Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Singh, Udai P.' 'Gorner, Helmut' 'Sharma, Chokhe Lal' 'Tyagi, Shalu' 'Weyhermuller, Thomas' _publ_contact_author_name 'Dr Udai P Singh' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Roorkee Roorkee 247 667 INDIA ; _publ_contact_author_email 'UDAIPFCY@IITR.ERNET.IN' _publ_section_title ; Synthesis, molecular structure and emission properties of benzoato-bridged lanthanide complexes with hydrotis(pyrazolyl)borate ; data_1 _database_code_CSD 186521 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C46 H40 B2 Gd2 N12 O8], (C H2 Cl2)' _chemical_formula_analytical ? _chemical_formula_sum 'C47 H42 B2 Cl2 Gd2 N12 O8' _chemical_formula_weight 1309.94 _chemical_melting_point ? _chemical_compound_source ? 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' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5351(8) _cell_length_b 13.0435(8) _cell_length_c 16.3461(12) _cell_angle_alpha 72.56(1) _cell_angle_beta 83.37(1) _cell_angle_gamma 89.58(1) _cell_volume 2531.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7914 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method ? _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 2.767 _exptl_absorpt_correction_type 'Gaussian, Face indexed' _exptl_absorpt_correction_T_min 0.527 _exptl_absorpt_correction_T_max 0.721 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD-Detector' _diffrn_measurement_method '\w, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28063 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 33.18 _reflns_number_total 16666 _reflns_number_observed 12664 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT 6' _computing_cell_refinement 'Siemens SAINT 6' _computing_data_reduction 'Siemens SAINT 6' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0236P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16662 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_obs 0.0292 _refine_ls_wR_factor_all 0.0584 _refine_ls_wR_factor_obs 0.0553 _refine_ls_goodness_of_fit_all 0.917 _refine_ls_goodness_of_fit_obs 1.002 _refine_ls_restrained_S_all 0.917 _refine_ls_restrained_S_obs 1.002 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Gd1 Gd 0.464121(9) -0.023383(9) -0.107472(7) 0.01155(3) Uani 1 d . . B1 B 0.3672(2) -0.1533(2) -0.2553(2) 0.0181(6) Uani 1 d . . H1 H 0.3407(2) -0.1882(2) -0.2961(2) 0.022 Uiso 1 calc R . N1 N 0.2707(2) -0.1228(2) -0.20086(14) 0.0181(4) Uani 1 d . . N2 N 0.2840(2) -0.0718(2) -0.14033(13) 0.0168(4) Uani 1 d . . C3 C 0.1850(2) -0.0584(2) -0.1051(2) 0.0232(6) Uani 1 d . . H3 H 0.1698(2) -0.0249(2) -0.0610(2) 0.028 Uiso 1 calc R . C4 C 0.1076(2) -0.1000(2) -0.1419(2) 0.0293(7) Uani 1 d . . H4 H 0.0318(2) -0.1011(2) -0.1283(2) 0.035 Uiso 1 calc R . C5 C 0.1652(2) -0.1394(2) -0.2026(2) 0.0244(6) Uani 1 d . . H5 H 0.1354(2) -0.1727(2) -0.2394(2) 0.029 Uiso 1 calc R . N6 N 0.4363(2) -0.2318(2) -0.19534(14) 0.0179(4) Uani 1 d . . N7 N 0.4755(2) -0.2078(2) -0.12848(14) 0.0183(4) Uani 1 d . . C8 C 0.5260(2) -0.2952(2) -0.0874(2) 0.0234(6) Uani 1 d . . H8 H 0.5610(2) -0.3017(2) -0.0376(2) 0.028 Uiso 1 calc R . C9 C 0.5211(2) -0.3757(2) -0.1269(2) 0.0275(6) Uani 1 d . . H9 H 0.5504(2) -0.4452(2) -0.1103(2) 0.033 Uiso 1 calc R . C10 C 0.4643(2) -0.3320(2) -0.1951(2) 0.0234(6) Uani 1 d . . H10 H 0.4473(2) -0.3666(2) -0.2357(2) 0.028 Uiso 1 calc R . N11 N 0.4338(2) -0.0500(2) -0.30711(13) 0.0173(4) Uani 1 d . . N12 N 0.4849(2) 0.0111(2) -0.26735(13) 0.0157(4) Uani 1 d . . C13 C 0.5337(2) 0.0928(2) -0.3315(2) 0.0184(5) Uani 1 d . . H13 H 0.5757(2) 0.1483(2) -0.3231(2) 0.022 Uiso 1 calc R . C14 C 0.5149(2) 0.0857(2) -0.4115(2) 0.0233(6) Uani 1 d . . H14 H 0.5402(2) 0.1334(2) -0.4668(2) 0.028 Uiso 1 calc R . C15 C 0.4515(2) -0.0055(2) -0.3931(2) 0.0219(6) Uani 1 d . . H15 H 0.4245(2) -0.0329(2) -0.4346(2) 0.026 Uiso 1 calc R . O16 O 0.55424(14) 0.14657(14) -0.17321(11) 0.0174(4) Uani 1 d . . O17 O 0.57371(14) 0.11611(14) -0.03593(11) 0.0170(4) Uani 1 d . . C16 C 0.5903(2) 0.1744(2) -0.1140(2) 0.0145(5) Uani 1 d . . C17 C 0.6530(2) 0.2778(2) -0.1366(2) 0.0157(5) Uani 1 d . . C18 C 0.7010(2) 0.3085(2) -0.0746(2) 0.0242(6) Uani 1 d . . H18 H 0.6944(2) 0.2633(2) -0.0165(2) 0.029 Uiso 1 calc R . C19 C 0.7586(2) 0.4056(2) -0.0980(2) 0.0311(7) Uani 1 d . . H19 H 0.7920(2) 0.4265(2) -0.0560(2) 0.037 Uiso 1 calc R . C20 C 0.7675(2) 0.4722(2) -0.1826(2) 0.0319(7) Uani 1 d . . H20 H 0.8062(2) 0.5389(2) -0.1980(2) 0.038 Uiso 1 calc R . C21 C 0.7204(2) 0.4422(2) -0.2446(2) 0.0265(6) Uani 1 d . . H21 H 0.7272(2) 0.4877(2) -0.3026(2) 0.032 Uiso 1 calc R . C22 C 0.6630(2) 0.3451(2) -0.2214(2) 0.0192(5) Uani 1 d . . H22 H 0.6302(2) 0.3244(2) -0.2638(2) 0.023 Uiso 1 calc R . O23 O 0.63202(13) -0.08692(14) -0.07387(11) 0.0156(3) Uani 1 d . . O24 O 0.65567(13) -0.09061(14) 0.06067(11) 0.0162(4) Uani 1 d . . C23 C 0.6790(2) -0.1188(2) -0.0068(2) 0.0153(5) Uani 1 d . . C24 C 0.7682(2) -0.1963(2) -0.0068(2) 0.0147(5) Uani 1 d . . C25 C 0.7948(2) -0.2325(2) -0.0780(2) 0.0181(5) Uani 1 d . . H25 H 0.7574(2) -0.2070(2) -0.1273(2) 0.022 Uiso 1 calc R . C26 C 0.8756(2) -0.3057(2) -0.0776(2) 0.0216(5) Uani 1 d . . H26 H 0.8941(2) -0.3297(2) -0.1267(2) 0.026 Uiso 1 calc R . C27 C 0.9295(2) -0.3439(2) -0.0052(2) 0.0225(6) Uani 1 d . . H27 H 0.9846(2) -0.3945(2) -0.0045(2) 0.027 Uiso 1 calc R . C28 C 0.9028(2) -0.3080(2) 0.0657(2) 0.0203(5) Uani 1 d . . H28 H 0.9396(2) -0.3343(2) 0.1152(2) 0.024 Uiso 1 calc R . C29 C 0.8230(2) -0.2342(2) 0.0654(2) 0.0168(5) Uani 1 d . . H29 H 0.8056(2) -0.2094(2) 0.1142(2) 0.020 Uiso 1 calc R . Gd2 Gd 0.873240(9) 0.485932(9) 0.440512(7) 0.01141(3) Uani 1 d . . B101 B 0.6667(2) 0.5528(2) 0.2927(2) 0.0178(6) Uani 1 d . . H101 H 0.6106(2) 0.5710(2) 0.2522(2) 0.021 Uiso 1 calc R . N101 N 0.7621(2) 0.4987(2) 0.25337(13) 0.0164(4) Uani 1 d . . N102 N 0.8514(2) 0.4688(2) 0.29415(13) 0.0180(4) Uani 1 d . . C103 C 0.9134(2) 0.4204(2) 0.2447(2) 0.0212(5) Uani 1 d . . H103 H 0.9816(2) 0.3916(2) 0.2570(2) 0.025 Uiso 1 calc R . C104 C 0.8643(2) 0.4183(2) 0.1733(2) 0.0240(6) Uani 1 d . . H104 H 0.8907(2) 0.3882(2) 0.1290(2) 0.029 Uiso 1 calc R . C105 C 0.7691(2) 0.4694(2) 0.1809(2) 0.0205(5) Uani 1 d . . H105 H 0.7169(2) 0.4820(2) 0.1415(2) 0.025 Uiso 1 calc R . N106 N 0.7075(2) 0.6555(2) 0.30739(13) 0.0163(4) Uani 1 d . . N107 N 0.7859(2) 0.6524(2) 0.35967(14) 0.0176(4) Uani 1 d . . C108 C 0.8023(2) 0.7542(2) 0.3583(2) 0.0192(5) Uani 1 d . . H108 H 0.8528(2) 0.7763(2) 0.3892(2) 0.023 Uiso 1 calc R . C109 C 0.7361(2) 0.8233(2) 0.3061(2) 0.0222(6) Uani 1 d . . H109 H 0.7321(2) 0.8990(2) 0.2946(2) 0.027 Uiso 1 calc R . C110 C 0.6772(2) 0.7573(2) 0.2747(2) 0.0208(5) Uani 1 d . . H110 H 0.6242(2) 0.7801(2) 0.2364(2) 0.025 Uiso 1 calc R . N111 N 0.6186(2) 0.4740(2) 0.37944(13) 0.0165(4) Uani 1 d . . N112 N 0.6792(2) 0.4332(2) 0.44590(13) 0.0168(4) Uani 1 d . . C113 C 0.6127(2) 0.3696(2) 0.5105(2) 0.0197(5) Uani 1 d . . H113 H 0.6332(2) 0.3301(2) 0.5651(2) 0.024 Uiso 1 calc R . C114 C 0.5094(2) 0.3688(2) 0.4876(2) 0.0232(6) Uani 1 d . . H114 H 0.4476(2) 0.3304(2) 0.5218(2) 0.028 Uiso 1 calc R . C115 C 0.5167(2) 0.4357(2) 0.4044(2) 0.0192(5) Uani 1 d . . H115 H 0.4592(2) 0.4524(2) 0.3699(2) 0.023 Uiso 1 calc R . O116 O 0.83276(14) 0.33320(14) 0.56078(11) 0.0193(4) Uani 1 d . . O117 O 0.97944(13) 0.39742(14) 0.59247(11) 0.0174(4) Uani 1 d . . C116 C 0.9026(2) 0.3281(2) 0.6111(2) 0.0162(5) Uani 1 d . . C117 C 0.8936(2) 0.2388(2) 0.6934(2) 0.0145(5) Uani 1 d . . C118 C 0.8234(2) 0.1519(2) 0.7044(2) 0.0175(5) Uani 1 d . . H118 H 0.7847(2) 0.1489(2) 0.6584(2) 0.021 Uiso 1 calc R . C119 C 0.8100(2) 0.0702(2) 0.7818(2) 0.0189(5) Uani 1 d . . H119 H 0.7624(2) 0.0109(2) 0.7890(2) 0.023 Uiso 1 calc R . C120 C 0.8660(2) 0.0750(2) 0.8488(2) 0.0251(6) Uani 1 d . . H120 H 0.8559(2) 0.0195(2) 0.9024(2) 0.030 Uiso 1 calc R . C121 C 0.9367(2) 0.1603(2) 0.8380(2) 0.0295(7) Uani 1 d . . H121 H 0.9759(2) 0.1623(2) 0.8839(2) 0.035 Uiso 1 calc R . C122 C 0.9509(2) 0.2428(2) 0.7606(2) 0.0221(6) Uani 1 d . . H122 H 0.9992(2) 0.3014(2) 0.7534(2) 0.026 Uiso 1 calc R . O123 O 0.83845(13) 0.57997(14) 0.54040(11) 0.0158(3) Uani 1 d . . O124 O 0.98805(13) 0.62349(14) 0.58668(11) 0.0177(4) Uani 1 d . . C123 C 0.8899(2) 0.6335(2) 0.57643(15) 0.0146(5) Uani 1 d . . C124 C 0.8285(2) 0.7143(2) 0.6105(2) 0.0155(5) Uani 1 d . . C125 C 0.8787(2) 0.7772(2) 0.6508(2) 0.0187(5) Uani 1 d . . H125 H 0.9536(2) 0.7716(2) 0.6549(2) 0.022 Uiso 1 calc R . C126 C 0.8196(2) 0.8481(2) 0.6851(2) 0.0253(6) Uani 1 d . . H126 H 0.8541(2) 0.8906(2) 0.7131(2) 0.030 Uiso 1 calc R . C127 C 0.7106(2) 0.8572(2) 0.6787(2) 0.0279(6) Uani 1 d . . H127 H 0.6699(2) 0.9047(2) 0.7033(2) 0.033 Uiso 1 calc R . C128 C 0.6609(2) 0.7967(2) 0.6364(2) 0.0254(6) Uani 1 d . . H128 H 0.5865(2) 0.8042(2) 0.6306(2) 0.030 Uiso 1 calc R . C129 C 0.7194(2) 0.7256(2) 0.6024(2) 0.0185(5) Uani 1 d . . H129 H 0.6850(2) 0.6844(2) 0.5734(2) 0.022 Uiso 1 calc R . C200 C 0.8326(3) 0.9954(3) 0.4534(2) 0.0428(8) Uani 1 d . . H20A H 0.8267(3) 0.9469(3) 0.5134(2) 0.051 Uiso 1 calc R . H20B H 0.7720(3) 0.9772(3) 0.4260(2) 0.051 Uiso 1 calc R . Cl1 Cl 0.95265(7) 0.97143(7) 0.39781(6) 0.0472(2) Uani 1 d . . Cl2 Cl 0.82029(7) 1.12830(7) 0.45633(6) 0.0445(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01362(6) 0.01117(6) 0.00983(5) -0.00272(4) -0.00243(4) 0.00059(4) B1 0.0189(13) 0.0195(14) 0.0199(14) -0.0115(12) -0.0040(12) -0.0002(11) N1 0.0166(10) 0.0191(11) 0.0211(11) -0.0091(9) -0.0049(9) -0.0002(8) N2 0.0166(10) 0.0194(10) 0.0159(10) -0.0072(9) -0.0028(8) 0.0002(8) C3 0.0165(12) 0.0249(14) 0.0290(15) -0.0110(12) 0.0012(11) 0.0011(10) C4 0.0145(12) 0.032(2) 0.047(2) -0.0201(14) -0.0029(13) -0.0011(11) C5 0.0188(13) 0.0235(14) 0.036(2) -0.0145(12) -0.0106(12) 0.0008(11) N6 0.0156(10) 0.0175(10) 0.0225(11) -0.0090(9) -0.0022(9) 0.0000(8) N7 0.0185(10) 0.0160(10) 0.0231(11) -0.0087(9) -0.0059(9) 0.0008(8) C8 0.0206(13) 0.0152(12) 0.034(2) -0.0046(11) -0.0098(12) 0.0021(10) C9 0.0263(14) 0.0139(12) 0.045(2) -0.0114(12) -0.0067(13) 0.0052(11) C10 0.0209(13) 0.0182(13) 0.034(2) -0.0138(12) 0.0025(12) -0.0009(10) N11 0.0199(10) 0.0201(11) 0.0144(10) -0.0084(9) -0.0029(8) 0.0018(9) N12 0.0184(10) 0.0160(10) 0.0147(10) -0.0074(8) -0.0020(8) 0.0000(8) C13 0.0219(12) 0.0166(12) 0.0159(12) -0.0045(10) -0.0004(10) 0.0029(10) C14 0.034(2) 0.0226(13) 0.0120(11) -0.0055(10) 0.0008(11) 0.0020(12) C15 0.0310(14) 0.0253(14) 0.0130(12) -0.0107(11) -0.0047(11) 0.0063(11) O16 0.0219(9) 0.0160(8) 0.0148(8) -0.0043(7) -0.0049(7) -0.0023(7) O17 0.0191(9) 0.0173(9) 0.0117(8) -0.0005(7) -0.0004(7) -0.0011(7) C16 0.0144(11) 0.0142(11) 0.0140(11) -0.0033(9) -0.0013(9) 0.0004(9) C17 0.0152(11) 0.0139(11) 0.0175(12) -0.0051(9) 0.0006(10) 0.0006(9) C18 0.0252(14) 0.0251(14) 0.0229(14) -0.0077(11) -0.0035(11) -0.0054(11) C19 0.035(2) 0.029(2) 0.034(2) -0.0158(14) -0.0048(14) -0.0112(13) C20 0.031(2) 0.0204(14) 0.042(2) -0.0088(13) 0.0035(14) -0.0088(12) C21 0.0265(14) 0.0194(13) 0.0281(15) -0.0015(11) 0.0043(12) -0.0052(11) C22 0.0222(13) 0.0167(12) 0.0173(12) -0.0040(10) 0.0011(10) -0.0018(10) O23 0.0153(8) 0.0179(9) 0.0137(8) -0.0045(7) -0.0023(7) 0.0002(7) O24 0.0180(8) 0.0169(9) 0.0157(8) -0.0074(7) -0.0031(7) 0.0031(7) C23 0.0138(11) 0.0133(11) 0.0168(12) -0.0025(9) 0.0007(10) -0.0025(9) C24 0.0128(11) 0.0135(11) 0.0174(12) -0.0046(9) 0.0001(9) -0.0014(9) C25 0.0199(12) 0.0200(12) 0.0157(12) -0.0068(10) -0.0030(10) 0.0007(10) C26 0.0247(13) 0.0231(13) 0.0183(13) -0.0102(11) 0.0022(11) 0.0030(11) C27 0.0191(12) 0.0197(13) 0.0285(14) -0.0079(11) -0.0013(11) 0.0057(10) C28 0.0206(12) 0.0216(13) 0.0193(12) -0.0056(10) -0.0067(10) 0.0027(10) C29 0.0176(12) 0.0164(12) 0.0167(12) -0.0059(10) -0.0015(10) -0.0003(9) Gd2 0.01028(5) 0.01034(5) 0.01399(6) -0.00358(4) -0.00322(4) 0.00042(4) B101 0.0163(13) 0.0200(14) 0.0181(14) -0.0055(11) -0.0073(11) 0.0040(11) N101 0.0157(10) 0.0191(10) 0.0153(10) -0.0058(8) -0.0037(8) 0.0001(8) N102 0.0185(10) 0.0203(11) 0.0167(10) -0.0073(9) -0.0036(9) 0.0029(9) C103 0.0222(13) 0.0197(13) 0.0196(13) -0.0041(10) 0.0006(11) 0.0040(10) C104 0.0319(15) 0.0245(14) 0.0159(12) -0.0078(11) 0.0011(11) 0.0016(12) C105 0.0257(13) 0.0235(13) 0.0133(11) -0.0058(10) -0.0049(10) -0.0033(11) N106 0.0150(10) 0.0187(10) 0.0152(10) -0.0040(8) -0.0049(8) 0.0037(8) N107 0.0172(10) 0.0180(10) 0.0193(11) -0.0055(9) -0.0087(9) 0.0020(8) C108 0.0217(12) 0.0138(11) 0.0220(13) -0.0046(10) -0.0045(10) 0.0008(10) C109 0.0302(14) 0.0146(12) 0.0205(13) -0.0031(10) -0.0039(11) 0.0061(11) C110 0.0226(13) 0.0206(13) 0.0171(12) -0.0016(10) -0.0045(11) 0.0079(11) N111 0.0134(9) 0.0198(10) 0.0166(10) -0.0048(8) -0.0045(8) -0.0008(8) N112 0.0139(10) 0.0185(10) 0.0176(10) -0.0041(8) -0.0038(8) -0.0011(8) C113 0.0171(12) 0.0206(13) 0.0192(12) -0.0023(10) -0.0022(10) -0.0024(10) C114 0.0163(12) 0.0259(14) 0.0257(14) -0.0060(12) 0.0005(11) -0.0056(11) C115 0.0129(11) 0.0244(13) 0.0218(13) -0.0085(11) -0.0036(10) 0.0009(10) O116 0.0173(9) 0.0172(9) 0.0209(9) 0.0001(7) -0.0070(7) -0.0013(7) O117 0.0161(8) 0.0125(8) 0.0214(9) -0.0027(7) 0.0004(7) -0.0033(7) C116 0.0142(11) 0.0137(11) 0.0196(12) -0.0037(10) -0.0012(10) 0.0020(9) C117 0.0140(11) 0.0132(11) 0.0148(11) -0.0022(9) -0.0008(9) 0.0008(9) C118 0.0171(11) 0.0154(11) 0.0207(12) -0.0066(10) -0.0020(10) 0.0008(9) C119 0.0198(12) 0.0148(11) 0.0201(13) -0.0044(10) 0.0039(10) -0.0033(10) C120 0.0269(14) 0.0232(14) 0.0189(13) 0.0016(11) 0.0010(11) -0.0019(11) C121 0.033(2) 0.033(2) 0.0195(14) -0.0008(12) -0.0085(12) -0.0073(13) C122 0.0227(13) 0.0214(13) 0.0202(13) -0.0025(11) -0.0047(11) -0.0068(11) O123 0.0154(8) 0.0161(8) 0.0172(8) -0.0068(7) -0.0032(7) 0.0008(7) O124 0.0154(8) 0.0177(9) 0.0232(9) -0.0094(7) -0.0062(7) 0.0043(7) C123 0.0170(11) 0.0128(11) 0.0126(11) -0.0021(9) -0.0013(9) 0.0007(9) C124 0.0166(11) 0.0138(11) 0.0145(11) -0.0026(9) 0.0007(9) 0.0014(9) C125 0.0171(12) 0.0198(12) 0.0204(13) -0.0079(10) -0.0028(10) 0.0029(10) C126 0.0275(14) 0.0242(14) 0.0277(15) -0.0139(12) -0.0018(12) 0.0039(11) C127 0.0273(14) 0.0264(15) 0.031(2) -0.0135(13) 0.0041(13) 0.0054(12) C128 0.0154(12) 0.0269(14) 0.032(2) -0.0073(12) 0.0007(11) 0.0038(11) C129 0.0162(11) 0.0167(12) 0.0221(13) -0.0061(10) -0.0004(10) 0.0008(9) C200 0.038(2) 0.032(2) 0.052(2) -0.005(2) 0.000(2) -0.0013(15) Cl1 0.0391(5) 0.0440(5) 0.0632(6) -0.0266(5) 0.0032(4) -0.0087(4) Cl2 0.0510(5) 0.0390(5) 0.0470(5) -0.0170(4) -0.0088(4) 0.0021(4) _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 Gd1 O17 2.288(2) 2_655 ? Gd1 O23 2.321(2) . ? Gd1 O24 2.331(2) 2_655 ? Gd1 O16 2.382(2) . ? Gd1 N12 2.498(2) . ? Gd1 N2 2.507(2) . ? Gd1 N7 2.530(2) . ? Gd1 O17 2.872(2) . ? Gd1 C16 3.004(2) . ? Gd1 Gd1 3.9430(4) 2_655 ? B1 N6 1.530(4) . ? B1 N1 1.539(4) . ? B1 N11 1.549(4) . ? N1 C5 1.347(3) . ? N1 N2 1.372(3) . ? N2 C3 1.339(3) . ? C3 C4 1.392(4) . ? C4 C5 1.380(4) . ? N6 C10 1.350(3) . ? N6 N7 1.366(3) . ? N7 C8 1.334(3) . ? C8 C9 1.393(4) . ? C9 C10 1.367(4) . ? N11 C15 1.343(3) . ? N11 N12 1.372(3) . ? N12 C13 1.342(3) . ? C13 C14 1.385(4) . ? C14 C15 1.372(4) . ? O16 C16 1.259(3) . ? O17 C16 1.269(3) . ? O17 Gd1 2.288(2) 2_655 ? C16 C17 1.492(3) . ? C17 C22 1.392(3) . ? C17 C18 1.393(4) . ? C18 C19 1.390(4) . ? C19 C20 1.387(4) . ? C20 C21 1.380(4) . ? C21 C22 1.389(4) . ? O23 C23 1.262(3) . ? O24 C23 1.266(3) . ? O24 Gd1 2.331(2) 2_655 ? C23 C24 1.502(3) . ? C24 C25 1.389(3) . ? C24 C29 1.393(3) . ? C25 C26 1.387(4) . ? C26 C27 1.389(4) . ? C27 C28 1.383(4) . ? C28 C29 1.382(4) . ? Gd2 O117 2.310(2) 2_766 ? Gd2 O123 2.321(2) . ? Gd2 O124 2.329(2) 2_766 ? Gd2 O116 2.351(2) . ? Gd2 N107 2.497(2) . ? Gd2 N102 2.514(2) . ? Gd2 N112 2.518(2) . ? Gd2 O117 2.880(2) . ? Gd2 C116 2.989(2) . ? Gd2 Gd2 3.9860(4) 2_766 ? B101 N106 1.531(4) . ? B101 N111 1.540(4) . ? B101 N101 1.556(4) . ? N101 C105 1.343(3) . ? N101 N102 1.363(3) . ? N102 C103 1.344(3) . ? C103 C104 1.389(4) . ? C104 C105 1.374(4) . ? N106 C110 1.345(3) . ? N106 N107 1.367(3) . ? N107 C108 1.339(3) . ? C108 C109 1.385(4) . ? C109 C110 1.383(4) . ? N111 C115 1.346(3) . ? N111 N112 1.371(3) . ? N112 C113 1.334(3) . ? C113 C114 1.390(4) . ? C114 C115 1.371(4) . ? O116 C116 1.257(3) . ? O117 C116 1.271(3) . ? O117 Gd2 2.310(2) 2_766 ? C116 C117 1.486(3) . ? C117 C122 1.393(4) . ? C117 C118 1.396(3) . ? C118 C119 1.382(4) . ? C119 C120 1.385(4) . ? C120 C121 1.384(4) . ? C121 C122 1.388(4) . ? O123 C123 1.262(3) . ? O124 C123 1.261(3) . ? O124 Gd2 2.329(2) 2_766 ? C123 C124 1.501(3) . ? C124 C125 1.390(4) . ? C124 C129 1.392(3) . ? C125 C126 1.387(4) . ? C126 C127 1.384(4) . ? C127 C128 1.387(4) . ? C128 C129 1.382(4) . ? C200 Cl1 1.743(4) . ? C200 Cl2 1.754(4) . ? 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 O17 Gd1 O23 78.77(6) 2_655 . ? O17 Gd1 O24 78.82(6) 2_655 2_655 ? O23 Gd1 O24 134.54(6) . 2_655 ? O17 Gd1 O16 129.17(6) 2_655 . ? O23 Gd1 O16 85.65(6) . . ? O24 Gd1 O16 78.77(6) 2_655 . ? O17 Gd1 N12 158.58(7) 2_655 . ? O23 Gd1 N12 101.45(6) . . ? O24 Gd1 N12 113.35(6) 2_655 . ? O16 Gd1 N12 71.85(6) . . ? O17 Gd1 N2 92.33(6) 2_655 . ? O23 Gd1 N2 144.92(6) . . ? O24 Gd1 N2 74.81(6) 2_655 . ? O16 Gd1 N2 124.22(6) . . ? N12 Gd1 N2 75.10(7) . . ? O17 Gd1 N7 84.69(7) 2_655 . ? O23 Gd1 N7 73.35(6) . . ? O24 Gd1 N7 142.15(6) 2_655 . ? O16 Gd1 N7 136.00(6) . . ? N12 Gd1 N7 75.03(7) . . ? N2 Gd1 N7 72.07(7) . . ? O17 Gd1 O17 80.96(6) 2_655 . ? O23 Gd1 O17 68.66(5) . . ? O24 Gd1 O17 69.09(5) 2_655 . ? O16 Gd1 O17 48.43(5) . . ? N12 Gd1 O17 119.38(6) . . ? N2 Gd1 O17 143.91(6) . . ? N7 Gd1 O17 141.28(6) . . ? O17 Gd1 C16 105.69(6) 2_655 . ? O23 Gd1 C16 75.99(6) . . ? O24 Gd1 C16 72.81(6) 2_655 . ? O16 Gd1 C16 23.63(6) . . ? N12 Gd1 C16 95.00(7) . . ? N2 Gd1 C16 138.70(7) . . ? N7 Gd1 C16 144.92(7) . . ? O17 Gd1 C16 24.81(5) . . ? O17 Gd1 Gd1 46.00(4) 2_655 2_655 ? O23 Gd1 Gd1 67.79(4) . 2_655 ? O24 Gd1 Gd1 68.14(4) 2_655 2_655 ? O16 Gd1 Gd1 83.29(4) . 2_655 ? N12 Gd1 Gd1 153.82(5) . 2_655 ? N2 Gd1 Gd1 127.74(5) . 2_655 ? N7 Gd1 Gd1 120.97(5) . 2_655 ? O17 Gd1 Gd1 34.96(3) . 2_655 ? C16 Gd1 Gd1 59.72(5) . 2_655 ? N6 B1 N1 109.3(2) . . ? N6 B1 N11 110.2(2) . . ? N1 B1 N11 109.0(2) . . ? C5 N1 N2 109.6(2) . . ? C5 N1 B1 128.6(2) . . ? N2 N1 B1 121.7(2) . . ? C3 N2 N1 106.1(2) . . ? C3 N2 Gd1 130.3(2) . . ? N1 N2 Gd1 123.58(15) . . ? N2 C3 C4 110.8(3) . . ? C5 C4 C3 104.8(2) . . ? N1 C5 C4 108.6(2) . . ? C10 N6 N7 109.6(2) . . ? C10 N6 B1 128.7(2) . . ? N7 N6 B1 121.6(2) . . ? C8 N7 N6 105.7(2) . . ? C8 N7 Gd1 130.9(2) . . ? N6 N7 Gd1 123.1(2) . . ? N7 C8 C9 111.4(2) . . ? C10 C9 C8 104.4(2) . . ? N6 C10 C9 108.9(2) . . ? C15 N11 N12 109.5(2) . . ? C15 N11 B1 128.4(2) . . ? N12 N11 B1 122.1(2) . . ? C13 N12 N11 105.5(2) . . ? C13 N12 Gd1 130.8(2) . . ? N11 N12 Gd1 123.28(15) . . ? N12 C13 C14 111.3(2) . . ? C15 C14 C13 104.5(2) . . ? N11 C15 C14 109.2(2) . . ? C16 O16 Gd1 107.08(15) . . ? C16 O17 Gd1 175.0(2) . 2_655 ? C16 O17 Gd1 83.41(14) . . ? Gd1 O17 Gd1 99.04(6) 2_655 . ? O16 C16 O17 121.1(2) . . ? O16 C16 C17 119.1(2) . . ? O17 C16 C17 119.9(2) . . ? O16 C16 Gd1 49.29(12) . . ? O17 C16 Gd1 71.78(13) . . ? C17 C16 Gd1 168.3(2) . . ? C22 C17 C18 119.6(2) . . ? C22 C17 C16 119.2(2) . . ? C18 C17 C16 121.3(2) . . ? C19 C18 C17 119.6(3) . . ? C20 C19 C18 120.2(3) . . ? C21 C20 C19 120.5(3) . . ? C20 C21 C22 119.4(3) . . ? C21 C22 C17 120.6(3) . . ? C23 O23 Gd1 136.9(2) . . ? C23 O24 Gd1 137.6(2) . 2_655 ? O23 C23 O24 124.6(2) . . ? O23 C23 C24 117.7(2) . . ? O24 C23 C24 117.7(2) . . ? C25 C24 C29 119.6(2) . . ? C25 C24 C23 120.1(2) . . ? C29 C24 C23 120.3(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 119.9(2) . . ? C28 C27 C26 119.7(2) . . ? C29 C28 C27 120.6(2) . . ? C28 C29 C24 119.8(2) . . ? O117 Gd2 O123 78.01(6) 2_766 . ? O117 Gd2 O124 78.16(6) 2_766 2_766 ? O123 Gd2 O124 133.57(6) . 2_766 ? O117 Gd2 O116 128.65(6) 2_766 . ? O123 Gd2 O116 84.30(6) . . ? O124 Gd2 O116 80.41(6) 2_766 . ? O117 Gd2 N107 81.59(6) 2_766 . ? O123 Gd2 N107 76.00(6) . . ? O124 Gd2 N107 137.80(7) 2_766 . ? O116 Gd2 N107 139.46(7) . . ? O117 Gd2 N102 101.03(7) 2_766 . ? O123 Gd2 N102 148.62(6) . . ? O124 Gd2 N102 75.23(6) 2_766 . ? O116 Gd2 N102 117.60(7) . . ? N107 Gd2 N102 72.87(7) . . ? O117 Gd2 N112 155.74(6) 2_766 . ? O123 Gd2 N112 94.19(6) . . ? O124 Gd2 N112 121.61(7) 2_766 . ? O116 Gd2 N112 72.28(6) . . ? N107 Gd2 N112 74.22(7) . . ? N102 Gd2 N112 73.74(7) . . ? O117 Gd2 O117 80.24(6) 2_766 . ? O123 Gd2 O117 67.59(5) . . ? O124 Gd2 O117 69.48(6) 2_766 . ? O116 Gd2 O117 48.52(5) . . ? N107 Gd2 O117 141.88(6) . . ? N102 Gd2 O117 143.66(6) . . ? N112 Gd2 O117 118.30(6) . . ? O117 Gd2 C116 105.14(6) 2_766 . ? O123 Gd2 C116 74.75(6) . . ? O124 Gd2 C116 73.90(6) 2_766 . ? O116 Gd2 C116 23.59(6) . . ? N107 Gd2 C116 147.75(7) . . ? N102 Gd2 C116 133.88(7) . . ? N112 Gd2 C116 94.64(7) . . ? O117 Gd2 C116 24.93(6) . . ? O117 Gd2 Gd2 45.42(4) 2_766 2_766 ? O123 Gd2 Gd2 66.68(4) . 2_766 ? O124 Gd2 Gd2 68.15(4) 2_766 2_766 ? O116 Gd2 Gd2 83.30(4) . 2_766 ? N107 Gd2 Gd2 118.93(5) . 2_766 ? N102 Gd2 Gd2 133.87(5) . 2_766 ? N112 Gd2 Gd2 150.57(5) . 2_766 ? O117 Gd2 Gd2 34.83(3) . 2_766 ? C116 Gd2 Gd2 59.73(5) . 2_766 ? N106 B101 N111 109.6(2) . . ? N106 B101 N101 109.4(2) . . ? N111 B101 N101 108.9(2) . . ? C105 N101 N102 110.1(2) . . ? C105 N101 B101 127.9(2) . . ? N102 N101 B101 121.8(2) . . ? C103 N102 N101 105.7(2) . . ? C103 N102 Gd2 130.1(2) . . ? N101 N102 Gd2 123.9(2) . . ? N102 C103 C104 110.8(2) . . ? C105 C104 C103 104.8(2) . . ? N101 C105 C104 108.6(2) . . ? C110 N106 N107 109.9(2) . . ? C110 N106 B101 129.0(2) . . ? N107 N106 B101 121.1(2) . . ? C108 N107 N106 105.7(2) . . ? C108 N107 Gd2 129.2(2) . . ? N106 N107 Gd2 125.1(2) . . ? N107 C108 C109 111.4(2) . . ? C110 C109 C108 104.5(2) . . ? N106 C110 C109 108.5(2) . . ? C115 N111 N112 109.3(2) . . ? C115 N111 B101 128.8(2) . . ? N112 N111 B101 121.8(2) . . ? C113 N112 N111 106.0(2) . . ? C113 N112 Gd2 130.1(2) . . ? N111 N112 Gd2 123.74(15) . . ? N112 C113 C114 111.1(2) . . ? C115 C114 C113 104.5(2) . . ? N111 C115 C114 109.0(2) . . ? C116 O116 Gd2 107.97(15) . . ? C116 O117 Gd2 176.2(2) . 2_766 ? C116 O117 Gd2 82.31(14) . . ? Gd2 O117 Gd2 99.76(6) 2_766 . ? O116 C116 O117 121.2(2) . . ? O116 C116 C117 118.4(2) . . ? O117 C116 C117 120.4(2) . . ? O116 C116 Gd2 48.44(12) . . ? O117 C116 Gd2 72.76(13) . . ? C117 C116 Gd2 166.8(2) . . ? C122 C117 C118 119.9(2) . . ? C122 C117 C116 120.9(2) . . ? C118 C117 C116 119.2(2) . . ? C119 C118 C117 120.2(2) . . ? C118 C119 C120 119.8(2) . . ? C121 C120 C119 120.2(2) . . ? C120 C121 C122 120.5(3) . . ? C121 C122 C117 119.4(3) . . ? C123 O123 Gd2 138.4(2) . . ? C123 O124 Gd2 137.1(2) . 2_766 ? O124 C123 O123 125.1(2) . . ? O124 C123 C124 117.9(2) . . ? O123 C123 C124 117.0(2) . . ? C125 C124 C129 119.4(2) . . ? C125 C124 C123 121.0(2) . . ? C129 C124 C123 119.6(2) . . ? C126 C125 C124 120.1(2) . . ? C127 C126 C125 120.1(3) . . ? C126 C127 C128 119.8(3) . . ? C129 C128 C127 120.2(2) . . ? C128 C129 C124 120.2(2) . . ? Cl1 C200 Cl2 114.2(2) . . ? _refine_diff_density_max 1.298 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.124 #===END data_2 _database_code_CSD 186522 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C46 H40 B2 N12 O8 Tb2], (C H2 Cl2)' _chemical_formula_analytical ? _chemical_formula_sum 'C47 H42 B2 Cl2 N12 O8 Tb2' _chemical_formula_weight 1313.29 _chemical_melting_point ? _chemical_compound_source ? 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 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5382(9) _cell_length_b 13.0146(9) _cell_length_c 16.3211(12) _cell_angle_alpha 72.710(10) _cell_angle_beta 83.640(10) _cell_angle_gamma 89.570(10) _cell_volume 2526.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6042 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method ? _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 2.947 _exptl_absorpt_correction_type 'Gaussian, Face Indexed' _exptl_absorpt_correction_T_min 0.295 _exptl_absorpt_correction_T_max 0.755 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD-Detector' _diffrn_measurement_method '\w, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27882 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 33.16 _reflns_number_total 16579 _reflns_number_observed 13087 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens Saint 6.01' _computing_cell_refinement 'Siemens Saint 6.01' _computing_data_reduction 'Siemens Saint 6.01' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0288P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16579 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_obs 0.0273 _refine_ls_wR_factor_all 0.0603 _refine_ls_wR_factor_obs 0.0584 _refine_ls_goodness_of_fit_all 0.927 _refine_ls_goodness_of_fit_obs 1.017 _refine_ls_restrained_S_all 0.927 _refine_ls_restrained_S_obs 1.017 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tb1 Tb 0.463515(8) -0.024079(8) -0.107495(7) 0.01145(3) Uani 1 d . . B1 B 0.3677(2) -0.1528(2) -0.2560(2) 0.0189(5) Uani 1 d . . H1 H 0.3413(2) -0.1875(2) -0.2972(2) 0.023 Uiso 1 calc R . N1 N 0.2715(2) -0.1221(2) -0.20195(14) 0.0169(4) Uani 1 d . . N2 N 0.2847(2) -0.0711(2) -0.14130(13) 0.0162(4) Uani 1 d . . C3 C 0.1856(2) -0.0577(2) -0.1065(2) 0.0224(5) Uani 1 d . . H3 H 0.1702(2) -0.0239(2) -0.0624(2) 0.027 Uiso 1 calc R . C4 C 0.1084(2) -0.0998(2) -0.1434(2) 0.0297(6) Uani 1 d . . H4 H 0.0326(2) -0.1010(2) -0.1301(2) 0.036 Uiso 1 calc R . C5 C 0.1662(2) -0.1392(2) -0.2037(2) 0.0237(6) Uani 1 d . . H5 H 0.1366(2) -0.1730(2) -0.2406(2) 0.028 Uiso 1 calc R . N6 N 0.4370(2) -0.2317(2) -0.19580(14) 0.0176(4) Uani 1 d . . N7 N 0.4761(2) -0.2079(2) -0.12841(14) 0.0175(4) Uani 1 d . . C8 C 0.5263(2) -0.2955(2) -0.0865(2) 0.0228(5) Uani 1 d . . H8 H 0.5609(2) -0.3019(2) -0.0364(2) 0.027 Uiso 1 calc R . C9 C 0.5211(2) -0.3764(2) -0.1261(2) 0.0267(6) Uani 1 d . . H9 H 0.5499(2) -0.4463(2) -0.1091(2) 0.032 Uiso 1 calc R . C10 C 0.4647(2) -0.3319(2) -0.1953(2) 0.0227(5) Uani 1 d . . H10 H 0.4479(2) -0.3665(2) -0.2362(2) 0.027 Uiso 1 calc R . N11 N 0.4347(2) -0.0501(2) -0.30699(13) 0.0171(4) Uani 1 d . . N12 N 0.4855(2) 0.0111(2) -0.26658(13) 0.0158(4) Uani 1 d . . C13 C 0.5346(2) 0.0927(2) -0.3298(2) 0.0179(5) Uani 1 d . . H13 H 0.5761(2) 0.1482(2) -0.3206(2) 0.021 Uiso 1 calc R . C14 C 0.5172(2) 0.0857(2) -0.4106(2) 0.0234(5) Uani 1 d . . H14 H 0.5433(2) 0.1332(2) -0.4656(2) 0.028 Uiso 1 calc R . C15 C 0.4532(2) -0.0057(2) -0.3930(2) 0.0217(5) Uani 1 d . . H15 H 0.4265(2) -0.0330(2) -0.4349(2) 0.026 Uiso 1 calc R . O16 O 0.55343(14) 0.14448(13) -0.17050(11) 0.0169(3) Uani 1 d . . O17 O 0.57497(14) 0.11780(14) -0.03375(11) 0.0178(3) Uani 1 d . . C16 C 0.5903(2) 0.1746(2) -0.1124(2) 0.0143(4) Uani 1 d . . C17 C 0.6529(2) 0.2782(2) -0.1368(2) 0.0155(4) Uani 1 d . . C18 C 0.7017(2) 0.3104(2) -0.0754(2) 0.0238(5) Uani 1 d . . H18 H 0.6957(2) 0.2660(2) -0.0171(2) 0.029 Uiso 1 calc R . C19 C 0.7589(2) 0.4076(2) -0.0998(2) 0.0317(7) Uani 1 d . . H19 H 0.7929(2) 0.4296(2) -0.0583(2) 0.038 Uiso 1 calc R . C20 C 0.7668(2) 0.4729(2) -0.1847(2) 0.0310(7) Uani 1 d . . H20 H 0.8052(2) 0.5398(2) -0.2009(2) 0.037 Uiso 1 calc R . C21 C 0.7191(2) 0.4410(2) -0.2460(2) 0.0258(6) Uani 1 d . . H21 H 0.7258(2) 0.4853(2) -0.3044(2) 0.031 Uiso 1 calc R . C22 C 0.6614(2) 0.3441(2) -0.2219(2) 0.0201(5) Uani 1 d . . H22 H 0.6276(2) 0.3225(2) -0.2636(2) 0.024 Uiso 1 calc R . O23 O 0.63103(13) -0.08543(13) -0.07417(11) 0.0151(3) Uani 1 d . . O24 O 0.65461(13) -0.09023(14) 0.06099(11) 0.0166(3) Uani 1 d . . C23 C 0.6779(2) -0.1181(2) -0.0066(2) 0.0141(4) Uani 1 d . . C24 C 0.7668(2) -0.1954(2) -0.0066(2) 0.0140(4) Uani 1 d . . C25 C 0.7937(2) -0.2312(2) -0.0786(2) 0.0180(5) Uani 1 d . . H25 H 0.7564(2) -0.2053(2) -0.1280(2) 0.022 Uiso 1 calc R . C26 C 0.8747(2) -0.3043(2) -0.0783(2) 0.0229(5) Uani 1 d . . H26 H 0.8934(2) -0.3279(2) -0.1277(2) 0.027 Uiso 1 calc R . C27 C 0.9285(2) -0.3430(2) -0.0059(2) 0.0230(5) Uani 1 d . . H27 H 0.9837(2) -0.3936(2) -0.0055(2) 0.028 Uiso 1 calc R . C28 C 0.9018(2) -0.3081(2) 0.0659(2) 0.0204(5) Uani 1 d . . H28 H 0.9383(2) -0.3353(2) 0.1156(2) 0.024 Uiso 1 calc R . C29 C 0.8222(2) -0.2336(2) 0.0654(2) 0.0171(5) Uani 1 d . . H29 H 0.8053(2) -0.2087(2) 0.1143(2) 0.021 Uiso 1 calc R . Tb2 Tb 0.873307(8) 0.486053(8) 0.439716(7) 0.01116(3) Uani 1 d . . B101 B 0.6667(2) 0.5512(2) 0.2930(2) 0.0169(5) Uani 1 d . . H101 H 0.6102(2) 0.5690(2) 0.2526(2) 0.020 Uiso 1 calc R . N101 N 0.7617(2) 0.4976(2) 0.25357(13) 0.0160(4) Uani 1 d . . N102 N 0.8514(2) 0.4676(2) 0.29422(13) 0.0175(4) Uani 1 d . . C103 C 0.9132(2) 0.4200(2) 0.2450(2) 0.0213(5) Uani 1 d . . H103 H 0.9815(2) 0.3913(2) 0.2576(2) 0.026 Uiso 1 calc R . C104 C 0.8645(2) 0.4177(2) 0.1728(2) 0.0239(5) Uani 1 d . . H104 H 0.8913(2) 0.3878(2) 0.1283(2) 0.029 Uiso 1 calc R . C105 C 0.7691(2) 0.4685(2) 0.1805(2) 0.0200(5) Uani 1 d . . H105 H 0.7170(2) 0.4810(2) 0.1409(2) 0.024 Uiso 1 calc R . N106 N 0.7073(2) 0.6545(2) 0.30733(13) 0.0152(4) Uani 1 d . . N107 N 0.7853(2) 0.6519(2) 0.36005(14) 0.0174(4) Uani 1 d . . C108 C 0.8023(2) 0.7537(2) 0.3584(2) 0.0185(5) Uani 1 d . . H108 H 0.8535(2) 0.7759(2) 0.3889(2) 0.022 Uiso 1 calc R . C109 C 0.7354(2) 0.8229(2) 0.3061(2) 0.0214(5) Uani 1 d . . H109 H 0.7313(2) 0.8987(2) 0.2945(2) 0.026 Uiso 1 calc R . C110 C 0.6761(2) 0.7564(2) 0.2748(2) 0.0191(5) Uani 1 d . . H110 H 0.6225(2) 0.7788(2) 0.2369(2) 0.023 Uiso 1 calc R . N111 N 0.6194(2) 0.4729(2) 0.37987(13) 0.0165(4) Uani 1 d . . N112 N 0.6807(2) 0.4331(2) 0.44594(13) 0.0169(4) Uani 1 d . . C113 C 0.6146(2) 0.3696(2) 0.5112(2) 0.0184(5) Uani 1 d . . H113 H 0.6358(2) 0.3308(2) 0.5658(2) 0.022 Uiso 1 calc R . C114 C 0.5112(2) 0.3677(2) 0.4888(2) 0.0225(5) Uani 1 d . . H114 H 0.4498(2) 0.3293(2) 0.5233(2) 0.027 Uiso 1 calc R . C115 C 0.5179(2) 0.4343(2) 0.4050(2) 0.0196(5) Uani 1 d . . H115 H 0.4601(2) 0.4504(2) 0.3705(2) 0.024 Uiso 1 calc R . O116 O 0.83583(13) 0.33487(14) 0.55971(11) 0.0189(4) Uani 1 d . . O117 O 0.98207(13) 0.39711(13) 0.59442(11) 0.0169(3) Uani 1 d . . C116 C 0.9052(2) 0.3283(2) 0.6110(2) 0.0149(4) Uani 1 d . . C117 C 0.8946(2) 0.2393(2) 0.6934(2) 0.0143(4) Uani 1 d . . C118 C 0.8232(2) 0.1530(2) 0.7033(2) 0.0168(5) Uani 1 d . . H118 H 0.7848(2) 0.1505(2) 0.6569(2) 0.020 Uiso 1 calc R . C119 C 0.8088(2) 0.0713(2) 0.7810(2) 0.0196(5) Uani 1 d . . H119 H 0.7602(2) 0.0128(2) 0.7880(2) 0.024 Uiso 1 calc R . C120 C 0.8651(2) 0.0749(2) 0.8483(2) 0.0237(5) Uani 1 d . . H120 H 0.8548(2) 0.0189(2) 0.9015(2) 0.028 Uiso 1 calc R . C121 C 0.9363(2) 0.1595(2) 0.8388(2) 0.0286(6) Uani 1 d . . H121 H 0.9748(2) 0.1613(2) 0.8853(2) 0.034 Uiso 1 calc R . C122 C 0.9515(2) 0.2416(2) 0.7613(2) 0.0224(5) Uani 1 d . . H122 H 1.0007(2) 0.2994(2) 0.7547(2) 0.027 Uiso 1 calc R . O123 O 0.83936(13) 0.57874(13) 0.53985(11) 0.0156(3) Uani 1 d . . O124 O 0.98864(13) 0.62326(14) 0.58602(12) 0.0174(3) Uani 1 d . . C123 C 0.8905(2) 0.6327(2) 0.5757(2) 0.0135(4) Uani 1 d . . C124 C 0.8288(2) 0.7135(2) 0.6099(2) 0.0143(4) Uani 1 d . . C125 C 0.8790(2) 0.7771(2) 0.6504(2) 0.0189(5) Uani 1 d . . H125 H 0.9539(2) 0.7720(2) 0.6548(2) 0.023 Uiso 1 calc R . C126 C 0.8192(2) 0.8478(2) 0.6843(2) 0.0236(5) Uani 1 d . . H126 H 0.8533(2) 0.8908(2) 0.7124(2) 0.028 Uiso 1 calc R . C127 C 0.7100(2) 0.8565(2) 0.6777(2) 0.0261(6) Uani 1 d . . H127 H 0.6693(2) 0.9042(2) 0.7021(2) 0.031 Uiso 1 calc R . C128 C 0.6603(2) 0.7954(2) 0.6355(2) 0.0245(6) Uani 1 d . . H128 H 0.5858(2) 0.8023(2) 0.6300(2) 0.029 Uiso 1 calc R . C129 C 0.7198(2) 0.7242(2) 0.6014(2) 0.0183(5) Uani 1 d . . H129 H 0.6859(2) 0.6826(2) 0.5722(2) 0.022 Uiso 1 calc R . C200 C 0.8317(3) 0.9959(3) 0.4527(2) 0.0402(8) Uani 1 d . . H20A H 0.8243(3) 0.9468(3) 0.5125(2) 0.048 Uiso 1 calc R . H20B H 0.7717(3) 0.9789(3) 0.4238(2) 0.048 Uiso 1 calc R . Cl1 Cl 0.95293(7) 0.97126(7) 0.39853(6) 0.0439(2) Uani 1 d . . Cl2 Cl 0.82060(7) 1.12886(7) 0.45638(6) 0.0428(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01329(5) 0.01079(5) 0.01083(5) -0.00371(4) -0.00244(4) 0.00132(4) B1 0.0195(12) 0.0193(14) 0.0224(14) -0.0121(12) -0.0054(11) 0.0018(10) N1 0.0171(9) 0.0165(10) 0.0202(10) -0.0089(9) -0.0053(8) 0.0016(7) N2 0.0154(9) 0.0190(10) 0.0166(10) -0.0085(8) -0.0027(8) 0.0018(7) C3 0.0169(11) 0.0234(13) 0.0281(14) -0.0118(11) 0.0034(11) 0.0012(9) C4 0.0158(11) 0.033(2) 0.047(2) -0.0223(14) -0.0032(12) 0.0018(10) C5 0.0184(11) 0.0236(13) 0.034(2) -0.0153(12) -0.0076(11) 0.0004(10) N6 0.0169(9) 0.0162(10) 0.0225(11) -0.0099(9) -0.0019(8) 0.0000(7) N7 0.0188(9) 0.0148(10) 0.0217(10) -0.0084(9) -0.0066(9) 0.0027(7) C8 0.0203(11) 0.0155(12) 0.0333(15) -0.0067(11) -0.0078(11) 0.0015(9) C9 0.0242(13) 0.0141(12) 0.045(2) -0.0121(12) -0.0078(13) 0.0055(10) C10 0.0210(12) 0.0174(12) 0.0334(15) -0.0142(11) 0.0001(11) -0.0001(9) N11 0.0200(10) 0.0195(10) 0.0158(10) -0.0107(9) -0.0035(8) 0.0032(8) N12 0.0176(9) 0.0170(10) 0.0155(9) -0.0086(8) -0.0027(8) 0.0008(7) C13 0.0221(11) 0.0169(12) 0.0149(11) -0.0059(10) 0.0003(10) 0.0033(9) C14 0.0325(14) 0.0229(14) 0.0139(11) -0.0060(10) 0.0028(11) 0.0014(11) C15 0.0288(13) 0.0249(14) 0.0145(11) -0.0104(10) -0.0036(11) 0.0061(10) O16 0.0203(8) 0.0159(8) 0.0151(8) -0.0051(7) -0.0035(7) -0.0015(6) O17 0.0197(8) 0.0168(9) 0.0151(8) -0.0023(7) -0.0007(7) 0.0012(7) C16 0.0152(10) 0.0137(11) 0.0134(10) -0.0033(9) -0.0014(9) 0.0025(8) C17 0.0160(10) 0.0133(11) 0.0174(11) -0.0055(9) -0.0005(9) 0.0001(8) C18 0.0258(13) 0.0243(14) 0.0219(13) -0.0073(11) -0.0041(11) -0.0030(10) C19 0.0316(15) 0.029(2) 0.039(2) -0.0162(14) -0.0048(13) -0.0113(12) C20 0.0289(14) 0.0182(14) 0.044(2) -0.0081(13) 0.0028(13) -0.0083(11) C21 0.0268(13) 0.0176(13) 0.0271(14) -0.0001(11) 0.0042(12) -0.0025(10) C22 0.0232(12) 0.0165(12) 0.0202(12) -0.0058(10) -0.0004(10) -0.0017(9) O23 0.0152(7) 0.0160(8) 0.0147(8) -0.0050(7) -0.0036(7) 0.0020(6) O24 0.0177(8) 0.0180(9) 0.0162(8) -0.0083(7) -0.0018(7) 0.0038(6) C23 0.0136(10) 0.0117(10) 0.0165(11) -0.0048(9) 0.0014(9) -0.0013(8) C24 0.0143(10) 0.0124(11) 0.0154(11) -0.0048(9) 0.0002(9) 0.0001(8) C25 0.0186(11) 0.0191(12) 0.0175(11) -0.0071(10) -0.0024(10) 0.0008(9) C26 0.0242(12) 0.0256(14) 0.0224(13) -0.0137(11) 0.0000(11) 0.0051(10) C27 0.0223(12) 0.0198(13) 0.0269(14) -0.0077(11) -0.0007(11) 0.0055(10) C28 0.0203(11) 0.0185(12) 0.0221(12) -0.0048(10) -0.0053(10) 0.0046(9) C29 0.0166(10) 0.0169(12) 0.0183(11) -0.0061(10) -0.0013(10) 0.0020(9) Tb2 0.00971(5) 0.00994(5) 0.01488(5) -0.00466(4) -0.00329(4) 0.00117(4) B101 0.0150(11) 0.0203(14) 0.0164(13) -0.0055(11) -0.0057(10) 0.0030(10) N101 0.0148(9) 0.0181(10) 0.0161(9) -0.0061(8) -0.0030(8) 0.0009(7) N102 0.0146(9) 0.0227(11) 0.0166(10) -0.0075(9) -0.0032(8) 0.0043(8) C103 0.0219(12) 0.0207(13) 0.0223(13) -0.0082(11) -0.0016(11) 0.0055(10) C104 0.0315(14) 0.0213(13) 0.0202(13) -0.0095(11) 0.0003(11) 0.0032(11) C105 0.0246(12) 0.0220(13) 0.0152(11) -0.0075(10) -0.0038(10) -0.0023(10) N106 0.0138(9) 0.0171(10) 0.0152(9) -0.0047(8) -0.0042(8) 0.0039(7) N107 0.0166(9) 0.0151(10) 0.0215(10) -0.0059(8) -0.0065(8) 0.0031(7) C108 0.0217(11) 0.0141(11) 0.0213(12) -0.0069(10) -0.0045(10) 0.0019(9) C109 0.0301(13) 0.0130(12) 0.0213(12) -0.0045(10) -0.0055(11) 0.0076(10) C110 0.0210(11) 0.0177(12) 0.0177(11) -0.0033(10) -0.0037(10) 0.0081(9) N111 0.0127(8) 0.0190(10) 0.0189(10) -0.0061(8) -0.0059(8) 0.0014(7) N112 0.0129(9) 0.0211(11) 0.0166(10) -0.0049(8) -0.0043(8) 0.0002(8) C113 0.0154(10) 0.0203(12) 0.0187(12) -0.0040(10) -0.0027(10) -0.0001(9) C114 0.0140(10) 0.0250(14) 0.0266(14) -0.0053(11) -0.0005(10) -0.0018(9) C115 0.0122(10) 0.0231(13) 0.0254(13) -0.0094(11) -0.0044(10) 0.0005(9) O116 0.0159(8) 0.0182(9) 0.0212(9) -0.0022(7) -0.0063(7) -0.0007(6) O117 0.0144(7) 0.0117(8) 0.0229(9) -0.0034(7) 0.0000(7) -0.0013(6) C116 0.0122(9) 0.0108(10) 0.0214(12) -0.0053(9) 0.0000(9) 0.0012(8) C117 0.0123(9) 0.0133(11) 0.0168(11) -0.0041(9) -0.0007(9) 0.0011(8) C118 0.0165(10) 0.0144(11) 0.0202(12) -0.0064(10) -0.0015(10) 0.0002(8) C119 0.0226(12) 0.0130(11) 0.0214(12) -0.0047(10) 0.0042(10) -0.0028(9) C120 0.0274(13) 0.0192(13) 0.0186(12) 0.0020(10) 0.0009(11) -0.0021(10) C121 0.0314(14) 0.031(2) 0.0210(13) -0.0021(12) -0.0090(12) -0.0084(12) C122 0.0215(12) 0.0232(13) 0.0219(13) -0.0045(11) -0.0055(11) -0.0062(10) O123 0.0139(7) 0.0176(8) 0.0176(8) -0.0086(7) -0.0029(7) 0.0022(6) O124 0.0138(7) 0.0175(9) 0.0253(9) -0.0119(7) -0.0053(7) 0.0046(6) C123 0.0142(10) 0.0105(10) 0.0147(10) -0.0025(9) -0.0013(9) 0.0017(8) C124 0.0144(10) 0.0122(11) 0.0162(11) -0.0047(9) 0.0000(9) 0.0028(8) C125 0.0184(11) 0.0171(12) 0.0236(13) -0.0095(10) -0.0036(10) 0.0035(9) C126 0.0265(13) 0.0219(13) 0.0273(14) -0.0151(11) -0.0019(11) 0.0012(10) C127 0.0255(13) 0.0248(14) 0.0299(15) -0.0140(12) 0.0049(12) 0.0071(11) C128 0.0156(11) 0.0229(13) 0.035(2) -0.0096(12) 0.0004(11) 0.0045(9) C129 0.0152(10) 0.0165(12) 0.0234(12) -0.0066(10) -0.0008(10) 0.0011(9) C200 0.036(2) 0.031(2) 0.049(2) -0.006(2) 0.000(2) -0.0033(13) Cl1 0.0355(4) 0.0413(5) 0.0608(6) -0.0260(4) -0.0002(4) -0.0062(3) Cl2 0.0486(5) 0.0373(4) 0.0465(5) -0.0173(4) -0.0094(4) 0.0043(4) _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 O17 2.264(2) 2_655 ? Tb1 O23 2.305(2) . ? Tb1 O24 2.318(2) 2_655 ? Tb1 O16 2.362(2) . ? Tb1 N12 2.483(2) . ? Tb1 N2 2.491(2) . ? Tb1 N7 2.517(2) . ? Tb1 C16 3.021(2) . ? Tb1 Tb1 3.9458(4) 2_655 ? B1 N6 1.534(4) . ? B1 N1 1.535(3) . ? B1 N11 1.545(4) . ? N1 C5 1.344(3) . ? N1 N2 1.370(3) . ? N2 C3 1.340(3) . ? C3 C4 1.391(4) . ? C4 C5 1.376(4) . ? N6 C10 1.345(3) . ? N6 N7 1.367(3) . ? N7 C8 1.336(3) . ? C8 C9 1.394(4) . ? C9 C10 1.376(4) . ? N11 C15 1.343(3) . ? N11 N12 1.374(3) . ? N12 C13 1.337(3) . ? C13 C14 1.390(4) . ? C14 C15 1.379(4) . ? O16 C16 1.260(3) . ? O17 C16 1.271(3) . ? O17 Tb1 2.264(2) 2_655 ? C16 C17 1.490(3) . ? C17 C22 1.391(4) . ? C17 C18 1.394(3) . ? C18 C19 1.388(4) . ? C19 C20 1.386(4) . ? C20 C21 1.383(4) . ? C21 C22 1.388(4) . ? O23 C23 1.266(3) . ? O24 C23 1.264(3) . ? O24 Tb1 2.318(2) 2_655 ? C23 C24 1.496(3) . ? C24 C29 1.392(3) . ? C24 C25 1.396(3) . ? C25 C26 1.386(4) . ? C26 C27 1.387(4) . ? C27 C28 1.385(4) . ? C28 C29 1.386(3) . ? Tb2 O117 2.286(2) 2_766 ? Tb2 O123 2.306(2) . ? Tb2 O124 2.314(2) 2_766 ? Tb2 O116 2.334(2) . ? Tb2 N107 2.486(2) . ? Tb2 N112 2.499(2) . ? Tb2 N102 2.501(2) . ? Tb2 C116 3.002(2) . ? Tb2 Tb2 3.9906(4) 2_766 ? B101 N106 1.532(3) . ? B101 N111 1.538(4) . ? B101 N101 1.551(3) . ? N101 C105 1.348(3) . ? N101 N102 1.364(3) . ? N102 C103 1.335(3) . ? C103 C104 1.394(4) . ? C104 C105 1.374(4) . ? N106 C110 1.346(3) . ? N106 N107 1.366(3) . ? N107 C108 1.335(3) . ? C108 C109 1.390(3) . ? C109 C110 1.386(4) . ? N111 C115 1.346(3) . ? N111 N112 1.367(3) . ? N112 C113 1.340(3) . ? C113 C114 1.389(3) . ? C114 C115 1.378(4) . ? O116 C116 1.258(3) . ? O117 C116 1.271(3) . ? O117 Tb2 2.286(2) 2_766 ? C116 C117 1.485(3) . ? C117 C122 1.391(3) . ? C117 C118 1.401(3) . ? C118 C119 1.387(4) . ? C119 C120 1.382(4) . ? C120 C121 1.384(4) . ? C121 C122 1.387(4) . ? O123 C123 1.257(3) . ? O124 C123 1.261(3) . ? O124 Tb2 2.314(2) 2_766 ? C123 C124 1.501(3) . ? C124 C129 1.391(3) . ? C124 C125 1.395(3) . ? C125 C126 1.384(3) . ? C126 C127 1.386(4) . ? C127 C128 1.386(4) . ? C128 C129 1.389(3) . ? C200 Cl1 1.749(3) . ? C200 Cl2 1.753(3) . ? 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 O17 Tb1 O23 79.39(6) 2_655 . ? O17 Tb1 O24 79.20(6) 2_655 2_655 ? O23 Tb1 O24 133.91(6) . 2_655 ? O17 Tb1 O16 129.33(6) 2_655 . ? O23 Tb1 O16 84.60(6) . . ? O24 Tb1 O16 78.35(6) 2_655 . ? O17 Tb1 N12 158.16(6) 2_655 . ? O23 Tb1 N12 100.98(6) . . ? O24 Tb1 N12 113.51(6) 2_655 . ? O16 Tb1 N12 72.06(6) . . ? O17 Tb1 N2 91.86(7) 2_655 . ? O23 Tb1 N2 145.80(6) . . ? O24 Tb1 N2 75.01(6) 2_655 . ? O16 Tb1 N2 124.49(6) . . ? N12 Tb1 N2 75.49(7) . . ? O17 Tb1 N7 83.90(7) 2_655 . ? O23 Tb1 N7 73.58(6) . . ? O24 Tb1 N7 142.77(6) 2_655 . ? O16 Tb1 N7 136.19(6) . . ? N12 Tb1 N7 75.42(7) . . ? N2 Tb1 N7 72.64(7) . . ? O17 Tb1 C16 106.30(6) 2_655 . ? O23 Tb1 C16 75.22(6) . . ? O24 Tb1 C16 72.43(6) 2_655 . ? O16 Tb1 C16 23.17(6) . . ? N12 Tb1 C16 94.76(6) . . ? N2 Tb1 C16 138.56(6) . . ? N7 Tb1 C16 144.63(6) . . ? O17 Tb1 Tb1 47.15(4) 2_655 2_655 ? O23 Tb1 Tb1 67.54(4) . 2_655 ? O24 Tb1 Tb1 67.92(4) 2_655 2_655 ? O16 Tb1 Tb1 82.30(4) . 2_655 ? N12 Tb1 Tb1 153.00(5) . 2_655 ? N2 Tb1 Tb1 128.03(5) . 2_655 ? N7 Tb1 Tb1 120.91(5) . 2_655 ? C16 Tb1 Tb1 59.18(5) . 2_655 ? N6 B1 N1 109.3(2) . . ? N6 B1 N11 109.8(2) . . ? N1 B1 N11 109.2(2) . . ? C5 N1 N2 109.6(2) . . ? C5 N1 B1 128.7(2) . . ? N2 N1 B1 121.8(2) . . ? C3 N2 N1 106.0(2) . . ? C3 N2 Tb1 130.5(2) . . ? N1 N2 Tb1 123.45(14) . . ? N2 C3 C4 110.9(2) . . ? C5 C4 C3 104.6(2) . . ? N1 C5 C4 108.9(2) . . ? C10 N6 N7 109.4(2) . . ? C10 N6 B1 128.9(2) . . ? N7 N6 B1 121.6(2) . . ? C8 N7 N6 106.2(2) . . ? C8 N7 Tb1 130.8(2) . . ? N6 N7 Tb1 122.73(15) . . ? N7 C8 C9 111.0(2) . . ? C10 C9 C8 104.3(2) . . ? N6 C10 C9 109.1(2) . . ? C15 N11 N12 109.5(2) . . ? C15 N11 B1 128.4(2) . . ? N12 N11 B1 122.2(2) . . ? C13 N12 N11 105.8(2) . . ? C13 N12 Tb1 130.9(2) . . ? N11 N12 Tb1 122.96(15) . . ? N12 C13 C14 111.3(2) . . ? C15 C14 C13 104.3(2) . . ? N11 C15 C14 109.1(2) . . ? C16 O16 Tb1 109.26(15) . . ? C16 O17 Tb1 175.7(2) . 2_655 ? O16 C16 O17 120.9(2) . . ? O16 C16 C17 119.2(2) . . ? O17 C16 C17 119.9(2) . . ? O16 C16 Tb1 47.57(11) . . ? O17 C16 Tb1 73.35(13) . . ? C17 C16 Tb1 166.8(2) . . ? C22 C17 C18 119.8(2) . . ? C22 C17 C16 119.3(2) . . ? C18 C17 C16 120.9(2) . . ? C19 C18 C17 119.6(3) . . ? C20 C19 C18 120.2(3) . . ? C21 C20 C19 120.4(3) . . ? C20 C21 C22 119.6(3) . . ? C21 C22 C17 120.3(2) . . ? C23 O23 Tb1 136.71(15) . . ? C23 O24 Tb1 137.7(2) . 2_655 ? O24 C23 O23 124.6(2) . . ? O24 C23 C24 117.7(2) . . ? O23 C23 C24 117.7(2) . . ? C29 C24 C25 119.4(2) . . ? C29 C24 C23 120.6(2) . . ? C25 C24 C23 120.0(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 119.9(2) . . ? C28 C27 C26 120.1(2) . . ? C27 C28 C29 120.3(2) . . ? C28 C29 C24 120.1(2) . . ? O117 Tb2 O123 78.43(6) 2_766 . ? O117 Tb2 O124 78.39(6) 2_766 2_766 ? O123 Tb2 O124 132.83(6) . 2_766 ? O117 Tb2 O116 128.68(6) 2_766 . ? O123 Tb2 O116 83.62(6) . . ? O124 Tb2 O116 79.78(6) 2_766 . ? O117 Tb2 N107 81.04(6) 2_766 . ? O123 Tb2 N107 76.12(6) . . ? O124 Tb2 N107 138.56(7) 2_766 . ? O116 Tb2 N107 139.65(6) . . ? O117 Tb2 N112 155.33(6) 2_766 . ? O123 Tb2 N112 93.96(6) . . ? O124 Tb2 N112 121.83(6) 2_766 . ? O116 Tb2 N112 72.66(6) . . ? N107 Tb2 N112 74.34(7) . . ? O117 Tb2 N102 100.49(7) 2_766 . ? O123 Tb2 N102 149.32(6) . . ? O124 Tb2 N102 75.45(6) 2_766 . ? O116 Tb2 N102 117.90(7) . . ? N107 Tb2 N102 73.46(7) . . ? N112 Tb2 N102 74.17(7) . . ? O117 Tb2 C116 105.53(6) 2_766 . ? O123 Tb2 C116 74.28(6) . . ? O124 Tb2 C116 73.26(6) 2_766 . ? O116 Tb2 C116 23.22(6) . . ? N107 Tb2 C116 147.54(7) . . ? N112 Tb2 C116 94.66(6) . . ? N102 Tb2 C116 133.74(7) . . ? O117 Tb2 Tb2 46.43(4) 2_766 2_766 ? O123 Tb2 Tb2 66.33(4) . 2_766 ? O124 Tb2 Tb2 67.86(4) 2_766 2_766 ? O116 Tb2 Tb2 82.32(4) . 2_766 ? N107 Tb2 Tb2 118.98(5) . 2_766 ? N112 Tb2 Tb2 149.90(5) . 2_766 ? N102 Tb2 Tb2 133.99(5) . 2_766 ? C116 Tb2 Tb2 59.12(4) . 2_766 ? N106 B101 N111 109.6(2) . . ? N106 B101 N101 109.3(2) . . ? N111 B101 N101 109.2(2) . . ? C105 N101 N102 109.7(2) . . ? C105 N101 B101 128.2(2) . . ? N102 N101 B101 122.0(2) . . ? C103 N102 N101 106.0(2) . . ? C103 N102 Tb2 130.2(2) . . ? N101 N102 Tb2 123.45(15) . . ? N102 C103 C104 111.1(2) . . ? C105 C104 C103 104.4(2) . . ? N101 C105 C104 108.8(2) . . ? C110 N106 N107 109.9(2) . . ? C110 N106 B101 129.1(2) . . ? N107 N106 B101 121.0(2) . . ? C108 N107 N106 106.1(2) . . ? C108 N107 Tb2 129.2(2) . . ? N106 N107 Tb2 124.75(14) . . ? N107 C108 C109 111.2(2) . . ? C110 C109 C108 104.4(2) . . ? N106 C110 C109 108.4(2) . . ? C115 N111 N112 109.5(2) . . ? C115 N111 B101 128.8(2) . . ? N112 N111 B101 121.6(2) . . ? C113 N112 N111 105.9(2) . . ? C113 N112 Tb2 130.2(2) . . ? N111 N112 Tb2 123.83(15) . . ? N112 C113 C114 111.3(2) . . ? C115 C114 C113 104.2(2) . . ? N111 C115 C114 109.0(2) . . ? C116 O116 Tb2 109.75(14) . . ? C116 O117 Tb2 176.3(2) . 2_766 ? O116 C116 O117 121.4(2) . . ? O116 C116 C117 118.7(2) . . ? O117 C116 C117 119.9(2) . . ? O116 C116 Tb2 47.03(12) . . ? O117 C116 Tb2 74.41(13) . . ? C117 C116 Tb2 165.6(2) . . ? C122 C117 C118 119.7(2) . . ? C122 C117 C116 121.4(2) . . ? C118 C117 C116 118.9(2) . . ? C119 C118 C117 119.8(2) . . ? C120 C119 C118 120.0(2) . . ? C119 C120 C121 120.5(2) . . ? C120 C121 C122 120.0(3) . . ? C121 C122 C117 120.0(2) . . ? C123 O123 Tb2 138.59(15) . . ? C123 O124 Tb2 137.15(15) . 2_766 ? O123 C123 O124 125.1(2) . . ? O123 C123 C124 117.1(2) . . ? O124 C123 C124 117.8(2) . . ? C129 C124 C125 119.6(2) . . ? C129 C124 C123 119.3(2) . . ? C125 C124 C123 121.1(2) . . ? C126 C125 C124 119.8(2) . . ? C125 C126 C127 120.5(2) . . ? C126 C127 C128 120.0(2) . . ? C127 C128 C129 119.8(2) . . ? C128 C129 C124 120.3(2) . . ? Cl1 C200 Cl2 113.8(2) . . ? _refine_diff_density_max 1.547 _refine_diff_density_min -1.586 _refine_diff_density_rms 0.123 #===END data_3 _database_code_CSD 186523 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C46 H36 B2 Cl4 Gd2 N12 O8], 4 CH2Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C50 H44 B2 Cl12 Gd2 N12 O8' _chemical_formula_weight 1702.49 _chemical_melting_point ? _chemical_compound_source ? 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' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3945(5) _cell_length_b 12.6965(8) _cell_length_c 14.2564(9) _cell_angle_alpha 74.750(10) _cell_angle_beta 76.040(10) _cell_angle_gamma 83.290(10) _cell_volume 1589.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12159 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method ? _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 2.633 _exptl_absorpt_correction_type 'Gaussian, Face Indexed' _exptl_absorpt_correction_T_min 0.4038 _exptl_absorpt_correction_T_max 0.6785 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\w, 422 frames a 1 deg./170 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17689 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 33.18 _reflns_number_total 12046 _reflns_number_observed 11339 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Nonius Collect' _computing_data_reduction 'Nonius Collect' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+3.5196P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12035 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_obs 0.0404 _refine_ls_wR_factor_all 0.1104 _refine_ls_wR_factor_obs 0.1067 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.076 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Gd1 Gd 0.610932(12) 1.951579(9) 0.605171(8) 0.01278(4) Uani 1 d . . Cl1 Cl 1.12817(9) 1.81916(7) 0.03628(6) 0.02823(15) Uani 1 d . . Cl2 Cl 0.22700(14) 1.33952(8) 0.61460(11) 0.0518(3) Uani 1 d . . B1 B 0.6745(3) 1.9014(2) 0.8565(2) 0.0178(5) Uani 1 d . . H1 H 0.6936(3) 1.8874(2) 0.9248(2) 0.021 Uiso 1 calc R . N1 N 0.6126(3) 2.0193(2) 0.8249(2) 0.0175(4) Uani 1 d . . N2 N 0.5877(3) 2.0611(2) 0.7321(2) 0.0185(4) Uani 1 d . . N6 N 0.8180(3) 1.8814(2) 0.7826(2) 0.0173(4) Uani 1 d . . N7 N 0.8244(3) 1.8935(2) 0.6843(2) 0.0170(4) Uani 1 d . . N11 N 0.5605(3) 1.8225(2) 0.8566(2) 0.0179(4) Uani 1 d . . N12 N 0.5128(3) 1.8261(2) 0.7731(2) 0.0177(4) Uani 1 d . . C3 C 0.5332(3) 2.1637(2) 0.7294(2) 0.0207(5) Uani 1 d . . H3 H 0.5060(3) 2.2130(2) 0.6729(2) 0.025 Uiso 1 calc R . C4 C 0.5219(4) 2.1885(3) 0.8203(2) 0.0238(5) Uani 1 d . . H4 H 0.4862(4) 2.2554(3) 0.8380(2) 0.029 Uiso 1 calc R . C5 C 0.5739(3) 2.0946(2) 0.8788(2) 0.0207(5) Uani 1 d . . H5 H 0.5812(3) 2.0847(2) 0.9459(2) 0.025 Uiso 1 calc R . C8 C 0.9636(3) 1.8674(2) 0.6440(2) 0.0203(5) Uani 1 d . . H8 H 1.0003(3) 1.8688(2) 0.5755(2) 0.024 Uiso 1 calc R . C9 C 1.0474(3) 1.8379(3) 0.7159(2) 0.0228(5) Uani 1 d . . H9 H 1.1490(3) 1.8160(3) 0.7069(2) 0.027 Uiso 1 calc R . C10 C 0.9505(3) 1.8476(2) 0.8032(2) 0.0210(5) Uani 1 d . . H10 H 0.9734(3) 1.8329(2) 0.8669(2) 0.025 Uiso 1 calc R . C13 C 0.4179(3) 1.7469(2) 0.7988(2) 0.0206(5) Uani 1 d . . H13 H 0.3671(3) 1.7305(2) 0.7547(2) 0.025 Uiso 1 calc R . C14 C 0.4037(4) 1.6922(3) 0.8983(2) 0.0247(5) Uani 1 d . . H14 H 0.3441(4) 1.6329(3) 0.9347(2) 0.030 Uiso 1 calc R . C15 C 0.4955(4) 1.7432(3) 0.9321(2) 0.0233(5) Uani 1 d . . H15 H 0.5105(4) 1.7251(3) 0.9982(2) 0.028 Uiso 1 calc R . O17 O 0.6258(2) 1.9804(2) 0.4010(2) 0.0174(3) Uani 1 d . . O16 O 0.8062(2) 1.9146(2) 0.4774(2) 0.0202(4) Uani 1 d . . C16 C 0.7556(3) 1.9389(2) 0.4001(2) 0.0159(4) Uani 1 d . . C17 C 0.8491(3) 1.9154(2) 0.3073(2) 0.0147(4) Uani 1 d . . C18 C 0.9879(3) 1.8642(2) 0.3099(2) 0.0181(4) Uani 1 d . . H18 H 1.0233(3) 1.8493(2) 0.3694(2) 0.022 Uiso 1 calc R . C19 C 1.0746(3) 1.8347(2) 0.2264(2) 0.0206(5) Uani 1 d . . H19 H 1.1692(3) 1.7993(2) 0.2279(2) 0.025 Uiso 1 calc R . C20 C 1.0206(3) 1.8580(2) 0.1404(2) 0.0204(5) Uani 1 d . . C21 C 0.8840(3) 1.9111(3) 0.1356(2) 0.0213(5) Uani 1 d . . H21 H 0.8498(3) 1.9272(3) 0.0756(2) 0.026 Uiso 1 calc R . C22 C 0.7984(3) 1.9402(2) 0.2194(2) 0.0186(4) Uani 1 d . . H22 H 0.7049(3) 1.9772(2) 0.2171(2) 0.022 Uiso 1 calc R . O23 O 0.5124(2) 1.8080(2) 0.5748(2) 0.0190(4) Uani 1 d . . O24 O 0.3465(2) 1.8695(2) 0.4815(2) 0.0192(4) Uani 1 d . . C23 C 0.4122(3) 1.7946(2) 0.5348(2) 0.0170(4) Uani 1 d . . C24 C 0.3680(3) 1.6808(2) 0.5526(2) 0.0203(5) Uani 1 d . . C25 C 0.4422(4) 1.5937(2) 0.6065(2) 0.0255(6) Uani 1 d . . H25 H 0.5226(4) 1.6068(2) 0.6308(2) 0.031 Uiso 1 calc R . C26 C 0.3997(5) 1.4878(3) 0.6252(3) 0.0328(7) Uani 1 d . . H26 H 0.4500(5) 1.4280(3) 0.6621(3) 0.039 Uiso 1 calc R . C27 C 0.2821(4) 1.4713(3) 0.5888(3) 0.0349(8) Uani 1 d . . C28 C 0.2092(4) 1.5559(3) 0.5339(4) 0.0378(8) Uani 1 d . . H28 H 0.1304(4) 1.5423(3) 0.5085(4) 0.045 Uiso 1 calc R . C29 C 0.2520(4) 1.6618(3) 0.5159(3) 0.0287(6) Uani 1 d . . H29 H 0.2018(4) 1.7212(3) 0.4785(3) 0.034 Uiso 1 calc R . C30 C 0.9015(9) 1.5754(5) 1.1208(7) 0.075(2) Uani 1 d . . H30A H 1.0035(9) 1.5919(5) 1.0847(7) 0.090 Uiso 1 calc R . H30B H 0.8778(9) 1.6092(5) 1.1783(7) 0.090 Uiso 1 calc R . Cl31 Cl 0.7837(3) 1.6330(2) 1.0424(2) 0.1080(9) Uani 1 d . . Cl32 Cl 0.8911(2) 1.43620(12) 1.1642(2) 0.0682(4) Uani 1 d . . C40 C 1.2366(7) 1.4021(5) 0.2353(5) 0.0566(13) Uani 1 d . . H40A H 1.3304(7) 1.3593(5) 0.2193(5) 0.068 Uiso 1 calc R . H40B H 1.1631(7) 1.3758(5) 0.2087(5) 0.068 Uiso 1 calc R . Cl41 Cl 1.2613(4) 1.5386(2) 0.1772(2) 0.1078(8) Uani 1 d . . Cl42 Cl 1.1777(2) 1.3788(2) 0.3650(2) 0.0853(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01385(6) 0.01310(6) 0.01188(6) -0.00325(4) -0.00339(4) -0.00101(4) Cl1 0.0273(3) 0.0364(4) 0.0202(3) -0.0130(3) 0.0022(2) -0.0002(3) Cl2 0.0525(6) 0.0194(4) 0.0811(8) -0.0119(4) -0.0038(6) -0.0161(4) B1 0.0212(12) 0.0184(12) 0.0150(11) -0.0044(9) -0.0060(10) -0.0016(10) N1 0.0205(10) 0.0195(10) 0.0135(9) -0.0054(7) -0.0032(7) -0.0031(8) N2 0.0232(10) 0.0185(10) 0.0156(9) -0.0056(8) -0.0065(8) -0.0002(8) N6 0.0178(9) 0.0183(9) 0.0163(9) -0.0045(7) -0.0047(8) -0.0006(7) N7 0.0168(9) 0.0204(10) 0.0148(9) -0.0044(7) -0.0056(7) -0.0005(7) N11 0.0209(10) 0.0193(10) 0.0134(9) -0.0029(7) -0.0033(8) -0.0038(8) N12 0.0177(9) 0.0205(10) 0.0149(9) -0.0020(7) -0.0052(7) -0.0036(8) C3 0.0243(12) 0.0195(11) 0.0195(11) -0.0072(9) -0.0055(10) 0.0010(9) C4 0.0277(13) 0.0235(12) 0.0223(12) -0.0118(10) -0.0033(10) 0.0010(10) C5 0.0232(12) 0.0235(12) 0.0173(11) -0.0088(9) -0.0031(9) -0.0030(9) C8 0.0172(11) 0.0225(12) 0.0213(12) -0.0054(9) -0.0046(9) -0.0009(9) C9 0.0171(11) 0.0252(13) 0.0267(13) -0.0050(10) -0.0088(10) 0.0017(9) C10 0.0215(12) 0.0222(12) 0.0209(12) -0.0023(9) -0.0109(10) -0.0016(9) C13 0.0193(11) 0.0228(12) 0.0185(11) -0.0035(9) -0.0017(9) -0.0051(9) C14 0.0274(14) 0.0253(13) 0.0190(12) -0.0030(10) 0.0010(10) -0.0104(11) C15 0.0298(14) 0.0239(12) 0.0146(11) -0.0031(9) -0.0007(10) -0.0072(10) O17 0.0151(8) 0.0175(8) 0.0197(9) -0.0056(7) -0.0034(7) -0.0002(6) O16 0.0191(9) 0.0258(9) 0.0151(8) -0.0049(7) -0.0036(7) 0.0002(7) C16 0.0155(10) 0.0174(10) 0.0147(10) -0.0043(8) -0.0017(8) -0.0027(8) C17 0.0141(9) 0.0162(10) 0.0133(9) -0.0040(8) -0.0012(8) -0.0020(8) C18 0.0154(10) 0.0211(11) 0.0172(11) -0.0036(9) -0.0038(8) -0.0002(8) C19 0.0165(11) 0.0246(12) 0.0190(11) -0.0050(9) -0.0014(9) -0.0002(9) C20 0.0203(11) 0.0233(12) 0.0166(11) -0.0070(9) 0.0008(9) -0.0026(9) C21 0.0221(12) 0.0271(13) 0.0154(11) -0.0065(9) -0.0033(9) -0.0024(10) C22 0.0174(10) 0.0220(11) 0.0160(10) -0.0048(9) -0.0029(8) -0.0014(9) O23 0.0261(9) 0.0157(8) 0.0170(8) -0.0044(6) -0.0063(7) -0.0043(7) O24 0.0250(9) 0.0157(8) 0.0177(8) -0.0023(7) -0.0065(7) -0.0044(7) C23 0.0237(11) 0.0141(10) 0.0133(10) -0.0038(8) -0.0016(8) -0.0051(8) C24 0.0242(12) 0.0148(10) 0.0216(12) -0.0057(9) -0.0011(9) -0.0057(9) C25 0.0332(15) 0.0162(11) 0.0270(14) -0.0042(10) -0.0056(12) -0.0057(10) C26 0.042(2) 0.0148(12) 0.039(2) -0.0030(11) -0.0058(15) -0.0060(12) C27 0.038(2) 0.0160(12) 0.048(2) -0.0092(13) 0.001(2) -0.0103(12) C28 0.031(2) 0.0230(14) 0.064(3) -0.016(2) -0.011(2) -0.0085(12) C29 0.0280(14) 0.0193(12) 0.043(2) -0.0093(12) -0.0111(13) -0.0055(11) C30 0.083(5) 0.039(3) 0.101(6) 0.006(3) -0.038(4) -0.005(3) Cl31 0.0862(13) 0.123(2) 0.0747(12) 0.0141(12) -0.0121(10) 0.0518(13) Cl32 0.0534(7) 0.0434(6) 0.1021(13) 0.0003(7) -0.0239(8) -0.0069(5) C40 0.060(3) 0.049(3) 0.069(4) -0.022(2) -0.030(3) 0.014(2) Cl41 0.144(2) 0.0589(10) 0.122(2) -0.0001(11) -0.056(2) -0.0058(12) Cl42 0.0704(10) 0.0998(14) 0.0957(14) -0.0521(12) 0.0080(9) -0.0351(10) _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 Gd1 O17 2.303(2) 2_696 ? Gd1 O24 2.311(2) 2_696 ? Gd1 O23 2.317(2) . ? Gd1 O16 2.353(2) . ? Gd1 N7 2.479(2) . ? Gd1 N2 2.513(2) . ? Gd1 N12 2.528(2) . ? Gd1 O17 2.808(2) . ? Gd1 C16 2.950(3) . ? Gd1 Gd1 3.9148(4) 2_696 ? Cl1 C20 1.736(3) . ? Cl2 C27 1.729(3) . ? B1 N1 1.533(4) . ? B1 N6 1.538(4) . ? B1 N11 1.548(4) . ? N1 C5 1.345(4) . ? N1 N2 1.356(3) . ? N2 C3 1.337(4) . ? N6 C10 1.344(4) . ? N6 N7 1.356(3) . ? N7 C8 1.337(4) . ? N11 C15 1.343(4) . ? N11 N12 1.358(3) . ? N12 C13 1.342(4) . ? C3 C4 1.389(4) . ? C4 C5 1.376(4) . ? C8 C9 1.388(4) . ? C9 C10 1.379(4) . ? C13 C14 1.387(4) . ? C14 C15 1.375(4) . ? O17 C16 1.269(3) . ? O17 Gd1 2.303(2) 2_696 ? O16 C16 1.255(3) . ? C16 C17 1.483(4) . ? C17 C18 1.392(4) . ? C17 C22 1.393(4) . ? C18 C19 1.385(4) . ? C19 C20 1.385(4) . ? C20 C21 1.387(4) . ? C21 C22 1.382(4) . ? O23 C23 1.261(3) . ? O24 C23 1.254(3) . ? O24 Gd1 2.311(2) 2_696 ? C23 C24 1.491(4) . ? C24 C29 1.386(4) . ? C24 C25 1.389(4) . ? C25 C26 1.387(4) . ? C26 C27 1.387(6) . ? C27 C28 1.371(6) . ? C28 C29 1.389(4) . ? C30 Cl32 1.718(6) . ? C30 Cl31 1.728(7) . ? C40 Cl41 1.729(6) . ? C40 Cl42 1.751(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O17 Gd1 O24 79.71(7) 2_696 2_696 ? O17 Gd1 O23 78.14(7) 2_696 . ? O24 Gd1 O23 134.29(7) 2_696 . ? O17 Gd1 O16 129.98(7) 2_696 . ? O24 Gd1 O16 82.34(8) 2_696 . ? O23 Gd1 O16 82.12(8) . . ? O17 Gd1 N7 155.01(8) 2_696 . ? O24 Gd1 N7 103.55(8) 2_696 . ? O23 Gd1 N7 113.23(8) . . ? O16 Gd1 N7 74.76(7) . . ? O17 Gd1 N2 84.46(8) 2_696 . ? O24 Gd1 N2 72.87(8) 2_696 . ? O23 Gd1 N2 142.59(8) . . ? O16 Gd1 N2 132.97(8) . . ? N7 Gd1 N2 73.20(8) . . ? O17 Gd1 N12 89.00(8) 2_696 . ? O24 Gd1 N12 145.39(8) 2_696 . ? O23 Gd1 N12 73.29(7) . . ? O16 Gd1 N12 128.00(8) . . ? N7 Gd1 N12 74.23(8) . . ? N2 Gd1 N12 73.54(8) . . ? O17 Gd1 O17 80.50(7) 2_696 . ? O24 Gd1 O17 68.72(7) 2_696 . ? O23 Gd1 O17 68.51(7) . . ? O16 Gd1 O17 49.49(6) . . ? N7 Gd1 O17 124.05(7) . . ? N2 Gd1 O17 140.60(7) . . ? N12 Gd1 O17 141.68(7) . . ? O17 Gd1 C16 105.78(7) 2_696 . ? O24 Gd1 C16 75.03(7) 2_696 . ? O23 Gd1 C16 73.34(7) . . ? O16 Gd1 C16 24.21(7) . . ? N7 Gd1 C16 98.93(8) . . ? N2 Gd1 C16 143.84(8) . . ? N12 Gd1 C16 139.54(8) . . ? O17 Gd1 C16 25.31(6) . . ? O17 Gd1 Gd1 45.03(5) 2_696 2_696 ? O24 Gd1 Gd1 68.56(5) 2_696 2_696 ? O23 Gd1 Gd1 67.44(5) . 2_696 ? O16 Gd1 Gd1 84.96(5) . 2_696 ? N7 Gd1 Gd1 159.21(5) . 2_696 ? N2 Gd1 Gd1 119.84(6) . 2_696 ? N12 Gd1 Gd1 123.54(5) . 2_696 ? O17 Gd1 Gd1 35.47(4) . 2_696 ? C16 Gd1 Gd1 60.76(5) . 2_696 ? N1 B1 N6 110.3(2) . . ? N1 B1 N11 108.7(2) . . ? N6 B1 N11 108.8(2) . . ? C5 N1 N2 110.1(2) . . ? C5 N1 B1 128.7(2) . . ? N2 N1 B1 121.2(2) . . ? C3 N2 N1 106.0(2) . . ? C3 N2 Gd1 129.1(2) . . ? N1 N2 Gd1 124.3(2) . . ? C10 N6 N7 110.2(2) . . ? C10 N6 B1 127.3(2) . . ? N7 N6 B1 122.5(2) . . ? C8 N7 N6 106.1(2) . . ? C8 N7 Gd1 129.8(2) . . ? N6 N7 Gd1 124.1(2) . . ? C15 N11 N12 109.8(2) . . ? C15 N11 B1 128.7(2) . . ? N12 N11 B1 121.5(2) . . ? C13 N12 N11 106.0(2) . . ? C13 N12 Gd1 130.3(2) . . ? N11 N12 Gd1 123.6(2) . . ? N2 C3 C4 110.9(3) . . ? C5 C4 C3 104.5(3) . . ? N1 C5 C4 108.4(2) . . ? N7 C8 C9 110.8(3) . . ? C10 C9 C8 104.7(3) . . ? N6 C10 C9 108.2(2) . . ? N12 C13 C14 111.0(3) . . ? C15 C14 C13 104.4(3) . . ? N11 C15 C14 108.9(3) . . ? C16 O17 Gd1 175.9(2) . 2_696 ? C16 O17 Gd1 83.6(2) . . ? Gd1 O17 Gd1 99.50(7) 2_696 . ? C16 O16 Gd1 105.6(2) . . ? O16 C16 O17 121.2(2) . . ? O16 C16 C17 118.7(2) . . ? O17 C16 C17 120.0(2) . . ? O16 C16 Gd1 50.23(13) . . ? O17 C16 Gd1 71.10(14) . . ? C17 C16 Gd1 168.1(2) . . ? C18 C17 C22 120.0(2) . . ? C18 C17 C16 118.8(2) . . ? C22 C17 C16 121.2(2) . . ? C19 C18 C17 120.4(2) . . ? C18 C19 C20 118.6(3) . . ? C19 C20 C21 122.0(3) . . ? C19 C20 Cl1 118.6(2) . . ? C21 C20 Cl1 119.5(2) . . ? C22 C21 C20 118.9(3) . . ? C21 C22 C17 120.1(3) . . ? C23 O23 Gd1 137.8(2) . . ? C23 O24 Gd1 135.8(2) . 2_696 ? O24 C23 O23 125.2(2) . . ? O24 C23 C24 117.5(2) . . ? O23 C23 C24 117.3(2) . . ? C29 C24 C25 119.9(3) . . ? C29 C24 C23 120.0(3) . . ? C25 C24 C23 120.1(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 118.5(3) . . ? C28 C27 C26 121.9(3) . . ? C28 C27 Cl2 119.8(3) . . ? C26 C27 Cl2 118.3(3) . . ? C27 C28 C29 119.2(4) . . ? C24 C29 C28 120.0(3) . . ? Cl32 C30 Cl31 112.9(4) . . ? Cl41 C40 Cl42 112.7(3) . . ? _refine_diff_density_max 2.928 _refine_diff_density_min -2.239 _refine_diff_density_rms 0.174 #===END data_4 _database_code_CSD 186524 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C46 H36 B2 Cl4 N12 O8 Tb2], 4 CH2Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C50 H44 B2 Cl12 N12 O8 Tb2' _chemical_formula_weight 1705.83 _chemical_melting_point ? _chemical_compound_source ? 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 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4247(7) _cell_length_b 12.7294(11) _cell_length_c 14.274(2) _cell_angle_alpha 74.74(1) _cell_angle_beta 76.25(1) _cell_angle_gamma 83.30(1) _cell_volume 1602.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5594 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method ? _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 2.749 _exptl_absorpt_correction_type 'Gausssian, Face Indexed' _exptl_absorpt_correction_T_min 0.5738 _exptl_absorpt_correction_T_max 0.7779 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SAMRT CCD-Detector' _diffrn_measurement_method '\w, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17660 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.1060 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 33.81 _reflns_number_total 10626 _reflns_number_observed 7675 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 21 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0615P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10605 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_obs 0.0564 _refine_ls_wR_factor_all 0.1264 _refine_ls_wR_factor_obs 0.1150 _refine_ls_goodness_of_fit_all 0.992 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_restrained_S_all 0.996 _refine_ls_restrained_S_obs 1.071 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tb1 Tb 0.61042(2) 1.95121(2) 0.60576(2) 0.01384(7) Uani 1 d . . Cl1 Cl 1.12961(15) 1.81895(12) 0.03705(10) 0.0300(3) Uani 1 d . . Cl2 Cl 0.2258(2) 1.34110(12) 0.6127(2) 0.0555(5) Uani 1 d . . B1 B 0.6777(6) 1.9003(4) 0.8564(4) 0.0171(10) Uani 1 d . . H1 H 0.6976(6) 1.8860(4) 0.9245(4) 0.021 Uiso 1 calc R . N1 N 0.6146(5) 2.0191(3) 0.8248(3) 0.0194(8) Uani 1 d . . N2 N 0.5882(4) 2.0605(3) 0.7316(3) 0.0187(8) Uani 1 d . . N6 N 0.8190(5) 1.8816(3) 0.7820(3) 0.0193(8) Uani 1 d . . N7 N 0.8239(4) 1.8936(3) 0.6837(3) 0.0187(8) Uani 1 d . . N11 N 0.5616(5) 1.8218(3) 0.8562(3) 0.0193(8) Uani 1 d . . N12 N 0.5132(4) 1.8259(3) 0.7731(3) 0.0186(8) Uani 1 d . . C3 C 0.5339(5) 2.1625(4) 0.7292(4) 0.0207(10) Uani 1 d . . H3 H 0.5062(5) 2.2117(4) 0.6729(4) 0.025 Uiso 1 calc R . C4 C 0.5231(6) 2.1876(4) 0.8203(4) 0.0243(11) Uani 1 d . . H4 H 0.4875(6) 2.2542(4) 0.8381(4) 0.029 Uiso 1 calc R . C5 C 0.5753(6) 2.0947(4) 0.8781(4) 0.0217(10) Uani 1 d . . H5 H 0.5827(6) 2.0850(4) 0.9451(4) 0.026 Uiso 1 calc R . C8 C 0.9633(5) 1.8687(4) 0.6425(4) 0.0204(10) Uani 1 d . . H8 H 0.9997(5) 1.8717(4) 0.5739(4) 0.024 Uiso 1 calc R . C9 C 1.0467(6) 1.8381(4) 0.7148(4) 0.0227(10) Uani 1 d . . H9 H 1.1476(6) 1.8153(4) 0.7062(4) 0.027 Uiso 1 calc R . C10 C 0.9500(6) 1.8482(4) 0.8018(4) 0.0230(10) Uani 1 d . . H10 H 0.9733(6) 1.8337(4) 0.8654(4) 0.028 Uiso 1 calc R . C13 C 0.4191(6) 1.7472(4) 0.7985(4) 0.0230(10) Uani 1 d . . H13 H 0.3688(6) 1.7307(4) 0.7542(4) 0.028 Uiso 1 calc R . C14 C 0.4043(6) 1.6922(4) 0.8988(4) 0.0251(11) Uani 1 d . . H14 H 0.3443(6) 1.6336(4) 0.9353(4) 0.030 Uiso 1 calc R . C15 C 0.4960(6) 1.7423(4) 0.9321(4) 0.0246(11) Uani 1 d . . H15 H 0.5114(6) 1.7243(4) 0.9980(4) 0.030 Uiso 1 calc R . O17 O 0.6246(4) 1.9812(3) 0.3988(2) 0.0184(7) Uani 1 d . . O16 O 0.8017(4) 1.9147(3) 0.4777(2) 0.0208(7) Uani 1 d . . C16 C 0.7529(5) 1.9393(4) 0.3990(3) 0.0160(9) Uani 1 d . . C17 C 0.8484(5) 1.9150(4) 0.3067(3) 0.0166(9) Uani 1 d . . C18 C 0.9863(5) 1.8642(4) 0.3105(4) 0.0181(9) Uani 1 d . . H18 H 1.0212(5) 1.8498(4) 0.3701(4) 0.022 Uiso 1 calc R . C19 C 1.0730(5) 1.8344(4) 0.2273(4) 0.0209(10) Uani 1 d . . H19 H 1.1666(5) 1.7984(4) 0.2298(4) 0.025 Uiso 1 calc R . C20 C 1.0211(6) 1.8581(4) 0.1407(4) 0.0220(10) Uani 1 d . . C21 C 0.8858(5) 1.9112(4) 0.1347(4) 0.0220(10) Uani 1 d . . H21 H 0.8528(5) 1.9275(4) 0.0743(4) 0.026 Uiso 1 calc R . C22 C 0.7990(5) 1.9402(4) 0.2184(4) 0.0207(10) Uani 1 d . . H22 H 0.7061(5) 1.9772(4) 0.2153(4) 0.025 Uiso 1 calc R . O23 O 0.5131(4) 1.8090(3) 0.5740(2) 0.0209(7) Uani 1 d . . O24 O 0.3454(4) 1.8717(3) 0.4818(2) 0.0199(7) Uani 1 d . . C23 C 0.4123(5) 1.7957(4) 0.5348(3) 0.0178(9) Uani 1 d . . C24 C 0.3671(6) 1.6820(4) 0.5518(4) 0.0207(10) Uani 1 d . . C25 C 0.4408(6) 1.5947(4) 0.6062(4) 0.0283(12) Uani 1 d . . H25 H 0.5205(6) 1.6073(4) 0.6312(4) 0.034 Uiso 1 calc R . C26 C 0.3977(7) 1.4890(4) 0.6241(4) 0.0335(13) Uani 1 d . . H26 H 0.4470(7) 1.4291(4) 0.6614(4) 0.040 Uiso 1 calc R . C27 C 0.2828(7) 1.4732(4) 0.5868(5) 0.0362(15) Uani 1 d . . C28 C 0.2100(7) 1.5578(5) 0.5331(5) 0.0383(15) Uani 1 d . . H28 H 0.1305(7) 1.5447(5) 0.5082(5) 0.046 Uiso 1 calc R . C29 C 0.2532(6) 1.6630(4) 0.5153(4) 0.0293(12) Uani 1 d . . H29 H 0.2035(6) 1.7223(4) 0.4776(4) 0.035 Uiso 1 calc R . C30 C 0.9026(13) 1.5745(8) 1.1231(9) 0.089(3) Uani 1 d . . H30A H 1.0044(13) 1.5908(8) 1.0877(9) 0.107 Uiso 1 calc R . H30B H 0.8788(13) 1.6072(8) 1.1811(9) 0.107 Uiso 1 calc R . Cl31 Cl 0.7851(4) 1.6339(3) 1.0439(2) 0.1211(13) Uani 1 d . . Cl32 Cl 0.8912(3) 1.4367(2) 1.1641(2) 0.0826(7) Uani 1 d . . C40 C 1.2362(10) 1.4035(7) 0.2349(7) 0.069(2) Uani 1 d . . H40A H 1.3281(10) 1.3590(7) 0.2198(7) 0.083 Uiso 1 calc R . H40B H 1.1621(10) 1.3793(7) 0.2075(7) 0.083 Uiso 1 calc R . Cl41 Cl 1.2663(4) 1.5392(2) 0.1770(3) 0.1203(12) Uani 1 d . . Cl42 Cl 1.1762(3) 1.3809(3) 0.3638(2) 0.0984(10) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01491(11) 0.01375(10) 0.01387(11) -0.00508(7) -0.00285(8) -0.00143(7) Cl1 0.0292(7) 0.0388(7) 0.0222(6) -0.0153(6) 0.0018(5) -0.0001(6) Cl2 0.0540(11) 0.0213(7) 0.0891(14) -0.0147(8) -0.0036(10) -0.0159(7) B1 0.021(3) 0.014(2) 0.016(2) -0.003(2) -0.006(2) -0.001(2) N1 0.026(2) 0.019(2) 0.016(2) -0.008(2) -0.002(2) -0.007(2) N2 0.022(2) 0.020(2) 0.016(2) -0.008(2) -0.002(2) -0.003(2) N6 0.022(2) 0.020(2) 0.017(2) -0.003(2) -0.007(2) -0.003(2) N7 0.020(2) 0.021(2) 0.016(2) -0.006(2) -0.004(2) -0.001(2) N11 0.024(2) 0.021(2) 0.012(2) -0.005(2) 0.000(2) -0.005(2) N12 0.018(2) 0.024(2) 0.016(2) -0.007(2) -0.004(2) -0.004(2) C3 0.023(2) 0.017(2) 0.021(2) -0.006(2) -0.003(2) 0.000(2) C4 0.026(3) 0.024(2) 0.026(3) -0.012(2) -0.002(2) -0.001(2) C5 0.025(3) 0.025(2) 0.018(2) -0.012(2) 0.000(2) -0.007(2) C8 0.018(2) 0.022(2) 0.022(2) -0.008(2) -0.004(2) -0.001(2) C9 0.017(2) 0.025(2) 0.027(3) -0.007(2) -0.005(2) -0.002(2) C10 0.023(3) 0.022(2) 0.025(3) -0.003(2) -0.011(2) -0.001(2) C13 0.023(3) 0.028(3) 0.018(2) -0.009(2) -0.002(2) -0.005(2) C14 0.026(3) 0.023(2) 0.024(3) -0.005(2) 0.002(2) -0.007(2) C15 0.032(3) 0.027(3) 0.014(2) -0.005(2) -0.001(2) -0.004(2) O17 0.019(2) 0.017(2) 0.019(2) -0.0049(13) -0.0017(13) -0.0003(13) O16 0.018(2) 0.024(2) 0.020(2) -0.0048(14) -0.0040(14) 0.0024(14) C16 0.016(2) 0.014(2) 0.018(2) -0.004(2) -0.004(2) -0.003(2) C17 0.019(2) 0.015(2) 0.016(2) -0.006(2) 0.000(2) -0.006(2) C18 0.017(2) 0.020(2) 0.018(2) -0.005(2) -0.004(2) 0.000(2) C19 0.015(2) 0.024(2) 0.022(2) -0.007(2) 0.000(2) -0.001(2) C20 0.024(3) 0.022(2) 0.020(2) -0.011(2) 0.002(2) -0.003(2) C21 0.023(3) 0.024(2) 0.018(2) -0.006(2) -0.003(2) -0.001(2) C22 0.019(2) 0.021(2) 0.023(2) -0.008(2) -0.003(2) -0.002(2) O23 0.028(2) 0.018(2) 0.018(2) -0.0046(13) -0.0049(14) -0.0046(14) O24 0.025(2) 0.020(2) 0.015(2) -0.0041(13) -0.0028(14) -0.0044(14) C23 0.020(2) 0.021(2) 0.014(2) -0.008(2) 0.000(2) -0.006(2) C24 0.024(3) 0.016(2) 0.022(2) -0.005(2) -0.001(2) -0.007(2) C25 0.030(3) 0.021(2) 0.034(3) -0.010(2) -0.004(2) -0.004(2) C26 0.045(4) 0.016(2) 0.035(3) -0.003(2) -0.004(3) -0.002(2) C27 0.036(3) 0.017(2) 0.054(4) -0.014(3) 0.005(3) -0.011(2) C28 0.031(3) 0.027(3) 0.062(4) -0.017(3) -0.009(3) -0.012(2) C29 0.031(3) 0.019(2) 0.039(3) -0.008(2) -0.006(2) -0.007(2) C30 0.100(8) 0.058(6) 0.102(8) 0.004(6) -0.028(7) -0.012(5) Cl31 0.095(2) 0.140(3) 0.089(2) 0.010(2) -0.014(2) 0.050(2) Cl32 0.0668(15) 0.0562(13) 0.121(2) -0.0036(13) -0.0305(14) -0.0082(11) C40 0.070(6) 0.065(6) 0.077(6) -0.021(5) -0.032(5) 0.014(4) Cl41 0.161(3) 0.067(2) 0.129(3) 0.001(2) -0.050(2) -0.010(2) Cl42 0.089(2) 0.111(2) 0.105(2) -0.053(2) 0.008(2) -0.041(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O17 2.291(3) 2_696 ? Tb1 O24 2.303(3) 2_696 ? Tb1 O23 2.311(3) . ? Tb1 O16 2.344(3) . ? Tb1 N7 2.473(4) . ? Tb1 N2 2.505(4) . ? Tb1 N12 2.527(4) . ? Tb1 O17 2.850(3) . ? Tb1 C16 2.974(5) . ? Tb1 Tb1 3.9242(7) 2_696 ? Cl1 C20 1.742(5) . ? Cl2 C27 1.744(5) . ? B1 N6 1.532(7) . ? B1 N1 1.550(7) . ? B1 N11 1.567(7) . ? N1 C5 1.346(6) . ? N1 N2 1.366(6) . ? N2 C3 1.334(6) . ? N6 C10 1.329(6) . ? N6 N7 1.360(6) . ? N7 C8 1.344(6) . ? N11 C15 1.352(6) . ? N11 N12 1.355(6) . ? N12 C13 1.335(6) . ? C3 C4 1.396(7) . ? C4 C5 1.365(7) . ? C8 C9 1.391(7) . ? C9 C10 1.382(7) . ? C13 C14 1.401(7) . ? C14 C15 1.365(8) . ? O17 C16 1.263(6) . ? O17 Tb1 2.291(3) 2_696 ? O16 C16 1.265(6) . ? C16 C17 1.493(6) . ? C17 C18 1.389(7) . ? C17 C22 1.393(7) . ? C18 C19 1.387(6) . ? C19 C20 1.384(7) . ? C20 C21 1.382(7) . ? C21 C22 1.389(7) . ? O23 C23 1.259(6) . ? O24 C23 1.267(6) . ? O24 Tb1 2.303(3) 2_696 ? C23 C24 1.498(6) . ? C24 C29 1.369(8) . ? C24 C25 1.394(8) . ? C25 C26 1.392(7) . ? C26 C27 1.370(9) . ? C27 C28 1.364(9) . ? C28 C29 1.387(7) . ? C30 Cl32 1.704(10) . ? C30 Cl31 1.740(11) . ? C40 Cl41 1.731(9) . ? C40 Cl42 1.748(10) . ? 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 O17 Tb1 O24 80.30(12) 2_696 2_696 ? O17 Tb1 O23 78.45(12) 2_696 . ? O24 Tb1 O23 133.62(12) 2_696 . ? O17 Tb1 O16 129.93(12) 2_696 . ? O24 Tb1 O16 81.59(12) 2_696 . ? O23 Tb1 O16 81.34(12) . . ? O17 Tb1 N7 154.72(13) 2_696 . ? O24 Tb1 N7 103.18(13) 2_696 . ? O23 Tb1 N7 113.41(13) . . ? O16 Tb1 N7 75.10(12) . . ? O17 Tb1 N2 83.96(13) 2_696 . ? O24 Tb1 N2 73.23(12) 2_696 . ? O23 Tb1 N2 143.20(12) . . ? O16 Tb1 N2 133.38(13) . . ? N7 Tb1 N2 73.43(13) . . ? O17 Tb1 N12 88.56(12) 2_696 . ? O24 Tb1 N12 146.10(12) 2_696 . ? O23 Tb1 N12 73.67(12) . . ? O16 Tb1 N12 128.22(12) . . ? N7 Tb1 N12 74.58(13) . . ? N2 Tb1 N12 73.82(13) . . ? O17 Tb1 O17 81.05(11) 2_696 . ? O24 Tb1 O17 68.09(10) 2_696 . ? O23 Tb1 O17 68.19(11) . . ? O16 Tb1 O17 48.89(11) . . ? N7 Tb1 O17 123.75(11) . . ? N2 Tb1 O17 140.27(11) . . ? N12 Tb1 O17 141.73(11) . . ? O17 Tb1 C16 105.95(12) 2_696 . ? O24 Tb1 C16 74.25(12) 2_696 . ? O23 Tb1 C16 72.78(12) . . ? O16 Tb1 C16 23.98(12) . . ? N7 Tb1 C16 99.03(13) . . ? N2 Tb1 C16 143.72(12) . . ? N12 Tb1 C16 139.62(12) . . ? O17 Tb1 C16 24.93(11) . . ? O17 Tb1 Tb1 45.83(8) 2_696 2_696 ? O24 Tb1 Tb1 68.33(9) 2_696 2_696 ? O23 Tb1 Tb1 67.25(9) . 2_696 ? O16 Tb1 Tb1 84.10(8) . 2_696 ? N7 Tb1 Tb1 158.63(9) . 2_696 ? N2 Tb1 Tb1 119.80(10) . 2_696 ? N12 Tb1 Tb1 123.74(9) . 2_696 ? O17 Tb1 Tb1 35.21(7) . 2_696 ? C16 Tb1 Tb1 60.12(9) . 2_696 ? N6 B1 N1 109.9(4) . . ? N6 B1 N11 109.1(4) . . ? N1 B1 N11 107.9(4) . . ? C5 N1 N2 109.8(4) . . ? C5 N1 B1 129.3(4) . . ? N2 N1 B1 120.9(4) . . ? C3 N2 N1 105.7(4) . . ? C3 N2 Tb1 129.4(3) . . ? N1 N2 Tb1 124.5(3) . . ? C10 N6 N7 110.3(4) . . ? C10 N6 B1 126.9(4) . . ? N7 N6 B1 122.7(4) . . ? C8 N7 N6 106.2(4) . . ? C8 N7 Tb1 129.6(3) . . ? N6 N7 Tb1 124.2(3) . . ? C15 N11 N12 109.7(4) . . ? C15 N11 B1 128.5(4) . . ? N12 N11 B1 121.8(4) . . ? C13 N12 N11 106.0(4) . . ? C13 N12 Tb1 130.3(3) . . ? N11 N12 Tb1 123.5(3) . . ? N2 C3 C4 111.1(5) . . ? C5 C4 C3 104.4(4) . . ? N1 C5 C4 109.0(4) . . ? N7 C8 C9 110.2(5) . . ? C10 C9 C8 104.6(4) . . ? N6 C10 C9 108.7(4) . . ? N12 C13 C14 111.1(5) . . ? C15 C14 C13 104.0(4) . . ? N11 C15 C14 109.1(4) . . ? C16 O17 Tb1 176.5(3) . 2_696 ? C16 O17 Tb1 83.0(3) . . ? Tb1 O17 Tb1 98.95(11) 2_696 . ? C16 O16 Tb1 107.1(3) . . ? O17 C16 O16 120.8(4) . . ? O17 C16 C17 120.5(4) . . ? O16 C16 C17 118.6(4) . . ? O17 C16 Tb1 72.0(3) . . ? O16 C16 Tb1 48.9(2) . . ? C17 C16 Tb1 166.8(3) . . ? C18 C17 C22 120.2(4) . . ? C18 C17 C16 119.1(4) . . ? C22 C17 C16 120.6(4) . . ? C19 C18 C17 120.0(4) . . ? C20 C19 C18 119.0(5) . . ? C21 C20 C19 121.8(4) . . ? C21 C20 Cl1 119.4(4) . . ? C19 C20 Cl1 118.8(4) . . ? C20 C21 C22 119.0(5) . . ? C21 C22 C17 119.9(5) . . ? C23 O23 Tb1 138.0(3) . . ? C23 O24 Tb1 135.8(3) . 2_696 ? O23 C23 O24 124.8(4) . . ? O23 C23 C24 118.1(4) . . ? O24 C23 C24 117.2(4) . . ? C29 C24 C25 119.7(5) . . ? C29 C24 C23 120.7(5) . . ? C25 C24 C23 119.7(5) . . ? C26 C25 C24 120.1(5) . . ? C27 C26 C25 118.7(6) . . ? C28 C27 C26 121.9(5) . . ? C28 C27 Cl2 119.6(5) . . ? C26 C27 Cl2 118.5(5) . . ? C27 C28 C29 119.3(6) . . ? C24 C29 C28 120.4(6) . . ? Cl32 C30 Cl31 112.6(6) . . ? Cl41 C40 Cl42 112.7(5) . . ? _refine_diff_density_max 1.510 _refine_diff_density_min -1.834 _refine_diff_density_rms 0.204 #===END data_7 _database_code_CSD 186525 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C72 H80 B8 N60 Tb4], 6 CH2Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C78 H92 B8 Cl12 N60 Tb4' _chemical_formula_weight 3017.68 _chemical_melting_point ? _chemical_compound_source ? 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' 'Tb' 'Tb' -0.1723 4.1537 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/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 15.8429(4) _cell_length_b 25.3237(8) _cell_length_c 15.9930(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.06(1) _cell_angle_gamma 90.00 _cell_volume 5812.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 66556 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method ? _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 2.750 _exptl_absorpt_correction_type 'Gaussian, face indexed' _exptl_absorpt_correction_T_min 0.6332 _exptl_absorpt_correction_T_max 0.8391 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa-CCD' _diffrn_measurement_method '\w, 382 images at 1 deg. and 180 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66556 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 33.13 _reflns_number_total 22112 _reflns_number_observed 17192 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect' _computing_cell_refinement 'DENZO, Nonius Collect' _computing_data_reduction 'DENZO, Nonius Collect' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 90 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+4.0321P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22022 _refine_ls_number_parameters 747 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_obs 0.0343 _refine_ls_wR_factor_all 0.0733 _refine_ls_wR_factor_obs 0.0664 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.030 _refine_ls_restrained_S_obs 1.063 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tb1 Tb 0.348954(7) 0.404568(4) 0.285231(7) 0.01210(3) Uani 1 d . . Tb2 Tb 0.263285(7) 0.650757(4) 0.343659(7) 0.01244(3) Uani 1 d . . N1 N 0.24764(13) 0.34235(8) 0.07050(13) 0.0160(4) Uani 1 d . . B1 B 0.2680(2) 0.39475(11) 0.0340(2) 0.0177(5) Uani 1 d . . H1 H 0.2460(2) 0.39250(11) -0.0344(2) 0.021 Uiso 1 calc R . N2 N 0.27655(14) 0.33368(8) 0.16268(14) 0.0170(4) Uani 1 d . . C3 C 0.2408(2) 0.28657(10) 0.1695(2) 0.0189(5) Uani 1 d . . H3 H 0.2492(2) 0.27038(10) 0.2261(2) 0.023 Uiso 1 calc R . C4 C 0.1901(2) 0.26472(10) 0.0829(2) 0.0214(5) Uani 1 d . . H4 H 0.1585(2) 0.23177(10) 0.0688(2) 0.026 Uiso 1 calc R . C5 C 0.1957(2) 0.30130(10) 0.0222(2) 0.0198(5) Uani 1 d . . H5 H 0.1677(2) 0.29820(10) -0.0432(2) 0.024 Uiso 1 calc R . N6 N 0.37322(14) 0.40633(8) 0.07956(14) 0.0166(4) Uani 1 d . . N7 N 0.42160(14) 0.41258(8) 0.17285(14) 0.0165(4) Uani 1 d . . C8 C 0.5085(2) 0.42553(10) 0.1866(2) 0.0206(5) Uani 1 d . . H8 H 0.5580(2) 0.43193(10) 0.2454(2) 0.025 Uiso 1 calc R . C9 C 0.5166(2) 0.42839(11) 0.1035(2) 0.0241(5) Uani 1 d . . H9 H 0.5705(2) 0.43718(11) 0.0946(2) 0.029 Uiso 1 calc R . C10 C 0.4295(2) 0.41569(10) 0.0372(2) 0.0214(5) Uani 1 d . . H10 H 0.4119(2) 0.41384(10) -0.0274(2) 0.026 Uiso 1 calc R . N11 N 0.21602(13) 0.43988(8) 0.05761(13) 0.0156(4) Uani 1 d . . N12 N 0.23459(13) 0.45221(8) 0.14665(13) 0.0152(4) Uani 1 d . . C13 C 0.1795(2) 0.49337(9) 0.1424(2) 0.0163(4) Uani 1 d . . H13 H 0.1779(2) 0.51043(9) 0.1947(2) 0.020 Uiso 1 calc R . C14 C 0.1249(2) 0.50768(10) 0.0512(2) 0.0201(5) Uani 1 d . . H14 H 0.0799(2) 0.53515(10) 0.0293(2) 0.024 Uiso 1 calc R . C15 C 0.1508(2) 0.47297(10) -0.0002(2) 0.0186(5) Uani 1 d . . H15 H 0.1266(2) 0.47248(10) -0.0657(2) 0.022 Uiso 1 calc R . B2 B 0.2669(2) 0.33492(11) 0.4342(2) 0.0191(5) Uani 1 d . . H2 H 0.2452(2) 0.31514(11) 0.4757(2) 0.023 Uiso 1 calc R . N21 N 0.32092(14) 0.38419(8) 0.48456(13) 0.0178(4) Uani 1 d . . N22 N 0.35802(14) 0.41902(8) 0.44390(14) 0.0175(4) Uani 1 d . . C23 C 0.4009(2) 0.45626(10) 0.5075(2) 0.0206(5) Uani 1 d . . H23 H 0.4332(2) 0.48567(10) 0.4984(2) 0.025 Uiso 1 calc R . C24 C 0.3915(2) 0.44602(11) 0.5888(2) 0.0251(6) Uani 1 d . . H24 H 0.4149(2) 0.46633(11) 0.6439(2) 0.030 Uiso 1 calc R . C25 C 0.3411(2) 0.40008(11) 0.5714(2) 0.0239(5) Uani 1 d . . H25 H 0.3232(2) 0.38233(11) 0.6137(2) 0.029 Uiso 1 calc R . N26 N 0.18185(14) 0.35183(8) 0.34639(14) 0.0170(4) Uani 1 d . . N27 N 0.19076(14) 0.38082(8) 0.27833(13) 0.0157(4) Uani 1 d . . C28 C 0.1040(2) 0.38603(10) 0.2119(2) 0.0186(5) Uani 1 d . . H28 H 0.0886(2) 0.40436(10) 0.1555(2) 0.022 Uiso 1 calc R . C29 C 0.0395(2) 0.36123(10) 0.2362(2) 0.0215(5) Uani 1 d . . H29 H -0.0261(2) 0.35939(10) 0.2016(2) 0.026 Uiso 1 calc R . C30 C 0.0921(2) 0.33985(10) 0.3219(2) 0.0216(5) Uani 1 d . . H30 H 0.0686(2) 0.31992(10) 0.3577(2) 0.026 Uiso 1 calc R . N31 N 0.33069(14) 0.29900(8) 0.40822(14) 0.0171(4) Uani 1 d . . N32 N 0.38204(14) 0.31902(8) 0.36539(14) 0.0168(4) Uani 1 d . . C33 C 0.4333(2) 0.27903(10) 0.3575(2) 0.0188(5) Uani 1 d . . H33 H 0.4767(2) 0.28178(10) 0.3311(2) 0.023 Uiso 1 calc R . C34 C 0.4141(2) 0.23267(10) 0.3934(2) 0.0213(5) Uani 1 d . . H34 H 0.4401(2) 0.19863(10) 0.3953(2) 0.026 Uiso 1 calc R . C35 C 0.3496(2) 0.24705(10) 0.4253(2) 0.0204(5) Uani 1 d . . H35 H 0.3226(2) 0.22427(10) 0.4545(2) 0.024 Uiso 1 calc R . B3 B 0.3589(2) 0.78349(11) 0.4010(2) 0.0174(5) Uani 1 d . . H3A H 0.3865(2) 0.81955(11) 0.4186(2) 0.021 Uiso 1 calc R . N41 N 0.26479(14) 0.78727(8) 0.31499(14) 0.0170(4) Uani 1 d . . N42 N 0.21642(14) 0.74290(8) 0.27389(14) 0.0172(4) Uani 1 d . . C43 C 0.1398(2) 0.75982(10) 0.2015(2) 0.0204(5) Uani 1 d . . H43 H 0.0924(2) 0.73744(10) 0.1602(2) 0.025 Uiso 1 calc R . C44 C 0.1396(2) 0.81453(10) 0.1954(2) 0.0229(5) Uani 1 d . . H44 H 0.0937(2) 0.83620(10) 0.1506(2) 0.027 Uiso 1 calc R . C45 C 0.2201(2) 0.83059(10) 0.2684(2) 0.0222(5) Uani 1 d . . H45 H 0.2406(2) 0.86603(10) 0.2832(2) 0.027 Uiso 1 calc R . N46 N 0.34345(14) 0.75916(8) 0.48188(14) 0.0159(4) Uani 1 d . . N47 N 0.31294(14) 0.70836(8) 0.47956(14) 0.0167(4) Uani 1 d . . C48 C 0.3079(2) 0.70056(10) 0.5602(2) 0.0182(5) Uani 1 d . . H48 H 0.2891(2) 0.66840(10) 0.5779(2) 0.022 Uiso 1 calc R . C49 C 0.3336(2) 0.74567(10) 0.6145(2) 0.0199(5) Uani 1 d . . H49 H 0.3353(2) 0.75062(10) 0.6740(2) 0.024 Uiso 1 calc R . C50 C 0.3563(2) 0.78169(10) 0.5627(2) 0.0187(5) Uani 1 d . . H50 H 0.3774(2) 0.81673(10) 0.5810(2) 0.022 Uiso 1 calc R . N51 N 0.42406(13) 0.74860(8) 0.37504(13) 0.0157(4) Uani 1 d . . N52 N 0.40584(13) 0.69643(8) 0.35177(14) 0.0159(4) Uani 1 d . . C53 C 0.4737(2) 0.68039(10) 0.3286(2) 0.0177(5) Uani 1 d . . H53 H 0.4793(2) 0.64551(10) 0.3097(2) 0.021 Uiso 1 calc R . C54 C 0.5349(2) 0.72149(10) 0.3359(2) 0.0202(5) Uani 1 d . . H54 H 0.5885(2) 0.72031(10) 0.3236(2) 0.024 Uiso 1 calc R . C55 C 0.5005(2) 0.76416(10) 0.3649(2) 0.0186(5) Uani 1 d . . H55 H 0.5263(2) 0.79872(10) 0.3759(2) 0.022 Uiso 1 calc R . B4 B 0.0191(2) 0.61285(11) 0.2195(2) 0.0163(5) Uani 1 d . . H4A H -0.0479(2) 0.60282(11) 0.1850(2) 0.020 Uiso 1 calc R . N61 N 0.02726(13) 0.65952(8) 0.28451(14) 0.0166(4) Uani 1 d . . N62 N 0.11126(14) 0.67772(8) 0.34785(14) 0.0170(4) Uani 1 d . . C63 C 0.0914(2) 0.71907(10) 0.3888(2) 0.0210(5) Uani 1 d . . H63 H 0.1369(2) 0.73978(10) 0.4361(2) 0.025 Uiso 1 calc R . C64 C -0.0039(2) 0.72772(11) 0.3534(2) 0.0253(6) Uani 1 d . . H64 H -0.0357(2) 0.75421(11) 0.3711(2) 0.030 Uiso 1 calc R . C65 C -0.0422(2) 0.68929(10) 0.2870(2) 0.0232(5) Uani 1 d . . H65 H -0.1068(2) 0.68454(10) 0.2493(2) 0.028 Uiso 1 calc R . N66 N 0.05953(13) 0.62848(8) 0.15014(13) 0.0159(4) Uani 1 d . . N67 N 0.15279(13) 0.63812(8) 0.17973(13) 0.0158(4) Uani 1 d . . C68 C 0.1655(2) 0.64960(9) 0.1050(2) 0.0190(5) Uani 1 d . . H68 H 0.2242(2) 0.65754(9) 0.1052(2) 0.023 Uiso 1 calc R . C69 C 0.0814(2) 0.64847(10) 0.0261(2) 0.0210(5) Uani 1 d . . H69 H 0.0712(2) 0.65564(10) -0.0358(2) 0.025 Uiso 1 calc R . C70 C 0.0164(2) 0.63461(10) 0.0582(2) 0.0200(5) Uani 1 d . . H70 H -0.0484(2) 0.63012(10) 0.0213(2) 0.024 Uiso 1 calc R . N71 N 0.07376(13) 0.56588(8) 0.27776(13) 0.0162(4) Uani 1 d . . N72 N 0.16664(13) 0.56969(8) 0.33617(13) 0.0157(4) Uani 1 d . . C73 C 0.1903(2) 0.52324(9) 0.3798(2) 0.0181(5) Uani 1 d . . H73 H 0.2511(2) 0.51465(9) 0.4245(2) 0.022 Uiso 1 calc R . C74 C 0.1140(2) 0.48898(10) 0.3508(2) 0.0209(5) Uani 1 d . . H74 H 0.1123(2) 0.45393(10) 0.3712(2) 0.025 Uiso 1 calc R . C75 C 0.0421(2) 0.51741(10) 0.2862(2) 0.0197(5) Uani 1 d . . H75 H -0.0198(2) 0.50506(10) 0.2529(2) 0.024 Uiso 1 calc R . N80 N 0.38186(15) 0.49781(8) 0.31574(14) 0.0197(4) Uani 1 d . . N81 N 0.35863(13) 0.54184(8) 0.29888(13) 0.0158(4) Uani 1 d . . N82 N 0.33614(14) 0.58622(8) 0.28065(14) 0.0179(4) Uani 1 d . . N90 N 0.51615(14) 0.40337(8) 0.37731(14) 0.0199(4) Uani 1 d . . N91 N 0.42305(14) 0.59796(8) 0.54841(14) 0.0159(4) Uani 1 d . . N92 N 0.36067(15) 0.59791(8) 0.47478(15) 0.0223(5) Uani 1 d . . C80 C 0.0580(5) 0.9180(3) -0.0103(4) 0.0480(13) Uiso 0.575(11) d PD 1 H80A H 0.0433(5) 0.9446(3) -0.0598(4) 0.058 Uiso 0.575(11) calc PR 1 H80B H 0.0925(5) 0.8887(3) -0.0227(4) 0.058 Uiso 0.575(11) calc PR 1 Cl1 Cl 0.1281(3) 0.94706(13) 0.0976(2) 0.0649(11) Uani 0.575(11) d PD 1 Cl2 Cl -0.0450(2) 0.89395(11) -0.0104(2) 0.0481(8) Uani 0.575(11) d PD 1 C80X C 0.0879(7) 0.9112(4) 0.0016(6) 0.0480(13) Uiso 0.425(11) d PD 2 H80C H 0.1003(7) 0.8734(4) -0.0045(6) 0.058 Uiso 0.425(11) calc PR 2 H80D H 0.0828(7) 0.9295(4) -0.0550(6) 0.058 Uiso 0.425(11) calc PR 2 Cl1X Cl 0.1822(9) 0.9374(2) 0.0957(3) 0.100(3) Uani 0.425(11) d PD 2 Cl2X Cl -0.0198(8) 0.9165(6) 0.0088(8) 0.148(4) Uani 0.425(11) d PD 2 C90 C 0.7813(3) 0.5650(2) 0.2759(3) 0.0586(11) Uani 1 d . . H90A H 0.8492(3) 0.5719(2) 0.3029(3) 0.070 Uiso 1 calc R . H90B H 0.7654(3) 0.5521(2) 0.3259(3) 0.070 Uiso 1 calc R . Cl3 Cl 0.75418(7) 0.51559(3) 0.19078(6) 0.0454(2) Uani 1 d . . Cl4 Cl 0.72106(6) 0.62450(3) 0.23153(5) 0.0374(2) Uani 1 d . . C100 C 0.3606(2) 0.95119(12) 0.5858(2) 0.0346(7) Uani 1 d . . H10A H 0.3680(2) 0.98899(12) 0.5746(2) 0.041 Uiso 1 calc R . H10B H 0.3290(2) 0.94903(12) 0.6274(2) 0.041 Uiso 1 calc R . Cl5 Cl 0.47176(5) 0.92155(3) 0.63997(5) 0.0326(2) Uani 1 d . . Cl6 Cl 0.29047(5) 0.92029(3) 0.47975(5) 0.0317(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01329(5) 0.01122(5) 0.01107(5) 0.00026(4) 0.00446(4) 0.00031(4) Tb2 0.01270(5) 0.01054(5) 0.01214(5) -0.00021(4) 0.00340(4) 0.00031(4) N1 0.0160(9) 0.0168(10) 0.0144(9) -0.0026(8) 0.0056(8) 0.0007(8) B1 0.0175(12) 0.0199(13) 0.0145(12) -0.0007(10) 0.0057(10) 0.0001(11) N2 0.0186(9) 0.0157(9) 0.0159(9) -0.0021(8) 0.0066(8) -0.0002(8) C3 0.0217(11) 0.0150(11) 0.0219(12) -0.0014(9) 0.0109(10) -0.0005(9) C4 0.0210(12) 0.0172(12) 0.0290(13) -0.0077(10) 0.0136(11) -0.0035(10) C5 0.0164(11) 0.0215(12) 0.0202(12) -0.0080(10) 0.0064(10) -0.0012(10) N6 0.0172(9) 0.0199(10) 0.0143(9) -0.0005(8) 0.0081(8) 0.0011(8) N7 0.0158(9) 0.0181(10) 0.0143(9) 0.0000(8) 0.0051(8) -0.0002(8) C8 0.0168(11) 0.0232(13) 0.0218(12) -0.0006(10) 0.0081(10) -0.0007(10) C9 0.0200(12) 0.0281(14) 0.0296(14) 0.0013(11) 0.0156(11) -0.0008(11) C10 0.0240(12) 0.0254(13) 0.0203(12) 0.0017(10) 0.0148(10) 0.0010(10) N11 0.0149(9) 0.0158(9) 0.0143(9) -0.0012(8) 0.0045(8) -0.0002(8) N12 0.0165(9) 0.0163(9) 0.0130(9) 0.0001(8) 0.0063(8) 0.0012(8) C13 0.0156(10) 0.0150(11) 0.0196(11) -0.0019(9) 0.0086(9) -0.0009(9) C14 0.0181(11) 0.0133(11) 0.0238(12) 0.0026(10) 0.0041(10) 0.0027(9) C15 0.0153(10) 0.0190(12) 0.0160(11) 0.0022(9) 0.0013(9) -0.0010(9) B2 0.0235(13) 0.0178(13) 0.0194(13) 0.0037(11) 0.0125(11) 0.0011(11) N21 0.0223(10) 0.0190(10) 0.0134(9) 0.0028(8) 0.0090(8) 0.0041(8) N22 0.0194(10) 0.0175(10) 0.0140(9) 0.0019(8) 0.0054(8) 0.0015(8) C23 0.0189(11) 0.0191(12) 0.0183(11) -0.0020(10) 0.0026(10) 0.0030(10) C24 0.0295(13) 0.0265(14) 0.0148(11) -0.0028(10) 0.0051(10) 0.0091(11) C25 0.0301(13) 0.0290(14) 0.0153(11) 0.0030(10) 0.0121(11) 0.0093(12) N26 0.0190(9) 0.0169(10) 0.0183(10) 0.0007(8) 0.0110(8) 0.0009(8) N27 0.0176(9) 0.0162(9) 0.0147(9) -0.0001(8) 0.0083(8) -0.0002(8) C28 0.0201(11) 0.0180(12) 0.0168(11) -0.0037(9) 0.0069(10) -0.0027(10) C29 0.0168(11) 0.0258(13) 0.0213(12) -0.0051(10) 0.0076(10) -0.0056(10) C30 0.0226(12) 0.0207(12) 0.0273(13) -0.0051(10) 0.0163(11) -0.0052(10) N31 0.0182(9) 0.0143(9) 0.0192(10) 0.0040(8) 0.0084(8) 0.0013(8) N32 0.0181(9) 0.0157(9) 0.0179(10) 0.0019(8) 0.0090(8) 0.0014(8) C33 0.0186(11) 0.0182(11) 0.0191(11) -0.0011(9) 0.0076(10) 0.0019(9) C34 0.0198(11) 0.0164(11) 0.0236(12) 0.0003(10) 0.0053(10) 0.0027(10) C35 0.0221(12) 0.0157(11) 0.0204(12) 0.0038(10) 0.0062(10) -0.0007(10) B3 0.0200(12) 0.0113(12) 0.0198(13) -0.0012(10) 0.0073(11) 0.0004(10) N41 0.0198(10) 0.0126(9) 0.0192(10) 0.0007(8) 0.0090(8) 0.0006(8) N42 0.0179(9) 0.0132(9) 0.0189(10) 0.0003(8) 0.0063(8) 0.0011(8) C43 0.0184(11) 0.0183(12) 0.0213(12) 0.0021(10) 0.0052(10) 0.0028(10) C44 0.0226(12) 0.0199(12) 0.0258(13) 0.0078(10) 0.0098(11) 0.0068(10) C45 0.0269(13) 0.0128(11) 0.0281(13) 0.0046(10) 0.0127(11) 0.0035(10) N46 0.0178(9) 0.0126(9) 0.0161(9) -0.0021(8) 0.0059(8) -0.0005(8) N47 0.0203(10) 0.0132(9) 0.0165(9) -0.0004(8) 0.0077(8) -0.0013(8) C48 0.0186(11) 0.0196(12) 0.0156(11) -0.0024(9) 0.0063(9) -0.0009(9) C49 0.0204(11) 0.0219(12) 0.0165(11) -0.0018(10) 0.0068(10) 0.0038(10) C50 0.0175(11) 0.0165(11) 0.0204(11) -0.0052(9) 0.0065(10) 0.0014(9) N51 0.0179(9) 0.0134(9) 0.0162(9) 0.0010(8) 0.0076(8) -0.0008(8) N52 0.0172(9) 0.0117(9) 0.0181(9) 0.0001(8) 0.0067(8) 0.0002(7) C53 0.0179(11) 0.0165(11) 0.0179(11) 0.0013(9) 0.0067(9) 0.0030(9) C54 0.0155(11) 0.0243(13) 0.0214(12) 0.0031(10) 0.0085(10) 0.0012(10) C55 0.0183(11) 0.0188(12) 0.0171(11) 0.0017(9) 0.0059(9) -0.0030(9) B4 0.0130(11) 0.0185(13) 0.0158(12) 0.0010(10) 0.0046(10) -0.0007(10) N61 0.0144(9) 0.0173(10) 0.0188(10) 0.0009(8) 0.0076(8) 0.0012(8) N62 0.0159(9) 0.0147(9) 0.0192(10) -0.0017(8) 0.0061(8) -0.0001(8) C63 0.0230(12) 0.0173(12) 0.0253(13) -0.0009(10) 0.0130(11) 0.0026(10) C64 0.0250(13) 0.0203(12) 0.036(2) -0.0023(11) 0.0185(12) 0.0031(11) C65 0.0189(11) 0.0209(12) 0.0322(14) 0.0012(11) 0.0132(11) 0.0020(10) N66 0.0136(9) 0.0147(9) 0.0156(9) 0.0002(8) 0.0024(8) 0.0011(8) N67 0.0148(9) 0.0165(9) 0.0135(9) 0.0004(8) 0.0037(8) -0.0008(8) C68 0.0207(11) 0.0176(12) 0.0194(11) 0.0005(9) 0.0091(10) -0.0006(10) C69 0.0253(12) 0.0203(12) 0.0146(11) 0.0003(9) 0.0059(10) -0.0001(10) C70 0.0195(11) 0.0189(12) 0.0168(11) 0.0029(10) 0.0030(10) 0.0036(10) N71 0.0156(9) 0.0166(10) 0.0153(9) -0.0018(8) 0.0055(8) -0.0021(8) N72 0.0158(9) 0.0132(9) 0.0154(9) 0.0003(8) 0.0040(8) 0.0002(8) C73 0.0222(12) 0.0150(11) 0.0160(11) 0.0015(9) 0.0070(10) 0.0041(9) C74 0.0297(13) 0.0128(11) 0.0236(12) 0.0009(10) 0.0146(11) -0.0004(10) C75 0.0225(12) 0.0159(11) 0.0232(12) -0.0030(10) 0.0119(10) -0.0055(10) N80 0.0220(10) 0.0123(9) 0.0189(10) -0.0015(8) 0.0030(9) -0.0010(8) N81 0.0166(9) 0.0162(9) 0.0140(9) -0.0040(8) 0.0058(8) -0.0029(8) N82 0.0198(10) 0.0132(9) 0.0209(10) -0.0014(8) 0.0087(9) 0.0015(8) N90 0.0159(9) 0.0231(11) 0.0163(10) 0.0018(8) 0.0027(8) 0.0003(8) N91 0.0192(9) 0.0114(9) 0.0172(9) 0.0007(8) 0.0078(8) 0.0003(8) N92 0.0223(10) 0.0166(10) 0.0179(10) 0.0005(8) -0.0013(9) 0.0003(8) Cl1 0.108(3) 0.0331(12) 0.0457(11) -0.0025(9) 0.0254(13) -0.0203(13) Cl2 0.0625(13) 0.0487(13) 0.0363(12) 0.0162(10) 0.0240(11) 0.0133(12) Cl1X 0.205(8) 0.038(2) 0.044(2) 0.0037(13) 0.040(3) -0.015(3) Cl2X 0.189(7) 0.165(8) 0.174(6) 0.130(6) 0.160(6) 0.140(6) C90 0.075(3) 0.057(3) 0.035(2) -0.002(2) 0.015(2) 0.026(2) Cl3 0.0575(5) 0.0399(5) 0.0357(4) 0.0000(4) 0.0165(4) 0.0003(4) Cl4 0.0402(4) 0.0416(4) 0.0345(4) 0.0036(3) 0.0199(3) 0.0036(3) C100 0.047(2) 0.0274(15) 0.033(2) -0.0026(13) 0.0208(14) 0.0107(14) Cl5 0.0373(4) 0.0290(4) 0.0337(4) 0.0000(3) 0.0171(3) 0.0016(3) Cl6 0.0370(4) 0.0315(4) 0.0315(4) 0.0010(3) 0.0194(3) 0.0073(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 N80 2.423(2) . ? Tb1 N90 2.425(2) . ? Tb1 N32 2.458(2) . ? Tb1 N12 2.500(2) . ? Tb1 N22 2.507(2) . ? Tb1 N7 2.520(2) . ? Tb1 N27 2.534(2) . ? Tb1 N2 2.545(2) . ? Tb2 N92 2.414(2) . ? Tb2 N82 2.450(2) . ? Tb2 N47 2.454(2) . ? Tb2 N67 2.480(2) . ? Tb2 N52 2.492(2) . ? Tb2 N62 2.531(2) . ? Tb2 N72 2.533(2) . ? Tb2 N42 2.557(2) . ? N1 C5 1.347(3) . ? N1 N2 1.364(3) . ? N1 B1 1.538(3) . ? B1 N6 1.538(3) . ? B1 N11 1.546(3) . ? N2 C3 1.345(3) . ? C3 C4 1.388(3) . ? C4 C5 1.372(4) . ? N6 C10 1.350(3) . ? N6 N7 1.367(3) . ? N7 C8 1.339(3) . ? C8 C9 1.390(4) . ? C9 C10 1.376(4) . ? N11 C15 1.348(3) . ? N11 N12 1.363(3) . ? N12 C13 1.343(3) . ? C13 C14 1.393(3) . ? C14 C15 1.379(4) . ? B2 N21 1.535(4) . ? B2 N26 1.539(3) . ? B2 N31 1.542(3) . ? N21 C25 1.348(3) . ? N21 N22 1.368(3) . ? N22 C23 1.342(3) . ? C23 C24 1.393(4) . ? C24 C25 1.372(4) . ? N26 C30 1.340(3) . ? N26 N27 1.369(3) . ? N27 C28 1.341(3) . ? C28 C29 1.387(3) . ? C29 C30 1.378(4) . ? N31 C35 1.351(3) . ? N31 N32 1.364(3) . ? N32 C33 1.337(3) . ? C33 C34 1.396(3) . ? C34 C35 1.371(4) . ? B3 N46 1.542(3) . ? B3 N51 1.544(3) . ? B3 N41 1.545(3) . ? N41 C45 1.346(3) . ? N41 N42 1.362(3) . ? N42 C43 1.344(3) . ? C43 C44 1.389(4) . ? C44 C45 1.376(4) . ? N46 C50 1.348(3) . ? N46 N47 1.369(3) . ? N47 C48 1.341(3) . ? C48 C49 1.387(3) . ? C49 C50 1.377(4) . ? N51 C55 1.347(3) . ? N51 N52 1.370(3) . ? N52 C53 1.339(3) . ? C53 C54 1.393(3) . ? C54 C55 1.376(4) . ? B4 N71 1.533(3) . ? B4 N61 1.543(3) . ? B4 N66 1.549(3) . ? N61 C65 1.349(3) . ? N61 N62 1.367(3) . ? N62 C63 1.341(3) . ? C63 C64 1.388(4) . ? C64 C65 1.377(4) . ? N66 C70 1.342(3) . ? N66 N67 1.369(3) . ? N67 C68 1.326(3) . ? C68 C69 1.395(3) . ? C69 C70 1.376(4) . ? N71 C75 1.354(3) . ? N71 N72 1.372(3) . ? N72 C73 1.337(3) . ? C73 C74 1.398(3) . ? C74 C75 1.373(4) . ? N80 N81 1.169(3) . ? N81 N82 1.178(3) . ? N90 N91 1.171(3) 3_666 ? N91 N90 1.171(3) 3_666 ? N91 N92 1.174(3) . ? C80 Cl2 1.741(6) . ? C80 Cl1 1.769(5) . ? C80X Cl1X 1.742(6) . ? C80X Cl2X 1.763(6) . ? C90 Cl3 1.762(4) . ? C90 Cl4 1.764(4) . ? C100 Cl5 1.767(3) . ? C100 Cl6 1.768(3) . ? 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 N80 Tb1 N90 78.66(7) . . ? N80 Tb1 N32 140.69(7) . . ? N90 Tb1 N32 74.66(7) . . ? N80 Tb1 N12 73.83(7) . . ? N90 Tb1 N12 137.69(7) . . ? N32 Tb1 N12 143.34(7) . . ? N80 Tb1 N22 74.85(7) . . ? N90 Tb1 N22 78.91(7) . . ? N32 Tb1 N22 72.10(7) . . ? N12 Tb1 N22 122.43(6) . . ? N80 Tb1 N7 86.61(7) . . ? N90 Tb1 N7 73.90(7) . . ? N32 Tb1 N7 112.46(7) . . ? N12 Tb1 N7 72.98(6) . . ? N22 Tb1 N7 149.61(7) . . ? N80 Tb1 N27 111.38(7) . . ? N90 Tb1 N27 146.02(7) . . ? N32 Tb1 N27 78.59(6) . . ? N12 Tb1 N27 75.16(6) . . ? N22 Tb1 N27 73.16(6) . . ? N7 Tb1 N27 136.91(6) . . ? N80 Tb1 N2 146.20(7) . . ? N90 Tb1 N2 118.62(7) . . ? N32 Tb1 N2 72.96(7) . . ? N12 Tb1 N2 74.73(6) . . ? N22 Tb1 N2 134.15(7) . . ? N7 Tb1 N2 72.57(7) . . ? N27 Tb1 N2 71.59(6) . . ? N92 Tb2 N82 75.43(7) . . ? N92 Tb2 N47 73.32(7) . . ? N82 Tb2 N47 136.93(7) . . ? N92 Tb2 N67 138.75(7) . . ? N82 Tb2 N67 73.96(7) . . ? N47 Tb2 N67 146.18(7) . . ? N92 Tb2 N52 88.88(7) . . ? N82 Tb2 N52 75.91(7) . . ? N47 Tb2 N52 74.60(7) . . ? N67 Tb2 N52 109.47(7) . . ? N92 Tb2 N62 113.06(7) . . ? N82 Tb2 N62 144.09(7) . . ? N47 Tb2 N62 76.58(7) . . ? N67 Tb2 N62 79.01(7) . . ? N52 Tb2 N62 136.47(6) . . ? N92 Tb2 N72 75.11(7) . . ? N82 Tb2 N72 79.67(7) . . ? N47 Tb2 N72 118.96(7) . . ? N67 Tb2 N72 72.76(6) . . ? N52 Tb2 N72 153.52(6) . . ? N62 Tb2 N72 69.94(6) . . ? N92 Tb2 N42 147.72(7) . . ? N82 Tb2 N42 121.97(7) . . ? N47 Tb2 N42 76.64(6) . . ? N67 Tb2 N42 73.26(6) . . ? N52 Tb2 N42 71.84(6) . . ? N62 Tb2 N42 70.24(6) . . ? N72 Tb2 N42 131.37(6) . . ? C5 N1 N2 109.9(2) . . ? C5 N1 B1 128.6(2) . . ? N2 N1 B1 121.4(2) . . ? N1 B1 N6 110.2(2) . . ? N1 B1 N11 109.0(2) . . ? N6 B1 N11 109.0(2) . . ? C3 N2 N1 105.7(2) . . ? C3 N2 Tb1 129.2(2) . . ? N1 N2 Tb1 123.68(15) . . ? N2 C3 C4 111.0(2) . . ? C5 C4 C3 104.7(2) . . ? N1 C5 C4 108.8(2) . . ? C10 N6 N7 110.1(2) . . ? C10 N6 B1 127.5(2) . . ? N7 N6 B1 122.2(2) . . ? C8 N7 N6 105.6(2) . . ? C8 N7 Tb1 130.6(2) . . ? N6 N7 Tb1 123.69(14) . . ? N7 C8 C9 111.2(2) . . ? C10 C9 C8 104.8(2) . . ? N6 C10 C9 108.3(2) . . ? C15 N11 N12 109.8(2) . . ? C15 N11 B1 128.7(2) . . ? N12 N11 B1 121.5(2) . . ? C13 N12 N11 106.1(2) . . ? C13 N12 Tb1 129.1(2) . . ? N11 N12 Tb1 124.78(14) . . ? N12 C13 C14 110.9(2) . . ? C15 C14 C13 104.4(2) . . ? N11 C15 C14 108.8(2) . . ? N21 B2 N26 109.3(2) . . ? N21 B2 N31 109.7(2) . . ? N26 B2 N31 109.8(2) . . ? C25 N21 N22 109.6(2) . . ? C25 N21 B2 128.3(2) . . ? N22 N21 B2 122.1(2) . . ? C23 N22 N21 105.9(2) . . ? C23 N22 Tb1 131.6(2) . . ? N21 N22 Tb1 122.36(14) . . ? N22 C23 C24 110.9(2) . . ? C25 C24 C23 104.6(2) . . ? N21 C25 C24 109.0(2) . . ? C30 N26 N27 110.1(2) . . ? C30 N26 B2 127.9(2) . . ? N27 N26 B2 122.0(2) . . ? C28 N27 N26 105.4(2) . . ? C28 N27 Tb1 132.4(2) . . ? N26 N27 Tb1 121.72(14) . . ? N27 C28 C29 111.3(2) . . ? C30 C29 C28 104.5(2) . . ? N26 C30 C29 108.7(2) . . ? C35 N31 N32 109.6(2) . . ? C35 N31 B2 129.3(2) . . ? N32 N31 B2 121.0(2) . . ? C33 N32 N31 106.3(2) . . ? C33 N32 Tb1 128.5(2) . . ? N31 N32 Tb1 123.28(14) . . ? N32 C33 C34 110.6(2) . . ? C35 C34 C33 104.8(2) . . ? N31 C35 C34 108.6(2) . . ? N46 B3 N51 111.0(2) . . ? N46 B3 N41 109.6(2) . . ? N51 B3 N41 107.4(2) . . ? C45 N41 N42 110.4(2) . . ? C45 N41 B3 128.8(2) . . ? N42 N41 B3 120.8(2) . . ? C43 N42 N41 105.7(2) . . ? C43 N42 Tb2 131.0(2) . . ? N41 N42 Tb2 122.83(14) . . ? N42 C43 C44 110.7(2) . . ? C45 C44 C43 105.2(2) . . ? N41 C45 C44 108.1(2) . . ? C50 N46 N47 109.4(2) . . ? C50 N46 B3 128.5(2) . . ? N47 N46 B3 122.2(2) . . ? C48 N47 N46 106.1(2) . . ? C48 N47 Tb2 129.6(2) . . ? N46 N47 Tb2 124.02(14) . . ? N47 C48 C49 111.0(2) . . ? C50 C49 C48 104.6(2) . . ? N46 C50 C49 108.9(2) . . ? C55 N51 N52 110.3(2) . . ? C55 N51 B3 127.1(2) . . ? N52 N51 B3 122.5(2) . . ? C53 N52 N51 105.4(2) . . ? C53 N52 Tb2 131.3(2) . . ? N51 N52 Tb2 122.95(14) . . ? N52 C53 C54 111.2(2) . . ? C55 C54 C53 104.7(2) . . ? N51 C55 C54 108.4(2) . . ? N71 B4 N61 108.7(2) . . ? N71 B4 N66 109.6(2) . . ? N61 B4 N66 110.2(2) . . ? C65 N61 N62 109.9(2) . . ? C65 N61 B4 127.7(2) . . ? N62 N61 B4 122.3(2) . . ? C63 N62 N61 105.6(2) . . ? C63 N62 Tb2 130.2(2) . . ? N61 N62 Tb2 121.89(14) . . ? N62 C63 C64 111.3(2) . . ? C65 C64 C63 104.5(2) . . ? N61 C65 C64 108.6(2) . . ? C70 N66 N67 109.4(2) . . ? C70 N66 B4 129.9(2) . . ? N67 N66 B4 120.7(2) . . ? C68 N67 N66 106.4(2) . . ? C68 N67 Tb2 128.0(2) . . ? N66 N67 Tb2 124.31(15) . . ? N67 C68 C69 111.0(2) . . ? C70 C69 C68 104.3(2) . . ? N66 C70 C69 108.9(2) . . ? C75 N71 N72 109.3(2) . . ? C75 N71 B4 128.8(2) . . ? N72 N71 B4 121.7(2) . . ? C73 N72 N71 106.0(2) . . ? C73 N72 Tb2 131.1(2) . . ? N71 N72 Tb2 122.78(14) . . ? N72 C73 C74 111.2(2) . . ? C75 C74 C73 104.4(2) . . ? N71 C75 C74 109.0(2) . . ? N81 N80 Tb1 149.7(2) . . ? N80 N81 N82 178.6(2) . . ? N81 N82 Tb2 132.9(2) . . ? N91 N90 Tb1 146.5(2) 3_666 . ? N90 N91 N92 177.7(3) 3_666 . ? N91 N92 Tb2 145.9(2) . . ? Cl2 C80 Cl1 110.3(4) . . ? Cl1X C80X Cl2X 114.5(6) . . ? Cl3 C90 Cl4 112.5(2) . . ? Cl5 C100 Cl6 111.9(2) . . ? _refine_diff_density_max 1.004 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.137 #===END