Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Thomas Braun' _publ_contact_author_address ; Fakultat fur Chemie Universitat Bielefeld Universitatsstr.25 Bielefeld 33615 GERMANY ; _publ_contact_author_email THOMAS.BRAUN@UNI-BIELEFELD.DE _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Routes to Unique Palladium A-Frame Complexes Bearing a Bridging Fluoro- Ligand ; loop_ _publ_author_name _publ_author_address 'Braun, Thomas' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Steffen, Andreas' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Schorlemer, Verena' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Neumann, Beate' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; data_complex5cx2THF _database_code_depnum_ccdc_archive 'CCDC 276221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 F P4 Pd2, 2(C4 H8 O), F2 H' _chemical_formula_sum 'C60 H67 F3 O2 P4 Pd2' _chemical_formula_weight 1213.82 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.6810(3) _cell_length_b 9.23800(10) _cell_length_c 25.2280(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.8150(6) _cell_angle_gamma 90.00 _cell_volume 5444.70(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8351 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8514 _exptl_absorpt_correction_T_max 0.9441 _exptl_absorpt_process_details 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57348 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7922 _reflns_number_gt 6861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 Rfactors 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^)+(0.0277P)^2^+5.5484P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7922 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _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 Pd1 Pd 0.436491(5) 0.708743(12) 0.238097(4) 0.01098(4) Uani 1 1 d . . . P1 P 0.417051(17) 0.76713(4) 0.144908(16) 0.01138(8) Uani 1 1 d . . . P2 P 0.454751(17) 0.68453(4) 0.333107(16) 0.01125(8) Uani 1 1 d . . . F1 F 0.5000 0.87688(14) 0.2500 0.0156(3) Uani 1 2 d S . . F2 F 0.46512(4) 1.06254(11) 0.51119(4) 0.0225(2) Uani 1 1 d . . . H2A H 0.5000 1.0000 0.5000 0.075(13) Uiso 1 2 d S . . C1 C 0.37058(7) 0.66143(17) 0.08703(6) 0.0133(3) Uani 1 1 d . . . C2 C 0.31189(7) 0.66391(18) 0.07880(7) 0.0159(3) Uani 1 1 d . . . H2 H 0.2977 0.7186 0.1034 0.019 Uiso 1 1 calc R . . C3 C 0.27404(7) 0.58722(19) 0.03501(7) 0.0185(3) Uani 1 1 d . . . H3 H 0.2341 0.5903 0.0296 0.022 Uiso 1 1 calc R . . C4 C 0.29441(7) 0.50587(19) -0.00097(7) 0.0198(3) Uani 1 1 d . . . H4 H 0.2685 0.4537 -0.0310 0.024 Uiso 1 1 calc R . . C5 C 0.35268(8) 0.5015(2) 0.00736(7) 0.0209(3) Uani 1 1 d . . . H5 H 0.3667 0.4452 -0.0169 0.025 Uiso 1 1 calc R . . C6 C 0.39092(7) 0.57883(19) 0.05100(7) 0.0184(3) Uani 1 1 d . . . H6 H 0.4308 0.5754 0.0563 0.022 Uiso 1 1 calc R . . C7 C 0.38424(6) 0.94618(17) 0.13281(6) 0.0136(3) Uani 1 1 d . . . C8 C 0.37165(7) 1.01194(18) 0.08022(7) 0.0163(3) Uani 1 1 d . . . H8 H 0.3781 0.9613 0.0500 0.020 Uiso 1 1 calc R . . C9 C 0.34962(7) 1.15180(19) 0.07241(7) 0.0187(3) Uani 1 1 d . . . H9 H 0.3411 1.1967 0.0368 0.022 Uiso 1 1 calc R . . C10 C 0.34005(7) 1.22621(18) 0.11650(7) 0.0194(3) Uani 1 1 d . . . H10 H 0.3253 1.3220 0.1110 0.023 Uiso 1 1 calc R . . C11 C 0.35202(7) 1.16107(19) 0.16841(7) 0.0192(3) Uani 1 1 d . . . H11 H 0.3453 1.2119 0.1984 0.023 Uiso 1 1 calc R . . C12 C 0.37391(7) 1.02079(18) 0.17658(7) 0.0166(3) Uani 1 1 d . . . H12 H 0.3818 0.9759 0.2122 0.020 Uiso 1 1 calc R . . C13 C 0.39829(7) 0.74975(18) 0.35919(6) 0.0135(3) Uani 1 1 d . . . C14 C 0.41002(7) 0.82492(19) 0.40954(7) 0.0184(3) Uani 1 1 d . . . H14 H 0.4484 0.8490 0.4304 0.022 Uiso 1 1 calc R . . C15 C 0.36563(7) 0.8648(2) 0.42932(7) 0.0210(3) Uani 1 1 d . . . H15 H 0.3738 0.9171 0.4634 0.025 Uiso 1 1 calc R . . C16 C 0.30971(7) 0.8287(2) 0.39954(8) 0.0226(4) Uani 1 1 d . . . H16 H 0.2797 0.8532 0.4138 0.027 Uiso 1 1 calc R . . C17 C 0.29751(7) 0.7566(2) 0.34880(8) 0.0244(4) Uani 1 1 d . . . H17 H 0.2590 0.7336 0.3280 0.029 Uiso 1 1 calc R . . C18 C 0.34146(7) 0.71804(19) 0.32829(7) 0.0195(3) Uani 1 1 d . . . H18 H 0.3329 0.6700 0.2932 0.023 Uiso 1 1 calc R . . C19 C 0.47053(6) 0.50333(17) 0.36218(6) 0.0134(3) Uani 1 1 d . . . C20 C 0.46156(7) 0.46359(19) 0.41225(7) 0.0173(3) Uani 1 1 d . . . H20 H 0.4453 0.5309 0.4313 0.021 Uiso 1 1 calc R . . C21 C 0.47648(7) 0.32544(19) 0.43420(7) 0.0207(3) Uani 1 1 d . . . H21 H 0.4704 0.2987 0.4682 0.025 Uiso 1 1 calc R . . C22 C 0.50026(8) 0.22681(19) 0.40658(8) 0.0220(4) Uani 1 1 d . . . H22 H 0.5107 0.1329 0.4218 0.026 Uiso 1 1 calc R . . C23 C 0.50884(8) 0.26525(19) 0.35649(8) 0.0213(3) Uani 1 1 d . . . H23 H 0.5250 0.1976 0.3375 0.026 Uiso 1 1 calc R . . C24 C 0.49376(7) 0.40266(18) 0.33438(7) 0.0164(3) Uani 1 1 d . . . H24 H 0.4993 0.4283 0.3000 0.020 Uiso 1 1 calc R . . C25 C 0.48383(6) 0.79882(17) 0.12920(6) 0.0134(3) Uani 1 1 d . . . H25A H 0.4950 0.9013 0.1376 0.016 Uiso 1 1 calc R . . H25B H 0.4760 0.7845 0.0885 0.016 Uiso 1 1 calc R . . C26 C 0.37900(7) 0.54242(18) 0.22016(7) 0.0176(3) Uani 1 1 d . . . H26A H 0.3402 0.5812 0.2038 0.026 Uiso 1 1 calc R . . H26B H 0.3817 0.4898 0.2546 0.026 Uiso 1 1 calc R . . H26C H 0.3875 0.4764 0.1935 0.026 Uiso 1 1 calc R . . O1 O 0.29313(8) 0.2286(2) 0.27571(6) 0.0460(4) Uani 1 1 d . . . C27 C 0.26724(9) 0.3458(2) 0.29602(9) 0.0335(4) Uani 1 1 d . . . H27A H 0.2265 0.3242 0.2907 0.040 Uiso 1 1 calc R . . H27B H 0.2693 0.4362 0.2757 0.040 Uiso 1 1 calc R . . C28 C 0.30060(10) 0.3618(2) 0.35790(8) 0.0346(5) Uani 1 1 d . . . H28A H 0.2754 0.3930 0.3794 0.042 Uiso 1 1 calc R . . H28B H 0.3324 0.4318 0.3640 0.042 Uiso 1 1 calc R . . C29 C 0.32294(9) 0.2090(2) 0.37383(9) 0.0313(4) Uani 1 1 d . . . H29A H 0.3577 0.2089 0.4072 0.038 Uiso 1 1 calc R . . H29B H 0.2935 0.1462 0.3810 0.038 Uiso 1 1 calc R . . C30 C 0.33621(9) 0.1621(3) 0.32168(9) 0.0357(5) Uani 1 1 d . . . H30A H 0.3748 0.1953 0.3232 0.043 Uiso 1 1 calc R . . H30B H 0.3345 0.0554 0.3179 0.043 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 Pd1 0.01146(6) 0.01156(6) 0.00978(6) 0.00008(4) 0.00323(4) -0.00073(4) P1 0.01135(17) 0.01251(19) 0.01009(16) 0.00022(14) 0.00321(13) 0.00016(14) P2 0.01150(17) 0.01215(18) 0.01016(16) 0.00029(14) 0.00360(13) -0.00026(14) F1 0.0130(6) 0.0169(7) 0.0167(6) 0.000 0.0042(5) 0.000 F2 0.0272(5) 0.0233(5) 0.0172(5) -0.0006(4) 0.0074(4) -0.0042(4) C1 0.0142(7) 0.0137(7) 0.0109(6) 0.0018(5) 0.0026(5) -0.0006(6) C2 0.0143(7) 0.0162(7) 0.0171(7) -0.0003(6) 0.0049(6) -0.0004(6) C3 0.0142(7) 0.0193(8) 0.0196(7) 0.0025(6) 0.0023(6) -0.0032(6) C4 0.0210(8) 0.0198(8) 0.0151(7) -0.0002(6) 0.0010(6) -0.0060(6) C5 0.0224(8) 0.0231(9) 0.0169(7) -0.0054(7) 0.0059(6) -0.0009(7) C6 0.0156(7) 0.0224(8) 0.0159(7) -0.0028(6) 0.0032(6) 0.0005(6) C7 0.0109(7) 0.0135(7) 0.0166(7) 0.0006(6) 0.0047(5) -0.0002(5) C8 0.0174(7) 0.0158(8) 0.0145(7) -0.0004(6) 0.0037(6) 0.0005(6) C9 0.0188(8) 0.0165(8) 0.0178(7) 0.0028(6) 0.0017(6) 0.0007(6) C10 0.0161(7) 0.0142(8) 0.0266(8) 0.0000(6) 0.0051(6) 0.0030(6) C11 0.0177(8) 0.0186(8) 0.0227(8) -0.0038(7) 0.0086(6) 0.0015(6) C12 0.0162(7) 0.0173(8) 0.0171(7) 0.0006(6) 0.0065(6) 0.0015(6) C13 0.0137(7) 0.0140(7) 0.0142(7) 0.0002(6) 0.0063(6) -0.0007(6) C14 0.0154(7) 0.0232(9) 0.0169(7) -0.0024(6) 0.0057(6) -0.0007(6) C15 0.0212(8) 0.0251(9) 0.0193(8) -0.0048(7) 0.0101(7) 0.0000(7) C16 0.0175(8) 0.0267(9) 0.0265(9) -0.0029(7) 0.0110(7) 0.0012(7) C17 0.0136(8) 0.0328(10) 0.0265(9) -0.0070(8) 0.0062(7) -0.0007(7) C18 0.0148(7) 0.0231(9) 0.0200(8) -0.0040(7) 0.0047(6) 0.0003(6) C19 0.0130(7) 0.0130(7) 0.0132(7) 0.0021(6) 0.0028(5) -0.0005(5) C20 0.0181(7) 0.0189(8) 0.0157(7) 0.0017(6) 0.0066(6) 0.0008(6) C21 0.0212(8) 0.0216(9) 0.0190(8) 0.0069(7) 0.0061(6) -0.0006(7) C22 0.0214(8) 0.0175(8) 0.0268(9) 0.0078(7) 0.0074(7) 0.0033(6) C23 0.0208(8) 0.0172(8) 0.0279(9) 0.0020(7) 0.0104(7) 0.0042(7) C24 0.0164(7) 0.0163(8) 0.0180(7) 0.0018(6) 0.0077(6) 0.0003(6) C25 0.0116(7) 0.0149(7) 0.0135(7) 0.0020(6) 0.0040(5) 0.0007(6) C26 0.0183(8) 0.0168(8) 0.0176(7) -0.0016(6) 0.0054(6) -0.0070(6) O1 0.0506(10) 0.0597(11) 0.0238(7) 0.0007(7) 0.0066(7) 0.0231(9) C27 0.0305(10) 0.0317(11) 0.0341(10) -0.0006(9) 0.0045(8) 0.0016(9) C28 0.0394(12) 0.0318(11) 0.0299(10) 0.0000(9) 0.0074(9) -0.0071(9) C29 0.0313(10) 0.0345(11) 0.0287(10) 0.0024(8) 0.0107(8) -0.0044(9) C30 0.0290(10) 0.0479(13) 0.0311(10) 0.0090(10) 0.0110(8) 0.0094(10) _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 Pd1 C26 2.0407(16) . ? Pd1 F1 2.1578(10) . ? Pd1 P2 2.3025(4) . ? Pd1 P1 2.3066(4) . ? Pd1 Pd1 2.9956(2) 2_655 ? P1 C1 1.8223(16) . ? P1 C7 1.8236(16) . ? P1 C25 1.8387(15) . ? P2 C19 1.8187(16) . ? P2 C13 1.8247(16) . ? P2 C25 1.8405(16) 2_655 ? F1 Pd1 2.1578(10) 2_655 ? F2 H2A 1.1452(10) . ? C1 C2 1.396(2) . ? C1 C6 1.398(2) . ? C2 C3 1.389(2) . ? C3 C4 1.391(2) . ? C4 C5 1.385(2) . ? C5 C6 1.394(2) . ? C7 C12 1.393(2) . ? C7 C8 1.400(2) . ? C8 C9 1.391(2) . ? C9 C10 1.391(2) . ? C10 C11 1.384(2) . ? C11 C12 1.394(2) . ? C13 C14 1.394(2) . ? C13 C18 1.398(2) . ? C14 C15 1.392(2) . ? C15 C16 1.383(2) . ? C16 C17 1.387(2) . ? C17 C18 1.391(2) . ? C19 C24 1.395(2) . ? C19 C20 1.400(2) . ? C20 C21 1.393(2) . ? C21 C22 1.387(3) . ? C22 C23 1.393(2) . ? C23 C24 1.388(2) . ? C25 P2 1.8404(16) 2_655 ? O1 C27 1.433(3) . ? O1 C30 1.434(3) . ? C27 C28 1.519(3) . ? C28 C29 1.521(3) . ? C29 C30 1.518(3) . ? 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 C26 Pd1 F1 174.11(5) . . ? C26 Pd1 P2 92.66(5) . . ? F1 Pd1 P2 92.038(11) . . ? C26 Pd1 P1 92.80(5) . . ? F1 Pd1 P1 82.906(12) . . ? P2 Pd1 P1 171.997(15) . . ? C26 Pd1 Pd1 130.71(5) . 2_655 ? F1 Pd1 Pd1 46.04(2) . 2_655 ? P2 Pd1 Pd1 87.162(11) . 2_655 ? P1 Pd1 Pd1 93.702(11) . 2_655 ? C1 P1 C7 102.77(7) . . ? C1 P1 C25 106.79(7) . . ? C7 P1 C25 101.54(7) . . ? C1 P1 Pd1 124.17(5) . . ? C7 P1 Pd1 108.53(5) . . ? C25 P1 Pd1 110.53(5) . . ? C19 P2 C13 104.33(7) . . ? C19 P2 C25 106.62(7) . 2_655 ? C13 P2 C25 102.82(7) . 2_655 ? C19 P2 Pd1 116.99(5) . . ? C13 P2 Pd1 115.31(5) . . ? C25 P2 Pd1 109.53(5) 2_655 . ? Pd1 F1 Pd1 87.92(5) 2_655 . ? C2 C1 C6 119.03(14) . . ? C2 C1 P1 117.72(12) . . ? C6 C1 P1 123.25(12) . . ? C3 C2 C1 120.63(15) . . ? C2 C3 C4 120.17(15) . . ? C5 C4 C3 119.52(15) . . ? C4 C5 C6 120.67(16) . . ? C5 C6 C1 119.98(15) . . ? C12 C7 C8 119.67(15) . . ? C12 C7 P1 120.07(12) . . ? C8 C7 P1 120.20(12) . . ? C9 C8 C7 119.64(15) . . ? C10 C9 C8 120.34(15) . . ? C11 C10 C9 120.16(15) . . ? C10 C11 C12 119.90(15) . . ? C7 C12 C11 120.28(15) . . ? C14 C13 C18 119.26(15) . . ? C14 C13 P2 122.33(12) . . ? C18 C13 P2 118.37(12) . . ? C15 C14 C13 120.16(15) . . ? C16 C15 C14 120.28(16) . . ? C15 C16 C17 119.92(16) . . ? C16 C17 C18 120.22(16) . . ? C17 C18 C13 120.09(16) . . ? C24 C19 C20 119.30(15) . . ? C24 C19 P2 118.69(11) . . ? C20 C19 P2 121.98(12) . . ? C21 C20 C19 120.04(16) . . ? C22 C21 C20 120.17(16) . . ? C21 C22 C23 120.07(16) . . ? C24 C23 C22 119.88(16) . . ? C23 C24 C19 120.53(15) . . ? P1 C25 P2 116.32(8) . 2_655 ? C27 O1 C30 109.52(16) . . ? O1 C27 C28 106.52(17) . . ? C27 C28 C29 102.22(17) . . ? C30 C29 C28 101.34(17) . . ? O1 C30 C29 105.53(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.776 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.077