data_vijayn6m(PBB-92) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 O10' _chemical_formula_weight 518.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8631(10) _cell_length_b 20.512(2) _cell_length_c 13.5322(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.616(2) _cell_angle_gamma 90.00 _cell_volume 2609.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCKS _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12634 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4575 _reflns_number_gt 3730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP, PLATON' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+0.7434P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4575 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1477 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.09899(15) 0.05414(7) 0.78683(12) 0.0567(4) Uani 1 d . . . O4 O 0.14461(17) 0.18674(8) 0.73229(12) 0.0619(4) Uani 1 d . . . O1 O 0.55907(16) 0.03560(8) 0.75550(14) 0.0666(5) Uani 1 d . . . C10 C 0.2189(2) 0.03688(9) 0.79489(15) 0.0422(4) Uani 1 d . . . C24 C 0.4008(2) 0.12079(9) 0.53526(16) 0.0491(5) Uani 1 d . . . C7 C 0.42093(19) -0.03066(9) 0.83827(14) 0.0404(4) Uani 1 d . . . O6 O 0.49196(18) 0.20841(9) 0.77059(12) 0.0686(5) Uani 1 d . . . C18 C 0.3015(2) 0.11783(9) 0.68266(15) 0.0446(4) Uani 1 d . . . C21 C 0.4092(2) 0.13832(9) 0.63110(16) 0.0471(5) Uani 1 d . . . O9 O 0.4828(2) 0.19853(8) 0.43476(14) 0.0738(5) Uani 1 d . . . C9 C 0.3207(2) 0.06707(9) 0.74634(15) 0.0436(4) Uani 1 d . . . C8 C 0.4492(2) 0.02503(10) 0.77538(15) 0.0458(5) Uani 1 d . . . C6 C 0.52814(19) -0.08116(9) 0.88174(14) 0.0410(4) Uani 1 d . . . C1 C 0.5450(2) -0.10843(10) 0.97910(15) 0.0473(5) Uani 1 d . . . H1 H 0.4861 -0.0951 1.0175 0.057 Uiso 1 calc R . . O10 O 0.60228(19) 0.10554(8) 0.48235(15) 0.0725(5) Uani 1 d . . . C12 C 0.21945(19) -0.06389(9) 0.90980(15) 0.0439(4) Uani 1 d . . . C11 C 0.29021(19) -0.02243(9) 0.85081(14) 0.0405(4) Uani 1 d . . . C22 C 0.5244(2) 0.18451(11) 0.69036(16) 0.0519(5) Uani 1 d . . . O5 O 0.62719(19) 0.19842(10) 0.66673(15) 0.0817(6) Uani 1 d . . . C5 C 0.6172(2) -0.10245(10) 0.82602(17) 0.0527(5) Uani 1 d . . . H5 H 0.6079 -0.0849 0.7609 0.063 Uiso 1 calc R . . C27 C 0.5000(2) 0.14749(11) 0.47916(17) 0.0539(5) Uani 1 d . . . O3 O 0.0935(2) 0.16265(11) 0.56484(13) 0.0888(6) Uani 1 d . . . C2 C 0.6476(2) -0.15474(10) 1.01904(18) 0.0573(5) Uani 1 d . . . H2 H 0.6576 -0.1724 1.0842 0.069 Uiso 1 calc R . . C19 C 0.1664(2) 0.15797(10) 0.65242(16) 0.0501(5) Uani 1 d . . . C3 C 0.7353(2) -0.17518(11) 0.9637(2) 0.0646(6) Uani 1 d . . . H3 H 0.8052 -0.2063 0.9912 0.077 Uiso 1 calc R . . C4 C 0.7191(2) -0.14915(11) 0.8662(2) 0.0651(6) Uani 1 d . . . H4 H 0.7773 -0.1633 0.8278 0.078 Uiso 1 calc R . . O8 O 0.2601(2) 0.08177(12) 0.37686(15) 0.0954(7) Uani 1 d . . . C13 C 0.1741(2) -0.03704(12) 0.98767(18) 0.0592(6) Uani 1 d . . . H13 H 0.1815 0.0077 0.9994 0.071 Uiso 1 calc R . . O7 O 0.2359(3) 0.03269(9) 0.51442(17) 0.0954(7) Uani 1 d . . . C17 C 0.2034(2) -0.13040(11) 0.89083(19) 0.0616(6) Uani 1 d . . . H17 H 0.2316 -0.1490 0.8375 0.074 Uiso 1 calc R . . C25 C 0.2908(3) 0.07339(12) 0.4767(2) 0.0625(6) Uani 1 d . . . C15 C 0.1044(3) -0.14181(16) 1.0304(2) 0.0830(8) Uani 1 d . . . H15 H 0.0673 -0.1681 1.0720 0.100 Uiso 1 calc R . . C14 C 0.1178(3) -0.07624(16) 1.0484(2) 0.0767(8) Uani 1 d . . . H14 H 0.0890 -0.0580 1.1017 0.092 Uiso 1 calc R . . C20 C 0.0134(3) 0.22299(17) 0.7118(2) 0.0909(9) Uani 1 d . . . H20A H 0.0066 0.2537 0.6570 0.136 Uiso 1 calc R . . H20B H 0.0120 0.2460 0.7733 0.136 Uiso 1 calc R . . H20C H -0.0657 0.1934 0.6916 0.136 Uiso 1 calc R . . C26 C 0.1572(5) 0.0325(2) 0.3169(3) 0.1354(17) Uani 1 d . . . H26A H 0.2079 -0.0055 0.3060 0.203 Uiso 1 calc R . . H26B H 0.1041 0.0505 0.2511 0.203 Uiso 1 calc R . . H26C H 0.0931 0.0205 0.3549 0.203 Uiso 1 calc R . . C16 C 0.1452(3) -0.16885(13) 0.9516(2) 0.0807(8) Uani 1 d . . . H16 H 0.1338 -0.2134 0.9387 0.097 Uiso 1 calc R . . C28 C 0.7071(3) 0.12585(15) 0.4337(3) 0.0881(9) Uani 1 d . . . H28A H 0.6606 0.1367 0.3625 0.132 Uiso 1 calc R . . H28B H 0.7733 0.0910 0.4371 0.132 Uiso 1 calc R . . H28C H 0.7572 0.1633 0.4692 0.132 Uiso 1 calc R . . C23 C 0.5881(4) 0.25691(17) 0.8322(2) 0.0971(10) Uani 1 d . . . H23A H 0.6846 0.2431 0.8435 0.146 Uiso 1 calc R . . H23B H 0.5704 0.2619 0.8977 0.146 Uiso 1 calc R . . H23C H 0.5730 0.2978 0.7961 0.146 Uiso 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 O2 0.0430(8) 0.0593(9) 0.0718(10) 0.0099(7) 0.0233(7) 0.0056(7) O4 0.0673(9) 0.0643(10) 0.0536(9) 0.0008(7) 0.0174(7) 0.0235(8) O1 0.0513(9) 0.0700(10) 0.0892(12) 0.0287(9) 0.0372(8) 0.0094(7) C10 0.0419(10) 0.0427(10) 0.0441(10) -0.0015(8) 0.0160(8) -0.0007(8) C24 0.0548(11) 0.0427(11) 0.0527(12) 0.0001(9) 0.0207(9) 0.0014(9) C7 0.0441(10) 0.0402(10) 0.0387(10) -0.0012(7) 0.0154(8) -0.0001(8) O6 0.0775(11) 0.0795(11) 0.0533(9) -0.0153(8) 0.0267(8) -0.0245(9) C18 0.0472(10) 0.0451(11) 0.0433(10) 0.0033(8) 0.0165(8) 0.0018(8) C21 0.0518(11) 0.0427(10) 0.0494(11) 0.0087(8) 0.0194(9) 0.0054(8) O9 0.0966(13) 0.0649(10) 0.0755(11) 0.0188(9) 0.0491(10) 0.0079(9) C9 0.0441(10) 0.0435(10) 0.0455(10) 0.0038(8) 0.0169(8) 0.0007(8) C8 0.0437(10) 0.0489(11) 0.0482(11) 0.0059(8) 0.0190(9) 0.0014(8) C6 0.0422(10) 0.0389(10) 0.0424(10) -0.0014(8) 0.0134(8) -0.0016(8) C1 0.0505(11) 0.0488(11) 0.0410(10) -0.0010(8) 0.0112(8) -0.0016(9) O10 0.0748(11) 0.0615(10) 0.0996(13) 0.0043(9) 0.0539(10) 0.0070(8) C12 0.0394(10) 0.0444(10) 0.0490(11) 0.0039(8) 0.0150(8) -0.0044(8) C11 0.0437(10) 0.0388(9) 0.0407(10) -0.0021(8) 0.0154(8) -0.0027(8) C22 0.0549(12) 0.0562(12) 0.0449(11) 0.0060(9) 0.0154(9) -0.0049(10) O5 0.0722(11) 0.0999(14) 0.0817(12) -0.0123(10) 0.0365(10) -0.0287(10) C5 0.0545(12) 0.0528(12) 0.0549(12) 0.0041(9) 0.0229(10) 0.0061(9) C27 0.0648(13) 0.0527(12) 0.0504(12) -0.0027(10) 0.0267(10) -0.0005(10) O3 0.0815(12) 0.1300(17) 0.0506(10) 0.0101(10) 0.0138(9) 0.0454(12) C2 0.0596(13) 0.0534(12) 0.0500(12) 0.0064(10) 0.0034(10) -0.0007(10) C19 0.0538(11) 0.0529(12) 0.0454(12) 0.0123(9) 0.0178(10) 0.0075(9) C3 0.0522(12) 0.0495(12) 0.0835(17) 0.0086(12) 0.0076(12) 0.0082(10) C4 0.0588(13) 0.0573(13) 0.0874(18) 0.0012(12) 0.0344(12) 0.0115(11) O8 0.0962(14) 0.1321(18) 0.0618(11) -0.0228(11) 0.0299(10) -0.0504(13) C13 0.0597(13) 0.0610(13) 0.0672(14) 0.0045(11) 0.0348(11) -0.0002(10) O7 0.1324(18) 0.0736(12) 0.0926(14) -0.0217(10) 0.0528(13) -0.0518(12) C17 0.0670(14) 0.0510(13) 0.0673(15) -0.0010(10) 0.0213(11) -0.0147(10) C25 0.0670(14) 0.0633(14) 0.0665(15) -0.0195(11) 0.0339(12) -0.0057(11) C15 0.0733(17) 0.094(2) 0.087(2) 0.0266(17) 0.0325(15) -0.0221(15) C14 0.0714(16) 0.099(2) 0.0736(17) 0.0139(15) 0.0432(14) -0.0007(14) C20 0.089(2) 0.105(2) 0.0806(19) 0.0029(16) 0.0286(15) 0.0518(17) C26 0.126(3) 0.180(4) 0.096(3) -0.053(3) 0.028(2) -0.079(3) C16 0.0880(19) 0.0571(15) 0.092(2) 0.0089(14) 0.0200(16) -0.0299(13) C28 0.0813(18) 0.087(2) 0.120(2) -0.0054(17) 0.0664(18) -0.0051(15) C23 0.117(2) 0.106(2) 0.0645(17) -0.0283(16) 0.0211(16) -0.044(2) _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 C10 1.207(2) . ? O4 C19 1.305(3) . ? O4 C20 1.445(3) . ? O1 C8 1.212(2) . ? C10 C9 1.491(3) . ? C10 C11 1.492(3) . ? C24 C21 1.324(3) . ? C24 C25 1.494(3) . ? C24 C27 1.511(3) . ? C7 C11 1.361(3) . ? C7 C6 1.470(3) . ? C7 C8 1.500(3) . ? O6 C22 1.316(3) . ? O6 C23 1.451(3) . ? C18 C9 1.328(3) . ? C18 C21 1.497(3) . ? C18 C19 1.513(3) . ? C21 C22 1.510(3) . ? O9 C27 1.193(3) . ? C9 C8 1.485(3) . ? C6 C5 1.390(3) . ? C6 C1 1.394(3) . ? C1 C2 1.374(3) . ? C1 H1 0.9300 . ? O10 C27 1.316(3) . ? O10 C28 1.445(3) . ? C12 C13 1.378(3) . ? C12 C17 1.388(3) . ? C12 C11 1.478(3) . ? C22 O5 1.186(3) . ? C5 C4 1.375(3) . ? C5 H5 0.9300 . ? O3 C19 1.190(3) . ? C2 C3 1.371(3) . ? C2 H2 0.9300 . ? C3 C4 1.387(4) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? O8 C25 1.303(3) . ? O8 C26 1.488(4) . ? C13 C14 1.381(3) . ? C13 H13 0.9300 . ? O7 C25 1.191(3) . ? C17 C16 1.383(3) . ? C17 H17 0.9300 . ? C15 C14 1.366(4) . ? C15 C16 1.367(4) . ? C15 H15 0.9300 . ? C14 H14 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C16 H16 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? 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 C19 O4 C20 115.90(19) . . ? O2 C10 C9 127.60(18) . . ? O2 C10 C11 125.71(17) . . ? C9 C10 C11 106.57(15) . . ? C21 C24 C25 121.10(19) . . ? C21 C24 C27 122.40(19) . . ? C25 C24 C27 116.50(18) . . ? C11 C7 C6 129.16(17) . . ? C11 C7 C8 108.78(16) . . ? C6 C7 C8 121.93(16) . . ? C22 O6 C23 116.7(2) . . ? C9 C18 C21 122.75(17) . . ? C9 C18 C19 122.88(17) . . ? C21 C18 C19 114.32(16) . . ? C24 C21 C18 122.53(19) . . ? C24 C21 C22 120.27(18) . . ? C18 C21 C22 117.07(17) . . ? C18 C9 C8 124.72(17) . . ? C18 C9 C10 128.98(17) . . ? C8 C9 C10 106.09(16) . . ? O1 C8 C9 125.90(18) . . ? O1 C8 C7 126.45(18) . . ? C9 C8 C7 107.57(15) . . ? C5 C6 C1 118.19(18) . . ? C5 C6 C7 120.04(17) . . ? C1 C6 C7 121.77(16) . . ? C2 C1 C6 120.81(19) . . ? C2 C1 H1 119.6 . . ? C6 C1 H1 119.6 . . ? C27 O10 C28 116.3(2) . . ? C13 C12 C17 119.27(19) . . ? C13 C12 C11 119.89(18) . . ? C17 C12 C11 120.78(18) . . ? C7 C11 C12 128.01(17) . . ? C7 C11 C10 110.92(16) . . ? C12 C11 C10 121.06(16) . . ? O5 C22 O6 125.0(2) . . ? O5 C22 C21 125.1(2) . . ? O6 C22 C21 109.85(17) . . ? C4 C5 C6 120.7(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? O9 C27 O10 125.5(2) . . ? O9 C27 C24 123.8(2) . . ? O10 C27 C24 110.66(18) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? O3 C19 O4 125.9(2) . . ? O3 C19 C18 122.06(19) . . ? O4 C19 C18 111.99(17) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C25 O8 C26 112.4(2) . . ? C12 C13 C14 120.3(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C16 C17 C12 119.7(2) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? O7 C25 O8 123.0(2) . . ? O7 C25 C24 125.5(2) . . ? O8 C25 C24 111.6(2) . . ? C14 C15 C16 120.2(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O8 C26 H26A 109.5 . . ? O8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C15 C16 C17 120.4(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? O10 C28 H28A 109.5 . . ? O10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O6 C23 H23A 109.5 . . ? O6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.504 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.040