# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Tavarekere K Chandrashekar' _publ_contact_author_address ; Chemistry IIT Kanpur Kanpur Uttar Pradesh 208 016 INDIA ; _publ_contact_author_email TKC@IITK.AC.IN _publ_section_title ; Figure-Eight Aromatic Core-modified Octaphyrins With Six meso links: Syntheses and Structural Characterization ; loop_ _publ_author_name 'Tavarekere K. Chandrashekar' 'B. S. Joshi' 'Viswanathan PrabhuRaja' 'Harapriya Rath' 'Raja Roy' 'Jeyaraman Sankar' data_12maya _database_code_depnum_ccdc_archive 'CCDC 262999' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H56 Cl4 F10 N4 S4' _chemical_formula_weight 1581.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P12(1)/n1 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 18.713(4) _cell_length_b 13.740(3) _cell_length_c 29.251(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.38(3) _cell_angle_gamma 90.00 _cell_volume 7459(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4713 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 20.99 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3240 _exptl_absorpt_coefficient_mu 0.345 _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 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48863 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.32 _reflns_number_total 18441 _reflns_number_gt 10394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1251P)^2^+0.0755P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18441 _refine_ls_number_parameters 963 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2417 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.14522(5) 0.13885(6) 0.17397(3) 0.0219(2) Uani 1 1 d . . . S2 S 0.01372(5) 0.16544(7) 0.28488(4) 0.0285(2) Uani 1 1 d . . . S3 S -0.11887(5) 0.08200(7) 0.19828(4) 0.0299(2) Uani 1 1 d . . . S4 S 0.05834(5) -0.07353(7) 0.15065(4) 0.0278(2) Uani 1 1 d . . . Cl1 Cl 0.60918(14) 0.11884(15) 0.22810(7) 0.1139(8) Uani 1 1 d . . . Cl2 Cl 0.54002(11) -0.07018(12) 0.20831(7) 0.0898(6) Uani 1 1 d . . . Cl3 Cl 0.16054(9) 0.75159(12) 0.03908(7) 0.0878(6) Uani 1 1 d . . . Cl4 Cl 0.09157(10) 0.93965(11) 0.02927(6) 0.0778(5) Uani 1 1 d . . . F1 F 0.33519(13) -0.19017(17) 0.03151(9) 0.0399(6) Uani 1 1 d . . . F2 F 0.46147(14) -0.2138(2) -0.00191(9) 0.0520(7) Uani 1 1 d . . . F3 F 0.57465(13) -0.0962(2) 0.02679(10) 0.0550(8) Uani 1 1 d . . . F4 F 0.55970(13) 0.04832(19) 0.08910(12) 0.0584(8) Uani 1 1 d . . . F5 F 0.43462(12) 0.06990(17) 0.12351(10) 0.0418(6) Uani 1 1 d . . . F6 F -0.18617(15) 0.4326(2) 0.39074(11) 0.0610(8) Uani 1 1 d . . . F7 F -0.27991(18) 0.5042(2) 0.44431(10) 0.0689(9) Uani 1 1 d . . . F8 F -0.40696(18) 0.4132(2) 0.44877(11) 0.0715(10) Uani 1 1 d . . . F9 F -0.43976(14) 0.2477(2) 0.39993(11) 0.0609(9) Uani 1 1 d . . . F10 F -0.34714(13) 0.1765(2) 0.34544(10) 0.0499(7) Uani 1 1 d . . . N1 N -0.10423(17) 0.1595(3) 0.33753(12) 0.0378(9) Uani 1 1 d . . . N2 N -0.18281(17) 0.2422(2) 0.25827(12) 0.0303(8) Uani 1 1 d . . . N3 N 0.21894(15) -0.1092(2) 0.14165(11) 0.0221(7) Uani 1 1 d . . . N4 N 0.22199(15) 0.0851(2) 0.10277(11) 0.0209(7) Uani 1 1 d . . . C1 C 0.12231(19) 0.2295(2) 0.13380(13) 0.0210(8) Uani 1 1 d . . . C2 C 0.07175(19) 0.2914(3) 0.14894(13) 0.0223(8) Uani 1 1 d . . . H2 H 0.0524 0.3446 0.1320 0.027 Uiso 1 1 calc R . . C3 C 0.05265(19) 0.2663(3) 0.19189(13) 0.0229(8) Uani 1 1 d . . . H3 H 0.0196 0.3010 0.2066 0.027 Uiso 1 1 calc R . . C4 C 0.08796(18) 0.1848(3) 0.21008(13) 0.0203(8) Uani 1 1 d . . . C5 C 0.08023(18) 0.1327(3) 0.25241(12) 0.0204(8) Uani 1 1 d . . . C6 C 0.11763(19) 0.0523(3) 0.26999(13) 0.0222(8) Uani 1 1 d . . . H6 H 0.1559 0.0247 0.2572 0.027 Uiso 1 1 calc R . . C7 C 0.09138(18) 0.0166(3) 0.30956(13) 0.0225(8) Uani 1 1 d . . . H7 H 0.1108 -0.0376 0.3257 0.027 Uiso 1 1 calc R . . C8 C 0.03454(19) 0.0686(3) 0.32249(13) 0.0239(8) Uani 1 1 d . . . C9 C -0.0038(2) 0.0493(3) 0.36154(14) 0.0298(9) Uani 1 1 d . . . C10 C -0.0657(2) 0.0957(3) 0.36895(16) 0.0381(11) Uani 1 1 d . . . C11 C -0.0994(2) 0.0922(4) 0.41123(17) 0.0506(14) Uani 1 1 d . . . H11 H -0.0848 0.0549 0.4373 0.061 Uiso 1 1 calc R . . C12 C -0.1555(2) 0.1532(4) 0.40509(17) 0.0508(14) Uani 1 1 d . . . H12 H -0.1870 0.1670 0.4263 0.061 Uiso 1 1 calc R . . C13 C -0.1580(2) 0.1938(3) 0.35900(16) 0.0405(11) Uani 1 1 d . . . C14 C -0.2111(2) 0.2594(3) 0.33740(15) 0.0329(10) Uani 1 1 d . . . C15 C -0.2190(2) 0.2842(3) 0.29174(15) 0.0295(9) Uani 1 1 d . . . C16 C -0.2673(2) 0.3553(3) 0.26822(15) 0.0316(9) Uani 1 1 d . . . H16 H -0.2997 0.3936 0.2818 0.038 Uiso 1 1 calc R . . C17 C -0.2578(2) 0.3571(3) 0.22344(15) 0.0323(9) Uani 1 1 d . . . H17 H -0.2812 0.3987 0.2013 0.039 Uiso 1 1 calc R . . C18 C -0.2051(2) 0.2840(3) 0.21519(14) 0.0278(9) Uani 1 1 d . . . C19 C -0.18512(19) 0.2616(3) 0.17379(14) 0.0279(9) Uani 1 1 d . . . C20 C -0.13845(19) 0.1829(3) 0.16300(14) 0.0264(9) Uani 1 1 d . . . C21 C -0.1029(2) 0.1757(3) 0.12502(14) 0.0295(9) Uani 1 1 d . . . H21 H -0.1072 0.2218 0.1016 0.035 Uiso 1 1 calc R . . C22 C -0.0593(2) 0.0927(3) 0.12460(14) 0.0280(9) Uani 1 1 d . . . H22 H -0.0320 0.0787 0.1010 0.034 Uiso 1 1 calc R . . C23 C -0.06104(19) 0.0344(3) 0.16235(14) 0.0256(8) Uani 1 1 d . . . C24 C -0.01847(19) -0.0509(3) 0.17599(14) 0.0263(9) Uani 1 1 d . . . C25 C -0.0261(2) -0.1191(3) 0.20922(14) 0.0282(9) Uani 1 1 d . . . H25 H -0.0650 -0.1209 0.2260 0.034 Uiso 1 1 calc R . . C26 C 0.0313(2) -0.1863(3) 0.21521(14) 0.0280(9) Uani 1 1 d . . . H26 H 0.0340 -0.2368 0.2365 0.034 Uiso 1 1 calc R . . C27 C 0.0830(2) -0.1700(3) 0.18659(14) 0.0253(8) Uani 1 1 d . . . C28 C 0.14998(19) -0.2233(3) 0.18671(13) 0.0214(8) Uani 1 1 d . . . C29 C 0.20833(19) -0.1944(3) 0.16637(13) 0.0228(8) Uani 1 1 d . . . C30 C 0.27414(19) -0.2500(3) 0.16590(13) 0.0246(8) Uani 1 1 d . . . H30 H 0.2839 -0.3096 0.1804 0.029 Uiso 1 1 calc R . . C31 C 0.3189(2) -0.2020(3) 0.14140(13) 0.0251(8) Uani 1 1 d . . . H31 H 0.3642 -0.2233 0.1359 0.030 Uiso 1 1 calc R . . C32 C 0.28507(19) -0.1120(3) 0.12500(13) 0.0214(8) Uani 1 1 d . . . C33 C 0.31043(19) -0.0430(3) 0.09696(13) 0.0221(8) Uani 1 1 d . . . C34 C 0.27429(19) 0.0455(3) 0.08245(13) 0.0227(8) Uani 1 1 d . . . C35 C 0.2903(2) 0.1045(3) 0.04338(13) 0.0261(8) Uani 1 1 d . . . H35 H 0.3253 0.0920 0.0243 0.031 Uiso 1 1 calc R . . C36 C 0.2446(2) 0.1803(3) 0.04045(13) 0.0253(8) Uani 1 1 d . . . H36 H 0.2407 0.2295 0.0184 0.030 Uiso 1 1 calc R . . C37 C 0.20240(19) 0.1701(3) 0.07875(12) 0.0214(8) Uani 1 1 d . . . C38 C 0.15510(18) 0.2373(3) 0.09226(13) 0.0205(8) Uani 1 1 d . . . C39 C 0.1379(2) 0.3259(3) 0.06272(13) 0.0252(8) Uani 1 1 d . . . C40 C 0.1818(2) 0.4082(3) 0.06938(14) 0.0290(9) Uani 1 1 d . . . C41 C 0.1660(2) 0.4883(3) 0.03997(15) 0.0383(11) Uani 1 1 d . . . H41 H 0.1948 0.5436 0.0438 0.046 Uiso 1 1 calc R . . C42 C 0.1090(3) 0.4860(3) 0.00583(17) 0.0418(11) Uani 1 1 d . . . H42 H 0.0991 0.5398 -0.0132 0.050 Uiso 1 1 calc R . . C43 C 0.0660(2) 0.4046(3) -0.00053(15) 0.0384(11) Uani 1 1 d . . . H43 H 0.0277 0.4039 -0.0241 0.046 Uiso 1 1 calc R . . C44 C 0.0789(2) 0.3234(3) 0.02762(14) 0.0313(9) Uani 1 1 d . . . C45 C 0.0301(2) 0.2365(3) 0.02135(16) 0.0380(10) Uani 1 1 d . . . H45A H -0.0023 0.2374 0.0443 0.057 Uiso 1 1 calc R . . H45B H 0.0584 0.1781 0.0245 0.057 Uiso 1 1 calc R . . H45C H 0.0028 0.2384 -0.0088 0.057 Uiso 1 1 calc R . . C46 C 0.2433(2) 0.4134(3) 0.10754(16) 0.0357(10) Uani 1 1 d . . . H46A H 0.2256 0.4042 0.1366 0.054 Uiso 1 1 calc R . . H46B H 0.2661 0.4760 0.1071 0.054 Uiso 1 1 calc R . . H46C H 0.2777 0.3634 0.1033 0.054 Uiso 1 1 calc R . . C47 C 0.02683(19) -0.0281(3) 0.39407(13) 0.0238(8) Uani 1 1 d . . . C48 C 0.0030(2) -0.1236(3) 0.38658(15) 0.0363(10) Uani 1 1 d . . . C49 C 0.0318(3) -0.1966(3) 0.41668(16) 0.0419(11) Uani 1 1 d . . . H49 H 0.0163 -0.2606 0.4119 0.050 Uiso 1 1 calc R . . C50 C 0.0823(2) -0.1747(3) 0.45291(16) 0.0395(11) Uani 1 1 d . . . H50 H 0.1011 -0.2235 0.4730 0.047 Uiso 1 1 calc R . . C51 C 0.1053(2) -0.0813(3) 0.45972(15) 0.0409(11) Uani 1 1 d . . . H51 H 0.1394 -0.0672 0.4848 0.049 Uiso 1 1 calc R . . C52 C 0.0793(2) -0.0061(3) 0.43024(13) 0.0285(9) Uani 1 1 d . . . C53 C 0.1072(3) 0.0953(3) 0.43801(17) 0.0545(14) Uani 1 1 d . . . H53A H 0.1233 0.1193 0.4103 0.082 Uiso 1 1 calc R . . H53B H 0.1467 0.0953 0.4624 0.082 Uiso 1 1 calc R . . H53C H 0.0695 0.1364 0.4463 0.082 Uiso 1 1 calc R . . C54 C -0.0543(4) -0.1483(5) 0.34636(19) 0.084(2) Uani 1 1 d . . . H54A H -0.0959 -0.1080 0.3477 0.125 Uiso 1 1 calc R . . H54B H -0.0677 -0.2155 0.3482 0.125 Uiso 1 1 calc R . . H54C H -0.0354 -0.1370 0.3178 0.125 Uiso 1 1 calc R . . C55 C -0.2630(2) 0.3021(3) 0.36673(14) 0.0321(10) Uani 1 1 d . . . C56 C -0.3294(2) 0.2572(3) 0.36931(15) 0.0346(10) Uani 1 1 d . . . C57 C -0.3770(2) 0.2930(4) 0.39759(16) 0.0413(11) Uani 1 1 d . . . C58 C -0.3604(3) 0.3752(4) 0.42186(15) 0.0431(12) Uani 1 1 d . . . C59 C -0.2966(3) 0.4219(4) 0.42030(16) 0.0462(12) Uani 1 1 d . . . C60 C -0.2486(2) 0.3852(3) 0.39204(16) 0.0405(11) Uani 1 1 d . . . C61 C -0.2108(2) 0.3254(3) 0.13260(14) 0.0298(9) Uani 1 1 d . . . C62 C -0.2686(2) 0.2935(3) 0.10076(15) 0.0352(10) Uani 1 1 d . . . C63 C -0.2906(2) 0.3513(4) 0.06337(16) 0.0439(12) Uani 1 1 d . . . H63 H -0.3292 0.3315 0.0422 0.053 Uiso 1 1 calc R . . C64 C -0.2564(3) 0.4388(4) 0.05650(17) 0.0483(13) Uani 1 1 d . . . H64 H -0.2716 0.4768 0.0308 0.058 Uiso 1 1 calc R . . C65 C -0.1995(3) 0.4690(3) 0.08835(16) 0.0424(11) Uani 1 1 d . . . H65 H -0.1765 0.5275 0.0838 0.051 Uiso 1 1 calc R . . C66 C -0.1765(2) 0.4132(3) 0.12681(15) 0.0333(10) Uani 1 1 d . . . C67 C -0.1135(2) 0.4485(3) 0.16050(17) 0.0448(12) Uani 1 1 d . . . H67A H -0.1307 0.4704 0.1883 0.067 Uiso 1 1 calc R . . H67B H -0.0900 0.5013 0.1470 0.067 Uiso 1 1 calc R . . H67C H -0.0800 0.3961 0.1676 0.067 Uiso 1 1 calc R . . C68 C -0.3060(2) 0.1968(4) 0.10702(18) 0.0479(12) Uani 1 1 d . . . H68A H -0.3507 0.1944 0.0868 0.072 Uiso 1 1 calc R . . H68B H -0.3154 0.1908 0.1384 0.072 Uiso 1 1 calc R . . H68C H -0.2755 0.1444 0.0998 0.072 Uiso 1 1 calc R . . C69 C 0.15410(19) -0.3175(3) 0.21235(13) 0.0233(8) Uani 1 1 d . . . C70 C 0.1313(2) -0.4031(3) 0.18878(15) 0.0325(9) Uani 1 1 d . . . C71 C 0.1351(3) -0.4911(3) 0.21306(16) 0.0392(11) Uani 1 1 d . . . H71 H 0.1220 -0.5487 0.1975 0.047 Uiso 1 1 calc R . . C72 C 0.1579(2) -0.4933(3) 0.25941(15) 0.0348(10) Uani 1 1 d . . . H72 H 0.1599 -0.5524 0.2750 0.042 Uiso 1 1 calc R . . C73 C 0.1779(2) -0.4095(3) 0.28304(15) 0.0311(9) Uani 1 1 d . . . H73 H 0.1922 -0.4117 0.3147 0.037 Uiso 1 1 calc R . . C74 C 0.17679(19) -0.3204(3) 0.25965(14) 0.0269(9) Uani 1 1 d . . . C75 C 0.1999(2) -0.2281(3) 0.28592(15) 0.0373(10) Uani 1 1 d . . . H75A H 0.2444 -0.2053 0.2768 0.056 Uiso 1 1 calc R . . H75B H 0.2063 -0.2414 0.3184 0.056 Uiso 1 1 calc R . . H75C H 0.1634 -0.1791 0.2792 0.056 Uiso 1 1 calc R . . C76 C 0.1038(3) -0.4011(3) 0.13805(16) 0.0453(12) Uani 1 1 d . . . H76A H 0.0637 -0.3572 0.1327 0.068 Uiso 1 1 calc R . . H76B H 0.0886 -0.4653 0.1281 0.068 Uiso 1 1 calc R . . H76C H 0.1415 -0.3796 0.1211 0.068 Uiso 1 1 calc R . . C77 C 0.38114(19) -0.0607(3) 0.07974(13) 0.0243(8) Uani 1 1 d . . . C78 C 0.3912(2) -0.1322(3) 0.04730(14) 0.0290(9) Uani 1 1 d . . . C79 C 0.4548(2) -0.1452(3) 0.02971(15) 0.0341(10) Uani 1 1 d . . . C80 C 0.5119(2) -0.0853(3) 0.04410(17) 0.0396(11) Uani 1 1 d . . . C81 C 0.5050(2) -0.0122(3) 0.07579(17) 0.0367(11) Uani 1 1 d . . . C82 C 0.4405(2) -0.0019(3) 0.09279(15) 0.0288(9) Uani 1 1 d . . . C83 C 0.5304(3) 0.0529(4) 0.2273(2) 0.0766(19) Uani 1 1 d . . . H83A H 0.4924 0.0847 0.2070 0.092 Uiso 1 1 calc R . . H83B H 0.5162 0.0522 0.2581 0.092 Uiso 1 1 calc R . . C84 C 0.1601(3) 0.8657(4) 0.0141(2) 0.0621(15) Uani 1 1 d . . . H84A H 0.1545 0.8586 -0.0191 0.075 Uiso 1 1 calc R . . H84B H 0.2061 0.8969 0.0235 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0237(5) 0.0183(4) 0.0258(5) 0.0045(4) 0.0109(4) 0.0033(4) S2 0.0248(5) 0.0328(5) 0.0305(6) 0.0129(4) 0.0134(4) 0.0095(4) S3 0.0269(5) 0.0253(5) 0.0394(6) 0.0027(4) 0.0117(4) 0.0040(4) S4 0.0244(5) 0.0206(5) 0.0406(6) 0.0046(4) 0.0127(4) 0.0015(4) Cl1 0.168(2) 0.0901(14) 0.0843(14) 0.0209(11) 0.0185(14) -0.0406(14) Cl2 0.1272(15) 0.0556(10) 0.0826(13) -0.0027(8) -0.0019(11) 0.0141(10) Cl3 0.0775(11) 0.0559(9) 0.1231(16) 0.0165(10) -0.0133(10) -0.0084(8) Cl4 0.1016(12) 0.0534(9) 0.0779(12) 0.0006(8) 0.0093(9) -0.0039(8) F1 0.0397(14) 0.0361(14) 0.0457(16) -0.0174(12) 0.0120(12) 0.0010(11) F2 0.0547(16) 0.0572(17) 0.0491(17) -0.0170(14) 0.0257(14) 0.0181(14) F3 0.0373(14) 0.0625(19) 0.073(2) 0.0079(16) 0.0375(14) 0.0141(13) F4 0.0261(13) 0.0455(16) 0.106(3) -0.0029(16) 0.0186(15) -0.0054(12) F5 0.0309(13) 0.0292(13) 0.0663(19) -0.0155(12) 0.0105(12) -0.0025(10) F6 0.0487(17) 0.0597(19) 0.076(2) -0.0056(16) 0.0145(16) -0.0134(14) F7 0.102(3) 0.0559(19) 0.051(2) -0.0071(16) 0.0187(18) 0.0080(18) F8 0.088(2) 0.078(2) 0.060(2) 0.0192(17) 0.0511(18) 0.0344(18) F9 0.0343(15) 0.079(2) 0.074(2) 0.0222(17) 0.0271(14) 0.0053(14) F10 0.0400(15) 0.0513(17) 0.0601(19) -0.0033(15) 0.0124(13) -0.0056(12) N1 0.0240(17) 0.052(2) 0.041(2) 0.0236(18) 0.0149(16) 0.0148(16) N2 0.0302(18) 0.0312(19) 0.032(2) 0.0071(15) 0.0122(15) 0.0099(14) N3 0.0205(15) 0.0174(15) 0.0306(18) 0.0015(13) 0.0113(13) 0.0008(12) N4 0.0228(15) 0.0166(15) 0.0249(17) 0.0018(13) 0.0093(13) 0.0030(12) C1 0.0251(18) 0.0142(17) 0.025(2) 0.0005(15) 0.0063(15) -0.0009(14) C2 0.0243(18) 0.0178(18) 0.025(2) 0.0022(15) 0.0055(16) 0.0053(15) C3 0.0230(18) 0.0209(19) 0.026(2) -0.0015(16) 0.0086(16) 0.0002(15) C4 0.0186(17) 0.0200(18) 0.0234(19) -0.0026(15) 0.0075(15) -0.0033(14) C5 0.0169(17) 0.0223(19) 0.023(2) 0.0020(15) 0.0052(15) -0.0038(14) C6 0.0234(18) 0.0206(19) 0.023(2) -0.0001(15) 0.0061(15) 0.0023(15) C7 0.0208(18) 0.0220(19) 0.025(2) 0.0033(16) 0.0043(15) 0.0019(15) C8 0.0216(18) 0.028(2) 0.022(2) 0.0093(16) 0.0039(15) 0.0012(15) C9 0.026(2) 0.036(2) 0.028(2) 0.0105(18) 0.0083(17) 0.0048(17) C10 0.033(2) 0.046(3) 0.038(3) 0.020(2) 0.015(2) 0.009(2) C11 0.039(3) 0.075(4) 0.042(3) 0.035(3) 0.022(2) 0.028(2) C12 0.040(3) 0.068(3) 0.050(3) 0.026(3) 0.026(2) 0.022(2) C13 0.029(2) 0.050(3) 0.046(3) 0.016(2) 0.018(2) 0.013(2) C14 0.030(2) 0.037(2) 0.034(2) 0.0072(19) 0.0147(18) 0.0091(18) C15 0.0215(19) 0.030(2) 0.038(2) 0.0019(18) 0.0071(17) 0.0039(16) C16 0.025(2) 0.036(2) 0.035(2) 0.0006(19) 0.0054(18) 0.0098(17) C17 0.029(2) 0.031(2) 0.037(3) 0.0007(19) 0.0043(18) 0.0092(17) C18 0.026(2) 0.027(2) 0.031(2) 0.0028(17) 0.0071(17) 0.0053(16) C19 0.0219(19) 0.023(2) 0.038(2) 0.0013(17) 0.0029(17) 0.0026(15) C20 0.0214(19) 0.0218(19) 0.036(2) -0.0007(17) 0.0039(17) 0.0005(15) C21 0.030(2) 0.028(2) 0.032(2) 0.0005(18) 0.0061(17) -0.0002(17) C22 0.025(2) 0.026(2) 0.033(2) -0.0066(17) 0.0066(17) 0.0023(16) C23 0.0177(18) 0.025(2) 0.034(2) -0.0044(17) 0.0048(16) -0.0007(15) C24 0.0217(18) 0.022(2) 0.036(2) -0.0078(17) 0.0075(17) -0.0012(15) C25 0.028(2) 0.023(2) 0.036(2) -0.0017(17) 0.0128(18) -0.0017(16) C26 0.029(2) 0.025(2) 0.031(2) -0.0021(17) 0.0080(17) 0.0005(16) C27 0.0256(19) 0.0192(19) 0.032(2) -0.0019(16) 0.0077(17) -0.0029(15) C28 0.0220(18) 0.0176(18) 0.026(2) -0.0013(15) 0.0078(15) -0.0001(14) C29 0.0255(19) 0.0167(18) 0.027(2) 0.0017(15) 0.0063(16) 0.0022(15) C30 0.029(2) 0.0191(19) 0.027(2) -0.0005(16) 0.0085(17) 0.0064(15) C31 0.0238(19) 0.0218(19) 0.032(2) -0.0013(16) 0.0111(16) 0.0076(15) C32 0.0246(19) 0.0154(17) 0.025(2) -0.0027(15) 0.0067(16) 0.0038(14) C33 0.0218(18) 0.0206(18) 0.026(2) -0.0047(16) 0.0111(15) 0.0013(15) C34 0.0236(18) 0.0165(18) 0.029(2) -0.0047(15) 0.0076(16) -0.0018(14) C35 0.0258(19) 0.028(2) 0.027(2) -0.0008(17) 0.0147(17) -0.0001(16) C36 0.031(2) 0.0217(19) 0.025(2) 0.0041(16) 0.0117(16) 0.0013(16) C37 0.0237(18) 0.0199(18) 0.0215(19) 0.0006(15) 0.0065(15) 0.0001(15) C38 0.0194(17) 0.0184(18) 0.025(2) 0.0009(15) 0.0064(15) -0.0002(14) C39 0.028(2) 0.0226(19) 0.028(2) 0.0050(16) 0.0157(17) 0.0078(16) C40 0.037(2) 0.026(2) 0.027(2) 0.0036(17) 0.0158(18) 0.0033(17) C41 0.056(3) 0.023(2) 0.041(3) 0.0094(19) 0.024(2) 0.004(2) C42 0.051(3) 0.032(2) 0.045(3) 0.017(2) 0.016(2) 0.016(2) C43 0.040(2) 0.045(3) 0.031(2) 0.010(2) 0.0057(19) 0.022(2) C44 0.035(2) 0.033(2) 0.029(2) 0.0029(18) 0.0141(18) 0.0140(18) C45 0.033(2) 0.042(3) 0.039(3) -0.004(2) 0.003(2) 0.0001(19) C46 0.039(2) 0.023(2) 0.045(3) 0.0039(19) 0.007(2) -0.0049(18) C47 0.0214(18) 0.028(2) 0.024(2) 0.0076(16) 0.0105(16) 0.0042(15) C48 0.044(2) 0.038(2) 0.028(2) 0.0047(19) 0.0066(19) -0.013(2) C49 0.063(3) 0.026(2) 0.041(3) 0.005(2) 0.024(2) -0.004(2) C50 0.034(2) 0.042(3) 0.045(3) 0.028(2) 0.015(2) 0.006(2) C51 0.041(2) 0.053(3) 0.029(2) 0.014(2) 0.003(2) -0.004(2) C52 0.039(2) 0.029(2) 0.018(2) 0.0041(16) 0.0054(17) -0.0032(17) C53 0.090(4) 0.035(3) 0.036(3) 0.002(2) -0.002(3) -0.019(3) C54 0.114(5) 0.085(4) 0.043(3) 0.021(3) -0.023(3) -0.069(4) C55 0.024(2) 0.043(3) 0.030(2) 0.0117(19) 0.0071(17) 0.0089(18) C56 0.027(2) 0.044(3) 0.034(2) 0.007(2) 0.0081(18) 0.0079(19) C57 0.033(2) 0.052(3) 0.042(3) 0.019(2) 0.014(2) 0.009(2) C58 0.048(3) 0.056(3) 0.031(3) 0.019(2) 0.024(2) 0.029(2) C59 0.069(3) 0.041(3) 0.028(3) 0.001(2) 0.006(2) 0.014(3) C60 0.032(2) 0.047(3) 0.043(3) 0.008(2) 0.007(2) 0.004(2) C61 0.026(2) 0.032(2) 0.033(2) -0.0042(18) 0.0083(17) 0.0081(17) C62 0.026(2) 0.049(3) 0.031(2) -0.007(2) 0.0045(18) 0.0064(19) C63 0.037(2) 0.059(3) 0.034(3) -0.006(2) -0.001(2) 0.007(2) C64 0.051(3) 0.059(3) 0.032(3) 0.009(2) -0.004(2) 0.016(3) C65 0.051(3) 0.031(2) 0.045(3) 0.007(2) 0.005(2) 0.005(2) C66 0.033(2) 0.033(2) 0.034(2) 0.0021(19) 0.0007(19) 0.0101(18) C67 0.045(3) 0.037(3) 0.050(3) 0.001(2) -0.002(2) -0.002(2) C68 0.036(2) 0.057(3) 0.049(3) -0.006(2) 0.001(2) -0.011(2) C69 0.0234(18) 0.0185(18) 0.030(2) 0.0004(16) 0.0112(16) 0.0017(14) C70 0.046(2) 0.020(2) 0.033(2) -0.0034(17) 0.012(2) -0.0006(18) C71 0.060(3) 0.017(2) 0.040(3) 0.0030(18) 0.005(2) -0.0074(19) C72 0.044(2) 0.025(2) 0.034(3) 0.0081(18) 0.002(2) -0.0090(18) C73 0.032(2) 0.035(2) 0.027(2) 0.0029(18) 0.0074(18) 0.0007(18) C74 0.0246(19) 0.024(2) 0.033(2) -0.0025(17) 0.0076(17) 0.0011(16) C75 0.045(3) 0.025(2) 0.040(3) -0.0086(19) -0.003(2) 0.0031(19) C76 0.076(3) 0.025(2) 0.034(3) -0.0053(19) 0.003(2) -0.005(2) C77 0.0254(19) 0.0189(19) 0.030(2) 0.0012(16) 0.0102(16) 0.0038(15) C78 0.027(2) 0.026(2) 0.036(2) 0.0016(18) 0.0111(18) 0.0048(16) C79 0.039(2) 0.034(2) 0.033(2) 0.0029(19) 0.0177(19) 0.0103(19) C80 0.033(2) 0.040(3) 0.051(3) 0.014(2) 0.025(2) 0.013(2) C81 0.024(2) 0.031(2) 0.057(3) 0.008(2) 0.014(2) -0.0014(17) C82 0.027(2) 0.020(2) 0.041(3) 0.0017(18) 0.0126(18) 0.0064(16) C83 0.080(4) 0.079(5) 0.067(4) 0.010(4) -0.004(3) 0.008(4) C84 0.065(4) 0.059(4) 0.060(4) 0.011(3) -0.002(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C4 1.718(4) . ? S1 C1 1.728(4) . ? S2 C5 1.719(4) . ? S2 C8 1.738(4) . ? S3 C23 1.731(4) . ? S3 C20 1.739(4) . ? S4 C27 1.717(4) . ? S4 C24 1.728(4) . ? Cl1 C83 1.728(7) . ? Cl2 C83 1.797(7) . ? Cl3 C84 1.729(6) . ? Cl4 C84 1.738(6) . ? F1 C78 1.349(4) . ? F2 C79 1.337(5) . ? F3 C80 1.345(5) . ? F4 C81 1.338(5) . ? F5 C82 1.348(5) . ? F6 C60 1.343(5) . ? F7 C59 1.346(5) . ? F8 C58 1.352(5) . ? F9 C57 1.338(5) . ? F10 C56 1.329(5) . ? N1 C13 1.339(5) . ? N1 C10 1.401(5) . ? N2 C15 1.387(5) . ? N2 C18 1.399(5) . ? N3 C32 1.387(4) . ? N3 C29 1.403(4) . ? N4 C34 1.325(4) . ? N4 C37 1.388(4) . ? C1 C2 1.387(5) . ? C1 C38 1.434(5) . ? C2 C3 1.393(5) . ? C3 C4 1.373(5) . ? C4 C5 1.453(5) . ? C5 C6 1.372(5) . ? C6 C7 1.403(5) . ? C7 C8 1.374(5) . ? C8 C9 1.449(5) . ? C9 C10 1.363(5) . ? C9 C47 1.491(5) . ? C10 C11 1.460(6) . ? C11 C12 1.336(6) . ? C12 C13 1.454(6) . ? C13 C14 1.427(6) . ? C14 C15 1.368(6) . ? C14 C55 1.495(5) . ? C15 C16 1.443(5) . ? C16 C17 1.344(6) . ? C17 C18 1.449(5) . ? C18 C19 1.348(6) . ? C19 C20 1.450(5) . ? C19 C61 1.518(6) . ? C20 C21 1.370(6) . ? C21 C22 1.403(5) . ? C22 C23 1.368(6) . ? C23 C24 1.444(5) . ? C24 C25 1.371(5) . ? C25 C26 1.410(5) . ? C26 C27 1.377(5) . ? C27 C28 1.451(5) . ? C28 C29 1.368(5) . ? C28 C69 1.494(5) . ? C29 C30 1.451(5) . ? C30 C31 1.343(5) . ? C31 C32 1.443(5) . ? C32 C33 1.377(5) . ? C33 C34 1.429(5) . ? C33 C77 1.495(5) . ? C34 C35 1.463(5) . ? C35 C36 1.343(5) . ? C36 C37 1.458(5) . ? C37 C38 1.372(5) . ? C38 C39 1.503(5) . ? C39 C40 1.396(5) . ? C39 C44 1.409(6) . ? C40 C41 1.405(5) . ? C40 C46 1.499(6) . ? C41 C42 1.365(6) . ? C42 C43 1.376(7) . ? C43 C44 1.389(6) . ? C44 C45 1.500(6) . ? C47 C52 1.381(5) . ? C47 C48 1.394(6) . ? C48 C49 1.397(6) . ? C48 C54 1.525(6) . ? C49 C50 1.360(6) . ? C50 C51 1.360(6) . ? C51 C52 1.393(6) . ? C52 C53 1.495(6) . ? C55 C60 1.369(6) . ? C55 C56 1.399(6) . ? C56 C57 1.382(6) . ? C57 C58 1.349(7) . ? C58 C59 1.361(7) . ? C59 C60 1.391(6) . ? C61 C66 1.387(6) . ? C61 C62 1.403(6) . ? C62 C63 1.371(6) . ? C62 C68 1.523(6) . ? C63 C64 1.388(7) . ? C64 C65 1.385(7) . ? C65 C66 1.384(6) . ? C66 C67 1.516(6) . ? C69 C74 1.395(5) . ? C69 C70 1.401(5) . ? C70 C71 1.399(5) . ? C70 C76 1.507(6) . ? C71 C72 1.369(6) . ? C72 C73 1.371(6) . ? C73 C74 1.401(5) . ? C74 C75 1.517(5) . ? C77 C82 1.387(5) . ? C77 C78 1.396(5) . ? C78 C79 1.369(5) . ? C79 C80 1.371(6) . ? C80 C81 1.384(6) . ? C81 C82 1.370(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 S1 C1 91.93(17) . . ? C5 S2 C8 91.74(18) . . ? C23 S3 C20 92.37(19) . . ? C27 S4 C24 92.83(19) . . ? C13 N1 C10 105.5(3) . . ? C15 N2 C18 110.4(3) . . ? C32 N3 C29 110.5(3) . . ? C34 N4 C37 106.3(3) . . ? C2 C1 C38 127.4(3) . . ? C2 C1 S1 110.2(3) . . ? C38 C1 S1 122.3(3) . . ? C1 C2 C3 113.6(3) . . ? C4 C3 C2 112.6(3) . . ? C3 C4 C5 129.5(3) . . ? C3 C4 S1 111.6(3) . . ? C5 C4 S1 118.8(3) . . ? C6 C5 C4 127.9(3) . . ? C6 C5 S2 112.0(3) . . ? C4 C5 S2 120.0(3) . . ? C5 C6 C7 112.0(3) . . ? C8 C7 C6 114.3(3) . . ? C7 C8 C9 126.9(3) . . ? C7 C8 S2 110.0(3) . . ? C9 C8 S2 123.1(3) . . ? C10 C9 C8 123.8(4) . . ? C10 C9 C47 119.7(3) . . ? C8 C9 C47 116.4(3) . . ? C9 C10 N1 124.4(4) . . ? C9 C10 C11 126.0(4) . . ? N1 C10 C11 109.5(4) . . ? C12 C11 C10 106.5(4) . . ? C11 C12 C13 107.3(4) . . ? N1 C13 C14 122.5(4) . . ? N1 C13 C12 111.3(4) . . ? C14 C13 C12 126.2(4) . . ? C15 C14 C13 124.9(4) . . ? C15 C14 C55 117.7(3) . . ? C13 C14 C55 117.4(4) . . ? C14 C15 N2 125.7(4) . . ? C14 C15 C16 128.1(4) . . ? N2 C15 C16 106.1(4) . . ? C17 C16 C15 108.9(4) . . ? C16 C17 C18 109.1(4) . . ? C19 C18 N2 129.0(3) . . ? C19 C18 C17 125.5(4) . . ? N2 C18 C17 105.4(3) . . ? C18 C19 C20 127.6(4) . . ? C18 C19 C61 119.0(3) . . ? C20 C19 C61 113.4(3) . . ? C21 C20 C19 126.8(4) . . ? C21 C20 S3 109.7(3) . . ? C19 C20 S3 123.5(3) . . ? C20 C21 C22 114.1(4) . . ? C23 C22 C21 113.3(4) . . ? C22 C23 C24 129.0(4) . . ? C22 C23 S3 110.5(3) . . ? C24 C23 S3 120.3(3) . . ? C25 C24 C23 130.3(4) . . ? C25 C24 S4 110.4(3) . . ? C23 C24 S4 119.2(3) . . ? C24 C25 C26 112.9(4) . . ? C27 C26 C25 113.7(4) . . ? C26 C27 C28 126.2(4) . . ? C26 C27 S4 110.1(3) . . ? C28 C27 S4 123.7(3) . . ? C29 C28 C27 126.1(3) . . ? C29 C28 C69 118.5(3) . . ? C27 C28 C69 115.3(3) . . ? C28 C29 N3 129.8(3) . . ? C28 C29 C30 125.3(3) . . ? N3 C29 C30 104.9(3) . . ? C31 C30 C29 109.6(3) . . ? C30 C31 C32 108.7(3) . . ? C33 C32 N3 125.6(3) . . ? C33 C32 C31 128.2(3) . . ? N3 C32 C31 106.2(3) . . ? C32 C33 C34 125.2(3) . . ? C32 C33 C77 118.5(3) . . ? C34 C33 C77 116.3(3) . . ? N4 C34 C33 124.3(3) . . ? N4 C34 C35 111.1(3) . . ? C33 C34 C35 124.6(3) . . ? C36 C35 C34 106.7(3) . . ? C35 C36 C37 106.2(3) . . ? C38 C37 N4 124.0(3) . . ? C38 C37 C36 126.1(3) . . ? N4 C37 C36 109.6(3) . . ? C37 C38 C1 123.7(3) . . ? C37 C38 C39 118.5(3) . . ? C1 C38 C39 117.7(3) . . ? C40 C39 C44 121.0(4) . . ? C40 C39 C38 119.8(3) . . ? C44 C39 C38 119.2(3) . . ? C39 C40 C41 118.3(4) . . ? C39 C40 C46 121.7(3) . . ? C41 C40 C46 120.0(4) . . ? C42 C41 C40 120.9(4) . . ? C41 C42 C43 120.4(4) . . ? C42 C43 C44 121.3(4) . . ? C43 C44 C39 118.1(4) . . ? C43 C44 C45 120.7(4) . . ? C39 C44 C45 121.1(4) . . ? C52 C47 C48 120.5(4) . . ? C52 C47 C9 120.7(4) . . ? C48 C47 C9 118.8(4) . . ? C47 C48 C49 119.2(4) . . ? C47 C48 C54 120.7(4) . . ? C49 C48 C54 120.2(4) . . ? C50 C49 C48 120.4(4) . . ? C51 C50 C49 119.9(4) . . ? C50 C51 C52 122.1(4) . . ? C47 C52 C51 118.0(4) . . ? C47 C52 C53 121.3(4) . . ? C51 C52 C53 120.7(4) . . ? C60 C55 C56 116.9(4) . . ? C60 C55 C14 122.8(4) . . ? C56 C55 C14 120.4(4) . . ? F10 C56 C57 118.3(4) . . ? F10 C56 C55 120.2(4) . . ? C57 C56 C55 121.4(4) . . ? F9 C57 C58 120.4(4) . . ? F9 C57 C56 120.2(5) . . ? C58 C57 C56 119.4(4) . . ? C57 C58 F8 120.5(5) . . ? C57 C58 C59 121.4(4) . . ? F8 C58 C59 118.1(5) . . ? F7 C59 C58 121.6(4) . . ? F7 C59 C60 119.3(5) . . ? C58 C59 C60 119.0(5) . . ? F6 C60 C55 120.0(4) . . ? F6 C60 C59 118.2(5) . . ? C55 C60 C59 121.8(4) . . ? C66 C61 C62 121.3(4) . . ? C66 C61 C19 119.6(4) . . ? C62 C61 C19 119.0(4) . . ? C63 C62 C61 118.3(4) . . ? C63 C62 C68 120.4(4) . . ? C61 C62 C68 121.3(4) . . ? C62 C63 C64 121.4(4) . . ? C65 C64 C63 119.4(4) . . ? C66 C65 C64 120.9(4) . . ? C65 C66 C61 118.7(4) . . ? C65 C66 C67 119.1(4) . . ? C61 C66 C67 122.2(4) . . ? C74 C69 C70 119.9(4) . . ? C74 C69 C28 120.8(3) . . ? C70 C69 C28 119.2(3) . . ? C71 C70 C69 118.8(4) . . ? C71 C70 C76 120.2(4) . . ? C69 C70 C76 120.9(4) . . ? C72 C71 C70 120.8(4) . . ? C71 C72 C73 120.7(4) . . ? C72 C73 C74 120.1(4) . . ? C69 C74 C73 119.5(4) . . ? C69 C74 C75 120.6(4) . . ? C73 C74 C75 119.8(4) . . ? C82 C77 C78 115.1(3) . . ? C82 C77 C33 121.7(3) . . ? C78 C77 C33 123.1(3) . . ? F1 C78 C79 118.0(4) . . ? F1 C78 C77 118.8(3) . . ? C79 C78 C77 123.1(4) . . ? F2 C79 C78 120.9(4) . . ? F2 C79 C80 119.8(4) . . ? C78 C79 C80 119.2(4) . . ? F3 C80 C79 120.0(4) . . ? F3 C80 C81 119.7(4) . . ? C79 C80 C81 120.3(4) . . ? F4 C81 C82 120.5(4) . . ? F4 C81 C80 120.8(4) . . ? C82 C81 C80 118.7(4) . . ? F5 C82 C81 117.9(4) . . ? F5 C82 C77 118.6(3) . . ? C81 C82 C77 123.5(4) . . ? Cl1 C83 Cl2 112.2(4) . . ? Cl3 C84 Cl4 112.7(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.645 _refine_diff_density_min -1.162 _refine_diff_density_rms 0.096