# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mx983 #TrackingRef '19825_web_deposit_cif_file_0_WeiXu_1366877472.mx983.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 S4' _chemical_formula_sum 'C36 H26 S4' _chemical_formula_weight 586.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.262(3) _cell_length_b 9.148(5) _cell_length_c 11.131(5) _cell_angle_alpha 102.635(8) _cell_angle_beta 94.961(7) _cell_angle_gamma 106.756(5) _cell_volume 682.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2524 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.47 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 306 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9220 _exptl_absorpt_correction_T_max 0.9888 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6509 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3105 _reflns_number_gt 2888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and 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^)+(0.0638P)^2^+0.3724P] 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 3105 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 S1 S 0.13085(6) 0.31345(5) 0.47879(4) 0.02111(15) Uani 1 1 d . . . S2 S 0.23825(6) 0.64082(5) 0.65208(4) 0.02181(15) Uani 1 1 d . . . C1 C 0.9998(3) 0.2635(3) 0.98348(19) 0.0285(4) Uani 1 1 d . . . H1A H 1.1289 0.2882 0.9582 0.043 Uiso 1 1 calc R . . H1B H 0.9470 0.1495 0.9743 0.043 Uiso 1 1 calc R . . H1C H 1.0107 0.3199 1.0708 0.043 Uiso 1 1 calc R . . C2 C 0.8655(3) 0.3140(2) 0.90210(17) 0.0218(4) Uani 1 1 d . . . C3 C 0.6930(3) 0.3320(2) 0.93982(17) 0.0253(4) Uani 1 1 d . . . H3A H 0.6624 0.3147 1.0179 0.030 Uiso 1 1 calc R . . C4 C 0.5661(3) 0.3749(2) 0.86468(17) 0.0244(4) Uani 1 1 d . . . H4A H 0.4503 0.3876 0.8926 0.029 Uiso 1 1 calc R . . C5 C 0.6050(3) 0.3998(2) 0.74891(17) 0.0202(4) Uani 1 1 d . . . C6 C 0.7788(3) 0.3846(2) 0.71198(17) 0.0220(4) Uani 1 1 d . . . H6A H 0.8098 0.4024 0.6341 0.026 Uiso 1 1 calc R . . C7 C 0.9078(3) 0.3435(2) 0.78876(17) 0.0225(4) Uani 1 1 d . . . H7A H 1.0266 0.3355 0.7629 0.027 Uiso 1 1 calc R . . C8 C 0.4549(3) 0.4357(2) 0.66898(17) 0.0201(4) Uani 1 1 d . . . C9 C 0.3385(3) 0.3101(2) 0.56975(17) 0.0211(4) Uani 1 1 d . . . C10 C 0.3655(3) 0.1620(2) 0.52772(18) 0.0256(4) Uani 1 1 d . . . H10A H 0.4691 0.1343 0.5648 0.031 Uiso 1 1 calc R . . C11 C 0.2290(3) 0.0608(2) 0.42831(19) 0.0273(4) Uani 1 1 d . . . H11A H 0.2326 -0.0416 0.3898 0.033 Uiso 1 1 calc R . . C12 C 0.0833(3) 0.1214(2) 0.38832(17) 0.0227(4) Uani 1 1 d . . . C13 C -0.0738(3) 0.0306(2) 0.29332(18) 0.0259(4) Uani 1 1 d . . . H13A H -0.0612 -0.0693 0.2565 0.031 Uiso 1 1 calc R . . C14 C 0.4346(3) 0.5862(2) 0.70700(17) 0.0211(4) Uani 1 1 d . . . C15 C 0.5679(3) 0.7174(2) 0.79531(17) 0.0237(4) Uani 1 1 d . . . H15A H 0.6863 0.7140 0.8362 0.028 Uiso 1 1 calc R . . C16 C 0.5111(3) 0.8502(2) 0.81679(18) 0.0250(4) Uani 1 1 d . . . H16A H 0.5877 0.9468 0.8737 0.030 Uiso 1 1 calc R . . C17 C 0.3302(3) 0.8321(2) 0.74781(17) 0.0222(4) Uani 1 1 d . . . C18 C 0.2429(3) 0.9517(2) 0.76113(18) 0.0260(4) Uani 1 1 d . . . H18A H 0.3185 1.0440 0.8231 0.031 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 S1 0.0211(2) 0.0203(2) 0.0224(2) 0.00361(17) -0.00210(17) 0.01012(18) S2 0.0200(2) 0.0197(2) 0.0250(2) 0.00335(18) -0.00258(18) 0.00881(18) C1 0.0295(10) 0.0303(10) 0.0281(10) 0.0096(8) -0.0033(8) 0.0137(8) C2 0.0226(9) 0.0181(8) 0.0234(9) 0.0056(7) -0.0035(7) 0.0063(7) C3 0.0280(10) 0.0295(10) 0.0202(8) 0.0100(7) 0.0043(7) 0.0092(8) C4 0.0207(9) 0.0302(10) 0.0248(9) 0.0089(8) 0.0054(7) 0.0101(8) C5 0.0190(8) 0.0185(8) 0.0231(8) 0.0065(7) -0.0004(7) 0.0064(7) C6 0.0237(9) 0.0250(9) 0.0202(8) 0.0087(7) 0.0024(7) 0.0102(7) C7 0.0225(9) 0.0238(9) 0.0233(9) 0.0065(7) 0.0028(7) 0.0105(7) C8 0.0179(8) 0.0242(9) 0.0213(8) 0.0083(7) 0.0029(7) 0.0095(7) C9 0.0196(9) 0.0263(9) 0.0211(8) 0.0090(7) 0.0026(7) 0.0107(7) C10 0.0246(9) 0.0263(10) 0.0291(10) 0.0071(8) -0.0007(7) 0.0142(8) C11 0.0288(10) 0.0238(9) 0.0298(10) 0.0028(8) 0.0001(8) 0.0135(8) C12 0.0253(9) 0.0212(9) 0.0232(9) 0.0046(7) 0.0034(7) 0.0108(7) C13 0.0324(11) 0.0185(9) 0.0271(9) 0.0025(7) 0.0003(8) 0.0121(8) C14 0.0191(8) 0.0242(9) 0.0218(8) 0.0080(7) 0.0023(7) 0.0084(7) C15 0.0195(9) 0.0264(10) 0.0249(9) 0.0087(7) -0.0006(7) 0.0064(7) C16 0.0244(9) 0.0229(9) 0.0249(9) 0.0054(7) -0.0015(7) 0.0053(7) C17 0.0229(9) 0.0200(9) 0.0234(9) 0.0061(7) 0.0011(7) 0.0068(7) C18 0.0288(10) 0.0189(9) 0.0272(9) 0.0024(7) -0.0022(8) 0.0073(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 S1 C12 1.743(2) . ? S1 C9 1.7539(19) . ? S2 C17 1.741(2) . ? S2 C14 1.747(2) . ? C1 C2 1.508(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.388(3) . ? C2 C3 1.397(3) . ? C3 C4 1.386(3) . ? C3 H3A 0.9500 . ? C4 C5 1.395(3) . ? C4 H4A 0.9500 . ? C5 C6 1.395(3) . ? C5 C8 1.502(2) . ? C6 C7 1.398(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C14 1.404(3) . ? C8 C9 1.406(3) . ? C9 C10 1.409(3) . ? C10 C11 1.377(3) . ? C10 H10A 0.9500 . ? C11 C12 1.411(3) . ? C11 H11A 0.9500 . ? C12 C13 1.404(3) . ? C13 C18 1.389(3) 2_566 ? C13 H13A 0.9500 . ? C14 C15 1.411(3) . ? C15 C16 1.372(3) . ? C15 H15A 0.9500 . ? C16 C17 1.410(3) . ? C16 H16A 0.9500 . ? C17 C18 1.402(3) . ? C18 C13 1.389(3) 2_566 ? C18 H18A 0.9500 . ? 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 C12 S1 C9 93.41(9) . . ? C17 S2 C14 93.35(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 118.11(17) . . ? C7 C2 C1 121.75(18) . . ? C3 C2 C1 120.13(18) . . ? C4 C3 C2 120.76(18) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 121.29(18) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C4 C5 C6 118.06(17) . . ? C4 C5 C8 118.34(16) . . ? C6 C5 C8 123.56(17) . . ? C5 C6 C7 120.47(17) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C2 C7 C6 121.25(18) . . ? C2 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C14 C8 C9 126.79(17) . . ? C14 C8 C5 116.76(16) . . ? C9 C8 C5 116.22(16) . . ? C8 C9 C10 126.62(17) . . ? C8 C9 S1 124.61(14) . . ? C10 C9 S1 108.77(14) . . ? C11 C10 C9 114.33(17) . . ? C11 C10 H10A 122.8 . . ? C9 C10 H10A 122.8 . . ? C10 C11 C12 114.58(18) . . ? C10 C11 H11A 122.7 . . ? C12 C11 H11A 122.7 . . ? C13 C12 C11 122.14(18) . . ? C13 C12 S1 128.92(15) . . ? C11 C12 S1 108.89(14) . . ? C18 C13 C12 136.84(18) 2_566 . ? C18 C13 H13A 111.6 2_566 . ? C12 C13 H13A 111.6 . . ? C8 C14 C15 125.94(17) . . ? C8 C14 S2 125.07(14) . . ? C15 C14 S2 109.00(14) . . ? C16 C15 C14 114.04(18) . . ? C16 C15 H15A 123.0 . . ? C14 C15 H15A 123.0 . . ? C15 C16 C17 114.77(18) . . ? C15 C16 H16A 122.6 . . ? C17 C16 H16A 122.6 . . ? C18 C17 C16 123.34(18) . . ? C18 C17 S2 127.81(15) . . ? C16 C17 S2 108.82(14) . . ? C13 C18 C17 136.14(18) 2_566 . ? C13 C18 H18A 111.9 2_566 . ? C17 C18 H18A 111.9 . . ? 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 C7 C2 C3 C4 1.3(3) . . . . ? C1 C2 C3 C4 -178.52(18) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C6 -1.8(3) . . . . ? C3 C4 C5 C8 176.09(18) . . . . ? C4 C5 C6 C7 0.9(3) . . . . ? C8 C5 C6 C7 -176.86(17) . . . . ? C3 C2 C7 C6 -2.2(3) . . . . ? C1 C2 C7 C6 177.63(17) . . . . ? C5 C6 C7 C2 1.1(3) . . . . ? C4 C5 C8 C14 72.8(2) . . . . ? C6 C5 C8 C14 -109.4(2) . . . . ? C4 C5 C8 C9 -102.1(2) . . . . ? C6 C5 C8 C9 75.7(2) . . . . ? C14 C8 C9 C10 176.39(18) . . . . ? C5 C8 C9 C10 -9.3(3) . . . . ? C14 C8 C9 S1 -4.5(3) . . . . ? C5 C8 C9 S1 169.81(13) . . . . ? C12 S1 C9 C8 -179.02(17) . . . . ? C12 S1 C9 C10 0.21(15) . . . . ? C8 C9 C10 C11 179.97(18) . . . . ? S1 C9 C10 C11 0.8(2) . . . . ? C9 C10 C11 C12 -1.7(3) . . . . ? C10 C11 C12 C13 -176.01(19) . . . . ? C10 C11 C12 S1 1.7(2) . . . . ? C9 S1 C12 C13 176.47(19) . . . . ? C9 S1 C12 C11 -1.07(15) . . . . ? C11 C12 C13 C18 174.7(2) . . . 2_566 ? S1 C12 C13 C18 -2.5(4) . . . 2_566 ? C9 C8 C14 C15 -170.75(18) . . . . ? C5 C8 C14 C15 14.9(3) . . . . ? C9 C8 C14 S2 9.4(3) . . . . ? C5 C8 C14 S2 -164.86(14) . . . . ? C17 S2 C14 C8 178.51(17) . . . . ? C17 S2 C14 C15 -1.32(14) . . . . ? C8 C14 C15 C16 -179.04(18) . . . . ? S2 C14 C15 C16 0.8(2) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C15 C16 C17 C18 176.83(19) . . . . ? C15 C16 C17 S2 -1.3(2) . . . . ? C14 S2 C17 C18 -176.55(19) . . . . ? C14 S2 C17 C16 1.51(15) . . . . ? C16 C17 C18 C13 178.6(2) . . . 2_566 ? S2 C17 C18 C13 -3.6(4) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.380 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 936012' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mx974 #TrackingRef 'web_deposit_cif_file_1_WeiXu_1366877472.mx974.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H20 Cl2 S4' _chemical_formula_sum 'C34 H20 Cl2 S4' _chemical_formula_weight 627.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 11.102(3) _cell_length_b 11.949(3) _cell_length_c 12.195(3) _cell_angle_alpha 108.950(2) _cell_angle_beta 112.420(2) _cell_angle_gamma 95.820(2) _cell_volume 1366.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4702 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9195 _exptl_absorpt_correction_T_max 0.9721 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15405 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6247 _reflns_number_gt 5627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and 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^)+(0.0455P)^2^+0.5036P] 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 6247 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 Cl1 Cl 1.08843(6) -0.43957(6) 0.42273(5) 0.03705(15) Uani 1 1 d . . . Cl2 Cl -0.29692(5) 0.45209(5) -0.10630(5) 0.03279(14) Uani 1 1 d . . . S1 S 0.25924(5) 0.01069(5) -0.01880(5) 0.02283(12) Uani 1 1 d . . . S2 S 0.46438(5) -0.13919(5) 0.07090(5) 0.02304(12) Uani 1 1 d . . . S3 S 0.57284(5) 0.04091(5) 0.34932(4) 0.02214(12) Uani 1 1 d . . . S4 S 0.33802(5) 0.16676(5) 0.26280(5) 0.02303(12) Uani 1 1 d . . . C1 C 0.13067(19) 0.0864(2) -0.03947(19) 0.0224(4) Uani 1 1 d . . . C2 C 0.0286(2) 0.0253(2) -0.1677(2) 0.0287(5) Uani 1 1 d . . . H2A H -0.0525 0.0494 -0.1993 0.034 Uiso 1 1 calc R . . C3 C 0.0568(2) -0.0710(2) -0.2421(2) 0.0277(5) Uani 1 1 d . . . H3A H -0.0025 -0.1186 -0.3304 0.033 Uiso 1 1 calc R . . C4 C 0.1807(2) -0.0945(2) -0.17803(18) 0.0229(4) Uani 1 1 d . . . C5 C 0.2269(2) -0.1890(2) -0.24015(19) 0.0244(4) Uani 1 1 d . . . H5A H 0.1706 -0.2271 -0.3304 0.029 Uiso 1 1 calc R . . C6 C 0.3336(2) -0.24062(19) -0.20319(19) 0.0237(4) Uani 1 1 d . . . H6A H 0.3406 -0.2959 -0.2754 0.028 Uiso 1 1 calc R . . C7 C 0.4348(2) -0.23185(19) -0.08521(18) 0.0221(4) Uani 1 1 d . . . C8 C 0.5267(2) -0.3044(2) -0.07871(19) 0.0250(4) Uani 1 1 d . . . H8A H 0.5277 -0.3617 -0.1534 0.030 Uiso 1 1 calc R . . C9 C 0.6153(2) -0.2862(2) 0.0444(2) 0.0248(4) Uani 1 1 d . . . H9A H 0.6828 -0.3294 0.0622 0.030 Uiso 1 1 calc R . . C10 C 0.5972(2) -0.19771(19) 0.14184(19) 0.0222(4) Uani 1 1 d . . . C11 C 0.67396(19) -0.16103(19) 0.27605(19) 0.0213(4) Uani 1 1 d . . . C12 C 0.66506(19) -0.06603(19) 0.37411(19) 0.0208(4) Uani 1 1 d . . . C13 C 0.72741(19) -0.0408(2) 0.50790(19) 0.0232(4) Uani 1 1 d . . . H13A H 0.7831 -0.0877 0.5429 0.028 Uiso 1 1 calc R . . C14 C 0.70028(19) 0.0570(2) 0.58215(19) 0.0229(4) Uani 1 1 d . . . H14A H 0.7358 0.0837 0.6733 0.028 Uiso 1 1 calc R . . C15 C 0.61551(19) 0.11486(19) 0.51289(18) 0.0211(4) Uani 1 1 d . . . C16 C 0.5819(2) 0.2200(2) 0.57320(19) 0.0238(4) Uani 1 1 d . . . H16A H 0.6242 0.2474 0.6646 0.029 Uiso 1 1 calc R . . C17 C 0.5021(2) 0.2939(2) 0.53219(19) 0.0242(4) Uani 1 1 d . . . H17A H 0.5160 0.3672 0.6018 0.029 Uiso 1 1 calc R . . C18 C 0.4059(2) 0.28767(19) 0.41375(19) 0.0233(4) Uani 1 1 d . . . C19 C 0.3428(2) 0.3826(2) 0.4022(2) 0.0270(4) Uani 1 1 d . . . H19A H 0.3642 0.4571 0.4737 0.032 Uiso 1 1 calc R . . C20 C 0.2481(2) 0.3594(2) 0.2800(2) 0.0251(4) Uani 1 1 d . . . H20A H 0.1999 0.4168 0.2595 0.030 Uiso 1 1 calc R . . C21 C 0.22841(19) 0.2428(2) 0.18750(19) 0.0218(4) Uani 1 1 d . . . C22 C 0.13437(19) 0.19365(19) 0.05626(19) 0.0214(4) Uani 1 1 d . . . C23 C 0.7759(2) -0.2296(2) 0.31732(18) 0.0217(4) Uani 1 1 d . . . C24 C 0.7377(2) -0.3526(2) 0.2947(2) 0.0293(5) Uani 1 1 d . . . H24A H 0.6446 -0.3933 0.2551 0.035 Uiso 1 1 calc R . . C25 C 0.8334(2) -0.4172(2) 0.3290(2) 0.0311(5) Uani 1 1 d . . . H25A H 0.8063 -0.5009 0.3140 0.037 Uiso 1 1 calc R . . C26 C 0.9680(2) -0.3579(2) 0.38518(19) 0.0258(5) Uani 1 1 d . . . C27 C 1.0099(2) -0.2357(2) 0.41001(19) 0.0250(4) Uani 1 1 d . . . H27A H 1.1031 -0.1957 0.4496 0.030 Uiso 1 1 calc R . . C28 C 0.9133(2) -0.1725(2) 0.37610(18) 0.0240(4) Uani 1 1 d . . . H28A H 0.9414 -0.0883 0.3933 0.029 Uiso 1 1 calc R . . C29 C 0.02979(19) 0.25963(19) 0.01558(19) 0.0212(4) Uani 1 1 d . . . C30 C -0.0476(2) 0.2904(2) 0.0826(2) 0.0254(4) Uani 1 1 d . . . H30A H -0.0316 0.2700 0.1551 0.031 Uiso 1 1 calc R . . C31 C -0.1468(2) 0.3497(2) 0.0459(2) 0.0262(4) Uani 1 1 d . . . H31A H -0.1989 0.3697 0.0923 0.031 Uiso 1 1 calc R . . C32 C -0.16920(19) 0.37952(19) -0.05946(19) 0.0233(4) Uani 1 1 d . . . C33 C -0.0932(2) 0.35335(19) -0.12699(18) 0.0229(4) Uani 1 1 d . . . H33A H -0.1089 0.3756 -0.1983 0.027 Uiso 1 1 calc R . . C34 C 0.0064(2) 0.29394(19) -0.08888(18) 0.0222(4) Uani 1 1 d . . . H34A H 0.0597 0.2762 -0.1344 0.027 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 Cl1 0.0434(3) 0.0441(4) 0.0350(3) 0.0209(3) 0.0190(3) 0.0322(3) Cl2 0.0301(3) 0.0320(3) 0.0292(3) 0.0076(2) 0.0070(2) 0.0193(2) S1 0.0221(3) 0.0219(3) 0.0186(2) 0.0058(2) 0.00424(19) 0.0091(2) S2 0.0237(3) 0.0252(3) 0.0182(2) 0.0071(2) 0.00697(19) 0.0119(2) S3 0.0252(3) 0.0240(3) 0.0183(2) 0.0093(2) 0.00844(19) 0.0122(2) S4 0.0254(3) 0.0216(3) 0.0175(2) 0.0068(2) 0.00445(19) 0.0103(2) C1 0.0212(10) 0.0234(11) 0.0225(10) 0.0113(9) 0.0069(8) 0.0091(8) C2 0.0226(10) 0.0286(12) 0.0260(10) 0.0096(9) 0.0024(8) 0.0085(9) C3 0.0272(11) 0.0259(12) 0.0197(10) 0.0073(9) 0.0015(8) 0.0065(9) C4 0.0247(10) 0.0231(11) 0.0184(9) 0.0097(8) 0.0059(8) 0.0054(8) C5 0.0279(11) 0.0253(11) 0.0165(9) 0.0094(8) 0.0057(8) 0.0054(9) C6 0.0300(11) 0.0208(11) 0.0176(9) 0.0047(8) 0.0102(8) 0.0055(9) C7 0.0239(10) 0.0197(10) 0.0193(9) 0.0054(8) 0.0087(8) 0.0035(8) C8 0.0279(11) 0.0210(11) 0.0234(10) 0.0051(8) 0.0116(8) 0.0069(9) C9 0.0239(10) 0.0219(11) 0.0279(10) 0.0093(9) 0.0105(9) 0.0088(9) C10 0.0208(10) 0.0214(11) 0.0240(10) 0.0094(8) 0.0084(8) 0.0082(8) C11 0.0204(9) 0.0200(10) 0.0262(10) 0.0115(8) 0.0103(8) 0.0084(8) C12 0.0187(9) 0.0223(10) 0.0233(9) 0.0123(8) 0.0078(8) 0.0079(8) C13 0.0205(10) 0.0253(11) 0.0227(10) 0.0120(9) 0.0058(8) 0.0075(8) C14 0.0194(10) 0.0278(11) 0.0179(9) 0.0089(8) 0.0047(8) 0.0061(8) C15 0.0202(9) 0.0219(10) 0.0171(9) 0.0062(8) 0.0056(7) 0.0045(8) C16 0.0225(10) 0.0258(11) 0.0161(9) 0.0051(8) 0.0041(8) 0.0057(9) C17 0.0247(10) 0.0229(11) 0.0196(9) 0.0046(8) 0.0072(8) 0.0072(9) C18 0.0252(10) 0.0220(11) 0.0192(9) 0.0053(8) 0.0084(8) 0.0072(9) C19 0.0295(11) 0.0226(11) 0.0244(10) 0.0056(9) 0.0098(9) 0.0090(9) C20 0.0273(11) 0.0245(11) 0.0262(10) 0.0123(9) 0.0110(8) 0.0131(9) C21 0.0192(9) 0.0250(11) 0.0229(10) 0.0118(9) 0.0081(8) 0.0092(8) C22 0.0200(9) 0.0243(11) 0.0228(9) 0.0119(8) 0.0091(8) 0.0095(8) C23 0.0234(10) 0.0236(11) 0.0191(9) 0.0092(8) 0.0086(8) 0.0103(8) C24 0.0249(11) 0.0242(12) 0.0346(12) 0.0114(10) 0.0094(9) 0.0047(9) C25 0.0359(12) 0.0232(12) 0.0338(12) 0.0128(10) 0.0127(10) 0.0107(10) C26 0.0310(11) 0.0328(12) 0.0219(10) 0.0143(9) 0.0139(9) 0.0203(10) C27 0.0238(10) 0.0328(12) 0.0217(9) 0.0134(9) 0.0104(8) 0.0107(9) C28 0.0259(10) 0.0250(11) 0.0214(9) 0.0102(9) 0.0094(8) 0.0084(9) C29 0.0195(9) 0.0210(10) 0.0209(9) 0.0084(8) 0.0064(8) 0.0062(8) C30 0.0221(10) 0.0313(12) 0.0254(10) 0.0144(9) 0.0102(8) 0.0074(9) C31 0.0239(10) 0.0308(12) 0.0251(10) 0.0100(9) 0.0125(8) 0.0088(9) C32 0.0204(10) 0.0209(11) 0.0223(10) 0.0061(8) 0.0041(8) 0.0100(8) C33 0.0248(10) 0.0244(11) 0.0190(9) 0.0097(8) 0.0080(8) 0.0085(8) C34 0.0234(10) 0.0241(11) 0.0198(9) 0.0085(8) 0.0096(8) 0.0085(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 Cl1 C26 1.743(2) . ? Cl2 C32 1.744(2) . ? S1 C4 1.735(2) . ? S1 C1 1.748(2) . ? S2 C7 1.743(2) . ? S2 C10 1.744(2) . ? S3 C15 1.742(2) . ? S3 C12 1.747(2) . ? S4 C18 1.743(2) . ? S4 C21 1.751(2) . ? C1 C22 1.410(3) . ? C1 C2 1.415(3) . ? C2 C3 1.363(3) . ? C2 H2A 0.9500 . ? C3 C4 1.408(3) . ? C3 H3A 0.9500 . ? C4 C5 1.404(3) . ? C5 C6 1.381(3) . ? C5 H5A 0.9500 . ? C6 C7 1.410(3) . ? C6 H6A 0.9500 . ? C7 C8 1.401(3) . ? C8 C9 1.373(3) . ? C8 H8A 0.9500 . ? C9 C10 1.407(3) . ? C9 H9A 0.9500 . ? C10 C11 1.411(3) . ? C11 C12 1.400(3) . ? C11 C23 1.493(3) . ? C12 C13 1.417(3) . ? C13 C14 1.367(3) . ? C13 H13A 0.9500 . ? C14 C15 1.408(3) . ? C14 H14A 0.9500 . ? C15 C16 1.401(3) . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.404(3) . ? C17 H17A 0.9500 . ? C18 C19 1.410(3) . ? C19 C20 1.371(3) . ? C19 H19A 0.9500 . ? C20 C21 1.411(3) . ? C20 H20A 0.9500 . ? C21 C22 1.410(3) . ? C22 C29 1.489(3) . ? C23 C24 1.392(3) . ? C23 C28 1.395(3) . ? C24 C25 1.391(3) . ? C24 H24A 0.9500 . ? C25 C26 1.376(3) . ? C25 H25A 0.9500 . ? C26 C27 1.381(3) . ? C27 C28 1.385(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.394(3) . ? C29 C34 1.402(3) . ? C30 C31 1.381(3) . ? C30 H30A 0.9500 . ? C31 C32 1.382(3) . ? C31 H31A 0.9500 . ? C32 C33 1.380(3) . ? C33 C34 1.387(3) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? 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 C4 S1 C1 93.37(10) . . ? C7 S2 C10 92.96(10) . . ? C15 S3 C12 93.09(9) . . ? C18 S4 C21 93.36(10) . . ? C22 C1 C2 127.00(19) . . ? C22 C1 S1 124.32(15) . . ? C2 C1 S1 108.62(16) . . ? C3 C2 C1 114.17(19) . . ? C3 C2 H2A 122.9 . . ? C1 C2 H2A 122.9 . . ? C2 C3 C4 114.88(19) . . ? C2 C3 H3A 122.6 . . ? C4 C3 H3A 122.6 . . ? C5 C4 C3 122.62(19) . . ? C5 C4 S1 128.45(15) . . ? C3 C4 S1 108.93(16) . . ? C6 C5 C4 136.14(19) . . ? C6 C5 H5A 111.9 . . ? C4 C5 H5A 111.9 . . ? C5 C6 C7 136.05(19) . . ? C5 C6 H6A 112.0 . . ? C7 C6 H6A 112.0 . . ? C8 C7 C6 122.67(18) . . ? C8 C7 S2 109.21(14) . . ? C6 C7 S2 128.08(16) . . ? C9 C8 C7 114.59(19) . . ? C9 C8 H8A 122.7 . . ? C7 C8 H8A 122.7 . . ? C8 C9 C10 113.98(19) . . ? C8 C9 H9A 123.0 . . ? C10 C9 H9A 123.0 . . ? C9 C10 C11 125.83(19) . . ? C9 C10 S2 109.26(15) . . ? C11 C10 S2 124.91(16) . . ? C12 C11 C10 126.54(18) . . ? C12 C11 C23 116.84(17) . . ? C10 C11 C23 116.62(18) . . ? C11 C12 C13 126.33(18) . . ? C11 C12 S3 124.68(15) . . ? C13 C12 S3 108.99(15) . . ? C14 C13 C12 114.03(18) . . ? C14 C13 H13A 123.0 . . ? C12 C13 H13A 123.0 . . ? C13 C14 C15 114.71(18) . . ? C13 C14 H14A 122.6 . . ? C15 C14 H14A 122.6 . . ? C16 C15 C14 122.80(18) . . ? C16 C15 S3 127.91(15) . . ? C14 C15 S3 109.17(15) . . ? C17 C16 C15 135.64(19) . . ? C17 C16 H16A 112.2 . . ? C15 C16 H16A 112.2 . . ? C16 C17 C18 136.1(2) . . ? C16 C17 H17A 111.9 . . ? C18 C17 H17A 111.9 . . ? C17 C18 C19 122.77(19) . . ? C17 C18 S4 128.44(17) . . ? C19 C18 S4 108.72(15) . . ? C20 C19 C18 114.92(19) . . ? C20 C19 H19A 122.5 . . ? C18 C19 H19A 122.5 . . ? C19 C20 C21 114.11(19) . . ? C19 C20 H20A 122.9 . . ? C21 C20 H20A 122.9 . . ? C22 C21 C20 126.04(19) . . ? C22 C21 S4 125.08(16) . . ? C20 C21 S4 108.87(14) . . ? C21 C22 C1 125.27(18) . . ? C21 C22 C29 117.41(18) . . ? C1 C22 C29 117.32(17) . . ? C24 C23 C28 118.04(19) . . ? C24 C23 C11 121.54(18) . . ? C28 C23 C11 120.38(19) . . ? C25 C24 C23 121.2(2) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C26 C25 C24 119.0(2) . . ? C26 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? C25 C26 C27 121.49(19) . . ? C25 C26 Cl1 119.30(18) . . ? C27 C26 Cl1 119.20(17) . . ? C26 C27 C28 118.82(19) . . ? C26 C27 H27A 120.6 . . ? C28 C27 H27A 120.6 . . ? C27 C28 C23 121.5(2) . . ? C27 C28 H28A 119.3 . . ? C23 C28 H28A 119.3 . . ? C30 C29 C34 117.90(18) . . ? C30 C29 C22 120.15(17) . . ? C34 C29 C22 121.95(17) . . ? C31 C30 C29 121.49(19) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 118.99(19) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C33 C32 C31 121.57(18) . . ? C33 C32 Cl2 120.01(15) . . ? C31 C32 Cl2 118.42(16) . . ? C32 C33 C34 118.84(18) . . ? C32 C33 H33A 120.6 . . ? C34 C33 H33A 120.6 . . ? C33 C34 C29 121.18(18) . . ? C33 C34 H34A 119.4 . . ? C29 C34 H34A 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 S1 C1 C22 -175.31(19) . . . . ? C4 S1 C1 C2 2.04(17) . . . . ? C22 C1 C2 C3 175.0(2) . . . . ? S1 C1 C2 C3 -2.2(2) . . . . ? C1 C2 C3 C4 1.2(3) . . . . ? C2 C3 C4 C5 -179.1(2) . . . . ? C2 C3 C4 S1 0.4(3) . . . . ? C1 S1 C4 C5 178.0(2) . . . . ? C1 S1 C4 C3 -1.40(17) . . . . ? C3 C4 C5 C6 -173.1(2) . . . . ? S1 C4 C5 C6 7.6(4) . . . . ? C4 C5 C6 C7 9.4(5) . . . . ? C5 C6 C7 C8 175.4(2) . . . . ? C5 C6 C7 S2 -2.0(4) . . . . ? C10 S2 C7 C8 0.00(16) . . . . ? C10 S2 C7 C6 177.7(2) . . . . ? C6 C7 C8 C9 -178.0(2) . . . . ? S2 C7 C8 C9 -0.1(2) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 -179.9(2) . . . . ? C8 C9 C10 S2 -0.2(2) . . . . ? C7 S2 C10 C9 0.09(16) . . . . ? C7 S2 C10 C11 179.86(19) . . . . ? C9 C10 C11 C12 174.1(2) . . . . ? S2 C10 C11 C12 -5.7(3) . . . . ? C9 C10 C11 C23 -5.2(3) . . . . ? S2 C10 C11 C23 175.06(15) . . . . ? C10 C11 C12 C13 170.1(2) . . . . ? C23 C11 C12 C13 -10.7(3) . . . . ? C10 C11 C12 S3 -9.6(3) . . . . ? C23 C11 C12 S3 169.68(15) . . . . ? C15 S3 C12 C11 179.01(19) . . . . ? C15 S3 C12 C13 -0.69(16) . . . . ? C11 C12 C13 C14 -179.2(2) . . . . ? S3 C12 C13 C14 0.5(2) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 -176.9(2) . . . . ? C13 C14 C15 S3 -0.6(2) . . . . ? C12 S3 C15 C16 176.8(2) . . . . ? C12 S3 C15 C14 0.73(16) . . . . ? C14 C15 C16 C17 -178.8(2) . . . . ? S3 C15 C16 C17 5.7(4) . . . . ? C15 C16 C17 C18 10.8(5) . . . . ? C16 C17 C18 C19 -177.9(2) . . . . ? C16 C17 C18 S4 5.5(4) . . . . ? C21 S4 C18 C17 177.0(2) . . . . ? C21 S4 C18 C19 0.01(16) . . . . ? C17 C18 C19 C20 -177.9(2) . . . . ? S4 C18 C19 C20 -0.7(2) . . . . ? C18 C19 C20 C21 1.3(3) . . . . ? C19 C20 C21 C22 177.6(2) . . . . ? C19 C20 C21 S4 -1.2(2) . . . . ? C18 S4 C21 C22 -178.17(19) . . . . ? C18 S4 C21 C20 0.65(16) . . . . ? C20 C21 C22 C1 168.9(2) . . . . ? S4 C21 C22 C1 -12.5(3) . . . . ? C20 C21 C22 C29 -11.6(3) . . . . ? S4 C21 C22 C29 166.99(15) . . . . ? C2 C1 C22 C21 171.2(2) . . . . ? S1 C1 C22 C21 -12.0(3) . . . . ? C2 C1 C22 C29 -8.3(3) . . . . ? S1 C1 C22 C29 168.59(15) . . . . ? C12 C11 C23 C24 114.2(2) . . . . ? C10 C11 C23 C24 -66.5(3) . . . . ? C12 C11 C23 C28 -68.1(2) . . . . ? C10 C11 C23 C28 111.2(2) . . . . ? C28 C23 C24 C25 -0.3(3) . . . . ? C11 C23 C24 C25 177.5(2) . . . . ? C23 C24 C25 C26 -0.6(3) . . . . ? C24 C25 C26 C27 1.1(3) . . . . ? C24 C25 C26 Cl1 -177.51(17) . . . . ? C25 C26 C27 C28 -0.7(3) . . . . ? Cl1 C26 C27 C28 177.97(15) . . . . ? C26 C27 C28 C23 -0.3(3) . . . . ? C24 C23 C28 C27 0.7(3) . . . . ? C11 C23 C28 C27 -177.07(18) . . . . ? C21 C22 C29 C30 -51.2(3) . . . . ? C1 C22 C29 C30 128.3(2) . . . . ? C21 C22 C29 C34 128.1(2) . . . . ? C1 C22 C29 C34 -52.4(3) . . . . ? C34 C29 C30 C31 1.7(3) . . . . ? C22 C29 C30 C31 -178.9(2) . . . . ? C29 C30 C31 C32 -0.3(3) . . . . ? C30 C31 C32 C33 -1.2(3) . . . . ? C30 C31 C32 Cl2 178.90(16) . . . . ? C31 C32 C33 C34 1.0(3) . . . . ? Cl2 C32 C33 C34 -179.05(16) . . . . ? C32 C33 C34 C29 0.5(3) . . . . ? C30 C29 C34 C33 -1.9(3) . . . . ? C22 C29 C34 C33 178.77(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.367 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.073 _database_code_depnum_ccdc_archive 'CCDC 936013'