# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Shengming Ma' _publ_contact_author_address ; Chinese Academy of Sciences Shanghai Institute of Organic Chemistry 354 Fenglin Lu Shanghai 200032 CHINA ; _publ_contact_author_email MASM@MAIL.SIOC.AC.CN _publ_section_title ; From Allene to Allene: A Palladium-Catalyzed Approach to b-Allenyl Butenolides and Their Application to the Synthesis of Polysubstituted Benzene Derivatives ; loop_ _publ_author_name 'Shengming Ma.' 'Youqian Deng.' 'Zhenhua Gu.' data_cd24107 _database_code_depnum_ccdc_archive 'CCDC 270605' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 O2' _chemical_formula_weight 240.29 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.592(2) _cell_length_b 14.568(3) _cell_length_c 16.342(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2759.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 665 _cell_measurement_theta_min 5.136 _cell_measurement_theta_max 35.702 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.372 _exptl_crystal_size_mid 0.287 _exptl_crystal_size_min 0.217 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.63542 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15724 _diffrn_reflns_av_R_equivalents 0.1496 _diffrn_reflns_av_sigmaI/netI 0.1567 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3266 _reflns_number_gt 917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0041P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00244(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3266 _refine_ls_number_parameters 227 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1877 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 0.647 _refine_ls_restrained_S_all 0.648 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.66093(14) 0.21115(13) 0.50418(9) 0.0941(7) Uani 1 1 d . . . O2 O 0.82705(15) 0.22831(11) 0.43580(9) 0.0715(5) Uani 1 1 d . . . C1 C 0.7284(2) 0.2623(2) 0.47104(14) 0.0719(8) Uani 1 1 d . . . C2 C 0.7262(2) 0.3619(2) 0.46023(13) 0.0633(7) Uani 1 1 d . . . C3 C 0.8220(2) 0.38712(19) 0.42014(13) 0.0593(7) Uani 1 1 d . . . C4 C 0.89334(19) 0.30436(18) 0.40141(13) 0.0582(7) Uani 1 1 d D . . C5 C 0.6280(3) 0.4189(4) 0.4914(2) 0.1020(14) Uani 1 1 d D . . C6 C 0.8594(2) 0.4786(2) 0.39704(15) 0.0738(8) Uani 1 1 d D . . C7 C 0.9543(3) 0.49318(16) 0.35451(15) 0.0722(8) Uani 1 1 d . . . C8 C 1.0485(3) 0.50330(16) 0.31258(18) 0.0737(8) Uani 1 1 d . . . C9 C 1.0472(4) 0.5023(3) 0.2201(2) 0.0941(11) Uani 1 1 d D . . C10 C 1.1645(3) 0.5151(3) 0.3535(3) 0.1086(12) Uani 1 1 d D . . C11 C 0.91659(19) 0.28557(14) 0.31218(14) 0.0518(6) Uani 1 1 d . . . C12 C 1.0214(2) 0.24873(16) 0.28800(18) 0.0647(8) Uani 1 1 d . . . C13 C 1.0410(3) 0.22893(18) 0.2062(2) 0.0767(9) Uani 1 1 d . . . C14 C 0.9589(3) 0.24660(19) 0.14829(18) 0.0803(9) Uani 1 1 d . . . C15 C 0.8557(3) 0.28452(19) 0.17125(17) 0.0795(9) Uani 1 1 d . . . C16 C 0.8346(2) 0.30426(18) 0.25310(15) 0.0651(7) Uani 1 1 d D . . H1 H 0.9661(13) 0.3078(13) 0.4327(10) 0.078 Uiso 1 1 d D . . H2 H 0.643(3) 0.4837(14) 0.4786(19) 0.19(2) Uiso 1 1 d D . . H3 H 0.616(2) 0.4068(16) 0.5455(15) 0.117(12) Uiso 1 1 d . . . H4 H 0.561(2) 0.3962(19) 0.4722(15) 0.144(15) Uiso 1 1 d . . . H5 H 0.8165(17) 0.5311(13) 0.4157(13) 0.093(9) Uiso 1 1 d D . . H6 H 1.083(2) 0.5563(17) 0.1967(15) 0.115(12) Uiso 1 1 d . . . H7 H 1.087(2) 0.4497(18) 0.2004(16) 0.123(13) Uiso 1 1 d . . . H8 H 0.9719(16) 0.4971(18) 0.2001(17) 0.134(15) Uiso 1 1 d D . . H9 H 1.223(2) 0.4727(17) 0.3302(16) 0.156(15) Uiso 1 1 d D . . H10 H 1.194(3) 0.5732(15) 0.3311(16) 0.171(18) Uiso 1 1 d D . . H11 H 1.155(3) 0.513(2) 0.4137(19) 0.21(2) Uiso 1 1 d . . . H12 H 1.0772(17) 0.2357(12) 0.3308(11) 0.070(8) Uiso 1 1 d . . . H13 H 1.1156(18) 0.2040(14) 0.1878(12) 0.092(9) Uiso 1 1 d . . . H14 H 0.9792(17) 0.2306(12) 0.0917(11) 0.079(8) Uiso 1 1 d . . . H15 H 0.7960(18) 0.2982(15) 0.1307(12) 0.093(9) Uiso 1 1 d . . . H16 H 0.7614(14) 0.3316(12) 0.2705(10) 0.066(7) Uiso 1 1 d D . . 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 0.0700(13) 0.1487(19) 0.0635(12) 0.0300(11) 0.0037(10) -0.0264(12) O2 0.0622(11) 0.0896(14) 0.0628(11) 0.0180(9) 0.0045(9) -0.0039(11) C1 0.0558(19) 0.121(3) 0.0392(17) 0.0110(17) -0.0072(14) -0.002(2) C2 0.0497(17) 0.100(2) 0.0396(15) -0.0023(16) 0.0015(13) 0.0075(18) C3 0.0614(17) 0.078(2) 0.0387(15) -0.0053(14) -0.0024(13) 0.0075(17) C4 0.0498(16) 0.0759(19) 0.0488(17) 0.0042(15) -0.0022(12) -0.0041(16) C5 0.066(2) 0.172(5) 0.068(3) -0.020(3) 0.009(2) 0.019(3) C6 0.077(2) 0.080(3) 0.064(2) -0.0145(17) 0.0055(16) 0.007(2) C7 0.083(2) 0.069(2) 0.0647(19) -0.0076(15) -0.0062(17) -0.0039(19) C8 0.080(2) 0.0630(18) 0.078(2) -0.0103(15) 0.0085(19) -0.0045(17) C9 0.113(3) 0.092(3) 0.077(3) 0.003(2) 0.017(2) -0.001(3) C10 0.079(3) 0.123(4) 0.123(4) -0.027(3) -0.006(3) -0.013(3) C11 0.0443(15) 0.0615(17) 0.0496(15) 0.0024(13) 0.0009(13) -0.0042(13) C12 0.0502(18) 0.079(2) 0.065(2) -0.0035(16) 0.0030(16) 0.0020(15) C13 0.064(2) 0.080(2) 0.086(2) -0.0213(18) 0.024(2) -0.0064(17) C14 0.083(2) 0.095(2) 0.063(2) -0.0257(17) 0.021(2) -0.0195(19) C15 0.074(2) 0.110(3) 0.055(2) -0.0150(17) -0.0036(17) -0.0043(18) C16 0.0541(18) 0.087(2) 0.0542(17) -0.0119(15) 0.0012(15) 0.0041(16) _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 1.209(3) . ? O2 C1 1.373(3) . ? O2 C4 1.461(2) . ? C1 C2 1.462(3) . ? C2 C3 1.340(3) . ? C2 C5 1.497(4) . ? C3 C6 1.452(3) . ? C3 C4 1.494(3) . ? C4 C11 1.508(3) . ? C4 H1 0.988(14) . ? C5 H2 0.982(17) . ? C5 H3 0.91(2) . ? C5 H4 0.90(2) . ? C6 C7 1.319(3) . ? C6 H5 0.961(15) . ? C7 C8 1.298(3) . ? C8 C9 1.511(4) . ? C8 C10 1.511(4) . ? C9 H6 0.97(2) . ? C9 H7 0.95(2) . ? C9 H8 0.935(16) . ? C10 H9 0.990(16) . ? C10 H10 0.986(17) . ? C10 H11 0.99(3) . ? C11 C16 1.382(3) . ? C11 C12 1.386(3) . ? C12 C13 1.386(3) . ? C12 H12 0.971(17) . ? C13 C14 1.367(3) . ? C13 H13 0.99(2) . ? C14 C15 1.371(3) . ? C14 H14 0.982(17) . ? C15 C16 1.390(3) . ? C15 H15 0.979(19) . ? C16 H16 0.980(14) . ? 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 C4 109.0(2) . . ? O1 C1 O2 120.3(3) . . ? O1 C1 C2 130.9(3) . . ? O2 C1 C2 108.8(2) . . ? C3 C2 C1 108.4(3) . . ? C3 C2 C5 130.1(4) . . ? C1 C2 C5 121.5(3) . . ? C2 C3 C6 128.8(3) . . ? C2 C3 C4 109.8(2) . . ? C6 C3 C4 121.5(3) . . ? O2 C4 C3 103.99(19) . . ? O2 C4 C11 109.17(19) . . ? C3 C4 C11 116.33(19) . . ? O2 C4 H1 106.8(11) . . ? C3 C4 H1 109.0(12) . . ? C11 C4 H1 111.0(11) . . ? C2 C5 H2 109(2) . . ? C2 C5 H3 109.7(16) . . ? H2 C5 H3 115(3) . . ? C2 C5 H4 109.6(19) . . ? H2 C5 H4 115(3) . . ? H3 C5 H4 98(2) . . ? C7 C6 C3 122.3(3) . . ? C7 C6 H5 118.1(14) . . ? C3 C6 H5 119.6(14) . . ? C8 C7 C6 177.3(3) . . ? C7 C8 C9 121.2(3) . . ? C7 C8 C10 121.8(3) . . ? C9 C8 C10 116.9(3) . . ? C8 C9 H6 112.6(16) . . ? C8 C9 H7 109.9(17) . . ? H6 C9 H7 108(2) . . ? C8 C9 H8 111.1(19) . . ? H6 C9 H8 109(2) . . ? H7 C9 H8 106(2) . . ? C8 C10 H9 111.3(17) . . ? C8 C10 H10 104.3(19) . . ? H9 C10 H10 99(2) . . ? C8 C10 H11 110(2) . . ? H9 C10 H11 116(3) . . ? H10 C10 H11 116(3) . . ? C16 C11 C12 118.7(2) . . ? C16 C11 C4 121.1(2) . . ? C12 C11 C4 120.2(2) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 123.0(12) . . ? C11 C12 H12 117.0(12) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H13 117.9(12) . . ? C12 C13 H13 121.0(12) . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 116.2(12) . . ? C15 C14 H14 124.2(12) . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15 120.9(13) . . ? C16 C15 H15 119.1(13) . . ? C11 C16 C15 120.7(3) . . ? C11 C16 H16 118.2(11) . . ? C15 C16 H16 121.0(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 O2 C1 O1 -179.2(2) . . . . ? C4 O2 C1 C2 0.5(2) . . . . ? O1 C1 C2 C3 179.1(2) . . . . ? O2 C1 C2 C3 -0.6(3) . . . . ? O1 C1 C2 C5 -1.0(4) . . . . ? O2 C1 C2 C5 179.3(2) . . . . ? C1 C2 C3 C6 -178.5(2) . . . . ? C5 C2 C3 C6 1.7(4) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? C5 C2 C3 C4 -179.4(3) . . . . ? C1 O2 C4 C3 -0.3(2) . . . . ? C1 O2 C4 C11 -125.1(2) . . . . ? C2 C3 C4 O2 -0.1(2) . . . . ? C6 C3 C4 O2 178.87(19) . . . . ? C2 C3 C4 C11 119.9(2) . . . . ? C6 C3 C4 C11 -61.1(3) . . . . ? C2 C3 C6 C7 -177.3(2) . . . . ? C4 C3 C6 C7 4.0(4) . . . . ? C3 C6 C7 C8 1(6) . . . . ? C6 C7 C8 C9 89(6) . . . . ? C6 C7 C8 C10 -90(6) . . . . ? O2 C4 C11 C16 81.9(3) . . . . ? C3 C4 C11 C16 -35.3(3) . . . . ? O2 C4 C11 C12 -97.9(2) . . . . ? C3 C4 C11 C12 144.9(2) . . . . ? C16 C11 C12 C13 -1.9(3) . . . . ? C4 C11 C12 C13 178.0(2) . . . . ? C11 C12 C13 C14 1.1(4) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? C12 C11 C16 C15 1.5(4) . . . . ? C4 C11 C16 C15 -178.3(2) . . . . ? C14 C15 C16 C11 -0.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.113 _refine_diff_density_min -0.092 _refine_diff_density_rms 0.027 data_cd25217 _database_code_depnum_ccdc_archive 'CCDC 273892' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 O6' _chemical_formula_weight 438.50 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 P2(1)/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 10.0344(17) _cell_length_b 13.210(2) _cell_length_c 18.172(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.356(4) _cell_angle_gamma 90.00 _cell_volume 2376.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2209 _cell_measurement_theta_min 4.364 _cell_measurement_theta_max 44.548 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.267 _exptl_crystal_size_mid 0.248 _exptl_crystal_size_min 0.160 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.56621 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14147 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5404 _reflns_number_gt 2955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0043(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5404 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.001 _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 O1 O 0.20326(16) 0.64011(10) 0.05830(9) 0.0662(5) Uani 1 1 d . . . O2 O 0.31584(13) 0.78727(9) 0.07008(7) 0.0475(4) Uani 1 1 d . . . O3 O -0.01854(15) 0.56842(11) 0.19177(8) 0.0630(4) Uani 1 1 d . . . O4 O -0.09110(14) 0.63589(10) 0.07950(7) 0.0539(4) Uani 1 1 d . . . O5 O -0.23678(15) 0.73699(11) 0.21663(8) 0.0598(4) Uani 1 1 d . . . O6 O -0.09792(14) 0.74621(10) 0.32649(7) 0.0548(4) Uani 1 1 d . . . C1 C 0.2179(2) 0.72336(15) 0.08480(11) 0.0456(5) Uani 1 1 d . . . C2 C 0.14195(18) 0.77540(13) 0.13670(9) 0.0361(4) Uani 1 1 d . . . C3 C 0.19881(18) 0.86897(13) 0.15431(9) 0.0337(4) Uani 1 1 d . . . C4 C 0.32010(18) 0.88143(13) 0.11418(10) 0.0388(5) Uani 1 1 d . . . C5 C 0.03331(19) 0.74026(13) 0.16821(10) 0.0370(4) Uani 1 1 d . . . C6 C -0.01430(18) 0.80260(14) 0.22008(10) 0.0368(4) Uani 1 1 d . . . C7 C 0.03845(19) 0.90063(14) 0.23653(10) 0.0379(4) Uani 1 1 d . . . C8 C 0.14639(18) 0.93558(13) 0.20235(9) 0.0349(4) Uani 1 1 d . . . C9 C 0.45355(19) 0.87836(16) 0.16767(11) 0.0500(5) Uani 1 1 d . . . H9A H 0.4572 0.8183 0.1977 0.075 Uiso 1 1 calc R . . H9B H 0.4606 0.9369 0.1994 0.075 Uiso 1 1 calc R . . H9C H 0.5269 0.8780 0.1397 0.075 Uiso 1 1 calc R . . C10 C 0.30386(19) 0.96853(14) 0.05871(10) 0.0386(5) Uani 1 1 d . . . C11 C 0.3917(2) 1.04959(17) 0.06446(13) 0.0544(6) Uani 1 1 d . . . C12 C 0.3706(3) 1.12914(19) 0.01427(14) 0.0653(7) Uani 1 1 d . . . C13 C 0.2628(3) 1.1282(2) -0.04220(14) 0.0606(7) Uani 1 1 d . . . C14 C 0.1747(3) 1.0477(2) -0.04887(13) 0.0592(6) Uani 1 1 d . . . C15 C 0.1955(2) 0.96886(17) 0.00074(11) 0.0491(5) Uani 1 1 d . . . C16 C -0.0213(2) 0.97286(16) 0.28858(12) 0.0502(6) Uani 1 1 d . . . C17 C 0.0431(3) 0.95837(19) 0.37015(12) 0.0772(8) Uani 1 1 d . . . H17A H 0.0097 1.0092 0.4003 0.116 Uiso 1 1 calc R . . H17B H 0.1395 0.9644 0.3746 0.116 Uiso 1 1 calc R . . H17C H 0.0206 0.8925 0.3867 0.116 Uiso 1 1 calc R . . C18 C -0.1755(2) 0.97543(17) 0.27734(14) 0.0723(7) Uani 1 1 d . . . H18A H -0.2078 0.9206 0.3043 0.108 Uiso 1 1 calc R . . H18B H -0.2109 0.9687 0.2252 0.108 Uiso 1 1 calc R . . H18C H -0.2048 1.0386 0.2954 0.108 Uiso 1 1 calc R . . C19 C 0.20055(19) 1.04266(13) 0.21295(10) 0.0400(5) Uani 1 1 d . . . H19A H 0.2931 1.0438 0.2038 0.048 Uiso 1 1 calc R . . H19B H 0.2011 1.0629 0.2643 0.048 Uiso 1 1 calc R . . C20 C 0.1174(2) 1.11922(15) 0.16121(12) 0.0438(5) Uani 1 1 d . . . C21 C 0.1764(2) 1.22479(14) 0.16757(12) 0.0557(6) Uani 1 1 d . . . H21A H 0.1847 1.2469 0.2190 0.067 Uiso 1 1 calc R . . H21B H 0.2665 1.2226 0.1547 0.067 Uiso 1 1 calc R . . C22 C 0.0935(3) 1.30140(18) 0.11829(15) 0.0856(8) Uani 1 1 d . . . H22A H 0.0836 1.2797 0.0673 0.128 Uiso 1 1 calc R . . H22B H 0.1382 1.3659 0.1235 0.128 Uiso 1 1 calc R . . H22C H 0.0060 1.3074 0.1328 0.128 Uiso 1 1 calc R . . C23 C -0.02693(19) 0.63780(14) 0.14884(11) 0.0415(5) Uani 1 1 d . . . C24 C -0.1496(3) 0.53984(16) 0.05263(13) 0.0724(7) Uani 1 1 d . . . H24A H -0.0800 0.4894 0.0566 0.109 Uiso 1 1 calc R . . H24B H -0.1912 0.5466 0.0014 0.109 Uiso 1 1 calc R . . H24C H -0.2164 0.5199 0.0821 0.109 Uiso 1 1 calc R . . C25 C -0.1300(2) 0.75982(14) 0.25295(12) 0.0432(5) Uani 1 1 d . . . C26 C -0.2054(3) 0.7089(2) 0.36373(14) 0.0806(8) Uani 1 1 d . . . H26A H -0.2880 0.7433 0.3446 0.121 Uiso 1 1 calc R . . H26B H -0.1826 0.7210 0.4164 0.121 Uiso 1 1 calc R . . H26C H -0.2167 0.6375 0.3549 0.121 Uiso 1 1 calc R . . H11 H 0.464(2) 1.0511(15) 0.1025(11) 0.063(7) Uiso 1 1 d . . . H12 H 0.433(2) 1.1827(18) 0.0210(12) 0.079(8) Uiso 1 1 d . . . H13 H 0.249(2) 1.1817(17) -0.0768(12) 0.076(7) Uiso 1 1 d . . . H14 H 0.100(2) 1.0492(18) -0.0877(13) 0.091(9) Uiso 1 1 d . . . H15 H 0.1317(18) 0.9133(13) -0.0045(9) 0.043(5) Uiso 1 1 d . . . H16 H 0.0014(18) 1.0396(14) 0.2751(10) 0.049(6) Uiso 1 1 d . . . H20A H 0.0274(19) 1.1201(13) 0.1729(10) 0.049(6) Uiso 1 1 d . . . H20B H 0.1113(17) 1.0984(13) 0.1092(10) 0.047(5) Uiso 1 1 d . . . 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 0.0788(12) 0.0427(8) 0.0823(11) -0.0227(8) 0.0282(9) -0.0037(8) O2 0.0524(9) 0.0436(8) 0.0507(9) -0.0068(7) 0.0209(7) 0.0000(7) O3 0.0711(11) 0.0444(9) 0.0688(11) 0.0188(8) -0.0031(8) -0.0094(7) O4 0.0713(10) 0.0426(8) 0.0443(9) -0.0037(7) -0.0013(7) -0.0124(7) O5 0.0426(9) 0.0746(11) 0.0609(10) 0.0083(8) 0.0050(7) -0.0096(8) O6 0.0510(9) 0.0718(10) 0.0437(8) 0.0142(7) 0.0140(7) -0.0049(7) C1 0.0501(13) 0.0419(12) 0.0454(12) -0.0025(10) 0.0100(10) 0.0038(10) C2 0.0404(11) 0.0332(10) 0.0339(10) 0.0008(8) 0.0039(8) 0.0025(9) C3 0.0347(11) 0.0338(10) 0.0323(10) 0.0026(8) 0.0039(8) 0.0009(8) C4 0.0391(12) 0.0407(11) 0.0373(11) -0.0036(9) 0.0085(9) -0.0004(9) C5 0.0392(11) 0.0338(10) 0.0369(11) 0.0038(8) 0.0028(8) 0.0001(9) C6 0.0357(11) 0.0388(10) 0.0357(11) 0.0068(9) 0.0055(8) 0.0009(9) C7 0.0394(11) 0.0409(11) 0.0331(10) 0.0031(9) 0.0051(8) 0.0032(9) C8 0.0355(11) 0.0368(10) 0.0310(10) 0.0001(8) 0.0014(8) -0.0001(8) C9 0.0424(13) 0.0598(13) 0.0484(13) 0.0054(10) 0.0091(10) 0.0047(10) C10 0.0371(11) 0.0452(11) 0.0354(11) -0.0008(9) 0.0120(9) -0.0014(9) C11 0.0460(14) 0.0599(14) 0.0552(15) 0.0096(12) 0.0021(12) -0.0091(12) C12 0.0649(18) 0.0564(15) 0.0745(18) 0.0144(13) 0.0113(14) -0.0119(14) C13 0.0692(18) 0.0619(16) 0.0532(16) 0.0166(13) 0.0169(13) 0.0087(14) C14 0.0595(16) 0.0735(17) 0.0426(14) 0.0081(12) 0.0022(12) 0.0034(14) C15 0.0514(14) 0.0569(14) 0.0385(12) 0.0007(11) 0.0055(10) -0.0092(12) C16 0.0597(15) 0.0426(13) 0.0529(14) -0.0057(10) 0.0232(11) 0.0015(11) C17 0.098(2) 0.0874(19) 0.0495(16) -0.0213(14) 0.0218(14) -0.0083(16) C18 0.0671(17) 0.0677(16) 0.0884(19) -0.0033(14) 0.0320(14) 0.0201(13) C19 0.0415(12) 0.0403(11) 0.0382(11) -0.0059(9) 0.0066(9) -0.0026(9) C20 0.0465(14) 0.0406(12) 0.0438(13) -0.0015(10) 0.0062(10) -0.0032(10) C21 0.0691(16) 0.0399(12) 0.0585(14) -0.0049(11) 0.0119(12) -0.0038(11) C22 0.097(2) 0.0509(14) 0.108(2) 0.0245(15) 0.0121(17) -0.0011(14) C23 0.0390(12) 0.0382(11) 0.0473(13) 0.0034(10) 0.0072(9) -0.0003(9) C24 0.096(2) 0.0566(14) 0.0637(16) -0.0164(13) 0.0098(14) -0.0297(14) C25 0.0418(13) 0.0411(11) 0.0474(13) 0.0051(10) 0.0100(10) 0.0041(10) C26 0.0722(18) 0.107(2) 0.0701(17) 0.0194(15) 0.0344(14) -0.0130(16) _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 1.200(2) . ? O2 C1 1.355(2) . ? O2 C4 1.476(2) . ? O3 C23 1.198(2) . ? O4 C23 1.319(2) . ? O4 C24 1.449(2) . ? O5 C25 1.202(2) . ? O6 C25 1.335(2) . ? O6 C26 1.449(2) . ? C1 C2 1.475(2) . ? C2 C3 1.377(2) . ? C2 C5 1.391(2) . ? C3 C8 1.401(2) . ? C3 C4 1.526(2) . ? C4 C10 1.521(2) . ? C4 C9 1.522(3) . ? C5 C6 1.393(2) . ? C5 C23 1.501(2) . ? C6 C7 1.412(2) . ? C6 C25 1.500(2) . ? C7 C8 1.411(2) . ? C7 C16 1.533(2) . ? C8 C19 1.516(2) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.380(3) . ? C10 C15 1.386(3) . ? C11 C12 1.385(3) . ? C11 H11 0.92(2) . ? C12 C13 1.364(3) . ? C12 H12 0.94(2) . ? C13 C14 1.376(3) . ? C13 H13 0.94(2) . ? C14 C15 1.371(3) . ? C14 H14 0.94(2) . ? C15 H15 0.968(17) . ? C16 C18 1.528(3) . ? C16 C17 1.530(3) . ? C16 H16 0.952(18) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.532(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.512(3) . ? C20 H20A 0.961(18) . ? C20 H20B 0.976(18) . ? C21 C22 1.509(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 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 C1 O2 C4 112.07(13) . . ? C23 O4 C24 116.54(16) . . ? C25 O6 C26 115.90(17) . . ? O1 C1 O2 122.48(17) . . ? O1 C1 C2 129.91(19) . . ? O2 C1 C2 107.61(16) . . ? C3 C2 C5 121.78(16) . . ? C3 C2 C1 109.23(16) . . ? C5 C2 C1 128.94(17) . . ? C2 C3 C8 121.69(16) . . ? C2 C3 C4 108.56(15) . . ? C8 C3 C4 129.75(16) . . ? O2 C4 C10 106.68(14) . . ? O2 C4 C9 105.61(14) . . ? C10 C4 C9 115.59(16) . . ? O2 C4 C3 102.33(13) . . ? C10 C4 C3 112.99(15) . . ? C9 C4 C3 112.28(15) . . ? C2 C5 C6 117.34(16) . . ? C2 C5 C23 121.14(16) . . ? C6 C5 C23 121.50(16) . . ? C5 C6 C7 121.82(16) . . ? C5 C6 C25 114.81(16) . . ? C7 C6 C25 123.28(16) . . ? C8 C7 C6 119.66(16) . . ? C8 C7 C16 118.26(17) . . ? C6 C7 C16 122.05(17) . . ? C3 C8 C7 117.50(16) . . ? C3 C8 C19 120.13(16) . . ? C7 C8 C19 122.29(15) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.89(19) . . ? C11 C10 C4 122.59(19) . . ? C15 C10 C4 119.51(17) . . ? C10 C11 C12 120.8(2) . . ? C10 C11 H11 119.5(13) . . ? C12 C11 H11 119.8(13) . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 122.4(14) . . ? C11 C12 H12 117.2(14) . . ? C12 C13 C14 119.5(2) . . ? C12 C13 H13 120.7(14) . . ? C14 C13 H13 119.8(14) . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H14 121.8(15) . . ? C13 C14 H14 118.0(15) . . ? C14 C15 C10 121.3(2) . . ? C14 C15 H15 118.9(11) . . ? C10 C15 H15 119.8(11) . . ? C18 C16 C17 113.06(18) . . ? C18 C16 C7 114.88(18) . . ? C17 C16 C7 111.96(18) . . ? C18 C16 H16 103.0(11) . . ? C17 C16 H16 106.5(12) . . ? C7 C16 H16 106.4(11) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 C20 112.92(16) . . ? C8 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C8 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 113.22(18) . . ? C21 C20 H20A 110.0(11) . . ? C19 C20 H20A 108.1(11) . . ? C21 C20 H20B 107.2(10) . . ? C19 C20 H20B 110.5(11) . . ? H20A C20 H20B 107.7(15) . . ? C22 C21 C20 113.7(2) . . ? C22 C21 H21A 108.8 . . ? C20 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 O4 125.42(19) . . ? O3 C23 C5 123.67(19) . . ? O4 C23 C5 110.91(16) . . ? O4 C24 H24A 109.5 . . ? O4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 O6 124.32(18) . . ? O5 C25 C6 123.68(19) . . ? O6 C25 C6 111.94(17) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 O2 C1 O1 -175.20(19) . . . . ? C4 O2 C1 C2 4.3(2) . . . . ? O1 C1 C2 C3 177.5(2) . . . . ? O2 C1 C2 C3 -2.0(2) . . . . ? O1 C1 C2 C5 0.1(4) . . . . ? O2 C1 C2 C5 -179.38(17) . . . . ? C5 C2 C3 C8 -2.9(3) . . . . ? C1 C2 C3 C8 179.48(16) . . . . ? C5 C2 C3 C4 176.60(16) . . . . ? C1 C2 C3 C4 -1.0(2) . . . . ? C1 O2 C4 C10 -123.61(16) . . . . ? C1 O2 C4 C9 112.90(17) . . . . ? C1 O2 C4 C3 -4.74(19) . . . . ? C2 C3 C4 O2 3.33(18) . . . . ? C8 C3 C4 O2 -177.22(17) . . . . ? C2 C3 C4 C10 117.65(17) . . . . ? C8 C3 C4 C10 -62.9(2) . . . . ? C2 C3 C4 C9 -109.45(18) . . . . ? C8 C3 C4 C9 70.0(2) . . . . ? C3 C2 C5 C6 -1.5(3) . . . . ? C1 C2 C5 C6 175.55(18) . . . . ? C3 C2 C5 C23 -179.57(17) . . . . ? C1 C2 C5 C23 -2.5(3) . . . . ? C2 C5 C6 C7 4.4(3) . . . . ? C23 C5 C6 C7 -177.58(17) . . . . ? C2 C5 C6 C25 -179.04(16) . . . . ? C23 C5 C6 C25 -1.0(3) . . . . ? C5 C6 C7 C8 -2.9(3) . . . . ? C25 C6 C7 C8 -179.14(17) . . . . ? C5 C6 C7 C16 174.81(18) . . . . ? C25 C6 C7 C16 -1.5(3) . . . . ? C2 C3 C8 C7 4.4(3) . . . . ? C4 C3 C8 C7 -175.00(17) . . . . ? C2 C3 C8 C19 -172.44(17) . . . . ? C4 C3 C8 C19 8.2(3) . . . . ? C6 C7 C8 C3 -1.5(3) . . . . ? C16 C7 C8 C3 -179.31(17) . . . . ? C6 C7 C8 C19 175.21(17) . . . . ? C16 C7 C8 C19 -2.5(3) . . . . ? O2 C4 C10 C11 -128.47(19) . . . . ? C9 C4 C10 C11 -11.4(3) . . . . ? C3 C4 C10 C11 119.9(2) . . . . ? O2 C4 C10 C15 53.0(2) . . . . ? C9 C4 C10 C15 170.10(17) . . . . ? C3 C4 C10 C15 -58.6(2) . . . . ? C15 C10 C11 C12 0.8(3) . . . . ? C4 C10 C11 C12 -177.69(19) . . . . ? C10 C11 C12 C13 -0.5(4) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C13 C14 C15 C10 0.6(3) . . . . ? C11 C10 C15 C14 -0.8(3) . . . . ? C4 C10 C15 C14 177.72(19) . . . . ? C8 C7 C16 C18 135.29(19) . . . . ? C6 C7 C16 C18 -42.4(3) . . . . ? C8 C7 C16 C17 -94.0(2) . . . . ? C6 C7 C16 C17 88.3(2) . . . . ? C3 C8 C19 C20 94.2(2) . . . . ? C7 C8 C19 C20 -82.4(2) . . . . ? C8 C19 C20 C21 -175.90(16) . . . . ? C19 C20 C21 C22 -178.56(18) . . . . ? C24 O4 C23 O3 -3.5(3) . . . . ? C24 O4 C23 C5 177.61(16) . . . . ? C2 C5 C23 O3 111.4(2) . . . . ? C6 C5 C23 O3 -66.5(3) . . . . ? C2 C5 C23 O4 -69.7(2) . . . . ? C6 C5 C23 O4 112.39(19) . . . . ? C26 O6 C25 O5 -5.1(3) . . . . ? C26 O6 C25 C6 177.60(17) . . . . ? C5 C6 C25 O5 -59.9(3) . . . . ? C7 C6 C25 O5 116.6(2) . . . . ? C5 C6 C25 O6 117.41(18) . . . . ? C7 C6 C25 O6 -66.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.223 _refine_diff_density_min -0.165 _refine_diff_density_rms 0.038