Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_s92 _database_code_CSD 180509 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Amoroso, A. J.' 'Burrows, Miles W.' 'Gelbrich, Thomas' 'Haigh, Robert' 'Hursthouse, Michael B.' _publ_contact_author_name 'Dr A J Amoroso' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 UNITED KINGDOM ; _publ_contact_author_email 'AMOROSOAJ@CF.AC.UK' _publ_section_title ; The Oxidation and Subsequent Co-ordination Chemistries of Diphenylquaterpyridine ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H44 Gd N8 O8, 3(Cl O4)' _chemical_formula_sum 'C64 H44 Cl3 Gd N8 O20' _chemical_formula_weight 1508.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.783(3) _cell_length_b 19.408(4) _cell_length_c 19.979(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.93(3) _cell_angle_gamma 90.00 _cell_volume 6492(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.83 _exptl_crystal_description Prism _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3036 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 6 _diffrn_reflns_number 30729 _diffrn_reflns_av_R_equivalents 0.1208 _diffrn_reflns_av_sigmaI/netI 0.2039 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.83 _reflns_number_total 7535 _reflns_number_gt 3641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two unrefinable and disordered molecules of acetonitrile were removed using squeeze, ref: Spek, A.L. (1990), Acta Cryst. A46, C-34 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^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 'Calculated positions,riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7535 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1636 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.085 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.0000 0.25315(2) 0.2500 0.03124(16) Uani 1 2 d S . . Cl1 Cl 0.0000 -0.17933(12) 0.2500 0.0539(7) Uani 1 2 d S . . Cl2 Cl 0.27020(14) 0.00905(11) 0.31771(13) 0.0772(6) Uani 1 1 d . . . O1 O 0.0796(2) 0.23905(17) 0.15843(18) 0.0336(9) Uani 1 1 d . . . O5 O 0.0693(3) -0.1371(2) 0.2530(3) 0.0685(15) Uani 1 1 d . . . O2 O 0.0821(2) 0.15345(18) 0.26819(19) 0.0340(10) Uani 1 1 d . . . O6 O -0.0001(3) -0.2222(3) 0.3078(3) 0.0940(19) Uani 1 1 d . . . O3 O 0.0836(2) 0.35374(18) 0.24421(19) 0.0354(10) Uani 1 1 d . . . O4 O 0.0801(2) 0.26806(16) 0.35106(18) 0.0310(9) Uani 1 1 d . . . O7 O 0.3272(6) 0.0515(4) 0.3548(6) 0.218(5) Uani 1 1 d . . . O8 O 0.2673(5) -0.0525(3) 0.3550(4) 0.141(3) Uani 1 1 d . . . O9 O 0.2893(6) -0.0050(4) 0.2539(5) 0.181(4) Uani 1 1 d . . . O10 O 0.2026(4) 0.0465(4) 0.3132(4) 0.132(3) Uani 1 1 d . . . N1 N 0.1584(3) 0.2297(2) 0.1676(2) 0.0390(13) Uani 1 1 d . . . N2 N 0.0790(3) 0.1059(2) 0.2201(2) 0.0377(13) Uani 1 1 d . . . N3 N 0.0786(3) 0.4015(2) 0.2911(2) 0.0394(13) Uani 1 1 d . . . N4 N 0.1596(3) 0.2778(3) 0.3537(2) 0.0363(12) Uani 1 1 d . . . C1 C 0.2056(4) 0.2839(4) 0.1678(3) 0.0466(17) Uani 1 1 d . . . H1 H 0.1835 0.3276 0.1618 0.056 Uiso 1 1 calc R . . C2 C 0.2869(5) 0.2769(4) 0.1768(4) 0.068(2) Uani 1 1 d . . . H2 H 0.3197 0.3156 0.1788 0.082 Uiso 1 1 calc R . . C3 C 0.3188(5) 0.2125(4) 0.1829(4) 0.074(2) Uani 1 1 d . . . H3 H 0.3739 0.2069 0.1878 0.089 Uiso 1 1 calc R . . C4 C 0.2688(4) 0.1550(4) 0.1817(4) 0.061(2) Uani 1 1 d . . . H4 H 0.2898 0.1108 0.1862 0.073 Uiso 1 1 calc R . . C5 C 0.1879(4) 0.1655(3) 0.1736(3) 0.0438(17) Uani 1 1 d . . . C6 C 0.1319(4) 0.1081(3) 0.1708(3) 0.0380(15) Uani 1 1 d . . . C7 C 0.1285(4) 0.0587(3) 0.1223(3) 0.0441(17) Uani 1 1 d . . . H7 H 0.1644 0.0607 0.0889 0.053 Uiso 1 1 calc R . . C8 C 0.0730(4) 0.0052(3) 0.1211(3) 0.0423(17) Uani 1 1 d . . . C9 C 0.0230(4) 0.0036(3) 0.1737(3) 0.0395(16) Uani 1 1 d . . . H9 H -0.0135 -0.0322 0.1760 0.047 Uiso 1 1 calc R . . C10 C 0.0261(4) 0.0534(3) 0.2221(3) 0.0366(15) Uani 1 1 d . . . C11 C 0.0648(4) -0.0452(3) 0.0645(3) 0.0434(17) Uani 1 1 d . . . C12 C 0.0048(4) -0.0942(3) 0.0607(3) 0.056(2) Uani 1 1 d . . . H12 H -0.0295 -0.0975 0.0952 0.067 Uiso 1 1 calc R . . C13 C -0.0047(5) -0.1383(3) 0.0063(4) 0.065(2) Uani 1 1 d . . . H13 H -0.0472 -0.1692 0.0034 0.078 Uiso 1 1 calc R . . C14 C 0.0477(5) -0.1370(4) -0.0430(4) 0.066(2) Uani 1 1 d . . . H14 H 0.0428 -0.1683 -0.0783 0.079 Uiso 1 1 calc R . . C15 C 0.1079(5) -0.0887(4) -0.0396(4) 0.074(2) Uani 1 1 d . . . H15 H 0.1437 -0.0869 -0.0731 0.089 Uiso 1 1 calc R . . C16 C 0.1154(5) -0.0433(3) 0.0131(4) 0.063(2) Uani 1 1 d . . . H16 H 0.1557 -0.0104 0.0142 0.076 Uiso 1 1 calc R . . C17 C 0.0256(4) 0.4529(3) 0.2815(3) 0.0404(16) Uani 1 1 d . . . C18 C 0.0213(4) 0.5049(3) 0.3277(3) 0.0424(17) Uani 1 1 d . . . H18 H -0.0163 0.5397 0.3202 0.051 Uiso 1 1 calc R . . C19 C 0.0731(4) 0.5063(3) 0.3861(3) 0.0390(16) Uani 1 1 d . . . C20 C 0.1263(4) 0.4528(3) 0.3934(3) 0.0402(16) Uani 1 1 d . . . H20 H 0.1621 0.4521 0.4311 0.048 Uiso 1 1 calc R . . C21 C 0.1292(4) 0.3997(3) 0.3474(3) 0.0379(16) Uani 1 1 d . . . C22 C 0.1881(4) 0.3432(3) 0.3530(3) 0.0417(17) Uani 1 1 d . . . C23 C 0.2694(4) 0.3533(4) 0.3572(3) 0.0524(19) Uani 1 1 d . . . H23 H 0.2898 0.3978 0.3548 0.063 Uiso 1 1 calc R . . C24 C 0.3207(4) 0.2987(4) 0.3650(3) 0.0559(19) Uani 1 1 d . . . H24 H 0.3756 0.3056 0.3705 0.067 Uiso 1 1 calc R . . C25 C 0.2890(4) 0.2334(3) 0.3644(3) 0.0535(19) Uani 1 1 d . . . H25 H 0.3231 0.1956 0.3681 0.064 Uiso 1 1 calc R . . C26 C 0.2084(4) 0.2230(3) 0.3585(3) 0.0449(17) Uani 1 1 d . . . H26 H 0.1877 0.1785 0.3578 0.054 Uiso 1 1 calc R . . C27 C 0.0648(4) 0.5623(3) 0.4358(3) 0.0440(17) Uani 1 1 d . . . C28 C 0.0859(5) 0.5507(3) 0.5038(4) 0.061(2) Uani 1 1 d . . . H28 H 0.1091 0.5092 0.5182 0.073 Uiso 1 1 calc R . . C29 C 0.0713(5) 0.6029(4) 0.5497(4) 0.067(2) Uani 1 1 d . . . H29 H 0.0850 0.5961 0.5951 0.080 Uiso 1 1 calc R . . C30 C 0.0372(5) 0.6637(4) 0.5285(4) 0.071(2) Uani 1 1 d . . . H30 H 0.0278 0.6979 0.5596 0.086 Uiso 1 1 calc R . . C31 C 0.0169(5) 0.6746(4) 0.4620(4) 0.078(3) Uani 1 1 d . . . H31 H -0.0067 0.7160 0.4480 0.094 Uiso 1 1 calc R . . C32 C 0.0313(4) 0.6243(3) 0.4154(4) 0.0536(19) Uani 1 1 d . . . H32 H 0.0182 0.6323 0.3701 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0373(3) 0.0265(2) 0.0292(2) 0.000 -0.00337(16) 0.000 Cl1 0.0402(16) 0.0448(13) 0.076(2) 0.000 0.0023(13) 0.000 Cl2 0.0777(16) 0.0595(12) 0.0951(18) -0.0027(12) 0.0106(13) 0.0285(12) O1 0.030(2) 0.040(2) 0.031(2) -0.0015(18) 0.0018(16) -0.0072(19) O5 0.029(3) 0.055(3) 0.120(5) -0.004(3) -0.003(3) -0.001(2) O2 0.034(2) 0.030(2) 0.038(3) -0.0100(19) -0.0043(19) 0.0008(18) O6 0.087(4) 0.107(4) 0.092(5) 0.046(4) 0.031(3) 0.040(4) O3 0.046(3) 0.032(2) 0.028(2) -0.0030(19) -0.001(2) -0.0043(19) O4 0.033(2) 0.030(2) 0.030(2) 0.0003(16) -0.0045(17) -0.0016(17) O7 0.183(9) 0.121(7) 0.342(15) -0.034(8) -0.053(10) -0.024(7) O8 0.210(9) 0.075(4) 0.135(7) 0.024(4) 0.002(6) 0.045(5) O9 0.264(11) 0.126(7) 0.171(9) 0.007(6) 0.137(8) 0.053(7) O10 0.114(6) 0.158(6) 0.124(6) 0.015(5) 0.013(4) 0.096(5) N1 0.041(3) 0.045(3) 0.032(3) -0.012(2) 0.007(2) -0.011(3) N2 0.043(3) 0.035(3) 0.035(3) 0.002(2) -0.002(3) 0.002(3) N3 0.062(4) 0.027(3) 0.028(3) 0.001(2) -0.003(3) -0.010(3) N4 0.036(3) 0.043(3) 0.028(3) -0.001(2) -0.009(2) -0.001(3) C1 0.040(5) 0.049(4) 0.052(5) -0.010(3) 0.011(3) -0.006(4) C2 0.075(6) 0.054(5) 0.077(6) -0.013(4) 0.017(5) -0.016(5) C3 0.048(5) 0.083(6) 0.093(7) -0.032(5) 0.021(4) -0.017(5) C4 0.041(5) 0.055(5) 0.085(6) -0.020(4) 0.006(4) 0.006(4) C5 0.044(4) 0.046(4) 0.042(4) -0.013(3) 0.008(3) 0.008(4) C6 0.037(4) 0.036(3) 0.040(4) -0.009(3) -0.002(3) -0.001(3) C7 0.047(4) 0.046(4) 0.039(4) -0.010(3) 0.005(3) 0.015(3) C8 0.052(4) 0.028(3) 0.044(4) 0.000(3) -0.017(3) 0.007(3) C9 0.058(5) 0.029(3) 0.030(4) 0.002(3) -0.010(3) 0.005(3) C10 0.045(4) 0.027(3) 0.036(4) 0.003(3) -0.010(3) -0.001(3) C11 0.060(5) 0.034(3) 0.034(4) -0.003(3) -0.013(3) 0.014(3) C12 0.070(5) 0.046(4) 0.051(5) -0.019(4) -0.005(4) -0.003(4) C13 0.089(6) 0.040(4) 0.062(6) -0.016(4) -0.028(5) -0.007(4) C14 0.096(7) 0.045(4) 0.055(6) -0.022(4) -0.010(5) 0.012(5) C15 0.102(7) 0.078(5) 0.043(5) -0.015(4) 0.001(5) 0.015(5) C16 0.090(6) 0.058(4) 0.041(5) -0.013(4) -0.006(4) -0.007(4) C17 0.056(5) 0.028(3) 0.036(4) 0.005(3) -0.010(3) -0.001(3) C18 0.068(5) 0.029(3) 0.029(4) -0.001(3) -0.001(3) -0.001(3) C19 0.052(4) 0.027(3) 0.038(4) 0.000(3) -0.002(3) -0.013(3) C20 0.047(4) 0.040(4) 0.033(4) -0.003(3) -0.008(3) -0.012(3) C21 0.047(4) 0.036(3) 0.029(4) 0.003(3) -0.006(3) -0.008(3) C22 0.055(5) 0.037(4) 0.032(4) -0.003(3) -0.010(3) -0.006(3) C23 0.039(4) 0.058(4) 0.058(5) -0.009(4) -0.007(4) -0.017(4) C24 0.030(4) 0.077(5) 0.060(5) -0.009(4) -0.001(3) 0.001(4) C25 0.036(4) 0.065(5) 0.058(5) -0.007(3) -0.004(3) 0.019(4) C26 0.045(4) 0.040(3) 0.048(4) -0.008(3) -0.007(3) 0.007(3) C27 0.058(5) 0.042(4) 0.032(4) -0.007(3) 0.007(3) -0.010(3) C28 0.080(6) 0.051(4) 0.051(5) -0.009(4) 0.008(4) -0.015(4) C29 0.104(7) 0.064(5) 0.034(4) -0.015(4) 0.015(4) -0.030(5) C30 0.085(6) 0.062(5) 0.068(6) -0.029(4) 0.009(5) -0.005(5) C31 0.091(7) 0.069(5) 0.072(6) -0.037(5) -0.011(5) 0.020(5) C32 0.072(5) 0.042(4) 0.047(5) -0.015(3) 0.005(4) -0.004(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 O1 2.354(4) 2 ? Gd1 O1 2.354(4) . ? Gd1 O4 2.365(4) 2 ? Gd1 O4 2.365(4) . ? Gd1 O2 2.389(4) 2 ? Gd1 O2 2.389(4) . ? Gd1 O3 2.412(4) . ? Gd1 O3 2.412(4) 2 ? Cl1 O5 1.421(4) . ? Cl1 O5 1.421(4) 2 ? Cl1 O6 1.423(5) 2 ? Cl1 O6 1.423(5) . ? Cl2 O10 1.345(6) . ? Cl2 O9 1.363(8) . ? Cl2 O8 1.411(6) . ? Cl2 O7 1.430(9) . ? O1 N1 1.335(6) . ? O2 N2 1.330(6) . ? O3 N3 1.325(6) . ? O4 N4 1.345(6) . ? N1 C1 1.318(8) . ? N1 C5 1.343(7) . ? N2 C10 1.354(7) . ? N2 C6 1.371(8) . ? N3 C17 1.341(7) . ? N3 C21 1.363(7) . ? N4 C26 1.342(7) . ? N4 C22 1.359(7) . ? C1 C2 1.370(10) . ? C2 C3 1.362(10) . ? C3 C4 1.395(9) . ? C4 C5 1.372(9) . ? C5 C6 1.455(8) . ? C6 C7 1.361(8) . ? C7 C8 1.395(8) . ? C8 C9 1.390(9) . ? C8 C11 1.494(8) . ? C9 C10 1.365(8) . ? C10 C10 1.465(12) 2 ? C11 C16 1.378(10) . ? C11 C12 1.382(9) . ? C12 C13 1.385(9) . ? C13 C14 1.365(11) . ? C14 C15 1.378(10) . ? C15 C16 1.372(9) . ? C17 C18 1.372(8) . ? C17 C17 1.476(11) 2 ? C18 C19 1.407(8) . ? C19 C20 1.370(8) . ? C19 C27 1.486(8) . ? C20 C21 1.385(8) . ? C21 C22 1.475(8) . ? C22 C23 1.375(9) . ? C23 C24 1.368(9) . ? C24 C25 1.375(9) . ? C25 C26 1.364(9) . ? C27 C32 1.377(8) . ? C27 C28 1.399(9) . ? C28 C29 1.399(9) . ? C29 C30 1.366(10) . ? C30 C31 1.366(10) . ? C31 C32 1.382(9) . ? 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 O1 Gd1 O1 166.65(16) 2 . ? O1 Gd1 O4 110.99(13) 2 2 ? O1 Gd1 O4 70.75(13) . 2 ? O1 Gd1 O4 70.75(13) 2 . ? O1 Gd1 O4 110.99(13) . . ? O4 Gd1 O4 165.94(15) 2 . ? O1 Gd1 O2 70.84(13) 2 2 ? O1 Gd1 O2 98.04(13) . 2 ? O4 Gd1 O2 71.40(12) 2 2 ? O4 Gd1 O2 121.14(12) . 2 ? O1 Gd1 O2 98.04(13) 2 . ? O1 Gd1 O2 70.84(13) . . ? O4 Gd1 O2 121.14(12) 2 . ? O4 Gd1 O2 71.40(12) . . ? O2 Gd1 O2 71.83(17) 2 . ? O1 Gd1 O3 119.63(13) 2 . ? O1 Gd1 O3 72.17(12) . . ? O4 Gd1 O3 99.12(12) 2 . ? O4 Gd1 O3 69.11(12) . . ? O2 Gd1 O3 168.49(12) 2 . ? O2 Gd1 O3 109.35(13) . . ? O1 Gd1 O3 72.17(12) 2 2 ? O1 Gd1 O3 119.63(13) . 2 ? O4 Gd1 O3 69.11(12) 2 2 ? O4 Gd1 O3 99.12(12) . 2 ? O2 Gd1 O3 109.35(13) 2 2 ? O2 Gd1 O3 168.49(12) . 2 ? O3 Gd1 O3 71.90(19) . 2 ? O5 Cl1 O5 109.5(4) . 2 ? O5 Cl1 O6 109.0(3) . 2 ? O5 Cl1 O6 110.5(3) 2 2 ? O5 Cl1 O6 110.5(3) . . ? O5 Cl1 O6 109.0(3) 2 . ? O6 Cl1 O6 108.4(5) 2 . ? O10 Cl2 O9 107.2(5) . . ? O10 Cl2 O8 115.7(5) . . ? O9 Cl2 O8 110.1(5) . . ? O10 Cl2 O7 104.8(5) . . ? O9 Cl2 O7 114.1(7) . . ? O8 Cl2 O7 105.1(6) . . ? N1 O1 Gd1 121.2(3) . . ? N2 O2 Gd1 117.3(3) . . ? N3 O3 Gd1 117.9(3) . . ? N4 O4 Gd1 123.7(3) . . ? C1 N1 O1 118.8(5) . . ? C1 N1 C5 121.5(6) . . ? O1 N1 C5 119.6(5) . . ? O2 N2 C10 119.6(5) . . ? O2 N2 C6 120.1(5) . . ? C10 N2 C6 120.2(5) . . ? O3 N3 C17 119.6(5) . . ? O3 N3 C21 119.9(5) . . ? C17 N3 C21 120.4(5) . . ? C26 N4 O4 119.5(5) . . ? C26 N4 C22 121.8(5) . . ? O4 N4 C22 118.7(5) . . ? N1 C1 C2 121.0(7) . . ? C3 C2 C1 119.0(7) . . ? C2 C3 C4 120.0(7) . . ? C5 C4 C3 118.2(7) . . ? N1 C5 C4 120.2(6) . . ? N1 C5 C6 118.2(6) . . ? C4 C5 C6 121.6(6) . . ? C7 C6 N2 119.5(6) . . ? C7 C6 C5 124.2(6) . . ? N2 C6 C5 116.4(5) . . ? C6 C7 C8 122.1(6) . . ? C9 C8 C7 116.2(6) . . ? C9 C8 C11 121.9(6) . . ? C7 C8 C11 121.8(6) . . ? C10 C9 C8 121.6(6) . . ? N2 C10 C9 120.4(6) . . ? N2 C10 C10 116.8(4) . 2 ? C9 C10 C10 122.8(5) . 2 ? C16 C11 C12 117.5(6) . . ? C16 C11 C8 121.1(6) . . ? C12 C11 C8 121.4(7) . . ? C11 C12 C13 120.9(8) . . ? C14 C13 C12 120.6(8) . . ? C13 C14 C15 119.0(7) . . ? C16 C15 C14 120.2(8) . . ? C15 C16 C11 121.8(8) . . ? N3 C17 C18 121.1(5) . . ? N3 C17 C17 117.6(5) . 2 ? C18 C17 C17 121.3(5) . 2 ? C17 C18 C19 120.9(6) . . ? C20 C19 C18 115.8(5) . . ? C20 C19 C27 125.0(6) . . ? C18 C19 C27 119.2(6) . . ? C19 C20 C21 123.1(5) . . ? N3 C21 C20 118.7(5) . . ? N3 C21 C22 117.3(5) . . ? C20 C21 C22 123.8(5) . . ? N4 C22 C23 118.8(6) . . ? N4 C22 C21 117.4(6) . . ? C23 C22 C21 123.8(6) . . ? C24 C23 C22 120.7(6) . . ? C23 C24 C25 118.3(6) . . ? C26 C25 C24 121.2(6) . . ? N4 C26 C25 119.1(6) . . ? C32 C27 C28 120.0(6) . . ? C32 C27 C19 119.8(6) . . ? C28 C27 C19 120.1(6) . . ? C29 C28 C27 118.4(7) . . ? C30 C29 C28 120.7(7) . . ? C31 C30 C29 120.5(7) . . ? C30 C31 C32 120.1(7) . . ? C27 C32 C31 120.3(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Gd1 O1 N1 -84.9(3) 2 . . . ? O4 Gd1 O1 N1 175.3(4) 2 . . . ? O4 Gd1 O1 N1 10.1(4) . . . . ? O2 Gd1 O1 N1 -117.7(3) 2 . . . ? O2 Gd1 O1 N1 -50.2(3) . . . . ? O3 Gd1 O1 N1 68.5(3) . . . . ? O3 Gd1 O1 N1 124.6(3) 2 . . . ? O1 Gd1 O2 N2 118.5(4) 2 . . . ? O1 Gd1 O2 N2 -53.9(4) . . . . ? O4 Gd1 O2 N2 -2.0(4) 2 . . . ? O4 Gd1 O2 N2 -175.0(4) . . . . ? O2 Gd1 O2 N2 51.8(3) 2 . . . ? O3 Gd1 O2 N2 -116.1(4) . . . . ? O3 Gd1 O2 N2 149.6(6) 2 . . . ? O1 Gd1 O3 N3 -4.5(4) 2 . . . ? O1 Gd1 O3 N3 -177.7(4) . . . . ? O4 Gd1 O3 N3 116.1(3) 2 . . . ? O4 Gd1 O3 N3 -56.0(3) . . . . ? O2 Gd1 O3 N3 149.8(6) 2 . . . ? O2 Gd1 O3 N3 -116.3(3) . . . . ? O3 Gd1 O3 N3 51.7(3) 2 . . . ? O1 Gd1 O4 N4 175.4(4) 2 . . . ? O1 Gd1 O4 N4 9.5(4) . . . . ? O4 Gd1 O4 N4 -85.0(3) 2 . . . ? O2 Gd1 O4 N4 123.5(3) 2 . . . ? O2 Gd1 O4 N4 69.5(3) . . . . ? O3 Gd1 O4 N4 -50.7(3) . . . . ? O3 Gd1 O4 N4 -117.2(3) 2 . . . ? Gd1 O1 N1 C1 -92.2(5) . . . . ? Gd1 O1 N1 C5 90.5(5) . . . . ? Gd1 O2 N2 C10 -91.1(5) . . . . ? Gd1 O2 N2 C6 92.2(5) . . . . ? Gd1 O3 N3 C17 -89.6(5) . . . . ? Gd1 O3 N3 C21 92.9(5) . . . . ? Gd1 O4 N4 C26 -90.0(5) . . . . ? Gd1 O4 N4 C22 91.5(5) . . . . ? O1 N1 C1 C2 -179.8(6) . . . . ? C5 N1 C1 C2 -2.6(9) . . . . ? N1 C1 C2 C3 2.7(11) . . . . ? C1 C2 C3 C4 -1.7(12) . . . . ? C2 C3 C4 C5 0.6(11) . . . . ? C1 N1 C5 C4 1.4(9) . . . . ? O1 N1 C5 C4 178.6(5) . . . . ? C1 N1 C5 C6 -178.0(6) . . . . ? O1 N1 C5 C6 -0.8(8) . . . . ? C3 C4 C5 N1 -0.4(10) . . . . ? C3 C4 C5 C6 179.0(6) . . . . ? O2 N2 C6 C7 179.3(5) . . . . ? C10 N2 C6 C7 2.6(8) . . . . ? O2 N2 C6 C5 -1.8(8) . . . . ? C10 N2 C6 C5 -178.4(5) . . . . ? N1 C5 C6 C7 116.7(7) . . . . ? C4 C5 C6 C7 -62.8(9) . . . . ? N1 C5 C6 N2 -62.2(8) . . . . ? C4 C5 C6 N2 118.3(7) . . . . ? N2 C6 C7 C8 -0.3(9) . . . . ? C5 C6 C7 C8 -179.1(6) . . . . ? C6 C7 C8 C9 -2.3(9) . . . . ? C6 C7 C8 C11 174.4(5) . . . . ? C7 C8 C9 C10 2.6(8) . . . . ? C11 C8 C9 C10 -174.1(5) . . . . ? O2 N2 C10 C9 -179.0(5) . . . . ? C6 N2 C10 C9 -2.3(8) . . . . ? O2 N2 C10 C10 1.0(8) . . . 2 ? C6 N2 C10 C10 177.7(6) . . . 2 ? C8 C9 C10 N2 -0.4(9) . . . . ? C8 C9 C10 C10 179.6(6) . . . 2 ? C9 C8 C11 C16 -179.3(6) . . . . ? C7 C8 C11 C16 4.1(9) . . . . ? C9 C8 C11 C12 2.5(9) . . . . ? C7 C8 C11 C12 -174.0(6) . . . . ? C16 C11 C12 C13 -1.6(10) . . . . ? C8 C11 C12 C13 176.7(6) . . . . ? C11 C12 C13 C14 3.7(11) . . . . ? C12 C13 C14 C15 -3.3(11) . . . . ? C13 C14 C15 C16 0.8(11) . . . . ? C14 C15 C16 C11 1.3(11) . . . . ? C12 C11 C16 C15 -0.9(10) . . . . ? C8 C11 C16 C15 -179.2(6) . . . . ? O3 N3 C17 C18 -177.0(5) . . . . ? C21 N3 C17 C18 0.5(9) . . . . ? O3 N3 C17 C17 0.5(9) . . . 2 ? C21 N3 C17 C17 178.0(6) . . . 2 ? N3 C17 C18 C19 0.7(10) . . . . ? C17 C17 C18 C19 -176.7(7) 2 . . . ? C17 C18 C19 C20 -0.5(9) . . . . ? C17 C18 C19 C27 -178.0(6) . . . . ? C18 C19 C20 C21 -0.8(9) . . . . ? C27 C19 C20 C21 176.5(6) . . . . ? O3 N3 C21 C20 175.7(5) . . . . ? C17 N3 C21 C20 -1.8(9) . . . . ? O3 N3 C21 C22 0.0(8) . . . . ? C17 N3 C21 C22 -177.5(5) . . . . ? C19 C20 C21 N3 1.9(9) . . . . ? C19 C20 C21 C22 177.4(6) . . . . ? C26 N4 C22 C23 0.0(9) . . . . ? O4 N4 C22 C23 178.5(5) . . . . ? C26 N4 C22 C21 179.8(5) . . . . ? O4 N4 C22 C21 -1.6(8) . . . . ? N3 C21 C22 N4 -61.3(8) . . . . ? C20 C21 C22 N4 123.2(6) . . . . ? N3 C21 C22 C23 118.5(7) . . . . ? C20 C21 C22 C23 -57.0(9) . . . . ? N4 C22 C23 C24 -2.8(10) . . . . ? C21 C22 C23 C24 177.4(6) . . . . ? C22 C23 C24 C25 3.8(10) . . . . ? C23 C24 C25 C26 -2.1(10) . . . . ? O4 N4 C26 C25 -176.9(5) . . . . ? C22 N4 C26 C25 1.7(9) . . . . ? C24 C25 C26 N4 -0.6(10) . . . . ? C20 C19 C27 C32 157.8(6) . . . . ? C18 C19 C27 C32 -25.0(9) . . . . ? C20 C19 C27 C28 -26.5(10) . . . . ? C18 C19 C27 C28 150.7(6) . . . . ? C32 C27 C28 C29 0.7(10) . . . . ? C19 C27 C28 C29 -175.0(6) . . . . ? C27 C28 C29 C30 0.0(11) . . . . ? C28 C29 C30 C31 -0.1(13) . . . . ? C29 C30 C31 C32 -0.5(13) . . . . ? C28 C27 C32 C31 -1.3(11) . . . . ? C19 C27 C32 C31 174.4(7) . . . . ? C30 C31 C32 C27 1.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.650 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.118 data_s92 _database_code_CSD 178771 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Amoroso, A. J.' 'Burrows, Miles W.' 'Gelbrich, Thomas' 'Haigh, Robert' 'Hursthouse, Michael B.' _publ_contact_author_name 'Dr A J Amoroso' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 UNITED KINGDOM ; _publ_contact_author_email 'AMOROSOAJ@CF.AC.UK' _publ_section_title ; The Oxidation and Subsequent Co-ordination Chemistries of Diphenylquaterpyridine ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H50 Cl3 N10 O16 Tb' _chemical_formula_weight 1528.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 15.3287(5) _cell_length_b 15.4120(6) _cell_length_c 17.7298(10) _cell_angle_alpha 69.9040(15) _cell_angle_beta 65.6000(16) _cell_angle_gamma 66.882(2) _cell_volume 3424.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8377 _exptl_absorpt_correction_T_max 0.9527 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23857 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.2098 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11870 _reflns_number_gt 6655 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0007P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11870 _refine_ls_number_parameters 884 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.25615(3) 0.22879(3) 0.27328(3) 0.02292(14) Uani 1 1 d . . . O1' O 0.1741(4) 0.3130(4) 0.3801(3) 0.0278(14) Uani 1 1 d . . . O2' O 0.3172(4) 0.0893(3) 0.2253(3) 0.0242(13) Uani 1 1 d . . . N1' N 0.1087(5) 0.4010(5) 0.3675(4) 0.0259(17) Uani 1 1 d . . . N2' N 0.2953(4) 0.3903(4) 0.2191(4) 0.0207(15) Uani 1 1 d . . . N3' N 0.3757(5) 0.2551(4) 0.1268(4) 0.0250(16) Uani 1 1 d . . . N4' N 0.3024(4) 0.0908(4) 0.1555(4) 0.0227(16) Uani 1 1 d . . . O1 O 0.4007(4) 0.1950(4) 0.3002(3) 0.0287(14) Uani 1 1 d . . . O2 O 0.1600(4) 0.2958(4) 0.1883(3) 0.0340(15) Uani 1 1 d . . . N1 N 0.3944(4) 0.2088(4) 0.3725(4) 0.0248(16) Uani 1 1 d . . . N2 N 0.2545(4) 0.0980(4) 0.4083(4) 0.0233(16) Uani 1 1 d . . . N3 N 0.1071(4) 0.1595(4) 0.3392(4) 0.0217(16) Uani 1 1 d . . . N4 N 0.0616(5) 0.3438(5) 0.2146(4) 0.0279(17) Uani 1 1 d . . . C1 C 0.4309(5) 0.2794(6) 0.3673(5) 0.032(2) Uani 1 1 d . . . H1 H 0.4616 0.3143 0.3131 0.038 Uiso 1 1 calc R . . C2 C 0.4236(6) 0.3007(6) 0.4400(5) 0.034(2) Uani 1 1 d . . . H2 H 0.4464 0.3519 0.4356 0.041 Uiso 1 1 calc R . . C3 C 0.3831(5) 0.2474(6) 0.5188(5) 0.033(2) Uani 1 1 d . . . H3 H 0.3784 0.2603 0.5693 0.039 Uiso 1 1 calc R . . C4 C 0.3501(5) 0.1755(6) 0.5216(5) 0.026(2) Uani 1 1 d . . . H4 H 0.3228 0.1378 0.5755 0.032 Uiso 1 1 calc R . . C5 C 0.3543(5) 0.1552(5) 0.4507(5) 0.0211(19) Uani 1 1 d . . . C6 C 0.3135(5) 0.0790(5) 0.4552(5) 0.0213(19) Uani 1 1 d . . . C7 C 0.3305(6) -0.0072(5) 0.5142(5) 0.026(2) Uani 1 1 d . . . H7 H 0.3722 -0.0184 0.5460 0.031 Uiso 1 1 calc R . . C8 C 0.2872(6) -0.0765(6) 0.5270(5) 0.026(2) Uani 1 1 d . . . C9 C 0.2240(5) -0.0545(6) 0.4792(5) 0.026(2) Uani 1 1 d . . . H9 H 0.1923 -0.0999 0.4860 0.031 Uiso 1 1 calc R . . C10 C 0.2085(5) 0.0330(5) 0.4228(5) 0.0217(19) Uani 1 1 d . . . C11 C 0.1307(5) 0.0645(6) 0.3797(4) 0.024(2) Uani 1 1 d . . . C12 C 0.0851(5) 0.0007(5) 0.3827(4) 0.0196(19) Uani 1 1 d . . . H12 H 0.1055 -0.0654 0.4097 0.023 Uiso 1 1 calc R . . C13 C 0.0100(5) 0.0328(6) 0.3465(4) 0.0230(19) Uani 1 1 d . . . C14 C -0.0186(5) 0.1304(5) 0.3104(4) 0.0201(19) Uani 1 1 d . . . H14 H -0.0717 0.1559 0.2872 0.024 Uiso 1 1 calc R . . C15 C 0.0305(6) 0.1914(6) 0.3080(5) 0.024(2) Uani 1 1 d . . . C16 C -0.0055(6) 0.2955(6) 0.2719(5) 0.026(2) Uani 1 1 d . . . C17 C -0.1045(6) 0.3462(6) 0.2923(5) 0.033(2) Uani 1 1 d . . . H17 H -0.1527 0.3139 0.3313 0.040 Uiso 1 1 calc R . . C18 C -0.1365(6) 0.4437(6) 0.2573(5) 0.043(3) Uani 1 1 d . . . H18 H -0.2057 0.4786 0.2729 0.052 Uiso 1 1 calc R . . C19 C -0.0657(7) 0.4889(6) 0.1994(6) 0.047(3) Uani 1 1 d . . . H19 H -0.0858 0.5556 0.1739 0.056 Uiso 1 1 calc R . . C20 C 0.0339(7) 0.4373(7) 0.1786(6) 0.044(3) Uani 1 1 d . . . H20 H 0.0829 0.4682 0.1387 0.052 Uiso 1 1 calc R . . C21 C 0.3060(5) -0.1709(6) 0.5884(5) 0.030(2) Uani 1 1 d . . . C22 C 0.2964(5) -0.1695(6) 0.6706(5) 0.032(2) Uani 1 1 d . . . H22 H 0.2808 -0.1103 0.6855 0.038 Uiso 1 1 calc R . . C23 C 0.3101(6) -0.2572(7) 0.7299(5) 0.041(2) Uani 1 1 d . . . H23 H 0.3009 -0.2571 0.7862 0.050 Uiso 1 1 calc R . . C24 C 0.3361(6) -0.3417(7) 0.7081(6) 0.044(3) Uani 1 1 d . . . H24 H 0.3463 -0.4002 0.7493 0.053 Uiso 1 1 calc R . . C25 C 0.3483(6) -0.3455(6) 0.6271(6) 0.037(2) Uani 1 1 d . . . H25 H 0.3682 -0.4055 0.6118 0.044 Uiso 1 1 calc R . . C26 C 0.3301(5) -0.2573(6) 0.5686(5) 0.034(2) Uani 1 1 d . . . H26 H 0.3347 -0.2578 0.5136 0.040 Uiso 1 1 calc R . . C27 C -0.0340(5) -0.0340(5) 0.3410(5) 0.025(2) Uani 1 1 d . . . C28 C -0.0679(5) -0.0114(6) 0.2730(5) 0.030(2) Uani 1 1 d . . . H28 H -0.0612 0.0454 0.2303 0.036 Uiso 1 1 calc R . . C29 C -0.1122(6) -0.0723(6) 0.2671(5) 0.035(2) Uani 1 1 d . . . H29 H -0.1345 -0.0573 0.2202 0.042 Uiso 1 1 calc R . . C30 C -0.1230(5) -0.1551(6) 0.3308(5) 0.032(2) Uani 1 1 d . . . H30 H -0.1531 -0.1963 0.3273 0.039 Uiso 1 1 calc R . . C31 C -0.0896(5) -0.1776(5) 0.3998(5) 0.026(2) Uani 1 1 d . . . H31 H -0.0978 -0.2335 0.4434 0.031 Uiso 1 1 calc R . . C32 C -0.0445(5) -0.1174(6) 0.4040(5) 0.026(2) Uani 1 1 d . . . H32 H -0.0206 -0.1333 0.4501 0.031 Uiso 1 1 calc R . . C1' C 0.0110(6) 0.4133(7) 0.4126(5) 0.039(2) Uani 1 1 d . . . H1' H -0.0098 0.3595 0.4521 0.046 Uiso 1 1 calc R . . C2' C -0.0590(6) 0.5007(7) 0.4029(5) 0.043(2) Uani 1 1 d . . . H2' H -0.1278 0.5079 0.4349 0.051 Uiso 1 1 calc R . . C3' C -0.0284(6) 0.5789(6) 0.3460(6) 0.042(2) Uani 1 1 d . . . H3' H -0.0761 0.6402 0.3372 0.051 Uiso 1 1 calc R . . C4' C 0.0728(6) 0.5667(6) 0.3018(5) 0.035(2) Uani 1 1 d . . . H4' H 0.0948 0.6207 0.2643 0.042 Uiso 1 1 calc R . . C5' C 0.1413(6) 0.4775(5) 0.3120(5) 0.026(2) Uani 1 1 d . . . C6' C 0.2506(6) 0.4608(5) 0.2635(5) 0.0219(19) Uani 1 1 d . . . C7' C 0.2983(6) 0.5189(5) 0.2652(5) 0.026(2) Uani 1 1 d . . . H7' H 0.2629 0.5677 0.2973 0.032 Uiso 1 1 calc R . . C8' C 0.4020(6) 0.5043(6) 0.2178(5) 0.029(2) Uani 1 1 d . . . C9' C 0.4442(6) 0.4391(6) 0.1655(5) 0.023(2) Uani 1 1 d . . . H9' H 0.5113 0.4319 0.1285 0.028 Uiso 1 1 calc R . . C10' C 0.3910(6) 0.3842(5) 0.1659(4) 0.023(2) Uani 1 1 d . . . C11' C 0.4333(6) 0.3151(5) 0.1111(5) 0.026(2) Uani 1 1 d . . . C12' C 0.5233(6) 0.3107(6) 0.0439(4) 0.025(2) Uani 1 1 d . . . H12' H 0.5610 0.3519 0.0343 0.030 Uiso 1 1 calc R . . C13' C 0.5583(5) 0.2480(5) -0.0085(4) 0.0225(19) Uani 1 1 d . . . C14' C 0.4970(6) 0.1927(6) 0.0029(5) 0.028(2) Uani 1 1 d . . . H14' H 0.5160 0.1512 -0.0338 0.034 Uiso 1 1 calc R . . C15' C 0.4061(6) 0.2020(6) 0.0715(5) 0.024(2) Uani 1 1 d . . . C16' C 0.3422(5) 0.1446(6) 0.0792(5) 0.026(2) Uani 1 1 d . . . C17' C 0.3232(6) 0.1456(6) 0.0099(5) 0.030(2) Uani 1 1 d . . . H17' H 0.3497 0.1843 -0.0435 0.036 Uiso 1 1 calc R . . C18' C 0.2657(6) 0.0910(6) 0.0166(5) 0.031(2) Uani 1 1 d . . . H18' H 0.2510 0.0936 -0.0313 0.037 Uiso 1 1 calc R . . C19' C 0.2304(6) 0.0331(6) 0.0938(5) 0.031(2) Uani 1 1 d . . . H19' H 0.1939 -0.0077 0.0995 0.037 Uiso 1 1 calc R . . C20' C 0.2487(6) 0.0352(5) 0.1620(5) 0.028(2) Uani 1 1 d . . . H20' H 0.2231 -0.0036 0.2157 0.034 Uiso 1 1 calc R . . C21' C 0.4609(6) 0.5529(5) 0.2290(5) 0.027(2) Uani 1 1 d . . . C22' C 0.4382(6) 0.5718(5) 0.3069(5) 0.030(2) Uani 1 1 d . . . H22' H 0.3814 0.5575 0.3521 0.036 Uiso 1 1 calc R . . C23' C 0.4959(6) 0.6108(6) 0.3208(6) 0.043(2) Uani 1 1 d . . . H23' H 0.4786 0.6237 0.3747 0.052 Uiso 1 1 calc R . . C24' C 0.5778(6) 0.6307(6) 0.2563(6) 0.042(2) Uani 1 1 d . . . H24' H 0.6187 0.6560 0.2660 0.050 Uiso 1 1 calc R . . C25' C 0.6023(6) 0.6147(6) 0.1777(6) 0.032(2) Uani 1 1 d . . . H25' H 0.6586 0.6307 0.1328 0.039 Uiso 1 1 calc R . . C26' C 0.5431(6) 0.5742(5) 0.1638(5) 0.029(2) Uani 1 1 d . . . H26' H 0.5601 0.5619 0.1098 0.034 Uiso 1 1 calc R . . C27' C 0.6581(6) 0.2380(5) -0.0783(5) 0.025(2) Uani 1 1 d . . . C28' C 0.7395(6) 0.2398(6) -0.0635(5) 0.041(2) Uani 1 1 d . . . H28' H 0.7327 0.2491 -0.0109 0.049 Uiso 1 1 calc R . . C29' C 0.8315(6) 0.2275(7) -0.1283(6) 0.050(3) Uani 1 1 d . . . H29' H 0.8873 0.2306 -0.1197 0.060 Uiso 1 1 calc R . . C30' C 0.8440(7) 0.2114(6) -0.2021(6) 0.046(3) Uani 1 1 d . . . H30' H 0.9078 0.2025 -0.2447 0.055 Uiso 1 1 calc R . . C31' C 0.7627(6) 0.2078(5) -0.2159(5) 0.037(2) Uani 1 1 d . . . H31' H 0.7706 0.1975 -0.2685 0.044 Uiso 1 1 calc R . . C32' C 0.6693(6) 0.2192(5) -0.1525(5) 0.032(2) Uani 1 1 d . . . H32' H 0.6143 0.2139 -0.1606 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.75189(19) 0.44878(19) 0.99525(16) 0.0560(8) Uani 1 1 d . . . O10 O 0.7547(6) 0.3750(6) 1.0671(5) 0.111(3) Uani 1 1 d . . . O11 O 0.7568(6) 0.5348(6) 0.9999(5) 0.110(3) Uani 1 1 d . . . O12 O 0.8283(5) 0.4171(5) 0.9209(4) 0.076(2) Uani 1 1 d . . . O13 O 0.6537(5) 0.4706(5) 0.9867(4) 0.077(2) Uani 1 1 d . . . Cl2 Cl 0.80451(16) 0.30186(15) 0.53830(13) 0.0330(6) Uani 1 1 d . . . O20 O 0.7491(4) 0.3859(4) 0.4915(3) 0.0433(16) Uani 1 1 d . . . O21 O 0.8865(4) 0.2444(4) 0.4804(3) 0.0409(16) Uani 1 1 d . . . O22 O 0.7389(4) 0.2436(4) 0.5975(3) 0.0437(17) Uani 1 1 d . . . O23 O 0.8434(4) 0.3300(4) 0.5851(3) 0.0385(16) Uani 1 1 d . . . Cl3 Cl 0.21022(17) 0.24198(17) 0.79629(16) 0.0441(6) Uani 1 1 d . . . O30 O 0.1053(4) 0.2628(5) 0.8161(4) 0.0588(19) Uani 1 1 d . . . O31 O 0.2497(5) 0.2860(7) 0.7117(4) 0.102(3) Uani 1 1 d . . . O32 O 0.2526(7) 0.1401(6) 0.8109(7) 0.138(4) Uani 1 1 d . . . O33 O 0.2290(4) 0.2778(4) 0.8506(4) 0.0523(18) Uani 1 1 d . . . N1S N 0.5142(6) 0.0878(6) 0.8529(6) 0.058(2) Uani 1 1 d . . . C1S C 0.5380(7) 0.1295(7) 0.6918(5) 0.052(3) Uani 1 1 d . . . H1S1 H 0.5840 0.1691 0.6607 0.079 Uiso 1 1 calc R . . H1S2 H 0.4735 0.1648 0.6819 0.079 Uiso 1 1 calc R . . H1S3 H 0.5665 0.0690 0.6720 0.079 Uiso 1 1 calc R . . C2S C 0.5230(6) 0.1076(7) 0.7833(7) 0.039(3) Uani 1 1 d . . . N2S N 0.5763(6) 0.0121(6) 0.3401(5) 0.050(2) Uani 1 1 d . . . C3S C 0.6170(7) 0.0709(7) 0.1787(6) 0.059(3) Uani 1 1 d . . . H3S1 H 0.5871 0.0407 0.1590 0.088 Uiso 1 1 calc R . . H3S2 H 0.6898 0.0530 0.1508 0.088 Uiso 1 1 calc R . . H3S3 H 0.5890 0.1413 0.1648 0.088 Uiso 1 1 calc R . . C4S C 0.5952(6) 0.0378(6) 0.2695(7) 0.037(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0237(2) 0.0190(2) 0.0231(2) -0.00422(17) -0.00459(17) -0.00674(19) O1' 0.030(3) 0.016(3) 0.029(3) -0.011(3) 0.000(3) -0.003(3) O2' 0.036(3) 0.017(3) 0.018(3) -0.004(2) -0.010(3) -0.005(3) N1' 0.023(4) 0.025(4) 0.025(4) -0.011(3) 0.001(3) -0.006(4) N2' 0.021(4) 0.013(4) 0.023(4) -0.004(3) -0.002(3) -0.005(3) N3' 0.040(4) 0.006(4) 0.011(4) -0.002(3) -0.006(3) 0.010(3) N4' 0.026(4) 0.011(4) 0.023(4) -0.008(3) -0.005(3) 0.003(3) O1 0.028(3) 0.031(4) 0.023(3) -0.008(3) -0.005(3) -0.007(3) O2 0.022(3) 0.033(4) 0.035(4) 0.003(3) -0.011(3) -0.003(3) N1 0.017(4) 0.017(4) 0.036(5) -0.003(3) -0.011(3) 0.000(3) N2 0.016(4) 0.022(4) 0.021(4) -0.007(3) -0.003(3) 0.005(3) N3 0.023(4) 0.010(4) 0.022(4) -0.002(3) 0.000(3) -0.004(3) N4 0.037(5) 0.012(4) 0.035(4) 0.003(3) -0.018(4) -0.008(4) C1 0.019(5) 0.026(5) 0.044(6) -0.008(4) -0.003(4) -0.007(4) C2 0.027(5) 0.032(6) 0.049(6) -0.003(5) -0.014(4) -0.018(5) C3 0.030(5) 0.045(6) 0.032(5) -0.008(5) -0.013(4) -0.017(5) C4 0.018(5) 0.028(5) 0.027(5) -0.008(4) -0.005(4) -0.002(4) C5 0.011(4) 0.011(4) 0.029(5) 0.002(4) -0.007(4) 0.004(4) C6 0.017(4) 0.022(5) 0.023(5) -0.010(4) 0.000(4) -0.007(4) C7 0.031(5) 0.018(5) 0.024(5) -0.002(4) -0.013(4) 0.000(4) C8 0.023(5) 0.028(5) 0.019(5) -0.006(4) 0.001(4) -0.004(4) C9 0.014(4) 0.020(5) 0.038(5) -0.008(4) -0.008(4) 0.002(4) C10 0.017(4) 0.016(5) 0.027(5) -0.013(4) 0.003(4) -0.003(4) C11 0.016(4) 0.028(5) 0.015(5) -0.003(4) 0.004(4) -0.004(4) C12 0.021(5) 0.004(4) 0.026(5) 0.000(4) -0.003(4) -0.003(4) C13 0.021(5) 0.021(5) 0.018(5) -0.002(4) -0.002(4) -0.005(4) C14 0.016(4) 0.019(5) 0.023(5) -0.003(4) -0.007(4) -0.003(4) C15 0.016(5) 0.024(5) 0.024(5) -0.006(4) -0.005(4) 0.002(4) C16 0.020(5) 0.023(5) 0.032(5) -0.002(4) -0.008(4) -0.007(4) C17 0.030(5) 0.026(6) 0.040(6) -0.005(4) -0.014(4) -0.002(5) C18 0.030(5) 0.030(6) 0.057(7) -0.007(5) -0.018(5) 0.005(5) C19 0.064(7) 0.013(5) 0.054(7) 0.006(5) -0.025(6) -0.008(6) C20 0.038(6) 0.032(6) 0.060(7) 0.002(5) -0.021(5) -0.013(5) C21 0.015(5) 0.029(6) 0.032(6) 0.013(5) -0.011(4) -0.005(4) C22 0.026(5) 0.029(6) 0.034(6) 0.003(5) -0.011(4) -0.008(4) C23 0.032(6) 0.045(7) 0.034(6) 0.003(5) -0.005(4) -0.013(5) C24 0.034(6) 0.036(7) 0.051(7) 0.024(5) -0.027(5) -0.013(5) C25 0.025(5) 0.023(6) 0.060(7) 0.001(5) -0.023(5) -0.004(4) C26 0.021(5) 0.031(6) 0.049(6) 0.002(5) -0.020(4) -0.008(5) C27 0.024(5) 0.022(5) 0.024(5) -0.006(4) 0.000(4) -0.008(4) C28 0.019(5) 0.025(5) 0.035(6) -0.003(4) -0.009(4) 0.000(4) C29 0.031(5) 0.035(6) 0.043(6) -0.009(5) -0.017(4) -0.007(5) C30 0.019(5) 0.032(6) 0.042(6) -0.009(5) -0.007(4) -0.004(4) C31 0.028(5) 0.015(5) 0.033(5) -0.003(4) -0.005(4) -0.011(4) C32 0.017(4) 0.033(5) 0.025(5) -0.015(4) 0.002(4) -0.005(4) C1' 0.031(6) 0.037(6) 0.041(6) -0.015(5) 0.000(5) -0.010(5) C2' 0.014(5) 0.036(6) 0.060(7) -0.021(5) 0.002(4) 0.002(5) C3' 0.036(6) 0.016(5) 0.067(7) -0.011(5) -0.023(5) 0.009(5) C4' 0.020(5) 0.017(5) 0.053(6) -0.004(4) -0.008(4) 0.003(4) C5' 0.025(5) 0.013(5) 0.028(5) -0.005(4) -0.002(4) -0.001(4) C6' 0.028(5) 0.015(5) 0.024(5) 0.006(4) -0.013(4) -0.010(4) C7' 0.034(5) 0.011(5) 0.028(5) -0.006(4) -0.010(4) 0.000(4) C8' 0.031(5) 0.028(5) 0.024(5) 0.009(4) -0.009(4) -0.017(5) C9' 0.023(5) 0.022(5) 0.015(5) -0.003(4) -0.001(4) -0.005(4) C10' 0.032(5) 0.016(5) 0.017(5) -0.005(4) -0.001(4) -0.011(4) C11' 0.029(5) 0.014(5) 0.025(5) 0.004(4) -0.009(4) -0.003(4) C12' 0.027(5) 0.025(5) 0.022(5) 0.000(4) -0.006(4) -0.011(4) C13' 0.026(5) 0.017(5) 0.010(4) 0.001(4) -0.002(4) 0.001(4) C14' 0.029(5) 0.027(5) 0.023(5) -0.001(4) -0.011(4) -0.003(4) C15' 0.027(5) 0.029(5) 0.015(5) 0.001(4) -0.008(4) -0.011(4) C16' 0.020(5) 0.025(5) 0.023(5) -0.012(4) 0.001(4) -0.001(4) C17' 0.033(5) 0.025(5) 0.023(5) -0.004(4) -0.004(4) -0.006(4) C18' 0.037(5) 0.030(5) 0.029(5) -0.008(4) -0.017(4) -0.003(5) C19' 0.031(5) 0.029(5) 0.031(5) -0.011(4) -0.010(4) -0.003(4) C20' 0.037(5) 0.016(5) 0.025(5) 0.002(4) -0.006(4) -0.009(4) C21' 0.032(5) 0.015(5) 0.031(5) 0.001(4) -0.014(4) -0.006(4) C22' 0.026(5) 0.015(5) 0.043(6) -0.008(4) -0.008(4) -0.002(4) C23' 0.039(6) 0.040(6) 0.059(7) -0.034(5) -0.009(5) -0.007(5) C24' 0.029(6) 0.035(6) 0.065(7) -0.018(5) -0.016(5) -0.007(5) C25' 0.021(5) 0.011(5) 0.045(6) 0.008(4) -0.011(4) 0.004(4) C26' 0.033(5) 0.014(5) 0.034(5) 0.001(4) -0.011(4) -0.007(4) C27' 0.031(5) 0.013(5) 0.023(5) -0.004(4) -0.002(4) -0.006(4) C28' 0.039(6) 0.041(6) 0.026(5) -0.005(4) 0.004(5) -0.012(5) C29' 0.029(6) 0.058(7) 0.044(6) -0.018(6) 0.009(5) -0.010(5) C30' 0.038(6) 0.024(6) 0.049(7) -0.012(5) 0.017(5) -0.013(5) C31' 0.039(6) 0.022(6) 0.027(5) -0.005(4) 0.006(4) -0.005(5) C32' 0.030(5) 0.019(5) 0.036(6) -0.007(4) -0.004(4) 0.000(4) Cl1 0.0508(17) 0.0491(18) 0.0526(18) -0.0045(14) 0.0025(14) -0.0252(15) O10 0.131(7) 0.092(7) 0.055(5) 0.042(5) -0.039(5) -0.018(6) O11 0.103(7) 0.130(8) 0.106(7) -0.078(6) 0.043(5) -0.080(6) O12 0.053(5) 0.084(6) 0.074(5) -0.038(4) 0.021(4) -0.030(4) O13 0.056(5) 0.086(6) 0.090(6) -0.030(5) -0.016(4) -0.020(5) Cl2 0.0329(13) 0.0268(13) 0.0336(13) -0.0080(11) -0.0052(11) -0.0078(11) O20 0.044(4) 0.019(3) 0.052(4) -0.008(3) -0.015(3) 0.004(3) O21 0.037(4) 0.037(4) 0.040(4) -0.016(3) -0.003(3) -0.006(3) O22 0.044(4) 0.040(4) 0.044(4) -0.005(3) -0.002(3) -0.025(3) O23 0.040(4) 0.042(4) 0.039(4) -0.012(3) -0.006(3) -0.022(3) Cl3 0.0426(15) 0.0376(16) 0.0606(18) -0.0211(13) -0.0286(13) 0.0015(13) O30 0.043(4) 0.071(5) 0.075(5) -0.022(4) -0.023(3) -0.020(4) O31 0.060(5) 0.230(11) 0.035(5) -0.034(6) 0.000(4) -0.075(6) O32 0.173(9) 0.051(6) 0.224(11) -0.065(6) -0.158(9) 0.064(6) O33 0.066(4) 0.060(5) 0.053(4) -0.010(4) -0.032(3) -0.029(4) N1S 0.048(5) 0.055(6) 0.058(6) -0.023(5) -0.019(5) 0.010(5) C1S 0.054(6) 0.044(7) 0.046(7) -0.010(5) -0.013(5) -0.004(5) C2S 0.020(5) 0.037(6) 0.056(7) -0.018(6) -0.011(5) 0.001(5) N2S 0.049(5) 0.038(5) 0.058(6) -0.016(5) -0.026(5) 0.005(4) C3S 0.062(7) 0.034(6) 0.060(7) -0.016(5) -0.015(6) 0.006(5) C4S 0.041(6) 0.015(5) 0.046(7) -0.002(5) -0.021(5) 0.004(5) _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 O2 2.253(5) . ? Tb1 O1 2.282(5) . ? Tb1 O2' 2.290(5) . ? Tb1 O1' 2.301(5) . ? Tb1 N3' 2.489(6) . ? Tb1 N2 2.544(6) . ? Tb1 N2' 2.555(5) . ? Tb1 N3 2.566(5) . ? O1' N1' 1.342(7) . ? O2' N4' 1.337(7) . ? N1' C1' 1.345(9) . ? N1' C5' 1.366(8) . ? N2' C6' 1.352(9) . ? N2' C10' 1.364(8) . ? N3' C15' 1.312(9) . ? N3' C11' 1.406(9) . ? N4' C20' 1.354(9) . ? N4' C16' 1.355(8) . ? O1 N1 1.329(7) . ? O2 N4 1.349(7) . ? N1 C1 1.369(9) . ? N1 C5 1.374(8) . ? N2 C10 1.339(8) . ? N2 C6 1.357(9) . ? N3 C15 1.350(9) . ? N3 C11 1.366(9) . ? N4 C20 1.332(10) . ? N4 C16 1.366(8) . ? C1 C2 1.387(10) . ? C1 H1 0.9500 . ? C2 C3 1.382(10) . ? C2 H2 0.9500 . ? C3 C4 1.367(10) . ? C3 H3 0.9500 . ? C4 C5 1.368(10) . ? C4 H4 0.9500 . ? C5 C6 1.499(10) . ? C6 C7 1.387(9) . ? C7 C8 1.378(10) . ? C7 H7 0.9500 . ? C8 C9 1.411(10) . ? C8 C21 1.492(10) . ? C9 C10 1.377(10) . ? C9 H9 0.9500 . ? C10 C11 1.511(10) . ? C11 C12 1.390(10) . ? C12 C13 1.388(10) . ? C12 H12 0.9500 . ? C13 C14 1.384(10) . ? C13 C27 1.480(10) . ? C14 C15 1.399(10) . ? C14 H14 0.9500 . ? C15 C16 1.476(10) . ? C16 C17 1.361(10) . ? C17 C18 1.384(11) . ? C17 H17 0.9500 . ? C18 C19 1.378(10) . ? C18 H18 0.9500 . ? C19 C20 1.372(11) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.365(11) . ? C21 C22 1.410(11) . ? C22 C23 1.399(10) . ? C22 H22 0.9500 . ? C23 C24 1.347(12) . ? C23 H23 0.9500 . ? C24 C25 1.389(11) . ? C24 H24 0.9500 . ? C25 C26 1.405(10) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.391(10) . ? C27 C32 1.398(9) . ? C28 C29 1.406(10) . ? C28 H28 0.9500 . ? C29 C30 1.397(10) . ? C29 H29 0.9500 . ? C30 C31 1.403(10) . ? C30 H30 0.9500 . ? C31 C32 1.391(10) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C1' C2' 1.362(11) . ? C1' H1' 0.9500 . ? C2' C3' 1.381(10) . ? C2' H2' 0.9500 . ? C3' C4' 1.387(10) . ? C3' H3' 0.9500 . ? C4' C5' 1.371(10) . ? C4' H4' 0.9500 . ? C5' C6' 1.495(10) . ? C6' C7' 1.375(10) . ? C7' C8' 1.424(10) . ? C7' H7' 0.9500 . ? C8' C9' 1.388(11) . ? C8' C21' 1.483(10) . ? C9' C10' 1.384(10) . ? C9' H9' 0.9500 . ? C10' C11' 1.465(10) . ? C11' C12' 1.396(9) . ? C12' C13' 1.372(10) . ? C12' H12' 0.9500 . ? C13' C14' 1.416(10) . ? C13' C27' 1.509(10) . ? C14' C15' 1.415(10) . ? C14' H14' 0.9500 . ? C15' C16' 1.498(10) . ? C16' C17' 1.369(10) . ? C17' C18' 1.389(10) . ? C17' H17' 0.9500 . ? C18' C19' 1.376(10) . ? C18' H18' 0.9500 . ? C19' C20' 1.361(10) . ? C19' H19' 0.9500 . ? C20' H20' 0.9500 . ? C21' C26' 1.375(9) . ? C21' C22' 1.383(10) . ? C22' C23' 1.378(10) . ? C22' H22' 0.9500 . ? C23' C24' 1.362(10) . ? C23' H23' 0.9500 . ? C24' C25' 1.368(11) . ? C24' H24' 0.9500 . ? C25' C26' 1.417(11) . ? C25' H25' 0.9500 . ? C26' H26' 0.9500 . ? C27' C32' 1.370(10) . ? C27' C28' 1.389(11) . ? C28' C29' 1.396(10) . ? C28' H28' 0.9500 . ? C29' C30' 1.337(12) . ? C29' H29' 0.9500 . ? C30' C31' 1.390(11) . ? C30' H30' 0.9500 . ? C31' C32' 1.397(10) . ? C31' H31' 0.9500 . ? C32' H32' 0.9500 . ? Cl1 O10 1.389(6) . ? Cl1 O11 1.389(8) . ? Cl1 O12 1.437(7) . ? Cl1 O13 1.469(7) . ? Cl2 O20 1.437(6) . ? Cl2 O23 1.445(5) . ? Cl2 O21 1.449(6) . ? Cl2 O22 1.452(5) . ? Cl3 O31 1.397(6) . ? Cl3 O32 1.419(8) . ? Cl3 O30 1.421(6) . ? Cl3 O33 1.426(6) . ? N1S C2S 1.127(10) . ? C1S C2S 1.475(12) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? N2S C4S 1.121(10) . ? C3S C4S 1.446(12) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? 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 O2 Tb1 O1 152.30(16) . . ? O2 Tb1 O2' 89.41(19) . . ? O1 Tb1 O2' 90.79(19) . . ? O2 Tb1 O1' 104.4(2) . . ? O1 Tb1 O1' 87.95(19) . . ? O2' Tb1 O1' 151.88(16) . . ? O2 Tb1 N3' 75.02(19) . . ? O1 Tb1 N3' 78.80(19) . . ? O2' Tb1 N3' 71.49(18) . . ? O1' Tb1 N3' 135.38(18) . . ? O2 Tb1 N2 134.86(18) . . ? O1 Tb1 N2 71.81(18) . . ? O2' Tb1 N2 77.00(18) . . ? O1' Tb1 N2 75.94(19) . . ? N3' Tb1 N2 136.13(19) . . ? O2 Tb1 N2' 84.83(19) . . ? O1 Tb1 N2' 75.72(18) . . ? O2' Tb1 N2' 135.40(17) . . ? O1' Tb1 N2' 71.19(17) . . ? N3' Tb1 N2' 64.3(2) . . ? N2 Tb1 N2' 134.0(2) . . ? O2 Tb1 N3 71.10(18) . . ? O1 Tb1 N3 135.54(18) . . ? O2' Tb1 N3 76.16(18) . . ? O1' Tb1 N3 85.19(17) . . ? N3' Tb1 N3 132.7(2) . . ? N2 Tb1 N3 63.90(19) . . ? N2' Tb1 N3 140.91(19) . . ? N1' O1' Tb1 119.8(4) . . ? N4' O2' Tb1 119.3(4) . . ? O1' N1' C1' 118.9(6) . . ? O1' N1' C5' 120.5(6) . . ? C1' N1' C5' 120.6(7) . . ? C6' N2' C10' 116.8(6) . . ? C6' N2' Tb1 123.5(4) . . ? C10' N2' Tb1 113.2(5) . . ? C15' N3' C11' 116.8(6) . . ? C15' N3' Tb1 125.7(5) . . ? C11' N3' Tb1 115.4(5) . . ? O2' N4' C20' 118.7(6) . . ? O2' N4' C16' 121.1(6) . . ? C20' N4' C16' 120.2(7) . . ? N1 O1 Tb1 118.6(4) . . ? N4 O2 Tb1 123.6(4) . . ? O1 N1 C1 117.3(6) . . ? O1 N1 C5 123.2(6) . . ? C1 N1 C5 119.5(7) . . ? C10 N2 C6 118.4(6) . . ? C10 N2 Tb1 116.5(5) . . ? C6 N2 Tb1 123.6(5) . . ? C15 N3 C11 116.8(6) . . ? C15 N3 Tb1 123.6(4) . . ? C11 N3 Tb1 113.2(5) . . ? C20 N4 O2 117.1(6) . . ? C20 N4 C16 122.7(7) . . ? O2 N4 C16 120.1(6) . . ? N1 C1 C2 120.8(7) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C3 C2 C1 120.0(7) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 117.6(8) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 123.2(7) . . ? C3 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C4 C5 N1 118.8(7) . . ? C4 C5 C6 122.4(6) . . ? N1 C5 C6 118.7(7) . . ? N2 C6 C7 121.6(7) . . ? N2 C6 C5 120.5(7) . . ? C7 C6 C5 117.7(7) . . ? C8 C7 C6 120.5(7) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 117.0(7) . . ? C7 C8 C21 121.8(7) . . ? C9 C8 C21 121.2(7) . . ? C10 C9 C8 119.8(7) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 122.4(7) . . ? N2 C10 C11 116.2(7) . . ? C9 C10 C11 121.1(7) . . ? N3 C11 C12 122.4(7) . . ? N3 C11 C10 115.9(7) . . ? C12 C11 C10 121.7(7) . . ? C13 C12 C11 120.5(7) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 117.1(7) . . ? C14 C13 C27 120.4(7) . . ? C12 C13 C27 122.3(7) . . ? C13 C14 C15 120.2(7) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N3 C15 C14 122.8(7) . . ? N3 C15 C16 119.1(7) . . ? C14 C15 C16 118.1(7) . . ? C17 C16 N4 117.7(7) . . ? C17 C16 C15 122.6(7) . . ? N4 C16 C15 119.7(7) . . ? C16 C17 C18 121.5(8) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 118.5(8) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C18 119.8(8) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N4 C20 C19 119.8(8) . . ? N4 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C26 C21 C22 119.3(7) . . ? C26 C21 C8 122.7(8) . . ? C22 C21 C8 118.0(8) . . ? C23 C22 C21 118.6(8) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C22 120.9(9) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 121.8(8) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C24 C25 C26 117.4(9) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? C21 C26 C25 121.9(9) . . ? C21 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C28 C27 C32 119.7(7) . . ? C28 C27 C13 119.1(7) . . ? C32 C27 C13 121.3(7) . . ? C27 C28 C29 120.4(7) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 119.4(8) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.3(8) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 119.5(7) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C27 120.7(8) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? N1' C1' C2' 121.7(7) . . ? N1' C1' H1' 119.1 . . ? C2' C1' H1' 119.1 . . ? C1' C2' C3' 119.0(7) . . ? C1' C2' H2' 120.5 . . ? C3' C2' H2' 120.5 . . ? C2' C3' C4' 119.2(8) . . ? C2' C3' H3' 120.4 . . ? C4' C3' H3' 120.4 . . ? C5' C4' C3' 120.5(7) . . ? C5' C4' H4' 119.8 . . ? C3' C4' H4' 119.8 . . ? N1' C5' C4' 119.0(7) . . ? N1' C5' C6' 118.8(7) . . ? C4' C5' C6' 122.1(6) . . ? N2' C6' C7' 124.5(7) . . ? N2' C6' C5' 117.1(6) . . ? C7' C6' C5' 118.4(7) . . ? C6' C7' C8' 118.5(7) . . ? C6' C7' H7' 120.8 . . ? C8' C7' H7' 120.8 . . ? C9' C8' C7' 116.4(7) . . ? C9' C8' C21' 122.9(7) . . ? C7' C8' C21' 120.5(8) . . ? C10' C9' C8' 121.5(7) . . ? C10' C9' H9' 119.2 . . ? C8' C9' H9' 119.2 . . ? N2' C10' C9' 121.5(7) . . ? N2' C10' C11' 115.7(6) . . ? C9' C10' C11' 122.8(7) . . ? C12' C11' N3' 120.6(7) . . ? C12' C11' C10' 123.1(7) . . ? N3' C11' C10' 116.3(6) . . ? C13' C12' C11' 121.5(7) . . ? C13' C12' H12' 119.3 . . ? C11' C12' H12' 119.3 . . ? C12' C13' C14' 118.1(7) . . ? C12' C13' C27' 122.4(7) . . ? C14' C13' C27' 119.5(7) . . ? C15' C14' C13' 117.1(7) . . ? C15' C14' H14' 121.4 . . ? C13' C14' H14' 121.4 . . ? N3' C15' C14' 125.4(7) . . ? N3' C15' C16' 119.5(7) . . ? C14' C15' C16' 115.1(7) . . ? N4' C16' C17' 119.1(7) . . ? N4' C16' C15' 120.0(7) . . ? C17' C16' C15' 120.9(7) . . ? C16' C17' C18' 121.0(7) . . ? C16' C17' H17' 119.5 . . ? C18' C17' H17' 119.5 . . ? C19' C18' C17' 118.8(8) . . ? C19' C18' H18' 120.6 . . ? C17' C18' H18' 120.6 . . ? C20' C19' C18' 118.8(8) . . ? C20' C19' H19' 120.6 . . ? C18' C19' H19' 120.6 . . ? N4' C20' C19' 122.0(7) . . ? N4' C20' H20' 119.0 . . ? C19' C20' H20' 119.0 . . ? C26' C21' C22' 118.7(7) . . ? C26' C21' C8' 120.6(8) . . ? C22' C21' C8' 120.5(7) . . ? C23' C22' C21' 121.8(7) . . ? C23' C22' H22' 119.1 . . ? C21' C22' H22' 119.1 . . ? C24' C23' C22' 119.2(9) . . ? C24' C23' H23' 120.4 . . ? C22' C23' H23' 120.4 . . ? C23' C24' C25' 121.1(8) . . ? C23' C24' H24' 119.4 . . ? C25' C24' H24' 119.4 . . ? C24' C25' C26' 119.5(7) . . ? C24' C25' H25' 120.3 . . ? C26' C25' H25' 120.3 . . ? C21' C26' C25' 119.6(8) . . ? C21' C26' H26' 120.2 . . ? C25' C26' H26' 120.2 . . ? C32' C27' C28' 120.8(7) . . ? C32' C27' C13' 119.8(7) . . ? C28' C27' C13' 119.2(8) . . ? C27' C28' C29' 118.0(9) . . ? C27' C28' H28' 121.0 . . ? C29' C28' H28' 121.0 . . ? C30' C29' C28' 122.3(9) . . ? C30' C29' H29' 118.8 . . ? C28' C29' H29' 118.8 . . ? C29' C30' C31' 119.4(8) . . ? C29' C30' H30' 120.3 . . ? C31' C30' H30' 120.3 . . ? C30' C31' C32' 120.1(9) . . ? C30' C31' H31' 119.9 . . ? C32' C31' H31' 119.9 . . ? C27' C32' C31' 119.2(8) . . ? C27' C32' H32' 120.4 . . ? C31' C32' H32' 120.4 . . ? O10 Cl1 O11 115.2(6) . . ? O10 Cl1 O12 110.8(5) . . ? O11 Cl1 O12 110.2(4) . . ? O10 Cl1 O13 105.7(5) . . ? O11 Cl1 O13 106.2(5) . . ? O12 Cl1 O13 108.4(5) . . ? O20 Cl2 O23 110.4(3) . . ? O20 Cl2 O21 109.7(3) . . ? O23 Cl2 O21 109.7(3) . . ? O20 Cl2 O22 109.4(3) . . ? O23 Cl2 O22 109.0(3) . . ? O21 Cl2 O22 108.6(3) . . ? O31 Cl3 O32 111.6(6) . . ? O31 Cl3 O30 108.6(4) . . ? O32 Cl3 O30 108.0(5) . . ? O31 Cl3 O33 110.1(4) . . ? O32 Cl3 O33 108.7(4) . . ? O30 Cl3 O33 109.8(4) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? N1S C2S C1S 177.5(11) . . ? C4S C3S H3S1 109.5 . . ? C4S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C4S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? N2S C4S C3S 178.5(10) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.620 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.149