# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Takahiko Kojima' 'Shunichi Fukuzumi' 'Kakeru Hanabusa' 'Kei Ohkubo' 'Motoo Shiro' _publ_contact_author_name 'Takahiko Kojima' _publ_contact_author_email KOJIMA@CHEM.ENG.OSAKA-U.AC.JP _publ_section_title ; Formation of dodecaphenylporphodimethene via facile protonation of saddle-distorted dodecaphenylporphyrin ; # Attachment 'SnClDPP2hanabusa_Pnma.cif' data__HANDAI _database_code_depnum_ccdc_archive 'CCDC 702272' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C93 H61 Cl5 N4 Sn ' _chemical_formula_moiety 'C92 H60 Cl2 N4 Sn, C H Cl3 ' _chemical_formula_weight 1530.49 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 11.7235(2) _cell_length_b 28.4110(7) _cell_length_c 21.1529(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 7045.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 29052 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 25.4 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128.00 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.886 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.7059 _diffrn_reflns_number 44110 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_theta_max 25.34 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6450 _reflns_number_gt 4434 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2358 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6450 _refine_ls_number_parameters 476 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1123P)^2^+32.6609P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0020 _refine_diff_density_max 2.25 _refine_diff_density_min -1.07 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Sn Sn -0.654 1.425 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Sn1 Sn 0.25004(7) 0.7500 0.39216(2) 0.0453(2) Uani 1.00 2 d S . . Cl1 Cl 0.0581(3) 0.7500 0.35399(12) 0.0563(6) Uani 1.00 2 d S . . Cl2 Cl 0.4333(4) 0.7500 0.42442(17) 0.0996(12) Uani 1.00 2 d S . . Cl3 Cl 0.6607(6) 0.7500 0.6012(4) 0.179(2) Uani 1.00 2 d S . . Cl4 Cl 0.4565(5) 0.6999(2) 0.5888(2) 0.236(3) Uani 1.00 1 d . . . N1 N 0.1940(9) 0.7500 0.4872(3) 0.052(2) Uani 1.00 2 d S . . N3 N 0.2984(8) 0.7500 0.2967(3) 0.049(2) Uani 1.00 2 d S . . N4 N 0.2506(5) 0.67547(17) 0.3914(2) 0.0494(15) Uani 1.00 1 d . . . C1 C 0.1628(6) 0.7106(2) 0.5203(2) 0.0425(16) Uani 1.00 1 d . . . C2 C 0.1071(7) 0.7260(2) 0.5782(2) 0.0494(17) Uani 1.00 1 d . . . C13 C 0.2762(7) 0.7257(2) 0.1939(2) 0.053(2) Uani 1.00 1 d . . . C14 C 0.2921(6) 0.71066(19) 0.2585(2) 0.0451(17) Uani 1.00 1 d . . . C15 C 0.3068(6) 0.66420(19) 0.2801(2) 0.0445(16) Uani 1.00 1 d . . . C16 C 0.2938(6) 0.6478(2) 0.3425(2) 0.0444(16) Uani 1.00 1 d . . . C17 C 0.3072(6) 0.60064(19) 0.3673(2) 0.0425(15) Uani 1.00 1 d . . . C18 C 0.2734(6) 0.6014(2) 0.4301(2) 0.0447(17) Uani 1.00 1 d . . . C19 C 0.2356(6) 0.6486(2) 0.4442(2) 0.0435(16) Uani 1.00 1 d . . . C20 C 0.1841(6) 0.66404(19) 0.5012(2) 0.0435(16) Uani 1.00 1 d . . . C21 C 0.0582(8) 0.6997(2) 0.6318(3) 0.058(2) Uani 1.00 1 d . . . C22 C -0.0526(11) 0.6853(3) 0.6289(4) 0.088(3) Uani 1.00 1 d . . . C23 C -0.1106(12) 0.6646(3) 0.6817(6) 0.109(3) Uani 1.00 1 d . . . C24 C -0.0496(15) 0.6592(3) 0.7360(5) 0.112(4) Uani 1.00 1 d . . . C25 C 0.0634(14) 0.6730(3) 0.7413(4) 0.111(4) Uani 1.00 1 d . . . C26 C 0.1137(10) 0.6926(3) 0.6891(3) 0.087(3) Uani 1.00 1 d . . . C63 C 0.2380(7) 0.6961(2) 0.1385(2) 0.0518(19) Uani 1.00 1 d . . . C64 C 0.1285(7) 0.6780(2) 0.1380(3) 0.0536(19) Uani 1.00 1 d . . . C65 C 0.0915(8) 0.6519(2) 0.0862(3) 0.062(2) Uani 1.00 1 d . . . C66 C 0.1629(8) 0.6441(2) 0.0365(3) 0.064(2) Uani 1.00 1 d . . . C67 C 0.2694(8) 0.6610(3) 0.0362(3) 0.070(2) Uani 1.00 1 d . . . C68 C 0.3101(8) 0.6882(2) 0.0883(3) 0.061(2) Uani 1.00 1 d . . . C69 C 0.3463(6) 0.63036(18) 0.2306(2) 0.0409(16) Uani 1.00 1 d . . . C70 C 0.2827(6) 0.5918(2) 0.2114(2) 0.0447(17) Uani 1.00 1 d . . . C71 C 0.3271(7) 0.5615(2) 0.1655(2) 0.054(2) Uani 1.00 1 d . . . C72 C 0.4319(7) 0.5695(2) 0.1401(2) 0.056(2) Uani 1.00 1 d . . . C73 C 0.4944(7) 0.6071(2) 0.1578(2) 0.0511(18) Uani 1.00 1 d . . . C74 C 0.4521(6) 0.6378(2) 0.2041(2) 0.0482(18) Uani 1.00 1 d . . . C75 C 0.3535(6) 0.55761(19) 0.3374(2) 0.0442(17) Uani 1.00 1 d . . . C76 C 0.2823(7) 0.5183(2) 0.3311(3) 0.0513(19) Uani 1.00 1 d . . . C77 C 0.3247(8) 0.4766(2) 0.3060(3) 0.059(2) Uani 1.00 1 d . . . C78 C 0.4364(9) 0.4742(2) 0.2877(3) 0.065(2) Uani 1.00 1 d . . . C79 C 0.5065(7) 0.5122(2) 0.2923(3) 0.058(2) Uani 1.00 1 d . . . C80 C 0.4660(7) 0.5544(2) 0.3183(2) 0.0501(18) Uani 1.00 1 d . . . C81 C 0.2978(7) 0.5627(2) 0.4760(2) 0.0473(17) Uani 1.00 1 d . . . C82 C 0.3965(7) 0.5655(2) 0.5109(3) 0.059(2) Uani 1.00 1 d . . . C83 C 0.4260(8) 0.5288(2) 0.5514(3) 0.068(2) Uani 1.00 1 d . . . C84 C 0.3590(8) 0.4898(2) 0.5548(3) 0.068(2) Uani 1.00 1 d . . . C85 C 0.2614(8) 0.4866(2) 0.5208(3) 0.064(2) Uani 1.00 1 d . . . C86 C 0.2294(7) 0.5232(2) 0.4807(3) 0.057(2) Uani 1.00 1 d . . . C87 C 0.1413(6) 0.6250(2) 0.5440(2) 0.0467(17) Uani 1.00 1 d . . . C88 C 0.1977(8) 0.6117(2) 0.5977(2) 0.058(2) Uani 1.00 1 d . . . C89 C 0.1489(9) 0.5765(2) 0.6365(3) 0.075(2) Uani 1.00 1 d . . . C90 C 0.0481(10) 0.5569(2) 0.6205(3) 0.077(2) Uani 1.00 1 d . . . C91 C -0.0074(8) 0.5703(2) 0.5679(4) 0.068(2) Uani 1.00 1 d . . . C92 C 0.0398(7) 0.6047(2) 0.5291(3) 0.058(2) Uani 1.00 1 d . . . C93 C 0.5270(18) 0.7500 0.5633(10) 0.134(6) Uani 1.00 2 d S . . H1 H -0.0930 0.6891 0.5903 0.106 Uiso 1.00 1 c R . . H2 H -0.1881 0.6551 0.6790 0.131 Uiso 1.00 1 c R . . H3 H -0.0859 0.6455 0.7717 0.134 Uiso 1.00 1 c R . . H4 H 0.1045 0.6690 0.7796 0.133 Uiso 1.00 1 c R . . H5 H 0.1914 0.7019 0.6922 0.104 Uiso 1.00 1 c R . . H36 H 0.0788 0.6833 0.1728 0.064 Uiso 1.00 1 c R . . H37 H 0.0163 0.6394 0.0856 0.074 Uiso 1.00 1 c R . . H38 H 0.1365 0.6264 0.0013 0.076 Uiso 1.00 1 c R . . H39 H 0.3182 0.6548 0.0013 0.084 Uiso 1.00 1 c R . . H40 H 0.3854 0.7006 0.0882 0.073 Uiso 1.00 1 c R . . H41 H 0.2097 0.5860 0.2292 0.054 Uiso 1.00 1 c R . . H42 H 0.2836 0.5352 0.1519 0.065 Uiso 1.00 1 c R . . H43 H 0.4615 0.5482 0.1095 0.067 Uiso 1.00 1 c R . . H44 H 0.5668 0.6127 0.1391 0.061 Uiso 1.00 1 c R . . H45 H 0.4967 0.6640 0.2173 0.058 Uiso 1.00 1 c R . . H46 H 0.2048 0.5202 0.3440 0.062 Uiso 1.00 1 c R . . H47 H 0.2764 0.4499 0.3016 0.071 Uiso 1.00 1 c R . . H48 H 0.4656 0.4455 0.2715 0.078 Uiso 1.00 1 c R . . H49 H 0.5831 0.5101 0.2779 0.070 Uiso 1.00 1 c R . . H50 H 0.5155 0.5807 0.3227 0.060 Uiso 1.00 1 c R . . H51 H 0.4444 0.5924 0.5074 0.070 Uiso 1.00 1 c R . . H52 H 0.4929 0.5310 0.5765 0.081 Uiso 1.00 1 c R . . H53 H 0.3809 0.4644 0.5814 0.082 Uiso 1.00 1 c R . . H54 H 0.2147 0.4594 0.5244 0.077 Uiso 1.00 1 c R . . H55 H 0.1611 0.5209 0.4567 0.068 Uiso 1.00 1 c R . . H56 H 0.2684 0.6258 0.6088 0.069 Uiso 1.00 1 c R . . H57 H 0.1871 0.5667 0.6739 0.089 Uiso 1.00 1 c R . . H58 H 0.0160 0.5332 0.6468 0.092 Uiso 1.00 1 c R . . H59 H -0.0785 0.5564 0.5572 0.082 Uiso 1.00 1 c R . . H60 H 0.0007 0.6141 0.4919 0.069 Uiso 1.00 1 c R . . H61 H 0.5359 0.7500 0.5163 0.161 Uiso 1.00 2 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 0.1020(6) 0.0141(3) 0.0197(3) 0.0000 0.0011(3) 0.0000 Cl1 0.094(2) 0.0277(10) 0.0478(13) 0.0000 -0.0052(13) 0.0000 Cl2 0.165(3) 0.0623(19) 0.071(2) 0.0000 -0.004(2) 0.0000 Cl3 0.144(5) 0.152(5) 0.240(8) 0.0000 0.021(5) 0.0000 Cl4 0.240(6) 0.312(7) 0.156(4) -0.115(5) -0.038(4) 0.092(4) N1 0.116(7) 0.020(3) 0.020(3) 0.0000 0.004(3) 0.0000 N3 0.112(6) 0.014(3) 0.021(3) 0.0000 -0.003(3) 0.0000 N4 0.104(4) 0.017(2) 0.027(2) 0.003(2) 0.004(2) 0.0014(18) C1 0.085(5) 0.025(2) 0.017(2) -0.002(3) 0.005(2) 0.001(2) C2 0.097(5) 0.020(2) 0.031(3) 0.000(3) 0.003(3) -0.002(2) C13 0.119(6) 0.020(2) 0.021(2) 0.000(3) 0.002(3) 0.003(2) C14 0.094(5) 0.019(2) 0.021(2) 0.002(3) 0.003(3) -0.004(2) C15 0.093(5) 0.016(2) 0.024(2) -0.002(3) 0.002(3) -0.000(2) C16 0.093(5) 0.018(2) 0.023(2) -0.002(3) 0.002(3) -0.002(2) C17 0.089(4) 0.020(2) 0.019(2) -0.002(3) -0.005(3) 0.002(2) C18 0.087(5) 0.021(2) 0.026(2) 0.000(2) -0.007(3) 0.004(2) C19 0.080(5) 0.023(2) 0.028(2) -0.006(3) -0.001(3) 0.003(2) C20 0.086(5) 0.022(2) 0.023(2) -0.005(3) -0.002(3) 0.003(2) C21 0.105(6) 0.035(3) 0.033(3) -0.004(4) 0.011(3) -0.003(2) C22 0.143(10) 0.052(4) 0.069(5) -0.003(5) 0.021(6) -0.005(4) C23 0.148(11) 0.068(6) 0.112(9) -0.015(6) 0.040(8) -0.013(6) C24 0.205(14) 0.051(5) 0.080(7) 0.004(7) 0.064(9) -0.003(5) C25 0.201(14) 0.086(7) 0.044(5) 0.006(8) 0.020(7) 0.020(5) C26 0.150(9) 0.074(5) 0.036(4) 0.008(6) 0.008(4) 0.009(3) C63 0.111(6) 0.023(2) 0.022(3) 0.009(3) 0.001(3) 0.002(2) C64 0.096(6) 0.035(3) 0.030(3) -0.006(3) 0.001(3) -0.001(2) C65 0.109(6) 0.039(3) 0.038(3) -0.005(4) -0.008(4) -0.003(3) C66 0.112(7) 0.039(3) 0.040(3) 0.001(4) -0.006(4) -0.013(3) C67 0.115(8) 0.061(5) 0.035(3) 0.000(4) 0.008(4) -0.017(3) C68 0.116(6) 0.040(3) 0.028(3) -0.003(4) 0.001(3) -0.008(2) C69 0.087(5) 0.017(2) 0.018(2) 0.006(2) 0.001(2) -0.001(2) C70 0.088(5) 0.022(2) 0.023(2) 0.002(2) -0.001(2) 0.002(2) C71 0.113(6) 0.019(2) 0.030(3) -0.002(3) 0.003(3) -0.004(2) C72 0.114(6) 0.027(3) 0.028(3) 0.011(3) 0.005(3) -0.005(2) C73 0.093(5) 0.035(3) 0.025(2) 0.009(3) 0.005(3) 0.002(2) C74 0.096(5) 0.020(2) 0.028(3) 0.003(3) -0.000(3) 0.002(2) C75 0.095(5) 0.018(2) 0.019(2) 0.004(3) -0.001(3) 0.004(2) C76 0.100(6) 0.021(2) 0.032(3) -0.006(3) -0.006(3) 0.001(2) C77 0.126(7) 0.020(3) 0.032(3) 0.001(3) -0.006(4) -0.007(2) C78 0.139(8) 0.023(3) 0.032(3) 0.019(4) -0.005(4) -0.002(2) C79 0.102(6) 0.041(3) 0.032(3) 0.017(4) -0.005(3) 0.000(2) C80 0.098(6) 0.026(3) 0.026(3) 0.001(3) -0.008(3) 0.002(2) C81 0.098(5) 0.021(2) 0.023(2) 0.006(3) -0.002(3) 0.005(2) C82 0.103(6) 0.043(3) 0.029(3) -0.001(4) -0.000(3) 0.014(2) C83 0.101(6) 0.063(4) 0.039(3) 0.009(4) -0.011(4) 0.014(3) C84 0.122(7) 0.042(4) 0.040(3) 0.014(4) -0.000(4) 0.017(3) C85 0.124(7) 0.025(3) 0.043(3) -0.004(3) -0.003(4) 0.008(2) C86 0.115(6) 0.024(3) 0.031(3) 0.005(3) -0.005(3) 0.005(2) C87 0.101(5) 0.020(2) 0.020(2) -0.003(3) 0.006(3) -0.000(2) C88 0.117(6) 0.033(3) 0.022(3) -0.001(4) -0.001(3) 0.004(2) C89 0.154(9) 0.038(3) 0.032(3) 0.010(5) 0.013(4) 0.015(3) C90 0.162(9) 0.026(3) 0.041(4) -0.008(4) 0.027(5) 0.002(3) C91 0.108(6) 0.032(3) 0.065(5) -0.011(4) 0.011(4) 0.001(3) C92 0.106(6) 0.029(3) 0.039(3) -0.007(3) 0.001(3) 0.004(2) C93 0.150(18) 0.132(16) 0.121(15) 0.0000 0.024(13) 0.0000 #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sn1 Cl1 2.391(3) yes . . Sn1 Cl2 2.254(4) yes . . Sn1 N1 2.115(6) yes . . Sn1 N3 2.097(6) yes . . Sn1 N4 2.118(4) yes . . Sn1 N4 2.118(4) yes . 3_565 Cl3 C93 1.76(2) yes . . Cl4 C93 1.732(13) yes . . N1 C1 1.370(7) yes . . N1 C1 1.370(7) yes . 3_565 N3 C14 1.381(6) yes . . N3 C14 1.381(6) yes . 3_565 N4 C16 1.395(7) yes . . N4 C19 1.364(7) yes . . C1 C2 1.455(8) yes . . C1 C20 1.405(7) yes . . C2 C2 1.363(8) yes . 3_565 C2 C21 1.474(9) yes . . C13 C13 1.381(8) yes . 3_565 C13 C14 1.443(8) yes . . C13 C63 1.509(8) yes . . C14 C15 1.407(7) yes . . C15 C16 1.409(8) yes . . C15 C69 1.494(8) yes . . C16 C17 1.447(7) yes . . C17 C18 1.385(8) yes . . C17 C75 1.480(8) yes . . C18 C19 1.443(8) yes . . C18 C81 1.496(8) yes . . C19 C20 1.419(8) yes . . C20 C87 1.516(8) yes . . C21 C22 1.363(15) yes . . C21 C26 1.391(11) yes . . C22 C23 1.434(17) yes . . C23 C24 1.36(2) yes . . C24 C25 1.39(2) yes . . C25 C26 1.370(14) yes . . C63 C64 1.384(12) yes . . C63 C68 1.377(10) yes . . C64 C65 1.391(9) yes . . C65 C66 1.363(11) yes . . C66 C67 1.337(13) yes . . C67 C68 1.428(10) yes . . C69 C70 1.387(8) yes . . C69 C74 1.378(10) yes . . C70 C71 1.397(8) yes . . C71 C72 1.360(12) yes . . C72 C73 1.349(9) yes . . C73 C74 1.402(8) yes . . C75 C76 1.400(9) yes . . C75 C80 1.382(11) yes . . C76 C77 1.391(9) yes . . C77 C78 1.367(14) yes . . C78 C79 1.359(11) yes . . C79 C80 1.403(9) yes . . C81 C82 1.375(11) yes . . C81 C86 1.384(9) yes . . C82 C83 1.393(10) yes . . C83 C84 1.361(12) yes . . C84 C85 1.354(12) yes . . C85 C86 1.392(9) yes . . C87 C88 1.369(9) yes . . C87 C92 1.360(11) yes . . C88 C89 1.415(10) yes . . C89 C90 1.350(15) yes . . C90 C91 1.345(12) yes . . C91 C92 1.389(10) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl1 Sn1 Cl2 177.88(11) yes . . . Cl1 Sn1 N1 91.6(2) yes . . . Cl1 Sn1 N3 85.9(2) yes . . . Cl1 Sn1 N4 90.03(17) yes . . . Cl1 Sn1 N4 90.03(17) yes . . 3_565 Cl2 Sn1 N1 90.5(2) yes . . . Cl2 Sn1 N3 91.9(2) yes . . . Cl2 Sn1 N4 89.95(17) yes . . . Cl2 Sn1 N4 89.95(17) yes . . 3_565 N1 Sn1 N3 177.6(3) yes . . . N1 Sn1 N4 90.46(13) yes . . . N1 Sn1 N4 90.46(13) yes . . 3_565 N3 Sn1 N4 89.54(13) yes . . . N3 Sn1 N4 89.54(13) yes . . 3_565 N4 Sn1 N4 179.1(2) yes . . 3_565 Sn1 N1 C1 124.7(3) yes . . . Sn1 N1 C1 124.7(3) yes . . 3_565 C1 N1 C1 109.6(6) yes . . 3_565 Sn1 N3 C14 123.3(3) yes . . . Sn1 N3 C14 123.3(3) yes . . 3_565 C14 N3 C14 108.0(5) yes . . 3_565 Sn1 N4 C16 124.8(3) yes . . . Sn1 N4 C19 123.6(3) yes . . . C16 N4 C19 109.8(4) yes . . . N1 C1 C2 107.7(5) yes . . . N1 C1 C20 125.1(5) yes . . . C2 C1 C20 127.2(5) yes . . . C1 C2 C2 107.5(5) yes . . 3_565 C1 C2 C21 132.0(5) yes . . . C2 C2 C21 120.4(5) yes 3_565 . . C13 C13 C14 107.2(5) yes 3_565 . . C13 C13 C63 123.8(5) yes 3_565 . . C14 C13 C63 127.5(5) yes . . . N3 C14 C13 108.8(4) yes . . . N3 C14 C15 124.2(5) yes . . . C13 C14 C15 126.9(5) yes . . . C14 C15 C16 127.0(5) yes . . . C14 C15 C69 114.5(4) yes . . . C16 C15 C69 118.4(4) yes . . . N4 C16 C15 123.2(5) yes . . . N4 C16 C17 106.9(4) yes . . . C15 C16 C17 129.4(5) yes . . . C16 C17 C18 107.6(5) yes . . . C16 C17 C75 130.5(5) yes . . . C18 C17 C75 121.9(4) yes . . . C17 C18 C19 107.5(5) yes . . . C17 C18 C81 123.8(5) yes . . . C19 C18 C81 127.4(5) yes . . . N4 C19 C18 108.1(5) yes . . . N4 C19 C20 125.3(5) yes . . . C18 C19 C20 126.4(5) yes . . . C1 C20 C19 127.7(5) yes . . . C1 C20 C87 117.2(5) yes . . . C19 C20 C87 115.0(4) yes . . . C2 C21 C22 119.3(7) yes . . . C2 C21 C26 124.2(8) yes . . . C22 C21 C26 116.2(8) yes . . . C21 C22 C23 122.7(10) yes . . . C22 C23 C24 117.1(12) yes . . . C23 C24 C25 122.5(12) yes . . . C24 C25 C26 117.5(11) yes . . . C21 C26 C25 124.0(11) yes . . . C13 C63 C64 119.3(6) yes . . . C13 C63 C68 120.6(7) yes . . . C64 C63 C68 120.1(6) yes . . . C63 C64 C65 119.6(6) yes . . . C64 C65 C66 120.2(8) yes . . . C65 C66 C67 121.3(7) yes . . . C66 C67 C68 120.1(7) yes . . . C63 C68 C67 118.7(8) yes . . . C15 C69 C70 123.2(6) yes . . . C15 C69 C74 117.7(5) yes . . . C70 C69 C74 119.1(5) yes . . . C69 C70 C71 119.4(6) yes . . . C70 C71 C72 120.6(6) yes . . . C71 C72 C73 120.9(6) yes . . . C72 C73 C74 119.6(7) yes . . . C69 C74 C73 120.5(6) yes . . . C17 C75 C76 118.7(6) yes . . . C17 C75 C80 121.9(5) yes . . . C76 C75 C80 119.3(5) yes . . . C75 C76 C77 120.2(7) yes . . . C76 C77 C78 119.4(7) yes . . . C77 C78 C79 121.4(6) yes . . . C78 C79 C80 120.1(8) yes . . . C75 C80 C79 119.6(6) yes . . . C18 C81 C82 117.8(6) yes . . . C18 C81 C86 122.2(6) yes . . . C82 C81 C86 119.8(6) yes . . . C81 C82 C83 119.7(7) yes . . . C82 C83 C84 119.9(8) yes . . . C83 C84 C85 120.9(7) yes . . . C84 C85 C86 120.2(7) yes . . . C81 C86 C85 119.5(7) yes . . . C20 C87 C88 122.5(6) yes . . . C20 C87 C92 117.6(5) yes . . . C88 C87 C92 119.8(6) yes . . . C87 C88 C89 118.9(8) yes . . . C88 C89 C90 120.0(7) yes . . . C89 C90 C91 120.9(7) yes . . . C90 C91 C92 119.7(8) yes . . . C87 C92 C91 120.7(7) yes . . . Cl3 C93 Cl4 106.4(8) yes . . . Cl3 C93 Cl4 106.4(8) yes . . 3_565 Cl4 C93 Cl4 110.5(11) yes . . 3_565 #============================================================================== data__porphodimethene2 _database_code_depnum_ccdc_archive 'CCDC 702273' _audit_creation_date 2008-06-21 _audit_creation_method 'by CrystalStructure 3.8' # CHEMICAL DATA _chemical_formula_sum 'C93 H66 Cl2 N4 ' _chemical_formula_moiety 'C92 H64 N4, C H2 Cl2 ' _chemical_formula_weight 1310.48 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.042(3) _cell_length_b 25.066(9) _cell_length_c 19.584(4) _cell_angle_alpha 90.0000 _cell_angle_beta 111.594(5) _cell_angle_gamma 90.0000 _cell_volume 6866(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1976 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 26.3 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744.00 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_detector_area_resol_mean 14.7059 _diffrn_measurement_method dtintegrate.ref _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_reflns_number 45560 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_theta_max 25.68 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12967 _reflns_number_gt 7004 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.2372 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12967 _refine_ls_number_parameters 893 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0551P)^2^+14.1219P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0080 _refine_diff_density_max 0.56 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 N1 N 0.2151(3) 0.35490(15) 0.2199(2) 0.0327(9) Uani 1 1 d . . . N2 N 0.2103(3) 0.47209(16) 0.1699(2) 0.0366(10) Uani 1 1 d . . . H2N H 0.1580 0.4673 0.2021 0.044 Uiso 1 1 d . . . N3 N 0.0614(3) 0.48973(15) 0.2088(2) 0.0321(9) Uani 1 1 d . . . N4 N 0.0671(3) 0.37428(14) 0.2597(2) 0.0318(9) Uani 1 1 d . . . H4N H 0.1295 0.3845 0.2396 0.038 Uiso 1 1 d . . . C1 C 0.1843(3) 0.30114(19) 0.2091(2) 0.0328(11) Uani 1 1 d . . . C2 C 0.2493(3) 0.27205(19) 0.1846(2) 0.0327(11) Uani 1 1 d . . . C3 C 0.3207(3) 0.30728(18) 0.1840(2) 0.0300(11) Uani 1 1 d . . . C4 C 0.2944(3) 0.35823(18) 0.2047(2) 0.0313(11) Uani 1 1 d . . . C5 C 0.3500(3) 0.40943(18) 0.2129(3) 0.0335(11) Uani 1 1 d . . . H5 H 0.4008 0.4019 0.1942 0.040 Uiso 1 1 calc R . . C6 C 0.2906(3) 0.45378(19) 0.1651(3) 0.0352(12) Uani 1 1 d . . . C7 C 0.3138(3) 0.48354(19) 0.1123(3) 0.0356(12) Uani 1 1 d . . . C8 C 0.2430(3) 0.52189(18) 0.0843(3) 0.0328(11) Uani 1 1 d . . . C9 C 0.1769(3) 0.51470(19) 0.1207(3) 0.0336(11) Uani 1 1 d . . . C10 C 0.0943(3) 0.54414(18) 0.1171(2) 0.0295(11) Uani 1 1 d . . . C11 C 0.0394(3) 0.53302(18) 0.1596(2) 0.0305(11) Uani 1 1 d . . . C12 C -0.0381(3) 0.56342(18) 0.1697(3) 0.0326(11) Uani 1 1 d . . . C13 C -0.0560(3) 0.53828(18) 0.2266(3) 0.0330(11) Uani 1 1 d . . . C14 C 0.0050(3) 0.49287(18) 0.2473(2) 0.0315(11) Uani 1 1 d . . . C15 C 0.0100(3) 0.45465(18) 0.3075(2) 0.0327(11) Uani 1 1 d . . . H15 H -0.0476 0.4611 0.3185 0.039 Uiso 1 1 calc R . . C16 C 0.0080(3) 0.39656(19) 0.2885(2) 0.0318(11) Uani 1 1 d . . . C17 C -0.0480(3) 0.35641(18) 0.3054(3) 0.0312(11) Uani 1 1 d . . . C18 C -0.0190(3) 0.30760(18) 0.2863(3) 0.0320(11) Uani 1 1 d . . . C19 C 0.0530(3) 0.31893(18) 0.2560(3) 0.0318(11) Uani 1 1 d . . . C20 C 0.1070(3) 0.28449(18) 0.2285(2) 0.0300(11) Uani 1 1 d . . . C21 C 0.2496(3) 0.21498(19) 0.1639(3) 0.0355(11) Uani 1 1 d U . . C22 C 0.3255(4) 0.1825(2) 0.2034(3) 0.0398(12) Uani 1 1 d U . . H22 H 0.3743 0.1966 0.2440 0.048 Uiso 1 1 calc R . . C23 C 0.3310(4) 0.1299(2) 0.1843(3) 0.0493(14) Uani 1 1 d U . . H23 H 0.3817 0.1084 0.2125 0.059 Uiso 1 1 calc R . . C24 C 0.2604(4) 0.1098(2) 0.1231(3) 0.0545(15) Uani 1 1 d U . . H24 H 0.2637 0.0746 0.1093 0.065 Uiso 1 1 calc R . . C25 C 0.1846(4) 0.1414(2) 0.0818(3) 0.0566(15) Uani 1 1 d U . . H25 H 0.1375 0.1272 0.0402 0.068 Uiso 1 1 calc R . . C26 C 0.1778(4) 0.1937(2) 0.1015(3) 0.0441(12) Uani 1 1 d U . . H26 H 0.1261 0.2147 0.0737 0.053 Uiso 1 1 calc R . . C27 C 0.4061(3) 0.29654(19) 0.1663(3) 0.0345(11) Uani 1 1 d U . . C28 C 0.4975(3) 0.3124(2) 0.2145(3) 0.0379(11) Uani 1 1 d U . . H28 H 0.5037 0.3301 0.2578 0.046 Uiso 1 1 calc R . . C29 C 0.5785(4) 0.3023(2) 0.1987(3) 0.0465(13) Uani 1 1 d U . . H29 H 0.6381 0.3133 0.2311 0.056 Uiso 1 1 calc R . . C30 C 0.5704(4) 0.2758(2) 0.1349(3) 0.0509(14) Uani 1 1 d U . . H30 H 0.6246 0.2686 0.1243 0.061 Uiso 1 1 calc R . . C31 C 0.4817(4) 0.2600(2) 0.0870(3) 0.0507(14) Uani 1 1 d U . . H31 H 0.4763 0.2426 0.0438 0.061 Uiso 1 1 calc R . . C32 C 0.4000(4) 0.2699(2) 0.1025(3) 0.0438(12) Uani 1 1 d U . . H32 H 0.3408 0.2585 0.0698 0.053 Uiso 1 1 calc R . . C33 C 0.4000(4) 0.4248(2) 0.2929(3) 0.0535(10) Uani 1 1 d U . . C34 C 0.4369(4) 0.4749(2) 0.3130(3) 0.0649(11) Uani 1 1 d U . . H34 H 0.4256 0.5011 0.2773 0.078 Uiso 1 1 calc R . . C35 C 0.4908(5) 0.4874(3) 0.3859(3) 0.0699(11) Uani 1 1 d U . . H35 H 0.5143 0.5218 0.3981 0.084 Uiso 1 1 calc R . . C36 C 0.5094(4) 0.4498(2) 0.4393(3) 0.0646(11) Uani 1 1 d U . . H36 H 0.5496 0.4575 0.4872 0.077 Uiso 1 1 calc R . . C37 C 0.4685(4) 0.4006(2) 0.4221(3) 0.0561(10) Uani 1 1 d U . . H37 H 0.4770 0.3754 0.4588 0.067 Uiso 1 1 calc R . . C38 C 0.4143(4) 0.3886(2) 0.3497(3) 0.0514(10) Uani 1 1 d U . . H38 H 0.3864 0.3550 0.3386 0.062 Uiso 1 1 calc R . . C39 C 0.4003(3) 0.4752(2) 0.0953(3) 0.0375(11) Uani 1 1 d U . . C40 C 0.4686(3) 0.5158(2) 0.1090(3) 0.0450(13) Uani 1 1 d U . . H40 H 0.4571 0.5489 0.1255 0.054 Uiso 1 1 calc R . . C41 C 0.5542(4) 0.5068(3) 0.0980(3) 0.0566(14) Uani 1 1 d U . . H41 H 0.5993 0.5339 0.1070 0.068 Uiso 1 1 calc R . . C42 C 0.5718(4) 0.4575(3) 0.0737(3) 0.0585(15) Uani 1 1 d U . . H42 H 0.6286 0.4517 0.0662 0.070 Uiso 1 1 calc R . . C43 C 0.5049(4) 0.4166(3) 0.0604(3) 0.0557(14) Uani 1 1 d U . . H43 H 0.5171 0.3833 0.0446 0.067 Uiso 1 1 calc R . . C44 C 0.4194(4) 0.4260(2) 0.0710(3) 0.0454(12) Uani 1 1 d U . . H44 H 0.3743 0.3989 0.0615 0.054 Uiso 1 1 calc R . . C45 C 0.2358(3) 0.55952(19) 0.0235(3) 0.0337(11) Uani 1 1 d U . . C46 C 0.1923(4) 0.5432(2) -0.0496(3) 0.0437(12) Uani 1 1 d U . . H46 H 0.1702 0.5083 -0.0601 0.052 Uiso 1 1 calc R . . C47 C 0.1818(4) 0.5786(2) -0.1064(3) 0.0424(12) Uani 1 1 d U . . H47 H 0.1499 0.5677 -0.1546 0.051 Uiso 1 1 calc R . . C48 C 0.2175(4) 0.6296(2) -0.0929(3) 0.0436(12) Uani 1 1 d U . . H48 H 0.2107 0.6529 -0.1314 0.052 Uiso 1 1 calc R . . C49 C 0.2631(4) 0.6455(2) -0.0218(3) 0.0535(14) Uani 1 1 d U . . H49 H 0.2879 0.6798 -0.0120 0.064 Uiso 1 1 calc R . . C50 C 0.2730(4) 0.6107(2) 0.0366(3) 0.0461(13) Uani 1 1 d U . . H50 H 0.3049 0.6221 0.0846 0.055 Uiso 1 1 calc R . . C51 C 0.0680(3) 0.59154(19) 0.0668(3) 0.0335(11) Uani 1 1 d U . . C52 C 0.0206(4) 0.5862(2) -0.0073(3) 0.0474(13) Uani 1 1 d U . . H52 H 0.0056 0.5524 -0.0276 0.057 Uiso 1 1 calc R . . C53 C -0.0054(5) 0.6311(3) -0.0530(3) 0.0628(16) Uani 1 1 d U . . H53 H -0.0378 0.6272 -0.1033 0.075 Uiso 1 1 calc R . . C54 C 0.0172(5) 0.6802(2) -0.0227(4) 0.0602(15) Uani 1 1 d U . . H54 H 0.0002 0.7101 -0.0530 0.072 Uiso 1 1 calc R . . C55 C 0.0647(5) 0.6871(2) 0.0516(4) 0.0624(16) Uani 1 1 d U . . H55 H 0.0786 0.7212 0.0717 0.075 Uiso 1 1 calc R . . C56 C 0.0916(4) 0.6419(2) 0.0965(3) 0.0497(13) Uani 1 1 d U . . H56 H 0.1255 0.6458 0.1466 0.060 Uiso 1 1 calc R . . C57 C -0.0878(3) 0.61257(18) 0.1328(3) 0.0334(11) Uani 1 1 d U . . C58 C -0.1413(4) 0.6144(2) 0.0586(3) 0.0437(12) Uani 1 1 d U . . H58 H -0.1482 0.5838 0.0303 0.052 Uiso 1 1 calc R . . C59 C -0.1849(4) 0.6617(2) 0.0254(3) 0.0501(14) Uani 1 1 d U . . H59 H -0.2197 0.6625 -0.0249 0.060 Uiso 1 1 calc R . . C60 C -0.1770(4) 0.7070(2) 0.0665(3) 0.0471(13) Uani 1 1 d U . . H60 H -0.2073 0.7383 0.0446 0.057 Uiso 1 1 calc R . . C61 C -0.1235(4) 0.7054(2) 0.1405(3) 0.0486(13) Uani 1 1 d U . . H61 H -0.1165 0.7363 0.1684 0.058 Uiso 1 1 calc R . . C62 C -0.0797(4) 0.6586(2) 0.1746(3) 0.0432(12) Uani 1 1 d U . . H62 H -0.0452 0.6579 0.2249 0.052 Uiso 1 1 calc R . . C63 C -0.1231(4) 0.5539(2) 0.2625(3) 0.0432(12) Uani 1 1 d U . . C64 C -0.2164(4) 0.5384(3) 0.2355(3) 0.0569(15) Uani 1 1 d U . . H64 H -0.2399 0.5189 0.1922 0.068 Uiso 1 1 calc R . . C65 C -0.2775(5) 0.5516(3) 0.2725(4) 0.0712(17) Uani 1 1 d U . . H65 H -0.3411 0.5408 0.2538 0.085 Uiso 1 1 calc R . . C66 C -0.2430(5) 0.5805(3) 0.3362(4) 0.0751(18) Uani 1 1 d U . . H66 H -0.2837 0.5902 0.3602 0.090 Uiso 1 1 calc R . . C67 C -0.1493(6) 0.5951(3) 0.3644(4) 0.0842(19) Uani 1 1 d U . . H67 H -0.1257 0.6135 0.4087 0.101 Uiso 1 1 calc R . . C68 C -0.0881(5) 0.5828(3) 0.3276(3) 0.0681(16) Uani 1 1 d U . . H68 H -0.0246 0.5937 0.3464 0.082 Uiso 1 1 calc R . . C69 C 0.0949(4) 0.46702(19) 0.3785(3) 0.0381(11) Uani 1 1 d U . . C70 C 0.1891(4) 0.4590(2) 0.3855(3) 0.0459(13) Uani 1 1 d U . . H70 H 0.2020 0.4453 0.3460 0.055 Uiso 1 1 calc R . . C71 C 0.2645(4) 0.4710(2) 0.4503(3) 0.0530(14) Uani 1 1 d U . . H71 H 0.3270 0.4645 0.4541 0.064 Uiso 1 1 calc R . . C72 C 0.2475(5) 0.4924(3) 0.5087(3) 0.0630(16) Uani 1 1 d U . . H72 H 0.2982 0.5011 0.5517 0.076 Uiso 1 1 calc R . . C73 C 0.1553(5) 0.5008(3) 0.5031(3) 0.0705(17) Uani 1 1 d U . . H73 H 0.1432 0.5151 0.5426 0.085 Uiso 1 1 calc R . . C74 C 0.0790(5) 0.4880(3) 0.4382(3) 0.0605(15) Uani 1 1 d U . . H74 H 0.0166 0.4937 0.4352 0.073 Uiso 1 1 calc R . . C75 C -0.1212(4) 0.3651(2) 0.3382(3) 0.0388(11) Uani 1 1 d U . . C76 C -0.1105(4) 0.3423(2) 0.4051(3) 0.0534(14) Uani 1 1 d U . . H76 H -0.0564 0.3220 0.4299 0.064 Uiso 1 1 calc R . . C77 C -0.1796(5) 0.3494(2) 0.4356(4) 0.0659(16) Uani 1 1 d U . . H77 H -0.1714 0.3342 0.4809 0.079 Uiso 1 1 calc R . . C78 C -0.2604(5) 0.3789(2) 0.3988(4) 0.0609(15) Uani 1 1 d U . . H78 H -0.3073 0.3828 0.4189 0.073 Uiso 1 1 calc R . . C79 C -0.2722(4) 0.4026(2) 0.3326(3) 0.0559(14) Uani 1 1 d U . . H79 H -0.3262 0.4231 0.3082 0.067 Uiso 1 1 calc R . . C80 C -0.2017(4) 0.3955(2) 0.3025(3) 0.0456(12) Uani 1 1 d U . . H80 H -0.2092 0.4115 0.2578 0.055 Uiso 1 1 calc R . . C81 C -0.0572(4) 0.25587(19) 0.3007(3) 0.0366(11) Uani 1 1 d U . . C82 C 0.0006(4) 0.2206(2) 0.3538(3) 0.0444(12) Uani 1 1 d U . . H82 H 0.0658 0.2270 0.3764 0.053 Uiso 1 1 calc R . . C83 C -0.0402(5) 0.1755(2) 0.3729(3) 0.0551(14) Uani 1 1 d U . . H83 H -0.0020 0.1519 0.4081 0.066 Uiso 1 1 calc R . . C84 C -0.1362(5) 0.1662(2) 0.3399(4) 0.0590(15) Uani 1 1 d U . . H84 H -0.1631 0.1368 0.3541 0.071 Uiso 1 1 calc R . . C85 C -0.1934(5) 0.1997(2) 0.2862(4) 0.0601(15) Uani 1 1 d U . . H85 H -0.2580 0.1920 0.2625 0.072 Uiso 1 1 calc R . . C86 C -0.1547(4) 0.2448(2) 0.2673(3) 0.0462(13) Uani 1 1 d U . . H86 H -0.1941 0.2681 0.2321 0.055 Uiso 1 1 calc R . . C87 C 0.0789(3) 0.22738(18) 0.2195(3) 0.0327(10) Uani 1 1 d U . . C88 C 0.1394(4) 0.18746(19) 0.2605(3) 0.0386(11) Uani 1 1 d U . . H88 H 0.1993 0.1964 0.2945 0.046 Uiso 1 1 calc R . . C89 C 0.1110(4) 0.1344(2) 0.2509(3) 0.0512(14) Uani 1 1 d U . . H89 H 0.1521 0.1078 0.2779 0.061 Uiso 1 1 calc R . . C90 C 0.0217(5) 0.1214(2) 0.2012(3) 0.0578(15) Uani 1 1 d U . . H90 H 0.0023 0.0860 0.1955 0.069 Uiso 1 1 calc R . . C91 C -0.0394(4) 0.1601(2) 0.1598(3) 0.0512(14) Uani 1 1 d U . . H91 H -0.0994 0.1508 0.1262 0.061 Uiso 1 1 calc R . . C92 C -0.0110(4) 0.2133(2) 0.1685(3) 0.0394(12) Uani 1 1 d U . . H92 H -0.0518 0.2395 0.1403 0.047 Uiso 1 1 calc R . . C93 C 0.8059(5) 0.6690(2) 0.5445(4) 0.0679(19) Uani 1 1 d . . . H93A H 0.8666 0.6670 0.5855 0.082 Uiso 1 1 calc R . . H93B H 0.7855 0.6329 0.5286 0.082 Uiso 1 1 calc R . . Cl1 Cl 0.82078(19) 0.70308(8) 0.47437(12) 0.1000(8) Uani 1 1 d . . . Cl2 Cl 0.72196(16) 0.69935(13) 0.57299(14) 0.1287(10) 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 N1 0.026(2) 0.033(2) 0.038(2) 0.0022(18) 0.0112(18) 0.0000(17) N2 0.030(2) 0.037(2) 0.042(2) 0.0056(19) 0.0114(19) 0.0049(18) N3 0.031(2) 0.031(2) 0.034(2) 0.0045(18) 0.0110(19) -0.0014(17) N4 0.034(2) 0.025(2) 0.036(2) -0.0012(18) 0.0130(19) -0.0029(17) C1 0.029(3) 0.036(3) 0.030(3) 0.000(2) 0.006(2) 0.001(2) C2 0.029(3) 0.038(3) 0.028(3) 0.003(2) 0.007(2) 0.006(2) C3 0.023(2) 0.037(3) 0.026(2) 0.005(2) 0.004(2) 0.007(2) C4 0.031(3) 0.027(3) 0.033(3) 0.004(2) 0.008(2) 0.001(2) C5 0.025(2) 0.032(3) 0.042(3) 0.012(2) 0.009(2) 0.006(2) C6 0.021(2) 0.035(3) 0.046(3) 0.003(2) 0.008(2) 0.003(2) C7 0.033(3) 0.032(3) 0.045(3) 0.007(2) 0.018(2) 0.006(2) C8 0.031(3) 0.033(3) 0.033(3) 0.007(2) 0.012(2) -0.002(2) C9 0.025(2) 0.037(3) 0.036(3) 0.005(2) 0.008(2) 0.002(2) C10 0.027(2) 0.030(3) 0.028(2) 0.002(2) 0.006(2) 0.002(2) C11 0.029(2) 0.028(3) 0.032(3) 0.001(2) 0.008(2) 0.002(2) C12 0.028(3) 0.030(3) 0.036(3) -0.002(2) 0.007(2) 0.003(2) C13 0.033(3) 0.031(3) 0.033(3) -0.001(2) 0.009(2) 0.000(2) C14 0.029(3) 0.031(3) 0.029(3) 0.002(2) 0.004(2) 0.001(2) C15 0.036(3) 0.029(3) 0.034(3) 0.002(2) 0.014(2) 0.003(2) C16 0.030(3) 0.035(3) 0.029(3) 0.002(2) 0.009(2) -0.001(2) C17 0.032(3) 0.030(3) 0.035(3) 0.000(2) 0.017(2) 0.001(2) C18 0.034(3) 0.027(3) 0.035(3) 0.002(2) 0.013(2) -0.001(2) C19 0.033(3) 0.029(3) 0.031(3) 0.001(2) 0.008(2) 0.001(2) C20 0.027(2) 0.027(3) 0.033(3) 0.003(2) 0.008(2) 0.002(2) C21 0.033(2) 0.035(3) 0.037(3) -0.001(2) 0.011(2) 0.006(2) C22 0.038(3) 0.038(3) 0.039(3) -0.001(2) 0.008(2) 0.008(2) C23 0.046(3) 0.041(3) 0.051(3) -0.004(2) 0.006(2) 0.009(2) C24 0.050(3) 0.044(3) 0.059(3) -0.015(3) 0.009(3) 0.010(2) C25 0.050(3) 0.050(3) 0.053(3) -0.013(3) 0.000(3) 0.002(3) C26 0.038(3) 0.043(3) 0.044(3) -0.009(2) 0.007(2) 0.006(2) C27 0.028(2) 0.038(3) 0.037(3) 0.003(2) 0.012(2) 0.007(2) C28 0.029(2) 0.040(3) 0.041(3) 0.001(2) 0.009(2) 0.005(2) C29 0.032(3) 0.051(3) 0.053(3) 0.000(3) 0.011(2) 0.004(2) C30 0.035(3) 0.062(3) 0.058(3) -0.009(3) 0.020(2) 0.003(3) C31 0.038(3) 0.065(3) 0.051(3) -0.013(3) 0.019(2) 0.006(3) C32 0.034(3) 0.054(3) 0.042(3) -0.006(2) 0.013(2) 0.006(2) C33 0.0474(19) 0.0410(18) 0.0542(18) 0.0050(15) -0.0023(16) -0.0048(16) C34 0.060(2) 0.0448(18) 0.0609(19) 0.0084(16) -0.0123(17) -0.0107(17) C35 0.065(2) 0.0474(18) 0.063(2) 0.0076(15) -0.0163(18) -0.0120(17) C36 0.060(2) 0.0457(18) 0.0590(19) 0.0047(15) -0.0124(17) -0.0073(17) C37 0.052(2) 0.0433(18) 0.0534(18) 0.0028(16) -0.0041(17) -0.0045(16) C38 0.0468(19) 0.0415(18) 0.0513(19) 0.0028(14) 0.0011(16) -0.0041(16) C39 0.029(2) 0.039(3) 0.045(3) 0.009(2) 0.015(2) 0.002(2) C40 0.029(3) 0.051(3) 0.055(3) 0.009(3) 0.015(2) 0.000(2) C41 0.035(3) 0.072(3) 0.063(3) 0.012(3) 0.018(3) -0.001(3) C42 0.036(3) 0.085(4) 0.062(3) 0.018(3) 0.028(3) 0.013(3) C43 0.054(3) 0.063(3) 0.058(3) 0.014(3) 0.031(3) 0.019(3) C44 0.048(3) 0.044(3) 0.049(3) 0.011(2) 0.023(3) 0.008(2) C45 0.034(3) 0.032(2) 0.035(2) 0.003(2) 0.012(2) 0.001(2) C46 0.042(3) 0.044(3) 0.040(3) 0.003(2) 0.009(2) -0.007(2) C47 0.037(3) 0.051(3) 0.038(3) 0.004(2) 0.011(2) -0.001(2) C48 0.046(3) 0.045(3) 0.043(3) 0.008(2) 0.020(2) 0.000(2) C49 0.069(4) 0.042(3) 0.048(3) 0.005(2) 0.021(3) -0.010(3) C50 0.059(3) 0.038(3) 0.040(3) 0.002(2) 0.016(3) -0.007(2) C51 0.032(2) 0.034(2) 0.033(2) 0.006(2) 0.012(2) 0.005(2) C52 0.050(3) 0.046(3) 0.037(3) 0.004(2) 0.006(2) 0.012(3) C53 0.068(4) 0.069(4) 0.048(3) 0.016(3) 0.018(3) 0.023(3) C54 0.069(4) 0.053(3) 0.064(3) 0.029(3) 0.031(3) 0.023(3) C55 0.067(4) 0.042(3) 0.075(4) 0.013(3) 0.022(3) 0.003(3) C56 0.051(3) 0.040(3) 0.055(3) 0.003(2) 0.016(3) -0.001(2) C57 0.031(2) 0.030(2) 0.036(2) 0.003(2) 0.008(2) 0.005(2) C58 0.040(3) 0.038(3) 0.041(3) 0.002(2) 0.001(2) 0.001(2) C59 0.040(3) 0.049(3) 0.046(3) 0.002(2) -0.003(2) 0.006(2) C60 0.047(3) 0.042(3) 0.044(3) 0.004(2) 0.006(2) 0.012(2) C61 0.049(3) 0.036(3) 0.052(3) -0.003(2) 0.008(2) 0.011(2) C62 0.038(3) 0.039(3) 0.048(3) 0.001(2) 0.009(2) 0.007(2) C63 0.047(3) 0.046(3) 0.044(3) 0.008(2) 0.026(3) 0.013(2) C64 0.041(3) 0.077(4) 0.059(3) 0.009(3) 0.026(3) 0.018(3) C65 0.052(3) 0.099(5) 0.074(4) 0.021(3) 0.036(3) 0.027(3) C66 0.075(4) 0.100(5) 0.069(4) 0.019(3) 0.048(3) 0.047(4) C67 0.090(4) 0.099(5) 0.073(4) -0.011(4) 0.042(4) 0.023(4) C68 0.070(4) 0.078(4) 0.062(4) -0.015(3) 0.031(3) 0.007(3) C69 0.044(3) 0.035(3) 0.034(2) 0.001(2) 0.012(2) -0.004(2) C70 0.042(3) 0.037(3) 0.049(3) -0.001(2) 0.005(2) 0.001(2) C71 0.049(3) 0.038(3) 0.056(3) 0.003(3) 0.001(3) -0.004(2) C72 0.069(3) 0.065(4) 0.043(3) 0.001(3) 0.006(3) -0.021(3) C73 0.076(4) 0.097(4) 0.039(3) -0.019(3) 0.021(3) -0.027(4) C74 0.064(3) 0.080(4) 0.042(3) -0.015(3) 0.024(3) -0.018(3) C75 0.039(3) 0.037(3) 0.046(3) -0.003(2) 0.023(2) -0.002(2) C76 0.057(3) 0.054(3) 0.059(3) 0.011(3) 0.033(3) 0.011(3) C77 0.084(4) 0.060(4) 0.075(4) 0.013(3) 0.055(3) 0.009(3) C78 0.060(3) 0.057(4) 0.085(4) -0.005(3) 0.051(3) 0.000(3) C79 0.046(3) 0.059(3) 0.068(3) -0.011(3) 0.028(3) 0.007(3) C80 0.036(3) 0.051(3) 0.051(3) -0.001(2) 0.017(2) 0.004(2) C81 0.038(3) 0.031(3) 0.046(3) -0.005(2) 0.022(2) -0.008(2) C82 0.055(3) 0.032(3) 0.051(3) 0.002(2) 0.026(2) -0.001(2) C83 0.075(3) 0.036(3) 0.062(3) 0.008(3) 0.034(3) -0.002(3) C84 0.075(4) 0.043(3) 0.076(4) -0.002(3) 0.048(3) -0.016(3) C85 0.058(3) 0.049(3) 0.085(4) -0.007(3) 0.040(3) -0.015(3) C86 0.041(3) 0.041(3) 0.062(3) -0.005(2) 0.024(2) -0.009(2) C87 0.034(2) 0.030(2) 0.037(3) -0.001(2) 0.017(2) 0.000(2) C88 0.044(3) 0.033(3) 0.035(3) 0.000(2) 0.010(2) 0.002(2) C89 0.071(3) 0.031(3) 0.050(3) 0.007(2) 0.019(3) 0.005(3) C90 0.076(4) 0.033(3) 0.062(4) -0.004(3) 0.023(3) -0.008(3) C91 0.052(3) 0.043(3) 0.055(3) -0.007(3) 0.016(3) -0.014(2) C92 0.040(3) 0.038(3) 0.039(3) -0.004(2) 0.013(2) -0.008(2) C93 0.059(4) 0.048(4) 0.084(5) 0.015(3) 0.011(4) 0.000(3) Cl1 0.165(2) 0.0659(12) 0.1007(16) -0.0043(11) 0.0859(16) -0.0042(13) Cl2 0.0815(15) 0.212(3) 0.1115(19) 0.0135(19) 0.0578(14) 0.0040(17) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; 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 N1 C4 1.333(6) . ? N1 C1 1.415(6) . ? N2 C6 1.328(6) . ? N2 C9 1.402(6) . ? N3 C14 1.328(6) . ? N3 C11 1.407(6) . ? N4 C16 1.337(6) . ? N4 C19 1.401(6) . ? C1 C20 1.412(6) . ? C1 C2 1.438(6) . ? C2 C3 1.394(6) . ? C2 C21 1.487(7) . ? C3 C4 1.439(6) . ? C3 C27 1.473(6) . ? C4 C5 1.508(6) . ? C5 C6 1.515(6) . ? C5 C33 1.517(7) . ? C6 C7 1.418(7) . ? C7 C8 1.390(6) . ? C7 C39 1.471(6) . ? C8 C9 1.431(6) . ? C8 C45 1.492(6) . ? C9 C10 1.425(6) . ? C10 C11 1.399(6) . ? C10 C51 1.501(6) . ? C11 C12 1.466(6) . ? C12 C13 1.391(6) . ? C12 C57 1.484(6) . ? C13 C14 1.424(6) . ? C13 C63 1.480(7) . ? C14 C15 1.499(6) . ? C15 C16 1.500(6) . ? C15 C69 1.535(6) . ? C16 C17 1.427(6) . ? C17 C18 1.395(6) . ? C17 C75 1.481(6) . ? C18 C19 1.441(6) . ? C18 C81 1.487(6) . ? C19 C20 1.420(6) . ? C20 C87 1.485(6) . ? C21 C22 1.383(6) . ? C21 C26 1.405(7) . ? C22 C23 1.383(7) . ? C23 C24 1.371(7) . ? C24 C25 1.379(7) . ? C25 C26 1.383(7) . ? C27 C32 1.389(7) . ? C27 C28 1.409(6) . ? C28 C29 1.385(7) . ? C29 C30 1.381(7) . ? C30 C31 1.377(7) . ? C31 C32 1.391(7) . ? C33 C34 1.370(7) . ? C33 C38 1.390(7) . ? C34 C35 1.393(8) . ? C35 C36 1.357(8) . ? C36 C37 1.363(8) . ? C37 C38 1.385(7) . ? C39 C44 1.389(7) . ? C39 C40 1.399(7) . ? C40 C41 1.399(7) . ? C41 C42 1.382(8) . ? C42 C43 1.393(8) . ? C43 C44 1.396(7) . ? C45 C50 1.386(7) . ? C45 C46 1.397(7) . ? C46 C47 1.387(7) . ? C47 C48 1.373(7) . ? C48 C49 1.364(7) . ? C49 C50 1.401(7) . ? C51 C52 1.367(7) . ? C51 C56 1.380(7) . ? C52 C53 1.400(7) . ? C53 C54 1.354(8) . ? C54 C55 1.376(8) . ? C55 C56 1.400(7) . ? C57 C58 1.379(6) . ? C57 C62 1.393(7) . ? C58 C59 1.393(7) . ? C59 C60 1.371(7) . ? C60 C61 1.376(7) . ? C61 C62 1.391(7) . ? C63 C64 1.362(8) . ? C63 C68 1.390(8) . ? C64 C65 1.402(8) . ? C65 C66 1.369(9) . ? C66 C67 1.362(10) . ? C67 C68 1.397(9) . ? C69 C74 1.380(7) . ? C69 C70 1.387(7) . ? C70 C71 1.389(7) . ? C71 C72 1.370(8) . ? C72 C73 1.366(9) . ? C73 C74 1.401(8) . ? C75 C76 1.383(7) . ? C75 C80 1.385(7) . ? C76 C77 1.389(8) . ? C77 C78 1.377(8) . ? C78 C79 1.378(8) . ? C79 C80 1.401(7) . ? C81 C86 1.396(7) . ? C81 C82 1.399(7) . ? C82 C83 1.401(7) . ? C83 C84 1.367(8) . ? C84 C85 1.373(8) . ? C85 C86 1.383(7) . ? C87 C88 1.392(6) . ? C87 C92 1.399(6) . ? C88 C89 1.388(7) . ? C89 C90 1.377(8) . ? C90 C91 1.377(8) . ? C91 C92 1.390(7) . ? C93 Cl1 1.700(6) . ? C93 Cl2 1.734(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 C4 N1 C1 107.3(4) . . ? C6 N2 C9 108.6(4) . . ? C14 N3 C11 107.7(4) . . ? C16 N4 C19 109.0(4) . . ? C20 C1 N1 119.9(4) . . ? C20 C1 C2 132.0(4) . . ? N1 C1 C2 107.8(4) . . ? C3 C2 C1 107.6(4) . . ? C3 C2 C21 121.8(4) . . ? C1 C2 C21 130.5(4) . . ? C2 C3 C4 105.5(4) . . ? C2 C3 C27 128.9(4) . . ? C4 C3 C27 125.7(4) . . ? N1 C4 C3 111.6(4) . . ? N1 C4 C5 122.4(4) . . ? C3 C4 C5 125.9(4) . . ? C4 C5 C6 112.4(4) . . ? C4 C5 C33 111.8(4) . . ? C6 C5 C33 114.1(4) . . ? N2 C6 C7 110.1(4) . . ? N2 C6 C5 123.7(4) . . ? C7 C6 C5 126.1(4) . . ? C8 C7 C6 107.0(4) . . ? C8 C7 C39 128.5(4) . . ? C6 C7 C39 124.4(4) . . ? C7 C8 C9 106.8(4) . . ? C7 C8 C45 124.9(4) . . ? C9 C8 C45 128.1(4) . . ? N2 C9 C10 120.9(4) . . ? N2 C9 C8 107.5(4) . . ? C10 C9 C8 131.5(4) . . ? C11 C10 C9 124.2(4) . . ? C11 C10 C51 118.5(4) . . ? C9 C10 C51 117.2(4) . . ? C10 C11 N3 121.3(4) . . ? C10 C11 C12 130.5(4) . . ? N3 C11 C12 107.9(4) . . ? C13 C12 C11 105.7(4) . . ? C13 C12 C57 123.7(4) . . ? C11 C12 C57 130.5(4) . . ? C12 C13 C14 107.2(4) . . ? C12 C13 C63 128.9(4) . . ? C14 C13 C63 123.9(4) . . ? N3 C14 C13 111.5(4) . . ? N3 C14 C15 123.4(4) . . ? C13 C14 C15 125.0(4) . . ? C16 C15 C14 115.8(4) . . ? C16 C15 C69 110.7(4) . . ? C14 C15 C69 111.6(4) . . ? N4 C16 C17 110.1(4) . . ? N4 C16 C15 123.7(4) . . ? C17 C16 C15 125.9(4) . . ? C18 C17 C16 106.7(4) . . ? C18 C17 C75 126.9(4) . . ? C16 C17 C75 126.4(4) . . ? C17 C18 C19 107.1(4) . . ? C17 C18 C81 122.2(4) . . ? C19 C18 C81 130.6(4) . . ? N4 C19 C20 121.7(4) . . ? N4 C19 C18 107.2(4) . . ? C20 C19 C18 131.1(4) . . ? C1 C20 C19 124.4(4) . . ? C1 C20 C87 118.6(4) . . ? C19 C20 C87 117.0(4) . . ? C22 C21 C26 118.4(5) . . ? C22 C21 C2 119.9(4) . . ? C26 C21 C2 121.5(4) . . ? C21 C22 C23 122.0(5) . . ? C24 C23 C22 118.8(5) . . ? C23 C24 C25 120.7(5) . . ? C24 C25 C26 120.7(5) . . ? C25 C26 C21 119.4(5) . . ? C32 C27 C28 117.6(4) . . ? C32 C27 C3 121.6(4) . . ? C28 C27 C3 120.7(4) . . ? C29 C28 C27 121.3(5) . . ? C30 C29 C28 119.9(5) . . ? C31 C30 C29 119.6(5) . . ? C30 C31 C32 120.9(5) . . ? C27 C32 C31 120.6(5) . . ? C34 C33 C38 116.1(5) . . ? C34 C33 C5 121.6(5) . . ? C38 C33 C5 122.2(5) . . ? C33 C34 C35 121.5(6) . . ? C36 C35 C34 120.7(6) . . ? C35 C36 C37 119.4(6) . . ? C36 C37 C38 119.5(6) . . ? C37 C38 C33 122.5(5) . . ? C44 C39 C40 118.6(5) . . ? C44 C39 C7 121.0(5) . . ? C40 C39 C7 120.2(5) . . ? C41 C40 C39 120.4(5) . . ? C42 C41 C40 120.0(6) . . ? C41 C42 C43 120.4(5) . . ? C42 C43 C44 119.2(6) . . ? C39 C44 C43 121.3(5) . . ? C50 C45 C46 117.8(5) . . ? C50 C45 C8 122.1(4) . . ? C46 C45 C8 120.1(4) . . ? C47 C46 C45 120.3(5) . . ? C48 C47 C46 121.4(5) . . ? C49 C48 C47 118.8(5) . . ? C48 C49 C50 120.9(5) . . ? C45 C50 C49 120.7(5) . . ? C52 C51 C56 119.3(5) . . ? C52 C51 C10 121.9(5) . . ? C56 C51 C10 118.8(4) . . ? C51 C52 C53 120.9(5) . . ? C54 C53 C52 118.9(6) . . ? C53 C54 C55 121.8(6) . . ? C54 C55 C56 118.6(6) . . ? C51 C56 C55 120.4(5) . . ? C58 C57 C62 118.8(5) . . ? C58 C57 C12 122.4(4) . . ? C62 C57 C12 118.8(4) . . ? C57 C58 C59 120.8(5) . . ? C60 C59 C58 120.4(5) . . ? C59 C60 C61 119.1(5) . . ? C60 C61 C62 121.2(5) . . ? C61 C62 C57 119.6(5) . . ? C64 C63 C68 119.6(5) . . ? C64 C63 C13 121.7(5) . . ? C68 C63 C13 118.6(5) . . ? C63 C64 C65 120.6(6) . . ? C66 C65 C64 119.7(7) . . ? C67 C66 C65 120.0(6) . . ? C66 C67 C68 120.8(7) . . ? C63 C68 C67 119.3(7) . . ? C74 C69 C70 117.4(5) . . ? C74 C69 C15 119.9(5) . . ? C70 C69 C15 122.7(5) . . ? C69 C70 C71 121.3(6) . . ? C72 C71 C70 120.5(6) . . ? C71 C72 C73 119.2(6) . . ? C72 C73 C74 120.4(6) . . ? C69 C74 C73 121.1(6) . . ? C76 C75 C80 118.8(5) . . ? C76 C75 C17 120.3(5) . . ? C80 C75 C17 120.9(5) . . ? C75 C76 C77 120.7(6) . . ? C78 C77 C76 120.0(6) . . ? C77 C78 C79 120.5(6) . . ? C78 C79 C80 119.1(6) . . ? C75 C80 C79 121.0(5) . . ? C86 C81 C82 118.8(5) . . ? C86 C81 C18 119.8(5) . . ? C82 C81 C18 121.0(5) . . ? C81 C82 C83 119.7(5) . . ? C84 C83 C82 120.1(6) . . ? C83 C84 C85 120.8(5) . . ? C84 C85 C86 119.9(6) . . ? C85 C86 C81 120.6(6) . . ? C88 C87 C92 119.0(4) . . ? C88 C87 C20 121.8(4) . . ? C92 C87 C20 119.2(4) . . ? C89 C88 C87 120.5(5) . . ? C90 C89 C88 119.5(5) . . ? C91 C90 C89 121.1(5) . . ? C90 C91 C92 119.6(5) . . ? C91 C92 C87 120.2(5) . . ? Cl1 C93 Cl2 111.5(4) . . ? #==END=========================================================================