 
data_Pca21
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety
 'C14 H6 O10, C3 H6 O, 2(H2 O)' 
_chemical_formula_sum
 'C17 H16 O13' 
_chemical_formula_weight          428.30

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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            29
_space_group_name_H-M_alt         'P c a 21'
_space_group_name_Hall            'P 2c -2ac'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-x+1/2, y, z+1/2'
 'x+1/2, -y, z'
 
_cell_length_a                    19.3428(5)
_cell_length_b                    6.4501(2)
_cell_length_c                    28.2467(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3524.14(17)
_cell_formula_units_Z             8
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     21636
_cell_measurement_theta_min       3.13
_cell_measurement_theta_max       68.35
 
_exptl_crystal_description        'platelet'
_exptl_crystal_colour             'yellow'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.614
_exptl_crystal_F_000              1776
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.100
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     1.246
_shelx_estimated_absorpt_T_min    0.885
_shelx_estimated_absorpt_T_max    0.885
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.6878
_exptl_absorpt_correction_T_max   1.0000
_exptl_absorpt_process_details    'abscor(Rigaku, 2010)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54187
_diffrn_radiation_type            CuK\a
_diffrn_source                    'rotating-anode X-ray tube'
_diffrn_measurement_device_type   'Rigaku R-AXIS RAPID'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  10.000
_diffrn_reflns_number             36016
_diffrn_reflns_av_unetI/netI      0.0890
_diffrn_reflns_av_R_equivalents   0.0808
_diffrn_reflns_limit_h_min        -22
_diffrn_reflns_limit_h_max        23
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -33
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          3.129
_diffrn_reflns_theta_max          68.243
_diffrn_reflns_theta_full         67.687
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              6440
_reflns_number_gt                 3935
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.954
_reflns_Friedel_fraction_max      0.997
_reflns_Friedel_fraction_full     0.998
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'RAPID AUTO (Rigaku, 2011)'
_computing_cell_refinement        'RAPID AUTO (Rigaku, 2011)'
_computing_data_reduction         'RAPID AUTO (Rigaku, 2011)'
_computing_structure_solution     'SHELXL-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material   'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1267P)²+7.7647P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_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 x determined using 1317 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.2(3)
_chemical_absolute_configuration  'unk'
_refine_ls_number_reflns          6440
_refine_ls_number_parameters      553
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.1435
_refine_ls_R_factor_gt            0.0898
_refine_ls_wR_factor_ref          0.2584
_refine_ls_wR_factor_gt           0.2192
_refine_ls_goodness_of_fit_ref    1.033
_refine_ls_restrained_S_all       1.033
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
O1 O 0.2174(4) 0.6410(14) 0.4378(3) 0.035(2) Uani 1 1 d . . . . .
O2 O 0.3029(5) 0.4255(17) 0.4181(4) 0.042(2) Uani 1 1 d . . . . .
H1 H 0.3135 0.4381 0.4468 0.062 Uiso 1 1 calc R U . . .
O3 O -0.1246(6) 0.5008(14) 0.4955(4) 0.037(3) Uani 1 1 d . . . . .
O4 O -0.0343(5) 0.4550(17) 0.5436(4) 0.038(3) Uani 1 1 d . . . . .
H2 H -0.0657 0.4383 0.5639 0.057 Uiso 1 1 calc R U . . .
O5 O 0.2769(5) 0.4539(15) 0.2409(4) 0.030(2) Uani 1 1 d . . . . .
H3 H 0.2548 0.4363 0.2156 0.045 Uiso 1 1 calc R U . . .
O6 O 0.1415(5) 0.4607(15) 0.2236(4) 0.031(2) Uani 1 1 d . . . . .
H4 H 0.1019 0.4087 0.2209 0.047 Uiso 1 1 calc R U . . .
O7 O 0.0486(5) 0.4744(13) 0.2984(4) 0.027(2) Uani 1 1 d . . . . .
O8 O -0.0637(6) 0.5020(12) 0.3173(4) 0.029(3) Uani 1 1 d . . . . .
O9 O 0.1535(4) 0.2761(14) 0.4537(3) 0.035(2) Uani 1 1 d . . . . .
O10 O 0.0514(4) 0.4030(14) 0.4741(3) 0.032(2) Uani 1 1 d . . . . .
O11 O 0.4617(5) 1.1729(14) 0.2231(3) 0.037(2) Uani 1 1 d . . . . .
O12 O 0.5510(5) 0.9683(15) 0.2438(4) 0.035(2) Uani 1 1 d . . . . .
H5 H 0.5739 1.0441 0.2254 0.052 Uiso 1 1 calc R U . . .
O13 O 0.1227(6) 0.9571(18) 0.1650(4) 0.040(3) Uani 1 1 d . . . . .
O14 O 0.2158(5) 0.9363(19) 0.1195(3) 0.042(3) Uani 1 1 d . . . . .
H6 H 0.1871 0.9242 0.0974 0.063 Uiso 1 1 calc R U . . .
O15 O 0.5260(5) 1.0247(14) 0.4182(4) 0.027(2) Uani 1 1 d . . . . .
H7 H 0.5062 1.0038 0.4442 0.041 Uiso 1 1 calc R U . . .
O16 O 0.3870(6) 1.0034(13) 0.4347(4) 0.028(2) Uani 1 1 d . . . . .
H8 H 0.3444 1.0281 0.4342 0.041 Uiso 1 1 calc R U . . .
O17 O 0.2965(6) 0.9709(13) 0.3650(4) 0.028(2) Uani 1 1 d . . . . .
O18 O 0.1878(5) 0.9735(13) 0.3436(4) 0.026(2) Uani 1 1 d . . . . .
O19 O 0.4049(4) 0.7956(13) 0.2081(3) 0.033(2) Uani 1 1 d . . . . .
O20 O 0.3008(4) 0.8951(14) 0.1880(3) 0.030(2) Uani 1 1 d . . . . .
C1 C 0.2442(7) 0.510(2) 0.4107(5) 0.027(3) Uani 1 1 d . . . . .
C2 C -0.0623(8) 0.474(2) 0.5013(5) 0.029(3) Uani 1 1 d . . . . .
C3 C 0.1397(8) 0.4600(19) 0.3558(5) 0.025(3) Uani 1 1 d . . . . .
C4 C 0.2134(7) 0.4675(19) 0.3645(5) 0.025(3) Uani 1 1 d . . . . .
C5 C 0.2593(8) 0.4642(19) 0.3259(5) 0.023(3) Uani 1 1 d . . . . .
H9 H 0.3078 0.4679 0.3309 0.028 Uiso 1 1 calc R U . . .
C6 C 0.2316(7) 0.455(2) 0.2787(5) 0.023(3) Uani 1 1 d . . . . .
C7 C 0.1606(8) 0.464(2) 0.2719(5) 0.030(3) Uani 1 1 d . . . . .
C8 C 0.1159(8) 0.465(2) 0.3075(5) 0.024(3) Uani 1 1 d . . . . .
C9 C -0.0019(8) 0.4842(17) 0.3308(5) 0.018(3) Uani 1 1 d . . . . .
C10 C 0.0194(7) 0.4699(18) 0.3798(5) 0.022(3) Uani 1 1 d . . . . .
C11 C 0.0881(7) 0.444(2) 0.3921(5) 0.026(3) Uani 1 1 d . . . . .
C12 C 0.1017(6) 0.367(2) 0.4409(5) 0.032(3) Uani 1 1 d . . . . .
C13 C -0.0143(7) 0.451(2) 0.4615(5) 0.027(3) Uani 1 1 d . . . . .
C14 C -0.0333(7) 0.4746(19) 0.4154(5) 0.023(3) Uani 1 1 d . . . . .
H10 H -0.0804 0.4940 0.4070 0.028 Uiso 1 1 calc R U . . .
C15 C 0.4880(8) 1.053(2) 0.2510(6) 0.038(4) Uani 1 1 d . . . . .
C16 C 0.1836(7) 0.938(2) 0.1595(5) 0.029(3) Uani 1 1 d . . . . .
C17 C 0.3903(7) 0.9815(18) 0.3054(5) 0.023(3) Uani 1 1 d . . . . .
C18 C 0.4606(9) 1.0028(16) 0.2991(5) 0.023(3) Uani 1 1 d . . . . .
C19 C 0.5034(8) 1.0170(18) 0.3375(6) 0.024(3) Uani 1 1 d . . . . .
H11 H 0.5517 1.0299 0.3322 0.029 Uiso 1 1 calc R U . . .
C20 C 0.4803(8) 1.0136(17) 0.3834(5) 0.024(3) Uani 1 1 d . . . . .
C21 C 0.4106(7) 1.0006(19) 0.3921(5) 0.024(3) Uani 1 1 d . . . . .
C22 C 0.3662(7) 0.9858(18) 0.3496(6) 0.024(3) Uani 1 1 d . . . . .
C23 C 0.2439(10) 0.9711(19) 0.3307(5) 0.029(4) Uani 1 1 d . . . . .
C24 C 0.2684(9) 0.959(2) 0.2806(6) 0.034(4) Uani 1 1 d . . . . .
C25 C 0.3367(7) 0.949(2) 0.2700(5) 0.028(3) Uani 1 1 d . . . . .
C26 C 0.3522(6) 0.877(2) 0.2214(5) 0.030(3) Uani 1 1 d . . . . .
C27 C 0.2323(6) 0.928(2) 0.2011(5) 0.030(3) Uani 1 1 d . . . . .
C28 C 0.2147(9) 0.950(2) 0.2449(6) 0.033(3) Uani 1 1 d . . . . .
H12 H 0.1674 0.9604 0.2535 0.039 Uiso 1 1 calc R U . . .
O1S O 0.2397(5) 0.4333(18) 0.1461(4) 0.045(3) Uani 1 1 d . . . . .
O2S O 0.1036(7) 0.4659(19) 0.1164(5) 0.055(4) Uani 1 1 d . . . . .
O3S O 0.0154(5) 0.4750(14) 0.1901(3) 0.026(2) Uani 1 1 d . . . . .
O4S O 0.4869(5) 1.0479(17) 0.5147(4) 0.041(3) Uani 1 1 d . . . . .
O5S O 0.3522(6) 0.9788(16) 0.5468(4) 0.043(3) Uani 1 1 d . . . . .
O6S O 0.2606(6) 0.9975(13) 0.4721(4) 0.034(3) Uani 1 1 d . . . . .
C1S C 0.3571(8) 0.397(3) 0.1314(6) 0.052(4) Uani 1 1 d . . . . .
H16 H 0.3588 0.3442 0.1639 0.078 Uiso 1 1 calc R U . . .
H17 H 0.3804 0.5319 0.1299 0.078 Uiso 1 1 calc R U . . .
H18 H 0.3805 0.2993 0.1102 0.078 Uiso 1 1 calc R U . . .
C2S C 0.2837(7) 0.421(2) 0.1164(5) 0.037(3) Uani 1 1 d . . . . .
C3S C 0.2676(8) 0.427(3) 0.0654(6) 0.050(4) Uani 1 1 d . . . . .
H19 H 0.2232 0.3580 0.0598 0.074 Uiso 1 1 calc R U . . .
H20 H 0.3040 0.3554 0.0477 0.074 Uiso 1 1 calc R U . . .
H21 H 0.2647 0.5715 0.0549 0.074 Uiso 1 1 calc R U . . .
C4S C 0.5185(10) 1.053(3) 0.5960(6) 0.051(5) Uani 1 1 d . . . . .
H13 H 0.4686 1.0662 0.6014 0.077 Uiso 1 1 calc R U . . .
H14 H 0.5430 1.1613 0.6136 0.077 Uiso 1 1 calc R U . . .
H15 H 0.5341 0.9165 0.6067 0.077 Uiso 1 1 calc R U . . .
C5S C 0.5334(8) 1.077(2) 0.5435(5) 0.040(3) Uani 1 1 d . . . . .
C6S C 0.6054(7) 1.123(3) 0.5281(6) 0.053(5) Uani 1 1 d . . . . .
H22 H 0.6115 1.0800 0.4951 0.079 Uiso 1 1 calc R U . . .
H23 H 0.6381 1.0473 0.5482 0.079 Uiso 1 1 calc R U . . .
H24 H 0.6141 1.2722 0.5308 0.079 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O1 C1 1.252(16) . ?
O2 C1 1.278(17) . ?
O2 H1 0.8400 . ?
O3 C2 1.229(19) . ?
O4 C2 1.319(18) . ?
O4 H2 0.8400 . ?
O5 C6 1.381(16) . ?
O5 H3 0.8400 . ?
O6 C7 1.413(18) . ?
O6 H4 0.8400 . ?
O7 C8 1.329(18) . ?
O7 C9 1.339(17) . ?
O8 C9 1.260(17) . ?
O9 C12 1.218(14) . ?
O10 C13 1.354(15) . ?
O10 C12 1.369(14) . ?
O11 C15 1.216(17) . ?
O12 C15 1.349(18) . ?
O12 H5 0.8400 . ?
O13 C16 1.193(17) . ?
O14 C16 1.288(17) . ?
O14 H6 0.8400 . ?
O15 C20 1.323(17) . ?
O15 H7 0.8400 . ?
O16 C21 1.286(18) . ?
O16 H8 0.8400 . ?
O17 C23 1.404(17) . ?
O17 C22 1.420(18) . ?
O18 C23 1.14(2) . ?
O19 C26 1.205(14) . ?
O20 C26 1.374(15) . ?
O20 C27 1.393(14) . ?
C1 C4 1.46(2) . ?
C2 C13 1.47(2) . ?
C3 C11 1.435(19) . ?
C3 C8 1.44(2) . ?
C3 C4 1.45(2) . ?
C4 C5 1.406(19) . ?
C5 C6 1.438(18) . ?
C5 H9 0.9500 . ?
C6 C7 1.39(2) . ?
C7 C8 1.33(2) . ?
C9 C10 1.447(19) . ?
C10 C11 1.383(18) . ?
C10 C14 1.432(17) . ?
C11 C12 1.487(18) . ?
C13 C14 1.364(19) . ?
C14 H10 0.9500 . ?
C15 C18 1.49(2) . ?
C16 C27 1.508(19) . ?
C17 C22 1.33(2) . ?
C17 C18 1.38(2) . ?
C17 C25 1.45(2) . ?
C18 C19 1.37(2) . ?
C19 C20 1.37(2) . ?
C19 H11 0.9500 . ?
C20 C21 1.37(2) . ?
C21 C22 1.480(19) . ?
C23 C24 1.49(2) . ?
C24 C25 1.36(2) . ?
C24 C28 1.45(2) . ?
C25 C26 1.483(18) . ?
C27 C28 1.29(2) . ?
C28 H12 0.9500 . ?
O1S C2S 1.199(17) . ?
O4S C5S 1.226(18) . ?
C1S C2S 1.490(19) . ?
C1S H16 0.9800 . ?
C1S H17 0.9800 . ?
C1S H18 0.9800 . ?
C2S C3S 1.47(2) . ?
C3S H19 0.9800 . ?
C3S H20 0.9800 . ?
C3S H21 0.9800 . ?
C4S C5S 1.52(2) . ?
C4S H13 0.9800 . ?
C4S H14 0.9800 . ?
C4S H15 0.9800 . ?
C5S C6S 1.49(2) . ?
C6S H22 0.9800 . ?
C6S H23 0.9800 . ?
C6S H24 0.9800 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C1 O2 H1 109.5 . . ?
C2 O4 H2 109.5 . . ?
C6 O5 H3 109.5 . . ?
C7 O6 H4 109.5 . . ?
C8 O7 C9 125.7(12) . . ?
C13 O10 C12 121.6(9) . . ?
C15 O12 H5 109.5 . . ?
C16 O14 H6 109.5 . . ?
C20 O15 H7 109.5 . . ?
C21 O16 H8 109.5 . . ?
C23 O17 C22 118.5(13) . . ?
C26 O20 C27 121.4(10) . . ?
O1 C1 O2 123.8(13) . . ?
O1 C1 C4 120.3(13) . . ?
O2 C1 C4 115.4(13) . . ?
O3 C2 O4 122.5(14) . . ?
O3 C2 C13 122.3(14) . . ?
O4 C2 C13 115.2(13) . . ?
C11 C3 C8 117.2(14) . . ?
C11 C3 C4 124.5(14) . . ?
C8 C3 C4 118.2(13) . . ?
C5 C4 C3 119.4(14) . . ?
C5 C4 C1 116.0(13) . . ?
C3 C4 C1 124.0(13) . . ?
C4 C5 C6 119.0(13) . . ?
C4 C5 H9 120.5 . . ?
C6 C5 H9 120.5 . . ?
O5 C6 C7 121.5(13) . . ?
O5 C6 C5 118.8(11) . . ?
C7 C6 C5 119.6(13) . . ?
C8 C7 C6 122.8(15) . . ?
C8 C7 O6 124.1(14) . . ?
C6 C7 O6 113.0(13) . . ?
C7 C8 O7 119.5(14) . . ?
C7 C8 C3 120.7(14) . . ?
O7 C8 C3 119.8(13) . . ?
O8 C9 O7 119.3(12) . . ?
O8 C9 C10 124.4(13) . . ?
O7 C9 C10 116.3(12) . . ?
C11 C10 C14 120.7(13) . . ?
C11 C10 C9 121.5(12) . . ?
C14 C10 C9 117.8(12) . . ?
C10 C11 C3 118.6(13) . . ?
C10 C11 C12 116.3(11) . . ?
C3 C11 C12 124.3(12) . . ?
O9 C12 O10 117.5(11) . . ?
O9 C12 C11 125.5(12) . . ?
O10 C12 C11 117.0(10) . . ?
O10 C13 C14 122.0(11) . . ?
O10 C13 C2 114.7(11) . . ?
C14 C13 C2 123.3(13) . . ?
C13 C14 C10 118.4(13) . . ?
C13 C14 H10 120.8 . . ?
C10 C14 H10 120.8 . . ?
O11 C15 O12 122.6(16) . . ?
O11 C15 C18 125.2(14) . . ?
O12 C15 C18 111.7(13) . . ?
O13 C16 O14 126.4(13) . . ?
O13 C16 C27 121.2(13) . . ?
O14 C16 C27 112.3(12) . . ?
C22 C17 C18 117.6(14) . . ?
C22 C17 C25 113.4(13) . . ?
C18 C17 C25 128.9(14) . . ?
C19 C18 C17 120.0(14) . . ?
C19 C18 C15 119.5(14) . . ?
C17 C18 C15 119.3(14) . . ?
C18 C19 C20 123.5(14) . . ?
C18 C19 H11 118.2 . . ?
C20 C19 H11 118.2 . . ?
O15 C20 C19 118.8(13) . . ?
O15 C20 C21 121.8(13) . . ?
C19 C20 C21 119.4(14) . . ?
O16 C21 C20 120.9(13) . . ?
O16 C21 C22 123.7(13) . . ?
C20 C21 C22 115.3(13) . . ?
C17 C22 O17 128.1(13) . . ?
C17 C22 C21 124.0(14) . . ?
O17 C22 C21 107.8(13) . . ?
O18 C23 O17 117.9(15) . . ?
O18 C23 C24 127.0(15) . . ?
O17 C23 C24 115.0(15) . . ?
C25 C24 C28 122.9(14) . . ?
C25 C24 C23 121.4(14) . . ?
C28 C24 C23 115.7(14) . . ?
C24 C25 C17 122.4(13) . . ?
C24 C25 C26 114.6(12) . . ?
C17 C25 C26 122.5(12) . . ?
O19 C26 O20 115.9(12) . . ?
O19 C26 C25 126.6(12) . . ?
O20 C26 C25 117.4(11) . . ?
C28 C27 O20 121.4(13) . . ?
C28 C27 C16 125.3(13) . . ?
O20 C27 C16 113.3(11) . . ?
C27 C28 C24 118.9(15) . . ?
C27 C28 H12 120.5 . . ?
C24 C28 H12 120.5 . . ?
C2S C1S H16 109.5 . . ?
C2S C1S H17 109.5 . . ?
H16 C1S H17 109.5 . . ?
C2S C1S H18 109.5 . . ?
H16 C1S H18 109.5 . . ?
H17 C1S H18 109.5 . . ?
O1S C2S C3S 122.2(14) . . ?
O1S C2S C1S 118.9(13) . . ?
C3S C2S C1S 118.9(12) . . ?
C2S C3S H19 109.5 . . ?
C2S C3S H20 109.5 . . ?
H19 C3S H20 109.5 . . ?
C2S C3S H21 109.5 . . ?
H19 C3S H21 109.5 . . ?
H20 C3S H21 109.5 . . ?
C5S C4S H13 109.5 . . ?
C5S C4S H14 109.5 . . ?
H13 C4S H14 109.5 . . ?
C5S C4S H15 109.5 . . ?
H13 C4S H15 109.5 . . ?
H14 C4S H15 109.5 . . ?
O4S C5S C6S 121.6(14) . . ?
O4S C5S C4S 119.4(15) . . ?
C6S C5S C4S 118.9(14) . . ?
C5S C6S H22 109.5 . . ?
C5S C6S H23 109.5 . . ?
H22 C6S H23 109.5 . . ?
C5S C6S H24 109.5 . . ?
H22 C6S H24 109.5 . . ?
H23 C6S H24 109.5 . . ?
 
_refine_diff_density_max    0.745
_refine_diff_density_min   -0.342
_refine_diff_density_rms    0.103



