# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Pi Conjugated Macrocycles From Thiophenes and Benzenes ; _publ_contact_author_name 'Venkataramanarao Anand' _publ_contact_author_email VG.ANAND@IISERPUNE.AC.IN loop_ _publ_author_name 'Venkataramanarao Anand' 'J. Sreedhar Reddy' # Attachment 'B715553K-CIF.txt' data_sree3 _database_code_depnum_ccdc_archive 'CCDC 663304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H25 Cl9 F24 S4' _chemical_formula_weight 1805.22 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.7374(4) _cell_length_b 19.0689(4) _cell_length_c 22.0855(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.8180(10) _cell_angle_gamma 90.00 _cell_volume 7544.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8942 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 19.5 _exptl_crystal_description needle _exptl_crystal_colour green _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 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8530 _exptl_absorpt_correction_T_max 0.8984 _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 'Bruker axs (Kappa apex2)' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38463 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 19.34 _reflns_number_total 6385 _reflns_number_gt 4791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (WINGX)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (WINGX)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The three chloroform molecules of the asymmetric unit have large thermal motion. As the unconstrained refinement of these atoms led to abnormal bond distances, it was decided to restrain the C-Cl distances to be in the range of 1.75(1)\%A during the refinement. Also there was one disordered position (Cl4') for chloroform associated with carbon C72. The four chlorine positions were refined keeping sum of their occupancy as 3.0(0.001). ; _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^)+(0.1201P)^2^+25.9109P] 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 6385 _refine_ls_number_parameters 1004 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.035 _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 1.1224(4) 1.1493(4) 0.2185(4) 0.051(2) Uani 1 1 d . . . C2 C 1.0878(5) 1.1835(5) 0.1568(4) 0.067(2) Uani 1 1 d . . . H2 H 1.0643 1.1595 0.1167 0.080 Uiso 1 1 calc R . . C3 C 1.0912(5) 1.2545(5) 0.1604(4) 0.070(3) Uani 1 1 d . . . H3 H 1.0707 1.2830 0.1228 0.084 Uiso 1 1 calc R . . C4 C 1.1281(4) 1.2816(4) 0.2252(4) 0.054(2) Uani 1 1 d . . . C5 C 1.1401(4) 1.3522(4) 0.2425(4) 0.052(2) Uani 1 1 d . . . C6 C 1.1835(4) 1.3813(4) 0.3052(4) 0.048(2) Uani 1 1 d . . . C7 C 1.1858(5) 1.4530(4) 0.3206(4) 0.059(2) Uani 1 1 d . . . H7 H 1.1552 1.4860 0.2905 0.071 Uiso 1 1 calc R . . C8 C 1.2358(5) 1.4699(4) 0.3823(4) 0.058(2) Uani 1 1 d . . . H8 H 1.2416 1.5155 0.3985 0.069 Uiso 1 1 calc R . . C9 C 1.2792(4) 1.4133(4) 0.4212(4) 0.049(2) Uani 1 1 d . . . C10 C 1.3374(4) 1.4194(4) 0.4847(4) 0.049(2) Uani 1 1 d . . . C11 C 1.3910(4) 1.3695(4) 0.5242(4) 0.0458(19) Uani 1 1 d . . . C12 C 1.4007(4) 1.3022(4) 0.5031(4) 0.053(2) Uani 1 1 d . . . H12 H 1.3669 1.2866 0.4614 0.064 Uiso 1 1 calc R . . C13 C 1.4574(4) 1.2587(4) 0.5413(4) 0.056(2) Uani 1 1 d . . . H13 H 1.4607 1.2145 0.5250 0.067 Uiso 1 1 calc R . . C14 C 1.5111(4) 1.2785(4) 0.6047(4) 0.047(2) Uani 1 1 d . . . C15 C 1.5006(5) 1.3454(4) 0.6269(4) 0.063(2) Uani 1 1 d . . . H15 H 1.5339 1.3608 0.6689 0.076 Uiso 1 1 calc R . . C16 C 1.4438(5) 1.3879(4) 0.5890(4) 0.061(2) Uani 1 1 d . . . H16 H 1.4392 1.4312 0.6063 0.073 Uiso 1 1 calc R . . C17 C 1.5746(4) 1.2380(4) 0.6443(4) 0.046(2) Uani 1 1 d . . . C18 C 1.5840(4) 1.1641(4) 0.6420(4) 0.052(2) Uani 1 1 d . . . C19 C 1.6503(5) 1.1271(4) 0.6778(4) 0.062(2) Uani 1 1 d . . . H19 H 1.6962 1.1491 0.7003 0.074 Uiso 1 1 calc R . . C20 C 1.6416(4) 1.0558(4) 0.6769(4) 0.057(2) Uani 1 1 d . . . H20 H 1.6811 1.0254 0.6991 0.069 Uiso 1 1 calc R . . C21 C 1.5687(4) 1.0325(4) 0.6398(4) 0.048(2) Uani 1 1 d . . . C22 C 1.5425(4) 0.9646(4) 0.6377(4) 0.051(2) Uani 1 1 d . . . C23 C 1.4717(5) 0.9392(4) 0.5988(4) 0.055(2) Uani 1 1 d . . . C24 C 1.4422(5) 0.8754(4) 0.6094(4) 0.067(2) Uani 1 1 d . . . H24 H 1.4696 0.8445 0.6435 0.080 Uiso 1 1 calc R . . C25 C 1.3707(5) 0.8627(4) 0.5661(5) 0.068(2) Uani 1 1 d . . . H25 H 1.3446 0.8232 0.5691 0.082 Uiso 1 1 calc R . . C26 C 1.3389(4) 0.9138(4) 0.5161(4) 0.055(2) Uani 1 1 d . . . C27 C 1.2691(4) 0.9097(4) 0.4624(4) 0.053(2) Uani 1 1 d . . . C28 C 1.2354(4) 0.9547(4) 0.4064(4) 0.047(2) Uani 1 1 d . . . C29 C 1.1771(5) 0.9295(4) 0.3490(4) 0.062(2) Uani 1 1 d . . . H29 H 1.1601 0.8841 0.3494 0.074 Uiso 1 1 calc R . . C30 C 1.1439(5) 0.9679(4) 0.2927(4) 0.061(2) Uani 1 1 d . . . H30 H 1.1074 0.9471 0.2551 0.074 Uiso 1 1 calc R . . C31 C 1.1631(4) 1.0386(4) 0.2894(4) 0.051(2) Uani 1 1 d . . . C32 C 1.2206(5) 1.0649(4) 0.3471(4) 0.059(2) Uani 1 1 d . . . H32 H 1.2356 1.1113 0.3479 0.071 Uiso 1 1 calc R . . C33 C 1.2553(4) 1.0245(4) 0.4022(4) 0.060(2) Uani 1 1 d . . . H33 H 1.2941 1.0440 0.4390 0.072 Uiso 1 1 calc R . . C34 C 1.1243(4) 1.0775(4) 0.2281(4) 0.054(2) Uani 1 1 d . . . C35 C 1.1015(6) 1.4036(4) 0.1878(4) 0.062(2) Uani 1 1 d . . . C36 C 1.0309(8) 1.4287(6) 0.1733(6) 0.108(4) Uani 1 1 d . . . C37 C 0.9990(8) 1.4803(8) 0.1253(8) 0.140(6) Uani 1 1 d . . . H37 H 0.9516 1.4973 0.1165 0.167 Uiso 1 1 calc R . . C38 C 1.0359(13) 1.5053(8) 0.0919(7) 0.142(8) Uani 1 1 d . . . H38 H 1.0143 1.5406 0.0606 0.170 Uiso 1 1 calc R . . C39 C 1.1022(12) 1.4818(8) 0.1019(7) 0.134(6) Uani 1 1 d . . . H39 H 1.1268 1.4984 0.0770 0.161 Uiso 1 1 calc R . . C40 C 1.1345(8) 1.4310(6) 0.1511(6) 0.101(3) Uani 1 1 d . . . C41 C 1.3463(4) 1.4921(4) 0.5129(4) 0.046(2) Uani 1 1 d . . . C42 C 1.3921(5) 1.5399(5) 0.5021(4) 0.054(2) Uani 1 1 d . . . C43 C 1.4035(5) 1.6063(5) 0.5284(4) 0.063(2) Uani 1 1 d . . . C44 C 1.3665(6) 1.6261(4) 0.5649(4) 0.068(3) Uani 1 1 d . . . C45 C 1.3200(5) 1.5810(5) 0.5760(4) 0.068(2) Uani 1 1 d . . . C46 C 1.3106(4) 1.5151(4) 0.5499(4) 0.050(2) Uani 1 1 d . . . C47 C 1.6378(4) 1.2738(4) 0.6980(4) 0.048(2) Uani 1 1 d . . . C48 C 1.6595(5) 1.2577(4) 0.7646(4) 0.056(2) Uani 1 1 d . . . C49 C 1.7193(6) 1.2883(5) 0.8151(5) 0.071(3) Uani 1 1 d . . . C50 C 1.7588(6) 1.3378(5) 0.8005(6) 0.081(3) Uani 1 1 d . . . C51 C 1.7391(6) 1.3566(5) 0.7360(7) 0.089(3) Uani 1 1 d . . . C52 C 1.6788(5) 1.3257(4) 0.6853(4) 0.062(2) Uani 1 1 d . . . C53 C 1.5946(4) 0.9128(4) 0.6850(4) 0.051(2) Uani 1 1 d . . . C54 C 1.6175(5) 0.8533(5) 0.6629(5) 0.064(2) Uani 1 1 d . . . C55 C 1.6601(5) 0.8007(5) 0.7038(6) 0.081(3) Uani 1 1 d . . . H55 H 1.6733 0.7613 0.6865 0.097 Uiso 1 1 calc R . . C56 C 1.6823(6) 0.8087(6) 0.7706(7) 0.095(3) Uani 1 1 d . . . H56 H 1.7107 0.7737 0.7993 0.114 Uiso 1 1 calc R . . C57 C 1.6639(6) 0.8665(6) 0.7963(5) 0.090(3) Uani 1 1 d . . . H57 H 1.6806 0.8718 0.8422 0.108 Uiso 1 1 calc R . . C58 C 1.6204(5) 0.9167(5) 0.7535(5) 0.065(2) Uani 1 1 d . . . C59 C 1.2236(5) 0.8469(5) 0.4636(4) 0.060(2) Uani 1 1 d . . . C60 C 1.1656(6) 0.8534(6) 0.4812(4) 0.073(3) Uani 1 1 d . . . C61 C 1.1200(6) 0.7965(10) 0.4789(5) 0.100(4) Uani 1 1 d . . . C62 C 1.1351(9) 0.7323(9) 0.4585(6) 0.104(4) Uani 1 1 d . . . C63 C 1.1919(8) 0.7236(6) 0.4420(6) 0.102(4) Uani 1 1 d . . . C64 C 1.2356(6) 0.7808(6) 0.4447(5) 0.082(3) Uani 1 1 d . . . C65 C 1.0803(5) 1.0346(4) 0.1682(4) 0.058(2) Uani 1 1 d . . . C66 C 1.1135(7) 0.9931(5) 0.1376(5) 0.075(3) Uani 1 1 d . . . C67 C 1.0758(10) 0.9516(6) 0.0859(6) 0.102(4) Uani 1 1 d . . . C68 C 1.0020(11) 0.9484(7) 0.0606(5) 0.106(5) Uani 1 1 d . . . C69 C 0.9634(7) 0.9886(7) 0.0872(6) 0.098(4) Uani 1 1 d . . . C70 C 1.0032(6) 1.0320(5) 0.1407(5) 0.072(3) Uani 1 1 d . . . C71 C 0.2022(9) 0.2098(7) 0.4879(9) 0.34(2) Uani 1 1 d D . . H71 H 0.2029 0.2186 0.4444 0.413 Uiso 1 1 calc R . . C73 C 0.3823(9) 1.0745(7) 0.7461(6) 0.38(2) Uani 1 1 d D . . H73 H 0.3360 1.1013 0.7239 0.451 Uiso 1 1 calc R . . F1 F 0.9975(4) 1.4022(6) 0.2089(6) 0.218(5) Uani 1 1 d . . . F2 F 1.2033(6) 1.4083(5) 0.1631(4) 0.178(4) Uani 1 1 d . . . F3 F 1.2642(3) 1.4713(2) 0.5623(3) 0.0799(14) Uani 1 1 d . . . F4 F 1.2841(4) 1.6017(3) 0.6131(3) 0.117(2) Uani 1 1 d . . . F5 F 1.3763(4) 1.6916(3) 0.5904(3) 0.112(2) Uani 1 1 d . . . F6 F 1.4491(4) 1.6515(3) 0.5176(3) 0.1049(19) Uani 1 1 d . . . F7 F 1.4268(3) 1.5221(3) 0.4638(3) 0.0884(16) Uani 1 1 d . . . F8 F 1.6213(3) 1.2100(3) 0.7816(2) 0.0855(15) Uani 1 1 d . . . F9 F 1.7397(3) 1.2690(3) 0.8791(3) 0.1024(18) Uani 1 1 d . . . F10 F 1.8176(4) 1.3680(4) 0.8498(3) 0.141(3) Uani 1 1 d . . . F11 F 1.7787(4) 1.4057(3) 0.7211(4) 0.145(3) Uani 1 1 d . . . F12 F 1.6617(3) 1.3462(3) 0.6235(3) 0.0903(16) Uani 1 1 d . . . F13 F 1.5966(3) 0.8457(3) 0.5969(3) 0.0947(17) Uani 1 1 d . . . F14 F 1.5997(3) 0.9725(3) 0.7789(2) 0.0969(18) Uani 1 1 d . . . F15 F 1.1509(3) 0.9151(4) 0.5004(3) 0.1088(19) Uani 1 1 d . . . F16 F 1.0637(4) 0.8061(5) 0.4962(4) 0.166(3) Uani 1 1 d . . . F17 F 1.0899(4) 0.6782(4) 0.4569(3) 0.171(4) Uani 1 1 d . . . F18 F 1.2041(4) 0.6614(4) 0.4221(4) 0.167(4) Uani 1 1 d . . . F19 F 1.2908(4) 0.7708(3) 0.4260(4) 0.130(2) Uani 1 1 d . . . F20 F 1.1884(4) 0.9939(4) 0.1627(3) 0.123(2) Uani 1 1 d . . . F21 F 1.1117(5) 0.9118(4) 0.0576(4) 0.173(3) Uani 1 1 d . . . F22 F 0.9625(5) 0.9068(4) 0.0086(3) 0.169(4) Uani 1 1 d . . . F23 F 0.8899(4) 0.9869(5) 0.0626(4) 0.166(3) Uani 1 1 d . . . F24 F 0.9662(3) 1.0691(4) 0.1676(3) 0.110(2) Uani 1 1 d . . . S1 S 1.15770(11) 1.21235(10) 0.28136(10) 0.0559(6) Uani 1 1 d . . . S2 S 1.24803(11) 1.33636(10) 0.37403(10) 0.0553(6) Uani 1 1 d . . . S3 S 1.51169(11) 1.10506(10) 0.60271(10) 0.0564(6) Uani 1 1 d . . . S4 S 1.40450(11) 0.98048(10) 0.52909(10) 0.0591(7) Uani 1 1 d . . . Cl1 Cl 0.1937(6) 0.2854(5) 0.5297(4) 0.326(5) Uani 1 1 d D . . Cl2 Cl 0.2836(7) 0.1736(6) 0.5471(8) 0.402(7) Uani 1 1 d D . . Cl3 Cl 0.1304(8) 0.1573(8) 0.4855(6) 0.509(11) Uani 1 1 d D . . C72 C -0.0424(6) 0.2506(6) 0.3005(7) 0.44(3) Uani 1 1 d D A 1 H72 H -0.0495 0.2588 0.2544 0.527 Uiso 1 1 calc R A 1 Cl4 Cl 0.0264(4) 0.3084(4) 0.3445(4) 0.239(5) Uani 0.795(13) 1 d PD A 1 Cl5 Cl -0.0234(6) 0.1615(5) 0.3108(7) 0.236(7) Uani 0.594(17) 1 d PD A 1 Cl4' Cl -0.0809(11) 0.2295(10) 0.2335(7) 0.404(15) Uani 0.74(2) 1 d PD A 2 Cl6 Cl -0.1174(6) 0.2966(4) 0.3048(8) 0.363(10) Uani 0.874(18) 1 d PD . . Cl7 Cl 0.4616(7) 1.1211(7) 0.7570(6) 0.387(6) Uani 1 1 d D . . Cl8 Cl 0.3992(6) 1.0475(6) 0.8261(4) 0.357(5) Uani 1 1 d D . . Cl9 Cl 0.3847(5) 0.9975(5) 0.7050(5) 0.331(5) Uani 1 1 d 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 0.057(5) 0.048(6) 0.038(5) -0.002(4) 0.010(4) -0.010(4) C2 0.083(6) 0.058(7) 0.041(6) -0.005(5) 0.008(5) -0.009(5) C3 0.081(6) 0.055(7) 0.044(6) 0.006(5) -0.004(5) -0.005(5) C4 0.052(5) 0.047(6) 0.049(6) 0.003(4) 0.009(4) 0.002(4) C5 0.049(5) 0.047(5) 0.047(6) 0.006(5) 0.008(4) 0.002(4) C6 0.044(5) 0.047(6) 0.042(5) 0.005(4) 0.007(4) 0.000(4) C7 0.060(5) 0.043(6) 0.051(6) 0.004(4) 0.000(5) 0.003(4) C8 0.071(6) 0.034(5) 0.054(6) 0.003(4) 0.011(5) 0.005(4) C9 0.055(5) 0.039(5) 0.050(6) -0.006(4) 0.018(5) -0.004(4) C10 0.059(5) 0.040(5) 0.042(5) -0.003(4) 0.016(5) 0.001(4) C11 0.051(5) 0.035(5) 0.042(5) -0.003(4) 0.011(5) 0.003(4) C12 0.058(5) 0.040(5) 0.040(5) -0.004(4) -0.001(4) -0.001(4) C13 0.063(6) 0.037(5) 0.050(6) -0.004(4) 0.005(5) 0.001(5) C14 0.054(5) 0.040(5) 0.037(5) 0.003(4) 0.009(5) 0.001(4) C15 0.071(6) 0.056(6) 0.039(5) -0.009(5) 0.000(5) 0.013(5) C16 0.069(6) 0.047(5) 0.050(6) -0.009(5) 0.010(5) 0.015(5) C17 0.049(5) 0.039(5) 0.040(5) -0.002(4) 0.008(4) -0.008(4) C18 0.053(5) 0.042(5) 0.051(5) -0.001(4) 0.012(4) -0.003(4) C19 0.047(5) 0.050(6) 0.074(6) -0.008(5) 0.010(5) -0.003(5) C20 0.049(6) 0.043(6) 0.064(6) -0.001(4) 0.009(5) 0.002(4) C21 0.046(5) 0.038(5) 0.051(5) -0.002(4) 0.011(4) 0.002(4) C22 0.051(5) 0.036(5) 0.057(5) -0.002(4) 0.014(5) 0.003(5) C23 0.054(6) 0.039(5) 0.060(5) 0.003(4) 0.013(5) -0.005(4) C24 0.057(6) 0.051(6) 0.066(6) 0.015(4) 0.000(5) 0.002(5) C25 0.067(7) 0.046(5) 0.079(6) 0.019(5) 0.018(6) -0.008(5) C26 0.051(5) 0.043(5) 0.058(6) -0.002(5) 0.010(5) -0.010(4) C27 0.055(6) 0.032(5) 0.063(6) -0.007(4) 0.016(5) -0.012(4) C28 0.043(5) 0.037(5) 0.049(6) -0.002(4) 0.007(5) -0.011(4) C29 0.069(6) 0.045(5) 0.061(6) 0.000(5) 0.016(5) -0.020(5) C30 0.067(6) 0.057(6) 0.043(6) -0.002(5) 0.006(5) -0.018(5) C31 0.055(5) 0.041(5) 0.051(6) -0.004(4) 0.018(5) -0.004(4) C32 0.060(6) 0.038(5) 0.057(6) 0.002(5) 0.002(5) -0.003(4) C33 0.053(5) 0.045(6) 0.055(6) -0.009(5) -0.004(5) -0.011(4) C34 0.055(5) 0.052(6) 0.044(6) -0.005(5) 0.009(5) -0.009(4) C35 0.076(7) 0.043(5) 0.047(6) 0.002(5) 0.008(6) -0.010(5) C36 0.089(9) 0.095(8) 0.110(10) 0.053(8) 0.013(8) 0.027(8) C37 0.111(11) 0.115(11) 0.127(13) 0.042(10) -0.014(10) 0.040(9) C38 0.22(2) 0.072(9) 0.067(9) 0.020(7) -0.009(12) -0.006(12) C39 0.191(17) 0.102(11) 0.079(10) 0.030(9) 0.027(11) -0.026(11) C40 0.105(10) 0.097(9) 0.080(8) 0.018(8) 0.018(8) -0.010(8) C41 0.052(5) 0.042(5) 0.036(5) 0.000(4) 0.010(4) 0.004(4) C42 0.066(6) 0.055(7) 0.042(5) -0.006(5) 0.024(5) -0.001(5) C43 0.087(7) 0.046(6) 0.057(6) -0.004(5) 0.030(6) -0.014(5) C44 0.113(8) 0.031(6) 0.053(6) -0.009(5) 0.029(6) -0.008(6) C45 0.092(7) 0.062(7) 0.059(6) -0.010(5) 0.041(6) 0.009(6) C46 0.060(5) 0.040(6) 0.049(5) -0.002(5) 0.022(5) -0.003(5) C47 0.050(5) 0.040(5) 0.045(6) 0.002(4) 0.011(5) -0.002(4) C48 0.056(6) 0.053(5) 0.049(7) -0.002(5) 0.012(6) -0.011(5) C49 0.074(7) 0.071(7) 0.047(7) -0.002(6) 0.005(6) -0.001(6) C50 0.079(7) 0.058(6) 0.067(8) -0.010(6) -0.007(7) -0.017(6) C51 0.094(8) 0.051(6) 0.104(10) 0.012(7) 0.025(8) -0.031(6) C52 0.074(6) 0.045(5) 0.044(6) 0.006(5) 0.003(5) -0.011(5) C53 0.054(5) 0.031(5) 0.060(7) -0.007(5) 0.016(5) 0.003(4) C54 0.059(6) 0.057(6) 0.068(7) -0.003(6) 0.019(5) 0.000(5) C55 0.072(7) 0.059(7) 0.100(9) -0.004(7) 0.024(6) 0.019(6) C56 0.086(8) 0.074(8) 0.096(10) 0.017(7) 0.010(7) 0.037(6) C57 0.101(8) 0.083(8) 0.059(6) 0.014(6) 0.007(6) 0.028(7) C58 0.071(6) 0.054(6) 0.059(7) -0.003(6) 0.016(5) 0.013(5) C59 0.056(6) 0.053(7) 0.052(5) 0.004(4) 0.004(5) -0.007(5) C60 0.067(7) 0.091(8) 0.053(6) 0.007(6) 0.017(5) -0.015(7) C61 0.062(8) 0.169(14) 0.054(7) 0.021(8) 0.011(6) -0.033(10) C62 0.096(11) 0.115(12) 0.072(8) 0.025(8) 0.005(7) -0.055(10) C63 0.106(10) 0.058(9) 0.107(9) 0.010(6) 0.011(8) -0.029(8) C64 0.075(8) 0.070(9) 0.093(8) 0.005(6) 0.026(6) -0.019(7) C65 0.069(7) 0.051(5) 0.042(6) -0.002(5) 0.013(6) -0.011(5) C66 0.084(8) 0.074(7) 0.059(7) -0.020(6) 0.022(7) -0.016(6) C67 0.153(13) 0.079(8) 0.070(9) -0.036(7) 0.042(9) -0.026(9) C68 0.159(14) 0.090(9) 0.043(7) -0.028(7) 0.019(9) -0.072(10) C69 0.097(10) 0.114(9) 0.057(8) -0.011(7) 0.008(8) -0.061(8) C70 0.075(8) 0.079(7) 0.047(6) -0.008(5) 0.012(6) -0.020(6) C71 0.38(5) 0.42(5) 0.35(4) 0.19(4) 0.26(4) 0.11(4) C73 0.24(3) 0.69(7) 0.23(3) -0.22(4) 0.12(2) -0.06(4) F1 0.112(6) 0.266(11) 0.299(12) 0.182(10) 0.107(8) 0.108(7) F2 0.154(7) 0.240(10) 0.171(8) 0.099(7) 0.100(7) 0.015(7) F3 0.094(4) 0.069(3) 0.094(4) -0.009(3) 0.056(3) -0.012(3) F4 0.165(6) 0.085(4) 0.140(5) -0.036(4) 0.103(5) -0.006(4) F5 0.191(6) 0.050(4) 0.103(4) -0.019(3) 0.070(4) -0.015(3) F6 0.145(5) 0.079(4) 0.097(4) -0.013(3) 0.057(4) -0.057(4) F7 0.105(4) 0.083(4) 0.099(4) -0.017(3) 0.064(4) -0.020(3) F8 0.090(4) 0.101(4) 0.057(3) 0.009(3) 0.023(3) -0.025(3) F9 0.104(4) 0.130(5) 0.045(4) -0.008(3) 0.003(3) -0.010(3) F10 0.121(5) 0.127(5) 0.110(5) -0.034(4) -0.016(4) -0.058(4) F11 0.141(6) 0.113(5) 0.143(6) 0.027(4) 0.022(5) -0.072(5) F12 0.109(4) 0.078(4) 0.070(4) 0.019(3) 0.024(3) -0.020(3) F13 0.119(4) 0.077(4) 0.077(4) -0.022(3) 0.030(3) 0.012(3) F14 0.137(5) 0.075(4) 0.069(3) -0.006(3) 0.033(3) 0.031(3) F15 0.099(4) 0.138(6) 0.098(5) -0.016(4) 0.051(4) -0.005(4) F16 0.110(5) 0.271(10) 0.126(6) 0.016(6) 0.059(5) -0.064(6) F17 0.148(6) 0.161(6) 0.132(6) 0.062(5) -0.010(5) -0.109(6) F18 0.171(7) 0.051(4) 0.214(8) -0.005(4) 0.018(6) -0.034(4) F19 0.129(5) 0.060(4) 0.211(8) -0.035(4) 0.080(6) -0.013(4) F20 0.113(6) 0.150(6) 0.106(5) -0.038(4) 0.046(4) 0.011(4) F21 0.234(9) 0.159(7) 0.132(6) -0.082(6) 0.082(6) -0.008(6) F22 0.254(9) 0.146(6) 0.077(4) -0.051(5) 0.039(5) -0.107(6) F23 0.103(5) 0.249(9) 0.105(5) -0.034(5) 0.003(4) -0.095(6) F24 0.066(4) 0.154(6) 0.093(4) -0.027(4) 0.017(3) -0.012(4) S1 0.0619(14) 0.0454(12) 0.0439(13) -0.0014(10) 0.0060(11) -0.0017(10) S2 0.0597(14) 0.0420(12) 0.0460(13) -0.0031(10) 0.0043(11) 0.0049(10) S3 0.0483(12) 0.0380(12) 0.0623(14) 0.0007(10) 0.0031(11) -0.0023(10) S4 0.0563(14) 0.0437(12) 0.0561(14) 0.0071(10) 0.0029(11) -0.0103(10) Cl1 0.386(12) 0.342(10) 0.233(8) -0.080(7) 0.112(8) 0.038(9) Cl2 0.345(13) 0.369(13) 0.58(2) 0.018(13) 0.279(14) -0.001(10) Cl3 0.472(18) 0.55(2) 0.368(14) 0.069(14) 0.043(13) -0.287(17) C72 0.063(11) 0.20(3) 0.85(9) 0.07(4) -0.01(3) 0.000(15) Cl4 0.214(8) 0.242(8) 0.261(9) -0.085(6) 0.101(6) 0.005(6) Cl5 0.227(11) 0.182(10) 0.295(16) -0.003(9) 0.106(10) -0.005(7) Cl4' 0.49(3) 0.39(2) 0.310(19) -0.160(17) 0.147(18) -0.19(2) Cl6 0.276(11) 0.189(8) 0.62(3) 0.031(10) 0.185(13) -0.037(7) Cl7 0.376(13) 0.497(16) 0.366(12) -0.028(11) 0.231(11) -0.119(12) Cl8 0.383(12) 0.520(15) 0.217(7) 0.070(9) 0.173(8) 0.043(11) Cl9 0.371(11) 0.328(10) 0.365(11) -0.095(9) 0.223(10) 0.012(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 C34 1.383(10) . ? C1 C2 1.403(11) . ? C1 S1 1.745(8) . ? C2 C3 1.355(11) . ? C2 H2 0.9300 . ? C3 C4 1.404(11) . ? C3 H3 0.9300 . ? C4 C5 1.392(10) . ? C4 S1 1.738(8) . ? C5 C6 1.403(10) . ? C5 C35 1.491(11) . ? C6 C7 1.403(10) . ? C6 S2 1.744(7) . ? C7 C8 1.345(10) . ? C7 H7 0.9300 . ? C8 C9 1.421(10) . ? C8 H8 0.9300 . ? C9 C10 1.396(10) . ? C9 S2 1.754(7) . ? C10 C11 1.418(10) . ? C10 C41 1.500(10) . ? C11 C12 1.405(10) . ? C11 C16 1.416(10) . ? C12 C13 1.363(10) . ? C12 H12 0.9300 . ? C13 C14 1.408(10) . ? C13 H13 0.9300 . ? C14 C15 1.413(10) . ? C14 C17 1.418(10) . ? C15 C16 1.350(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.426(10) . ? C17 C47 1.478(10) . ? C18 C19 1.402(10) . ? C18 S3 1.737(8) . ? C19 C20 1.370(10) . ? C19 H19 0.9300 . ? C20 C21 1.397(10) . ? C20 H20 0.9300 . ? C21 C22 1.387(10) . ? C21 S3 1.754(7) . ? C22 C23 1.385(10) . ? C22 C53 1.491(10) . ? C23 C24 1.411(11) . ? C23 S4 1.742(8) . ? C24 C25 1.354(11) . ? C24 H24 0.9300 . ? C25 C26 1.408(11) . ? C25 H25 0.9300 . ? C26 C27 1.392(10) . ? C26 S4 1.751(8) . ? C27 C28 1.421(10) . ? C27 C59 1.504(11) . ? C28 C29 1.391(10) . ? C28 C33 1.402(10) . ? C29 C30 1.352(10) . ? C29 H29 0.9300 . ? C30 C31 1.412(10) . ? C30 H30 0.9300 . ? C31 C32 1.397(10) . ? C31 C34 1.449(11) . ? C32 C33 1.358(10) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C65 1.486(11) . ? C35 C40 1.341(14) . ? C35 C36 1.378(14) . ? C36 F1 1.322(14) . ? C36 C37 1.388(17) . ? C37 C38 1.32(2) . ? C37 H37 0.9300 . ? C38 C39 1.31(2) . ? C38 H38 0.9300 . ? C39 C40 1.394(17) . ? C39 H39 0.9300 . ? C40 F2 1.341(14) . ? C41 C46 1.358(10) . ? C41 C42 1.372(11) . ? C42 F7 1.337(9) . ? C42 C43 1.371(11) . ? C43 F6 1.338(9) . ? C43 C44 1.348(12) . ? C44 F5 1.349(9) . ? C44 C45 1.353(12) . ? C45 F4 1.348(10) . ? C45 C46 1.362(11) . ? C46 F3 1.348(9) . ? C47 C52 1.381(11) . ? C47 C48 1.382(11) . ? C48 F8 1.332(9) . ? C48 C49 1.367(12) . ? C49 C50 1.347(13) . ? C49 F9 1.348(10) . ? C50 F10 1.343(10) . ? C50 C51 1.358(13) . ? C51 F11 1.344(11) . ? C51 C52 1.378(12) . ? C52 F12 1.320(9) . ? C53 C58 1.381(11) . ? C53 C54 1.384(11) . ? C54 F13 1.346(10) . ? C54 C55 1.375(12) . ? C55 C56 1.359(13) . ? C55 H55 0.9300 . ? C56 C57 1.357(13) . ? C56 H56 0.9300 . ? C57 C58 1.367(12) . ? C57 H57 0.9300 . ? C58 F14 1.345(9) . ? C59 C60 1.360(13) . ? C59 C64 1.378(13) . ? C60 F15 1.324(11) . ? C60 C61 1.398(16) . ? C61 F16 1.331(14) . ? C61 C62 1.378(17) . ? C62 C63 1.327(18) . ? C62 F17 1.354(13) . ? C63 F18 1.323(14) . ? C63 C64 1.376(15) . ? C64 F19 1.331(12) . ? C65 C66 1.373(12) . ? C65 C70 1.382(12) . ? C66 C67 1.330(14) . ? C66 F20 1.344(11) . ? C67 C68 1.325(17) . ? C67 F21 1.356(14) . ? C68 F22 1.342(12) . ? C68 C69 1.374(17) . ? C69 F23 1.320(13) . ? C69 C70 1.385(14) . ? C70 F24 1.324(11) . ? C71 Cl3 1.719(10) . ? C71 Cl2 1.734(10) . ? C71 Cl1 1.758(10) . ? C71 H71 0.9800 . ? C73 Cl7 1.726(10) . ? C73 Cl8 1.735(10) . ? C73 Cl9 1.737(10) . ? C73 H73 0.9800 . ? C72 Cl4 1.701(9) . ? C72 Cl5 1.735(9) . ? C72 Cl6 1.756(9) . ? C72 H72 0.9800 . ? Cl4' Cl6 2.37(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 C34 C1 C2 125.4(7) . . ? C34 C1 S1 125.7(6) . . ? C2 C1 S1 108.7(6) . . ? C3 C2 C1 114.5(7) . . ? C3 C2 H2 122.7 . . ? C1 C2 H2 122.7 . . ? C2 C3 C4 114.8(7) . . ? C2 C3 H3 122.6 . . ? C4 C3 H3 122.6 . . ? C5 C4 C3 126.3(7) . . ? C5 C4 S1 124.9(6) . . ? C3 C4 S1 108.8(6) . . ? C4 C5 C6 128.1(7) . . ? C4 C5 C35 116.3(7) . . ? C6 C5 C35 115.6(7) . . ? C5 C6 C7 124.6(7) . . ? C5 C6 S2 125.9(6) . . ? C7 C6 S2 109.3(6) . . ? C8 C7 C6 114.4(7) . . ? C8 C7 H7 122.8 . . ? C6 C7 H7 122.8 . . ? C7 C8 C9 115.5(7) . . ? C7 C8 H8 122.2 . . ? C9 C8 H8 122.2 . . ? C10 C9 C8 125.2(7) . . ? C10 C9 S2 127.0(6) . . ? C8 C9 S2 107.7(6) . . ? C9 C10 C11 130.5(7) . . ? C9 C10 C41 113.4(6) . . ? C11 C10 C41 116.0(6) . . ? C12 C11 C16 114.6(7) . . ? C12 C11 C10 125.4(7) . . ? C16 C11 C10 119.9(7) . . ? C13 C12 C11 122.7(7) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C14 122.2(7) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C15 115.3(7) . . ? C13 C14 C17 124.7(7) . . ? C15 C14 C17 119.9(7) . . ? C16 C15 C14 122.1(7) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C11 123.1(7) . . ? C15 C16 H16 118.5 . . ? C11 C16 H16 118.5 . . ? C14 C17 C18 127.7(7) . . ? C14 C17 C47 118.2(6) . . ? C18 C17 C47 113.9(7) . . ? C19 C18 C17 125.6(7) . . ? C19 C18 S3 109.4(6) . . ? C17 C18 S3 124.5(6) . . ? C20 C19 C18 114.1(7) . . ? C20 C19 H19 122.9 . . ? C18 C19 H19 122.9 . . ? C19 C20 C21 114.7(7) . . ? C19 C20 H20 122.7 . . ? C21 C20 H20 122.7 . . ? C22 C21 C20 126.5(7) . . ? C22 C21 S3 124.3(6) . . ? C20 C21 S3 108.9(5) . . ? C23 C22 C21 127.7(7) . . ? C23 C22 C53 115.0(7) . . ? C21 C22 C53 117.2(7) . . ? C22 C23 C24 125.3(7) . . ? C22 C23 S4 125.9(6) . . ? C24 C23 S4 108.8(6) . . ? C25 C24 C23 114.7(7) . . ? C25 C24 H24 122.6 . . ? C23 C24 H24 122.6 . . ? C24 C25 C26 114.8(7) . . ? C24 C25 H25 122.6 . . ? C26 C25 H25 122.6 . . ? C27 C26 C25 125.8(7) . . ? C27 C26 S4 125.4(6) . . ? C25 C26 S4 108.6(6) . . ? C26 C27 C28 130.0(7) . . ? C26 C27 C59 114.5(7) . . ? C28 C27 C59 115.5(7) . . ? C29 C28 C33 114.5(7) . . ? C29 C28 C27 119.4(7) . . ? C33 C28 C27 126.1(7) . . ? C30 C29 C28 123.2(7) . . ? C30 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? C29 C30 C31 121.9(7) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C32 C31 C30 115.4(7) . . ? C32 C31 C34 125.3(7) . . ? C30 C31 C34 119.3(7) . . ? C33 C32 C31 121.6(7) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C28 123.3(7) . . ? C32 C33 H33 118.3 . . ? C28 C33 H33 118.3 . . ? C1 C34 C31 128.2(7) . . ? C1 C34 C65 116.1(7) . . ? C31 C34 C65 115.6(7) . . ? C40 C35 C36 115.0(10) . . ? C40 C35 C5 122.3(10) . . ? C36 C35 C5 122.6(10) . . ? F1 C36 C35 115.9(9) . . ? F1 C36 C37 123.1(14) . . ? C35 C36 C37 121.0(14) . . ? C38 C37 C36 120.1(16) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 121.7(17) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C40 117.8(17) . . ? C38 C39 H39 121.1 . . ? C40 C39 H39 121.1 . . ? C35 C40 F2 117.6(11) . . ? C35 C40 C39 124.2(14) . . ? F2 C40 C39 118.2(15) . . ? C46 C41 C42 115.9(7) . . ? C46 C41 C10 123.2(8) . . ? C42 C41 C10 120.9(8) . . ? F7 C42 C43 117.8(8) . . ? F7 C42 C41 119.3(8) . . ? C43 C42 C41 122.9(8) . . ? F6 C43 C44 120.0(9) . . ? F6 C43 C42 121.5(9) . . ? C44 C43 C42 118.6(8) . . ? C43 C44 F5 119.3(10) . . ? C43 C44 C45 120.5(8) . . ? F5 C44 C45 120.1(10) . . ? F4 C45 C44 119.6(9) . . ? F4 C45 C46 120.9(9) . . ? C44 C45 C46 119.6(8) . . ? F3 C46 C41 119.4(7) . . ? F3 C46 C45 118.0(8) . . ? C41 C46 C45 122.5(8) . . ? C52 C47 C48 115.4(7) . . ? C52 C47 C17 122.5(7) . . ? C48 C47 C17 122.1(7) . . ? F8 C48 C49 117.3(8) . . ? F8 C48 C47 119.4(7) . . ? C49 C48 C47 123.3(8) . . ? C50 C49 F9 119.6(9) . . ? C50 C49 C48 119.5(9) . . ? F9 C49 C48 121.0(10) . . ? F10 C50 C49 119.8(11) . . ? F10 C50 C51 120.4(11) . . ? C49 C50 C51 119.8(9) . . ? F11 C51 C50 120.0(11) . . ? F11 C51 C52 119.5(11) . . ? C50 C51 C52 120.5(9) . . ? F12 C52 C51 118.1(9) . . ? F12 C52 C47 120.4(8) . . ? C51 C52 C47 121.5(8) . . ? C58 C53 C54 114.0(8) . . ? C58 C53 C22 124.1(7) . . ? C54 C53 C22 121.8(8) . . ? F13 C54 C55 117.3(9) . . ? F13 C54 C53 118.3(8) . . ? C55 C54 C53 124.4(9) . . ? C56 C55 C54 117.5(9) . . ? C56 C55 H55 121.2 . . ? C54 C55 H55 121.2 . . ? C57 C56 C55 121.6(9) . . ? C57 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C56 C57 C58 118.6(9) . . ? C56 C57 H57 120.7 . . ? C58 C57 H57 120.7 . . ? F14 C58 C57 118.5(9) . . ? F14 C58 C53 117.6(7) . . ? C57 C58 C53 123.8(8) . . ? C60 C59 C64 116.2(9) . . ? C60 C59 C27 120.9(9) . . ? C64 C59 C27 122.9(9) . . ? F15 C60 C59 119.8(9) . . ? F15 C60 C61 118.6(12) . . ? C59 C60 C61 121.7(12) . . ? F16 C61 C62 122.5(15) . . ? F16 C61 C60 119.0(16) . . ? C62 C61 C60 118.5(12) . . ? C63 C62 F17 121.3(17) . . ? C63 C62 C61 121.6(12) . . ? F17 C62 C61 117.1(17) . . ? F18 C63 C62 119.7(13) . . ? F18 C63 C64 122.0(16) . . ? C62 C63 C64 118.3(13) . . ? F19 C64 C63 116.8(12) . . ? F19 C64 C59 119.5(9) . . ? C63 C64 C59 123.7(12) . . ? C66 C65 C70 115.4(9) . . ? C66 C65 C34 122.3(9) . . ? C70 C65 C34 122.3(9) . . ? C67 C66 F20 118.9(12) . . ? C67 C66 C65 123.7(11) . . ? F20 C66 C65 117.4(9) . . ? C68 C67 C66 120.7(13) . . ? C68 C67 F21 118.3(13) . . ? C66 C67 F21 121.0(15) . . ? C67 C68 F22 122.0(17) . . ? C67 C68 C69 120.1(11) . . ? F22 C68 C69 118.0(16) . . ? F23 C69 C68 121.4(13) . . ? F23 C69 C70 119.8(15) . . ? C68 C69 C70 118.8(12) . . ? F24 C70 C65 119.8(8) . . ? F24 C70 C69 118.7(11) . . ? C65 C70 C69 121.4(11) . . ? Cl3 C71 Cl2 106.3(11) . . ? Cl3 C71 Cl1 103.5(10) . . ? Cl2 C71 Cl1 101.1(9) . . ? Cl3 C71 H71 114.8 . . ? Cl2 C71 H71 114.8 . . ? Cl1 C71 H71 114.8 . . ? Cl7 C73 Cl8 103.7(9) . . ? Cl7 C73 Cl9 106.6(10) . . ? Cl8 C73 Cl9 104.2(9) . . ? Cl7 C73 H73 113.8 . . ? Cl8 C73 H73 113.8 . . ? Cl9 C73 H73 113.8 . . ? C4 S1 C1 93.1(4) . . ? C6 S2 C9 93.0(4) . . ? C18 S3 C21 92.7(4) . . ? C23 S4 C26 93.0(4) . . ? Cl4 C72 Cl5 118.8(8) . . ? Cl4 C72 Cl6 97.7(7) . . ? Cl5 C72 Cl6 128.5(10) . . ? Cl4 C72 H72 102.8 . . ? Cl5 C72 H72 102.8 . . ? Cl6 C72 H72 102.8 . . ? C72 Cl6 Cl4' 36.4(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 C34 C1 C2 C3 177.8(8) . . . . ? S1 C1 C2 C3 1.3(10) . . . . ? C1 C2 C3 C4 -0.6(12) . . . . ? C2 C3 C4 C5 179.2(8) . . . . ? C2 C3 C4 S1 -0.3(10) . . . . ? C3 C4 C5 C6 -172.2(8) . . . . ? S1 C4 C5 C6 7.3(12) . . . . ? C3 C4 C5 C35 8.3(13) . . . . ? S1 C4 C5 C35 -172.2(7) . . . . ? C4 C5 C6 C7 -172.0(8) . . . . ? C35 C5 C6 C7 7.5(12) . . . . ? C4 C5 C6 S2 13.3(12) . . . . ? C35 C5 C6 S2 -167.2(7) . . . . ? C5 C6 C7 C8 -174.9(7) . . . . ? S2 C6 C7 C8 0.5(9) . . . . ? C6 C7 C8 C9 1.4(11) . . . . ? C7 C8 C9 C10 175.6(8) . . . . ? C7 C8 C9 S2 -2.6(9) . . . . ? C8 C9 C10 C11 -169.9(8) . . . . ? S2 C9 C10 C11 8.0(12) . . . . ? C8 C9 C10 C41 5.9(11) . . . . ? S2 C9 C10 C41 -176.2(6) . . . . ? C9 C10 C11 C12 6.6(13) . . . . ? C41 C10 C11 C12 -169.2(7) . . . . ? C9 C10 C11 C16 -177.8(8) . . . . ? C41 C10 C11 C16 6.4(11) . . . . ? C16 C11 C12 C13 -1.6(11) . . . . ? C10 C11 C12 C13 174.2(8) . . . . ? C11 C12 C13 C14 -0.6(12) . . . . ? C12 C13 C14 C15 2.1(11) . . . . ? C12 C13 C14 C17 -174.7(7) . . . . ? C13 C14 C15 C16 -1.4(12) . . . . ? C17 C14 C15 C16 175.5(8) . . . . ? C14 C15 C16 C11 -0.8(13) . . . . ? C12 C11 C16 C15 2.3(12) . . . . ? C10 C11 C16 C15 -173.7(8) . . . . ? C13 C14 C17 C18 -24.1(12) . . . . ? C15 C14 C17 C18 159.2(8) . . . . ? C13 C14 C17 C47 160.4(7) . . . . ? C15 C14 C17 C47 -16.3(11) . . . . ? C14 C17 C18 C19 173.6(8) . . . . ? C47 C17 C18 C19 -10.7(11) . . . . ? C14 C17 C18 S3 -15.3(12) . . . . ? C47 C17 C18 S3 160.4(6) . . . . ? C17 C18 C19 C20 168.3(8) . . . . ? S3 C18 C19 C20 -3.9(9) . . . . ? C18 C19 C20 C21 0.8(11) . . . . ? C19 C20 C21 C22 -170.9(8) . . . . ? C19 C20 C21 S3 2.6(9) . . . . ? C20 C21 C22 C23 -176.3(8) . . . . ? S3 C21 C22 C23 11.2(12) . . . . ? C20 C21 C22 C53 7.2(12) . . . . ? S3 C21 C22 C53 -165.3(6) . . . . ? C21 C22 C23 C24 -163.7(8) . . . . ? C53 C22 C23 C24 12.9(12) . . . . ? C21 C22 C23 S4 16.2(13) . . . . ? C53 C22 C23 S4 -167.2(6) . . . . ? C22 C23 C24 C25 178.0(8) . . . . ? S4 C23 C24 C25 -1.9(10) . . . . ? C23 C24 C25 C26 2.5(12) . . . . ? C24 C25 C26 C27 173.7(8) . . . . ? C24 C25 C26 S4 -1.8(10) . . . . ? C25 C26 C27 C28 -173.2(8) . . . . ? S4 C26 C27 C28 1.6(13) . . . . ? C25 C26 C27 C59 5.4(12) . . . . ? S4 C26 C27 C59 -179.8(7) . . . . ? C26 C27 C28 C29 159.2(8) . . . . ? C59 C27 C28 C29 -19.4(11) . . . . ? C26 C27 C28 C33 -20.4(14) . . . . ? C59 C27 C28 C33 161.0(8) . . . . ? C33 C28 C29 C30 2.4(12) . . . . ? C27 C28 C29 C30 -177.3(8) . . . . ? C28 C29 C30 C31 -4.0(13) . . . . ? C29 C30 C31 C32 2.6(12) . . . . ? C29 C30 C31 C34 -178.5(8) . . . . ? C30 C31 C32 C33 0.2(12) . . . . ? C34 C31 C32 C33 -178.6(8) . . . . ? C31 C32 C33 C28 -1.7(13) . . . . ? C29 C28 C33 C32 0.4(12) . . . . ? C27 C28 C33 C32 -179.9(8) . . . . ? C2 C1 C34 C31 175.4(8) . . . . ? S1 C1 C34 C31 -8.7(13) . . . . ? C2 C1 C34 C65 -5.3(12) . . . . ? S1 C1 C34 C65 170.6(6) . . . . ? C32 C31 C34 C1 -16.6(13) . . . . ? C30 C31 C34 C1 164.6(8) . . . . ? C32 C31 C34 C65 164.1(8) . . . . ? C30 C31 C34 C65 -14.7(11) . . . . ? C4 C5 C35 C40 -93.3(10) . . . . ? C6 C5 C35 C40 87.1(11) . . . . ? C4 C5 C35 C36 89.6(11) . . . . ? C6 C5 C35 C36 -90.0(11) . . . . ? C40 C35 C36 F1 179.9(11) . . . . ? C5 C35 C36 F1 -2.8(16) . . . . ? C40 C35 C36 C37 -2.0(16) . . . . ? C5 C35 C36 C37 175.2(10) . . . . ? F1 C36 C37 C38 179.0(15) . . . . ? C35 C36 C37 C38 1(2) . . . . ? C36 C37 C38 C39 1(3) . . . . ? C37 C38 C39 C40 -3(2) . . . . ? C36 C35 C40 F2 -179.8(10) . . . . ? C5 C35 C40 F2 2.9(15) . . . . ? C36 C35 C40 C39 0.7(16) . . . . ? C5 C35 C40 C39 -176.6(10) . . . . ? C38 C39 C40 C35 2(2) . . . . ? C38 C39 C40 F2 -177.9(14) . . . . ? C9 C10 C41 C46 89.8(9) . . . . ? C11 C10 C41 C46 -93.7(9) . . . . ? C9 C10 C41 C42 -90.1(9) . . . . ? C11 C10 C41 C42 86.3(9) . . . . ? C46 C41 C42 F7 -177.3(7) . . . . ? C10 C41 C42 F7 2.7(11) . . . . ? C46 C41 C42 C43 1.9(11) . . . . ? C10 C41 C42 C43 -178.2(7) . . . . ? F7 C42 C43 F6 -1.6(12) . . . . ? C41 C42 C43 F6 179.3(7) . . . . ? F7 C42 C43 C44 177.2(7) . . . . ? C41 C42 C43 C44 -1.9(13) . . . . ? F6 C43 C44 F5 -0.3(13) . . . . ? C42 C43 C44 F5 -179.2(7) . . . . ? F6 C43 C44 C45 179.8(8) . . . . ? C42 C43 C44 C45 1.0(13) . . . . ? C43 C44 C45 F4 179.4(8) . . . . ? F5 C44 C45 F4 -0.5(13) . . . . ? C43 C44 C45 C46 -0.2(13) . . . . ? F5 C44 C45 C46 180.0(8) . . . . ? C42 C41 C46 F3 179.5(6) . . . . ? C10 C41 C46 F3 -0.4(11) . . . . ? C42 C41 C46 C45 -1.0(11) . . . . ? C10 C41 C46 C45 179.0(7) . . . . ? F4 C45 C46 F3 0.2(12) . . . . ? C44 C45 C46 F3 179.7(7) . . . . ? F4 C45 C46 C41 -179.3(8) . . . . ? C44 C45 C46 C41 0.2(13) . . . . ? C14 C17 C47 C52 -63.7(10) . . . . ? C18 C17 C47 C52 120.1(8) . . . . ? C14 C17 C47 C48 115.8(8) . . . . ? C18 C17 C47 C48 -60.3(10) . . . . ? C52 C47 C48 F8 177.6(7) . . . . ? C17 C47 C48 F8 -2.0(11) . . . . ? C52 C47 C48 C49 -2.8(12) . . . . ? C17 C47 C48 C49 177.7(8) . . . . ? F8 C48 C49 C50 -178.8(8) . . . . ? C47 C48 C49 C50 1.6(14) . . . . ? F8 C48 C49 F9 2.0(12) . . . . ? C47 C48 C49 F9 -177.6(8) . . . . ? F9 C49 C50 F10 -0.8(14) . . . . ? C48 C49 C50 F10 -180.0(8) . . . . ? F9 C49 C50 C51 179.0(9) . . . . ? C48 C49 C50 C51 -0.2(15) . . . . ? F10 C50 C51 F11 0.2(16) . . . . ? C49 C50 C51 F11 -179.6(9) . . . . ? F10 C50 C51 C52 -180.0(9) . . . . ? C49 C50 C51 C52 0.3(16) . . . . ? F11 C51 C52 F12 -0.5(14) . . . . ? C50 C51 C52 F12 179.6(9) . . . . ? F11 C51 C52 C47 178.2(9) . . . . ? C50 C51 C52 C47 -1.6(15) . . . . ? C48 C47 C52 F12 -178.5(7) . . . . ? C17 C47 C52 F12 1.0(12) . . . . ? C48 C47 C52 C51 2.7(12) . . . . ? C17 C47 C52 C51 -177.7(8) . . . . ? C23 C22 C53 C58 -111.3(9) . . . . ? C21 C22 C53 C58 65.7(11) . . . . ? C23 C22 C53 C54 64.3(10) . . . . ? C21 C22 C53 C54 -118.8(8) . . . . ? C58 C53 C54 F13 -178.5(7) . . . . ? C22 C53 C54 F13 5.6(11) . . . . ? C58 C53 C54 C55 1.9(12) . . . . ? C22 C53 C54 C55 -174.1(8) . . . . ? F13 C54 C55 C56 179.1(9) . . . . ? C53 C54 C55 C56 -1.3(14) . . . . ? C54 C55 C56 C57 -0.7(16) . . . . ? C55 C56 C57 C58 1.8(17) . . . . ? C56 C57 C58 F14 177.3(9) . . . . ? C56 C57 C58 C53 -1.2(15) . . . . ? C54 C53 C58 F14 -179.1(7) . . . . ? C22 C53 C58 F14 -3.2(12) . . . . ? C54 C53 C58 C57 -0.6(13) . . . . ? C22 C53 C58 C57 175.2(9) . . . . ? C26 C27 C59 C60 103.9(9) . . . . ? C28 C27 C59 C60 -77.3(10) . . . . ? C26 C27 C59 C64 -78.8(10) . . . . ? C28 C27 C59 C64 100.0(10) . . . . ? C64 C59 C60 F15 179.6(8) . . . . ? C27 C59 C60 F15 -3.0(12) . . . . ? C64 C59 C60 C61 -1.3(13) . . . . ? C27 C59 C60 C61 176.2(8) . . . . ? F15 C60 C61 F16 -0.3(13) . . . . ? C59 C60 C61 F16 -179.5(8) . . . . ? F15 C60 C61 C62 179.6(9) . . . . ? C59 C60 C61 C62 0.4(14) . . . . ? F16 C61 C62 C63 -179.3(10) . . . . ? C60 C61 C62 C63 0.8(17) . . . . ? F16 C61 C62 F17 -0.2(16) . . . . ? C60 C61 C62 F17 179.9(8) . . . . ? F17 C62 C63 F18 1.6(17) . . . . ? C61 C62 C63 F18 -179.4(10) . . . . ? F17 C62 C63 C64 180.0(9) . . . . ? C61 C62 C63 C64 -1.0(18) . . . . ? F18 C63 C64 F19 0.3(15) . . . . ? C62 C63 C64 F19 -178.1(10) . . . . ? F18 C63 C64 C59 178.4(9) . . . . ? C62 C63 C64 C59 0.0(16) . . . . ? C60 C59 C64 F19 179.1(8) . . . . ? C27 C59 C64 F19 1.7(14) . . . . ? C60 C59 C64 C63 1.1(14) . . . . ? C27 C59 C64 C63 -176.3(9) . . . . ? C1 C34 C65 C66 109.1(9) . . . . ? C31 C34 C65 C66 -71.6(10) . . . . ? C1 C34 C65 C70 -73.1(10) . . . . ? C31 C34 C65 C70 106.3(9) . . . . ? C70 C65 C66 C67 -1.3(14) . . . . ? C34 C65 C66 C67 176.6(9) . . . . ? C70 C65 C66 F20 -179.9(8) . . . . ? C34 C65 C66 F20 -2.0(13) . . . . ? F20 C66 C67 C68 178.8(10) . . . . ? C65 C66 C67 C68 0.2(17) . . . . ? F20 C66 C67 F21 -1.6(16) . . . . ? C65 C66 C67 F21 179.8(9) . . . . ? C66 C67 C68 F22 -179.8(9) . . . . ? F21 C67 C68 F22 0.5(17) . . . . ? C66 C67 C68 C69 0.6(18) . . . . ? F21 C67 C68 C69 -179.0(10) . . . . ? C67 C68 C69 F23 179.4(10) . . . . ? F22 C68 C69 F23 -0.3(16) . . . . ? C67 C68 C69 C70 -0.2(17) . . . . ? F22 C68 C69 C70 -179.8(8) . . . . ? C66 C65 C70 F24 178.6(8) . . . . ? C34 C65 C70 F24 0.7(13) . . . . ? C66 C65 C70 C69 1.7(13) . . . . ? C34 C65 C70 C69 -176.3(8) . . . . ? F23 C69 C70 F24 2.4(14) . . . . ? C68 C69 C70 F24 -178.0(9) . . . . ? F23 C69 C70 C65 179.4(9) . . . . ? C68 C69 C70 C65 -1.0(15) . . . . ? C5 C4 S1 C1 -178.6(7) . . . . ? C3 C4 S1 C1 0.9(6) . . . . ? C34 C1 S1 C4 -177.7(7) . . . . ? C2 C1 S1 C4 -1.2(6) . . . . ? C5 C6 S2 C9 173.7(7) . . . . ? C7 C6 S2 C9 -1.8(6) . . . . ? C10 C9 S2 C6 -175.8(7) . . . . ? C8 C9 S2 C6 2.4(6) . . . . ? C19 C18 S3 C21 4.5(6) . . . . ? C17 C18 S3 C21 -167.8(7) . . . . ? C22 C21 S3 C18 169.6(7) . . . . ? C20 C21 S3 C18 -4.1(6) . . . . ? C22 C23 S4 C26 -179.2(7) . . . . ? C24 C23 S4 C26 0.7(6) . . . . ? C27 C26 S4 C23 -175.0(7) . . . . ? C25 C26 S4 C23 0.5(7) . . . . ? Cl4 C72 Cl6 Cl4' 139.4(14) . . . . ? Cl5 C72 Cl6 Cl4' -83.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 19.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.629 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.068 # start Validation Reply Form _vrf_DIFF019_sree3 ; PROBLEM: _diffrn_standards_number is missing RESPONSE: In the Kappa apex2 CCD diffractometer there is no provision for repeat measurement of standard intensity. Instead, the decay correction is achieved indirectly by noting the intensity of equivalent reflections and time of their measurement during the data collection. ; _vrf_DIFF020_sree3 ; PROBLEM: _diffrn_standards_interval_count and RESPONSE: In the Kappa apex2 CCD diffractometer there is no provision for repeat measurement of standard intensity. Instead, the decay correction is achieved indirectly by noting the intensity of equivalent reflections and time of their measurement during the data collection. ; _vrf_THETM01_sree3 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The compound has high mosaic spread and practically there are no reflections present above 19.5\%.During data collection maximum theta was set as 28\%(d=0.75). However after integration it was found that there are no reflections above 19.5\%.The repeatetion of data collection with new crop of crystals didnot improve the situation. ; _vrf_PLAT023_sree3 ; PROBLEM: Resolution (too) Low [sin(th)/Lambda < 0.6]..... 19.34 Deg. RESPONSE: The compound has high mosaic spread and practically there are no reflections present above 19.5\%.During data collection maximum theta was set as 28\%(d=0.75). However after integration it was found that there are no reflections above 19.5\%.The repeatetion of data collection with new crop of crystals didnot improve the situation. ; _vrf_PLAT027_sree3 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 19.34 Deg. RESPONSE: The compound has high mosaic spread and practically there are no reflections present above 19.5\%.During data collection maximum theta was set as 28\%(d=0.75). However after integration it was found that there are no reflections above 19.5\%.The repeatetion of data collection with new crop of crystals didnot improve the situation. ; # end Validation Reply Form.