44 C 0.4164(8) 0.1350(5) 0.2966(3) 0.0398(19) Uani 1 1 d . . .
H44A H 0.3608 0.1354 0.2543 0.060 Uiso 1 1 calc R . .
H44B H 0.4950 0.1960 0.3128 0.060 Uiso 1 1 calc R . .
H44C H 0.3229 0.1302 0.3259 0.060 Uiso 1 1 calc R . .
C45 C 1.1599(7) 0.1450(5) 0.0840(3) 0.0292(17) Uani 1 1 d . . .
H45 H 1.1399 0.2125 0.0969 0.035 Uiso 1 1 calc R . .
C46 C 0.1528(7) 0.6302(4) 0.1744(3) 0.0372(19) Uani 1 1 d . . .
H46A H 0.1287 0.6772 0.2133 0.056 Uiso 1 1 calc R . .
H46B H 0.0537 0.5778 0.1628 0.056 Uiso 1 1 calc R . .
H46C H 0.1646 0.6644 0.1395 0.056 Uiso 1 1 calc R . .
C47 C 0.6174(8) 0.5923(5) 0.1998(3) 0.0280(17) Uani 1 1 d . . .
H47 H 0.7431 0.6242 0.2047 0.034 Uiso 1 1 calc R . .
C48 C 0.3282(9) 0.2869(5) -0.0661(3) 0.040(2) Uani 1 1 d . . .
H48 H 0.2543 0.2515 -0.1026 0.048 Uiso 1 1 calc R . .
C49 C 1.2335(9) 0.1120(5) 0.0284(4) 0.048(2) Uani 1 1 d . . .
H49 H 1.2688 0.1557 0.0023 0.057 Uiso 1 1 calc R . .
C50 C 0.5636(7) 0.5499(5) 0.2566(3) 0.0246(17) Uani 1 1 d . . .
H50 H 0.6118 0.5944 0.2982 0.030 Uiso 1 1 calc R . .
C51 C 0.1216(7) 0.3829(4) 0.2121(3) 0.0302(17) Uani 1 1 d . . .
H51A H 0.0958 0.4050 0.1727 0.045 Uiso 1 1 calc R . .
H51B H 0.0276 0.4002 0.2410 0.045 Uiso 1 1 calc R . .
H51C H 0.1254 0.3113 0.2020 0.045 Uiso 1 1 calc R . .
C52 C 1.2560(8) 0.0127(6) 0.0107(3) 0.045(2) Uani 1 1 d . . .
H52 H 1.3097 -0.0111 -0.0279 0.054 Uiso 1 1 calc R . .
C53 C 0.5917(8) 0.4421(5) 0.2552(3) 0.0321(19) Uani 1 1 d . . .
H53 H 0.7134 0.4234 0.2442 0.039 Uiso 1 1 calc R . .
C54 C 0.9099(8) 0.1868(5) 0.3130(3) 0.044(2) Uani 1 1 d . . .
H54A H 0.8436 0.1912 0.3512 0.066 Uiso 1 1 calc R . .
H54B H 0.8694 0.2339 0.2888 0.066 Uiso 1 1 calc R . .
H54C H 1.0382 0.2024 0.3258 0.066 Uiso 1 1 calc R . .
C55 C 0.8149(7) -0.0058(5) 0.5663(4) 0.038(2) Uani 1 1 d . . .
H55 H 0.8562 -0.0283 0.6026 0.046 Uiso 1 1 calc R . .
C56 C 0.6464(9) 0.2076(5) 0.1353(3) 0.053(2) Uani 1 1 d . . .
H56A H 0.6884 0.1612 0.0995 0.080 Uiso 1 1 calc R . .
H56B H 0.7193 0.2711 0.1425 0.080 Uiso 1 1 calc R . .
H56C H 0.5209 0.2168 0.1255 0.080 Uiso 1 1 calc R . .
C57 C 0.0111(8) 0.6250(5) 0.3601(3) 0.057(3) Uani 1 1 d . . .
H57A H 0.0969 0.6507 0.3974 0.085 Uiso 1 1 calc R . .
H57B H -0.0823 0.5798 0.3710 0.085 Uiso 1 1 calc R . .
H57C H -0.0435 0.6799 0.3476 0.085 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C32 1.335(7) . ?
O1 C42 1.417(7) . ?
O2 C53 1.441(7) . ?
O2 C4 1.452(6) . ?
O3 C5 1.347(7) . ?
O3 C21 1.391(7) . ?
O4 C10 1.346(7) . ?
O4 C30 1.386(7) . ?
O5 C35 1.432(7) . ?
O5 C19 1.450(7) . ?
O6 C1 1.353(7) . ?
O6 C27 1.382(7) . ?
O7 C12 1.332(8) . ?
O7 C56 1.468(7) . ?
O8 C26 1.446(7) . ?
O8 C37 1.463(7) . ?
O9 C23 1.252(6) . ?
O10 C14 1.476(7) . ?
O10 C47 1.483(7) . ?
O11 C36 1.268(8) . ?
O12 C16 1.240(7) . ?
O13 C12 1.206(7) . ?
C1 C25 1.312(7) . ?
C1 C14 1.515(8) . ?
O17 C39 1.228(7) . ?
O14 C39 1.320(7) . ?
O14 C57 1.445(7) . ?
C3 C7 1.546(8) . ?
C3 C19 1.561(8) . ?
C3 C37 1.571(7) . ?
C3 H3 1.0000 . ?
C4 C51 1.513(7) . ?
C4 C13 1.521(8) . ?
C4 C10 1.519(9) . ?
C5 C15 1.320(9) . ?
C5 C26 1.505(8) . ?
O15 C29 1.242(7) . ?
C6 C30 1.401(8) . ?
C6 C20 1.389(8) . ?
C6 C16 1.515(8) . ?
C7 C12 1.484(8) . ?
C7 C35 1.570(8) . ?
C7 C26 1.605(8) . ?
C8 C42 1.370(9) . ?
C8 C17 1.389(8) . ?
C8 C29 1.462(8) . ?
C9 C27 1.392(8) . ?
C9 C33 1.425(8) . ?
C9 C23 1.463(8) . ?
C10 C18 1.348(8) . ?
C11 C32 1.345(8) . ?
C11 C29 1.411(8) . ?
C11 C19 1.515(8) . ?
C13 C39 1.520(8) . ?
C13 C50 1.586(8) . ?
C13 C14 1.615(9) . ?
C14 C46 1.498(7) . ?
C15 C36 1.433(9) . ?
C15 C37 1.505(8) . ?
C16 C18 1.421(9) . ?
C17 C52 1.383(8) . ?
C17 H17 0.9500 . ?
C18 C53 1.515(8) . ?
C19 H19 1.0000 . ?
C20 C41 1.356(8) . ?
C20 H20 0.9500 . ?
C21 C34 1.366(8) . ?
C21 C28 1.392(9) . ?
C22 C48 1.374(9) . ?
C22 C27 1.380(8) . ?
C22 H22 0.9500 . ?
C23 C25 1.407(8) . ?
C24 C34 1.401(8) . ?
C24 C55 1.395(9) . ?
C24 H24 0.9500 . ?
C25 C47 1.516(8) . ?
C26 C44 1.495(8) . ?
C28 C43 1.377(8) . ?
C28 C36 1.420(9) . ?
C30 C31 1.391(8) . ?
C31 C40 1.381(9) . ?
C31 H31 0.9500 . ?
C32 C35 1.533(8) . ?
C33 C38 1.375(8) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C54 1.514(8) . ?
C37 H37 1.0000 . ?
C38 C48 1.397(8) . ?
C38 H38 0.9500 . ?
C40 C41 1.388(8) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C45 1.385(8) . ?
C43 C55 1.380(9) . ?
C43 H43 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C49 1.353(8) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C50 1.532(8) . ?
C47 H47 1.0000 . ?
C48 H48 0.9500 . ?
C49 C52 1.385(9) . ?
C49 H49 0.9500 . ?
C50 C53 1.534(8) . ?
C50 H50 1.0000 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52 0.9500 . ?
C53 H53 1.0000 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 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
C32 O1 C42 114.4(5) . . ?
C53 O2 C4 97.7(5) . . ?
C5 O3 C21 115.3(5) . . ?
C10 O4 C30 115.6(5) . . ?
C35 O5 C19 97.7(5) . . ?
C1 O6 C27 114.6(5) . . ?
C12 O7 C56 116.2(5) . . ?
C26 O8 C37 98.0(4) . . ?
C14 O10 C47 96.5(5) . . ?
C25 C1 O6 127.0(6) . . ?
C25 C1 C14 111.7(6) . . ?
O6 C1 C14 121.2(5) . . ?
C39 O14 C57 117.3(5) . . ?
C7 C3 C19 101.8(5) . . ?
C7 C3 C37 103.4(5) . . ?
C19 C3 C37 120.0(5) . . ?
C7 C3 H3 110.3 . . ?
C19 C3 H3 110.3 . . ?
C37 C3 H3 110.3 . . ?
O2 C4 C51 111.0(5) . . ?
O2 C4 C13 101.1(4) . . ?
C51 C4 C13 120.8(5) . . ?
O2 C4 C10 97.2(5) . . ?
C51 C4 C10 116.6(5) . . ?
C13 C4 C10 106.4(5) . . ?
C15 C5 O3 126.2(6) . . ?
C15 C5 C26 110.3(6) . . ?
O3 C5 C26 123.2(6) . . ?
C30 C6 C20 117.6(6) . . ?
C30 C6 C16 122.0(6) . . ?
C20 C6 C16 120.5(6) . . ?
C12 C7 C3 112.6(5) . . ?
C12 C7 C35 111.1(5) . . ?
C3 C7 C35 101.2(5) . . ?
C12 C7 C26 111.8(5) . . ?
C3 C7 C26 100.2(5) . . ?
C35 C7 C26 118.9(5) . . ?
C42 C8 C17 117.6(6) . . ?
C42 C8 C29 122.1(6) . . ?
C17 C8 C29 120.4(7) . . ?
C27 C9 C33 116.4(5) . . ?
C27 C9 C23 122.9(6) . . ?
C33 C9 C23 120.6(6) . . ?
O4 C10 C18 127.7(7) . . ?
O4 C10 C4 123.2(6) . . ?
C18 C10 C4 109.1(5) . . ?
C32 C11 C29 121.1(6) . . ?
C32 C11 C19 102.8(6) . . ?
C29 C11 C19 135.2(6) . . ?
O13 C12 O7 124.0(7) . . ?
O13 C12 C7 125.3(7) . . ?
O7 C12 C7 110.6(6) . . ?
C39 C13 C4 113.5(5) . . ?
C39 C13 C50 114.0(5) . . ?
C4 C13 C50 102.7(5) . . ?
C39 C13 C14 106.7(6) . . ?
C4 C13 C14 119.6(6) . . ?
C50 C13 C14 99.7(5) . . ?
O10 C14 C1 96.9(4) . . ?
O10 C14 C46 111.4(5) . . ?
C1 C14 C46 117.9(6) . . ?
O10 C14 C13 98.7(5) . . ?
C1 C14 C13 108.6(5) . . ?
C46 C14 C13 119.4(5) . . ?
C5 C15 C36 121.3(6) . . ?
C5 C15 C37 103.5(6) . . ?
C36 C15 C37 134.3(7) . . ?
O12 C16 C18 126.6(6) . . ?
O12 C16 C6 122.2(6) . . ?
C18 C16 C6 111.2(6) . . ?
C52 C17 C8 119.1(7) . . ?
C52 C17 H17 120.5 . . ?
C8 C17 H17 120.5 . . ?
C10 C18 C16 122.0(6) . . ?
C10 C18 C53 102.7(6) . . ?
C16 C18 C53 135.2(6) . . ?
O5 C19 C11 102.7(5) . . ?
O5 C19 C3 101.0(4) . . ?
C11 C19 C3 105.5(5) . . ?
O5 C19 H19 115.3 . . ?
C11 C19 H19 115.3 . . ?
C3 C19 H19 115.3 . . ?
C41 C20 C6 122.4(7) . . ?
C41 C20 H20 118.8 . . ?
C6 C20 H20 118.8 . . ?
C34 C21 O3 115.5(6) . . ?
C34 C21 C28 123.5(7) . . ?
O3 C21 C28 121.0(6) . . ?
C48 C22 C27 120.4(6) . . ?
C48 C22 H22 119.8 . . ?
C27 C22 H22 119.8 . . ?
O9 C23 C25 124.2(6) . . ?
O9 C23 C9 124.8(6) . . ?
C25 C23 C9 111.0(6) . . ?
C34 C24 C55 119.4(7) . . ?
C34 C24 H24 120.3 . . ?
C55 C24 H24 120.3 . . ?
C1 C25 C23 122.8(6) . . ?
C1 C25 C47 102.8(5) . . ?
C23 C25 C47 133.8(6) . . ?
O8 C26 C44 112.6(5) . . ?
O8 C26 C5 97.6(5) . . ?
C44 C26 C5 117.3(6) . . ?
O8 C26 C7 98.7(5) . . ?
C44 C26 C7 118.1(5) . . ?
C5 C26 C7 109.1(5) . . ?
C22 C27 O6 117.2(6) . . ?
C22 C27 C9 122.1(6) . . ?
O6 C27 C9 120.7(5) . . ?
C43 C28 C21 114.8(6) . . ?
C43 C28 C36 122.8(7) . . ?
C21 C28 C36 122.3(7) . . ?
O15 C29 C11 123.4(6) . . ?
O15 C29 C8 123.4(6) . . ?
C11 C29 C8 113.2(6) . . ?
C6 C30 C31 122.1(7) . . ?
C6 C30 O4 121.4(6) . . ?
C31 C30 O4 116.5(6) . . ?
C40 C31 C30 116.5(6) . . ?
C40 C31 H31 121.8 . . ?
C30 C31 H31 121.8 . . ?
O1 C32 C11 127.5(6) . . ?
O1 C32 C35 123.3(6) . . ?
C11 C32 C35 108.6(6) . . ?
C38 C33 C9 121.6(6) . . ?
C38 C33 H33 119.2 . . ?
C9 C33 H33 119.2 . . ?
C21 C34 C24 119.4(7) . . ?
C21 C34 H34 120.3 . . ?
C24 C34 H34 120.3 . . ?
O5 C35 C54 111.6(5) . . ?
O5 C35 C32 98.8(5) . . ?
C54 C35 C32 117.5(5) . . ?
O5 C35 C7 102.3(5) . . ?
C54 C35 C7 120.2(5) . . ?
C32 C35 C7 103.5(5) . . ?
O11 C36 C28 123.1(7) . . ?
O11 C36 C15 124.2(7) . . ?
C28 C36 C15 112.7(7) . . ?
O8 C37 C15 101.1(5) . . ?
O8 C37 C3 98.1(5) . . ?
C15 C37 C3 109.6(5) . . ?
O8 C37 H37 115.3 . . ?
C15 C37 H37 115.3 . . ?
C3 C37 H37 115.3 . . ?
C33 C38 C48 119.7(7) . . ?
C33 C38 H38 120.1 . . ?
C48 C38 H38 120.1 . . ?
O17 C39 O14 124.4(6) . . ?
O17 C39 C13 124.6(6) . . ?
O14 C39 C13 111.0(6) . . ?
C31 C40 C41 123.4(6) . . ?
C31 C40 H40 118.3 . . ?
C41 C40 H40 118.3 . . ?
C20 C41 C40 118.0(7) . . ?
C20 C41 H41 121.0 . . ?
C40 C41 H41 121.0 . . ?
C8 C42 C45 122.8(6) . . ?
C8 C42 O1 121.6(6) . . ?
C45 C42 O1 115.3(6) . . ?
C55 C43 C28 125.0(7) . . ?
C55 C43 H43 117.5 . . ?
C28 C43 H43 117.5 . . ?
C26 C44 H44A 109.5 . . ?
C26 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C26 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C49 C45 C42 119.9(7) . . ?
C49 C45 H45 120.1 . . ?
C42 C45 H45 120.1 . . ?
C14 C46 H46A 109.5 . . ?
C14 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C14 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O10 C47 C25 101.5(5) . . ?
O10 C47 C50 99.4(4) . . ?
C25 C47 C50 111.5(5) . . ?
O10 C47 H47 114.3 . . ?
C25 C47 H47 114.3 . . ?
C50 C47 H47 114.3 . . ?
C22 C48 C38 119.8(6) . . ?
C22 C48 H48 120.1 . . ?
C38 C48 H48 120.1 . . ?
C45 C49 C52 118.1(7) . . ?
C45 C49 H49 121.0 . . ?
C52 C49 H49 121.0 . . ?
C53 C50 C47 118.4(6) . . ?
C53 C50 C13 99.7(5) . . ?
C47 C50 C13 103.1(5) . . ?
C53 C50 H50 111.5 . . ?
C47 C50 H50 111.5 . . ?
C13 C50 H50 111.5 . . ?
C4 C51 H51A 109.5 . . ?
C4 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C4 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 C17 122.5(7) . . ?
C49 C52 H52 118.8 . . ?
C17 C52 H52 118.8 . . ?
O2 C53 C18 101.3(5) . . ?
O2 C53 C50 102.5(5) . . ?
C18 C53 C50 107.8(5) . . ?
O2 C53 H53 114.6 . . ?
C18 C53 H53 114.6 . . ?
C50 C53 H53 114.6 . . ?
C35 C54 H54A 109.5 . . ?
C35 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C35 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C43 C55 C24 117.8(7) . . ?
C43 C55 H55 121.1 . . ?
C24 C55 H55 121.1 . . ?
O7 C56 H56A 109.5 . . ?
O7 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O7 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O14 C57 H57A 109.5 . . ?
O14 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O14 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.668
_diffrn_reflns_theta_full              24.78
_diffrn_measured_fraction_theta_full   0.668
_refine_diff_density_max    0.181
_refine_diff_density_min   -0.168
_refine_diff_density_rms    0.045
