# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/115 data_1 _audit_creation_method SHELXL-97 _publ_contact_author ; Dr Erkki Kolehmainen ; _publ_contact_author_email ekolehma@cc.jyu.fi _publ_author_name ; Kolehmainen, Erkki Koivisto, Jari Nissinen Maij Laihia, Katri Rissanen, Kari ; _publ_requested_journal 'New Journal of Chemistry' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C24 H16 Cl8 O4, C H Cl3' _chemical_formula_sum 'C25 H17 Cl11 O4' _chemical_formula_weight 771.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _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 13.281(1) _cell_length_b 13.328(1) _cell_length_c 19.818(1) _cell_angle_alpha 105.40(1) _cell_angle_beta 92.78(1) _cell_angle_gamma 113.24(1) _cell_volume 3060.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 3953 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7827 _exptl_absorpt_correction_T_max 0.9503 _exptl_special_details ; Structure solution by direct methods ; _diffrn_ambient_temperature 173.0(1) _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 'Nonius KappaCCD diffractometer' _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 14140 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1973 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.90 _reflns_number_total 14140 _reflns_number_gt 6512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'Denzo v0.93.0 (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo v0.93.0 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX-98 (Farrugia,1998)' _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 w=1/[\s^2^(Fo^2^)+(0.1368P)^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 14140 _refine_ls_number_parameters 729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2089 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2648 _refine_ls_wR_factor_gt 0.2065 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C5 C 0.2176(6) 0.9322(5) 0.1361(4) 0.0289(15) Uani 1 d . . . C5B C -0.3472(6) 0.2519(6) 0.2515(4) 0.0343(16) Uani 1 d . . . C5C C -0.3492(6) 0.8565(6) 0.3242(4) 0.0330(16) Uani 1 d . . . C5D C -0.6958(5) 0.5742(6) 0.1912(4) 0.0283(15) Uani 1 d . . . C4 C 0.1025(6) 0.9240(6) 0.1532(4) 0.0299(15) Uani 1 d . . . C4B C -0.2337(5) 0.2607(6) 0.2327(4) 0.0294(15) Uani 1 d . . . C4C C -0.2757(5) 0.7920(5) 0.3187(3) 0.0260(14) Uani 1 d . . . C4D C -0.6764(5) 0.5681(5) 0.1150(4) 0.0291(15) Uani 1 d . . . C3A C 0.0463(6) 0.8095(6) 0.1653(4) 0.0284(15) Uani 1 d . . . C3AB C -0.1780(6) 0.3726(6) 0.2176(4) 0.0309(16) Uani 1 d . . . C3AC C -0.1826(5) 0.8618(6) 0.3809(3) 0.0283(15) Uani 1 d . . . C3AD C -0.7868(5) 0.5418(5) 0.0753(4) 0.0280(15) Uani 1 d . . . C3 C -0.0387(6) 0.7042(6) 0.1400(4) 0.0301(16) Uani 1 d . . . H3 H -0.0944 0.6762 0.0992 0.036 Uiso 1 calc R . . C3B C -0.0884(6) 0.4739(5) 0.2384(3) 0.0272(15) Uani 1 d . . . H3B H -0.0305 0.5012 0.2777 0.033 Uiso 1 calc R . . C3C C -0.0725(6) 0.9256(6) 0.4010(4) 0.0310(16) Uani 1 d . . . H3C H -0.0190 0.9420 0.3707 0.037 Uiso 1 calc R . . C3D C -0.8434(5) 0.5861(5) 0.0427(3) 0.0279(15) Uani 1 d . . . H3D H -0.8147 0.6600 0.0364 0.033 Uiso 1 calc R . . C2 C -0.0272(5) 0.6410(5) 0.1894(3) 0.0257(14) Uani 1 d . . . C2B C -0.0983(5) 0.5357(5) 0.1867(4) 0.0281(15) Uani 1 d . . . C2C C -0.0508(5) 0.9654(6) 0.4795(4) 0.0296(15) Uani 1 d . . . C2D C -0.9574(5) 0.4975(5) 0.0192(4) 0.0272(15) Uani 1 d . . . C1 C 0.0739(5) 0.7192(5) 0.2439(4) 0.0304(16) Uani 1 d . . . H1 H 0.1030 0.7020 0.2819 0.036 Uiso 1 calc R . . C1B C -0.2020(5) 0.4593(5) 0.1354(4) 0.0261(15) Uani 1 d . . . H1B H -0.2308 0.4746 0.0963 0.031 Uiso 1 calc R . . C1C C -0.1572(5) 0.9164(6) 0.5028(4) 0.0307(15) Uani 1 d . . . H1C H -0.1688 0.9265 0.5506 0.037 Uiso 1 calc R . . C1D C -0.9657(6) 0.3969(6) 0.0419(4) 0.0304(16) Uani 1 d . . . H1D H -1.0302 0.3275 0.0349 0.036 Uiso 1 calc R . . C7A C 0.1158(5) 0.8185(5) 0.2291(3) 0.0260(14) Uani 1 d . . . C7AB C -0.2479(5) 0.3634(5) 0.1546(3) 0.0252(14) Uani 1 d . . . C7AC C -0.2344(5) 0.8554(5) 0.4454(4) 0.0281(15) Uani 1 d . . . C7AD C -0.8635(5) 0.4247(5) 0.0743(3) 0.0253(14) Uani 1 d . . . C7 C 0.2077(5) 0.9385(5) 0.2529(4) 0.0277(15) Uani 1 d . . . C7B C -0.3429(5) 0.2456(5) 0.1343(3) 0.0258(14) Uani 1 d . . . C7C C -0.3570(6) 0.7830(6) 0.4174(4) 0.0320(16) Uani 1 d . . . C7D C -0.7920(5) 0.3882(5) 0.1148(4) 0.0287(15) Uani 1 d . . . C6 C 0.2787(6) 0.9432(5) 0.1953(4) 0.0302(16) Uani 1 d . . . C6B C -0.4097(5) 0.2436(5) 0.1947(4) 0.0299(15) Uani 1 d . . . C6C C -0.3966(6) 0.8512(6) 0.3806(4) 0.0336(16) Uani 1 d . . . C6D C -0.7633(5) 0.4701(6) 0.1907(4) 0.0295(15) Uani 1 d . . . C8 C 0.1422(6) 1.0067(5) 0.2324(4) 0.0296(15) Uani 1 d . . . C8B C -0.2765(5) 0.1759(5) 0.1534(3) 0.0241(14) Uani 1 d . . . C8C C -0.3496(6) 0.6929(6) 0.3496(4) 0.0319(16) Uani 1 d . . . C8D C -0.6777(5) 0.4445(6) 0.0888(4) 0.0305(16) Uani 1 d . . . C10 C 0.2606(6) 1.2026(6) 0.2986(4) 0.0427(19) Uani 1 d . . . H10A H 0.2155 1.1867 0.3354 0.064 Uiso 1 calc R . . H10B H 0.2729 1.2783 0.2950 0.064 Uiso 1 calc R . . H10C H 0.3324 1.2015 0.3111 0.064 Uiso 1 calc R . . C10B C -0.1186(6) 0.1392(7) 0.1216(4) 0.045(2) Uani 1 d . . . H10D H -0.0574 0.1979 0.1594 0.067 Uiso 1 calc R . . H10E H -0.0893 0.1198 0.0779 0.067 Uiso 1 calc R . . H10F H -0.1544 0.0703 0.1361 0.067 Uiso 1 calc R . . C9C C -0.5266(7) 0.5286(7) 0.3190(5) 0.048(2) Uani 1 d . . . H9C1 H -0.4894 0.5039 0.3509 0.073 Uiso 1 calc R . . H9C2 H -0.5682 0.4637 0.2762 0.073 Uiso 1 calc R . . H9C3 H -0.5779 0.5557 0.3432 0.073 Uiso 1 calc R . . C10D C -0.4862(6) 0.4766(6) 0.1134(5) 0.0418(19) Uani 1 d . . . H10G H -0.4858 0.4866 0.0661 0.063 Uiso 1 calc R . . H10H H -0.4487 0.4276 0.1171 0.063 Uiso 1 calc R . . H10I H -0.4472 0.5518 0.1497 0.063 Uiso 1 calc R . . C9 C -0.0149(6) 1.0466(7) 0.2597(4) 0.0434(19) Uani 1 d . . . H9A H 0.0246 1.1136 0.2442 0.065 Uiso 1 calc R . . H9B H -0.0439 1.0700 0.3028 0.065 Uiso 1 calc R . . H9C H -0.0767 0.9888 0.2221 0.065 Uiso 1 calc R . . C9B C -0.3914(7) -0.0222(6) 0.0926(4) 0.046(2) Uani 1 d . . . H9B1 H -0.4598 -0.0182 0.0756 0.069 Uiso 1 calc R . . H9B2 H -0.4098 -0.0967 0.1002 0.069 Uiso 1 calc R . . H9B3 H -0.3423 -0.0133 0.0572 0.069 Uiso 1 calc R . . C10C C -0.2642(7) 0.5626(6) 0.3204(4) 0.046(2) Uani 1 d . . . H10J H -0.3233 0.5222 0.2785 0.068 Uiso 1 calc R . . H10K H -0.2522 0.5064 0.3392 0.068 Uiso 1 calc R . . H10L H -0.1953 0.6095 0.3069 0.068 Uiso 1 calc R . . C9D C -0.6949(7) 0.3027(6) -0.0209(4) 0.045(2) Uani 1 d . . . H9D1 H -0.6552 0.2776 0.0092 0.068 Uiso 1 calc R . . H9D2 H -0.6648 0.3022 -0.0651 0.068 Uiso 1 calc R . . H9D3 H -0.7742 0.2504 -0.0320 0.068 Uiso 1 calc R . . C100 C 0.1372(11) 0.7330(12) 0.4706(6) 0.098(4) Uani 1 d . . . H100 H 0.0970 0.6641 0.4861 0.117 Uiso 1 calc R . . C101 C -0.1866(8) 0.5890(8) 0.5092(5) 0.063(3) Uani 1 d . . . H101 H -0.1901 0.6398 0.4809 0.076 Uiso 1 calc R . . Cl5 Cl 0.24872(17) 0.91548(16) 0.05318(10) 0.0442(5) Uani 1 d . . . Cl5B Cl -0.38105(18) 0.25706(17) 0.33389(10) 0.0486(5) Uani 1 d . . . Cl5C Cl -0.34857(16) 0.93718(16) 0.26995(11) 0.0461(5) Uani 1 d . . . Cl5D Cl -0.65230(15) 0.69846(15) 0.25913(10) 0.0397(4) Uani 1 d . . . Cl4 Cl 0.02733(15) 0.95521(15) 0.09210(10) 0.0391(4) Uani 1 d . . . Cl4B Cl -0.15492(15) 0.23082(15) 0.29180(10) 0.0386(4) Uani 1 d . . . Cl4C Cl -0.23897(15) 0.75145(15) 0.23505(9) 0.0380(4) Uani 1 d . . . Cl7 Cl 0.27929(15) 0.98607(15) 0.34028(9) 0.0366(4) Uani 1 d . . . Cl4D Cl -0.56128(15) 0.68386(15) 0.10447(10) 0.0386(4) Uani 1 d . . . Cl7B Cl -0.41864(15) 0.19554(15) 0.04830(10) 0.0386(4) Uani 1 d . . . Cl7C Cl -0.43651(16) 0.72839(17) 0.47868(11) 0.0469(5) Uani 1 d . . . Cl7D Cl -0.83834(15) 0.24184(14) 0.10769(10) 0.0383(4) Uani 1 d . . . Cl6 Cl 0.40869(15) 0.94946(16) 0.20478(11) 0.0418(5) Uani 1 d . . . Cl6B Cl -0.54072(15) 0.23735(16) 0.18641(11) 0.0427(5) Uani 1 d . . . Cl6C Cl -0.47647(17) 0.91830(18) 0.41451(13) 0.0552(6) Uani 1 d . . . Cl6D Cl -0.82681(16) 0.42988(17) 0.25792(10) 0.0434(5) Uani 1 d . . . Cl50 Cl 0.0365(3) 0.7517(3) 0.42684(14) 0.0805(8) Uani 1 d . . . Cl51 Cl 0.2047(4) 0.8439(3) 0.5478(2) 0.1449(18) Uani 1 d . . . Cl52 Cl 0.2206(4) 0.6963(5) 0.4157(2) 0.174(2) Uani 1 d . . . Cl53 Cl -0.1424(3) 0.4877(2) 0.45828(15) 0.0861(9) Uani 1 d . . . Cl54 Cl -0.3165(2) 0.5222(3) 0.5288(2) 0.1101(12) Uani 1 d . . . Cl55 Cl -0.0888(2) 0.6739(3) 0.58694(15) 0.1019(11) Uani 1 d . . . O2 O 0.2027(4) 1.1155(4) 0.2309(3) 0.0339(11) Uani 1 d . . . O2B O -0.1991(4) 0.1829(4) 0.1090(2) 0.0305(11) Uani 1 d . . . O1C O -0.4447(4) 0.6202(4) 0.2993(2) 0.0336(11) Uani 1 d . . . O2D O -0.5991(4) 0.4238(4) 0.1239(2) 0.0315(11) Uani 1 d . . . O1 O 0.0613(4) 0.9983(4) 0.2747(3) 0.0326(11) Uani 1 d . . . O1B O -0.3366(4) 0.0672(3) 0.1576(2) 0.0298(11) Uani 1 d . . . O2C O -0.2961(4) 0.6351(4) 0.3738(2) 0.0337(11) Uani 1 d . . . O1D O -0.6811(4) 0.4172(4) 0.0160(3) 0.0350(11) Uani 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 C5 0.033(4) 0.024(3) 0.030(4) 0.013(3) 0.013(3) 0.008(3) C5B 0.043(4) 0.030(4) 0.028(4) 0.015(3) 0.013(3) 0.009(3) C5C 0.028(4) 0.029(4) 0.035(4) 0.009(3) -0.003(3) 0.005(3) C5D 0.024(4) 0.034(4) 0.025(4) 0.011(3) -0.002(3) 0.011(3) C4 0.033(4) 0.031(4) 0.025(4) 0.014(3) 0.005(3) 0.010(3) C4B 0.029(4) 0.032(4) 0.027(4) 0.014(3) 0.002(3) 0.011(3) C4C 0.028(4) 0.025(3) 0.020(4) 0.007(3) 0.000(3) 0.007(3) C4D 0.025(4) 0.028(3) 0.036(4) 0.016(3) 0.002(3) 0.010(3) C3A 0.032(4) 0.033(4) 0.022(4) 0.011(3) 0.008(3) 0.014(3) C3AB 0.038(4) 0.029(4) 0.026(4) 0.008(3) 0.008(3) 0.015(3) C3AC 0.025(4) 0.036(4) 0.022(4) 0.009(3) 0.000(3) 0.011(3) C3AD 0.026(4) 0.026(3) 0.027(4) 0.008(3) 0.006(3) 0.006(3) C3 0.032(4) 0.040(4) 0.024(4) 0.015(3) 0.012(3) 0.017(3) C3B 0.032(4) 0.032(4) 0.019(4) 0.007(3) 0.004(3) 0.015(3) C3C 0.036(4) 0.036(4) 0.022(4) 0.013(3) 0.003(3) 0.014(3) C3D 0.034(4) 0.027(3) 0.025(4) 0.011(3) 0.001(3) 0.014(3) C2 0.026(4) 0.027(3) 0.027(4) 0.011(3) 0.010(3) 0.012(3) C2B 0.031(4) 0.027(3) 0.032(4) 0.015(3) 0.013(3) 0.012(3) C2C 0.031(4) 0.036(4) 0.023(4) 0.009(3) 0.009(3) 0.015(3) C2D 0.032(4) 0.030(4) 0.025(4) 0.011(3) 0.010(3) 0.016(3) C1 0.031(4) 0.026(3) 0.041(4) 0.022(3) 0.009(3) 0.012(3) C1B 0.027(4) 0.026(3) 0.029(4) 0.013(3) 0.008(3) 0.012(3) C1C 0.029(4) 0.040(4) 0.020(4) 0.007(3) 0.010(3) 0.011(3) C1D 0.033(4) 0.030(4) 0.033(4) 0.016(3) 0.002(3) 0.015(3) C7A 0.029(4) 0.029(3) 0.022(4) 0.011(3) 0.004(3) 0.013(3) C7AB 0.027(4) 0.026(3) 0.024(4) 0.011(3) 0.008(3) 0.011(3) C7AC 0.024(4) 0.031(4) 0.031(4) 0.012(3) 0.011(3) 0.012(3) C7AD 0.031(4) 0.024(3) 0.023(4) 0.014(3) 0.003(3) 0.010(3) C7 0.030(4) 0.032(4) 0.031(4) 0.023(3) 0.014(3) 0.014(3) C7B 0.026(4) 0.028(3) 0.024(4) 0.012(3) 0.005(3) 0.010(3) C7C 0.027(4) 0.045(4) 0.026(4) 0.016(3) 0.010(3) 0.014(3) C7D 0.029(4) 0.032(4) 0.035(4) 0.024(3) 0.011(3) 0.014(3) C6 0.034(4) 0.026(3) 0.035(4) 0.016(3) 0.010(3) 0.013(3) C6B 0.030(4) 0.024(3) 0.031(4) 0.014(3) 0.008(3) 0.004(3) C6C 0.025(4) 0.039(4) 0.035(4) 0.010(3) 0.004(3) 0.012(3) C6D 0.025(4) 0.038(4) 0.029(4) 0.016(3) 0.001(3) 0.013(3) C8 0.038(4) 0.027(4) 0.028(4) 0.013(3) 0.010(3) 0.014(3) C8B 0.028(4) 0.023(3) 0.018(3) 0.010(3) 0.005(3) 0.005(3) C8C 0.029(4) 0.035(4) 0.030(4) 0.009(3) 0.001(3) 0.013(3) C8D 0.028(4) 0.030(4) 0.035(4) 0.015(3) 0.004(3) 0.012(3) C10 0.044(5) 0.025(4) 0.049(5) 0.013(4) 0.014(4) 0.003(3) C10B 0.035(4) 0.054(5) 0.054(5) 0.023(4) 0.004(4) 0.023(4) C9C 0.042(5) 0.042(4) 0.048(5) 0.019(4) 0.004(4) 0.002(4) C10D 0.021(4) 0.045(4) 0.065(6) 0.025(4) 0.005(4) 0.015(3) C9 0.039(4) 0.054(5) 0.051(5) 0.027(4) 0.017(4) 0.026(4) C9B 0.057(5) 0.031(4) 0.032(5) 0.000(4) 0.004(4) 0.007(4) C10C 0.059(5) 0.045(5) 0.038(5) 0.007(4) 0.003(4) 0.032(4) C9D 0.055(5) 0.032(4) 0.045(5) 0.011(4) 0.009(4) 0.014(4) C100 0.120(11) 0.121(10) 0.063(8) 0.013(7) 0.001(7) 0.074(9) C101 0.068(6) 0.080(7) 0.036(5) 0.020(5) -0.005(4) 0.027(5) Cl5 0.0568(13) 0.0500(11) 0.0308(10) 0.0203(9) 0.0229(9) 0.0209(10) Cl5B 0.0595(13) 0.0523(12) 0.0307(11) 0.0178(9) 0.0186(9) 0.0158(10) Cl5C 0.0440(11) 0.0432(11) 0.0534(13) 0.0252(10) -0.0017(9) 0.0153(9) Cl5D 0.0418(11) 0.0414(10) 0.0332(10) 0.0090(8) 0.0013(8) 0.0170(9) Cl4 0.0436(11) 0.0406(10) 0.0368(10) 0.0226(9) 0.0028(8) 0.0151(9) Cl4B 0.0442(11) 0.0360(9) 0.0332(10) 0.0182(8) -0.0039(8) 0.0109(8) Cl4C 0.0413(11) 0.0439(10) 0.0241(9) 0.0118(8) 0.0055(8) 0.0125(9) Cl7 0.0393(10) 0.0393(10) 0.0301(10) 0.0134(8) 0.0038(8) 0.0140(8) Cl4D 0.0323(10) 0.0342(9) 0.0487(12) 0.0226(9) 0.0079(8) 0.0072(8) Cl7B 0.0360(10) 0.0441(10) 0.0304(10) 0.0091(8) -0.0027(8) 0.0142(8) Cl7C 0.0414(11) 0.0538(12) 0.0401(12) 0.0186(10) 0.0168(9) 0.0109(10) Cl7D 0.0350(10) 0.0336(9) 0.0515(12) 0.0261(9) 0.0073(8) 0.0115(8) Cl6 0.0327(10) 0.0462(11) 0.0553(13) 0.0230(10) 0.0166(9) 0.0199(9) Cl6B 0.0314(10) 0.0476(11) 0.0541(13) 0.0212(10) 0.0143(9) 0.0173(9) Cl6C 0.0447(12) 0.0558(13) 0.0683(15) 0.0101(11) 0.0105(11) 0.0303(11) Cl6D 0.0410(11) 0.0588(12) 0.0410(11) 0.0313(10) 0.0147(9) 0.0208(10) Cl50 0.094(2) 0.109(2) 0.0596(17) 0.0362(16) 0.0185(15) 0.0567(18) Cl51 0.172(4) 0.088(2) 0.104(3) 0.028(2) -0.068(3) -0.003(2) Cl52 0.214(5) 0.348(7) 0.142(4) 0.166(5) 0.125(4) 0.234(6) Cl53 0.109(2) 0.0799(18) 0.0677(18) 0.0233(15) -0.0008(16) 0.0396(17) Cl54 0.0596(18) 0.141(3) 0.134(3) 0.083(3) 0.0121(18) 0.0206(19) Cl55 0.0695(19) 0.140(3) 0.0519(17) -0.0033(18) -0.0012(14) 0.0221(19) O2 0.043(3) 0.023(2) 0.035(3) 0.011(2) 0.012(2) 0.012(2) O2B 0.032(3) 0.033(3) 0.030(3) 0.012(2) 0.011(2) 0.014(2) O1C 0.030(3) 0.035(3) 0.029(3) 0.012(2) -0.001(2) 0.005(2) O2D 0.027(3) 0.037(3) 0.037(3) 0.022(2) 0.007(2) 0.014(2) O1 0.031(3) 0.038(3) 0.038(3) 0.018(2) 0.014(2) 0.019(2) O1B 0.034(3) 0.023(2) 0.028(3) 0.012(2) 0.004(2) 0.006(2) O2C 0.039(3) 0.040(3) 0.027(3) 0.014(2) 0.007(2) 0.018(2) O1D 0.034(3) 0.035(3) 0.038(3) 0.014(2) 0.007(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C5 C6 1.333(9) . ? C5 C4 1.549(9) . ? C5 Cl5 1.693(7) . ? C5B C6B 1.319(9) . ? C5B C4B 1.537(10) . ? C5B Cl5B 1.705(7) . ? C5C C6C 1.314(10) . ? C5C C4C 1.526(9) . ? C5C Cl5C 1.709(7) . ? C5D C6D 1.319(9) . ? C5D C4D 1.530(10) . ? C5D Cl5D 1.696(7) . ? C4 C3A 1.503(9) . ? C4 C8 1.581(9) . ? C4 Cl4 1.765(6) . ? C4B C3AB 1.500(9) . ? C4B C8B 1.592(9) . ? C4B Cl4B 1.755(6) . ? C4C C3AC 1.499(9) . ? C4C C8C 1.597(9) . ? C4C Cl4C 1.757(7) . ? C4D C3AD 1.493(9) . ? C4D C8D 1.583(9) . ? C4D Cl4D 1.761(7) . ? C3A C3 1.348(9) . ? C3A C7A 1.477(9) . ? C3AB C3B 1.341(9) . ? C3AB C7AB 1.466(9) . ? C3AC C3C 1.343(9) . ? C3AC C7AC 1.488(9) . ? C3AD C3D 1.356(8) . ? C3AD C7AD 1.484(9) . ? C3 C2 1.489(9) . ? C3B C2B 1.504(9) . ? C3C C2C 1.478(9) . ? C3D C2D 1.461(9) . ? C2 C2B 1.332(9) . ? C2 C1 1.487(9) . ? C2B C1B 1.476(9) . ? C2C C2C 1.358(13) 2_576 ? C2C C1C 1.460(9) . ? C2D C2D 1.365(12) 2_365 ? C2D C1D 1.491(8) . ? C1 C7A 1.337(8) . ? C1B C7AB 1.348(8) . ? C1C C7AC 1.320(9) . ? C1D C7AD 1.336(9) . ? C7A C7 1.508(9) . ? C7AB C7B 1.507(9) . ? C7AC C7C 1.509(9) . ? C7AD C7D 1.510(8) . ? C7 C6 1.514(9) . ? C7 C8 1.592(8) . ? C7 Cl7 1.756(7) . ? C7B C6B 1.525(9) . ? C7B C8B 1.608(8) . ? C7B Cl7B 1.749(7) . ? C7C C6C 1.524(9) . ? C7C C8C 1.583(10) . ? C7C Cl7C 1.763(7) . ? C7D C6D 1.531(10) . ? C7D C8D 1.586(9) . ? C7D Cl7D 1.761(6) . ? C6 Cl6 1.694(7) . ? C6B Cl6B 1.706(7) . ? C6C Cl6C 1.696(7) . ? C6D Cl6D 1.704(7) . ? C8 O2 1.362(8) . ? C8 O1 1.382(8) . ? C8B O2B 1.377(8) . ? C8B O1B 1.379(7) . ? C8C O2C 1.386(7) . ? C8C O1C 1.387(8) . ? C8D O2D 1.382(7) . ? C8D O1D 1.385(8) . ? C10 O2 1.452(9) . ? C10B O2B 1.446(7) . ? C9C O1C 1.439(8) . ? C10D O2D 1.436(8) . ? C9 O1 1.454(8) . ? C9B O1B 1.421(8) . ? C10C O2C 1.434(8) . ? C9D O1D 1.439(8) . ? C100 Cl50 1.694(11) . ? C100 Cl52 1.706(13) . ? C100 Cl51 1.718(12) . ? C101 Cl54 1.719(10) . ? C101 Cl55 1.750(9) . ? C101 Cl53 1.774(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C5 C4 108.1(6) . . ? C6 C5 Cl5 128.4(6) . . ? C4 C5 Cl5 123.2(5) . . ? C6B C5B C4B 108.7(6) . . ? C6B C5B Cl5B 127.2(6) . . ? C4B C5B Cl5B 124.1(5) . . ? C6C C5C C4C 109.4(6) . . ? C6C C5C Cl5C 128.2(6) . . ? C4C C5C Cl5C 121.8(5) . . ? C6D C5D C4D 107.7(6) . . ? C6D C5D Cl5D 127.7(6) . . ? C4D C5D Cl5D 124.0(5) . . ? C3A C4 C5 105.2(5) . . ? C3A C4 C8 100.7(5) . . ? C5 C4 C8 98.1(5) . . ? C3A C4 Cl4 117.1(5) . . ? C5 C4 Cl4 114.5(5) . . ? C8 C4 Cl4 118.6(4) . . ? C3AB C4B C5B 106.9(5) . . ? C3AB C4B C8B 99.5(5) . . ? C5B C4B C8B 97.9(5) . . ? C3AB C4B Cl4B 116.9(5) . . ? C5B C4B Cl4B 115.0(5) . . ? C8B C4B Cl4B 118.0(4) . . ? C3AC C4C C5C 104.9(5) . . ? C3AC C4C C8C 99.2(5) . . ? C5C C4C C8C 98.3(5) . . ? C3AC C4C Cl4C 117.1(5) . . ? C5C C4C Cl4C 116.2(5) . . ? C8C C4C Cl4C 118.1(4) . . ? C3AD C4D C5D 104.5(5) . . ? C3AD C4D C8D 99.1(5) . . ? C5D C4D C8D 99.8(5) . . ? C3AD C4D Cl4D 116.4(5) . . ? C5D C4D Cl4D 116.6(5) . . ? C8D C4D Cl4D 117.7(5) . . ? C3 C3A C7A 110.6(6) . . ? C3 C3A C4 144.6(6) . . ? C7A C3A C4 104.7(5) . . ? C3B C3AB C7AB 110.2(6) . . ? C3B C3AB C4B 143.9(6) . . ? C7AB C3AB C4B 105.9(5) . . ? C3C C3AC C7AC 108.9(6) . . ? C3C C3AC C4C 145.1(7) . . ? C7AC C3AC C4C 106.0(6) . . ? C3D C3AD C7AD 109.3(6) . . ? C3D C3AD C4D 143.7(6) . . ? C7AD C3AD C4D 106.9(5) . . ? C3A C3 C2 105.5(6) . . ? C3AB C3B C2B 106.1(6) . . ? C3AC C3C C2C 106.6(6) . . ? C3AD C3D C2D 106.1(5) . . ? C2B C2 C1 126.8(6) . . ? C2B C2 C3 125.6(6) . . ? C1 C2 C3 107.6(5) . . ? C2 C2B C1B 127.6(6) . . ? C2 C2B C3B 125.4(6) . . ? C1B C2B C3B 107.0(5) . . ? C2C C2C C1C 128.0(8) 2_576 . ? C2C C2C C3C 124.8(8) 2_576 . ? C1C C2C C3C 107.2(6) . . ? C2D C2D C3D 126.6(7) 2_365 . ? C2D C2D C1D 124.8(8) 2_365 . ? C3D C2D C1D 108.6(5) . . ? C7A C1 C2 106.7(6) . . ? C7AB C1B C2B 106.5(5) . . ? C7AC C1C C2C 107.7(6) . . ? C7AD C1D C2D 105.6(6) . . ? C1 C7A C3A 109.6(6) . . ? C1 C7A C7 144.0(6) . . ? C3A C7A C7 106.4(5) . . ? C1B C7AB C3AB 110.2(6) . . ? C1B C7AB C7B 143.8(6) . . ? C3AB C7AB C7B 105.9(5) . . ? C1C C7AC C3AC 109.6(6) . . ? C1C C7AC C7C 145.6(7) . . ? C3AC C7AC C7C 104.8(5) . . ? C1D C7AD C3AD 110.3(5) . . ? C1D C7AD C7D 145.7(6) . . ? C3AD C7AD C7D 103.8(5) . . ? C7A C7 C6 105.5(5) . . ? C7A C7 C8 99.9(5) . . ? C6 C7 C8 98.7(5) . . ? C7A C7 Cl7 115.7(4) . . ? C6 C7 Cl7 115.9(5) . . ? C8 C7 Cl7 118.5(5) . . ? C7AB C7B C6B 106.9(5) . . ? C7AB C7B C8B 98.9(5) . . ? C6B C7B C8B 98.4(5) . . ? C7AB C7B Cl7B 115.7(5) . . ? C6B C7B Cl7B 116.5(5) . . ? C8B C7B Cl7B 117.8(4) . . ? C7AC C7C C6C 106.3(6) . . ? C7AC C7C C8C 99.3(5) . . ? C6C C7C C8C 99.3(5) . . ? C7AC C7C Cl7C 115.5(5) . . ? C6C C7C Cl7C 116.6(5) . . ? C8C C7C Cl7C 117.3(5) . . ? C7AD C7D C6D 104.5(5) . . ? C7AD C7D C8D 99.9(5) . . ? C6D C7D C8D 99.4(5) . . ? C7AD C7D Cl7D 119.1(5) . . ? C6D C7D Cl7D 115.2(4) . . ? C8D C7D Cl7D 115.9(4) . . ? C5 C6 C7 108.0(6) . . ? C5 C6 Cl6 127.3(6) . . ? C7 C6 Cl6 124.5(5) . . ? C5B C6B C7B 108.2(6) . . ? C5B C6B Cl6B 128.6(6) . . ? C7B C6B Cl6B 123.1(5) . . ? C5C C6C C7C 107.8(6) . . ? C5C C6C Cl6C 128.0(6) . . ? C7C C6C Cl6C 123.8(5) . . ? C5D C6D C7D 108.8(6) . . ? C5D C6D Cl6D 128.0(6) . . ? C7D C6D Cl6D 122.6(5) . . ? O2 C8 O1 113.8(5) . . ? O2 C8 C4 108.0(5) . . ? O1 C8 C4 116.6(6) . . ? O2 C8 C7 118.1(6) . . ? O1 C8 C7 106.9(5) . . ? C4 C8 C7 92.0(5) . . ? O2B C8B O1B 114.7(5) . . ? O2B C8B C4B 117.2(5) . . ? O1B C8B C4B 107.0(5) . . ? O2B C8B C7B 106.3(5) . . ? O1B C8B C7B 118.7(5) . . ? C4B C8B C7B 91.3(4) . . ? O2C C8C O1C 113.2(5) . . ? O2C C8C C7C 107.0(5) . . ? O1C C8C C7C 119.3(5) . . ? O2C C8C C4C 116.2(5) . . ? O1C C8C C4C 107.7(5) . . ? C7C C8C C4C 92.0(5) . . ? O2D C8D O1D 113.7(5) . . ? O2D C8D C4D 118.6(5) . . ? O1D C8D C4D 106.8(5) . . ? O2D C8D C7D 107.9(5) . . ? O1D C8D C7D 116.4(6) . . ? C4D C8D C7D 92.0(5) . . ? Cl50 C100 Cl52 112.2(7) . . ? Cl50 C100 Cl51 112.0(6) . . ? Cl52 C100 Cl51 115.9(8) . . ? Cl54 C101 Cl55 110.9(5) . . ? Cl54 C101 Cl53 111.4(6) . . ? Cl55 C101 Cl53 109.0(5) . . ? C8 O2 C10 116.8(5) . . ? C8B O2B C10B 117.3(5) . . ? C8C O1C C9C 116.5(5) . . ? C8D O2D C10D 117.4(5) . . ? C8 O1 C9 115.6(5) . . ? C8B O1B C9B 117.0(5) . . ? C8C O2C C10C 116.0(5) . . ? C8D O1D C9D 116.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C5 C4 C3A -69.4(7) . . . . ? Cl5 C5 C4 C3A 105.0(6) . . . . ? C6 C5 C4 C8 34.0(6) . . . . ? Cl5 C5 C4 C8 -151.6(5) . . . . ? C6 C5 C4 Cl4 160.6(5) . . . . ? Cl5 C5 C4 Cl4 -25.0(7) . . . . ? C6B C5B C4B C3AB 66.0(7) . . . . ? Cl5B C5B C4B C3AB -112.1(6) . . . . ? C6B C5B C4B C8B -36.4(6) . . . . ? Cl5B C5B C4B C8B 145.5(5) . . . . ? C6B C5B C4B Cl4B -162.4(5) . . . . ? Cl5B C5B C4B Cl4B 19.5(8) . . . . ? C6C C5C C4C C3AC -67.6(7) . . . . ? Cl5C C5C C4C C3AC 104.2(6) . . . . ? C6C C5C C4C C8C 34.3(7) . . . . ? Cl5C C5C C4C C8C -153.9(5) . . . . ? C6C C5C C4C Cl4C 161.3(5) . . . . ? Cl5C C5C C4C Cl4C -26.8(7) . . . . ? C6D C5D C4D C3AD 67.2(6) . . . . ? Cl5D C5D C4D C3AD -104.4(6) . . . . ? C6D C5D C4D C8D -35.0(6) . . . . ? Cl5D C5D C4D C8D 153.4(5) . . . . ? C6D C5D C4D Cl4D -162.9(4) . . . . ? Cl5D C5D C4D Cl4D 25.5(7) . . . . ? C5 C4 C3A C3 -113.3(10) . . . . ? C8 C4 C3A C3 145.2(10) . . . . ? Cl4 C4 C3A C3 15.1(13) . . . . ? C5 C4 C3A C7A 64.1(6) . . . . ? C8 C4 C3A C7A -37.4(6) . . . . ? Cl4 C4 C3A C7A -167.4(5) . . . . ? C5B C4B C3AB C3B 119.3(10) . . . . ? C8B C4B C3AB C3B -139.4(10) . . . . ? Cl4B C4B C3AB C3B -11.2(13) . . . . ? C5B C4B C3AB C7AB -64.0(7) . . . . ? C8B C4B C3AB C7AB 37.3(6) . . . . ? Cl4B C4B C3AB C7AB 165.5(5) . . . . ? C5C C4C C3AC C3C -115.8(10) . . . . ? C8C C4C C3AC C3C 143.0(10) . . . . ? Cl4C C4C C3AC C3C 14.7(13) . . . . ? C5C C4C C3AC C7AC 65.5(6) . . . . ? C8C C4C C3AC C7AC -35.8(6) . . . . ? Cl4C C4C C3AC C7AC -164.0(4) . . . . ? C5D C4D C3AD C3D 110.0(11) . . . . ? C8D C4D C3AD C3D -147.3(10) . . . . ? Cl4D C4D C3AD C3D -20.0(13) . . . . ? C5D C4D C3AD C7AD -66.3(6) . . . . ? C8D C4D C3AD C7AD 36.4(7) . . . . ? Cl4D C4D C3AD C7AD 163.7(5) . . . . ? C7A C3A C3 C2 1.1(7) . . . . ? C4 C3A C3 C2 178.5(9) . . . . ? C7AB C3AB C3B C2B -0.2(7) . . . . ? C4B C3AB C3B C2B 176.5(9) . . . . ? C7AC C3AC C3C C2C -1.8(7) . . . . ? C4C C3AC C3C C2C 179.4(9) . . . . ? C7AD C3AD C3D C2D -0.8(8) . . . . ? C4D C3AD C3D C2D -177.1(9) . . . . ? C3A C3 C2 C2B 175.4(6) . . . . ? C3A C3 C2 C1 -1.4(7) . . . . ? C1 C2 C2B C1B 176.5(6) . . . . ? C3 C2 C2B C1B 0.2(11) . . . . ? C1 C2 C2B C3B -1.4(11) . . . . ? C3 C2 C2B C3B -177.6(6) . . . . ? C3AB C3B C2B C2 178.3(6) . . . . ? C3AB C3B C2B C1B 0.1(7) . . . . ? C3AC C3C C2C C2C -178.5(8) . . . 2_576 ? C3AC C3C C2C C1C 1.6(7) . . . . ? C3AD C3D C2D C2D -176.7(9) . . . 2_365 ? C3AD C3D C2D C1D 1.4(7) . . . . ? C2B C2 C1 C7A -175.6(7) . . . . ? C3 C2 C1 C7A 1.2(7) . . . . ? C2 C2B C1B C7AB -178.2(7) . . . . ? C3B C2B C1B C7AB 0.0(7) . . . . ? C2C C2C C1C C7AC 179.4(9) 2_576 . . . ? C3C C2C C1C C7AC -0.7(7) . . . . ? C2D C2D C1D C7AD 176.6(8) 2_365 . . . ? C3D C2D C1D C7AD -1.5(7) . . . . ? C2 C1 C7A C3A -0.5(7) . . . . ? C2 C1 C7A C7 178.8(9) . . . . ? C3 C3A C7A C1 -0.4(8) . . . . ? C4 C3A C7A C1 -178.8(6) . . . . ? C3 C3A C7A C7 180.0(5) . . . . ? C4 C3A C7A C7 1.6(7) . . . . ? C2B C1B C7AB C3AB -0.1(7) . . . . ? C2B C1B C7AB C7B -176.2(8) . . . . ? C3B C3AB C7AB C1B 0.2(8) . . . . ? C4B C3AB C7AB C1B -177.8(5) . . . . ? C3B C3AB C7AB C7B 177.8(6) . . . . ? C4B C3AB C7AB C7B -0.1(7) . . . . ? C2C C1C C7AC C3AC -0.4(7) . . . . ? C2C C1C C7AC C7C -177.4(9) . . . . ? C3C C3AC C7AC C1C 1.5(8) . . . . ? C4C C3AC C7AC C1C -179.3(6) . . . . ? C3C C3AC C7AC C7C 179.7(5) . . . . ? C4C C3AC C7AC C7C -1.0(6) . . . . ? C2D C1D C7AD C3AD 1.0(7) . . . . ? C2D C1D C7AD C7D 176.4(10) . . . . ? C3D C3AD C7AD C1D -0.1(8) . . . . ? C4D C3AD C7AD C1D 177.6(6) . . . . ? C3D C3AD C7AD C7D -177.5(6) . . . . ? C4D C3AD C7AD C7D 0.2(7) . . . . ? C1 C7A C7 C6 113.2(10) . . . . ? C3A C7A C7 C6 -67.5(6) . . . . ? C1 C7A C7 C8 -144.9(10) . . . . ? C3A C7A C7 C8 34.5(6) . . . . ? C1 C7A C7 Cl7 -16.4(12) . . . . ? C3A C7A C7 Cl7 162.9(4) . . . . ? C1B C7AB C7B C6B -118.7(10) . . . . ? C3AB C7AB C7B C6B 65.0(6) . . . . ? C1B C7AB C7B C8B 139.7(9) . . . . ? C3AB C7AB C7B C8B -36.6(6) . . . . ? C1B C7AB C7B Cl7B 12.8(12) . . . . ? C3AB C7AB C7B Cl7B -163.4(4) . . . . ? C1C C7AC C7C C6C 112.3(11) . . . . ? C3AC C7AC C7C C6C -64.8(6) . . . . ? C1C C7AC C7C C8C -145.1(10) . . . . ? C3AC C7AC C7C C8C 37.8(6) . . . . ? C1C C7AC C7C Cl7C -18.7(13) . . . . ? C3AC C7AC C7C Cl7C 164.2(4) . . . . ? C1D C7AD C7D C6D -109.9(11) . . . . ? C3AD C7AD C7D C6D 65.7(6) . . . . ? C1D C7AD C7D C8D 147.6(10) . . . . ? C3AD C7AD C7D C8D -36.8(6) . . . . ? C1D C7AD C7D Cl7D 20.5(14) . . . . ? C3AD C7AD C7D Cl7D -164.0(5) . . . . ? C4 C5 C6 C7 2.1(7) . . . . ? Cl5 C5 C6 C7 -172.0(5) . . . . ? C4 C5 C6 Cl6 177.0(5) . . . . ? Cl5 C5 C6 Cl6 2.9(10) . . . . ? C7A C7 C6 C5 65.7(6) . . . . ? C8 C7 C6 C5 -37.2(6) . . . . ? Cl7 C7 C6 C5 -164.9(5) . . . . ? C7A C7 C6 Cl6 -109.3(6) . . . . ? C8 C7 C6 Cl6 147.8(5) . . . . ? Cl7 C7 C6 Cl6 20.1(7) . . . . ? C4B C5B C6B C7B 0.3(7) . . . . ? Cl5B C5B C6B C7B 178.3(5) . . . . ? C4B C5B C6B Cl6B -177.2(5) . . . . ? Cl5B C5B C6B Cl6B 0.8(10) . . . . ? C7AB C7B C6B C5B -66.5(6) . . . . ? C8B C7B C6B C5B 35.5(6) . . . . ? Cl7B C7B C6B C5B 162.4(5) . . . . ? C7AB C7B C6B Cl6B 111.2(6) . . . . ? C8B C7B C6B Cl6B -146.8(5) . . . . ? Cl7B C7B C6B Cl6B -20.0(7) . . . . ? C4C C5C C6C C7C 0.5(8) . . . . ? Cl5C C5C C6C C7C -170.7(5) . . . . ? C4C C5C C6C Cl6C 174.1(5) . . . . ? Cl5C C5C C6C Cl6C 2.9(11) . . . . ? C7AC C7C C6C C5C 67.1(7) . . . . ? C8C C7C C6C C5C -35.5(7) . . . . ? Cl7C C7C C6C C5C -162.5(5) . . . . ? C7AC C7C C6C Cl6C -106.8(6) . . . . ? C8C C7C C6C Cl6C 150.6(5) . . . . ? Cl7C C7C C6C Cl6C 23.6(8) . . . . ? C4D C5D C6D C7D 0.5(7) . . . . ? Cl5D C5D C6D C7D 171.8(5) . . . . ? C4D C5D C6D Cl6D -170.9(5) . . . . ? Cl5D C5D C6D Cl6D 0.3(9) . . . . ? C7AD C7D C6D C5D -68.9(7) . . . . ? C8D C7D C6D C5D 34.0(6) . . . . ? Cl7D C7D C6D C5D 158.5(5) . . . . ? C7AD C7D C6D Cl6D 103.1(5) . . . . ? C8D C7D C6D Cl6D -154.0(4) . . . . ? Cl7D C7D C6D Cl6D -29.5(7) . . . . ? C3A C4 C8 O2 175.8(5) . . . . ? C5 C4 C8 O2 68.6(6) . . . . ? Cl4 C4 C8 O2 -55.1(7) . . . . ? C3A C4 C8 O1 -54.7(6) . . . . ? C5 C4 C8 O1 -161.9(5) . . . . ? Cl4 C4 C8 O1 74.4(7) . . . . ? C3A C4 C8 C7 55.4(5) . . . . ? C5 C4 C8 C7 -51.9(5) . . . . ? Cl4 C4 C8 C7 -175.5(5) . . . . ? C7A C7 C8 O2 -165.4(6) . . . . ? C6 C7 C8 O2 -57.9(7) . . . . ? Cl7 C7 C8 O2 68.0(7) . . . . ? C7A C7 C8 O1 64.9(6) . . . . ? C6 C7 C8 O1 172.4(5) . . . . ? Cl7 C7 C8 O1 -61.7(7) . . . . ? C7A C7 C8 C4 -53.7(6) . . . . ? C6 C7 C8 C4 53.8(6) . . . . ? Cl7 C7 C8 C4 179.7(5) . . . . ? C3AB C4B C8B O2B 53.1(6) . . . . ? C5B C4B C8B O2B 161.8(5) . . . . ? Cl4B C4B C8B O2B -74.4(6) . . . . ? C3AB C4B C8B O1B -176.6(5) . . . . ? C5B C4B C8B O1B -67.9(6) . . . . ? Cl4B C4B C8B O1B 55.9(6) . . . . ? C3AB C4B C8B C7B -56.0(5) . . . . ? C5B C4B C8B C7B 52.7(5) . . . . ? Cl4B C4B C8B C7B 176.5(5) . . . . ? C7AB C7B C8B O2B -63.2(6) . . . . ? C6B C7B C8B O2B -171.9(5) . . . . ? Cl7B C7B C8B O2B 62.2(6) . . . . ? C7AB C7B C8B O1B 165.9(5) . . . . ? C6B C7B C8B O1B 57.2(7) . . . . ? Cl7B C7B C8B O1B -68.7(7) . . . . ? C7AB C7B C8B C4B 55.6(5) . . . . ? C6B C7B C8B C4B -53.0(5) . . . . ? Cl7B C7B C8B C4B -179.0(5) . . . . ? C7AC C7C C8C O2C 61.6(6) . . . . ? C6C C7C C8C O2C 169.9(5) . . . . ? Cl7C C7C C8C O2C -63.5(6) . . . . ? C7AC C7C C8C O1C -168.2(6) . . . . ? C6C C7C C8C O1C -59.9(7) . . . . ? Cl7C C7C C8C O1C 66.6(7) . . . . ? C7AC C7C C8C C4C -56.6(5) . . . . ? C6C C7C C8C C4C 51.7(5) . . . . ? Cl7C C7C C8C C4C 178.2(4) . . . . ? C3AC C4C C8C O2C -54.2(7) . . . . ? C5C C4C C8C O2C -160.9(5) . . . . ? Cl4C C4C C8C O2C 73.4(7) . . . . ? C3AC C4C C8C O1C 177.5(5) . . . . ? C5C C4C C8C O1C 70.8(6) . . . . ? Cl4C C4C C8C O1C -54.9(6) . . . . ? C3AC C4C C8C C7C 55.8(5) . . . . ? C5C C4C C8C C7C -50.9(5) . . . . ? Cl4C C4C C8C C7C -176.6(4) . . . . ? C3AD C4D C8D O2D -167.2(6) . . . . ? C5D C4D C8D O2D -60.7(7) . . . . ? Cl4D C4D C8D O2D 66.5(8) . . . . ? C3AD C4D C8D O1D 62.9(6) . . . . ? C5D C4D C8D O1D 169.4(5) . . . . ? Cl4D C4D C8D O1D -63.5(6) . . . . ? C3AD C4D C8D C7D -55.5(6) . . . . ? C5D C4D C8D C7D 51.0(5) . . . . ? Cl4D C4D C8D C7D 178.2(5) . . . . ? C7AD C7D C8D O2D 177.2(5) . . . . ? C6D C7D C8D O2D 70.6(6) . . . . ? Cl7D C7D C8D O2D -53.5(7) . . . . ? C7AD C7D C8D O1D -53.6(7) . . . . ? C6D C7D C8D O1D -160.3(5) . . . . ? Cl7D C7D C8D O1D 75.7(6) . . . . ? C7AD C7D C8D C4D 56.3(5) . . . . ? C6D C7D C8D C4D -50.4(5) . . . . ? Cl7D C7D C8D C4D -174.4(4) . . . . ? O1 C8 O2 C10 57.5(7) . . . . ? C4 C8 O2 C10 -171.4(5) . . . . ? C7 C8 O2 C10 -69.0(8) . . . . ? O1B C8B O2B C10B -54.5(7) . . . . ? C4B C8B O2B C10B 72.1(7) . . . . ? C7B C8B O2B C10B 172.3(5) . . . . ? O2C C8C O1C C9C 54.0(8) . . . . ? C7C C8C O1C C9C -73.3(8) . . . . ? C4C C8C O1C C9C -176.0(5) . . . . ? O1D C8D O2D C10D 55.0(8) . . . . ? C4D C8D O2D C10D -71.7(8) . . . . ? C7D C8D O2D C10D -174.3(6) . . . . ? O2 C8 O1 C9 53.2(8) . . . . ? C4 C8 O1 C9 -73.6(7) . . . . ? C7 C8 O1 C9 -174.7(5) . . . . ? O2B C8B O1B C9B -53.5(7) . . . . ? C4B C8B O1B C9B 174.8(5) . . . . ? C7B C8B O1B C9B 73.6(7) . . . . ? O1C C8C O2C C10C 56.5(8) . . . . ? C7C C8C O2C C10C -170.0(6) . . . . ? C4C C8C O2C C10C -69.0(8) . . . . ? O2D C8D O1D C9D 53.8(8) . . . . ? C4D C8D O1D C9D -173.5(5) . . . . ? C7D C8D O1D C9D -72.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.975 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.158 # = END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Cl8 O4' _chemical_formula_sum 'C24 H16 Cl8 O4' _chemical_formula_weight 651.97 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.134(1) _cell_length_b 13.357(1) _cell_length_c 15.331(1) _cell_angle_alpha 90.00 _cell_angle_beta 118.89(1) _cell_angle_gamma 90.00 _cell_volume 2713.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 3257 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'red-brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7246 _exptl_absorpt_correction_T_max 0.8467 _exptl_absorpt_process_details ? _exptl_special_details ; Structure solution by direct methods ; _diffrn_ambient_temperature 173.0(1) _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 'Nonius KappaCCD diffractometer' _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 6352 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6352 _reflns_number_gt 4416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius,1998)' _computing_cell_refinement 'Denzo-SMN v0.93.0 (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN v0.93.0 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX-98 (Farrugia, 1998)' _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^)+(0.0193P)^2^+9.6889P] 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 6352 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8816(3) -0.3371(3) 0.2591(3) 0.0302(10) Uani 1 1 d . . . H1 H 0.8535 -0.3935 0.2746 0.036 Uiso 1 1 calc R . . C1B C 1.0117(3) -0.5210(3) 0.2598(3) 0.0272(9) Uani 1 1 d . . . H1B H 0.9585 -0.5483 0.2685 0.033 Uiso 1 1 calc R . . C2 C 0.9737(3) -0.3348(3) 0.2488(3) 0.0283(9) Uani 1 1 d . . . C2B C 1.0324(3) -0.4139(3) 0.2539(3) 0.0270(9) Uani 1 1 d . . . C3 C 0.9878(3) -0.2312(3) 0.2242(3) 0.0278(9) Uani 1 1 d . . . H3 H 1.0417 -0.2068 0.2152 0.033 Uiso 1 1 calc R . . C3B C 1.1245(3) -0.4069(3) 0.2435(3) 0.0289(9) Uani 1 1 d . . . H3B H 1.1565 -0.3476 0.2384 0.035 Uiso 1 1 calc R . . C3A C 0.9098(3) -0.1787(3) 0.2173(3) 0.0277(9) Uani 1 1 d . . . C3AB C 1.1535(3) -0.5022(3) 0.2426(3) 0.0265(9) Uani 1 1 d . . . C4 C 0.8608(3) -0.0778(3) 0.1931(3) 0.0279(9) Uani 1 1 d . . . C4B C 1.2299(3) -0.5671(3) 0.2325(3) 0.0273(9) Uani 1 1 d . . . Cl4B Cl 1.31103(9) -0.50986(9) 0.19558(10) 0.0421(3) Uani 1 1 d . . . Cl7B Cl 1.03160(10) -0.77335(9) 0.21350(12) 0.0517(4) Uani 1 1 d . . . C5 C 0.8720(3) -0.0392(3) 0.2906(3) 0.0324(10) Uani 1 1 d . . . C5B C 1.2843(3) -0.6250(3) 0.3308(3) 0.0298(9) Uani 1 1 d . . . Cl5 Cl 0.96121(11) 0.04511(10) 0.36326(10) 0.0505(3) Uani 1 1 d . . . Cl5B Cl 1.40367(9) -0.59766(10) 0.42111(9) 0.0470(3) Uani 1 1 d . . . C6 C 0.8143(3) -0.0953(3) 0.3140(3) 0.0339(10) Uani 1 1 d . . . C6B C 1.2197(3) -0.6874(3) 0.3360(3) 0.0318(10) Uani 1 1 d . . . Cl6 Cl 0.80684(13) -0.09004(12) 0.42136(11) 0.0627(4) Uani 1 1 d . . . C7 C 0.7626(3) -0.1754(3) 0.2348(3) 0.0313(10) Uani 1 1 d . . . C7AB C 1.0829(3) -0.5719(3) 0.2505(3) 0.0272(9) Uani 1 1 d . . . C7A C 0.8457(3) -0.2428(3) 0.2420(3) 0.0291(9) Uani 1 1 d . . . C7B C 1.1181(3) -0.6751(3) 0.2425(3) 0.0302(10) Uani 1 1 d . . . Cl7 Cl 0.65744(10) -0.23057(9) 0.23392(11) 0.0491(3) Uani 1 1 d . . . Cl4 Cl 0.89602(9) 0.00463(8) 0.12597(9) 0.0386(3) Uani 1 1 d . . . Cl6B Cl 1.23747(13) -0.75716(10) 0.43583(11) 0.0601(4) Uani 1 1 d . . . C8 C 0.7454(3) -0.1110(3) 0.1399(3) 0.0287(9) Uani 1 1 d . . . C8B C 1.1564(3) -0.6511(3) 0.1641(3) 0.0281(9) Uani 1 1 d . . . C9 C 0.6390(4) -0.2265(4) 0.0090(5) 0.0609(16) Uani 1 1 d . . . H9A H 0.6456 -0.2836 0.0519 0.091 Uiso 1 1 calc R . . H9B H 0.6300 -0.2510 -0.0550 0.091 Uiso 1 1 calc R . . H9C H 0.5803 -0.1863 -0.0021 0.091 Uiso 1 1 calc R . . C9B C 1.1559(4) -0.8064(4) 0.0843(4) 0.0468(13) Uani 1 1 d . . . H9B1 H 1.1360 -0.8535 0.1207 0.070 Uiso 1 1 calc R . . H9B2 H 1.1978 -0.8411 0.0611 0.070 Uiso 1 1 calc R . . H9B3 H 1.0954 -0.7797 0.0269 0.070 Uiso 1 1 calc R . . C10 C 0.6487(4) 0.0275(5) 0.0404(4) 0.0585(16) Uani 1 1 d . . . H10A H 0.6958 0.0840 0.0636 0.088 Uiso 1 1 calc R . . H10B H 0.5795 0.0522 0.0146 0.088 Uiso 1 1 calc R . . H10C H 0.6544 -0.0080 -0.0126 0.088 Uiso 1 1 calc R . . C10B C 1.0961(4) -0.5755(5) 0.0039(4) 0.0591(16) Uani 1 1 d . . . H10D H 1.1242 -0.5082 0.0251 0.089 Uiso 1 1 calc R . . H10E H 1.0338 -0.5713 -0.0601 0.089 Uiso 1 1 calc R . . H10F H 1.1452 -0.6176 -0.0034 0.089 Uiso 1 1 calc R . . O1 O 0.7294(2) -0.1655(2) 0.0567(2) 0.0386(8) Uani 1 1 d . . . O1B O 1.2128(2) -0.7250(2) 0.1495(2) 0.0311(7) Uani 1 1 d . . . O2 O 0.6726(2) -0.0400(2) 0.1220(2) 0.0371(7) Uani 1 1 d . . . O2B O 1.0741(2) -0.6189(2) 0.0780(2) 0.0376(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(2) 0.022(2) 0.042(3) 0.0058(19) 0.023(2) 0.0004(17) C1B 0.031(2) 0.0165(19) 0.040(2) 0.0001(18) 0.021(2) -0.0032(16) C2 0.030(2) 0.021(2) 0.038(2) 0.0002(18) 0.0196(19) 0.0005(17) C2B 0.029(2) 0.020(2) 0.032(2) 0.0044(18) 0.0145(18) 0.0013(17) C3 0.029(2) 0.022(2) 0.039(2) 0.0036(19) 0.0220(19) 0.0010(17) C3B 0.026(2) 0.021(2) 0.043(3) 0.0018(19) 0.0185(19) 0.0010(17) C3A 0.027(2) 0.024(2) 0.035(2) 0.0022(18) 0.0174(19) -0.0003(17) C3AB 0.023(2) 0.023(2) 0.034(2) 0.0005(18) 0.0145(18) -0.0002(16) C4 0.033(2) 0.021(2) 0.036(2) 0.0052(18) 0.022(2) 0.0022(17) C4B 0.025(2) 0.023(2) 0.036(2) 0.0062(18) 0.0157(19) 0.0023(16) Cl4B 0.0364(6) 0.0355(6) 0.0658(8) 0.0099(6) 0.0337(6) 0.0006(5) Cl7B 0.0499(7) 0.0242(6) 0.1022(11) -0.0130(6) 0.0536(8) -0.0097(5) C5 0.034(2) 0.025(2) 0.037(2) 0.0027(19) 0.016(2) 0.0036(18) C5B 0.029(2) 0.026(2) 0.032(2) -0.0031(19) 0.0134(19) 0.0050(18) Cl5 0.0582(8) 0.0358(7) 0.0485(7) -0.0057(6) 0.0186(6) -0.0090(6) Cl5B 0.0315(6) 0.0575(8) 0.0386(6) -0.0129(6) 0.0064(5) 0.0106(6) C6 0.042(3) 0.032(2) 0.034(2) 0.004(2) 0.024(2) 0.004(2) C6B 0.044(3) 0.024(2) 0.035(2) 0.0068(19) 0.024(2) 0.0112(19) Cl6 0.0953(12) 0.0628(9) 0.0510(8) -0.0002(7) 0.0519(8) -0.0059(8) C7 0.034(2) 0.024(2) 0.047(3) 0.003(2) 0.028(2) 0.0020(18) C7AB 0.028(2) 0.021(2) 0.035(2) 0.0010(18) 0.0165(19) -0.0002(16) C7A 0.030(2) 0.024(2) 0.039(2) 0.0041(19) 0.022(2) 0.0006(17) C7B 0.031(2) 0.020(2) 0.048(3) -0.0015(19) 0.026(2) -0.0023(17) Cl7 0.0441(7) 0.0367(6) 0.0865(10) 0.0038(7) 0.0474(7) -0.0014(5) Cl4 0.0474(7) 0.0280(6) 0.0528(7) 0.0132(5) 0.0341(6) 0.0047(5) Cl6B 0.1001(12) 0.0414(7) 0.0576(8) 0.0227(7) 0.0530(9) 0.0229(7) C8 0.027(2) 0.027(2) 0.035(2) 0.0013(19) 0.0164(19) 0.0035(17) C8B 0.025(2) 0.026(2) 0.033(2) 0.0010(19) 0.0145(18) 0.0028(17) C9 0.052(3) 0.052(4) 0.060(4) -0.013(3) 0.012(3) -0.011(3) C9B 0.039(3) 0.043(3) 0.053(3) -0.020(3) 0.018(2) -0.001(2) C10 0.060(4) 0.059(4) 0.060(4) 0.026(3) 0.031(3) 0.027(3) C10B 0.055(3) 0.087(5) 0.032(3) 0.018(3) 0.019(3) 0.027(3) O1 0.0397(18) 0.0359(18) 0.0389(18) -0.0064(15) 0.0179(15) 0.0001(14) O1B 0.0279(15) 0.0278(16) 0.0360(17) -0.0085(14) 0.0141(13) 0.0027(12) O2 0.0340(17) 0.0336(17) 0.0472(19) 0.0094(15) 0.0224(15) 0.0102(14) O2B 0.0259(16) 0.047(2) 0.0320(17) -0.0009(15) 0.0075(13) 0.0089(14) _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 C7A 1.347(6) . ? C1 C2 1.479(6) . ? C1B C7AB 1.339(6) . ? C1B C2B 1.477(5) . ? C2 C2B 1.357(6) . ? C2 C3 1.475(6) . ? C2B C3B 1.481(6) . ? C3 C3A 1.332(6) . ? C3B C3AB 1.349(6) . ? C3A C7A 1.473(6) . ? C3A C4 1.496(6) . ? C3AB C7AB 1.465(6) . ? C3AB C4B 1.511(6) . ? C4 C5 1.512(6) . ? C4 C8 1.593(6) . ? C4 Cl4 1.756(4) . ? C4B C5B 1.533(6) . ? C4B C8B 1.571(6) . ? C4B Cl4B 1.756(4) . ? Cl7B C7B 1.752(4) . ? C5 C6 1.325(6) . ? C5 Cl5 1.697(5) . ? C5B C6B 1.316(6) . ? C5B Cl5B 1.702(4) . ? C6 C7 1.522(6) . ? C6 Cl6 1.704(4) . ? C6B C7B 1.523(6) . ? C6B Cl6B 1.698(4) . ? C7 C7A 1.507(6) . ? C7 C8 1.600(6) . ? C7 Cl7 1.748(4) . ? C7AB C7B 1.505(6) . ? C7B C8B 1.599(6) . ? C8 O2 1.377(5) . ? C8 O1 1.384(5) . ? C8B O2B 1.374(5) . ? C8B O1B 1.393(5) . ? C9 O1 1.450(6) . ? C9B O1B 1.446(5) . ? C10 O2 1.440(6) . ? C10B O2B 1.450(6) . ? 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 C7A C1 C2 105.7(4) . . ? C7AB C1B C2B 106.3(4) . . ? C2B C2 C3 125.0(4) . . ? C2B C2 C1 127.0(4) . . ? C3 C2 C1 107.9(3) . . ? C2 C2B C1B 127.3(4) . . ? C2 C2B C3B 124.6(4) . . ? C1B C2B C3B 107.8(3) . . ? C3A C3 C2 106.4(4) . . ? C3AB C3B C2B 105.6(4) . . ? C3 C3A C7A 110.0(4) . . ? C3 C3A C4 143.8(4) . . ? C7A C3A C4 106.2(3) . . ? C3B C3AB C7AB 110.2(4) . . ? C3B C3AB C4B 144.2(4) . . ? C7AB C3AB C4B 105.6(3) . . ? C3A C4 C5 104.9(3) . . ? C3A C4 C8 99.5(3) . . ? C5 C4 C8 99.9(3) . . ? C3A C4 Cl4 117.1(3) . . ? C5 C4 Cl4 116.4(3) . . ? C8 C4 Cl4 116.3(3) . . ? C3AB C4B C5B 105.2(3) . . ? C3AB C4B C8B 98.5(3) . . ? C5B C4B C8B 99.6(3) . . ? C3AB C4B Cl4B 118.2(3) . . ? C5B C4B Cl4B 114.2(3) . . ? C8B C4B Cl4B 118.4(3) . . ? C6 C5 C4 107.6(4) . . ? C6 C5 Cl5 128.1(4) . . ? C4 C5 Cl5 123.3(3) . . ? C6B C5B C4B 108.5(4) . . ? C6B C5B Cl5B 127.9(4) . . ? C4B C5B Cl5B 123.1(3) . . ? C5 C6 C7 109.5(4) . . ? C5 C6 Cl6 126.7(4) . . ? C7 C6 Cl6 123.5(3) . . ? C5B C6B C7B 108.4(4) . . ? C5B C6B Cl6B 127.1(4) . . ? C7B C6B Cl6B 123.8(3) . . ? C7A C7 C6 105.8(4) . . ? C7A C7 C8 98.7(3) . . ? C6 C7 C8 98.2(3) . . ? C7A C7 Cl7 118.2(3) . . ? C6 C7 Cl7 114.7(3) . . ? C8 C7 Cl7 118.2(3) . . ? C1B C7AB C3AB 110.1(4) . . ? C1B C7AB C7B 144.0(4) . . ? C3AB C7AB C7B 105.9(3) . . ? C1 C7A C3A 109.9(4) . . ? C1 C7A C7 144.8(4) . . ? C3A C7A C7 105.3(3) . . ? C7AB C7B C6B 105.0(4) . . ? C7AB C7B C8B 98.5(3) . . ? C6B C7B C8B 99.3(3) . . ? C7AB C7B Cl7B 117.2(3) . . ? C6B C7B Cl7B 116.7(3) . . ? C8B C7B Cl7B 117.2(3) . . ? O2 C8 O1 114.3(4) . . ? O2 C8 C4 119.0(3) . . ? O1 C8 C4 106.2(3) . . ? O2 C8 C7 108.3(3) . . ? O1 C8 C7 115.7(3) . . ? C4 C8 C7 91.6(3) . . ? O2B C8B O1B 114.1(3) . . ? O2B C8B C4B 116.0(3) . . ? O1B C8B C4B 108.8(3) . . ? O2B C8B C7B 107.2(3) . . ? O1B C8B C7B 116.9(3) . . ? C4B C8B C7B 92.2(3) . . ? C8 O1 C9 117.6(4) . . ? C8B O1B C9B 116.0(3) . . ? C8 O2 C10 116.4(4) . . ? C8B O2B C10B 115.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7A C1 C2 C2B -175.9(5) . . . . ? C7A C1 C2 C3 0.0(5) . . . . ? C3 C2 C2B C1B -167.9(4) . . . . ? C1 C2 C2B C1B 7.3(8) . . . . ? C3 C2 C2B C3B 5.1(7) . . . . ? C1 C2 C2B C3B -179.7(4) . . . . ? C7AB C1B C2B C2 172.2(4) . . . . ? C7AB C1B C2B C3B -1.8(5) . . . . ? C2B C2 C3 C3A 174.0(4) . . . . ? C1 C2 C3 C3A -2.0(5) . . . . ? C2 C2B C3B C3AB -173.7(4) . . . . ? C1B C2B C3B C3AB 0.5(5) . . . . ? C2 C3 C3A C7A 3.1(5) . . . . ? C2 C3 C3A C4 -176.5(6) . . . . ? C2B C3B C3AB C7AB 0.9(5) . . . . ? C2B C3B C3AB C4B 177.3(6) . . . . ? C3 C3A C4 C5 -112.9(7) . . . . ? C7A C3A C4 C5 67.5(4) . . . . ? C3 C3A C4 C8 144.1(6) . . . . ? C7A C3A C4 C8 -35.5(4) . . . . ? C3 C3A C4 Cl4 18.0(9) . . . . ? C7A C3A C4 Cl4 -161.7(3) . . . . ? C3B C3AB C4B C5B 119.4(7) . . . . ? C7AB C3AB C4B C5B -64.2(4) . . . . ? C3B C3AB C4B C8B -138.2(6) . . . . ? C7AB C3AB C4B C8B 38.3(4) . . . . ? C3B C3AB C4B Cl4B -9.5(8) . . . . ? C7AB C3AB C4B Cl4B 167.0(3) . . . . ? C3A C4 C5 C6 -68.2(4) . . . . ? C8 C4 C5 C6 34.5(4) . . . . ? Cl4 C4 C5 C6 160.6(3) . . . . ? C3A C4 C5 Cl5 100.9(4) . . . . ? C8 C4 C5 Cl5 -156.4(3) . . . . ? Cl4 C4 C5 Cl5 -30.4(5) . . . . ? C3AB C4B C5B C6B 67.3(4) . . . . ? C8B C4B C5B C6B -34.3(4) . . . . ? Cl4B C4B C5B C6B -161.5(3) . . . . ? C3AB C4B C5B Cl5B -105.4(4) . . . . ? C8B C4B C5B Cl5B 153.0(3) . . . . ? Cl4B C4B C5B Cl5B 25.8(5) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? Cl5 C5 C6 C7 -167.5(3) . . . . ? C4 C5 C6 Cl6 174.4(3) . . . . ? Cl5 C5 C6 Cl6 6.0(7) . . . . ? C4B C5B C6B C7B -0.4(5) . . . . ? Cl5B C5B C6B C7B 171.8(3) . . . . ? C4B C5B C6B Cl6B -171.2(3) . . . . ? Cl5B C5B C6B Cl6B 1.0(6) . . . . ? C5 C6 C7 C7A 66.0(5) . . . . ? Cl6 C6 C7 C7A -107.8(4) . . . . ? C5 C6 C7 C8 -35.5(4) . . . . ? Cl6 C6 C7 C8 150.7(3) . . . . ? C5 C6 C7 Cl7 -161.8(3) . . . . ? Cl6 C6 C7 Cl7 24.4(5) . . . . ? C2B C1B C7AB C3AB 2.4(5) . . . . ? C2B C1B C7AB C7B -175.7(6) . . . . ? C3B C3AB C7AB C1B -2.2(5) . . . . ? C4B C3AB C7AB C1B -180.0(4) . . . . ? C3B C3AB C7AB C7B 176.6(4) . . . . ? C4B C3AB C7AB C7B -1.2(5) . . . . ? C2 C1 C7A C3A 1.9(5) . . . . ? C2 C1 C7A C7 179.1(6) . . . . ? C3 C3A C7A C1 -3.3(5) . . . . ? C4 C3A C7A C1 176.4(4) . . . . ? C3 C3A C7A C7 178.3(4) . . . . ? C4 C3A C7A C7 -1.9(5) . . . . ? C6 C7 C7A C1 119.9(7) . . . . ? C8 C7 C7A C1 -139.0(7) . . . . ? Cl7 C7 C7A C1 -10.3(9) . . . . ? C6 C7 C7A C3A -62.8(4) . . . . ? C8 C7 C7A C3A 38.3(4) . . . . ? Cl7 C7 C7A C3A 167.0(3) . . . . ? C1B C7AB C7B C6B -115.4(7) . . . . ? C3AB C7AB C7B C6B 66.5(4) . . . . ? C1B C7AB C7B C8B 142.5(6) . . . . ? C3AB C7AB C7B C8B -35.6(4) . . . . ? C1B C7AB C7B Cl7B 15.9(9) . . . . ? C3AB C7AB C7B Cl7B -162.2(3) . . . . ? C5B C6B C7B C7AB -67.2(4) . . . . ? Cl6B C6B C7B C7AB 104.0(4) . . . . ? C5B C6B C7B C8B 34.3(4) . . . . ? Cl6B C6B C7B C8B -154.5(3) . . . . ? C5B C6B C7B Cl7B 161.2(3) . . . . ? Cl6B C6B C7B Cl7B -27.6(5) . . . . ? C3A C4 C8 O2 167.5(4) . . . . ? C5 C4 C8 O2 60.4(4) . . . . ? Cl4 C4 C8 O2 -65.7(5) . . . . ? C3A C4 C8 O1 -61.9(4) . . . . ? C5 C4 C8 O1 -169.0(3) . . . . ? Cl4 C4 C8 O1 64.9(4) . . . . ? C3A C4 C8 C7 55.5(3) . . . . ? C5 C4 C8 C7 -51.6(3) . . . . ? Cl4 C4 C8 C7 -177.7(3) . . . . ? C7A C7 C8 O2 -177.8(3) . . . . ? C6 C7 C8 O2 -70.3(4) . . . . ? Cl7 C7 C8 O2 53.5(4) . . . . ? C7A C7 C8 O1 52.3(4) . . . . ? C6 C7 C8 O1 159.8(3) . . . . ? Cl7 C7 C8 O1 -76.4(4) . . . . ? C7A C7 C8 C4 -56.5(3) . . . . ? C6 C7 C8 C4 51.0(3) . . . . ? Cl7 C7 C8 C4 174.8(3) . . . . ? C3AB C4B C8B O2B 53.6(4) . . . . ? C5B C4B C8B O2B 160.7(3) . . . . ? Cl4B C4B C8B O2B -75.0(4) . . . . ? C3AB C4B C8B O1B -176.2(3) . . . . ? C5B C4B C8B O1B -69.1(4) . . . . ? Cl4B C4B C8B O1B 55.2(4) . . . . ? C3AB C4B C8B C7B -56.8(3) . . . . ? C5B C4B C8B C7B 50.3(3) . . . . ? Cl4B C4B C8B C7B 174.6(3) . . . . ? C7AB C7B C8B O2B -62.0(4) . . . . ? C6B C7B C8B O2B -168.8(3) . . . . ? Cl7B C7B C8B O2B 64.6(4) . . . . ? C7AB C7B C8B O1B 168.6(3) . . . . ? C6B C7B C8B O1B 61.8(4) . . . . ? Cl7B C7B C8B O1B -64.8(4) . . . . ? C7AB C7B C8B C4B 56.2(3) . . . . ? C6B C7B C8B C4B -50.6(3) . . . . ? Cl7B C7B C8B C4B -177.2(3) . . . . ? O2 C8 O1 C9 -62.5(5) . . . . ? C4 C8 O1 C9 164.2(4) . . . . ? C7 C8 O1 C9 64.4(5) . . . . ? O2B C8B O1B C9B -46.2(5) . . . . ? C4B C8B O1B C9B -177.5(4) . . . . ? C7B C8B O1B C9B 79.9(5) . . . . ? O1 C8 O2 C10 -51.0(5) . . . . ? C4 C8 O2 C10 75.9(5) . . . . ? C7 C8 O2 C10 178.4(4) . . . . ? O1B C8B O2B C10B -60.1(5) . . . . ? C4B C8B O2B C10B 67.5(5) . . . . ? C7B C8B O2B C10B 168.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.616 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.091