# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Hideki Yamochi' _publ_contact_author_address ; Research Center for Low Temperature & Materials Kyoto University Kyoto Sakyo-ku 606-8502 JAPAN ; _publ_contact_author_email YAMOCHI@KUCHEM.KYOTO-U.AC.JP _publ_section_title ; Synthesis and Charge-transfer Complexes of a New Donor Molecule, TP-EDOT ; loop_ _publ_author_name 'Hideki Yamochi' 'Jun Hagiwara' 'G. Saito' 'Masaya Soeda' data_soe4-2 _database_code_depnum_ccdc_archive 'CCDC 280993' _publ_section_abstract ; We present the crystal and molecular structure of PF6-no.3. ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description needle _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.742 _exptl_crystal_F_000 1332 _chemical_formula_moiety 'C20 H16 O4 S6 P1 F6' _chemical_formula_sum 'C20 H16 F6 O4 P1 S6' _chemical_formula_weight 657.70 _cell_length_a 16.029(3) _cell_length_b 23.026(4) _cell_length_c 7.003(4) _cell_angle_alpha 90.000000(0) _cell_angle_beta 103.96(3) _cell_angle_gamma 90.000000(0) _cell_volume 2508(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_formula_units_Z 4 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.650 _cell_measurement_temperature 'room temperature' _diffrn_measurement_device 'Mac Science M03XHF22' _diffrn_measurement_method theta/2theta _exptl_absorpt_correction_type none _diffrn_reflns_number 3291 _reflns_number_total 2558 _reflns_number_observed 1913 _reflns_observed_criterion refl_observed_if_I_>_2.00_sigma(I) _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.052 _refine_ls_wR_factor_obs 0.060 _refine_ls_hydrogen_treatment refU _refine_ls_number_reflns 1913 _refine_ls_number_parameters 176 _refine_ls_goodness_of_fit_obs 2.872 _refine_ls_weighting_scheme Unit _refine_ls_shift/esd_max 0.4341 _refine_ls_shift/esd_mean 0.0217 _refine_diff_density_min -0.39 _refine_diff_density_max 0.39 _refine_ls_extinction_method None _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_molecular_graphics Crystan _computing_publication_material Crystan _computing_structure_refinement Crystan _computing_structure_solution Crystan _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.02647 _diffrn_orient_matrix_UB_12 -0.03956 _diffrn_orient_matrix_UB_13 -0.01794 _diffrn_orient_matrix_UB_21 0.05853 _diffrn_orient_matrix_UB_22 -0.01790 _diffrn_orient_matrix_UB_23 0.03682 _diffrn_orient_matrix_UB_31 -0.00246 _diffrn_orient_matrix_UB_32 -0.00036 _diffrn_orient_matrix_UB_33 0.14133 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X+1/2,-Y+1/2,-Z +X+1/2,+Y+1/2,+Z -X,+Y,-Z+1/2 +X,-Y,+Z+1/2 +X+1/2,-Y+1/2,+Z+1/2 -X+1/2,+Y+1/2,-Z+1/2 _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_cell_setting Monoclinic #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.13780(9) 0.17910(6) 0.09270(24) 0.0455(7) 1.000 Uij S2 0.07950(9) 0.05780(6) 0.04880(27) 0.0536(7) 1.000 Uij S3 -0.22560(9) 0.19300(7) -0.15210(26) 0.0562(8) 1.000 Uij P1 0.00000 0.38920(9) 0.25000 0.0494(6) 1.000 Uij F1 0.0012(3) 0.4379(2) 0.0908(7) 0.083(3) 1.000 Uij F2 -0.1024(2) 0.3903(2) 0.1887(7) 0.087(3) 1.000 Uij F3 0.0012(3) 0.3420(2) 0.0892(8) 0.109(3) 1.000 Uij O1 0.2987(2) 0.1428(2) 0.1804(7) 0.057(2) 1.000 Uij O2 0.2423(2) 0.0229(2) 0.1393(7) 0.063(2) 1.000 Uij C1 0.0513(3) 0.1311(2) 0.0330(8) 0.037(2) 1.000 Uij C2 0.2156(3) 0.1250(2) 0.1314(9) 0.044(3) 1.000 Uij C3 0.1899(3) 0.0700(2) 0.1111(9) 0.047(3) 1.000 Uij C4 0.3556(4) 0.0940(3) 0.1645(12) 0.072(4) 1.000 Uij C5 0.3282(4) 0.0401(3) 0.2494(13) 0.075(4) 1.000 Uij C6 -0.0325(3) 0.1497(2) -0.0212(8) 0.038(2) 1.000 Uij C7 -0.0522(3) 0.2108(2) -0.0355(9) 0.047(3) 1.000 Uij C8 -0.1027(3) 0.1091(2) -0.0669(9) 0.044(3) 1.000 Uij C9 -0.1321(4) 0.2324(2) -0.0899(10) 0.056(3) 1.000 Uij C10 -0.1863(3) 0.1233(3) -0.1229(9) 0.049(3) 1.000 Uij H4A 0.342(6) 0.073(4) 0.036(15) 0.12(3) 1.000 Uiso H4B 0.415(5) 0.107(3) 0.230(10) 0.11(3) 1.000 Uiso H5A 0.319(5) 0.041(4) 0.386(14) 0.11(3) 1.000 Uiso H5B 0.365(5) 0.007(3) 0.225(11) 0.10(3) 1.000 Uiso H7 -0.005(4) 0.239(3) 0.016(10) 0.08(2) 1.000 Uiso H8 -0.088(4) 0.067(3) -0.045(9) 0.06(2) 1.000 Uiso H9 -0.142(5) 0.275(3) -0.074(11) 0.09(2) 1.000 Uiso H10 -0.228(5) 0.091(4) -0.126(12) 0.13(3) 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0379(7) 0.0325(6) 0.0631(9) -.0056(5) 0.0123(6) -.0045(6) S2 0.0334(7) 0.0303(7) 0.0901(12) -.0004(6) 0.0021(7) -.0013(7) S3 0.0390(8) 0.0561(9) 0.0703(11) 0.0143(7) 0.0135(7) -.0012(8) P1 0.033(1) 0.041(1) 0.068(2) 0.000 0.002(1) 0.000 F1 0.065(2) 0.080(3) 0.095(3) -0.010(2) 0.008(2) 0.027(2) F2 0.035(2) 0.110(3) 0.108(4) -0.015(2) 0.002(2) 0.009(3) F3 0.098(3) 0.080(3) 0.141(4) -0.011(3) 0.022(3) -0.058(3) O1 0.034(2) 0.059(3) 0.074(3) -0.009(2) 0.007(2) -0.008(2) O2 0.035(2) 0.047(2) 0.099(4) 0.010(2) -0.007(2) -0.005(2) C1 0.036(3) 0.027(2) 0.045(3) -0.001(2) 0.008(2) -0.002(2) C2 0.029(2) 0.049(3) 0.050(3) -0.002(2) 0.005(2) -0.001(3) C3 0.033(3) 0.040(3) 0.062(4) 0.003(2) 0.004(3) -0.002(3) C4 0.031(3) 0.087(5) 0.092(6) 0.005(3) 0.008(3) -0.009(5) C5 0.041(3) 0.069(5) 0.105(7) 0.012(3) -0.002(4) 0.001(4) C6 0.038(3) 0.032(3) 0.041(3) 0.001(2) 0.010(2) -0.001(2) C7 0.041(3) 0.030(3) 0.068(4) 0.000(2) 0.016(3) -0.002(3) C8 0.037(3) 0.032(3) 0.059(4) -0.001(2) 0.006(2) -0.001(2) C9 0.048(3) 0.038(3) 0.079(4) 0.009(3) 0.023(3) 0.002(3) C10 0.038(3) 0.045(3) 0.058(4) 0.001(2) 0.008(3) -0.004(3) 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 C2 S1 C1 S2 2.5(4) . . . . yes C1 S1 C2 O1 178.7(5) . . . . yes C1 S1 C2 C3 -1.3(5) . . . . yes C2 S1 C1 C6 -177.8(5) . . . . yes C3 S2 C1 S1 -2.7(4) . . . . yes C1 S2 C3 O2 -179.6(5) . . . . yes C1 S2 C3 C2 1.9(5) . . . . yes C3 S2 C1 C6 177.6(5) . . . . yes C10 S3 C9 C7 0.3(6) . . . . yes C9 S3 C10 C8 -0.5(6) . . . . yes C4 O1 C2 S1 -167.3(6) . . . . yes C4 O1 C2 C3 12.6(6) . . . . yes C2 O1 C4 C5 -43.2(6) . . . . yes C5 O2 C3 S2 -161.8(7) . . . . yes C5 O2 C3 C2 16.5(6) . . . . yes C3 O2 C5 C4 -46.6(6) . . . . yes S1 C1 C6 C7 1.5(5) . . . . yes S1 C1 C6 C8 -179.1(8) . . . . yes S2 C1 C6 C7 -178.8(8) . . . . yes S2 C1 C6 C8 0.6(4) . . . . yes S1 C2 C3 S2 -0.5(3) . . . . yes S1 C2 C3 O2 -178.8(8) . . . . yes O1 C2 C3 S2 179.6(8) . . . . yes O1 C2 C3 O2 1.2(6) . . . . yes O1 C4 C5 O2 62.8(7) . . . . yes C1 C6 C7 C9 179.1(9) . . . . yes C1 C6 C8 C10 -179.3(9) . . . . yes C8 C6 C7 C9 -0.4(6) . . . . yes C7 C6 C8 C10 0.1(6) . . . . yes C6 C7 C9 S3 0.1(5) . . . . yes C6 C8 C10 S3 0.4(5) . . . . yes C10 S3 C9 H9 -169.4(45) . . . . yes C9 S3 C10 H10 169.1(53) . . . . yes C2 O1 C4 H4A 52.6(61) . . . . yes C2 O1 C4 H4B -167.7(43) . . . . yes C3 O2 C5 H5A 79.8(53) . . . . yes C3 O2 C5 H5B -162.3(45) . . . . yes O1 C4 C5 H5A -52.1(59) . . . . yes O1 C4 C5 H5B 175.3(46) . . . . yes H4A C4 C5 O2 -53.7(55) . . . . yes H4A C4 C5 H5A -168.6(81) . . . . yes H4A C4 C5 H5B 58.8(71) . . . . yes H4B C4 C5 O2 -177.0(45) . . . . yes H4B C4 C5 H5A 68.1(74) . . . . yes H4B C4 C5 H5B -64.5(63) . . . . yes C1 C6 C7 H7 -10.1(45) . . . . yes C1 C6 C8 H8 5.9(39) . . . . yes C8 C6 C7 H7 170.5(45) . . . . yes C7 C6 C8 H8 -174.7(40) . . . . yes C6 C7 C9 H9 169.1(48) . . . . yes H7 C7 C9 S3 -170.9(44) . . . . yes H7 C7 C9 H9 -1.9(64) . . . . yes C6 C8 C10 H10 -169.4(53) . . . . yes H8 C8 C10 S3 175.2(40) . . . . yes H8 C8 C10 H10 5.4(65) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.743(5) . . yes S1 C2 1.737(6) . . yes S2 C1 1.744(5) . . yes S2 C3 1.740(6) . . yes S3 C9 1.716(7) . . yes S3 C10 1.718(6) . . yes P1 F1 1.585(5) . . yes P1 F1 1.585(5) . 5_555 yes P1 F2 1.593(4) . . yes P1 F2 1.593(4) . 5_555 yes P1 F3 1.568(6) . . yes P1 F3 1.568(6) . 5_555 yes O1 C2 1.356(7) . . yes O1 C4 1.468(9) . . yes O2 C3 1.357(7) . . yes O2 C5 1.461(8) . . yes C1 C6 1.373(7) . . yes C2 C3 1.329(8) . . yes C4 C5 1.488(12) . . yes C6 C7 1.440(8) . . yes C6 C8 1.438(8) . . yes C7 C9 1.341(8) . . yes C8 C10 1.343(8) . . yes C4 H4A 1.00(10) . . yes C4 H4B 1.00(8) . . yes C5 H5A 1.00(10) . . yes C5 H5B 1.00(8) . . yes C7 H7 1.00(7) . . yes C8 H8 1.00(7) . . yes C9 H9 1.00(7) . . yes C10 H10 1.00(9) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 94.7(3) . . . yes C1 S2 C3 95.3(3) . . . yes C9 S3 C10 101.0(3) . . . yes F1 P1 F1 89.9(3) . . 5_555 yes F1 P1 F2 89.2(3) . . . yes F1 P1 F2 89.5(3) . . 5_555 yes F1 P1 F3 88.9(3) . . . yes F1 P1 F3 178.8(3) . . 5_555 yes F1 P1 F2 89.5(3) 5_555 . . yes F1 P1 F2 89.2(3) 5_555 . 5_555 yes F1 P1 F3 178.8(3) 5_555 . . yes F1 P1 F3 88.9(3) 5_555 . 5_555 yes F2 P1 F2 178.2(3) . . 5_555 yes F2 P1 F3 90.4(3) . . . yes F2 P1 F3 90.8(3) . . 5_555 yes F2 P1 F3 90.8(3) 5_555 . . yes F2 P1 F3 90.4(3) 5_555 . 5_555 yes F3 P1 F3 92.3(3) . . 5_555 yes C2 O1 C4 109.9(5) . . . yes C3 O2 C5 109.4(5) . . . yes S1 C1 S2 114.8(3) . . . yes S1 C1 C6 122.5(4) . . . yes S2 C1 C6 122.7(4) . . . yes S1 C2 O1 116.6(4) . . . yes S1 C2 C3 118.3(5) . . . yes O1 C2 C3 125.1(5) . . . yes S2 C3 O2 117.6(4) . . . yes S2 C3 C2 116.8(5) . . . yes O2 C3 C2 125.5(5) . . . yes O1 C4 C5 111.1(6) . . . yes O2 C5 C4 110.3(7) . . . yes C1 C6 C7 120.5(5) . . . yes C1 C6 C8 121.3(5) . . . yes C7 C6 C8 118.2(5) . . . yes C6 C7 C9 124.1(5) . . . yes C6 C8 C10 125.4(5) . . . yes S3 C9 C7 126.3(5) . . . yes S3 C10 C8 125.0(5) . . . yes O1 C4 H4A 116.2(54) . . . yes O1 C4 H4B 106.6(41) . . . yes C5 C4 H4A 85.8(55) . . . yes C5 C4 H4B 113.8(41) . . . yes H4A C4 H4B 122.0(66) . . . yes O2 C5 H5A 100.1(50) . . . yes O2 C5 H5B 103.4(43) . . . yes C4 C5 H5A 119.1(51) . . . yes C4 C5 H5B 108.4(43) . . . yes H5A C5 H5B 114.0(67) . . . yes C6 C7 H7 119.0(39) . . . yes C9 C7 H7 116.3(39) . . . yes C6 C8 H8 116.8(34) . . . yes C10 C8 H8 117.6(34) . . . yes S3 C9 H9 113.0(41) . . . yes C7 C9 H9 119.9(41) . . . yes S3 C10 H10 118.2(47) . . . yes C8 C10 H10 116.0(47) . . . yes #=================================================== #===END data_sb _database_code_depnum_ccdc_archive 'CCDC 280994' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (TP-EDOT)3Sb2F11(benzene) _chemical_formula_moiety 'C36 H30 F11 O6 S9 Sb2' _chemical_formula_sum 'C36 H30 F11 O6 S9 Sb2' _chemical_formula_weight 1299.64 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' S S 0.1246 0.1234 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 19.599(5) _cell_length_b 10.953(3) _cell_length_c 10.555(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.11(2) _cell_angle_gamma 90.00 _cell_volume 2223.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 'room temperature' _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.6268 _exptl_crystal_size_mid 0.1454 _exptl_crystal_size_min 0.08332 _exptl_crystal_density_diffrn 1.942 _exptl_crystal_F_000 1278 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.866 _exptl_special_details ; ? ; _diffrn_ambient_temperature 'room temperature' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science M03XHF22' _diffrn_measurement_method theta/2theta _diffrn_reflns_number 5023 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5372 _reflns_number_gt 3196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Crystan _computing_publication_material Crystan _refine_special_details ; Refinement of F^2^ against ALL reflections. Although it is not recommended, F^2^ data were obtained as the square of F having non-zero intensity due to the limitation of the diffractometer which outputs F as the diffraction data. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+14.2618P] 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 4611 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1749 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _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 Sb1 Sb 0.21185(5) 0.2500 0.73614(9) 0.0435(3) Uani 1 d S . . Sb2 Sb 0.22755(5) 0.2500 0.40344(9) 0.0473(3) Uani 1 d S . . S1 S 0.09398(18) 0.7500 0.2158(4) 0.0564(10) Uani 1 d S . . S2 S 0.37537(11) 0.6166(2) 0.2488(2) 0.0401(5) Uani 1 d . . . S3 S 0.4693(2) 0.7500 0.5808(4) 0.0670(12) Uani 1 d S . . S4 S 0.18881(12) 0.6175(2) 0.5593(2) 0.0458(6) Uani 1 d . . . S5 S 0.16266(19) 0.7500 0.8968(4) 0.0556(10) Uani 1 d S . . S6 S 0.44488(12) 0.8852(2) 0.9120(2) 0.0428(5) Uani 1 d . . . F1 F 0.2279(12) 0.2933(12) 0.5730(14) 0.137(8) Uani 0.50 d P . . F2 F 0.2014(8) 0.2097(17) 0.9036(11) 0.097(9) Uani 0.50 d P . . F3 F 0.2871(13) 0.143(3) 0.810(2) 0.080(7) Uani 0.50 d P . . F4 F 0.2735(13) 0.121(3) 0.751(2) 0.074(7) Uani 0.50 d P . . F5 F 0.141(2) 0.127(4) 0.730(4) 0.125(15) Uani 0.50 d P . . F6 F 0.1455(15) 0.135(3) 0.681(3) 0.083(8) Uani 0.50 d P . . F7 F 0.2287(9) 0.2072(18) 0.2321(12) 0.114(10) Uani 0.50 d P . . F8 F 0.1608(14) 0.125(2) 0.4029(17) 0.075(6) Uani 0.50 d P . . F9 F 0.1579(17) 0.141(3) 0.339(2) 0.111(9) Uani 0.50 d P . . F10 F 0.2929(11) 0.1246(19) 0.3913(19) 0.083(6) Uani 0.50 d P . . F11 F 0.2978(13) 0.139(3) 0.460(2) 0.133(11) Uani 0.50 d P . . O1 O 0.5128(3) 0.6186(6) 0.2757(7) 0.0499(16) Uani 1 d . . . O2 O 0.0518(4) 0.6185(8) 0.5366(8) 0.071(2) Uani 1 d . . . O3 O 0.5765(3) 0.8817(6) 0.8834(6) 0.0498(16) Uani 1 d . . . C1 C 0.1500(5) 0.6289(9) 0.2305(9) 0.045(2) Uani 1 d . . . H1 H 0.1301 0.5450 0.2318 0.054 Uiso 1 calc . . . C2 C 0.2201(5) 0.6393(9) 0.2407(9) 0.044(2) Uani 1 d . . . H2 H 0.2480 0.5623 0.2495 0.053 Uiso 1 calc . . . C3 C 0.2560(7) 0.7500 0.2395(11) 0.037(3) Uani 1 d S . . C4 C 0.3291(7) 0.7500 0.2472(11) 0.034(3) Uani 1 d S . . C5 C 0.4549(4) 0.6892(8) 0.2627(8) 0.0392(19) Uani 1 d . . . C6 C 0.5730(6) 0.6922(15) 0.2816(18) 0.121(7) Uani 1 d . . . H6A H 0.6062 0.6667 0.3614 0.145 Uiso 1 calc . . . H6B H 0.5944 0.6667 0.2070 0.145 Uiso 1 calc . . . C7 C 0.4116(5) 0.8722(9) 0.5734(9) 0.049(2) Uani 1 d . . . H7 H 0.4310 0.9564 0.5700 0.058 Uiso 1 calc . . . C8 C 0.3446(5) 0.8623(10) 0.5721(10) 0.054(3) Uani 1 d . . . H8 H 0.3177 0.9397 0.5739 0.065 Uiso 1 calc . . . C9 C 0.3068(7) 0.7500 0.5683(11) 0.039(3) Uani 1 d S . . C10 C 0.2355(6) 0.7500 0.5668(11) 0.032(3) Uani 1 d S . . C11 C 0.1098(5) 0.6894(10) 0.5460(9) 0.049(2) Uani 1 d . . . C12A C -0.0061(16) 0.691(3) 0.561(3) 0.089(9) Uiso 0.50 d P . . C12B C -0.0115(13) 0.691(2) 0.489(3) 0.070(7) Uiso 0.50 d P . . C13 C 0.2212(5) 0.6268(8) 0.9016(9) 0.044(2) Uani 1 d . . . H13 H 0.2015 0.5428 0.9032 0.053 Uiso 1 calc . . . C14 C 0.2875(4) 0.6351(8) 0.9031(8) 0.0366(19) Uani 1 d . . . H14 H 0.3143 0.5577 0.9007 0.044 Uiso 1 calc . . . C15 C 0.3250(7) 0.7500 0.9080(11) 0.036(3) Uani 1 d S . . C16 C 0.3961(7) 0.7500 0.9063(12) 0.037(3) Uani 1 d S . . C17 C 0.5204(4) 0.8106(8) 0.8946(8) 0.039(2) Uani 1 d . . . C18A C 0.6412(10) 0.8187(18) 0.916(2) 0.045(5) Uiso 0.50 d P . . C18B C 0.6338(10) 0.8078(19) 0.850(2) 0.049(5) Uiso 0.50 d P . . C19 C 0.0257(12) 0.4192(17) 0.096(2) 0.120(7) Uani 1 d . . . H19 H 0.0463 0.3610 0.1662 0.144 Uiso 1 calc . . . C20 C 0.0517(8) 0.4262(18) -0.019(3) 0.112(7) Uani 1 d . . . H20 H 0.0893 0.3686 -0.0330 0.135 Uiso 1 calc . . . C21 C 0.0276(11) 0.507(2) -0.1105(19) 0.108(6) Uani 1 d . . . H21 H 0.0487 0.5134 -0.1893 0.129 Uiso 1 calc . . . 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 Sb1 0.0371(5) 0.0495(6) 0.0440(5) 0.000 0.0076(4) 0.000 Sb2 0.0526(6) 0.0459(6) 0.0461(5) 0.000 0.0164(4) 0.000 S1 0.0306(17) 0.072(3) 0.066(2) 0.000 0.0075(16) 0.000 S2 0.0354(11) 0.0316(11) 0.0530(13) -0.0030(10) 0.0081(9) 0.0022(9) S3 0.047(2) 0.107(4) 0.046(2) 0.000 0.0050(17) 0.000 S4 0.0450(13) 0.0396(13) 0.0513(13) 0.0032(11) 0.0055(10) -0.0019(11) S5 0.0403(19) 0.071(3) 0.055(2) 0.000 0.0078(16) 0.000 S6 0.0464(13) 0.0290(11) 0.0565(14) -0.0039(10) 0.0184(11) -0.0017(10) F1 0.30(2) 0.059(10) 0.075(9) -0.001(7) 0.083(13) -0.016(12) F2 0.101(9) 0.15(3) 0.049(6) 0.009(8) 0.026(7) -0.020(11) F3 0.047(12) 0.087(18) 0.100(18) 0.044(16) -0.002(11) 0.020(11) F4 0.047(10) 0.053(10) 0.108(19) 0.025(13) -0.022(11) 0.009(8) F5 0.110(19) 0.092(18) 0.19(4) 0.02(2) 0.077(19) -0.010(15) F6 0.049(10) 0.070(13) 0.13(2) -0.017(15) 0.027(12) -0.045(9) F7 0.140(13) 0.16(3) 0.057(7) -0.025(9) 0.049(8) -0.037(13) F8 0.098(14) 0.063(10) 0.078(13) -0.019(12) 0.052(14) -0.036(10) F9 0.120(17) 0.117(19) 0.092(17) -0.031(18) 0.009(17) -0.035(14) F10 0.080(12) 0.070(11) 0.106(15) -0.034(11) 0.037(12) 0.017(9) F11 0.104(14) 0.15(2) 0.122(19) -0.071(16) -0.029(14) 0.085(13) O1 0.030(3) 0.041(4) 0.075(4) -0.001(3) 0.003(3) 0.009(3) O2 0.048(4) 0.071(5) 0.090(6) 0.003(5) 0.007(4) -0.015(4) O3 0.041(4) 0.039(4) 0.072(4) -0.007(3) 0.018(3) -0.008(3) C1 0.052(6) 0.039(5) 0.045(5) -0.010(4) 0.011(4) -0.011(5) C2 0.038(5) 0.040(5) 0.053(6) -0.007(4) 0.007(4) -0.006(4) C3 0.042(7) 0.042(7) 0.026(6) 0.000 0.003(5) 0.000 C4 0.056(8) 0.018(5) 0.028(6) 0.000 0.008(6) 0.000 C5 0.037(5) 0.042(5) 0.039(5) -0.002(4) 0.006(4) 0.002(4) C6 0.029(6) 0.124(14) 0.209(18) 0.000(12) 0.023(8) 0.025(7) C7 0.059(6) 0.049(6) 0.037(5) -0.011(4) 0.006(4) -0.020(5) C8 0.049(6) 0.055(6) 0.060(6) -0.008(5) 0.016(5) -0.006(5) C9 0.045(7) 0.044(7) 0.028(6) 0.000 0.005(5) 0.000 C10 0.033(6) 0.031(6) 0.032(6) 0.000 0.004(5) 0.000 C11 0.036(5) 0.068(6) 0.044(5) 0.005(5) 0.007(4) -0.005(5) C13 0.053(6) 0.032(5) 0.051(5) -0.009(4) 0.018(4) -0.014(4) C14 0.044(5) 0.032(4) 0.034(4) 0.001(4) 0.009(4) 0.005(4) C15 0.044(7) 0.037(7) 0.025(6) 0.000 0.007(5) 0.000 C16 0.046(7) 0.027(6) 0.044(7) 0.000 0.023(6) 0.000 C17 0.044(5) 0.038(5) 0.037(5) -0.008(4) 0.010(4) 0.010(4) C19 0.103(13) 0.079(12) 0.159(19) -0.019(12) -0.021(13) -0.029(11) C20 0.078(10) 0.086(13) 0.19(2) -0.060(14) 0.057(13) -0.030(10) C21 0.107(14) 0.095(13) 0.127(15) -0.023(12) 0.037(12) -0.047(12) _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 Sb1 F6 1.82(2) . ? Sb1 F6 1.82(2) 4_565 ? Sb1 F4 1.84(3) 4_565 ? Sb1 F4 1.84(3) . ? Sb1 F1 1.870(14) 4_565 ? Sb1 F1 1.870(14) . ? Sb1 F2 1.871(12) . ? Sb1 F2 1.871(12) 4_565 ? Sb1 F3 1.93(3) 4_565 ? Sb1 F3 1.93(3) . ? Sb1 F5 1.93(3) . ? Sb1 F5 1.93(3) 4_565 ? Sb2 F9 1.84(3) . ? Sb2 F9 1.84(3) 4_565 ? Sb2 F11 1.84(2) 4_565 ? Sb2 F11 1.84(2) . ? Sb2 F1 1.850(14) . ? Sb2 F1 1.850(14) 4_565 ? Sb2 F7 1.873(12) . ? Sb2 F7 1.873(12) 4_565 ? Sb2 F8 1.89(2) . ? Sb2 F8 1.89(2) 4_565 ? Sb2 F10 1.899(19) 4_565 ? Sb2 F10 1.899(19) . ? S1 C1 1.710(10) 4_575 ? S1 C1 1.710(10) . ? S2 C4 1.718(7) . ? S2 C5 1.731(9) . ? S3 C7 1.745(11) 4_575 ? S3 C7 1.745(11) . ? S4 C10 1.710(6) . ? S4 C11 1.718(9) . ? S5 C13 1.765(10) 4_575 ? S5 C13 1.765(10) . ? S6 C17 1.732(8) . ? S6 C16 1.757(7) . ? F1 F1 0.95(3) 4_565 ? F2 F2 0.88(4) 4_565 ? F3 F4 0.68(3) . ? F5 F6 0.55(6) . ? F7 F7 0.94(4) 4_565 ? F8 F9 0.69(3) . ? F10 F11 0.73(2) . ? O1 C5 1.358(10) . ? O1 C6 1.421(15) . ? O2 C11 1.364(11) . ? O2 C12A 1.45(3) . ? O2 C12B 1.47(3) . ? O3 C17 1.370(10) . ? O3 C18A 1.43(2) . ? O3 C18B 1.48(2) . ? C1 C2 1.361(13) . ? C2 C3 1.403(11) . ? C3 C2 1.403(11) 4_575 ? C3 C4 1.420(18) . ? C4 S2 1.718(7) 4_575 ? C5 C5 1.333(18) 4_575 ? C6 C6 1.27(3) 4_575 ? C7 C8 1.315(13) . ? C8 C9 1.432(12) . ? C9 C10 1.395(17) . ? C9 C8 1.432(12) 4_575 ? C10 S4 1.710(6) 4_575 ? C11 C11 1.33(2) 4_575 ? C12A C12B 0.75(3) . ? C12A C12A 1.29(6) 4_575 ? C12A C12B 1.50(3) 4_575 ? C12B C12B 1.30(5) 4_575 ? C12B C12A 1.50(3) 4_575 ? C13 C14 1.299(12) . ? C14 C15 1.453(11) . ? C15 C16 1.398(17) . ? C15 C14 1.453(11) 4_575 ? C16 S6 1.757(7) 4_575 ? C17 C17 1.327(17) 4_575 ? C18A C18B 0.69(2) . ? C18A C18A 1.50(4) 4_575 ? C18A C18B 1.54(2) 4_575 ? C18B C18B 1.27(4) 4_575 ? C18B C18A 1.54(2) 4_575 ? C19 C21 1.35(2) 3_565 ? C19 C20 1.41(3) . ? C20 C21 1.32(3) . ? C21 C19 1.35(2) 3_565 ? 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 F6 Sb1 F6 87(3) . 4_565 ? F6 Sb1 F4 166.1(13) . 4_565 ? F6 Sb1 F4 85.2(15) 4_565 4_565 ? F6 Sb1 F4 85.2(15) . . ? F6 Sb1 F4 166.1(13) 4_565 . ? F4 Sb1 F4 99.7(17) 4_565 . ? F6 Sb1 F1 76.6(12) . 4_565 ? F6 Sb1 F1 96.8(12) 4_565 4_565 ? F4 Sb1 F1 92.7(11) 4_565 4_565 ? F4 Sb1 F1 70.1(10) . 4_565 ? F6 Sb1 F1 96.8(12) . . ? F6 Sb1 F1 76.6(12) 4_565 . ? F4 Sb1 F1 70.1(10) 4_565 . ? F4 Sb1 F1 92.7(11) . . ? F1 Sb1 F1 29.4(8) 4_565 . ? F6 Sb1 F2 86.3(12) . . ? F6 Sb1 F2 105.2(11) 4_565 . ? F4 Sb1 F2 106.9(9) 4_565 . ? F4 Sb1 F2 86.0(10) . . ? F1 Sb1 F2 151.5(7) 4_565 . ? F1 Sb1 F2 176.5(8) . . ? F6 Sb1 F2 105.2(11) . 4_565 ? F6 Sb1 F2 86.3(12) 4_565 4_565 ? F4 Sb1 F2 86.0(10) 4_565 4_565 ? F4 Sb1 F2 106.9(9) . 4_565 ? F1 Sb1 F2 176.5(8) 4_565 4_565 ? F1 Sb1 F2 151.5(7) . 4_565 ? F2 Sb1 F2 27.3(11) . 4_565 ? F6 Sb1 F3 172.9(15) . 4_565 ? F6 Sb1 F3 98.9(16) 4_565 4_565 ? F4 Sb1 F3 20.5(11) 4_565 4_565 ? F4 Sb1 F3 89.5(7) . 4_565 ? F1 Sb1 F3 106.0(11) 4_565 4_565 ? F1 Sb1 F3 88.2(10) . 4_565 ? F2 Sb1 F3 88.5(10) . 4_565 ? F2 Sb1 F3 71.8(10) 4_565 4_565 ? F6 Sb1 F3 98.9(16) . . ? F6 Sb1 F3 172.9(15) 4_565 . ? F4 Sb1 F3 89.5(7) 4_565 . ? F4 Sb1 F3 20.5(11) . . ? F1 Sb1 F3 88.2(10) 4_565 . ? F1 Sb1 F3 106.0(11) . . ? F2 Sb1 F3 71.8(10) . . ? F2 Sb1 F3 88.5(10) 4_565 . ? F3 Sb1 F3 74.8(17) 4_565 . ? F6 Sb1 F5 16(2) . . ? F6 Sb1 F5 90.3(7) 4_565 . ? F4 Sb1 F5 173.6(17) 4_565 . ? F4 Sb1 F5 85.8(18) . . ? F1 Sb1 F5 92.3(13) 4_565 . ? F1 Sb1 F5 113.2(13) . . ? F2 Sb1 F5 70.0(13) . . ? F2 Sb1 F5 89.3(13) 4_565 . ? F3 Sb1 F5 158.3(15) 4_565 . ? F3 Sb1 F5 94.6(18) . . ? F6 Sb1 F5 90.3(8) . 4_565 ? F6 Sb1 F5 16(2) 4_565 4_565 ? F4 Sb1 F5 85.8(18) 4_565 4_565 ? F4 Sb1 F5 173.6(17) . 4_565 ? F1 Sb1 F5 113.2(13) 4_565 4_565 ? F1 Sb1 F5 92.3(13) . 4_565 ? F2 Sb1 F5 89.3(13) . 4_565 ? F2 Sb1 F5 70.0(13) 4_565 4_565 ? F3 Sb1 F5 94.6(18) 4_565 4_565 ? F3 Sb1 F5 158.3(15) . 4_565 ? F5 Sb1 F5 89(3) . 4_565 ? F9 Sb2 F9 81(2) . 4_565 ? F9 Sb2 F11 177.2(9) . 4_565 ? F9 Sb2 F11 98.4(14) 4_565 4_565 ? F9 Sb2 F11 98.4(14) . . ? F9 Sb2 F11 177.2(9) 4_565 . ? F11 Sb2 F11 82.1(18) 4_565 . ? F9 Sb2 F1 112.8(9) . . ? F9 Sb2 F1 93.1(9) 4_565 . ? F11 Sb2 F1 69.9(10) 4_565 . ? F11 Sb2 F1 89.6(9) . . ? F9 Sb2 F1 93.1(9) . 4_565 ? F9 Sb2 F1 112.8(9) 4_565 4_565 ? F11 Sb2 F1 89.6(9) 4_565 4_565 ? F11 Sb2 F1 69.9(10) . 4_565 ? F1 Sb2 F1 29.7(8) . 4_565 ? F9 Sb2 F7 68.2(8) . . ? F9 Sb2 F7 87.3(9) 4_565 . ? F11 Sb2 F7 109.2(9) 4_565 . ? F11 Sb2 F7 90.0(8) . . ? F1 Sb2 F7 179.0(9) . . ? F1 Sb2 F7 150.7(7) 4_565 . ? F9 Sb2 F7 87.3(9) . 4_565 ? F9 Sb2 F7 68.2(8) 4_565 4_565 ? F11 Sb2 F7 90.0(8) 4_565 4_565 ? F11 Sb2 F7 109.2(9) . 4_565 ? F1 Sb2 F7 150.7(7) . 4_565 ? F1 Sb2 F7 179.0(9) 4_565 4_565 ? F7 Sb2 F7 29.0(12) . 4_565 ? F9 Sb2 F8 21.1(8) . . ? F9 Sb2 F8 90.3(8) 4_565 . ? F11 Sb2 F8 161.5(8) 4_565 . ? F11 Sb2 F8 89.9(13) . . ? F1 Sb2 F8 93.5(8) . . ? F1 Sb2 F8 72.0(8) 4_565 . ? F7 Sb2 F8 87.3(7) . . ? F7 Sb2 F8 108.4(8) 4_565 . ? F9 Sb2 F8 90.3(8) . 4_565 ? F9 Sb2 F8 21.1(8) 4_565 4_565 ? F11 Sb2 F8 89.9(13) 4_565 4_565 ? F11 Sb2 F8 161.5(8) . 4_565 ? F1 Sb2 F8 72.0(8) . 4_565 ? F1 Sb2 F8 93.5(8) 4_565 4_565 ? F7 Sb2 F8 108.4(8) . 4_565 ? F7 Sb2 F8 87.3(7) 4_565 4_565 ? F8 Sb2 F8 92.7(17) . 4_565 ? F9 Sb2 F10 154.9(9) . 4_565 ? F9 Sb2 F10 88.1(13) 4_565 4_565 ? F11 Sb2 F10 22.4(7) 4_565 4_565 ? F11 Sb2 F10 91.5(9) . 4_565 ? F1 Sb2 F10 90.2(8) . 4_565 ? F1 Sb2 F10 112.0(8) 4_565 4_565 ? F7 Sb2 F10 88.9(8) . 4_565 ? F7 Sb2 F10 67.6(8) 4_565 4_565 ? F8 Sb2 F10 176.0(8) . 4_565 ? F8 Sb2 F10 87.2(11) 4_565 4_565 ? F9 Sb2 F10 88.1(13) . . ? F9 Sb2 F10 154.9(9) 4_565 . ? F11 Sb2 F10 91.5(9) 4_565 . ? F11 Sb2 F10 22.4(7) . . ? F1 Sb2 F10 112.0(8) . . ? F1 Sb2 F10 90.2(8) 4_565 . ? F7 Sb2 F10 67.6(8) . . ? F7 Sb2 F10 88.9(8) 4_565 . ? F8 Sb2 F10 87.2(11) . . ? F8 Sb2 F10 176.0(8) 4_565 . ? F10 Sb2 F10 92.7(13) 4_565 . ? C1 S1 C1 101.7(6) 4_575 . ? C4 S2 C5 94.3(5) . . ? C7 S3 C7 100.2(6) 4_575 . ? C10 S4 C11 94.6(5) . . ? C13 S5 C13 99.7(6) 4_575 . ? C17 S6 C16 94.0(5) . . ? F1 F1 Sb2 75.2(4) 4_565 . ? F1 F1 Sb1 75.3(4) 4_565 . ? Sb2 F1 Sb1 148.8(9) . . ? F2 F2 Sb1 76.4(6) 4_565 . ? F4 F3 Sb1 73(4) . . ? F3 F4 Sb1 87(5) . . ? F6 F5 Sb1 70(5) . . ? F5 F6 Sb1 94(6) . . ? F7 F7 Sb2 75.5(6) 4_565 . ? F9 F8 Sb2 75(4) . . ? F8 F9 Sb2 84(4) . . ? F11 F10 Sb2 75(3) . . ? F10 F11 Sb2 83(3) . . ? C5 O1 C6 110.6(8) . . ? C11 O2 C12A 110.1(14) . . ? C11 O2 C12B 110.8(12) . . ? C12A O2 C12B 29.6(13) . . ? C17 O3 C18A 113.2(10) . . ? C17 O3 C18B 111.5(10) . . ? C18A O3 C18B 27.5(9) . . ? C2 C1 S1 124.3(7) . . ? C1 C2 C3 124.9(9) . . ? C2 C3 C2 119.6(12) . 4_575 ? C2 C3 C4 120.1(6) . . ? C2 C3 C4 120.1(6) 4_575 . ? C3 C4 S2 121.7(4) . 4_575 ? C3 C4 S2 121.7(4) . . ? S2 C4 S2 116.5(8) 4_575 . ? C5 C5 O1 124.7(5) 4_575 . ? C5 C5 S2 117.3(3) 4_575 . ? O1 C5 S2 117.9(7) . . ? C6 C6 O1 124.6(6) 4_575 . ? C8 C7 S3 125.1(8) . . ? C7 C8 C9 125.5(11) . . ? C10 C9 C8 120.7(6) . 4_575 ? C10 C9 C8 120.7(6) . . ? C8 C9 C8 118.4(12) 4_575 . ? C9 C10 S4 121.8(3) . . ? C9 C10 S4 121.8(3) . 4_575 ? S4 C10 S4 116.2(7) . 4_575 ? C11 C11 O2 124.7(6) 4_575 . ? C11 C11 S4 117.3(3) 4_575 . ? O2 C11 S4 118.0(8) . . ? C12B C12A C12A 91(4) . 4_575 ? C12B C12A O2 77(3) . . ? C12A C12A O2 123.3(12) 4_575 . ? C12B C12A C12B 61(4) . 4_575 ? C12A C12A C12B 30.0(13) 4_575 4_575 ? O2 C12A C12B 111(2) . 4_575 ? C12A C12B C12B 89(4) . 4_575 ? C12A C12B O2 73(3) . . ? C12B C12B O2 122.4(10) 4_575 . ? C12A C12B C12A 59(4) . 4_575 ? C12B C12B C12A 30.0(13) 4_575 4_575 ? O2 C12B C12A 109(2) . 4_575 ? C14 C13 S5 126.2(7) . . ? C13 C14 C15 124.0(9) . . ? C16 C15 C14 119.9(6) . . ? C16 C15 C14 119.9(6) . 4_575 ? C14 C15 C14 120.0(11) . 4_575 ? C15 C16 S6 122.4(3) . 4_575 ? C15 C16 S6 122.4(3) . . ? S6 C16 S6 114.9(7) 4_575 . ? C17 C17 O3 124.7(4) 4_575 . ? C17 C17 S6 118.2(3) 4_575 . ? O3 C17 S6 117.2(6) . . ? C18B C18A O3 81(3) . . ? C18B C18A C18A 80(3) . 4_575 ? O3 C18A C18A 118.9(8) . 4_575 ? C18B C18A C18B 54(3) . 4_575 ? O3 C18A C18B 108.9(15) . 4_575 ? C18A C18A C18B 26.3(9) 4_575 4_575 ? C18A C18B C18B 100(3) . 4_575 ? C18A C18B O3 72(3) . . ? C18B C18B O3 123.1(8) 4_575 . ? C18A C18B C18A 74(3) . 4_575 ? C18B C18B C18A 26.3(9) 4_575 4_575 ? O3 C18B C18A 113.1(15) . 4_575 ? C21 C19 C20 118.6(18) 3_565 . ? C21 C20 C19 121.7(18) . . ? C20 C21 C19 119.6(19) . 3_565 ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 1.610 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.151