# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Takuji Ogawa' _publ_contact_author_address ; Department of Chemistry Graduate School of Science Osaka University Machikaneyama1-1 Toyonaka Osaka 560-0043 Japan ; _publ_contact_author_email ogawa@chem.sci.osaka-u.ac.jp _publ_contact_author_fax +81-6-6850-5395 _publ_contact_author_phone +81-6-6850-5392 _publ_section_title 'Structure of Tb(TPP)(TPPH)' _publ_author_address ; Department of Chemistry Graduate School of Science Osaka University Machikaneyama1-1 Toyonaka Osaka 560-0043 Japan ; loop_ _publ_author_name 'Daisuke Tanaka' 'Tomoko Inose' 'Hirofumi Tanaka' 'Sunri Lee' 'Naoto Ishikawa' 'Takuji Ogawa' data_compound _database_code_depnum_ccdc_archive 'CCDC 862023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H61 Cl12 N8 Tb' _chemical_formula_weight 1862.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0300(5) _cell_length_b 17.0927(5) _cell_length_c 30.0170(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.7771(8) _cell_angle_gamma 90.00 _cell_volume 8220.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31428 _cell_measurement_theta_min 6.01 _cell_measurement_theta_max 54.92 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3752 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8807 _exptl_absorpt_correction_T_max 0.9619 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IP _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62010 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14442 _reflns_number_gt 9945 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _refine_special_details ; Due to the high disordering of the chloroforms, we employed the restrain to get the reasonable structure using the following commands in SHELX format. DFIX 1.75 C92 Cl10 C92 Cl11 C92 Cl12 DANG 2.88 Cl10 Cl11 Cl11 Cl12 Cl12 Cl10 DFIX 1.75 C91 Cl7 C91 Cl8 C91 Cl9 DANG 2.88 Cl7 Cl8 Cl8 Cl9 Cl9 Cl7 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^)+(0.1201P)^2^+62.6478P] 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 14442 _refine_ls_number_parameters 1010 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2120 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.17553(2) 0.24788(2) 0.640413(11) 0.02331(15) Uani 1 1 d . . . Cl1 Cl 0.2863(3) 0.5293(3) 0.60256(19) 0.0663(16) Uiso 0.70 1 d P A 2 Cl2 Cl 0.4268(3) 0.4357(3) 0.61488(17) 0.0625(13) Uiso 0.70 1 d P A 2 Cl3 Cl -0.0081(3) -0.0006(3) 0.55516(15) 0.0579(12) Uiso 0.70 1 d P B 1 Cl4 Cl 0.3384(4) 0.4784(4) 0.6947(2) 0.0756(19) Uiso 0.70 1 d P A 2 N1 N 0.3109(4) 0.2568(4) 0.6052(2) 0.0256(15) Uani 1 1 d . . . Cl5 Cl -0.0422(3) 0.0477(3) 0.64653(16) 0.0723(12) Uiso 0.70 1 d P B 1 C1 C -0.0336(5) 0.2536(5) 0.6019(3) 0.0282(17) Uani 1 1 d . . . N6 N 0.0148(4) 0.2371(4) 0.6394(2) 0.0269(15) Uani 1 1 d . . . C2 C -0.0401(6) 0.2428(5) 0.6737(3) 0.0332(19) Uani 1 1 d . . . C3 C -0.0087(5) 0.2462(4) 0.5570(3) 0.0272(17) Uani 1 1 d . . . N2 N 0.2794(4) 0.2655(4) 0.7010(2) 0.0280(15) Uani 1 1 d . . . Cl6 Cl 0.0821(4) -0.0641(4) 0.6265(2) 0.0998(17) Uiso 0.70 1 d P B 1 C4 C 0.4054(6) 0.2446(5) 0.5491(3) 0.038(2) Uani 1 1 d . . . H41 H 0.4288 0.2472 0.5205 0.045 Uiso 1 1 calc R . . N7 N 0.1243(4) 0.1788(4) 0.5725(2) 0.0263(14) Uani 1 1 d . . . C5 C 0.1995(5) 0.3555(5) 0.5452(2) 0.0274(17) Uani 1 1 d . . . C6 C -0.0896(6) 0.2388(5) 0.7518(3) 0.035(2) Uani 1 1 d . . . N5 N 0.1104(4) 0.1544(4) 0.7094(2) 0.0292(15) Uani 1 1 d . . . H66 H 0.1138 0.1595 0.6804 0.035 Uiso 1 1 calc R . . C7 C 0.1761(6) 0.1365(5) 0.5461(3) 0.0333(19) Uani 1 1 d . . . C8 C 0.0917(5) 0.4407(5) 0.5416(3) 0.0288(18) Uani 1 1 d . . . H42 H 0.0503 0.4770 0.5317 0.035 Uiso 1 1 calc R . . N4 N 0.1671(4) 0.3559(4) 0.58757(19) 0.0252(14) Uani 1 1 d . . . C9 C 0.0647(5) 0.2111(5) 0.5442(2) 0.0275(17) Uani 1 1 d . . . C10 C 0.3085(5) 0.0010(5) 0.6189(3) 0.035(2) Uani 1 1 d . . . H43 H 0.3379 -0.0323 0.5994 0.042 Uiso 1 1 calc R . . N3 N 0.1320(4) 0.3612(4) 0.6827(2) 0.0266(14) Uani 1 1 d . . . C11 C 0.3254(6) 0.2566(6) 0.7742(3) 0.042(2) Uani 1 1 d . . . H44 H 0.3257 0.2597 0.8058 0.051 Uiso 1 1 calc R . . N8 N 0.2243(4) 0.1012(4) 0.6431(2) 0.0294(15) Uani 1 1 d . . . C12 C 0.1372(6) 0.3706(5) 0.7283(3) 0.0321(19) Uani 1 1 d . . . C13 C 0.1963(5) 0.3338(5) 0.7575(2) 0.0282(18) Uani 1 1 d . . . C14 C 0.1027(5) 0.4100(5) 0.5864(3) 0.0269(17) Uani 1 1 d . . . C15 C -0.1141(6) 0.3155(6) 0.7618(3) 0.047(2) Uani 1 1 d . . . H1 H -0.0886 0.3583 0.7473 0.057 Uiso 1 1 calc R . . C16 C 0.0756(5) 0.4168(5) 0.6680(2) 0.0281(18) Uani 1 1 d . . . C17 C -0.0725(5) 0.2671(5) 0.5208(3) 0.0313(19) Uani 1 1 d . . . C18 C 0.2708(5) 0.3171(5) 0.5327(3) 0.0315(18) Uani 1 1 d . . . C19 C 0.2399(5) -0.0255(5) 0.7883(3) 0.0334(19) Uani 1 1 d . . . H2 H 0.1809 -0.0302 0.7857 0.040 Uiso 1 1 calc R . . C20 C -0.1230(5) 0.2668(5) 0.6576(3) 0.036(2) Uani 1 1 d . . . H45 H -0.1705 0.2762 0.6750 0.043 Uiso 1 1 calc R . . C21 C 0.2549(5) 0.0587(5) 0.6791(3) 0.0306(18) Uani 1 1 d . . . C22 C 0.2341(5) 0.0689(5) 0.7241(3) 0.0289(18) Uani 1 1 d . . . C23 C 0.1679(5) 0.1154(5) 0.7376(3) 0.0308(18) Uani 1 1 d . . . C24 C -0.0995(5) 0.3435(5) 0.5136(3) 0.036(2) Uani 1 1 d . . . H3 H -0.0789 0.3846 0.5322 0.043 Uiso 1 1 calc R . . C25 C 0.0806(6) 0.4309(5) 0.7421(3) 0.035(2) Uani 1 1 d . . . H46 H 0.0720 0.4475 0.7718 0.042 Uiso 1 1 calc R . . C26 C 0.2786(6) 0.0346(5) 0.5259(3) 0.034(2) Uani 1 1 d . . . C27 C 0.0419(6) 0.4593(5) 0.7048(3) 0.034(2) Uani 1 1 d . . . H47 H 0.0008 0.4994 0.7032 0.041 Uiso 1 1 calc R . . C28 C 0.0694(5) 0.1704(5) 0.7807(3) 0.0312(18) Uani 1 1 d . . . H48 H 0.0386 0.1863 0.8056 0.037 Uiso 1 1 calc R . . C29 C -0.1291(6) 0.1785(6) 0.7734(3) 0.046(2) Uani 1 1 d . . . H4 H -0.1141 0.1260 0.7670 0.055 Uiso 1 1 calc R . . C30 C 0.2621(5) 0.2861(5) 0.7439(3) 0.0295(18) Uani 1 1 d . . . C31 C 0.4054(5) 0.2099(5) 0.6670(3) 0.035(2) Uani 1 1 d . . . C32 C 0.3836(5) 0.2238(5) 0.6224(3) 0.0336(19) Uani 1 1 d . . . C33 C 0.2370(5) 0.0838(5) 0.5612(3) 0.0287(18) Uani 1 1 d . . . C34 C -0.1884(6) 0.3018(6) 0.4529(3) 0.043(2) Uani 1 1 d . . . H5 H -0.2282 0.3140 0.4298 0.051 Uiso 1 1 calc R . . C35 C 0.1514(5) 0.4083(5) 0.5166(3) 0.0313(19) Uani 1 1 d . . . H49 H 0.1601 0.4182 0.4860 0.038 Uiso 1 1 calc R . . C36 C 0.0831(6) 0.1928(5) 0.4984(3) 0.035(2) Uani 1 1 d . . . H50 H 0.0534 0.2105 0.4724 0.042 Uiso 1 1 calc R . . C37 C 0.2570(5) 0.0657(5) 0.6060(3) 0.0312(18) Uani 1 1 d . . . C38 C -0.0242(5) 0.2226(5) 0.7191(3) 0.0294(18) Uani 1 1 d . . . C39 C 0.3242(5) 0.2729(5) 0.5610(3) 0.0296(18) Uani 1 1 d . . . C40 C 0.1994(6) 0.3598(5) 0.8048(3) 0.037(2) Uani 1 1 d . . . C41 C 0.2825(6) -0.0673(5) 0.8214(3) 0.041(2) Uani 1 1 d . . . H6 H 0.2531 -0.0990 0.8416 0.049 Uiso 1 1 calc R . . C42 C 0.0002(5) 0.5051(5) 0.6150(2) 0.0295(18) Uani 1 1 d . . . C43 C 0.0593(5) 0.4382(5) 0.6233(3) 0.0274(17) Uani 1 1 d . . . C44 C -0.1387(6) 0.5580(6) 0.6079(3) 0.044(2) Uani 1 1 d . . . H7 H -0.1975 0.5506 0.6075 0.053 Uiso 1 1 calc R . . C45 C 0.3079(5) -0.0041(5) 0.6637(3) 0.035(2) Uani 1 1 d . . . H51 H 0.3367 -0.0416 0.6817 0.042 Uiso 1 1 calc R . . C46 C 0.1439(5) 0.1303(5) 0.7819(3) 0.0322(19) Uani 1 1 d . . . H52 H 0.1744 0.1151 0.8081 0.039 Uiso 1 1 calc R . . C47 C 0.1416(6) 0.3404(5) 0.8354(3) 0.041(2) Uani 1 1 d . . . H8 H 0.0968 0.3069 0.8267 0.050 Uiso 1 1 calc R . . C48 C -0.1566(6) 0.3594(6) 0.4790(3) 0.047(2) Uani 1 1 d . . . H9 H -0.1736 0.4119 0.4736 0.056 Uiso 1 1 calc R . . C49 C 0.3681(6) 0.0272(6) 0.7626(3) 0.043(2) Uani 1 1 d . . . H10 H 0.3979 0.0593 0.7427 0.052 Uiso 1 1 calc R . . C50 C 0.2107(8) 0.4176(6) 0.8915(3) 0.058(3) Uani 1 1 d . . . H11 H 0.2145 0.4372 0.9211 0.070 Uiso 1 1 calc R . . C51 C -0.2112(8) 0.2685(8) 0.8145(4) 0.067(3) Uani 1 1 d . . . H12 H -0.2508 0.2783 0.8368 0.080 Uiso 1 1 calc R . . C52 C 0.2805(5) 0.0228(5) 0.7588(3) 0.0317(19) Uani 1 1 d . . . C53 C 0.3597(7) 0.3538(8) 0.4003(3) 0.058(3) Uani 1 1 d . . . H13 H 0.3795 0.3620 0.3712 0.069 Uiso 1 1 calc R . . C54 C -0.1755(7) 0.3297(7) 0.7927(3) 0.058(3) Uani 1 1 d . . . H14 H -0.1925 0.3818 0.7986 0.069 Uiso 1 1 calc R . . C55 C -0.1064(7) 0.6324(6) 0.6011(3) 0.048(3) Uani 1 1 d . . . H15 H -0.1428 0.6757 0.5965 0.057 Uiso 1 1 calc R . . C56 C 0.3568(6) 0.2306(5) 0.7034(3) 0.034(2) Uani 1 1 d . . . C57 C 0.1508(6) 0.1457(5) 0.4999(3) 0.036(2) Uani 1 1 d . . . H53 H 0.1770 0.1228 0.4751 0.043 Uiso 1 1 calc R . . C58 C 0.2361(6) -0.0273(5) 0.5069(3) 0.043(2) Uani 1 1 d . . . H16 H 0.1819 -0.0395 0.5168 0.052 Uiso 1 1 calc R . . C59 C -0.0205(7) 0.6427(5) 0.6011(3) 0.046(2) Uani 1 1 d . . . H17 H 0.0024 0.6931 0.5961 0.055 Uiso 1 1 calc R . . C60 C 0.3573(7) 0.0511(7) 0.5110(3) 0.055(3) Uani 1 1 d . . . H18 H 0.3882 0.0932 0.5239 0.065 Uiso 1 1 calc R . . C61 C 0.3007(5) 0.3305(5) 0.4860(3) 0.0331(19) Uani 1 1 d . . . C62 C 0.2939(7) 0.2744(7) 0.4534(3) 0.055(3) Uani 1 1 d . . . H19 H 0.2687 0.2259 0.4605 0.066 Uiso 1 1 calc R . . C63 C 0.0473(5) 0.1836(5) 0.7350(2) 0.0296(18) Uani 1 1 d . . . C64 C 0.3850(6) 0.2234(6) 0.7491(3) 0.041(2) Uani 1 1 d . . . H54 H 0.4355 0.1999 0.7597 0.050 Uiso 1 1 calc R . . C65 C 0.5516(7) 0.2284(7) 0.6944(4) 0.056(3) Uani 1 1 d . . . H20 H 0.5394 0.2823 0.6982 0.067 Uiso 1 1 calc R . . C66 C -0.1180(5) 0.2729(5) 0.6130(3) 0.035(2) Uani 1 1 d . . . H55 H -0.1619 0.2873 0.5927 0.043 Uiso 1 1 calc R . . C67 C 0.3694(6) -0.0618(6) 0.8245(3) 0.046(2) Uani 1 1 d . . . H21 H 0.3997 -0.0904 0.8468 0.055 Uiso 1 1 calc R . . C68 C -0.1897(7) 0.1924(7) 0.8042(4) 0.060(3) Uani 1 1 d . . . H22 H -0.2166 0.1499 0.8182 0.072 Uiso 1 1 calc R . . C69 C 0.5097(6) 0.1002(6) 0.6719(3) 0.051(3) Uani 1 1 d . . . H23 H 0.4684 0.0658 0.6597 0.061 Uiso 1 1 calc R . . C70 C 0.1463(7) 0.3683(5) 0.8791(3) 0.047(3) Uani 1 1 d . . . H24 H 0.1058 0.3534 0.8999 0.057 Uiso 1 1 calc R . . C71 C 0.4904(6) 0.1782(6) 0.6773(3) 0.041(2) Uani 1 1 d . . . C72 C 0.0315(6) 0.5792(5) 0.6084(3) 0.035(2) Uani 1 1 d . . . H25 H 0.0902 0.5868 0.6090 0.042 Uiso 1 1 calc R . . C73 C -0.1051(6) 0.2071(6) 0.4932(3) 0.042(2) Uani 1 1 d . . . H26 H -0.0873 0.1546 0.4977 0.051 Uiso 1 1 calc R . . C74 C 0.4111(6) -0.0153(6) 0.7954(3) 0.049(3) Uani 1 1 d . . . H27 H 0.4703 -0.0121 0.7976 0.059 Uiso 1 1 calc R . . C75 C 0.3220(8) 0.2851(8) 0.4107(3) 0.064(3) Uani 1 1 d . . . H28 H 0.3151 0.2451 0.3889 0.076 Uiso 1 1 calc R . . C76 C 0.3917(7) 0.0075(7) 0.4775(4) 0.061(3) Uani 1 1 d . . . H29 H 0.4454 0.0203 0.4672 0.073 Uiso 1 1 calc R . . C77 C 0.2675(11) 0.4379(9) 0.8625(4) 0.095(5) Uani 1 1 d . . . H30 H 0.3108 0.4731 0.8713 0.114 Uiso 1 1 calc R . . C78 C -0.1634(7) 0.2251(6) 0.4595(3) 0.052(3) Uani 1 1 d . . . H31 H -0.1861 0.1847 0.4410 0.062 Uiso 1 1 calc R . . C79 C 0.2702(7) -0.0727(6) 0.4734(3) 0.052(3) Uani 1 1 d . . . H32 H 0.2400 -0.1155 0.4607 0.063 Uiso 1 1 calc R . . C80 C 0.3481(7) -0.0544(6) 0.4591(3) 0.051(3) Uani 1 1 d . . . H33 H 0.3722 -0.0847 0.4363 0.061 Uiso 1 1 calc R . . C81 C 0.3689(8) 0.4108(7) 0.4317(4) 0.071(4) Uani 1 1 d . . . H34 H 0.3948 0.4589 0.4245 0.085 Uiso 1 1 calc R . . C82 C 0.6331(7) 0.1993(11) 0.7062(4) 0.080(4) Uani 1 1 d . . . H35 H 0.6756 0.2332 0.7176 0.096 Uiso 1 1 calc R . . C83 C -0.0864(5) 0.4947(6) 0.6151(3) 0.037(2) Uani 1 1 d . . . H36 H -0.1091 0.4443 0.6202 0.044 Uiso 1 1 calc R . . C84 C 0.317(2) 0.456(2) 0.6474(12) 0.032(9) Uiso 0.30 1 d P C 1 H57 H 0.2777 0.4107 0.6503 0.039 Uiso 0.30 1 calc PR C 1 C85 C 0.3398(8) 0.3983(7) 0.4749(3) 0.061(3) Uani 1 1 d . . . H37 H 0.3476 0.4380 0.4968 0.073 Uiso 1 1 calc R . . C86 C 0.2643(9) 0.4080(8) 0.8191(3) 0.076(4) Uani 1 1 d . . . H38 H 0.3072 0.4209 0.7992 0.091 Uiso 1 1 calc R . . C87 C 0.0332(11) 0.0187(10) 0.6059(5) 0.048(4) Uiso 0.70 1 d P B 1 H58 H 0.0756 0.0612 0.6033 0.058 Uiso 0.70 1 calc PR B 1 C88 C 0.5882(7) 0.0707(8) 0.6838(4) 0.067(3) Uani 1 1 d . . . H39 H 0.6000 0.0166 0.6804 0.081 Uiso 1 1 calc R . . C89 C 0.6480(8) 0.1208(9) 0.7005(4) 0.074(4) Uani 1 1 d . . . H40 H 0.7017 0.1006 0.7084 0.089 Uiso 1 1 calc R . . Cl7 Cl 0.2857(5) 0.5847(4) 0.44161(19) 0.164(3) Uani 1 1 d D . . Cl8 Cl 0.3482(4) 0.7274(4) 0.4205(3) 0.195(4) Uani 1 1 d D . . Cl9 Cl 0.4327(4) 0.6209(5) 0.4919(3) 0.206(4) Uani 1 1 d D . . C90 C 0.4419(6) 0.2140(6) 0.5863(3) 0.039(2) Uani 1 1 d . . . H56 H 0.4955 0.1904 0.5885 0.047 Uiso 1 1 calc R . . C91 C 0.3459(10) 0.6594(9) 0.4627(7) 0.175(12) Uani 1 1 d D . . H64 H 0.3113 0.6841 0.4860 0.210 Uiso 1 1 calc R . . Cl10 Cl 0.4114(6) 0.6756(5) 0.0554(4) 0.283(6) Uani 1 1 d D . . Cl11 Cl 0.4210(5) 0.7928(5) 0.1306(5) 0.343(9) Uani 1 1 d D . . Cl12 Cl 0.4928(6) 0.6499(6) 0.1457(8) 0.512(17) Uani 1 1 d D . . C92 C 0.4645(12) 0.7097(13) 0.1030(6) 0.29(3) Uani 1 1 d D . . H65 H 0.5187 0.7294 0.0918 0.350 Uiso 1 1 calc R . . Cl13 Cl -0.0848(6) 0.0643(5) 0.6373(3) 0.050(2) Uiso 0.30 1 d P D 2 Cl14 Cl -0.0330(6) 0.0195(6) 0.5560(3) 0.045(2) Uiso 0.30 1 d P D 2 Cl15 Cl 0.4179(6) 0.4192(6) 0.6293(3) 0.047(2) Uiso 0.30 1 d P C 1 Cl16 Cl 0.0595(7) -0.0340(6) 0.6447(4) 0.064(2) Uiso 0.30 1 d P D 2 Cl17 Cl 0.2689(6) 0.5301(5) 0.6143(3) 0.040(2) Uiso 0.30 1 d P C 1 Cl18 Cl 0.3262(9) 0.5022(9) 0.6958(5) 0.068(4) Uiso 0.30 1 d P C 1 C93 C 0.005(2) 0.0347(19) 0.6117(10) 0.031(7) Uiso 0.30 1 d P D 2 H61 H 0.0419 0.0820 0.6107 0.037 Uiso 0.30 1 calc PR D 2 C94 C 0.3300(11) 0.4545(10) 0.6355(6) 0.043(5) Uiso 0.70 1 d P A 2 H62 H 0.2948 0.4066 0.6317 0.052 Uiso 0.70 1 calc PR A 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 Tb1 0.0282(2) 0.0254(2) 0.0163(2) 0.00023(15) -0.00093(15) 0.00171(16) N1 0.021(3) 0.030(4) 0.027(3) 0.007(3) 0.005(3) 0.004(3) C1 0.032(4) 0.029(4) 0.023(4) -0.001(3) 0.001(3) 0.001(4) N6 0.026(3) 0.031(4) 0.024(3) -0.002(3) 0.002(3) 0.002(3) C2 0.037(5) 0.031(5) 0.031(4) 0.001(4) -0.007(4) 0.007(4) C3 0.033(4) 0.027(4) 0.022(4) -0.001(3) -0.005(3) 0.001(3) N2 0.030(4) 0.036(4) 0.018(3) 0.002(3) -0.001(3) -0.004(3) C4 0.038(5) 0.045(5) 0.031(5) 0.005(4) 0.009(4) 0.004(4) N7 0.029(4) 0.030(4) 0.019(3) 0.000(3) -0.003(3) 0.001(3) C5 0.034(4) 0.031(4) 0.018(4) -0.002(3) -0.005(3) 0.002(4) C6 0.039(5) 0.045(5) 0.022(4) 0.008(4) 0.002(4) 0.013(4) N5 0.033(4) 0.037(4) 0.018(3) 0.000(3) 0.000(3) 0.005(3) C7 0.044(5) 0.030(4) 0.026(4) -0.004(3) 0.004(4) 0.006(4) C8 0.034(4) 0.026(4) 0.027(4) 0.001(3) -0.007(4) 0.000(3) N4 0.031(4) 0.028(3) 0.016(3) 0.006(3) -0.002(3) 0.001(3) C9 0.039(5) 0.030(4) 0.014(4) 0.004(3) -0.002(3) -0.001(4) C10 0.039(5) 0.033(5) 0.033(4) -0.003(4) 0.007(4) 0.005(4) N3 0.033(4) 0.028(4) 0.019(3) 0.003(3) -0.002(3) 0.002(3) C11 0.043(5) 0.061(6) 0.023(4) 0.001(4) -0.005(4) -0.002(5) N8 0.033(4) 0.034(4) 0.021(3) -0.001(3) -0.002(3) 0.000(3) C12 0.045(5) 0.029(4) 0.023(4) -0.003(3) 0.006(4) -0.004(4) C13 0.041(5) 0.027(4) 0.017(4) 0.005(3) -0.003(3) -0.003(4) C14 0.029(4) 0.027(4) 0.025(4) 0.004(3) 0.000(3) -0.001(3) C15 0.057(6) 0.046(6) 0.041(5) 0.003(4) 0.015(5) 0.016(5) C16 0.040(5) 0.025(4) 0.019(4) -0.001(3) 0.002(3) -0.001(4) C17 0.032(4) 0.041(5) 0.021(4) 0.004(3) -0.004(3) -0.001(4) C18 0.036(5) 0.037(5) 0.022(4) 0.005(3) 0.004(4) 0.001(4) C19 0.032(4) 0.034(5) 0.033(4) 0.005(4) -0.008(4) 0.003(4) C20 0.027(4) 0.046(5) 0.035(5) 0.003(4) 0.007(4) 0.011(4) C21 0.034(5) 0.034(5) 0.024(4) 0.001(3) -0.003(3) 0.006(4) C22 0.024(4) 0.032(4) 0.030(4) 0.000(3) -0.004(3) 0.003(3) C23 0.039(5) 0.031(4) 0.022(4) 0.005(3) -0.007(4) -0.002(4) C24 0.042(5) 0.032(5) 0.033(4) 0.000(4) -0.008(4) -0.006(4) C25 0.055(6) 0.026(4) 0.023(4) 0.001(3) 0.007(4) 0.005(4) C26 0.046(5) 0.033(5) 0.024(4) -0.002(4) 0.001(4) 0.008(4) C27 0.050(5) 0.027(4) 0.025(4) 0.001(3) 0.003(4) 0.010(4) C28 0.041(5) 0.030(4) 0.024(4) 0.003(3) 0.005(4) 0.002(4) C29 0.039(5) 0.049(6) 0.051(6) 0.014(5) 0.007(5) 0.006(4) C30 0.031(4) 0.037(5) 0.021(4) 0.005(3) -0.006(3) -0.001(4) C31 0.033(5) 0.036(5) 0.036(5) 0.005(4) -0.005(4) 0.000(4) C32 0.026(4) 0.037(5) 0.039(5) 0.002(4) 0.004(4) 0.004(4) C33 0.035(5) 0.027(4) 0.024(4) -0.004(3) -0.002(3) 0.000(4) C34 0.043(5) 0.044(6) 0.041(5) 0.010(4) -0.016(4) 0.001(4) C35 0.041(5) 0.034(5) 0.019(4) 0.006(3) -0.002(4) 0.002(4) C36 0.049(5) 0.037(5) 0.019(4) -0.003(3) -0.003(4) 0.004(4) C37 0.038(5) 0.032(4) 0.024(4) -0.001(3) 0.002(4) 0.000(4) C38 0.033(4) 0.029(4) 0.027(4) -0.001(3) 0.000(4) -0.003(4) C39 0.026(4) 0.039(5) 0.024(4) 0.002(3) 0.003(3) 0.002(4) C40 0.053(6) 0.038(5) 0.019(4) 0.002(4) -0.003(4) -0.003(4) C41 0.050(6) 0.036(5) 0.036(5) 0.009(4) -0.006(4) 0.002(4) C42 0.039(5) 0.036(5) 0.013(3) -0.002(3) 0.001(3) 0.014(4) C43 0.033(4) 0.026(4) 0.024(4) -0.001(3) 0.005(3) 0.000(3) C44 0.041(5) 0.066(7) 0.025(4) -0.004(4) -0.005(4) 0.021(5) C45 0.043(5) 0.036(5) 0.026(4) 0.003(4) 0.001(4) 0.014(4) C46 0.042(5) 0.032(4) 0.023(4) 0.008(3) -0.003(4) -0.001(4) C47 0.060(6) 0.038(5) 0.026(4) 0.000(4) -0.002(4) -0.010(4) C48 0.049(6) 0.042(6) 0.049(6) 0.018(5) -0.011(5) -0.003(5) C49 0.038(5) 0.056(6) 0.035(5) 0.018(4) 0.001(4) 0.002(4) C50 0.103(9) 0.052(6) 0.020(5) -0.005(4) 0.000(5) -0.022(6) C51 0.057(7) 0.105(11) 0.038(6) 0.006(6) 0.016(5) 0.009(7) C52 0.034(5) 0.034(5) 0.027(4) 0.004(4) 0.001(4) 0.011(4) C53 0.050(6) 0.090(9) 0.034(5) 0.019(6) 0.019(5) 0.017(6) C54 0.060(7) 0.066(7) 0.048(6) -0.011(5) 0.014(5) 0.019(6) C55 0.075(8) 0.047(6) 0.021(4) -0.001(4) -0.002(5) 0.025(5) C56 0.035(5) 0.041(5) 0.027(4) 0.002(4) -0.005(4) 0.000(4) C57 0.051(5) 0.041(5) 0.016(4) -0.001(4) 0.004(4) 0.003(4) C58 0.055(6) 0.039(5) 0.035(5) -0.007(4) 0.006(4) 0.010(5) C59 0.075(7) 0.029(5) 0.033(5) 0.007(4) 0.009(5) 0.022(5) C60 0.052(6) 0.063(7) 0.050(6) -0.008(5) 0.010(5) 0.004(5) C61 0.040(5) 0.042(5) 0.018(4) 0.007(4) 0.004(4) 0.009(4) C62 0.071(7) 0.058(6) 0.037(5) -0.003(5) 0.018(5) -0.009(6) C63 0.043(5) 0.027(4) 0.019(4) 0.001(3) 0.002(4) 0.004(4) C64 0.036(5) 0.057(6) 0.031(5) 0.012(4) -0.011(4) 0.004(4) C65 0.042(6) 0.065(7) 0.061(7) 0.004(6) -0.010(5) 0.004(5) C66 0.026(4) 0.046(5) 0.034(5) 0.005(4) -0.004(4) 0.006(4) C67 0.045(6) 0.049(6) 0.043(5) 0.018(5) -0.008(4) 0.014(5) C68 0.048(6) 0.073(8) 0.061(7) 0.020(6) 0.021(6) 0.000(6) C69 0.046(6) 0.058(7) 0.049(6) 0.005(5) -0.003(5) 0.012(5) C70 0.086(8) 0.033(5) 0.025(4) 0.007(4) 0.017(5) 0.000(5) C71 0.034(5) 0.054(6) 0.036(5) 0.014(4) 0.003(4) 0.003(4) C72 0.041(5) 0.035(5) 0.030(4) 0.004(4) 0.007(4) 0.007(4) C73 0.054(6) 0.036(5) 0.036(5) 0.000(4) -0.017(4) -0.003(4) C74 0.031(5) 0.065(7) 0.051(6) 0.013(5) -0.007(4) 0.009(5) C75 0.074(8) 0.085(9) 0.033(5) -0.009(6) 0.017(5) -0.001(7) C76 0.047(6) 0.076(8) 0.060(7) -0.009(6) 0.020(5) 0.018(6) C77 0.150(14) 0.101(11) 0.036(6) -0.022(6) 0.018(8) -0.072(10) C78 0.061(7) 0.052(6) 0.041(5) -0.002(5) -0.025(5) -0.009(5) C79 0.069(7) 0.049(6) 0.039(5) -0.015(5) 0.011(5) 0.004(5) C80 0.072(7) 0.051(6) 0.030(5) -0.001(4) 0.011(5) 0.031(6) C81 0.100(10) 0.065(8) 0.049(7) 0.016(6) 0.031(7) -0.017(7) C82 0.040(6) 0.140(14) 0.060(8) 0.002(8) -0.009(6) -0.002(8) C83 0.038(5) 0.045(5) 0.027(4) -0.004(4) 0.000(4) 0.003(4) C85 0.092(9) 0.054(7) 0.037(5) -0.007(5) 0.020(6) -0.019(6) C86 0.101(10) 0.096(10) 0.031(5) -0.015(6) 0.014(6) -0.051(8) C88 0.051(7) 0.077(8) 0.075(8) 0.018(7) 0.007(6) 0.036(6) C89 0.045(7) 0.106(11) 0.071(8) 0.013(8) -0.002(6) 0.031(7) Cl7 0.221(7) 0.152(5) 0.117(4) -0.039(4) -0.030(4) 0.082(5) Cl8 0.094(4) 0.161(6) 0.331(11) -0.030(7) 0.030(5) -0.025(4) Cl9 0.120(5) 0.191(7) 0.304(10) -0.042(7) -0.029(6) -0.045(5) C90 0.037(5) 0.046(5) 0.033(5) 0.004(4) 0.000(4) 0.004(4) C91 0.095(14) 0.086(14) 0.35(4) 0.053(19) 0.045(19) -0.017(11) Cl10 0.240(9) 0.168(7) 0.434(16) 0.101(9) -0.107(10) -0.105(7) Cl11 0.131(6) 0.170(7) 0.74(3) -0.045(12) 0.198(11) -0.022(5) Cl12 0.174(8) 0.149(8) 1.19(5) 0.100(16) -0.298(17) -0.037(6) C92 0.070(15) 0.50(7) 0.31(4) -0.23(5) 0.07(2) -0.10(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 Tb1 N3 2.431(6) . ? Tb1 N4 2.435(6) . ? Tb1 N2 2.447(6) . ? Tb1 N1 2.448(6) . ? Tb1 N7 2.475(6) . ? Tb1 N6 2.583(7) . ? Tb1 N8 2.627(7) . ? Tb1 N5 2.841(7) . ? Cl1 C94 1.749(18) . ? Cl2 C94 1.719(19) . ? Cl3 C87 1.674(17) . ? Cl4 C94 1.824(19) . ? N1 C39 1.378(10) . ? N1 C32 1.379(10) . ? Cl5 C87 1.813(18) . ? C1 N6 1.376(10) . ? C1 C3 1.422(11) . ? C1 C66 1.441(12) . ? N6 C2 1.377(11) . ? C2 C38 1.421(11) . ? C2 C20 1.458(12) . ? C3 C9 1.385(11) . ? C3 C17 1.513(11) . ? N2 C30 1.371(10) . ? N2 C56 1.376(11) . ? Cl6 C87 1.723(18) . ? C4 C90 1.349(13) . ? C4 C39 1.444(12) . ? C4 H41 0.9500 . ? N7 C7 1.370(10) . ? N7 C9 1.373(10) . ? C5 C18 1.380(11) . ? C5 N4 1.389(9) . ? C5 C35 1.450(11) . ? C6 C29 1.383(13) . ? C6 C15 1.404(12) . ? C6 C38 1.485(12) . ? N5 C63 1.380(10) . ? N5 C23 1.401(10) . ? N5 H66 0.8800 . ? C7 C33 1.393(12) . ? C7 C57 1.442(11) . ? C8 C35 1.353(12) . ? C8 C14 1.448(11) . ? C8 H42 0.9500 . ? N4 C14 1.386(10) . ? C9 C36 1.449(11) . ? C10 C45 1.349(11) . ? C10 C37 1.427(12) . ? C10 H43 0.9500 . ? N3 C16 1.376(10) . ? N3 C12 1.377(10) . ? C11 C64 1.359(14) . ? C11 C30 1.433(12) . ? C11 H44 0.9500 . ? N8 C21 1.378(10) . ? N8 C37 1.384(10) . ? C12 C13 1.416(12) . ? C12 C25 1.442(12) . ? C13 C30 1.404(12) . ? C13 C40 1.489(11) . ? C14 C43 1.411(11) . ? C15 C54 1.395(13) . ? C15 H1 0.9500 . ? C16 C43 1.407(11) . ? C16 C27 1.443(11) . ? C17 C24 1.391(12) . ? C17 C73 1.407(12) . ? C18 C39 1.407(11) . ? C18 C61 1.513(10) . ? C19 C41 1.385(12) . ? C19 C52 1.387(12) . ? C19 H2 0.9500 . ? C20 C66 1.349(12) . ? C20 H45 0.9500 . ? C21 C22 1.413(11) . ? C21 C45 1.453(11) . ? C22 C23 1.395(11) . ? C22 C52 1.488(11) . ? C23 C46 1.418(11) . ? C24 C48 1.389(12) . ? C24 H3 0.9500 . ? C25 C27 1.353(12) . ? C25 H46 0.9500 . ? C26 C58 1.373(13) . ? C26 C60 1.380(13) . ? C26 C33 1.524(11) . ? C27 H47 0.9500 . ? C28 C46 1.377(12) . ? C28 C63 1.425(11) . ? C28 H48 0.9500 . ? C29 C68 1.383(14) . ? C29 H4 0.9500 . ? C31 C32 1.394(12) . ? C31 C56 1.408(12) . ? C31 C71 1.491(12) . ? C32 C90 1.463(12) . ? C33 C37 1.409(11) . ? C34 C48 1.348(13) . ? C34 C78 1.384(14) . ? C34 H5 0.9500 . ? C35 H49 0.9500 . ? C36 C57 1.351(12) . ? C36 H50 0.9500 . ? C38 C63 1.397(12) . ? C40 C47 1.366(12) . ? C40 C86 1.384(14) . ? C41 C67 1.396(13) . ? C41 H6 0.9500 . ? C42 C72 1.379(12) . ? C42 C83 1.399(12) . ? C42 C43 1.501(11) . ? C44 C83 1.383(13) . ? C44 C55 1.389(15) . ? C44 H7 0.9500 . ? C45 H51 0.9500 . ? C46 H52 0.9500 . ? C47 C70 1.394(12) . ? C47 H8 0.9500 . ? C48 H9 0.9500 . ? C49 C74 1.388(13) . ? C49 C52 1.408(12) . ? C49 H10 0.9500 . ? C50 C77 1.324(16) . ? C50 C70 1.375(15) . ? C50 H11 0.9500 . ? C51 C54 1.369(17) . ? C51 C68 1.383(17) . ? C51 H12 0.9500 . ? C53 C75 1.360(17) . ? C53 C81 1.360(16) . ? C53 H13 0.9500 . ? C54 H14 0.9500 . ? C55 C59 1.390(15) . ? C55 H15 0.9500 . ? C56 C64 1.436(12) . ? C57 H53 0.9500 . ? C58 C79 1.395(12) . ? C58 H16 0.9500 . ? C59 C72 1.381(12) . ? C59 H17 0.9500 . ? C60 C76 1.378(14) . ? C60 H18 0.9500 . ? C61 C85 1.363(13) . ? C61 C62 1.372(13) . ? C62 C75 1.386(14) . ? C62 H19 0.9500 . ? C64 H54 0.9500 . ? C65 C71 1.389(14) . ? C65 C82 1.432(16) . ? C65 H20 0.9500 . ? C66 H55 0.9500 . ? C67 C74 1.371(14) . ? C67 H21 0.9500 . ? C68 H22 0.9500 . ? C69 C71 1.379(14) . ? C69 C88 1.392(14) . ? C69 H23 0.9500 . ? C70 H24 0.9500 . ? C72 H25 0.9500 . ? C73 C78 1.392(13) . ? C73 H26 0.9500 . ? C74 H27 0.9500 . ? C75 H28 0.9500 . ? C76 C80 1.375(16) . ? C76 H29 0.9500 . ? C77 C86 1.400(14) . ? C77 H30 0.9500 . ? C78 H31 0.9500 . ? C79 C80 1.369(15) . ? C79 H32 0.9500 . ? C80 H33 0.9500 . ? C81 C85 1.408(14) . ? C81 H34 0.9500 . ? C82 C89 1.37(2) . ? C82 H35 0.9500 . ? C83 H36 0.9500 . ? C84 Cl18 1.66(4) . ? C84 Cl17 1.78(4) . ? C84 Cl15 1.83(4) . ? C84 H57 1.0000 . ? C85 H37 0.9500 . ? C86 H38 0.9500 . ? C87 H58 1.0000 . ? C88 C89 1.369(19) . ? C88 H39 0.9500 . ? C89 H40 0.9500 . ? Cl7 C91 1.709(15) . ? Cl8 C91 1.720(15) . ? Cl9 C91 1.751(14) . ? C90 H56 0.9500 . ? C91 H64 1.0000 . ? Cl10 C92 1.742(16) . ? Cl11 C92 1.796(17) . ? Cl12 C92 1.688(18) . ? C92 H65 1.0000 . ? Cl13 C93 1.73(4) . ? Cl14 C93 1.78(3) . ? Cl16 C93 1.75(3) . ? C93 H61 1.0000 . ? C94 H62 1.0000 . ? 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 N3 Tb1 N4 74.1(2) . . ? N3 Tb1 N2 73.3(2) . . ? N4 Tb1 N2 114.4(2) . . ? N3 Tb1 N1 116.7(2) . . ? N4 Tb1 N1 72.8(2) . . ? N2 Tb1 N1 73.8(2) . . ? N3 Tb1 N7 135.9(2) . . ? N4 Tb1 N7 79.3(2) . . ? N2 Tb1 N7 150.7(2) . . ? N1 Tb1 N7 87.1(2) . . ? N3 Tb1 N6 76.1(2) . . ? N4 Tb1 N6 90.6(2) . . ? N2 Tb1 N6 132.3(2) . . ? N1 Tb1 N6 153.8(2) . . ? N7 Tb1 N6 69.6(2) . . ? N3 Tb1 N8 146.5(2) . . ? N4 Tb1 N8 139.0(2) . . ? N2 Tb1 N8 84.2(2) . . ? N1 Tb1 N8 78.8(2) . . ? N7 Tb1 N8 70.2(2) . . ? N6 Tb1 N8 103.2(2) . . ? N3 Tb1 N5 87.07(19) . . ? N4 Tb1 N5 152.5(2) . . ? N2 Tb1 N5 77.5(2) . . ? N1 Tb1 N5 134.49(19) . . ? N7 Tb1 N5 102.3(2) . . ? N6 Tb1 N5 65.1(2) . . ? N8 Tb1 N5 63.67(19) . . ? C39 N1 C32 106.7(6) . . ? C39 N1 Tb1 126.4(5) . . ? C32 N1 Tb1 124.3(5) . . ? N6 C1 C3 126.1(7) . . ? N6 C1 C66 111.5(7) . . ? C3 C1 C66 122.2(7) . . ? C1 N6 C2 103.9(6) . . ? C1 N6 Tb1 122.1(5) . . ? C2 N6 Tb1 130.3(5) . . ? N6 C2 C38 126.9(8) . . ? N6 C2 C20 111.7(7) . . ? C38 C2 C20 121.2(8) . . ? C9 C3 C1 124.6(7) . . ? C9 C3 C17 117.6(7) . . ? C1 C3 C17 117.1(7) . . ? C30 N2 C56 105.7(6) . . ? C30 N2 Tb1 125.2(5) . . ? C56 N2 Tb1 125.2(5) . . ? C90 C4 C39 107.3(8) . . ? C90 C4 H41 126.4 . . ? C39 C4 H41 126.4 . . ? C7 N7 C9 106.2(6) . . ? C7 N7 Tb1 122.4(5) . . ? C9 N7 Tb1 121.6(5) . . ? C18 C5 N4 125.9(7) . . ? C18 C5 C35 124.5(7) . . ? N4 C5 C35 109.3(7) . . ? C29 C6 C15 117.4(8) . . ? C29 C6 C38 121.0(8) . . ? C15 C6 C38 121.6(8) . . ? C63 N5 C23 108.5(6) . . ? C63 N5 Tb1 119.6(5) . . ? C23 N5 Tb1 117.2(5) . . ? C63 N5 H66 125.7 . . ? C23 N5 H66 125.7 . . ? Tb1 N5 H66 35.5 . . ? N7 C7 C33 125.9(7) . . ? N7 C7 C57 109.9(7) . . ? C33 C7 C57 123.7(7) . . ? C35 C8 C14 107.4(7) . . ? C35 C8 H42 126.3 . . ? C14 C8 H42 126.3 . . ? C14 N4 C5 106.2(6) . . ? C14 N4 Tb1 123.3(5) . . ? C5 N4 Tb1 125.3(5) . . ? N7 C9 C3 125.6(7) . . ? N7 C9 C36 109.9(7) . . ? C3 C9 C36 123.8(7) . . ? C45 C10 C37 107.3(7) . . ? C45 C10 H43 126.4 . . ? C37 C10 H43 126.4 . . ? C16 N3 C12 105.0(6) . . ? C16 N3 Tb1 125.3(5) . . ? C12 N3 Tb1 127.1(5) . . ? C64 C11 C30 106.9(8) . . ? C64 C11 H44 126.5 . . ? C30 C11 H44 126.5 . . ? C21 N8 C37 105.3(7) . . ? C21 N8 Tb1 128.8(5) . . ? C37 N8 Tb1 120.8(5) . . ? N3 C12 C13 125.5(7) . . ? N3 C12 C25 110.4(7) . . ? C13 C12 C25 123.7(7) . . ? C30 C13 C12 125.0(7) . . ? C30 C13 C40 116.5(7) . . ? C12 C13 C40 117.4(7) . . ? N4 C14 C43 126.3(7) . . ? N4 C14 C8 109.6(7) . . ? C43 C14 C8 123.8(7) . . ? C54 C15 C6 120.9(10) . . ? C54 C15 H1 119.6 . . ? C6 C15 H1 119.6 . . ? N3 C16 C43 126.0(7) . . ? N3 C16 C27 111.0(7) . . ? C43 C16 C27 122.5(7) . . ? C24 C17 C73 119.0(8) . . ? C24 C17 C3 122.3(7) . . ? C73 C17 C3 118.7(8) . . ? C5 C18 C39 125.8(7) . . ? C5 C18 C61 117.9(7) . . ? C39 C18 C61 115.9(7) . . ? C41 C19 C52 122.2(8) . . ? C41 C19 H2 118.9 . . ? C52 C19 H2 118.9 . . ? C66 C20 C2 105.5(7) . . ? C66 C20 H45 127.2 . . ? C2 C20 H45 127.2 . . ? N8 C21 C22 126.5(7) . . ? N8 C21 C45 109.8(7) . . ? C22 C21 C45 123.6(7) . . ? C23 C22 C21 123.5(7) . . ? C23 C22 C52 117.8(7) . . ? C21 C22 C52 118.5(7) . . ? C22 C23 N5 126.1(7) . . ? C22 C23 C46 127.3(8) . . ? N5 C23 C46 106.7(7) . . ? C48 C24 C17 119.6(8) . . ? C48 C24 H3 120.2 . . ? C17 C24 H3 120.2 . . ? C27 C25 C12 107.2(7) . . ? C27 C25 H46 126.4 . . ? C12 C25 H46 126.4 . . ? C58 C26 C60 118.1(8) . . ? C58 C26 C33 119.4(8) . . ? C60 C26 C33 122.5(8) . . ? C25 C27 C16 106.3(7) . . ? C25 C27 H47 126.8 . . ? C16 C27 H47 126.8 . . ? C46 C28 C63 107.0(7) . . ? C46 C28 H48 126.5 . . ? C63 C28 H48 126.5 . . ? C68 C29 C6 121.8(10) . . ? C68 C29 H4 119.1 . . ? C6 C29 H4 119.1 . . ? N2 C30 C13 126.6(7) . . ? N2 C30 C11 110.2(7) . . ? C13 C30 C11 123.0(7) . . ? C32 C31 C56 125.1(8) . . ? C32 C31 C71 117.6(8) . . ? C56 C31 C71 117.0(8) . . ? N1 C32 C31 127.7(8) . . ? N1 C32 C90 108.8(7) . . ? C31 C32 C90 123.1(8) . . ? C7 C33 C37 126.0(7) . . ? C7 C33 C26 116.7(7) . . ? C37 C33 C26 116.9(7) . . ? C48 C34 C78 120.5(8) . . ? C48 C34 H5 119.8 . . ? C78 C34 H5 119.8 . . ? C8 C35 C5 107.4(7) . . ? C8 C35 H49 126.3 . . ? C5 C35 H49 126.3 . . ? C57 C36 C9 106.5(7) . . ? C57 C36 H50 126.8 . . ? C9 C36 H50 126.8 . . ? N8 C37 C33 126.3(7) . . ? N8 C37 C10 110.7(7) . . ? C33 C37 C10 122.7(7) . . ? C63 C38 C2 124.3(8) . . ? C63 C38 C6 116.8(7) . . ? C2 C38 C6 118.7(7) . . ? N1 C39 C18 125.4(7) . . ? N1 C39 C4 109.8(7) . . ? C18 C39 C4 124.5(7) . . ? C47 C40 C86 117.1(8) . . ? C47 C40 C13 124.5(8) . . ? C86 C40 C13 118.4(8) . . ? C19 C41 C67 118.8(9) . . ? C19 C41 H6 120.6 . . ? C67 C41 H6 120.6 . . ? C72 C42 C83 118.9(8) . . ? C72 C42 C43 119.6(8) . . ? C83 C42 C43 121.6(8) . . ? C14 C43 C16 125.3(7) . . ? C14 C43 C42 117.0(7) . . ? C16 C43 C42 116.9(7) . . ? C83 C44 C55 120.8(9) . . ? C83 C44 H7 119.6 . . ? C55 C44 H7 119.6 . . ? C10 C45 C21 106.9(7) . . ? C10 C45 H51 126.5 . . ? C21 C45 H51 126.5 . . ? C28 C46 C23 109.0(7) . . ? C28 C46 H52 125.5 . . ? C23 C46 H52 125.5 . . ? C40 C47 C70 122.1(9) . . ? C40 C47 H8 118.9 . . ? C70 C47 H8 118.9 . . ? C34 C48 C24 121.3(9) . . ? C34 C48 H9 119.3 . . ? C24 C48 H9 119.3 . . ? C74 C49 C52 120.1(8) . . ? C74 C49 H10 120.0 . . ? C52 C49 H10 120.0 . . ? C77 C50 C70 120.6(9) . . ? C77 C50 H11 119.7 . . ? C70 C50 H11 119.7 . . ? C54 C51 C68 120.0(10) . . ? C54 C51 H12 120.0 . . ? C68 C51 H12 120.0 . . ? C19 C52 C49 117.8(8) . . ? C19 C52 C22 121.9(8) . . ? C49 C52 C22 120.3(7) . . ? C75 C53 C81 120.0(9) . . ? C75 C53 H13 120.0 . . ? C81 C53 H13 120.0 . . ? C51 C54 C15 120.0(11) . . ? C51 C54 H14 120.0 . . ? C15 C54 H14 120.0 . . ? C44 C55 C59 119.3(9) . . ? C44 C55 H15 120.3 . . ? C59 C55 H15 120.3 . . ? N2 C56 C31 126.0(7) . . ? N2 C56 C64 110.1(8) . . ? C31 C56 C64 123.7(8) . . ? C36 C57 C7 107.4(7) . . ? C36 C57 H53 126.3 . . ? C7 C57 H53 126.3 . . ? C26 C58 C79 121.8(10) . . ? C26 C58 H16 119.1 . . ? C79 C58 H16 119.1 . . ? C72 C59 C55 119.6(9) . . ? C72 C59 H17 120.2 . . ? C55 C59 H17 120.2 . . ? C76 C60 C26 121.0(11) . . ? C76 C60 H18 119.5 . . ? C26 C60 H18 119.5 . . ? C85 C61 C62 116.5(8) . . ? C85 C61 C18 121.2(8) . . ? C62 C61 C18 122.2(8) . . ? C61 C62 C75 123.2(11) . . ? C61 C62 H19 118.4 . . ? C75 C62 H19 118.4 . . ? N5 C63 C38 126.2(7) . . ? N5 C63 C28 108.2(7) . . ? C38 C63 C28 125.5(7) . . ? C11 C64 C56 106.7(8) . . ? C11 C64 H54 126.6 . . ? C56 C64 H54 126.6 . . ? C71 C65 C82 120.3(12) . . ? C71 C65 H20 119.8 . . ? C82 C65 H20 119.8 . . ? C20 C66 C1 107.3(7) . . ? C20 C66 H55 126.4 . . ? C1 C66 H55 126.4 . . ? C74 C67 C41 120.1(8) . . ? C74 C67 H21 119.9 . . ? C41 C67 H21 119.9 . . ? C51 C68 C29 119.8(10) . . ? C51 C68 H22 120.1 . . ? C29 C68 H22 120.1 . . ? C71 C69 C88 121.5(11) . . ? C71 C69 H23 119.2 . . ? C88 C69 H23 119.2 . . ? C50 C70 C47 118.8(9) . . ? C50 C70 H24 120.6 . . ? C47 C70 H24 120.6 . . ? C69 C71 C65 118.9(9) . . ? C69 C71 C31 122.2(9) . . ? C65 C71 C31 118.9(9) . . ? C42 C72 C59 121.6(9) . . ? C42 C72 H25 119.2 . . ? C59 C72 H25 119.2 . . ? C78 C73 C17 119.8(9) . . ? C78 C73 H26 120.1 . . ? C17 C73 H26 120.1 . . ? C67 C74 C49 120.9(9) . . ? C67 C74 H27 119.5 . . ? C49 C74 H27 119.5 . . ? C53 C75 C62 118.9(11) . . ? C53 C75 H28 120.5 . . ? C62 C75 H28 120.5 . . ? C80 C76 C60 120.0(10) . . ? C80 C76 H29 120.0 . . ? C60 C76 H29 120.0 . . ? C50 C77 C86 120.7(12) . . ? C50 C77 H30 119.6 . . ? C86 C77 H30 119.6 . . ? C34 C78 C73 119.8(9) . . ? C34 C78 H31 120.1 . . ? C73 C78 H31 120.1 . . ? C80 C79 C58 118.7(10) . . ? C80 C79 H32 120.7 . . ? C58 C79 H32 120.7 . . ? C79 C80 C76 120.5(9) . . ? C79 C80 H33 119.8 . . ? C76 C80 H33 119.8 . . ? C53 C81 C85 119.8(11) . . ? C53 C81 H34 120.1 . . ? C85 C81 H34 120.1 . . ? C89 C82 C65 118.0(13) . . ? C89 C82 H35 121.0 . . ? C65 C82 H35 121.0 . . ? C44 C83 C42 119.8(9) . . ? C44 C83 H36 120.1 . . ? C42 C83 H36 120.1 . . ? Cl18 C84 Cl17 99.8(19) . . ? Cl18 C84 Cl15 112(2) . . ? Cl17 C84 Cl15 117(2) . . ? Cl18 C84 H57 109.4 . . ? Cl17 C84 H57 109.4 . . ? Cl15 C84 H57 109.4 . . ? C61 C85 C81 121.5(10) . . ? C61 C85 H37 119.3 . . ? C81 C85 H37 119.3 . . ? C40 C86 C77 120.6(11) . . ? C40 C86 H38 119.7 . . ? C77 C86 H38 119.7 . . ? Cl3 C87 Cl6 109.2(10) . . ? Cl3 C87 Cl5 114.4(10) . . ? Cl6 C87 Cl5 106.7(9) . . ? Cl3 C87 H58 108.8 . . ? Cl6 C87 H58 108.8 . . ? Cl5 C87 H58 108.8 . . ? C89 C88 C69 119.1(12) . . ? C89 C88 H39 120.5 . . ? C69 C88 H39 120.5 . . ? C88 C89 C82 122.2(11) . . ? C88 C89 H40 118.9 . . ? C82 C89 H40 118.9 . . ? C4 C90 C32 107.3(8) . . ? C4 C90 H56 126.3 . . ? C32 C90 H56 126.3 . . ? Cl7 C91 Cl8 104.9(11) . . ? Cl7 C91 Cl9 109.6(9) . . ? Cl8 C91 Cl9 126.0(10) . . ? Cl7 C91 H64 104.8 . . ? Cl8 C91 H64 104.8 . . ? Cl9 C91 H64 104.8 . . ? Cl12 C92 Cl10 122.1(15) . . ? Cl12 C92 Cl11 103.3(11) . . ? Cl10 C92 Cl11 117.1(13) . . ? Cl12 C92 H65 104.1 . . ? Cl10 C92 H65 104.1 . . ? Cl11 C92 H65 104.1 . . ? Cl13 C93 Cl16 110.6(17) . . ? Cl13 C93 Cl14 101.0(17) . . ? Cl16 C93 Cl14 126(2) . . ? Cl13 C93 H61 106.0 . . ? Cl16 C93 H61 106.0 . . ? Cl14 C93 H61 106.0 . . ? Cl2 C94 Cl1 106.5(10) . . ? Cl2 C94 Cl4 110.7(10) . . ? Cl1 C94 Cl4 113.8(10) . . ? Cl2 C94 H62 108.6 . . ? Cl1 C94 H62 108.6 . . ? Cl4 C94 H62 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Tb1 N1 C39 -100.7(6) . . . . ? N4 Tb1 N1 C39 -39.2(6) . . . . ? N2 Tb1 N1 C39 -162.0(7) . . . . ? N7 Tb1 N1 C39 40.4(6) . . . . ? N6 Tb1 N1 C39 13.6(9) . . . . ? N8 Tb1 N1 C39 110.8(6) . . . . ? N5 Tb1 N1 C39 144.9(6) . . . . ? N3 Tb1 N1 C32 100.2(7) . . . . ? N4 Tb1 N1 C32 161.7(7) . . . . ? N2 Tb1 N1 C32 38.9(6) . . . . ? N7 Tb1 N1 C32 -118.6(7) . . . . ? N6 Tb1 N1 C32 -145.4(6) . . . . ? N8 Tb1 N1 C32 -48.3(6) . . . . ? N5 Tb1 N1 C32 -14.2(8) . . . . ? C3 C1 N6 C2 -171.9(8) . . . . ? C66 C1 N6 C2 2.6(9) . . . . ? C3 C1 N6 Tb1 27.8(10) . . . . ? C66 C1 N6 Tb1 -157.7(5) . . . . ? N3 Tb1 N6 C1 106.2(6) . . . . ? N4 Tb1 N6 C1 32.8(6) . . . . ? N2 Tb1 N6 C1 157.5(5) . . . . ? N1 Tb1 N6 C1 -16.8(8) . . . . ? N7 Tb1 N6 C1 -45.6(5) . . . . ? N8 Tb1 N6 C1 -108.3(6) . . . . ? N5 Tb1 N6 C1 -160.6(6) . . . . ? N3 Tb1 N6 C2 -48.4(6) . . . . ? N4 Tb1 N6 C2 -121.8(7) . . . . ? N2 Tb1 N6 C2 2.9(8) . . . . ? N1 Tb1 N6 C2 -171.4(6) . . . . ? N7 Tb1 N6 C2 159.9(7) . . . . ? N8 Tb1 N6 C2 97.2(6) . . . . ? N5 Tb1 N6 C2 44.8(6) . . . . ? C1 N6 C2 C38 172.3(8) . . . . ? Tb1 N6 C2 C38 -29.7(12) . . . . ? C1 N6 C2 C20 -2.8(9) . . . . ? Tb1 N6 C2 C20 155.2(6) . . . . ? N6 C1 C3 C9 9.2(13) . . . . ? C66 C1 C3 C9 -164.7(8) . . . . ? N6 C1 C3 C17 179.6(7) . . . . ? C66 C1 C3 C17 5.7(11) . . . . ? N3 Tb1 N2 C30 40.0(6) . . . . ? N4 Tb1 N2 C30 103.2(6) . . . . ? N1 Tb1 N2 C30 165.1(7) . . . . ? N7 Tb1 N2 C30 -143.6(6) . . . . ? N6 Tb1 N2 C30 -12.3(8) . . . . ? N8 Tb1 N2 C30 -114.9(6) . . . . ? N5 Tb1 N2 C30 -50.6(6) . . . . ? N3 Tb1 N2 C56 -165.3(7) . . . . ? N4 Tb1 N2 C56 -102.1(6) . . . . ? N1 Tb1 N2 C56 -40.2(6) . . . . ? N7 Tb1 N2 C56 11.1(9) . . . . ? N6 Tb1 N2 C56 142.4(6) . . . . ? N8 Tb1 N2 C56 39.8(6) . . . . ? N5 Tb1 N2 C56 104.1(7) . . . . ? N3 Tb1 N7 C7 153.6(6) . . . . ? N4 Tb1 N7 C7 100.2(6) . . . . ? N2 Tb1 N7 C7 -21.5(8) . . . . ? N1 Tb1 N7 C7 27.2(6) . . . . ? N6 Tb1 N7 C7 -165.1(6) . . . . ? N8 Tb1 N7 C7 -52.0(6) . . . . ? N5 Tb1 N7 C7 -107.8(6) . . . . ? N3 Tb1 N7 C9 12.6(7) . . . . ? N4 Tb1 N7 C9 -40.9(6) . . . . ? N2 Tb1 N7 C9 -162.5(5) . . . . ? N1 Tb1 N7 C9 -113.9(6) . . . . ? N6 Tb1 N7 C9 53.9(6) . . . . ? N8 Tb1 N7 C9 167.0(6) . . . . ? N5 Tb1 N7 C9 111.1(6) . . . . ? N3 Tb1 N5 C63 26.1(6) . . . . ? N4 Tb1 N5 C63 -19.9(8) . . . . ? N2 Tb1 N5 C63 99.7(6) . . . . ? N1 Tb1 N5 C63 151.5(5) . . . . ? N7 Tb1 N5 C63 -110.3(6) . . . . ? N6 Tb1 N5 C63 -49.9(6) . . . . ? N8 Tb1 N5 C63 -170.6(6) . . . . ? N3 Tb1 N5 C23 -108.5(6) . . . . ? N4 Tb1 N5 C23 -154.5(5) . . . . ? N2 Tb1 N5 C23 -35.0(5) . . . . ? N1 Tb1 N5 C23 16.9(7) . . . . ? N7 Tb1 N5 C23 115.1(5) . . . . ? N6 Tb1 N5 C23 175.4(6) . . . . ? N8 Tb1 N5 C23 54.7(5) . . . . ? C9 N7 C7 C33 -168.8(8) . . . . ? Tb1 N7 C7 C33 45.1(11) . . . . ? C9 N7 C7 C57 3.0(9) . . . . ? Tb1 N7 C7 C57 -143.1(6) . . . . ? C18 C5 N4 C14 171.8(8) . . . . ? C35 C5 N4 C14 -2.5(9) . . . . ? C18 C5 N4 Tb1 -33.2(11) . . . . ? C35 C5 N4 Tb1 152.5(5) . . . . ? N3 Tb1 N4 C14 -42.4(6) . . . . ? N2 Tb1 N4 C14 -105.2(6) . . . . ? N1 Tb1 N4 C14 -167.7(6) . . . . ? N7 Tb1 N4 C14 102.0(6) . . . . ? N6 Tb1 N4 C14 32.9(6) . . . . ? N8 Tb1 N4 C14 144.1(5) . . . . ? N5 Tb1 N4 C14 5.9(8) . . . . ? N3 Tb1 N4 C5 166.6(6) . . . . ? N2 Tb1 N4 C5 103.8(6) . . . . ? N1 Tb1 N4 C5 41.3(6) . . . . ? N7 Tb1 N4 C5 -49.0(6) . . . . ? N6 Tb1 N4 C5 -118.0(6) . . . . ? N8 Tb1 N4 C5 -6.9(8) . . . . ? N5 Tb1 N4 C5 -145.1(6) . . . . ? C7 N7 C9 C3 167.3(8) . . . . ? Tb1 N7 C9 C3 -46.3(10) . . . . ? C7 N7 C9 C36 -4.1(9) . . . . ? Tb1 N7 C9 C36 142.4(6) . . . . ? C1 C3 C9 N7 -0.4(13) . . . . ? C17 C3 C9 N7 -170.8(7) . . . . ? C1 C3 C9 C36 169.7(8) . . . . ? C17 C3 C9 C36 -0.6(12) . . . . ? N4 Tb1 N3 C16 40.4(6) . . . . ? N2 Tb1 N3 C16 162.7(6) . . . . ? N1 Tb1 N3 C16 101.2(6) . . . . ? N7 Tb1 N3 C16 -14.7(7) . . . . ? N6 Tb1 N3 C16 -54.3(6) . . . . ? N8 Tb1 N3 C16 -147.4(6) . . . . ? N5 Tb1 N3 C16 -119.4(6) . . . . ? N4 Tb1 N3 C12 -160.8(7) . . . . ? N2 Tb1 N3 C12 -38.4(6) . . . . ? N1 Tb1 N3 C12 -100.0(7) . . . . ? N7 Tb1 N3 C12 144.1(6) . . . . ? N6 Tb1 N3 C12 104.5(7) . . . . ? N8 Tb1 N3 C12 11.4(9) . . . . ? N5 Tb1 N3 C12 39.4(7) . . . . ? N3 Tb1 N8 C21 -17.3(9) . . . . ? N4 Tb1 N8 C21 151.2(6) . . . . ? N2 Tb1 N8 C21 30.1(7) . . . . ? N1 Tb1 N8 C21 104.7(7) . . . . ? N7 Tb1 N8 C21 -164.3(7) . . . . ? N6 Tb1 N8 C21 -102.1(7) . . . . ? N5 Tb1 N8 C21 -48.8(6) . . . . ? N3 Tb1 N8 C37 -168.3(5) . . . . ? N4 Tb1 N8 C37 0.3(7) . . . . ? N2 Tb1 N8 C37 -120.9(6) . . . . ? N1 Tb1 N8 C37 -46.3(6) . . . . ? N7 Tb1 N8 C37 44.7(6) . . . . ? N6 Tb1 N8 C37 107.0(6) . . . . ? N5 Tb1 N8 C37 160.2(6) . . . . ? C16 N3 C12 C13 -170.5(8) . . . . ? Tb1 N3 C12 C13 27.2(12) . . . . ? C16 N3 C12 C25 2.3(9) . . . . ? Tb1 N3 C12 C25 -159.9(5) . . . . ? N3 C12 C13 C30 4.4(14) . . . . ? C25 C12 C13 C30 -167.5(8) . . . . ? N3 C12 C13 C40 171.7(8) . . . . ? C25 C12 C13 C40 -0.2(12) . . . . ? C5 N4 C14 C43 -170.5(8) . . . . ? Tb1 N4 C14 C43 33.8(11) . . . . ? C5 N4 C14 C8 3.2(9) . . . . ? Tb1 N4 C14 C8 -152.4(5) . . . . ? C35 C8 C14 N4 -2.8(9) . . . . ? C35 C8 C14 C43 171.2(8) . . . . ? C29 C6 C15 C54 0.5(15) . . . . ? C38 C6 C15 C54 -179.8(9) . . . . ? C12 N3 C16 C43 169.4(8) . . . . ? Tb1 N3 C16 C43 -27.9(11) . . . . ? C12 N3 C16 C27 -2.6(9) . . . . ? Tb1 N3 C16 C27 160.0(5) . . . . ? C9 C3 C17 C24 -120.3(9) . . . . ? C1 C3 C17 C24 68.6(11) . . . . ? C9 C3 C17 C73 59.1(11) . . . . ? C1 C3 C17 C73 -112.0(9) . . . . ? N4 C5 C18 C39 -1.4(14) . . . . ? C35 C5 C18 C39 172.1(8) . . . . ? N4 C5 C18 C61 -173.8(8) . . . . ? C35 C5 C18 C61 -0.3(13) . . . . ? N6 C2 C20 C66 2.1(10) . . . . ? C38 C2 C20 C66 -173.3(8) . . . . ? C37 N8 C21 C22 -175.1(8) . . . . ? Tb1 N8 C21 C22 30.6(12) . . . . ? C37 N8 C21 C45 0.3(9) . . . . ? Tb1 N8 C21 C45 -154.0(6) . . . . ? N8 C21 C22 C23 11.7(14) . . . . ? C45 C21 C22 C23 -163.1(8) . . . . ? N8 C21 C22 C52 -173.6(8) . . . . ? C45 C21 C22 C52 11.6(13) . . . . ? C21 C22 C23 N5 3.8(14) . . . . ? C52 C22 C23 N5 -171.0(8) . . . . ? C21 C22 C23 C46 -178.4(8) . . . . ? C52 C22 C23 C46 6.8(13) . . . . ? C63 N5 C23 C22 170.7(8) . . . . ? Tb1 N5 C23 C22 -50.0(10) . . . . ? C63 N5 C23 C46 -7.5(9) . . . . ? Tb1 N5 C23 C46 131.8(5) . . . . ? C73 C17 C24 C48 -1.1(13) . . . . ? C3 C17 C24 C48 178.3(8) . . . . ? N3 C12 C25 C27 -1.1(10) . . . . ? C13 C12 C25 C27 171.9(8) . . . . ? C12 C25 C27 C16 -0.5(10) . . . . ? N3 C16 C27 C25 2.0(10) . . . . ? C43 C16 C27 C25 -170.4(8) . . . . ? C15 C6 C29 C68 -0.7(15) . . . . ? C38 C6 C29 C68 179.6(9) . . . . ? C56 N2 C30 C13 169.5(8) . . . . ? Tb1 N2 C30 C13 -31.7(12) . . . . ? C56 N2 C30 C11 -6.0(9) . . . . ? Tb1 N2 C30 C11 152.8(6) . . . . ? C12 C13 C30 N2 -1.5(14) . . . . ? C40 C13 C30 N2 -169.0(8) . . . . ? C12 C13 C30 C11 173.4(8) . . . . ? C40 C13 C30 C11 6.0(12) . . . . ? C64 C11 C30 N2 4.8(11) . . . . ? C64 C11 C30 C13 -170.8(8) . . . . ? C39 N1 C32 C31 168.3(9) . . . . ? Tb1 N1 C32 C31 -29.1(13) . . . . ? C39 N1 C32 C90 -4.3(10) . . . . ? Tb1 N1 C32 C90 158.3(6) . . . . ? C56 C31 C32 N1 -2.7(15) . . . . ? C71 C31 C32 N1 -176.0(9) . . . . ? C56 C31 C32 C90 168.9(9) . . . . ? C71 C31 C32 C90 -4.4(13) . . . . ? N7 C7 C33 C37 -1.2(14) . . . . ? C57 C7 C33 C37 -171.9(8) . . . . ? N7 C7 C33 C26 171.4(8) . . . . ? C57 C7 C33 C26 0.7(13) . . . . ? C58 C26 C33 C7 -75.8(11) . . . . ? C60 C26 C33 C7 102.2(11) . . . . ? C58 C26 C33 C37 97.5(10) . . . . ? C60 C26 C33 C37 -84.5(11) . . . . ? C14 C8 C35 C5 1.1(9) . . . . ? C18 C5 C35 C8 -173.6(8) . . . . ? N4 C5 C35 C8 0.8(9) . . . . ? N7 C9 C36 C57 3.7(10) . . . . ? C3 C9 C36 C57 -167.9(8) . . . . ? C21 N8 C37 C33 173.5(8) . . . . ? Tb1 N8 C37 C33 -29.7(11) . . . . ? C21 N8 C37 C10 -0.3(9) . . . . ? Tb1 N8 C37 C10 156.5(5) . . . . ? C7 C33 C37 N8 -5.2(14) . . . . ? C26 C33 C37 N8 -177.8(8) . . . . ? C7 C33 C37 C10 167.9(8) . . . . ? C26 C33 C37 C10 -4.7(12) . . . . ? C45 C10 C37 N8 0.2(10) . . . . ? C45 C10 C37 C33 -173.8(8) . . . . ? N6 C2 C38 C63 -9.0(14) . . . . ? C20 C2 C38 C63 165.7(8) . . . . ? N6 C2 C38 C6 175.3(8) . . . . ? C20 C2 C38 C6 -10.1(12) . . . . ? C29 C6 C38 C63 -61.4(12) . . . . ? C15 C6 C38 C63 119.0(10) . . . . ? C29 C6 C38 C2 114.7(10) . . . . ? C15 C6 C38 C2 -64.9(12) . . . . ? C32 N1 C39 C18 -170.2(8) . . . . ? Tb1 N1 C39 C18 27.8(12) . . . . ? C32 N1 C39 C4 3.9(9) . . . . ? Tb1 N1 C39 C4 -158.2(5) . . . . ? C5 C18 C39 N1 4.3(14) . . . . ? C61 C18 C39 N1 176.9(8) . . . . ? C5 C18 C39 C4 -168.8(9) . . . . ? C61 C18 C39 C4 3.7(13) . . . . ? C90 C4 C39 N1 -1.9(10) . . . . ? C90 C4 C39 C18 172.2(9) . . . . ? C30 C13 C40 C47 -116.8(10) . . . . ? C12 C13 C40 C47 74.8(11) . . . . ? C30 C13 C40 C86 64.3(12) . . . . ? C12 C13 C40 C86 -104.1(12) . . . . ? C52 C19 C41 C67 -1.5(14) . . . . ? N4 C14 C43 C16 1.3(13) . . . . ? C8 C14 C43 C16 -171.6(8) . . . . ? N4 C14 C43 C42 171.4(7) . . . . ? C8 C14 C43 C42 -1.5(12) . . . . ? N3 C16 C43 C14 -4.9(13) . . . . ? C27 C16 C43 C14 166.3(8) . . . . ? N3 C16 C43 C42 -175.0(8) . . . . ? C27 C16 C43 C42 -3.8(12) . . . . ? C72 C42 C43 C14 -74.0(10) . . . . ? C83 C42 C43 C14 108.0(9) . . . . ? C72 C42 C43 C16 97.0(9) . . . . ? C83 C42 C43 C16 -81.1(10) . . . . ? C37 C10 C45 C21 0.0(10) . . . . ? N8 C21 C45 C10 -0.2(10) . . . . ? C22 C21 C45 C10 175.3(8) . . . . ? C63 C28 C46 C23 -2.1(10) . . . . ? C22 C23 C46 C28 -172.2(8) . . . . ? N5 C23 C46 C28 5.9(9) . . . . ? C86 C40 C47 C70 0.8(15) . . . . ? C13 C40 C47 C70 -178.1(9) . . . . ? C78 C34 C48 C24 -1.2(15) . . . . ? C17 C24 C48 C34 1.8(14) . . . . ? C41 C19 C52 C49 1.6(13) . . . . ? C41 C19 C52 C22 -178.5(8) . . . . ? C74 C49 C52 C19 -0.8(14) . . . . ? C74 C49 C52 C22 179.4(9) . . . . ? C23 C22 C52 C19 51.4(12) . . . . ? C21 C22 C52 C19 -123.6(9) . . . . ? C23 C22 C52 C49 -128.7(9) . . . . ? C21 C22 C52 C49 56.3(12) . . . . ? C68 C51 C54 C15 -3.5(18) . . . . ? C6 C15 C54 C51 1.6(17) . . . . ? C83 C44 C55 C59 0.8(13) . . . . ? C30 N2 C56 C31 -170.4(9) . . . . ? Tb1 N2 C56 C31 30.8(12) . . . . ? C30 N2 C56 C64 4.9(10) . . . . ? Tb1 N2 C56 C64 -153.8(6) . . . . ? C32 C31 C56 N2 2.0(15) . . . . ? C71 C31 C56 N2 175.4(8) . . . . ? C32 C31 C56 C64 -172.8(9) . . . . ? C71 C31 C56 C64 0.6(14) . . . . ? C9 C36 C57 C7 -1.7(10) . . . . ? N7 C7 C57 C36 -0.7(10) . . . . ? C33 C7 C57 C36 171.2(8) . . . . ? C60 C26 C58 C79 -0.2(14) . . . . ? C33 C26 C58 C79 177.9(8) . . . . ? C44 C55 C59 C72 -0.9(13) . . . . ? C58 C26 C60 C76 1.0(15) . . . . ? C33 C26 C60 C76 -177.0(9) . . . . ? C5 C18 C61 C85 75.5(12) . . . . ? C39 C18 C61 C85 -97.7(11) . . . . ? C5 C18 C61 C62 -107.8(11) . . . . ? C39 C18 C61 C62 79.1(12) . . . . ? C85 C61 C62 C75 -2.1(17) . . . . ? C18 C61 C62 C75 -179.0(10) . . . . ? C23 N5 C63 C38 -176.4(8) . . . . ? Tb1 N5 C63 C38 45.5(10) . . . . ? C23 N5 C63 C28 6.3(9) . . . . ? Tb1 N5 C63 C28 -131.8(6) . . . . ? C2 C38 C63 N5 -4.4(14) . . . . ? C6 C38 C63 N5 171.5(8) . . . . ? C2 C38 C63 C28 172.4(8) . . . . ? C6 C38 C63 C28 -11.7(13) . . . . ? C46 C28 C63 N5 -2.6(9) . . . . ? C46 C28 C63 C38 -179.9(8) . . . . ? C30 C11 C64 C56 -1.6(11) . . . . ? N2 C56 C64 C11 -2.0(11) . . . . ? C31 C56 C64 C11 173.5(9) . . . . ? C2 C20 C66 C1 -0.4(10) . . . . ? N6 C1 C66 C20 -1.4(10) . . . . ? C3 C1 C66 C20 173.3(8) . . . . ? C19 C41 C67 C74 0.6(15) . . . . ? C54 C51 C68 C29 3.3(18) . . . . ? C6 C29 C68 C51 -1.1(17) . . . . ? C77 C50 C70 C47 -0.4(19) . . . . ? C40 C47 C70 C50 0.8(15) . . . . ? C88 C69 C71 C65 1.2(15) . . . . ? C88 C69 C71 C31 -176.7(9) . . . . ? C82 C65 C71 C69 -0.2(16) . . . . ? C82 C65 C71 C31 177.7(10) . . . . ? C32 C31 C71 C69 -78.8(12) . . . . ? C56 C31 C71 C69 107.3(11) . . . . ? C32 C31 C71 C65 103.2(11) . . . . ? C56 C31 C71 C65 -70.6(12) . . . . ? C83 C42 C72 C59 -1.3(12) . . . . ? C43 C42 C72 C59 -179.4(7) . . . . ? C55 C59 C72 C42 1.2(13) . . . . ? C24 C17 C73 C78 -0.1(14) . . . . ? C3 C17 C73 C78 -179.5(9) . . . . ? C41 C67 C74 C49 0.3(16) . . . . ? C52 C49 C74 C67 -0.2(16) . . . . ? C81 C53 C75 C62 -0.3(19) . . . . ? C61 C62 C75 C53 1.2(19) . . . . ? C26 C60 C76 C80 -1.3(17) . . . . ? C70 C50 C77 C86 -2(2) . . . . ? C48 C34 C78 C73 0.0(16) . . . . ? C17 C73 C78 C34 0.7(15) . . . . ? C26 C58 C79 C80 -0.3(15) . . . . ? C58 C79 C80 C76 0.1(16) . . . . ? C60 C76 C80 C79 0.7(17) . . . . ? C75 C53 C81 C85 0.4(19) . . . . ? C71 C65 C82 C89 -0.6(18) . . . . ? C55 C44 C83 C42 -1.0(12) . . . . ? C72 C42 C83 C44 1.2(11) . . . . ? C43 C42 C83 C44 179.3(7) . . . . ? C62 C61 C85 C81 2.2(17) . . . . ? C18 C61 C85 C81 179.1(10) . . . . ? C53 C81 C85 C61 -1(2) . . . . ? C47 C40 C86 C77 -2.8(19) . . . . ? C13 C40 C86 C77 176.2(12) . . . . ? C50 C77 C86 C40 3(2) . . . . ? C71 C69 C88 C89 -1.3(17) . . . . ? C69 C88 C89 C82 0.5(19) . . . . ? C65 C82 C89 C88 0(2) . . . . ? C39 C4 C90 C32 -0.8(10) . . . . ? N1 C32 C90 C4 3.2(11) . . . . ? C31 C32 C90 C4 -169.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.617 _refine_diff_density_min -1.933 _refine_diff_density_rms 0.160 # Attachment '- 2.cif' data_tbtpp _database_code_depnum_ccdc_archive 'CCDC 862024' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H75 Cl6 N10 Tb' _chemical_formula_weight 1776.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 14.6111(12) _cell_length_b 14.6111(12) _cell_length_c 19.3957(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4140.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7072 _cell_measurement_theta_min 6.58 _cell_measurement_theta_max 54.88 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8095 _exptl_absorpt_correction_T_max 0.8976 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IP _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20354 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1377 _reflns_number_gt 1376 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _refine_special_details ; Due to the high symmetry space group, the phenyl rings in the TPP are highly disordered and the structure is distorted. We employed the restrain to avoid such unreasonable distortion, using the following commands in SHELX format. DFIX 1.39 0.02 C7 C9 C9 C11 DFIX 1.39 0.02 C11 C12 C12 C10 C10 C8 C8 C7 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^)+(0.0679P)^2^+12.7609P] 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 1377 _refine_ls_number_parameters 114 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.123 _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 Tb1 Tb 0.0000 0.0000 0.0000 0.01881(17) Uani 1 16 d S . 1 C1 C 0.0000 0.2101(2) 0.08584(18) 0.0276(7) Uani 1 2 d S . 1 C2 C 0.14862(17) 0.14862(17) 0.08605(18) 0.0257(7) Uani 1 2 d S A 1 N1 N 0.0548(3) 0.1308(3) 0.0733(2) 0.0227(8) Uani 0.50 1 d P . 1 C3 C 0.1542(4) 0.2480(4) 0.1027(3) 0.0308(11) Uani 0.50 1 d P A 1 H3 H 0.2090 0.2810 0.1116 0.037 Uiso 0.50 1 calc PR A 1 C4 C 0.0697(4) 0.2836(4) 0.1033(3) 0.0302(11) Uani 0.50 1 d P A 1 H4 H 0.0554 0.3457 0.1132 0.036 Uiso 0.50 1 calc PR A 1 C5 C 0.0000 0.0000 0.2195(6) 0.048(2) Uiso 1 8 d S . . H8 H 0.0000 0.0000 0.1679 0.057 Uiso 1 8 calc SR . . Cl1 Cl 0.0594(3) 0.0992(3) 0.2490(2) 0.0598(9) Uiso 0.25 1 d P . . Cl2 Cl 0.1096(5) 0.0000 0.2475(4) 0.0700(15) Uiso 0.25 2 d SP . . C6 C 0.2180(4) 0.0891(4) 0.0905(2) 0.0250(10) Uani 0.50 1 d P A 1 C7 C 0.3102(4) 0.1247(4) 0.1130(3) 0.0282(10) Uani 0.50 1 d PD A 1 C8 C 0.3852(4) 0.1215(5) 0.0696(3) 0.0436(14) Uani 0.50 1 d PD A 1 H1 H 0.3781 0.1000 0.0236 0.052 Uiso 0.50 1 calc PR A 1 C9 C 0.3221(4) 0.1553(5) 0.1805(3) 0.0434(15) Uani 0.50 1 d PD A 1 H2 H 0.2714 0.1571 0.2111 0.052 Uiso 0.50 1 calc PR A 1 C10 C 0.4711(4) 0.1495(6) 0.0927(4) 0.0525(19) Uani 0.50 1 d PD A 1 H5 H 0.5219 0.1473 0.0622 0.063 Uiso 0.50 1 calc PR A 1 C11 C 0.4084(5) 0.1833(6) 0.2031(3) 0.0540(19) Uani 0.50 1 d PD A 1 H6 H 0.4156 0.2046 0.2491 0.065 Uiso 0.50 1 calc PR A 1 C12 C 0.4834(6) 0.1806(5) 0.1600(3) 0.054(3) Uani 0.50 1 d PD A 1 H7 H 0.5420 0.1995 0.1758 0.065 Uiso 0.50 1 calc PR A 1 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 Tb1 0.0203(2) 0.0203(2) 0.0158(2) 0.000 0.000 0.000 C1 0.042(2) 0.0215(16) 0.0193(15) -0.0003(13) 0.000 0.000 C2 0.0289(11) 0.0289(11) 0.0193(15) -0.0010(9) -0.0010(9) -0.0069(14) N1 0.025(2) 0.023(2) 0.0199(18) -0.0013(15) 0.0013(15) 0.0009(16) C3 0.035(3) 0.029(3) 0.028(3) -0.003(2) 0.001(2) -0.008(2) C4 0.039(3) 0.023(3) 0.028(3) -0.004(2) 0.003(2) -0.003(2) C6 0.025(3) 0.031(2) 0.019(2) -0.0016(19) 0.0014(18) -0.004(2) C7 0.026(3) 0.029(3) 0.030(3) -0.003(2) -0.004(2) -0.003(2) C8 0.033(3) 0.066(4) 0.032(3) -0.010(3) 0.000(2) -0.006(3) C9 0.040(3) 0.062(4) 0.028(3) -0.005(3) -0.001(2) -0.012(3) C10 0.030(3) 0.079(5) 0.048(4) -0.011(4) 0.002(2) -0.008(3) C11 0.049(4) 0.080(5) 0.034(3) -0.007(3) -0.010(3) -0.020(4) C12 0.045(9) 0.069(4) 0.050(3) -0.010(3) -0.019(4) -0.013(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 Tb1 N1 2.512(4) 5 ? Tb1 N1 2.512(4) 17 ? Tb1 N1 2.512(4) 23 ? Tb1 N1 2.512(4) 7 ? Tb1 N1 2.512(4) 3 ? Tb1 N1 2.512(4) 22 ? Tb1 N1 2.512(4) 18 ? Tb1 N1 2.512(4) 2 ? Tb1 N1 2.512(4) 6 ? Tb1 N1 2.512(4) 24 ? Tb1 N1 2.512(4) 8 ? Tb1 N1 2.512(4) 20 ? C1 C1 0.000(7) 19 ? C1 C6 1.310(5) 8 ? C1 C6 1.310(5) 21 ? C1 N1 1.430(5) 19 ? C1 N1 1.430(5) . ? C1 C4 1.518(6) . ? C2 C2 0.000(12) 21 ? C2 C6 1.338(5) 21 ? C2 C6 1.338(6) . ? C2 N1 1.418(5) . ? C2 N1 1.418(5) 21 ? C2 C3 1.490(6) . ? N1 C2 1.418(5) 21 ? N1 C1 1.430(5) 19 ? C3 C4 1.340(8) . ? C3 H3 0.9500 . ? C4 C9 2.030(9) 21 ? C4 H4 0.9500 . ? C5 Cl2 1.691(8) . ? C5 Cl1 1.784(5) 19 ? C5 Cl1 1.784(5) 2 ? C5 H8 1.0000 . ? Cl1 C5 1.784(5) 2 ? Cl2 Cl2 0.00(2) 20 ? Cl2 Cl1 0.881(4) 7 ? Cl2 C5 1.691(8) 22 ? Cl2 C5 1.691(8) 21 ? Cl2 C5 1.691(8) 20 ? Cl2 Cl2 2.264(10) 21 ? C6 C1 1.310(5) 21 ? C6 C2 1.338(6) 21 ? C6 C7 1.509(7) . ? C7 C8 1.383(8) . ? C7 C9 1.394(7) . ? C8 C10 1.394(8) . ? C8 H1 0.9500 . ? C9 C11 1.397(8) . ? C9 C4 2.030(9) 21 ? C9 H2 0.9500 . ? C10 C12 1.394(9) . ? C10 H5 0.9500 . ? C11 C12 1.378(10) . ? C11 H6 0.9500 . ? C12 H7 0.9500 . ? 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 N1 Tb1 N1 36.42(18) 5 17 ? N1 Tb1 N1 37.16(18) 5 23 ? N1 Tb1 N1 71.34(9) 17 23 ? N1 Tb1 N1 142.84(18) 5 7 ? N1 Tb1 N1 108.66(9) 17 7 ? N1 Tb1 N1 180.0(3) 23 7 ? N1 Tb1 N1 71.34(9) 5 3 ? N1 Tb1 N1 37.16(18) 17 3 ? N1 Tb1 N1 99.48(18) 23 3 ? N1 Tb1 N1 80.52(18) 7 3 ? N1 Tb1 N1 68.90(19) 5 22 ? N1 Tb1 N1 80.52(18) 17 22 ? N1 Tb1 N1 80.97(18) 23 22 ? N1 Tb1 N1 99.03(18) 7 22 ? N1 Tb1 N1 108.66(9) 3 22 ? N1 Tb1 N1 99.48(18) 5 18 ? N1 Tb1 N1 111.10(19) 17 18 ? N1 Tb1 N1 71.34(9) 23 18 ? N1 Tb1 N1 108.66(9) 7 18 ? N1 Tb1 N1 99.03(18) 3 18 ? N1 Tb1 N1 143.58(18) 22 18 ? N1 Tb1 N1 80.52(18) 5 2 ? N1 Tb1 N1 68.90(19) 17 2 ? N1 Tb1 N1 108.66(9) 23 2 ? N1 Tb1 N1 71.34(9) 7 2 ? N1 Tb1 N1 80.97(18) 3 2 ? N1 Tb1 N1 36.42(18) 22 2 ? N1 Tb1 N1 180.0(3) 18 2 ? N1 Tb1 N1 111.10(19) 5 6 ? N1 Tb1 N1 99.48(18) 17 6 ? N1 Tb1 N1 99.03(18) 23 6 ? N1 Tb1 N1 80.97(18) 7 6 ? N1 Tb1 N1 71.34(9) 3 6 ? N1 Tb1 N1 180.0(3) 22 6 ? N1 Tb1 N1 36.42(18) 18 6 ? N1 Tb1 N1 143.58(18) 2 6 ? N1 Tb1 N1 99.03(18) 5 24 ? N1 Tb1 N1 71.34(9) 17 24 ? N1 Tb1 N1 111.10(19) 23 24 ? N1 Tb1 N1 68.90(19) 7 24 ? N1 Tb1 N1 36.42(18) 3 24 ? N1 Tb1 N1 142.84(18) 22 24 ? N1 Tb1 N1 71.34(9) 18 24 ? N1 Tb1 N1 108.66(9) 2 24 ? N1 Tb1 N1 37.16(18) 6 24 ? N1 Tb1 N1 80.97(18) 5 8 ? N1 Tb1 N1 108.66(9) 17 8 ? N1 Tb1 N1 68.90(19) 23 8 ? N1 Tb1 N1 111.10(19) 7 8 ? N1 Tb1 N1 143.58(18) 3 8 ? N1 Tb1 N1 37.16(18) 22 8 ? N1 Tb1 N1 108.66(9) 18 8 ? N1 Tb1 N1 71.34(9) 2 8 ? N1 Tb1 N1 142.84(18) 6 8 ? N1 Tb1 N1 180.00(19) 24 8 ? N1 Tb1 N1 108.66(9) 5 20 ? N1 Tb1 N1 80.97(18) 17 20 ? N1 Tb1 N1 143.58(18) 23 20 ? N1 Tb1 N1 36.42(18) 7 20 ? N1 Tb1 N1 68.90(19) 3 20 ? N1 Tb1 N1 71.34(9) 22 20 ? N1 Tb1 N1 142.84(18) 18 20 ? N1 Tb1 N1 37.16(18) 2 20 ? N1 Tb1 N1 108.66(9) 6 20 ? N1 Tb1 N1 80.52(18) 24 20 ? N1 Tb1 N1 99.48(18) 8 20 ? C1 C1 C6 0(10) 19 8 ? C1 C1 C6 0(10) 19 21 ? C6 C1 C6 167.2(6) 8 21 ? C1 C1 N1 0(10) 19 19 ? C6 C1 N1 61.7(3) 8 19 ? C6 C1 N1 129.7(4) 21 19 ? C1 C1 N1 0(10) 19 . ? C6 C1 N1 129.7(4) 8 . ? C6 C1 N1 61.7(3) 21 . ? N1 C1 N1 68.1(4) 19 . ? C1 C1 C4 0(10) 19 . ? C6 C1 C4 126.1(4) 8 . ? C6 C1 C4 42.0(3) 21 . ? N1 C1 C4 170.8(4) 19 . ? N1 C1 C4 103.7(3) . . ? C2 C2 C6 0(10) 21 21 ? C2 C2 C6 0(10) 21 . ? C6 C2 C6 168.6(5) 21 . ? C2 C2 N1 0(10) 21 . ? C6 C2 N1 61.5(3) 21 . ? C6 C2 N1 128.6(4) . . ? C2 C2 N1 0(10) 21 21 ? C6 C2 N1 128.6(4) 21 21 ? C6 C2 N1 61.5(3) . 21 ? N1 C2 N1 67.3(4) . 21 ? C2 C2 C3 0(10) 21 . ? C6 C2 C3 44.2(3) 21 . ? C6 C2 C3 125.3(4) . . ? N1 C2 C3 105.7(3) . . ? N1 C2 C3 172.2(4) 21 . ? C2 N1 C2 0.0(4) 21 . ? C2 N1 C1 111.2(3) 21 19 ? C2 N1 C1 111.2(3) . 19 ? C2 N1 C1 111.2(3) 21 . ? C2 N1 C1 111.2(3) . . ? C1 N1 C1 0.0(3) 19 . ? C2 N1 Tb1 123.2(2) 21 . ? C2 N1 Tb1 123.2(2) . . ? C1 N1 Tb1 122.3(2) 19 . ? C1 N1 Tb1 122.3(2) . . ? C4 C3 C2 109.3(4) . . ? C4 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? C3 C4 C1 110.0(4) . . ? C3 C4 C9 63.0(4) . 21 ? C1 C4 C9 140.7(4) . 21 ? C3 C4 H4 125.0 . . ? C1 C4 H4 125.0 . . ? C9 C4 H4 73.8 21 . ? Cl2 C5 Cl1 110.9(4) . 19 ? Cl2 C5 Cl1 110.9(4) . 2 ? Cl1 C5 Cl1 108.7(4) 19 2 ? Cl2 C5 H8 108.7 . . ? Cl1 C5 H8 108.7 19 . ? Cl1 C5 H8 108.7 2 . ? Cl2 Cl2 Cl1 0(10) 20 7 ? Cl2 Cl2 C5 0(10) 20 22 ? Cl1 Cl2 C5 81.3(5) 7 22 ? Cl2 Cl2 C5 0(10) 20 . ? Cl1 Cl2 C5 81.3(5) 7 . ? C5 Cl2 C5 0.0(7) 22 . ? Cl2 Cl2 C5 0(10) 20 21 ? Cl1 Cl2 C5 81.3(5) 7 21 ? C5 Cl2 C5 0.0(7) 22 21 ? C5 Cl2 C5 0.0(7) . 21 ? Cl2 Cl2 C5 0(10) 20 20 ? Cl1 Cl2 C5 81.3(5) 7 20 ? C5 Cl2 C5 0.0(7) 22 20 ? C5 Cl2 C5 0.0(7) . 20 ? C5 Cl2 C5 0.0(7) 21 20 ? Cl2 Cl2 Cl2 0(10) 20 21 ? Cl1 Cl2 Cl2 125.1(5) 7 21 ? C5 Cl2 Cl2 47.97(13) 22 21 ? C5 Cl2 Cl2 47.97(13) . 21 ? C5 Cl2 Cl2 47.97(13) 21 21 ? C5 Cl2 Cl2 47.97(13) 20 21 ? C1 C6 C2 125.1(5) 21 21 ? C1 C6 C2 125.1(5) 21 . ? C2 C6 C2 0.0(3) 21 . ? C1 C6 C7 116.1(5) 21 . ? C2 C6 C7 118.1(4) 21 . ? C2 C6 C7 118.1(4) . . ? C8 C7 C9 118.9(5) . . ? C8 C7 C6 121.3(5) . . ? C9 C7 C6 119.6(5) . . ? C7 C8 C10 120.5(6) . . ? C7 C8 H1 119.8 . . ? C10 C8 H1 119.8 . . ? C7 C9 C11 120.1(6) . . ? C7 C9 C4 22.4(3) . 21 ? C11 C9 C4 131.5(6) . 21 ? C7 C9 H2 119.9 . . ? C11 C9 H2 119.9 . . ? C4 C9 H2 105.2 21 . ? C12 C10 C8 120.9(7) . . ? C12 C10 H5 119.6 . . ? C8 C10 H5 119.6 . . ? C12 C11 C9 121.2(6) . . ? C12 C11 H6 119.4 . . ? C9 C11 H6 119.4 . . ? C11 C12 C10 118.3(7) . . ? C11 C12 H7 120.8 . . ? C10 C12 H7 120.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C2 N1 C2 0(96) 21 . . 21 ? C6 C2 N1 C2 0(100) . . . 21 ? N1 C2 N1 C2 0(100) 21 . . 21 ? C3 C2 N1 C2 0(96) . . . 21 ? C2 C2 N1 C1 0.00(7) 21 . . 19 ? C6 C2 N1 C1 -4.9(4) 21 . . 19 ? C6 C2 N1 C1 168.6(4) . . . 19 ? N1 C2 N1 C1 172.0(2) 21 . . 19 ? C3 C2 N1 C1 -4.4(5) . . . 19 ? C2 C2 N1 C1 0.00(7) 21 . . . ? C6 C2 N1 C1 -4.9(4) 21 . . . ? C6 C2 N1 C1 168.6(4) . . . . ? N1 C2 N1 C1 172.0(2) 21 . . . ? C3 C2 N1 C1 -4.4(5) . . . . ? C2 C2 N1 Tb1 0.00(7) 21 . . . ? C6 C2 N1 Tb1 155.1(4) 21 . . . ? C6 C2 N1 Tb1 -31.4(6) . . . . ? N1 C2 N1 Tb1 -28.0(4) 21 . . . ? C3 C2 N1 Tb1 155.5(3) . . . . ? C1 C1 N1 C2 0.00(10) 19 . . 21 ? C6 C1 N1 C2 -168.1(4) 8 . . 21 ? C6 C1 N1 C2 5.0(4) 21 . . 21 ? N1 C1 N1 C2 -171.8(2) 19 . . 21 ? C4 C1 N1 C2 3.9(4) . . . 21 ? C1 C1 N1 C2 0.00(10) 19 . . . ? C6 C1 N1 C2 -168.1(4) 8 . . . ? C6 C1 N1 C2 5.0(4) 21 . . . ? N1 C1 N1 C2 -171.8(2) 19 . . . ? C4 C1 N1 C2 3.9(4) . . . . ? C6 C1 N1 C1 0(100) 8 . . 19 ? C6 C1 N1 C1 0(14) 21 . . 19 ? N1 C1 N1 C1 0(100) 19 . . 19 ? C4 C1 N1 C1 0(15) . . . 19 ? C1 C1 N1 Tb1 0.00(4) 19 . . . ? C6 C1 N1 Tb1 31.7(6) 8 . . . ? C6 C1 N1 Tb1 -155.2(4) 21 . . . ? N1 C1 N1 Tb1 28.0(4) 19 . . . ? C4 C1 N1 Tb1 -156.3(3) . . . . ? N1 Tb1 N1 C2 -155.7(3) 5 . . 21 ? N1 Tb1 N1 C2 115(3) 17 . . 21 ? N1 Tb1 N1 C2 -139.3(4) 23 . . 21 ? N1 Tb1 N1 C2 40.7(4) 7 . . 21 ? N1 Tb1 N1 C2 -2.1(3) 3 . . 21 ? N1 Tb1 N1 C2 137.1(3) 22 . . 21 ? N1 Tb1 N1 C2 -78.8(3) 18 . . 21 ? N1 Tb1 N1 C2 101.2(3) 2 . . 21 ? N1 Tb1 N1 C2 -42.9(3) 6 . . 21 ? N1 Tb1 N1 C2 -18.3(3) 24 . . 21 ? N1 Tb1 N1 C2 161.7(3) 8 . . 21 ? N1 Tb1 N1 C2 64.7(4) 20 . . 21 ? N1 Tb1 N1 C2 -155.7(3) 5 . . . ? N1 Tb1 N1 C2 115(3) 17 . . . ? N1 Tb1 N1 C2 -139.3(4) 23 . . . ? N1 Tb1 N1 C2 40.7(4) 7 . . . ? N1 Tb1 N1 C2 -2.1(3) 3 . . . ? N1 Tb1 N1 C2 137.1(3) 22 . . . ? N1 Tb1 N1 C2 -78.8(3) 18 . . . ? N1 Tb1 N1 C2 101.2(3) 2 . . . ? N1 Tb1 N1 C2 -42.9(3) 6 . . . ? N1 Tb1 N1 C2 -18.3(3) 24 . . . ? N1 Tb1 N1 C2 161.7(3) 8 . . . ? N1 Tb1 N1 C2 64.7(4) 20 . . . ? N1 Tb1 N1 C1 2.1(3) 5 . . 19 ? N1 Tb1 N1 C1 -87(3) 17 . . 19 ? N1 Tb1 N1 C1 18.6(3) 23 . . 19 ? N1 Tb1 N1 C1 -161.4(3) 7 . . 19 ? N1 Tb1 N1 C1 155.7(3) 3 . . 19 ? N1 Tb1 N1 C1 -65.0(4) 22 . . 19 ? N1 Tb1 N1 C1 79.1(3) 18 . . 19 ? N1 Tb1 N1 C1 -100.9(3) 2 . . 19 ? N1 Tb1 N1 C1 115.0(4) 6 . . 19 ? N1 Tb1 N1 C1 139.6(4) 24 . . 19 ? N1 Tb1 N1 C1 -40.4(4) 8 . . 19 ? N1 Tb1 N1 C1 -137.4(2) 20 . . 19 ? N1 Tb1 N1 C1 2.1(3) 5 . . . ? N1 Tb1 N1 C1 -87(3) 17 . . . ? N1 Tb1 N1 C1 18.6(3) 23 . . . ? N1 Tb1 N1 C1 -161.4(3) 7 . . . ? N1 Tb1 N1 C1 155.7(3) 3 . . . ? N1 Tb1 N1 C1 -65.0(4) 22 . . . ? N1 Tb1 N1 C1 79.1(3) 18 . . . ? N1 Tb1 N1 C1 -100.9(3) 2 . . . ? N1 Tb1 N1 C1 115.0(4) 6 . . . ? N1 Tb1 N1 C1 139.6(4) 24 . . . ? N1 Tb1 N1 C1 -40.4(4) 8 . . . ? N1 Tb1 N1 C1 -137.4(2) 20 . . . ? C2 C2 C3 C4 0.00(14) 21 . . . ? C6 C2 C3 C4 3.8(4) 21 . . . ? C6 C2 C3 C4 -170.2(5) . . . . ? N1 C2 C3 C4 3.2(5) . . . . ? N1 C2 C3 C4 -22(3) 21 . . . ? C2 C3 C4 C1 -0.8(6) . . . . ? C2 C3 C4 C9 136.8(5) . . . 21 ? C1 C1 C4 C3 0.00(7) 19 . . . ? C6 C1 C4 C3 170.6(5) 8 . . . ? C6 C1 C4 C3 -3.3(4) 21 . . . ? N1 C1 C4 C3 24(3) 19 . . . ? N1 C1 C4 C3 -1.8(5) . . . . ? C1 C1 C4 C9 0.00(10) 19 . . 21 ? C6 C1 C4 C9 99.2(7) 8 . . 21 ? C6 C1 C4 C9 -74.7(7) 21 . . 21 ? N1 C1 C4 C9 -47(3) 19 . . 21 ? N1 C1 C4 C9 -73.2(7) . . . 21 ? Cl1 C5 Cl2 Cl2 0.0(4) 19 . . 20 ? Cl1 C5 Cl2 Cl2 0.0(4) 2 . . 20 ? Cl1 C5 Cl2 Cl1 145.5(8) 19 . . 7 ? Cl1 C5 Cl2 Cl1 24.5(7) 2 . . 7 ? Cl1 C5 Cl2 C5 0(100) 19 . . 22 ? Cl1 C5 Cl2 C5 0(100) 2 . . 22 ? Cl1 C5 Cl2 C5 0(100) 19 . . 21 ? Cl1 C5 Cl2 C5 0(100) 2 . . 21 ? Cl1 C5 Cl2 C5 0(100) 19 . . 20 ? Cl1 C5 Cl2 C5 0(100) 2 . . 20 ? Cl1 C5 Cl2 Cl2 -11.7(2) 19 . . 21 ? Cl1 C5 Cl2 Cl2 -132.6(8) 2 . . 21 ? C2 C2 C6 C1 0.00(8) 21 . . 21 ? C6 C2 C6 C1 147(2) 21 . . 21 ? N1 C2 C6 C1 -2.5(8) . . . 21 ? N1 C2 C6 C1 -6.1(4) 21 . . 21 ? C3 C2 C6 C1 169.2(5) . . . 21 ? C6 C2 C6 C2 0(95) 21 . . 21 ? N1 C2 C6 C2 0(100) . . . 21 ? N1 C2 C6 C2 0(100) 21 . . 21 ? C3 C2 C6 C2 0(45) . . . 21 ? C2 C2 C6 C7 0.00(10) 21 . . . ? C6 C2 C6 C7 -23(3) 21 . . . ? N1 C2 C6 C7 -172.8(4) . . . . ? N1 C2 C6 C7 -176.4(5) 21 . . . ? C3 C2 C6 C7 -1.1(7) . . . . ? C1 C6 C7 C8 72.1(7) 21 . . . ? C2 C6 C7 C8 -116.7(6) 21 . . . ? C2 C6 C7 C8 -116.7(6) . . . . ? C1 C6 C7 C9 -103.1(6) 21 . . . ? C2 C6 C7 C9 68.1(7) 21 . . . ? C2 C6 C7 C9 68.1(7) . . . . ? C9 C7 C8 C10 -0.8(11) . . . . ? C6 C7 C8 C10 -176.0(7) . . . . ? C8 C7 C9 C11 0.9(11) . . . . ? C6 C7 C9 C11 176.2(6) . . . . ? C8 C7 C9 C4 -126.1(11) . . . 21 ? C6 C7 C9 C4 49.2(6) . . . 21 ? C7 C8 C10 C12 0.4(13) . . . . ? C7 C9 C11 C12 -0.6(13) . . . . ? C4 C9 C11 C12 23.4(13) 21 . . . ? C9 C11 C12 C10 0.3(13) . . . . ? C8 C10 C12 C11 -0.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.545 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 309 34 ' ' 2 0.000 0.500 0.250 12 0 ' ' 3 0.000 0.500 0.750 12 0 ' ' 4 0.500 0.500 0.000 309 34 ' ' 5 0.500 0.000 0.250 12 0 ' ' 6 0.500 0.000 0.750 12 0 ' ' _platon_squeeze_details ; ;