# Supplementary Material (ESI) for Catalysis Science & Technology # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_Cambridge 1486 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Enthaler, Stephan' _publ_contact_author_email stephan.enthaler@tu-berlin.de _publ_section_title ; A straightforward zinc-catalysed reduction of sulfoxides to sulfides ; _publ_author_name S.Enthaler # Attachment '- CCDC-782191.CIF' data_c:\dokume~1\sebast~1\desktop\e44\r-3 _database_code_depnum_ccdc_archive 'CCDC 782191' #TrackingRef '- CCDC-782191.CIF' _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 F6 O12 S8 Zn' _chemical_formula_weight 1204.67 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 12.5877(4) _cell_length_b 12.5877(4) _cell_length_c 29.1803(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4004.2(2) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2812 _cell_measurement_theta_min 3.2334 _cell_measurement_theta_max 32.3007 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8483 _exptl_absorpt_correction_T_max 0.8551 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5363 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1575 _reflns_number_gt 1246 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1575 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Zn1 Zn 0.0000 0.0000 0.0000 0.02230(18) Uani 1 6 d S . . S1 S 0.17651(5) 0.23917(5) 0.052816(18) 0.02972(18) Uani 1 1 d . . . S2 S 0.6667 0.3333 -0.04873(3) 0.0320(3) Uani 1 3 d S . . O1 O 0.15180(13) 0.11135(13) 0.04049(5) 0.0288(4) Uani 1 1 d . . . O2 O 0.64826(19) 0.21475(18) -0.05951(6) 0.0581(6) Uani 1 1 d . . . F1 F 0.56183(17) 0.24413(17) 0.02992(5) 0.0750(6) Uani 1 1 d . . . C1 C 0.3346(2) 0.3364(2) 0.03941(8) 0.0413(6) Uani 1 1 d . . . H1A H 0.3460 0.3381 0.0061 0.062 Uiso 1 1 calc R . . H1B H 0.3832 0.3050 0.0543 0.062 Uiso 1 1 calc R . . H1C H 0.3616 0.4196 0.0504 0.062 Uiso 1 1 calc R . . C2 C 0.1857(2) 0.2459(2) 0.11383(7) 0.0276(5) Uani 1 1 d . . . C3 C 0.1830(2) 0.3425(2) 0.13533(8) 0.0344(6) Uani 1 1 d . . . H3 H 0.1773 0.4032 0.1179 0.041 Uiso 1 1 calc R . . C4 C 0.1889(2) 0.3489(2) 0.18285(8) 0.0412(6) Uani 1 1 d . . . H4 H 0.1893 0.4156 0.1982 0.049 Uiso 1 1 calc R . . C5 C 0.1943(2) 0.2582(2) 0.20781(8) 0.0402(6) Uani 1 1 d . . . H5 H 0.2002 0.2637 0.2403 0.048 Uiso 1 1 calc R . . C6 C 0.1911(2) 0.1606(2) 0.18591(8) 0.0399(6) Uani 1 1 d . . . H6 H 0.1919 0.0972 0.2034 0.048 Uiso 1 1 calc R . . C7 C 0.1867(2) 0.1532(2) 0.13852(8) 0.0353(6) Uani 1 1 d . . . H7 H 0.1844 0.0854 0.1233 0.042 Uiso 1 1 calc R . . C8 C 0.6667 0.3333 0.01318(14) 0.0403(11) Uani 1 3 d S . . 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 Zn1 0.0258(2) 0.0258(2) 0.0154(3) 0.000 0.000 0.01288(12) S1 0.0363(4) 0.0306(3) 0.0235(3) -0.0042(2) -0.0070(2) 0.0176(3) S2 0.0389(4) 0.0389(4) 0.0183(5) 0.000 0.000 0.0195(2) O1 0.0316(9) 0.0302(9) 0.0266(8) -0.0067(7) -0.0076(7) 0.0170(7) O2 0.0746(14) 0.0520(12) 0.0510(12) -0.0175(10) 0.0064(11) 0.0342(11) F1 0.0754(12) 0.0845(14) 0.0466(10) 0.0251(9) 0.0311(9) 0.0261(11) C1 0.0441(16) 0.0357(15) 0.0304(13) -0.0019(11) 0.0043(12) 0.0097(13) C2 0.0261(12) 0.0300(13) 0.0226(11) -0.0019(10) -0.0020(10) 0.0109(11) C3 0.0355(14) 0.0369(14) 0.0331(13) -0.0016(11) 0.0005(11) 0.0199(12) C4 0.0458(16) 0.0469(16) 0.0336(14) -0.0062(12) 0.0021(12) 0.0252(14) C5 0.0410(15) 0.0509(17) 0.0220(12) 0.0014(12) 0.0026(11) 0.0178(13) C6 0.0459(16) 0.0413(15) 0.0316(13) 0.0089(12) -0.0014(12) 0.0210(13) C7 0.0398(15) 0.0305(14) 0.0340(14) -0.0030(11) -0.0039(11) 0.0165(12) C8 0.0473(17) 0.0473(17) 0.026(2) 0.000 0.000 0.0237(9) _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 Zn1 O1 2.0817(14) 10 ? Zn1 O1 2.0817(14) . ? Zn1 O1 2.0817(14) 12 ? Zn1 O1 2.0817(14) 3 ? Zn1 O1 2.0817(14) 11 ? Zn1 O1 2.0817(14) 2 ? S1 O1 1.5213(15) . ? S1 C1 1.782(2) . ? S1 C2 1.783(2) . ? S2 O2 1.4265(18) . ? S2 O2 1.4265(18) 2_655 ? S2 O2 1.4265(18) 3_665 ? S2 C8 1.806(4) . ? F1 C8 1.326(2) . ? C2 C7 1.376(3) . ? C2 C3 1.383(3) . ? C3 C4 1.389(3) . ? C4 C5 1.384(3) . ? C5 C6 1.368(3) . ? C6 C7 1.385(3) . ? C8 F1 1.326(2) 2_655 ? C8 F1 1.326(2) 3_665 ? 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 O1 Zn1 O1 180.00(10) 10 . ? O1 Zn1 O1 90.96(6) 10 12 ? O1 Zn1 O1 89.04(6) . 12 ? O1 Zn1 O1 89.04(6) 10 3 ? O1 Zn1 O1 90.96(6) . 3 ? O1 Zn1 O1 180.00(6) 12 3 ? O1 Zn1 O1 90.96(6) 10 11 ? O1 Zn1 O1 89.04(6) . 11 ? O1 Zn1 O1 90.96(6) 12 11 ? O1 Zn1 O1 89.04(6) 3 11 ? O1 Zn1 O1 89.04(6) 10 2 ? O1 Zn1 O1 90.96(6) . 2 ? O1 Zn1 O1 89.04(6) 12 2 ? O1 Zn1 O1 90.96(6) 3 2 ? O1 Zn1 O1 180.00(8) 11 2 ? O1 S1 C1 104.01(10) . . ? O1 S1 C2 105.09(10) . . ? C1 S1 C2 99.38(11) . . ? O2 S2 O2 115.28(6) . 2_655 ? O2 S2 O2 115.28(6) . 3_665 ? O2 S2 O2 115.28(6) 2_655 3_665 ? O2 S2 C8 102.74(9) . . ? O2 S2 C8 102.74(9) 2_655 . ? O2 S2 C8 102.74(9) 3_665 . ? S1 O1 Zn1 118.66(8) . . ? C7 C2 C3 121.5(2) . . ? C7 C2 S1 120.67(17) . . ? C3 C2 S1 117.71(18) . . ? C2 C3 C4 118.7(2) . . ? C5 C4 C3 120.0(2) . . ? C6 C5 C4 120.2(2) . . ? C5 C6 C7 120.6(2) . . ? C2 C7 C6 118.9(2) . . ? F1 C8 F1 107.3(2) 2_655 . ? F1 C8 F1 107.3(2) 2_655 3_665 ? F1 C8 F1 107.3(2) . 3_665 ? F1 C8 S2 111.61(18) 2_655 . ? F1 C8 S2 111.61(18) . . ? F1 C8 S2 111.61(18) 3_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.306 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.048 # Attachment '- CCDC-796905.CIF' data_x:\x-ray\e48\e48 _database_code_depnum_ccdc_archive 'CCDC 796905' #TrackingRef '- CCDC-796905.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.33 H0 F4 O6.67 S4 Zn0.67' _chemical_formula_weight 754.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5817(4) _cell_length_b 13.8939(5) _cell_length_c 19.8576(8) _cell_angle_alpha 83.554(3) _cell_angle_beta 88.085(3) _cell_angle_gamma 73.117(3) _cell_volume 2775.99(18) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21815 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.1608 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9791 _reflns_number_gt 5071 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9791 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _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 Zn1 Zn 0.68598(6) 0.73934(5) 0.73986(3) 0.02238(16) Uani 1 1 d . . . S2 S 0.91820(12) 0.80185(10) 0.66159(6) 0.0232(3) Uani 1 1 d . . . S3 S 0.45326(12) 0.68650(9) 0.82362(6) 0.0222(3) Uani 1 1 d . . . S4 S 0.52853(12) 0.96773(9) 0.75889(6) 0.0239(3) Uani 1 1 d . . . S5 S 0.85514(12) 0.50595(9) 0.74214(6) 0.0215(3) Uani 1 1 d . . . S7 S 0.48157(14) 0.67059(11) 0.64045(8) 0.0364(4) Uani 1 1 d . . . C10 C 0.2664(5) 0.9874(4) 0.7884(2) 0.0277(13) Uani 1 1 d . . . H10 H 0.2765 0.9304 0.7642 0.033 Uiso 1 1 calc R . . C14 C 0.8637(6) 0.7118(4) 0.5541(3) 0.0312(14) Uani 1 1 d . . . H14 H 0.7738 0.7351 0.5673 0.037 Uiso 1 1 calc R . . O16 O 1.0238(3) 0.7306(3) 0.84796(19) 0.0456(11) Uani 1 1 d . . . O3 O 0.6013(3) 0.6576(2) 0.81160(15) 0.0247(8) Uani 1 1 d . . . O4 O 0.8484(3) 0.6174(2) 0.73613(15) 0.0248(8) Uani 1 1 d . . . O5 O 0.7696(3) 0.8224(2) 0.66904(15) 0.0238(8) Uani 1 1 d . . . O6 O 0.5251(3) 0.8601(2) 0.75335(16) 0.0282(9) Uani 1 1 d . . . O7 O 0.5926(3) 0.7044(3) 0.65647(17) 0.0331(9) Uani 1 1 d . . . O8 O 0.7907(3) 0.7844(2) 0.82079(16) 0.0262(8) Uani 1 1 d . . . C1 C 0.9419(5) 0.9194(4) 0.6250(2) 0.0245(12) Uani 1 1 d . . . O2 O 0.9203(4) 0.9029(3) 0.79762(18) 0.0456(11) Uani 1 1 d . . . C7 C 1.0219(5) 0.4469(4) 0.7184(2) 0.0209(12) Uani 1 1 d . . . C34 C 0.9604(5) 0.7326(4) 0.5892(2) 0.0237(12) Uani 1 1 d . . . C17 C 0.4957(5) 1.0304(4) 0.6751(2) 0.0221(12) Uani 1 1 d . . . C19 C 0.8654(5) 0.4648(4) 0.8316(2) 0.0214(12) Uani 1 1 d . . . C4 C 0.5117(5) 0.5042(4) 0.9047(2) 0.0250(13) Uani 1 1 d . . . H4 H 0.5940 0.5148 0.9137 0.030 Uiso 1 1 calc R . . C6 C 0.2981(5) 0.7968(4) 0.9175(3) 0.0300(14) Uani 1 1 d . . . H6 H 0.2266 0.7825 0.8971 0.036 Uiso 1 1 calc R . . C9 C 0.5317(6) 0.7782(4) 0.9235(2) 0.0311(14) Uani 1 1 d . . . H9 H 0.6188 0.7515 0.9071 0.037 Uiso 1 1 calc R . . C3 C 0.4809(5) 0.4189(4) 0.9342(2) 0.0280(13) Uani 1 1 d . . . H3 H 0.5420 0.3705 0.9640 0.034 Uiso 1 1 calc R . . C15 C 0.4273(5) 0.7565(3) 0.8959(2) 0.0225(12) Uani 1 1 d . . . C8 C 0.3615(5) 0.4039(4) 0.9206(3) 0.0317(14) Uani 1 1 d . . . H8 H 0.3408 0.3452 0.9412 0.038 Uiso 1 1 calc R . . C5 C 0.4206(5) 0.5741(3) 0.8617(2) 0.0191(11) Uani 1 1 d . . . C35 C 0.8552(5) 0.3692(4) 0.8524(3) 0.0289(13) Uani 1 1 d . . . H35 H 0.8475 0.3257 0.8201 0.035 Uiso 1 1 calc R . . C13 C 0.3712(5) 1.0245(4) 0.7958(2) 0.0204(12) Uani 1 1 d . . . C16 C 1.0560(6) 0.9399(4) 0.6407(3) 0.0371(15) Uani 1 1 d . . . H16 H 1.1202 0.8933 0.6698 0.045 Uiso 1 1 calc R . . C18 C 1.1101(5) 0.5028(4) 0.7122(3) 0.0299(13) Uani 1 1 d . . . H18 H 1.0831 0.5718 0.7208 0.036 Uiso 1 1 calc R . . C20 C 0.2718(5) 0.4730(4) 0.8773(3) 0.0321(14) Uani 1 1 d . . . H20 H 0.1899 0.4622 0.8678 0.038 Uiso 1 1 calc R . . C21 C 0.3818(6) 0.8790(4) 0.9982(3) 0.0394(16) Uani 1 1 d . . . H21 H 0.3660 0.9212 1.0339 0.047 Uiso 1 1 calc R . . C22 C 0.5084(6) 0.8397(4) 0.9758(3) 0.0370(15) Uani 1 1 d . . . H22 H 0.5798 0.8544 0.9961 0.044 Uiso 1 1 calc R . . C23 C 1.2388(5) 0.4575(4) 0.6933(3) 0.0374(15) Uani 1 1 d . . . H23 H 1.3015 0.4947 0.6894 0.045 Uiso 1 1 calc R . . C24 C 0.8564(5) 0.3379(4) 0.9208(3) 0.0340(14) Uani 1 1 d . . . H24 H 0.8489 0.2724 0.9360 0.041 Uiso 1 1 calc R . . C25 C 1.0309(7) 0.6204(4) 0.4810(3) 0.0422(16) Uani 1 1 d . . . H25 H 1.0554 0.5819 0.4436 0.051 Uiso 1 1 calc R . . C26 C 1.1262(6) 0.6410(4) 0.5179(3) 0.0429(16) Uani 1 1 d . . . H26 H 1.2165 0.6164 0.5056 0.051 Uiso 1 1 calc R . . C27 C 1.0578(5) 0.3467(4) 0.7050(3) 0.0351(14) Uani 1 1 d . . . H27 H 0.9950 0.3095 0.7078 0.042 Uiso 1 1 calc R . . C28 C 0.8778(5) 0.5278(4) 0.8772(2) 0.0253(12) Uani 1 1 d . . . H28 H 0.8864 0.5929 0.8618 0.030 Uiso 1 1 calc R . . C29 C 1.0926(5) 0.6967(4) 0.5723(3) 0.0326(14) Uani 1 1 d . . . H29 H 1.1587 0.7103 0.5978 0.039 Uiso 1 1 calc R . . C30 C 0.3032(5) 0.5590(4) 0.8478(3) 0.0281(13) Uani 1 1 d . . . H30 H 0.2424 0.6072 0.8178 0.034 Uiso 1 1 calc R . . C31 C 0.8777(5) 0.4973(4) 0.9450(3) 0.0317(14) Uani 1 1 d . . . H31 H 0.8840 0.5418 0.9769 0.038 Uiso 1 1 calc R . . C32 C 0.2766(6) 0.8580(4) 0.9693(3) 0.0398(15) Uani 1 1 d . . . H32 H 0.1894 0.8860 0.9852 0.048 Uiso 1 1 calc R . . C33 C 0.8683(5) 0.4014(4) 0.9674(3) 0.0391(15) Uani 1 1 d . . . H33 H 0.8702 0.3795 1.0146 0.047 Uiso 1 1 calc R . . C36 C 0.5350(5) 1.1162(4) 0.6583(3) 0.0286(13) Uani 1 1 d . . . H36 H 0.5783 1.1407 0.6909 0.034 Uiso 1 1 calc R . . C37 C 0.5110(6) 1.1661(4) 0.5944(3) 0.0368(15) Uani 1 1 d . . . H37 H 0.5377 1.2253 0.5823 0.044 Uiso 1 1 calc R . . C38 C 0.4483(6) 1.1303(4) 0.5477(3) 0.0409(16) Uani 1 1 d . . . H38 H 0.4317 1.1650 0.5035 0.049 Uiso 1 1 calc R . . C39 C 0.3577(6) 1.1079(4) 0.8309(3) 0.0408(15) Uani 1 1 d . . . H39 H 0.4305 1.1335 0.8360 0.049 Uiso 1 1 calc R . . C40 C 0.4351(5) 0.9915(4) 0.6289(3) 0.0298(13) Uani 1 1 d . . . H40 H 0.4119 0.9306 0.6406 0.036 Uiso 1 1 calc R . . C41 C 0.8992(6) 0.6562(4) 0.4989(3) 0.0427(16) Uani 1 1 d . . . H41 H 0.8330 0.6428 0.4734 0.051 Uiso 1 1 calc R . . C42 C 0.4088(6) 1.0436(5) 0.5647(3) 0.0418(16) Uani 1 1 d . . . H42 H 0.3638 1.0201 0.5325 0.050 Uiso 1 1 calc R . . F1 F 0.6593(4) 0.5206(3) 0.59314(17) 0.0679(12) Uani 1 1 d . . . F2 F 0.5742(4) 0.6393(3) 0.51812(15) 0.0643(11) Uani 1 1 d . . . O1 O 0.4469(4) 0.6037(3) 0.6923(2) 0.0645(14) Uani 1 1 d . . . F6 F 0.4629(4) 0.5403(3) 0.56119(19) 0.0818(13) Uani 1 1 d . . . O10 O 0.3770(4) 0.7478(3) 0.6074(3) 0.0864(17) Uani 1 1 d . . . C43 C 1.2755(5) 0.3570(4) 0.6800(3) 0.0402(15) Uani 1 1 d . . . H43 H 1.3631 0.3261 0.6658 0.048 Uiso 1 1 calc R . . C44 C 0.9834(6) 1.0977(4) 0.5697(3) 0.0406(16) Uani 1 1 d . . . H44 H 0.9986 1.1589 0.5500 0.049 Uiso 1 1 calc R . . C45 C 0.8459(5) 0.9861(4) 0.5834(2) 0.0289(13) Uani 1 1 d . . . H45 H 0.7665 0.9710 0.5743 0.035 Uiso 1 1 calc R . . C46 C 0.1322(6) 1.1158(5) 0.8509(3) 0.0481(17) Uani 1 1 d . . . H46 H 0.0489 1.1473 0.8699 0.058 Uiso 1 1 calc R . . C47 C 0.8685(6) 1.0753(4) 0.5552(3) 0.0328(14) Uani 1 1 d . . . H47 H 0.8048 1.1216 0.5256 0.039 Uiso 1 1 calc R . . C48 C 0.1465(5) 1.0335(4) 0.8163(3) 0.0394(15) Uani 1 1 d . . . H48 H 0.0734 1.0081 0.8117 0.047 Uiso 1 1 calc R . . C49 C 0.5464(7) 0.5906(5) 0.5742(3) 0.0409(16) Uani 1 1 d . . . F4 F 0.8463(3) 0.7781(3) 0.96463(16) 0.0614(11) Uani 1 1 d . . . F5 F 0.7543(4) 0.9278(3) 0.92005(19) 0.0722(12) Uani 1 1 d . . . F3 F 0.9612(4) 0.8825(4) 0.9448(2) 0.0960(16) Uani 1 1 d . . . C50 C 1.0748(6) 1.0313(4) 0.6126(3) 0.0410(16) Uani 1 1 d . . . H50 H 1.1524 1.0478 0.6234 0.049 Uiso 1 1 calc R . . C51 C 0.2355(7) 1.1529(5) 0.8583(3) 0.0563(19) Uani 1 1 d . . . H51 H 0.2239 1.2102 0.8824 0.068 Uiso 1 1 calc R . . C52 C 0.8663(6) 0.8513(5) 0.9203(3) 0.0495(17) Uani 1 1 d . . . S17 S 0.90618(14) 0.81351(10) 0.83666(7) 0.0285(3) Uani 1 1 d . . . C55 C 1.1869(3) 0.3027(2) 0.68735(14) 0.0443(16) Uani 1 1 d . . . H55 H 1.2145 0.2332 0.6802 0.053 Uiso 1 1 calc R . . C11 C 0.6455(3) 0.2276(2) 0.81797(14) 0.0350(14) Uiso 1 1 d R . . C2 C 0.8087(3) 1.1683(2) 0.73377(14) 0.0403(15) Uiso 1 1 d R . . C12 C 0.6395(3) 1.3312(2) 0.71137(14) 0.0372(15) Uiso 1 1 d R . . C53 C 0.7509(6) 1.1546(4) 0.7968(3) 0.0391(15) Uiso 1 1 d . . . C54 C 0.5869(5) 0.3173(4) 0.7756(3) 0.0341(14) Uiso 1 1 d . . . C56 C 0.7539(6) 1.2587(4) 0.6913(3) 0.0386(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0191(3) 0.0163(3) 0.0285(4) -0.0014(3) 0.0040(3) -0.0008(3) S2 0.0197(8) 0.0214(7) 0.0262(7) 0.0013(6) -0.0004(6) -0.0038(6) S3 0.0186(7) 0.0181(7) 0.0266(8) -0.0013(6) 0.0043(6) -0.0010(6) S4 0.0198(8) 0.0185(7) 0.0311(8) 0.0004(6) -0.0013(6) -0.0025(6) S5 0.0193(7) 0.0166(7) 0.0261(7) -0.0013(6) -0.0003(6) -0.0015(6) S7 0.0260(9) 0.0347(9) 0.0530(10) -0.0188(8) 0.0051(7) -0.0110(7) C10 0.029(3) 0.019(3) 0.032(3) -0.010(3) 0.004(3) -0.001(3) C14 0.034(4) 0.032(3) 0.030(3) -0.003(3) 0.001(3) -0.013(3) O16 0.022(2) 0.034(2) 0.073(3) -0.014(2) -0.007(2) 0.0078(19) O3 0.017(2) 0.0202(19) 0.032(2) -0.0024(16) 0.0089(16) 0.0002(16) O4 0.020(2) 0.0133(18) 0.033(2) 0.0011(16) 0.0029(16) 0.0066(15) O5 0.016(2) 0.0177(19) 0.034(2) 0.0026(16) 0.0014(16) -0.0011(15) O6 0.025(2) 0.0148(19) 0.041(2) -0.0007(17) 0.0035(17) 0.0005(16) O7 0.025(2) 0.036(2) 0.043(2) -0.0085(19) 0.0001(18) -0.0142(18) O8 0.021(2) 0.023(2) 0.034(2) -0.0027(16) -0.0031(16) -0.0061(16) C1 0.027(3) 0.012(3) 0.033(3) -0.003(2) 0.005(3) -0.004(2) O2 0.060(3) 0.030(2) 0.051(3) 0.001(2) 0.007(2) -0.023(2) C7 0.020(3) 0.020(3) 0.017(3) 0.000(2) 0.002(2) 0.003(2) C34 0.022(3) 0.015(3) 0.030(3) 0.005(2) 0.001(2) -0.001(2) C17 0.019(3) 0.020(3) 0.025(3) -0.003(2) 0.003(2) -0.004(2) C19 0.016(3) 0.021(3) 0.026(3) -0.001(2) 0.000(2) -0.003(2) C4 0.020(3) 0.028(3) 0.028(3) -0.004(3) 0.001(2) -0.007(2) C6 0.027(3) 0.028(3) 0.031(3) -0.006(3) 0.005(3) -0.001(3) C9 0.039(4) 0.022(3) 0.029(3) -0.004(3) 0.005(3) -0.003(3) C3 0.032(3) 0.024(3) 0.024(3) 0.002(3) 0.002(2) -0.005(3) C15 0.022(3) 0.014(3) 0.026(3) 0.006(2) 0.002(2) 0.000(2) C8 0.038(4) 0.025(3) 0.033(3) -0.002(3) 0.011(3) -0.010(3) C5 0.019(3) 0.015(3) 0.024(3) -0.008(2) 0.008(2) -0.004(2) C35 0.031(3) 0.027(3) 0.028(3) -0.008(3) 0.003(3) -0.007(3) C13 0.022(3) 0.015(3) 0.021(3) 0.000(2) 0.001(2) -0.001(2) C16 0.031(4) 0.036(4) 0.043(4) 0.002(3) -0.004(3) -0.010(3) C18 0.029(3) 0.021(3) 0.040(3) -0.006(3) 0.007(3) -0.008(3) C20 0.022(3) 0.033(3) 0.043(4) -0.003(3) 0.006(3) -0.012(3) C21 0.064(5) 0.018(3) 0.032(3) -0.005(3) 0.013(3) -0.006(3) C22 0.050(4) 0.031(3) 0.031(3) -0.009(3) 0.005(3) -0.013(3) C23 0.020(3) 0.035(4) 0.056(4) 0.001(3) -0.001(3) -0.008(3) C24 0.037(4) 0.020(3) 0.039(4) 0.004(3) 0.004(3) -0.002(3) C25 0.062(5) 0.026(3) 0.033(4) -0.002(3) 0.009(3) -0.005(3) C26 0.038(4) 0.037(4) 0.041(4) -0.004(3) 0.011(3) 0.007(3) C27 0.026(3) 0.028(3) 0.052(4) -0.014(3) 0.004(3) -0.005(3) C28 0.023(3) 0.021(3) 0.029(3) -0.005(3) -0.004(2) -0.002(2) C29 0.024(3) 0.031(3) 0.034(3) -0.002(3) 0.000(3) 0.004(3) C30 0.025(3) 0.021(3) 0.034(3) 0.001(3) 0.001(3) -0.001(3) C31 0.031(3) 0.035(3) 0.028(3) -0.010(3) -0.002(3) -0.004(3) C32 0.042(4) 0.024(3) 0.045(4) -0.003(3) 0.014(3) 0.001(3) C33 0.039(4) 0.043(4) 0.027(3) 0.003(3) -0.001(3) -0.002(3) C36 0.033(3) 0.019(3) 0.031(3) 0.000(3) -0.005(3) -0.004(3) C37 0.043(4) 0.024(3) 0.038(4) -0.001(3) 0.008(3) -0.005(3) C38 0.037(4) 0.043(4) 0.031(4) 0.008(3) -0.002(3) 0.004(3) C39 0.041(4) 0.031(3) 0.055(4) -0.024(3) 0.008(3) -0.011(3) C40 0.033(3) 0.025(3) 0.030(3) 0.001(3) 0.001(3) -0.008(3) C41 0.054(5) 0.043(4) 0.038(4) -0.002(3) -0.003(3) -0.024(3) C42 0.040(4) 0.056(4) 0.033(4) -0.011(3) -0.012(3) -0.018(3) F1 0.083(3) 0.044(2) 0.060(2) -0.0062(19) 0.022(2) 0.006(2) F2 0.113(3) 0.061(3) 0.028(2) 0.0092(19) -0.001(2) -0.046(2) O1 0.080(3) 0.085(4) 0.057(3) -0.040(3) 0.047(2) -0.062(3) F6 0.112(4) 0.093(3) 0.074(3) -0.048(2) 0.019(2) -0.071(3) O10 0.037(3) 0.056(3) 0.157(5) -0.034(3) -0.029(3) 0.013(2) C43 0.025(3) 0.035(4) 0.053(4) -0.008(3) 0.007(3) 0.004(3) C44 0.053(4) 0.029(3) 0.039(4) -0.006(3) 0.023(3) -0.013(3) C45 0.028(3) 0.022(3) 0.037(3) -0.004(3) 0.004(3) -0.009(3) C46 0.034(4) 0.036(4) 0.061(4) 0.002(3) 0.011(3) 0.007(3) C47 0.038(4) 0.023(3) 0.030(3) 0.003(3) 0.002(3) 0.001(3) C48 0.026(4) 0.029(3) 0.059(4) -0.003(3) 0.005(3) -0.003(3) C49 0.063(5) 0.040(4) 0.028(4) -0.007(3) -0.005(3) -0.027(4) F4 0.057(3) 0.084(3) 0.038(2) -0.002(2) 0.0010(18) -0.014(2) F5 0.081(3) 0.047(2) 0.087(3) -0.041(2) 0.033(2) -0.007(2) F3 0.080(3) 0.160(5) 0.084(3) -0.076(3) 0.011(2) -0.069(3) C50 0.030(4) 0.043(4) 0.059(4) -0.004(3) 0.010(3) -0.026(3) C51 0.060(5) 0.039(4) 0.070(5) -0.035(4) 0.014(4) -0.004(4) C52 0.037(4) 0.066(5) 0.055(4) -0.030(4) 0.011(3) -0.021(4) S17 0.0257(8) 0.0230(8) 0.0365(8) -0.0084(7) 0.0010(6) -0.0044(7) C55 0.039(4) 0.024(3) 0.064(4) -0.018(3) 0.005(3) 0.004(3) _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 Zn1 O4 2.039(3) . ? Zn1 O6 2.049(3) . ? Zn1 O5 2.059(3) . ? Zn1 O3 2.065(3) . ? Zn1 O7 2.126(3) . ? Zn1 O8 2.225(3) . ? S2 O5 1.520(3) . ? S2 C1 1.793(5) . ? S2 C34 1.792(5) . ? S3 O3 1.518(3) . ? S3 C5 1.777(5) . ? S3 C15 1.792(5) . ? S4 O6 1.522(3) . ? S4 C17 1.785(5) . ? S4 C13 1.793(5) . ? S5 O4 1.520(3) . ? S5 C7 1.789(5) . ? S5 C19 1.802(5) . ? S7 O10 1.416(4) . ? S7 O1 1.420(4) . ? S7 O7 1.443(3) . ? S7 C49 1.806(6) . ? C10 C13 1.370(7) . ? C10 C48 1.374(7) . ? C14 C34 1.371(7) . ? C14 C41 1.391(7) . ? O16 S17 1.433(4) . ? O8 S17 1.448(3) . ? C1 C45 1.382(6) . ? C1 C16 1.372(7) . ? O2 S17 1.431(4) . ? C7 C18 1.371(7) . ? C7 C27 1.388(7) . ? C34 C29 1.386(7) . ? C17 C36 1.376(6) . ? C17 C40 1.378(7) . ? C19 C28 1.361(6) . ? C19 C35 1.380(7) . ? C4 C3 1.382(6) . ? C4 C5 1.389(6) . ? C6 C32 1.379(7) . ? C6 C15 1.392(7) . ? C9 C15 1.372(7) . ? C9 C22 1.389(7) . ? C3 C8 1.379(7) . ? C8 C20 1.379(7) . ? C5 C30 1.361(6) . ? C35 C24 1.379(7) . ? C13 C39 1.389(7) . ? C16 C50 1.395(7) . ? C18 C23 1.383(7) . ? C20 C30 1.393(7) . ? C21 C22 1.370(8) . ? C21 C32 1.387(8) . ? C23 C43 1.389(7) . ? C24 C33 1.381(7) . ? C25 C26 1.379(8) . ? C25 C41 1.386(8) . ? C26 C29 1.376(7) . ? C27 C55 1.376(6) . ? C28 C31 1.366(6) . ? C31 C33 1.387(7) . ? C36 C37 1.372(7) . ? C37 C38 1.371(8) . ? C38 C42 1.389(8) . ? C39 C51 1.385(8) . ? C40 C42 1.387(7) . ? F1 C49 1.337(7) . ? F2 C49 1.307(6) . ? F6 C49 1.323(6) . ? C43 C55 1.360(6) . ? C44 C50 1.368(7) . ? C44 C47 1.386(7) . ? C45 C47 1.384(7) . ? C46 C51 1.355(8) . ? C46 C48 1.367(8) . ? F4 C52 1.329(7) . ? F5 C52 1.342(7) . ? F3 C52 1.328(6) . ? C52 S17 1.798(6) . ? C11 C53 1.363(6) 1_545 ? C11 C54 1.412(5) . ? C2 C53 1.393(6) . ? C2 C56 1.413(6) . ? C12 C54 1.392(6) 1_565 ? C12 C56 1.410(6) . ? C53 C11 1.363(6) 1_565 ? C54 C12 1.392(6) 1_545 ? 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 O4 Zn1 O6 174.58(13) . . ? O4 Zn1 O5 90.20(12) . . ? O6 Zn1 O5 93.10(12) . . ? O4 Zn1 O3 90.32(12) . . ? O6 Zn1 O3 86.33(12) . . ? O5 Zn1 O3 179.27(14) . . ? O4 Zn1 O7 93.74(14) . . ? O6 Zn1 O7 90.77(14) . . ? O5 Zn1 O7 86.08(13) . . ? O3 Zn1 O7 94.38(13) . . ? O4 Zn1 O8 86.59(13) . . ? O6 Zn1 O8 89.18(13) . . ? O5 Zn1 O8 89.00(12) . . ? O3 Zn1 O8 90.53(12) . . ? O7 Zn1 O8 175.07(13) . . ? O5 S2 C1 105.3(2) . . ? O5 S2 C34 104.8(2) . . ? C1 S2 C34 98.6(2) . . ? O3 S3 C5 105.4(2) . . ? O3 S3 C15 104.9(2) . . ? C5 S3 C15 99.1(2) . . ? O6 S4 C17 104.8(2) . . ? O6 S4 C13 103.0(2) . . ? C17 S4 C13 98.0(2) . . ? O4 S5 C7 102.9(2) . . ? O4 S5 C19 105.5(2) . . ? C7 S5 C19 99.4(2) . . ? O10 S7 O1 117.2(3) . . ? O10 S7 O7 113.8(3) . . ? O1 S7 O7 114.5(2) . . ? O10 S7 C49 102.7(3) . . ? O1 S7 C49 103.3(3) . . ? O7 S7 C49 102.7(3) . . ? C13 C10 C48 119.3(5) . . ? C34 C14 C41 119.1(5) . . ? S3 O3 Zn1 121.80(18) . . ? S5 O4 Zn1 128.4(2) . . ? S2 O5 Zn1 122.30(17) . . ? S4 O6 Zn1 125.6(2) . . ? S7 O7 Zn1 141.3(2) . . ? S17 O8 Zn1 145.0(2) . . ? C45 C1 C16 122.4(5) . . ? C45 C1 S2 119.9(4) . . ? C16 C1 S2 117.7(4) . . ? C18 C7 C27 121.7(5) . . ? C18 C7 S5 119.1(4) . . ? C27 C7 S5 119.2(4) . . ? C14 C34 C29 121.6(5) . . ? C14 C34 S2 120.1(4) . . ? C29 C34 S2 118.2(4) . . ? C36 C17 C40 121.9(5) . . ? C36 C17 S4 118.1(4) . . ? C40 C17 S4 120.0(4) . . ? C28 C19 C35 121.4(5) . . ? C28 C19 S5 120.8(4) . . ? C35 C19 S5 117.8(4) . . ? C3 C4 C5 119.0(5) . . ? C32 C6 C15 118.3(5) . . ? C15 C9 C22 119.2(5) . . ? C8 C3 C4 120.1(5) . . ? C9 C15 C6 121.8(5) . . ? C9 C15 S3 119.8(4) . . ? C6 C15 S3 118.0(4) . . ? C3 C8 C20 120.8(5) . . ? C30 C5 C4 120.9(5) . . ? C30 C5 S3 118.0(4) . . ? C4 C5 S3 121.1(4) . . ? C24 C35 C19 118.9(5) . . ? C10 C13 C39 120.9(5) . . ? C10 C13 S4 120.7(4) . . ? C39 C13 S4 118.4(4) . . ? C1 C16 C50 118.0(5) . . ? C7 C18 C23 119.1(5) . . ? C8 C20 C30 118.9(5) . . ? C22 C21 C32 120.8(6) . . ? C21 C22 C9 119.7(6) . . ? C18 C23 C43 119.5(5) . . ? C35 C24 C33 120.2(5) . . ? C26 C25 C41 119.6(6) . . ? C29 C26 C25 121.0(5) . . ? C55 C27 C7 118.1(5) . . ? C19 C28 C31 119.8(5) . . ? C34 C29 C26 118.7(5) . . ? C5 C30 C20 120.3(5) . . ? C28 C31 C33 120.1(5) . . ? C21 C32 C6 120.2(5) . . ? C24 C33 C31 119.6(5) . . ? C17 C36 C37 119.4(5) . . ? C38 C37 C36 119.9(5) . . ? C37 C38 C42 120.5(5) . . ? C13 C39 C51 118.4(6) . . ? C17 C40 C42 118.2(5) . . ? C25 C41 C14 120.1(6) . . ? C38 C42 C40 120.0(5) . . ? C55 C43 C23 120.4(5) . . ? C50 C44 C47 119.8(5) . . ? C1 C45 C47 118.3(5) . . ? C51 C46 C48 120.8(6) . . ? C45 C47 C44 120.5(5) . . ? C46 C48 C10 120.2(6) . . ? F2 C49 F1 105.4(5) . . ? F2 C49 F6 109.6(5) . . ? F1 C49 F6 106.1(5) . . ? F2 C49 S7 113.9(4) . . ? F1 C49 S7 111.3(4) . . ? F6 C49 S7 110.2(4) . . ? C44 C50 C16 121.0(6) . . ? C46 C51 C39 120.4(6) . . ? F3 C52 F4 107.7(6) . . ? F3 C52 F5 107.4(6) . . ? F4 C52 F5 105.5(5) . . ? F3 C52 S17 111.4(4) . . ? F4 C52 S17 113.4(5) . . ? F5 C52 S17 111.2(5) . . ? O16 S17 O2 116.6(3) . . ? O16 S17 O8 114.3(2) . . ? O2 S17 O8 115.0(2) . . ? O16 S17 C52 102.6(3) . . ? O2 S17 C52 104.0(3) . . ? O8 S17 C52 101.4(2) . . ? C43 C55 C27 121.1(4) . . ? C53 C11 C54 121.4(4) 1_545 . ? C53 C2 C56 118.6(4) . . ? C54 C12 C56 119.6(3) 1_565 . ? C11 C53 C2 120.9(4) 1_565 . ? C12 C54 C11 118.9(4) 1_545 . ? C2 C56 C12 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.559 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.074