# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Yamamoto, Yohsuke' _publ_contact_author_email yyama@sci.hiroshima-u.ac.jp _publ_section_title ; Formation of Epoxides from Pentacoordinated Organoarsenic Compounds with a \^I^2^-Hydroxyethyl Group ; loop_ _publ_author_name X.-D.Jiang S.Matsukawa Yu.Fukuzaki Y.Yamamoto # Attachment '- Jiang06_4a_CCDC761610_rev.cif' data_Rf2AsCH2CH2OH _database_code_depnum_ccdc_archive 'CCDC 761610' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 149 _chemical_formula_moiety ? _chemical_formula_sum 'C20 H13 As F12 O3' _chemical_formula_weight 604.22 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' As As 0.0499 2.0058 '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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 9.81100(10) _cell_length_b 17.1930(3) _cell_length_c 24.8070(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4184.46(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.03 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MacScience DIP2030 Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4676 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 28.03 _reflns_number_total 4676 _reflns_number_gt 4238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL(Otwinowski, 1997)' _computing_cell_refinement 'HKL(Otwinowski, 1997)' _computing_data_reduction 'HKL(Otwinowski, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+4.7388P] 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 4676 _refine_ls_number_parameters 329 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 C1 C 0.8091(3) 0.94157(15) 0.35934(10) 0.0230(5) Uani 1 1 d . . . C2 C 0.7279(3) 0.88214(16) 0.37965(11) 0.0277(5) Uani 1 1 d . . . H1 H 0.7670 0.8336 0.3896 0.033 Uiso 1 1 calc R . . C3 C 0.5888(3) 0.89478(19) 0.38524(12) 0.0333(6) Uani 1 1 d . . . H2 H 0.5319 0.8548 0.3992 0.040 Uiso 1 1 calc R . . C4 C 0.5325(3) 0.9661(2) 0.37035(12) 0.0342(6) Uani 1 1 d . . . H3 H 0.4371 0.9741 0.3738 0.041 Uiso 1 1 calc R . . C5 C 0.6140(3) 1.02566(18) 0.35059(11) 0.0301(6) Uani 1 1 d . . . H4 H 0.5750 1.0743 0.3410 0.036 Uiso 1 1 calc R . . C6 C 0.7539(3) 1.01328(16) 0.34496(9) 0.0240(5) Uani 1 1 d . . . C7 C 0.8577(3) 1.07235(15) 0.32396(10) 0.0239(5) Uani 1 1 d . . . C8 C 0.8594(3) 1.14509(18) 0.36014(13) 0.0345(6) Uani 1 1 d . . . C9 C 0.8267(3) 1.09423(17) 0.26480(11) 0.0296(6) Uani 1 1 d . . . C10 C 1.1280(2) 0.96008(15) 0.40445(10) 0.0237(5) Uani 1 1 d . . . C11 C 1.1754(3) 1.03415(16) 0.41710(12) 0.0293(5) Uani 1 1 d . . . H5 H 1.1485 1.0779 0.3963 0.035 Uiso 1 1 calc R . . C12 C 1.2628(3) 1.04291(18) 0.46076(12) 0.0348(6) Uani 1 1 d . . . H6 H 1.2945 1.0932 0.4703 0.042 Uiso 1 1 calc R . . C13 C 1.3038(3) 0.97891(19) 0.49041(12) 0.0347(6) Uani 1 1 d . . . H7 H 1.3636 0.9857 0.5202 0.042 Uiso 1 1 calc R . . C14 C 1.2583(3) 0.90465(18) 0.47705(10) 0.0300(6) Uani 1 1 d . . . H8 H 1.2881 0.8608 0.4972 0.036 Uiso 1 1 calc R . . C15 C 1.1689(3) 0.89519(15) 0.43404(10) 0.0237(5) Uani 1 1 d . . . C16 C 1.1062(3) 0.81848(15) 0.41545(10) 0.0236(5) Uani 1 1 d . . . C17 C 1.0283(3) 0.77906(18) 0.46203(12) 0.0323(6) Uani 1 1 d . . . C18 C 1.2178(3) 0.76439(17) 0.39292(11) 0.0308(6) Uani 1 1 d . . . C19 C 1.0738(3) 0.90548(17) 0.27793(11) 0.0308(6) Uani 1 1 d . . . H9 H 1.0454 0.9447 0.2510 0.037 Uiso 1 1 calc R . . H10 H 1.1746 0.9062 0.2797 0.037 Uiso 1 1 calc R . . C20 C 1.0283(4) 0.82609(19) 0.25885(12) 0.0383(7) Uani 1 1 d . . . H11 H 1.0625 0.8163 0.2219 0.046 Uiso 1 1 calc R . . H12 H 1.0650 0.7853 0.2830 0.046 Uiso 1 1 calc R . . O1 O 0.98797(17) 1.04132(12) 0.32531(8) 0.0241(4) Uani 1 1 d . . . O2 O 1.01228(18) 0.83119(11) 0.37466(8) 0.0235(4) Uani 1 1 d . . . O3 O 0.8831(3) 0.82425(18) 0.25934(12) 0.0599(7) Uani 1 1 d D . . H13 H 0.875(13) 0.767(3) 0.248(6) 0.26(6) Uiso 1 1 d D . . As1 As 1.00189(2) 0.935130(15) 0.347574(10) 0.01943(11) Uani 1 1 d . . . F1 F 0.9592(3) 1.19433(12) 0.34668(8) 0.0451(5) Uani 1 1 d . . . F2 F 0.8807(2) 1.12484(12) 0.41087(8) 0.0499(5) Uani 1 1 d . . . F3 F 0.7421(2) 1.18509(12) 0.35818(12) 0.0598(6) Uani 1 1 d . . . F4 F 0.92093(19) 1.14131(11) 0.24413(7) 0.0388(4) Uani 1 1 d . . . F5 F 0.7069(2) 1.12952(14) 0.25857(9) 0.0512(5) Uani 1 1 d . . . F6 F 0.8249(2) 1.03061(11) 0.23421(7) 0.0423(4) Uani 1 1 d . . . F7 F 0.9593(3) 0.71699(13) 0.44522(8) 0.0513(5) Uani 1 1 d . . . F8 F 0.9391(2) 0.82849(13) 0.48310(8) 0.0486(5) Uani 1 1 d . . . F9 F 1.1097(2) 0.75501(12) 0.50203(7) 0.0431(4) Uani 1 1 d . . . F10 F 1.1673(2) 0.69864(11) 0.37305(9) 0.0475(5) Uani 1 1 d . . . F11 F 1.3123(2) 0.74527(12) 0.42917(8) 0.0448(5) Uani 1 1 d . . . F12 F 1.2827(2) 0.79995(12) 0.35250(7) 0.0405(4) Uani 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 C1 0.0224(11) 0.0221(13) 0.0244(11) -0.0007(9) -0.0005(9) 0.0004(9) C2 0.0281(13) 0.0220(14) 0.0329(13) 0.0021(10) 0.0019(9) -0.0045(10) C3 0.0284(13) 0.0366(17) 0.0349(14) 0.0006(11) 0.0024(10) -0.0078(11) C4 0.0235(12) 0.0432(19) 0.0359(14) -0.0021(12) 0.0024(11) -0.0006(12) C5 0.0279(13) 0.0316(16) 0.0306(13) 0.0003(10) 0.0002(9) 0.0060(11) C6 0.0253(12) 0.0234(13) 0.0232(11) -0.0002(9) 0.0008(8) 0.0017(10) C7 0.0262(12) 0.0162(13) 0.0294(12) 0.0017(9) 0.0002(9) 0.0037(9) C8 0.0393(15) 0.0211(15) 0.0432(15) -0.0063(11) 0.0014(12) 0.0029(11) C9 0.0288(13) 0.0254(15) 0.0347(13) 0.0087(11) -0.0009(10) 0.0026(10) C10 0.0229(11) 0.0225(13) 0.0256(11) 0.0009(9) -0.0024(9) -0.0001(9) C11 0.0286(13) 0.0209(14) 0.0383(14) -0.0010(10) -0.0034(10) -0.0010(10) C12 0.0361(15) 0.0272(15) 0.0412(15) -0.0068(12) -0.0044(12) -0.0054(11) C13 0.0341(14) 0.0391(17) 0.0309(13) -0.0040(11) -0.0083(11) -0.0046(12) C14 0.0350(14) 0.0303(16) 0.0248(12) 0.0021(10) -0.0029(10) 0.0017(11) C15 0.0262(11) 0.0228(13) 0.0221(11) 0.0015(9) 0.0006(9) 0.0016(9) C16 0.0294(12) 0.0180(12) 0.0235(11) 0.0039(9) -0.0010(9) 0.0006(9) C17 0.0400(14) 0.0268(16) 0.0302(13) 0.0058(11) 0.0020(11) -0.0029(12) C18 0.0361(14) 0.0259(14) 0.0304(12) 0.0017(10) -0.0022(10) 0.0084(11) C19 0.0401(15) 0.0268(15) 0.0255(12) 0.0028(10) 0.0056(10) 0.0041(11) C20 0.0565(18) 0.0306(17) 0.0278(13) -0.0050(11) -0.0017(13) 0.0056(14) O1 0.0223(9) 0.0158(10) 0.0341(10) 0.0049(7) -0.0012(6) 0.0015(6) O2 0.0277(9) 0.0161(9) 0.0268(9) 0.0022(7) -0.0035(6) 0.0008(6) O3 0.0572(16) 0.0616(19) 0.0608(16) -0.0177(14) -0.0157(13) -0.0072(14) As1 0.02101(18) 0.01505(19) 0.02222(17) 0.00115(8) -0.00008(7) 0.00012(8) F1 0.0554(12) 0.0220(10) 0.0578(13) -0.0038(8) -0.0002(9) -0.0103(9) F2 0.0743(14) 0.0422(12) 0.0333(9) -0.0113(8) 0.0041(9) -0.0082(10) F3 0.0508(13) 0.0334(13) 0.0951(18) -0.0215(11) 0.0022(11) 0.0155(10) F4 0.0416(10) 0.0334(10) 0.0416(9) 0.0158(7) 0.0016(7) -0.0037(7) F5 0.0357(10) 0.0673(14) 0.0506(11) 0.0239(10) -0.0028(8) 0.0181(10) F6 0.0572(12) 0.0394(11) 0.0304(8) -0.0010(7) -0.0047(8) -0.0098(9) F7 0.0671(13) 0.0420(12) 0.0449(11) 0.0113(9) -0.0008(10) -0.0283(10) F8 0.0486(11) 0.0506(12) 0.0467(10) 0.0104(9) 0.0227(9) 0.0068(9) F9 0.0590(11) 0.0390(11) 0.0312(8) 0.0154(7) -0.0027(8) -0.0029(9) F10 0.0585(13) 0.0229(10) 0.0609(12) -0.0129(8) -0.0057(10) 0.0102(8) F11 0.0463(10) 0.0478(12) 0.0401(9) 0.0037(8) -0.0085(8) 0.0229(9) F12 0.0404(10) 0.0454(11) 0.0358(9) 0.0050(8) 0.0109(7) 0.0137(8) _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 C1 C2 1.390(4) . ? C1 C6 1.393(4) . ? C1 As1 1.917(3) . ? C2 C3 1.389(4) . ? C2 H1 0.9500 . ? C3 C4 1.395(5) . ? C3 H2 0.9500 . ? C4 C5 1.388(4) . ? C4 H3 0.9500 . ? C5 C6 1.396(4) . ? C5 H4 0.9500 . ? C6 C7 1.530(4) . ? C7 O1 1.385(3) . ? C7 C8 1.540(4) . ? C7 C9 1.545(4) . ? C8 F2 1.322(4) . ? C8 F1 1.337(4) . ? C8 F3 1.342(4) . ? C9 F6 1.331(4) . ? C9 F4 1.331(3) . ? C9 F5 1.332(3) . ? C10 C11 1.392(4) . ? C10 C15 1.395(4) . ? C10 As1 1.925(2) . ? C11 C12 1.389(4) . ? C11 H5 0.9500 . ? C12 C13 1.384(5) . ? C12 H6 0.9500 . ? C13 C14 1.393(4) . ? C13 H7 0.9500 . ? C14 C15 1.391(4) . ? C14 H8 0.9500 . ? C15 C16 1.527(4) . ? C16 O2 1.386(3) . ? C16 C18 1.541(4) . ? C16 C17 1.542(4) . ? C17 F8 1.327(4) . ? C17 F7 1.331(4) . ? C17 F9 1.339(4) . ? C18 F10 1.329(4) . ? C18 F11 1.333(3) . ? C18 F12 1.336(3) . ? C19 C20 1.512(4) . ? C19 As1 1.935(3) . ? C19 H9 0.9900 . ? C19 H10 0.9900 . ? C20 O3 1.425(5) . ? C20 H11 0.9900 . ? C20 H12 0.9900 . ? O1 As1 1.912(2) . ? O2 As1 1.9119(19) . ? O3 H13 1.02(2) . ? 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 C2 C1 C6 121.4(2) . . ? C2 C1 As1 125.3(2) . . ? C6 C1 As1 113.28(19) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H1 120.5 . . ? C1 C2 H1 120.5 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H2 120.0 . . ? C4 C3 H2 120.0 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H3 119.5 . . ? C3 C4 H3 119.5 . . ? C4 C5 C6 119.3(3) . . ? C4 C5 H4 120.4 . . ? C6 C5 H4 120.4 . . ? C1 C6 C5 119.4(3) . . ? C1 C6 C7 114.6(2) . . ? C5 C6 C7 126.0(2) . . ? O1 C7 C6 110.5(2) . . ? O1 C7 C8 106.8(2) . . ? C6 C7 C8 110.4(2) . . ? O1 C7 C9 107.4(2) . . ? C6 C7 C9 110.7(2) . . ? C8 C7 C9 111.0(2) . . ? F2 C8 F1 106.8(3) . . ? F2 C8 F3 107.7(3) . . ? F1 C8 F3 107.2(3) . . ? F2 C8 C7 110.0(2) . . ? F1 C8 C7 112.1(2) . . ? F3 C8 C7 112.7(3) . . ? F6 C9 F4 106.8(2) . . ? F6 C9 F5 107.2(2) . . ? F4 C9 F5 106.9(2) . . ? F6 C9 C7 110.1(2) . . ? F4 C9 C7 112.2(2) . . ? F5 C9 C7 113.3(2) . . ? C11 C10 C15 121.1(2) . . ? C11 C10 As1 125.7(2) . . ? C15 C10 As1 113.12(19) . . ? C12 C11 C10 118.8(3) . . ? C12 C11 H5 120.6 . . ? C10 C11 H5 120.6 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H6 119.7 . . ? C11 C12 H6 119.7 . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H7 119.7 . . ? C14 C13 H7 119.7 . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H8 120.3 . . ? C13 C14 H8 120.3 . . ? C14 C15 C10 119.5(2) . . ? C14 C15 C16 125.9(2) . . ? C10 C15 C16 114.6(2) . . ? O2 C16 C15 110.6(2) . . ? O2 C16 C18 107.6(2) . . ? C15 C16 C18 110.2(2) . . ? O2 C16 C17 106.6(2) . . ? C15 C16 C17 110.7(2) . . ? C18 C16 C17 111.0(2) . . ? F8 C17 F7 107.6(3) . . ? F8 C17 F9 107.4(2) . . ? F7 C17 F9 106.7(2) . . ? F8 C17 C16 109.9(2) . . ? F7 C17 C16 111.7(2) . . ? F9 C17 C16 113.3(3) . . ? F10 C18 F11 107.4(2) . . ? F10 C18 F12 106.8(2) . . ? F11 C18 F12 106.7(2) . . ? F10 C18 C16 112.5(2) . . ? F11 C18 C16 113.5(2) . . ? F12 C18 C16 109.5(2) . . ? C20 C19 As1 114.2(2) . . ? C20 C19 H9 108.7 . . ? As1 C19 H9 108.7 . . ? C20 C19 H10 108.7 . . ? As1 C19 H10 108.7 . . ? H9 C19 H10 107.6 . . ? O3 C20 C19 108.2(3) . . ? O3 C20 H11 110.1 . . ? C19 C20 H11 110.1 . . ? O3 C20 H12 110.1 . . ? C19 C20 H12 110.1 . . ? H11 C20 H12 108.4 . . ? C7 O1 As1 116.14(16) . . ? C16 O2 As1 116.07(16) . . ? C20 O3 H13 96(7) . . ? O2 As1 O1 176.09(8) . . ? O2 As1 C1 93.04(10) . . ? O1 As1 C1 85.32(9) . . ? O2 As1 C10 85.21(9) . . ? O1 As1 C10 92.57(10) . . ? C1 As1 C10 120.64(11) . . ? O2 As1 C19 92.76(10) . . ? O1 As1 C19 91.13(11) . . ? C1 As1 C19 120.73(12) . . ? C10 As1 C19 118.62(12) . . ? 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 C6 C1 C2 C3 0.5(4) . . . . ? As1 C1 C2 C3 -179.0(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C2 C1 C6 C5 -0.6(4) . . . . ? As1 C1 C6 C5 179.0(2) . . . . ? C2 C1 C6 C7 179.3(2) . . . . ? As1 C1 C6 C7 -1.1(3) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? C4 C5 C6 C7 -180.0(2) . . . . ? C1 C6 C7 O1 -1.7(3) . . . . ? C5 C6 C7 O1 178.2(2) . . . . ? C1 C6 C7 C8 -119.6(3) . . . . ? C5 C6 C7 C8 60.3(3) . . . . ? C1 C6 C7 C9 117.1(2) . . . . ? C5 C6 C7 C9 -63.0(3) . . . . ? O1 C7 C8 F2 -65.8(3) . . . . ? C6 C7 C8 F2 54.4(3) . . . . ? C9 C7 C8 F2 177.5(2) . . . . ? O1 C7 C8 F1 52.9(3) . . . . ? C6 C7 C8 F1 173.1(2) . . . . ? C9 C7 C8 F1 -63.8(3) . . . . ? O1 C7 C8 F3 173.9(3) . . . . ? C6 C7 C8 F3 -65.9(3) . . . . ? C9 C7 C8 F3 57.2(3) . . . . ? O1 C7 C9 F6 64.0(3) . . . . ? C6 C7 C9 F6 -56.7(3) . . . . ? C8 C7 C9 F6 -179.7(2) . . . . ? O1 C7 C9 F4 -54.8(3) . . . . ? C6 C7 C9 F4 -175.5(2) . . . . ? C8 C7 C9 F4 61.6(3) . . . . ? O1 C7 C9 F5 -175.9(2) . . . . ? C6 C7 C9 F5 63.4(3) . . . . ? C8 C7 C9 F5 -59.6(3) . . . . ? C15 C10 C11 C12 -1.3(4) . . . . ? As1 C10 C11 C12 177.7(2) . . . . ? C10 C11 C12 C13 1.2(4) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 -1.1(4) . . . . ? C13 C14 C15 C10 1.0(4) . . . . ? C13 C14 C15 C16 -177.9(3) . . . . ? C11 C10 C15 C14 0.2(4) . . . . ? As1 C10 C15 C14 -178.9(2) . . . . ? C11 C10 C15 C16 179.2(2) . . . . ? As1 C10 C15 C16 0.1(3) . . . . ? C14 C15 C16 O2 174.5(2) . . . . ? C10 C15 C16 O2 -4.4(3) . . . . ? C14 C15 C16 C18 -66.6(3) . . . . ? C10 C15 C16 C18 114.4(2) . . . . ? C14 C15 C16 C17 56.5(3) . . . . ? C10 C15 C16 C17 -122.4(2) . . . . ? O2 C16 C17 F8 -67.2(3) . . . . ? C15 C16 C17 F8 53.2(3) . . . . ? C18 C16 C17 F8 175.9(2) . . . . ? O2 C16 C17 F7 52.2(3) . . . . ? C15 C16 C17 F7 172.5(2) . . . . ? C18 C16 C17 F7 -64.8(3) . . . . ? O2 C16 C17 F9 172.7(2) . . . . ? C15 C16 C17 F9 -66.9(3) . . . . ? C18 C16 C17 F9 55.7(3) . . . . ? O2 C16 C18 F10 -55.4(3) . . . . ? C15 C16 C18 F10 -176.1(2) . . . . ? C17 C16 C18 F10 61.0(3) . . . . ? O2 C16 C18 F11 -177.6(2) . . . . ? C15 C16 C18 F11 61.7(3) . . . . ? C17 C16 C18 F11 -61.3(3) . . . . ? O2 C16 C18 F12 63.2(3) . . . . ? C15 C16 C18 F12 -57.4(3) . . . . ? C17 C16 C18 F12 179.6(2) . . . . ? As1 C19 C20 O3 55.2(3) . . . . ? C6 C7 O1 As1 3.8(3) . . . . ? C8 C7 O1 As1 123.9(2) . . . . ? C9 C7 O1 As1 -117.0(2) . . . . ? C15 C16 O2 As1 6.9(3) . . . . ? C18 C16 O2 As1 -113.5(2) . . . . ? C17 C16 O2 As1 127.31(18) . . . . ? C16 O2 As1 O1 -61.2(11) . . . . ? C16 O2 As1 C1 -126.29(18) . . . . ? C16 O2 As1 C10 -5.78(18) . . . . ? C16 O2 As1 C19 112.72(19) . . . . ? C7 O1 As1 O2 -69.1(11) . . . . ? C7 O1 As1 C1 -3.73(19) . . . . ? C7 O1 As1 C10 -124.28(19) . . . . ? C7 O1 As1 C19 117.0(2) . . . . ? C2 C1 As1 O2 -1.5(2) . . . . ? C6 C1 As1 O2 179.02(19) . . . . ? C2 C1 As1 O1 -177.9(2) . . . . ? C6 C1 As1 O1 2.58(19) . . . . ? C2 C1 As1 C10 -87.7(3) . . . . ? C6 C1 As1 C10 92.8(2) . . . . ? C2 C1 As1 C19 93.6(3) . . . . ? C6 C1 As1 C19 -85.9(2) . . . . ? C11 C10 As1 O2 -176.2(2) . . . . ? C15 C10 As1 O2 2.94(18) . . . . ? C11 C10 As1 O1 0.6(2) . . . . ? C15 C10 As1 O1 179.71(19) . . . . ? C11 C10 As1 C1 -85.5(3) . . . . ? C15 C10 As1 C1 93.6(2) . . . . ? C11 C10 As1 C19 93.3(3) . . . . ? C15 C10 As1 C19 -87.6(2) . . . . ? C20 C19 As1 O2 35.9(2) . . . . ? C20 C19 As1 O1 -144.5(2) . . . . ? C20 C19 As1 C1 -59.2(3) . . . . ? C20 C19 As1 C10 122.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H13 F5 1.02(2) 2.51(6) 3.463(4) 155(11) 7_755 O3 H13 F12 1.02(2) 2.72(15) 2.974(3) 94(8) 6_556 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.603 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.197 # Attachment '- Jiang06_5a_CCDC761611.cif' data_Rf2AsCH2COPh _database_code_depnum_ccdc_archive 'CCDC 761611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 98 _chemical_formula_moiety ? _chemical_formula_sum 'C26 H15 As F12 O3' _chemical_formula_weight 678.30 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.23400(10) _cell_length_b 10.9850(2) _cell_length_c 14.1180(4) _cell_angle_alpha 85.0940(10) _cell_angle_beta 80.6210(10) _cell_angle_gamma 66.9950(10) _cell_volume 1300.18(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.95 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.422 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MacScience DIP2030 Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5599 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.95 _reflns_number_total 5599 _reflns_number_gt 5135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL(Otwinowski, 1997)' _computing_cell_refinement 'HKL(Otwinowski, 1997)' _computing_data_reduction 'HKL(Otwinowski, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+0.6847P] 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 5599 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 C1 C 0.7134(3) 0.7334(3) 0.8656(2) 0.0386(6) Uani 1 1 d . . . C2 C 0.5628(4) 0.7314(4) 0.8946(3) 0.0505(8) Uani 1 1 d . . . H2A H 0.5169 0.6971 0.8554 0.061 Uiso 1 1 calc R . . C3 C 0.4834(4) 0.7816(4) 0.9831(3) 0.0614(10) Uani 1 1 d . . . H3A H 0.3828 0.7810 1.0040 0.074 Uiso 1 1 calc R . . C4 C 0.5514(5) 0.8325(5) 1.0407(3) 0.0649(10) Uani 1 1 d . . . H4A H 0.4965 0.8654 1.1003 0.078 Uiso 1 1 calc R . . C5 C 0.7014(5) 0.8354(4) 1.0112(3) 0.0581(9) Uani 1 1 d . . . H5A H 0.7469 0.8700 1.0505 0.070 Uiso 1 1 calc R . . C6 C 0.7820(4) 0.7858(3) 0.9222(2) 0.0421(6) Uani 1 1 d . . . C7 C 0.9454(4) 0.7844(3) 0.8781(2) 0.0410(6) Uani 1 1 d . . . C8 C 1.0718(5) 0.7038(4) 0.9422(3) 0.0577(9) Uani 1 1 d . . . C9 C 0.9376(5) 0.9277(4) 0.8638(3) 0.0528(8) Uani 1 1 d . . . C10 C 0.9986(3) 0.4863(3) 0.7388(2) 0.0402(6) Uani 1 1 d . . . C11 C 1.1570(4) 0.4448(4) 0.7520(3) 0.0522(8) Uani 1 1 d . . . H11A H 1.1990 0.5055 0.7639 0.063 Uiso 1 1 calc R . . C12 C 1.2503(4) 0.3114(4) 0.7471(3) 0.0631(10) Uani 1 1 d . . . H12A H 1.3572 0.2820 0.7541 0.076 Uiso 1 1 calc R . . C13 C 1.1865(5) 0.2212(4) 0.7318(3) 0.0621(10) Uani 1 1 d . . . H13A H 1.2504 0.1314 0.7302 0.075 Uiso 1 1 calc R . . C14 C 1.0295(4) 0.2624(3) 0.7190(3) 0.0547(8) Uani 1 1 d . . . H14A H 0.9871 0.2011 0.7093 0.066 Uiso 1 1 calc R . . C15 C 0.9358(3) 0.3964(3) 0.7206(2) 0.0413(6) Uani 1 1 d . . . C16 C 0.7624(4) 0.4581(3) 0.7029(3) 0.0472(7) Uani 1 1 d . . . C17 C 0.6584(4) 0.4065(4) 0.7792(5) 0.0704(13) Uani 1 1 d . . . C18 C 0.7510(6) 0.4290(4) 0.6007(4) 0.0754(14) Uani 1 1 d . . . C19 C 0.8431(4) 0.7686(3) 0.6297(2) 0.0480(7) Uani 1 1 d . . . H19A H 0.9413 0.7837 0.6156 0.058 Uiso 1 1 calc R . . H19B H 0.8385 0.7189 0.5775 0.058 Uiso 1 1 calc R . . C20 C 0.7042(4) 0.9007(3) 0.6344(2) 0.0489(7) Uani 1 1 d . . . C21 C 0.7011(5) 0.9968(3) 0.5529(3) 0.0510(8) Uani 1 1 d . . . C22 C 0.5666(6) 1.1108(5) 0.5501(4) 0.0773(13) Uani 1 1 d . . . H22A H 0.4813 1.1265 0.5990 0.093 Uiso 1 1 calc R . . C23 C 0.5576(8) 1.2011(6) 0.4760(6) 0.103(2) Uani 1 1 d . . . H23A H 0.4666 1.2779 0.4753 0.123 Uiso 1 1 calc R . . C24 C 0.6818(10) 1.1795(6) 0.4025(5) 0.102(2) Uani 1 1 d . . . H24A H 0.6740 1.2403 0.3516 0.123 Uiso 1 1 calc R . . C25 C 0.8168(10) 1.0679(6) 0.4048(4) 0.102(2) Uani 1 1 d . . . H25A H 0.9022 1.0536 0.3560 0.123 Uiso 1 1 calc R . . C26 C 0.8265(7) 0.9760(5) 0.4798(3) 0.0787(14) Uani 1 1 d . . . H26A H 0.9181 0.8998 0.4807 0.094 Uiso 1 1 calc R . . As1 As 0.84583(3) 0.66481(3) 0.74739(2) 0.03566(12) Uani 1 1 d . . . O1 O 0.9900(3) 0.7292(2) 0.78856(16) 0.0446(5) Uani 1 1 d . . . O2 O 0.7046(2) 0.5942(2) 0.71016(18) 0.0443(5) Uani 1 1 d . . . O3 O 0.5977(4) 0.9250(3) 0.7007(2) 0.0779(9) Uani 1 1 d . . . F1 F 1.2184(3) 0.6836(3) 0.8998(2) 0.0813(8) Uani 1 1 d . . . F2 F 1.0680(3) 0.5855(3) 0.9607(2) 0.0859(8) Uani 1 1 d . . . F3 F 1.0511(4) 0.7620(4) 1.0255(2) 0.0884(9) Uani 1 1 d . . . F4 F 1.0794(3) 0.9318(3) 0.8310(2) 0.0744(7) Uani 1 1 d . . . F5 F 0.8824(3) 0.9983(3) 0.9426(2) 0.0775(8) Uani 1 1 d . . . F6 F 0.8421(4) 0.9914(3) 0.7994(2) 0.0787(7) Uani 1 1 d . . . F7 F 0.5044(3) 0.4712(3) 0.7747(3) 0.0996(11) Uani 1 1 d . . . F8 F 0.6812(3) 0.4223(3) 0.8667(2) 0.0875(9) Uani 1 1 d . . . F9 F 0.6890(4) 0.2786(3) 0.7697(4) 0.1206(15) Uani 1 1 d . . . F10 F 0.6016(4) 0.4805(3) 0.5819(3) 0.1046(12) Uani 1 1 d . . . F11 F 0.8073(4) 0.3006(3) 0.5824(3) 0.1106(14) Uani 1 1 d . . . F12 F 0.8330(5) 0.4831(4) 0.5370(2) 0.1008(10) Uani 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 C1 0.0338(13) 0.0409(14) 0.0441(14) 0.0000(12) -0.0017(11) -0.0193(11) C2 0.0359(14) 0.0553(19) 0.067(2) -0.0037(16) -0.0019(14) -0.0260(14) C3 0.0411(17) 0.076(3) 0.070(2) -0.004(2) 0.0104(16) -0.0313(17) C4 0.058(2) 0.089(3) 0.0476(18) -0.0091(19) 0.0136(16) -0.035(2) C5 0.057(2) 0.081(3) 0.0473(17) -0.0107(17) 0.0008(15) -0.0395(19) C6 0.0414(14) 0.0506(17) 0.0428(14) -0.0009(13) -0.0025(12) -0.0282(13) C7 0.0396(14) 0.0471(16) 0.0465(15) -0.0052(13) -0.0031(12) -0.0277(12) C8 0.0535(19) 0.066(2) 0.068(2) 0.0059(19) -0.0210(17) -0.0347(17) C9 0.0590(19) 0.0521(19) 0.0609(19) -0.0089(16) -0.0012(16) -0.0370(16) C10 0.0320(13) 0.0371(14) 0.0533(16) -0.0026(13) -0.0080(11) -0.0141(11) C11 0.0295(13) 0.0512(18) 0.078(2) -0.0088(17) -0.0095(14) -0.0155(12) C12 0.0341(15) 0.059(2) 0.091(3) -0.005(2) -0.0155(17) -0.0088(14) C13 0.0462(18) 0.0418(17) 0.089(3) -0.0027(19) -0.0139(18) -0.0047(14) C14 0.0459(17) 0.0362(15) 0.082(2) -0.0022(17) -0.0126(16) -0.0147(13) C15 0.0328(13) 0.0352(14) 0.0578(17) -0.0027(13) -0.0106(12) -0.0132(11) C16 0.0363(14) 0.0340(14) 0.078(2) -0.0060(15) -0.0192(14) -0.0149(11) C17 0.0387(17) 0.0463(19) 0.133(4) 0.001(2) -0.011(2) -0.0244(15) C18 0.069(3) 0.056(2) 0.106(4) -0.026(2) -0.046(3) -0.0109(19) C19 0.0543(18) 0.0384(15) 0.0474(16) -0.0011(14) -0.0030(14) -0.0151(13) C20 0.0478(17) 0.0470(17) 0.0490(16) -0.0039(15) -0.0068(14) -0.0146(14) C21 0.063(2) 0.0414(17) 0.0514(17) 0.0006(15) -0.0178(15) -0.0192(15) C22 0.065(3) 0.056(2) 0.105(4) 0.016(3) -0.025(2) -0.0157(19) C23 0.111(5) 0.061(3) 0.144(6) 0.046(4) -0.071(5) -0.030(3) C24 0.173(7) 0.075(4) 0.090(4) 0.036(3) -0.068(4) -0.070(4) C25 0.165(6) 0.078(4) 0.058(3) 0.013(3) -0.004(3) -0.048(4) C26 0.109(4) 0.055(2) 0.054(2) 0.004(2) 0.005(2) -0.019(2) As1 0.03216(16) 0.03309(17) 0.04565(18) -0.00303(12) -0.00504(11) -0.01648(12) O1 0.0395(10) 0.0540(13) 0.0509(11) -0.0138(10) 0.0041(9) -0.0310(10) O2 0.0351(10) 0.0335(10) 0.0685(14) -0.0072(10) -0.0190(9) -0.0116(8) O3 0.0560(16) 0.076(2) 0.0725(18) 0.0139(16) 0.0064(14) -0.0032(14) F1 0.0416(11) 0.100(2) 0.113(2) 0.0042(17) -0.0172(12) -0.0368(12) F2 0.0813(17) 0.0700(16) 0.122(2) 0.0359(17) -0.0425(17) -0.0427(14) F3 0.0855(18) 0.117(2) 0.0738(16) -0.0069(16) -0.0374(14) -0.0395(17) F4 0.0754(15) 0.0750(15) 0.0929(17) -0.0087(13) 0.0119(13) -0.0582(14) F5 0.0901(18) 0.0743(16) 0.0841(16) -0.0350(14) 0.0121(14) -0.0514(14) F6 0.0962(19) 0.0533(13) 0.0962(19) 0.0127(14) -0.0307(16) -0.0353(13) F7 0.0354(11) 0.0831(18) 0.186(3) -0.013(2) -0.0135(15) -0.0277(11) F8 0.0667(16) 0.093(2) 0.101(2) 0.0275(18) -0.0026(15) -0.0380(15) F9 0.0777(18) 0.0519(15) 0.235(5) -0.010(2) 0.016(2) -0.0415(14) F10 0.088(2) 0.0788(18) 0.153(3) -0.027(2) -0.081(2) -0.0092(15) F11 0.113(2) 0.0609(16) 0.160(3) -0.0488(19) -0.075(2) -0.0046(15) F12 0.123(3) 0.113(3) 0.0681(17) -0.0218(17) -0.0228(18) -0.040(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.379(4) . ? C1 C2 1.393(4) . ? C1 As1 1.917(3) . ? C2 C3 1.381(5) . ? C2 H2A 0.9300 . ? C3 C4 1.373(6) . ? C3 H3A 0.9300 . ? C4 C5 1.392(5) . ? C4 H4A 0.9300 . ? C5 C6 1.388(5) . ? C5 H5A 0.9300 . ? C6 C7 1.530(4) . ? C7 O1 1.379(4) . ? C7 C8 1.538(5) . ? C7 C9 1.544(4) . ? C8 F2 1.316(5) . ? C8 F1 1.328(5) . ? C8 F3 1.337(5) . ? C9 F5 1.324(4) . ? C9 F6 1.328(5) . ? C9 F4 1.333(4) . ? C10 C15 1.385(4) . ? C10 C11 1.391(4) . ? C10 As1 1.916(3) . ? C11 C12 1.380(5) . ? C11 H11A 0.9300 . ? C12 C13 1.382(6) . ? C12 H12A 0.9300 . ? C13 C14 1.378(5) . ? C13 H13A 0.9300 . ? C14 C15 1.385(4) . ? C14 H14A 0.9300 . ? C15 C16 1.529(4) . ? C16 O2 1.384(4) . ? C16 C18 1.534(6) . ? C16 C17 1.545(6) . ? C17 F8 1.323(6) . ? C17 F7 1.327(4) . ? C17 F9 1.336(5) . ? C18 F12 1.331(7) . ? C18 F11 1.331(5) . ? C18 F10 1.333(5) . ? C19 C20 1.513(5) . ? C19 As1 1.931(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O3 1.205(4) . ? C20 C21 1.489(5) . ? C21 C26 1.380(6) . ? C21 C22 1.380(6) . ? C22 C23 1.368(8) . ? C22 H22A 0.9300 . ? C23 C24 1.374(10) . ? C23 H23A 0.9300 . ? C24 C25 1.368(10) . ? C24 H24A 0.9300 . ? C25 C26 1.388(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? As1 O2 1.914(2) . ? As1 O1 1.915(2) . ? 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 C6 C1 C2 121.5(3) . . ? C6 C1 As1 113.4(2) . . ? C2 C1 As1 125.0(2) . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 118.9(3) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C1 C6 C5 119.7(3) . . ? C1 C6 C7 114.8(3) . . ? C5 C6 C7 125.5(3) . . ? O1 C7 C6 110.5(2) . . ? O1 C7 C8 108.6(3) . . ? C6 C7 C8 110.7(3) . . ? O1 C7 C9 106.9(3) . . ? C6 C7 C9 109.7(3) . . ? C8 C7 C9 110.5(3) . . ? F2 C8 F1 105.9(4) . . ? F2 C8 F3 108.5(4) . . ? F1 C8 F3 107.2(3) . . ? F2 C8 C7 110.0(3) . . ? F1 C8 C7 112.4(3) . . ? F3 C8 C7 112.5(3) . . ? F5 C9 F6 106.6(3) . . ? F5 C9 F4 106.8(3) . . ? F6 C9 F4 107.1(3) . . ? F5 C9 C7 114.2(3) . . ? F6 C9 C7 109.7(3) . . ? F4 C9 C7 112.1(3) . . ? C15 C10 C11 120.9(3) . . ? C15 C10 As1 113.5(2) . . ? C11 C10 As1 125.5(2) . . ? C12 C11 C10 118.4(3) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C10 C15 C14 120.0(3) . . ? C10 C15 C16 114.7(3) . . ? C14 C15 C16 125.4(3) . . ? O2 C16 C15 110.3(2) . . ? O2 C16 C18 107.2(3) . . ? C15 C16 C18 109.7(3) . . ? O2 C16 C17 107.5(3) . . ? C15 C16 C17 110.2(3) . . ? C18 C16 C17 111.9(4) . . ? F8 C17 F7 106.8(4) . . ? F8 C17 F9 108.0(5) . . ? F7 C17 F9 106.5(3) . . ? F8 C17 C16 110.6(3) . . ? F7 C17 C16 112.1(4) . . ? F9 C17 C16 112.6(4) . . ? F12 C18 F11 107.1(5) . . ? F12 C18 F10 106.8(5) . . ? F11 C18 F10 106.9(3) . . ? F12 C18 C16 110.0(3) . . ? F11 C18 C16 113.8(4) . . ? F10 C18 C16 111.9(4) . . ? C20 C19 As1 112.9(2) . . ? C20 C19 H19A 109.0 . . ? As1 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? As1 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? O3 C20 C21 121.5(3) . . ? O3 C20 C19 120.7(3) . . ? C21 C20 C19 117.8(3) . . ? C26 C21 C22 118.6(4) . . ? C26 C21 C20 122.7(4) . . ? C22 C21 C20 118.6(4) . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 120.7(6) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C25 C24 C23 119.5(5) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.3 . . ? C24 C25 C26 120.0(6) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C21 C26 C25 120.5(5) . . ? C21 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? O2 As1 O1 177.51(10) . . ? O2 As1 C10 85.00(10) . . ? O1 As1 C10 93.26(11) . . ? O2 As1 C1 94.30(11) . . ? O1 As1 C1 85.10(11) . . ? C10 As1 C1 121.73(13) . . ? O2 As1 C19 92.15(13) . . ? O1 As1 C19 90.19(13) . . ? C10 As1 C19 114.53(14) . . ? C1 As1 C19 123.71(13) . . ? C7 O1 As1 116.04(16) . . ? C16 O2 As1 116.18(17) . . ? 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 C6 C1 C2 C3 -1.0(5) . . . . ? As1 C1 C2 C3 178.3(3) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C2 C1 C6 C5 1.3(5) . . . . ? As1 C1 C6 C5 -178.1(3) . . . . ? C2 C1 C6 C7 -178.0(3) . . . . ? As1 C1 C6 C7 2.6(4) . . . . ? C4 C5 C6 C1 -0.8(6) . . . . ? C4 C5 C6 C7 178.5(4) . . . . ? C1 C6 C7 O1 -0.1(4) . . . . ? C5 C6 C7 O1 -179.4(3) . . . . ? C1 C6 C7 C8 -120.4(3) . . . . ? C5 C6 C7 C8 60.3(4) . . . . ? C1 C6 C7 C9 117.4(3) . . . . ? C5 C6 C7 C9 -61.9(5) . . . . ? O1 C7 C8 F2 -68.6(4) . . . . ? C6 C7 C8 F2 52.9(4) . . . . ? C9 C7 C8 F2 174.6(3) . . . . ? O1 C7 C8 F1 49.1(4) . . . . ? C6 C7 C8 F1 170.6(3) . . . . ? C9 C7 C8 F1 -67.7(4) . . . . ? O1 C7 C8 F3 170.4(3) . . . . ? C6 C7 C8 F3 -68.2(4) . . . . ? C9 C7 C8 F3 53.5(4) . . . . ? O1 C7 C9 F5 174.3(3) . . . . ? C6 C7 C9 F5 54.5(4) . . . . ? C8 C7 C9 F5 -67.8(4) . . . . ? O1 C7 C9 F6 54.7(4) . . . . ? C6 C7 C9 F6 -65.1(4) . . . . ? C8 C7 C9 F6 172.6(3) . . . . ? O1 C7 C9 F4 -64.1(4) . . . . ? C6 C7 C9 F4 176.1(3) . . . . ? C8 C7 C9 F4 53.8(4) . . . . ? C15 C10 C11 C12 -0.3(6) . . . . ? As1 C10 C11 C12 177.5(3) . . . . ? C10 C11 C12 C13 -1.6(7) . . . . ? C11 C12 C13 C14 1.5(7) . . . . ? C12 C13 C14 C15 0.6(7) . . . . ? C11 C10 C15 C14 2.4(5) . . . . ? As1 C10 C15 C14 -175.6(3) . . . . ? C11 C10 C15 C16 -177.1(3) . . . . ? As1 C10 C15 C16 4.8(4) . . . . ? C13 C14 C15 C10 -2.5(6) . . . . ? C13 C14 C15 C16 177.0(4) . . . . ? C10 C15 C16 O2 -0.6(4) . . . . ? C14 C15 C16 O2 179.9(3) . . . . ? C10 C15 C16 C18 117.2(4) . . . . ? C14 C15 C16 C18 -62.3(5) . . . . ? C10 C15 C16 C17 -119.2(3) . . . . ? C14 C15 C16 C17 61.3(5) . . . . ? O2 C16 C17 F8 -68.1(4) . . . . ? C15 C16 C17 F8 52.1(4) . . . . ? C18 C16 C17 F8 174.5(3) . . . . ? O2 C16 C17 F7 50.9(5) . . . . ? C15 C16 C17 F7 171.2(3) . . . . ? C18 C16 C17 F7 -66.5(5) . . . . ? O2 C16 C17 F9 171.0(4) . . . . ? C15 C16 C17 F9 -68.7(5) . . . . ? C18 C16 C17 F9 53.6(5) . . . . ? O2 C16 C18 F12 58.0(4) . . . . ? C15 C16 C18 F12 -61.8(4) . . . . ? C17 C16 C18 F12 175.6(3) . . . . ? O2 C16 C18 F11 178.2(4) . . . . ? C15 C16 C18 F11 58.4(5) . . . . ? C17 C16 C18 F11 -64.2(5) . . . . ? O2 C16 C18 F10 -60.5(5) . . . . ? C15 C16 C18 F10 179.8(4) . . . . ? C17 C16 C18 F10 57.1(5) . . . . ? As1 C19 C20 O3 -10.1(5) . . . . ? As1 C19 C20 C21 172.1(2) . . . . ? O3 C20 C21 C26 175.0(5) . . . . ? C19 C20 C21 C26 -7.2(6) . . . . ? O3 C20 C21 C22 -5.6(6) . . . . ? C19 C20 C21 C22 172.2(4) . . . . ? C26 C21 C22 C23 0.3(8) . . . . ? C20 C21 C22 C23 -179.2(5) . . . . ? C21 C22 C23 C24 0.6(9) . . . . ? C22 C23 C24 C25 -1.4(10) . . . . ? C23 C24 C25 C26 1.4(10) . . . . ? C22 C21 C26 C25 -0.3(8) . . . . ? C20 C21 C26 C25 179.2(5) . . . . ? C24 C25 C26 C21 -0.6(9) . . . . ? C15 C10 As1 O2 -5.6(3) . . . . ? C11 C10 As1 O2 176.5(3) . . . . ? C15 C10 As1 O1 172.7(2) . . . . ? C11 C10 As1 O1 -5.3(3) . . . . ? C15 C10 As1 C1 86.4(3) . . . . ? C11 C10 As1 C1 -91.5(3) . . . . ? C15 C10 As1 C19 -95.6(3) . . . . ? C11 C10 As1 C19 86.4(3) . . . . ? C6 C1 As1 O2 174.4(2) . . . . ? C2 C1 As1 O2 -4.9(3) . . . . ? C6 C1 As1 O1 -3.1(2) . . . . ? C2 C1 As1 O1 177.5(3) . . . . ? C6 C1 As1 C10 87.7(3) . . . . ? C2 C1 As1 C10 -91.7(3) . . . . ? C6 C1 As1 C19 -90.1(3) . . . . ? C2 C1 As1 C19 90.6(3) . . . . ? C20 C19 As1 O2 85.0(3) . . . . ? C20 C19 As1 O1 -95.8(3) . . . . ? C20 C19 As1 C10 170.5(2) . . . . ? C20 C19 As1 C1 -11.6(3) . . . . ? C6 C7 O1 As1 -2.5(3) . . . . ? C8 C7 O1 As1 119.1(2) . . . . ? C9 C7 O1 As1 -121.7(2) . . . . ? O2 As1 O1 C7 -73(2) . . . . ? C10 As1 O1 C7 -118.4(2) . . . . ? C1 As1 O1 C7 3.2(2) . . . . ? C19 As1 O1 C7 127.0(2) . . . . ? C15 C16 O2 As1 -4.0(4) . . . . ? C18 C16 O2 As1 -123.3(3) . . . . ? C17 C16 O2 As1 116.3(3) . . . . ? O1 As1 O2 C16 -40(2) . . . . ? C10 As1 O2 C16 5.4(3) . . . . ? C1 As1 O2 C16 -116.1(3) . . . . ? C19 As1 O2 C16 119.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 0.518 _refine_diff_density_min -1.705 _refine_diff_density_rms 0.181 # Attachment 'JiangYamamoto6a_CCDC761612.cif' data_Rf2AsCH2CPh2OH_a _database_code_depnum_ccdc_archive 'CCDC 761612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 57 _chemical_formula_moiety ? _chemical_formula_sum 'C32 H21 As F12 O3' _chemical_formula_weight 756.41 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 40.3950(8) _cell_length_b 12.0720(2) _cell_length_c 26.7000(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.5260(10) _cell_angle_gamma 90.00 _cell_volume 12995.6(4) _cell_formula_units_Z 16 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 27.89 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6048 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MacScience DIP2030 Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14609 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.89 _reflns_number_total 14609 _reflns_number_gt 11392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL(Otwinowski, 1997)' _computing_cell_refinement 'HKL(Otwinowski, 1997)' _computing_data_reduction 'HKL(Otwinowski, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1171P)^2^+44.3521P] 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 14609 _refine_ls_number_parameters 912 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 C1 C 0.07247(11) 1.0054(4) 0.49956(16) 0.0357(9) Uani 1 1 d . . . C2 C 0.06157(12) 0.9279(5) 0.53355(16) 0.0422(11) Uani 1 1 d . . . H1 H 0.0710 0.8559 0.5359 0.051 Uiso 1 1 calc R . . C3 C 0.03642(15) 0.9590(6) 0.5639(2) 0.0584(16) Uani 1 1 d . . . H2 H 0.0288 0.9083 0.5879 0.070 Uiso 1 1 calc R . . C4 C 0.02253(16) 1.0619(7) 0.5595(2) 0.070(2) Uani 1 1 d . . . H3 H 0.0053 1.0816 0.5804 0.084 Uiso 1 1 calc R . . C5 C 0.03294(17) 1.1381(6) 0.5252(2) 0.0673(18) Uani 1 1 d . . . H4 H 0.0225 1.2086 0.5220 0.081 Uiso 1 1 calc R . . C6 C 0.05895(14) 1.1104(5) 0.49544(19) 0.0475(12) Uani 1 1 d . . . C7 C 0.07415(14) 1.1839(5) 0.4567(2) 0.0490(12) Uani 1 1 d . . . C8 C 0.04894(16) 1.1934(5) 0.4103(2) 0.0584(15) Uani 1 1 d . . . C9 C 0.08354(18) 1.2980(5) 0.4782(3) 0.0662(18) Uani 1 1 d . . . C10 C 0.10446(12) 0.9345(5) 0.38737(16) 0.0435(12) Uani 1 1 d . . . C11 C 0.10521(14) 1.0058(6) 0.34713(18) 0.0563(15) Uani 1 1 d . . . H5 H 0.1064 1.0838 0.3516 0.068 Uiso 1 1 calc R . . C12 C 0.10417(16) 0.9567(8) 0.2983(2) 0.074(2) Uani 1 1 d . . . H6 H 0.1050 1.0025 0.2694 0.089 Uiso 1 1 calc R . . C13 C 0.10194(18) 0.8439(8) 0.2928(2) 0.072(2) Uani 1 1 d . . . H7 H 0.1011 0.8131 0.2600 0.087 Uiso 1 1 calc R . . C14 C 0.10087(16) 0.7738(7) 0.3335(2) 0.0670(18) Uani 1 1 d . . . H8 H 0.0990 0.6960 0.3291 0.080 Uiso 1 1 calc R . . C15 C 0.10269(13) 0.8214(5) 0.38187(18) 0.0473(12) Uani 1 1 d . . . C16 C 0.10278(12) 0.7566(4) 0.43025(18) 0.0409(11) Uani 1 1 d . . . C17 C 0.06866(14) 0.7014(5) 0.4362(2) 0.0561(15) Uani 1 1 d . . . C18 C 0.13051(14) 0.6667(5) 0.4332(2) 0.0515(13) Uani 1 1 d . . . C19 C 0.15285(11) 0.9964(4) 0.49016(16) 0.0348(9) Uani 1 1 d . . . H9 H 0.1499 1.0098 0.5262 0.042 Uiso 1 1 calc R . . H10 H 0.1642 0.9240 0.4878 0.042 Uiso 1 1 calc R . . C20 C 0.17669(12) 1.0851(4) 0.47263(18) 0.0385(10) Uani 1 1 d . A . C21 C 0.20998(12) 1.0703(4) 0.50318(17) 0.0372(9) Uani 1 1 d . . . C22 C 0.2213(3) 0.9864(10) 0.5336(5) 0.057(3) Uani 0.50 1 d P A 2 H11 H 0.2065 0.9270 0.5388 0.068 Uiso 0.50 1 calc PR A 2 C23 C 0.2530(3) 0.9797(13) 0.5581(5) 0.062(4) Uani 0.50 1 d P A 2 H12 H 0.2592 0.9163 0.5775 0.074 Uiso 0.50 1 calc PR A 2 C24 C 0.2746(4) 1.0637(14) 0.5538(6) 0.047(3) Uani 0.50 1 d P A 2 H13 H 0.2958 1.0603 0.5711 0.056 Uiso 0.50 1 calc PR A 2 C25 C 0.2661(3) 1.1543(10) 0.5246(5) 0.054(3) Uani 0.50 1 d P A 2 H14 H 0.2817 1.2123 0.5212 0.065 Uiso 0.50 1 calc PR A 2 C26 C 0.2350(3) 1.1616(8) 0.5001(4) 0.046(2) Uani 0.50 1 d P A 2 H15 H 0.2293 1.2258 0.4809 0.055 Uiso 0.50 1 calc PR A 2 C27 C 0.18066(12) 1.0774(5) 0.41615(19) 0.0447(12) Uani 1 1 d . . . C28 C 0.18696(14) 0.9776(6) 0.3931(2) 0.0545(14) Uani 1 1 d . A . H16 H 0.1892 0.9121 0.4127 0.065 Uiso 1 1 calc R . . C29 C 0.19008(17) 0.9719(8) 0.3413(2) 0.075(2) Uani 1 1 d . . . H17 H 0.1941 0.9025 0.3259 0.090 Uiso 1 1 calc R A . C30 C 0.18739(16) 1.0660(10) 0.3124(3) 0.087(3) Uani 1 1 d . A . H18 H 0.1889 1.0615 0.2771 0.104 Uiso 1 1 calc R . . C31 C 0.18262(18) 1.1656(8) 0.3345(3) 0.077(2) Uani 1 1 d . . . H19 H 0.1818 1.2310 0.3147 0.093 Uiso 1 1 calc R A . C32 C 0.17886(15) 1.1732(6) 0.3866(2) 0.0630(17) Uani 1 1 d . A . H20 H 0.1751 1.2431 0.4016 0.076 Uiso 1 1 calc R . . O1 O 0.10327(9) 1.1363(3) 0.44090(13) 0.0432(8) Uani 1 1 d . . . O2 O 0.10945(8) 0.8251(3) 0.47096(11) 0.0365(7) Uani 1 1 d . . . O3 O 0.16526(10) 1.1915(3) 0.48646(16) 0.0521(9) Uani 1 1 d . . . H21 H 0.1451 1.1979 0.4774 0.078 Uiso 1 1 calc R A . As1 As 0.108714(11) 0.98061(4) 0.457002(15) 0.03101(13) Uani 1 1 d . . . F1 F 0.06200(11) 1.2501(4) 0.37253(16) 0.0823(13) Uani 1 1 d . . . F2 F 0.04162(9) 1.0938(3) 0.39171(12) 0.0579(8) Uani 1 1 d . . . F3 F 0.02081(10) 1.2426(4) 0.42110(17) 0.0810(12) Uani 1 1 d . . . F4 F 0.10190(13) 1.3548(3) 0.44655(19) 0.0895(14) Uani 1 1 d . . . F5 F 0.05744(13) 1.3610(4) 0.48690(19) 0.0938(15) Uani 1 1 d . . . F6 F 0.10175(11) 1.2874(3) 0.52081(16) 0.0810(13) Uani 1 1 d . . . F7 F 0.06659(11) 0.6500(4) 0.48004(15) 0.0746(11) Uani 1 1 d . . . F8 F 0.04511(8) 0.7810(4) 0.43320(14) 0.0688(10) Uani 1 1 d . . . F9 F 0.06028(10) 0.6295(4) 0.39953(16) 0.0853(14) Uani 1 1 d . . . F10 F 0.13247(11) 0.6131(3) 0.47640(15) 0.0659(10) Uani 1 1 d . . . F11 F 0.12650(11) 0.5910(3) 0.39640(16) 0.0761(12) Uani 1 1 d . . . F12 F 0.15995(8) 0.7155(3) 0.42775(14) 0.0594(8) Uani 1 1 d . . . C33 C 0.2082(3) 1.0808(9) 0.5534(4) 0.046(2) Uani 0.50 1 d P A 1 H22 H 0.1878 1.0988 0.5674 0.055 Uiso 0.50 1 calc PR A 1 C34 C 0.2368(3) 1.0646(11) 0.5844(4) 0.053(3) Uani 0.50 1 d P A 1 H23 H 0.2360 1.0746 0.6196 0.064 Uiso 0.50 1 calc PR A 1 C35 C 0.2662(4) 1.0342(14) 0.5645(7) 0.049(3) Uani 0.50 1 d P A 1 H24 H 0.2858 1.0249 0.5857 0.058 Uiso 0.50 1 calc PR A 1 C36 C 0.2667(3) 1.0174(9) 0.5128(4) 0.045(2) Uani 0.50 1 d P A 1 H25 H 0.2867 0.9965 0.4986 0.054 Uiso 0.50 1 calc PR A 1 C37 C 0.2381(2) 1.0310(8) 0.4822(4) 0.039(2) Uani 0.50 1 d P A 1 H26 H 0.2378 1.0136 0.4475 0.047 Uiso 0.50 1 calc PR A 1 C38 C 0.10474(11) 0.4373(3) 0.24008(17) 0.0343(9) Uani 1 1 d . . . C39 C 0.10892(14) 0.4367(4) 0.29205(18) 0.0413(11) Uani 1 1 d . . . H27 H 0.1300 0.4221 0.3085 0.050 Uiso 1 1 calc R . . C40 C 0.08147(16) 0.4583(5) 0.3193(2) 0.0562(16) Uani 1 1 d . . . H28 H 0.0834 0.4564 0.3550 0.067 Uiso 1 1 calc R . . C41 C 0.05154(16) 0.4823(6) 0.2946(3) 0.071(2) Uani 1 1 d . . . H29 H 0.0330 0.4985 0.3136 0.086 Uiso 1 1 calc R . . C42 C 0.04748(15) 0.4835(6) 0.2422(3) 0.0660(19) Uani 1 1 d . . . H30 H 0.0267 0.5020 0.2257 0.079 Uiso 1 1 calc R . . C43 C 0.07461(11) 0.4569(4) 0.2147(2) 0.0403(11) Uani 1 1 d . . . C44 C 0.07420(11) 0.4469(4) 0.15811(19) 0.0390(10) Uani 1 1 d . . . C45 C 0.06688(17) 0.5603(6) 0.1338(3) 0.0668(18) Uani 1 1 d . . . C46 C 0.04824(13) 0.3598(5) 0.1391(2) 0.0515(13) Uani 1 1 d . . . C47 C 0.16762(11) 0.4994(3) 0.16150(18) 0.0334(9) Uani 1 1 d . . . C48 C 0.16219(13) 0.5324(4) 0.11230(19) 0.0421(11) Uani 1 1 d . . . H31 H 0.1430 0.5090 0.0927 0.051 Uiso 1 1 calc R . . C49 C 0.18565(16) 0.6013(5) 0.0920(2) 0.0558(14) Uani 1 1 d . . . H32 H 0.1826 0.6250 0.0581 0.067 Uiso 1 1 calc R . . C50 C 0.21330(16) 0.6349(5) 0.1212(3) 0.0596(16) Uani 1 1 d . . . H33 H 0.2292 0.6811 0.1068 0.072 Uiso 1 1 calc R . . C51 C 0.21820(13) 0.6032(4) 0.1704(2) 0.0508(13) Uani 1 1 d . . . H34 H 0.2370 0.6287 0.1902 0.061 Uiso 1 1 calc R . . C52 C 0.19529(11) 0.5333(4) 0.1911(2) 0.0381(10) Uani 1 1 d . . . C53 C 0.19637(12) 0.4916(4) 0.2453(2) 0.0402(11) Uani 1 1 d . . . C54 C 0.18709(14) 0.5885(4) 0.2796(2) 0.0496(13) Uani 1 1 d . . . C55 C 0.23016(14) 0.4438(5) 0.2630(2) 0.0534(14) Uani 1 1 d . . . C56 C 0.14218(11) 0.2375(3) 0.19081(16) 0.0308(8) Uani 1 1 d . . . H35 H 0.1611 0.2123 0.2132 0.037 Uiso 1 1 calc R . . H36 H 0.1218 0.2061 0.2041 0.037 Uiso 1 1 calc R . . C57 C 0.14612(11) 0.1862(3) 0.13850(16) 0.0332(9) Uani 1 1 d . . . C58 C 0.17755(13) 0.2281(4) 0.11468(19) 0.0433(11) Uani 1 1 d . . . C59 C 0.20744(14) 0.2439(5) 0.1422(2) 0.0528(13) Uani 1 1 d . . . H37 H 0.2087 0.2302 0.1773 0.063 Uiso 1 1 calc R . . C60 C 0.23530(17) 0.2787(8) 0.1198(3) 0.085(3) Uani 1 1 d . . . H38 H 0.2558 0.2866 0.1389 0.102 Uiso 1 1 calc R . . C61 C 0.2333(2) 0.3025(11) 0.0686(3) 0.124(5) Uani 1 1 d . . . H39 H 0.2523 0.3282 0.0528 0.149 Uiso 1 1 calc R . . C62 C 0.2040(2) 0.2887(10) 0.0414(3) 0.105(4) Uani 1 1 d . . . H40 H 0.2028 0.3049 0.0065 0.127 Uiso 1 1 calc R . . C63 C 0.17594(15) 0.2514(6) 0.0635(2) 0.0584(16) Uani 1 1 d . . . H41 H 0.1557 0.2418 0.0439 0.070 Uiso 1 1 calc R . . C64 C 0.14683(13) 0.0600(4) 0.14698(17) 0.0376(10) Uani 1 1 d . . . C65 C 0.17485(19) 0.0032(5) 0.1634(4) 0.106(4) Uani 1 1 d . . . H42 H 0.1952 0.0423 0.1685 0.128 Uiso 1 1 calc R . . C66 C 0.1743(2) -0.1102(5) 0.1729(5) 0.118(4) Uani 1 1 d . . . H43 H 0.1937 -0.1464 0.1865 0.141 Uiso 1 1 calc R . . C67 C 0.14604(17) -0.1691(4) 0.1628(2) 0.0581(15) Uani 1 1 d . . . H44 H 0.1459 -0.2474 0.1664 0.070 Uiso 1 1 calc R . . C68 C 0.11805(18) -0.1140(5) 0.1475(3) 0.070(2) Uani 1 1 d . . . H45 H 0.0979 -0.1540 0.1415 0.085 Uiso 1 1 calc R . . C69 C 0.11824(16) -0.0005(5) 0.1405(3) 0.0615(17) Uani 1 1 d . . . H46 H 0.0981 0.0363 0.1309 0.074 Uiso 1 1 calc R . . As2 As 0.139565(10) 0.39934(3) 0.196330(15) 0.02750(12) Uani 1 1 d . . . O4 O 0.10483(8) 0.4114(3) 0.14324(11) 0.0335(6) Uani 1 1 d . . . O5 O 0.17338(8) 0.4064(2) 0.24973(12) 0.0353(7) Uani 1 1 d . . . O6 O 0.11757(8) 0.2064(3) 0.10579(12) 0.0364(7) Uani 1 1 d . . . H47 H 0.1121 0.2733 0.1078 0.055 Uiso 1 1 calc R . . F13 F 0.06816(14) 0.5549(4) 0.08362(19) 0.1016(17) Uani 1 1 d . . . F14 F 0.03729(13) 0.6013(4) 0.1434(3) 0.1121(19) Uani 1 1 d . . . F15 F 0.08973(12) 0.6326(3) 0.1499(2) 0.0868(14) Uani 1 1 d . . . F16 F 0.05019(9) 0.3384(4) 0.09025(13) 0.0695(11) Uani 1 1 d . . . F17 F 0.05391(10) 0.2649(3) 0.16315(14) 0.0653(10) Uani 1 1 d . . . F18 F 0.01731(9) 0.3894(4) 0.14677(17) 0.0820(14) Uani 1 1 d . . . F19 F 0.18630(11) 0.5573(3) 0.32794(13) 0.0698(10) Uani 1 1 d . . . F20 F 0.20767(10) 0.6744(3) 0.27844(17) 0.0767(12) Uani 1 1 d . . . F21 F 0.15669(8) 0.6258(2) 0.26593(13) 0.0521(8) Uani 1 1 d . . . F22 F 0.22924(10) 0.3931(3) 0.30743(16) 0.0732(11) Uani 1 1 d . . . F23 F 0.24065(9) 0.3694(4) 0.23103(16) 0.0771(12) Uani 1 1 d . . . F24 F 0.25381(9) 0.5215(3) 0.26841(16) 0.0725(11) Uani 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 C1 0.028(2) 0.050(3) 0.0293(19) 0.0007(19) 0.0018(15) 0.0109(18) C2 0.028(2) 0.067(3) 0.032(2) 0.006(2) 0.0032(17) 0.006(2) C3 0.039(3) 0.099(5) 0.039(2) 0.011(3) 0.008(2) 0.017(3) C4 0.043(3) 0.117(6) 0.051(3) 0.005(4) 0.017(3) 0.034(4) C5 0.056(4) 0.081(4) 0.065(4) -0.002(3) 0.005(3) 0.039(3) C6 0.040(3) 0.060(3) 0.042(3) -0.003(2) -0.001(2) 0.020(2) C7 0.042(3) 0.047(3) 0.057(3) 0.009(2) -0.008(2) 0.019(2) C8 0.048(3) 0.058(3) 0.068(4) 0.027(3) -0.009(3) 0.009(3) C9 0.059(4) 0.050(3) 0.086(5) 0.000(3) -0.019(3) 0.019(3) C10 0.026(2) 0.077(4) 0.0266(19) -0.004(2) 0.0015(16) 0.008(2) C11 0.041(3) 0.095(5) 0.032(2) 0.012(3) 0.001(2) 0.010(3) C12 0.043(3) 0.146(8) 0.032(3) 0.014(4) 0.001(2) 0.009(4) C13 0.056(4) 0.124(7) 0.037(3) -0.021(4) 0.001(2) 0.002(4) C14 0.052(4) 0.110(6) 0.038(3) -0.024(3) -0.001(2) -0.001(3) C15 0.031(2) 0.072(4) 0.039(2) -0.018(2) -0.0003(18) 0.001(2) C16 0.032(2) 0.050(3) 0.041(2) -0.019(2) 0.0026(18) -0.0055(19) C17 0.037(3) 0.071(4) 0.060(3) -0.027(3) 0.004(2) -0.013(3) C18 0.041(3) 0.045(3) 0.069(4) -0.024(3) 0.003(2) -0.004(2) C19 0.027(2) 0.042(2) 0.035(2) 0.0083(18) -0.0015(16) 0.0017(17) C20 0.027(2) 0.041(2) 0.047(2) 0.009(2) 0.0017(18) -0.0006(17) C21 0.036(2) 0.039(2) 0.037(2) 0.0081(19) 0.0000(17) -0.0017(18) C22 0.038(6) 0.063(7) 0.067(7) 0.026(6) -0.017(5) -0.023(5) C23 0.033(6) 0.069(8) 0.082(9) 0.036(7) -0.014(6) -0.012(6) C24 0.035(8) 0.049(9) 0.054(9) 0.015(6) -0.010(5) -0.013(6) C25 0.040(6) 0.053(6) 0.068(7) 0.002(5) 0.001(5) -0.022(5) C26 0.042(6) 0.035(5) 0.061(6) 0.012(4) -0.003(4) -0.012(4) C27 0.024(2) 0.067(3) 0.043(2) 0.020(2) -0.0015(18) 0.001(2) C28 0.039(3) 0.079(4) 0.046(3) 0.012(3) 0.004(2) 0.021(3) C29 0.046(4) 0.129(7) 0.052(3) 0.001(4) 0.008(3) 0.034(4) C30 0.038(3) 0.170(9) 0.054(4) 0.043(5) 0.013(3) 0.025(4) C31 0.055(4) 0.117(7) 0.059(4) 0.047(4) 0.002(3) -0.016(4) C32 0.045(3) 0.079(4) 0.064(3) 0.038(3) -0.005(3) -0.010(3) O1 0.0353(19) 0.0460(18) 0.0477(18) 0.0112(16) -0.0027(14) 0.0080(14) O2 0.0357(18) 0.0386(16) 0.0348(15) -0.0063(13) -0.0002(12) -0.0014(13) O3 0.037(2) 0.0372(18) 0.082(3) 0.0053(18) -0.0034(18) -0.0004(14) As1 0.0244(2) 0.0416(2) 0.0271(2) 0.00105(17) 0.00143(15) 0.00406(16) F1 0.077(3) 0.087(3) 0.079(2) 0.044(2) -0.026(2) -0.006(2) F2 0.047(2) 0.072(2) 0.0536(18) 0.0105(16) -0.0079(14) 0.0006(16) F3 0.056(2) 0.081(3) 0.102(3) 0.011(2) -0.023(2) 0.035(2) F4 0.097(4) 0.051(2) 0.118(4) 0.005(2) -0.015(3) -0.005(2) F5 0.085(3) 0.069(2) 0.124(4) -0.019(3) -0.022(3) 0.044(2) F6 0.076(3) 0.072(2) 0.091(3) -0.025(2) -0.026(2) 0.026(2) F7 0.067(3) 0.082(3) 0.076(2) -0.001(2) 0.0153(19) -0.030(2) F8 0.0310(17) 0.100(3) 0.076(2) -0.026(2) 0.0069(15) -0.0015(17) F9 0.052(2) 0.111(3) 0.094(3) -0.059(3) 0.012(2) -0.034(2) F10 0.079(3) 0.0419(17) 0.077(2) -0.0035(17) 0.0037(19) 0.0048(16) F11 0.066(3) 0.070(2) 0.093(3) -0.049(2) 0.006(2) -0.0011(19) F12 0.0324(17) 0.0593(19) 0.086(2) -0.0124(18) 0.0023(15) 0.0025(14) C33 0.036(5) 0.060(6) 0.041(5) -0.010(5) -0.009(4) -0.002(4) C34 0.049(7) 0.071(7) 0.037(5) -0.001(5) -0.018(4) -0.010(6) C35 0.040(10) 0.046(9) 0.058(9) 0.022(6) -0.017(7) -0.014(6) C36 0.033(5) 0.053(6) 0.048(5) 0.007(5) -0.005(4) -0.002(4) C37 0.035(5) 0.045(5) 0.037(4) 0.002(4) 0.000(4) -0.003(4) C38 0.029(2) 0.0274(19) 0.047(2) -0.0087(18) 0.0098(17) -0.0091(16) C39 0.049(3) 0.033(2) 0.043(2) -0.010(2) 0.011(2) -0.016(2) C40 0.060(4) 0.058(3) 0.053(3) -0.024(3) 0.023(3) -0.029(3) C41 0.041(3) 0.096(5) 0.081(4) -0.050(4) 0.031(3) -0.027(3) C42 0.029(3) 0.085(4) 0.085(4) -0.044(4) 0.014(3) -0.010(3) C43 0.023(2) 0.038(2) 0.061(3) -0.019(2) 0.0067(19) -0.0087(17) C44 0.020(2) 0.039(2) 0.057(3) -0.002(2) -0.0019(18) -0.0022(17) C45 0.045(4) 0.056(3) 0.098(5) 0.020(4) -0.004(3) 0.012(3) C46 0.031(3) 0.068(4) 0.056(3) -0.017(3) 0.004(2) -0.011(2) C47 0.026(2) 0.0273(19) 0.049(2) -0.0010(18) 0.0105(17) -0.0034(15) C48 0.041(3) 0.039(2) 0.048(3) 0.002(2) 0.014(2) -0.0054(19) C49 0.054(4) 0.052(3) 0.064(3) 0.007(3) 0.026(3) -0.007(3) C50 0.049(3) 0.047(3) 0.086(4) 0.005(3) 0.038(3) -0.014(2) C51 0.031(3) 0.038(2) 0.084(4) -0.012(3) 0.014(2) -0.0115(19) C52 0.024(2) 0.029(2) 0.062(3) -0.009(2) 0.0100(19) -0.0043(16) C53 0.024(2) 0.038(2) 0.058(3) -0.015(2) -0.0017(19) -0.0114(17) C54 0.040(3) 0.047(3) 0.061(3) -0.023(2) 0.003(2) -0.015(2) C55 0.036(3) 0.056(3) 0.067(3) -0.018(3) -0.010(2) -0.002(2) C56 0.032(2) 0.0221(17) 0.038(2) -0.0028(16) 0.0003(16) -0.0026(15) C57 0.034(2) 0.0271(19) 0.038(2) -0.0082(17) -0.0041(17) -0.0022(16) C58 0.038(3) 0.044(3) 0.049(3) -0.017(2) 0.007(2) -0.007(2) C59 0.039(3) 0.067(4) 0.052(3) -0.017(3) 0.001(2) -0.013(2) C60 0.041(4) 0.145(7) 0.069(4) -0.038(5) 0.010(3) -0.036(4) C61 0.060(5) 0.244(13) 0.072(5) -0.046(6) 0.033(4) -0.077(7) C62 0.071(5) 0.198(11) 0.050(3) -0.036(5) 0.023(3) -0.064(6) C63 0.048(3) 0.085(4) 0.043(3) -0.023(3) 0.012(2) -0.022(3) C64 0.042(3) 0.029(2) 0.041(2) -0.0116(18) -0.0051(18) -0.0012(18) C65 0.051(4) 0.030(3) 0.231(11) -0.022(4) -0.054(6) 0.002(3) C66 0.062(5) 0.036(3) 0.247(13) -0.016(5) -0.054(6) 0.013(3) C67 0.071(4) 0.028(2) 0.075(4) -0.007(2) -0.003(3) -0.001(2) C68 0.061(4) 0.044(3) 0.104(5) 0.019(3) -0.015(4) -0.018(3) C69 0.044(3) 0.044(3) 0.094(5) 0.018(3) -0.016(3) -0.008(2) As2 0.0225(2) 0.0243(2) 0.0358(2) -0.00326(16) 0.00247(15) -0.00456(14) O4 0.0253(15) 0.0381(16) 0.0365(15) -0.0009(13) -0.0019(11) -0.0027(12) O5 0.0325(17) 0.0303(15) 0.0423(16) -0.0039(13) -0.0051(12) -0.0064(12) O6 0.0358(18) 0.0341(15) 0.0381(16) -0.0043(13) -0.0067(12) -0.0010(13) F13 0.102(4) 0.104(4) 0.096(3) 0.053(3) -0.015(3) 0.013(3) F14 0.063(3) 0.091(3) 0.182(5) 0.032(3) 0.005(3) 0.042(3) F15 0.079(3) 0.0349(17) 0.146(4) 0.015(2) 0.002(3) -0.0032(18) F16 0.043(2) 0.108(3) 0.0561(19) -0.026(2) -0.0054(15) -0.0129(19) F17 0.066(2) 0.0547(19) 0.077(2) -0.0180(18) 0.0178(18) -0.0351(17) F18 0.0243(17) 0.119(3) 0.102(3) -0.054(3) 0.0034(17) -0.0150(19) F19 0.076(3) 0.074(2) 0.058(2) -0.0273(19) -0.0018(18) -0.004(2) F20 0.061(2) 0.058(2) 0.113(3) -0.046(2) 0.025(2) -0.0307(18) F21 0.0430(18) 0.0400(15) 0.075(2) -0.0154(15) 0.0141(15) -0.0014(12) F22 0.050(2) 0.082(3) 0.083(3) 0.003(2) -0.0248(19) 0.0014(18) F23 0.042(2) 0.084(3) 0.102(3) -0.038(2) -0.0231(19) 0.0262(19) F24 0.0319(18) 0.087(3) 0.097(3) -0.022(2) -0.0115(17) -0.0187(17) _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 C1 C6 1.382(7) . ? C1 C2 1.394(7) . ? C1 As1 1.931(4) . ? C2 C3 1.390(7) . ? C2 H1 0.9500 . ? C3 C4 1.366(10) . ? C3 H2 0.9500 . ? C4 C5 1.381(10) . ? C4 H3 0.9500 . ? C5 C6 1.397(8) . ? C5 H4 0.9500 . ? C6 C7 1.520(8) . ? C7 O1 1.398(6) . ? C7 C9 1.530(9) . ? C7 C8 1.559(7) . ? C8 F2 1.328(8) . ? C8 F3 1.330(7) . ? C8 F1 1.352(7) . ? C9 F6 1.323(7) . ? C9 F5 1.332(8) . ? C9 F4 1.345(9) . ? C10 C15 1.374(8) . ? C10 C11 1.379(8) . ? C10 As1 1.938(4) . ? C11 C12 1.431(9) . ? C11 H5 0.9500 . ? C12 C13 1.372(12) . ? C12 H6 0.9500 . ? C13 C14 1.379(11) . ? C13 H7 0.9500 . ? C14 C15 1.411(7) . ? C14 H8 0.9500 . ? C15 C16 1.510(8) . ? C16 O2 1.379(5) . ? C16 C17 1.547(7) . ? C16 C18 1.558(7) . ? C17 F7 1.333(8) . ? C17 F9 1.336(6) . ? C17 F8 1.351(7) . ? C18 F10 1.319(7) . ? C18 F12 1.343(6) . ? C18 F11 1.345(6) . ? C19 C20 1.533(6) . ? C19 As1 1.951(4) . ? C19 H9 0.9900 . ? C19 H10 0.9900 . ? C20 O3 1.421(6) . ? C20 C27 1.529(7) . ? C20 C21 1.540(6) . ? C21 C33 1.354(11) . ? C21 C22 1.361(12) . ? C21 C37 1.382(11) . ? C21 C26 1.500(10) . ? C22 C23 1.403(15) . ? C22 H11 0.9500 . ? C23 C24 1.345(16) . ? C23 H12 0.9500 . ? C24 C25 1.38(2) . ? C24 H13 0.9500 . ? C25 C26 1.383(15) . ? C25 H14 0.9500 . ? C26 H15 0.9500 . ? C27 C28 1.384(9) . ? C27 C32 1.399(8) . ? C28 C29 1.399(8) . ? C28 H16 0.9500 . ? C29 C30 1.374(12) . ? C29 H17 0.9500 . ? C30 C31 1.358(13) . ? C30 H18 0.9500 . ? C31 C32 1.412(10) . ? C31 H19 0.9500 . ? C32 H20 0.9500 . ? O1 As1 1.937(3) . ? O2 As1 1.914(3) . ? O3 H21 0.8400 . ? C33 C34 1.390(14) . ? C33 H22 0.9500 . ? C34 C35 1.38(2) . ? C34 H23 0.9500 . ? C35 C36 1.40(2) . ? C35 H24 0.9500 . ? C36 C37 1.382(13) . ? C36 H25 0.9500 . ? C37 H26 0.9500 . ? C38 C43 1.376(7) . ? C38 C39 1.387(7) . ? C38 As2 1.938(4) . ? C39 C40 1.388(7) . ? C39 H27 0.9500 . ? C40 C41 1.373(10) . ? C40 H28 0.9500 . ? C41 C42 1.398(10) . ? C41 H29 0.9500 . ? C42 C43 1.393(7) . ? C42 H30 0.9500 . ? C43 C44 1.516(7) . ? C44 O4 1.390(5) . ? C44 C45 1.536(8) . ? C44 C46 1.549(7) . ? C45 F15 1.323(8) . ? C45 F14 1.334(8) . ? C45 F13 1.345(9) . ? C46 F17 1.327(8) . ? C46 F18 1.328(6) . ? C46 F16 1.337(6) . ? C47 C48 1.378(7) . ? C47 C52 1.391(6) . ? C47 As2 1.933(4) . ? C48 C49 1.395(7) . ? C48 H31 0.9500 . ? C49 C50 1.383(10) . ? C49 H32 0.9500 . ? C50 C51 1.373(9) . ? C50 H33 0.9500 . ? C51 C52 1.391(6) . ? C51 H34 0.9500 . ? C52 C53 1.531(8) . ? C53 O5 1.395(5) . ? C53 C55 1.529(7) . ? C53 C54 1.546(7) . ? C54 F20 1.331(6) . ? C54 F21 1.338(7) . ? C54 F19 1.346(7) . ? C55 F23 1.326(7) . ? C55 F22 1.338(7) . ? C55 F24 1.341(6) . ? C56 C57 1.545(6) . ? C56 As2 1.963(4) . ? C56 H35 0.9900 . ? C56 H36 0.9900 . ? C57 O6 1.424(5) . ? C57 C58 1.540(7) . ? C57 C64 1.540(6) . ? C58 C59 1.387(7) . ? C58 C63 1.393(8) . ? C59 C60 1.373(8) . ? C59 H37 0.9500 . ? C60 C61 1.393(11) . ? C60 H38 0.9500 . ? C61 C62 1.359(11) . ? C61 H39 0.9500 . ? C62 C63 1.386(9) . ? C62 H40 0.9500 . ? C63 H41 0.9500 . ? C64 C69 1.369(7) . ? C64 C65 1.372(8) . ? C65 C66 1.394(9) . ? C65 H42 0.9500 . ? C66 C67 1.356(10) . ? C66 H43 0.9500 . ? C67 C68 1.353(9) . ? C67 H44 0.9500 . ? C68 C69 1.383(8) . ? C68 H45 0.9500 . ? C69 H46 0.9500 . ? As2 O5 1.915(3) . ? As2 O4 1.938(3) . ? O6 H47 0.8400 . ? 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 C6 C1 C2 121.9(4) . . ? C6 C1 As1 113.9(4) . . ? C2 C1 As1 124.1(4) . . ? C3 C2 C1 118.0(5) . . ? C3 C2 H1 121.0 . . ? C1 C2 H1 121.0 . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H2 119.8 . . ? C2 C3 H2 119.8 . . ? C3 C4 C5 121.6(5) . . ? C3 C4 H3 119.2 . . ? C5 C4 H3 119.2 . . ? C4 C5 C6 119.2(6) . . ? C4 C5 H4 120.4 . . ? C6 C5 H4 120.4 . . ? C1 C6 C5 118.8(6) . . ? C1 C6 C7 114.5(4) . . ? C5 C6 C7 126.6(5) . . ? O1 C7 C6 110.4(4) . . ? O1 C7 C9 106.8(5) . . ? C6 C7 C9 111.8(5) . . ? O1 C7 C8 108.1(5) . . ? C6 C7 C8 108.2(5) . . ? C9 C7 C8 111.5(4) . . ? F2 C8 F3 108.2(5) . . ? F2 C8 F1 105.5(5) . . ? F3 C8 F1 108.3(5) . . ? F2 C8 C7 110.5(4) . . ? F3 C8 C7 112.7(5) . . ? F1 C8 C7 111.4(5) . . ? F6 C9 F5 108.0(6) . . ? F6 C9 F4 106.9(6) . . ? F5 C9 F4 107.0(5) . . ? F6 C9 C7 110.3(5) . . ? F5 C9 C7 113.5(6) . . ? F4 C9 C7 110.9(6) . . ? C15 C10 C11 122.7(5) . . ? C15 C10 As1 112.9(4) . . ? C11 C10 As1 124.3(5) . . ? C10 C11 C12 116.8(7) . . ? C10 C11 H5 121.6 . . ? C12 C11 H5 121.6 . . ? C13 C12 C11 120.4(6) . . ? C13 C12 H6 119.8 . . ? C11 C12 H6 119.8 . . ? C12 C13 C14 122.0(6) . . ? C12 C13 H7 119.0 . . ? C14 C13 H7 119.0 . . ? C13 C14 C15 117.9(7) . . ? C13 C14 H8 121.0 . . ? C15 C14 H8 121.0 . . ? C10 C15 C14 120.1(6) . . ? C10 C15 C16 115.2(4) . . ? C14 C15 C16 124.7(6) . . ? O2 C16 C15 110.7(4) . . ? O2 C16 C17 108.0(4) . . ? C15 C16 C17 110.8(4) . . ? O2 C16 C18 105.8(4) . . ? C15 C16 C18 111.6(4) . . ? C17 C16 C18 109.7(5) . . ? F7 C17 F9 108.3(5) . . ? F7 C17 F8 107.5(5) . . ? F9 C17 F8 105.9(5) . . ? F7 C17 C16 113.2(5) . . ? F9 C17 C16 113.1(5) . . ? F8 C17 C16 108.4(5) . . ? F10 C18 F12 107.7(5) . . ? F10 C18 F11 107.7(5) . . ? F12 C18 F11 106.6(5) . . ? F10 C18 C16 113.0(5) . . ? F12 C18 C16 109.1(4) . . ? F11 C18 C16 112.4(5) . . ? C20 C19 As1 120.2(3) . . ? C20 C19 H9 107.3 . . ? As1 C19 H9 107.3 . . ? C20 C19 H10 107.3 . . ? As1 C19 H10 107.3 . . ? H9 C19 H10 106.9 . . ? O3 C20 C27 111.5(4) . . ? O3 C20 C19 109.4(4) . . ? C27 C20 C19 111.4(4) . . ? O3 C20 C21 104.8(4) . . ? C27 C20 C21 112.0(4) . . ? C19 C20 C21 107.5(4) . . ? C33 C21 C22 60.9(8) . . ? C33 C21 C37 121.9(7) . . ? C22 C21 C37 74.4(7) . . ? C33 C21 C26 93.6(7) . . ? C22 C21 C26 112.1(7) . . ? C37 C21 C26 69.9(6) . . ? C33 C21 C20 114.7(6) . . ? C22 C21 C20 130.9(6) . . ? C37 C21 C20 122.6(5) . . ? C26 C21 C20 117.0(5) . . ? C21 C22 C23 125.8(10) . . ? C21 C22 H11 117.1 . . ? C23 C22 H11 117.1 . . ? C24 C23 C22 119.7(14) . . ? C24 C23 H12 120.2 . . ? C22 C23 H12 120.2 . . ? C23 C24 C25 120.4(15) . . ? C23 C24 H13 119.8 . . ? C25 C24 H13 119.8 . . ? C24 C25 C26 120.4(11) . . ? C24 C25 H14 119.8 . . ? C26 C25 H14 119.8 . . ? C25 C26 C21 121.5(9) . . ? C25 C26 H15 119.3 . . ? C21 C26 H15 119.3 . . ? C28 C27 C32 118.3(5) . . ? C28 C27 C20 121.7(5) . . ? C32 C27 C20 120.0(6) . . ? C27 C28 C29 120.9(6) . . ? C27 C28 H16 119.6 . . ? C29 C28 H16 119.6 . . ? C30 C29 C28 120.4(8) . . ? C30 C29 H17 119.8 . . ? C28 C29 H17 119.8 . . ? C31 C30 C29 119.8(7) . . ? C31 C30 H18 120.1 . . ? C29 C30 H18 120.1 . . ? C30 C31 C32 120.9(7) . . ? C30 C31 H19 119.6 . . ? C32 C31 H19 119.6 . . ? C27 C32 C31 119.8(7) . . ? C27 C32 H20 120.1 . . ? C31 C32 H20 120.1 . . ? C7 O1 As1 114.7(3) . . ? C16 O2 As1 115.8(3) . . ? C20 O3 H21 109.5 . . ? O2 As1 C1 92.33(18) . . ? O2 As1 O1 174.23(15) . . ? C1 As1 O1 84.28(18) . . ? O2 As1 C10 84.5(2) . . ? C1 As1 C10 125.7(2) . . ? O1 As1 C10 93.7(2) . . ? O2 As1 C19 90.27(17) . . ? C1 As1 C19 115.01(19) . . ? O1 As1 C19 95.39(17) . . ? C10 As1 C19 119.22(19) . . ? C21 C33 C34 118.9(10) . . ? C21 C33 H22 120.5 . . ? C34 C33 H22 120.5 . . ? C35 C34 C33 120.8(12) . . ? C35 C34 H23 119.6 . . ? C33 C34 H23 119.6 . . ? C34 C35 C36 118.7(13) . . ? C34 C35 H24 120.6 . . ? C36 C35 H24 120.6 . . ? C37 C36 C35 120.5(11) . . ? C37 C36 H25 119.8 . . ? C35 C36 H25 119.8 . . ? C36 C37 C21 118.6(9) . . ? C36 C37 H26 120.7 . . ? C21 C37 H26 120.7 . . ? C43 C38 C39 122.8(4) . . ? C43 C38 As2 113.4(3) . . ? C39 C38 As2 123.6(4) . . ? C38 C39 C40 118.2(5) . . ? C38 C39 H27 120.9 . . ? C40 C39 H27 120.9 . . ? C41 C40 C39 119.7(5) . . ? C41 C40 H28 120.2 . . ? C39 C40 H28 120.2 . . ? C40 C41 C42 121.9(5) . . ? C40 C41 H29 119.0 . . ? C42 C41 H29 119.0 . . ? C43 C42 C41 118.5(6) . . ? C43 C42 H30 120.8 . . ? C41 C42 H30 120.8 . . ? C38 C43 C42 118.7(5) . . ? C38 C43 C44 115.6(4) . . ? C42 C43 C44 125.7(5) . . ? O4 C44 C43 110.7(4) . . ? O4 C44 C45 107.8(4) . . ? C43 C44 C45 110.0(5) . . ? O4 C44 C46 107.0(4) . . ? C43 C44 C46 110.3(4) . . ? C45 C44 C46 111.0(5) . . ? F15 C45 F14 107.9(6) . . ? F15 C45 F13 106.7(6) . . ? F14 C45 F13 107.4(6) . . ? F15 C45 C44 109.7(5) . . ? F14 C45 C44 113.6(6) . . ? F13 C45 C44 111.1(6) . . ? F17 C46 F18 107.1(5) . . ? F17 C46 F16 106.6(5) . . ? F18 C46 F16 108.4(5) . . ? F17 C46 C44 109.6(4) . . ? F18 C46 C44 113.1(5) . . ? F16 C46 C44 111.8(4) . . ? C48 C47 C52 122.1(4) . . ? C48 C47 As2 125.2(4) . . ? C52 C47 As2 112.6(3) . . ? C47 C48 C49 118.1(5) . . ? C47 C48 H31 121.0 . . ? C49 C48 H31 121.0 . . ? C50 C49 C48 120.1(6) . . ? C50 C49 H32 120.0 . . ? C48 C49 H32 120.0 . . ? C51 C50 C49 121.4(5) . . ? C51 C50 H33 119.3 . . ? C49 C50 H33 119.3 . . ? C50 C51 C52 119.3(5) . . ? C50 C51 H34 120.4 . . ? C52 C51 H34 120.4 . . ? C47 C52 C51 119.0(5) . . ? C47 C52 C53 114.6(4) . . ? C51 C52 C53 126.4(5) . . ? O5 C53 C55 106.4(4) . . ? O5 C53 C52 110.0(4) . . ? C55 C53 C52 112.9(4) . . ? O5 C53 C54 108.7(4) . . ? C55 C53 C54 110.3(4) . . ? C52 C53 C54 108.5(4) . . ? F20 C54 F21 107.1(5) . . ? F20 C54 F19 107.0(4) . . ? F21 C54 F19 106.3(5) . . ? F20 C54 C53 113.7(5) . . ? F21 C54 C53 110.2(4) . . ? F19 C54 C53 112.2(5) . . ? F23 C55 F22 106.8(5) . . ? F23 C55 F24 106.8(5) . . ? F22 C55 F24 106.4(5) . . ? F23 C55 C53 111.8(4) . . ? F22 C55 C53 111.9(5) . . ? F24 C55 C53 112.7(5) . . ? C57 C56 As2 118.4(3) . . ? C57 C56 H35 107.7 . . ? As2 C56 H35 107.7 . . ? C57 C56 H36 107.7 . . ? As2 C56 H36 107.7 . . ? H35 C56 H36 107.1 . . ? O6 C57 C58 110.3(4) . . ? O6 C57 C64 105.5(3) . . ? C58 C57 C64 112.2(4) . . ? O6 C57 C56 111.2(4) . . ? C58 C57 C56 112.0(3) . . ? C64 C57 C56 105.4(4) . . ? C59 C58 C63 118.6(5) . . ? C59 C58 C57 122.6(5) . . ? C63 C58 C57 118.8(4) . . ? C60 C59 C58 121.4(6) . . ? C60 C59 H37 119.3 . . ? C58 C59 H37 119.3 . . ? C59 C60 C61 119.4(6) . . ? C59 C60 H38 120.3 . . ? C61 C60 H38 120.3 . . ? C62 C61 C60 119.7(6) . . ? C62 C61 H39 120.1 . . ? C60 C61 H39 120.1 . . ? C61 C62 C63 121.3(7) . . ? C61 C62 H40 119.4 . . ? C63 C62 H40 119.4 . . ? C62 C63 C58 119.6(6) . . ? C62 C63 H41 120.2 . . ? C58 C63 H41 120.2 . . ? C69 C64 C65 116.5(5) . . ? C69 C64 C57 120.1(5) . . ? C65 C64 C57 123.3(5) . . ? C64 C65 C66 121.7(6) . . ? C64 C65 H42 119.1 . . ? C66 C65 H42 119.1 . . ? C67 C66 C65 120.2(7) . . ? C67 C66 H43 119.9 . . ? C65 C66 H43 119.9 . . ? C68 C67 C66 118.6(5) . . ? C68 C67 H44 120.7 . . ? C66 C67 H44 120.7 . . ? C67 C68 C69 121.1(6) . . ? C67 C68 H45 119.5 . . ? C69 C68 H45 119.5 . . ? C64 C69 C68 121.6(6) . . ? C64 C69 H46 119.2 . . ? C68 C69 H46 119.2 . . ? O5 As2 C47 85.29(17) . . ? O5 As2 C38 92.96(17) . . ? C47 As2 C38 127.66(18) . . ? O5 As2 O4 173.07(13) . . ? C47 As2 O4 91.19(17) . . ? C38 As2 O4 84.45(17) . . ? O5 As2 C56 93.51(15) . . ? C47 As2 C56 123.36(18) . . ? C38 As2 C56 108.96(18) . . ? O4 As2 C56 93.42(15) . . ? C44 O4 As2 115.6(3) . . ? C53 O5 As2 114.7(3) . . ? C57 O6 H47 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 C6 C1 C2 C3 -0.2(8) . . . . ? As1 C1 C2 C3 176.4(4) . . . . ? C1 C2 C3 C4 1.3(9) . . . . ? C2 C3 C4 C5 -0.3(11) . . . . ? C3 C4 C5 C6 -1.9(11) . . . . ? C2 C1 C6 C5 -2.0(8) . . . . ? As1 C1 C6 C5 -178.9(5) . . . . ? C2 C1 C6 C7 179.5(5) . . . . ? As1 C1 C6 C7 2.6(6) . . . . ? C4 C5 C6 C1 3.0(10) . . . . ? C4 C5 C6 C7 -178.7(6) . . . . ? C1 C6 C7 O1 -12.2(7) . . . . ? C5 C6 C7 O1 169.4(6) . . . . ? C1 C6 C7 C9 -131.0(5) . . . . ? C5 C6 C7 C9 50.6(8) . . . . ? C1 C6 C7 C8 105.9(5) . . . . ? C5 C6 C7 C8 -72.6(8) . . . . ? O1 C7 C8 F2 61.7(6) . . . . ? C6 C7 C8 F2 -57.8(6) . . . . ? C9 C7 C8 F2 178.8(6) . . . . ? O1 C7 C8 F3 -177.1(5) . . . . ? C6 C7 C8 F3 63.4(6) . . . . ? C9 C7 C8 F3 -60.0(7) . . . . ? O1 C7 C8 F1 -55.3(6) . . . . ? C6 C7 C8 F1 -174.8(5) . . . . ? C9 C7 C8 F1 61.8(7) . . . . ? O1 C7 C9 F6 -69.5(7) . . . . ? C6 C7 C9 F6 51.3(8) . . . . ? C8 C7 C9 F6 172.6(6) . . . . ? O1 C7 C9 F5 169.2(5) . . . . ? C6 C7 C9 F5 -70.0(7) . . . . ? C8 C7 C9 F5 51.3(8) . . . . ? O1 C7 C9 F4 48.7(6) . . . . ? C6 C7 C9 F4 169.5(5) . . . . ? C8 C7 C9 F4 -69.2(7) . . . . ? C15 C10 C11 C12 -0.2(8) . . . . ? As1 C10 C11 C12 175.5(4) . . . . ? C10 C11 C12 C13 1.1(9) . . . . ? C11 C12 C13 C14 -0.5(10) . . . . ? C12 C13 C14 C15 -1.0(10) . . . . ? C11 C10 C15 C14 -1.3(8) . . . . ? As1 C10 C15 C14 -177.5(4) . . . . ? C11 C10 C15 C16 178.9(5) . . . . ? As1 C10 C15 C16 2.7(6) . . . . ? C13 C14 C15 C10 1.9(9) . . . . ? C13 C14 C15 C16 -178.3(6) . . . . ? C10 C15 C16 O2 -8.6(6) . . . . ? C14 C15 C16 O2 171.6(5) . . . . ? C10 C15 C16 C17 111.2(5) . . . . ? C14 C15 C16 C17 -68.6(7) . . . . ? C10 C15 C16 C18 -126.2(5) . . . . ? C14 C15 C16 C18 54.0(7) . . . . ? O2 C16 C17 F7 -53.8(6) . . . . ? C15 C16 C17 F7 -175.2(5) . . . . ? C18 C16 C17 F7 61.1(6) . . . . ? O2 C16 C17 F9 -177.5(5) . . . . ? C15 C16 C17 F9 61.1(7) . . . . ? C18 C16 C17 F9 -62.6(7) . . . . ? O2 C16 C17 F8 65.4(6) . . . . ? C15 C16 C17 F8 -56.0(5) . . . . ? C18 C16 C17 F8 -179.7(4) . . . . ? O2 C16 C18 F10 55.7(5) . . . . ? C15 C16 C18 F10 176.2(4) . . . . ? C17 C16 C18 F10 -60.6(5) . . . . ? O2 C16 C18 F12 -64.1(6) . . . . ? C15 C16 C18 F12 56.4(6) . . . . ? C17 C16 C18 F12 179.6(4) . . . . ? O2 C16 C18 F11 177.9(5) . . . . ? C15 C16 C18 F11 -61.6(6) . . . . ? C17 C16 C18 F11 61.6(6) . . . . ? As1 C19 C20 O3 71.1(5) . . . . ? As1 C19 C20 C27 -52.6(5) . . . . ? As1 C19 C20 C21 -175.6(3) . . . . ? O3 C20 C21 C33 56.5(7) . . . . ? C27 C20 C21 C33 177.5(6) . . . . ? C19 C20 C21 C33 -59.9(7) . . . . ? O3 C20 C21 C22 128.3(10) . . . . ? C27 C20 C21 C22 -110.6(10) . . . . ? C19 C20 C21 C22 12.0(11) . . . . ? O3 C20 C21 C37 -134.1(6) . . . . ? C27 C20 C21 C37 -13.1(8) . . . . ? C19 C20 C21 C37 109.6(7) . . . . ? O3 C20 C21 C26 -51.7(7) . . . . ? C27 C20 C21 C26 69.4(7) . . . . ? C19 C20 C21 C26 -168.0(6) . . . . ? C33 C21 C22 C23 -84.4(15) . . . . ? C37 C21 C22 C23 57.1(15) . . . . ? C26 C21 C22 C23 -3.0(18) . . . . ? C20 C21 C22 C23 177.0(11) . . . . ? C21 C22 C23 C24 3(2) . . . . ? C22 C23 C24 C25 -2(3) . . . . ? C23 C24 C25 C26 2(2) . . . . ? C24 C25 C26 C21 -1.9(19) . . . . ? C33 C21 C26 C25 62.4(12) . . . . ? C22 C21 C26 C25 2.5(14) . . . . ? C37 C21 C26 C25 -60.3(11) . . . . ? C20 C21 C26 C25 -177.5(9) . . . . ? O3 C20 C27 C28 -170.7(5) . . . . ? C19 C20 C27 C28 -48.2(6) . . . . ? C21 C20 C27 C28 72.2(6) . . . . ? O3 C20 C27 C32 11.1(6) . . . . ? C19 C20 C27 C32 133.6(5) . . . . ? C21 C20 C27 C32 -106.0(5) . . . . ? C32 C27 C28 C29 -2.6(9) . . . . ? C20 C27 C28 C29 179.1(5) . . . . ? C27 C28 C29 C30 0.9(10) . . . . ? C28 C29 C30 C31 1.9(11) . . . . ? C29 C30 C31 C32 -2.9(11) . . . . ? C28 C27 C32 C31 1.6(8) . . . . ? C20 C27 C32 C31 179.8(5) . . . . ? C30 C31 C32 C27 1.2(10) . . . . ? C6 C7 O1 As1 16.3(5) . . . . ? C9 C7 O1 As1 138.1(4) . . . . ? C8 C7 O1 As1 -101.8(4) . . . . ? C15 C16 O2 As1 10.7(5) . . . . ? C17 C16 O2 As1 -110.8(4) . . . . ? C18 C16 O2 As1 131.8(4) . . . . ? C16 O2 As1 C1 117.9(3) . . . . ? C16 O2 As1 O1 63.9(15) . . . . ? C16 O2 As1 C10 -7.8(3) . . . . ? C16 O2 As1 C19 -127.1(3) . . . . ? C6 C1 As1 O2 -170.2(4) . . . . ? C2 C1 As1 O2 12.9(4) . . . . ? C6 C1 As1 O1 5.1(4) . . . . ? C2 C1 As1 O1 -171.8(4) . . . . ? C6 C1 As1 C10 -85.3(5) . . . . ? C2 C1 As1 C10 97.8(5) . . . . ? C6 C1 As1 C19 98.4(4) . . . . ? C2 C1 As1 C19 -78.5(5) . . . . ? C7 O1 As1 O2 41.8(15) . . . . ? C7 O1 As1 C1 -12.5(4) . . . . ? C7 O1 As1 C10 113.0(4) . . . . ? C7 O1 As1 C19 -127.2(4) . . . . ? C15 C10 As1 O2 2.5(4) . . . . ? C11 C10 As1 O2 -173.6(5) . . . . ? C15 C10 As1 C1 -86.5(4) . . . . ? C11 C10 As1 C1 97.5(5) . . . . ? C15 C10 As1 O1 -172.0(4) . . . . ? C11 C10 As1 O1 11.9(5) . . . . ? C15 C10 As1 C19 89.7(4) . . . . ? C11 C10 As1 C19 -86.4(5) . . . . ? C20 C19 As1 O2 149.0(4) . . . . ? C20 C19 As1 C1 -118.3(4) . . . . ? C20 C19 As1 O1 -32.1(4) . . . . ? C20 C19 As1 C10 65.1(5) . . . . ? C22 C21 C33 C34 53.0(11) . . . . ? C37 C21 C33 C34 8.1(14) . . . . ? C26 C21 C33 C34 -60.4(11) . . . . ? C20 C21 C33 C34 177.6(9) . . . . ? C21 C33 C34 C35 -2.4(19) . . . . ? C33 C34 C35 C36 -1(2) . . . . ? C34 C35 C36 C37 0(2) . . . . ? C35 C36 C37 C21 5.3(16) . . . . ? C33 C21 C37 C36 -9.5(13) . . . . ? C22 C21 C37 C36 -49.3(10) . . . . ? C26 C21 C37 C36 71.9(9) . . . . ? C20 C21 C37 C36 -178.2(7) . . . . ? C43 C38 C39 C40 -0.8(7) . . . . ? As2 C38 C39 C40 -175.7(4) . . . . ? C38 C39 C40 C41 -1.8(8) . . . . ? C39 C40 C41 C42 1.4(10) . . . . ? C40 C41 C42 C43 1.5(10) . . . . ? C39 C38 C43 C42 3.7(7) . . . . ? As2 C38 C43 C42 179.1(4) . . . . ? C39 C38 C43 C44 -176.2(4) . . . . ? As2 C38 C43 C44 -0.7(5) . . . . ? C41 C42 C43 C38 -3.9(9) . . . . ? C41 C42 C43 C44 175.9(5) . . . . ? C38 C43 C44 O4 4.2(6) . . . . ? C42 C43 C44 O4 -175.6(5) . . . . ? C38 C43 C44 C45 -114.8(5) . . . . ? C42 C43 C44 C45 65.4(7) . . . . ? C38 C43 C44 C46 122.5(5) . . . . ? C42 C43 C44 C46 -57.3(7) . . . . ? O4 C44 C45 F15 -62.0(7) . . . . ? C43 C44 C45 F15 58.9(7) . . . . ? C46 C44 C45 F15 -178.9(5) . . . . ? O4 C44 C45 F14 177.1(6) . . . . ? C43 C44 C45 F14 -62.1(7) . . . . ? C46 C44 C45 F14 60.2(8) . . . . ? O4 C44 C45 F13 55.8(6) . . . . ? C43 C44 C45 F13 176.7(5) . . . . ? C46 C44 C45 F13 -61.1(7) . . . . ? O4 C44 C46 F17 66.7(5) . . . . ? C43 C44 C46 F17 -53.9(6) . . . . ? C45 C44 C46 F17 -175.9(5) . . . . ? O4 C44 C46 F18 -174.0(5) . . . . ? C43 C44 C46 F18 65.5(6) . . . . ? C45 C44 C46 F18 -56.6(7) . . . . ? O4 C44 C46 F16 -51.3(6) . . . . ? C43 C44 C46 F16 -171.9(5) . . . . ? C45 C44 C46 F16 66.0(7) . . . . ? C52 C47 C48 C49 0.6(7) . . . . ? As2 C47 C48 C49 -177.1(4) . . . . ? C47 C48 C49 C50 -0.4(8) . . . . ? C48 C49 C50 C51 -0.8(9) . . . . ? C49 C50 C51 C52 1.7(9) . . . . ? C48 C47 C52 C51 0.2(7) . . . . ? As2 C47 C52 C51 178.3(4) . . . . ? C48 C47 C52 C53 177.8(4) . . . . ? As2 C47 C52 C53 -4.1(5) . . . . ? C50 C51 C52 C47 -1.4(7) . . . . ? C50 C51 C52 C53 -178.7(5) . . . . ? C47 C52 C53 O5 14.5(6) . . . . ? C51 C52 C53 O5 -168.0(4) . . . . ? C47 C52 C53 C55 133.2(4) . . . . ? C51 C52 C53 C55 -49.4(6) . . . . ? C47 C52 C53 C54 -104.2(4) . . . . ? C51 C52 C53 C54 73.2(6) . . . . ? O5 C53 C54 F20 179.7(5) . . . . ? C55 C53 C54 F20 63.4(7) . . . . ? C52 C53 C54 F20 -60.7(6) . . . . ? O5 C53 C54 F21 -60.1(6) . . . . ? C55 C53 C54 F21 -176.3(5) . . . . ? C52 C53 C54 F21 59.5(5) . . . . ? O5 C53 C54 F19 58.2(6) . . . . ? C55 C53 C54 F19 -58.1(6) . . . . ? C52 C53 C54 F19 177.8(4) . . . . ? O5 C53 C55 F23 69.7(6) . . . . ? C52 C53 C55 F23 -51.0(6) . . . . ? C54 C53 C55 F23 -172.6(5) . . . . ? O5 C53 C55 F22 -50.0(6) . . . . ? C52 C53 C55 F22 -170.8(4) . . . . ? C54 C53 C55 F22 67.7(6) . . . . ? O5 C53 C55 F24 -169.9(5) . . . . ? C52 C53 C55 F24 69.4(6) . . . . ? C54 C53 C55 F24 -52.2(7) . . . . ? As2 C56 C57 O6 -65.4(4) . . . . ? As2 C56 C57 C58 58.6(5) . . . . ? As2 C56 C57 C64 -179.2(3) . . . . ? O6 C57 C58 C59 164.1(5) . . . . ? C64 C57 C58 C59 -78.7(6) . . . . ? C56 C57 C58 C59 39.6(7) . . . . ? O6 C57 C58 C63 -15.8(6) . . . . ? C64 C57 C58 C63 101.5(6) . . . . ? C56 C57 C58 C63 -140.2(5) . . . . ? C63 C58 C59 C60 -1.8(10) . . . . ? C57 C58 C59 C60 178.4(6) . . . . ? C58 C59 C60 C61 2.2(13) . . . . ? C59 C60 C61 C62 -1.4(17) . . . . ? C60 C61 C62 C63 0.1(18) . . . . ? C61 C62 C63 C58 0.4(15) . . . . ? C59 C58 C63 C62 0.5(10) . . . . ? C57 C58 C63 C62 -179.7(7) . . . . ? O6 C57 C64 C69 -23.4(6) . . . . ? C58 C57 C64 C69 -143.6(5) . . . . ? C56 C57 C64 C69 94.3(6) . . . . ? O6 C57 C64 C65 159.9(7) . . . . ? C58 C57 C64 C65 39.7(8) . . . . ? C56 C57 C64 C65 -82.4(8) . . . . ? C69 C64 C65 C66 0.1(15) . . . . ? C57 C64 C65 C66 177.0(9) . . . . ? C64 C65 C66 C67 4.4(19) . . . . ? C65 C66 C67 C68 -5.6(16) . . . . ? C66 C67 C68 C69 2.3(13) . . . . ? C65 C64 C69 C68 -3.4(11) . . . . ? C57 C64 C69 C68 179.6(6) . . . . ? C67 C68 C69 C64 2.3(12) . . . . ? C48 C47 As2 O5 173.2(4) . . . . ? C52 C47 As2 O5 -4.8(3) . . . . ? C48 C47 As2 C38 -96.7(4) . . . . ? C52 C47 As2 C38 85.3(4) . . . . ? C48 C47 As2 O4 -12.8(4) . . . . ? C52 C47 As2 O4 169.2(3) . . . . ? C48 C47 As2 C56 82.1(4) . . . . ? C52 C47 As2 C56 -95.9(4) . . . . ? C43 C38 As2 O5 171.6(3) . . . . ? C39 C38 As2 O5 -13.0(4) . . . . ? C43 C38 As2 C47 85.3(4) . . . . ? C39 C38 As2 C47 -99.3(4) . . . . ? C43 C38 As2 O4 -2.0(3) . . . . ? C39 C38 As2 O4 173.5(4) . . . . ? C43 C38 As2 C56 -93.7(4) . . . . ? C39 C38 As2 C56 81.7(4) . . . . ? C57 C56 As2 O5 -129.1(3) . . . . ? C57 C56 As2 C47 -42.4(4) . . . . ? C57 C56 As2 C38 136.6(3) . . . . ? C57 C56 As2 O4 51.3(3) . . . . ? C43 C44 O4 As2 -5.8(5) . . . . ? C45 C44 O4 As2 114.5(4) . . . . ? C46 C44 O4 As2 -126.1(4) . . . . ? O5 As2 O4 C44 -63.8(12) . . . . ? C47 As2 O4 C44 -123.2(3) . . . . ? C38 As2 O4 C44 4.5(3) . . . . ? C56 As2 O4 C44 113.3(3) . . . . ? C55 C53 O5 As2 -141.0(3) . . . . ? C52 C53 O5 As2 -18.4(5) . . . . ? C54 C53 O5 As2 100.2(4) . . . . ? C47 As2 O5 C53 13.7(3) . . . . ? C38 As2 O5 C53 -113.9(3) . . . . ? O4 As2 O5 C53 -46.0(13) . . . . ? C56 As2 O5 C53 136.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 2.144 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.319 # Attachment 'JiangYamamoto5b_CCDC761613.cif' data_Rfee2AsCH2COPh _database_code_depnum_ccdc_archive 'CCDC 761613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 149 _chemical_formula_moiety ? _chemical_formula_sum 'C30 H15 As F20 O3' _chemical_formula_weight 878.34 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.99600(10) _cell_length_b 12.3680(2) _cell_length_c 14.9450(3) _cell_angle_alpha 105.9260(10) _cell_angle_beta 105.8450(10) _cell_angle_gamma 103.1500(10) _cell_volume 1615.31(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 27.91 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MacScience DIP2030 Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7112 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.91 _reflns_number_total 7112 _reflns_number_gt 6544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL(Otwinowski, 1997)' _computing_cell_refinement 'HKL(Otwinowski, 1997)' _computing_data_reduction 'HKL(Otwinowski, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.9109P] 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 7112 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _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 C1 C -0.0367(3) 0.2632(2) 0.30078(18) 0.0355(5) Uani 1 1 d . . . C2 C -0.0521(3) 0.2725(3) 0.3918(2) 0.0451(6) Uani 1 1 d . . . H2A H -0.0155 0.2287 0.4281 0.054 Uiso 1 1 calc R . . C3 C -0.1235(4) 0.3488(3) 0.4272(2) 0.0560(7) Uani 1 1 d . . . H3A H -0.1370 0.3553 0.4873 0.067 Uiso 1 1 calc R . . C4 C -0.1745(4) 0.4152(3) 0.3740(3) 0.0586(8) Uani 1 1 d . . . H4A H -0.2207 0.4671 0.3994 0.070 Uiso 1 1 calc R . . C5 C -0.1583(4) 0.4061(3) 0.2835(2) 0.0499(6) Uani 1 1 d . . . H5A H -0.1932 0.4514 0.2480 0.060 Uiso 1 1 calc R . . C6 C -0.0890(3) 0.3281(2) 0.24623(19) 0.0366(5) Uani 1 1 d . . . C7 C -0.0649(3) 0.3052(2) 0.14641(19) 0.0379(5) Uani 1 1 d . . . C8 C 0.0327(4) 0.4212(3) 0.1440(3) 0.0540(7) Uani 1 1 d . . . C9 C 0.1729(4) 0.4957(3) 0.2352(3) 0.0663(9) Uani 1 1 d . . . C10 C -0.2193(3) 0.2499(3) 0.0607(2) 0.0467(6) Uani 1 1 d . . . C11 C -0.2302(5) 0.2087(4) -0.0492(3) 0.0705(10) Uani 1 1 d . . . C12 C 0.2358(3) 0.1628(2) 0.22741(19) 0.0387(5) Uani 1 1 d . . . C13 C 0.2847(3) 0.1906(3) 0.1552(2) 0.0486(6) Uani 1 1 d . . . H13A H 0.2271 0.2131 0.1080 0.058 Uiso 1 1 calc R . . C14 C 0.4212(4) 0.1839(3) 0.1550(3) 0.0632(8) Uani 1 1 d . . . H14A H 0.4553 0.2015 0.1070 0.076 Uiso 1 1 calc R . . C15 C 0.5071(4) 0.1514(3) 0.2255(3) 0.0647(9) Uani 1 1 d . . . H15A H 0.5986 0.1478 0.2246 0.078 Uiso 1 1 calc R . . C16 C 0.4587(4) 0.1241(3) 0.2972(3) 0.0595(8) Uani 1 1 d . . . H16A H 0.5172 0.1023 0.3446 0.071 Uiso 1 1 calc R . . C17 C 0.3212(3) 0.1295(3) 0.2980(2) 0.0446(6) Uani 1 1 d . . . C18 C 0.2496(3) 0.1016(3) 0.3716(2) 0.0460(6) Uani 1 1 d . . . C19 C 0.3421(4) 0.1920(4) 0.4799(2) 0.0648(9) Uani 1 1 d . . . C20 C 0.3966(5) 0.3245(4) 0.4944(3) 0.0712(10) Uani 1 1 d . . . C21 C 0.2318(4) -0.0310(3) 0.3619(3) 0.0580(8) Uani 1 1 d . . . C22 C 0.1571(6) -0.0860(4) 0.4240(3) 0.0786(12) Uani 1 1 d . . . C23 C -0.0911(3) -0.0046(2) 0.14863(19) 0.0411(5) Uani 1 1 d . . . H23A H -0.1446 -0.0024 0.0848 0.049 Uiso 1 1 calc R . . H23B H -0.0357 -0.0587 0.1370 0.049 Uiso 1 1 calc R . . C24 C -0.2000(3) -0.0517(2) 0.1934(2) 0.0429(6) Uani 1 1 d . . . C25 C -0.2586(3) -0.1824(2) 0.1688(2) 0.0428(5) Uani 1 1 d . . . C26 C -0.3483(4) -0.2224(3) 0.2173(3) 0.0623(8) Uani 1 1 d . . . H26A H -0.3693 -0.1682 0.2638 0.075 Uiso 1 1 calc R . . C27 C -0.4062(5) -0.3429(4) 0.1964(3) 0.0766(11) Uani 1 1 d . . . H27A H -0.4652 -0.3694 0.2297 0.092 Uiso 1 1 calc R . . C28 C -0.3777(5) -0.4238(3) 0.1268(3) 0.0725(10) Uani 1 1 d . . . H28A H -0.4185 -0.5048 0.1125 0.087 Uiso 1 1 calc R . . C29 C -0.2897(5) -0.3855(3) 0.0789(3) 0.0686(9) Uani 1 1 d . . . H29A H -0.2705 -0.4406 0.0319 0.082 Uiso 1 1 calc R . . C30 C -0.2287(4) -0.2650(3) 0.0994(2) 0.0539(7) Uani 1 1 d . . . H30A H -0.1678 -0.2394 0.0669 0.065 Uiso 1 1 calc R . . O1 O 0.0053(2) 0.22133(16) 0.13282(13) 0.0383(4) Uani 1 1 d . . . O2 O 0.1100(2) 0.11059(17) 0.34698(13) 0.0408(4) Uani 1 1 d . . . O3 O -0.2412(3) 0.0162(2) 0.2459(2) 0.0730(8) Uani 1 1 d . . . As1 As 0.04461(3) 0.15312(2) 0.233666(16) 0.03126(9) Uani 1 1 d . . . F1 F -0.0450(3) 0.4947(2) 0.1300(2) 0.0861(8) Uani 1 1 d . . . F2 F 0.0772(3) 0.3925(2) 0.06562(19) 0.0809(7) Uani 1 1 d . . . F3 F 0.2525(3) 0.4312(2) 0.2605(2) 0.1053(10) Uani 1 1 d . . . F4 F 0.1453(4) 0.5472(3) 0.3146(2) 0.1161(11) Uani 1 1 d . . . F5 F 0.2528(3) 0.5824(3) 0.2186(3) 0.1187(12) Uani 1 1 d . . . F6 F -0.3018(2) 0.3219(2) 0.06810(16) 0.0694(6) Uani 1 1 d . . . F7 F -0.2904(2) 0.15081(17) 0.07263(14) 0.0580(4) Uani 1 1 d . . . F8 F -0.1559(3) 0.1357(3) -0.06689(16) 0.1035(10) Uani 1 1 d . . . F9 F -0.1879(4) 0.3000(3) -0.0749(2) 0.1231(12) Uani 1 1 d . . . F10 F -0.3687(3) 0.1510(3) -0.10703(17) 0.1017(9) Uani 1 1 d . . . F11 F 0.4626(3) 0.1648(3) 0.52005(19) 0.1007(9) Uani 1 1 d . . . F12 F 0.2589(3) 0.1846(2) 0.53719(15) 0.0849(7) Uani 1 1 d . . . F13 F 0.2919(3) 0.3589(2) 0.44778(19) 0.0846(7) Uani 1 1 d . . . F14 F 0.5058(4) 0.3501(3) 0.4624(3) 0.1083(10) Uani 1 1 d . . . F15 F 0.4462(4) 0.3910(3) 0.58999(19) 0.1161(11) Uani 1 1 d . . . F16 F 0.3619(3) -0.0509(2) 0.3795(2) 0.0909(8) Uani 1 1 d . . . F17 F 0.1476(3) -0.09842(17) 0.26596(15) 0.0696(6) Uani 1 1 d . . . F18 F 0.0285(4) -0.0729(3) 0.4146(3) 0.1036(10) Uani 1 1 d . . . F19 F 0.2406(5) -0.0402(3) 0.5196(2) 0.1290(13) Uani 1 1 d . . . F20 F 0.1383(5) -0.2007(3) 0.3947(3) 0.1194(12) Uani 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 C1 0.0374(13) 0.0366(11) 0.0366(11) 0.0117(9) 0.0184(9) 0.0149(9) C2 0.0527(17) 0.0494(14) 0.0382(13) 0.0142(11) 0.0222(11) 0.0204(12) C3 0.066(2) 0.0587(17) 0.0463(15) 0.0083(13) 0.0333(14) 0.0229(15) C4 0.065(2) 0.0537(17) 0.0613(18) 0.0072(14) 0.0337(16) 0.0303(15) C5 0.0553(18) 0.0459(14) 0.0566(16) 0.0167(12) 0.0239(13) 0.0286(13) C6 0.0367(13) 0.0358(11) 0.0421(12) 0.0137(9) 0.0181(9) 0.0161(9) C7 0.0407(14) 0.0459(13) 0.0436(12) 0.0254(11) 0.0213(10) 0.0249(10) C8 0.0571(19) 0.0602(17) 0.0695(19) 0.0431(16) 0.0316(15) 0.0290(14) C9 0.064(2) 0.0523(18) 0.091(3) 0.0367(18) 0.0321(19) 0.0155(15) C10 0.0473(17) 0.0590(16) 0.0463(14) 0.0242(12) 0.0183(11) 0.0316(13) C11 0.081(3) 0.095(3) 0.0474(17) 0.0326(18) 0.0187(16) 0.046(2) C12 0.0375(14) 0.0419(12) 0.0454(13) 0.0191(10) 0.0183(10) 0.0201(10) C13 0.0437(17) 0.0635(17) 0.0589(16) 0.0316(14) 0.0307(13) 0.0279(13) C14 0.051(2) 0.080(2) 0.083(2) 0.0389(19) 0.0429(17) 0.0305(16) C15 0.0401(19) 0.076(2) 0.091(3) 0.0316(19) 0.0319(16) 0.0301(15) C16 0.0442(18) 0.068(2) 0.073(2) 0.0299(17) 0.0164(14) 0.0303(15) C17 0.0374(15) 0.0525(14) 0.0507(14) 0.0227(12) 0.0152(11) 0.0229(11) C18 0.0495(16) 0.0552(15) 0.0434(13) 0.0261(12) 0.0144(11) 0.0280(12) C19 0.066(2) 0.082(2) 0.0461(16) 0.0278(16) 0.0059(14) 0.0347(18) C20 0.064(2) 0.069(2) 0.0565(19) 0.0108(16) 0.0025(16) 0.0172(17) C21 0.074(2) 0.0647(19) 0.0602(18) 0.0377(16) 0.0286(16) 0.0432(17) C22 0.118(4) 0.075(2) 0.075(2) 0.049(2) 0.046(2) 0.050(2) C23 0.0462(15) 0.0388(12) 0.0408(12) 0.0134(10) 0.0185(10) 0.0158(10) C24 0.0377(15) 0.0409(13) 0.0506(14) 0.0134(11) 0.0180(11) 0.0149(10) C25 0.0372(14) 0.0432(13) 0.0482(14) 0.0187(11) 0.0130(10) 0.0136(10) C26 0.062(2) 0.0608(19) 0.065(2) 0.0211(16) 0.0332(16) 0.0118(15) C27 0.070(3) 0.072(2) 0.092(3) 0.041(2) 0.037(2) 0.0054(18) C28 0.068(2) 0.0484(17) 0.099(3) 0.0325(19) 0.024(2) 0.0133(16) C29 0.075(3) 0.0437(16) 0.086(3) 0.0188(16) 0.0305(19) 0.0222(15) C30 0.062(2) 0.0457(15) 0.0599(17) 0.0194(13) 0.0285(14) 0.0206(13) O1 0.0446(10) 0.0511(10) 0.0394(9) 0.0257(8) 0.0239(7) 0.0301(8) O2 0.0461(11) 0.0513(10) 0.0387(9) 0.0253(8) 0.0185(7) 0.0257(8) O3 0.0698(18) 0.0503(12) 0.107(2) 0.0130(13) 0.0595(16) 0.0187(11) As1 0.03384(15) 0.03668(13) 0.03224(13) 0.01641(9) 0.01599(9) 0.01788(9) F1 0.0810(16) 0.0742(14) 0.141(2) 0.0764(15) 0.0427(15) 0.0441(12) F2 0.0925(18) 0.1024(17) 0.0842(15) 0.0612(14) 0.0567(13) 0.0338(13) F3 0.0754(17) 0.0694(15) 0.128(2) 0.0262(15) -0.0151(15) 0.0193(12) F4 0.103(2) 0.0799(17) 0.114(2) -0.0138(16) 0.0470(18) -0.0138(15) F5 0.085(2) 0.100(2) 0.167(3) 0.081(2) 0.0382(19) -0.0082(15) F6 0.0608(13) 0.0811(13) 0.0720(12) 0.0232(10) 0.0142(9) 0.0506(11) F7 0.0465(11) 0.0653(11) 0.0584(10) 0.0214(9) 0.0161(8) 0.0152(8) F8 0.120(2) 0.163(3) 0.0466(11) 0.0235(14) 0.0314(12) 0.097(2) F9 0.163(3) 0.146(3) 0.0729(17) 0.0748(19) 0.0342(18) 0.039(2) F10 0.0895(19) 0.133(2) 0.0555(13) 0.0138(14) -0.0064(12) 0.0512(17) F11 0.0913(19) 0.114(2) 0.0785(15) 0.0356(15) -0.0151(13) 0.0543(16) F12 0.112(2) 0.1006(18) 0.0423(10) 0.0280(11) 0.0260(11) 0.0341(15) F13 0.0812(16) 0.0591(12) 0.0897(16) 0.0205(11) 0.0005(12) 0.0240(11) F14 0.086(2) 0.0835(18) 0.131(3) 0.0161(17) 0.0411(18) 0.0085(14) F15 0.132(3) 0.097(2) 0.0575(14) -0.0032(13) -0.0083(14) 0.0151(17) F16 0.0969(19) 0.1019(18) 0.124(2) 0.0725(17) 0.0481(16) 0.0743(16) F17 0.1093(18) 0.0522(10) 0.0611(11) 0.0251(9) 0.0363(11) 0.0388(11) F18 0.132(3) 0.105(2) 0.139(3) 0.082(2) 0.091(2) 0.0586(19) F19 0.205(4) 0.130(3) 0.0742(17) 0.0709(19) 0.046(2) 0.058(3) F20 0.204(4) 0.0778(17) 0.141(3) 0.0774(19) 0.099(3) 0.073(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.379(3) . ? C1 C2 1.386(3) . ? C1 As1 1.929(2) . ? C2 C3 1.385(4) . ? C2 H2A 0.9300 . ? C3 C4 1.376(5) . ? C3 H3A 0.9300 . ? C4 C5 1.384(4) . ? C4 H4A 0.9300 . ? C5 C6 1.393(3) . ? C5 H5A 0.9300 . ? C6 C7 1.536(3) . ? C7 O1 1.379(3) . ? C7 C8 1.557(4) . ? C7 C10 1.565(4) . ? C8 F1 1.346(3) . ? C8 F2 1.350(4) . ? C8 C9 1.534(5) . ? C9 F3 1.304(4) . ? C9 F5 1.309(4) . ? C9 F4 1.316(5) . ? C10 F6 1.347(3) . ? C10 F7 1.354(4) . ? C10 C11 1.545(4) . ? C11 F9 1.308(5) . ? C11 F8 1.311(4) . ? C11 F10 1.316(5) . ? C12 C17 1.385(4) . ? C12 C13 1.392(4) . ? C12 As1 1.917(3) . ? C13 C14 1.386(4) . ? C13 H13A 0.9300 . ? C14 C15 1.379(5) . ? C14 H14A 0.9300 . ? C15 C16 1.381(5) . ? C15 H15A 0.9300 . ? C16 C17 1.394(4) . ? C16 H16A 0.9300 . ? C17 C18 1.539(4) . ? C18 O2 1.381(3) . ? C18 C19 1.563(5) . ? C18 C21 1.570(4) . ? C19 F11 1.351(4) . ? C19 F12 1.353(5) . ? C19 C20 1.538(6) . ? C20 F13 1.314(4) . ? C20 F14 1.315(5) . ? C20 F15 1.321(4) . ? C21 F16 1.348(4) . ? C21 F17 1.351(4) . ? C21 C22 1.542(5) . ? C22 F18 1.306(6) . ? C22 F20 1.316(5) . ? C22 F19 1.322(5) . ? C23 C24 1.515(4) . ? C23 As1 1.938(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O3 1.210(3) . ? C24 C25 1.489(4) . ? C25 C26 1.386(4) . ? C25 C30 1.391(4) . ? C26 C27 1.380(5) . ? C26 H26A 0.9300 . ? C27 C28 1.373(6) . ? C27 H27A 0.9300 . ? C28 C29 1.361(6) . ? C28 H28A 0.9300 . ? C29 C30 1.386(4) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? O1 As1 1.9138(16) . ? O2 As1 1.9009(16) . ? 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 C6 C1 C2 121.8(2) . . ? C6 C1 As1 113.41(17) . . ? C2 C1 As1 124.6(2) . . ? C3 C2 C1 118.2(3) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C1 C6 C5 119.4(2) . . ? C1 C6 C7 114.9(2) . . ? C5 C6 C7 125.7(2) . . ? O1 C7 C6 110.10(19) . . ? O1 C7 C8 108.0(2) . . ? C6 C7 C8 110.8(2) . . ? O1 C7 C10 106.5(2) . . ? C6 C7 C10 108.1(2) . . ? C8 C7 C10 113.2(2) . . ? F1 C8 F2 107.0(3) . . ? F1 C8 C9 106.3(3) . . ? F2 C8 C9 106.0(3) . . ? F1 C8 C7 110.9(3) . . ? F2 C8 C7 108.7(3) . . ? C9 C8 C7 117.4(2) . . ? F3 C9 F5 109.0(4) . . ? F3 C9 F4 106.3(4) . . ? F5 C9 F4 105.6(3) . . ? F3 C9 C8 111.8(3) . . ? F5 C9 C8 111.0(3) . . ? F4 C9 C8 112.8(3) . . ? F6 C10 F7 106.4(3) . . ? F6 C10 C11 105.9(2) . . ? F7 C10 C11 105.1(3) . . ? F6 C10 C7 112.3(2) . . ? F7 C10 C7 106.3(2) . . ? C11 C10 C7 120.0(3) . . ? F9 C11 F8 110.9(4) . . ? F9 C11 F10 106.5(3) . . ? F8 C11 F10 107.2(4) . . ? F9 C11 C10 110.8(3) . . ? F8 C11 C10 112.0(3) . . ? F10 C11 C10 109.2(3) . . ? C17 C12 C13 121.0(3) . . ? C17 C12 As1 113.7(2) . . ? C13 C12 As1 125.1(2) . . ? C14 C13 C12 118.6(3) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? C15 C14 C13 120.7(3) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 120.8(3) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C12 C17 C16 119.7(3) . . ? C12 C17 C18 113.9(2) . . ? C16 C17 C18 126.4(3) . . ? O2 C18 C17 110.5(2) . . ? O2 C18 C19 107.7(2) . . ? C17 C18 C19 110.5(3) . . ? O2 C18 C21 106.9(3) . . ? C17 C18 C21 108.3(2) . . ? C19 C18 C21 112.9(2) . . ? F11 C19 F12 107.4(3) . . ? F11 C19 C20 106.3(3) . . ? F12 C19 C20 105.4(3) . . ? F11 C19 C18 111.0(3) . . ? F12 C19 C18 108.6(3) . . ? C20 C19 C18 117.6(3) . . ? F13 C20 F14 107.4(4) . . ? F13 C20 F15 107.6(4) . . ? F14 C20 F15 106.7(4) . . ? F13 C20 C19 112.3(3) . . ? F14 C20 C19 112.2(4) . . ? F15 C20 C19 110.4(4) . . ? F16 C21 F17 107.0(3) . . ? F16 C21 C22 105.8(3) . . ? F17 C21 C22 105.1(3) . . ? F16 C21 C18 111.7(3) . . ? F17 C21 C18 106.3(2) . . ? C22 C21 C18 120.1(3) . . ? F18 C22 F20 108.0(4) . . ? F18 C22 F19 108.8(4) . . ? F20 C22 F19 106.6(3) . . ? F18 C22 C21 112.7(3) . . ? F20 C22 C21 109.2(3) . . ? F19 C22 C21 111.4(4) . . ? C24 C23 As1 112.53(17) . . ? C24 C23 H23A 109.1 . . ? As1 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? As1 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? O3 C24 C25 121.0(3) . . ? O3 C24 C23 120.0(3) . . ? C25 C24 C23 118.9(2) . . ? C26 C25 C30 119.2(3) . . ? C26 C25 C24 117.7(3) . . ? C30 C25 C24 123.1(3) . . ? C27 C26 C25 119.9(3) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C28 C27 C26 120.6(4) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C29 C30 C25 119.8(3) . . ? C29 C30 H30A 120.1 . . ? C25 C30 H30A 120.1 . . ? C7 O1 As1 116.70(14) . . ? C18 O2 As1 116.51(16) . . ? O2 As1 O1 170.17(8) . . ? O2 As1 C12 85.23(9) . . ? O1 As1 C12 90.26(9) . . ? O2 As1 C1 92.19(9) . . ? O1 As1 C1 84.76(9) . . ? C12 As1 C1 134.60(11) . . ? O2 As1 C23 94.79(10) . . ? O1 As1 C23 94.94(10) . . ? C12 As1 C23 108.89(11) . . ? C1 As1 C23 116.49(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 C6 C1 C2 C3 0.6(4) . . . . ? As1 C1 C2 C3 -174.8(2) . . . . ? C1 C2 C3 C4 -1.4(5) . . . . ? C2 C3 C4 C5 1.1(6) . . . . ? C3 C4 C5 C6 0.0(5) . . . . ? C2 C1 C6 C5 0.5(4) . . . . ? As1 C1 C6 C5 176.4(2) . . . . ? C2 C1 C6 C7 -179.0(2) . . . . ? As1 C1 C6 C7 -3.1(3) . . . . ? C4 C5 C6 C1 -0.8(5) . . . . ? C4 C5 C6 C7 178.6(3) . . . . ? C1 C6 C7 O1 0.4(3) . . . . ? C5 C6 C7 O1 -179.1(3) . . . . ? C1 C6 C7 C8 -119.1(3) . . . . ? C5 C6 C7 C8 61.4(4) . . . . ? C1 C6 C7 C10 116.3(2) . . . . ? C5 C6 C7 C10 -63.2(3) . . . . ? O1 C7 C8 F1 163.5(3) . . . . ? C6 C7 C8 F1 -75.8(3) . . . . ? C10 C7 C8 F1 45.9(4) . . . . ? O1 C7 C8 F2 46.2(3) . . . . ? C6 C7 C8 F2 166.9(2) . . . . ? C10 C7 C8 F2 -71.4(3) . . . . ? O1 C7 C8 C9 -74.0(3) . . . . ? C6 C7 C8 C9 46.7(4) . . . . ? C10 C7 C8 C9 168.4(3) . . . . ? F1 C8 C9 F3 175.3(3) . . . . ? F2 C8 C9 F3 -71.1(4) . . . . ? C7 C8 C9 F3 50.5(4) . . . . ? F1 C8 C9 F5 -62.7(4) . . . . ? F2 C8 C9 F5 50.9(4) . . . . ? C7 C8 C9 F5 172.5(3) . . . . ? F1 C8 C9 F4 55.5(4) . . . . ? F2 C8 C9 F4 169.2(3) . . . . ? C7 C8 C9 F4 -69.2(4) . . . . ? O1 C7 C10 F6 177.4(2) . . . . ? C6 C7 C10 F6 59.2(3) . . . . ? C8 C7 C10 F6 -64.0(3) . . . . ? O1 C7 C10 F7 61.5(3) . . . . ? C6 C7 C10 F7 -56.8(3) . . . . ? C8 C7 C10 F7 180.0(2) . . . . ? O1 C7 C10 C11 -57.3(3) . . . . ? C6 C7 C10 C11 -175.6(3) . . . . ? C8 C7 C10 C11 61.2(3) . . . . ? F6 C10 C11 F9 56.6(4) . . . . ? F7 C10 C11 F9 169.0(3) . . . . ? C7 C10 C11 F9 -71.6(4) . . . . ? F6 C10 C11 F8 -178.9(4) . . . . ? F7 C10 C11 F8 -66.6(4) . . . . ? C7 C10 C11 F8 52.8(5) . . . . ? F6 C10 C11 F10 -60.3(4) . . . . ? F7 C10 C11 F10 52.1(4) . . . . ? C7 C10 C11 F10 171.4(3) . . . . ? C17 C12 C13 C14 0.2(5) . . . . ? As1 C12 C13 C14 -174.3(3) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C17 0.1(6) . . . . ? C13 C12 C17 C16 0.3(5) . . . . ? As1 C12 C17 C16 175.4(2) . . . . ? C13 C12 C17 C18 -179.7(3) . . . . ? As1 C12 C17 C18 -4.7(3) . . . . ? C15 C16 C17 C12 -0.4(5) . . . . ? C15 C16 C17 C18 179.6(3) . . . . ? C12 C17 C18 O2 3.0(4) . . . . ? C16 C17 C18 O2 -177.0(3) . . . . ? C12 C17 C18 C19 -116.1(3) . . . . ? C16 C17 C18 C19 63.9(4) . . . . ? C12 C17 C18 C21 119.8(3) . . . . ? C16 C17 C18 C21 -60.2(4) . . . . ? O2 C18 C19 F11 161.7(3) . . . . ? C17 C18 C19 F11 -77.5(4) . . . . ? C21 C18 C19 F11 43.9(4) . . . . ? O2 C18 C19 F12 43.9(3) . . . . ? C17 C18 C19 F12 164.6(2) . . . . ? C21 C18 C19 F12 -73.9(3) . . . . ? O2 C18 C19 C20 -75.6(4) . . . . ? C17 C18 C19 C20 45.1(4) . . . . ? C21 C18 C19 C20 166.6(3) . . . . ? F11 C19 C20 F13 172.3(3) . . . . ? F12 C19 C20 F13 -73.9(4) . . . . ? C18 C19 C20 F13 47.4(5) . . . . ? F11 C19 C20 F14 51.2(4) . . . . ? F12 C19 C20 F14 165.0(3) . . . . ? C18 C19 C20 F14 -73.8(4) . . . . ? F11 C19 C20 F15 -67.6(5) . . . . ? F12 C19 C20 F15 46.2(4) . . . . ? C18 C19 C20 F15 167.4(3) . . . . ? O2 C18 C21 F16 176.8(2) . . . . ? C17 C18 C21 F16 57.7(3) . . . . ? C19 C18 C21 F16 -64.9(4) . . . . ? O2 C18 C21 F17 60.4(3) . . . . ? C17 C18 C21 F17 -58.7(3) . . . . ? C19 C18 C21 F17 178.6(3) . . . . ? O2 C18 C21 C22 -58.5(4) . . . . ? C17 C18 C21 C22 -177.6(3) . . . . ? C19 C18 C21 C22 59.7(4) . . . . ? F16 C21 C22 F18 179.7(4) . . . . ? F17 C21 C22 F18 -67.2(4) . . . . ? C18 C21 C22 F18 52.3(5) . . . . ? F16 C21 C22 F20 -60.3(5) . . . . ? F17 C21 C22 F20 52.8(4) . . . . ? C18 C21 C22 F20 172.3(4) . . . . ? F16 C21 C22 F19 57.1(4) . . . . ? F17 C21 C22 F19 170.2(3) . . . . ? C18 C21 C22 F19 -70.3(5) . . . . ? As1 C23 C24 O3 32.0(4) . . . . ? As1 C23 C24 C25 -150.1(2) . . . . ? O3 C24 C25 C26 -7.5(5) . . . . ? C23 C24 C25 C26 174.7(3) . . . . ? O3 C24 C25 C30 171.9(3) . . . . ? C23 C24 C25 C30 -6.0(4) . . . . ? C30 C25 C26 C27 0.1(5) . . . . ? C24 C25 C26 C27 179.5(3) . . . . ? C25 C26 C27 C28 -0.9(7) . . . . ? C26 C27 C28 C29 1.0(7) . . . . ? C27 C28 C29 C30 -0.2(7) . . . . ? C28 C29 C30 C25 -0.7(6) . . . . ? C26 C25 C30 C29 0.7(5) . . . . ? C24 C25 C30 C29 -178.6(3) . . . . ? C6 C7 O1 As1 2.7(3) . . . . ? C8 C7 O1 As1 123.8(2) . . . . ? C10 C7 O1 As1 -114.29(19) . . . . ? C17 C18 O2 As1 0.0(3) . . . . ? C19 C18 O2 As1 120.8(2) . . . . ? C21 C18 O2 As1 -117.6(2) . . . . ? C18 O2 As1 O1 -65.0(5) . . . . ? C18 O2 As1 C12 -2.05(19) . . . . ? C18 O2 As1 C1 -136.6(2) . . . . ? C18 O2 As1 C23 106.5(2) . . . . ? C7 O1 As1 O2 -75.9(5) . . . . ? C7 O1 As1 C12 -138.4(2) . . . . ? C7 O1 As1 C1 -3.58(19) . . . . ? C7 O1 As1 C23 112.6(2) . . . . ? C17 C12 As1 O2 3.8(2) . . . . ? C13 C12 As1 O2 178.6(3) . . . . ? C17 C12 As1 O1 175.0(2) . . . . ? C13 C12 As1 O1 -10.1(3) . . . . ? C17 C12 As1 C1 92.1(2) . . . . ? C13 C12 As1 C1 -93.0(3) . . . . ? C17 C12 As1 C23 -89.7(2) . . . . ? C13 C12 As1 C23 85.2(3) . . . . ? C6 C1 As1 O2 174.3(2) . . . . ? C2 C1 As1 O2 -10.0(2) . . . . ? C6 C1 As1 O1 3.64(19) . . . . ? C2 C1 As1 O1 179.4(3) . . . . ? C6 C1 As1 C12 88.8(2) . . . . ? C2 C1 As1 C12 -95.5(3) . . . . ? C6 C1 As1 C23 -89.3(2) . . . . ? C2 C1 As1 C23 86.4(3) . . . . ? C24 C23 As1 O2 54.82(19) . . . . ? C24 C23 As1 O1 -126.63(18) . . . . ? C24 C23 As1 C12 141.41(18) . . . . ? C24 C23 As1 C1 -40.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.481 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.173 # Attachment 'JiangYamamoto6b_CCDC761614.cif' data_Rfee2AsCH2CPh2OH _database_code_depnum_ccdc_archive 'CCDC 761614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 139 _chemical_formula_moiety ? _chemical_formula_sum 'C37 H23 As Cl2 F20 O3' _chemical_formula_weight 1041.37 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 39.96740(10) _cell_length_b 9.5830(5) _cell_length_c 26.4609(6) _cell_angle_alpha 90.00 _cell_angle_beta 127.3997(10) _cell_angle_gamma 90.00 _cell_volume 8051.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.96 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4128 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MacScience DIP2030 Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15491 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.96 _reflns_number_total 8829 _reflns_number_gt 6911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL(Otwinowski, 1997)' _computing_cell_refinement 'HKL(Otwinowski, 1997)' _computing_data_reduction 'HKL(Otwinowski, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+25.2075P] 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 8829 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.2053 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.004 _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 As1 As 0.149643(12) 0.18279(4) 0.040519(18) 0.03213(14) Uani 1 1 d . . . O1 O 0.20212(9) 0.0812(3) 0.08095(14) 0.0385(6) Uani 1 1 d . . . O2 O 0.10343(10) 0.2955(3) 0.01898(16) 0.0437(7) Uani 1 1 d . . . O3 O 0.15152(13) -0.0937(3) -0.02324(16) 0.0570(9) Uani 1 1 d . . . H1 H 0.1754 -0.0673 -0.0085 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.10771(9) 0.4844(3) 0.38773(13) 0.1236(9) Uani 1 1 d . . . Cl2 Cl 0.0553(2) 0.4990(7) 0.2532(2) 0.295(4) Uani 1 1 d . . . C1 C 0.18555(14) 0.3454(4) 0.07015(19) 0.0372(9) Uani 1 1 d . . . C2 C 0.17080(16) 0.4819(5) 0.0552(2) 0.0450(10) Uani 1 1 d . . . H2 H 0.1423 0.5009 0.0330 0.054 Uiso 1 1 calc R . . C3 C 0.19939(19) 0.5888(5) 0.0741(3) 0.0590(13) Uani 1 1 d . . . H3 H 0.1901 0.6807 0.0636 0.071 Uiso 1 1 calc R . . C4 C 0.24146(19) 0.5587(6) 0.1082(3) 0.0667(16) Uani 1 1 d . . . H4 H 0.2606 0.6314 0.1221 0.080 Uiso 1 1 calc R . . C5 C 0.25594(17) 0.4247(6) 0.1224(3) 0.0626(15) Uani 1 1 d . . . H5 H 0.2846 0.4069 0.1454 0.075 Uiso 1 1 calc R . . C6 C 0.22784(14) 0.3152(5) 0.1023(2) 0.0431(10) Uani 1 1 d . . . C7 C 0.23849(13) 0.1601(5) 0.1113(2) 0.0428(10) Uani 1 1 d . . . C8 C 0.26757(15) 0.1206(6) 0.1830(2) 0.0552(13) Uani 1 1 d . . . C9 C 0.25595(19) 0.1752(7) 0.2251(3) 0.0666(16) Uani 1 1 d . . . C10 C 0.25926(16) 0.1236(6) 0.0779(3) 0.0560(13) Uani 1 1 d . . . C11 C 0.2748(2) -0.0265(8) 0.0803(4) 0.0785(19) Uani 1 1 d . . . C12 C 0.13156(13) 0.0592(4) 0.07699(19) 0.0362(8) Uani 1 1 d . . . C13 C 0.14996(15) -0.0694(5) 0.1048(2) 0.0454(10) Uani 1 1 d . . . H6 H 0.1745 -0.0975 0.1111 0.054 Uiso 1 1 calc R . . C14 C 0.13094(17) -0.1543(6) 0.1229(3) 0.0591(14) Uani 1 1 d . . . H7 H 0.1425 -0.2410 0.1411 0.071 Uiso 1 1 calc R . . C15 C 0.09470(18) -0.1101(7) 0.1140(3) 0.0631(15) Uani 1 1 d . . . H8 H 0.0821 -0.1679 0.1263 0.076 Uiso 1 1 calc R . . C16 C 0.07704(17) 0.0176(6) 0.0874(2) 0.0561(13) Uani 1 1 d . . . H9 H 0.0528 0.0461 0.0820 0.067 Uiso 1 1 calc R . . C17 C 0.09552(14) 0.1040(5) 0.0685(2) 0.0417(9) Uani 1 1 d . . . C18 C 0.07932(14) 0.2469(5) 0.0368(2) 0.0447(10) Uani 1 1 d . . . C19 C 0.0817(2) 0.3553(7) 0.0828(4) 0.0727(17) Uani 1 1 d . . . C20 C 0.1233(3) 0.3719(8) 0.1492(4) 0.085(2) Uani 1 1 d . . . C21 C 0.03320(16) 0.2299(6) -0.0256(3) 0.0596(14) Uani 1 1 d . . . C22 C 0.0133(2) 0.3426(8) -0.0764(4) 0.0774(19) Uani 1 1 d . . . C23 C 0.12944(14) 0.1501(4) -0.04645(18) 0.0377(9) Uani 1 1 d . . . H10 H 0.1032 0.2008 -0.0743 0.045 Uiso 1 1 calc R . . H11 H 0.1496 0.1922 -0.0510 0.045 Uiso 1 1 calc R . . C24 C 0.12162(15) -0.0007(5) -0.0720(2) 0.0432(10) Uani 1 1 d . . . C25 C 0.07805(18) -0.0563(6) -0.0968(2) 0.0558(13) Uani 1 1 d . . . C26 C 0.0740(2) -0.1605(6) -0.0648(4) 0.0748(18) Uani 1 1 d . . . H12 H 0.0979 -0.1980 -0.0276 0.090 Uiso 1 1 calc R . . C27 C 0.0339(3) -0.2095(9) -0.0884(5) 0.102(3) Uani 1 1 d . . . H13 H 0.0312 -0.2778 -0.0661 0.123 Uiso 1 1 calc R . . C28 C -0.0012(3) -0.1584(11) -0.1436(5) 0.112(3) Uani 1 1 d . . . H14 H -0.0276 -0.1934 -0.1593 0.134 Uiso 1 1 calc R . . C29 C 0.0023(2) -0.0567(12) -0.1757(4) 0.110(3) Uani 1 1 d . . . H15 H -0.0217 -0.0211 -0.2132 0.132 Uiso 1 1 calc R . . C30 C 0.04220(19) -0.0052(9) -0.1521(3) 0.086(2) Uani 1 1 d . . . H16 H 0.0444 0.0648 -0.1743 0.104 Uiso 1 1 calc R . . C31 C 0.12532(15) -0.0028(5) -0.1267(2) 0.0443(10) Uani 1 1 d . . . C32 C 0.1376(2) -0.1255(6) -0.1392(3) 0.0631(14) Uani 1 1 d . . . H17 H 0.1448 -0.2031 -0.1134 0.076 Uiso 1 1 calc R . . C33 C 0.1393(2) -0.1328(8) -0.1900(3) 0.0766(18) Uani 1 1 d . . . H18 H 0.1474 -0.2155 -0.1980 0.092 Uiso 1 1 calc R . . C34 C 0.1290(2) -0.0205(7) -0.2283(3) 0.0712(17) Uani 1 1 d . . . H19 H 0.1298 -0.0271 -0.2626 0.085 Uiso 1 1 calc R . . C35 C 0.1176(2) 0.1019(7) -0.2162(3) 0.0644(15) Uani 1 1 d . . . H20 H 0.1110 0.1793 -0.2420 0.077 Uiso 1 1 calc R . . C36 C 0.11575(18) 0.1113(6) -0.1656(2) 0.0544(12) Uani 1 1 d . . . H21 H 0.1080 0.1951 -0.1577 0.065 Uiso 1 1 calc R . . F1 F 0.30761(9) 0.1645(4) 0.21088(17) 0.0813(12) Uani 1 1 d . . . F2 F 0.26890(11) -0.0213(4) 0.18839(16) 0.0698(9) Uani 1 1 d . . . F3 F 0.21664(12) 0.1454(5) 0.20033(17) 0.0909(13) Uani 1 1 d . . . F4 F 0.26137(16) 0.3098(5) 0.2343(2) 0.0981(14) Uani 1 1 d . . . F5 F 0.28040(14) 0.1147(5) 0.28185(16) 0.0985(14) Uani 1 1 d . . . F6 F 0.29244(11) 0.2073(4) 0.09803(19) 0.0766(10) Uani 1 1 d . . . F7 F 0.22942(10) 0.1504(4) 0.01537(15) 0.0631(8) Uani 1 1 d . . . F8 F 0.24597(15) -0.1208(4) 0.0646(3) 0.1009(15) Uani 1 1 d . . . F9 F 0.30960(15) -0.0547(5) 0.1382(3) 0.1099(16) Uani 1 1 d . . . F10 F 0.28418(17) -0.0349(6) 0.0406(3) 0.1127(16) Uani 1 1 d . . . F11 F 0.05298(19) 0.3249(6) 0.0928(3) 0.138(2) Uani 1 1 d . . . F12 F 0.07276(18) 0.4848(5) 0.0559(3) 0.1179(17) Uani 1 1 d . . . F13 F 0.15388(16) 0.3943(7) 0.1483(2) 0.123(2) Uani 1 1 d . . . F14 F 0.1315(2) 0.2623(7) 0.1835(2) 0.156(3) Uani 1 1 d . . . F15 F 0.1195(2) 0.4776(6) 0.1785(3) 0.142(2) Uani 1 1 d . . . F16 F 0.03276(15) 0.1171(5) -0.0545(2) 0.123(2) Uani 1 1 d . . . F17 F 0.00612(12) 0.2067(7) -0.0129(3) 0.130(2) Uani 1 1 d . . . F18 F -0.02446(12) 0.3074(6) -0.1252(3) 0.125(2) Uani 1 1 d . . . F19 F 0.03338(15) 0.3699(10) -0.0970(3) 0.191(4) Uani 1 1 d . . . F20 F 0.0097(3) 0.4565(8) -0.0564(4) 0.231(5) Uani 1 1 d . . . C37 C 0.0639(3) 0.4230(13) 0.3176(6) 0.148(5) Uani 1 1 d . . . H22 H 0.0668 0.3231 0.3154 0.178 Uiso 1 1 calc R . . H23 H 0.0396 0.4384 0.3167 0.178 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 As1 0.0304(2) 0.0342(2) 0.0299(2) 0.00320(15) 0.01737(17) -0.00399(15) O1 0.0307(14) 0.0396(16) 0.0419(16) 0.0081(12) 0.0202(13) -0.0016(11) O2 0.0376(16) 0.0433(17) 0.0553(19) 0.0086(13) 0.0310(15) 0.0006(12) O3 0.071(2) 0.0398(18) 0.0454(18) 0.0052(14) 0.0276(18) -0.0007(15) Cl1 0.129(2) 0.1029(17) 0.1123(18) -0.0230(13) 0.0593(16) -0.0011(14) Cl2 0.327(7) 0.312(7) 0.107(3) 0.030(4) 0.059(3) -0.123(6) C1 0.040(2) 0.038(2) 0.035(2) 0.0009(15) 0.0230(18) -0.0092(16) C2 0.050(3) 0.037(2) 0.051(3) 0.0035(18) 0.032(2) -0.0033(18) C3 0.071(4) 0.034(3) 0.075(4) 0.003(2) 0.046(3) -0.007(2) C4 0.060(3) 0.047(3) 0.084(4) -0.002(3) 0.039(3) -0.022(2) C5 0.040(3) 0.059(3) 0.073(4) 0.005(3) 0.025(3) -0.014(2) C6 0.034(2) 0.045(2) 0.038(2) 0.0066(17) 0.0159(18) -0.0088(17) C7 0.031(2) 0.047(3) 0.044(2) 0.0122(18) 0.0188(19) -0.0019(17) C8 0.036(2) 0.061(3) 0.050(3) 0.015(2) 0.017(2) -0.001(2) C9 0.053(3) 0.084(4) 0.040(3) 0.008(3) 0.016(2) -0.008(3) C10 0.045(3) 0.059(3) 0.071(3) 0.018(2) 0.038(3) 0.001(2) C11 0.076(4) 0.077(4) 0.109(6) 0.020(4) 0.070(4) 0.020(3) C12 0.040(2) 0.037(2) 0.0328(19) 0.0012(15) 0.0225(18) -0.0090(16) C13 0.044(2) 0.048(3) 0.038(2) 0.0122(18) 0.022(2) -0.0071(19) C14 0.054(3) 0.059(3) 0.051(3) 0.019(2) 0.025(3) -0.010(2) C15 0.061(3) 0.078(4) 0.050(3) 0.011(3) 0.034(3) -0.023(3) C16 0.053(3) 0.071(3) 0.055(3) 0.002(2) 0.038(3) -0.015(2) C17 0.038(2) 0.051(3) 0.039(2) -0.0011(18) 0.025(2) -0.0088(18) C18 0.038(2) 0.050(3) 0.054(3) 0.001(2) 0.032(2) -0.0049(19) C19 0.076(4) 0.068(4) 0.104(5) -0.018(3) 0.070(4) -0.011(3) C20 0.116(6) 0.091(5) 0.083(5) -0.033(4) 0.078(5) -0.046(4) C21 0.037(3) 0.062(3) 0.078(4) 0.010(3) 0.034(3) -0.004(2) C22 0.052(3) 0.078(5) 0.093(5) 0.023(4) 0.039(4) 0.014(3) C23 0.041(2) 0.041(2) 0.0280(19) 0.0048(15) 0.0191(18) -0.0017(16) C24 0.051(3) 0.041(2) 0.035(2) 0.0019(17) 0.024(2) -0.0040(18) C25 0.066(3) 0.061(3) 0.045(3) -0.015(2) 0.036(3) -0.022(3) C26 0.100(5) 0.053(3) 0.093(5) -0.011(3) 0.070(4) -0.023(3) C27 0.136(8) 0.083(5) 0.145(8) -0.035(5) 0.115(8) -0.056(5) C28 0.105(7) 0.150(8) 0.098(6) -0.063(6) 0.071(6) -0.077(7) C29 0.065(4) 0.201(10) 0.056(4) -0.022(5) 0.033(4) -0.047(6) C30 0.051(3) 0.150(7) 0.042(3) 0.000(4) 0.020(3) -0.034(4) C31 0.047(3) 0.047(3) 0.040(2) -0.0041(18) 0.027(2) -0.0064(19) C32 0.085(4) 0.052(3) 0.059(3) -0.001(2) 0.047(3) 0.003(3) C33 0.100(5) 0.073(4) 0.072(4) -0.013(3) 0.060(4) 0.007(4) C34 0.081(4) 0.091(5) 0.053(3) -0.009(3) 0.046(3) -0.008(3) C35 0.077(4) 0.075(4) 0.044(3) 0.005(2) 0.038(3) -0.004(3) C36 0.064(3) 0.057(3) 0.044(3) 0.001(2) 0.034(3) -0.001(2) F1 0.0284(14) 0.112(3) 0.066(2) 0.0234(19) 0.0094(15) -0.0067(16) F2 0.064(2) 0.065(2) 0.066(2) 0.0304(16) 0.0315(17) 0.0140(15) F3 0.058(2) 0.155(4) 0.056(2) -0.020(2) 0.0334(18) -0.018(2) F4 0.126(4) 0.085(3) 0.070(3) -0.012(2) 0.053(3) -0.014(2) F5 0.087(3) 0.137(4) 0.0391(17) 0.023(2) 0.0214(19) -0.001(3) F6 0.0512(19) 0.091(3) 0.100(3) 0.017(2) 0.052(2) -0.0107(17) F7 0.0606(19) 0.082(2) 0.0607(19) 0.0170(16) 0.0440(17) 0.0042(16) F8 0.105(3) 0.058(2) 0.175(5) 0.002(2) 0.103(4) 0.007(2) F9 0.084(3) 0.115(4) 0.136(4) 0.050(3) 0.070(3) 0.051(3) F10 0.125(4) 0.122(4) 0.152(4) 0.012(3) 0.116(4) 0.027(3) F11 0.130(4) 0.164(5) 0.205(6) -0.085(4) 0.146(5) -0.057(4) F12 0.144(4) 0.062(3) 0.140(4) -0.006(3) 0.082(4) 0.026(3) F13 0.093(3) 0.211(6) 0.083(3) -0.046(3) 0.062(3) -0.049(4) F14 0.246(8) 0.120(4) 0.069(3) -0.014(3) 0.079(4) -0.055(5) F15 0.170(5) 0.143(5) 0.157(5) -0.096(4) 0.121(5) -0.050(4) F16 0.092(3) 0.076(3) 0.076(3) -0.022(2) -0.014(2) 0.014(2) F17 0.047(2) 0.220(6) 0.115(4) 0.054(4) 0.045(2) -0.019(3) F18 0.042(2) 0.165(5) 0.113(4) 0.067(3) 0.018(2) 0.006(2) F19 0.053(3) 0.350(11) 0.124(4) 0.143(6) 0.031(3) 0.005(4) F20 0.286(11) 0.124(6) 0.151(6) 0.037(5) 0.064(7) 0.108(7) C37 0.106(8) 0.129(9) 0.137(9) 0.036(7) 0.037(7) -0.008(6) _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 As1 O2 1.904(3) . ? As1 C12 1.924(4) . ? As1 C1 1.933(4) . ? As1 O1 1.940(3) . ? As1 C23 1.946(4) . ? O1 C7 1.382(5) . ? O2 C18 1.386(5) . ? O3 C24 1.418(6) . ? O3 H1 0.8200 . ? Cl1 C37 1.706(11) . ? Cl2 C37 1.684(12) . ? C1 C6 1.385(6) . ? C1 C2 1.390(6) . ? C2 C3 1.383(7) . ? C2 H2 0.9300 . ? C3 C4 1.372(8) . ? C3 H3 0.9300 . ? C4 C5 1.364(8) . ? C4 H4 0.9300 . ? C5 C6 1.386(6) . ? C5 H5 0.9300 . ? C6 C7 1.525(6) . ? C7 C8 1.555(7) . ? C7 C10 1.576(7) . ? C8 F1 1.359(6) . ? C8 F2 1.366(6) . ? C8 C9 1.535(9) . ? C9 F4 1.306(7) . ? C9 F3 1.315(7) . ? C9 F5 1.328(6) . ? C10 F6 1.352(6) . ? C10 F7 1.352(6) . ? C10 C11 1.554(9) . ? C11 F10 1.314(8) . ? C11 F8 1.318(8) . ? C11 F9 1.329(9) . ? C12 C17 1.384(6) . ? C12 C13 1.394(6) . ? C13 C14 1.383(6) . ? C13 H6 0.9300 . ? C14 C15 1.384(9) . ? C14 H7 0.9300 . ? C15 C16 1.375(8) . ? C15 H8 0.9300 . ? C16 C17 1.389(6) . ? C16 H9 0.9300 . ? C17 C18 1.529(7) . ? C18 C19 1.559(8) . ? C18 C21 1.566(7) . ? C19 F11 1.359(7) . ? C19 F12 1.366(8) . ? C19 C20 1.525(11) . ? C20 F13 1.257(8) . ? C20 F14 1.292(9) . ? C20 F15 1.338(8) . ? C21 F16 1.318(8) . ? C21 F17 1.333(7) . ? C21 C22 1.520(9) . ? C22 F19 1.240(9) . ? C22 F20 1.261(10) . ? C22 F18 1.301(8) . ? C23 C24 1.544(6) . ? C23 H10 0.9700 . ? C23 H11 0.9700 . ? C24 C25 1.535(7) . ? C24 C31 1.543(6) . ? C25 C30 1.374(9) . ? C25 C26 1.381(8) . ? C26 C27 1.403(10) . ? C26 H12 0.9300 . ? C27 C28 1.360(14) . ? C27 H13 0.9300 . ? C28 C29 1.354(13) . ? C28 H14 0.9300 . ? C29 C30 1.403(9) . ? C29 H15 0.9300 . ? C30 H16 0.9300 . ? C31 C36 1.387(7) . ? C31 C32 1.390(7) . ? C32 C33 1.386(8) . ? C32 H17 0.9300 . ? C33 C34 1.359(10) . ? C33 H18 0.9300 . ? C34 C35 1.365(9) . ? C34 H19 0.9300 . ? C35 C36 1.388(7) . ? C35 H20 0.9300 . ? C36 H21 0.9300 . ? C37 H22 0.9700 . ? C37 H23 0.9700 . ? 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 O2 As1 C12 84.70(16) . . ? O2 As1 C1 90.59(16) . . ? C12 As1 C1 134.84(17) . . ? O2 As1 O1 167.67(14) . . ? C12 As1 O1 91.38(15) . . ? C1 As1 O1 83.87(16) . . ? O2 As1 C23 96.14(17) . . ? C12 As1 C23 118.76(17) . . ? C1 As1 C23 106.39(17) . . ? O1 As1 C23 95.99(16) . . ? C7 O1 As1 116.7(3) . . ? C18 O2 As1 117.2(3) . . ? C24 O3 H1 109.5 . . ? C6 C1 C2 121.4(4) . . ? C6 C1 As1 114.1(3) . . ? C2 C1 As1 124.1(3) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 121.7(5) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 119.8(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 118.7(4) . . ? C1 C6 C7 114.9(4) . . ? C5 C6 C7 126.4(4) . . ? O1 C7 C6 110.3(4) . . ? O1 C7 C8 108.6(3) . . ? C6 C7 C8 111.0(4) . . ? O1 C7 C10 106.2(4) . . ? C6 C7 C10 108.7(4) . . ? C8 C7 C10 111.9(4) . . ? F1 C8 F2 107.0(4) . . ? F1 C8 C9 106.1(5) . . ? F2 C8 C9 105.9(4) . . ? F1 C8 C7 110.3(4) . . ? F2 C8 C7 108.8(4) . . ? C9 C8 C7 118.2(4) . . ? F4 C9 F3 108.7(6) . . ? F4 C9 F5 107.2(5) . . ? F3 C9 F5 107.8(5) . . ? F4 C9 C8 112.4(5) . . ? F3 C9 C8 111.2(5) . . ? F5 C9 C8 109.4(6) . . ? F6 C10 F7 107.2(4) . . ? F6 C10 C11 105.1(5) . . ? F7 C10 C11 105.1(5) . . ? F6 C10 C7 111.8(5) . . ? F7 C10 C7 105.7(4) . . ? C11 C10 C7 121.1(4) . . ? F10 C11 F8 108.9(7) . . ? F10 C11 F9 107.7(6) . . ? F8 C11 F9 109.1(6) . . ? F10 C11 C10 108.9(5) . . ? F8 C11 C10 111.7(5) . . ? F9 C11 C10 110.3(6) . . ? C17 C12 C13 121.5(4) . . ? C17 C12 As1 113.5(3) . . ? C13 C12 As1 124.8(3) . . ? C14 C13 C12 118.6(5) . . ? C14 C13 H6 120.7 . . ? C12 C13 H6 120.7 . . ? C13 C14 C15 120.0(5) . . ? C13 C14 H7 120.0 . . ? C15 C14 H7 120.0 . . ? C16 C15 C14 121.2(4) . . ? C16 C15 H8 119.4 . . ? C14 C15 H8 119.4 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H9 120.1 . . ? C17 C16 H9 120.1 . . ? C12 C17 C16 119.0(5) . . ? C12 C17 C18 114.8(4) . . ? C16 C17 C18 126.2(4) . . ? O2 C18 C17 109.7(4) . . ? O2 C18 C19 108.4(4) . . ? C17 C18 C19 111.4(4) . . ? O2 C18 C21 107.0(4) . . ? C17 C18 C21 108.7(4) . . ? C19 C18 C21 111.6(4) . . ? F11 C19 F12 108.1(6) . . ? F11 C19 C20 104.8(6) . . ? F12 C19 C20 105.3(6) . . ? F11 C19 C18 110.5(5) . . ? F12 C19 C18 109.1(6) . . ? C20 C19 C18 118.5(6) . . ? F13 C20 F14 108.5(9) . . ? F13 C20 F15 109.6(6) . . ? F14 C20 F15 106.2(6) . . ? F13 C20 C19 112.7(6) . . ? F14 C20 C19 111.0(6) . . ? F15 C20 C19 108.6(7) . . ? F16 C21 F17 106.5(6) . . ? F16 C21 C22 104.7(6) . . ? F17 C21 C22 105.9(5) . . ? F16 C21 C18 106.8(4) . . ? F17 C21 C18 111.6(5) . . ? C22 C21 C18 120.5(5) . . ? F19 C22 F20 105.9(9) . . ? F19 C22 F18 106.9(7) . . ? F20 C22 F18 106.3(7) . . ? F19 C22 C21 114.1(6) . . ? F20 C22 C21 112.0(7) . . ? F18 C22 C21 111.2(6) . . ? C24 C23 As1 119.7(3) . . ? C24 C23 H10 107.4 . . ? As1 C23 H10 107.4 . . ? C24 C23 H11 107.4 . . ? As1 C23 H11 107.4 . . ? H10 C23 H11 106.9 . . ? O3 C24 C25 106.4(4) . . ? O3 C24 C31 109.7(4) . . ? C25 C24 C31 108.9(4) . . ? O3 C24 C23 110.8(3) . . ? C25 C24 C23 112.8(4) . . ? C31 C24 C23 108.2(3) . . ? C30 C25 C26 118.5(6) . . ? C30 C25 C24 120.7(5) . . ? C26 C25 C24 120.8(5) . . ? C25 C26 C27 119.8(8) . . ? C25 C26 H12 120.1 . . ? C27 C26 H12 120.1 . . ? C28 C27 C26 120.8(8) . . ? C28 C27 H13 119.6 . . ? C26 C27 H13 119.6 . . ? C29 C28 C27 120.1(8) . . ? C29 C28 H14 120.0 . . ? C27 C28 H14 120.0 . . ? C28 C29 C30 119.7(9) . . ? C28 C29 H15 120.1 . . ? C30 C29 H15 120.1 . . ? C25 C30 C29 121.1(7) . . ? C25 C30 H16 119.4 . . ? C29 C30 H16 119.4 . . ? C36 C31 C32 117.9(5) . . ? C36 C31 C24 123.2(4) . . ? C32 C31 C24 118.9(4) . . ? C33 C32 C31 120.3(6) . . ? C33 C32 H17 119.8 . . ? C31 C32 H17 119.8 . . ? C34 C33 C32 120.8(6) . . ? C34 C33 H18 119.6 . . ? C32 C33 H18 119.6 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H19 120.1 . . ? C35 C34 H19 120.1 . . ? C34 C35 C36 120.1(5) . . ? C34 C35 H20 119.9 . . ? C36 C35 H20 119.9 . . ? C31 C36 C35 120.9(5) . . ? C31 C36 H21 119.5 . . ? C35 C36 H21 119.5 . . ? Cl2 C37 Cl1 113.3(7) . . ? Cl2 C37 H22 108.9 . . ? Cl1 C37 H22 108.9 . . ? Cl2 C37 H23 108.9 . . ? Cl1 C37 H23 108.9 . . ? H22 C37 H23 107.7 . . ? 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 O2 As1 O1 C7 -62.5(7) . . . . ? C12 As1 O1 C7 -133.7(3) . . . . ? C1 As1 O1 C7 1.3(3) . . . . ? C23 As1 O1 C7 107.2(3) . . . . ? C12 As1 O2 C18 0.2(3) . . . . ? C1 As1 O2 C18 -134.8(3) . . . . ? O1 As1 O2 C18 -71.7(7) . . . . ? C23 As1 O2 C18 118.7(3) . . . . ? O2 As1 C1 C6 170.0(3) . . . . ? C12 As1 C1 C6 86.9(4) . . . . ? O1 As1 C1 C6 1.0(3) . . . . ? C23 As1 C1 C6 -93.4(3) . . . . ? O2 As1 C1 C2 -16.9(4) . . . . ? C12 As1 C1 C2 -100.0(4) . . . . ? O1 As1 C1 C2 174.1(4) . . . . ? C23 As1 C1 C2 79.7(4) . . . . ? C6 C1 C2 C3 -1.0(7) . . . . ? As1 C1 C2 C3 -173.7(4) . . . . ? C1 C2 C3 C4 -1.7(8) . . . . ? C2 C3 C4 C5 2.4(10) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? C2 C1 C6 C5 3.0(7) . . . . ? As1 C1 C6 C5 176.4(4) . . . . ? C2 C1 C6 C7 -176.3(4) . . . . ? As1 C1 C6 C7 -2.9(5) . . . . ? C4 C5 C6 C1 -2.4(8) . . . . ? C4 C5 C6 C7 176.9(6) . . . . ? As1 O1 C7 C6 -3.0(5) . . . . ? As1 O1 C7 C8 118.8(4) . . . . ? As1 O1 C7 C10 -120.7(3) . . . . ? C1 C6 C7 O1 3.8(6) . . . . ? C5 C6 C7 O1 -175.4(5) . . . . ? C1 C6 C7 C8 -116.6(4) . . . . ? C5 C6 C7 C8 64.2(7) . . . . ? C1 C6 C7 C10 119.9(4) . . . . ? C5 C6 C7 C10 -59.3(7) . . . . ? O1 C7 C8 F1 162.9(4) . . . . ? C6 C7 C8 F1 -75.7(6) . . . . ? C10 C7 C8 F1 45.9(6) . . . . ? O1 C7 C8 F2 45.7(5) . . . . ? C6 C7 C8 F2 167.1(4) . . . . ? C10 C7 C8 F2 -71.2(5) . . . . ? O1 C7 C8 C9 -74.9(6) . . . . ? C6 C7 C8 C9 46.5(6) . . . . ? C10 C7 C8 C9 168.2(5) . . . . ? F1 C8 C9 F4 54.2(6) . . . . ? F2 C8 C9 F4 167.7(5) . . . . ? C7 C8 C9 F4 -70.1(6) . . . . ? F1 C8 C9 F3 176.3(5) . . . . ? F2 C8 C9 F3 -70.2(6) . . . . ? C7 C8 C9 F3 51.9(7) . . . . ? F1 C8 C9 F5 -64.8(6) . . . . ? F2 C8 C9 F5 48.7(6) . . . . ? C7 C8 C9 F5 170.8(5) . . . . ? O1 C7 C10 F6 172.2(4) . . . . ? C6 C7 C10 F6 53.6(5) . . . . ? C8 C7 C10 F6 -69.4(5) . . . . ? O1 C7 C10 F7 56.0(5) . . . . ? C6 C7 C10 F7 -62.7(5) . . . . ? C8 C7 C10 F7 174.3(4) . . . . ? O1 C7 C10 C11 -63.0(6) . . . . ? C6 C7 C10 C11 178.3(5) . . . . ? C8 C7 C10 C11 55.3(7) . . . . ? F6 C10 C11 F10 -62.6(7) . . . . ? F7 C10 C11 F10 50.3(7) . . . . ? C7 C10 C11 F10 169.6(5) . . . . ? F6 C10 C11 F8 177.0(6) . . . . ? F7 C10 C11 F8 -70.1(7) . . . . ? C7 C10 C11 F8 49.2(8) . . . . ? F6 C10 C11 F9 55.4(6) . . . . ? F7 C10 C11 F9 168.4(5) . . . . ? C7 C10 C11 F9 -72.4(7) . . . . ? O2 As1 C12 C17 2.5(3) . . . . ? C1 As1 C12 C17 88.1(4) . . . . ? O1 As1 C12 C17 170.8(3) . . . . ? C23 As1 C12 C17 -91.6(4) . . . . ? O2 As1 C12 C13 177.3(4) . . . . ? C1 As1 C12 C13 -97.1(4) . . . . ? O1 As1 C12 C13 -14.4(4) . . . . ? C23 As1 C12 C13 83.2(4) . . . . ? C17 C12 C13 C14 1.3(7) . . . . ? As1 C12 C13 C14 -173.0(4) . . . . ? C12 C13 C14 C15 -0.8(8) . . . . ? C13 C14 C15 C16 -0.1(9) . . . . ? C14 C15 C16 C17 0.5(8) . . . . ? C13 C12 C17 C16 -0.9(7) . . . . ? As1 C12 C17 C16 174.1(4) . . . . ? C13 C12 C17 C18 -179.6(4) . . . . ? As1 C12 C17 C18 -4.6(5) . . . . ? C15 C16 C17 C12 0.0(7) . . . . ? C15 C16 C17 C18 178.5(5) . . . . ? As1 O2 C18 C17 -2.6(5) . . . . ? As1 O2 C18 C19 119.2(4) . . . . ? As1 O2 C18 C21 -120.3(4) . . . . ? C12 C17 C18 O2 4.7(6) . . . . ? C16 C17 C18 O2 -173.9(5) . . . . ? C12 C17 C18 C19 -115.3(5) . . . . ? C16 C17 C18 C19 66.1(6) . . . . ? C12 C17 C18 C21 121.3(4) . . . . ? C16 C17 C18 C21 -57.2(6) . . . . ? O2 C18 C19 F11 169.3(6) . . . . ? C17 C18 C19 F11 -69.9(7) . . . . ? C21 C18 C19 F11 51.7(8) . . . . ? O2 C18 C19 F12 50.6(6) . . . . ? C17 C18 C19 F12 171.4(5) . . . . ? C21 C18 C19 F12 -67.0(6) . . . . ? O2 C18 C19 C20 -69.7(7) . . . . ? C17 C18 C19 C20 51.0(7) . . . . ? C21 C18 C19 C20 172.7(5) . . . . ? F11 C19 C20 F13 176.9(7) . . . . ? F12 C19 C20 F13 -69.1(8) . . . . ? C18 C19 C20 F13 53.1(9) . . . . ? F11 C19 C20 F14 54.9(8) . . . . ? F12 C19 C20 F14 168.9(6) . . . . ? C18 C19 C20 F14 -68.8(8) . . . . ? F11 C19 C20 F15 -61.5(7) . . . . ? F12 C19 C20 F15 52.5(7) . . . . ? C18 C19 C20 F15 174.7(5) . . . . ? O2 C18 C21 F16 74.8(6) . . . . ? C17 C18 C21 F16 -43.6(6) . . . . ? C19 C18 C21 F16 -166.8(5) . . . . ? O2 C18 C21 F17 -169.2(5) . . . . ? C17 C18 C21 F17 72.4(6) . . . . ? C19 C18 C21 F17 -50.8(7) . . . . ? O2 C18 C21 C22 -44.2(7) . . . . ? C17 C18 C21 C22 -162.6(5) . . . . ? C19 C18 C21 C22 74.2(7) . . . . ? F16 C21 C22 F19 -62.9(9) . . . . ? F17 C21 C22 F19 -175.2(8) . . . . ? C18 C21 C22 F19 57.1(10) . . . . ? F16 C21 C22 F20 176.8(8) . . . . ? F17 C21 C22 F20 64.5(9) . . . . ? C18 C21 C22 F20 -63.2(10) . . . . ? F16 C21 C22 F18 58.0(7) . . . . ? F17 C21 C22 F18 -54.2(8) . . . . ? C18 C21 C22 F18 178.1(6) . . . . ? O2 As1 C23 C24 -121.0(3) . . . . ? C12 As1 C23 C24 -33.7(4) . . . . ? C1 As1 C23 C24 146.5(3) . . . . ? O1 As1 C23 C24 61.2(4) . . . . ? As1 C23 C24 O3 -35.0(5) . . . . ? As1 C23 C24 C25 84.1(4) . . . . ? As1 C23 C24 C31 -155.3(3) . . . . ? O3 C24 C25 C30 -167.7(6) . . . . ? C31 C24 C25 C30 -49.6(7) . . . . ? C23 C24 C25 C30 70.6(7) . . . . ? O3 C24 C25 C26 11.1(7) . . . . ? C31 C24 C25 C26 129.3(5) . . . . ? C23 C24 C25 C26 -110.5(6) . . . . ? C30 C25 C26 C27 -1.1(10) . . . . ? C24 C25 C26 C27 180.0(6) . . . . ? C25 C26 C27 C28 1.9(12) . . . . ? C26 C27 C28 C29 -1.6(14) . . . . ? C27 C28 C29 C30 0.6(15) . . . . ? C26 C25 C30 C29 0.2(11) . . . . ? C24 C25 C30 C29 179.1(7) . . . . ? C28 C29 C30 C25 0.1(14) . . . . ? O3 C24 C31 C36 -150.4(5) . . . . ? C25 C24 C31 C36 93.5(6) . . . . ? C23 C24 C31 C36 -29.4(6) . . . . ? O3 C24 C31 C32 31.5(6) . . . . ? C25 C24 C31 C32 -84.5(6) . . . . ? C23 C24 C31 C32 152.5(5) . . . . ? C36 C31 C32 C33 -1.4(9) . . . . ? C24 C31 C32 C33 176.8(6) . . . . ? C31 C32 C33 C34 0.2(11) . . . . ? C32 C33 C34 C35 1.0(11) . . . . ? C33 C34 C35 C36 -1.0(10) . . . . ? C32 C31 C36 C35 1.3(8) . . . . ? C24 C31 C36 C35 -176.8(5) . . . . ? C34 C35 C36 C31 -0.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.603 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.212