Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Jeffery, J.' 'Mamula, Olimpia' 'McCleverty, J. A.' 'Motson, Graham R.' 'von Zelewsky, A.' _publ_contact_author 'Dr. Mike Ward' _publ_contact_author_address ; Dr. Mike Ward School of Chemistry Cantock's Close BRISTOL BS8 1TS ; _publ_contact_author_fax '0117 9287655' _publ_contact_author_email 'mike.ward@bristol.ac.uk' _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'A C3 symmetric chiral hexadentate podand...' by G. R. Motson et al, submitted to Dalton Transactions for publication. ; #======================================================== data_1 _database_code_CSD 161557 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H49 B N9 Tl' _chemical_formula_weight 931.11 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' 'B' 'B' 0.0013 0.0007 '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' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 20.3970(18) _cell_length_b 20.3970(18) _cell_length_c 17.347(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6250.1(12) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _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 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 3.920 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.5078 _exptl_absorpt_correction_T_max 0.6953 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21871 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6361 _reflns_number_gt 5565 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0230P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(5) _refine_ls_number_reflns 6361 _refine_ls_number_parameters 358 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 1.143 _refine_ls_shift/su_mean 0.003 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 Tl1 Tl 0.6667 0.3333 0.424739(10) 0.04137(12) Uani 1 3 d S . . B1 B 0.6667 0.3333 0.6452(4) 0.063(3) Uani 1 3 d S . . H1 H 0.6667 0.3333 0.7029 0.076 Uiso 1 3 calc SR . . N11 N 0.6070(2) 0.3525(2) 0.61787(18) 0.0628(10) Uani 1 1 d . . . N12 N 0.6003(2) 0.3670(2) 0.54239(18) 0.0546(9) Uani 1 1 d . . . C13 C 0.5445(2) 0.3823(2) 0.5390(2) 0.0554(10) Uani 1 1 d . . . C14 C 0.5152(3) 0.3763(3) 0.6128(3) 0.0831(17) Uani 1 1 d . . . H14 H 0.4742 0.3834 0.6268 0.100 Uiso 1 1 calc R . . C15 C 0.5558(3) 0.3587(3) 0.6602(3) 0.0829(16) Uani 1 1 d . . . H15 H 0.5493 0.3518 0.7144 0.099 Uiso 1 1 calc R . . N21 N 0.54487(18) 0.38011(19) 0.4012(2) 0.0511(8) Uani 1 1 d . . . C22 C 0.5227(2) 0.4003(2) 0.4651(2) 0.0516(10) Uani 1 1 d . . . C23 C 0.4814(3) 0.4380(3) 0.4596(3) 0.0693(15) Uani 1 1 d . . . H23 H 0.4666 0.4525 0.5055 0.083 Uiso 1 1 calc R . . C24 C 0.4619(3) 0.4544(2) 0.3902(3) 0.0647(13) Uani 1 1 d . . . C25 C 0.4848(2) 0.4325(2) 0.3240(3) 0.0606(12) Uani 1 1 d . . . C26 C 0.5256(2) 0.3958(3) 0.3336(3) 0.0595(11) Uani 1 1 d . . . H26 H 0.5410 0.3806 0.2886 0.071 Uiso 1 1 calc R . . C31 C 0.4184(3) 0.4964(3) 0.3788(4) 0.0923(18) Uani 1 1 d . . . H31A H 0.3668 0.4658 0.4004 0.111 Uiso 1 1 calc R . . H31B H 0.4442 0.5450 0.4070 0.111 Uiso 1 1 calc R . . C32 C 0.4130(3) 0.5114(3) 0.2946(4) 0.100(2) Uani 1 1 d . . . H32 H 0.3888 0.5425 0.2832 0.120 Uiso 1 1 calc R . . C33 C 0.4919(4) 0.5387(3) 0.2549(5) 0.125(3) Uani 1 1 d . . . H33A H 0.4983 0.5648 0.2050 0.150 Uiso 1 1 calc R . . H33B H 0.5359 0.5678 0.2892 0.150 Uiso 1 1 calc R . . C34 C 0.4671(3) 0.4543(3) 0.2477(3) 0.0809(16) Uani 1 1 d . . . H34 H 0.4848 0.4391 0.2009 0.097 Uiso 1 1 calc R . . C35 C 0.3829(3) 0.4373(3) 0.2467(3) 0.0718(14) Uani 1 1 d . . . C36 C 0.3230(3) 0.3637(3) 0.2814(3) 0.0670(15) Uani 1 1 d . . . H36A H 0.2752 0.3641 0.2852 0.101 Uiso 1 1 calc R . . H36B H 0.3390 0.3577 0.3329 0.101 Uiso 1 1 calc R . . H36C H 0.3158 0.3215 0.2486 0.101 Uiso 1 1 calc R . . C37 C 0.3588(3) 0.4454(4) 0.1644(3) 0.104(2) Uani 1 1 d . . . H37A H 0.3499 0.4015 0.1334 0.155 Uiso 1 1 calc R . . H37B H 0.3990 0.4917 0.1406 0.155 Uiso 1 1 calc R . . H37C H 0.3121 0.4480 0.1669 0.155 Uiso 1 1 calc R . . Tl2 Tl 0.0000 0.0000 0.575041(10) 0.04899(14) Uani 1 3 d S . . B2 B 0.0000 0.0000 0.7985(7) 0.072(4) Uani 1 3 d S . . H2 H 0.0000 0.0000 0.8562 0.000(17) Uiso 1 3 calc SR . . N41 N 0.0800(2) 0.0215(2) 0.76872(18) 0.0657(10) Uani 1 1 d . . . N42 N 0.0994(2) 0.0309(2) 0.69285(18) 0.0577(9) Uani 1 1 d . . . C43 C 0.1720(3) 0.0491(2) 0.6903(2) 0.0576(11) Uani 1 1 d . . . C44 C 0.1989(3) 0.0511(3) 0.7647(3) 0.0787(15) Uani 1 1 d . . . H44 H 0.2485 0.0629 0.7793 0.080(15) Uiso 1 1 calc R . . C45 C 0.1387(4) 0.0326(3) 0.8119(3) 0.0803(15) Uani 1 1 d . . . H45 H 0.1386 0.0283 0.8664 0.12(2) Uiso 1 1 calc R . . N51 N 0.1668(2) 0.03509(19) 0.55259(19) 0.0553(8) Uani 1 1 d . . . C52 C 0.2101(3) 0.0595(2) 0.6164(2) 0.0532(10) Uani 1 1 d . . . C53 C 0.2888(3) 0.0903(3) 0.6107(3) 0.0683(16) Uani 1 1 d . . . H53 H 0.3188 0.1079 0.6561 0.078(15) Uiso 1 1 calc R . . C54 C 0.3228(3) 0.0954(3) 0.5425(3) 0.0631(12) Uani 1 1 d . . . C55A C 0.2778(3) 0.0666(2) 0.4775(3) 0.0603(11) Uani 1 1 d . . . C56A C 0.2007(3) 0.0387(2) 0.4859(2) 0.0592(11) Uani 1 1 d . . . H56 H 0.1701 0.0209 0.4410 0.032(9) Uiso 1 1 calc R . . C61 C 0.4088(4) 0.1336(6) 0.5323(4) 0.111(3) Uani 1 1 d . . . H61A H 0.4327 0.1880 0.5456 0.23(6) Uiso 1 1 calc R . . H61B H 0.4295 0.1099 0.5672 0.15(3) Uiso 1 1 calc R . . C62 C 0.4266(4) 0.1251(6) 0.4495(4) 0.123(3) Uani 1 1 d . . . H62 H 0.4816 0.1457 0.4383 0.094(17) Uiso 1 1 calc R . . C63 C 0.3749(6) 0.0434(6) 0.4237(5) 0.123(3) Uani 1 1 d . . . H63A H 0.3593 0.0056 0.4657 0.12(2) Uiso 1 1 calc R . . H63B H 0.3938 0.0281 0.3784 0.15(3) Uiso 1 1 calc R . . C64 C 0.3159(3) 0.0680(3) 0.4040(3) 0.0796(15) Uani 1 1 d . . . H64 H 0.2827 0.0435 0.3582 0.096(17) Uiso 1 1 calc R . . C65 C 0.3853(3) 0.1497(4) 0.3922(3) 0.0821(16) Uani 1 1 d . . . C66 C 0.4179(4) 0.1618(5) 0.3113(4) 0.121(3) Uani 1 1 d . . . H66A H 0.3882 0.1746 0.2765 0.17(3) Uiso 1 1 calc R . . H66B H 0.4161 0.1153 0.2935 0.078(18) Uiso 1 1 calc R . . H66C H 0.4706 0.2032 0.3119 0.17(3) Uiso 1 1 calc R . . C67 C 0.3752(3) 0.2154(3) 0.4106(4) 0.085(2) Uani 1 1 d . . . H67A H 0.4247 0.2618 0.4116 0.071(16) Uiso 1 1 calc R . . H67B H 0.3509 0.2077 0.4611 0.082(19) Uiso 1 1 calc R . . H67C H 0.3433 0.2200 0.3712 0.070(15) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.04302(12) 0.04302(12) 0.0381(4) 0.000 0.000 0.02151(6) B1 0.078(4) 0.078(4) 0.034(5) 0.000 0.000 0.039(2) N11 0.071(3) 0.071(3) 0.0443(19) -0.0104(16) 0.0047(17) 0.033(2) N12 0.059(2) 0.062(2) 0.0469(18) -0.0014(16) 0.0083(15) 0.033(2) C13 0.040(2) 0.052(3) 0.068(3) -0.022(2) 0.0004(19) 0.019(2) C14 0.058(3) 0.111(5) 0.076(3) -0.040(3) 0.006(3) 0.039(3) C15 0.073(3) 0.109(5) 0.051(3) -0.028(3) 0.006(2) 0.033(3) N21 0.0387(18) 0.048(2) 0.069(2) 0.0112(16) 0.0124(15) 0.0234(16) C22 0.029(2) 0.036(2) 0.082(3) -0.0098(19) 0.0044(19) 0.0111(17) C23 0.046(3) 0.044(3) 0.116(4) -0.035(3) -0.009(3) 0.022(2) C24 0.038(2) 0.036(2) 0.120(4) -0.018(2) -0.017(3) 0.018(2) C25 0.037(2) 0.043(2) 0.102(3) 0.017(2) 0.007(2) 0.020(2) C26 0.047(2) 0.064(3) 0.075(3) 0.019(2) 0.019(2) 0.033(2) C31 0.076(4) 0.059(3) 0.159(6) -0.039(3) -0.032(4) 0.047(3) C32 0.061(4) 0.046(3) 0.204(7) 0.004(4) -0.024(4) 0.034(3) C33 0.053(4) 0.059(4) 0.245(10) 0.057(5) -0.016(5) 0.013(3) C34 0.050(3) 0.076(4) 0.124(4) 0.050(3) 0.023(3) 0.037(3) C35 0.047(3) 0.055(3) 0.120(4) 0.016(3) -0.002(3) 0.030(2) C36 0.049(3) 0.056(3) 0.091(4) 0.001(3) -0.004(3) 0.022(2) C37 0.073(4) 0.121(5) 0.137(5) 0.056(4) 0.010(4) 0.064(4) Tl2 0.05492(15) 0.05492(15) 0.0371(4) 0.000 0.000 0.02746(7) B2 0.083(6) 0.083(6) 0.051(4) 0.000 0.000 0.041(3) N41 0.081(3) 0.075(3) 0.0436(19) -0.0077(17) -0.0120(18) 0.041(2) N42 0.067(3) 0.061(2) 0.0418(18) -0.0018(16) -0.0063(16) 0.029(2) C43 0.066(3) 0.052(3) 0.057(2) -0.0141(19) -0.020(2) 0.031(2) C44 0.082(4) 0.086(4) 0.071(3) -0.029(3) -0.032(3) 0.044(3) C45 0.105(4) 0.091(4) 0.052(3) -0.021(3) -0.028(3) 0.055(4) N51 0.054(2) 0.045(2) 0.057(2) -0.0076(16) -0.0098(17) 0.0180(17) C52 0.058(3) 0.038(2) 0.059(2) -0.0069(18) -0.010(2) 0.019(2) C53 0.070(4) 0.060(3) 0.084(4) -0.012(3) -0.033(3) 0.039(3) C54 0.062(3) 0.059(3) 0.081(3) 0.013(2) 0.000(2) 0.039(3) C55A 0.071(3) 0.042(2) 0.069(3) 0.001(2) 0.001(2) 0.029(2) C56A 0.067(3) 0.035(2) 0.059(3) -0.0062(18) -0.010(2) 0.014(2) C61 0.072(4) 0.185(9) 0.103(5) 0.043(5) 0.006(3) 0.085(5) C62 0.091(5) 0.203(9) 0.123(6) 0.043(6) 0.020(4) 0.111(6) C63 0.180(9) 0.155(8) 0.110(6) 0.025(6) 0.042(6) 0.141(8) C64 0.096(4) 0.072(4) 0.082(3) 0.000(3) 0.012(3) 0.050(3) C65 0.055(3) 0.106(5) 0.088(4) 0.027(3) 0.014(3) 0.043(3) C66 0.089(6) 0.178(9) 0.113(5) 0.038(5) 0.031(4) 0.079(6) C67 0.051(3) 0.055(4) 0.130(6) 0.014(4) -0.013(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 Tl1 N12 2.719(3) 3_665 ? Tl1 N12 2.719(3) 2_655 ? Tl1 N12 2.719(3) . ? B1 N11 1.527(4) 2_655 ? B1 N11 1.527(4) 3_665 ? B1 N11 1.527(4) . ? N11 C15 1.334(6) . ? N11 N12 1.364(4) . ? N12 C13 1.324(5) . ? C13 C14 1.392(6) . ? C13 C22 1.462(6) . ? C14 C15 1.337(8) . ? N21 C26 1.325(5) . ? N21 C22 1.338(5) . ? C22 C23 1.400(6) . ? C23 C24 1.362(7) . ? C24 C25 1.394(7) . ? C24 C31 1.522(6) . ? C25 C26 1.381(6) . ? C25 C34 1.497(7) . ? C31 C32 1.508(8) . ? C32 C35 1.556(8) . ? C32 C33 1.572(10) . ? C33 C34 1.538(8) . ? C34 C35 1.573(6) . ? C35 C36 1.509(7) . ? C35 C37 1.546(7) . ? Tl2 N42 2.721(3) . ? Tl2 N42 2.721(3) 2 ? Tl2 N42 2.721(3) 3 ? B2 N41 1.550(6) 3 ? B2 N41 1.550(6) . ? B2 N41 1.550(6) 2 ? N41 C45 1.333(6) . ? N41 N42 1.360(4) . ? N42 C43 1.335(5) . ? C43 C44 1.395(6) . ? C43 C52 1.458(6) . ? C44 C45 1.363(7) . ? N51 C56A 1.332(5) . ? N51 C52 1.347(5) . ? C52 C53 1.405(7) . ? C53 C54 1.350(7) . ? C54 C55A 1.385(6) . ? C54 C61 1.533(7) . ? C55A C56A 1.385(6) . ? C55A C64 1.487(6) . ? C61 C62 1.513(9) . ? C62 C63 1.527(11) . ? C62 C65 1.539(8) . ? C63 C64 1.557(9) . ? C64 C65 1.570(8) . ? C65 C67 1.489(8) . ? C65 C66 1.519(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Tl1 N12 69.83(12) 3_665 2_655 ? N12 Tl1 N12 69.83(12) 3_665 . ? N12 Tl1 N12 69.83(12) 2_655 . ? N11 B1 N11 110.8(3) 2_655 3_665 ? N11 B1 N11 110.8(3) 2_655 . ? N11 B1 N11 110.8(3) 3_665 . ? C15 N11 N12 109.8(4) . . ? C15 N11 B1 128.0(4) . . ? N12 N11 B1 122.2(4) . . ? C13 N12 N11 106.6(3) . . ? C13 N12 Tl1 128.4(3) . . ? N11 N12 Tl1 123.3(2) . . ? N12 C13 C14 108.7(4) . . ? N12 C13 C22 120.3(4) . . ? C14 C13 C22 131.1(4) . . ? C15 C14 C13 107.0(4) . . ? N11 C15 C14 107.9(4) . . ? C26 N21 C22 118.2(4) . . ? N21 C22 C23 120.1(4) . . ? N21 C22 C13 117.2(4) . . ? C23 C22 C13 122.7(4) . . ? C24 C23 C22 121.7(5) . . ? C23 C24 C25 117.6(4) . . ? C23 C24 C31 125.2(5) . . ? C25 C24 C31 117.2(5) . . ? C26 C25 C24 117.7(5) . . ? C26 C25 C34 124.6(5) . . ? C24 C25 C34 117.6(4) . . ? N21 C26 C25 124.7(4) . . ? C32 C31 C24 111.2(5) . . ? C31 C32 C35 110.7(4) . . ? C31 C32 C33 109.3(5) . . ? C35 C32 C33 87.1(5) . . ? C34 C33 C32 86.2(4) . . ? C25 C34 C33 105.5(5) . . ? C25 C34 C35 110.1(4) . . ? C33 C34 C35 87.6(4) . . ? C36 C35 C37 109.4(5) . . ? C36 C35 C32 118.9(5) . . ? C37 C35 C32 112.5(4) . . ? C36 C35 C34 117.8(4) . . ? C37 C35 C34 110.9(4) . . ? C32 C35 C34 85.5(4) . . ? N42 Tl2 N42 69.75(12) . 2 ? N42 Tl2 N42 69.75(12) . 3 ? N42 Tl2 N42 69.75(12) 2 3 ? N41 B2 N41 109.5(5) 3 . ? N41 B2 N41 109.5(5) 3 2 ? N41 B2 N41 109.5(5) . 2 ? C45 N41 N42 110.2(4) . . ? C45 N41 B2 126.1(6) . . ? N42 N41 B2 123.6(6) . . ? C43 N42 N41 106.0(3) . . ? C43 N42 Tl2 129.3(3) . . ? N41 N42 Tl2 124.3(3) . . ? N42 C43 C44 110.1(4) . . ? N42 C43 C52 120.4(4) . . ? C44 C43 C52 129.4(5) . . ? C45 C44 C43 105.1(5) . . ? N41 C45 C44 108.6(4) . . ? C56A N51 C52 117.8(4) . . ? N51 C52 C53 120.0(4) . . ? N51 C52 C43 117.7(4) . . ? C53 C52 C43 122.3(4) . . ? C54 C53 C52 121.6(5) . . ? C53 C54 C55A 118.3(5) . . ? C53 C54 C61 123.6(5) . . ? C55A C54 C61 118.0(5) . . ? C54 C55A C56A 117.7(4) . . ? C54 C55A C64 117.4(5) . . ? C56A C55A C64 124.9(4) . . ? N51 C56A C55A 124.4(4) . . ? C62 C61 C54 109.2(6) . . ? C61 C62 C63 109.3(7) . . ? C61 C62 C65 111.9(5) . . ? C63 C62 C65 88.6(6) . . ? C62 C63 C64 86.3(5) . . ? C55A C64 C63 106.7(5) . . ? C55A C64 C65 108.5(4) . . ? C63 C64 C65 86.5(5) . . ? C67 C65 C66 107.4(6) . . ? C67 C65 C62 120.0(6) . . ? C66 C65 C62 112.5(5) . . ? C67 C65 C64 118.1(4) . . ? C66 C65 C64 112.4(6) . . ? C62 C65 C64 85.4(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.962 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.052 #=END data_sad _database_code_CSD 161558 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H55 B Cl6 N11 O6 Tb' _chemical_formula_weight 1264.46 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.6126(17) _cell_length_b 17.623(2) _cell_length_c 24.975(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5551.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.4192 _exptl_absorpt_correction_T_max 0.7378 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58949 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.51 _reflns_number_total 12704 _reflns_number_gt 11464 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(7) _refine_ls_number_reflns 12704 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.611529(15) 0.584318(11) 0.772297(7) 0.02511(5) Uani 1 1 d . . . B1 B 0.4829(4) 0.5832(3) 0.63667(19) 0.0351(10) Uani 1 1 d . . . H1 H 0.447(3) 0.591(3) 0.5965(17) 0.028(11) Uiso 1 1 d . . . N11 N 0.4464(3) 0.5149(2) 0.67065(15) 0.0334(8) Uani 1 1 d . . . N12 N 0.4787(3) 0.5081(2) 0.72176(15) 0.0288(7) Uani 1 1 d . . . C13 C 0.4293(4) 0.4478(3) 0.74274(18) 0.0305(10) Uani 1 1 d . . . C14 C 0.3622(3) 0.4162(3) 0.70575(18) 0.0340(9) Uani 1 1 d . . . H14 H 0.3164 0.3740 0.7107 0.041 Uiso 1 1 calc R . . C15 C 0.3751(4) 0.4586(3) 0.65987(19) 0.0361(10) Uani 1 1 d . . . H15 H 0.3406 0.4501 0.6266 0.043 Uiso 1 1 calc R . . N21 N 0.5034(3) 0.48269(19) 0.82776(15) 0.0267(8) Uani 1 1 d . . . C22 C 0.4444(3) 0.4314(2) 0.80000(18) 0.0280(10) Uani 1 1 d . . . C23 C 0.4009(4) 0.3677(2) 0.82451(19) 0.0320(9) Uani 1 1 d . . . H23 H 0.3621 0.3318 0.8040 0.038 Uiso 1 1 calc R . . C24 C 0.4145(3) 0.3569(2) 0.87878(19) 0.0344(10) Uani 1 1 d . . . C25 C 0.4722(3) 0.4092(3) 0.90787(17) 0.0313(9) Uani 1 1 d . . . C26 C 0.5166(3) 0.4713(2) 0.88050(17) 0.0299(9) Uani 1 1 d . . . H26 H 0.5578 0.5068 0.9002 0.036 Uiso 1 1 calc R . . C31 C 0.3692(4) 0.2885(3) 0.9089(2) 0.0487(13) Uani 1 1 d . . . H31A H 0.3968 0.2410 0.8929 0.058 Uiso 1 1 calc R . . H31B H 0.2910 0.2881 0.9056 0.058 Uiso 1 1 calc R . . C32 C 0.4005(5) 0.2923(3) 0.9685(2) 0.0539(13) Uani 1 1 d . . . H32 H 0.3773 0.2480 0.9905 0.065 Uiso 1 1 calc R . . C33 C 0.5197(4) 0.3119(3) 0.9725(2) 0.0490(13) Uani 1 1 d . . . H33A H 0.5524 0.2992 1.0074 0.059 Uiso 1 1 calc R . . H33B H 0.5630 0.2929 0.9422 0.059 Uiso 1 1 calc R . . C34 C 0.4848(4) 0.3955(3) 0.9670(2) 0.0388(11) Uani 1 1 d . . . H34 H 0.5276 0.4338 0.9872 0.047 Uiso 1 1 calc R . . C35 C 0.3755(4) 0.3713(3) 0.9929(2) 0.0495(13) Uani 1 1 d . . . C36 C 0.2760(4) 0.4113(4) 0.9766(2) 0.0631(16) Uani 1 1 d . . . H36A H 0.2156 0.3894 0.9958 0.095 Uiso 1 1 calc R . . H36B H 0.2654 0.4054 0.9380 0.095 Uiso 1 1 calc R . . H36C H 0.2819 0.4654 0.9853 0.095 Uiso 1 1 calc R . . C37 C 0.3846(6) 0.3713(4) 1.0542(2) 0.0651(15) Uani 1 1 d . . . H37A H 0.3760 0.4232 1.0676 0.098 Uiso 1 1 calc R . . H37B H 0.4543 0.3519 1.0647 0.098 Uiso 1 1 calc R . . H37C H 0.3291 0.3389 1.0694 0.098 Uiso 1 1 calc R . . N41 N 0.4512(3) 0.6554(2) 0.66734(14) 0.0319(8) Uani 1 1 d . . . N42 N 0.4835(3) 0.6643(2) 0.71899(15) 0.0322(8) Uani 1 1 d . . . C43 C 0.4256(3) 0.7212(2) 0.73987(17) 0.0259(10) Uani 1 1 d . . . C44 C 0.3587(3) 0.7521(3) 0.69902(18) 0.0337(10) Uani 1 1 d . . . H44 H 0.3122 0.7944 0.7017 0.040 Uiso 1 1 calc R . . C45 C 0.3758(4) 0.7085(3) 0.65644(18) 0.0366(10) Uani 1 1 d . . . H45 H 0.3404 0.7137 0.6231 0.044 Uiso 1 1 calc R . . N51 N 0.4727(3) 0.6758(2) 0.82630(15) 0.0289(8) Uani 1 1 d . . . C52 C 0.4316(4) 0.7339(2) 0.79704(18) 0.0282(9) Uani 1 1 d . . . C53 C 0.3889(4) 0.7986(2) 0.82037(17) 0.0320(8) Uani 1 1 d . . . H53 H 0.3627 0.8388 0.7987 0.038 Uiso 1 1 calc R . . C54 C 0.3850(4) 0.8035(2) 0.87594(18) 0.0339(9) Uani 1 1 d . . . C55 C 0.4205(4) 0.7418(3) 0.90649(17) 0.0351(10) Uani 1 1 d . . . C56 C 0.4656(4) 0.6807(2) 0.87977(18) 0.0333(10) Uani 1 1 d . . . H56 H 0.4930 0.6400 0.9006 0.040 Uiso 1 1 calc R . . C61 C 0.3426(5) 0.8731(3) 0.9058(2) 0.0503(13) Uani 1 1 d . . . H61A H 0.3887 0.9174 0.8985 0.060 Uiso 1 1 calc R . . H61B H 0.2703 0.8852 0.8930 0.060 Uiso 1 1 calc R . . C62 C 0.3400(5) 0.8572(3) 0.9660(2) 0.0524(13) Uani 1 1 d . . . H62 H 0.3093 0.8988 0.9883 0.063 Uiso 1 1 calc R . . C63 C 0.2919(5) 0.7765(3) 0.9765(3) 0.0591(16) Uani 1 1 d . . . H63A H 0.2658 0.7686 1.0135 0.071 Uiso 1 1 calc R . . H63B H 0.2389 0.7601 0.9496 0.071 Uiso 1 1 calc R . . C64 C 0.4060(4) 0.7463(3) 0.96619(18) 0.0441(11) Uani 1 1 d . . . H64 H 0.4283 0.7008 0.9873 0.053 Uiso 1 1 calc R . . C65 C 0.4482(5) 0.8256(3) 0.9862(2) 0.0482(13) Uani 1 1 d . . . C66 C 0.5492(5) 0.8560(3) 0.9631(2) 0.0547(14) Uani 1 1 d . . . H66A H 0.5495 0.8480 0.9243 0.082 Uiso 1 1 calc R . . H66B H 0.6096 0.8294 0.9792 0.082 Uiso 1 1 calc R . . H66C H 0.5546 0.9104 0.9708 0.082 Uiso 1 1 calc R . . C67 C 0.4540(6) 0.8271(4) 1.0483(2) 0.0659(17) Uani 1 1 d . . . H67A H 0.5175 0.7999 1.0602 0.099 Uiso 1 1 calc R . . H67B H 0.3908 0.8027 1.0632 0.099 Uiso 1 1 calc R . . H67C H 0.4574 0.8799 1.0606 0.099 Uiso 1 1 calc R . . N71 N 0.6054(3) 0.5809(2) 0.63185(12) 0.0325(7) Uani 1 1 d . . . N72 N 0.6656(2) 0.5845(2) 0.67696(13) 0.0273(6) Uani 1 1 d . . . C73 C 0.7667(3) 0.5820(3) 0.66041(16) 0.0330(9) Uani 1 1 d . . . C74 C 0.7709(4) 0.5774(3) 0.60426(18) 0.0396(10) Uani 1 1 d . . . H74 H 0.8322 0.5748 0.5822 0.048 Uiso 1 1 calc R . . C75 C 0.6675(4) 0.5775(3) 0.58844(17) 0.0388(10) Uani 1 1 d . . . H75 H 0.6434 0.5755 0.5524 0.047 Uiso 1 1 calc R . . N81 N 0.8165(3) 0.5952(2) 0.75172(14) 0.0312(8) Uani 1 1 d . . . C82 C 0.8505(3) 0.5863(3) 0.70081(16) 0.0299(8) Uani 1 1 d . . . C83 C 0.9581(3) 0.5832(3) 0.68762(18) 0.0370(9) Uani 1 1 d . . . H83 H 0.9792 0.5754 0.6515 0.044 Uiso 1 1 calc R . . C84 C 1.0342(3) 0.5914(2) 0.7274(2) 0.0356(9) Uani 1 1 d . . . C85 C 0.9997(3) 0.6062(2) 0.7788(2) 0.0337(10) Uani 1 1 d . . . C86 C 0.8908(4) 0.6057(2) 0.78985(17) 0.0321(8) Uani 1 1 d . . . H86 H 0.8683 0.6132 0.8258 0.038 Uiso 1 1 calc R . . C91 C 1.1524(3) 0.5850(3) 0.71740(19) 0.0432(11) Uani 1 1 d . . . H91A H 1.1741 0.6221 0.6897 0.052 Uiso 1 1 calc R . . H91B H 1.1694 0.5334 0.7041 0.052 Uiso 1 1 calc R . . C92 C 1.2134(3) 0.6004(2) 0.7696(2) 0.0389(11) Uani 1 1 d . . . H92 H 1.2924 0.5993 0.7663 0.047 Uiso 1 1 calc R . . C93 C 1.1674(4) 0.6727(3) 0.7964(2) 0.0478(12) Uani 1 1 d . . . H93A H 1.1394 0.7106 0.7709 0.057 Uiso 1 1 calc R . . H93B H 1.2152 0.6965 0.8230 0.057 Uiso 1 1 calc R . . C94 C 1.0812(3) 0.6202(3) 0.8213(2) 0.0379(10) Uani 1 1 d . . . H94 H 1.0540 0.6346 0.8575 0.045 Uiso 1 1 calc R . . C95 C 1.1669(4) 0.5550(3) 0.8192(2) 0.0371(10) Uani 1 1 d . . . C96 C 1.1298(4) 0.4749(3) 0.8099(2) 0.0479(12) Uani 1 1 d . . . H96A H 1.1912 0.4421 0.8034 0.072 Uiso 1 1 calc R . . H96B H 1.0827 0.4736 0.7787 0.072 Uiso 1 1 calc R . . H96C H 1.0914 0.4569 0.8415 0.072 Uiso 1 1 calc R . . C97 C 1.2357(4) 0.5578(3) 0.8680(2) 0.0569(15) Uani 1 1 d . . . H97A H 1.1977 0.5354 0.8983 0.085 Uiso 1 1 calc R . . H97B H 1.2534 0.6107 0.8761 0.085 Uiso 1 1 calc R . . H97C H 1.3009 0.5292 0.8614 0.085 Uiso 1 1 calc R . . N1 N 0.7025(3) 0.7111(2) 0.83198(16) 0.0362(9) Uani 1 1 d . . . O2 O 0.6740(2) 0.71914(16) 0.78361(12) 0.0346(7) Uani 1 1 d . . . O3 O 0.6895(2) 0.64643(17) 0.85275(12) 0.0342(7) Uani 1 1 d . . . O4 O 0.7423(3) 0.7635(2) 0.85701(17) 0.0579(10) Uani 1 1 d . . . N5 N 0.7431(3) 0.4500(2) 0.79564(16) 0.0326(8) Uani 1 1 d . . . O6 O 0.7299(2) 0.49934(17) 0.83087(13) 0.0314(7) Uani 1 1 d . . . O7 O 0.6892(2) 0.45631(17) 0.75316(13) 0.0351(7) Uani 1 1 d . . . O8 O 0.8073(3) 0.39694(18) 0.80116(17) 0.0503(10) Uani 1 1 d . . . C100 C 0.6264(5) 0.5494(4) 0.4214(2) 0.0658(17) Uani 1 1 d . . . H10A H 0.6521 0.4966 0.4174 0.079 Uiso 1 1 calc R . . H10B H 0.6070 0.5683 0.3854 0.079 Uiso 1 1 calc R . . Cl1 Cl 0.51264(12) 0.54958(12) 0.46247(7) 0.0736(5) Uani 1 1 d . . . Cl2 Cl 0.72924(13) 0.60583(13) 0.44736(7) 0.0853(7) Uani 1 1 d . . . C110 C 0.5121(5) 0.2102(4) 0.1862(3) 0.078(2) Uani 1 1 d . . . H11A H 0.4619 0.2519 0.1941 0.094 Uiso 1 1 calc R . . H11B H 0.4774 0.1617 0.1959 0.094 Uiso 1 1 calc R . . Cl3 Cl 0.62778(13) 0.22181(8) 0.22456(8) 0.0731(4) Uani 1 1 d . . . Cl4 Cl 0.5424(2) 0.21019(14) 0.11741(9) 0.1053(7) Uani 1 1 d . . . C120 C 1.0424(10) 0.3630(7) 0.6471(4) 0.140(4) Uani 1 1 d . . . H12A H 1.0406 0.3092 0.6356 0.168 Uiso 1 1 calc R A 1 H12B H 1.1025 0.3676 0.6724 0.168 Uiso 1 1 calc R A 1 Cl5 Cl 0.92837(19) 0.37804(13) 0.68405(12) 0.1069(7) Uani 1 1 d . B . Cl6A Cl 1.0770(7) 0.4161(6) 0.5905(4) 0.128(3) Uani 0.50 1 d P B 1 Cl6B Cl 1.0089(9) 0.4031(6) 0.5827(4) 0.153(4) Uani 0.50 1 d P B 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 0.02407(8) 0.02591(8) 0.02534(8) -0.00160(9) 0.00106(9) -0.00003(9) B1 0.034(2) 0.041(2) 0.030(2) 0.000(3) -0.0055(19) 0.000(3) N11 0.029(2) 0.042(2) 0.028(2) -0.0047(16) -0.0007(16) -0.0008(16) N12 0.0274(18) 0.0369(18) 0.0223(18) -0.0002(16) 0.0001(15) -0.0027(14) C13 0.028(2) 0.032(2) 0.031(2) -0.0019(17) 0.0062(17) 0.0104(18) C14 0.027(2) 0.034(2) 0.041(2) -0.008(2) 0.0024(16) -0.002(2) C15 0.028(3) 0.040(2) 0.040(2) -0.0120(18) -0.005(2) 0.000(2) N21 0.0250(18) 0.0273(18) 0.0279(19) -0.0024(14) 0.0051(15) 0.0009(14) C22 0.0192(19) 0.026(2) 0.039(2) -0.0030(17) 0.0034(17) 0.0020(16) C23 0.026(2) 0.0237(18) 0.046(3) -0.0021(17) 0.003(2) -0.0006(17) C24 0.032(3) 0.026(2) 0.045(3) 0.0054(18) 0.0075(19) 0.0040(17) C25 0.0242(19) 0.034(2) 0.036(2) 0.0091(19) 0.0037(16) 0.0063(19) C26 0.026(2) 0.029(2) 0.035(2) -0.0012(17) 0.0005(17) -0.0005(17) C31 0.048(3) 0.041(3) 0.057(3) 0.014(2) 0.004(2) -0.011(2) C32 0.056(3) 0.046(3) 0.060(3) 0.018(2) 0.000(3) -0.011(3) C33 0.049(3) 0.046(3) 0.052(3) 0.016(2) 0.007(3) 0.010(2) C34 0.037(2) 0.042(3) 0.037(2) 0.0094(19) 0.003(2) 0.0041(19) C35 0.040(3) 0.061(3) 0.048(3) 0.017(2) 0.012(2) 0.004(3) C36 0.043(3) 0.100(5) 0.046(3) 0.014(4) 0.014(2) 0.010(4) C37 0.071(4) 0.080(4) 0.044(3) 0.015(3) 0.016(3) 0.000(4) N41 0.031(2) 0.039(2) 0.0262(19) 0.0021(15) -0.0011(15) 0.0012(16) N42 0.0322(19) 0.0365(19) 0.028(2) -0.0014(16) -0.0038(16) -0.0024(15) C43 0.023(2) 0.0197(18) 0.036(3) 0.0076(16) 0.0005(16) 0.0066(15) C44 0.027(2) 0.039(2) 0.035(2) 0.016(2) -0.0013(16) 0.0027(19) C45 0.031(3) 0.046(2) 0.033(2) 0.0128(19) -0.004(2) -0.001(2) N51 0.0273(19) 0.0245(17) 0.035(2) -0.0010(14) 0.0018(15) 0.0007(14) C52 0.022(2) 0.031(2) 0.031(2) -0.0016(17) 0.0053(17) -0.0054(17) C53 0.031(2) 0.0263(19) 0.039(2) 0.0016(16) -0.002(2) 0.008(2) C54 0.029(2) 0.0275(19) 0.045(2) -0.0040(16) 0.005(2) 0.001(2) C55 0.039(2) 0.037(2) 0.030(2) 0.0000(18) 0.0054(18) -0.0021(19) C56 0.036(2) 0.031(2) 0.033(2) 0.0052(17) 0.0020(19) 0.0013(19) C61 0.053(3) 0.043(3) 0.055(3) -0.016(2) -0.002(3) 0.017(2) C62 0.056(3) 0.046(3) 0.056(3) -0.016(2) 0.008(3) 0.007(3) C63 0.057(4) 0.062(4) 0.058(4) -0.008(3) 0.025(3) 0.000(3) C64 0.055(3) 0.041(2) 0.036(2) -0.003(2) 0.009(2) -0.003(2) C65 0.066(4) 0.044(3) 0.035(3) -0.008(2) -0.003(2) 0.006(3) C66 0.063(4) 0.058(3) 0.044(3) -0.003(2) -0.005(3) -0.007(3) C67 0.091(5) 0.064(4) 0.042(3) -0.003(3) 0.000(3) 0.001(4) N71 0.0345(17) 0.0366(16) 0.0264(15) -0.0017(15) 0.0054(15) 0.000(2) N72 0.0233(15) 0.0307(15) 0.0280(16) -0.0020(16) 0.0038(13) -0.0058(17) C73 0.036(2) 0.0296(19) 0.034(2) 0.002(2) 0.0080(17) 0.001(2) C74 0.039(2) 0.044(3) 0.036(2) -0.001(2) 0.0141(18) -0.001(2) C75 0.047(3) 0.043(2) 0.027(2) -0.004(2) 0.0065(19) -0.007(2) N81 0.0271(17) 0.031(2) 0.0353(17) -0.0037(15) 0.0039(14) 0.0027(15) C82 0.0297(19) 0.0264(18) 0.033(2) -0.0041(19) 0.0070(16) -0.0053(19) C83 0.033(2) 0.038(2) 0.040(2) -0.003(2) 0.0128(18) -0.007(2) C84 0.0286(19) 0.033(2) 0.046(2) 0.003(2) 0.014(2) -0.0025(18) C85 0.027(2) 0.0277(19) 0.047(3) -0.0040(18) 0.006(2) 0.0007(15) C86 0.0279(19) 0.034(2) 0.035(2) -0.0036(15) 0.0059(19) -0.0001(18) C91 0.028(2) 0.048(2) 0.053(3) -0.001(3) 0.0150(19) -0.003(2) C92 0.0199(18) 0.045(3) 0.052(3) -0.002(2) 0.010(2) -0.0012(17) C93 0.032(3) 0.040(3) 0.071(4) -0.012(2) 0.003(2) -0.007(2) C94 0.023(2) 0.044(2) 0.047(3) -0.005(2) 0.0024(19) 0.0026(18) C95 0.027(2) 0.044(2) 0.040(3) -0.001(2) 0.002(2) 0.0027(19) C96 0.038(3) 0.041(3) 0.064(3) 0.003(2) 0.003(2) 0.004(2) C97 0.029(3) 0.074(4) 0.068(4) -0.002(3) -0.005(2) 0.008(2) N1 0.0270(19) 0.035(2) 0.046(2) -0.0102(17) -0.0040(17) 0.0044(16) O2 0.0306(16) 0.0293(14) 0.044(2) 0.0012(12) 0.0011(14) -0.0024(12) O3 0.0340(17) 0.0319(16) 0.0366(17) -0.0037(13) -0.0020(14) 0.0027(13) O4 0.063(2) 0.0362(19) 0.075(3) -0.0190(18) -0.027(2) -0.0044(17) N5 0.0259(19) 0.0265(17) 0.045(2) -0.0028(16) 0.0010(17) -0.0010(15) O6 0.0286(16) 0.0285(15) 0.0370(17) -0.0033(13) -0.0001(13) 0.0023(12) O7 0.0299(16) 0.0354(16) 0.0400(17) -0.0058(13) -0.0004(14) -0.0006(13) O8 0.041(2) 0.0327(19) 0.077(3) -0.0010(16) -0.0083(18) 0.0146(14) C100 0.045(3) 0.100(5) 0.053(3) -0.016(3) 0.014(3) -0.015(3) Cl1 0.0424(8) 0.1163(14) 0.0619(10) -0.0070(9) 0.0075(7) -0.0068(8) Cl2 0.0499(9) 0.1429(19) 0.0632(10) -0.0337(11) 0.0116(7) -0.0252(10) C110 0.056(4) 0.064(4) 0.114(6) -0.027(4) -0.007(4) 0.004(3) Cl3 0.0701(10) 0.0504(7) 0.0990(12) -0.0166(8) -0.0174(11) -0.0034(7) Cl4 0.127(2) 0.1023(15) 0.0864(15) 0.0184(12) -0.0102(13) 0.0082(14) C120 0.161(11) 0.161(10) 0.099(8) 0.009(7) 0.017(7) 0.059(9) Cl5 0.0975(16) 0.0809(13) 0.142(2) 0.0087(13) -0.0090(15) 0.0030(12) Cl6A 0.149(7) 0.119(5) 0.118(5) 0.007(4) 0.015(5) 0.003(5) Cl6B 0.243(11) 0.108(5) 0.109(5) -0.013(4) 0.051(8) 0.008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 N72 2.477(3) . ? Tb1 O3 2.491(3) . ? Tb1 N12 2.491(3) . ? Tb1 O7 2.506(3) . ? Tb1 O2 2.519(3) . ? Tb1 N42 2.523(4) . ? Tb1 O6 2.571(3) . ? Tb1 N81 2.642(3) . ? Tb1 N21 2.643(4) . ? Tb1 N51 2.735(4) . ? Tb1 N1 2.921(4) . ? Tb1 N5 2.950(4) . ? B1 N41 1.539(7) . ? B1 N11 1.543(7) . ? B1 N71 1.551(6) . ? N11 N12 1.346(5) . ? N11 C15 1.366(6) . ? N12 C13 1.339(6) . ? C13 C14 1.371(6) . ? C13 C22 1.471(6) . ? C14 C15 1.378(7) . ? N21 C26 1.343(6) . ? N21 C22 1.361(5) . ? C22 C23 1.392(6) . ? C23 C24 1.379(6) . ? C24 C25 1.381(6) . ? C24 C31 1.532(6) . ? C25 C26 1.407(6) . ? C25 C34 1.504(6) . ? C31 C32 1.540(7) . ? C32 C33 1.546(8) . ? C32 C35 1.553(8) . ? C33 C34 1.545(7) . ? C34 C35 1.582(7) . ? C35 C36 1.496(8) . ? C35 C37 1.534(7) . ? N41 C45 1.361(6) . ? N41 N42 1.362(5) . ? N42 C43 1.345(6) . ? C43 C44 1.432(6) . ? C43 C52 1.448(6) . ? C44 C45 1.329(7) . ? N51 C56 1.341(6) . ? N51 C52 1.362(6) . ? C52 C53 1.389(6) . ? C53 C54 1.392(6) . ? C54 C55 1.401(6) . ? C54 C61 1.531(6) . ? C55 C56 1.390(6) . ? C55 C64 1.504(6) . ? C61 C62 1.531(8) . ? C62 C65 1.557(8) . ? C62 C63 1.568(8) . ? C63 C64 1.556(8) . ? C64 C65 1.577(7) . ? C65 C66 1.497(8) . ? C65 C67 1.553(8) . ? N71 C75 1.339(5) . ? N71 N72 1.360(5) . ? N72 C73 1.341(5) . ? C73 C74 1.406(6) . ? C73 C82 1.463(6) . ? C74 C75 1.363(7) . ? N81 C86 1.349(6) . ? N81 C82 1.351(5) . ? C82 C83 1.397(6) . ? C83 C84 1.389(7) . ? C84 C85 1.379(7) . ? C84 C91 1.517(6) . ? C85 C86 1.402(6) . ? C85 C94 1.498(7) . ? C91 C92 1.539(7) . ? C92 C93 1.552(6) . ? C92 C95 1.586(7) . ? C93 C94 1.557(7) . ? C94 C95 1.578(6) . ? C95 C97 1.496(7) . ? C95 C96 1.505(7) . ? N1 O4 1.222(5) . ? N1 O3 1.263(5) . ? N1 O2 1.268(5) . ? N5 O8 1.244(5) . ? N5 O6 1.249(5) . ? N5 O7 1.265(5) . ? C100 Cl2 1.758(6) . ? C100 Cl1 1.764(6) . ? C110 Cl3 1.758(7) . ? C110 Cl4 1.760(9) . ? C120 Cl5 1.730(11) . ? C120 Cl6A 1.750(15) . ? C120 Cl6B 1.807(15) . ? 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 N72 Tb1 O3 131.78(11) . . ? N72 Tb1 N12 72.47(11) . . ? O3 Tb1 N12 155.71(11) . . ? N72 Tb1 O7 73.16(11) . . ? O3 Tb1 O7 113.28(10) . . ? N12 Tb1 O7 71.39(11) . . ? N72 Tb1 O2 91.16(11) . . ? O3 Tb1 O2 51.06(10) . . ? N12 Tb1 O2 140.88(11) . . ? O7 Tb1 O2 138.44(10) . . ? N72 Tb1 N42 70.62(12) . . ? O3 Tb1 N42 115.66(11) . . ? N12 Tb1 N42 66.62(10) . . ? O7 Tb1 N42 130.73(11) . . ? O2 Tb1 N42 74.50(11) . . ? N72 Tb1 O6 112.83(11) . . ? O3 Tb1 O6 64.39(10) . . ? N12 Tb1 O6 111.39(11) . . ? O7 Tb1 O6 49.99(10) . . ? O2 Tb1 O6 107.69(10) . . ? N42 Tb1 O6 175.63(12) . . ? N72 Tb1 N81 62.84(11) . . ? O3 Tb1 N81 74.87(11) . . ? N12 Tb1 N81 126.75(11) . . ? O7 Tb1 N81 69.23(11) . . ? O2 Tb1 N81 69.37(11) . . ? N42 Tb1 N81 118.89(12) . . ? O6 Tb1 N81 65.46(11) . . ? N72 Tb1 N21 130.31(11) . . ? O3 Tb1 N21 94.51(11) . . ? N12 Tb1 N21 63.46(11) . . ? O7 Tb1 N21 72.04(10) . . ? O2 Tb1 N21 137.88(10) . . ? N42 Tb1 N21 108.95(12) . . ? O6 Tb1 N21 66.84(10) . . ? N81 Tb1 N21 130.96(11) . . ? N72 Tb1 N51 130.50(12) . . ? O3 Tb1 N51 66.16(10) . . ? N12 Tb1 N51 97.89(12) . . ? O7 Tb1 N51 151.03(10) . . ? O2 Tb1 N51 65.74(10) . . ? N42 Tb1 N51 61.41(11) . . ? O6 Tb1 N51 115.73(11) . . ? N81 Tb1 N51 132.80(11) . . ? N21 Tb1 N51 79.08(10) . . ? N72 Tb1 N1 112.42(12) . . ? O3 Tb1 N1 25.44(11) . . ? N12 Tb1 N1 159.29(11) . . ? O7 Tb1 N1 129.24(10) . . ? O2 Tb1 N1 25.62(10) . . ? N42 Tb1 N1 95.37(11) . . ? O6 Tb1 N1 85.82(11) . . ? N81 Tb1 N1 70.11(11) . . ? N21 Tb1 N1 116.97(12) . . ? N51 Tb1 N1 63.19(11) . . ? N72 Tb1 N5 92.07(12) . . ? O3 Tb1 N5 88.35(10) . . ? N12 Tb1 N5 92.62(11) . . ? O7 Tb1 N5 25.16(10) . . ? O2 Tb1 N5 123.98(10) . . ? N42 Tb1 N5 155.88(12) . . ? O6 Tb1 N5 24.96(10) . . ? N81 Tb1 N5 63.00(11) . . ? N21 Tb1 N5 69.07(10) . . ? N51 Tb1 N5 137.36(11) . . ? N1 Tb1 N5 106.99(11) . . ? N41 B1 N11 107.1(3) . . ? N41 B1 N71 108.6(4) . . ? N11 B1 N71 108.7(4) . . ? N12 N11 C15 108.8(4) . . ? N12 N11 B1 120.1(4) . . ? C15 N11 B1 130.9(4) . . ? C13 N12 N11 107.5(4) . . ? C13 N12 Tb1 122.9(3) . . ? N11 N12 Tb1 129.5(3) . . ? N12 C13 C14 110.2(4) . . ? N12 C13 C22 118.4(4) . . ? C14 C13 C22 130.9(4) . . ? C13 C14 C15 105.5(4) . . ? N11 C15 C14 108.0(4) . . ? C26 N21 C22 117.9(4) . . ? C26 N21 Tb1 123.5(3) . . ? C22 N21 Tb1 117.7(3) . . ? N21 C22 C23 121.8(4) . . ? N21 C22 C13 115.8(4) . . ? C23 C22 C13 122.3(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 119.4(4) . . ? C23 C24 C31 123.0(4) . . ? C25 C24 C31 117.6(4) . . ? C24 C25 C26 118.3(4) . . ? C24 C25 C34 117.7(4) . . ? C26 C25 C34 124.0(4) . . ? N21 C26 C25 122.9(4) . . ? C24 C31 C32 110.1(4) . . ? C31 C32 C33 108.8(5) . . ? C31 C32 C35 111.6(4) . . ? C33 C32 C35 88.4(4) . . ? C34 C33 C32 86.0(4) . . ? C25 C34 C33 105.7(4) . . ? C25 C34 C35 110.7(4) . . ? C33 C34 C35 87.4(4) . . ? C36 C35 C37 109.5(5) . . ? C36 C35 C32 119.0(5) . . ? C37 C35 C32 112.2(4) . . ? C36 C35 C34 119.5(4) . . ? C37 C35 C34 110.1(5) . . ? C32 C35 C34 84.5(4) . . ? C45 N41 N42 108.7(4) . . ? C45 N41 B1 130.6(4) . . ? N42 N41 B1 119.2(4) . . ? C43 N42 N41 106.8(4) . . ? C43 N42 Tb1 124.0(3) . . ? N41 N42 Tb1 128.9(3) . . ? N42 C43 C44 109.1(4) . . ? N42 C43 C52 118.0(4) . . ? C44 C43 C52 132.4(4) . . ? C45 C44 C43 104.7(4) . . ? C44 C45 N41 110.5(4) . . ? C56 N51 C52 117.4(4) . . ? C56 N51 Tb1 124.9(3) . . ? C52 N51 Tb1 115.0(3) . . ? N51 C52 C53 122.7(4) . . ? N51 C52 C43 115.6(4) . . ? C53 C52 C43 121.4(4) . . ? C52 C53 C54 118.9(4) . . ? C53 C54 C55 118.9(4) . . ? C53 C54 C61 123.1(4) . . ? C55 C54 C61 117.9(4) . . ? C56 C55 C54 118.1(4) . . ? C56 C55 C64 124.5(4) . . ? C54 C55 C64 117.4(4) . . ? N51 C56 C55 123.7(4) . . ? C62 C61 C54 109.8(4) . . ? C61 C62 C65 111.4(5) . . ? C61 C62 C63 109.8(5) . . ? C65 C62 C63 87.8(4) . . ? C64 C63 C62 85.7(4) . . ? C55 C64 C63 107.1(4) . . ? C55 C64 C65 108.6(4) . . ? C63 C64 C65 87.5(4) . . ? C66 C65 C67 109.7(5) . . ? C66 C65 C62 119.6(5) . . ? C67 C65 C62 111.0(5) . . ? C66 C65 C64 118.9(4) . . ? C67 C65 C64 110.3(5) . . ? C62 C65 C64 85.4(4) . . ? C75 N71 N72 110.3(4) . . ? C75 N71 B1 130.3(4) . . ? N72 N71 B1 119.4(3) . . ? C73 N72 N71 105.9(3) . . ? C73 N72 Tb1 123.9(3) . . ? N71 N72 Tb1 130.0(2) . . ? N72 C73 C74 110.2(4) . . ? N72 C73 C82 118.2(3) . . ? C74 C73 C82 131.6(4) . . ? C75 C74 C73 104.7(4) . . ? N71 C75 C74 109.0(4) . . ? C86 N81 C82 117.4(3) . . ? C86 N81 Tb1 123.5(3) . . ? C82 N81 Tb1 119.0(3) . . ? N81 C82 C83 122.3(4) . . ? N81 C82 C73 115.2(3) . . ? C83 C82 C73 122.5(4) . . ? C84 C83 C82 119.9(4) . . ? C85 C84 C83 117.9(4) . . ? C85 C84 C91 118.5(4) . . ? C83 C84 C91 123.6(4) . . ? C84 C85 C86 119.4(4) . . ? C84 C85 C94 118.4(4) . . ? C86 C85 C94 122.2(4) . . ? N81 C86 C85 122.9(4) . . ? C84 C91 C92 109.8(4) . . ? C91 C92 C93 108.9(4) . . ? C91 C92 C95 112.8(4) . . ? C93 C92 C95 86.5(4) . . ? C92 C93 C94 86.9(3) . . ? C85 C94 C93 107.1(4) . . ? C85 C94 C95 109.0(4) . . ? C93 C94 C95 86.6(3) . . ? C97 C95 C96 109.7(4) . . ? C97 C95 C94 110.3(4) . . ? C96 C95 C94 118.3(4) . . ? C97 C95 C92 113.8(4) . . ? C96 C95 C92 117.8(4) . . ? C94 C95 C92 85.0(3) . . ? O4 N1 O3 121.6(4) . . ? O4 N1 O2 121.3(4) . . ? O3 N1 O2 117.1(3) . . ? O4 N1 Tb1 178.8(3) . . ? O3 N1 Tb1 57.9(2) . . ? O2 N1 Tb1 59.20(19) . . ? N1 O2 Tb1 95.2(2) . . ? N1 O3 Tb1 96.7(2) . . ? O8 N5 O6 122.2(4) . . ? O8 N5 O7 120.6(4) . . ? O6 N5 O7 117.2(3) . . ? O8 N5 Tb1 172.3(3) . . ? O6 N5 Tb1 60.3(2) . . ? O7 N5 Tb1 57.4(2) . . ? N5 O6 Tb1 94.7(2) . . ? N5 O7 Tb1 97.5(2) . . ? Cl2 C100 Cl1 112.7(3) . . ? Cl3 C110 Cl4 110.6(4) . . ? Cl5 C120 Cl6A 123.8(7) . . ? Cl5 C120 Cl6B 102.7(7) . . ? Cl6A C120 Cl6B 29.6(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.088 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.096 #=END