data_cs1833 _audit_creation_date 2012-02-08 _audit_creation_method ; Olex2 1.1 (compiled Feb 15 2011 20:38:53, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H30 O8' _chemical_formula_sum 'C25 H30 O8' _chemical_formula_weight 458.49 _chemical_melting_point ? _chemical_oxdiff_formula 'C21 H24 O8' _chemical_oxdiff_usercomment 'Liva/Kingston (LH-215-235-3)' 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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 12.88614(12) _cell_length_b 12.34409(7) _cell_length_c 14.84644(13) _cell_angle_alpha 90.00 _cell_angle_beta 110.4761(10) _cell_angle_gamma 90.00 _cell_volume 2212.38(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25622 _cell_measurement_temperature 100.05(10) _cell_measurement_theta_max 76.1432 _cell_measurement_theta_min 3.1748 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_T_max 1.266 _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.4149 _exptl_crystal_size_mid 0.1458 _exptl_crystal_size_min 0.1287 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_unetI/netI 0.0073 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 37837 _diffrn_reflns_theta_full 76.34 _diffrn_reflns_theta_max 76.34 _diffrn_reflns_theta_min 3.66 _diffrn_ambient_temperature 100.05(10) _diffrn_detector CCD _diffrn_detector_area_resol_mean 10.4372 _diffrn_detector_type 'Oxford Diffraction Atlas' _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -71.00 32.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 57.0000 90.0000 103 #__ type_ start__ end____ width___ exp.time_ 2 omega -71.00 32.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 57.0000 -150.0000 103 #__ type_ start__ end____ width___ exp.time_ 3 omega -124.00 -80.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -99.0000 -150.0000 44 #__ type_ start__ end____ width___ exp.time_ 4 omega -114.00 -79.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -99.0000 120.0000 35 #__ type_ start__ end____ width___ exp.time_ 5 omega -116.00 -79.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -99.0000 0.0000 37 #__ type_ start__ end____ width___ exp.time_ 6 omega 8.00 84.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 41.6052 -99.0000 -60.0000 76 #__ type_ start__ end____ width___ exp.time_ 7 omega 38.00 98.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 120.0000 60 #__ type_ start__ end____ width___ exp.time_ 8 omega 82.00 143.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -61.0000 -60.0000 61 #__ type_ start__ end____ width___ exp.time_ 9 omega 39.00 79.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -30.0000 40 #__ type_ start__ end____ width___ exp.time_ 10 omega 43.00 90.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 -150.0000 47 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 63.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -117.0000 -163.0000 26 #__ type_ start__ end____ width___ exp.time_ 12 omega 54.00 85.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 -60.0000 31 #__ type_ start__ end____ width___ exp.time_ 13 omega 70.00 96.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 178.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 14 omega 122.00 148.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 178.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 15 omega 35.00 113.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 120.0000 78 #__ type_ start__ end____ width___ exp.time_ 16 omega 32.00 109.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -94.0000 -120.0000 77 #__ type_ start__ end____ width___ exp.time_ 17 omega 109.00 147.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 -180.0000 38 #__ type_ start__ end____ width___ exp.time_ 18 omega 62.00 96.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 -180.0000 34 #__ type_ start__ end____ width___ exp.time_ 19 omega 35.00 92.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 150.0000 57 #__ type_ start__ end____ width___ exp.time_ 20 omega 148.00 174.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 111.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 21 omega 75.00 116.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 22 omega 40.00 76.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -61.0000 -60.0000 36 #__ type_ start__ end____ width___ exp.time_ 23 omega 109.00 140.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 111.0000 -90.0000 31 #__ type_ start__ end____ width___ exp.time_ 24 omega 82.00 176.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -90.0000 94 #__ type_ start__ end____ width___ exp.time_ 25 omega 70.00 111.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -117.0000 -163.0000 41 #__ type_ start__ end____ width___ exp.time_ 26 omega 27.00 176.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 0.0000 -150.0000 149 #__ type_ start__ end____ width___ exp.time_ 27 omega -116.00 -12.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -57.0000 -30.0000 104 #__ type_ start__ end____ width___ exp.time_ 28 omega -120.00 -8.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -77.0000 -120.0000 112 #__ type_ start__ end____ width___ exp.time_ 29 omega -120.00 -8.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -77.0000 60.0000 112 #__ type_ start__ end____ width___ exp.time_ 30 omega -116.00 -12.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -41.6052 -57.0000 120.0000 104 #__ type_ start__ end____ width___ exp.time_ 31 omega 70.00 121.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 41.6052 162.0000 74.0000 51 #__ type_ start__ end____ width___ exp.time_ 32 omega -140.00 -28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -61.5000 -77.0000 90.0000 112 #__ type_ start__ end____ width___ exp.time_ 33 omega -140.00 -28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -61.5000 -77.0000 -180.0000 112 #__ type_ start__ end____ width___ exp.time_ 34 omega -140.00 -28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -61.5000 -77.0000 -30.0000 112 #__ type_ start__ end____ width___ exp.time_ 35 omega 82.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -30.0000 96 #__ type_ start__ end____ width___ exp.time_ 36 omega 83.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -90.0000 95 #__ type_ start__ end____ width___ exp.time_ 37 omega 82.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 30.0000 96 #__ type_ start__ end____ width___ exp.time_ 38 omega 79.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 30.0000 99 #__ type_ start__ end____ width___ exp.time_ 39 omega 82.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -120.0000 96 #__ type_ start__ end____ width___ exp.time_ 40 omega 83.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 150.0000 95 #__ type_ start__ end____ width___ exp.time_ 41 omega 83.00 141.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 120.0000 58 #__ type_ start__ end____ width___ exp.time_ 42 omega 83.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 90.0000 95 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'phi and omega scans' _diffrn_orient_matrix_UB_11 -0.0066529000 _diffrn_orient_matrix_UB_12 0.0609300000 _diffrn_orient_matrix_UB_13 -0.0923590000 _diffrn_orient_matrix_UB_21 -0.0253160000 _diffrn_orient_matrix_UB_22 -0.1073084000 _diffrn_orient_matrix_UB_23 -0.0565486000 _diffrn_orient_matrix_UB_31 -0.1249341000 _diffrn_orient_matrix_UB_32 0.0185398000 _diffrn_orient_matrix_UB_33 -0.0232252000 _diffrn_radiation_monochromator mirrors _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Nova Micro-focus X-ray Source (Cu)' _diffrn_source_target Cu _diffrn_source_type 'Nova Micro-focus X-ray Source (Cu)' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4489 _reflns_number_total 4619 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.279 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.9601P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.0979 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.74974(6) 1.01219(7) 0.68903(6) 0.02401(18) Uani 1 1 d . . . O2 O 0.45173(8) 0.79324(8) 0.69710(7) 0.0313(2) Uani 1 1 d . . . H2 H 0.4008(15) 0.7485(16) 0.6559(13) 0.047 Uiso 1 1 d . . . O3 O 0.35475(8) 0.67564(9) 0.55318(8) 0.0404(3) Uani 1 1 d . . . O4 O 0.53800(7) 0.81336(7) 0.41031(6) 0.02448(18) Uani 1 1 d . . . H4 H 0.5859(14) 0.8402(14) 0.3867(12) 0.037 Uiso 1 1 d . . . O5 O 0.68373(6) 0.86046(7) 0.32204(6) 0.02297(18) Uani 1 1 d . . . O6 O 1.06257(7) 0.76174(7) 0.42978(7) 0.0288(2) Uani 1 1 d . . . H6 H 1.1204(15) 0.7686(15) 0.4849(13) 0.043 Uiso 1 1 d . . . O7 O 1.18136(7) 0.80408(8) 0.59972(7) 0.0333(2) Uani 1 1 d . . . O8 O 0.92063(7) 0.95971(7) 0.63741(6) 0.02518(19) Uani 1 1 d . . . H8 H 0.8622(15) 0.9825(14) 0.6437(12) 0.038 Uiso 1 1 d . . . C1 C 0.66054(9) 0.94517(9) 0.64308(8) 0.0209(2) Uani 1 1 d . . . C2 C 0.60025(9) 0.90176(10) 0.69589(8) 0.0233(2) Uani 1 1 d . . . C3 C 0.51457(9) 0.83061(10) 0.64779(9) 0.0238(2) Uani 1 1 d . . . C4 C 0.49732(9) 0.79474(9) 0.55263(8) 0.0219(2) Uani 1 1 d . . . C5 C 0.56128(9) 0.84351(9) 0.50300(8) 0.0206(2) Uani 1 1 d . . . C6 C 0.64176(9) 0.92125(9) 0.54645(8) 0.0200(2) Uani 1 1 d . . . C7 C 0.70432(9) 0.97911(9) 0.49069(8) 0.0209(2) Uani 1 1 d . . . H7A H 0.7334 1.0481 0.5239 0.025 Uiso 1 1 calc R . . H7B H 0.6509 0.9975 0.4262 0.025 Uiso 1 1 calc R . . C8 C 0.80033(9) 0.91727(9) 0.47764(8) 0.0200(2) Uani 1 1 d . . . C9 C 0.79013(9) 0.86626(9) 0.39097(8) 0.0208(2) Uani 1 1 d . . . C10 C 0.87654(10) 0.81527(9) 0.37224(8) 0.0224(2) Uani 1 1 d . . . C11 C 0.97928(10) 0.81277(9) 0.44780(9) 0.0232(2) Uani 1 1 d . . . C12 C 0.99460(9) 0.85818(9) 0.53934(8) 0.0219(2) Uani 1 1 d . . . C13 C 0.90329(9) 0.91191(9) 0.55162(8) 0.0205(2) Uani 1 1 d . . . C14 C 0.72628(12) 1.11888(11) 0.71611(12) 0.0407(3) Uani 1 1 d . . . H14A H 0.7574 1.1262 0.7862 0.061 Uiso 1 1 calc R . . H14B H 0.6459 1.1298 0.6941 0.061 Uiso 1 1 calc R . . H14C H 0.7595 1.1733 0.6864 0.061 Uiso 1 1 calc R . . C15 C 0.62984(11) 0.92342(11) 0.80180(9) 0.0307(3) Uani 1 1 d . . . H15A H 0.7104 0.9304 0.8320 0.046 Uiso 1 1 calc R . . H15B H 0.6040 0.8632 0.8315 0.046 Uiso 1 1 calc R . . H15C H 0.5943 0.9907 0.8108 0.046 Uiso 1 1 calc R . . C16 C 0.42072(10) 0.70329(10) 0.51382(9) 0.0255(2) Uani 1 1 d . . . C17 C 0.42662(11) 0.63401(10) 0.43236(9) 0.0288(3) Uani 1 1 d . . . H17A H 0.3807 0.5693 0.4267 0.043 Uiso 1 1 calc R . . H17B H 0.5036 0.6122 0.4451 0.043 Uiso 1 1 calc R . . H17C H 0.3994 0.6753 0.3723 0.043 Uiso 1 1 calc R . . C18 C 0.65828(10) 0.94078(10) 0.24698(8) 0.0271(3) Uani 1 1 d . . . H18A H 0.6573 1.0127 0.2745 0.041 Uiso 1 1 calc R . . H18B H 0.5855 0.9253 0.1986 0.041 Uiso 1 1 calc R . . H18C H 0.7148 0.9389 0.2167 0.041 Uiso 1 1 calc R . . C19 C 0.86582(10) 0.76542(10) 0.27595(8) 0.0248(2) Uani 1 1 d . . . H19A H 0.8985 0.6919 0.2861 0.030 Uiso 1 1 calc R . . H19B H 0.7865 0.7588 0.2358 0.030 Uiso 1 1 calc R . . C20 C 0.92429(10) 0.83471(9) 0.22453(9) 0.0240(2) Uani 1 1 d . . . H20 H 0.9986 0.8536 0.2611 0.029 Uiso 1 1 calc R . . C21 C 0.88608(10) 0.87307(10) 0.13496(9) 0.0249(2) Uani 1 1 d . . . C22 C 0.77243(11) 0.85229(11) 0.06249(9) 0.0303(3) Uani 1 1 d . . . H22A H 0.7791 0.8130 0.0074 0.046 Uiso 1 1 calc R . . H22B H 0.7348 0.9215 0.0406 0.046 Uiso 1 1 calc R . . H22C H 0.7294 0.8089 0.0922 0.046 Uiso 1 1 calc R . . C23 C 0.95770(12) 0.94355(11) 0.09803(10) 0.0335(3) Uani 1 1 d . . . H23A H 1.0298 0.9543 0.1490 0.050 Uiso 1 1 calc R . . H23B H 0.9216 1.0139 0.0783 0.050 Uiso 1 1 calc R . . H23C H 0.9684 0.9084 0.0427 0.050 Uiso 1 1 calc R . . C24 C 1.10269(9) 0.84519(9) 0.61743(9) 0.0245(2) Uani 1 1 d . . . C25 C 1.12203(10) 0.87615(10) 0.71938(9) 0.0263(3) Uani 1 1 d . . . H25A H 1.1978 0.8568 0.7597 0.039 Uiso 1 1 calc R . . H25B H 1.0694 0.8375 0.7421 0.039 Uiso 1 1 calc R . . H25C H 1.1115 0.9544 0.7232 0.039 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 0.0182(4) 0.0247(4) 0.0282(4) -0.0062(3) 0.0069(3) -0.0010(3) O2 0.0293(5) 0.0389(5) 0.0325(5) -0.0060(4) 0.0194(4) -0.0078(4) O3 0.0375(5) 0.0430(6) 0.0526(6) -0.0153(5) 0.0306(5) -0.0173(4) O4 0.0216(4) 0.0306(4) 0.0219(4) -0.0024(3) 0.0085(3) -0.0061(3) O5 0.0191(4) 0.0269(4) 0.0222(4) 0.0032(3) 0.0062(3) -0.0025(3) O6 0.0245(4) 0.0331(5) 0.0316(4) 0.0029(4) 0.0134(4) 0.0082(4) O7 0.0216(4) 0.0418(5) 0.0369(5) 0.0057(4) 0.0108(4) 0.0096(4) O8 0.0168(4) 0.0318(4) 0.0261(4) -0.0039(3) 0.0064(3) 0.0012(3) C1 0.0153(5) 0.0204(5) 0.0255(5) -0.0016(4) 0.0051(4) 0.0026(4) C2 0.0200(5) 0.0259(6) 0.0249(6) -0.0014(4) 0.0089(4) 0.0039(4) C3 0.0204(5) 0.0255(6) 0.0288(6) 0.0003(4) 0.0129(5) 0.0023(4) C4 0.0173(5) 0.0229(5) 0.0265(6) -0.0004(4) 0.0088(4) 0.0013(4) C5 0.0162(5) 0.0226(5) 0.0223(5) 0.0002(4) 0.0059(4) 0.0029(4) C6 0.0155(5) 0.0203(5) 0.0240(5) 0.0015(4) 0.0064(4) 0.0031(4) C7 0.0180(5) 0.0199(5) 0.0237(5) 0.0017(4) 0.0060(4) 0.0009(4) C8 0.0181(5) 0.0183(5) 0.0247(5) 0.0032(4) 0.0088(4) -0.0005(4) C9 0.0192(5) 0.0197(5) 0.0232(5) 0.0044(4) 0.0070(4) -0.0022(4) C10 0.0239(6) 0.0202(5) 0.0252(6) 0.0029(4) 0.0113(5) -0.0011(4) C11 0.0225(5) 0.0204(5) 0.0300(6) 0.0055(4) 0.0133(5) 0.0027(4) C12 0.0189(5) 0.0206(5) 0.0266(6) 0.0047(4) 0.0085(4) 0.0005(4) C13 0.0197(5) 0.0184(5) 0.0239(5) 0.0023(4) 0.0083(4) -0.0017(4) C14 0.0287(7) 0.0276(7) 0.0619(9) -0.0163(6) 0.0109(6) -0.0007(5) C15 0.0280(6) 0.0397(7) 0.0269(6) -0.0067(5) 0.0128(5) -0.0015(5) C16 0.0205(5) 0.0270(6) 0.0304(6) 0.0004(5) 0.0105(5) -0.0013(4) C17 0.0313(6) 0.0265(6) 0.0301(6) -0.0039(5) 0.0127(5) -0.0079(5) C18 0.0243(6) 0.0320(6) 0.0234(6) 0.0063(5) 0.0065(5) 0.0005(5) C19 0.0263(6) 0.0224(5) 0.0283(6) -0.0010(4) 0.0129(5) -0.0015(4) C20 0.0231(5) 0.0233(5) 0.0279(6) -0.0040(4) 0.0120(5) -0.0021(4) C21 0.0287(6) 0.0220(5) 0.0272(6) -0.0045(4) 0.0137(5) -0.0016(4) C22 0.0336(7) 0.0308(6) 0.0259(6) -0.0041(5) 0.0095(5) -0.0009(5) C23 0.0404(7) 0.0326(7) 0.0330(7) 0.0008(5) 0.0198(6) -0.0045(6) C24 0.0194(5) 0.0211(5) 0.0329(6) 0.0061(4) 0.0091(5) 0.0008(4) C25 0.0191(5) 0.0246(6) 0.0306(6) 0.0019(5) 0.0030(5) 0.0008(4) _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 1.3865(13) . ? O1 C14 1.4396(15) . ? O2 C3 1.3488(14) . ? O3 C16 1.2363(15) . ? O4 C5 1.3540(14) . ? O5 C9 1.3966(13) . ? O5 C18 1.4411(14) . ? O6 C11 1.3496(14) . ? O7 C24 1.2413(15) . ? O8 C13 1.3496(14) . ? C1 C2 1.3897(16) . ? C1 C6 1.4004(16) . ? C2 C3 1.3960(17) . ? C2 C15 1.5066(16) . ? C3 C4 1.4219(16) . ? C4 C5 1.4175(16) . ? C4 C16 1.4775(16) . ? C5 C6 1.3945(16) . ? C6 C7 1.5205(15) . ? C7 C8 1.5227(15) . ? C8 C9 1.3969(16) . ? C8 C13 1.3970(16) . ? C9 C10 1.3892(16) . ? C10 C11 1.4047(17) . ? C10 C19 1.5177(16) . ? C11 C12 1.4186(17) . ? C12 C13 1.4169(16) . ? C12 C24 1.4766(16) . ? C16 C17 1.5046(17) . ? C19 C20 1.5114(16) . ? C20 C21 1.3330(17) . ? C21 C22 1.5052(17) . ? C21 C23 1.5045(17) . ? C24 C25 1.4950(17) . ? 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 O1 C14 117.67(9) . . ? C9 O5 C18 115.53(8) . . ? O1 C1 C2 118.90(10) . . ? O1 C1 C6 116.51(10) . . ? C2 C1 C6 124.49(10) . . ? C1 C2 C3 116.89(10) . . ? C1 C2 C15 122.21(11) . . ? C3 C2 C15 120.77(11) . . ? O2 C3 C2 117.07(11) . . ? O2 C3 C4 121.20(11) . . ? C2 C3 C4 121.66(10) . . ? C3 C4 C16 118.45(10) . . ? C5 C4 C3 117.84(10) . . ? C5 C4 C16 123.53(10) . . ? O4 C5 C4 116.69(10) . . ? O4 C5 C6 121.58(10) . . ? C6 C5 C4 121.70(10) . . ? C1 C6 C7 121.61(10) . . ? C5 C6 C1 116.94(10) . . ? C5 C6 C7 121.44(10) . . ? C6 C7 C8 116.29(9) . . ? C9 C8 C7 121.63(10) . . ? C9 C8 C13 117.41(10) . . ? C13 C8 C7 120.94(10) . . ? O5 C9 C8 116.74(10) . . ? C10 C9 O5 118.70(10) . . ? C10 C9 C8 124.40(10) . . ? C9 C10 C11 116.59(10) . . ? C9 C10 C19 123.86(10) . . ? C11 C10 C19 119.55(10) . . ? O6 C11 C10 116.40(11) . . ? O6 C11 C12 121.37(11) . . ? C10 C11 C12 122.20(10) . . ? C11 C12 C24 119.09(10) . . ? C13 C12 C11 117.69(10) . . ? C13 C12 C24 123.20(11) . . ? O8 C13 C8 121.30(10) . . ? O8 C13 C12 117.08(10) . . ? C8 C13 C12 121.61(11) . . ? O3 C16 C4 120.18(11) . . ? O3 C16 C17 117.36(11) . . ? C4 C16 C17 122.21(10) . . ? C20 C19 C10 110.43(9) . . ? C21 C20 C19 129.00(11) . . ? C20 C21 C22 125.46(11) . . ? C20 C21 C23 120.62(11) . . ? C23 C21 C22 113.93(11) . . ? O7 C24 C12 119.61(11) . . ? O7 C24 C25 117.37(11) . . ? C12 C24 C25 122.99(10) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 -1 1 0.0647 0.0000 -1.0000 1.0000 -0.1533 0.0508 -0.0418 0 1 -1 0.0647 -0.0000 1.0000 -1.0000 0.1533 -0.0508 0.0418 0 1 1 0.0648 -0.0000 1.0000 1.0000 -0.0314 -0.1639 -0.0047 0 -1 -1 0.0638 0.0000 -1.0000 -1.0000 0.0314 0.1639 0.0047 -1 -1 0 0.1251 -1.0000 -1.0000 -0.0000 -0.0543 0.1326 0.1064 1 1 0 0.1251 1.0000 1.0000 0.0000 0.0543 -0.1326 -0.1064 1 -1 0 0.1220 1.0000 -1.0000 -0.0000 -0.0676 0.0820 -0.1435 -1 1 0 0.1220 -1.0000 1.0000 0.0000 0.0676 -0.0820 0.1435 6 -1 -9 0.1555 6.0000 -1.0000 -9.0000 0.7304 0.4644 -0.5591 6 -1 3 0.1460 6.0000 -1.0000 3.0000 -0.3779 -0.2142 -0.8378