data_diamide _audit_creation_method ; 1. CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) 2. SXELXL-97 ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _cell_measurement_reflns_used 15557 _cell_measurement_theta_min 4.1289 _cell_measurement_theta_max 38.5079 _exptl_crystal_size_max 0.4893 _exptl_crystal_size_mid 0.2659 _exptl_crystal_size_min 0.2364 _exptl_absorpt_coefficient_mu 0.316 _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Goniometer Xcalibur, detector: Onyx' _diffrn_detector_area_resol_mean 8.1956 _diffrn_orient_matrix_UB_11 -0.0026235822 _diffrn_orient_matrix_UB_12 0.0265214582 _diffrn_orient_matrix_UB_13 -0.0315039908 _diffrn_orient_matrix_UB_21 -0.0470820511 _diffrn_orient_matrix_UB_22 0.0091471746 _diffrn_orient_matrix_UB_23 -0.0004968508 _diffrn_orient_matrix_UB_31 0.0163364260 _diffrn_orient_matrix_UB_32 0.0306523388 _diffrn_orient_matrix_UB_33 0.0273770661 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 phi 0.00 100.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames 0.0000 14.0000 0.0000 - 100 #__ type_ start__ end____ width___ exp.time_ 2 omega -60.00 84.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 -79.0000 0.0000 144 #__ type_ start__ end____ width___ exp.time_ 3 omega -60.00 84.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 -79.0000 120.0000 144 #__ type_ start__ end____ width___ exp.time_ 4 omega -60.00 20.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 -79.0000 240.0000 80 ; _diffrn_measurement_method '\w and \p scans' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_cell_setting monoclinic _chemical_name_systematic ; 5,15,20,30-tetramesityl-10,25-diphenyl-8,23-dioxo-7,22-diaza-33,37-dicarba-A,D-di-p-benzi[28]hexaphyrin(1.1.1.1.1.1) dichloromethane tetrasolvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H96 N4 O2, 4(C H2 Cl2)' _chemical_formula_sum 'C98 H104 Cl8 N4 O2' _chemical_formula_weight 1653.45 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' 'O' 'O' 0.0106 0.0060 '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' 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 14.7357(4) _cell_length_b 17.0703(3) _cell_length_c 17.6198(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.354(3) _cell_angle_gamma 90.00 _cell_volume 4273.94(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _exptl_crystal_description 'block' _exptl_crystal_colour 'dark' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66843 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 38.59 _reflns_number_total 23396 _reflns_number_gt 11814 _reflns_threshold_expression >2sigma(I) _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. ; _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^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23396 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1334 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.026 _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 C1 C 0.23789(8) 0.54041(7) 1.05683(7) 0.0126(2) Uani 1 1 d . . . C2 C 0.26390(8) 0.58412(7) 0.99865(7) 0.0132(2) Uani 1 1 d . . . H2 H 0.2708 0.5585 0.9526 0.016 Uiso 1 1 calc R . . C3 C 0.27955(8) 0.66351(7) 1.00705(7) 0.0130(2) Uani 1 1 d . . . H3 H 0.2966 0.6917 0.9665 0.016 Uiso 1 1 calc R . . C4 C 0.72918(8) 0.29617(7) 0.92560(7) 0.0122(2) Uani 1 1 d . . . C5 C 0.69845(8) 0.21458(7) 0.91248(7) 0.0126(2) Uani 1 1 d . . . C6 C 0.61793(8) 0.19083(7) 0.93046(7) 0.0127(2) Uani 1 1 d . . . C7 C 0.47619(8) 0.19712(7) 0.96043(7) 0.0130(2) Uani 1 1 d . . . C8 C 0.39704(8) 0.22590(7) 0.97788(7) 0.0127(2) Uani 1 1 d . . . C9 C 0.37540(8) 0.30579(7) 0.99293(7) 0.0129(2) Uani 1 1 d . . . C10 C 0.42897(8) 0.38001(7) 0.98836(7) 0.0129(2) Uani 1 1 d . . . C11 C 0.29669(8) 0.41146(7) 1.02745(7) 0.0132(2) Uani 1 1 d . . . C12 C 0.23266(8) 0.45450(7) 1.05270(7) 0.0123(2) Uani 1 1 d . . . C13 C 0.15626(8) 0.41426(7) 1.07941(7) 0.0133(2) Uani 1 1 d . B . C14 C 0.06727(8) 0.40289(7) 1.02664(7) 0.0139(2) Uani 1 1 d . B . C15 C -0.00506(9) 0.37054(7) 1.05371(7) 0.0167(2) Uani 1 1 d . . . H15 H -0.0645 0.3619 1.0174 0.020 Uiso 1 1 calc R A 5 C18 C 0.17141(9) 0.39153(7) 1.15842(7) 0.0157(2) Uani 1 1 d . . . C19 C 0.04714(9) 0.42379(8) 0.94042(7) 0.0174(2) Uani 1 1 d . . . H19A H 0.0982 0.4579 0.9324 0.021 Uiso 1 1 calc R B . H19B H -0.0124 0.4538 0.9247 0.021 Uiso 1 1 calc R . . C20 C 0.03918(11) 0.35187(9) 0.88814(8) 0.0259(3) Uani 1 1 d . B . H20A H 0.0997 0.3244 0.9004 0.039 Uiso 1 1 calc R . . H20B H 0.0221 0.3681 0.8328 0.039 Uiso 1 1 calc R . . H20C H -0.0094 0.3168 0.8975 0.039 Uiso 1 1 calc R . . C23 C 0.26606(9) 0.39993(8) 1.21783(8) 0.0191(2) Uani 1 1 d . B . H23A H 0.2563 0.4176 1.2686 0.023 Uiso 1 1 calc R . . H23B H 0.3030 0.4407 1.1994 0.023 Uiso 1 1 calc R . . C24 C 0.32214(10) 0.32367(9) 1.23083(9) 0.0249(3) Uani 1 1 d . . . H24A H 0.2848 0.2824 1.2468 0.037 Uiso 1 1 calc R B . H24B H 0.3807 0.3313 1.2722 0.037 Uiso 1 1 calc R . . H24C H 0.3369 0.3083 1.1818 0.037 Uiso 1 1 calc R . . C16A C 0.00692(10) 0.35056(9) 1.13209(8) 0.0140(3) Uani 0.928(3) 1 d P B 5 C17A C 0.09583(11) 0.36075(10) 1.18306(8) 0.0150(3) Uani 0.928(3) 1 d P B 5 H17 H 0.1057 0.3463 1.2367 0.018 Uiso 0.928(3) 1 calc PR B 5 C21A C -0.07632(10) 0.32099(8) 1.15900(8) 0.0170(3) Uani 0.928(3) 1 d P B 5 H21A H -0.1112 0.2827 1.1198 0.020 Uiso 0.928(3) 1 calc PR B 5 H21B H -0.1191 0.3657 1.1594 0.020 Uiso 0.928(3) 1 calc PR B 5 C22A C -0.05282(11) 0.28239(10) 1.23979(9) 0.0245(4) Uani 0.928(3) 1 d P B 5 H22A H -0.0094 0.2386 1.2409 0.037 Uiso 0.928(3) 1 calc PR B 5 H22B H -0.1107 0.2628 1.2505 0.037 Uiso 0.928(3) 1 calc PR B 5 H22C H -0.0232 0.3209 1.2800 0.037 Uiso 0.928(3) 1 calc PR B 5 C21B C -0.0448(12) 0.2748(10) 1.1647(10) 0.015(4) Uiso 0.072(3) 1 d P B 6 H21C H -0.0936 0.2573 1.1175 0.018 Uiso 0.072(3) 1 calc PR B 6 H21D H -0.0157 0.2277 1.1940 0.018 Uiso 0.072(3) 1 calc PR B 6 C16B C 0.0313(13) 0.3229(11) 1.1390(10) 0.009(3) Uiso 0.072(3) 1 d P B 6 C22B C -0.0880(18) 0.3220(15) 1.2143(14) 0.033(6) Uiso 0.072(3) 1 d P B 6 H22D H -0.0391 0.3427 1.2588 0.049 Uiso 0.072(3) 1 calc PR B 6 H22E H -0.1317 0.2896 1.2341 0.049 Uiso 0.072(3) 1 calc PR B 6 H22F H -0.1225 0.3656 1.1835 0.049 Uiso 0.072(3) 1 calc PR B 6 C17B C 0.1139(17) 0.3360(14) 1.1806(14) 0.020(5) Uiso 0.072(3) 1 d P B 6 H17B H 0.1374 0.3073 1.2279 0.024 Uiso 0.072(3) 1 calc PR B 6 C25 C 0.74903(8) 0.15803(7) 0.87343(7) 0.0136(2) Uani 1 1 d . . . C26 C 0.70530(9) 0.13007(7) 0.79718(7) 0.0160(2) Uani 1 1 d . . . C27 C 0.75172(10) 0.07315(8) 0.76473(8) 0.0204(3) Uani 1 1 d . . . H27 H 0.7223 0.0534 0.7137 0.024 Uiso 1 1 calc R . . C28 C 0.83962(10) 0.04442(8) 0.80460(8) 0.0207(3) Uani 1 1 d . . . C29 C 0.88374(9) 0.07583(7) 0.87779(8) 0.0188(2) Uani 1 1 d . . . H29 H 0.9452 0.0585 0.9043 0.023 Uiso 1 1 calc R . . C30 C 0.83984(9) 0.13230(7) 0.91336(7) 0.0149(2) Uani 1 1 d . . . C31 C 0.61102(10) 0.16334(8) 0.75177(8) 0.0202(3) Uani 1 1 d . . . H31A H 0.5622 0.1439 0.7763 0.024 Uiso 1 1 calc R . . H31B H 0.6135 0.2210 0.7576 0.024 Uiso 1 1 calc R . . C32 C 0.58041(12) 0.14406(10) 0.66466(8) 0.0294(3) Uani 1 1 d . . . H32A H 0.6298 0.1598 0.6399 0.044 Uiso 1 1 calc R . . H32B H 0.5222 0.1724 0.6400 0.044 Uiso 1 1 calc R . . H32C H 0.5694 0.0876 0.6578 0.044 Uiso 1 1 calc R . . C33 C 0.88452(12) -0.02102(8) 0.76925(9) 0.0287(3) Uani 1 1 d . . . H33A H 0.9507 -0.0276 0.8003 0.034 Uiso 1 1 calc R . . H33B H 0.8847 -0.0067 0.7149 0.034 Uiso 1 1 calc R . . C34 C 0.83220(13) -0.09860(9) 0.76790(11) 0.0348(4) Uani 1 1 d . . . H34A H 0.8305 -0.1123 0.8215 0.052 Uiso 1 1 calc R . . H34B H 0.8648 -0.1399 0.7468 0.052 Uiso 1 1 calc R . . H34C H 0.7678 -0.0933 0.7345 0.052 Uiso 1 1 calc R . . C35 C 0.88611(9) 0.16552(8) 0.99419(8) 0.0188(2) Uani 1 1 d . . . H35A H 0.8469 0.1510 1.0298 0.023 Uiso 1 1 calc R . . H35B H 0.8851 0.2234 0.9900 0.023 Uiso 1 1 calc R . . C36 C 0.98669(10) 0.14040(9) 1.03286(10) 0.0288(3) Uani 1 1 d . . . H36A H 0.9890 0.0834 1.0397 0.043 Uiso 1 1 calc R . . H36B H 1.0086 0.1658 1.0843 0.043 Uiso 1 1 calc R . . H36C H 1.0273 0.1558 0.9995 0.043 Uiso 1 1 calc R . . C37 C 0.32341(8) 0.16709(7) 0.98217(7) 0.0130(2) Uani 1 1 d . . . C38 C 0.24279(9) 0.15907(7) 0.91997(7) 0.0174(2) Uani 1 1 d . . . H38 H 0.2339 0.1924 0.8754 0.021 Uiso 1 1 calc R . . C39 C 0.17528(10) 0.10294(8) 0.92223(8) 0.0210(3) Uani 1 1 d . . . H39 H 0.1210 0.0975 0.8792 0.025 Uiso 1 1 calc R . . C40 C 0.18757(10) 0.05475(7) 0.98784(8) 0.0202(3) Uani 1 1 d . . . H40 H 0.1420 0.0158 0.9893 0.024 Uiso 1 1 calc R . . C41 C 0.26555(9) 0.06332(7) 1.05063(8) 0.0191(3) Uani 1 1 d . . . H41 H 0.2729 0.0311 1.0958 0.023 Uiso 1 1 calc R . . C42 C 0.33383(9) 0.11902(7) 1.04818(8) 0.0172(2) Uani 1 1 d . . . H42 H 0.3877 0.1244 1.0916 0.021 Uiso 1 1 calc R . . C43 C 0.21778(8) 0.58189(7) 1.11948(7) 0.0135(2) Uani 1 1 d . . . H43 H 0.1927 0.5547 1.1564 0.016 Uiso 1 1 calc R . . C44 C 0.23398(8) 0.66183(7) 1.12804(7) 0.0134(2) Uani 1 1 d . . . H44 H 0.2199 0.6886 1.1708 0.016 Uiso 1 1 calc R . . C45 C 0.57857(8) 0.11249(7) 0.92661(7) 0.0142(2) Uani 1 1 d . . . H45 H 0.6068 0.0662 0.9134 0.017 Uiso 1 1 calc R . . C46 C 0.49546(9) 0.11625(7) 0.94483(7) 0.0148(2) Uani 1 1 d . . . H46 H 0.4558 0.0729 0.9471 0.018 Uiso 1 1 calc R . . C47 C 0.29789(8) 0.32820(7) 1.01667(7) 0.0138(2) Uani 1 1 d . . . H47 H 0.2512 0.2933 1.0249 0.017 Uiso 1 1 calc R . . N1 N 0.55321(7) 0.23894(6) 0.95284(6) 0.01346(19) Uani 1 1 d . . . H1 H 0.5606 0.2897 0.9611 0.016 Uiso 1 1 calc R . . N2 N 0.37773(7) 0.43939(6) 1.00817(6) 0.01381(19) Uani 1 1 d . . . H2A H 0.3934 0.4892 1.0088 0.017 Uiso 1 1 calc R . . O O 0.50400(6) 0.39085(5) 0.97101(5) 0.01531(17) Uani 1 1 d . . . C48 C 0.27779(11) 0.57792(9) 0.36597(10) 0.0309(3) Uani 1 1 d . . . H48A H 0.2823 0.5676 0.4221 0.037 Uiso 1 1 calc R C 3 H48B H 0.3107 0.5350 0.3464 0.037 Uiso 1 1 calc R C 3 Cl1 Cl 0.15823(3) 0.57853(2) 0.31239(2) 0.03116(9) Uani 1 1 d . D . Cl2A Cl 0.33334(4) 0.66700(2) 0.35755(2) 0.03802(14) Uani 0.9575(15) 1 d P D 3 Cl2B Cl 0.3780(15) 0.5707(12) 0.3445(12) 0.095(7) Uiso 0.0425(15) 1 d P D 4 C49 C 0.47052(12) 0.59131(11) 0.20493(10) 0.0356(4) Uani 1 1 d . . . H49A H 0.4702 0.5679 0.1535 0.043 Uiso 1 1 calc R E 1 H49B H 0.4088 0.6168 0.1993 0.043 Uiso 1 1 calc R E 1 Cl3 Cl 0.48473(3) 0.51630(2) 0.27558(2) 0.03400(10) Uani 1 1 d . D . Cl4A Cl 0.55807(5) 0.66164(4) 0.22885(3) 0.0396(2) Uani 0.892(3) 1 d P F 1 Cl4B Cl 0.5929(5) 0.6283(5) 0.2199(4) 0.063(2) Uiso 0.108(3) 1 d P F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0097(5) 0.0126(5) 0.0162(5) -0.0013(4) 0.0046(4) 0.0003(4) C2 0.0111(5) 0.0148(5) 0.0145(5) -0.0018(4) 0.0050(4) 0.0008(4) C3 0.0120(5) 0.0135(5) 0.0144(5) -0.0001(4) 0.0050(4) 0.0007(4) C4 0.0089(5) 0.0127(5) 0.0152(5) -0.0009(4) 0.0035(4) 0.0015(4) C5 0.0123(5) 0.0128(5) 0.0135(5) -0.0007(4) 0.0045(4) 0.0014(4) C6 0.0121(5) 0.0122(5) 0.0143(5) -0.0009(4) 0.0044(4) 0.0024(4) C7 0.0127(5) 0.0124(5) 0.0148(5) -0.0005(4) 0.0050(4) -0.0008(4) C8 0.0124(5) 0.0119(5) 0.0147(5) -0.0010(4) 0.0049(4) -0.0008(4) C9 0.0114(5) 0.0126(5) 0.0153(5) -0.0011(4) 0.0048(4) 0.0002(4) C10 0.0123(5) 0.0130(5) 0.0139(5) -0.0003(4) 0.0043(4) 0.0002(4) C11 0.0106(5) 0.0128(5) 0.0173(5) -0.0011(4) 0.0057(4) -0.0007(4) C12 0.0111(5) 0.0129(5) 0.0139(5) -0.0018(4) 0.0051(4) -0.0009(4) C13 0.0129(5) 0.0118(5) 0.0172(5) -0.0020(4) 0.0075(4) -0.0003(4) C14 0.0136(5) 0.0144(5) 0.0149(5) -0.0018(4) 0.0057(4) -0.0005(4) C15 0.0128(5) 0.0204(6) 0.0175(5) -0.0021(4) 0.0052(5) -0.0036(4) C18 0.0152(6) 0.0148(5) 0.0175(5) -0.0004(4) 0.0049(5) -0.0020(4) C19 0.0150(6) 0.0205(6) 0.0172(5) 0.0011(4) 0.0053(5) -0.0020(5) C20 0.0319(8) 0.0301(8) 0.0166(6) -0.0029(5) 0.0080(6) 0.0024(6) C23 0.0161(6) 0.0218(6) 0.0185(6) 0.0010(5) 0.0030(5) -0.0036(5) C24 0.0217(7) 0.0286(7) 0.0234(6) 0.0003(5) 0.0043(6) 0.0023(5) C16A 0.0129(6) 0.0131(6) 0.0173(6) 0.0003(5) 0.0062(5) 0.0000(5) C17A 0.0155(7) 0.0155(7) 0.0150(6) 0.0006(5) 0.0058(5) -0.0001(5) C21A 0.0153(6) 0.0202(7) 0.0174(6) 0.0008(5) 0.0076(5) -0.0037(5) C22A 0.0227(8) 0.0283(8) 0.0255(7) 0.0093(6) 0.0116(6) -0.0018(6) C25 0.0135(5) 0.0118(5) 0.0177(5) -0.0004(4) 0.0082(5) 0.0008(4) C26 0.0164(6) 0.0164(6) 0.0166(5) -0.0010(4) 0.0069(5) -0.0004(4) C27 0.0258(7) 0.0187(6) 0.0197(6) -0.0046(5) 0.0114(5) -0.0004(5) C28 0.0251(7) 0.0156(6) 0.0278(7) -0.0017(5) 0.0181(6) 0.0028(5) C29 0.0173(6) 0.0148(6) 0.0279(6) 0.0027(5) 0.0122(5) 0.0042(4) C30 0.0138(5) 0.0133(5) 0.0194(5) 0.0016(4) 0.0080(5) 0.0010(4) C31 0.0198(6) 0.0228(6) 0.0176(6) -0.0009(5) 0.0042(5) 0.0007(5) C32 0.0309(8) 0.0375(9) 0.0175(6) -0.0007(6) 0.0025(6) -0.0010(6) C33 0.0366(9) 0.0218(7) 0.0354(8) -0.0035(6) 0.0232(7) 0.0074(6) C34 0.0403(10) 0.0237(8) 0.0456(9) -0.0089(7) 0.0206(8) 0.0054(6) C35 0.0145(6) 0.0198(6) 0.0221(6) 0.0013(5) 0.0045(5) 0.0024(5) C36 0.0189(7) 0.0259(7) 0.0371(8) 0.0003(6) -0.0006(6) 0.0046(6) C37 0.0124(5) 0.0111(5) 0.0174(5) -0.0020(4) 0.0074(4) 0.0003(4) C38 0.0194(6) 0.0169(6) 0.0172(5) 0.0002(4) 0.0070(5) -0.0031(5) C39 0.0174(6) 0.0202(6) 0.0250(6) -0.0019(5) 0.0049(5) -0.0043(5) C40 0.0193(6) 0.0137(6) 0.0317(7) -0.0006(5) 0.0137(6) -0.0019(5) C41 0.0203(6) 0.0152(6) 0.0254(6) 0.0053(5) 0.0127(5) 0.0032(5) C42 0.0150(6) 0.0179(6) 0.0197(6) 0.0023(4) 0.0061(5) 0.0019(4) C43 0.0116(5) 0.0146(5) 0.0157(5) 0.0000(4) 0.0063(4) 0.0005(4) C44 0.0129(5) 0.0140(5) 0.0149(5) -0.0015(4) 0.0065(4) 0.0010(4) C45 0.0147(6) 0.0119(5) 0.0170(5) -0.0013(4) 0.0059(5) 0.0015(4) C46 0.0159(6) 0.0120(5) 0.0181(5) -0.0013(4) 0.0071(5) -0.0004(4) C47 0.0126(5) 0.0132(5) 0.0167(5) -0.0009(4) 0.0060(4) -0.0002(4) N1 0.0120(5) 0.0101(4) 0.0201(5) -0.0017(4) 0.0074(4) 0.0003(3) N2 0.0116(5) 0.0105(4) 0.0212(5) -0.0023(4) 0.0078(4) -0.0007(3) O 0.0118(4) 0.0151(4) 0.0215(4) -0.0010(3) 0.0087(3) -0.0004(3) C48 0.0311(8) 0.0259(8) 0.0358(8) 0.0053(6) 0.0091(7) -0.0017(6) Cl1 0.0304(2) 0.0383(2) 0.02608(17) 0.00298(15) 0.00976(15) 0.00488(15) Cl2A 0.0560(3) 0.0288(2) 0.0278(2) -0.00183(15) 0.0086(2) -0.01641(19) C49 0.0253(8) 0.0457(10) 0.0303(8) 0.0121(7) -0.0022(7) -0.0089(7) Cl3 0.0346(2) 0.0275(2) 0.0369(2) 0.00487(15) 0.00442(17) -0.00666(15) Cl4A 0.0452(4) 0.0302(3) 0.0354(3) 0.00685(19) -0.0035(2) -0.0160(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 C1 C2 1.4009(16) . ? C1 C43 1.4075(16) . ? C1 C12 1.4693(16) . ? C2 C3 1.3760(17) . ? C3 C4 1.4068(16) 3_667 ? C4 C44 1.4049(16) 3_667 ? C4 C3 1.4068(16) 3_667 ? C4 C5 1.4639(16) . ? C5 C6 1.3680(16) . ? C5 C25 1.4942(15) . ? C6 N1 1.3923(14) . ? C6 C45 1.4521(17) . ? C7 C8 1.3734(16) . ? C7 N1 1.3769(15) . ? C7 C46 1.4502(17) . ? C8 C9 1.4410(16) . ? C8 C37 1.4948(16) . ? C9 C47 1.3707(16) . ? C9 C10 1.5062(16) . ? C10 O 1.2366(14) . ? C10 N2 1.3635(15) . ? C11 C12 1.3603(16) . ? C11 N2 1.4084(15) . ? C11 C47 1.4347(17) . ? C12 C13 1.4970(16) . ? C13 C18 1.4049(17) . ? C13 C14 1.4058(18) . ? C14 C15 1.3920(16) . ? C14 C19 1.5116(17) . ? C15 C16A 1.3876(18) . ? C15 C16B 1.668(18) . ? C18 C17B 1.39(2) . ? C18 C17A 1.4002(19) . ? C18 C23 1.5129(18) . ? C19 C20 1.5206(19) . ? C23 C24 1.526(2) . ? C16A C17A 1.389(2) . ? C16A C21A 1.5139(18) . ? C21A C22A 1.523(2) . ? C21B C22B 1.45(3) . ? C21B C16B 1.55(2) . ? C16B C17B 1.26(3) . ? C25 C30 1.4071(17) . ? C25 C26 1.4105(17) . ? C26 C27 1.3951(17) . ? C26 C31 1.5178(19) . ? C27 C28 1.389(2) . ? C28 C29 1.3890(19) . ? C28 C33 1.5138(18) . ? C29 C30 1.3983(17) . ? C30 C35 1.5167(18) . ? C31 C32 1.5168(19) . ? C33 C34 1.529(2) . ? C35 C36 1.5198(19) . ? C37 C38 1.3935(18) . ? C37 C42 1.3983(17) . ? C38 C39 1.3892(18) . ? C39 C40 1.3912(19) . ? C40 C41 1.376(2) . ? C41 C42 1.3932(18) . ? C43 C44 1.3865(17) . ? C44 C4 1.4050(16) 3_667 ? C45 C46 1.3473(17) . ? C48 Cl2B 1.62(2) . ? C48 Cl2A 1.7517(16) . ? C48 Cl1 1.7647(17) . ? Cl2B Cl3 2.41(2) . ? C49 Cl4A 1.7307(17) . ? C49 Cl3 1.7592(16) . ? C49 Cl4B 1.863(7) . ? 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 C2 C1 C43 117.45(10) . . ? C2 C1 C12 121.09(10) . . ? C43 C1 C12 121.46(10) . . ? C3 C2 C1 121.09(10) . . ? C2 C3 C4 121.49(11) . 3_667 ? C44 C4 C3 117.11(10) 3_667 3_667 ? C44 C4 C5 122.53(10) 3_667 . ? C3 C4 C5 120.34(10) 3_667 . ? C6 C5 C4 119.75(10) . . ? C6 C5 C25 118.96(10) . . ? C4 C5 C25 121.09(10) . . ? C5 C6 N1 126.29(11) . . ? C5 C6 C45 128.48(11) . . ? N1 C6 C45 105.15(10) . . ? C8 C7 N1 127.37(11) . . ? C8 C7 C46 127.11(11) . . ? N1 C7 C46 105.51(10) . . ? C7 C8 C9 128.48(11) . . ? C7 C8 C37 116.23(10) . . ? C9 C8 C37 115.30(10) . . ? C47 C9 C8 124.27(11) . . ? C47 C9 C10 105.81(10) . . ? C8 C9 C10 129.91(10) . . ? O C10 N2 122.96(11) . . ? O C10 C9 130.90(11) . . ? N2 C10 C9 106.14(10) . . ? C12 C11 N2 127.01(11) . . ? C12 C11 C47 127.76(11) . . ? N2 C11 C47 105.22(9) . . ? C11 C12 C1 121.56(10) . . ? C11 C12 C13 119.97(10) . . ? C1 C12 C13 118.45(10) . . ? C18 C13 C14 119.53(11) . . ? C18 C13 C12 120.19(11) . . ? C14 C13 C12 120.19(10) . . ? C15 C14 C13 119.53(11) . . ? C15 C14 C19 118.28(11) . . ? C13 C14 C19 122.18(11) . . ? C16A C15 C14 122.10(12) . . ? C14 C15 C16B 114.2(6) . . ? C17B C18 C13 121.1(10) . . ? C17A C18 C13 118.69(12) . . ? C17B C18 C23 112.8(10) . . ? C17A C18 C23 118.96(11) . . ? C13 C18 C23 122.34(11) . . ? C14 C19 C20 112.42(11) . . ? C18 C23 C24 112.73(11) . . ? C15 C16A C17A 117.53(12) . . ? C15 C16A C21A 119.57(12) . . ? C17A C16A C21A 122.88(12) . . ? C16A C17A C18 122.54(13) . . ? C16A C21A C22A 115.75(12) . . ? C22B C21B C16B 110.3(16) . . ? C17B C16B C21B 125.8(17) . . ? C17B C16B C15 117.8(16) . . ? C21B C16B C15 115.9(13) . . ? C16B C17B C18 121.4(19) . . ? C30 C25 C26 120.32(11) . . ? C30 C25 C5 119.71(11) . . ? C26 C25 C5 119.96(11) . . ? C27 C26 C25 118.43(12) . . ? C27 C26 C31 121.62(11) . . ? C25 C26 C31 119.94(11) . . ? C28 C27 C26 122.10(12) . . ? C29 C28 C27 118.54(12) . . ? C29 C28 C33 121.24(13) . . ? C27 C28 C33 120.20(13) . . ? C28 C29 C30 121.59(12) . . ? C29 C30 C25 118.86(12) . . ? C29 C30 C35 122.16(11) . . ? C25 C30 C35 118.97(10) . . ? C32 C31 C26 115.95(12) . . ? C28 C33 C34 111.83(12) . . ? C30 C35 C36 117.26(11) . . ? C38 C37 C42 118.65(11) . . ? C38 C37 C8 120.35(11) . . ? C42 C37 C8 120.99(11) . . ? C39 C38 C37 120.87(12) . . ? C38 C39 C40 119.67(13) . . ? C41 C40 C39 120.17(12) . . ? C40 C41 C42 120.26(12) . . ? C41 C42 C37 120.34(12) . . ? C44 C43 C1 120.97(11) . . ? C43 C44 C4 121.00(10) . 3_667 ? C46 C45 C6 108.78(10) . . ? C45 C46 C7 109.05(11) . . ? C9 C47 C11 110.93(10) . . ? C7 N1 C6 111.45(10) . . ? C10 N2 C11 111.86(10) . . ? Cl2B C48 Cl2A 64.6(7) . . ? Cl2B C48 Cl1 135.8(7) . . ? Cl2A C48 Cl1 111.86(9) . . ? C48 Cl2B Cl3 154.2(12) . . ? Cl4A C49 Cl3 113.03(9) . . ? Cl3 C49 Cl4B 102.5(2) . . ? C49 Cl3 Cl2B 96.0(5) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 38.59 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.704 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.078