# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'S. I. Troyanov' _publ_contact_author_email stroyano@thermo.chem.msu.ru loop_ _publ_author_name I.N.Ioffe O.N.Mazaleva C.Chen S.Yang E.Kemnitz S.I.Troyanov # Attachment '- c76cl-I_805557.CIF' data_c76cl-I_805557 _database_code_depnum_ccdc_archive 'CCDC 805557' #TrackingRef '- .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl24.24' _chemical_formula_weight 1772.16 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' 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 P2(1)/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 22.9210(10) _cell_length_b 11.4760(10) _cell_length_c 23.3150(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.580(3) _cell_angle_gamma 90.00 _cell_volume 5961.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81081 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 36.83 _reflns_number_total 12856 _reflns_number_gt 9260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Several Cl atoms are disordered over two positions each. Five Cl atoms with low occupancies are due to the presence of a molecule with a higher Cl:C ratio in the same crystallographic site. All restraints concern ADP of Cl atoms (ISOR). ; _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^)+(0.0900P)^2^+18.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12856 _refine_ls_number_parameters 1038 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2217 _refine_ls_wR_factor_gt 0.2076 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.304 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.33872(11) 0.59640(17) 0.84893(8) 0.0384(5) Uani 0.925(3) 1 d P . . Cl1A Cl 0.3120(12) 0.622(2) 0.8536(11) 0.039(6) Uani 0.075(3) 1 d PU . . Cl2 Cl 0.25954(8) 0.44152(14) 0.90594(6) 0.0412(4) Uani 1 1 d . . . Cl3 Cl 0.15500(7) 0.64131(12) 0.81149(6) 0.0349(3) Uani 1 1 d . . . Cl4 Cl 0.07871(12) 0.74364(19) 0.64460(11) 0.0422(6) Uani 0.925(3) 1 d P . . Cl4A Cl 0.1040(12) 0.7491(19) 0.6360(10) 0.023(5) Uani 0.075(3) 1 d PU . . Cl5 Cl 0.16685(13) 0.80954(15) 0.54770(9) 0.0517(6) Uani 0.925(3) 1 d P . . Cl5A Cl 0.2039(9) 0.7984(14) 0.5504(8) 0.023(4) Uani 0.075(3) 1 d PU . . Cl6 Cl 0.29349(12) 0.7969(2) 0.52962(9) 0.0692(8) Uani 0.925(3) 1 d P . . Cl7 Cl 0.24051(18) 0.6430(3) 0.42366(9) 0.0801(10) Uani 0.925(3) 1 d P . . Cl7A Cl 0.199(2) 0.653(3) 0.4264(12) 0.070(8) Uani 0.075(3) 1 d PU . . Cl8 Cl 0.35455(14) 0.5042(3) 0.42840(10) 0.0973(10) Uani 1 1 d U . . Cl9 Cl 0.4264(2) 0.6386(4) 0.5358(2) 0.0797(15) Uani 0.86 1 d PU . . Cl9A Cl 0.4487(10) 0.587(2) 0.5404(8) 0.055(6) Uani 0.14 1 d P . . Cl10 Cl 0.50357(16) 0.4300(5) 0.58251(19) 0.0856(13) Uani 0.86 1 d PU . . C10A Cl 0.5196(10) 0.364(3) 0.5982(11) 0.076(7) Uani 0.14 1 d P . . Cl11 Cl 0.13910(9) 0.15889(15) 0.86370(7) 0.0455(4) Uani 1 1 d . . . Cl12 Cl 0.04516(8) 0.40850(16) 0.79908(8) 0.0454(4) Uani 1 1 d . . . Cl13 Cl -0.01067(8) 0.22774(17) 0.71036(9) 0.0407(5) Uani 0.925(3) 1 d P . . C13A Cl 0.0126(12) 0.191(4) 0.7413(15) 0.082(12) Uani 0.075(3) 1 d P . . Cl14 Cl -0.02969(7) 0.48172(16) 0.60843(9) 0.0417(4) Uani 0.925(3) 1 d P . . C14A Cl -0.0212(12) 0.446(3) 0.6496(16) 0.068(8) Uani 0.075(3) 1 d PU . . Cl15 Cl 0.44480(12) 0.2518(3) 0.49039(14) 0.1057(11) Uani 1 1 d U . . Cl16 Cl 0.45835(11) 0.0438(3) 0.57031(14) 0.0997(10) Uani 1 1 d U . . Cl17 Cl 0.52454(9) 0.1714(3) 0.68230(15) 0.1021(11) Uani 1 1 d U . . Cl18 Cl 0.47181(11) 0.0247(3) 0.76689(14) 0.0884(10) Uani 0.925(3) 1 d P . . Cl19 Cl 0.39678(11) -0.1293(2) 0.67233(13) 0.0779(9) Uani 0.925(3) 1 d P . . Cl20 Cl 0.31434(12) -0.14854(17) 0.75639(12) 0.0577(7) Uani 0.925(3) 1 d P . . C20A Cl 0.3277(15) -0.140(2) 0.7239(17) 0.060(7) Uani 0.075(3) 1 d PU . . Cl21 Cl 0.17030(13) -0.09686(16) 0.76882(9) 0.0412(5) Uani 0.925(3) 1 d P . . C21A Cl 0.1977(16) -0.100(3) 0.7611(15) 0.050(8) Uani 0.075(3) 1 d PU . . Cl22 Cl 0.04020(7) 0.00490(12) 0.62189(6) 0.0330(3) Uani 1 1 d . . . Cl23 Cl -0.00252(7) 0.20783(15) 0.50050(7) 0.0414(4) Uani 1 1 d . . . Cl24 Cl 0.09929(7) 0.06325(13) 0.47145(6) 0.0354(3) Uani 1 1 d . . . Cl25 Cl 0.4151(5) 0.4161(9) 0.8673(4) 0.044(4) Uani 0.168(8) 1 d P . . Cl26 Cl 0.4660(8) 0.180(2) 0.8294(10) 0.049(6) Uani 0.075(3) 1 d P . . Cl27 Cl 0.0290(13) 0.390(3) 0.4537(13) 0.066(8) Uani 0.075(3) 1 d P . . Cl28 Cl 0.3291(15) 0.251(2) 0.9033(12) 0.070(9) Uani 0.075(3) 1 d P . . Cl29 Cl 0.1186(16) 0.649(2) 0.4653(10) 0.067(9) Uani 0.075(3) 1 d P . . C1 C 0.3089(3) 0.5615(5) 0.7031(3) 0.0324(13) Uani 1 1 d . . . C2 C 0.2714(3) 0.5423(5) 0.7434(3) 0.0291(12) Uani 1 1 d . . . C3 C 0.2101(3) 0.5693(4) 0.7257(2) 0.0264(11) Uani 1 1 d . . . C4 C 0.1849(3) 0.6184(5) 0.6691(3) 0.0324(13) Uani 1 1 d . . . C5 C 0.2221(3) 0.6484(5) 0.6335(3) 0.0345(13) Uani 1 1 d . . . C6 C 0.2818(3) 0.6181(6) 0.6488(3) 0.0398(15) Uani 1 1 d . . . C7 C 0.3073(3) 0.6119(6) 0.5993(3) 0.0448(17) Uani 1 1 d . . . C8 C 0.3581(4) 0.5507(8) 0.6020(3) 0.053(2) Uani 1 1 d . . . C9 C 0.3847(3) 0.4897(7) 0.6545(3) 0.0506(19) Uani 1 1 d . . . C10 C 0.3629(3) 0.4977(6) 0.7056(3) 0.0388(15) Uani 1 1 d . . . C11 C 0.3772(3) 0.4033(6) 0.7476(3) 0.0373(14) Uani 1 1 d . . . C12 C 0.3453(3) 0.3918(6) 0.7913(3) 0.0400(14) Uani 1 1 d . . . C13 C 0.3007(3) 0.4823(5) 0.8014(3) 0.0289(12) Uani 1 1 d . . . C14 C 0.2559(3) 0.4077(5) 0.8293(2) 0.0290(12) Uani 1 1 d . . . C15 C 0.1926(3) 0.4203(5) 0.7964(2) 0.0258(11) Uani 1 1 d . . . C16 C 0.1680(3) 0.5258(5) 0.7622(2) 0.0271(11) Uani 1 1 d . . . C17 C 0.1103(2) 0.4788(5) 0.7234(3) 0.0271(11) Uani 1 1 d . . . C18 C 0.0892(2) 0.5124(5) 0.6684(3) 0.0274(11) Uani 1 1 d . . . C19 C 0.1186(3) 0.6072(5) 0.6403(3) 0.0319(13) Uani 1 1 d . . . C20 C 0.1129(3) 0.5592(5) 0.5781(3) 0.0325(13) Uani 1 1 d . . . C21 C 0.1545(3) 0.5774(5) 0.5450(3) 0.0409(15) Uani 1 1 d . . . C22 C 0.2026(4) 0.6691(6) 0.5659(3) 0.0441(17) Uani 1 1 d . . . C23 C 0.2651(4) 0.6566(7) 0.5449(3) 0.056(2) Uani 1 1 d . . . C24 C 0.2660(4) 0.5698(8) 0.4928(3) 0.060(2) Uani 1 1 d . . . C25 C 0.3299(5) 0.4940(10) 0.4957(3) 0.076(3) Uani 1 1 d . . . C26 C 0.3835(4) 0.5137(9) 0.5501(4) 0.070(3) Uani 1 1 d . . . C27 C 0.4265(4) 0.3986(11) 0.5790(4) 0.082(4) Uani 1 1 d . . . C28 C 0.4195(3) 0.3932(9) 0.6425(4) 0.060(2) Uani 1 1 d . . . C29 C 0.4278(3) 0.2999(9) 0.6790(4) 0.057(2) Uani 1 1 d . . . C30 C 0.4046(3) 0.3028(7) 0.7307(3) 0.0464(17) Uani 1 1 d . . . C31 C 0.3915(3) 0.1914(7) 0.7470(4) 0.0502(18) Uani 1 1 d . . . C32 C 0.3464(3) 0.1763(6) 0.7787(3) 0.0410(15) Uani 1 1 d . . . C33 C 0.3280(3) 0.2782(5) 0.8049(3) 0.0349(13) Uani 1 1 d . . . C34 C 0.2753(3) 0.2832(5) 0.8242(2) 0.0296(12) Uani 1 1 d . . . C35 C 0.2348(3) 0.1911(5) 0.8106(2) 0.0299(12) Uani 1 1 d . . . C36 C 0.1691(3) 0.2073(5) 0.8020(2) 0.0295(12) Uani 1 1 d . . . C37 C 0.1527(3) 0.3312(5) 0.7874(2) 0.0273(11) Uani 1 1 d . . . C38 C 0.0923(3) 0.3691(5) 0.7498(3) 0.0295(12) Uani 1 1 d . . . C39 C 0.0635(3) 0.2742(5) 0.7039(3) 0.0301(12) Uani 1 1 d . . . C40 C 0.0575(2) 0.3137(5) 0.6415(2) 0.0264(11) Uani 1 1 d . . . C41 C 0.0493(3) 0.4380(5) 0.6223(3) 0.0327(13) Uani 1 1 d . . . C42 C 0.0759(3) 0.4592(5) 0.5707(3) 0.0311(12) Uani 1 1 d . . . C43 C 0.0850(3) 0.3702(5) 0.5346(3) 0.0308(12) Uani 1 1 d . . . C44 C 0.1330(3) 0.3794(5) 0.5073(2) 0.0331(13) Uani 1 1 d . . . C45 C 0.1670(3) 0.4844(6) 0.5086(2) 0.0380(15) Uani 1 1 d . . . C46 C 0.2221(4) 0.4725(7) 0.4932(3) 0.0478(18) Uani 1 1 d . . . C47 C 0.2465(3) 0.3647(7) 0.4916(3) 0.0445(17) Uani 1 1 d . . . C48 C 0.3088(4) 0.3715(9) 0.5002(3) 0.056(2) Uani 1 1 d . . . C49 C 0.3427(3) 0.2774(9) 0.5242(3) 0.062(3) Uani 1 1 d . . . C50 C 0.4100(4) 0.2741(11) 0.5514(4) 0.078(3) Uani 1 1 d . . . C51 C 0.4184(3) 0.1596(10) 0.5969(4) 0.073(3) Uani 1 1 d . . . C52 C 0.4442(3) 0.1779(9) 0.6651(4) 0.071(3) Uani 1 1 d . . . C53 C 0.4158(3) 0.0982(8) 0.7129(4) 0.062(2) Uani 1 1 d . . . C54 C 0.3641(3) 0.0102(7) 0.6859(4) 0.059(2) Uani 1 1 d . . . C55 C 0.3116(3) -0.0078(6) 0.7202(3) 0.0477(18) Uani 1 1 d . . . C56 C 0.3051(3) 0.0827(5) 0.7662(3) 0.0400(15) Uani 1 1 d . . . C57 C 0.2499(3) 0.0948(5) 0.7793(3) 0.0330(13) Uani 1 1 d . . . C58 C 0.1914(3) 0.0424(5) 0.7423(2) 0.0329(13) Uani 1 1 d . . . C59 C 0.1455(3) 0.1330(5) 0.7484(2) 0.0288(12) Uani 1 1 d . . . C60 C 0.1010(2) 0.1667(5) 0.7040(2) 0.0253(11) Uani 1 1 d . . . C61 C 0.0945(2) 0.1224(5) 0.6420(2) 0.0255(11) Uani 1 1 d . . . C62 C 0.0717(2) 0.2283(5) 0.6075(2) 0.0249(11) Uani 1 1 d . . . C63 C 0.0720(2) 0.2437(5) 0.5445(2) 0.0285(12) Uani 1 1 d . . . C64 C 0.1243(2) 0.1737(5) 0.5268(2) 0.0254(11) Uani 1 1 d . . . C65 C 0.1577(3) 0.2688(5) 0.5035(2) 0.0316(12) Uani 1 1 d . . . C66 C 0.2167(3) 0.2602(6) 0.5017(2) 0.0368(14) Uani 1 1 d . . . C67 C 0.2530(3) 0.1659(6) 0.5325(3) 0.0386(15) Uani 1 1 d . . . C68 C 0.3150(3) 0.1778(7) 0.5424(3) 0.0486(18) Uani 1 1 d . . . C69 C 0.3547(3) 0.1174(8) 0.5886(4) 0.056(2) Uani 1 1 d . . . C70 C 0.3320(3) 0.0530(7) 0.6265(3) 0.0501(19) Uani 1 1 d . . . C71 C 0.2693(3) 0.0427(6) 0.6192(3) 0.0396(15) Uani 1 1 d . . . C72 C 0.2542(3) 0.0090(5) 0.6707(3) 0.0369(14) Uani 1 1 d . . . C73 C 0.1979(3) 0.0343(5) 0.6788(3) 0.0301(12) Uani 1 1 d . . . C74 C 0.1543(2) 0.0831(4) 0.6313(2) 0.0251(11) Uani 1 1 d . . . C75 C 0.1683(3) 0.1128(5) 0.5784(2) 0.0264(11) Uani 1 1 d . . . C76 C 0.2283(3) 0.0985(5) 0.5725(3) 0.0324(13) 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 Cl1 0.0515(12) 0.0311(9) 0.0303(9) -0.0070(7) 0.0051(9) -0.0188(9) Cl1A 0.043(12) 0.037(11) 0.050(12) -0.016(8) 0.035(10) 0.006(9) Cl2 0.0618(10) 0.0379(8) 0.0228(7) -0.0049(6) 0.0077(6) -0.0123(7) Cl3 0.0485(8) 0.0216(6) 0.0355(7) -0.0098(6) 0.0118(6) -0.0012(6) Cl4 0.0521(14) 0.0198(8) 0.0460(13) -0.0056(8) -0.0058(11) 0.0114(10) Cl4A 0.035(11) 0.011(8) 0.023(8) -0.003(6) 0.008(9) 0.012(8) Cl5 0.0818(18) 0.0209(8) 0.0417(10) 0.0116(7) -0.0073(10) -0.0124(10) Cl5A 0.019(7) 0.009(6) 0.038(8) 0.013(5) 0.001(6) 0.008(6) Cl6 0.1109(19) 0.0581(13) 0.0361(10) 0.0094(9) 0.0124(11) -0.0566(13) Cl7 0.123(3) 0.0885(19) 0.0265(10) 0.0102(10) 0.0135(13) -0.0628(19) Cl7A 0.107(18) 0.069(15) 0.034(11) 0.016(10) 0.020(13) -0.036(14) Cl8 0.1103(19) 0.145(2) 0.0506(12) -0.0244(13) 0.0472(13) -0.0769(18) Cl9 0.075(3) 0.113(4) 0.065(2) -0.024(2) 0.045(2) -0.059(2) Cl9A 0.068(13) 0.084(15) 0.024(6) -0.020(8) 0.028(8) -0.053(10) Cl10 0.0402(18) 0.142(4) 0.088(3) -0.047(3) 0.0413(18) -0.035(2) C10A 0.039(10) 0.12(2) 0.076(13) -0.012(13) 0.034(9) -0.008(10) Cl11 0.0727(11) 0.0401(9) 0.0263(7) 0.0010(6) 0.0168(7) -0.0235(8) Cl12 0.0468(9) 0.0496(10) 0.0479(9) -0.0148(8) 0.0276(7) -0.0064(7) Cl13 0.0325(9) 0.0463(10) 0.0485(11) -0.0102(9) 0.0198(9) -0.0128(8) C13A 0.032(13) 0.14(3) 0.061(17) 0.05(2) -0.011(12) -0.022(15) Cl14 0.0291(8) 0.0407(9) 0.0501(11) -0.0056(8) -0.0012(7) 0.0116(7) C14A 0.045(12) 0.089(16) 0.069(15) -0.002(14) 0.011(11) 0.013(12) Cl15 0.0712(15) 0.167(3) 0.0995(18) -0.0610(19) 0.0620(14) -0.0406(16) Cl16 0.0499(12) 0.140(2) 0.113(2) -0.0650(18) 0.0281(12) 0.0143(13) Cl17 0.0285(10) 0.145(3) 0.129(2) -0.068(2) 0.0099(12) 0.0130(12) Cl18 0.0476(12) 0.094(2) 0.102(2) -0.0280(16) -0.0253(13) 0.0358(13) Cl19 0.0606(13) 0.0671(15) 0.0928(18) -0.0361(13) -0.0087(12) 0.0363(12) Cl20 0.0783(15) 0.0249(9) 0.0546(13) -0.0032(9) -0.0152(11) 0.0189(9) C20A 0.086(16) 0.026(10) 0.074(15) 0.017(11) 0.032(13) 0.008(10) Cl21 0.0722(15) 0.0166(8) 0.0284(9) 0.0050(6) -0.0014(10) -0.0133(10) C21A 0.069(16) 0.033(12) 0.058(14) 0.000(9) 0.035(12) -0.022(12) Cl22 0.0413(8) 0.0217(6) 0.0351(7) -0.0054(5) 0.0075(6) -0.0131(6) Cl23 0.0365(8) 0.0422(9) 0.0397(8) -0.0084(7) -0.0025(6) -0.0042(7) Cl24 0.0487(8) 0.0277(7) 0.0265(7) -0.0091(6) 0.0019(6) -0.0052(6) Cl25 0.050(6) 0.040(6) 0.030(5) 0.005(4) -0.015(4) -0.014(4) Cl26 0.019(9) 0.068(15) 0.044(12) -0.006(11) -0.024(8) 0.000(9) Cl27 0.062(16) 0.058(16) 0.058(16) -0.013(13) -0.027(13) 0.004(13) Cl28 0.10(2) 0.040(13) 0.048(14) 0.008(11) -0.028(14) -0.010(13) Cl29 0.12(2) 0.028(11) 0.033(11) -0.002(9) -0.016(13) 0.004(13) C1 0.037(3) 0.033(3) 0.027(3) -0.003(2) 0.005(2) -0.019(3) C2 0.036(3) 0.022(3) 0.030(3) -0.005(2) 0.010(2) -0.011(2) C3 0.040(3) 0.013(2) 0.026(3) -0.001(2) 0.008(2) -0.008(2) C4 0.050(4) 0.014(2) 0.030(3) -0.001(2) 0.003(3) -0.006(2) C5 0.047(4) 0.025(3) 0.028(3) 0.001(2) 0.001(3) -0.016(3) C6 0.055(4) 0.032(3) 0.034(3) -0.001(3) 0.013(3) -0.025(3) C7 0.055(4) 0.049(4) 0.033(3) -0.003(3) 0.014(3) -0.031(3) C8 0.058(5) 0.071(5) 0.039(4) -0.012(4) 0.025(3) -0.045(4) C9 0.033(3) 0.074(5) 0.049(4) -0.014(4) 0.019(3) -0.027(3) C10 0.027(3) 0.055(4) 0.036(3) -0.010(3) 0.011(2) -0.021(3) C11 0.021(3) 0.043(4) 0.044(3) -0.010(3) 0.002(2) -0.008(2) C12 0.036(3) 0.035(3) 0.048(4) 0.000(3) 0.006(3) -0.003(3) C13 0.030(3) 0.026(3) 0.030(3) -0.002(2) 0.005(2) -0.010(2) C14 0.045(3) 0.021(3) 0.020(2) 0.002(2) 0.006(2) -0.008(2) C15 0.034(3) 0.021(3) 0.025(3) -0.007(2) 0.013(2) -0.007(2) C16 0.036(3) 0.017(2) 0.029(3) -0.008(2) 0.009(2) -0.002(2) C17 0.025(3) 0.022(3) 0.035(3) -0.009(2) 0.010(2) 0.001(2) C18 0.028(3) 0.019(2) 0.034(3) -0.006(2) 0.004(2) 0.005(2) C19 0.042(3) 0.017(3) 0.031(3) 0.001(2) -0.001(2) 0.002(2) C20 0.045(3) 0.018(3) 0.027(3) 0.004(2) -0.005(2) 0.003(2) C21 0.057(4) 0.022(3) 0.036(3) 0.008(3) -0.005(3) -0.008(3) C22 0.071(5) 0.026(3) 0.031(3) 0.004(3) 0.003(3) -0.017(3) C23 0.084(6) 0.049(4) 0.033(3) 0.009(3) 0.010(3) -0.038(4) C24 0.080(6) 0.077(6) 0.027(3) 0.001(3) 0.019(3) -0.044(5) C25 0.093(7) 0.111(8) 0.035(4) -0.021(4) 0.037(4) -0.064(6) C26 0.073(6) 0.101(7) 0.046(4) -0.020(5) 0.037(4) -0.052(6) C27 0.039(4) 0.148(10) 0.071(6) -0.043(6) 0.035(4) -0.048(6) C28 0.028(3) 0.103(7) 0.053(4) -0.028(5) 0.021(3) -0.025(4) C29 0.026(3) 0.084(6) 0.060(5) -0.021(5) 0.010(3) -0.005(4) C30 0.027(3) 0.058(5) 0.050(4) -0.017(3) 0.001(3) -0.001(3) C31 0.035(4) 0.053(4) 0.056(4) -0.015(4) -0.002(3) 0.009(3) C32 0.037(3) 0.033(3) 0.043(4) -0.005(3) -0.010(3) 0.011(3) C33 0.036(3) 0.029(3) 0.032(3) -0.004(2) -0.008(2) 0.000(2) C34 0.043(3) 0.023(3) 0.020(2) 0.003(2) 0.003(2) -0.007(2) C35 0.050(3) 0.018(3) 0.019(2) 0.005(2) 0.002(2) -0.003(2) C36 0.050(3) 0.020(3) 0.019(2) 0.003(2) 0.007(2) -0.012(2) C37 0.041(3) 0.022(3) 0.023(3) -0.003(2) 0.015(2) -0.005(2) C38 0.031(3) 0.028(3) 0.032(3) -0.007(2) 0.014(2) -0.007(2) C39 0.028(3) 0.032(3) 0.033(3) -0.006(2) 0.014(2) -0.008(2) C40 0.024(3) 0.024(3) 0.031(3) -0.004(2) 0.007(2) -0.003(2) C41 0.029(3) 0.028(3) 0.039(3) -0.003(2) 0.004(2) 0.002(2) C42 0.037(3) 0.021(3) 0.028(3) 0.000(2) -0.005(2) 0.002(2) C43 0.034(3) 0.023(3) 0.031(3) 0.003(2) -0.002(2) 0.000(2) C44 0.050(4) 0.027(3) 0.019(3) 0.000(2) 0.002(2) -0.013(3) C45 0.058(4) 0.034(3) 0.019(3) 0.005(2) 0.002(3) -0.014(3) C46 0.070(5) 0.051(4) 0.022(3) -0.001(3) 0.010(3) -0.029(4) C47 0.058(4) 0.061(5) 0.019(3) -0.009(3) 0.019(3) -0.024(4) C48 0.058(5) 0.082(6) 0.035(4) -0.013(4) 0.025(3) -0.028(4) C49 0.044(4) 0.107(7) 0.044(4) -0.040(5) 0.029(3) -0.031(5) C50 0.044(4) 0.127(9) 0.075(6) -0.048(6) 0.039(4) -0.029(5) C51 0.036(4) 0.109(8) 0.075(6) -0.038(6) 0.018(4) 0.006(4) C52 0.021(3) 0.107(7) 0.084(6) -0.050(6) 0.007(3) 0.006(4) C53 0.036(4) 0.073(6) 0.068(5) -0.025(5) -0.002(4) 0.017(4) C54 0.041(4) 0.059(5) 0.069(5) -0.025(4) -0.003(4) 0.022(4) C55 0.054(4) 0.033(3) 0.047(4) -0.008(3) -0.006(3) 0.017(3) C56 0.054(4) 0.023(3) 0.034(3) 0.003(2) -0.008(3) 0.007(3) C57 0.051(4) 0.015(2) 0.027(3) 0.004(2) -0.004(3) -0.002(2) C58 0.055(4) 0.016(3) 0.024(3) 0.002(2) 0.002(3) -0.007(2) C59 0.044(3) 0.018(2) 0.026(3) 0.001(2) 0.012(2) -0.014(2) C60 0.031(3) 0.023(3) 0.025(3) -0.001(2) 0.012(2) -0.013(2) C61 0.032(3) 0.019(2) 0.025(3) -0.003(2) 0.005(2) -0.007(2) C62 0.025(3) 0.019(2) 0.029(3) -0.001(2) 0.006(2) -0.004(2) C63 0.028(3) 0.026(3) 0.028(3) -0.003(2) 0.001(2) -0.003(2) C64 0.030(3) 0.025(3) 0.021(2) -0.006(2) 0.007(2) -0.003(2) C65 0.044(3) 0.031(3) 0.020(3) -0.004(2) 0.009(2) -0.007(3) C66 0.045(4) 0.047(4) 0.021(3) -0.009(3) 0.014(2) -0.015(3) C67 0.038(3) 0.048(4) 0.032(3) -0.020(3) 0.013(3) -0.004(3) C68 0.041(4) 0.073(5) 0.038(3) -0.028(4) 0.021(3) -0.009(3) C69 0.035(4) 0.078(6) 0.058(5) -0.031(4) 0.014(3) 0.006(4) C70 0.042(4) 0.055(4) 0.050(4) -0.025(4) 0.004(3) 0.014(3) C71 0.035(3) 0.038(3) 0.043(4) -0.017(3) 0.004(3) 0.008(3) C72 0.047(4) 0.021(3) 0.038(3) -0.008(2) 0.000(3) 0.008(2) C73 0.044(3) 0.014(2) 0.030(3) -0.004(2) 0.004(2) -0.001(2) C74 0.034(3) 0.017(2) 0.022(2) -0.004(2) 0.002(2) -0.005(2) C75 0.034(3) 0.018(2) 0.026(3) -0.007(2) 0.005(2) -0.003(2) C76 0.033(3) 0.032(3) 0.032(3) -0.014(3) 0.006(2) 0.002(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 Cl1 Cl1A 0.71(2) . ? Cl1 C13 1.802(6) . ? Cl1A C13 1.99(2) . ? Cl2 C14 1.811(6) . ? Cl3 C16 1.825(5) . ? Cl4 Cl4A 0.66(2) . ? Cl4 C19 1.827(6) . ? Cl4A C19 1.66(2) . ? Cl5 Cl5A 0.848(19) . ? Cl5 C22 1.813(7) . ? Cl5A C22 1.529(17) . ? Cl5A C23 2.17(2) . ? Cl5A Cl6 2.22(2) . ? Cl6 C23 1.802(7) . ? Cl7 Cl7A 0.97(4) . ? Cl7 C24 1.790(8) . ? Cl7A C24 2.13(4) . ? Cl7A Cl29 2.25(6) . ? Cl8 C25 1.791(7) . ? Cl9 Cl9A 0.77(2) . ? Cl9 C26 1.813(9) . ? Cl9A C26 1.78(2) . ? Cl9A Cl10 2.28(3) . ? Cl10 C10A 0.88(3) . ? Cl10 C27 1.787(8) . ? C10A C27 2.11(2) . ? Cl11 C36 1.821(5) . ? Cl12 C38 1.809(6) . ? Cl13 C13A 0.89(3) . ? Cl13 C39 1.822(6) . ? C13A C39 1.87(3) . ? Cl14 C14A 1.02(4) . ? Cl14 C41 1.832(6) . ? Cl14 Cl27 2.07(3) 3_566 ? C14A C41 1.87(3) . ? Cl15 C50 1.805(8) . ? Cl16 C51 1.804(9) . ? Cl17 C52 1.792(7) . ? Cl18 C53 1.785(9) . ? Cl18 Cl26 2.33(3) . ? Cl19 C54 1.826(7) . ? Cl19 C20A 2.21(3) . ? Cl20 C20A 0.89(3) . ? Cl20 C55 1.816(8) . ? C20A C55 1.55(3) . ? C20A C54 2.19(3) . ? Cl21 C21A 0.69(3) . ? Cl21 C58 1.819(6) . ? C21A C58 1.68(3) . ? Cl22 C61 1.820(5) . ? Cl23 C63 1.820(6) . ? Cl24 C64 1.803(5) . ? Cl25 C12 2.108(11) . ? Cl26 C31 2.255(19) . ? Cl27 C43 2.03(2) . ? Cl27 Cl14 2.07(3) 3_566 ? Cl28 C34 2.00(2) . ? Cl29 C21 2.03(2) . ? C1 C10 1.427(10) . ? C1 C6 1.429(9) . ? C1 C2 1.432(8) . ? C2 C3 1.403(8) . ? C2 C13 1.526(8) . ? C3 C4 1.426(8) . ? C3 C16 1.512(8) . ? C4 C5 1.367(9) . ? C4 C19 1.517(9) . ? C5 C6 1.374(10) . ? C5 C22 1.552(9) . ? C6 C7 1.413(9) . ? C7 C8 1.349(12) . ? C7 C23 1.494(11) . ? C8 C9 1.417(12) . ? C8 C26 1.520(10) . ? C9 C10 1.400(9) . ? C9 C28 1.430(12) . ? C10 C11 1.445(10) . ? C11 C12 1.393(9) . ? C11 C30 1.414(10) . ? C12 C33 1.420(9) . ? C12 C13 1.513(9) . ? C13 C14 1.590(8) . ? C14 C15 1.480(8) . ? C14 C34 1.510(8) . ? C15 C37 1.355(8) . ? C15 C16 1.486(8) . ? C16 C17 1.516(8) . ? C17 C18 1.318(8) . ? C17 C38 1.501(8) . ? C18 C41 1.503(8) . ? C18 C19 1.509(8) . ? C19 C20 1.527(8) . ? C20 C21 1.376(10) . ? C20 C42 1.414(8) . ? C21 C45 1.434(10) . ? C21 C22 1.519(9) . ? C22 C23 1.626(12) . ? C23 C24 1.574(11) . ? C24 C46 1.505(10) . ? C24 C25 1.691(16) . ? C25 C48 1.499(13) . ? C25 C26 1.563(13) . ? C26 C27 1.690(17) . ? C27 C28 1.528(12) . ? C27 C50 1.576(15) . ? C28 C29 1.353(13) . ? C29 C30 1.426(11) . ? C29 C52 1.505(13) . ? C30 C31 1.386(11) . ? C31 C32 1.417(11) . ? C31 C53 1.515(10) . ? C32 C56 1.416(10) . ? C32 C33 1.427(9) . ? C33 C34 1.385(9) . ? C34 C35 1.393(8) . ? C35 C57 1.411(8) . ? C35 C36 1.484(9) . ? C36 C37 1.490(8) . ? C36 C59 1.505(8) . ? C37 C38 1.517(9) . ? C38 C39 1.561(8) . ? C39 C40 1.498(8) . ? C39 C60 1.503(8) . ? C40 C62 1.347(8) . ? C40 C41 1.494(8) . ? C41 C42 1.491(9) . ? C42 C43 1.370(8) . ? C43 C44 1.399(9) . ? C43 C63 1.511(8) . ? C44 C65 1.401(9) . ? C44 C45 1.431(8) . ? C45 C46 1.398(11) . ? C46 C47 1.361(11) . ? C47 C48 1.396(11) . ? C47 C66 1.427(9) . ? C48 C49 1.371(14) . ? C49 C68 1.421(12) . ? C49 C50 1.524(12) . ? C50 C51 1.671(17) . ? C51 C69 1.507(11) . ? C51 C52 1.577(13) . ? C52 C53 1.684(15) . ? C53 C54 1.573(12) . ? C54 C70 1.490(12) . ? C54 C55 1.607(12) . ? C55 C56 1.527(9) . ? C55 C72 1.544(9) . ? C56 C57 1.376(10) . ? C57 C58 1.537(8) . ? C58 C59 1.509(9) . ? C58 C73 1.525(8) . ? C59 C60 1.328(8) . ? C60 C61 1.506(7) . ? C61 C62 1.483(8) . ? C61 C74 1.519(8) . ? C62 C63 1.481(8) . ? C63 C64 1.578(8) . ? C64 C65 1.505(8) . ? C64 C75 1.544(8) . ? C65 C66 1.365(9) . ? C66 C67 1.448(10) . ? C67 C68 1.392(9) . ? C67 C76 1.426(9) . ? C68 C69 1.417(12) . ? C69 C70 1.346(13) . ? C70 C71 1.410(10) . ? C71 C72 1.381(10) . ? C71 C76 1.415(9) . ? C72 C73 1.378(9) . ? C73 C74 1.420(8) . ? C74 C75 1.388(8) . ? C75 C76 1.423(8) . ? 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 Cl1A Cl1 C13 95(2) . . ? Cl1 Cl1A C13 64.6(17) . . ? Cl4A Cl4 C19 65(2) . . ? Cl4 Cl4A C19 94(2) . . ? Cl5A Cl5 C22 57.1(11) . . ? Cl5 Cl5A C22 95.1(15) . . ? Cl5 Cl5A C23 139.4(16) . . ? C22 Cl5A C23 48.4(6) . . ? Cl5 Cl5A Cl6 161.7(17) . . ? C22 Cl5A Cl6 96.6(9) . . ? C23 Cl5A Cl6 48.5(5) . . ? C23 Cl6 Cl5A 64.4(5) . . ? Cl7A Cl7 C24 96.6(16) . . ? Cl7 Cl7A C24 56.6(18) . . ? Cl7 Cl7A Cl29 159(2) . . ? C24 Cl7A Cl29 102.5(12) . . ? Cl9A Cl9 C26 75.0(18) . . ? Cl9 Cl9A C26 80.2(18) . . ? Cl9 Cl9A Cl10 161(2) . . ? C26 Cl9A Cl10 88.0(10) . . ? C10A Cl10 C27 99.1(17) . . ? C10A Cl10 Cl9A 171.6(18) . . ? C27 Cl10 Cl9A 72.6(7) . . ? Cl10 C10A C27 56.6(13) . . ? C13A Cl13 C39 79.2(17) . . ? Cl13 C13A C39 72.9(18) . . ? C14A Cl14 C41 76.2(15) . . ? C14A Cl14 Cl27 156(2) . 3_566 ? C41 Cl14 Cl27 98.6(9) . 3_566 ? Cl14 C14A C41 71.8(17) . . ? C53 Cl18 Cl26 86.7(6) . . ? C54 Cl19 C20A 64.9(7) . . ? C20A Cl20 C55 58.7(17) . . ? Cl20 C20A C55 92(2) . . ? Cl20 C20A C54 133(3) . . ? C55 C20A C54 47.2(8) . . ? Cl20 C20A Cl19 155(3) . . ? C55 C20A Cl19 96.2(14) . . ? C54 C20A Cl19 49.1(7) . . ? C21A Cl21 C58 68(3) . . ? Cl21 C21A C58 90(3) . . ? C31 Cl26 Cl18 69.7(6) . . ? C43 Cl27 Cl14 128.5(15) . 3_566 ? C21 Cl29 Cl7A 100.5(16) . . ? C10 C1 C6 117.6(6) . . ? C10 C1 C2 122.9(6) . . ? C6 C1 C2 116.5(6) . . ? C3 C2 C1 119.2(5) . . ? C3 C2 C13 124.2(5) . . ? C1 C2 C13 116.3(5) . . ? C2 C3 C4 121.3(5) . . ? C2 C3 C16 119.3(5) . . ? C4 C3 C16 118.5(5) . . ? C5 C4 C3 119.1(6) . . ? C5 C4 C19 117.1(5) . . ? C3 C4 C19 121.5(5) . . ? C4 C5 C6 120.2(6) . . ? C4 C5 C22 125.7(6) . . ? C6 C5 C22 109.6(6) . . ? C5 C6 C7 112.2(6) . . ? C5 C6 C1 123.0(6) . . ? C7 C6 C1 121.5(7) . . ? C8 C7 C6 120.5(7) . . ? C8 C7 C23 126.7(7) . . ? C6 C7 C23 111.5(7) . . ? C7 C8 C9 119.3(6) . . ? C7 C8 C26 126.6(8) . . ? C9 C8 C26 112.4(8) . . ? C10 C9 C8 122.4(7) . . ? C10 C9 C28 122.9(8) . . ? C8 C9 C28 111.2(7) . . ? C9 C10 C1 118.5(6) . . ? C9 C10 C11 117.4(7) . . ? C1 C10 C11 117.9(5) . . ? C12 C11 C30 118.1(7) . . ? C12 C11 C10 119.6(6) . . ? C30 C11 C10 117.9(6) . . ? C11 C12 C33 118.1(6) . . ? C11 C12 C13 122.5(6) . . ? C33 C12 C13 111.2(5) . . ? C11 C12 Cl25 100.2(5) . . ? C33 C12 Cl25 97.5(5) . . ? C13 C12 Cl25 100.7(5) . . ? C12 C13 C2 110.2(5) . . ? C12 C13 C14 102.6(5) . . ? C2 C13 C14 114.4(5) . . ? C12 C13 Cl1 110.3(4) . . ? C2 C13 Cl1 105.4(4) . . ? C14 C13 Cl1 113.9(4) . . ? C12 C13 Cl1A 130.6(9) . . ? C2 C13 Cl1A 98.5(9) . . ? C14 C13 Cl1A 100.7(8) . . ? Cl1 C13 Cl1A 20.8(7) . . ? C15 C14 C34 108.8(5) . . ? C15 C14 C13 112.6(4) . . ? C34 C14 C13 104.2(5) . . ? C15 C14 Cl2 107.6(4) . . ? C34 C14 Cl2 109.6(4) . . ? C13 C14 Cl2 113.8(4) . . ? C37 C15 C14 123.4(5) . . ? C37 C15 C16 112.0(5) . . ? C14 C15 C16 124.0(5) . . ? C15 C16 C3 111.1(5) . . ? C15 C16 C17 101.4(4) . . ? C3 C16 C17 111.4(5) . . ? C15 C16 Cl3 110.6(4) . . ? C3 C16 Cl3 109.6(4) . . ? C17 C16 Cl3 112.6(4) . . ? C18 C17 C38 124.8(5) . . ? C18 C17 C16 123.1(5) . . ? C38 C17 C16 109.9(5) . . ? C17 C18 C41 123.6(5) . . ? C17 C18 C19 122.3(5) . . ? C41 C18 C19 110.9(5) . . ? C18 C19 C4 111.8(5) . . ? C18 C19 C20 101.9(5) . . ? C4 C19 C20 107.6(5) . . ? C18 C19 Cl4A 129.0(10) . . ? C4 C19 Cl4A 96.3(10) . . ? C20 C19 Cl4A 109.1(9) . . ? C18 C19 Cl4 108.3(4) . . ? C4 C19 Cl4 111.4(4) . . ? C20 C19 Cl4 115.4(4) . . ? Cl4A C19 Cl4 21.1(8) . . ? C21 C20 C42 122.0(6) . . ? C21 C20 C19 124.2(5) . . ? C42 C20 C19 108.9(5) . . ? C20 C21 C45 118.7(5) . . ? C20 C21 C22 118.2(6) . . ? C45 C21 C22 118.3(7) . . ? C20 C21 Cl29 113.0(12) . . ? C45 C21 Cl29 81.7(8) . . ? C22 C21 Cl29 96.9(9) . . ? C21 C22 Cl5A 130.5(10) . . ? C21 C22 C5 103.5(5) . . ? Cl5A C22 C5 111.8(9) . . ? C21 C22 C23 117.9(6) . . ? Cl5A C22 C23 86.9(9) . . ? C5 C22 C23 103.2(6) . . ? C21 C22 Cl5 106.7(5) . . ? Cl5A C22 Cl5 27.8(7) . . ? C5 C22 Cl5 112.4(5) . . ? C23 C22 Cl5 113.0(4) . . ? C7 C23 C24 108.3(7) . . ? C7 C23 C22 102.4(5) . . ? C24 C23 C22 117.4(6) . . ? C7 C23 Cl6 106.4(5) . . ? C24 C23 Cl6 110.0(5) . . ? C22 C23 Cl6 111.4(6) . . ? C7 C23 Cl5A 120.3(7) . . ? C24 C23 Cl5A 130.2(8) . . ? C22 C23 Cl5A 44.7(6) . . ? Cl6 C23 Cl5A 67.1(6) . . ? C46 C24 C23 109.6(6) . . ? C46 C24 C25 101.0(7) . . ? C23 C24 C25 117.6(7) . . ? C46 C24 Cl7 106.0(5) . . ? C23 C24 Cl7 109.7(6) . . ? C25 C24 Cl7 111.9(5) . . ? C46 C24 Cl7A 88.3(10) . . ? C23 C24 Cl7A 98.0(11) . . ? C25 C24 Cl7A 136.5(11) . . ? Cl7 C24 Cl7A 26.8(10) . . ? C48 C25 C26 106.5(8) . . ? C48 C25 C24 101.2(6) . . ? C26 C25 C24 117.8(7) . . ? C48 C25 Cl8 107.3(6) . . ? C26 C25 Cl8 110.6(6) . . ? C24 C25 Cl8 112.3(7) . . ? C8 C26 C25 108.2(7) . . ? C8 C26 C27 101.4(7) . . ? C25 C26 C27 118.9(8) . . ? C8 C26 Cl9A 117.4(8) . . ? C25 C26 Cl9A 119.3(9) . . ? C27 C26 Cl9A 89.6(10) . . ? C8 C26 Cl9 104.5(6) . . ? C25 C26 Cl9 108.8(7) . . ? C27 C26 Cl9 113.6(6) . . ? Cl9A C26 Cl9 24.8(8) . . ? C28 C27 C50 106.9(9) . . ? C28 C27 C26 103.5(7) . . ? C50 C27 C26 119.0(8) . . ? C28 C27 Cl10 106.9(6) . . ? C50 C27 Cl10 109.9(7) . . ? C26 C27 Cl10 109.8(7) . . ? C28 C27 C10A 96.7(9) . . ? C50 C27 C10A 92.9(10) . . ? C26 C27 C10A 134.1(10) . . ? Cl10 C27 C10A 24.3(8) . . ? C29 C28 C9 119.5(7) . . ? C29 C28 C27 127.6(9) . . ? C9 C28 C27 110.3(9) . . ? C28 C29 C30 119.2(8) . . ? C28 C29 C52 127.3(8) . . ? C30 C29 C52 111.4(9) . . ? C31 C30 C11 122.5(7) . . ? C31 C30 C29 110.9(7) . . ? C11 C30 C29 122.2(8) . . ? C30 C31 C32 119.2(6) . . ? C30 C31 C53 112.2(7) . . ? C32 C31 C53 126.3(7) . . ? C30 C31 Cl26 96.7(8) . . ? C32 C31 Cl26 92.7(8) . . ? C53 C31 Cl26 96.2(8) . . ? C56 C32 C31 121.3(6) . . ? C56 C32 C33 117.4(6) . . ? C31 C32 C33 116.6(6) . . ? C34 C33 C12 110.1(5) . . ? C34 C33 C32 122.7(6) . . ? C12 C33 C32 122.1(6) . . ? C33 C34 C35 118.7(5) . . ? C33 C34 C14 111.2(5) . . ? C35 C34 C14 122.8(5) . . ? C33 C34 Cl28 84.0(12) . . ? C35 C34 Cl28 107.7(9) . . ? C14 C34 Cl28 103.4(9) . . ? C34 C35 C57 118.7(6) . . ? C34 C35 C36 122.5(5) . . ? C57 C35 C36 113.1(5) . . ? C35 C36 C37 110.1(5) . . ? C35 C36 C59 101.3(5) . . ? C37 C36 C59 109.2(5) . . ? C35 C36 Cl11 114.5(4) . . ? C37 C36 Cl11 110.4(4) . . ? C59 C36 Cl11 110.8(4) . . ? C15 C37 C36 124.0(5) . . ? C15 C37 C38 111.4(5) . . ? C36 C37 C38 123.5(5) . . ? C17 C38 C37 100.2(4) . . ? C17 C38 C39 114.6(5) . . ? C37 C38 C39 112.2(5) . . ? C17 C38 Cl12 108.2(4) . . ? C37 C38 Cl12 107.7(4) . . ? C39 C38 Cl12 113.0(4) . . ? C40 C39 C60 100.0(4) . . ? C40 C39 C38 112.5(5) . . ? C60 C39 C38 115.0(5) . . ? C40 C39 Cl13 107.1(4) . . ? C60 C39 Cl13 107.7(4) . . ? C38 C39 Cl13 113.5(4) . . ? C40 C39 C13A 132.9(10) . . ? C60 C39 C13A 90.0(14) . . ? C38 C39 C13A 104.1(13) . . ? Cl13 C39 C13A 27.9(9) . . ? C62 C40 C41 123.3(5) . . ? C62 C40 C39 111.7(5) . . ? C41 C40 C39 123.8(5) . . ? C42 C41 C40 110.5(5) . . ? C42 C41 C18 101.0(5) . . ? C40 C41 C18 108.4(5) . . ? C42 C41 Cl14 112.7(4) . . ? C40 C41 Cl14 111.3(4) . . ? C18 C41 Cl14 112.4(4) . . ? C42 C41 C14A 144.6(12) . . ? C40 C41 C14A 90.0(12) . . ? C18 C41 C14A 99.1(11) . . ? Cl14 C41 C14A 32.0(11) . . ? C43 C42 C20 120.4(6) . . ? C43 C42 C41 121.6(5) . . ? C20 C42 C41 112.3(5) . . ? C42 C43 C44 118.2(5) . . ? C42 C43 C63 124.0(5) . . ? C44 C43 C63 110.3(5) . . ? C42 C43 Cl27 109.4(9) . . ? C44 C43 Cl27 87.8(11) . . ? C63 C43 Cl27 98.2(9) . . ? C43 C44 C65 109.4(5) . . ? C43 C44 C45 122.4(6) . . ? C65 C44 C45 122.6(6) . . ? C46 C45 C44 115.6(6) . . ? C46 C45 C21 122.9(6) . . ? C44 C45 C21 117.1(6) . . ? C47 C46 C45 119.8(6) . . ? C47 C46 C24 113.3(7) . . ? C45 C46 C24 125.0(7) . . ? C46 C47 C48 111.0(7) . . ? C46 C47 C66 122.9(6) . . ? C48 C47 C66 122.5(8) . . ? C49 C48 C47 118.5(7) . . ? C49 C48 C25 127.3(8) . . ? C47 C48 C25 112.3(9) . . ? C48 C49 C68 120.4(7) . . ? C48 C49 C50 127.7(9) . . ? C68 C49 C50 109.6(9) . . ? C49 C50 C27 105.6(9) . . ? C49 C50 C51 103.7(7) . . ? C27 C50 C51 118.2(8) . . ? C49 C50 Cl15 105.5(6) . . ? C27 C50 Cl15 110.0(6) . . ? C51 C50 Cl15 112.5(7) . . ? C69 C51 C52 107.2(7) . . ? C69 C51 C50 102.0(7) . . ? C52 C51 C50 119.7(8) . . ? C69 C51 Cl16 105.9(7) . . ? C52 C51 Cl16 110.1(7) . . ? C50 C51 Cl16 110.7(6) . . ? C29 C52 C51 106.7(8) . . ? C29 C52 C53 102.0(6) . . ? C51 C52 C53 118.9(7) . . ? C29 C52 Cl17 106.6(6) . . ? C51 C52 Cl17 110.0(5) . . ? C53 C52 Cl17 111.5(6) . . ? C31 C53 C54 109.1(6) . . ? C31 C53 C52 102.1(7) . . ? C54 C53 C52 117.1(7) . . ? C31 C53 Cl18 104.8(6) . . ? C54 C53 Cl18 109.2(6) . . ? C52 C53 Cl18 113.4(5) . . ? C70 C54 C53 108.8(8) . . ? C70 C54 C55 104.0(6) . . ? C53 C54 C55 117.8(6) . . ? C70 C54 Cl19 105.2(5) . . ? C53 C54 Cl19 109.3(5) . . ? C55 C54 Cl19 111.0(6) . . ? C70 C54 C20A 119.0(11) . . ? C53 C54 C20A 131.7(12) . . ? C55 C54 C20A 45.2(9) . . ? Cl19 C54 C20A 66.0(9) . . ? C56 C55 C72 103.5(5) . . ? C56 C55 C20A 133.1(15) . . ? C72 C55 C20A 108.3(15) . . ? C56 C55 C54 118.1(6) . . ? C72 C55 C54 102.6(6) . . ? C20A C55 C54 87.6(13) . . ? C56 C55 Cl20 106.0(5) . . ? C72 C55 Cl20 112.9(5) . . ? C20A C55 Cl20 29.2(13) . . ? C54 C55 Cl20 113.4(5) . . ? C57 C56 C32 118.8(6) . . ? C57 C56 C55 118.1(6) . . ? C32 C56 C55 119.3(7) . . ? C56 C57 C35 122.9(6) . . ? C56 C57 C58 124.3(6) . . ? C35 C57 C58 108.1(5) . . ? C59 C58 C73 111.2(5) . . ? C59 C58 C57 102.3(5) . . ? C73 C58 C57 107.2(5) . . ? C59 C58 C21A 131.4(12) . . ? C73 C58 C21A 99.9(11) . . ? C57 C58 C21A 102.8(13) . . ? C59 C58 Cl21 109.1(4) . . ? C73 C58 Cl21 111.8(4) . . ? C57 C58 Cl21 114.8(4) . . ? C21A C58 Cl21 22.4(11) . . ? C60 C59 C36 122.9(5) . . ? C60 C59 C58 123.5(5) . . ? C36 C59 C58 110.2(5) . . ? C59 C60 C39 125.1(5) . . ? C59 C60 C61 122.3(5) . . ? C39 C60 C61 110.3(5) . . ? C62 C61 C60 100.8(4) . . ? C62 C61 C74 111.8(4) . . ? C60 C61 C74 111.6(4) . . ? C62 C61 Cl22 109.5(4) . . ? C60 C61 Cl22 113.9(4) . . ? C74 C61 Cl22 109.1(4) . . ? C40 C62 C63 123.6(5) . . ? C40 C62 C61 112.3(5) . . ? C63 C62 C61 123.6(5) . . ? C62 C63 C43 108.3(5) . . ? C62 C63 C64 112.3(5) . . ? C43 C63 C64 105.0(5) . . ? C62 C63 Cl23 108.0(4) . . ? C43 C63 Cl23 109.0(4) . . ? C64 C63 Cl23 114.0(4) . . ? C65 C64 C75 108.3(5) . . ? C65 C64 C63 102.0(4) . . ? C75 C64 C63 115.0(4) . . ? C65 C64 Cl24 110.8(4) . . ? C75 C64 Cl24 106.2(4) . . ? C63 C64 Cl24 114.3(4) . . ? C66 C65 C44 119.0(6) . . ? C66 C65 C64 123.3(6) . . ? C44 C65 C64 112.8(5) . . ? C65 C66 C47 117.4(7) . . ? C65 C66 C67 119.8(6) . . ? C47 C66 C67 117.9(6) . . ? C68 C67 C76 119.4(6) . . ? C68 C67 C66 117.0(7) . . ? C76 C67 C66 117.3(5) . . ? C67 C68 C69 121.8(7) . . ? C67 C68 C49 122.7(8) . . ? C69 C68 C49 111.6(7) . . ? C70 C69 C68 119.3(7) . . ? C70 C69 C51 127.2(8) . . ? C68 C69 C51 111.7(9) . . ? C69 C70 C71 120.4(7) . . ? C69 C70 C54 127.4(7) . . ? C71 C70 C54 110.5(7) . . ? C72 C71 C70 112.1(6) . . ? C72 C71 C76 122.6(6) . . ? C70 C71 C76 121.9(7) . . ? C73 C72 C71 119.7(6) . . ? C73 C72 C55 125.8(6) . . ? C71 C72 C55 109.9(6) . . ? C72 C73 C74 119.1(5) . . ? C72 C73 C58 117.1(5) . . ? C74 C73 C58 121.4(5) . . ? C75 C74 C73 121.6(5) . . ? C75 C74 C61 118.6(5) . . ? C73 C74 C61 119.1(5) . . ? C74 C75 C76 119.2(5) . . ? C74 C75 C64 124.1(5) . . ? C76 C75 C64 116.4(5) . . ? C71 C76 C75 117.4(6) . . ? C71 C76 C67 117.0(6) . . ? C75 C76 C67 122.8(6) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.092 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.119 # Attachment '- c76cl-II_805558.CIF' data_c76cl-II_805558 _database_code_depnum_ccdc_archive 'CCDC 805558' #TrackingRef '- .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl26.24' _chemical_formula_weight 1842.97 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5350(10) _cell_length_b 12.5840(10) _cell_length_c 22.517(2) _cell_angle_alpha 101.465(4) _cell_angle_beta 94.609(5) _cell_angle_gamma 105.838(5) _cell_volume 3050.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38203 _diffrn_reflns_av_R_equivalents 0.1449 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 36.75 _reflns_number_total 10719 _reflns_number_gt 7173 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Three Cl atoms are disordered over two positions each. Two additional Cl atoms with partial occupancy, CL27 and CL28, indicate the presence of a small portion of C76Cl28 molecules in the same crystallographic site. All constraints concern ADP of Cl atoms (ISOR). ; _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^)+(0.0900P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10719 _refine_ls_number_parameters 957 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1618 _refine_ls_R_factor_gt 0.1172 _refine_ls_wR_factor_ref 0.3062 _refine_ls_wR_factor_gt 0.2848 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.5620(7) 0.1433(6) 0.3587(4) 0.027(4) Uani 0.69(8) 1 d P . . Cl1A Cl 0.554(4) 0.117(8) 0.339(5) 0.105(13) Uani 0.31(8) 1 d P . . Cl2 Cl 0.3836(4) -0.0509(3) 0.26726(19) 0.0718(12) Uani 1 1 d . . . Cl3 Cl 0.5693(3) 0.0321(3) 0.16494(16) 0.0477(8) Uani 1 1 d . . . Cl4 Cl 0.1731(4) -0.0272(3) 0.3214(2) 0.0745(12) Uani 1 1 d . . . Cl5 Cl 0.0544(3) -0.1076(2) 0.14394(15) 0.0466(8) Uani 1 1 d . . . Cl6 Cl 0.3062(4) -0.0596(3) 0.04835(18) 0.0647(11) Uani 1 1 d . . . Cl7 Cl 0.7331(3) 0.2893(3) 0.08382(14) 0.0399(7) Uani 1 1 d . . . Cl8 Cl 0.8705(2) 0.5576(3) 0.16989(15) 0.0427(7) Uani 1 1 d . . . Cl9 Cl 0.9105(3) 0.7085(3) 0.29590(17) 0.0524(9) Uani 1 1 d . . . Cl10 Cl 0.7888(3) 0.8510(3) 0.23372(19) 0.0477(11) Uani 0.848(7) 1 d P . . Cl11 Cl 0.6898(3) 0.9413(2) 0.34621(17) 0.0548(9) Uani 1 1 d . . . Cl12 Cl 0.7892(3) 0.8153(3) 0.42916(16) 0.0575(9) Uani 1 1 d . . . Cl13 Cl 0.5815(3) 0.7876(3) 0.50244(13) 0.0516(8) Uani 1 1 d . . . Cl14 Cl 0.4317(3) 0.8999(2) 0.43444(15) 0.0531(9) Uani 1 1 d . . . Cl15 Cl 0.1848(3) 0.7524(3) 0.44511(13) 0.0486(8) Uani 1 1 d . . . Cl16 Cl 0.2793(3) 0.6094(3) 0.51892(11) 0.0431(7) Uani 1 1 d . . . Cl17 Cl 0.0785(3) 0.3911(3) 0.46735(11) 0.0417(7) Uani 1 1 d . . . Cl18 Cl -0.0563(3) 0.4955(3) 0.38501(12) 0.0393(7) Uani 1 1 d . . . Cl19 Cl -0.1527(2) 0.2730(3) 0.29586(14) 0.0450(8) Uani 1 1 d . . . Cl20 Cl -0.0407(4) 0.1251(3) 0.34649(19) 0.0665(10) Uani 1 1 d . . . Cl21 Cl -0.1484(2) 0.0986(2) 0.16209(12) 0.0343(6) Uani 1 1 d . . . Cl22 Cl 0.1553(3) 0.0470(3) -0.01712(14) 0.0540(9) Uani 1 1 d . . . Cl23 Cl 0.4479(3) 0.2356(3) -0.03331(13) 0.0501(8) Uani 1 1 d . . . Cl24 Cl -0.0240(2) 0.2511(2) 0.02696(11) 0.0356(6) Uani 1 1 d . . . Cl25 Cl 0.2303(3) 0.4549(3) -0.01813(12) 0.0442(7) Uani 1 1 d . . . Cl26 Cl 0.133(2) 0.5985(13) 0.0773(8) 0.033(3) Uani 0.69(8) 1 d P . . C26A Cl 0.097(5) 0.565(7) 0.078(2) 0.046(9) Uani 0.31(8) 1 d P . . Cl27 Cl 0.3379(13) 0.7466(11) 0.1058(6) 0.047(5) Uani 0.236(11) 1 d P . . Cl28 Cl 0.643(4) 0.837(3) 0.1772(18) 0.109(14) Uani 0.152(7) 1 d P . . C1 C 0.5433(8) 0.2684(8) 0.2771(4) 0.023(2) Uani 1 1 d U . . C2 C 0.5962(9) 0.3815(8) 0.3132(4) 0.028(2) Uani 1 1 d . . . C3 C 0.5453(9) 0.4263(9) 0.3660(5) 0.029(2) Uani 1 1 d . . . C4 C 0.4344(9) 0.3577(8) 0.3778(4) 0.025(2) Uani 1 1 d . . . C5 C 0.3889(9) 0.2461(8) 0.3448(4) 0.023(2) Uani 1 1 d U . . C6 C 0.4609(10) 0.1874(9) 0.3057(5) 0.033(2) Uani 1 1 d U . . C7 C 0.3593(10) 0.0842(9) 0.2621(5) 0.033(2) Uani 1 1 d . . . C8 C 0.3664(9) 0.0893(8) 0.1980(5) 0.027(2) Uani 1 1 d . . . C9 C 0.4803(9) 0.1345(9) 0.1741(5) 0.032(2) Uani 1 1 d . . . C10 C 0.5584(9) 0.2451(8) 0.2159(5) 0.027(2) Uani 1 1 d . . . C11 C 0.6284(8) 0.3312(9) 0.1884(5) 0.027(2) Uani 1 1 d U . . C12 C 0.6870(8) 0.4367(8) 0.2254(5) 0.027(2) Uani 1 1 d . . . C13 C 0.6703(8) 0.4622(8) 0.2862(5) 0.026(2) Uani 1 1 d . . . C14 C 0.6962(9) 0.5795(9) 0.3094(5) 0.029(2) Uani 1 1 d . . . C15 C 0.6503(9) 0.6211(9) 0.3589(5) 0.033(3) Uani 1 1 d . . . C16 C 0.5713(10) 0.5417(9) 0.3863(4) 0.030(2) Uani 1 1 d . . . C17 C 0.4921(10) 0.5963(10) 0.4189(4) 0.035(3) Uani 1 1 d . . . C18 C 0.3792(10) 0.5292(9) 0.4250(4) 0.029(2) Uani 1 1 d . . . C19 C 0.3528(10) 0.4108(9) 0.4034(4) 0.028(2) Uani 1 1 d . . . C20 C 0.2257(9) 0.3602(9) 0.3864(4) 0.026(2) Uani 1 1 d . . . C21 C 0.1813(9) 0.2607(8) 0.3452(4) 0.024(2) Uani 1 1 d . . . C22 C 0.2637(10) 0.1952(8) 0.3296(5) 0.029(2) Uani 1 1 d U . . C23 C 0.2361(10) 0.0910(10) 0.2827(5) 0.036(3) Uani 1 1 d . . . C24 C 0.1400(9) 0.0894(8) 0.2342(5) 0.024(2) Uani 1 1 d . . . C25 C 0.1419(9) 0.0425(8) 0.1675(5) 0.027(2) Uani 1 1 d . . . C26 C 0.2685(9) 0.0619(8) 0.1539(5) 0.026(2) Uani 1 1 d . . . C27 C 0.3041(9) 0.0792(9) 0.0946(5) 0.032(2) Uani 1 1 d . . . C28 C 0.4349(9) 0.1504(9) 0.1129(5) 0.030(2) Uani 1 1 d . . . C29 C 0.4899(10) 0.2358(9) 0.0895(5) 0.031(2) Uani 1 1 d . . . C30 C 0.6069(9) 0.3212(9) 0.1206(5) 0.029(2) Uani 1 1 d U . . C31 C 0.5861(9) 0.4343(9) 0.1113(5) 0.030(2) Uani 1 1 d . . . C32 C 0.6315(9) 0.5368(9) 0.1527(5) 0.029(2) Uani 1 1 d . . . C33 C 0.7319(10) 0.5482(9) 0.2037(5) 0.034(2) Uani 1 1 d . . . C34 C 0.7487(10) 0.6450(9) 0.2662(5) 0.033(2) Uani 1 1 d . . . C35 C 0.6877(11) 0.7398(9) 0.2622(5) 0.037(3) Uani 1 1 d . . . C36 C 0.6307(12) 0.7896(9) 0.3241(6) 0.046(3) Uani 1 1 d . . . C37 C 0.6430(11) 0.7376(9) 0.3807(5) 0.040(3) Uani 1 1 d . . . C38 C 0.5281(11) 0.7206(9) 0.4228(5) 0.038(3) Uani 1 1 d . . . C39 C 0.4113(11) 0.7525(9) 0.4021(5) 0.040(3) Uani 1 1 d . . . C40 C 0.2758(11) 0.6685(9) 0.4081(5) 0.037(3) Uani 1 1 d . . . C41 C 0.2707(10) 0.5657(10) 0.4379(4) 0.032(2) Uani 1 1 d . . . C42 C 0.1577(10) 0.4444(9) 0.4088(4) 0.030(2) Uani 1 1 d . . . C43 C 0.0636(9) 0.4444(9) 0.3551(4) 0.027(2) Uani 1 1 d . . . C44 C 0.0091(9) 0.3262(9) 0.3021(4) 0.028(2) Uani 1 1 d . . . C45 C 0.0626(9) 0.2259(10) 0.3053(5) 0.034(3) Uani 1 1 d . . . C46 C 0.0657(9) 0.1549(8) 0.2443(4) 0.027(2) Uani 1 1 d . . . C47 C 0.0132(8) 0.1718(8) 0.1834(4) 0.024(2) Uani 1 1 d . . . C48 C 0.0845(9) 0.1183(8) 0.1387(5) 0.027(2) Uani 1 1 d . . . C49 C 0.1240(8) 0.1615(8) 0.0942(4) 0.024(2) Uani 1 1 d . . . C50 C 0.2255(10) 0.1356(9) 0.0606(5) 0.033(2) Uani 1 1 d . . . C51 C 0.2887(9) 0.2469(9) 0.0511(4) 0.029(2) Uani 1 1 d . . . C52 C 0.4234(10) 0.2825(9) 0.0464(5) 0.033(2) Uani 1 1 d . . . C53 C 0.4761(9) 0.4080(9) 0.0710(4) 0.030(2) Uani 1 1 d . . . C54 C 0.4057(9) 0.4809(9) 0.0767(4) 0.028(2) Uani 1 1 d . . . C55 C 0.4434(9) 0.5782(9) 0.1223(5) 0.028(2) Uani 1 1 d . . . C56 C 0.5618(9) 0.6148(8) 0.1602(5) 0.028(2) Uani 1 1 d . . . C57 C 0.5762(10) 0.6958(9) 0.2137(5) 0.036(3) Uani 1 1 d . . . C58 C 0.4765(10) 0.7196(8) 0.2360(5) 0.033(3) Uani 1 1 d . . . C59 C 0.4984(10) 0.7578(8) 0.3002(5) 0.028(2) Uani 1 1 d . . . C60 C 0.4035(11) 0.7407(9) 0.3330(5) 0.036(3) Uani 1 1 d . . . C61 C 0.2860(10) 0.6760(8) 0.3033(5) 0.027(2) Uani 1 1 d . . . C62 C 0.2179(10) 0.6252(9) 0.3430(4) 0.029(2) Uani 1 1 d . . . C63 C 0.1248(9) 0.5261(9) 0.3215(4) 0.027(2) Uani 1 1 d . . . C64 C 0.1016(8) 0.4785(8) 0.2564(4) 0.020(2) Uani 1 1 d . . . C65 C 0.0415(8) 0.3642(8) 0.2446(4) 0.021(2) Uani 1 1 d . . . C66 C 0.0419(8) 0.2962(8) 0.1878(4) 0.023(2) Uani 1 1 d . . . C67 C 0.0976(8) 0.3480(8) 0.1427(4) 0.021(2) Uani 1 1 d . . . C68 C 0.1087(8) 0.2720(8) 0.0829(4) 0.023(2) Uani 1 1 d . . . C69 C 0.2233(10) 0.3213(9) 0.0608(5) 0.032(3) Uani 1 1 d . . . C70 C 0.2711(10) 0.4421(9) 0.0592(4) 0.029(2) Uani 1 1 d . . . C71 C 0.2249(9) 0.5219(9) 0.1092(4) 0.027(2) Uani 1 1 d . . . C72 C 0.3450(9) 0.6100(8) 0.1429(5) 0.029(2) Uani 1 1 d . . . C73 C 0.3540(9) 0.6650(8) 0.2042(5) 0.030(3) Uani 1 1 d . . . C74 C 0.2608(9) 0.6369(8) 0.2396(4) 0.020(2) Uani 1 1 d . . . C75 C 0.1641(8) 0.5315(8) 0.2143(4) 0.022(2) Uani 1 1 d . . . C76 C 0.1564(8) 0.4635(8) 0.1549(4) 0.023(2) 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 Cl1 0.025(4) 0.032(5) 0.032(5) 0.016(2) 0.002(2) 0.016(3) Cl1A 0.090(17) 0.13(2) 0.12(4) 0.04(3) -0.015(18) 0.067(17) Cl2 0.105(3) 0.0439(18) 0.073(2) 0.0181(17) -0.005(2) 0.0338(19) Cl3 0.0315(14) 0.0457(16) 0.075(2) 0.0107(15) 0.0152(16) 0.0259(13) Cl4 0.077(3) 0.059(2) 0.091(3) 0.034(2) 0.010(2) 0.0152(19) Cl5 0.0440(17) 0.0294(13) 0.0560(18) -0.0001(12) 0.0075(15) 0.0008(12) Cl6 0.062(2) 0.0525(19) 0.069(2) -0.0167(17) 0.0072(19) 0.0229(17) Cl7 0.0272(14) 0.0562(17) 0.0485(15) 0.0161(13) 0.0234(14) 0.0244(13) Cl8 0.0172(12) 0.0591(17) 0.0592(18) 0.0289(15) 0.0120(14) 0.0105(12) Cl9 0.0269(15) 0.0571(18) 0.065(2) 0.0190(16) -0.0061(15) -0.0012(13) Cl10 0.038(2) 0.0350(17) 0.070(2) 0.0277(17) 0.0044(19) 0.0008(14) Cl11 0.0481(18) 0.0312(14) 0.078(2) 0.0068(14) -0.0016(18) 0.0071(13) Cl12 0.0492(19) 0.0521(18) 0.0553(19) 0.0037(15) -0.0178(17) 0.0024(14) Cl13 0.062(2) 0.0506(17) 0.0318(14) -0.0035(12) -0.0133(15) 0.0144(15) Cl14 0.069(2) 0.0363(15) 0.0478(16) -0.0066(13) -0.0081(16) 0.0214(14) Cl15 0.066(2) 0.0527(17) 0.0343(14) -0.0002(13) 0.0074(15) 0.0357(16) Cl16 0.0528(18) 0.0613(18) 0.0161(11) 0.0023(11) 0.0036(12) 0.0233(15) Cl17 0.0480(18) 0.0628(18) 0.0230(12) 0.0160(12) 0.0168(13) 0.0231(15) Cl18 0.0352(15) 0.0620(17) 0.0328(13) 0.0114(12) 0.0188(13) 0.0298(14) Cl19 0.0178(13) 0.0701(19) 0.0457(16) 0.0059(15) 0.0132(13) 0.0136(13) Cl20 0.056(2) 0.075(2) 0.071(2) 0.026(2) 0.014(2) 0.0163(18) Cl21 0.0154(12) 0.0457(14) 0.0366(13) 0.0071(11) 0.0021(11) 0.0028(10) Cl22 0.0495(19) 0.0621(19) 0.0373(15) -0.0099(14) 0.0062(15) 0.0105(15) Cl23 0.0519(19) 0.072(2) 0.0298(14) 0.0081(14) 0.0200(15) 0.0230(16) Cl24 0.0245(13) 0.0554(16) 0.0241(11) 0.0022(11) -0.0034(11) 0.0143(11) Cl25 0.0382(16) 0.080(2) 0.0267(12) 0.0274(14) 0.0112(13) 0.0249(15) Cl26 0.032(6) 0.046(5) 0.034(3) 0.025(3) 0.004(5) 0.022(4) C26A 0.033(16) 0.09(2) 0.036(8) 0.038(15) 0.018(11) 0.032(16) Cl27 0.056(9) 0.049(8) 0.046(7) 0.030(6) 0.003(6) 0.018(6) Cl28 0.14(3) 0.067(18) 0.11(3) 0.041(18) 0.06(3) -0.012(19) C1 0.016(4) 0.028(4) 0.032(4) 0.010(3) 0.002(3) 0.016(3) C2 0.022(5) 0.037(5) 0.030(5) 0.011(4) -0.005(5) 0.017(4) C3 0.023(5) 0.041(6) 0.029(5) 0.014(4) -0.003(5) 0.016(4) C4 0.022(5) 0.035(5) 0.021(4) 0.013(4) 0.002(4) 0.010(4) C5 0.019(4) 0.033(4) 0.024(4) 0.016(4) 0.005(4) 0.013(4) C6 0.029(5) 0.034(5) 0.036(5) 0.007(4) -0.004(4) 0.012(4) C7 0.023(5) 0.034(5) 0.049(6) 0.013(5) 0.014(5) 0.013(4) C8 0.025(5) 0.027(5) 0.036(5) 0.009(4) 0.009(5) 0.014(4) C9 0.020(5) 0.038(6) 0.043(6) 0.008(5) 0.008(5) 0.016(4) C10 0.017(5) 0.036(5) 0.036(5) 0.010(4) 0.005(5) 0.020(4) C11 0.013(4) 0.039(5) 0.037(5) 0.006(4) 0.008(4) 0.018(4) C12 0.006(4) 0.037(5) 0.040(6) 0.013(5) 0.006(5) 0.006(4) C13 0.010(4) 0.036(5) 0.034(5) 0.019(4) 0.000(4) 0.007(4) C14 0.013(5) 0.041(6) 0.036(5) 0.017(5) 0.000(5) 0.011(4) C15 0.023(5) 0.039(6) 0.035(6) 0.018(5) -0.011(5) 0.001(4) C16 0.032(6) 0.038(5) 0.022(4) 0.005(4) -0.007(5) 0.017(5) C17 0.035(6) 0.049(6) 0.017(5) 0.004(4) -0.007(5) 0.013(5) C18 0.035(6) 0.041(6) 0.012(4) 0.006(4) -0.003(4) 0.015(5) C19 0.034(6) 0.040(5) 0.014(4) 0.010(4) -0.001(4) 0.015(5) C20 0.023(5) 0.045(6) 0.019(4) 0.015(4) 0.011(4) 0.017(4) C21 0.020(5) 0.034(5) 0.025(5) 0.014(4) 0.010(4) 0.012(4) C22 0.030(5) 0.034(5) 0.027(4) 0.013(4) 0.003(4) 0.013(4) C23 0.027(6) 0.048(6) 0.040(6) 0.016(5) 0.010(5) 0.015(5) C24 0.015(5) 0.025(5) 0.033(5) 0.015(4) 0.009(5) 0.003(4) C25 0.018(5) 0.027(5) 0.037(5) 0.008(4) 0.012(5) 0.004(4) C26 0.026(5) 0.023(5) 0.033(5) 0.007(4) 0.015(5) 0.008(4) C27 0.018(5) 0.037(5) 0.041(6) 0.007(5) 0.010(5) 0.007(4) C28 0.022(5) 0.036(6) 0.033(5) -0.004(5) 0.003(5) 0.016(4) C29 0.025(5) 0.041(6) 0.031(5) 0.003(5) 0.008(5) 0.020(5) C30 0.014(4) 0.038(5) 0.040(5) 0.009(4) 0.015(4) 0.011(4) C31 0.019(5) 0.049(6) 0.032(5) 0.019(5) 0.014(5) 0.017(5) C32 0.015(5) 0.042(6) 0.036(5) 0.020(5) 0.014(5) 0.008(4) C33 0.020(5) 0.046(6) 0.040(6) 0.019(5) 0.004(5) 0.010(5) C34 0.022(5) 0.037(6) 0.039(6) 0.020(5) 0.001(5) 0.000(4) C35 0.035(6) 0.040(6) 0.038(6) 0.018(5) -0.002(5) 0.010(5) C36 0.045(7) 0.031(6) 0.063(8) 0.011(5) -0.008(7) 0.017(5) C37 0.038(6) 0.037(6) 0.038(6) 0.004(5) -0.012(6) 0.008(5) C38 0.046(7) 0.034(6) 0.025(5) 0.002(4) -0.005(5) 0.005(5) C39 0.049(7) 0.029(5) 0.039(6) 0.005(5) -0.003(6) 0.011(5) C40 0.050(7) 0.033(5) 0.026(5) 0.002(4) -0.001(5) 0.015(5) C41 0.034(6) 0.054(6) 0.009(4) 0.001(4) 0.003(4) 0.021(5) C42 0.037(6) 0.044(6) 0.014(4) 0.004(4) 0.007(5) 0.023(5) C43 0.024(5) 0.041(5) 0.023(4) 0.011(4) 0.007(5) 0.017(4) C44 0.025(5) 0.041(6) 0.022(5) 0.005(4) 0.005(5) 0.017(4) C45 0.021(5) 0.051(6) 0.033(5) 0.006(5) 0.005(5) 0.018(5) C46 0.017(5) 0.036(5) 0.025(5) 0.008(4) -0.001(4) 0.004(4) C47 0.011(4) 0.040(5) 0.021(4) 0.005(4) 0.010(4) 0.005(4) C48 0.016(5) 0.034(5) 0.028(5) -0.003(4) 0.004(5) 0.008(4) C49 0.008(4) 0.038(5) 0.020(4) 0.000(4) 0.003(4) -0.002(4) C50 0.030(6) 0.045(6) 0.022(5) -0.002(4) 0.008(5) 0.012(5) C51 0.025(5) 0.046(6) 0.018(4) 0.004(4) 0.008(4) 0.016(5) C52 0.026(6) 0.045(6) 0.034(5) 0.010(5) 0.013(5) 0.017(5) C53 0.019(5) 0.051(6) 0.022(5) 0.012(5) 0.017(5) 0.007(5) C54 0.023(5) 0.047(6) 0.021(4) 0.021(4) 0.008(5) 0.012(5) C55 0.020(5) 0.043(6) 0.032(5) 0.026(5) 0.012(5) 0.010(4) C56 0.019(5) 0.037(5) 0.031(5) 0.020(4) 0.004(5) 0.006(4) C57 0.032(6) 0.036(6) 0.039(6) 0.016(5) -0.003(5) 0.007(5) C58 0.034(6) 0.023(5) 0.043(6) 0.011(4) -0.001(5) 0.008(4) C59 0.027(6) 0.019(4) 0.038(5) 0.012(4) 0.001(5) 0.002(4) C60 0.050(8) 0.028(5) 0.032(5) 0.004(4) -0.005(6) 0.018(5) C61 0.031(6) 0.022(4) 0.032(5) 0.007(4) 0.003(5) 0.014(4) C62 0.030(6) 0.036(5) 0.026(5) 0.002(4) 0.005(5) 0.022(5) C63 0.021(5) 0.045(6) 0.021(4) 0.004(4) 0.006(4) 0.020(4) C64 0.012(4) 0.036(5) 0.018(4) 0.006(4) 0.009(4) 0.013(4) C65 0.014(5) 0.037(5) 0.020(4) 0.009(4) 0.010(4) 0.015(4) C66 0.009(4) 0.038(5) 0.020(4) 0.003(4) 0.002(4) 0.007(4) C67 0.007(4) 0.042(5) 0.014(4) 0.003(4) 0.004(4) 0.009(4) C68 0.012(5) 0.042(5) 0.012(4) 0.004(4) 0.006(4) 0.004(4) C69 0.025(5) 0.048(6) 0.025(5) 0.002(5) 0.001(5) 0.018(5) C70 0.031(6) 0.043(6) 0.015(4) 0.008(4) 0.008(5) 0.013(5) C71 0.022(5) 0.044(6) 0.024(5) 0.019(4) 0.010(5) 0.013(4) C72 0.025(5) 0.032(5) 0.031(5) 0.013(4) 0.006(5) 0.004(4) C73 0.028(6) 0.027(5) 0.038(6) 0.016(4) -0.004(5) 0.011(4) C74 0.020(5) 0.030(5) 0.018(4) 0.012(4) 0.011(4) 0.011(4) C75 0.018(5) 0.036(5) 0.018(4) 0.009(4) 0.006(4) 0.016(4) C76 0.013(5) 0.044(5) 0.016(4) 0.009(4) 0.002(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C6 1.867(12) . ? Cl1A C6 1.78(3) . ? Cl2 C7 1.822(10) . ? Cl3 C9 1.846(10) . ? Cl4 C23 1.879(13) . ? Cl5 C25 1.828(10) . ? Cl6 C27 1.855(11) . ? Cl7 C30 1.828(10) . ? Cl8 C33 1.811(12) . ? Cl9 C34 1.828(11) . ? Cl10 C35 1.822(12) . ? Cl10 Cl28 1.97(5) . ? Cl11 C36 1.794(12) . ? Cl12 C37 1.836(11) . ? Cl13 C38 1.802(10) . ? Cl14 C39 1.795(11) . ? Cl15 C40 1.819(12) . ? Cl16 C41 1.784(9) . ? Cl17 C42 1.797(11) . ? Cl18 C43 1.801(10) . ? Cl19 C44 1.786(11) . ? Cl20 C45 1.926(13) . ? Cl21 C47 1.815(9) . ? Cl22 C50 1.861(10) . ? Cl23 C52 1.845(11) . ? Cl24 C68 1.827(9) . ? Cl25 C70 1.816(10) . ? Cl26 C26A 0.50(6) . ? Cl26 C71 1.813(14) . ? C26A C71 1.85(3) . ? Cl27 C72 2.073(15) . ? Cl28 C57 2.09(3) . ? C1 C10 1.386(14) . ? C1 C2 1.430(14) . ? C1 C6 1.479(16) . ? C2 C13 1.409(15) . ? C2 C3 1.450(15) . ? C3 C16 1.372(14) . ? C3 C4 1.413(15) . ? C4 C5 1.385(13) . ? C4 C19 1.393(14) . ? C5 C22 1.393(14) . ? C5 C6 1.485(14) . ? C6 C7 1.581(15) . ? C7 C8 1.465(16) . ? C7 C23 1.549(15) . ? C8 C26 1.361(14) . ? C8 C9 1.472(16) . ? C9 C28 1.504(15) . ? C9 C10 1.515(14) . ? C10 C11 1.441(16) . ? C11 C12 1.376(14) . ? C11 C30 1.502(15) . ? C12 C13 1.385(15) . ? C12 C33 1.546(15) . ? C13 C14 1.403(14) . ? C14 C15 1.346(16) . ? C14 C34 1.461(15) . ? C15 C16 1.430(16) . ? C15 C37 1.479(16) . ? C16 C17 1.448(15) . ? C17 C18 1.379(16) . ? C17 C38 1.487(16) . ? C18 C19 1.411(14) . ? C18 C41 1.477(15) . ? C19 C20 1.417(15) . ? C20 C21 1.343(14) . ? C20 C42 1.515(13) . ? C21 C22 1.440(14) . ? C21 C45 1.480(13) . ? C22 C23 1.450(15) . ? C23 C24 1.484(14) . ? C24 C46 1.344(14) . ? C24 C25 1.505(14) . ? C25 C26 1.481(15) . ? C25 C48 1.513(14) . ? C26 C27 1.467(16) . ? C27 C28 1.505(14) . ? C27 C50 1.539(15) . ? C28 C29 1.319(16) . ? C29 C30 1.491(15) . ? C29 C52 1.493(14) . ? C30 C31 1.556(14) . ? C31 C32 1.372(15) . ? C31 C53 1.418(14) . ? C32 C56 1.424(14) . ? C32 C33 1.520(13) . ? C33 C34 1.626(16) . ? C34 C35 1.554(15) . ? C35 C57 1.517(14) . ? C35 C36 1.670(19) . ? C36 C59 1.493(15) . ? C36 C37 1.558(17) . ? C37 C38 1.682(19) . ? C38 C39 1.570(16) . ? C39 C60 1.524(16) . ? C39 C40 1.663(18) . ? C40 C62 1.489(13) . ? C40 C41 1.562(15) . ? C41 C42 1.684(16) . ? C42 C43 1.559(12) . ? C43 C63 1.458(15) . ? C43 C44 1.642(14) . ? C44 C65 1.508(14) . ? C44 C45 1.560(14) . ? C45 C46 1.491(14) . ? C46 C47 1.532(13) . ? C47 C66 1.490(14) . ? C47 C48 1.519(13) . ? C48 C49 1.290(15) . ? C49 C68 1.516(14) . ? C49 C50 1.516(14) . ? C50 C51 1.458(16) . ? C51 C69 1.350(14) . ? C51 C52 1.514(15) . ? C52 C53 1.498(16) . ? C53 C54 1.376(14) . ? C54 C55 1.370(15) . ? C54 C70 1.488(15) . ? C55 C72 1.387(15) . ? C55 C56 1.455(13) . ? C56 C57 1.381(15) . ? C57 C58 1.373(17) . ? C58 C59 1.407(15) . ? C58 C73 1.447(14) . ? C59 C60 1.363(17) . ? C60 C61 1.409(16) . ? C61 C62 1.375(16) . ? C61 C74 1.400(13) . ? C62 C63 1.374(15) . ? C63 C64 1.443(12) . ? C64 C65 1.376(14) . ? C64 C75 1.401(14) . ? C65 C66 1.390(12) . ? C66 C67 1.418(14) . ? C67 C76 1.386(14) . ? C67 C68 1.526(12) . ? C68 C69 1.469(16) . ? C69 C70 1.478(16) . ? C70 C71 1.582(14) . ? C71 C76 1.529(15) . ? C71 C72 1.543(14) . ? C72 C73 1.399(15) . ? C73 C74 1.398(16) . ? C74 C75 1.455(14) . ? C75 C76 1.419(12) . ? 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 C35 Cl10 Cl28 84.9(9) . . ? C26A Cl26 C71 86(5) . . ? Cl26 C26A C71 78(4) . . ? Cl10 Cl28 C57 80.5(15) . . ? C10 C1 C2 118.8(10) . . ? C10 C1 C6 123.7(9) . . ? C2 C1 C6 116.9(9) . . ? C13 C2 C1 118.3(9) . . ? C13 C2 C3 116.2(9) . . ? C1 C2 C3 122.0(10) . . ? C16 C3 C4 117.5(9) . . ? C16 C3 C2 119.2(10) . . ? C4 C3 C2 117.5(9) . . ? C5 C4 C19 118.1(9) . . ? C5 C4 C3 119.2(9) . . ? C19 C4 C3 118.4(9) . . ? C4 C5 C22 120.4(9) . . ? C4 C5 C6 123.1(9) . . ? C22 C5 C6 113.1(8) . . ? C1 C6 C5 110.2(8) . . ? C1 C6 C7 117.9(9) . . ? C5 C6 C7 102.8(8) . . ? C1 C6 Cl1A 105.7(14) . . ? C5 C6 Cl1A 119(4) . . ? C7 C6 Cl1A 102(4) . . ? C1 C6 Cl1 105.7(7) . . ? C5 C6 Cl1 106.1(7) . . ? C7 C6 Cl1 113.5(7) . . ? Cl1A C6 Cl1 15(4) . . ? C8 C7 C23 113.6(9) . . ? C8 C7 C6 110.2(9) . . ? C23 C7 C6 106.4(9) . . ? C8 C7 Cl2 104.7(7) . . ? C23 C7 Cl2 110.7(8) . . ? C6 C7 Cl2 111.4(7) . . ? C26 C8 C7 124.7(10) . . ? C26 C8 C9 110.9(9) . . ? C7 C8 C9 124.2(9) . . ? C8 C9 C28 102.5(8) . . ? C8 C9 C10 111.3(9) . . ? C28 C9 C10 112.1(9) . . ? C8 C9 Cl3 111.1(7) . . ? C28 C9 Cl3 111.0(7) . . ? C10 C9 Cl3 108.8(6) . . ? C1 C10 C11 121.7(9) . . ? C1 C10 C9 119.1(10) . . ? C11 C10 C9 118.2(9) . . ? C12 C11 C10 118.3(9) . . ? C12 C11 C30 117.9(10) . . ? C10 C11 C30 120.8(9) . . ? C11 C12 C13 120.6(10) . . ? C11 C12 C33 126.0(10) . . ? C13 C12 C33 109.2(9) . . ? C12 C13 C14 111.8(9) . . ? C12 C13 C2 122.0(9) . . ? C14 C13 C2 122.5(10) . . ? C15 C14 C13 121.3(10) . . ? C15 C14 C34 124.7(10) . . ? C13 C14 C34 112.3(10) . . ? C14 C15 C16 117.8(10) . . ? C14 C15 C37 128.4(10) . . ? C16 C15 C37 111.8(10) . . ? C3 C16 C15 123.0(10) . . ? C3 C16 C17 123.8(11) . . ? C15 C16 C17 109.2(9) . . ? C18 C17 C16 118.0(10) . . ? C18 C17 C38 126.5(10) . . ? C16 C17 C38 112.2(11) . . ? C17 C18 C19 117.5(10) . . ? C17 C18 C41 127.4(10) . . ? C19 C18 C41 113.4(10) . . ? C4 C19 C18 124.2(10) . . ? C4 C19 C20 120.5(9) . . ? C18 C19 C20 110.2(9) . . ? C21 C20 C19 120.8(9) . . ? C21 C20 C42 127.2(9) . . ? C19 C20 C42 110.5(9) . . ? C20 C21 C22 117.7(9) . . ? C20 C21 C45 124.0(8) . . ? C22 C21 C45 116.9(8) . . ? C5 C22 C21 119.8(9) . . ? C5 C22 C23 111.3(9) . . ? C21 C22 C23 125.9(9) . . ? C22 C23 C24 109.6(8) . . ? C22 C23 C7 106.0(9) . . ? C24 C23 C7 116.4(9) . . ? C22 C23 Cl4 105.9(8) . . ? C24 C23 Cl4 108.3(8) . . ? C7 C23 Cl4 110.1(7) . . ? C46 C24 C23 121.9(9) . . ? C46 C24 C25 113.9(8) . . ? C23 C24 C25 121.9(9) . . ? C26 C25 C24 110.9(8) . . ? C26 C25 C48 108.8(8) . . ? C24 C25 C48 100.4(7) . . ? C26 C25 Cl5 111.8(7) . . ? C24 C25 Cl5 111.1(7) . . ? C48 C25 Cl5 113.3(7) . . ? C8 C26 C27 112.2(9) . . ? C8 C26 C25 123.1(9) . . ? C27 C26 C25 123.3(9) . . ? C26 C27 C28 101.6(9) . . ? C26 C27 C50 114.3(8) . . ? C28 C27 C50 113.3(9) . . ? C26 C27 Cl6 107.8(7) . . ? C28 C27 Cl6 106.4(7) . . ? C50 C27 Cl6 112.5(7) . . ? C29 C28 C9 123.3(9) . . ? C29 C28 C27 125.6(9) . . ? C9 C28 C27 108.5(10) . . ? C28 C29 C30 122.1(9) . . ? C28 C29 C52 122.7(10) . . ? C30 C29 C52 111.0(9) . . ? C29 C30 C11 113.6(10) . . ? C29 C30 C31 102.2(8) . . ? C11 C30 C31 107.0(8) . . ? C29 C30 Cl7 109.6(7) . . ? C11 C30 Cl7 111.2(6) . . ? C31 C30 Cl7 113.0(8) . . ? C32 C31 C53 121.5(9) . . ? C32 C31 C30 124.6(9) . . ? C53 C31 C30 108.5(9) . . ? C31 C32 C56 119.9(9) . . ? C31 C32 C33 118.0(9) . . ? C56 C32 C33 118.9(9) . . ? C32 C33 C12 103.1(8) . . ? C32 C33 C34 117.9(8) . . ? C12 C33 C34 102.7(8) . . ? C32 C33 Cl8 107.1(8) . . ? C12 C33 Cl8 112.1(7) . . ? C34 C33 Cl8 113.5(7) . . ? C14 C34 C35 110.6(9) . . ? C14 C34 C33 103.1(8) . . ? C35 C34 C33 116.6(8) . . ? C14 C34 Cl9 106.2(7) . . ? C35 C34 Cl9 109.9(7) . . ? C33 C34 Cl9 109.8(8) . . ? C57 C35 C34 110.7(9) . . ? C57 C35 C36 102.0(9) . . ? C34 C35 C36 116.9(9) . . ? C57 C35 Cl10 103.3(7) . . ? C34 C35 Cl10 109.5(8) . . ? C36 C35 Cl10 113.3(7) . . ? C59 C36 C37 107.6(11) . . ? C59 C36 C35 101.9(9) . . ? C37 C36 C35 117.6(9) . . ? C59 C36 Cl11 108.9(7) . . ? C37 C36 Cl11 110.2(8) . . ? C35 C36 Cl11 110.1(9) . . ? C15 C37 C36 108.3(9) . . ? C15 C37 C38 103.8(9) . . ? C36 C37 C38 118.2(9) . . ? C15 C37 Cl12 104.9(7) . . ? C36 C37 Cl12 109.7(8) . . ? C38 C37 Cl12 111.0(7) . . ? C17 C38 C39 108.0(9) . . ? C17 C38 C37 102.1(9) . . ? C39 C38 C37 119.0(9) . . ? C17 C38 Cl13 106.0(7) . . ? C39 C38 Cl13 109.3(8) . . ? C37 C38 Cl13 111.4(7) . . ? C60 C39 C38 106.5(10) . . ? C60 C39 C40 101.8(9) . . ? C38 C39 C40 118.5(9) . . ? C60 C39 Cl14 105.8(7) . . ? C38 C39 Cl14 109.6(7) . . ? C40 C39 Cl14 113.3(8) . . ? C62 C40 C41 109.1(8) . . ? C62 C40 C39 102.3(9) . . ? C41 C40 C39 118.6(9) . . ? C62 C40 Cl15 105.9(7) . . ? C41 C40 Cl15 109.8(8) . . ? C39 C40 Cl15 110.2(7) . . ? C18 C41 C40 107.1(10) . . ? C18 C41 C42 101.5(8) . . ? C40 C41 C42 117.8(8) . . ? C18 C41 Cl16 108.1(6) . . ? C40 C41 Cl16 109.9(7) . . ? C42 C41 Cl16 111.6(7) . . ? C20 C42 C43 109.2(7) . . ? C20 C42 C41 102.9(8) . . ? C43 C42 C41 117.3(8) . . ? C20 C42 Cl17 104.9(7) . . ? C43 C42 Cl17 109.5(8) . . ? C41 C42 Cl17 112.0(6) . . ? C63 C43 C42 108.0(8) . . ? C63 C43 C44 103.5(8) . . ? C42 C43 C44 117.0(7) . . ? C63 C43 Cl18 106.0(6) . . ? C42 C43 Cl18 109.9(6) . . ? C44 C43 Cl18 111.6(7) . . ? C65 C44 C45 107.0(8) . . ? C65 C44 C43 102.4(8) . . ? C45 C44 C43 118.6(7) . . ? C65 C44 Cl19 108.9(6) . . ? C45 C44 Cl19 107.9(7) . . ? C43 C44 Cl19 111.6(6) . . ? C21 C45 C46 111.8(8) . . ? C21 C45 C44 113.4(9) . . ? C46 C45 C44 114.1(8) . . ? C21 C45 Cl20 102.3(7) . . ? C46 C45 Cl20 105.7(8) . . ? C44 C45 Cl20 108.3(7) . . ? C24 C46 C45 124.1(8) . . ? C24 C46 C47 109.9(9) . . ? C45 C46 C47 123.9(8) . . ? C66 C47 C48 111.5(9) . . ? C66 C47 C46 107.8(7) . . ? C48 C47 C46 101.9(8) . . ? C66 C47 Cl21 112.5(6) . . ? C48 C47 Cl21 109.8(6) . . ? C46 C47 Cl21 112.9(7) . . ? C49 C48 C25 123.5(9) . . ? C49 C48 C47 122.6(9) . . ? C25 C48 C47 109.8(9) . . ? C48 C49 C68 123.6(9) . . ? C48 C49 C50 125.0(9) . . ? C68 C49 C50 108.3(9) . . ? C51 C50 C49 101.4(8) . . ? C51 C50 C27 115.7(9) . . ? C49 C50 C27 113.9(9) . . ? C51 C50 Cl22 105.4(7) . . ? C49 C50 Cl22 107.7(7) . . ? C27 C50 Cl22 111.8(7) . . ? C69 C51 C50 113.0(10) . . ? C69 C51 C52 123.0(10) . . ? C50 C51 C52 122.4(9) . . ? C29 C52 C53 102.4(8) . . ? C29 C52 C51 109.8(9) . . ? C53 C52 C51 109.8(8) . . ? C29 C52 Cl23 111.7(7) . . ? C53 C52 Cl23 112.9(8) . . ? C51 C52 Cl23 110.0(7) . . ? C54 C53 C31 120.2(9) . . ? C54 C53 C52 122.7(9) . . ? C31 C53 C52 111.3(9) . . ? C55 C54 C53 118.8(9) . . ? C55 C54 C70 112.0(9) . . ? C53 C54 C70 123.0(10) . . ? C54 C55 C72 111.2(9) . . ? C54 C55 C56 122.8(9) . . ? C72 C55 C56 121.6(9) . . ? C57 C56 C32 122.5(9) . . ? C57 C56 C55 116.6(9) . . ? C32 C56 C55 116.1(9) . . ? C58 C57 C56 120.3(10) . . ? C58 C57 C35 111.6(10) . . ? C56 C57 C35 125.6(10) . . ? C58 C57 Cl28 100.2(15) . . ? C56 C57 Cl28 96.6(13) . . ? C35 C57 Cl28 88.9(14) . . ? C57 C58 C59 111.2(9) . . ? C57 C58 C73 122.3(10) . . ? C59 C58 C73 120.9(11) . . ? C60 C59 C58 119.7(9) . . ? C60 C59 C36 127.1(10) . . ? C58 C59 C36 111.6(11) . . ? C59 C60 C61 119.8(10) . . ? C59 C60 C39 126.9(10) . . ? C61 C60 C39 110.8(11) . . ? C62 C61 C74 123.5(9) . . ? C62 C61 C60 110.9(9) . . ? C74 C61 C60 121.8(11) . . ? C63 C62 C61 120.6(9) . . ? C63 C62 C40 124.2(10) . . ? C61 C62 C40 113.1(10) . . ? C62 C63 C64 117.6(10) . . ? C62 C63 C43 129.0(9) . . ? C64 C63 C43 111.5(9) . . ? C65 C64 C75 123.7(8) . . ? C65 C64 C63 110.0(9) . . ? C75 C64 C63 123.3(9) . . ? C64 C65 C66 119.0(9) . . ? C64 C65 C44 111.9(8) . . ? C66 C65 C44 127.4(9) . . ? C65 C66 C67 118.9(9) . . ? C65 C66 C47 117.1(9) . . ? C67 C66 C47 122.1(8) . . ? C76 C67 C66 121.4(8) . . ? C76 C67 C68 119.3(9) . . ? C66 C67 C68 118.6(9) . . ? C69 C68 C49 102.2(8) . . ? C69 C68 C67 110.6(8) . . ? C49 C68 C67 110.2(8) . . ? C69 C68 Cl24 112.0(7) . . ? C49 C68 Cl24 112.9(6) . . ? C67 C68 Cl24 108.8(6) . . ? C51 C69 C68 111.4(10) . . ? C51 C69 C70 123.4(11) . . ? C68 C69 C70 124.5(9) . . ? C69 C70 C54 109.6(8) . . ? C69 C70 C71 112.0(9) . . ? C54 C70 C71 103.8(8) . . ? C69 C70 Cl25 107.8(7) . . ? C54 C70 Cl25 110.7(8) . . ? C71 C70 Cl25 112.9(6) . . ? C76 C71 C72 109.7(8) . . ? C76 C71 C70 115.1(8) . . ? C72 C71 C70 102.2(8) . . ? C76 C71 Cl26 108.4(11) . . ? C72 C71 Cl26 107.3(9) . . ? C70 C71 Cl26 113.6(9) . . ? C76 C71 C26A 96(2) . . ? C72 C71 C26A 122(3) . . ? C70 C71 C26A 113.2(18) . . ? Cl26 C71 C26A 16(2) . . ? C55 C72 C73 119.4(9) . . ? C55 C72 C71 110.0(9) . . ? C73 C72 C71 120.5(10) . . ? C55 C72 Cl27 105.5(9) . . ? C73 C72 Cl27 96.9(7) . . ? C71 C72 Cl27 100.0(7) . . ? C74 C73 C72 122.7(9) . . ? C74 C73 C58 117.7(10) . . ? C72 C73 C58 115.6(11) . . ? C73 C74 C61 119.3(9) . . ? C73 C74 C75 116.6(8) . . ? C61 C74 C75 118.1(9) . . ? C64 C75 C76 117.0(9) . . ? C64 C75 C74 116.6(8) . . ? C76 C75 C74 123.2(9) . . ? C67 C76 C75 119.7(9) . . ? C67 C76 C71 123.4(8) . . ? C75 C76 C71 116.7(9) . . ? _diffrn_measured_fraction_theta_max 0.725 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 1.068 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.172 data_c76cl-III_805559 _database_code_depnum_ccdc_archive 'CCDC 805559' #TrackingRef '- .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl25.92' _chemical_formula_weight 1831.54 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' 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 P2(1)/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 11.5460(10) _cell_length_b 37.895(3) _cell_length_c 14.953(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.500(10) _cell_angle_gamma 90.00 _cell_volume 6167.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3586 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54184 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 36.54 _reflns_number_total 11018 _reflns_number_gt 7449 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Several Cl atoms are disordered over two positions each. All restraints concern ADP of minor components of disordered Cl atoms. ; _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^)+(0.0700P)^2^+130.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11018 _refine_ls_number_parameters 1039 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1760 _refine_ls_R_factor_gt 0.1283 _refine_ls_wR_factor_ref 0.3007 _refine_ls_wR_factor_gt 0.2860 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.1409(3) 0.50343(8) 0.6795(2) 0.0549(9) Uani 1 1 d . . . Cl2 Cl 0.1961(7) 0.50117(18) 0.4900(4) 0.044(2) Uani 0.70(3) 1 d P . . Cl2A Cl 0.145(3) 0.5146(8) 0.4944(12) 0.075(7) Uani 0.30(3) 1 d PU . . Cl3 Cl -0.0199(3) 0.57510(15) 0.4755(3) 0.0567(12) Uani 0.837(6) 1 d P . . Cl3A Cl -0.0352(18) 0.5946(7) 0.4989(19) 0.064(7) Uani 0.163(6) 1 d P . . Cl4 Cl 0.387(3) 0.4869(5) 0.5470(19) 0.080(8) Uani 0.163(6) 1 d P . . Cl5 Cl 0.3898(4) 0.55548(12) 0.3496(2) 0.0513(11) Uani 0.837(6) 1 d P . . Cl5A Cl 0.345(2) 0.5750(7) 0.3461(12) 0.059(6) Uani 0.163(6) 1 d P . . Cl6 Cl 0.1181(4) 0.61554(15) 0.3134(3) 0.0702(14) Uani 0.837(6) 1 d P . . Cl6A Cl 0.094(3) 0.6386(7) 0.334(2) 0.094(11) Uani 0.163(6) 1 d P . . Cl7 Cl -0.0717(3) 0.67242(13) 0.5780(4) 0.0591(12) Uani 0.837(6) 1 d P . . Cl7A Cl -0.058(2) 0.6876(7) 0.627(2) 0.088(10) Uani 0.163(6) 1 d PU . . Cl8 Cl 0.1271(4) 0.74144(12) 0.7956(4) 0.0757(13) Uani 0.86 1 d P . . Cl8A Cl 0.174(3) 0.7490(10) 0.864(3) 0.104(12) Uani 0.14 1 d PU . . Cl9 Cl -0.0062(7) 0.6759(2) 0.8155(6) 0.053(2) Uani 0.70(3) 1 d P . . Cl9A Cl 0.007(3) 0.6847(8) 0.851(3) 0.109(10) Uani 0.30(3) 1 d PU . . Cl10 Cl 0.1367(4) 0.65448(11) 1.0183(3) 0.0643(12) Uani 0.837(6) 1 d P . . Cl11 Cl 0.3074(5) 0.71747(11) 1.0479(4) 0.0756(17) Uani 0.919(11) 1 d P . . C11A Cl 0.377(5) 0.7179(11) 1.102(3) 0.057(13) Uani 0.081(11) 1 d PU . . Cl12 Cl 0.5236(4) 0.67823(12) 1.1846(3) 0.0745(16) Uani 0.919(11) 1 d P . . Cl13 Cl 0.3917(4) 0.60819(11) 1.1743(3) 0.0737(11) Uani 1 1 d . . . Cl14 Cl 0.6141(3) 0.56303(11) 1.2007(2) 0.0669(10) Uani 1 1 d . . . Cl15 Cl 0.7919(4) 0.62300(12) 1.2118(2) 0.0761(12) Uani 1 1 d . . . Cl16 Cl 0.9458(3) 0.58492(11) 1.1135(2) 0.0654(10) Uani 1 1 d . . . Cl17 Cl 0.8026(3) 0.51604(9) 1.0869(2) 0.0588(9) Uani 1 1 d . . . Cl18 Cl 0.8399(3) 0.49660(9) 0.9022(2) 0.0588(9) Uani 1 1 d . . . Cl19 Cl 0.9885(2) 0.56212(9) 0.8971(2) 0.0566(9) Uani 1 1 d . . . Cl20 Cl 0.8901(5) 0.55365(13) 0.6845(4) 0.0445(11) Uani 0.837(6) 1 d P . . C20A Cl 0.892(2) 0.5685(7) 0.693(2) 0.049(7) Uani 0.163(6) 1 d PU . . Cl21 Cl 0.7176(18) 0.5072(6) 0.6516(18) 0.070(7) Uani 0.163(6) 1 d P . . Cl22 Cl 0.7087(3) 0.59282(9) 0.4723(2) 0.0597(9) Uani 1 1 d . . . Cl23 Cl 0.3002(4) 0.67270(11) 0.3238(3) 0.0794(12) Uani 1 1 d . . . Cl24 Cl 0.1135(4) 0.72262(15) 0.4392(4) 0.0692(14) Uani 0.837(6) 1 d P . . C24A Cl 0.133(3) 0.7403(7) 0.482(2) 0.091(10) Uani 0.163(6) 1 d P . . Cl25 Cl 0.3152(4) 0.77462(11) 0.6726(4) 0.0777(15) Uani 0.837(6) 1 d P . . Cl26 Cl 0.6135(3) 0.69391(9) 0.4735(3) 0.0618(9) Uani 1 1 d . . . Cl27 Cl 0.4870(5) 0.75885(14) 0.5652(5) 0.0667(14) Uani 0.837(6) 1 d P . . C27A Cl 0.520(5) 0.7683(10) 0.615(3) 0.14(2) Uani 0.163(6) 1 d P . . Cl28 Cl 0.7043(3) 0.74287(9) 0.7453(3) 0.0673(10) Uani 1 1 d . . . C1 C 0.2105(9) 0.5708(3) 0.7051(8) 0.045(3) Uani 1 1 d . . . C2 C 0.2468(9) 0.5770(3) 0.8072(8) 0.040(3) Uani 1 1 d . . . C3 C 0.3511(9) 0.5577(3) 0.8711(8) 0.041(3) Uani 1 1 d . . . C4 C 0.4192(9) 0.5356(3) 0.8337(8) 0.037(3) Uani 1 1 d . . . C5 C 0.3767(9) 0.5283(3) 0.7375(8) 0.038(3) Uani 1 1 d . . . C6 C 0.2492(10) 0.5367(3) 0.6736(8) 0.047(3) Uani 1 1 d . . . C7 C 0.2658(12) 0.5386(4) 0.5711(8) 0.056(4) Uani 1 1 d . . . C8 C 0.2249(9) 0.5726(3) 0.5231(8) 0.048(3) Uani 1 1 d U . . C9 C 0.1309(10) 0.5945(4) 0.5392(10) 0.062(4) Uani 1 1 d . . . C10 C 0.1493(10) 0.5982(3) 0.6461(10) 0.050(3) Uani 1 1 d . . . C11 C 0.1246(11) 0.6303(4) 0.6789(10) 0.055(3) Uani 1 1 d . . . C12 C 0.1525(11) 0.6352(4) 0.7759(13) 0.065(4) Uani 1 1 d . . . C13 C 0.2152(10) 0.6077(3) 0.8382(9) 0.049(3) Uani 1 1 d . . . C14 C 0.2712(11) 0.6209(3) 0.9341(10) 0.053(3) Uani 1 1 d . . . C15 C 0.3658(12) 0.6031(4) 0.9929(10) 0.057(3) Uani 1 1 d . . . C16 C 0.4090(10) 0.5717(3) 0.9624(8) 0.042(3) Uani 1 1 d . . . C17 C 0.5362(11) 0.5663(3) 1.0127(9) 0.049(3) Uani 1 1 d . . . C18 C 0.6048(9) 0.5486(3) 0.9723(7) 0.036(2) Uani 1 1 d . . . C19 C 0.5506(8) 0.5340(3) 0.8802(7) 0.032(2) Uani 1 1 d . . . C20 C 0.6322(9) 0.5313(3) 0.8311(8) 0.037(3) Uani 1 1 d . . . C21 C 0.5887(9) 0.5325(3) 0.7314(7) 0.035(2) Uani 1 1 d . . . C22 C 0.4609(10) 0.5264(3) 0.6880(8) 0.041(3) Uani 1 1 d . . . C23 C 0.4029(9) 0.5337(3) 0.5912(8) 0.041(3) Uani 1 1 d . . . C24 C 0.4682(10) 0.5531(3) 0.5454(7) 0.043(3) Uani 1 1 d . . . C25 C 0.4020(12) 0.5771(4) 0.4621(8) 0.056(3) Uani 1 1 d . . . C26 C 0.2807(11) 0.5883(4) 0.4682(9) 0.052(3) Uani 1 1 d . . . C27 C 0.2270(10) 0.6235(4) 0.4370(9) 0.058(4) Uani 1 1 d . . . C28 C 0.1520(10) 0.6288(4) 0.4974(10) 0.056(4) Uani 1 1 d . . . C29 C 0.1395(11) 0.6586(4) 0.5351(10) 0.063(4) Uani 1 1 d . . . C30 C 0.0937(11) 0.6632(4) 0.6205(11) 0.059(4) Uani 1 1 d . . . C31 C 0.1714(13) 0.6924(4) 0.6760(11) 0.061(4) Uani 1 1 d . . . C32 C 0.2017(13) 0.6996(4) 0.7841(13) 0.076(5) Uani 1 1 d . . . C33 C 0.1528(13) 0.6689(4) 0.8350(12) 0.068(4) Uani 1 1 d . . . C34 C 0.2325(13) 0.6576(4) 0.9456(12) 0.069(4) Uani 1 1 d . . . C35 C 0.3467(13) 0.6796(4) 0.9936(11) 0.064(4) Uani 1 1 d . . . C36 C 0.4724(14) 0.6573(4) 1.0717(11) 0.069(4) Uani 1 1 d . . . C37 C 0.4562(12) 0.6168(4) 1.0859(10) 0.061(4) Uani 1 1 d . . . C38 C 0.5817(12) 0.5907(4) 1.0992(8) 0.052(3) Uani 1 1 d . . . C39 C 0.7015(12) 0.6088(4) 1.0923(9) 0.059(4) Uani 1 1 d . . . C40 C 0.7867(10) 0.5865(4) 1.0401(8) 0.051(3) Uani 1 1 d . . . C41 C 0.7415(10) 0.5496(3) 0.9993(8) 0.048(3) Uani 1 1 d . . . C42 C 0.7612(11) 0.5385(3) 0.8959(9) 0.051(3) Uani 1 1 d . . . C43 C 0.8226(9) 0.5668(3) 0.8500(8) 0.043(3) Uani 1 1 d . . . C44 C 0.7723(10) 0.5686(3) 0.7337(8) 0.045(3) Uani 1 1 d . . . C45 C 0.6580(10) 0.5496(3) 0.6824(7) 0.038(3) Uani 1 1 d . . . C46 C 0.5898(10) 0.5619(3) 0.5903(8) 0.043(3) Uani 1 1 d . . . C47 C 0.6163(11) 0.5969(3) 0.5494(8) 0.047(3) Uani 1 1 d . . . C48 C 0.4879(11) 0.6081(4) 0.4873(8) 0.050(3) Uani 1 1 d . . . C49 C 0.4529(10) 0.6412(4) 0.4810(8) 0.047(3) Uani 1 1 d . . . C50 C 0.3210(13) 0.6530(4) 0.4409(10) 0.065(4) Uani 1 1 d . . . C51 C 0.3162(11) 0.6813(4) 0.5061(10) 0.059(4) Uani 1 1 d . . . C52 C 0.2084(11) 0.6922(4) 0.5293(10) 0.056(3) Uani 1 1 d . . . C53 C 0.2411(11) 0.7068(3) 0.6258(10) 0.055(4) Uani 1 1 d . . . C54 C 0.3518(13) 0.7275(4) 0.6723(11) 0.067(4) Uani 1 1 d . . . C55 C 0.4061(13) 0.7162(3) 0.7746(12) 0.064(4) Uani 1 1 d . . . C56 C 0.3369(11) 0.7052(3) 0.8311(11) 0.055(3) Uani 1 1 d . . . C57 C 0.4013(13) 0.6931(3) 0.9230(11) 0.059(4) Uani 1 1 d . . . C58 C 0.5256(12) 0.6860(3) 0.9472(10) 0.055(3) Uani 1 1 d . . . C59 C 0.5646(12) 0.6626(4) 1.0254(10) 0.059(4) Uani 1 1 d . . . C60 C 0.6653(11) 0.6416(3) 1.0349(9) 0.050(3) Uani 1 1 d . . . C61 C 0.7254(11) 0.6431(4) 0.9668(9) 0.051(3) Uani 1 1 d . . . C62 C 0.7774(10) 0.6113(3) 0.9594(9) 0.047(3) Uani 1 1 d . . . C63 C 0.7959(8) 0.6017(3) 0.8765(7) 0.037(3) Uani 1 1 d . . . C64 C 0.7592(9) 0.6258(3) 0.7993(8) 0.038(3) Uani 1 1 d . . . C65 C 0.7420(10) 0.6081(3) 0.7152(8) 0.040(3) Uani 1 1 d . . . C66 C 0.6675(10) 0.6219(3) 0.6301(7) 0.038(3) Uani 1 1 d . . . C67 C 0.6193(9) 0.6565(3) 0.6290(8) 0.040(3) Uani 1 1 d . . . C68 C 0.5298(11) 0.6705(4) 0.5393(9) 0.052(3) Uani 1 1 d . . . C69 C 0.4355(13) 0.6933(3) 0.5575(9) 0.055(3) Uani 1 1 d . . . C70 C 0.4661(15) 0.7213(4) 0.6305(11) 0.069(4) Uani 1 1 d . . . C71 C 0.5780(12) 0.7112(3) 0.7191(10) 0.058(4) Uani 1 1 d . . . C72 C 0.5293(11) 0.7090(3) 0.8004(9) 0.047(3) Uani 1 1 d . . . C73 C 0.5911(11) 0.6911(3) 0.8855(10) 0.049(3) Uani 1 1 d . . . C74 C 0.6913(10) 0.6677(3) 0.8924(8) 0.043(3) Uani 1 1 d . . . C75 C 0.7049(9) 0.6584(3) 0.8027(8) 0.042(3) Uani 1 1 d . . . C76 C 0.6410(9) 0.6754(3) 0.7149(9) 0.043(3) 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 Cl1 0.0271(14) 0.0682(19) 0.0557(19) 0.0091(14) -0.0044(14) -0.0174(12) Cl2 0.032(3) 0.049(3) 0.036(3) -0.0087(19) -0.008(2) -0.004(2) Cl2A 0.075(12) 0.087(12) 0.065(8) -0.022(7) 0.024(8) -0.014(11) Cl3 0.0209(18) 0.076(3) 0.055(3) 0.006(2) -0.0114(17) -0.0057(19) Cl3A 0.027(10) 0.061(14) 0.078(17) -0.003(12) -0.017(10) 0.012(9) Cl4 0.103(19) 0.046(11) 0.093(18) -0.030(11) 0.036(15) -0.003(11) Cl5 0.065(3) 0.060(3) 0.0199(18) -0.0013(15) 0.0016(17) 0.006(2) Cl5A 0.091(17) 0.066(14) 0.014(9) 0.002(8) 0.008(10) 0.026(12) Cl6 0.054(3) 0.099(4) 0.034(2) 0.011(2) -0.0166(19) 0.003(2) Cl6A 0.11(2) 0.052(13) 0.086(19) -0.023(13) -0.006(16) 0.032(14) Cl7 0.0227(17) 0.074(3) 0.071(3) 0.014(2) 0.0037(19) 0.0106(17) Cl7A 0.043(12) 0.088(16) 0.115(19) -0.055(15) 0.002(12) 0.020(11) Cl8 0.068(3) 0.068(3) 0.102(4) 0.006(3) 0.043(3) 0.013(2) Cl8A 0.084(19) 0.11(2) 0.11(2) -0.074(17) 0.008(16) 0.006(15) Cl9 0.029(3) 0.067(4) 0.068(5) -0.012(3) 0.023(3) 0.001(2) Cl9A 0.074(14) 0.105(14) 0.18(2) -0.043(14) 0.082(15) 0.025(11) Cl10 0.052(2) 0.073(3) 0.084(3) 0.007(2) 0.045(2) 0.0041(18) Cl11 0.083(4) 0.073(3) 0.086(4) -0.020(2) 0.048(3) -0.006(2) C11A 0.058(17) 0.059(15) 0.042(16) -0.025(11) -0.001(12) -0.003(11) Cl12 0.090(3) 0.089(3) 0.054(3) -0.032(2) 0.036(2) -0.029(2) Cl13 0.088(3) 0.093(3) 0.052(2) -0.0094(18) 0.039(2) -0.015(2) Cl14 0.065(2) 0.102(3) 0.0262(16) 0.0057(15) 0.0040(16) -0.0062(18) Cl15 0.065(2) 0.119(3) 0.0312(17) -0.0197(18) -0.0012(17) -0.024(2) Cl16 0.0279(15) 0.112(3) 0.0373(17) 0.0002(16) -0.0148(14) -0.0078(15) Cl17 0.0379(16) 0.085(2) 0.0387(17) 0.0211(15) -0.0076(14) 0.0032(14) Cl18 0.0446(17) 0.0650(19) 0.059(2) 0.0159(15) 0.0072(16) 0.0121(14) Cl19 0.0178(13) 0.084(2) 0.058(2) 0.0036(16) -0.0002(13) 0.0031(12) Cl20 0.035(2) 0.052(3) 0.049(2) -0.005(2) 0.0185(17) 0.002(2) C20A 0.021(8) 0.069(13) 0.067(12) 0.002(10) 0.028(8) -0.004(9) Cl21 0.039(11) 0.066(13) 0.099(18) -0.027(12) 0.017(11) 0.011(9) Cl22 0.061(2) 0.078(2) 0.0447(19) 0.0032(15) 0.0246(17) -0.0027(16) Cl23 0.084(3) 0.101(3) 0.048(2) 0.0334(19) 0.015(2) 0.021(2) Cl24 0.071(3) 0.067(3) 0.064(3) 0.029(2) 0.016(3) 0.029(2) C24A 0.12(2) 0.047(14) 0.09(2) -0.010(13) 0.007(17) 0.042(14) Cl25 0.078(3) 0.051(2) 0.122(4) 0.021(2) 0.056(3) 0.013(2) Cl26 0.056(2) 0.074(2) 0.058(2) 0.0237(16) 0.0231(17) 0.0002(16) Cl27 0.075(3) 0.050(3) 0.086(4) 0.016(2) 0.042(3) 0.001(2) C27A 0.22(5) 0.056(19) 0.10(3) 0.003(18) 0.02(3) 0.02(2) Cl28 0.069(2) 0.0544(19) 0.090(3) -0.0103(17) 0.042(2) -0.0208(16) C1 0.013(5) 0.072(8) 0.044(7) 0.012(6) 0.003(5) -0.011(5) C2 0.014(5) 0.054(7) 0.046(7) 0.009(5) 0.004(5) -0.011(4) C3 0.022(5) 0.066(7) 0.031(6) 0.009(5) 0.004(5) -0.011(5) C4 0.028(5) 0.043(6) 0.033(6) 0.005(4) 0.001(5) -0.009(4) C5 0.018(5) 0.060(7) 0.037(7) 0.008(5) 0.010(5) -0.008(4) C6 0.024(5) 0.063(7) 0.043(7) 0.011(5) -0.005(5) -0.013(5) C7 0.048(7) 0.080(9) 0.025(6) 0.003(6) -0.007(6) -0.027(6) C8 0.013(5) 0.083(8) 0.033(6) 0.004(6) -0.012(5) -0.011(5) C9 0.022(6) 0.077(9) 0.069(10) 0.023(7) -0.009(6) -0.004(5) C10 0.020(5) 0.061(8) 0.067(9) 0.010(6) 0.009(6) -0.004(5) C11 0.031(6) 0.076(9) 0.054(9) 0.022(7) 0.008(6) 0.002(6) C12 0.023(6) 0.073(9) 0.107(13) 0.018(8) 0.033(8) 0.001(5) C13 0.030(6) 0.070(8) 0.041(7) 0.014(6) 0.003(6) -0.009(5) C14 0.029(6) 0.070(8) 0.069(9) 0.006(7) 0.028(7) -0.006(5) C15 0.042(7) 0.071(9) 0.052(8) 0.012(6) 0.008(6) -0.005(6) C16 0.026(5) 0.061(7) 0.035(7) 0.008(5) 0.007(5) -0.006(5) C17 0.036(6) 0.065(8) 0.039(7) 0.005(5) 0.002(6) -0.008(5) C18 0.025(5) 0.054(6) 0.024(6) 0.006(4) 0.003(5) -0.002(4) C19 0.015(5) 0.048(6) 0.025(5) 0.010(4) -0.005(4) 0.002(4) C20 0.028(5) 0.048(6) 0.033(6) 0.001(4) 0.007(5) -0.007(4) C21 0.022(5) 0.052(6) 0.031(6) -0.006(4) 0.010(5) -0.007(4) C22 0.029(6) 0.054(7) 0.028(6) 0.004(5) -0.005(5) -0.012(5) C23 0.025(5) 0.062(7) 0.029(6) -0.005(5) 0.001(5) -0.002(5) C24 0.028(6) 0.065(7) 0.024(6) -0.003(5) -0.007(5) -0.010(5) C25 0.054(8) 0.081(9) 0.029(7) 0.010(6) 0.008(6) -0.006(6) C26 0.042(7) 0.073(8) 0.036(7) 0.003(6) 0.006(6) -0.003(6) C27 0.021(6) 0.098(10) 0.044(8) 0.019(7) -0.007(6) -0.004(6) C28 0.024(6) 0.070(9) 0.057(9) 0.012(7) -0.009(6) 0.017(6) C29 0.023(6) 0.099(12) 0.060(9) 0.039(8) 0.003(6) 0.009(6) C30 0.026(6) 0.077(9) 0.076(10) 0.021(7) 0.020(7) 0.012(6) C31 0.052(8) 0.065(8) 0.071(10) 0.021(7) 0.028(8) 0.020(6) C32 0.052(8) 0.068(9) 0.114(14) 0.021(9) 0.035(9) 0.019(7) C33 0.054(8) 0.065(9) 0.097(12) 0.015(8) 0.041(9) 0.003(7) C34 0.047(8) 0.079(10) 0.089(12) 0.013(8) 0.034(8) -0.002(7) C35 0.062(9) 0.058(8) 0.084(11) -0.013(7) 0.041(8) -0.017(6) C36 0.072(10) 0.089(11) 0.056(9) -0.024(7) 0.036(8) -0.024(8) C37 0.051(8) 0.084(10) 0.046(8) -0.012(7) 0.015(7) -0.003(7) C38 0.050(7) 0.084(9) 0.026(6) -0.006(6) 0.016(6) -0.011(6) C39 0.055(8) 0.076(9) 0.032(7) -0.006(6) -0.005(6) -0.010(6) C40 0.025(6) 0.085(9) 0.032(7) -0.010(6) -0.006(5) -0.001(5) C41 0.029(6) 0.081(9) 0.027(6) 0.010(5) -0.001(5) 0.005(5) C42 0.034(6) 0.066(8) 0.043(7) 0.011(6) 0.000(6) 0.008(5) C43 0.018(5) 0.066(7) 0.030(6) 0.000(5) -0.011(5) -0.007(5) C44 0.029(6) 0.067(8) 0.038(7) -0.004(5) 0.011(5) -0.003(5) C45 0.036(6) 0.051(6) 0.025(6) -0.003(4) 0.007(5) 0.003(5) C46 0.040(6) 0.056(7) 0.032(6) -0.006(5) 0.012(5) -0.009(5) C47 0.045(7) 0.066(8) 0.023(6) 0.002(5) 0.005(5) -0.008(5) C48 0.050(7) 0.073(9) 0.017(6) 0.005(5) -0.001(5) -0.010(6) C49 0.029(6) 0.076(9) 0.037(7) 0.016(6) 0.014(5) 0.004(5) C50 0.057(9) 0.073(9) 0.052(9) 0.022(7) 0.002(7) 0.011(7) C51 0.030(6) 0.083(10) 0.056(9) 0.042(7) 0.006(6) 0.014(6) C52 0.033(6) 0.075(9) 0.052(8) 0.025(6) 0.003(6) 0.007(6) C53 0.033(6) 0.059(8) 0.070(10) 0.027(7) 0.013(7) 0.015(5) C54 0.060(9) 0.064(9) 0.077(11) 0.015(7) 0.025(8) 0.010(7) C55 0.059(9) 0.048(7) 0.097(12) -0.009(7) 0.044(9) -0.016(6) C56 0.041(7) 0.054(7) 0.087(11) 0.008(7) 0.043(8) 0.014(5) C57 0.061(9) 0.059(8) 0.066(9) -0.013(7) 0.033(8) -0.011(6) C58 0.053(8) 0.046(7) 0.063(9) -0.006(6) 0.015(7) -0.005(5) C59 0.046(8) 0.063(8) 0.068(10) -0.026(7) 0.020(7) -0.017(6) C60 0.042(7) 0.064(8) 0.040(7) -0.021(6) 0.009(6) -0.021(6) C61 0.036(6) 0.072(9) 0.039(7) -0.016(6) 0.006(6) -0.024(6) C62 0.024(6) 0.057(7) 0.047(8) -0.008(5) -0.003(5) -0.016(5) C63 0.011(4) 0.061(7) 0.028(6) 0.002(5) -0.009(4) -0.010(4) C64 0.024(5) 0.050(6) 0.036(6) 0.000(5) 0.006(5) -0.009(4) C65 0.032(6) 0.061(7) 0.027(6) 0.001(5) 0.010(5) -0.015(5) C66 0.032(6) 0.053(6) 0.023(6) 0.006(4) 0.003(5) -0.008(5) C67 0.022(5) 0.064(7) 0.035(6) 0.007(5) 0.011(5) -0.012(5) C68 0.036(6) 0.078(9) 0.037(7) 0.017(6) 0.007(6) -0.003(6) C69 0.064(9) 0.048(7) 0.052(8) 0.016(6) 0.019(7) 0.000(6) C70 0.079(10) 0.060(9) 0.068(10) 0.020(7) 0.023(9) 0.010(7) C71 0.051(8) 0.050(7) 0.069(9) 0.005(6) 0.015(7) -0.014(6) C72 0.036(6) 0.053(7) 0.055(8) -0.001(6) 0.020(6) -0.007(5) C73 0.035(6) 0.063(8) 0.058(8) -0.017(6) 0.026(7) -0.016(5) C74 0.039(6) 0.048(6) 0.038(7) -0.013(5) 0.007(5) -0.017(5) C75 0.019(5) 0.058(7) 0.041(7) -0.004(5) -0.001(5) -0.014(4) C76 0.020(5) 0.050(6) 0.062(8) -0.002(5) 0.017(6) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C6 1.798(11) . ? Cl2 Cl2A 0.80(3) . ? Cl2 C7 1.864(14) . ? Cl2 Cl4 2.15(3) . ? Cl2A C7 1.735(19) . ? Cl3 Cl3A 0.86(3) . ? Cl3 C9 1.835(12) . ? Cl3A C9 1.81(2) . ? Cl4 C23 1.88(2) . ? Cl5 Cl5A 0.89(2) . ? Cl5 C25 1.834(14) . ? Cl5A C25 1.64(2) . ? Cl5A C26 2.25(3) . ? Cl6 Cl6A 0.99(2) . ? Cl6 C27 1.881(12) . ? Cl6A C27 1.86(3) . ? Cl7 Cl7A 0.91(3) . ? Cl7 C30 1.833(12) . ? Cl7A C30 2.02(3) . ? Cl8 Cl8A 1.03(3) . ? Cl8 C32 1.839(15) . ? Cl9 Cl9A 0.60(3) . ? Cl9 C33 1.780(16) . ? Cl9A C33 1.88(3) . ? Cl10 C34 1.795(16) . ? Cl11 C11A 0.93(5) . ? Cl11 C35 1.779(14) . ? C11A C35 2.11(4) . ? C11A Cl12 2.29(5) . ? Cl12 C36 1.780(14) . ? Cl13 C37 1.750(15) . ? Cl14 C38 1.778(13) . ? Cl15 C39 1.824(12) . ? Cl16 C40 1.799(11) . ? Cl17 C41 1.791(12) . ? Cl18 C42 1.817(13) . ? Cl19 C43 1.816(10) . ? Cl20 C20A 0.58(3) . ? Cl20 C44 1.838(13) . ? C20A C44 1.68(3) . ? Cl21 C45 1.86(2) . ? Cl22 C47 1.821(13) . ? Cl23 C50 1.844(14) . ? Cl24 C24A 0.90(3) . ? Cl24 C52 1.832(12) . ? C24A C52 2.04(3) . ? Cl25 C54 1.835(15) . ? Cl26 C68 1.823(13) . ? Cl27 C27A 0.79(4) . ? Cl27 C70 1.789(15) . ? C27A C70 1.93(5) . ? Cl28 C71 1.828(12) . ? C1 C10 1.392(16) . ? C1 C2 1.461(17) . ? C1 C6 1.495(18) . ? C2 C13 1.347(18) . ? C2 C3 1.461(15) . ? C3 C4 1.388(16) . ? C3 C16 1.408(16) . ? C4 C5 1.384(16) . ? C4 C19 1.444(13) . ? C5 C22 1.407(17) . ? C5 C6 1.498(14) . ? C6 C7 1.608(18) . ? C7 C8 1.475(18) . ? C7 C23 1.521(17) . ? C8 C26 1.339(17) . ? C8 C9 1.449(19) . ? C9 C28 1.497(19) . ? C9 C10 1.55(2) . ? C10 C11 1.375(19) . ? C11 C12 1.39(2) . ? C11 C30 1.498(18) . ? C12 C13 1.425(18) . ? C12 C33 1.55(2) . ? C13 C14 1.450(19) . ? C14 C15 1.335(17) . ? C14 C34 1.49(2) . ? C15 C16 1.423(19) . ? C15 C37 1.525(18) . ? C16 C17 1.424(15) . ? C17 C18 1.328(17) . ? C17 C38 1.532(17) . ? C18 C19 1.422(14) . ? C18 C41 1.494(15) . ? C19 C20 1.377(16) . ? C20 C21 1.406(15) . ? C20 C42 1.506(15) . ? C21 C45 1.411(15) . ? C21 C22 1.418(14) . ? C22 C23 1.404(15) . ? C23 C24 1.387(16) . ? C24 C46 1.380(15) . ? C24 C25 1.525(16) . ? C25 C26 1.495(19) . ? C25 C48 1.501(18) . ? C26 C27 1.481(19) . ? C27 C28 1.46(2) . ? C27 C50 1.546(19) . ? C28 C29 1.29(2) . ? C29 C52 1.522(19) . ? C29 C30 1.55(2) . ? C30 C31 1.49(2) . ? C31 C53 1.384(19) . ? C31 C32 1.56(2) . ? C32 C56 1.50(2) . ? C32 C33 1.59(2) . ? C33 C34 1.66(2) . ? C34 C35 1.523(19) . ? C35 C57 1.49(2) . ? C35 C36 1.75(2) . ? C36 C59 1.46(2) . ? C36 C37 1.57(2) . ? C37 C38 1.713(19) . ? C38 C39 1.578(19) . ? C39 C60 1.490(19) . ? C39 C40 1.673(19) . ? C40 C62 1.503(18) . ? C40 C41 1.547(18) . ? C41 C42 1.688(18) . ? C42 C43 1.564(17) . ? C43 C63 1.444(16) . ? C43 C44 1.640(16) . ? C44 C45 1.473(15) . ? C44 C65 1.541(17) . ? C45 C46 1.419(15) . ? C46 C47 1.532(16) . ? C47 C66 1.494(15) . ? C47 C48 1.524(16) . ? C48 C49 1.313(18) . ? C49 C68 1.504(18) . ? C49 C50 1.506(17) . ? C50 C51 1.46(2) . ? C51 C69 1.409(18) . ? C51 C52 1.460(19) . ? C52 C53 1.47(2) . ? C53 C54 1.46(2) . ? C54 C55 1.51(2) . ? C54 C70 1.65(2) . ? C55 C72 1.372(18) . ? C55 C56 1.406(19) . ? C56 C57 1.40(2) . ? C57 C58 1.385(19) . ? C58 C73 1.387(19) . ? C58 C59 1.41(2) . ? C59 C60 1.378(19) . ? C60 C61 1.411(19) . ? C61 C62 1.366(18) . ? C61 C74 1.405(17) . ? C62 C63 1.376(17) . ? C63 C64 1.420(15) . ? C64 C65 1.379(16) . ? C64 C75 1.395(16) . ? C65 C66 1.380(14) . ? C66 C67 1.422(16) . ? C67 C76 1.419(17) . ? C67 C68 1.492(15) . ? C68 C69 1.484(19) . ? C69 C70 1.48(2) . ? C70 C71 1.559(19) . ? C71 C72 1.50(2) . ? C71 C76 1.547(18) . ? C72 C73 1.408(18) . ? C73 C74 1.433(17) . ? C74 C75 1.446(17) . ? C75 C76 1.428(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2A Cl2 C7 68.3(14) . . ? Cl2A Cl2 Cl4 144.5(15) . . ? C7 Cl2 Cl4 76.7(7) . . ? Cl2 Cl2A C7 86(2) . . ? Cl3A Cl3 C9 74.5(15) . . ? Cl3 Cl3A C9 78.1(16) . . ? C23 Cl4 Cl2 82.5(10) . . ? Cl5A Cl5 C25 63.3(12) . . ? Cl5 Cl5A C25 87.7(15) . . ? Cl5 Cl5A C26 118.6(16) . . ? C25 Cl5A C26 41.7(8) . . ? Cl6A Cl6 C27 73.6(16) . . ? Cl6 Cl6A C27 75.6(16) . . ? Cl7A Cl7 C30 88.0(15) . . ? Cl7 Cl7A C30 65.3(14) . . ? Cl8A Cl8 C32 103(2) . . ? Cl9A Cl9 C33 90(3) . . ? Cl9 Cl9A C33 72(3) . . ? C11A Cl11 C35 98(3) . . ? Cl11 C11A C35 57(2) . . ? Cl11 C11A Cl12 137(3) . . ? C35 C11A Cl12 82.4(15) . . ? C36 Cl12 C11A 80.1(12) . . ? C20A Cl20 C44 66(3) . . ? Cl20 C20A C44 96(3) . . ? C24A Cl24 C52 89.8(18) . . ? Cl24 C24A C52 64.0(14) . . ? C27A Cl27 C70 88(3) . . ? Cl27 C27A C70 68(3) . . ? C10 C1 C2 116.7(12) . . ? C10 C1 C6 126.0(12) . . ? C2 C1 C6 117.2(10) . . ? C13 C2 C1 118.9(10) . . ? C13 C2 C3 117.8(11) . . ? C1 C2 C3 119.3(11) . . ? C4 C3 C16 117.9(10) . . ? C4 C3 C2 119.6(10) . . ? C16 C3 C2 117.8(11) . . ? C5 C4 C3 119.2(10) . . ? C5 C4 C19 116.3(11) . . ? C3 C4 C19 118.5(10) . . ? C4 C5 C22 119.3(9) . . ? C4 C5 C6 123.5(11) . . ? C22 C5 C6 112.3(10) . . ? C1 C6 C5 108.5(9) . . ? C1 C6 C7 113.9(10) . . ? C5 C6 C7 102.3(10) . . ? C1 C6 Cl1 107.8(9) . . ? C5 C6 Cl1 111.8(8) . . ? C7 C6 Cl1 112.5(8) . . ? C8 C7 C23 110.1(10) . . ? C8 C7 C6 112.5(12) . . ? C23 C7 C6 104.7(9) . . ? C8 C7 Cl2A 94.6(13) . . ? C23 C7 Cl2A 128.3(16) . . ? C6 C7 Cl2A 106.5(10) . . ? C8 C7 Cl2 110.4(8) . . ? C23 C7 Cl2 103.4(10) . . ? C6 C7 Cl2 115.1(8) . . ? Cl2A C7 Cl2 25.2(10) . . ? C26 C8 C9 112.9(12) . . ? C26 C8 C7 123.0(12) . . ? C9 C8 C7 123.6(12) . . ? C8 C9 C28 101.0(12) . . ? C8 C9 C10 111.9(10) . . ? C28 C9 C10 111.5(12) . . ? C8 C9 Cl3A 135.8(14) . . ? C28 C9 Cl3A 99.2(11) . . ? C10 C9 Cl3A 96.3(13) . . ? C8 C9 Cl3 108.6(10) . . ? C28 C9 Cl3 112.9(8) . . ? C10 C9 Cl3 110.7(9) . . ? Cl3A C9 Cl3 27.3(8) . . ? C11 C10 C1 123.7(13) . . ? C11 C10 C9 118.5(12) . . ? C1 C10 C9 116.8(12) . . ? C10 C11 C12 119.2(12) . . ? C10 C11 C30 124.5(14) . . ? C12 C11 C30 115.0(14) . . ? C11 C12 C13 118.3(14) . . ? C11 C12 C33 131.5(13) . . ? C13 C12 C33 108.9(14) . . ? C2 C13 C12 122.9(13) . . ? C2 C13 C14 123.7(11) . . ? C12 C13 C14 110.9(13) . . ? C15 C14 C13 118.3(13) . . ? C15 C14 C34 127.4(14) . . ? C13 C14 C34 112.6(12) . . ? C14 C15 C16 120.6(13) . . ? C14 C15 C37 126.0(13) . . ? C16 C15 C37 111.9(11) . . ? C3 C16 C15 121.5(10) . . ? C3 C16 C17 122.1(12) . . ? C15 C16 C17 111.1(11) . . ? C18 C17 C16 119.9(11) . . ? C18 C17 C38 126.9(11) . . ? C16 C17 C38 111.3(12) . . ? C17 C18 C19 120.1(9) . . ? C17 C18 C41 127.0(10) . . ? C19 C18 C41 110.8(10) . . ? C20 C19 C18 112.8(9) . . ? C20 C19 C4 122.9(9) . . ? C18 C19 C4 120.1(10) . . ? C19 C20 C21 119.7(9) . . ? C19 C20 C42 110.4(10) . . ? C21 C20 C42 127.1(10) . . ? C20 C21 C45 120.1(9) . . ? C20 C21 C22 115.4(10) . . ? C45 C21 C22 121.3(10) . . ? C23 C22 C5 110.9(10) . . ? C23 C22 C21 120.4(11) . . ? C5 C22 C21 123.1(10) . . ? C24 C23 C22 117.6(9) . . ? C24 C23 C7 122.7(10) . . ? C22 C23 C7 109.5(10) . . ? C24 C23 Cl4 109.3(12) . . ? C22 C23 Cl4 97.7(12) . . ? C7 C23 Cl4 94.0(11) . . ? C46 C24 C23 121.3(10) . . ? C46 C24 C25 113.8(10) . . ? C23 C24 C25 120.8(10) . . ? C26 C25 C48 108.5(12) . . ? C26 C25 C24 110.1(11) . . ? C48 C25 C24 98.8(9) . . ? C26 C25 Cl5A 91.5(12) . . ? C48 C25 Cl5A 107.5(12) . . ? C24 C25 Cl5A 138.5(14) . . ? C26 C25 Cl5 113.3(9) . . ? C48 C25 Cl5 114.9(9) . . ? C24 C25 Cl5 110.2(10) . . ? Cl5A C25 Cl5 29.1(8) . . ? C8 C26 C27 110.8(12) . . ? C8 C26 C25 124.3(12) . . ? C27 C26 C25 122.6(12) . . ? C8 C26 Cl5A 139.2(12) . . ? C27 C26 Cl5A 99.5(11) . . ? C25 C26 Cl5A 46.8(8) . . ? C28 C27 C26 101.6(11) . . ? C28 C27 C50 115.7(13) . . ? C26 C27 C50 115.2(10) . . ? C28 C27 Cl6A 88.7(13) . . ? C26 C27 Cl6A 132.7(13) . . ? C50 C27 Cl6A 100.6(13) . . ? C28 C27 Cl6 106.9(8) . . ? C26 C27 Cl6 103.7(10) . . ? C50 C27 Cl6 112.6(9) . . ? Cl6A C27 Cl6 30.8(7) . . ? C29 C28 C27 124.4(14) . . ? C29 C28 C9 121.3(15) . . ? C27 C28 C9 110.7(13) . . ? C28 C29 C52 125.0(15) . . ? C28 C29 C30 125.4(14) . . ? C52 C29 C30 106.2(14) . . ? C31 C30 C11 108.1(11) . . ? C31 C30 C29 103.8(11) . . ? C11 C30 C29 107.8(12) . . ? C31 C30 Cl7 114.6(10) . . ? C11 C30 Cl7 112.2(9) . . ? C29 C30 Cl7 109.9(9) . . ? C31 C30 Cl7A 90.3(12) . . ? C11 C30 Cl7A 113.3(14) . . ? C29 C30 Cl7A 129.6(14) . . ? Cl7 C30 Cl7A 26.7(7) . . ? C53 C31 C30 109.9(13) . . ? C53 C31 C32 121.6(14) . . ? C30 C31 C32 126.4(13) . . ? C56 C32 C31 110.4(13) . . ? C56 C32 C33 111.1(12) . . ? C31 C32 C33 112.0(13) . . ? C56 C32 Cl8 106.3(11) . . ? C31 C32 Cl8 107.3(10) . . ? C33 C32 Cl8 109.5(11) . . ? C12 C33 C32 105.2(13) . . ? C12 C33 C34 104.6(11) . . ? C32 C33 C34 119.8(12) . . ? C12 C33 Cl9 102.9(10) . . ? C32 C33 Cl9 108.8(10) . . ? C34 C33 Cl9 113.7(11) . . ? C12 C33 Cl9A 120.3(16) . . ? C32 C33 Cl9A 107.6(13) . . ? C34 C33 Cl9A 100.4(17) . . ? Cl9 C33 Cl9A 18.6(12) . . ? C14 C34 C35 108.7(11) . . ? C14 C34 C33 102.3(13) . . ? C35 C34 C33 115.7(12) . . ? C14 C34 Cl10 106.2(10) . . ? C35 C34 Cl10 111.2(12) . . ? C33 C34 Cl10 111.8(9) . . ? C57 C35 C34 111.0(13) . . ? C57 C35 C36 100.7(11) . . ? C34 C35 C36 116.3(11) . . ? C57 C35 Cl11 106.3(9) . . ? C34 C35 Cl11 110.2(10) . . ? C36 C35 Cl11 111.6(10) . . ? C57 C35 C11A 107.9(16) . . ? C34 C35 C11A 129.3(18) . . ? C36 C35 C11A 86.2(16) . . ? Cl11 C35 C11A 25.8(13) . . ? C59 C36 C37 109.8(12) . . ? C59 C36 C35 100.9(12) . . ? C37 C36 C35 117.1(11) . . ? C59 C36 Cl12 108.9(10) . . ? C37 C36 Cl12 108.9(10) . . ? C35 C36 Cl12 110.8(10) . . ? C15 C37 C36 106.6(11) . . ? C15 C37 C38 101.7(10) . . ? C36 C37 C38 116.6(11) . . ? C15 C37 Cl13 106.9(10) . . ? C36 C37 Cl13 112.7(10) . . ? C38 C37 Cl13 111.2(9) . . ? C17 C38 C39 105.6(10) . . ? C17 C38 C37 102.3(9) . . ? C39 C38 C37 117.9(11) . . ? C17 C38 Cl14 106.3(9) . . ? C39 C38 Cl14 111.9(9) . . ? C37 C38 Cl14 111.6(9) . . ? C60 C39 C38 108.5(11) . . ? C60 C39 C40 104.3(11) . . ? C38 C39 C40 118.4(10) . . ? C60 C39 Cl15 106.0(9) . . ? C38 C39 Cl15 106.9(9) . . ? C40 C39 Cl15 111.9(8) . . ? C62 C40 C41 108.9(9) . . ? C62 C40 C39 99.4(10) . . ? C41 C40 C39 117.9(10) . . ? C62 C40 Cl16 107.2(8) . . ? C41 C40 Cl16 110.6(8) . . ? C39 C40 Cl16 111.8(8) . . ? C18 C41 C40 108.4(10) . . ? C18 C41 C42 101.5(8) . . ? C40 C41 C42 117.0(10) . . ? C18 C41 Cl17 107.6(8) . . ? C40 C41 Cl17 110.8(8) . . ? C42 C41 Cl17 110.7(8) . . ? C20 C42 C43 109.8(9) . . ? C20 C42 C41 103.2(9) . . ? C43 C42 C41 116.9(10) . . ? C20 C42 Cl18 104.1(8) . . ? C43 C42 Cl18 109.2(9) . . ? C41 C42 Cl18 112.8(8) . . ? C63 C43 C42 109.8(10) . . ? C63 C43 C44 102.8(9) . . ? C42 C43 C44 116.2(9) . . ? C63 C43 Cl19 106.1(7) . . ? C42 C43 Cl19 109.7(7) . . ? C44 C43 Cl19 111.7(8) . . ? C45 C44 C65 105.7(9) . . ? C45 C44 C43 118.1(10) . . ? C65 C44 C43 102.0(9) . . ? C45 C44 C20A 120.9(14) . . ? C65 C44 C20A 95.8(12) . . ? C43 C44 C20A 109.7(13) . . ? C45 C44 Cl20 107.2(8) . . ? C65 C44 Cl20 112.4(8) . . ? C43 C44 Cl20 111.4(7) . . ? C20A C44 Cl20 18.2(9) . . ? C21 C45 C46 115.4(10) . . ? C21 C45 C44 121.3(9) . . ? C46 C45 C44 117.1(10) . . ? C21 C45 Cl21 93.0(11) . . ? C46 C45 Cl21 100.1(11) . . ? C44 C45 Cl21 102.1(10) . . ? C24 C46 C45 122.6(11) . . ? C24 C46 C47 108.7(10) . . ? C45 C46 C47 123.5(10) . . ? C66 C47 C48 110.9(10) . . ? C66 C47 C46 107.8(9) . . ? C48 C47 C46 101.6(10) . . ? C66 C47 Cl22 114.1(8) . . ? C48 C47 Cl22 107.1(8) . . ? C46 C47 Cl22 114.7(9) . . ? C49 C48 C25 124.7(12) . . ? C49 C48 C47 121.6(11) . . ? C25 C48 C47 111.1(11) . . ? C48 C49 C68 123.8(11) . . ? C48 C49 C50 123.9(12) . . ? C68 C49 C50 109.5(11) . . ? C51 C50 C49 102.2(11) . . ? C51 C50 C27 111.9(13) . . ? C49 C50 C27 113.9(11) . . ? C51 C50 Cl23 108.3(9) . . ? C49 C50 Cl23 106.9(10) . . ? C27 C50 Cl23 112.9(9) . . ? C69 C51 C52 122.3(14) . . ? C69 C51 C50 110.6(12) . . ? C52 C51 C50 126.3(13) . . ? C51 C52 C53 112.4(11) . . ? C51 C52 C29 106.2(12) . . ? C53 C52 C29 103.2(12) . . ? C51 C52 Cl24 110.6(9) . . ? C53 C52 Cl24 112.3(10) . . ? C29 C52 Cl24 111.9(8) . . ? C51 C52 C24A 118.0(14) . . ? C53 C52 C24A 86.8(12) . . ? C29 C52 C24A 126.7(13) . . ? Cl24 C52 C24A 26.3(8) . . ? C31 C53 C54 121.9(14) . . ? C31 C53 C52 112.3(12) . . ? C54 C53 C52 124.4(13) . . ? C53 C54 C55 109.4(12) . . ? C53 C54 C70 115.1(13) . . ? C55 C54 C70 103.2(11) . . ? C53 C54 Cl25 110.9(10) . . ? C55 C54 Cl25 107.0(11) . . ? C70 C54 Cl25 110.7(9) . . ? C72 C55 C56 121.0(14) . . ? C72 C55 C54 112.5(13) . . ? C56 C55 C54 124.5(13) . . ? C57 C56 C55 117.7(12) . . ? C57 C56 C32 122.8(13) . . ? C55 C56 C32 118.2(14) . . ? C58 C57 C56 118.9(13) . . ? C58 C57 C35 113.3(14) . . ? C56 C57 C35 126.5(13) . . ? C57 C58 C73 123.1(13) . . ? C57 C58 C59 110.7(13) . . ? C73 C58 C59 122.9(13) . . ? C60 C59 C58 118.1(14) . . ? C60 C59 C36 126.4(15) . . ? C58 C59 C36 113.4(13) . . ? C59 C60 C61 120.3(13) . . ? C59 C60 C39 127.4(13) . . ? C61 C60 C39 109.7(12) . . ? C62 C61 C74 122.5(13) . . ? C62 C61 C60 111.1(12) . . ? C74 C61 C60 121.4(13) . . ? C61 C62 C63 120.7(12) . . ? C61 C62 C40 113.6(12) . . ? C63 C62 C40 124.6(11) . . ? C62 C63 C64 118.0(11) . . ? C62 C63 C43 126.9(11) . . ? C64 C63 C43 113.5(10) . . ? C65 C64 C75 122.3(10) . . ? C65 C64 C63 109.9(10) . . ? C75 C64 C63 123.8(11) . . ? C64 C65 C66 120.7(11) . . ? C64 C65 C44 110.8(9) . . ? C66 C65 C44 124.7(10) . . ? C65 C66 C67 118.9(10) . . ? C65 C66 C47 117.4(10) . . ? C67 C66 C47 121.9(9) . . ? C76 C67 C66 120.4(10) . . ? C76 C67 C68 119.6(11) . . ? C66 C67 C68 119.4(11) . . ? C69 C68 C67 111.9(11) . . ? C69 C68 C49 102.0(10) . . ? C67 C68 C49 110.9(10) . . ? C69 C68 Cl26 111.7(9) . . ? C67 C68 Cl26 109.0(8) . . ? C49 C68 Cl26 111.2(9) . . ? C51 C69 C70 125.7(14) . . ? C51 C69 C68 110.8(12) . . ? C70 C69 C68 122.9(12) . . ? C69 C70 C71 112.2(12) . . ? C69 C70 C54 110.9(13) . . ? C71 C70 C54 104.7(12) . . ? C69 C70 Cl27 102.1(10) . . ? C71 C70 Cl27 115.8(11) . . ? C54 C70 Cl27 111.3(9) . . ? C69 C70 C27A 125.3(18) . . ? C71 C70 C27A 97.0(18) . . ? C54 C70 C27A 104.3(19) . . ? Cl27 C70 C27A 24.3(13) . . ? C72 C71 C76 107.0(10) . . ? C72 C71 C70 105.8(11) . . ? C76 C71 C70 116.6(11) . . ? C72 C71 Cl28 110.4(9) . . ? C76 C71 Cl28 103.4(8) . . ? C70 C71 Cl28 113.4(9) . . ? C55 C72 C73 121.0(12) . . ? C55 C72 C71 113.2(12) . . ? C73 C72 C71 123.0(11) . . ? C58 C73 C72 116.4(12) . . ? C58 C73 C74 118.2(12) . . ? C72 C73 C74 121.1(12) . . ? C61 C74 C73 118.3(12) . . ? C61 C74 C75 118.9(11) . . ? C73 C74 C75 114.8(11) . . ? C64 C75 C76 117.9(11) . . ? C64 C75 C74 116.1(10) . . ? C76 C75 C74 124.1(11) . . ? C67 C76 C75 119.0(10) . . ? C67 C76 C71 122.4(11) . . ? C75 C76 C71 117.6(11) . . ? _diffrn_measured_fraction_theta_max 0.748 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 0.970 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.148 # Attachment '- c76cl-IV_805560.CIF' data_c76cl-IV_805560 _database_code_depnum_ccdc_archive 'CCDC 805560' #TrackingRef '- .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl28.68' _chemical_formula_weight 1929.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.5730(10) _cell_length_b 20.984(2) _cell_length_c 41.190(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12595.9(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 33 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7548 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 169458 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 36.54 _reflns_number_total 14371 _reflns_number_gt 12605 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. CL20 is slightly disordered over two positions with 0.92(2) occupancy of the main component. The presence of CL29 with the occupancy of 0.20 indicates the availability of a molecule with a different addition pattern. All restraints were used for ADP (ISOR). ; _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^)+(0.0800P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14371 _refine_ls_number_parameters 993 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.61224(9) 0.07639(6) 0.72209(3) 0.0408(3) Uani 1 1 d . . . Cl2 Cl 0.40554(10) 0.08092(6) 0.72641(4) 0.0469(3) Uani 1 1 d . . . Cl3 Cl 0.45087(9) 0.22593(6) 0.76019(3) 0.0387(3) Uani 1 1 d . . . Cl4 Cl 0.37638(9) 0.01329(5) 0.66385(4) 0.0456(3) Uani 1 1 d . . . Cl5 Cl 0.18415(7) 0.14331(6) 0.66604(4) 0.0420(3) Uani 1 1 d . . . Cl6 Cl 0.22921(8) 0.27330(6) 0.72330(3) 0.0413(3) Uani 1 1 d . . . Cl7 Cl 0.55840(9) 0.40539(5) 0.75101(3) 0.0338(2) Uani 1 1 d . . . Cl8 Cl 0.70013(10) 0.50710(6) 0.68375(4) 0.0452(3) Uani 1 1 d . . . Cl9 Cl 0.77994(9) 0.40949(7) 0.72635(3) 0.0429(3) Uani 1 1 d . . . Cl10 Cl 0.93528(8) 0.35784(6) 0.68851(3) 0.0384(3) Uani 1 1 d . . . Cl11 Cl 0.90351(7) 0.45085(6) 0.63445(3) 0.0353(3) Uani 1 1 d . . . Cl12 Cl 0.97735(7) 0.36363(6) 0.58308(3) 0.0370(3) Uani 1 1 d . . . Cl13 Cl 1.01993(7) 0.25268(6) 0.62763(3) 0.0391(3) Uani 1 1 d . . . Cl14 Cl 0.97920(7) 0.15143(6) 0.57890(3) 0.0381(3) Uani 1 1 d . . . Cl15 Cl 0.92543(8) 0.23951(6) 0.52477(3) 0.0382(3) Uani 1 1 d . . . Cl16 Cl 0.78416(9) 0.15313(7) 0.49588(3) 0.0401(3) Uani 1 1 d . . . Cl17 Cl 0.81069(8) 0.04551(6) 0.54441(3) 0.0383(3) Uani 1 1 d . . . Cl18 Cl 0.61400(8) 0.00228(6) 0.54450(3) 0.0393(3) Uani 1 1 d . . . Cl19 Cl 0.55277(9) 0.10043(7) 0.49508(3) 0.0435(3) Uani 1 1 d . . . Cl20 Cl 0.36461(10) 0.10883(13) 0.52242(5) 0.0413(5) Uani 0.932(6) 1 d P . . C20A Cl 0.3663(14) 0.0831(10) 0.5335(7) 0.031(5) Uani 0.068(6) 1 d P . . Cl21 Cl 0.37872(9) 0.01773(6) 0.57847(4) 0.0427(5) Uani 0.932(6) 1 d P . . Cl22 Cl 0.20438(7) 0.17556(7) 0.57179(4) 0.0444(3) Uani 1 1 d . . . Cl23 Cl 0.17344(7) 0.35809(6) 0.66860(4) 0.0384(3) Uani 1 1 d . . . Cl24 Cl 0.34755(8) 0.47041(5) 0.70126(3) 0.0315(2) Uani 1 1 d . . . Cl25 Cl 0.50932(10) 0.54248(6) 0.63629(4) 0.0469(3) Uani 1 1 d . . . Cl26 Cl 0.22057(7) 0.36518(6) 0.58128(3) 0.0353(3) Uani 1 1 d . . . Cl27 Cl 0.35143(10) 0.49723(6) 0.59864(4) 0.0458(3) Uani 1 1 d . . . Cl28 Cl 0.46245(9) 0.45037(6) 0.54164(3) 0.0382(3) Uani 1 1 d . . . Cl29 Cl 0.6298(5) 0.3704(4) 0.50565(18) 0.0523(17) Uani 0.20 1 d P . . Cl30 Cl 0.5328(12) 0.6038(11) 0.6828(7) 0.115(8) Uani 0.140(4) 1 d P . . Cl31 Cl 0.6574(16) 0.4329(11) 0.4941(5) 0.106(7) Uani 0.140(4) 1 d PU . . Cl32 Cl 0.595(2) 0.3962(14) 0.4820(6) 0.118(8) Uani 0.126(4) 1 d PU . . Cl33 Cl 0.6336(14) 0.5640(9) 0.6980(6) 0.102(7) Uani 0.140(4) 1 d P . . C1 C 0.6049(3) 0.19321(19) 0.69598(10) 0.0233(8) Uani 1 1 d . . . C2 C 0.6943(3) 0.20148(19) 0.68207(10) 0.0216(8) Uani 1 1 d . . . C3 C 0.7299(3) 0.15934(19) 0.65745(10) 0.0224(8) Uani 1 1 d . . . C4 C 0.6689(3) 0.11446(18) 0.64389(11) 0.0220(8) Uani 1 1 d . . . C5 C 0.5828(3) 0.10434(18) 0.65851(11) 0.0243(8) Uani 1 1 d . . . C6 C 0.5605(3) 0.12762(19) 0.69187(11) 0.0268(9) Uani 1 1 d . . . C7 C 0.4512(3) 0.1250(2) 0.69236(12) 0.0288(9) Uani 1 1 d . . . C8 C 0.4130(3) 0.19002(19) 0.69651(11) 0.0254(9) Uani 1 1 d . . . C9 C 0.4594(3) 0.24033(19) 0.71684(11) 0.0252(8) Uani 1 1 d . . . C10 C 0.5599(3) 0.24639(19) 0.70812(10) 0.0226(8) Uani 1 1 d . . . C11 C 0.6011(3) 0.3082(2) 0.70811(10) 0.0224(8) Uani 1 1 d . . . C12 C 0.6900(3) 0.3148(2) 0.69688(10) 0.0235(8) Uani 1 1 d . . . C13 C 0.7350(3) 0.2617(2) 0.68406(10) 0.0224(8) Uani 1 1 d . . . C14 C 0.8102(3) 0.2810(2) 0.66443(10) 0.0234(8) Uani 1 1 d . . . C15 C 0.8438(3) 0.2412(2) 0.64141(11) 0.0238(8) Uani 1 1 d . . . C16 C 0.8011(2) 0.18111(19) 0.63725(11) 0.0220(8) Uani 1 1 d . . . C17 C 0.8138(2) 0.1606(2) 0.60497(11) 0.0231(8) Uani 1 1 d . . . C18 C 0.7504(3) 0.12061(19) 0.59153(11) 0.0239(8) Uani 1 1 d . . . C19 C 0.6767(3) 0.09999(18) 0.61108(11) 0.0231(8) Uani 1 1 d . . . C20 C 0.5996(3) 0.08618(19) 0.59168(11) 0.0248(8) Uani 1 1 d . . . C21 C 0.5127(3) 0.08727(18) 0.60544(12) 0.0253(9) Uani 1 1 d . . . C22 C 0.5083(3) 0.09001(18) 0.63977(12) 0.0248(9) Uani 1 1 d . . . C23 C 0.4214(3) 0.0936(2) 0.65868(13) 0.0308(10) Uani 1 1 d . . . C24 C 0.3554(3) 0.13120(19) 0.63895(12) 0.0269(9) Uani 1 1 d . . . C25 C 0.2914(3) 0.1797(2) 0.65367(12) 0.0285(9) Uani 1 1 d . . . C26 C 0.3377(3) 0.21241(19) 0.68154(12) 0.0272(9) Uani 1 1 d . . . C27 C 0.3163(3) 0.2793(2) 0.69138(12) 0.0276(9) Uani 1 1 d . . . C28 C 0.4064(3) 0.29919(19) 0.70688(11) 0.0244(8) Uani 1 1 d . . . C29 C 0.4450(3) 0.35618(19) 0.70411(11) 0.0238(8) Uani 1 1 d . . . C30 C 0.5452(3) 0.36807(19) 0.71150(10) 0.0237(8) Uani 1 1 d . . . C31 C 0.5731(3) 0.41255(19) 0.68411(10) 0.0226(8) Uani 1 1 d . . . C32 C 0.6709(3) 0.4235(2) 0.67272(11) 0.0291(9) Uani 1 1 d . . . C33 C 0.7405(3) 0.3762(2) 0.68908(10) 0.0246(8) Uani 1 1 d . . . C34 C 0.8291(3) 0.3505(2) 0.66702(11) 0.0262(9) Uani 1 1 d . . . C35 C 0.8398(3) 0.3783(2) 0.63258(11) 0.0245(8) Uani 1 1 d . . . C36 C 0.8812(3) 0.3293(2) 0.60369(11) 0.0257(9) Uani 1 1 d . . . C37 C 0.9043(3) 0.2588(2) 0.61336(11) 0.0268(9) Uani 1 1 d . . . C38 C 0.8814(3) 0.2006(2) 0.58665(11) 0.0262(9) Uani 1 1 d . . . C39 C 0.8370(3) 0.2204(2) 0.55343(11) 0.0264(9) Uani 1 1 d . . . C40 C 0.7583(3) 0.1707(2) 0.53747(11) 0.0283(9) Uani 1 1 d . . . C41 C 0.7348(3) 0.1083(2) 0.55632(12) 0.0285(9) Uani 1 1 d . . . C42 C 0.6239(3) 0.0840(2) 0.55626(12) 0.0294(9) Uani 1 1 d . . . C43 C 0.5540(3) 0.1251(2) 0.53686(12) 0.0294(9) Uani 1 1 d . . . C44 C 0.4486(3) 0.1312(2) 0.55225(12) 0.0310(10) Uani 1 1 d . . . C45 C 0.4276(3) 0.0972(2) 0.58538(13) 0.0332(10) Uani 1 1 d . . . C46 C 0.3600(3) 0.1356(2) 0.60618(12) 0.0286(9) Uani 1 1 d . . . C47 C 0.3077(3) 0.1943(2) 0.59456(12) 0.0285(9) Uani 1 1 d . . . C48 C 0.2824(3) 0.2257(2) 0.62605(12) 0.0263(9) Uani 1 1 d . . . C49 C 0.2856(3) 0.2885(2) 0.63037(12) 0.0261(9) Uani 1 1 d . . . C50 C 0.2858(3) 0.32261(19) 0.66262(12) 0.0264(9) Uani 1 1 d . . . C51 C 0.3522(3) 0.37573(18) 0.65562(11) 0.0232(8) Uani 1 1 d . . . C52 C 0.4098(3) 0.40674(18) 0.68111(10) 0.0224(8) Uani 1 1 d . . . C53 C 0.4985(3) 0.43000(18) 0.66672(10) 0.0217(8) Uani 1 1 d . . . C54 C 0.5046(3) 0.4541(2) 0.63329(11) 0.0269(9) Uani 1 1 d . . . C55 C 0.5909(2) 0.43226(18) 0.61856(10) 0.0201(7) Uani 1 1 d . . . C56 C 0.6730(3) 0.42106(18) 0.63660(10) 0.0201(7) Uani 1 1 d . . . C57 C 0.7468(3) 0.39641(19) 0.61948(10) 0.0214(8) Uani 1 1 d . . . C58 C 0.7337(3) 0.37255(19) 0.58796(10) 0.0208(8) Uani 1 1 d . . . C59 C 0.8031(2) 0.3277(2) 0.57997(10) 0.0221(8) Uani 1 1 d . . . C60 C 0.7831(3) 0.2807(2) 0.55862(10) 0.0222(8) Uani 1 1 d . . . C61 C 0.6930(3) 0.2764(2) 0.54557(10) 0.0232(8) Uani 1 1 d . . . C62 C 0.6745(3) 0.2126(2) 0.53704(10) 0.0243(8) Uani 1 1 d . . . C63 C 0.5860(3) 0.1925(2) 0.53719(11) 0.0258(8) Uani 1 1 d . . . C64 C 0.5154(3) 0.2359(2) 0.54615(10) 0.0240(8) Uani 1 1 d . . . C65 C 0.4386(3) 0.2029(2) 0.55682(11) 0.0265(9) Uani 1 1 d . . . C66 C 0.3731(3) 0.2344(2) 0.57524(11) 0.0249(8) Uani 1 1 d . . . C67 C 0.3832(3) 0.3010(2) 0.58078(10) 0.0230(8) Uani 1 1 d . . . C68 C 0.3174(3) 0.3332(2) 0.60410(11) 0.0256(8) Uani 1 1 d . . . C69 C 0.3659(3) 0.38347(19) 0.62384(11) 0.0235(8) Uani 1 1 d . . . C70 C 0.4273(3) 0.4321(2) 0.60895(11) 0.0257(8) Uani 1 1 d . . . C71 C 0.4799(3) 0.4041(2) 0.57818(10) 0.0244(8) Uani 1 1 d . . . C72 C 0.5786(3) 0.40832(19) 0.58811(10) 0.0216(8) Uani 1 1 d . . . C73 C 0.6475(3) 0.37326(19) 0.57289(10) 0.0209(8) Uani 1 1 d . . . C74 C 0.6243(3) 0.3217(2) 0.55201(11) 0.0257(8) Uani 1 1 d . . . C75 C 0.5301(3) 0.3005(2) 0.55297(10) 0.0224(8) Uani 1 1 d . . . C76 C 0.4597(3) 0.3342(2) 0.56985(10) 0.0219(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 Cl1 0.0432(7) 0.0311(6) 0.0480(7) 0.0186(5) 0.0135(5) 0.0108(5) Cl2 0.0459(7) 0.0300(6) 0.0648(9) 0.0133(6) 0.0266(6) -0.0015(5) Cl3 0.0504(7) 0.0317(6) 0.0340(6) 0.0053(5) 0.0167(5) 0.0020(5) Cl4 0.0324(6) 0.0215(5) 0.0830(10) -0.0006(6) 0.0234(6) -0.0070(4) Cl5 0.0164(5) 0.0298(5) 0.0797(9) -0.0043(6) 0.0178(5) -0.0072(4) Cl6 0.0314(6) 0.0355(6) 0.0569(8) -0.0043(5) 0.0231(5) -0.0007(5) Cl7 0.0432(6) 0.0315(5) 0.0268(5) -0.0048(4) 0.0045(4) -0.0069(5) Cl8 0.0438(7) 0.0334(6) 0.0584(8) -0.0041(6) -0.0046(6) -0.0134(5) Cl9 0.0396(6) 0.0501(7) 0.0392(6) -0.0115(5) -0.0095(5) -0.0167(6) Cl10 0.0225(5) 0.0466(7) 0.0460(6) 0.0062(5) -0.0172(5) -0.0098(5) Cl11 0.0211(5) 0.0305(5) 0.0545(7) 0.0052(5) -0.0039(4) -0.0148(4) Cl12 0.0152(5) 0.0386(6) 0.0572(7) 0.0119(5) 0.0085(4) -0.0072(4) Cl13 0.0105(4) 0.0465(7) 0.0604(8) 0.0100(6) -0.0068(4) -0.0006(4) Cl14 0.0140(4) 0.0422(6) 0.0581(7) 0.0104(5) 0.0085(4) 0.0073(4) Cl15 0.0243(5) 0.0458(7) 0.0446(6) 0.0094(5) 0.0173(5) 0.0032(5) Cl16 0.0359(6) 0.0495(7) 0.0349(6) -0.0053(5) 0.0123(5) 0.0059(5) Cl17 0.0282(5) 0.0330(6) 0.0536(7) -0.0043(5) 0.0145(5) 0.0092(4) Cl18 0.0339(6) 0.0283(5) 0.0556(7) -0.0177(5) 0.0099(5) -0.0008(4) Cl19 0.0367(6) 0.0536(8) 0.0401(6) -0.0199(6) -0.0028(5) 0.0014(5) Cl20 0.0247(6) 0.0458(12) 0.0535(10) -0.0235(9) -0.0085(6) -0.0048(7) C20A 0.038(9) 0.005(7) 0.052(13) -0.004(7) -0.006(8) -0.002(6) Cl21 0.0264(7) 0.0289(7) 0.0727(11) -0.0202(6) 0.0086(6) -0.0112(5) Cl22 0.0121(4) 0.0530(7) 0.0681(8) -0.0224(7) -0.0060(5) -0.0048(4) Cl23 0.0177(5) 0.0306(5) 0.0668(8) -0.0076(5) 0.0125(5) 0.0036(4) Cl24 0.0343(5) 0.0191(4) 0.0412(6) -0.0037(4) 0.0105(4) 0.0045(4) Cl25 0.0470(7) 0.0260(6) 0.0678(9) 0.0075(6) 0.0072(6) 0.0009(5) Cl26 0.0139(4) 0.0417(6) 0.0504(7) -0.0054(5) -0.0073(4) 0.0091(4) Cl27 0.0410(7) 0.0387(6) 0.0577(8) 0.0132(6) 0.0029(6) 0.0204(5) Cl28 0.0347(6) 0.0393(6) 0.0405(6) 0.0117(5) -0.0090(5) 0.0047(5) Cl29 0.050(4) 0.064(5) 0.042(3) 0.006(3) 0.000(3) 0.008(3) Cl30 0.053(8) 0.107(14) 0.18(2) 0.035(14) -0.001(11) -0.018(9) Cl31 0.106(12) 0.103(11) 0.107(12) 0.048(10) 0.057(10) 0.051(10) Cl32 0.144(16) 0.121(15) 0.088(12) 0.037(11) 0.029(12) 0.048(13) Cl33 0.090(12) 0.079(11) 0.136(17) -0.010(11) 0.021(11) -0.028(9) C1 0.0211(19) 0.0209(18) 0.028(2) 0.0058(16) 0.0012(15) 0.0010(15) C2 0.0166(17) 0.0216(18) 0.0265(19) 0.0059(16) -0.0027(14) 0.0005(14) C3 0.0149(17) 0.0211(18) 0.031(2) 0.0076(16) 0.0018(15) 0.0021(14) C4 0.0155(17) 0.0154(17) 0.035(2) 0.0048(16) 0.0053(15) 0.0029(13) C5 0.0193(18) 0.0139(17) 0.040(2) 0.0037(16) 0.0092(16) 0.0003(14) C6 0.023(2) 0.0176(18) 0.040(2) 0.0042(17) 0.0110(17) 0.0012(15) C7 0.023(2) 0.0184(19) 0.045(3) 0.0011(18) 0.0141(18) 0.0010(15) C8 0.0209(19) 0.0148(17) 0.041(2) 0.0002(16) 0.0129(17) -0.0035(14) C9 0.026(2) 0.0169(18) 0.033(2) 0.0033(16) 0.0108(17) 0.0006(15) C10 0.0218(19) 0.0218(19) 0.0242(19) 0.0052(15) 0.0025(15) -0.0003(15) C11 0.0230(19) 0.0222(19) 0.0220(18) 0.0018(15) 0.0013(15) -0.0024(15) C12 0.0217(19) 0.0244(19) 0.0243(19) 0.0035(16) -0.0073(15) -0.0048(15) C13 0.0155(17) 0.028(2) 0.0241(18) 0.0055(16) -0.0050(14) -0.0011(15) C14 0.0120(16) 0.026(2) 0.032(2) 0.0085(17) -0.0091(15) -0.0034(14) C15 0.0115(16) 0.026(2) 0.034(2) 0.0075(17) -0.0034(15) -0.0015(14) C16 0.0100(16) 0.0198(18) 0.036(2) 0.0076(16) 0.0000(14) 0.0021(13) C17 0.0092(15) 0.0236(19) 0.036(2) 0.0080(17) 0.0049(15) 0.0045(14) C18 0.0138(17) 0.0198(18) 0.038(2) 0.0022(17) 0.0063(16) 0.0051(14) C19 0.0133(17) 0.0145(17) 0.042(2) 0.0008(16) 0.0079(16) 0.0030(13) C20 0.0177(18) 0.0161(17) 0.041(2) -0.0056(17) 0.0072(16) 0.0006(14) C21 0.0146(17) 0.0144(17) 0.047(3) -0.0076(17) 0.0077(17) -0.0032(13) C22 0.0147(17) 0.0130(16) 0.047(2) -0.0024(17) 0.0099(16) -0.0014(13) C23 0.0205(19) 0.0192(19) 0.053(3) -0.0040(19) 0.0148(19) -0.0009(15) C24 0.0118(17) 0.0169(17) 0.052(3) -0.0061(18) 0.0078(17) -0.0046(14) C25 0.0118(17) 0.0210(19) 0.052(3) -0.0057(19) 0.0114(17) -0.0036(14) C26 0.0193(18) 0.0178(18) 0.045(2) -0.0008(17) 0.0161(17) -0.0017(15) C27 0.0220(19) 0.0190(19) 0.042(2) -0.0031(17) 0.0132(18) -0.0015(15) C28 0.0227(19) 0.0185(18) 0.032(2) 0.0005(16) 0.0124(16) 0.0019(15) C29 0.0222(19) 0.0182(18) 0.031(2) -0.0022(16) 0.0063(16) 0.0001(15) C30 0.026(2) 0.0202(18) 0.0250(19) -0.0010(16) 0.0016(16) -0.0039(15) C31 0.0231(19) 0.0163(17) 0.028(2) 0.0004(15) -0.0007(15) -0.0059(14) C32 0.023(2) 0.031(2) 0.034(2) 0.0084(18) 0.0002(17) -0.0035(17) C33 0.0193(18) 0.026(2) 0.029(2) 0.0028(16) -0.0051(15) -0.0076(15) C34 0.0167(18) 0.032(2) 0.030(2) 0.0042(18) -0.0083(15) -0.0046(16) C35 0.0139(17) 0.0246(19) 0.035(2) 0.0054(17) -0.0041(15) -0.0073(14) C36 0.0098(16) 0.030(2) 0.037(2) 0.0082(18) -0.0014(15) -0.0048(14) C37 0.0108(17) 0.031(2) 0.038(2) 0.0072(18) -0.0027(16) -0.0041(15) C38 0.0116(17) 0.027(2) 0.040(2) 0.0087(18) 0.0036(16) 0.0006(15) C39 0.0122(17) 0.032(2) 0.035(2) 0.0053(18) 0.0061(15) 0.0013(15) C40 0.0177(18) 0.033(2) 0.034(2) -0.0004(18) 0.0061(16) 0.0058(16) C41 0.0166(18) 0.029(2) 0.040(2) -0.0024(19) 0.0053(16) 0.0018(16) C42 0.0198(19) 0.025(2) 0.043(3) -0.0070(19) 0.0060(17) 0.0014(16) C43 0.0190(19) 0.032(2) 0.037(2) -0.0097(19) 0.0007(17) 0.0011(16) C44 0.0156(18) 0.032(2) 0.045(3) -0.014(2) -0.0011(17) -0.0001(16) C45 0.0168(19) 0.028(2) 0.055(3) -0.010(2) 0.0081(19) 0.0007(16) C46 0.0129(17) 0.0214(19) 0.051(3) -0.0100(19) 0.0037(17) -0.0044(14) C47 0.0094(16) 0.027(2) 0.049(3) -0.0115(19) 0.0006(16) -0.0039(15) C48 0.0062(15) 0.026(2) 0.047(3) -0.0089(18) 0.0025(15) -0.0021(14) C49 0.0073(15) 0.027(2) 0.044(2) -0.0053(18) 0.0030(15) 0.0008(14) C50 0.0145(17) 0.0172(18) 0.047(3) -0.0021(18) 0.0055(16) -0.0001(14) C51 0.0156(17) 0.0152(17) 0.039(2) -0.0012(16) 0.0052(15) 0.0027(14) C52 0.0211(18) 0.0153(17) 0.031(2) -0.0013(15) 0.0058(15) 0.0005(14) C53 0.0207(18) 0.0136(16) 0.031(2) -0.0026(15) 0.0041(15) -0.0031(14) C54 0.0187(19) 0.026(2) 0.037(2) 0.0068(18) 0.0013(16) -0.0010(15) C55 0.0122(16) 0.0177(17) 0.030(2) 0.0050(15) 0.0000(14) -0.0028(13) C56 0.0151(17) 0.0158(17) 0.030(2) 0.0045(15) -0.0040(14) -0.0049(13) C57 0.0138(16) 0.0210(18) 0.0292(19) 0.0077(16) -0.0033(15) -0.0063(14) C58 0.0123(16) 0.0217(18) 0.0286(19) 0.0075(16) -0.0010(14) -0.0015(14) C59 0.0095(16) 0.028(2) 0.029(2) 0.0089(16) 0.0015(14) -0.0017(14) C60 0.0106(16) 0.030(2) 0.0261(19) 0.0080(16) 0.0040(14) 0.0019(14) C61 0.0162(17) 0.029(2) 0.0248(19) 0.0028(16) 0.0021(14) 0.0011(15) C62 0.0168(18) 0.030(2) 0.0262(19) 0.0012(17) 0.0013(15) 0.0039(16) C63 0.0197(19) 0.031(2) 0.027(2) -0.0056(17) -0.0021(15) 0.0012(16) C64 0.0139(17) 0.032(2) 0.0264(19) -0.0023(17) -0.0041(14) 0.0016(15) C65 0.0152(17) 0.031(2) 0.034(2) -0.0084(18) -0.0052(16) -0.0011(16) C66 0.0099(16) 0.031(2) 0.034(2) -0.0062(18) -0.0050(15) -0.0010(15) C67 0.0091(16) 0.028(2) 0.032(2) -0.0028(17) -0.0061(14) 0.0045(14) C68 0.0095(16) 0.027(2) 0.041(2) -0.0033(18) -0.0026(15) 0.0019(14) C69 0.0125(16) 0.0176(17) 0.040(2) -0.0019(17) -0.0010(15) 0.0045(14) C70 0.0145(17) 0.029(2) 0.033(2) 0.0018(17) -0.0004(15) 0.0010(15) C71 0.0147(17) 0.028(2) 0.030(2) 0.0027(17) -0.0029(15) 0.0021(15) C72 0.0125(16) 0.0211(18) 0.031(2) 0.0069(16) -0.0034(14) -0.0004(14) C73 0.0146(17) 0.0222(18) 0.0259(19) 0.0061(15) -0.0019(14) -0.0002(14) C74 0.0150(18) 0.031(2) 0.031(2) 0.0000(18) -0.0027(15) 0.0016(15) C75 0.0116(16) 0.030(2) 0.0255(19) -0.0005(16) -0.0049(14) 0.0014(14) C76 0.0107(16) 0.027(2) 0.0277(19) 0.0014(16) -0.0073(14) 0.0033(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 Cl1 C6 1.809(5) . ? Cl2 C7 1.807(5) . ? Cl3 C9 1.815(5) . ? Cl4 C23 1.821(4) . ? Cl5 C25 1.813(4) . ? Cl6 C27 1.832(4) . ? Cl7 C30 1.816(4) . ? Cl8 Cl33 1.65(2) . ? Cl8 C32 1.862(5) . ? Cl9 C33 1.782(4) . ? Cl10 C34 1.789(4) . ? Cl11 C35 1.784(4) . ? Cl12 C36 1.789(4) . ? Cl13 C37 1.789(4) . ? Cl14 C38 1.787(4) . ? Cl15 C39 1.793(4) . ? Cl16 C40 1.792(5) . ? Cl17 C41 1.789(4) . ? Cl18 C42 1.787(5) . ? Cl19 C43 1.797(5) . ? Cl20 C20A 0.71(3) . ? Cl20 C44 1.797(5) . ? C20A C44 1.748(19) . ? C20A Cl21 2.31(3) . ? Cl21 C45 1.835(5) . ? Cl22 C47 1.817(4) . ? Cl23 C50 1.816(4) . ? Cl24 C52 1.816(4) . ? Cl25 C54 1.859(5) . ? Cl25 Cl30 2.33(3) . ? Cl26 C68 1.824(4) . ? Cl27 C70 1.809(4) . ? Cl28 C71 1.809(4) . ? Cl29 Cl32 1.22(2) . ? Cl29 Cl31 1.45(2) . ? Cl29 C74 2.167(9) . ? Cl30 Cl33 1.80(3) . ? Cl31 Cl32 1.29(4) . ? C1 C10 1.387(6) . ? C1 C2 1.433(6) . ? C1 C6 1.530(6) . ? C2 C13 1.398(6) . ? C2 C3 1.442(6) . ? C3 C16 1.406(5) . ? C3 C4 1.410(6) . ? C4 C19 1.390(6) . ? C4 C5 1.408(5) . ? C5 C22 1.365(6) . ? C5 C6 1.494(6) . ? C6 C7 1.594(6) . ? C7 C8 1.484(6) . ? C7 C23 1.595(7) . ? C8 C26 1.343(7) . ? C8 C9 1.507(6) . ? C9 C28 1.513(6) . ? C9 C10 1.514(6) . ? C10 C11 1.428(6) . ? C11 C12 1.383(6) . ? C11 C30 1.504(6) . ? C12 C13 1.398(6) . ? C12 C33 1.517(6) . ? C13 C14 1.421(6) . ? C14 C15 1.355(6) . ? C14 C34 1.486(6) . ? C15 C16 1.417(6) . ? C15 C37 1.500(6) . ? C16 C17 1.410(6) . ? C17 C18 1.365(6) . ? C17 C38 1.498(5) . ? C18 C19 1.411(5) . ? C18 C41 1.491(7) . ? C19 C20 1.408(6) . ? C20 C21 1.388(5) . ? C20 C42 1.502(7) . ? C21 C22 1.416(7) . ? C21 C45 1.504(7) . ? C22 C23 1.489(5) . ? C23 C24 1.486(7) . ? C24 C46 1.355(7) . ? C24 C25 1.507(6) . ? C25 C48 1.498(7) . ? C25 C26 1.499(7) . ? C26 C27 1.494(6) . ? C27 C28 1.519(6) . ? C27 C50 1.558(7) . ? C28 C29 1.326(6) . ? C29 C52 1.512(6) . ? C29 C30 1.513(6) . ? C30 C31 1.520(6) . ? C31 C53 1.353(6) . ? C31 C32 1.518(6) . ? C32 C56 1.489(6) . ? C32 C33 1.570(6) . ? C33 C34 1.669(6) . ? C34 C35 1.543(6) . ? C35 C57 1.508(5) . ? C35 C36 1.684(7) . ? C36 C59 1.501(5) . ? C36 C37 1.570(6) . ? C37 C38 1.678(7) . ? C38 C39 1.570(6) . ? C39 C60 1.505(6) . ? C39 C40 1.684(6) . ? C40 C62 1.506(6) . ? C40 C41 1.561(6) . ? C41 C42 1.694(6) . ? C42 C43 1.556(7) . ? C43 C63 1.489(6) . ? C43 C44 1.667(6) . ? C44 C65 1.523(6) . ? C44 C45 1.570(7) . ? C45 C46 1.536(6) . ? C46 C47 1.524(6) . ? C47 C66 1.500(6) . ? C47 C48 1.501(6) . ? C48 C49 1.331(6) . ? C49 C68 1.504(6) . ? C49 C50 1.509(6) . ? C50 C51 1.504(5) . ? C51 C69 1.334(6) . ? C51 C52 1.493(6) . ? C52 C53 1.502(5) . ? C53 C54 1.470(6) . ? C54 C55 1.471(6) . ? C54 C70 1.577(6) . ? C55 C72 1.363(6) . ? C55 C56 1.427(5) . ? C56 C57 1.386(6) . ? C57 C58 1.404(6) . ? C58 C73 1.401(5) . ? C58 C59 1.420(6) . ? C59 C60 1.354(6) . ? C60 C61 1.421(5) . ? C61 C74 1.406(6) . ? C61 C62 1.409(6) . ? C62 C63 1.357(6) . ? C63 C64 1.423(6) . ? C64 C65 1.388(6) . ? C64 C75 1.401(6) . ? C65 C66 1.387(6) . ? C66 C67 1.423(6) . ? C67 C76 1.389(6) . ? C67 C68 1.516(6) . ? C68 C69 1.508(6) . ? C69 C70 1.490(6) . ? C70 C71 1.593(6) . ? C71 C72 1.498(5) . ? C71 C76 1.536(6) . ? C72 C73 1.394(6) . ? C73 C74 1.423(6) . ? C74 C75 1.445(5) . ? C75 C76 1.426(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 Cl33 Cl8 C32 129.5(6) . . ? C20A Cl20 C44 74.6(16) . . ? Cl20 C20A C44 82.5(15) . . ? Cl20 C20A Cl21 167(2) . . ? C44 C20A Cl21 86.3(11) . . ? C45 Cl21 C20A 67.4(5) . . ? C54 Cl25 Cl30 127.5(6) . . ? Cl32 Cl29 Cl31 57.0(17) . . ? Cl32 Cl29 C74 153.4(16) . . ? Cl31 Cl29 C74 136.4(12) . . ? Cl33 Cl30 Cl25 98.6(13) . . ? Cl32 Cl31 Cl29 52.6(14) . . ? Cl29 Cl32 Cl31 70(2) . . ? Cl8 Cl33 Cl30 133.8(17) . . ? C10 C1 C2 118.4(4) . . ? C10 C1 C6 124.3(4) . . ? C2 C1 C6 116.7(4) . . ? C13 C2 C1 118.2(4) . . ? C13 C2 C3 116.2(4) . . ? C1 C2 C3 122.3(4) . . ? C16 C3 C4 116.6(4) . . ? C16 C3 C2 118.8(4) . . ? C4 C3 C2 117.4(3) . . ? C19 C4 C5 117.1(4) . . ? C19 C4 C3 118.7(4) . . ? C5 C4 C3 119.5(4) . . ? C22 C5 C4 120.0(4) . . ? C22 C5 C6 114.8(4) . . ? C4 C5 C6 122.5(4) . . ? C5 C6 C1 107.7(3) . . ? C5 C6 C7 102.5(4) . . ? C1 C6 C7 116.9(3) . . ? C5 C6 Cl1 110.4(3) . . ? C1 C6 Cl1 106.4(3) . . ? C7 C6 Cl1 112.7(3) . . ? C8 C7 C6 110.1(3) . . ? C8 C7 C23 112.2(4) . . ? C6 C7 C23 106.0(3) . . ? C8 C7 Cl2 104.0(3) . . ? C6 C7 Cl2 113.3(3) . . ? C23 C7 Cl2 111.3(3) . . ? C26 C8 C7 125.1(4) . . ? C26 C8 C9 112.1(4) . . ? C7 C8 C9 122.7(4) . . ? C8 C9 C28 101.1(4) . . ? C8 C9 C10 111.1(3) . . ? C28 C9 C10 111.1(3) . . ? C8 C9 Cl3 113.5(3) . . ? C28 C9 Cl3 111.6(3) . . ? C10 C9 Cl3 108.3(3) . . ? C1 C10 C11 122.1(4) . . ? C1 C10 C9 118.4(4) . . ? C11 C10 C9 118.9(4) . . ? C12 C11 C10 119.1(4) . . ? C12 C11 C30 117.0(4) . . ? C10 C11 C30 122.1(4) . . ? C11 C12 C13 119.0(4) . . ? C11 C12 C33 127.7(4) . . ? C13 C12 C33 111.7(4) . . ? C2 C13 C12 122.9(4) . . ? C2 C13 C14 123.6(4) . . ? C12 C13 C14 110.4(4) . . ? C15 C14 C13 120.0(4) . . ? C15 C14 C34 125.9(4) . . ? C13 C14 C34 112.5(4) . . ? C14 C15 C16 118.3(4) . . ? C14 C15 C37 126.9(4) . . ? C16 C15 C37 112.6(4) . . ? C3 C16 C17 123.8(4) . . ? C3 C16 C15 122.8(4) . . ? C17 C16 C15 109.1(4) . . ? C18 C17 C16 118.8(4) . . ? C18 C17 C38 125.8(4) . . ? C16 C17 C38 113.0(4) . . ? C17 C18 C19 118.2(4) . . ? C17 C18 C41 127.2(4) . . ? C19 C18 C41 112.7(4) . . ? C4 C19 C20 122.2(4) . . ? C4 C19 C18 123.4(4) . . ? C20 C19 C18 110.2(4) . . ? C21 C20 C19 119.5(4) . . ? C21 C20 C42 127.8(4) . . ? C19 C20 C42 111.7(4) . . ? C20 C21 C22 116.7(4) . . ? C20 C21 C45 122.0(4) . . ? C22 C21 C45 120.4(4) . . ? C5 C22 C21 122.5(4) . . ? C5 C22 C23 111.6(4) . . ? C21 C22 C23 124.2(4) . . ? C24 C23 C22 107.0(4) . . ? C24 C23 C7 115.7(4) . . ? C22 C23 C7 104.1(4) . . ? C24 C23 Cl4 108.8(3) . . ? C22 C23 Cl4 108.7(3) . . ? C7 C23 Cl4 112.2(3) . . ? C46 C24 C23 123.3(4) . . ? C46 C24 C25 112.7(4) . . ? C23 C24 C25 122.6(4) . . ? C48 C25 C26 109.0(3) . . ? C48 C25 C24 100.6(4) . . ? C26 C25 C24 109.8(4) . . ? C48 C25 Cl5 114.1(3) . . ? C26 C25 Cl5 111.5(3) . . ? C24 C25 Cl5 111.3(3) . . ? C8 C26 C27 112.0(4) . . ? C8 C26 C25 124.0(4) . . ? C27 C26 C25 123.0(4) . . ? C26 C27 C28 101.0(3) . . ? C26 C27 C50 113.7(4) . . ? C28 C27 C50 113.9(3) . . ? C26 C27 Cl6 106.0(3) . . ? C28 C27 Cl6 108.4(3) . . ? C50 C27 Cl6 112.9(3) . . ? C29 C28 C9 122.9(4) . . ? C29 C28 C27 125.3(4) . . ? C9 C28 C27 109.3(3) . . ? C28 C29 C52 122.9(4) . . ? C28 C29 C30 122.7(4) . . ? C52 C29 C30 109.7(3) . . ? C11 C30 C29 111.5(3) . . ? C11 C30 C31 107.4(3) . . ? C29 C30 C31 102.2(3) . . ? C11 C30 Cl7 112.7(3) . . ? C29 C30 Cl7 110.7(3) . . ? C31 C30 Cl7 111.8(3) . . ? C53 C31 C32 123.4(4) . . ? C53 C31 C30 110.1(4) . . ? C32 C31 C30 125.0(4) . . ? C56 C32 C31 108.8(4) . . ? C56 C32 C33 113.2(4) . . ? C31 C32 C33 112.2(3) . . ? C56 C32 Cl8 105.7(3) . . ? C31 C32 Cl8 106.3(3) . . ? C33 C32 Cl8 110.0(3) . . ? C12 C33 C32 108.3(3) . . ? C12 C33 C34 102.4(3) . . ? C32 C33 C34 118.1(3) . . ? C12 C33 Cl9 107.9(3) . . ? C32 C33 Cl9 109.3(3) . . ? C34 C33 Cl9 110.2(3) . . ? C14 C34 C35 108.9(4) . . ? C14 C34 C33 102.3(3) . . ? C35 C34 C33 117.1(3) . . ? C14 C34 Cl10 106.3(3) . . ? C35 C34 Cl10 109.5(3) . . ? C33 C34 Cl10 111.8(3) . . ? C57 C35 C34 109.5(3) . . ? C57 C35 C36 102.9(3) . . ? C34 C35 C36 117.0(3) . . ? C57 C35 Cl11 105.6(3) . . ? C34 C35 Cl11 109.7(3) . . ? C36 C35 Cl11 111.4(3) . . ? C59 C36 C37 107.8(3) . . ? C59 C36 C35 101.7(3) . . ? C37 C36 C35 118.2(4) . . ? C59 C36 Cl12 107.1(3) . . ? C37 C36 Cl12 109.4(3) . . ? C35 C36 Cl12 111.7(3) . . ? C15 C37 C36 107.5(4) . . ? C15 C37 C38 102.1(3) . . ? C36 C37 C38 118.5(3) . . ? C15 C37 Cl13 106.5(3) . . ? C36 C37 Cl13 110.7(3) . . ? C38 C37 Cl13 110.5(3) . . ? C17 C38 C39 108.4(3) . . ? C17 C38 C37 102.0(3) . . ? C39 C38 C37 117.4(3) . . ? C17 C38 Cl14 107.0(3) . . ? C39 C38 Cl14 109.0(3) . . ? C37 C38 Cl14 112.2(3) . . ? C60 C39 C38 108.3(4) . . ? C60 C39 C40 102.7(3) . . ? C38 C39 C40 117.2(3) . . ? C60 C39 Cl15 106.3(3) . . ? C38 C39 Cl15 109.7(3) . . ? C40 C39 Cl15 111.8(3) . . ? C62 C40 C41 108.6(3) . . ? C62 C40 C39 101.3(3) . . ? C41 C40 C39 118.4(4) . . ? C62 C40 Cl16 106.2(3) . . ? C41 C40 Cl16 110.4(3) . . ? C39 C40 Cl16 110.9(3) . . ? C18 C41 C40 107.8(4) . . ? C18 C41 C42 101.5(3) . . ? C40 C41 C42 117.5(4) . . ? C18 C41 Cl17 107.5(3) . . ? C40 C41 Cl17 110.2(3) . . ? C42 C41 Cl17 111.6(3) . . ? C20 C42 C43 109.1(3) . . ? C20 C42 C41 102.4(4) . . ? C43 C42 C41 117.3(4) . . ? C20 C42 Cl18 105.9(3) . . ? C43 C42 Cl18 109.9(3) . . ? C41 C42 Cl18 111.5(3) . . ? C63 C43 C42 108.5(4) . . ? C63 C43 C44 102.3(3) . . ? C42 C43 C44 116.8(4) . . ? C63 C43 Cl19 106.6(3) . . ? C42 C43 Cl19 109.8(3) . . ? C44 C43 Cl19 112.1(3) . . ? C65 C44 C45 108.9(4) . . ? C65 C44 C43 102.2(3) . . ? C45 C44 C43 118.4(4) . . ? C65 C44 C20A 124.0(8) . . ? C45 C44 C20A 89.3(10) . . ? C43 C44 C20A 114.8(8) . . ? C65 C44 Cl20 106.1(3) . . ? C45 C44 Cl20 110.0(3) . . ? C43 C44 Cl20 110.3(3) . . ? C20A C44 Cl20 23.0(9) . . ? C21 C45 C46 107.2(4) . . ? C21 C45 C44 112.3(4) . . ? C46 C45 C44 111.8(4) . . ? C21 C45 Cl21 106.3(3) . . ? C46 C45 Cl21 108.3(3) . . ? C44 C45 Cl21 110.7(3) . . ? C24 C46 C47 110.1(4) . . ? C24 C46 C45 123.5(4) . . ? C47 C46 C45 124.7(4) . . ? C66 C47 C48 111.6(3) . . ? C66 C47 C46 107.6(3) . . ? C48 C47 C46 101.9(4) . . ? C66 C47 Cl22 111.9(3) . . ? C48 C47 Cl22 109.7(3) . . ? C46 C47 Cl22 113.7(3) . . ? C49 C48 C25 122.3(4) . . ? C49 C48 C47 122.8(4) . . ? C25 C48 C47 110.5(4) . . ? C48 C49 C68 122.1(4) . . ? C48 C49 C50 126.0(4) . . ? C68 C49 C50 109.7(4) . . ? C51 C50 C49 100.6(4) . . ? C51 C50 C27 113.2(4) . . ? C49 C50 C27 113.2(3) . . ? C51 C50 Cl23 107.6(3) . . ? C49 C50 Cl23 108.2(3) . . ? C27 C50 Cl23 113.1(3) . . ? C69 C51 C52 123.6(4) . . ? C69 C51 C50 112.0(4) . . ? C52 C51 C50 123.4(4) . . ? C51 C52 C53 110.3(3) . . ? C51 C52 C29 109.0(3) . . ? C53 C52 C29 100.6(3) . . ? C51 C52 Cl24 111.2(3) . . ? C53 C52 Cl24 111.8(3) . . ? C29 C52 Cl24 113.5(3) . . ? C31 C53 C54 122.7(4) . . ? C31 C53 C52 113.2(4) . . ? C54 C53 C52 122.2(4) . . ? C53 C54 C55 109.3(4) . . ? C53 C54 C70 116.9(3) . . ? C55 C54 C70 104.9(4) . . ? C53 C54 Cl25 106.5(3) . . ? C55 C54 Cl25 107.8(3) . . ? C70 C54 Cl25 111.2(3) . . ? C72 C55 C56 121.9(4) . . ? C72 C55 C54 112.5(4) . . ? C56 C55 C54 123.6(4) . . ? C57 C56 C55 116.5(4) . . ? C57 C56 C32 122.5(4) . . ? C55 C56 C32 119.8(4) . . ? C56 C57 C58 119.9(3) . . ? C56 C57 C35 127.5(4) . . ? C58 C57 C35 111.3(4) . . ? C73 C58 C57 121.8(4) . . ? C73 C58 C59 122.9(4) . . ? C57 C58 C59 110.7(3) . . ? C60 C59 C58 118.7(4) . . ? C60 C59 C36 127.1(4) . . ? C58 C59 C36 112.0(4) . . ? C59 C60 C61 119.4(4) . . ? C59 C60 C39 126.3(4) . . ? C61 C60 C39 112.1(4) . . ? C74 C61 C62 123.6(4) . . ? C74 C61 C60 122.9(4) . . ? C62 C61 C60 109.3(4) . . ? C63 C62 C61 118.5(4) . . ? C63 C62 C40 126.1(4) . . ? C61 C62 C40 113.4(4) . . ? C62 C63 C64 119.3(4) . . ? C62 C63 C43 126.4(4) . . ? C64 C63 C43 112.6(4) . . ? C65 C64 C75 122.8(4) . . ? C65 C64 C63 110.2(4) . . ? C75 C64 C63 124.2(4) . . ? C66 C65 C64 119.4(4) . . ? C66 C65 C44 127.2(4) . . ? C64 C65 C44 112.1(4) . . ? C65 C66 C67 119.0(4) . . ? C65 C66 C47 117.3(4) . . ? C67 C66 C47 122.2(4) . . ? C76 C67 C66 121.5(4) . . ? C76 C67 C68 119.3(4) . . ? C66 C67 C68 118.2(4) . . ? C49 C68 C69 101.1(4) . . ? C49 C68 C67 111.9(4) . . ? C69 C68 C67 110.9(3) . . ? C49 C68 Cl26 111.2(3) . . ? C69 C68 Cl26 112.5(3) . . ? C67 C68 Cl26 109.1(3) . . ? C51 C69 C70 125.2(4) . . ? C51 C69 C68 112.0(4) . . ? C70 C69 C68 122.6(4) . . ? C69 C70 C54 111.6(4) . . ? C69 C70 C71 111.4(4) . . ? C54 C70 C71 105.7(3) . . ? C69 C70 Cl27 104.3(3) . . ? C54 C70 Cl27 111.3(3) . . ? C71 C70 Cl27 112.7(3) . . ? C72 C71 C76 107.5(3) . . ? C72 C71 C70 102.9(3) . . ? C76 C71 C70 116.0(3) . . ? C72 C71 Cl28 109.3(3) . . ? C76 C71 Cl28 107.5(3) . . ? C70 C71 Cl28 113.4(3) . . ? C55 C72 C73 120.9(4) . . ? C55 C72 C71 113.5(4) . . ? C73 C72 C71 122.5(4) . . ? C72 C73 C58 116.9(4) . . ? C72 C73 C74 120.1(4) . . ? C58 C73 C74 118.2(4) . . ? C61 C74 C73 117.3(4) . . ? C61 C74 C75 118.3(4) . . ? C73 C74 C75 116.3(4) . . ? C61 C74 Cl29 97.3(4) . . ? C73 C74 Cl29 99.5(4) . . ? C75 C74 Cl29 101.8(4) . . ? C64 C75 C76 117.8(4) . . ? C64 C75 C74 115.9(4) . . ? C76 C75 C74 123.0(4) . . ? C67 C76 C75 119.2(4) . . ? C67 C76 C71 124.1(4) . . ? C75 C76 C71 116.3(4) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.062 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.111 # Attachment '- c76cl-V_805561.CIF' data_c76cl-va _database_code_depnum_ccdc_archive 'CCDC 805561' #TrackingRef '- c76cl-V_805561.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl28' _chemical_formula_weight 1905.36 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' 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 P2(1)/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 11.5750(10) _cell_length_b 27.495(2) _cell_length_c 22.1820(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.169(8) _cell_angle_gamma 90.00 _cell_volume 6948.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35405 _diffrn_reflns_av_R_equivalents 0.1674 _diffrn_reflns_av_sigmaI/netI 0.2175 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 35.94 _reflns_number_total 12376 _reflns_number_gt 6527 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was refined with PLATON/SQUEEZE resulting in an improvement of ESD's and R1/wR2 values: 0.178/0.421 vs. 0.216/0.496 respectively. All restraints were used for ADP (ISOR). ; _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^)+(0.1000P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12376 _refine_ls_number_parameters 937 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.2330 _refine_ls_R_factor_gt 0.1777 _refine_ls_wR_factor_ref 0.4210 _refine_ls_wR_factor_gt 0.3943 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.0514(3) 0.29587(19) 0.71815(17) 0.0499(12) Uani 1 1 d . . . Cl2 Cl 0.1718(4) 0.3929(2) 0.7275(2) 0.0618(13) Uani 1 1 d . . . Cl3 Cl -0.0390(3) 0.41929(16) 0.60474(18) 0.0429(10) Uani 1 1 d . . . Cl4 Cl 0.4113(4) 0.3540(2) 0.76441(19) 0.0598(13) Uani 1 1 d . . . Cl5 Cl 0.4525(4) 0.46140(17) 0.65217(18) 0.0499(11) Uani 1 1 d . . . Cl6 Cl 0.1759(4) 0.49803(18) 0.5522(2) 0.0598(13) Uani 1 1 d . . . Cl7 Cl -0.1975(3) 0.38500(18) 0.43143(19) 0.0497(11) Uani 1 1 d . . . Cl8 Cl -0.1581(3) 0.2854(2) 0.29624(19) 0.0651(15) Uani 1 1 d . . . Cl9 Cl -0.2737(3) 0.2686(2) 0.4047(2) 0.0559(13) Uani 1 1 d . . . Cl10 Cl -0.2391(3) 0.16314(19) 0.4279(2) 0.0644(14) Uani 1 1 d . . . Cl11 Cl -0.1197(4) 0.1509(2) 0.3174(3) 0.0692(15) Uani 1 1 d . . . Cl12 Cl 0.0321(5) 0.0684(2) 0.3735(3) 0.093(2) Uani 1 1 d . . . Cl13 Cl -0.0557(5) 0.0666(2) 0.4944(3) 0.0836(18) Uani 1 1 d . . . Cl14 Cl 0.1740(5) 0.03673(19) 0.5728(4) 0.092(2) Uani 1 1 d . . . Cl15 Cl 0.3075(6) 0.0331(2) 0.4672(4) 0.101(2) Uani 1 1 d . . . Cl16 Cl 0.5413(5) 0.0647(2) 0.5402(3) 0.093(2) Uani 1 1 d . . . Cl17 Cl 0.4529(5) 0.0746(2) 0.6614(3) 0.0791(17) Uani 1 1 d . . . Cl18 Cl 0.6092(4) 0.1582(2) 0.7105(2) 0.0623(13) Uani 1 1 d . . . Cl19 Cl 0.7296(4) 0.1648(2) 0.5994(2) 0.0685(15) Uani 1 1 d . . . Cl20 Cl 0.7680(3) 0.2716(2) 0.6160(2) 0.0592(13) Uani 1 1 d U . . Cl21 Cl 0.6526(3) 0.2931(2) 0.72191(19) 0.0609(14) Uani 1 1 d . . . Cl22 Cl 0.6902(3) 0.38761(17) 0.58167(17) 0.0463(11) Uani 1 1 d . . . Cl23 Cl 0.3184(4) 0.49541(19) 0.4544(2) 0.0600(13) Uani 1 1 d . . . Cl24 Cl 0.0405(4) 0.45430(16) 0.35585(18) 0.0470(10) Uani 1 1 d . . . Cl25 Cl 0.0808(4) 0.3439(2) 0.25116(19) 0.0642(15) Uani 1 1 d . . . Cl26 Cl 0.5326(3) 0.41286(19) 0.40737(18) 0.0496(12) Uani 1 1 d . . . Cl27 Cl 0.3225(4) 0.3816(2) 0.28612(18) 0.0644(15) Uani 1 1 d . . . Cl28 Cl 0.4421(3) 0.2852(2) 0.30171(18) 0.0603(14) Uani 1 1 d . . . C1 C 0.0619(11) 0.2969(6) 0.5993(6) 0.028(3) Uani 1 1 d U . . C2 C 0.0387(11) 0.2476(5) 0.5827(6) 0.028(3) Uani 1 1 d U . . C3 C 0.1098(12) 0.2078(5) 0.6068(8) 0.036(4) Uani 1 1 d . . . C4 C 0.2189(11) 0.2201(6) 0.6496(7) 0.034(4) Uani 1 1 d U . . C5 C 0.2363(11) 0.2672(6) 0.6667(6) 0.031(3) Uani 1 1 d . . . C6 C 0.1461(12) 0.3051(6) 0.6611(6) 0.037(4) Uani 1 1 d . . . C7 C 0.2155(11) 0.3532(7) 0.6692(7) 0.041(4) Uani 1 1 d U . . C8 C 0.1865(10) 0.3842(4) 0.6128(6) 0.019(3) Uani 1 1 d . . . C9 C 0.0669(12) 0.3830(6) 0.5728(6) 0.035(4) Uani 1 1 d . . . C10 C 0.0229(11) 0.3337(5) 0.5577(6) 0.027(3) Uani 1 1 d U . . C11 C -0.0422(11) 0.3228(6) 0.4969(6) 0.028(3) Uani 1 1 d U . . C12 C -0.0709(10) 0.2735(5) 0.4818(6) 0.026(3) Uani 1 1 d U . . C13 C -0.0348(12) 0.2382(6) 0.5241(7) 0.041(4) Uani 1 1 d . . . C14 C -0.0403(11) 0.1908(7) 0.4939(8) 0.044(4) Uani 1 1 d U . . C15 C 0.0273(14) 0.1556(6) 0.5176(10) 0.059(5) Uani 1 1 d . . . C16 C 0.1059(13) 0.1630(6) 0.5759(9) 0.050(5) Uani 1 1 d . . . C17 C 0.2045(14) 0.1321(6) 0.5814(8) 0.045(4) Uani 1 1 d U . . C18 C 0.3118(13) 0.1442(6) 0.6163(8) 0.045(4) Uani 1 1 d . . . C19 C 0.3144(12) 0.1909(6) 0.6445(8) 0.041(4) Uani 1 1 d . . . C20 C 0.4294(12) 0.2090(6) 0.6534(6) 0.031(3) Uani 1 1 d U . . C21 C 0.4458(11) 0.2576(7) 0.6630(6) 0.036(4) Uani 1 1 d . . . C22 C 0.3503(10) 0.2872(6) 0.6768(6) 0.027(3) Uani 1 1 d . . . C23 C 0.3496(12) 0.3392(7) 0.6836(6) 0.040(4) Uani 1 1 d . . . C24 C 0.4262(10) 0.3615(5) 0.6416(6) 0.024(3) Uani 1 1 d . . . C25 C 0.3920(11) 0.4076(5) 0.6080(7) 0.029(3) Uani 1 1 d . . . C26 C 0.2682(11) 0.4110(7) 0.5898(7) 0.043(4) Uani 1 1 d . . . C27 C 0.2124(11) 0.4347(6) 0.5315(7) 0.038(4) Uani 1 1 d . . . C28 C 0.0967(11) 0.4079(5) 0.5156(7) 0.031(3) Uani 1 1 d U . . C29 C 0.0449(11) 0.3966(6) 0.4588(6) 0.033(3) Uani 1 1 d . . . C30 C -0.0510(11) 0.3579(7) 0.4455(7) 0.040(4) Uani 1 1 d . . . C31 C -0.0222(11) 0.3316(6) 0.3887(6) 0.035(4) Uani 1 1 d . . . C32 C -0.0550(11) 0.2808(6) 0.3730(7) 0.039(4) Uani 1 1 d U . . C33 C -0.1213(11) 0.2536(6) 0.4207(5) 0.031(3) Uani 1 1 d U . . C34 C -0.1037(12) 0.1949(8) 0.4286(7) 0.056(6) Uani 1 1 d . . . C35 C -0.0270(14) 0.1676(6) 0.3912(10) 0.060(6) Uani 1 1 d . . . C36 C 0.0550(18) 0.1233(6) 0.4215(11) 0.064(6) Uani 1 1 d U . . C37 C 0.0595(16) 0.1115(6) 0.4876(8) 0.053(5) Uani 1 1 d . . . C38 C 0.1876(19) 0.0914(9) 0.5327(11) 0.076(6) Uani 1 1 d . . . C39 C 0.2964(14) 0.0926(7) 0.5007(11) 0.065(6) Uani 1 1 d . . . C40 C 0.4302(15) 0.1098(8) 0.5427(11) 0.070(6) Uani 1 1 d . . . C41 C 0.4289(14) 0.1267(6) 0.6111(9) 0.052(5) Uani 1 1 d . . . C42 C 0.5152(14) 0.1741(7) 0.6401(7) 0.051(5) Uani 1 1 d . . . C43 C 0.5921(14) 0.1974(6) 0.5956(8) 0.047(4) Uani 1 1 d . . . C44 C 0.6140(12) 0.2558(7) 0.6004(8) 0.047(4) Uani 1 1 d U . . C45 C 0.5513(13) 0.2882(7) 0.6481(7) 0.043(4) Uani 1 1 d U . . C46 C 0.5128(10) 0.3358(5) 0.6240(6) 0.026(3) Uani 1 1 d U . . C47 C 0.5426(11) 0.3586(6) 0.5682(6) 0.034(3) Uani 1 1 d U . . C48 C 0.4515(11) 0.3978(5) 0.5538(6) 0.028(3) Uani 1 1 d U . . C49 C 0.3996(10) 0.4072(5) 0.4980(7) 0.035(4) Uani 1 1 d . . . C50 C 0.2825(14) 0.4341(7) 0.4814(8) 0.046(4) Uani 1 1 d U . . C51 C 0.2303(13) 0.4076(5) 0.4264(8) 0.041(4) Uani 1 1 d . . . C52 C 0.0983(10) 0.4032(6) 0.4022(5) 0.032(4) Uani 1 1 d . . . C53 C 0.0670(11) 0.3528(6) 0.3712(6) 0.032(4) Uani 1 1 d . . . C54 C 0.1421(11) 0.3319(6) 0.3331(6) 0.035(4) Uani 1 1 d . . . C55 C 0.1429(11) 0.2783(6) 0.3435(6) 0.034(4) Uani 1 1 d . . . C56 C 0.0457(13) 0.2542(7) 0.3599(8) 0.044(4) Uani 1 1 d . . . C57 C 0.0584(13) 0.2076(9) 0.3684(7) 0.057(6) Uani 1 1 d . . . C58 C 0.1732(13) 0.1847(7) 0.3780(6) 0.044(4) Uani 1 1 d . . . C59 C 0.1793(13) 0.1420(8) 0.4163(9) 0.057(5) Uani 1 1 d . . . C60 C 0.2826(16) 0.1295(7) 0.4495(10) 0.059(5) Uani 1 1 d . . . C61 C 0.3789(13) 0.1595(7) 0.4499(7) 0.043(4) Uani 1 1 d U . . C62 C 0.4548(15) 0.1524(7) 0.5090(8) 0.047(4) Uani 1 1 d . . . C63 C 0.5274(14) 0.1913(6) 0.5292(7) 0.041(4) Uani 1 1 d U . . C64 C 0.5224(12) 0.2355(6) 0.4978(7) 0.038(4) Uani 1 1 d U . . C65 C 0.5631(12) 0.2747(6) 0.5357(7) 0.041(4) Uani 1 1 d U . . C66 C 0.5327(10) 0.3225(5) 0.5183(6) 0.023(3) Uani 1 1 d U . . C67 C 0.4696(12) 0.3290(6) 0.4595(7) 0.034(3) Uani 1 1 d U . . C68 C 0.4265(11) 0.3792(5) 0.4449(6) 0.029(3) Uani 1 1 d U . . C69 C 0.3056(12) 0.3765(7) 0.4010(6) 0.043(4) Uani 1 1 d . . . C70 C 0.2826(11) 0.3486(7) 0.3475(7) 0.041(4) Uani 1 1 d U . . C71 C 0.3484(12) 0.2985(7) 0.3589(7) 0.045(4) Uani 1 1 d . . . C72 C 0.2552(11) 0.2600(6) 0.3545(6) 0.031(3) Uani 1 1 d U . . C73 C 0.2738(11) 0.2132(6) 0.3769(7) 0.038(4) Uani 1 1 d U . . C74 C 0.3780(13) 0.2002(6) 0.4161(7) 0.039(4) Uani 1 1 d . . . C75 C 0.4487(14) 0.2421(7) 0.4384(7) 0.043(4) Uani 1 1 d U . . C76 C 0.4277(11) 0.2900(6) 0.4194(7) 0.033(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0142(16) 0.102(4) 0.037(2) 0.010(2) 0.0139(14) -0.0037(19) Cl2 0.046(3) 0.091(4) 0.052(3) -0.008(2) 0.019(2) -0.008(3) Cl3 0.0196(17) 0.053(3) 0.060(2) -0.0085(19) 0.0174(16) 0.0055(17) Cl4 0.035(2) 0.102(4) 0.042(2) -0.003(2) 0.0058(17) -0.013(2) Cl5 0.042(2) 0.061(3) 0.045(2) -0.0107(19) 0.0042(17) -0.014(2) Cl6 0.044(2) 0.049(3) 0.087(3) -0.013(2) 0.014(2) 0.003(2) Cl7 0.0120(16) 0.085(3) 0.055(2) -0.007(2) 0.0128(16) 0.0088(19) Cl8 0.0208(19) 0.128(5) 0.043(2) -0.015(2) -0.0022(17) 0.005(2) Cl9 0.0069(16) 0.096(4) 0.063(3) -0.008(2) 0.0031(16) -0.0049(19) Cl10 0.0169(18) 0.074(4) 0.098(4) -0.017(3) -0.002(2) -0.019(2) Cl11 0.033(2) 0.074(4) 0.095(4) -0.037(3) -0.003(2) -0.011(2) Cl12 0.057(3) 0.059(4) 0.153(6) -0.049(4) -0.004(3) -0.003(3) Cl13 0.050(3) 0.054(3) 0.141(5) -0.008(3) -0.001(3) -0.024(3) Cl14 0.062(3) 0.033(3) 0.174(6) 0.003(3) 0.001(4) -0.006(3) Cl15 0.073(4) 0.046(3) 0.177(7) -0.031(4) 0.000(4) 0.023(3) Cl16 0.056(3) 0.081(4) 0.137(5) -0.013(4) 0.003(3) 0.040(3) Cl17 0.061(3) 0.055(3) 0.119(5) 0.012(3) 0.007(3) 0.019(3) Cl18 0.028(2) 0.090(4) 0.064(3) 0.014(2) -0.0031(19) 0.012(2) Cl19 0.024(2) 0.103(4) 0.079(3) 0.003(3) 0.009(2) 0.030(2) Cl20 0.0011(15) 0.103(4) 0.072(3) -0.002(2) 0.0015(16) 0.0046(19) Cl21 0.0163(18) 0.119(4) 0.045(2) 0.007(2) -0.0002(16) -0.001(2) Cl22 0.0122(16) 0.082(3) 0.044(2) -0.0012(19) 0.0026(14) -0.0177(18) Cl23 0.042(2) 0.061(3) 0.077(3) 0.007(2) 0.010(2) -0.011(2) Cl24 0.039(2) 0.051(3) 0.050(2) 0.0063(19) 0.0066(17) 0.009(2) Cl25 0.033(2) 0.118(5) 0.040(2) -0.009(2) 0.0034(17) 0.011(3) Cl26 0.0154(17) 0.092(4) 0.045(2) 0.005(2) 0.0148(15) -0.0035(19) Cl27 0.042(2) 0.124(5) 0.031(2) 0.003(2) 0.0183(17) 0.009(3) Cl28 0.0164(17) 0.130(5) 0.037(2) -0.014(2) 0.0106(15) 0.005(2) C1 0.021(6) 0.045(7) 0.021(5) 0.001(5) 0.013(5) -0.001(5) C2 0.012(5) 0.031(7) 0.044(6) 0.008(5) 0.011(5) -0.004(5) C3 0.018(7) 0.025(9) 0.071(10) -0.002(7) 0.019(7) -0.013(6) C4 0.008(6) 0.041(9) 0.055(8) 0.011(7) 0.013(6) -0.006(6) C5 0.006(6) 0.047(10) 0.039(8) 0.008(7) 0.001(5) -0.011(6) C6 0.015(7) 0.064(12) 0.034(8) -0.005(7) 0.016(6) -0.002(7) C7 0.008(6) 0.079(11) 0.038(7) -0.003(7) 0.010(5) -0.004(7) C8 0.015(6) 0.006(6) 0.034(7) -0.003(5) 0.000(5) -0.003(5) C9 0.016(7) 0.059(11) 0.033(7) 0.014(7) 0.011(6) 0.008(7) C10 0.014(5) 0.035(6) 0.037(5) 0.002(5) 0.017(4) 0.003(5) C11 0.011(5) 0.042(6) 0.034(5) -0.003(5) 0.012(4) 0.005(5) C12 0.006(4) 0.037(6) 0.035(5) 0.006(5) 0.007(4) 0.006(4) C13 0.016(7) 0.056(12) 0.056(10) -0.003(8) 0.018(7) -0.016(7) C14 0.003(6) 0.059(11) 0.067(9) -0.002(8) 0.003(6) -0.009(7) C15 0.022(8) 0.030(11) 0.119(16) 0.007(10) -0.003(9) -0.025(8) C16 0.019(7) 0.026(10) 0.104(14) 0.021(9) 0.010(8) 0.008(7) C17 0.034(8) 0.030(9) 0.066(10) 0.000(7) -0.006(7) -0.020(7) C18 0.025(8) 0.046(11) 0.063(10) 0.011(8) 0.006(7) -0.008(7) C19 0.019(7) 0.041(11) 0.066(10) 0.016(8) 0.018(7) 0.007(7) C20 0.020(7) 0.032(8) 0.034(7) 0.014(6) -0.012(5) -0.003(6) C21 0.007(6) 0.077(13) 0.022(7) 0.018(7) -0.004(5) 0.003(7) C22 0.002(6) 0.056(11) 0.024(6) 0.015(6) 0.004(5) -0.003(6) C23 0.018(7) 0.073(13) 0.025(7) 0.004(7) -0.005(6) -0.005(8) C24 0.005(5) 0.027(8) 0.038(7) -0.007(6) -0.005(5) -0.004(5) C25 0.021(7) 0.020(8) 0.050(8) 0.004(6) 0.019(6) -0.009(6) C26 0.010(6) 0.075(13) 0.045(9) -0.029(8) 0.006(6) -0.002(7) C27 0.002(6) 0.057(11) 0.055(9) -0.010(8) 0.003(6) -0.002(6) C28 0.017(6) 0.028(8) 0.049(8) -0.007(6) 0.007(6) 0.016(6) C29 0.015(7) 0.043(10) 0.040(8) 0.013(7) -0.001(6) 0.013(6) C30 0.010(6) 0.072(12) 0.040(8) 0.005(7) 0.011(6) -0.001(7) C31 0.010(6) 0.068(12) 0.027(7) 0.006(7) 0.006(5) 0.007(7) C32 0.010(6) 0.047(10) 0.054(8) -0.006(7) -0.005(6) 0.001(6) C33 0.013(6) 0.064(10) 0.016(6) 0.002(6) -0.001(5) 0.006(6) C34 0.014(7) 0.113(17) 0.040(9) -0.037(9) -0.002(6) -0.004(9) C35 0.019(8) 0.032(10) 0.118(16) -0.017(10) -0.017(9) -0.004(7) C36 0.056(11) 0.023(10) 0.113(15) -0.021(9) 0.013(10) -0.009(9) C37 0.052(11) 0.035(11) 0.063(11) 0.000(8) -0.013(9) -0.018(9) C38 0.056(13) 0.075(16) 0.091(16) -0.009(12) 0.000(11) -0.005(12) C39 0.016(8) 0.035(11) 0.135(18) 0.001(11) -0.013(9) 0.003(7) C40 0.022(9) 0.054(13) 0.123(18) -0.015(12) -0.019(10) 0.006(9) C41 0.029(9) 0.030(10) 0.092(14) 0.011(9) -0.002(9) -0.008(7) C42 0.035(9) 0.078(14) 0.045(9) 0.012(8) 0.015(7) 0.026(9) C43 0.035(9) 0.036(10) 0.081(12) -0.006(8) 0.037(9) 0.018(8) C44 0.011(6) 0.074(11) 0.059(9) 0.018(8) 0.016(6) 0.025(7) C45 0.025(6) 0.060(8) 0.050(7) -0.004(6) 0.027(6) -0.003(6) C46 0.008(6) 0.046(9) 0.024(6) -0.003(6) 0.000(5) 0.000(6) C47 0.013(6) 0.064(10) 0.025(6) 0.010(6) 0.003(5) -0.005(6) C48 0.019(6) 0.029(7) 0.040(6) -0.003(5) 0.016(5) -0.013(5) C49 0.003(6) 0.033(9) 0.068(10) 0.000(7) 0.003(6) 0.006(6) C50 0.031(7) 0.051(8) 0.055(7) 0.004(6) 0.005(6) 0.001(6) C51 0.027(8) 0.021(9) 0.081(12) 0.012(8) 0.024(8) 0.004(7) C52 0.008(6) 0.071(11) 0.015(6) -0.004(6) -0.001(5) 0.002(7) C53 0.012(6) 0.065(11) 0.021(6) -0.009(6) 0.005(5) 0.005(7) C54 0.006(6) 0.063(12) 0.037(8) -0.016(7) 0.004(5) 0.000(7) C55 0.012(6) 0.058(12) 0.030(7) -0.020(7) 0.003(5) 0.005(7) C56 0.019(8) 0.051(12) 0.061(11) -0.012(9) 0.009(7) 0.013(8) C57 0.021(8) 0.13(2) 0.025(8) -0.029(9) 0.016(6) -0.015(10) C58 0.030(8) 0.082(14) 0.017(7) -0.013(7) -0.002(6) 0.011(8) C59 0.015(8) 0.075(14) 0.081(13) -0.020(11) 0.013(8) -0.013(8) C60 0.039(10) 0.049(12) 0.090(14) -0.014(10) 0.018(10) 0.009(9) C61 0.025(7) 0.058(11) 0.052(9) -0.001(8) 0.023(7) 0.014(7) C62 0.047(10) 0.052(12) 0.053(10) -0.013(8) 0.034(8) 0.003(9) C63 0.040(8) 0.036(9) 0.049(8) -0.003(7) 0.017(7) 0.027(7) C64 0.014(6) 0.043(8) 0.057(7) 0.004(6) 0.008(5) -0.001(6) C65 0.017(6) 0.057(8) 0.053(7) 0.001(6) 0.017(5) -0.005(6) C66 0.014(5) 0.032(6) 0.027(5) -0.007(4) 0.014(4) -0.003(4) C67 0.017(6) 0.045(8) 0.044(7) -0.008(6) 0.015(5) 0.004(6) C68 0.013(5) 0.040(7) 0.037(6) 0.001(5) 0.017(5) -0.006(5) C69 0.022(7) 0.083(13) 0.027(7) 0.018(7) 0.014(6) -0.007(8) C70 0.010(6) 0.069(11) 0.039(8) -0.013(7) -0.012(5) 0.010(7) C71 0.009(6) 0.076(13) 0.054(10) -0.017(8) 0.018(6) -0.003(7) C72 0.016(6) 0.038(7) 0.042(6) -0.016(5) 0.014(5) 0.003(5) C73 0.007(6) 0.065(11) 0.044(8) -0.024(7) 0.003(5) 0.007(6) C74 0.027(8) 0.043(11) 0.050(9) -0.018(8) 0.017(7) 0.000(7) C75 0.037(7) 0.058(8) 0.044(7) -0.014(6) 0.031(6) 0.007(6) C76 0.015(6) 0.042(7) 0.045(7) -0.008(6) 0.013(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C6 1.831(13) . ? Cl2 C7 1.831(16) . ? Cl3 C9 1.820(15) . ? Cl4 C23 1.854(14) . ? Cl5 C25 1.844(15) . ? Cl6 C27 1.869(17) . ? Cl7 C30 1.828(14) . ? Cl8 C32 1.904(15) . ? Cl9 C33 1.785(13) . ? Cl10 C34 1.791(17) . ? Cl11 C35 1.850(19) . ? Cl12 C36 1.840(18) . ? Cl13 C37 1.843(18) . ? Cl14 C38 1.77(3) . ? Cl15 C39 1.81(2) . ? Cl16 C40 1.79(2) . ? Cl17 C41 1.807(18) . ? Cl18 C42 1.792(17) . ? Cl19 C43 1.815(15) . ? Cl20 C44 1.808(16) . ? Cl21 C45 1.843(17) . ? Cl22 C47 1.861(14) . ? Cl23 C50 1.861(18) . ? Cl24 C52 1.798(15) . ? Cl25 C54 1.861(15) . ? Cl26 C68 1.848(13) . ? Cl27 C70 1.764(18) . ? Cl28 C71 1.844(14) . ? C1 C10 1.39(2) . ? C1 C2 1.42(2) . ? C1 C6 1.552(19) . ? C2 C3 1.42(2) . ? C2 C13 1.44(2) . ? C3 C16 1.41(2) . ? C3 C4 1.48(2) . ? C4 C5 1.35(2) . ? C4 C19 1.39(2) . ? C5 C22 1.411(17) . ? C5 C6 1.46(2) . ? C6 C7 1.54(2) . ? C7 C8 1.50(2) . ? C7 C23 1.576(19) . ? C8 C26 1.37(2) . ? C8 C9 1.507(18) . ? C9 C10 1.47(2) . ? C9 C28 1.53(2) . ? C10 C11 1.455(19) . ? C11 C12 1.42(2) . ? C11 C30 1.48(2) . ? C12 C13 1.36(2) . ? C12 C33 1.482(19) . ? C13 C14 1.46(2) . ? C14 C15 1.30(2) . ? C14 C34 1.51(2) . ? C15 C16 1.46(3) . ? C15 C37 1.46(3) . ? C16 C17 1.41(2) . ? C17 C18 1.38(2) . ? C17 C38 1.54(3) . ? C18 C19 1.43(2) . ? C18 C41 1.46(2) . ? C19 C20 1.40(2) . ? C20 C21 1.36(2) . ? C20 C42 1.45(2) . ? C21 C22 1.45(2) . ? C21 C45 1.57(2) . ? C22 C23 1.44(2) . ? C23 C24 1.52(2) . ? C24 C46 1.341(18) . ? C24 C25 1.49(2) . ? C25 C26 1.421(19) . ? C25 C48 1.510(18) . ? C26 C27 1.49(2) . ? C27 C50 1.49(2) . ? C27 C28 1.515(19) . ? C28 C29 1.33(2) . ? C29 C52 1.505(19) . ? C29 C30 1.53(2) . ? C30 C31 1.54(2) . ? C31 C53 1.30(2) . ? C31 C32 1.47(2) . ? C32 C56 1.45(2) . ? C32 C33 1.60(2) . ? C33 C34 1.63(3) . ? C34 C35 1.52(3) . ? C35 C36 1.62(3) . ? C35 C57 1.62(3) . ? C36 C37 1.49(3) . ? C36 C59 1.55(2) . ? C37 C38 1.73(3) . ? C38 C39 1.55(3) . ? C39 C60 1.51(3) . ? C39 C40 1.73(2) . ? C40 C62 1.45(3) . ? C40 C41 1.59(3) . ? C41 C42 1.70(3) . ? C42 C43 1.58(2) . ? C43 C63 1.54(2) . ? C43 C44 1.63(3) . ? C44 C65 1.54(2) . ? C44 C45 1.65(2) . ? C45 C46 1.45(2) . ? C46 C47 1.481(18) . ? C47 C66 1.48(2) . ? C47 C48 1.50(2) . ? C48 C49 1.30(2) . ? C49 C68 1.49(2) . ? C49 C50 1.53(2) . ? C50 C51 1.46(2) . ? C51 C69 1.41(2) . ? C51 C52 1.533(19) . ? C52 C53 1.56(2) . ? C53 C54 1.435(18) . ? C54 C55 1.49(2) . ? C54 C70 1.666(18) . ? C55 C72 1.375(19) . ? C55 C56 1.41(2) . ? C56 C57 1.30(3) . ? C57 C58 1.45(2) . ? C58 C73 1.41(2) . ? C58 C59 1.44(3) . ? C59 C60 1.33(3) . ? C60 C61 1.38(3) . ? C61 C74 1.35(2) . ? C61 C62 1.46(2) . ? C62 C63 1.39(2) . ? C63 C64 1.40(2) . ? C64 C65 1.40(2) . ? C64 C75 1.45(2) . ? C65 C66 1.40(2) . ? C66 C67 1.390(19) . ? C67 C76 1.42(2) . ? C67 C68 1.48(2) . ? C68 C69 1.558(19) . ? C69 C70 1.40(2) . ? C70 C71 1.57(2) . ? C71 C72 1.50(2) . ? C71 C76 1.51(2) . ? C72 C73 1.38(2) . ? C73 C74 1.40(2) . ? C74 C75 1.45(2) . ? C75 C76 1.39(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 C10 C1 C2 119.8(12) . . ? C10 C1 C6 124.2(14) . . ? C2 C1 C6 115.4(12) . . ? C3 C2 C1 124.7(13) . . ? C3 C2 C13 114.2(14) . . ? C1 C2 C13 117.4(13) . . ? C16 C3 C2 121.8(15) . . ? C16 C3 C4 117.6(14) . . ? C2 C3 C4 116.1(13) . . ? C5 C4 C19 119.6(13) . . ? C5 C4 C3 117.8(13) . . ? C19 C4 C3 114.7(15) . . ? C4 C5 C22 120.5(13) . . ? C4 C5 C6 126.0(12) . . ? C22 C5 C6 111.6(13) . . ? C5 C6 C7 104.6(11) . . ? C5 C6 C1 107.3(12) . . ? C7 C6 C1 117.4(13) . . ? C5 C6 Cl1 110.4(11) . . ? C7 C6 Cl1 113.7(10) . . ? C1 C6 Cl1 103.3(9) . . ? C8 C7 C6 110.8(11) . . ? C8 C7 C23 111.9(11) . . ? C6 C7 C23 106.8(14) . . ? C8 C7 Cl2 101.6(11) . . ? C6 C7 Cl2 113.0(9) . . ? C23 C7 Cl2 112.8(10) . . ? C26 C8 C7 123.3(12) . . ? C26 C8 C9 114.6(12) . . ? C7 C8 C9 121.6(11) . . ? C10 C9 C8 113.7(12) . . ? C10 C9 C28 110.1(12) . . ? C8 C9 C28 99.2(10) . . ? C10 C9 Cl3 111.4(9) . . ? C8 C9 Cl3 111.7(10) . . ? C28 C9 Cl3 110.0(10) . . ? C1 C10 C11 121.4(13) . . ? C1 C10 C9 117.5(13) . . ? C11 C10 C9 120.2(12) . . ? C12 C11 C10 118.3(12) . . ? C12 C11 C30 117.3(12) . . ? C10 C11 C30 122.2(13) . . ? C13 C12 C11 119.1(13) . . ? C13 C12 C33 113.0(14) . . ? C11 C12 C33 127.1(12) . . ? C12 C13 C2 123.4(15) . . ? C12 C13 C14 109.6(14) . . ? C2 C13 C14 123.0(15) . . ? C15 C14 C13 120.3(16) . . ? C15 C14 C34 127.2(18) . . ? C13 C14 C34 110.3(15) . . ? C14 C15 C16 119.6(17) . . ? C14 C15 C37 128.1(19) . . ? C16 C15 C37 110.5(15) . . ? C3 C16 C17 122.0(15) . . ? C3 C16 C15 121.1(14) . . ? C17 C16 C15 111.2(17) . . ? C18 C17 C16 122.5(16) . . ? C18 C17 C38 123.7(17) . . ? C16 C17 C38 112.1(15) . . ? C17 C18 C19 114.1(15) . . ? C17 C18 C41 129.2(17) . . ? C19 C18 C41 112.4(14) . . ? C4 C19 C20 122.2(15) . . ? C4 C19 C18 126.9(15) . . ? C20 C19 C18 109.2(13) . . ? C21 C20 C19 118.3(14) . . ? C21 C20 C42 127.0(14) . . ? C19 C20 C42 113.8(15) . . ? C20 C21 C22 119.7(13) . . ? C20 C21 C45 125.9(14) . . ? C22 C21 C45 113.3(14) . . ? C5 C22 C23 112.5(12) . . ? C5 C22 C21 118.3(14) . . ? C23 C22 C21 126.9(12) . . ? C22 C23 C24 108.7(12) . . ? C22 C23 C7 104.2(12) . . ? C24 C23 C7 115.9(12) . . ? C22 C23 Cl4 108.1(10) . . ? C24 C23 Cl4 109.6(10) . . ? C7 C23 Cl4 109.9(10) . . ? C46 C24 C25 116.7(12) . . ? C46 C24 C23 120.8(13) . . ? C25 C24 C23 121.2(12) . . ? C26 C25 C24 111.3(12) . . ? C26 C25 C48 111.3(12) . . ? C24 C25 C48 97.4(11) . . ? C26 C25 Cl5 111.6(11) . . ? C24 C25 Cl5 112.0(10) . . ? C48 C25 Cl5 112.4(9) . . ? C8 C26 C25 126.0(16) . . ? C8 C26 C27 109.7(11) . . ? C25 C26 C27 122.5(13) . . ? C50 C27 C26 115.7(12) . . ? C50 C27 C28 113.4(13) . . ? C26 C27 C28 102.7(13) . . ? C50 C27 Cl6 111.7(12) . . ? C26 C27 Cl6 106.1(11) . . ? C28 C27 Cl6 106.3(9) . . ? C29 C28 C27 124.4(14) . . ? C29 C28 C9 123.3(14) . . ? C27 C28 C9 110.0(12) . . ? C28 C29 C52 125.3(13) . . ? C28 C29 C30 122.3(13) . . ? C52 C29 C30 108.5(12) . . ? C11 C30 C29 110.9(12) . . ? C11 C30 C31 109.1(14) . . ? C29 C30 C31 103.3(11) . . ? C11 C30 Cl7 109.4(9) . . ? C29 C30 Cl7 111.7(12) . . ? C31 C30 Cl7 112.3(10) . . ? C53 C31 C32 122.6(14) . . ? C53 C31 C30 109.3(14) . . ? C32 C31 C30 123.8(13) . . ? C56 C32 C31 110.2(13) . . ? C56 C32 C33 113.2(14) . . ? C31 C32 C33 114.9(13) . . ? C56 C32 Cl8 104.7(11) . . ? C31 C32 Cl8 104.1(10) . . ? C33 C32 Cl8 108.9(9) . . ? C12 C33 C32 106.0(12) . . ? C12 C33 C34 104.1(11) . . ? C32 C33 C34 117.9(11) . . ? C12 C33 Cl9 108.2(9) . . ? C32 C33 Cl9 109.5(9) . . ? C34 C33 Cl9 110.5(10) . . ? C14 C34 C35 104.8(14) . . ? C14 C34 C33 102.0(12) . . ? C35 C34 C33 120.3(15) . . ? C14 C34 Cl10 104.4(12) . . ? C35 C34 Cl10 110.4(12) . . ? C33 C34 Cl10 112.9(10) . . ? C34 C35 C36 120.2(19) . . ? C34 C35 C57 106.4(15) . . ? C36 C35 C57 107.2(14) . . ? C34 C35 Cl11 107.6(10) . . ? C36 C35 Cl11 112.8(12) . . ? C57 C35 Cl11 100.6(13) . . ? C37 C36 C59 105.8(16) . . ? C37 C36 C35 119.2(17) . . ? C59 C36 C35 101.7(15) . . ? C37 C36 Cl12 111.5(13) . . ? C59 C36 Cl12 105.7(13) . . ? C35 C36 Cl12 111.3(14) . . ? C15 C37 C36 107.5(15) . . ? C15 C37 C38 105.3(14) . . ? C36 C37 C38 121.1(17) . . ? C15 C37 Cl13 105.7(13) . . ? C36 C37 Cl13 109.0(12) . . ? C38 C37 Cl13 107.3(12) . . ? C17 C38 C39 106.9(17) . . ? C17 C38 C37 99.3(15) . . ? C39 C38 C37 114.2(17) . . ? C17 C38 Cl14 106.0(15) . . ? C39 C38 Cl14 113.7(16) . . ? C37 C38 Cl14 114.9(14) . . ? C60 C39 C38 111.9(15) . . ? C60 C39 C40 100.9(15) . . ? C38 C39 C40 118.8(18) . . ? C60 C39 Cl15 107.7(16) . . ? C38 C39 Cl15 106.8(14) . . ? C40 C39 Cl15 110.3(11) . . ? C62 C40 C41 107.0(15) . . ? C62 C40 C39 100.4(16) . . ? C41 C40 C39 115.9(16) . . ? C62 C40 Cl16 109.6(15) . . ? C41 C40 Cl16 111.1(13) . . ? C39 C40 Cl16 112.0(13) . . ? C18 C41 C40 109.7(14) . . ? C18 C41 C42 102.1(14) . . ? C40 C41 C42 118.9(14) . . ? C18 C41 Cl17 104.7(12) . . ? C40 C41 Cl17 109.3(13) . . ? C42 C41 Cl17 111.0(11) . . ? C20 C42 C43 109.9(14) . . ? C20 C42 C41 102.0(13) . . ? C43 C42 C41 115.6(14) . . ? C20 C42 Cl18 108.5(11) . . ? C43 C42 Cl18 108.7(12) . . ? C41 C42 Cl18 111.7(12) . . ? C63 C43 C42 108.8(14) . . ? C63 C43 C44 102.3(13) . . ? C42 C43 C44 117.3(13) . . ? C63 C43 Cl19 105.4(10) . . ? C42 C43 Cl19 111.0(12) . . ? C44 C43 Cl19 111.1(10) . . ? C65 C44 C43 104.1(14) . . ? C65 C44 C45 106.0(12) . . ? C43 C44 C45 119.6(12) . . ? C65 C44 Cl20 107.4(10) . . ? C43 C44 Cl20 112.8(10) . . ? C45 C44 Cl20 106.1(12) . . ? C46 C45 C21 111.2(12) . . ? C46 C45 C44 113.1(12) . . ? C21 C45 C44 107.1(13) . . ? C46 C45 Cl21 111.5(11) . . ? C21 C45 Cl21 104.4(10) . . ? C44 C45 Cl21 109.1(10) . . ? C24 C46 C45 124.4(12) . . ? C24 C46 C47 108.4(13) . . ? C45 C46 C47 126.0(12) . . ? C66 C47 C46 110.0(13) . . ? C66 C47 C48 111.4(11) . . ? C46 C47 C48 102.9(11) . . ? C66 C47 Cl22 110.8(9) . . ? C46 C47 Cl22 113.0(9) . . ? C48 C47 Cl22 108.5(10) . . ? C49 C48 C47 122.2(13) . . ? C49 C48 C25 121.5(13) . . ? C47 C48 C25 111.1(12) . . ? C48 C49 C68 121.7(13) . . ? C48 C49 C50 124.3(14) . . ? C68 C49 C50 111.1(13) . . ? C51 C50 C27 115.6(14) . . ? C51 C50 C49 100.3(13) . . ? C27 C50 C49 113.7(14) . . ? C51 C50 Cl23 105.4(11) . . ? C27 C50 Cl23 114.4(13) . . ? C49 C50 Cl23 106.0(11) . . ? C69 C51 C50 116.4(14) . . ? C69 C51 C52 117.6(15) . . ? C50 C51 C52 124.9(13) . . ? C29 C52 C51 104.4(11) . . ? C29 C52 C53 99.3(12) . . ? C51 C52 C53 111.3(12) . . ? C29 C52 Cl24 114.0(10) . . ? C51 C52 Cl24 112.7(11) . . ? C53 C52 Cl24 114.1(9) . . ? C31 C53 C54 126.1(15) . . ? C31 C53 C52 113.7(12) . . ? C54 C53 C52 119.9(12) . . ? C53 C54 C55 107.1(13) . . ? C53 C54 C70 116.7(12) . . ? C55 C54 C70 105.3(11) . . ? C53 C54 Cl25 109.7(10) . . ? C55 C54 Cl25 108.5(9) . . ? C70 C54 Cl25 109.2(10) . . ? C72 C55 C56 123.7(16) . . ? C72 C55 C54 111.6(13) . . ? C56 C55 C54 121.4(13) . . ? C57 C56 C55 115.2(14) . . ? C57 C56 C32 123.0(16) . . ? C55 C56 C32 121.4(17) . . ? C56 C57 C58 121.8(16) . . ? C56 C57 C35 131.0(15) . . ? C58 C57 C35 104.6(18) . . ? C73 C58 C59 120.5(14) . . ? C73 C58 C57 119.7(17) . . ? C59 C58 C57 112.8(15) . . ? C60 C59 C58 118.8(16) . . ? C60 C59 C36 129(2) . . ? C58 C59 C36 111.4(16) . . ? C59 C60 C61 119.4(19) . . ? C59 C60 C39 123.7(18) . . ? C61 C60 C39 114.6(17) . . ? C74 C61 C60 124.3(16) . . ? C74 C61 C62 123.9(16) . . ? C60 C61 C62 106.4(16) . . ? C63 C62 C40 128.4(17) . . ? C63 C62 C61 115.0(16) . . ? C40 C62 C61 115.6(16) . . ? C62 C63 C64 122.8(16) . . ? C62 C63 C43 123.9(15) . . ? C64 C63 C43 110.7(15) . . ? C65 C64 C63 113.1(15) . . ? C65 C64 C75 122.2(15) . . ? C63 C64 C75 121.9(15) . . ? C66 C65 C64 121.2(14) . . ? C66 C65 C44 127.7(15) . . ? C64 C65 C44 109.4(15) . . ? C67 C66 C65 116.5(13) . . ? C67 C66 C47 125.1(13) . . ? C65 C66 C47 116.3(12) . . ? C66 C67 C76 123.6(14) . . ? C66 C67 C68 115.3(13) . . ? C76 C67 C68 120.0(13) . . ? C67 C68 C49 114.6(12) . . ? C67 C68 C69 108.9(13) . . ? C49 C68 C69 103.2(11) . . ? C67 C68 Cl26 109.9(9) . . ? C49 C68 Cl26 110.3(10) . . ? C69 C68 Cl26 109.7(9) . . ? C70 C69 C51 129.3(14) . . ? C70 C69 C68 124.8(13) . . ? C51 C69 C68 105.9(14) . . ? C69 C70 C71 109.3(13) . . ? C69 C70 C54 110.3(12) . . ? C71 C70 C54 102.5(13) . . ? C69 C70 Cl27 109.7(13) . . ? C71 C70 Cl27 112.8(10) . . ? C54 C70 Cl27 112.0(9) . . ? C72 C71 C76 105.4(14) . . ? C72 C71 C70 106.6(11) . . ? C76 C71 C70 118.7(13) . . ? C72 C71 Cl28 108.6(11) . . ? C76 C71 Cl28 104.0(9) . . ? C70 C71 Cl28 113.0(12) . . ? C55 C72 C73 119.1(14) . . ? C55 C72 C71 113.5(14) . . ? C73 C72 C71 124.7(13) . . ? C72 C73 C74 121.4(14) . . ? C72 C73 C58 116.6(13) . . ? C74 C73 C58 118.1(16) . . ? C61 C74 C73 118.6(15) . . ? C61 C74 C75 121.5(16) . . ? C73 C74 C75 112.4(15) . . ? C76 C75 C74 126.3(16) . . ? C76 C75 C64 115.9(15) . . ? C74 C75 C64 114.6(15) . . ? C75 C76 C67 120.2(14) . . ? C75 C76 C71 117.6(14) . . ? C67 C76 C71 121.8(15) . . ? _diffrn_measured_fraction_theta_max 0.780 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.023 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.194 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.005 0.002 0.291 297 137 ' ' 2 -0.027 -0.002 0.709 297 151 ' ' 3 -0.036 0.502 0.209 297 144 ' ' 4 -0.004 0.498 0.791 297 142 ' ' 5 0.244 0.223 1.010 32 8 ' ' 6 0.244 0.277 0.510 32 9 ' ' 7 0.756 0.723 0.490 32 5 ' ' 8 0.756 0.777 0.990 32 5 ' ' _platon_squeeze_details ; ; # Attachment '- c76cl-VI_805562.CIF' data_xne76vcl _database_code_depnum_ccdc_archive 'CCDC 805562' #TrackingRef '- c76cl-VI_805562.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl29.30' _chemical_formula_weight 1951.44 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.1080(10) _cell_length_b 27.592(2) _cell_length_c 11.5540(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.410(10) _cell_angle_gamma 90.00 _cell_volume 6948.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3816 _exptl_absorpt_coefficient_mu 1.194 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20208 _diffrn_reflns_av_R_equivalents 0.2499 _diffrn_reflns_av_sigmaI/netI 0.2650 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 36.73 _reflns_number_total 7082 _reflns_number_gt 2263 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ADP of CL17 were restrained using ISOR. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7082 _refine_ls_number_parameters 505 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.3231 _refine_ls_R_factor_gt 0.1249 _refine_ls_wR_factor_ref 0.3307 _refine_ls_wR_factor_gt 0.2936 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.5530(4) 0.46355(15) 0.3709(5) 0.146(3) Uani 1 1 d . . . Cl2 Cl 0.4779(3) 0.43279(15) 0.5261(5) 0.136(2) Uani 1 1 d . . . Cl3 Cl 0.3545(3) 0.42704(15) 0.3138(5) 0.135(2) Uani 1 1 d . . . Cl4 Cl 0.3038(2) 0.34455(15) 0.4178(4) 0.0962(15) Uani 1 1 d . . . Cl5 Cl 0.4150(2) 0.33562(14) 0.6491(3) 0.0979(15) Uani 1 1 d . . . Cl6 Cl 0.3940(2) 0.22953(14) 0.6650(3) 0.0809(12) Uani 1 1 d . . . Cl7 Cl 0.2872(2) 0.21049(15) 0.4425(3) 0.0857(13) Uani 1 1 d . . . Cl8 Cl 0.42511(17) 0.11366(12) 0.6183(2) 0.0652(10) Uani 1 1 d . . . Cl9 Cl 0.54897(19) 0.00397(12) 0.3708(3) 0.0718(11) Uani 1 1 d . . . Cl10 Cl 0.64833(18) 0.04255(12) 0.1935(3) 0.0684(10) Uani 1 1 d . . . Cl11 Cl 0.7567(2) 0.15136(16) 0.3410(3) 0.0826(12) Uani 1 1 d . . . Cl12 Cl 0.59954(17) 0.08415(13) 0.6351(2) 0.0652(10) Uani 1 1 d . . . Cl13 Cl 0.72184(19) 0.11270(16) 0.5481(3) 0.0869(13) Uani 1 1 d . . . Cl14 Cl 0.70875(19) 0.20972(16) 0.6541(3) 0.0815(12) Uani 1 1 d . . . Cl15 Cl 0.3098(18) 0.4498(11) 0.651(5) 0.213(17) Uani 0.25 1 d P . . Cl16 Cl 0.385(3) 0.4404(11) 0.804(4) 0.195(18) Uani 0.20 1 d P . . Cl17 Cl 0.285(4) 0.497(3) 0.506(8) 0.19(3) Uani 0.10 1 d PU . . Cl18 Cl 0.235(4) 0.466(3) 0.474(9) 0.21(5) Uani 0.10 1 d P . . C1 C 0.5149(12) 0.4059(6) 0.3178(15) 0.114(7) Uani 1 1 d . . . C2 C 0.4751(13) 0.3882(6) 0.4121(19) 0.115(8) Uani 1 1 d . . . C3 C 0.4046(12) 0.3762(5) 0.3417(17) 0.107(7) Uani 1 1 d . . . C4 C 0.3721(10) 0.3286(6) 0.3946(16) 0.111(7) Uani 1 1 d . . . C5 C 0.4168(9) 0.3026(5) 0.5150(12) 0.081(5) Uani 1 1 d . . . C6 C 0.4104(7) 0.2431(5) 0.5277(11) 0.059(4) Uani 1 1 d . . . C7 C 0.3616(7) 0.2166(5) 0.4161(10) 0.066(4) Uani 1 1 d . . . C8 C 0.3814(6) 0.1657(5) 0.3999(10) 0.053(3) Uani 1 1 d . . . C9 C 0.4388(6) 0.1414(5) 0.4861(11) 0.060(4) Uani 1 1 d . . . C10 C 0.4516(7) 0.1020(4) 0.4050(11) 0.056(4) Uani 1 1 d . . . C11 C 0.5083(6) 0.0930(4) 0.4105(9) 0.042(3) Uani 1 1 d . . . C12 C 0.5260(6) 0.0650(4) 0.3135(10) 0.049(3) Uani 1 1 d . . . C13 C 0.5825(6) 0.0906(4) 0.3140(9) 0.047(3) Uani 1 1 d . . . C14 C 0.6024(7) 0.0945(4) 0.2067(10) 0.057(4) Uani 1 1 d . . . C15 C 0.6356(6) 0.1428(5) 0.2063(11) 0.059(4) Uani 1 1 d . . . C16 C 0.6760(7) 0.1636(5) 0.3233(10) 0.062(4) Uani 1 1 d . . . C17 C 0.6657(6) 0.2170(5) 0.3108(10) 0.052(3) Uani 1 1 d . . . C18 C 0.6534(6) 0.2438(5) 0.2045(11) 0.058(4) Uani 1 1 d . . . C19 C 0.6438(7) 0.2919(6) 0.2089(12) 0.069(4) Uani 1 1 d . . . C20 C 0.6338(8) 0.3119(5) 0.3134(12) 0.073(5) Uani 1 1 d . . . C21 C 0.6009(9) 0.3560(5) 0.2832(13) 0.082(5) Uani 1 1 d . . . C22 C 0.5630(9) 0.3690(6) 0.3538(14) 0.085(5) Uani 1 1 d . . . C23 C 0.5634(9) 0.3375(5) 0.4485(12) 0.076(5) Uani 1 1 d . . . C24 C 0.5046(10) 0.3457(5) 0.4682(15) 0.092(6) Uani 1 1 d . . . C25 C 0.4817(9) 0.3081(6) 0.5154(13) 0.079(5) Uani 1 1 d . . . C26 C 0.5129(9) 0.2646(6) 0.5390(11) 0.078(5) Uani 1 1 d . . . C27 C 0.4751(8) 0.2268(5) 0.5411(10) 0.070(5) Uani 1 1 d . . . C28 C 0.4889(6) 0.1776(5) 0.5266(9) 0.055(4) Uani 1 1 d . . . C29 C 0.5496(6) 0.1688(4) 0.5227(9) 0.048(3) Uani 1 1 d . . . C30 C 0.5653(7) 0.1180(5) 0.4936(10) 0.058(4) Uani 1 1 d . . . C31 C 0.6047(5) 0.1184(5) 0.4150(9) 0.046(3) Uani 1 1 d . . . C32 C 0.6594(7) 0.1484(5) 0.4423(10) 0.064(4) Uani 1 1 d . . . C33 C 0.6512(7) 0.1992(5) 0.5054(11) 0.063(4) Uani 1 1 d . . . C34 C 0.6573(7) 0.2360(5) 0.4144(10) 0.065(4) Uani 1 1 d . . . C35 C 0.6362(7) 0.2839(5) 0.4138(10) 0.065(4) Uani 1 1 d . . . C36 C 0.5950(7) 0.2943(5) 0.4781(11) 0.062(4) Uani 1 1 d . . . C37 C 0.5730(6) 0.2542(6) 0.5268(10) 0.060(4) Uani 1 1 d . . . C38 C 0.5885(6) 0.2062(5) 0.5237(9) 0.051(3) 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 Cl1 0.287(8) 0.057(3) 0.157(5) -0.026(3) 0.157(6) -0.021(3) Cl2 0.263(8) 0.068(3) 0.135(4) -0.028(3) 0.143(5) -0.012(3) Cl3 0.256(7) 0.066(3) 0.138(4) 0.012(3) 0.138(5) 0.038(3) Cl4 0.150(4) 0.089(3) 0.078(3) 0.007(2) 0.077(3) 0.029(3) Cl5 0.163(5) 0.091(3) 0.071(2) -0.016(2) 0.079(3) 0.006(3) Cl6 0.117(3) 0.103(3) 0.0446(18) -0.0013(18) 0.056(2) 0.003(2) Cl7 0.100(3) 0.118(3) 0.055(2) 0.010(2) 0.048(2) 0.018(3) Cl8 0.089(3) 0.083(2) 0.0351(15) 0.0131(15) 0.0352(17) 0.004(2) Cl9 0.100(3) 0.065(2) 0.0568(19) 0.0061(16) 0.034(2) 0.003(2) Cl10 0.084(3) 0.076(2) 0.0517(18) -0.0087(16) 0.0317(18) 0.006(2) Cl11 0.089(3) 0.115(3) 0.0520(19) -0.0140(19) 0.034(2) -0.008(2) Cl12 0.080(3) 0.086(2) 0.0349(15) 0.0012(16) 0.0263(16) 0.005(2) Cl13 0.081(3) 0.131(3) 0.0465(19) -0.012(2) 0.0176(19) -0.008(3) Cl14 0.088(3) 0.127(3) 0.0356(16) -0.0193(18) 0.0282(18) -0.028(2) Cl15 0.20(3) 0.15(2) 0.35(5) 0.00(3) 0.17(4) -0.05(2) Cl16 0.29(6) 0.11(2) 0.24(4) -0.02(2) 0.15(4) 0.00(3) Cl17 0.16(4) 0.18(4) 0.21(4) -0.04(3) 0.06(3) 0.02(3) Cl18 0.14(6) 0.24(8) 0.34(11) 0.18(8) 0.19(8) 0.10(6) C1 0.22(2) 0.061(10) 0.104(12) 0.003(9) 0.107(16) 0.016(13) C2 0.23(3) 0.052(11) 0.124(14) -0.031(10) 0.146(18) -0.031(14) C3 0.21(2) 0.046(9) 0.104(13) -0.001(9) 0.105(16) 0.004(12) C4 0.19(2) 0.081(11) 0.106(13) -0.018(10) 0.113(15) 0.003(12) C5 0.125(15) 0.082(11) 0.050(8) -0.004(7) 0.047(9) 0.032(10) C6 0.077(11) 0.070(9) 0.045(7) 0.002(6) 0.039(7) 0.010(8) C7 0.083(11) 0.084(10) 0.035(7) 0.010(6) 0.025(7) 0.010(8) C8 0.057(9) 0.075(9) 0.032(6) 0.004(6) 0.023(6) -0.004(7) C9 0.055(9) 0.095(10) 0.043(7) 0.001(7) 0.032(7) -0.012(8) C10 0.078(11) 0.056(8) 0.045(7) 0.013(6) 0.036(7) -0.010(7) C11 0.041(8) 0.058(8) 0.028(5) 0.008(5) 0.015(5) 0.008(6) C12 0.059(9) 0.059(8) 0.045(6) 0.001(5) 0.037(6) 0.008(6) C13 0.058(9) 0.062(8) 0.022(5) -0.008(5) 0.015(5) 0.000(7) C14 0.091(11) 0.053(8) 0.031(6) -0.018(5) 0.025(7) -0.002(7) C15 0.079(10) 0.059(8) 0.060(8) -0.011(7) 0.052(8) -0.001(8) C16 0.080(11) 0.085(11) 0.032(6) -0.018(6) 0.032(7) -0.022(8) C17 0.048(8) 0.085(10) 0.034(6) -0.017(6) 0.027(6) -0.026(7) C18 0.072(10) 0.068(9) 0.044(7) -0.004(6) 0.035(7) -0.007(8) C19 0.068(10) 0.099(12) 0.055(8) -0.006(8) 0.040(8) -0.020(9) C20 0.112(13) 0.067(10) 0.054(8) -0.017(7) 0.049(9) -0.030(9) C21 0.145(16) 0.046(8) 0.081(10) -0.009(7) 0.074(11) -0.012(10) C22 0.122(15) 0.076(11) 0.080(11) -0.014(9) 0.063(11) -0.017(11) C23 0.141(16) 0.050(9) 0.061(8) -0.019(7) 0.066(10) -0.039(10) C24 0.174(19) 0.030(9) 0.107(12) -0.029(8) 0.095(13) -0.023(10) C25 0.135(16) 0.054(10) 0.072(9) -0.036(8) 0.068(10) -0.021(10) C26 0.151(17) 0.052(9) 0.050(8) -0.013(7) 0.059(10) -0.029(11) C27 0.125(15) 0.066(10) 0.031(6) -0.004(6) 0.043(8) 0.006(10) C28 0.066(10) 0.087(10) 0.024(5) 0.014(6) 0.031(6) 0.018(8) C29 0.067(10) 0.058(8) 0.019(5) 0.003(5) 0.013(6) -0.012(7) C30 0.079(10) 0.070(9) 0.029(6) -0.002(6) 0.026(7) -0.001(8) C31 0.028(7) 0.081(9) 0.028(5) 0.000(6) 0.008(5) 0.002(6) C32 0.067(10) 0.095(10) 0.040(7) -0.019(7) 0.032(7) -0.022(8) C33 0.075(11) 0.072(9) 0.045(7) -0.005(6) 0.025(7) -0.003(8) C34 0.095(12) 0.081(10) 0.028(6) -0.020(6) 0.032(7) -0.027(9) C35 0.101(12) 0.062(9) 0.040(7) -0.022(6) 0.034(8) -0.015(8) C36 0.097(12) 0.062(9) 0.046(7) -0.020(6) 0.049(8) -0.027(9) C37 0.060(10) 0.090(11) 0.031(6) -0.020(6) 0.018(6) -0.010(8) C38 0.067(10) 0.065(9) 0.027(6) -0.008(6) 0.025(6) -0.004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C1 1.823(19) . ? Cl2 C2 1.788(14) . ? Cl3 C3 1.778(19) . ? Cl4 C4 1.743(19) . ? Cl5 C5 1.810(12) . ? Cl6 C6 1.789(11) . ? Cl7 C7 1.852(15) . ? Cl8 C9 1.827(11) . ? Cl9 C12 1.822(12) . ? Cl10 C14 1.819(13) . ? Cl11 C16 1.839(15) . ? Cl12 C30 1.819(12) . ? Cl13 C32 1.837(16) . ? Cl14 C33 1.813(13) . ? Cl15 Cl16 2.04(6) . ? Cl15 Cl17 2.04(10) . ? Cl15 Cl18 2.24(11) . ? Cl17 Cl18 1.38(11) . ? C1 C22 1.46(2) . ? C1 C1 1.49(4) 2_655 ? C1 C2 1.71(2) . ? C2 C24 1.40(3) . ? C2 C3 1.60(3) . ? C3 C21 1.51(2) 2_655 ? C3 C4 1.72(2) . ? C4 C19 1.52(2) 2_655 ? C4 C5 1.60(2) . ? C5 C25 1.51(2) . ? C5 C6 1.66(2) . ? C6 C27 1.52(2) . ? C6 C7 1.582(19) . ? C7 C8 1.506(18) . ? C7 C18 1.518(16) 2_655 ? C8 C15 1.320(16) 2_655 ? C8 C9 1.524(19) . ? C9 C28 1.482(19) . ? C9 C10 1.528(17) . ? C10 C11 1.314(16) . ? C10 C14 1.481(18) 2_655 ? C11 C30 1.514(17) . ? C11 C12 1.525(14) . ? C12 C13 1.485(17) . ? C12 C12 1.56(2) 2_655 ? C13 C31 1.346(15) . ? C13 C14 1.463(14) . ? C14 C10 1.481(18) 2_655 ? C14 C15 1.538(17) . ? C15 C8 1.320(16) 2_655 ? C15 C16 1.480(18) . ? C16 C17 1.490(18) . ? C16 C32 1.601(15) . ? C17 C34 1.378(15) . ? C17 C18 1.381(17) . ? C18 C19 1.349(18) . ? C18 C7 1.518(16) 2_655 ? C19 C20 1.415(16) . ? C19 C4 1.52(2) 2_655 ? C20 C35 1.379(17) . ? C20 C21 1.42(2) . ? C21 C22 1.427(19) . ? C21 C3 1.51(2) 2_655 ? C22 C23 1.396(19) . ? C23 C36 1.38(2) . ? C23 C24 1.47(2) . ? C24 C25 1.36(2) . ? C25 C26 1.38(2) . ? C26 C27 1.366(19) . ? C26 C37 1.47(2) . ? C27 C28 1.417(18) . ? C28 C29 1.437(17) . ? C29 C38 1.365(16) . ? C29 C30 1.516(17) . ? C30 C31 1.484(15) . ? C31 C32 1.455(17) . ? C32 C33 1.620(18) . ? C33 C34 1.501(17) . ? C33 C38 1.545(18) . ? C34 C35 1.408(19) . ? C35 C36 1.418(17) . ? C36 C37 1.410(18) . ? C37 C38 1.376(17) . ? 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 Cl16 Cl15 Cl17 136(3) . . ? Cl16 Cl15 Cl18 173(2) . . ? Cl17 Cl15 Cl18 37(3) . . ? Cl18 Cl17 Cl15 79(6) . . ? Cl17 Cl18 Cl15 63(6) . . ? C22 C1 C1 110.0(13) . 2_655 ? C22 C1 C2 97.9(13) . . ? C1 C1 C2 121(2) 2_655 . ? C22 C1 Cl1 106.0(16) . . ? C1 C1 Cl1 111.0(7) 2_655 . ? C2 C1 Cl1 109.6(10) . . ? C24 C2 C3 108.6(14) . . ? C24 C2 C1 104.6(16) . . ? C3 C2 C1 114.0(16) . . ? C24 C2 Cl2 110.0(15) . . ? C3 C2 Cl2 107.4(13) . . ? C1 C2 Cl2 112.1(11) . . ? C21 C3 C2 108.1(15) 2_655 . ? C21 C3 C4 98.6(12) 2_655 . ? C2 C3 C4 117.9(16) . . ? C21 C3 Cl3 106.0(13) 2_655 . ? C2 C3 Cl3 114.9(13) . . ? C4 C3 Cl3 109.4(14) . . ? C19 C4 C5 107.7(12) 2_655 . ? C19 C4 C3 104.4(11) 2_655 . ? C5 C4 C3 114.8(17) . . ? C19 C4 Cl4 107.1(14) 2_655 . ? C5 C4 Cl4 109.6(10) . . ? C3 C4 Cl4 112.7(12) . . ? C25 C5 C4 108.2(13) . . ? C25 C5 C6 102.5(11) . . ? C4 C5 C6 118.1(13) . . ? C25 C5 Cl5 104.6(11) . . ? C4 C5 Cl5 109.1(9) . . ? C6 C5 Cl5 113.2(8) . . ? C27 C6 C7 110.9(10) . . ? C27 C6 C5 100.9(11) . . ? C7 C6 C5 116.5(11) . . ? C27 C6 Cl6 109.8(9) . . ? C7 C6 Cl6 108.8(9) . . ? C5 C6 Cl6 109.7(8) . . ? C8 C7 C18 109.4(10) . 2_655 ? C8 C7 C6 111.6(11) . . ? C18 C7 C6 113.8(11) 2_655 . ? C8 C7 Cl7 105.8(9) . . ? C18 C7 Cl7 104.7(10) 2_655 . ? C6 C7 Cl7 111.0(8) . . ? C15 C8 C7 123.6(12) 2_655 . ? C15 C8 C9 108.8(12) 2_655 . ? C7 C8 C9 124.3(11) . . ? C28 C9 C8 109.3(11) . . ? C28 C9 C10 112.5(10) . . ? C8 C9 C10 102.5(10) . . ? C28 C9 Cl8 110.6(8) . . ? C8 C9 Cl8 112.1(8) . . ? C10 C9 Cl8 109.6(9) . . ? C11 C10 C14 123.7(10) . 2_655 ? C11 C10 C9 119.8(12) . . ? C14 C10 C9 110.7(12) 2_655 . ? C10 C11 C30 126.0(11) . . ? C10 C11 C12 124.5(11) . . ? C30 C11 C12 107.9(10) . . ? C13 C12 C11 101.9(9) . . ? C13 C12 C12 114.0(9) . 2_655 ? C11 C12 C12 112.4(11) . 2_655 ? C13 C12 Cl9 106.8(8) . . ? C11 C12 Cl9 108.5(7) . . ? C12 C12 Cl9 112.5(4) 2_655 . ? C31 C13 C14 123.9(11) . . ? C31 C13 C12 110.8(9) . . ? C14 C13 C12 123.7(9) . . ? C13 C14 C10 109.7(11) . 2_655 ? C13 C14 C15 111.2(9) . . ? C10 C14 C15 98.8(10) 2_655 . ? C13 C14 Cl10 111.7(9) . . ? C10 C14 Cl10 112.5(7) 2_655 . ? C15 C14 Cl10 112.1(10) . . ? C8 C15 C16 124.4(12) 2_655 . ? C8 C15 C14 115.1(12) 2_655 . ? C16 C15 C14 119.9(10) . . ? C15 C16 C17 105.3(11) . . ? C15 C16 C32 115.1(10) . . ? C17 C16 C32 105.4(10) . . ? C15 C16 Cl11 109.7(8) . . ? C17 C16 Cl11 108.4(9) . . ? C32 C16 Cl11 112.3(10) . . ? C34 C17 C18 121.5(13) . . ? C34 C17 C16 110.9(11) . . ? C18 C17 C16 126.5(10) . . ? C19 C18 C17 118.8(11) . . ? C19 C18 C7 122.1(12) . 2_655 ? C17 C18 C7 117.9(12) . 2_655 ? C18 C19 C20 119.4(12) . . ? C18 C19 C4 128.8(12) . 2_655 ? C20 C19 C4 110.4(13) . 2_655 ? C35 C20 C19 121.9(13) . . ? C35 C20 C21 123.8(12) . . ? C19 C20 C21 110.5(13) . . ? C20 C21 C22 117.2(13) . . ? C20 C21 C3 114.9(12) . 2_655 ? C22 C21 C3 125.4(16) . 2_655 ? C23 C22 C21 116.5(15) . . ? C23 C22 C1 117.6(14) . . ? C21 C22 C1 124.4(14) . . ? C36 C23 C22 126.7(14) . . ? C36 C23 C24 122.4(12) . . ? C22 C23 C24 105.1(16) . . ? C25 C24 C2 129.1(19) . . ? C25 C24 C23 116.6(15) . . ? C2 C24 C23 112.9(15) . . ? C24 C25 C26 119.7(16) . . ? C24 C25 C5 126.5(17) . . ? C26 C25 C5 111.7(14) . . ? C27 C26 C25 111.9(17) . . ? C27 C26 C37 118.8(14) . . ? C25 C26 C37 126.9(14) . . ? C26 C27 C28 124.1(15) . . ? C26 C27 C6 112.6(13) . . ? C28 C27 C6 121.6(14) . . ? C27 C28 C29 115.1(13) . . ? C27 C28 C9 119.9(13) . . ? C29 C28 C9 123.1(12) . . ? C38 C29 C28 121.3(12) . . ? C38 C29 C30 119.7(12) . . ? C28 C29 C30 118.0(11) . . ? C31 C30 C11 101.3(8) . . ? C31 C30 C29 111.7(10) . . ? C11 C30 C29 109.9(11) . . ? C31 C30 Cl12 112.4(9) . . ? C11 C30 Cl12 111.3(8) . . ? C29 C30 Cl12 109.9(7) . . ? C13 C31 C32 124.3(10) . . ? C13 C31 C30 113.1(11) . . ? C32 C31 C30 122.5(10) . . ? C31 C32 C16 113.7(9) . . ? C31 C32 C33 111.5(11) . . ? C16 C32 C33 104.8(10) . . ? C31 C32 Cl13 105.8(9) . . ? C16 C32 Cl13 110.7(9) . . ? C33 C32 Cl13 110.4(8) . . ? C34 C33 C38 108.8(11) . . ? C34 C33 C32 102.6(9) . . ? C38 C33 C32 115.1(11) . . ? C34 C33 Cl14 110.2(9) . . ? C38 C33 Cl14 106.0(8) . . ? C32 C33 Cl14 114.0(9) . . ? C17 C34 C35 120.1(12) . . ? C17 C34 C33 115.1(12) . . ? C35 C34 C33 121.7(10) . . ? C20 C35 C34 116.6(11) . . ? C20 C35 C36 118.7(14) . . ? C34 C35 C36 118.6(12) . . ? C23 C36 C37 123.0(13) . . ? C23 C36 C35 115.9(12) . . ? C37 C36 C35 116.3(13) . . ? C38 C37 C36 127.9(12) . . ? C38 C37 C26 116.9(13) . . ? C36 C37 C26 111.2(13) . . ? C29 C38 C37 123.5(13) . . ? C29 C38 C33 123.4(12) . . ? C37 C38 C33 112.8(12) . . ? _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.735 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.152 # Attachment '- c76cl-VII_805563.CIF' data_c76cl-VII_805563 _database_code_depnum_ccdc_archive 'CCDC 805563' #TrackingRef '- .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl28.65' _chemical_formula_weight 1928.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monocl;inic _symmetry_space_group_name_H-M P2(1)/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 11.6025(8) _cell_length_b 41.703(2) _cell_length_c 14.7460(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.139(3) _cell_angle_gamma 90.00 _cell_volume 6740.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 33 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3772 _exptl_absorpt_coefficient_mu 1.205 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38697 _diffrn_reflns_av_R_equivalents 0.1310 _diffrn_reflns_av_sigmaI/netI 0.1118 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 34.94 _reflns_number_total 12063 _reflns_number_gt 8205 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two Cl atoms are disordered over two positions. All restraints concern ADP of Cl atoms. ; _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^)+(0.0900P)^2^+120.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12063 _refine_ls_number_parameters 991 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.1279 _refine_ls_wR_factor_ref 0.3180 _refine_ls_wR_factor_gt 0.3029 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.2838(3) 0.02585(7) 0.4558(3) 0.0333(7) Uani 0.90 1 d P . . Cl1A Cl 0.274(3) 0.0266(6) 0.404(2) 0.030(6) Uani 0.10 1 d PU . . Cl2 Cl 0.2907(4) 0.02758(9) 0.2538(3) 0.0591(10) Uani 0.90 1 d P . . Cl3 Cl 0.1094(3) 0.09329(9) 0.2406(3) 0.0617(9) Uani 1 1 d . . . Cl4 Cl 0.5402(4) 0.00728(8) 0.2962(3) 0.0647(10) Uani 1 1 d . . . Cl5 Cl 0.5044(4) 0.07257(8) 0.1031(2) 0.0557(9) Uani 1 1 d . . . Cl6 Cl 0.2429(4) 0.12761(11) 0.0737(3) 0.0750(12) Uani 1 1 d . . . Cl7 Cl 0.0633(3) 0.18105(8) 0.3439(3) 0.0666(11) Uani 1 1 d . . . Cl8 Cl 0.2667(4) 0.24368(8) 0.5623(4) 0.0826(14) Uani 1 1 d . . . Cl9 Cl 0.1325(3) 0.18576(8) 0.5882(3) 0.0673(11) Uani 1 1 d . . . Cl10 Cl 0.2756(4) 0.16582(8) 0.7865(3) 0.0668(11) Uani 1 1 d . . . Cl11 Cl 0.4481(4) 0.22286(8) 0.8129(3) 0.0790(13) Uani 1 1 d . . . Cl12 Cl 0.6614(5) 0.18759(11) 0.9482(3) 0.0834(14) Uani 1 1 d . . . Cl13 Cl 0.5308(4) 0.12436(9) 0.9439(3) 0.0732(12) Uani 1 1 d . . . Cl14 Cl 0.7509(4) 0.08350(11) 0.9678(2) 0.0739(11) Uani 1 1 d . . . Cl15 Cl 0.9263(4) 0.13768(12) 0.9723(3) 0.0847(14) Uani 1 1 d . . . Cl16 Cl 1.0774(4) 0.10148(12) 0.8735(3) 0.0784(12) Uani 1 1 d . . . Cl17 Cl 0.9333(4) 0.03958(10) 0.8511(2) 0.0666(10) Uani 1 1 d . . . Cl18 Cl 0.9668(3) 0.02056(7) 0.6654(2) 0.0491(8) Uani 1 1 d . . . Cl19 Cl 1.1182(3) 0.07899(9) 0.6547(3) 0.0601(9) Uani 1 1 d . . . Cl20 Cl 1.0256(3) 0.07814(9) 0.4409(3) 0.0588(9) Uani 1 1 d . . . Cl21 Cl 0.8535(4) 0.02442(8) 0.3993(3) 0.0625(10) Uani 1 1 d . . . Cl22 Cl 0.8330(3) 0.10594(7) 0.2233(2) 0.0500(8) Uani 1 1 d . . . Cl23 Cl 0.4199(4) 0.17940(9) 0.0763(3) 0.0712(12) Uani 1 1 d . . . Cl24 Cl 0.2428(4) 0.22572(9) 0.1972(3) 0.0821(15) Uani 1 1 d . . . Cl25 Cl 0.4474(5) 0.27271(7) 0.4290(3) 0.0819(14) Uani 1 1 d . . . Cl26 Cl 0.7381(3) 0.19783(6) 0.2218(2) 0.0548(9) Uani 1 1 d . . . Cl27 Cl 0.6158(4) 0.25833(7) 0.3174(3) 0.0789(14) Uani 1 1 d . . . Cl28 Cl 0.8297(7) 0.24349(19) 0.4952(6) 0.062(2) Uani 0.84 1 d P . . C28A Cl 0.861(3) 0.2412(8) 0.485(3) 0.056(9) Uani 0.16 1 d PU . . Cl29 Cl 0.356(2) 0.0504(5) 0.8463(15) 0.096(6) Uani 0.25 1 d P . . Cl30 Cl 0.227(5) 0.0106(12) 1.002(4) 0.094(14) Uani 0.10 1 d PU . . Cl31 Cl 0.200(4) -0.0225(8) 0.864(3) 0.105(10) Uani 0.15 1 d PU . . Cl32 Cl 0.335(3) 0.0101(5) 0.9339(17) 0.116(7) Uani 0.25 1 d PU . . C1 C 0.3415(9) 0.0882(2) 0.4694(8) 0.027(2) Uani 1 1 d . . . C2 C 0.3800(9) 0.0934(2) 0.5697(8) 0.029(2) Uani 1 1 d . . . C3 C 0.4836(9) 0.0766(2) 0.6373(7) 0.023(2) Uani 1 1 d . . . C4 C 0.5534(8) 0.05692(18) 0.5955(7) 0.020(2) Uani 1 1 d . . . C5 C 0.5118(9) 0.05008(19) 0.4983(7) 0.023(2) Uani 1 1 d U . . C6 C 0.3858(9) 0.0569(2) 0.4370(8) 0.028(2) Uani 1 1 d . . . C7 C 0.3932(10) 0.0571(2) 0.3316(8) 0.034(2) Uani 1 1 d . . . C8 C 0.3572(10) 0.0879(2) 0.2839(8) 0.033(2) Uani 1 1 d . . . C9 C 0.2616(10) 0.1087(3) 0.3038(9) 0.038(3) Uani 1 1 d . . . C10 C 0.2808(9) 0.1123(2) 0.4068(8) 0.031(2) Uani 1 1 d . . . C11 C 0.2568(9) 0.1424(2) 0.4463(9) 0.034(3) Uani 1 1 d . . . C12 C 0.2869(11) 0.1460(2) 0.5436(9) 0.041(3) Uani 1 1 d . . . C13 C 0.3460(10) 0.1223(2) 0.6032(9) 0.037(3) Uani 1 1 d . . . C14 C 0.4063(10) 0.1344(2) 0.6988(8) 0.034(3) Uani 1 1 d . . . C15 C 0.5024(11) 0.1186(3) 0.7590(8) 0.039(3) Uani 1 1 d . . . C16 C 0.5437(10) 0.0902(2) 0.7267(8) 0.033(2) Uani 1 1 d . . . C17 C 0.6680(11) 0.0853(3) 0.7769(7) 0.038(3) Uani 1 1 d . . . C18 C 0.7365(11) 0.0688(3) 0.7339(8) 0.037(3) Uani 1 1 d . . . C19 C 0.6791(10) 0.0557(2) 0.6416(7) 0.028(2) Uani 1 1 d . . . C20 C 0.7606(8) 0.0533(2) 0.5899(7) 0.023(2) Uani 1 1 d . . . C21 C 0.7211(9) 0.05259(19) 0.4935(7) 0.024(2) Uani 1 1 d . . . C22 C 0.5933(9) 0.04743(17) 0.4473(7) 0.0199(19) Uani 1 1 d U . . C23 C 0.5309(10) 0.0488(2) 0.3448(8) 0.034(2) Uani 1 1 d . . . C24 C 0.5954(9) 0.0701(2) 0.2998(7) 0.025(2) Uani 1 1 d . . . C25 C 0.5280(11) 0.0926(2) 0.2188(7) 0.034(2) Uani 1 1 d . . . C26 C 0.4090(10) 0.1027(2) 0.2263(7) 0.033(2) Uani 1 1 d . . . C27 C 0.3531(11) 0.1342(3) 0.1916(8) 0.040(3) Uani 1 1 d . . . C28 C 0.2817(10) 0.1407(3) 0.2606(8) 0.038(3) Uani 1 1 d . . . C29 C 0.2659(11) 0.1680(3) 0.2960(9) 0.044(3) Uani 1 1 d . . . C30 C 0.2254(11) 0.1720(2) 0.3826(9) 0.043(3) Uani 1 1 d . . . C31 C 0.3062(12) 0.1987(2) 0.4379(10) 0.048(3) Uani 1 1 d . . . C32 C 0.3371(12) 0.2046(2) 0.5460(10) 0.048(3) Uani 1 1 d . . . C33 C 0.2889(11) 0.1772(2) 0.5982(10) 0.043(3) Uani 1 1 d . . . C34 C 0.3686(13) 0.1675(3) 0.7089(10) 0.054(4) Uani 1 1 d . . . C35 C 0.4861(13) 0.1876(3) 0.7587(9) 0.050(3) Uani 1 1 d . . . C36 C 0.6032(14) 0.1682(3) 0.8326(9) 0.059(4) Uani 1 1 d . . . C37 C 0.5935(15) 0.1314(3) 0.8462(10) 0.059(4) Uani 1 1 d . . . C38 C 0.7172(13) 0.1078(3) 0.8608(9) 0.049(3) Uani 1 1 d . . . C39 C 0.8344(13) 0.1241(4) 0.8563(8) 0.054(3) Uani 1 1 d . . . C40 C 0.9185(13) 0.1036(3) 0.8004(9) 0.052(3) Uani 1 1 d . . . C41 C 0.8722(12) 0.0702(3) 0.7588(8) 0.046(3) Uani 1 1 d . . . C42 C 0.8906(11) 0.0594(3) 0.6556(8) 0.039(3) Uani 1 1 d . . . C43 C 0.9522(10) 0.0840(3) 0.6057(9) 0.042(3) Uani 1 1 d . . . C44 C 0.9029(9) 0.0853(2) 0.4878(7) 0.029(2) Uani 1 1 d . . . C45 C 0.7935(10) 0.0631(2) 0.4317(8) 0.035(2) Uani 1 1 d . . . C46 C 0.7131(10) 0.0780(2) 0.3414(7) 0.028(2) Uani 1 1 d . . . C47 C 0.7364(10) 0.1099(2) 0.2990(8) 0.035(3) Uani 1 1 d . . . C48 C 0.6143(10) 0.1202(2) 0.2389(7) 0.032(2) Uani 1 1 d . . . C49 C 0.5753(10) 0.1503(2) 0.2305(8) 0.034(2) Uani 1 1 d . . . C50 C 0.4459(12) 0.1611(3) 0.1934(9) 0.047(3) Uani 1 1 d . . . C51 C 0.4477(13) 0.1884(2) 0.2627(9) 0.042(3) Uani 1 1 d . . . C52 C 0.3384(13) 0.1982(3) 0.2878(11) 0.055(4) Uani 1 1 d . . . C53 C 0.3729(11) 0.2113(2) 0.3871(9) 0.043(3) Uani 1 1 d . . . C54 C 0.4830(13) 0.2296(3) 0.4277(10) 0.052(4) Uani 1 1 d . . . C55 C 0.5386(12) 0.2199(2) 0.5301(10) 0.045(3) Uani 1 1 d . . . C56 C 0.4702(12) 0.2099(2) 0.5903(9) 0.044(3) Uani 1 1 d . . . C57 C 0.5338(12) 0.2002(2) 0.6806(9) 0.045(3) Uani 1 1 d . . . C58 C 0.6613(14) 0.1940(3) 0.7069(9) 0.050(4) Uani 1 1 d . . . C59 C 0.7019(13) 0.1728(3) 0.7854(9) 0.051(4) Uani 1 1 d . . . C60 C 0.8006(13) 0.1536(3) 0.7951(9) 0.051(3) Uani 1 1 d . . . C61 C 0.8551(11) 0.1546(3) 0.7219(9) 0.044(3) Uani 1 1 d . . . C62 C 0.9108(11) 0.1253(3) 0.7170(8) 0.043(3) Uani 1 1 d . . . C63 C 0.9259(10) 0.1163(3) 0.6336(9) 0.038(3) Uani 1 1 d . . . C64 C 0.8859(10) 0.1365(2) 0.5528(9) 0.037(3) Uani 1 1 d . . . C65 C 0.8653(10) 0.1195(2) 0.4683(8) 0.032(2) Uani 1 1 d . . . C66 C 0.7903(9) 0.1323(2) 0.3812(8) 0.029(2) Uani 1 1 d . . . C67 C 0.7443(10) 0.1643(2) 0.3787(8) 0.034(3) Uani 1 1 d . . . C68 C 0.6526(11) 0.1768(2) 0.2898(9) 0.040(3) Uani 1 1 d . . . C69 C 0.5584(13) 0.1977(2) 0.3088(9) 0.042(3) Uani 1 1 d . . . C70 C 0.5929(14) 0.2241(2) 0.3843(11) 0.055(4) Uani 1 1 d . . . C71 C 0.7087(13) 0.2141(2) 0.4730(10) 0.048(3) Uani 1 1 d . . . C72 C 0.6606(12) 0.2134(2) 0.5541(9) 0.043(3) Uani 1 1 d U . . C73 C 0.7219(11) 0.1980(3) 0.6394(9) 0.045(3) Uani 1 1 d . . . C74 C 0.8215(11) 0.1764(3) 0.6451(9) 0.041(3) Uani 1 1 d . . . C75 C 0.8324(11) 0.1674(2) 0.5551(9) 0.041(3) Uani 1 1 d . . . C76 C 0.7656(11) 0.1818(2) 0.4657(9) 0.037(3) 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 Cl1 0.0327(19) 0.0203(14) 0.055(2) 0.0029(15) 0.0256(19) -0.0077(10) Cl1A 0.047(15) 0.007(9) 0.038(13) 0.006(10) 0.016(12) -0.006(8) Cl2 0.076(3) 0.054(2) 0.0476(19) -0.0126(15) 0.020(2) -0.0319(18) Cl3 0.034(2) 0.088(3) 0.066(2) 0.0125(18) 0.0193(19) 0.0007(15) Cl4 0.099(3) 0.0405(17) 0.072(2) -0.0129(15) 0.051(2) -0.0094(16) Cl5 0.085(3) 0.0562(18) 0.0348(15) -0.0040(12) 0.0325(18) 0.0022(16) Cl6 0.074(3) 0.105(3) 0.0434(19) 0.0173(19) 0.016(2) 0.017(2) Cl7 0.051(2) 0.059(2) 0.104(3) 0.0291(19) 0.045(2) 0.0314(16) Cl8 0.122(4) 0.0372(17) 0.132(4) 0.0105(19) 0.100(3) 0.0260(19) Cl9 0.059(2) 0.066(2) 0.106(3) -0.0013(19) 0.066(2) 0.0164(16) Cl10 0.098(3) 0.0527(18) 0.090(3) -0.0036(16) 0.085(2) 0.0019(17) Cl11 0.133(4) 0.0453(18) 0.099(3) -0.0293(18) 0.094(3) -0.0095(19) Cl12 0.118(4) 0.092(3) 0.063(2) -0.048(2) 0.060(3) -0.033(2) Cl13 0.116(3) 0.081(2) 0.0514(19) -0.0105(17) 0.066(2) -0.009(2) Cl14 0.093(3) 0.106(3) 0.0303(16) 0.0011(17) 0.030(2) -0.002(2) Cl15 0.083(3) 0.127(4) 0.0410(19) -0.037(2) 0.017(2) -0.025(3) Cl16 0.045(3) 0.134(4) 0.047(2) -0.020(2) 0.004(2) -0.016(2) Cl17 0.060(3) 0.096(3) 0.0434(18) 0.0141(17) 0.0160(19) 0.0164(19) Cl18 0.0363(19) 0.0539(17) 0.0590(19) 0.0130(14) 0.0180(16) 0.0158(13) Cl19 0.0181(17) 0.094(3) 0.069(2) -0.0013(18) 0.0160(18) -0.0031(14) Cl20 0.0340(18) 0.093(2) 0.067(2) 0.0061(17) 0.0409(18) 0.0148(15) Cl21 0.075(3) 0.0497(18) 0.085(2) -0.0019(16) 0.056(2) 0.0142(15) Cl22 0.061(2) 0.0565(17) 0.0560(18) 0.0027(13) 0.0512(18) 0.0054(14) Cl23 0.115(3) 0.067(2) 0.055(2) 0.0350(16) 0.059(2) 0.043(2) Cl24 0.116(4) 0.065(2) 0.091(3) 0.053(2) 0.069(3) 0.057(2) Cl25 0.139(4) 0.0187(14) 0.131(3) 0.0113(16) 0.103(3) 0.0131(17) Cl26 0.086(2) 0.0334(14) 0.075(2) 0.0126(13) 0.067(2) -0.0022(13) Cl27 0.141(4) 0.0215(14) 0.116(3) 0.0142(16) 0.100(3) -0.0029(17) Cl28 0.087(4) 0.030(2) 0.108(4) -0.025(2) 0.084(4) -0.034(2) C28A 0.070(15) 0.015(9) 0.089(15) -0.004(9) 0.035(11) -0.026(10) Cl29 0.103(16) 0.085(12) 0.092(13) 0.002(10) 0.020(12) 0.014(10) Cl30 0.09(2) 0.085(19) 0.084(19) 0.012(16) 0.001(16) -0.004(16) Cl31 0.110(19) 0.089(16) 0.100(17) 0.016(13) 0.013(14) 0.029(14) Cl32 0.141(16) 0.092(12) 0.098(12) -0.022(10) 0.015(12) -0.005(11) C1 0.021(6) 0.019(4) 0.055(7) 0.006(4) 0.030(5) 0.002(3) C2 0.031(6) 0.018(4) 0.053(6) -0.003(4) 0.034(6) -0.008(4) C3 0.023(6) 0.023(4) 0.032(5) 0.005(4) 0.020(5) -0.004(3) C4 0.024(6) 0.010(4) 0.035(5) 0.003(3) 0.022(5) -0.005(3) C5 0.026(5) 0.008(3) 0.039(5) 0.002(3) 0.015(4) -0.006(3) C6 0.020(6) 0.019(4) 0.051(6) 0.002(4) 0.020(5) -0.001(3) C7 0.035(7) 0.031(5) 0.041(6) 0.002(4) 0.019(6) 0.000(4) C8 0.022(6) 0.037(6) 0.036(6) 0.002(4) 0.006(5) 0.003(4) C9 0.031(7) 0.038(6) 0.050(7) 0.010(5) 0.019(6) 0.006(4) C10 0.020(6) 0.025(5) 0.056(7) 0.008(4) 0.024(6) 0.006(4) C11 0.023(6) 0.023(5) 0.068(8) 0.014(5) 0.032(6) 0.005(4) C12 0.053(8) 0.023(5) 0.070(8) 0.007(5) 0.053(7) 0.005(4) C13 0.049(7) 0.023(5) 0.062(7) 0.005(5) 0.049(7) 0.000(4) C14 0.046(7) 0.027(5) 0.046(6) 0.002(4) 0.039(6) -0.005(4) C15 0.054(8) 0.044(6) 0.033(6) -0.010(5) 0.033(6) -0.011(5) C16 0.040(7) 0.033(5) 0.037(6) 0.004(4) 0.029(6) 0.001(4) C17 0.051(8) 0.040(6) 0.027(5) 0.004(4) 0.020(6) -0.008(5) C18 0.046(8) 0.042(6) 0.030(6) 0.006(4) 0.022(6) -0.005(5) C19 0.039(7) 0.018(4) 0.034(5) 0.008(4) 0.021(5) -0.003(4) C20 0.017(6) 0.019(4) 0.034(5) 0.003(4) 0.012(5) 0.002(3) C21 0.028(6) 0.014(4) 0.039(6) 0.003(4) 0.021(5) 0.005(3) C22 0.030(5) 0.005(3) 0.033(4) 0.000(3) 0.020(4) 0.001(3) C23 0.040(7) 0.019(5) 0.048(6) 0.003(4) 0.023(6) 0.004(4) C24 0.031(6) 0.017(4) 0.031(5) -0.005(3) 0.018(5) 0.005(4) C25 0.054(8) 0.029(5) 0.027(5) -0.002(4) 0.023(6) -0.002(4) C26 0.037(7) 0.035(6) 0.028(5) 0.004(4) 0.012(5) 0.001(4) C27 0.040(7) 0.040(6) 0.045(7) 0.012(5) 0.019(6) 0.009(5) C28 0.027(7) 0.039(6) 0.046(7) 0.018(5) 0.012(6) 0.013(4) C29 0.039(7) 0.041(6) 0.059(8) 0.024(5) 0.027(7) 0.017(5) C30 0.043(7) 0.029(5) 0.069(8) 0.021(5) 0.035(7) 0.022(5) C31 0.056(8) 0.017(5) 0.087(9) 0.012(5) 0.046(8) 0.021(5) C32 0.059(9) 0.025(5) 0.083(9) 0.016(5) 0.052(8) 0.015(5) C33 0.049(8) 0.024(5) 0.077(9) 0.000(5) 0.047(7) 0.009(4) C34 0.081(10) 0.030(6) 0.086(10) -0.011(6) 0.077(9) -0.006(5) C35 0.081(10) 0.031(6) 0.062(8) -0.016(5) 0.057(8) -0.005(6) C36 0.077(11) 0.070(9) 0.047(7) -0.033(6) 0.043(8) -0.030(7) C37 0.099(12) 0.047(7) 0.054(8) -0.010(6) 0.056(9) -0.011(7) C38 0.054(9) 0.063(8) 0.036(6) -0.001(5) 0.024(7) -0.001(6) C39 0.050(9) 0.079(9) 0.025(6) -0.014(6) 0.004(6) -0.012(7) C40 0.043(9) 0.078(9) 0.032(6) -0.012(6) 0.008(7) -0.013(6) C41 0.053(9) 0.056(7) 0.034(6) 0.000(5) 0.021(6) 0.002(6) C42 0.034(7) 0.043(6) 0.046(7) 0.001(5) 0.021(6) 0.001(5) C43 0.016(6) 0.056(7) 0.060(8) -0.007(6) 0.019(6) -0.011(5) C44 0.016(6) 0.040(5) 0.040(6) 0.001(4) 0.023(5) 0.002(4) C45 0.033(7) 0.034(5) 0.045(6) -0.004(5) 0.024(6) -0.006(4) C46 0.036(7) 0.021(5) 0.035(5) -0.002(4) 0.025(5) 0.005(4) C47 0.039(7) 0.029(5) 0.056(7) 0.001(4) 0.041(6) 0.004(4) C48 0.047(7) 0.029(5) 0.030(5) -0.002(4) 0.030(6) 0.001(4) C49 0.045(7) 0.030(5) 0.040(6) 0.007(4) 0.034(6) 0.003(4) C50 0.066(9) 0.039(6) 0.051(7) 0.020(5) 0.040(7) 0.017(5) C51 0.067(9) 0.024(5) 0.050(7) 0.022(5) 0.040(7) 0.015(5) C52 0.072(10) 0.027(6) 0.084(10) 0.032(6) 0.050(8) 0.020(6) C53 0.056(8) 0.019(5) 0.073(8) 0.017(5) 0.048(7) 0.022(5) C54 0.084(10) 0.025(5) 0.072(9) 0.005(5) 0.060(9) 0.008(6) C55 0.064(8) 0.012(4) 0.081(9) -0.015(5) 0.055(8) -0.004(4) C56 0.080(9) 0.009(4) 0.069(8) -0.009(4) 0.059(8) -0.001(5) C57 0.074(9) 0.021(5) 0.065(8) -0.023(5) 0.057(8) -0.015(5) C58 0.089(11) 0.031(6) 0.047(7) -0.025(5) 0.044(8) -0.024(6) C59 0.064(9) 0.048(7) 0.056(8) -0.036(6) 0.041(7) -0.026(6) C60 0.054(9) 0.066(8) 0.041(7) -0.031(6) 0.025(7) -0.029(6) C61 0.044(8) 0.044(7) 0.048(7) -0.027(5) 0.019(6) -0.025(5) C62 0.023(7) 0.064(8) 0.036(6) -0.017(5) 0.004(6) -0.018(5) C63 0.021(6) 0.047(6) 0.048(7) -0.011(5) 0.015(6) -0.019(4) C64 0.039(7) 0.031(5) 0.054(7) -0.012(5) 0.030(6) -0.021(4) C65 0.027(6) 0.038(6) 0.044(6) -0.008(5) 0.027(6) -0.012(4) C66 0.030(6) 0.027(5) 0.045(6) -0.005(4) 0.033(6) -0.009(4) C67 0.047(7) 0.023(5) 0.049(6) -0.003(4) 0.040(6) -0.012(4) C68 0.064(8) 0.020(5) 0.058(7) 0.005(4) 0.051(7) -0.003(5) C69 0.070(9) 0.016(5) 0.061(7) 0.010(5) 0.049(8) 0.005(5) C70 0.092(11) 0.018(5) 0.091(10) -0.002(5) 0.080(10) -0.004(5) C71 0.072(9) 0.015(5) 0.078(9) -0.014(5) 0.053(8) -0.022(5) C72 0.063(7) 0.020(4) 0.060(6) -0.015(4) 0.039(6) -0.022(4) C73 0.051(8) 0.033(6) 0.066(8) -0.034(6) 0.040(7) -0.031(5) C74 0.040(7) 0.036(6) 0.055(7) -0.024(5) 0.027(6) -0.022(5) C75 0.042(7) 0.029(5) 0.066(8) -0.015(5) 0.036(7) -0.024(5) C76 0.048(7) 0.023(5) 0.060(7) -0.004(5) 0.046(7) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Cl1A 0.73(3) . ? Cl1 C6 1.837(9) . ? Cl1A C6 1.76(3) . ? Cl1A Cl2 2.29(3) . ? Cl2 C7 1.830(12) . ? Cl3 C9 1.822(13) . ? Cl4 C23 1.892(10) . ? Cl5 C25 1.838(10) . ? Cl6 C27 1.809(13) . ? Cl7 C30 1.816(12) . ? Cl8 C32 1.874(10) . ? Cl9 C33 1.807(11) . ? Cl10 C34 1.812(10) . ? Cl11 C35 1.796(10) . ? Cl12 C36 1.806(12) . ? Cl13 C37 1.838(11) . ? Cl14 C38 1.807(13) . ? Cl15 C39 1.786(12) . ? Cl16 C40 1.806(15) . ? Cl17 C41 1.830(13) . ? Cl18 C42 1.830(12) . ? Cl19 C43 1.833(12) . ? Cl20 C44 1.799(8) . ? Cl21 C45 1.878(11) . ? Cl22 C47 1.831(9) . ? Cl23 C50 1.821(11) . ? Cl24 C52 1.833(12) . ? Cl25 C54 1.848(11) . ? Cl26 C68 1.846(9) . ? Cl27 C70 1.805(11) . ? Cl28 C71 1.812(12) . ? C28A C71 2.06(3) . ? Cl29 Cl32 2.19(3) . ? Cl30 Cl32 1.84(7) . ? Cl30 Cl31 2.39(7) . ? Cl31 Cl32 2.07(5) . ? C1 C10 1.389(14) . ? C1 C2 1.415(15) . ? C1 C6 1.534(12) . ? C2 C13 1.409(13) . ? C2 C3 1.464(15) . ? C3 C16 1.394(15) . ? C3 C4 1.428(11) . ? C4 C5 1.384(13) . ? C4 C19 1.394(15) . ? C5 C22 1.392(12) . ? C5 C6 1.473(15) . ? C6 C7 1.583(14) . ? C7 C8 1.460(15) . ? C7 C23 1.582(15) . ? C8 C26 1.340(14) . ? C8 C9 1.511(14) . ? C9 C10 1.469(16) . ? C9 C28 1.530(14) . ? C10 C11 1.451(13) . ? C11 C12 1.369(17) . ? C11 C30 1.521(14) . ? C12 C13 1.351(16) . ? C12 C33 1.524(15) . ? C13 C14 1.444(17) . ? C14 C15 1.348(17) . ? C14 C34 1.470(14) . ? C15 C16 1.419(14) . ? C15 C37 1.471(19) . ? C16 C17 1.403(17) . ? C17 C18 1.354(15) . ? C17 C38 1.510(17) . ? C18 C19 1.415(15) . ? C18 C41 1.496(17) . ? C19 C20 1.398(12) . ? C20 C21 1.343(14) . ? C20 C42 1.524(16) . ? C21 C22 1.430(14) . ? C21 C45 1.494(12) . ? C22 C23 1.448(15) . ? C23 C24 1.454(13) . ? C24 C46 1.342(15) . ? C24 C25 1.518(14) . ? C25 C26 1.481(15) . ? C25 C48 1.488(15) . ? C26 C27 1.480(15) . ? C27 C28 1.533(15) . ? C27 C50 1.549(17) . ? C28 C29 1.291(16) . ? C29 C30 1.507(16) . ? C29 C52 1.541(17) . ? C30 C31 1.510(19) . ? C31 C53 1.347(15) . ? C31 C32 1.54(2) . ? C32 C56 1.483(19) . ? C32 C33 1.579(14) . ? C33 C34 1.64(2) . ? C34 C35 1.563(19) . ? C35 C57 1.525(15) . ? C35 C36 1.65(2) . ? C36 C59 1.535(16) . ? C36 C37 1.555(19) . ? C37 C38 1.70(2) . ? C38 C39 1.540(19) . ? C39 C60 1.50(2) . ? C39 C40 1.700(19) . ? C40 C62 1.505(18) . ? C40 C41 1.546(18) . ? C41 C42 1.666(15) . ? C42 C43 1.564(15) . ? C43 C63 1.468(16) . ? C43 C44 1.644(17) . ? C44 C65 1.492(15) . ? C44 C45 1.569(15) . ? C45 C46 1.488(16) . ? C46 C47 1.532(13) . ? C47 C48 1.467(16) . ? C47 C66 1.495(15) . ? C48 C49 1.326(14) . ? C49 C50 1.489(17) . ? C49 C68 1.510(16) . ? C50 C51 1.527(17) . ? C51 C69 1.300(18) . ? C51 C52 1.490(16) . ? C52 C53 1.49(2) . ? C53 C54 1.438(19) . ? C54 C55 1.489(19) . ? C54 C70 1.619(15) . ? C55 C72 1.368(18) . ? C55 C56 1.433(14) . ? C56 C57 1.355(19) . ? C57 C58 1.425(19) . ? C58 C73 1.405(15) . ? C58 C59 1.41(2) . ? C59 C60 1.37(2) . ? C60 C61 1.419(16) . ? C61 C62 1.395(18) . ? C61 C74 1.404(18) . ? C62 C63 1.351(15) . ? C63 C64 1.410(17) . ? C64 C65 1.386(15) . ? C64 C75 1.435(16) . ? C65 C66 1.401(16) . ? C66 C67 1.434(14) . ? C67 C76 1.424(15) . ? C67 C68 1.486(17) . ? C68 C69 1.494(14) . ? C69 C70 1.522(17) . ? C70 C71 1.59(2) . ? C71 C72 1.477(15) . ? C71 C76 1.518(15) . ? C72 C73 1.383(19) . ? C73 C74 1.447(17) . ? C74 C75 1.423(15) . ? C75 C76 1.424(18) . ? 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 Cl1A Cl1 C6 73(2) . . ? Cl1 Cl1A C6 84(2) . . ? Cl1 Cl1A Cl2 167(3) . . ? C6 Cl1A Cl2 87.9(13) . . ? C7 Cl2 Cl1A 69.4(7) . . ? Cl32 Cl30 Cl31 57(2) . . ? Cl32 Cl31 Cl30 48.1(18) . . ? Cl30 Cl32 Cl31 75(2) . . ? Cl30 Cl32 Cl29 123(2) . . ? Cl31 Cl32 Cl29 115.3(16) . . ? C10 C1 C2 120.1(9) . . ? C10 C1 C6 123.8(9) . . ? C2 C1 C6 115.7(9) . . ? C13 C2 C1 118.0(10) . . ? C13 C2 C3 115.7(10) . . ? C1 C2 C3 123.1(8) . . ? C16 C3 C4 117.6(9) . . ? C16 C3 C2 119.7(8) . . ? C4 C3 C2 115.9(8) . . ? C5 C4 C19 116.8(8) . . ? C5 C4 C3 120.8(9) . . ? C19 C4 C3 117.5(9) . . ? C4 C5 C22 120.5(9) . . ? C4 C5 C6 122.3(8) . . ? C22 C5 C6 113.4(9) . . ? C5 C6 C1 109.9(8) . . ? C5 C6 C7 103.9(7) . . ? C1 C6 C7 115.8(8) . . ? C5 C6 Cl1A 121.5(11) . . ? C1 C6 Cl1A 113.7(12) . . ? C7 C6 Cl1A 90.3(13) . . ? C5 C6 Cl1 109.2(6) . . ? C1 C6 Cl1 104.7(6) . . ? C7 C6 Cl1 113.2(7) . . ? Cl1A C6 Cl1 23.3(10) . . ? C8 C7 C23 111.5(8) . . ? C8 C7 C6 112.2(8) . . ? C23 C7 C6 104.9(8) . . ? C8 C7 Cl2 105.4(8) . . ? C23 C7 Cl2 110.7(7) . . ? C6 C7 Cl2 112.4(7) . . ? C26 C8 C7 126.4(10) . . ? C26 C8 C9 111.7(9) . . ? C7 C8 C9 121.5(9) . . ? C10 C9 C8 112.8(9) . . ? C10 C9 C28 110.4(9) . . ? C8 C9 C28 101.4(8) . . ? C10 C9 Cl3 111.0(7) . . ? C8 C9 Cl3 110.4(8) . . ? C28 C9 Cl3 110.4(8) . . ? C1 C10 C11 118.8(10) . . ? C1 C10 C9 119.0(9) . . ? C11 C10 C9 121.3(9) . . ? C12 C11 C10 119.9(9) . . ? C12 C11 C30 119.0(9) . . ? C10 C11 C30 119.6(10) . . ? C13 C12 C11 120.1(9) . . ? C13 C12 C33 111.3(11) . . ? C11 C12 C33 127.0(10) . . ? C12 C13 C2 122.7(11) . . ? C12 C13 C14 111.1(9) . . ? C2 C13 C14 122.7(10) . . ? C15 C14 C13 120.3(9) . . ? C15 C14 C34 127.0(11) . . ? C13 C14 C34 111.2(11) . . ? C14 C15 C16 119.0(10) . . ? C14 C15 C37 126.9(11) . . ? C16 C15 C37 111.9(11) . . ? C3 C16 C17 123.3(9) . . ? C3 C16 C15 122.5(10) . . ? C17 C16 C15 110.3(10) . . ? C18 C17 C16 119.1(10) . . ? C18 C17 C38 125.3(11) . . ? C16 C17 C38 112.8(10) . . ? C17 C18 C19 118.9(11) . . ? C17 C18 C41 126.7(11) . . ? C19 C18 C41 112.1(9) . . ? C4 C19 C20 121.6(9) . . ? C4 C19 C18 122.8(9) . . ? C20 C19 C18 111.3(9) . . ? C21 C20 C19 121.4(9) . . ? C21 C20 C42 126.9(8) . . ? C19 C20 C42 110.3(9) . . ? C20 C21 C22 116.6(8) . . ? C20 C21 C45 125.0(9) . . ? C22 C21 C45 117.1(9) . . ? C5 C22 C21 120.9(8) . . ? C5 C22 C23 111.4(9) . . ? C21 C22 C23 125.2(8) . . ? C22 C23 C24 110.2(9) . . ? C22 C23 C7 106.0(8) . . ? C24 C23 C7 117.5(8) . . ? C22 C23 Cl4 106.7(6) . . ? C24 C23 Cl4 106.5(6) . . ? C7 C23 Cl4 109.4(7) . . ? C46 C24 C23 122.7(9) . . ? C46 C24 C25 113.1(8) . . ? C23 C24 C25 121.8(9) . . ? C26 C25 C48 110.5(8) . . ? C26 C25 C24 111.6(8) . . ? C48 C25 C24 100.5(9) . . ? C26 C25 Cl5 109.8(8) . . ? C48 C25 Cl5 114.9(6) . . ? C24 C25 Cl5 109.3(6) . . ? C8 C26 C27 113.0(9) . . ? C8 C26 C25 122.7(9) . . ? C27 C26 C25 122.6(9) . . ? C26 C27 C28 101.5(8) . . ? C26 C27 C50 114.4(10) . . ? C28 C27 C50 112.6(10) . . ? C26 C27 Cl6 106.8(8) . . ? C28 C27 Cl6 107.4(8) . . ? C50 C27 Cl6 113.2(8) . . ? C29 C28 C9 122.7(10) . . ? C29 C28 C27 127.2(10) . . ? C9 C28 C27 108.1(9) . . ? C28 C29 C30 124.5(10) . . ? C28 C29 C52 122.4(10) . . ? C30 C29 C52 107.8(11) . . ? C29 C30 C31 103.2(9) . . ? C29 C30 C11 110.8(8) . . ? C31 C30 C11 106.5(11) . . ? C29 C30 Cl7 109.6(9) . . ? C31 C30 Cl7 114.4(7) . . ? C11 C30 Cl7 112.1(7) . . ? C53 C31 C30 110.9(11) . . ? C53 C31 C32 122.2(12) . . ? C30 C31 C32 124.8(9) . . ? C56 C32 C31 109.6(9) . . ? C56 C32 C33 112.2(10) . . ? C31 C32 C33 113.0(10) . . ? C56 C32 Cl8 104.4(8) . . ? C31 C32 Cl8 108.0(8) . . ? C33 C32 Cl8 109.2(7) . . ? C12 C33 C32 107.8(9) . . ? C12 C33 C34 102.9(9) . . ? C32 C33 C34 119.2(10) . . ? C12 C33 Cl9 106.5(8) . . ? C32 C33 Cl9 108.9(8) . . ? C34 C33 Cl9 110.7(7) . . ? C14 C34 C35 107.9(10) . . ? C14 C34 C33 102.6(9) . . ? C35 C34 C33 117.1(9) . . ? C14 C34 Cl10 106.6(7) . . ? C35 C34 Cl10 109.5(8) . . ? C33 C34 Cl10 112.3(8) . . ? C57 C35 C34 107.9(10) . . ? C57 C35 C36 104.1(10) . . ? C34 C35 C36 116.8(9) . . ? C57 C35 Cl11 104.8(7) . . ? C34 C35 Cl11 110.1(8) . . ? C36 C35 Cl11 112.1(8) . . ? C59 C36 C37 106.1(11) . . ? C59 C36 C35 102.4(11) . . ? C37 C36 C35 119.4(11) . . ? C59 C36 Cl12 105.6(9) . . ? C37 C36 Cl12 109.9(10) . . ? C35 C36 Cl12 112.1(9) . . ? C15 C37 C36 107.9(12) . . ? C15 C37 C38 103.6(9) . . ? C36 C37 C38 119.6(11) . . ? C15 C37 Cl13 105.7(9) . . ? C36 C37 Cl13 108.9(8) . . ? C38 C37 Cl13 110.1(9) . . ? C17 C38 C39 109.9(9) . . ? C17 C38 C37 100.4(10) . . ? C39 C38 C37 117.5(11) . . ? C17 C38 Cl14 106.3(8) . . ? C39 C38 Cl14 110.1(10) . . ? C37 C38 Cl14 111.6(7) . . ? C60 C39 C38 109.1(12) . . ? C60 C39 C40 101.5(9) . . ? C38 C39 C40 117.1(10) . . ? C60 C39 Cl15 105.8(9) . . ? C38 C39 Cl15 110.9(8) . . ? C40 C39 Cl15 111.5(9) . . ? C62 C40 C41 107.3(9) . . ? C62 C40 C39 101.7(11) . . ? C41 C40 C39 117.7(10) . . ? C62 C40 Cl16 107.0(9) . . ? C41 C40 Cl16 110.3(10) . . ? C39 C40 Cl16 111.8(8) . . ? C18 C41 C40 109.5(10) . . ? C18 C41 C42 101.9(9) . . ? C40 C41 C42 118.2(9) . . ? C18 C41 Cl17 106.0(8) . . ? C40 C41 Cl17 109.5(9) . . ? C42 C41 Cl17 110.9(8) . . ? C20 C42 C43 108.7(9) . . ? C20 C42 C41 103.2(8) . . ? C43 C42 C41 118.0(9) . . ? C20 C42 Cl18 104.7(7) . . ? C43 C42 Cl18 109.5(7) . . ? C41 C42 Cl18 111.7(8) . . ? C63 C43 C42 107.4(8) . . ? C63 C43 C44 103.6(9) . . ? C42 C43 C44 117.7(9) . . ? C63 C43 Cl19 106.4(8) . . ? C42 C43 Cl19 108.8(9) . . ? C44 C43 Cl19 112.1(6) . . ? C65 C44 C45 109.1(8) . . ? C65 C44 C43 102.3(8) . . ? C45 C44 C43 118.7(7) . . ? C65 C44 Cl20 107.6(6) . . ? C45 C44 Cl20 107.8(6) . . ? C43 C44 Cl20 110.9(7) . . ? C46 C45 C21 110.8(9) . . ? C46 C45 C44 112.8(8) . . ? C21 C45 C44 111.7(8) . . ? C46 C45 Cl21 107.9(7) . . ? C21 C45 Cl21 103.5(6) . . ? C44 C45 Cl21 109.7(7) . . ? C24 C46 C45 123.5(8) . . ? C24 C46 C47 108.4(9) . . ? C45 C46 C47 125.8(9) . . ? C48 C47 C66 111.8(8) . . ? C48 C47 C46 103.6(8) . . ? C66 C47 C46 107.2(8) . . ? C48 C47 Cl22 108.7(7) . . ? C66 C47 Cl22 112.0(7) . . ? C46 C47 Cl22 113.3(6) . . ? C49 C48 C47 124.4(10) . . ? C49 C48 C25 121.7(10) . . ? C47 C48 C25 110.4(9) . . ? C48 C49 C50 126.4(10) . . ? C48 C49 C68 121.3(11) . . ? C50 C49 C68 109.1(9) . . ? C49 C50 C51 100.9(11) . . ? C49 C50 C27 113.5(9) . . ? C51 C50 C27 114.1(9) . . ? C49 C50 Cl23 108.0(7) . . ? C51 C50 Cl23 106.4(7) . . ? C27 C50 Cl23 112.9(10) . . ? C69 C51 C52 124.4(12) . . ? C69 C51 C50 111.5(10) . . ? C52 C51 C50 123.0(13) . . ? C53 C52 C51 111.6(12) . . ? C53 C52 C29 101.6(9) . . ? C51 C52 C29 109.0(9) . . ? C53 C52 Cl24 112.9(8) . . ? C51 C52 Cl24 110.6(8) . . ? C29 C52 Cl24 110.7(10) . . ? C31 C53 C54 124.7(13) . . ? C31 C53 C52 112.6(12) . . ? C54 C53 C52 121.3(10) . . ? C53 C54 C55 108.0(9) . . ? C53 C54 C70 117.9(10) . . ? C55 C54 C70 103.2(11) . . ? C53 C54 Cl25 110.3(9) . . ? C55 C54 Cl25 106.1(8) . . ? C70 C54 Cl25 110.5(7) . . ? C72 C55 C56 121.2(12) . . ? C72 C55 C54 112.5(10) . . ? C56 C55 C54 124.3(12) . . ? C57 C56 C55 117.5(12) . . ? C57 C56 C32 122.8(10) . . ? C55 C56 C32 118.6(12) . . ? C56 C57 C58 120.2(10) . . ? C56 C57 C35 128.9(12) . . ? C58 C57 C35 109.5(12) . . ? C73 C58 C59 123.1(13) . . ? C73 C58 C57 120.2(12) . . ? C59 C58 C57 112.0(10) . . ? C60 C59 C58 119.8(11) . . ? C60 C59 C36 127.2(13) . . ? C58 C59 C36 110.6(13) . . ? C59 C60 C61 118.1(13) . . ? C59 C60 C39 126.0(11) . . ? C61 C60 C39 112.8(12) . . ? C62 C61 C74 122.5(10) . . ? C62 C61 C60 110.1(12) . . ? C74 C61 C60 123.8(12) . . ? C63 C62 C61 119.4(12) . . ? C63 C62 C40 125.9(11) . . ? C61 C62 C40 112.9(10) . . ? C62 C63 C64 119.8(11) . . ? C62 C63 C43 127.7(11) . . ? C64 C63 C43 110.7(10) . . ? C65 C64 C63 111.3(10) . . ? C65 C64 C75 122.3(12) . . ? C63 C64 C75 122.9(10) . . ? C64 C65 C66 120.0(10) . . ? C64 C65 C44 111.4(10) . . ? C66 C65 C44 126.7(9) . . ? C65 C66 C67 119.6(9) . . ? C65 C66 C47 118.2(9) . . ? C67 C66 C47 120.6(10) . . ? C76 C67 C66 120.0(10) . . ? C76 C67 C68 118.6(9) . . ? C66 C67 C68 120.1(9) . . ? C67 C68 C69 113.2(9) . . ? C67 C68 C49 111.8(8) . . ? C69 C68 C49 101.7(10) . . ? C67 C68 Cl26 106.8(7) . . ? C69 C68 Cl26 112.5(7) . . ? C49 C68 Cl26 110.9(7) . . ? C51 C69 C68 112.8(10) . . ? C51 C69 C70 125.1(10) . . ? C68 C69 C70 121.7(12) . . ? C69 C70 C71 111.0(9) . . ? C69 C70 C54 109.9(11) . . ? C71 C70 C54 105.9(10) . . ? C69 C70 Cl27 102.9(8) . . ? C71 C70 Cl27 114.8(8) . . ? C54 C70 Cl27 112.4(8) . . ? C72 C71 C76 109.3(9) . . ? C72 C71 C70 103.2(10) . . ? C76 C71 C70 116.3(10) . . ? C72 C71 Cl28 110.0(8) . . ? C76 C71 Cl28 106.5(8) . . ? C70 C71 Cl28 111.5(8) . . ? C72 C71 C28A 118.7(14) . . ? C76 C71 C28A 96.5(13) . . ? C70 C71 C28A 113.5(13) . . ? Cl28 C71 C28A 11.0(11) . . ? C55 C72 C73 120.5(10) . . ? C55 C72 C71 114.9(12) . . ? C73 C72 C71 121.7(12) . . ? C72 C73 C58 118.1(12) . . ? C72 C73 C74 120.4(10) . . ? C58 C73 C74 117.4(12) . . ? C61 C74 C75 119.7(10) . . ? C61 C74 C73 117.2(10) . . ? C75 C74 C73 115.0(12) . . ? C74 C75 C76 124.4(11) . . ? C74 C75 C64 115.4(11) . . ? C76 C75 C64 117.6(10) . . ? C67 C76 C75 120.0(9) . . ? C67 C76 C71 124.4(12) . . ? C75 C76 C71 115.1(10) . . ? _diffrn_measured_fraction_theta_max 0.842 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 1.114 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.169 # Attachment '- c76cl-VIII_805564.CIF' data_viiicorr _database_code_depnum_ccdc_archive 'CCDC 805564' #TrackingRef '- c76cl-VIII_805564.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl33.84' _chemical_formula_weight 2112.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/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 13.7770(5) _cell_length_b 19.5282(8) _cell_length_c 24.8550(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.065(2) _cell_angle_gamma 90.00 _cell_volume 6685.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 34 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4125 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93349 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 38.09 _reflns_number_total 15334 _reflns_number_gt 13721 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four Cl atoms, CL7, CL8, CL4, and {CL1A + CL1B), the latter disordered equally between two positions, have partial ocupancies of 0.739(5), which results in an averaged composition of the fullerene chloride: C76CL32.96. Two Cl atoms are disordered over two positions each, CL16 - CL35 and CL29 - CL39, with occupancies of main components being 0.815(4) for CL29 and 0.920(6) for CL16. This disorder corresponds to the presence of molecules with the addition pattern somewhat different from that of the main component. All restraints were used for ADP of Cl atoms (ISOR). ; _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^)+(0.0650P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15334 _refine_ls_number_parameters 1066 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1918 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.80694(10) 0.04364(6) 0.12380(5) 0.0269(3) Uani 1 1 d . . . Cl2 Cl 0.77913(10) 0.11685(6) 0.22983(5) 0.0280(3) Uani 1 1 d . . . Cl3 Cl 0.57882(10) 0.04865(6) 0.19778(5) 0.0303(3) Uani 1 1 d . . . Cl4 Cl 0.34871(10) 0.03539(6) -0.02555(5) 0.0286(3) Uani 1 1 d . . . Cl5 Cl 0.37406(10) 0.10070(6) -0.13478(5) 0.0275(3) Uani 1 1 d . . . Cl6 Cl 0.57672(11) 0.03541(6) -0.09961(6) 0.0316(3) Uani 1 1 d . . . Cl7 Cl 0.5838(2) 0.13451(11) -0.19133(7) 0.0538(8) Uani 0.739(5) 1 d P . . Cl8 Cl 0.7587(2) 0.18648(16) -0.18260(10) 0.0611(9) Uani 0.739(5) 1 d P . . Cl9 Cl 0.82187(12) 0.09615(9) -0.09647(7) 0.0447(4) Uani 1 1 d . . . Cl10 Cl 0.94872(10) 0.22798(8) -0.08714(6) 0.0340(3) Uani 1 1 d . . . Cl11 Cl 0.94521(9) 0.11830(7) 0.01692(6) 0.0307(3) Uani 1 1 d . . . Cl12 Cl 0.96511(10) 0.15669(7) 0.13495(6) 0.0317(3) Uani 1 1 d . . . Cl1A Cl 0.5821(4) 0.1519(3) 0.2837(3) 0.0221(13) Uani 0.370(2) 1 d P . . Cl1B Cl 0.5457(4) 0.1605(3) 0.2850(3) 0.0221(12) Uani 0.370(2) 1 d P . . Cl14 Cl 0.3955(3) 0.20515(18) 0.27287(11) 0.0721(11) Uani 0.739(5) 1 d P . . Cl15 Cl 0.33353(11) 0.10728(8) 0.19261(7) 0.0399(4) Uani 1 1 d . . . Cl16 Cl 0.20311(10) 0.23619(8) 0.17567(6) 0.0288(4) Uani 0.920(6) 1 d P . . Cl17 Cl 0.20982(9) 0.11723(7) 0.07819(6) 0.0293(3) Uani 1 1 d . . . Cl18 Cl 0.18861(9) 0.14474(6) -0.04189(6) 0.0283(3) Uani 1 1 d . . . Cl19 Cl 0.49617(10) 0.29149(7) -0.21561(5) 0.0283(3) Uani 1 1 d . . . Cl20 Cl 0.68748(11) 0.36586(8) -0.19474(5) 0.0333(3) Uani 1 1 d . . . Cl21 Cl 0.87474(13) 0.40323(10) -0.10854(7) 0.0480(4) Uani 1 1 d . . . Cl22 Cl 0.94434(10) 0.42488(7) 0.00282(7) 0.0349(3) Uani 1 1 d . . . Cl23 Cl 1.00713(9) 0.31755(7) 0.10391(6) 0.0327(3) Uani 1 1 d . . . Cl24 Cl 0.89696(10) 0.44892(6) 0.13454(6) 0.0308(3) Uani 1 1 d . . . Cl25 Cl 0.87877(10) 0.34367(7) 0.22673(5) 0.0292(3) Uani 1 1 d . . . Cl26 Cl 0.71457(10) 0.44621(6) 0.23998(5) 0.0279(3) Uani 1 1 d . . . Cl27 Cl 0.65404(11) 0.31548(7) 0.30066(5) 0.0302(3) Uani 1 1 d . . . Cl28 Cl 0.46129(12) 0.38596(8) 0.27542(5) 0.0359(3) Uani 1 1 d . . . Cl29 Cl 0.27552(16) 0.41457(12) 0.18747(8) 0.0463(6) Uani 0.815(4) 1 d P . . Cl30 Cl 0.20430(9) 0.42532(7) 0.07600(6) 0.0325(3) Uani 1 1 d . . . Cl31 Cl 0.14284(9) 0.30715(7) -0.01898(6) 0.0286(3) Uani 1 1 d . . . Cl32 Cl 0.24761(9) 0.43502(6) -0.05814(5) 0.0240(3) Uani 1 1 d . . . Cl33 Cl 0.27134(9) 0.32238(6) -0.14305(5) 0.0257(3) Uani 1 1 d . . . Cl34 Cl 0.43198(10) 0.42637(6) -0.16319(5) 0.0246(3) Uani 1 1 d . . . Cl35 Cl 0.225(2) 0.3006(18) 0.2029(16) 0.079(11) Uani 0.080(6) 1 d P . . Cl36 Cl 0.2327(8) 0.4663(5) 0.2295(4) 0.054(3) Uani 0.185(4) 1 d P . . Cl37 Cl 0.0962(9) 0.4719(11) 0.2097(5) 0.089(5) Uani 0.185(4) 1 d P . . Cl38 Cl 0.8859(18) -0.0367(11) -0.1875(9) 0.101(6) Uani 0.185(4) 1 d P . . Cl39 Cl 0.3813(16) 0.4893(9) 0.1718(7) 0.098(5) Uani 0.185(4) 1 d PU . . Cl40 Cl 0.938(2) -0.0135(10) -0.1433(12) 0.129(8) Uani 0.185(4) 1 d P . . Cl41 Cl 0.926(2) -0.0542(17) -0.2132(13) 0.099(8) Uani 0.129(3) 1 d PU . . C1 C 0.6006(3) 0.1302(2) 0.07278(18) 0.0162(8) Uani 1 1 d . . . C2 C 0.5535(3) 0.1277(2) 0.02128(18) 0.0163(8) Uani 1 1 d . . . C3 C 0.6062(4) 0.1333(2) -0.02758(18) 0.0179(9) Uani 1 1 d . . . C4 C 0.7035(4) 0.1492(2) -0.02452(19) 0.0190(9) Uani 1 1 d . . . C5 C 0.7504(3) 0.1478(2) 0.02658(19) 0.0188(9) Uani 1 1 d . . . C6 C 0.7019(3) 0.1342(2) 0.07271(19) 0.0169(9) Uani 1 1 d . . . C7 C 0.7666(3) 0.1313(2) 0.1209(2) 0.0190(9) Uani 1 1 d . . . C8 C 0.7126(4) 0.1507(2) 0.17286(18) 0.0198(9) Uani 1 1 d . . . C9 C 0.6007(4) 0.1339(2) 0.17548(18) 0.0193(9) Uani 1 1 d . . . C10 C 0.5486(4) 0.1393(2) 0.12095(18) 0.0169(9) Uani 1 1 d . . . C11 C 0.4504(3) 0.1546(2) 0.11716(18) 0.0176(9) Uani 1 1 d . . . C12 C 0.4033(3) 0.1483(2) 0.06648(19) 0.0171(9) Uani 1 1 d . . . C13 C 0.4519(3) 0.1309(2) 0.02135(19) 0.0179(9) Uani 1 1 d . . . C14 C 0.3880(4) 0.1235(2) -0.02642(19) 0.0186(9) Uani 1 1 d . . . C15 C 0.4409(4) 0.1381(2) -0.07950(19) 0.0186(9) Uani 1 1 d . . . C16 C 0.5536(4) 0.1222(2) -0.08137(19) 0.0197(9) Uani 1 1 d . . . C17 C 0.5931(4) 0.1750(3) -0.1242(2) 0.0286(11) Uani 1 1 d . . . C18 C 0.6953(4) 0.2021(3) -0.1164(2) 0.0319(12) Uani 1 1 d . . . C19 C 0.7621(4) 0.1710(3) -0.0719(2) 0.0249(10) Uani 1 1 d . . . C20 C 0.8330(4) 0.2328(3) -0.0534(2) 0.0235(10) Uani 1 1 d . . . C21 C 0.8539(3) 0.2420(3) 0.0071(2) 0.0202(9) Uani 1 1 d . . . C22 C 0.8514(4) 0.1750(2) 0.0390(2) 0.0215(9) Uani 1 1 d . . . C23 C 0.8523(4) 0.1802(2) 0.1027(2) 0.0221(10) Uani 1 1 d . . . C24 C 0.8350(3) 0.2525(2) 0.1193(2) 0.0187(9) Uani 1 1 d . . . C25 C 0.7781(4) 0.2702(2) 0.15952(19) 0.0197(9) Uani 1 1 d . . . C26 C 0.7105(4) 0.2255(2) 0.18281(18) 0.0204(9) Uani 1 1 d . . . C27 C 0.6325(4) 0.2468(2) 0.21016(18) 0.0205(9) Uani 1 1 d . . . C28 C 0.5599(4) 0.1902(3) 0.2156(2) 0.0282(11) Uani 1 1 d . . . C29 C 0.4574(4) 0.2158(3) 0.2053(2) 0.0303(12) Uani 1 1 d . . . C30 C 0.3910(4) 0.1800(3) 0.16320(19) 0.0226(10) Uani 1 1 d . . . C31 C 0.3194(4) 0.2390(3) 0.1417(2) 0.0235(10) Uani 1 1 d . . . C32 C 0.2986(3) 0.2430(3) 0.08036(19) 0.0196(9) Uani 1 1 d . . . C33 C 0.3021(3) 0.1726(2) 0.05279(19) 0.0195(9) Uani 1 1 d . . . C34 C 0.3005(4) 0.1726(2) -0.0110(2) 0.0203(9) Uani 1 1 d . . . C35 C 0.3171(3) 0.2432(2) -0.03118(18) 0.0172(9) Uani 1 1 d . . . C36 C 0.3744(3) 0.2579(2) -0.07221(19) 0.0184(9) Uani 1 1 d . . . C37 C 0.4425(4) 0.2125(2) -0.09331(18) 0.0188(9) Uani 1 1 d . . . C38 C 0.5202(4) 0.2314(2) -0.12167(18) 0.0186(9) Uani 1 1 d . . . C39 C 0.5285(4) 0.3012(2) -0.14614(17) 0.0190(9) Uani 1 1 d . . . C40 C 0.6363(4) 0.3284(3) -0.13605(18) 0.0208(9) Uani 1 1 d . . . C41 C 0.7045(4) 0.2754(3) -0.1118(2) 0.0236(10) Uani 1 1 d . . . C42 C 0.7802(4) 0.2929(3) -0.0766(2) 0.0264(10) Uani 1 1 d . . . C43 C 0.7963(4) 0.3627(3) -0.0582(2) 0.0260(10) Uani 1 1 d . . . C44 C 0.8387(4) 0.3708(2) 0.0008(2) 0.0214(9) Uani 1 1 d . . . C45 C 0.8598(3) 0.3042(3) 0.0304(2) 0.0216(9) Uani 1 1 d . . . C46 C 0.8772(4) 0.3129(2) 0.0915(2) 0.0227(10) Uani 1 1 d . . . C47 C 0.8224(3) 0.3758(2) 0.1211(2) 0.0197(9) Uani 1 1 d . . . C48 C 0.7852(4) 0.3437(2) 0.17503(19) 0.0207(9) Uani 1 1 d . . . C49 C 0.6894(4) 0.3717(2) 0.19901(18) 0.0191(9) Uani 1 1 d U . . C50 C 0.6213(4) 0.3182(3) 0.23082(19) 0.0222(10) Uani 1 1 d . . . C51 C 0.5134(4) 0.3431(2) 0.21902(19) 0.0219(10) Uani 1 1 d . . . C52 C 0.4460(4) 0.2880(3) 0.19793(19) 0.0221(9) Uani 1 1 d . . . C53 C 0.3701(4) 0.3021(3) 0.1620(2) 0.0253(10) Uani 1 1 d . . . C54 C 0.3543(4) 0.3689(3) 0.1387(2) 0.0258(10) Uani 1 1 d . . . C55 C 0.3111(4) 0.3719(2) 0.0798(2) 0.0205(9) Uani 1 1 d . . . C56 C 0.2912(3) 0.3028(2) 0.05413(19) 0.0190(9) Uani 1 1 d . . . C57 C 0.2732(4) 0.3051(2) -0.0068(2) 0.0208(9) Uani 1 1 d . . . C58 C 0.3267(3) 0.3657(2) -0.04007(18) 0.0164(8) Uani 1 1 d . . . C59 C 0.3650(3) 0.3293(2) -0.09181(18) 0.0176(9) Uani 1 1 d . . . C60 C 0.4602(4) 0.3567(2) -0.11731(18) 0.0183(9) Uani 1 1 d . . . C61 C 0.5285(3) 0.3870(2) -0.07702(17) 0.0161(8) Uani 1 1 d . . . C62 C 0.6229(4) 0.3798(2) -0.09204(18) 0.0185(9) Uani 1 1 d . . . C63 C 0.6996(3) 0.3966(2) -0.05742(19) 0.0180(9) Uani 1 1 d . . . C64 C 0.6776(3) 0.4179(2) -0.00576(19) 0.0168(8) Uani 1 1 d . . . C65 C 0.7551(3) 0.4035(2) 0.03066(19) 0.0175(9) Uani 1 1 d . . . C66 C 0.7408(3) 0.4007(2) 0.08500(19) 0.0182(9) Uani 1 1 d . . . C67 C 0.6462(3) 0.4144(2) 0.10423(18) 0.0155(8) Uani 1 1 d . . . C68 C 0.6195(4) 0.3971(2) 0.15678(18) 0.0189(9) Uani 1 1 d . . . C69 C 0.5259(4) 0.3908(2) 0.17278(18) 0.0189(9) Uani 1 1 d . . . C70 C 0.4492(4) 0.4046(2) 0.13676(19) 0.0195(9) Uani 1 1 d . . . C71 C 0.4708(3) 0.4217(2) 0.08412(18) 0.0157(8) Uani 1 1 d . . . C72 C 0.3925(3) 0.4033(2) 0.04867(18) 0.0165(8) Uani 1 1 d . . . C73 C 0.4073(3) 0.3954(2) -0.00555(18) 0.0151(8) Uani 1 1 d . . . C74 C 0.5024(3) 0.4086(2) -0.02542(17) 0.0138(8) Uani 1 1 d . . . C75 C 0.5818(3) 0.4253(2) 0.01114(18) 0.0162(8) Uani 1 1 d . . . C76 C 0.5665(3) 0.4278(2) 0.06709(17) 0.0150(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 Cl1 0.0346(6) 0.0108(5) 0.0345(6) 0.0000(4) -0.0200(5) 0.0039(4) Cl2 0.0434(7) 0.0185(5) 0.0213(6) 0.0038(4) -0.0252(5) -0.0008(5) Cl3 0.0422(7) 0.0166(5) 0.0312(6) 0.0117(5) -0.0202(6) -0.0074(5) Cl4 0.0436(7) 0.0106(5) 0.0308(6) -0.0003(4) -0.0224(5) -0.0059(5) Cl5 0.0419(7) 0.0187(5) 0.0208(5) -0.0073(4) -0.0247(5) 0.0014(5) Cl6 0.0440(7) 0.0174(5) 0.0324(7) -0.0156(5) -0.0228(6) 0.0107(5) Cl7 0.119(2) 0.0306(10) 0.0110(8) -0.0097(7) -0.0146(10) 0.0390(12) Cl8 0.086(2) 0.0656(17) 0.0320(11) -0.0007(11) 0.0111(12) 0.0361(15) Cl9 0.0367(8) 0.0415(8) 0.0559(10) -0.0268(7) -0.0019(7) 0.0116(6) Cl10 0.0262(6) 0.0406(8) 0.0351(7) -0.0028(6) 0.0008(5) 0.0052(5) Cl11 0.0255(6) 0.0276(6) 0.0386(7) -0.0024(5) -0.0080(5) 0.0105(5) Cl12 0.0281(6) 0.0243(6) 0.0418(7) -0.0020(5) -0.0216(6) 0.0036(5) Cl1A 0.037(3) 0.019(2) 0.0094(18) 0.0059(15) -0.013(2) -0.011(2) Cl1B 0.042(3) 0.019(2) 0.0056(15) 0.0049(12) -0.004(2) -0.002(2) Cl14 0.108(3) 0.0727(19) 0.0360(13) -0.0018(12) 0.0129(14) -0.0411(18) Cl15 0.0357(7) 0.0390(8) 0.0449(8) 0.0222(7) -0.0019(6) -0.0084(6) Cl16 0.0248(7) 0.0351(8) 0.0265(7) 0.0048(5) 0.0004(5) -0.0020(5) Cl17 0.0273(6) 0.0282(6) 0.0322(7) 0.0043(5) -0.0081(5) -0.0113(5) Cl18 0.0266(6) 0.0239(6) 0.0337(7) 0.0009(5) -0.0189(5) -0.0066(5) Cl19 0.0453(7) 0.0275(6) 0.0115(5) -0.0012(4) -0.0125(5) 0.0041(5) Cl20 0.0404(7) 0.0424(8) 0.0172(5) 0.0067(5) 0.0024(5) 0.0003(6) Cl21 0.0444(9) 0.0545(10) 0.0455(9) 0.0104(8) 0.0068(7) 0.0014(7) Cl22 0.0231(6) 0.0273(6) 0.0542(9) 0.0053(6) -0.0022(6) -0.0074(5) Cl23 0.0230(6) 0.0316(7) 0.0429(8) 0.0016(6) -0.0124(5) -0.0020(5) Cl24 0.0337(7) 0.0203(6) 0.0376(7) 0.0008(5) -0.0189(5) -0.0105(5) Cl25 0.0362(7) 0.0243(6) 0.0262(6) -0.0014(5) -0.0232(5) -0.0020(5) Cl26 0.0443(7) 0.0175(5) 0.0213(6) -0.0089(4) -0.0168(5) -0.0042(5) Cl27 0.0502(8) 0.0263(6) 0.0135(5) -0.0006(4) -0.0165(5) -0.0038(5) Cl28 0.0482(8) 0.0415(8) 0.0180(6) -0.0089(5) -0.0014(5) 0.0028(6) Cl29 0.0447(11) 0.0565(13) 0.0378(10) -0.0102(9) 0.0038(8) 0.0049(9) Cl30 0.0232(6) 0.0249(6) 0.0494(8) -0.0051(6) -0.0022(5) 0.0047(5) Cl31 0.0217(6) 0.0276(6) 0.0361(7) -0.0004(5) -0.0102(5) 0.0006(4) Cl32 0.0267(6) 0.0160(5) 0.0289(6) -0.0003(4) -0.0154(5) 0.0061(4) Cl33 0.0334(6) 0.0232(6) 0.0196(5) 0.0002(4) -0.0197(5) 0.0007(5) Cl34 0.0383(7) 0.0183(5) 0.0166(5) 0.0050(4) -0.0116(5) 0.0033(5) Cl35 0.064(18) 0.07(2) 0.10(3) 0.009(17) 0.033(17) 0.004(14) Cl36 0.061(6) 0.047(5) 0.055(6) 0.003(4) -0.016(5) -0.007(4) Cl37 0.049(6) 0.165(17) 0.054(7) 0.005(8) -0.011(5) 0.004(8) Cl38 0.132(17) 0.091(13) 0.080(12) 0.016(10) -0.013(12) -0.019(12) Cl39 0.130(13) 0.079(9) 0.086(10) -0.008(8) -0.009(9) 0.016(9) Cl40 0.17(2) 0.063(10) 0.16(2) -0.001(12) 0.009(18) 0.018(12) Cl41 0.104(15) 0.109(16) 0.084(14) 0.006(12) 0.007(12) 0.017(13) C1 0.023(2) 0.0103(18) 0.015(2) 0.0003(15) -0.0110(17) -0.0004(16) C2 0.024(2) 0.0095(18) 0.015(2) -0.0025(15) -0.0112(17) -0.0001(16) C3 0.030(2) 0.0088(18) 0.014(2) -0.0045(15) -0.0157(18) 0.0064(16) C4 0.024(2) 0.014(2) 0.018(2) -0.0029(16) -0.0076(18) 0.0047(17) C5 0.022(2) 0.0114(19) 0.022(2) -0.0039(16) -0.0108(18) 0.0041(16) C6 0.022(2) 0.0100(18) 0.018(2) -0.0018(16) -0.0141(17) 0.0023(16) C7 0.023(2) 0.0107(19) 0.023(2) -0.0007(16) -0.0177(18) 0.0000(16) C8 0.031(2) 0.014(2) 0.013(2) 0.0010(16) -0.0180(18) -0.0016(17) C9 0.031(2) 0.013(2) 0.013(2) 0.0007(16) -0.0134(18) -0.0026(17) C10 0.028(2) 0.0066(17) 0.015(2) -0.0009(15) -0.0138(18) -0.0015(16) C11 0.023(2) 0.014(2) 0.015(2) 0.0025(16) -0.0057(17) -0.0037(16) C12 0.021(2) 0.0107(18) 0.019(2) 0.0021(16) -0.0086(17) -0.0046(16) C13 0.025(2) 0.0103(18) 0.018(2) -0.0005(16) -0.0154(18) -0.0013(16) C14 0.027(2) 0.0078(18) 0.020(2) 0.0006(16) -0.0164(18) -0.0018(16) C15 0.028(2) 0.0108(19) 0.016(2) -0.0062(16) -0.0166(18) 0.0002(17) C16 0.031(2) 0.0116(19) 0.016(2) -0.0041(16) -0.0143(18) 0.0056(17) C17 0.028(3) 0.026(3) 0.032(3) 0.005(2) -0.004(2) 0.008(2) C18 0.032(3) 0.029(3) 0.035(3) 0.011(2) -0.010(2) 0.002(2) C19 0.025(2) 0.026(2) 0.023(2) -0.0030(19) -0.0071(19) 0.0034(19) C20 0.022(2) 0.022(2) 0.026(2) -0.0036(19) -0.0067(19) 0.0005(18) C21 0.017(2) 0.020(2) 0.023(2) 0.0036(18) -0.0089(18) 0.0011(17) C22 0.024(2) 0.015(2) 0.026(2) -0.0016(18) -0.0112(19) 0.0022(17) C23 0.026(2) 0.013(2) 0.027(2) -0.0016(18) -0.0125(19) 0.0007(17) C24 0.018(2) 0.015(2) 0.023(2) -0.0001(17) -0.0142(18) 0.0001(16) C25 0.027(2) 0.012(2) 0.019(2) 0.0000(17) -0.0135(18) -0.0029(17) C26 0.031(2) 0.016(2) 0.014(2) 0.0027(16) -0.0164(18) -0.0045(18) C27 0.032(3) 0.018(2) 0.0110(19) 0.0029(16) -0.0143(18) -0.0051(18) C28 0.033(3) 0.022(2) 0.029(3) -0.007(2) -0.009(2) -0.008(2) C29 0.032(3) 0.027(3) 0.032(3) -0.012(2) -0.011(2) -0.003(2) C30 0.026(2) 0.025(2) 0.016(2) -0.0001(18) -0.0067(18) -0.0041(19) C31 0.025(2) 0.024(2) 0.021(2) 0.0020(19) -0.0074(19) 0.0019(19) C32 0.018(2) 0.022(2) 0.019(2) -0.0028(18) -0.0050(17) -0.0023(17) C33 0.022(2) 0.016(2) 0.020(2) 0.0017(17) -0.0083(18) -0.0038(17) C34 0.026(2) 0.015(2) 0.020(2) 0.0006(17) -0.0121(18) -0.0027(17) C35 0.021(2) 0.014(2) 0.016(2) -0.0005(16) -0.0147(17) -0.0001(16) C36 0.025(2) 0.0117(19) 0.018(2) -0.0032(16) -0.0148(18) 0.0028(16) C37 0.032(2) 0.0102(19) 0.014(2) -0.0008(16) -0.0132(18) 0.0039(17) C38 0.031(2) 0.014(2) 0.0099(19) -0.0008(15) -0.0103(17) 0.0028(17) C39 0.032(2) 0.016(2) 0.0088(19) -0.0018(16) -0.0096(17) 0.0013(18) C40 0.028(2) 0.022(2) 0.012(2) -0.0002(17) -0.0042(18) 0.0048(19) C41 0.028(2) 0.021(2) 0.022(2) 0.0005(19) -0.0019(19) 0.0057(19) C42 0.032(3) 0.027(3) 0.019(2) -0.001(2) -0.005(2) 0.004(2) C43 0.029(3) 0.023(2) 0.026(2) 0.001(2) -0.001(2) 0.005(2) C44 0.020(2) 0.018(2) 0.027(2) 0.0016(18) -0.0047(19) -0.0027(17) C45 0.013(2) 0.025(2) 0.027(2) 0.0003(19) -0.0055(18) -0.0020(17) C46 0.025(2) 0.017(2) 0.026(2) 0.0010(18) -0.0073(19) 0.0019(18) C47 0.022(2) 0.014(2) 0.023(2) 0.0001(17) -0.0151(18) -0.0016(16) C48 0.026(2) 0.018(2) 0.017(2) -0.0008(17) -0.0166(18) -0.0026(17) C49 0.029(2) 0.0144(19) 0.0131(19) -0.0038(16) -0.0146(17) -0.0042(17) C50 0.032(3) 0.021(2) 0.013(2) 0.0010(17) -0.0139(19) 0.0006(19) C51 0.033(3) 0.019(2) 0.013(2) -0.0015(17) -0.0100(19) -0.0011(19) C52 0.030(3) 0.020(2) 0.016(2) 0.0000(17) -0.0045(19) -0.0029(19) C53 0.036(3) 0.026(2) 0.014(2) -0.0003(18) -0.006(2) -0.002(2) C54 0.030(3) 0.026(3) 0.022(2) 0.003(2) -0.005(2) -0.004(2) C55 0.022(2) 0.018(2) 0.021(2) -0.0024(18) -0.0043(18) 0.0020(17) C56 0.017(2) 0.019(2) 0.021(2) -0.0002(17) -0.0047(17) 0.0002(16) C57 0.024(2) 0.016(2) 0.022(2) -0.0005(17) -0.0090(18) -0.0010(17) C58 0.021(2) 0.0126(19) 0.015(2) 0.0011(16) -0.0111(17) 0.0013(16) C59 0.025(2) 0.016(2) 0.0113(19) 0.0002(16) -0.0116(17) 0.0025(17) C60 0.028(2) 0.015(2) 0.0111(19) 0.0026(16) -0.0093(17) 0.0023(17) C61 0.027(2) 0.0107(18) 0.0102(18) 0.0042(15) -0.0086(17) 0.0003(16) C62 0.029(2) 0.014(2) 0.0126(19) 0.0017(16) -0.0066(17) -0.0023(17) C63 0.024(2) 0.0132(19) 0.017(2) 0.0041(16) -0.0071(17) -0.0015(16) C64 0.023(2) 0.0089(18) 0.019(2) 0.0012(16) -0.0059(17) -0.0019(16) C65 0.020(2) 0.0110(19) 0.021(2) 0.0017(16) -0.0105(17) -0.0041(16) C66 0.023(2) 0.0080(18) 0.023(2) -0.0012(16) -0.0113(18) -0.0037(16) C67 0.023(2) 0.0080(17) 0.0145(19) 0.0000(15) -0.0122(17) -0.0030(15) C68 0.034(3) 0.0063(17) 0.016(2) -0.0039(15) -0.0132(19) 0.0010(17) C69 0.035(3) 0.0075(18) 0.015(2) -0.0059(15) -0.0053(18) 0.0013(17) C70 0.028(2) 0.0119(19) 0.019(2) -0.0012(16) -0.0080(18) 0.0002(17) C71 0.024(2) 0.0077(17) 0.016(2) -0.0020(15) -0.0075(17) 0.0019(15) C72 0.022(2) 0.0133(19) 0.014(2) -0.0013(16) -0.0104(17) 0.0040(16) C73 0.021(2) 0.0080(18) 0.016(2) -0.0009(15) -0.0104(17) 0.0028(15) C74 0.022(2) 0.0069(17) 0.0122(19) -0.0004(14) -0.0094(16) 0.0023(15) C75 0.024(2) 0.0099(18) 0.015(2) 0.0002(15) -0.0093(17) -0.0002(16) C76 0.024(2) 0.0085(18) 0.0118(19) -0.0003(15) -0.0106(16) 0.0010(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C7 1.801(5) . ? Cl2 C8 1.798(4) . ? Cl3 C9 1.781(5) . ? Cl4 C14 1.803(4) . ? Cl5 C15 1.795(4) . ? Cl6 C16 1.784(5) . ? Cl7 C17 1.849(6) . ? Cl8 C18 1.902(7) . ? Cl9 C19 1.790(5) . ? Cl10 C20 1.818(5) . ? Cl11 C22 1.795(5) . ? Cl12 C23 1.796(5) . ? Cl1A Cl1B 0.530(6) . ? Cl1A C28 1.871(9) . ? Cl1B C28 1.832(9) . ? Cl1B Cl14 2.260(7) . ? Cl14 C29 1.910(7) . ? Cl15 C30 1.789(5) . ? Cl16 Cl35 1.46(4) . ? Cl16 C31 1.826(6) . ? Cl17 C33 1.793(5) . ? Cl18 C34 1.794(5) . ? Cl19 C39 1.785(4) . ? Cl20 C40 1.789(5) . ? Cl21 C43 1.847(6) . ? Cl22 C44 1.798(5) . ? Cl23 C46 1.812(5) . ? Cl24 C47 1.787(5) . ? Cl25 C48 1.803(5) . ? Cl26 C49 1.806(4) . ? Cl27 C50 1.786(5) . ? Cl28 C51 1.794(5) . ? Cl29 Cl36 1.576(12) . ? Cl29 C54 1.868(6) . ? Cl29 Cl39 2.10(2) . ? Cl29 Cl35 2.37(3) . ? Cl30 C55 1.805(5) . ? Cl31 C57 1.815(5) . ? Cl32 C58 1.791(4) . ? Cl33 C59 1.801(4) . ? Cl34 C60 1.812(5) . ? Cl35 C53 2.26(3) . ? Cl36 Cl37 1.937(17) . ? Cl38 Cl41 0.92(3) . ? Cl38 Cl40 1.38(3) . ? Cl39 C70 2.098(18) . ? Cl40 Cl41 1.91(4) . ? C1 C6 1.399(6) . ? C1 C10 1.418(7) . ? C1 C2 1.425(6) . ? C2 C13 1.402(7) . ? C2 C3 1.430(7) . ? C3 C4 1.377(7) . ? C3 C16 1.524(6) . ? C4 C5 1.414(6) . ? C4 C19 1.501(7) . ? C5 C6 1.363(7) . ? C5 C22 1.516(7) . ? C6 C7 1.481(6) . ? C7 C8 1.549(7) . ? C7 C23 1.591(7) . ? C8 C26 1.482(6) . ? C8 C9 1.580(7) . ? C9 C10 1.526(6) . ? C9 C28 1.594(7) . ? C10 C11 1.387(7) . ? C11 C12 1.412(6) . ? C11 C30 1.503(7) . ? C12 C13 1.360(7) . ? C12 C33 1.506(6) . ? C13 C14 1.472(6) . ? C14 C15 1.546(7) . ? C14 C34 1.594(7) . ? C15 C37 1.494(6) . ? C15 C16 1.585(7) . ? C16 C17 1.586(7) . ? C17 C38 1.492(7) . ? C17 C18 1.513(8) . ? C18 C41 1.440(8) . ? C18 C19 1.550(7) . ? C19 C20 1.615(7) . ? C20 C42 1.493(7) . ? C20 C21 1.535(7) . ? C21 C45 1.348(7) . ? C21 C22 1.531(7) . ? C22 C23 1.586(7) . ? C23 C24 1.490(6) . ? C24 C25 1.329(7) . ? C24 C46 1.491(7) . ? C25 C26 1.409(7) . ? C25 C48 1.489(6) . ? C26 C27 1.348(8) . ? C27 C50 1.495(7) . ? C27 C28 1.499(7) . ? C28 C29 1.516(8) . ? C29 C52 1.430(8) . ? C29 C30 1.544(7) . ? C30 C31 1.602(7) . ? C31 C53 1.500(7) . ? C31 C32 1.547(7) . ? C32 C56 1.340(7) . ? C32 C33 1.536(7) . ? C33 C34 1.584(7) . ? C34 C35 1.487(6) . ? C35 C36 1.333(7) . ? C35 C57 1.486(7) . ? C36 C37 1.399(7) . ? C36 C59 1.483(6) . ? C37 C38 1.344(7) . ? C38 C39 1.498(6) . ? C39 C40 1.593(7) . ? C39 C60 1.613(7) . ? C40 C62 1.498(6) . ? C40 C41 1.516(7) . ? C41 C42 1.391(7) . ? C42 C43 1.453(8) . ? C43 C63 1.488(7) . ? C43 C44 1.576(7) . ? C44 C45 1.519(7) . ? C44 C65 1.522(7) . ? C45 C46 1.544(7) . ? C46 C47 1.625(7) . ? C47 C66 1.506(6) . ? C47 C48 1.574(7) . ? C48 C49 1.557(7) . ? C49 C68 1.496(6) . ? C49 C50 1.620(7) . ? C50 C51 1.587(7) . ? C51 C69 1.491(7) . ? C51 C52 1.509(7) . ? C52 C53 1.390(7) . ? C53 C54 1.441(7) . ? C54 C70 1.483(7) . ? C54 C55 1.571(7) . ? C55 C72 1.505(7) . ? C55 C56 1.516(6) . ? C56 C57 1.532(7) . ? C57 C58 1.627(7) . ? C58 C73 1.507(6) . ? C58 C59 1.568(6) . ? C59 C60 1.562(7) . ? C60 C61 1.484(6) . ? C61 C62 1.367(7) . ? C61 C74 1.404(6) . ? C62 C63 1.389(6) . ? C63 C64 1.388(7) . ? C64 C75 1.400(7) . ? C64 C65 1.415(6) . ? C65 C66 1.370(7) . ? C66 C67 1.422(7) . ? C67 C68 1.405(7) . ? C67 C76 1.444(6) . ? C68 C69 1.363(7) . ? C69 C70 1.398(7) . ? C70 C71 1.388(7) . ? C71 C76 1.398(7) . ? C71 C72 1.426(6) . ? C72 C73 1.375(6) . ? C73 C74 1.432(7) . ? C74 C75 1.446(6) . ? C75 C76 1.411(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 Cl1B Cl1A C28 77.7(14) . . ? Cl1A Cl1B C28 85.9(14) . . ? Cl1A Cl1B Cl14 168.2(16) . . ? C28 Cl1B Cl14 82.3(3) . . ? C29 Cl14 Cl1B 74.7(3) . . ? Cl35 Cl16 C31 90.7(11) . . ? Cl36 Cl29 C54 164.9(5) . . ? Cl36 Cl29 Cl39 87.0(6) . . ? C54 Cl29 Cl39 78.4(5) . . ? Cl36 Cl29 Cl35 112.4(9) . . ? C54 Cl29 Cl35 80.3(8) . . ? Cl39 Cl29 Cl35 152.8(9) . . ? Cl16 Cl35 C53 88.9(15) . . ? Cl16 Cl35 Cl29 143(2) . . ? C53 Cl35 Cl29 69.5(9) . . ? Cl29 Cl36 Cl37 104.0(8) . . ? Cl41 Cl38 Cl40 111(3) . . ? C70 Cl39 Cl29 81.1(7) . . ? Cl38 Cl40 Cl41 26.7(14) . . ? Cl38 Cl41 Cl40 42(2) . . ? C6 C1 C10 121.0(4) . . ? C6 C1 C2 116.0(4) . . ? C10 C1 C2 122.3(4) . . ? C13 C2 C1 115.8(4) . . ? C13 C2 C3 121.4(4) . . ? C1 C2 C3 122.1(4) . . ? C4 C3 C2 118.6(4) . . ? C4 C3 C16 121.8(4) . . ? C2 C3 C16 119.6(4) . . ? C3 C4 C5 118.2(5) . . ? C3 C4 C19 123.9(4) . . ? C5 C4 C19 117.9(4) . . ? C6 C5 C4 122.5(4) . . ? C6 C5 C22 111.0(4) . . ? C4 C5 C22 125.3(5) . . ? C5 C6 C1 121.1(4) . . ? C5 C6 C7 113.0(4) . . ? C1 C6 C7 125.6(4) . . ? C6 C7 C8 112.0(4) . . ? C6 C7 C23 100.6(4) . . ? C8 C7 C23 117.4(4) . . ? C6 C7 Cl1 104.5(3) . . ? C8 C7 Cl1 110.6(3) . . ? C23 C7 Cl1 110.6(3) . . ? C26 C8 C7 113.0(4) . . ? C26 C8 C9 100.2(4) . . ? C7 C8 C9 117.9(4) . . ? C26 C8 Cl2 104.0(3) . . ? C7 C8 Cl2 108.7(3) . . ? C9 C8 Cl2 112.0(3) . . ? C10 C9 C8 113.1(4) . . ? C10 C9 C28 110.0(4) . . ? C8 C9 C28 103.8(4) . . ? C10 C9 Cl3 105.2(3) . . ? C8 C9 Cl3 112.2(3) . . ? C28 C9 Cl3 112.7(4) . . ? C11 C10 C1 118.5(4) . . ? C11 C10 C9 121.2(4) . . ? C1 C10 C9 120.3(4) . . ? C10 C11 C12 118.2(4) . . ? C10 C11 C30 124.3(4) . . ? C12 C11 C30 117.4(4) . . ? C13 C12 C11 122.2(4) . . ? C13 C12 C33 111.1(4) . . ? C11 C12 C33 125.6(4) . . ? C12 C13 C2 121.3(4) . . ? C12 C13 C14 113.2(4) . . ? C2 C13 C14 125.3(5) . . ? C13 C14 C15 112.7(4) . . ? C13 C14 C34 101.0(4) . . ? C15 C14 C34 117.7(4) . . ? C13 C14 Cl4 105.0(3) . . ? C15 C14 Cl4 109.5(3) . . ? C34 C14 Cl4 110.0(3) . . ? C37 C15 C14 112.7(4) . . ? C37 C15 C16 99.5(4) . . ? C14 C15 C16 117.8(4) . . ? C37 C15 Cl5 103.3(3) . . ? C14 C15 Cl5 109.6(3) . . ? C16 C15 Cl5 112.7(3) . . ? C3 C16 C15 113.4(4) . . ? C3 C16 C17 109.4(4) . . ? C15 C16 C17 103.9(4) . . ? C3 C16 Cl6 105.9(3) . . ? C15 C16 Cl6 111.9(3) . . ? C17 C16 Cl6 112.5(4) . . ? C38 C17 C18 111.2(5) . . ? C38 C17 C16 102.2(4) . . ? C18 C17 C16 118.1(4) . . ? C38 C17 Cl7 108.6(4) . . ? C18 C17 Cl7 108.3(4) . . ? C16 C17 Cl7 108.0(4) . . ? C41 C18 C17 116.0(5) . . ? C41 C18 C19 106.4(5) . . ? C17 C18 C19 119.5(5) . . ? C41 C18 Cl8 100.8(4) . . ? C17 C18 Cl8 105.9(4) . . ? C19 C18 Cl8 106.1(4) . . ? C4 C19 C18 110.5(4) . . ? C4 C19 C20 108.5(4) . . ? C18 C19 C20 105.0(4) . . ? C4 C19 Cl9 107.1(4) . . ? C18 C19 Cl9 110.4(4) . . ? C20 C19 Cl9 115.3(4) . . ? C42 C20 C21 111.6(4) . . ? C42 C20 C19 100.9(4) . . ? C21 C20 C19 118.0(4) . . ? C42 C20 Cl10 106.7(4) . . ? C21 C20 Cl10 107.9(3) . . ? C19 C20 Cl10 111.1(3) . . ? C45 C21 C22 123.4(5) . . ? C45 C21 C20 122.3(4) . . ? C22 C21 C20 113.6(4) . . ? C5 C22 C21 102.9(4) . . ? C5 C22 C23 102.4(4) . . ? C21 C22 C23 117.5(4) . . ? C5 C22 Cl11 112.6(3) . . ? C21 C22 Cl11 110.2(4) . . ? C23 C22 Cl11 110.7(3) . . ? C24 C23 C22 109.8(4) . . ? C24 C23 C7 111.5(4) . . ? C22 C23 C7 104.7(4) . . ? C24 C23 Cl12 105.1(3) . . ? C22 C23 Cl12 114.8(4) . . ? C7 C23 Cl12 111.1(3) . . ? C25 C24 C23 123.7(4) . . ? C25 C24 C46 112.4(4) . . ? C23 C24 C46 123.8(5) . . ? C24 C25 C26 123.4(4) . . ? C24 C25 C48 114.2(4) . . ? C26 C25 C48 122.1(5) . . ? C27 C26 C25 123.7(5) . . ? C27 C26 C8 114.0(4) . . ? C25 C26 C8 121.8(5) . . ? C26 C27 C50 123.3(5) . . ? C26 C27 C28 111.0(4) . . ? C50 C27 C28 125.7(5) . . ? C27 C28 C29 111.2(5) . . ? C27 C28 C9 102.0(4) . . ? C29 C28 C9 117.4(4) . . ? C27 C28 Cl1B 113.7(4) . . ? C29 C28 Cl1B 98.5(4) . . ? C9 C28 Cl1B 114.6(4) . . ? C27 C28 Cl1A 106.2(4) . . ? C29 C28 Cl1A 114.9(5) . . ? C9 C28 Cl1A 103.7(4) . . ? Cl1B C28 Cl1A 16.42(19) . . ? C52 C29 C28 116.6(5) . . ? C52 C29 C30 107.3(5) . . ? C28 C29 C30 120.2(5) . . ? C52 C29 Cl14 99.8(4) . . ? C28 C29 Cl14 104.2(4) . . ? C30 C29 Cl14 106.1(4) . . ? C11 C30 C29 110.0(4) . . ? C11 C30 C31 108.9(4) . . ? C29 C30 C31 104.7(4) . . ? C11 C30 Cl15 107.5(3) . . ? C29 C30 Cl15 110.1(4) . . ? C31 C30 Cl15 115.6(4) . . ? C53 C31 C32 111.5(4) . . ? C53 C31 C30 101.4(4) . . ? C32 C31 C30 117.8(4) . . ? C53 C31 Cl16 106.0(4) . . ? C32 C31 Cl16 108.0(3) . . ? C30 C31 Cl16 111.4(3) . . ? C56 C32 C33 124.4(4) . . ? C56 C32 C31 122.3(4) . . ? C33 C32 C31 112.8(4) . . ? C12 C33 C32 102.6(4) . . ? C12 C33 C34 102.8(4) . . ? C32 C33 C34 116.5(4) . . ? C12 C33 Cl17 112.9(3) . . ? C32 C33 Cl17 110.7(3) . . ? C34 C33 Cl17 110.8(3) . . ? C35 C34 C33 109.8(4) . . ? C35 C34 C14 110.8(4) . . ? C33 C34 C14 104.2(4) . . ? C35 C34 Cl18 105.8(3) . . ? C33 C34 Cl18 115.1(3) . . ? C14 C34 Cl18 111.2(3) . . ? C36 C35 C57 112.8(4) . . ? C36 C35 C34 123.7(4) . . ? C57 C35 C34 123.4(4) . . ? C35 C36 C37 124.2(4) . . ? C35 C36 C59 113.9(4) . . ? C37 C36 C59 121.8(5) . . ? C38 C37 C36 124.7(4) . . ? C38 C37 C15 113.7(4) . . ? C36 C37 C15 121.1(5) . . ? C37 C38 C17 111.3(4) . . ? C37 C38 C39 122.0(4) . . ? C17 C38 C39 126.7(5) . . ? C38 C39 C40 108.5(4) . . ? C38 C39 C60 112.5(4) . . ? C40 C39 C60 104.8(4) . . ? C38 C39 Cl19 106.1(3) . . ? C40 C39 Cl19 113.7(3) . . ? C60 C39 Cl19 111.4(3) . . ? C62 C40 C41 104.5(4) . . ? C62 C40 C39 102.2(4) . . ? C41 C40 C39 113.8(4) . . ? C62 C40 Cl20 112.2(3) . . ? C41 C40 Cl20 110.7(4) . . ? C39 C40 Cl20 112.9(3) . . ? C42 C41 C18 111.1(5) . . ? C42 C41 C40 122.2(5) . . ? C18 C41 C40 126.4(5) . . ? C41 C42 C43 122.6(5) . . ? C41 C42 C20 113.8(5) . . ? C43 C42 C20 123.0(5) . . ? C42 C43 C63 106.9(5) . . ? C42 C43 C44 116.1(4) . . ? C63 C43 C44 105.1(4) . . ? C42 C43 Cl21 106.0(4) . . ? C63 C43 Cl21 110.7(4) . . ? C44 C43 Cl21 112.0(4) . . ? C45 C44 C65 105.2(4) . . ? C45 C44 C43 115.4(4) . . ? C65 C44 C43 103.0(4) . . ? C45 C44 Cl22 110.0(3) . . ? C65 C44 Cl22 111.0(3) . . ? C43 C44 Cl22 111.8(4) . . ? C21 C45 C44 123.7(5) . . ? C21 C45 C46 121.9(5) . . ? C44 C45 C46 114.1(4) . . ? C24 C46 C45 108.2(4) . . ? C24 C46 C47 101.6(4) . . ? C45 C46 C47 117.6(4) . . ? C24 C46 Cl23 110.7(3) . . ? C45 C46 Cl23 108.0(3) . . ? C47 C46 Cl23 110.6(3) . . ? C66 C47 C48 112.6(4) . . ? C66 C47 C46 108.8(4) . . ? C48 C47 C46 104.2(4) . . ? C66 C47 Cl24 105.9(3) . . ? C48 C47 Cl24 110.7(3) . . ? C46 C47 Cl24 114.7(3) . . ? C25 C48 C49 112.7(4) . . ? C25 C48 C47 100.6(4) . . ? C49 C48 C47 118.6(4) . . ? C25 C48 Cl25 103.1(3) . . ? C49 C48 Cl25 109.1(3) . . ? C47 C48 Cl25 111.6(3) . . ? C68 C49 C48 112.8(4) . . ? C68 C49 C50 100.7(4) . . ? C48 C49 C50 117.6(4) . . ? C68 C49 Cl26 104.0(3) . . ? C48 C49 Cl26 110.1(3) . . ? C50 C49 Cl26 110.6(3) . . ? C27 C50 C51 109.0(4) . . ? C27 C50 C49 111.7(4) . . ? C51 C50 C49 105.1(4) . . ? C27 C50 Cl27 106.3(3) . . ? C51 C50 Cl27 114.0(4) . . ? C49 C50 Cl27 110.8(3) . . ? C69 C51 C52 104.9(4) . . ? C69 C51 C50 102.3(4) . . ? C52 C51 C50 114.4(4) . . ? C69 C51 Cl28 111.4(3) . . ? C52 C51 Cl28 110.6(4) . . ? C50 C51 Cl28 112.7(3) . . ? C53 C52 C29 110.9(5) . . ? C53 C52 C51 122.2(4) . . ? C29 C52 C51 126.4(5) . . ? C52 C53 C54 122.9(5) . . ? C52 C53 C31 113.2(5) . . ? C54 C53 C31 122.9(4) . . ? C52 C53 Cl35 111.7(11) . . ? C54 C53 Cl35 93.7(9) . . ? C31 C53 Cl35 74.4(10) . . ? C53 C54 C70 108.2(5) . . ? C53 C54 C55 117.4(4) . . ? C70 C54 C55 105.7(4) . . ? C53 C54 Cl29 104.9(4) . . ? C70 C54 Cl29 108.6(4) . . ? C55 C54 Cl29 111.8(4) . . ? C72 C55 C56 106.0(4) . . ? C72 C55 C54 102.8(4) . . ? C56 C55 C54 114.9(4) . . ? C72 C55 Cl30 110.6(3) . . ? C56 C55 Cl30 110.6(3) . . ? C54 C55 Cl30 111.4(3) . . ? C32 C56 C55 124.0(4) . . ? C32 C56 C57 121.1(4) . . ? C55 C56 C57 114.5(4) . . ? C35 C57 C56 108.6(4) . . ? C35 C57 C58 101.1(4) . . ? C56 C57 C58 117.2(4) . . ? C35 C57 Cl31 111.0(3) . . ? C56 C57 Cl31 107.9(3) . . ? C58 C57 Cl31 110.9(3) . . ? C73 C58 C59 112.7(4) . . ? C73 C58 C57 109.1(4) . . ? C59 C58 C57 104.5(4) . . ? C73 C58 Cl32 106.9(3) . . ? C59 C58 Cl32 110.4(3) . . ? C57 C58 Cl32 113.4(3) . . ? C36 C59 C60 112.8(4) . . ? C36 C59 C58 100.6(4) . . ? C60 C59 C58 118.4(4) . . ? C36 C59 Cl33 102.6(3) . . ? C60 C59 Cl33 109.6(3) . . ? C58 C59 Cl33 111.5(3) . . ? C61 C60 C59 112.9(4) . . ? C61 C60 C39 101.5(4) . . ? C59 C60 C39 116.8(4) . . ? C61 C60 Cl34 104.6(3) . . ? C59 C60 Cl34 109.9(3) . . ? C39 C60 Cl34 110.2(3) . . ? C62 C61 C74 122.8(4) . . ? C62 C61 C60 111.7(4) . . ? C74 C61 C60 124.5(4) . . ? C61 C62 C63 121.5(4) . . ? C61 C62 C40 113.5(4) . . ? C63 C62 C40 120.5(4) . . ? C64 C63 C62 117.8(4) . . ? C64 C63 C43 110.9(4) . . ? C62 C63 C43 123.9(4) . . ? C63 C64 C75 122.1(4) . . ? C63 C64 C65 110.9(4) . . ? C75 C64 C65 122.2(4) . . ? C66 C65 C64 121.2(4) . . ? C66 C65 C44 126.1(4) . . ? C64 C65 C44 109.8(4) . . ? C65 C66 C67 118.3(4) . . ? C65 C66 C47 118.7(4) . . ? C67 C66 C47 122.7(4) . . ? C68 C67 C66 121.6(4) . . ? C68 C67 C76 115.4(4) . . ? C66 C67 C76 120.6(4) . . ? C69 C68 C67 123.9(4) . . ? C69 C68 C49 111.4(4) . . ? C67 C68 C49 123.8(5) . . ? C68 C69 C70 120.3(4) . . ? C68 C69 C51 113.9(4) . . ? C70 C69 C51 121.1(5) . . ? C71 C70 C69 118.5(5) . . ? C71 C70 C54 110.4(4) . . ? C69 C70 C54 123.0(4) . . ? C71 C70 Cl39 107.8(6) . . ? C69 C70 Cl39 102.9(6) . . ? C54 C70 Cl39 87.6(7) . . ? C70 C71 C76 121.8(4) . . ? C70 C71 C72 110.4(4) . . ? C76 C71 C72 122.8(4) . . ? C73 C72 C71 120.7(4) . . ? C73 C72 C55 125.7(4) . . ? C71 C72 C55 110.3(4) . . ? C72 C73 C74 118.1(4) . . ? C72 C73 C58 118.7(4) . . ? C74 C73 C58 122.8(4) . . ? C61 C74 C73 120.8(4) . . ? C61 C74 C75 116.0(4) . . ? C73 C74 C75 120.7(4) . . ? C64 C75 C76 117.2(4) . . ? C64 C75 C74 119.6(4) . . ? C76 C75 C74 120.2(4) . . ? C71 C76 C75 117.0(4) . . ? C71 C76 C67 120.1(4) . . ? C75 C76 C67 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.016 _refine_diff_density_min -1.113 _refine_diff_density_rms 0.154 # Attachment '- c76cl-VIa_805565.CIF' data_x76pcl1 _database_code_depnum_ccdc_archive 'CCDC 805565' #TrackingRef '- c76cl-VIa_805565.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 Cl33.25 O1.32 P1.32' _chemical_formula_weight 2153.59 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.6310(10) _cell_length_b 27.894(2) _cell_length_c 11.5340(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.380(10) _cell_angle_gamma 90.00 _cell_volume 7126.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4207 _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20367 _diffrn_reflns_av_R_equivalents 0.3050 _diffrn_reflns_av_sigmaI/netI 0.3411 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 35.46 _reflns_number_total 7346 _reflns_number_gt 2322 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ADP of two Cl atoms were restrained by ISOR. ; _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^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7346 _refine_ls_number_parameters 534 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.3342 _refine_ls_R_factor_gt 0.1170 _refine_ls_wR_factor_ref 0.2826 _refine_ls_wR_factor_gt 0.2498 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.5513(2) 0.46094(14) 0.3720(4) 0.0726(13) Uani 1 1 d . . . Cl2 Cl 0.4787(2) 0.43032(14) 0.5258(4) 0.0657(13) Uani 1 1 d . . . Cl3 Cl 0.3582(2) 0.42425(13) 0.3113(4) 0.0632(12) Uani 1 1 d . . . Cl4 Cl 0.30793(19) 0.34242(14) 0.4162(3) 0.0550(11) Uani 1 1 d . . . Cl5 Cl 0.41775(18) 0.33282(14) 0.6496(3) 0.0532(10) Uani 1 1 d . . . Cl6 Cl 0.39750(19) 0.22884(14) 0.6638(3) 0.0586(11) Uani 1 1 d . . . Cl7 Cl 0.2910(2) 0.21052(16) 0.4404(3) 0.0652(12) Uani 1 1 d . . . Cl8 Cl 0.42873(17) 0.11386(13) 0.6181(3) 0.0461(10) Uani 1 1 d . . . Cl9 Cl 0.5492(2) 0.00609(12) 0.3734(3) 0.0552(11) Uani 1 1 d . . . Cl10 Cl 0.64482(19) 0.04409(12) 0.1962(3) 0.0528(10) Uani 1 1 d . . . Cl11 Cl 0.7528(2) 0.15178(16) 0.3461(4) 0.0680(12) Uani 1 1 d . . . Cl12 Cl 0.59954(18) 0.08521(12) 0.6389(3) 0.0474(10) Uani 1 1 d . . . Cl13 Cl 0.7189(2) 0.11389(16) 0.5527(3) 0.0650(12) Uani 1 1 d . . . Cl14 Cl 0.70701(19) 0.20971(15) 0.6591(3) 0.0561(11) Uani 1 1 d . . . Cl15 Cl 0.3479(4) 0.4443(3) 0.6521(8) 0.078(3) Uani 0.662(10) 1 d P . . Cl16 Cl 0.2956(4) 0.5189(3) 0.4475(6) 0.081(3) Uani 0.662(10) 1 d P . . Cl17 Cl 0.2162(4) 0.4356(3) 0.4580(9) 0.095(3) Uani 0.662(10) 1 d P . . Cl19 Cl 0.372(3) 0.437(2) 0.759(5) 0.29(3) Uani 0.32(2) 1 d PU . . Cl20 Cl 0.248(2) 0.4236(17) 0.567(5) 0.24(2) Uani 0.32(2) 1 d PU . . P P 0.2745(3) 0.4806(2) 0.5688(7) 0.063(2) Uani 0.662(10) 1 d P . . O O 0.2532(7) 0.5071(5) 0.6509(14) 0.055(4) Uani 0.662(10) 1 d P . . C1 C 0.5162(8) 0.4043(5) 0.3210(14) 0.055(4) Uani 1 1 d . . . C2 C 0.4727(9) 0.3870(5) 0.4082(14) 0.059(5) Uani 1 1 d . . . C3 C 0.4071(7) 0.3733(5) 0.3398(13) 0.052(4) Uani 1 1 d . . . C4 C 0.3767(8) 0.3276(5) 0.3940(13) 0.058(5) Uani 1 1 d . . . C5 C 0.4215(7) 0.3028(5) 0.5162(12) 0.050(4) Uani 1 1 d . . . C6 C 0.4123(7) 0.2436(4) 0.5268(12) 0.043(4) Uani 1 1 d . . . C7 C 0.3638(6) 0.2161(5) 0.4140(10) 0.044(4) Uani 1 1 d . . . C8 C 0.3839(6) 0.1664(5) 0.3967(10) 0.033(3) Uani 1 1 d . . . C9 C 0.4422(7) 0.1426(5) 0.4873(11) 0.041(4) Uani 1 1 d . . . C10 C 0.4543(7) 0.1037(4) 0.4052(10) 0.035(3) Uani 1 1 d . . . C11 C 0.5087(6) 0.0920(5) 0.4105(11) 0.037(3) Uani 1 1 d . . . C12 C 0.5257(7) 0.0653(4) 0.3151(10) 0.036(3) Uani 1 1 d . . . C13 C 0.5797(6) 0.0915(4) 0.3153(10) 0.034(3) Uani 1 1 d . . . C14 C 0.6010(6) 0.0953(5) 0.2061(10) 0.035(3) Uani 1 1 d . . . C15 C 0.6325(6) 0.1424(5) 0.2093(11) 0.040(4) Uani 1 1 d . . . C16 C 0.6745(7) 0.1648(5) 0.3316(10) 0.043(4) Uani 1 1 d . . . C17 C 0.6638(6) 0.2174(5) 0.3153(10) 0.034(3) Uani 1 1 d . . . C18 C 0.6490(6) 0.2431(4) 0.2038(11) 0.036(3) Uani 1 1 d . . . C19 C 0.6399(6) 0.2912(5) 0.2106(10) 0.039(3) Uani 1 1 d . . . C20 C 0.6313(7) 0.3114(5) 0.3153(11) 0.043(4) Uani 1 1 d . . . C21 C 0.5975(8) 0.3538(5) 0.2853(13) 0.052(4) Uani 1 1 d . . . C22 C 0.5636(7) 0.3671(5) 0.3548(11) 0.044(4) Uani 1 1 d . . . C23 C 0.5617(7) 0.3361(5) 0.4512(11) 0.040(3) Uani 1 1 d . . . C24 C 0.5080(7) 0.3432(4) 0.4699(11) 0.038(3) Uani 1 1 d . . . C25 C 0.4824(7) 0.3065(5) 0.5154(11) 0.041(4) Uani 1 1 d . . . C26 C 0.5138(6) 0.2623(5) 0.5419(11) 0.036(3) Uani 1 1 d . . . C27 C 0.4755(7) 0.2259(5) 0.5428(10) 0.043(4) Uani 1 1 d . . . C28 C 0.4904(6) 0.1774(4) 0.5279(9) 0.032(3) Uani 1 1 d . . . C29 C 0.5501(6) 0.1680(5) 0.5254(9) 0.034(3) Uani 1 1 d . . . C30 C 0.5646(5) 0.1185(5) 0.4962(9) 0.030(3) Uani 1 1 d . . . C31 C 0.6055(6) 0.1200(4) 0.4190(9) 0.029(3) Uani 1 1 d . . . C32 C 0.6582(6) 0.1505(5) 0.4481(10) 0.039(3) Uani 1 1 d . . . C33 C 0.6507(7) 0.1979(5) 0.5097(11) 0.043(4) Uani 1 1 d . . . C34 C 0.6558(6) 0.2364(5) 0.4189(10) 0.036(3) Uani 1 1 d . . . C35 C 0.6326(6) 0.2819(5) 0.4143(10) 0.034(3) Uani 1 1 d . . . C36 C 0.5945(6) 0.2935(5) 0.4832(10) 0.035(3) Uani 1 1 d . . . C37 C 0.5704(7) 0.2540(5) 0.5303(10) 0.044(4) Uani 1 1 d . . . C38 C 0.5905(6) 0.2056(5) 0.5268(9) 0.031(3) 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 Cl1 0.098(4) 0.040(2) 0.087(3) -0.013(2) 0.042(3) -0.007(3) Cl2 0.087(3) 0.042(2) 0.073(3) -0.024(2) 0.034(3) -0.003(2) Cl3 0.079(3) 0.039(2) 0.077(3) 0.005(2) 0.035(2) 0.023(2) Cl4 0.064(3) 0.053(2) 0.049(2) -0.0051(18) 0.0211(19) 0.016(2) Cl5 0.063(3) 0.057(2) 0.0415(18) -0.0131(17) 0.0210(19) 0.006(2) Cl6 0.083(3) 0.064(3) 0.0383(17) -0.0035(18) 0.033(2) 0.007(2) Cl7 0.079(3) 0.075(3) 0.047(2) -0.003(2) 0.029(2) -0.003(3) Cl8 0.065(3) 0.050(2) 0.0280(15) 0.0093(15) 0.0223(17) 0.002(2) Cl9 0.085(3) 0.035(2) 0.054(2) 0.0078(18) 0.035(2) 0.007(2) Cl10 0.076(3) 0.039(2) 0.0520(19) -0.0040(17) 0.033(2) 0.008(2) Cl11 0.075(3) 0.076(3) 0.059(2) -0.005(2) 0.031(2) 0.003(3) Cl12 0.069(3) 0.046(2) 0.0282(15) 0.0129(15) 0.0183(16) 0.021(2) Cl13 0.076(3) 0.069(3) 0.047(2) 0.006(2) 0.018(2) 0.022(3) Cl14 0.057(2) 0.076(3) 0.0317(16) -0.0060(18) 0.0113(17) 0.001(2) Cl15 0.092(6) 0.052(4) 0.091(5) 0.003(4) 0.034(5) 0.005(4) Cl16 0.091(6) 0.101(6) 0.060(4) -0.008(4) 0.037(4) 0.013(5) Cl17 0.066(5) 0.098(6) 0.122(7) -0.056(5) 0.035(5) -0.008(5) Cl19 0.30(3) 0.27(3) 0.29(3) -0.062(18) 0.11(2) 0.028(18) Cl20 0.24(3) 0.24(3) 0.25(3) -0.018(17) 0.112(19) 0.031(17) P 0.066(5) 0.043(4) 0.091(5) -0.021(4) 0.042(4) -0.005(4) O 0.070(11) 0.032(8) 0.078(10) -0.019(8) 0.045(9) -0.012(8) C1 0.069(12) 0.022(8) 0.081(10) -0.010(7) 0.035(10) 0.005(9) C2 0.094(14) 0.026(8) 0.072(10) -0.010(8) 0.046(10) -0.002(10) C3 0.060(11) 0.042(9) 0.052(8) 0.003(7) 0.017(8) -0.015(9) C4 0.103(14) 0.040(9) 0.049(8) 0.005(7) 0.050(9) 0.016(10) C5 0.055(10) 0.058(10) 0.043(8) -0.005(7) 0.025(8) 0.013(9) C6 0.064(11) 0.022(7) 0.053(8) -0.009(6) 0.031(8) 0.009(8) C7 0.046(9) 0.056(10) 0.021(6) 0.001(6) 0.000(6) 0.013(8) C8 0.038(8) 0.038(8) 0.024(6) 0.000(6) 0.011(6) -0.006(7) C9 0.049(9) 0.048(9) 0.030(6) 0.001(6) 0.020(7) 0.001(8) C10 0.051(10) 0.019(7) 0.026(6) 0.005(5) 0.002(6) -0.009(7) C11 0.040(9) 0.029(8) 0.044(7) 0.017(6) 0.017(7) 0.009(7) C12 0.051(9) 0.034(7) 0.026(6) 0.000(5) 0.016(6) 0.001(8) C13 0.048(9) 0.027(7) 0.027(6) 0.002(5) 0.011(6) 0.013(7) C14 0.029(8) 0.043(9) 0.030(6) -0.004(6) 0.006(6) 0.006(7) C15 0.054(10) 0.044(8) 0.031(6) -0.006(6) 0.025(7) -0.010(8) C16 0.056(10) 0.048(9) 0.020(6) -0.010(6) 0.007(6) -0.011(8) C17 0.032(8) 0.045(9) 0.025(6) -0.007(6) 0.010(6) -0.001(7) C18 0.048(9) 0.030(8) 0.035(7) 0.001(6) 0.020(7) -0.006(8) C19 0.039(8) 0.044(9) 0.030(6) 0.005(6) 0.008(6) -0.007(8) C20 0.055(10) 0.041(9) 0.033(7) 0.001(6) 0.013(7) -0.011(8) C21 0.085(12) 0.033(9) 0.050(8) -0.007(7) 0.038(9) -0.013(9) C22 0.067(11) 0.024(8) 0.037(7) -0.019(6) 0.014(7) -0.021(8) C23 0.054(10) 0.027(8) 0.042(7) -0.013(6) 0.019(7) -0.001(8) C24 0.052(9) 0.017(7) 0.036(7) -0.004(6) 0.003(7) 0.003(7) C25 0.056(10) 0.033(8) 0.030(6) -0.019(6) 0.010(7) -0.003(8) C26 0.050(9) 0.028(8) 0.033(6) -0.005(6) 0.020(7) 0.013(8) C27 0.057(10) 0.058(10) 0.018(6) -0.006(6) 0.017(6) -0.001(9) C28 0.052(9) 0.030(8) 0.020(6) 0.004(5) 0.018(6) 0.009(8) C29 0.046(9) 0.043(8) 0.011(5) 0.006(5) 0.007(6) 0.009(7) C30 0.022(7) 0.043(9) 0.021(5) 0.003(6) 0.001(5) 0.000(7) C31 0.036(8) 0.030(7) 0.016(5) 0.008(5) 0.003(5) 0.017(7) C32 0.041(8) 0.049(9) 0.027(6) -0.003(6) 0.010(6) -0.007(8) C33 0.074(11) 0.032(8) 0.028(6) -0.001(6) 0.022(7) 0.005(8) C34 0.033(8) 0.043(9) 0.033(6) -0.008(6) 0.012(6) -0.011(7) C35 0.030(8) 0.037(8) 0.028(6) -0.005(6) 0.002(6) -0.010(7) C36 0.040(8) 0.037(8) 0.024(6) -0.017(6) 0.005(6) -0.011(7) C37 0.064(11) 0.049(9) 0.013(5) -0.011(6) 0.005(6) -0.002(8) C38 0.043(8) 0.041(8) 0.006(4) 0.001(5) 0.004(5) 0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C1 1.787(16) . ? Cl2 C2 1.786(14) . ? Cl3 C3 1.789(17) . ? Cl4 C4 1.779(16) . ? Cl5 C5 1.779(12) . ? Cl6 C6 1.782(12) . ? Cl7 C7 1.855(14) . ? Cl8 C9 1.830(11) . ? Cl9 C12 1.796(13) . ? Cl10 C14 1.791(13) . ? Cl11 C16 1.836(15) . ? Cl12 C30 1.818(11) . ? Cl13 C32 1.829(14) . ? Cl14 C33 1.804(15) . ? Cl15 Cl19 1.18(6) . ? Cl15 P 1.948(11) . ? Cl15 Cl20 2.30(5) . ? Cl16 P 1.958(9) . ? Cl17 Cl20 1.27(5) . ? Cl17 P 1.968(11) . ? Cl20 P 1.71(5) . ? P O 1.424(13) . ? C1 C22 1.48(2) . ? C1 C1 1.55(3) 2_655 ? C1 C2 1.738(19) . ? C2 C24 1.51(2) . ? C2 C3 1.52(2) . ? C3 C21 1.509(19) 2_655 ? C3 C4 1.686(19) . ? C4 C19 1.520(19) 2_655 ? C4 C5 1.60(2) . ? C5 C25 1.45(2) . ? C5 C6 1.677(19) . ? C6 C27 1.52(2) . ? C6 C7 1.60(2) . ? C7 C18 1.490(17) 2_655 ? C7 C8 1.499(19) . ? C8 C15 1.329(17) 2_655 ? C8 C9 1.559(19) . ? C9 C28 1.446(19) . ? C9 C10 1.532(17) . ? C10 C11 1.308(18) . ? C10 C14 1.496(18) 2_655 ? C11 C12 1.495(16) . ? C11 C30 1.537(18) . ? C12 C13 1.470(19) . ? C12 C12 1.57(3) 2_655 ? C13 C31 1.390(17) . ? C13 C14 1.513(15) . ? C14 C10 1.496(18) 2_655 ? C14 C15 1.505(18) . ? C15 C8 1.329(17) 2_655 ? C15 C16 1.547(18) . ? C16 C17 1.488(19) . ? C16 C32 1.573(15) . ? C17 C34 1.378(15) . ? C17 C18 1.406(16) . ? C18 C19 1.366(18) . ? C18 C7 1.490(17) 2_655 ? C19 C20 1.410(16) . ? C19 C4 1.520(19) 2_655 ? C20 C35 1.399(17) . ? C20 C21 1.40(2) . ? C21 C22 1.367(18) . ? C21 C3 1.509(19) 2_655 ? C22 C23 1.421(18) . ? C23 C24 1.374(18) . ? C23 C36 1.399(19) . ? C24 C25 1.382(18) . ? C25 C26 1.415(18) . ? C26 C27 1.365(18) . ? C26 C37 1.408(19) . ? C27 C28 1.422(18) . ? C28 C29 1.446(18) . ? C29 C38 1.414(18) . ? C29 C30 1.489(17) . ? C30 C31 1.525(14) . ? C31 C32 1.448(18) . ? C32 C33 1.540(18) . ? C33 C38 1.518(19) . ? C33 C34 1.535(17) . ? C34 C35 1.375(18) . ? C35 C36 1.429(16) . ? C36 C37 1.431(18) . ? C37 C38 1.436(18) . ? 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 Cl19 Cl15 P 128(3) . . ? Cl19 Cl15 Cl20 117(3) . . ? P Cl15 Cl20 46.5(12) . . ? Cl20 Cl17 P 59(2) . . ? Cl17 Cl20 P 81(3) . . ? Cl17 Cl20 Cl15 121(3) . . ? P Cl20 Cl15 55.9(15) . . ? O P Cl20 105.9(14) . . ? O P Cl15 113.7(9) . . ? Cl20 P Cl15 77.6(18) . . ? O P Cl16 115.3(7) . . ? Cl20 P Cl16 133.5(15) . . ? Cl15 P Cl16 103.4(4) . . ? O P Cl17 115.7(8) . . ? Cl20 P Cl17 39.5(17) . . ? Cl15 P Cl17 106.9(5) . . ? Cl16 P Cl17 100.3(5) . . ? C22 C1 C1 109.2(10) . 2_655 ? C22 C1 C2 101.5(11) . . ? C1 C1 C2 116.0(16) 2_655 . ? C22 C1 Cl1 108.1(11) . . ? C1 C1 Cl1 110.5(6) 2_655 . ? C2 C1 Cl1 110.9(8) . . ? C24 C2 C3 109.7(12) . . ? C24 C2 C1 99.0(11) . . ? C3 C2 C1 118.0(12) . . ? C24 C2 Cl2 107.8(11) . . ? C3 C2 Cl2 111.1(11) . . ? C1 C2 Cl2 110.2(10) . . ? C21 C3 C2 107.9(12) 2_655 . ? C21 C3 C4 100.6(11) 2_655 . ? C2 C3 C4 119.0(12) . . ? C21 C3 Cl3 106.5(10) 2_655 . ? C2 C3 Cl3 111.8(10) . . ? C4 C3 Cl3 109.7(10) . . ? C19 C4 C5 108.7(11) 2_655 . ? C19 C4 C3 103.6(9) 2_655 . ? C5 C4 C3 114.7(14) . . ? C19 C4 Cl4 105.8(12) 2_655 . ? C5 C4 Cl4 109.3(8) . . ? C3 C4 Cl4 114.0(10) . . ? C25 C5 C4 108.6(11) . . ? C25 C5 C6 102.9(11) . . ? C4 C5 C6 115.4(12) . . ? C25 C5 Cl5 108.8(10) . . ? C4 C5 Cl5 110.1(9) . . ? C6 C5 Cl5 110.7(8) . . ? C27 C6 C7 109.8(9) . . ? C27 C6 C5 100.6(11) . . ? C7 C6 C5 119.2(11) . . ? C27 C6 Cl6 107.7(9) . . ? C7 C6 Cl6 107.7(9) . . ? C5 C6 Cl6 111.2(7) . . ? C18 C7 C8 108.6(9) 2_655 . ? C18 C7 C6 111.1(12) 2_655 . ? C8 C7 C6 112.4(11) . . ? C18 C7 Cl7 106.6(9) 2_655 . ? C8 C7 Cl7 107.4(10) . . ? C6 C7 Cl7 110.5(7) . . ? C15 C8 C7 125.8(12) 2_655 . ? C15 C8 C9 107.9(11) 2_655 . ? C7 C8 C9 123.5(10) . . ? C28 C9 C10 112.3(10) . . ? C28 C9 C8 110.0(11) . . ? C10 C9 C8 101.5(10) . . ? C28 C9 Cl8 111.8(8) . . ? C10 C9 Cl8 108.9(9) . . ? C8 C9 Cl8 111.9(8) . . ? C11 C10 C14 123.5(11) . 2_655 ? C11 C10 C9 122.7(13) . . ? C14 C10 C9 110.3(12) 2_655 . ? C10 C11 C12 127.0(13) . . ? C10 C11 C30 121.4(11) . . ? C12 C11 C30 108.9(11) . . ? C13 C12 C11 101.9(10) . . ? C13 C12 C12 112.6(9) . 2_655 ? C11 C12 C12 112.8(13) . 2_655 ? C13 C12 Cl9 107.5(10) . . ? C11 C12 Cl9 108.0(8) . . ? C12 C12 Cl9 113.2(4) 2_655 . ? C31 C13 C12 114.0(9) . . ? C31 C13 C14 120.2(12) . . ? C12 C13 C14 124.9(11) . . ? C10 C14 C15 99.3(11) 2_655 . ? C10 C14 C13 106.4(10) 2_655 . ? C15 C14 C13 110.2(9) . . ? C10 C14 Cl10 114.9(9) 2_655 . ? C15 C14 Cl10 113.9(9) . . ? C13 C14 Cl10 111.4(9) . . ? C8 C15 C14 115.8(12) 2_655 . ? C8 C15 C16 121.5(12) 2_655 . ? C14 C15 C16 122.1(10) . . ? C17 C16 C15 104.9(10) . . ? C17 C16 C32 106.1(10) . . ? C15 C16 C32 114.0(11) . . ? C17 C16 Cl11 109.2(9) . . ? C15 C16 Cl11 108.0(8) . . ? C32 C16 Cl11 114.2(9) . . ? C34 C17 C18 122.1(12) . . ? C34 C17 C16 109.8(10) . . ? C18 C17 C16 126.5(10) . . ? C19 C18 C17 116.2(10) . . ? C19 C18 C7 124.3(11) . 2_655 ? C17 C18 C7 118.9(12) . 2_655 ? C18 C19 C20 120.9(11) . . ? C18 C19 C4 127.8(11) . 2_655 ? C20 C19 C4 109.8(12) . 2_655 ? C35 C20 C21 123.1(12) . . ? C35 C20 C19 119.7(13) . . ? C21 C20 C19 111.4(11) . . ? C22 C21 C20 119.0(11) . . ? C22 C21 C3 126.9(15) . 2_655 ? C20 C21 C3 112.6(11) . 2_655 ? C21 C22 C23 118.5(13) . . ? C21 C22 C1 125.6(12) . . ? C23 C22 C1 113.9(11) . . ? C24 C23 C36 122.6(12) . . ? C24 C23 C22 108.6(13) . . ? C36 C23 C22 124.0(11) . . ? C23 C24 C25 120.2(12) . . ? C23 C24 C2 115.5(12) . . ? C25 C24 C2 122.4(14) . . ? C24 C25 C26 117.4(12) . . ? C24 C25 C5 128.4(13) . . ? C26 C25 C5 112.7(12) . . ? C27 C26 C37 122.1(12) . . ? C27 C26 C25 110.5(13) . . ? C37 C26 C25 124.6(12) . . ? C26 C27 C28 121.0(12) . . ? C26 C27 C6 112.5(12) . . ? C28 C27 C6 124.6(13) . . ? C27 C28 C29 117.4(12) . . ? C27 C28 C9 118.5(12) . . ? C29 C28 C9 122.5(11) . . ? C38 C29 C28 121.7(11) . . ? C38 C29 C30 118.8(10) . . ? C28 C29 C30 118.4(11) . . ? C29 C30 C31 110.4(9) . . ? C29 C30 C11 112.2(10) . . ? C31 C30 C11 102.4(9) . . ? C29 C30 Cl12 109.7(7) . . ? C31 C30 Cl12 111.3(8) . . ? C11 C30 Cl12 110.7(8) . . ? C13 C31 C32 128.3(10) . . ? C13 C31 C30 108.1(11) . . ? C32 C31 C30 123.4(10) . . ? C31 C32 C33 112.4(11) . . ? C31 C32 C16 113.5(10) . . ? C33 C32 C16 106.0(10) . . ? C31 C32 Cl13 103.9(9) . . ? C33 C32 Cl13 111.4(9) . . ? C16 C32 Cl13 109.7(9) . . ? C38 C33 C34 106.8(11) . . ? C38 C33 C32 116.5(12) . . ? C34 C33 C32 103.8(9) . . ? C38 C33 Cl14 105.2(7) . . ? C34 C33 Cl14 108.4(10) . . ? C32 C33 Cl14 115.6(10) . . ? C35 C34 C17 119.7(11) . . ? C35 C34 C33 123.2(9) . . ? C17 C34 C33 112.8(12) . . ? C34 C35 C20 117.9(11) . . ? C34 C35 C36 120.5(11) . . ? C20 C35 C36 118.8(13) . . ? C23 C36 C35 116.4(11) . . ? C23 C36 C37 119.8(12) . . ? C35 C36 C37 116.6(12) . . ? C26 C37 C36 115.2(12) . . ? C26 C37 C38 119.5(12) . . ? C36 C37 C38 122.2(11) . . ? C29 C38 C37 117.9(12) . . ? C29 C38 C33 123.5(11) . . ? C37 C38 C33 118.1(11) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.848 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.193