# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Novel Dense Organic-Lanthanide Hybrid Architectures: Syntheses, Structures and Magnetic Properties ; loop_ _publ_author_name 'Wei-Yin Sun' 'Zhengshuai Bai' 'Man-Sheng Chen' 'Taka-aki Okamura' 'Jing Su' 'Norikazu Ueyama' # Attachment 'B816205K-rev-cif.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 702666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H7 La N2 O9, 3(H2 O)' _chemical_formula_sum 'C14 H13 La N2 O12' _chemical_formula_weight 540.17 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' 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 12.1200(17) _cell_length_b 12.8067(18) _cell_length_c 12.3605(17) _cell_angle_alpha 90.00 _cell_angle_beta 114.974(2) _cell_angle_gamma 90.00 _cell_volume 1739.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1752 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'SADBAS (Bruker,2000)' _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 'Bruker Smart Apex. CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8473 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3064 _reflns_number_gt 2554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart (Bruker,2000)' _computing_cell_refinement 'Saintplus (Bruker.2000)' _computing_data_reduction 'Saintplus (Bruker.2000)' _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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3064 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 La1 La 0.45178(3) 0.54480(3) 0.14630(3) 0.01331(13) Uani 1 1 d . . . O1 O 0.4790(3) 0.6970(3) 0.2890(4) 0.0209(11) Uani 1 1 d . . . O2 O 0.5600(4) 0.8495(4) 0.3644(4) 0.0299(12) Uani 1 1 d . . . O3 O 0.6181(3) 0.5023(3) 0.0753(4) 0.0201(10) Uani 1 1 d . . . O4 O 0.7863(4) 0.5425(4) 0.0544(4) 0.0273(11) Uani 1 1 d . . . O5 O 1.3011(4) 0.9894(3) 0.7333(4) 0.0212(10) Uani 1 1 d . . . O6 O 1.1165(4) 0.9735(4) 0.7322(4) 0.0373(13) Uani 1 1 d . . . O7 O 1.4332(3) 0.7853(3) 0.5201(4) 0.0220(11) Uani 1 1 d . . . O8 O 1.3038(4) 0.7267(4) 0.3408(4) 0.0399(14) Uani 1 1 d . . . H1 H 1.3663 0.7158 0.3322 0.060 Uiso 1 1 calc R . . O9 O 0.5916(4) 0.4772(4) 0.3541(4) 0.0387(13) Uani 1 1 d . . . H2 H 0.5884 0.5186 0.4064 0.058 Uiso 1 1 d R . . H3 H 0.6642 0.4744 0.3605 0.058 Uiso 1 1 d R . . O10 O 0.0788(7) 0.0954(6) 0.8934(6) 0.113(3) Uani 1 1 d . . . H4 H 0.0510 0.0412 0.8507 0.169 Uiso 1 1 d R . . H5 H 0.1432 0.0797 0.9545 0.169 Uiso 1 1 d R . . O11 O 0.3648(5) 0.1053(4) 0.9481(4) 0.0555(16) Uani 1 1 d . . . H6 H 0.3806 0.1690 0.9417 0.067 Uiso 1 1 d R . . H7 H 0.3894 0.0678 0.9059 0.083 Uiso 1 1 d R . . O12 O 0.8386(11) 0.0543(12) 0.9152(15) 0.065(5) Uiso 0.57(3) 1 d P A 1 O12' O 0.8146(16) 0.0963(19) 0.856(2) 0.076(8) Uiso 0.43(3) 1 d P A 2 N11 N 0.6571(4) 0.6561(4) 0.2300(4) 0.0161(12) Uani 1 1 d . . . N21 N 1.2474(4) 0.8499(4) 0.5629(4) 0.0176(12) Uani 1 1 d . . . C1 C 0.5637(5) 0.7646(5) 0.3219(5) 0.0160(14) Uani 1 1 d . . . C2 C 0.7205(5) 0.5520(5) 0.1068(6) 0.0197(15) Uani 1 1 d . . . C3 C 1.1920(5) 0.9540(5) 0.6951(5) 0.0196(14) Uani 1 1 d . . . C4 C 1.3314(6) 0.7666(5) 0.4455(6) 0.0220(16) Uani 1 1 d . . . C12 C 0.6750(5) 0.7326(5) 0.3079(5) 0.0147(14) Uani 1 1 d . . . C13 C 0.7881(5) 0.7798(5) 0.3705(5) 0.0192(15) Uani 1 1 d . . . H10 H 0.7973 0.8339 0.4238 0.023 Uiso 1 1 calc R . . C14 C 0.8862(5) 0.7445(5) 0.3515(5) 0.0157(14) Uani 1 1 d . . . C15 C 0.8651(5) 0.6697(5) 0.2653(5) 0.0190(15) Uani 1 1 d . . . H11 H 0.9285 0.6469 0.2477 0.023 Uiso 1 1 calc R . . C16 C 0.7500(5) 0.6282(5) 0.2047(5) 0.0169(14) Uani 1 1 d . . . C22 C 1.1566(5) 0.8795(5) 0.5898(5) 0.0197(15) Uani 1 1 d . . . C23 C 1.0391(5) 0.8477(5) 0.5246(5) 0.0197(15) Uani 1 1 d . . . H12 H 0.9779 0.8684 0.5467 0.024 Uiso 1 1 calc R . . C24 C 1.0115(5) 0.7841(5) 0.4251(5) 0.0183(15) Uani 1 1 d . . . C25 C 1.1082(5) 0.7572(5) 0.3969(6) 0.0214(16) Uani 1 1 d . . . H13 H 1.0946 0.7164 0.3302 0.026 Uiso 1 1 calc R . . C26 C 1.2226(5) 0.7914(5) 0.4682(5) 0.0182(15) 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 La1 0.01067(19) 0.0133(2) 0.0155(2) -0.00041(18) 0.00513(15) 0.00041(17) O1 0.013(2) 0.024(3) 0.029(3) -0.011(2) 0.012(2) -0.008(2) O2 0.029(3) 0.022(3) 0.043(3) -0.001(3) 0.020(2) 0.004(2) O3 0.014(2) 0.022(3) 0.022(2) -0.010(2) 0.0060(19) -0.009(2) O4 0.028(3) 0.031(3) 0.033(3) -0.005(2) 0.022(2) -0.002(2) O5 0.020(2) 0.020(3) 0.021(2) -0.008(2) 0.007(2) -0.007(2) O6 0.025(3) 0.054(4) 0.043(3) -0.028(3) 0.024(2) -0.008(3) O7 0.008(2) 0.027(3) 0.028(3) -0.002(2) 0.005(2) 0.000(2) O8 0.017(2) 0.064(4) 0.042(3) -0.031(3) 0.015(2) -0.008(3) O9 0.042(3) 0.040(4) 0.030(3) -0.002(3) 0.012(2) -0.002(3) O10 0.132(7) 0.136(8) 0.094(6) -0.064(6) 0.070(5) -0.005(6) O11 0.088(4) 0.040(4) 0.043(3) -0.014(3) 0.033(3) -0.010(3) N11 0.014(3) 0.016(3) 0.019(3) 0.002(2) 0.007(2) 0.001(2) N21 0.013(3) 0.021(3) 0.021(3) 0.002(3) 0.009(2) 0.001(2) C1 0.022(4) 0.015(4) 0.016(3) -0.002(3) 0.014(3) -0.001(3) C2 0.016(3) 0.018(4) 0.023(4) 0.001(3) 0.008(3) 0.004(3) C3 0.019(3) 0.017(4) 0.020(3) 0.003(3) 0.006(3) 0.005(3) C4 0.025(4) 0.019(4) 0.031(4) -0.008(3) 0.020(3) -0.004(3) C12 0.013(3) 0.016(4) 0.019(3) 0.000(3) 0.009(3) 0.001(3) C13 0.023(4) 0.017(4) 0.022(4) -0.007(3) 0.013(3) -0.005(3) C14 0.008(3) 0.017(4) 0.022(3) -0.005(3) 0.007(3) -0.004(3) C15 0.013(3) 0.023(4) 0.026(4) -0.003(3) 0.013(3) 0.002(3) C16 0.013(3) 0.019(4) 0.016(3) 0.002(3) 0.004(3) -0.003(3) C22 0.017(3) 0.023(4) 0.019(4) -0.006(3) 0.008(3) -0.006(3) C23 0.015(3) 0.022(4) 0.024(4) -0.006(3) 0.010(3) -0.003(3) C24 0.018(3) 0.018(4) 0.018(3) -0.003(3) 0.007(3) -0.003(3) C25 0.010(3) 0.023(4) 0.029(4) -0.013(3) 0.007(3) -0.007(3) C26 0.020(3) 0.021(4) 0.016(3) -0.006(3) 0.010(3) -0.001(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 La1 O2 2.505(5) 2_645 ? La1 O5 2.519(4) 4_475 ? La1 O1 2.555(4) . ? La1 O9 2.558(4) . ? La1 O3 2.573(4) . ? La1 O3 2.574(4) 3_665 ? La1 N21 2.619(5) 4_475 ? La1 O7 2.631(4) 4_475 ? La1 N11 2.668(5) . ? O1 C1 1.272(7) . ? O2 C1 1.217(7) . ? O2 La1 2.505(5) 2_655 ? O3 C2 1.300(7) . ? O3 La1 2.574(4) 3_665 ? O4 C2 1.227(7) . ? O5 C3 1.283(7) . ? O5 La1 2.519(4) 4_676 ? O6 C3 1.211(7) . ? O7 C4 1.213(7) . ? O7 La1 2.631(4) 4_676 ? O8 C4 1.297(7) . ? O8 H1 0.8200 . ? O9 H2 0.8499 . ? O9 H3 0.8501 . ? O10 H4 0.8500 . ? O10 H5 0.8499 . ? O11 H6 0.8501 . ? O11 H7 0.8499 . ? N11 C12 1.326(7) . ? N11 C16 1.339(7) . ? N21 C26 1.313(7) . ? N21 C22 1.333(7) . ? N21 La1 2.619(5) 4_676 ? C1 C12 1.489(8) . ? C2 C16 1.476(8) . ? C3 C22 1.522(8) . ? C4 C26 1.494(8) . ? C12 C13 1.395(8) . ? C13 C14 1.382(8) . ? C13 H10 0.9300 . ? C14 C15 1.374(8) . ? C14 C24 1.491(8) . ? C15 C16 1.381(8) . ? C15 H11 0.9300 . ? C22 C23 1.369(8) . ? C23 C24 1.393(8) . ? C23 H12 0.9300 . ? C24 C25 1.400(8) . ? C25 C26 1.363(8) . ? C25 H13 0.9300 . ? 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 La1 O5 79.26(14) 2_645 4_475 ? O2 La1 O1 141.78(14) 2_645 . ? O5 La1 O1 75.11(13) 4_475 . ? O2 La1 O9 73.36(15) 2_645 . ? O5 La1 O9 78.74(14) 4_475 . ? O1 La1 O9 74.17(15) . . ? O2 La1 O3 78.82(14) 2_645 . ? O5 La1 O3 157.29(14) 4_475 . ? O1 La1 O3 120.37(12) . . ? O9 La1 O3 89.35(15) . . ? O2 La1 O3 74.00(14) 2_645 3_665 ? O5 La1 O3 116.22(13) 4_475 3_665 ? O1 La1 O3 143.33(14) . 3_665 ? O9 La1 O3 140.36(15) . 3_665 ? O3 La1 O3 62.65(14) . 3_665 ? O2 La1 N21 118.04(15) 2_645 4_475 ? O5 La1 N21 61.43(14) 4_475 4_475 ? O1 La1 N21 72.77(14) . 4_475 ? O9 La1 N21 133.23(15) . 4_475 ? O3 La1 N21 136.17(14) . 4_475 ? O3 La1 N21 82.55(14) 3_665 4_475 ? O2 La1 O7 143.68(14) 2_645 4_475 ? O5 La1 O7 120.07(13) 4_475 4_475 ? O1 La1 O7 74.48(14) . 4_475 ? O9 La1 O7 136.87(14) . 4_475 ? O3 La1 O7 81.73(13) . 4_475 ? O3 La1 O7 69.84(13) 3_665 4_475 ? N21 La1 O7 60.71(14) 4_475 4_475 ? O2 La1 N11 125.21(15) 2_645 . ? O5 La1 N11 130.76(14) 4_475 . ? O1 La1 N11 59.83(13) . . ? O9 La1 N11 71.19(15) . . ? O3 La1 N11 60.59(14) . . ? O3 La1 N11 111.82(13) 3_665 . ? N21 La1 N11 116.71(15) 4_475 . ? O7 La1 N11 67.69(13) 4_475 . ? C1 O1 La1 126.3(4) . . ? C1 O2 La1 151.8(4) . 2_655 ? C2 O3 La1 125.5(4) . . ? C2 O3 La1 106.1(4) . 3_665 ? La1 O3 La1 117.35(14) . 3_665 ? C3 O5 La1 126.9(4) . 4_676 ? C4 O7 La1 114.8(4) . 4_676 ? C4 O8 H1 109.5 . . ? La1 O9 H2 109.2 . . ? La1 O9 H3 109.2 . . ? H2 O9 H3 109.5 . . ? H4 O10 H5 109.5 . . ? H6 O11 H7 109.5 . . ? C12 N11 C16 118.1(5) . . ? C12 N11 La1 121.1(4) . . ? C16 N11 La1 120.4(4) . . ? C26 N21 C22 118.8(5) . . ? C26 N21 La1 117.9(4) . 4_676 ? C22 N21 La1 119.9(4) . 4_676 ? O2 C1 O1 125.1(6) . . ? O2 C1 C12 119.8(6) . . ? O1 C1 C12 115.1(5) . . ? O4 C2 O3 123.0(6) . . ? O4 C2 C16 120.8(6) . . ? O3 C2 C16 116.1(5) . . ? O6 C3 O5 127.9(6) . . ? O6 C3 C22 117.8(6) . . ? O5 C3 C22 114.3(5) . . ? O7 C4 O8 126.0(6) . . ? O7 C4 C26 120.7(6) . . ? O8 C4 C26 113.3(5) . . ? N11 C12 C13 123.0(5) . . ? N11 C12 C1 114.1(5) . . ? C13 C12 C1 122.9(6) . . ? C14 C13 C12 118.6(6) . . ? C14 C13 H10 120.7 . . ? C12 C13 H10 120.7 . . ? C15 C14 C13 117.9(5) . . ? C15 C14 C24 121.2(5) . . ? C13 C14 C24 120.9(6) . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H11 119.8 . . ? C16 C15 H11 119.8 . . ? N11 C16 C15 121.8(6) . . ? N11 C16 C2 115.6(5) . . ? C15 C16 C2 122.6(6) . . ? N21 C22 C23 122.1(6) . . ? N21 C22 C3 115.3(5) . . ? C23 C22 C3 122.6(6) . . ? C22 C23 C24 119.7(6) . . ? C22 C23 H12 120.1 . . ? C24 C23 H12 120.1 . . ? C23 C24 C25 116.8(5) . . ? C23 C24 C14 122.6(5) . . ? C25 C24 C14 120.6(5) . . ? C26 C25 C24 119.3(6) . . ? C26 C25 H13 120.3 . . ? C24 C25 H13 120.3 . . ? N21 C26 C25 123.2(6) . . ? N21 C26 C4 113.6(5) . . ? C25 C26 C4 123.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.793 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.132 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 702667' _audit_creation_date 'Sun Jul 1 19:05:53 2007' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Ce(OH2){B1(H+)}]-3(H2O) ; _chemical_name_common (Ce(OH2)(B1(H+)))-3(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C14 H13 Ce N2 O12 ' _chemical_formula_sum 'C14 H13 Ce N2 O12' _chemical_formula_weight 541.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ce Ce -0.2486 2.6331 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.134(3) _cell_length_b 12.720(4) _cell_length_c 12.391(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.777(11) _cell_angle_gamma 90.00 _cell_volume 1736.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 11691 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 2.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.628 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 15919 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3955 _reflns_number_gt 3558 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0113P)^2^+3.5745P] 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 3955 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Ce1 Ce 0.455104(12) 0.453391(11) 0.146353(13) 0.00827(5) Uani 1 1 d . . . O1 O 0.61902(16) 0.49743(15) 0.07438(17) 0.0126(4) Uani 1 1 d . . . O2 O 0.78952(18) 0.45907(16) 0.05599(18) 0.0186(4) Uani 1 1 d . . . O3 O 0.47993(16) 0.30067(15) 0.28729(17) 0.0147(4) Uani 1 1 d . . . O4 O 0.56182(17) 0.14660(16) 0.36644(18) 0.0177(4) Uani 1 1 d . . . O5 O 1.43668(16) 0.21592(15) 0.51919(17) 0.0147(4) Uani 1 1 d . . . O6 O 1.30536(19) 0.2722(2) 0.3391(2) 0.0288(6) Uani 1 1 d . . . H1 H 1.379(3) 0.278(3) 0.327(3) 0.035 Uiso 1 1 d . . . O7 O 1.30666(17) 0.01099(15) 0.73614(17) 0.0143(4) Uani 1 1 d . . . O8 O 1.12193(19) 0.02571(18) 0.7353(2) 0.0248(5) Uani 1 1 d . . . O9 O 0.5915(2) 0.5224(2) 0.3519(2) 0.0271(5) Uani 1 1 d . . . H2 H 0.601(4) 0.492(3) 0.408(4) 0.032 Uiso 1 1 d . . . H3 H 0.655(4) 0.541(3) 0.364(4) 0.032 Uiso 1 1 d . . . O10 O 0.9160(4) 0.0930(4) 0.1010(4) 0.0758(12) Uani 1 1 d . . . H4 H 0.903(5) 0.060(5) 0.155(5) 0.091 Uiso 1 1 d . . . H5 H 0.852(5) 0.128(5) 0.083(6) 0.091 Uiso 1 1 d . . . O11 O 0.6341(3) 0.1074(2) 0.0504(2) 0.0372(6) Uani 1 1 d . . . H6 H 0.655(4) 0.074(3) 0.120(4) 0.045 Uiso 1 1 d . . . H7 H 0.576(4) 0.147(4) 0.044(4) 0.045 Uiso 1 1 d . . . O12 O 0.1634(4) 0.0604(4) 0.0936(4) 0.0850(14) Uani 1 1 d . . . N11 N 0.65882(19) 0.34267(17) 0.2294(2) 0.0108(5) Uani 1 1 d . . . N21 N 1.25167(19) 0.15019(18) 0.5649(2) 0.0115(5) Uani 1 1 d . . . C1 C 0.7215(2) 0.4488(2) 0.1057(2) 0.0118(5) Uani 1 1 d . . . C2 C 0.5651(2) 0.2325(2) 0.3228(2) 0.0102(5) Uani 1 1 d . . . C3 C 1.3330(2) 0.2340(2) 0.4437(3) 0.0150(6) Uani 1 1 d . . . C4 C 1.1982(2) 0.0460(2) 0.6973(2) 0.0149(6) Uani 1 1 d . . . C12 C 0.7521(2) 0.3716(2) 0.2052(2) 0.0116(5) Uani 1 1 d . . . C13 C 0.8678(2) 0.3308(2) 0.2650(2) 0.0138(6) Uani 1 1 d . . . H10 H 0.9321 0.3546 0.2465 0.017 Uiso 1 1 calc R . . C14 C 0.8893(2) 0.2547(2) 0.3526(2) 0.0126(5) Uani 1 1 d . . . C15 C 0.7895(2) 0.2188(2) 0.3709(2) 0.0113(5) Uani 1 1 d . . . H11 H 0.7984 0.1636 0.4256 0.014 Uiso 1 1 calc R . . C16 C 0.6774(2) 0.2653(2) 0.3079(2) 0.0106(5) Uani 1 1 d . . . C22 C 1.2251(2) 0.2093(2) 0.4685(2) 0.0137(6) Uani 1 1 d . . . C23 C 1.1093(2) 0.2428(2) 0.3957(3) 0.0159(6) Uani 1 1 d . . . H12 H 1.0946 0.2837 0.3269 0.019 Uiso 1 1 calc R . . C24 C 1.0142(2) 0.2152(2) 0.4257(2) 0.0121(5) Uani 1 1 d . . . C25 C 1.0417(2) 0.1522(2) 0.5256(2) 0.0141(6) Uani 1 1 d . . . H13 H 0.9795 0.1310 0.5485 0.017 Uiso 1 1 calc R . . C26 C 1.1612(2) 0.1203(2) 0.5918(2) 0.0124(5) 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 Ce1 0.00725(8) 0.00910(8) 0.00886(8) 0.00025(6) 0.00376(6) -0.00031(5) O1 0.0090(9) 0.0157(10) 0.0126(10) 0.0037(8) 0.0039(8) 0.0022(7) O2 0.0189(10) 0.0207(11) 0.0217(11) 0.0051(9) 0.0138(9) 0.0019(8) O3 0.0100(9) 0.0183(10) 0.0178(10) 0.0070(8) 0.0079(8) 0.0027(7) O4 0.0148(10) 0.0142(10) 0.0252(11) 0.0015(9) 0.0094(9) -0.0008(8) O5 0.0093(10) 0.0176(10) 0.0175(10) 0.0029(8) 0.0059(8) 0.0008(7) O6 0.0121(11) 0.0479(15) 0.0311(13) 0.0268(12) 0.0137(10) 0.0101(10) O7 0.0134(10) 0.0163(10) 0.0137(10) 0.0031(8) 0.0062(8) 0.0022(7) O8 0.0183(11) 0.0338(13) 0.0278(12) 0.0160(10) 0.0151(10) 0.0044(9) O9 0.0287(13) 0.0289(14) 0.0170(12) -0.0027(10) 0.0031(11) -0.0020(10) O10 0.086(3) 0.092(3) 0.067(3) 0.039(2) 0.049(2) 0.004(2) O11 0.0478(17) 0.0430(17) 0.0216(13) 0.0119(12) 0.0152(12) 0.0130(13) O12 0.056(2) 0.096(3) 0.110(3) 0.047(3) 0.040(2) 0.028(2) N11 0.0097(11) 0.0124(11) 0.0115(11) 0.0002(9) 0.0056(9) -0.0011(8) N21 0.0103(11) 0.0112(11) 0.0131(11) 0.0004(9) 0.0050(9) 0.0008(8) C1 0.0107(13) 0.0121(13) 0.0126(13) -0.0018(11) 0.0048(11) -0.0015(10) C2 0.0096(13) 0.0129(13) 0.0082(12) 0.0001(10) 0.0039(10) -0.0002(10) C3 0.0147(14) 0.0126(14) 0.0197(15) 0.0057(11) 0.0089(12) 0.0026(10) C4 0.0138(13) 0.0170(14) 0.0129(13) 0.0014(12) 0.0048(11) -0.0004(11) C12 0.0098(13) 0.0133(13) 0.0122(13) 0.0002(11) 0.0052(11) -0.0003(10) C13 0.0095(13) 0.0183(14) 0.0157(14) 0.0044(11) 0.0073(11) 0.0008(10) C14 0.0080(13) 0.0156(14) 0.0146(14) 0.0007(11) 0.0052(11) 0.0023(10) C15 0.0123(13) 0.0113(13) 0.0117(13) 0.0041(10) 0.0061(11) 0.0021(10) C16 0.0117(13) 0.0111(13) 0.0110(13) 0.0002(10) 0.0066(11) -0.0002(10) C22 0.0101(13) 0.0158(14) 0.0158(14) 0.0041(11) 0.0059(11) 0.0010(10) C23 0.0144(14) 0.0188(15) 0.0171(14) 0.0082(12) 0.0090(12) 0.0040(11) C24 0.0085(13) 0.0147(13) 0.0138(13) 0.0032(11) 0.0055(11) 0.0031(10) C25 0.0119(13) 0.0161(14) 0.0163(14) 0.0010(11) 0.0080(11) -0.0005(10) C26 0.0104(13) 0.0136(13) 0.0137(14) -0.0002(11) 0.0056(11) 0.0001(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 Ce1 O4 2.466(2) 2_655 ? Ce1 O7 2.523(2) 4_465 ? Ce1 O9 2.542(2) . ? Ce1 O3 2.544(2) . ? Ce1 O1 2.5596(19) . ? Ce1 O1 2.573(2) 3_665 ? Ce1 N21 2.600(2) 4_465 ? Ce1 O5 2.622(2) 4_465 ? Ce1 N11 2.650(2) . ? O1 C1 1.295(3) . ? O1 Ce1 2.573(2) 3_665 ? O2 C1 1.226(3) . ? O3 C2 1.278(3) . ? O4 C2 1.227(3) . ? O4 Ce1 2.466(2) 2_645 ? O5 C3 1.235(3) . ? O5 Ce1 2.622(2) 4_666 ? O6 C3 1.290(4) . ? O6 H1 0.97(4) . ? O7 C4 1.277(3) . ? O7 Ce1 2.523(2) 4_666 ? O8 C4 1.229(3) . ? O9 H2 0.76(4) . ? O9 H3 0.75(4) . ? O10 H4 0.85(6) . ? O10 H5 0.84(6) . ? O11 H6 0.89(4) . ? O11 H7 0.84(4) . ? N11 C16 1.335(3) . ? N11 C12 1.338(3) . ? N21 C26 1.330(3) . ? N21 C22 1.332(4) . ? N21 Ce1 2.600(2) 4_666 ? C1 C12 1.496(4) . ? C2 C16 1.509(4) . ? C3 C22 1.497(4) . ? C4 C26 1.521(4) . ? C12 C13 1.384(4) . ? C13 C14 1.396(4) . ? C13 H10 0.9500 . ? C14 C15 1.399(4) . ? C14 C24 1.489(4) . ? C15 C16 1.385(4) . ? C15 H11 0.9500 . ? C22 C23 1.381(4) . ? C23 C24 1.398(4) . ? C23 H12 0.9500 . ? C24 C25 1.393(4) . ? C25 C26 1.393(4) . ? C25 H13 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ce1 O7 78.10(6) 2_655 4_465 ? O4 Ce1 O9 73.85(8) 2_655 . ? O7 Ce1 O9 77.39(8) 4_465 . ? O4 Ce1 O3 141.99(7) 2_655 . ? O7 Ce1 O3 74.67(6) 4_465 . ? O9 Ce1 O3 74.70(8) . . ? O4 Ce1 O1 79.36(6) 2_655 . ? O7 Ce1 O1 156.46(6) 4_465 . ? O9 Ce1 O1 89.93(8) . . ? O3 Ce1 O1 121.36(6) . . ? O4 Ce1 O1 72.95(7) 2_655 3_665 ? O7 Ce1 O1 115.40(6) 4_465 3_665 ? O9 Ce1 O1 140.51(8) . 3_665 ? O3 Ce1 O1 143.45(6) . 3_665 ? O1 Ce1 O1 63.44(7) . 3_665 ? O4 Ce1 N21 116.12(7) 2_655 4_465 ? O7 Ce1 N21 61.65(7) 4_465 4_465 ? O9 Ce1 N21 132.65(8) . 4_465 ? O3 Ce1 N21 72.51(7) . 4_465 ? O1 Ce1 N21 136.52(7) . 4_465 ? O1 Ce1 N21 81.87(7) 3_665 4_465 ? O4 Ce1 O5 142.77(7) 2_655 4_465 ? O7 Ce1 O5 121.04(6) 4_465 4_465 ? O9 Ce1 O5 137.85(7) . 4_465 ? O3 Ce1 O5 74.99(7) . 4_465 ? O1 Ce1 O5 81.57(6) . 4_465 ? O1 Ce1 O5 69.94(6) 3_665 4_465 ? N21 Ce1 O5 61.48(6) 4_465 4_465 ? O4 Ce1 N11 126.42(7) 2_655 . ? O7 Ce1 N11 130.28(7) 4_465 . ? O9 Ce1 N11 71.64(8) . . ? O3 Ce1 N11 60.32(6) . . ? O1 Ce1 N11 61.11(7) . . ? O1 Ce1 N11 113.30(6) 3_665 . ? N21 Ce1 N11 117.44(7) 4_465 . ? O5 Ce1 N11 68.12(6) 4_465 . ? C1 O1 Ce1 125.47(17) . . ? C1 O1 Ce1 107.39(16) . 3_665 ? Ce1 O1 Ce1 116.56(7) . 3_665 ? C2 O3 Ce1 126.93(16) . . ? C2 O4 Ce1 151.23(19) . 2_645 ? C3 O5 Ce1 114.29(17) . 4_666 ? C3 O6 H1 109(2) . . ? C4 O7 Ce1 125.78(17) . 4_666 ? Ce1 O9 H2 122(3) . . ? Ce1 O9 H3 120(3) . . ? H2 O9 H3 103(4) . . ? H4 O10 H5 91(5) . . ? H6 O11 H7 105(4) . . ? C16 N11 C12 117.7(2) . . ? C16 N11 Ce1 121.33(17) . . ? C12 N11 Ce1 120.41(17) . . ? C26 N21 C22 118.1(2) . . ? C26 N21 Ce1 120.49(18) . 4_666 ? C22 N21 Ce1 117.90(17) . 4_666 ? O2 C1 O1 124.2(3) . . ? O2 C1 C12 119.8(2) . . ? O1 C1 C12 115.9(2) . . ? O4 C2 O3 125.8(2) . . ? O4 C2 C16 119.9(2) . . ? O3 C2 C16 114.3(2) . . ? O5 C3 O6 125.8(3) . . ? O5 C3 C22 120.4(3) . . ? O6 C3 C22 113.8(2) . . ? O8 C4 O7 127.2(3) . . ? O8 C4 C26 117.5(2) . . ? O7 C4 C26 115.3(2) . . ? N11 C12 C13 122.7(3) . . ? N11 C12 C1 115.1(2) . . ? C13 C12 C1 122.2(2) . . ? C12 C13 C14 119.6(2) . . ? C12 C13 H10 120.2 . . ? C14 C13 H10 120.2 . . ? C13 C14 C15 117.4(2) . . ? C13 C14 C24 121.2(2) . . ? C15 C14 C24 121.4(2) . . ? C16 C15 C14 118.8(2) . . ? C16 C15 H11 120.6 . . ? C14 C15 H11 120.6 . . ? N11 C16 C15 123.5(2) . . ? N11 C16 C2 114.1(2) . . ? C15 C16 C2 122.4(2) . . ? N21 C22 C23 123.9(2) . . ? N21 C22 C3 113.5(2) . . ? C23 C22 C3 122.6(3) . . ? C22 C23 C24 118.5(3) . . ? C22 C23 H12 120.8 . . ? C24 C23 H12 120.8 . . ? C25 C24 C23 117.6(2) . . ? C25 C24 C14 122.6(2) . . ? C23 C24 C14 119.8(2) . . ? C24 C25 C26 119.5(2) . . ? C24 C25 H13 120.2 . . ? C26 C25 H13 120.2 . . ? N21 C26 C25 122.3(3) . . ? N21 C26 C4 114.6(2) . . ? C25 C26 C4 123.1(2) . . ? 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 O4 Ce1 O1 C1 143.8(2) 2_655 . . . ? O7 Ce1 O1 C1 126.9(2) 4_465 . . . ? O9 Ce1 O1 C1 70.3(2) . . . . ? O3 Ce1 O1 C1 -1.7(2) . . . . ? O1 Ce1 O1 C1 -140.0(2) 3_665 . . . ? N21 Ce1 O1 C1 -99.2(2) 4_465 . . . ? O5 Ce1 O1 C1 -68.3(2) 4_465 . . . ? N11 Ce1 O1 C1 1.31(19) . . . . ? O4 Ce1 O1 Ce1 -76.13(8) 2_655 . . 3_665 ? O7 Ce1 O1 Ce1 -93.06(16) 4_465 . . 3_665 ? O9 Ce1 O1 Ce1 -149.70(9) . . . 3_665 ? O3 Ce1 O1 Ce1 138.35(8) . . . 3_665 ? O1 Ce1 O1 Ce1 0.0 3_665 . . 3_665 ? N21 Ce1 O1 Ce1 40.80(13) 4_465 . . 3_665 ? O5 Ce1 O1 Ce1 71.73(8) 4_465 . . 3_665 ? N11 Ce1 O1 Ce1 141.34(11) . . . 3_665 ? O4 Ce1 O3 C2 -121.7(2) 2_655 . . . ? O7 Ce1 O3 C2 -167.4(2) 4_465 . . . ? O9 Ce1 O3 C2 -86.6(2) . . . . ? O1 Ce1 O3 C2 -6.3(2) . . . . ? O1 Ce1 O3 C2 80.4(2) 3_665 . . . ? N21 Ce1 O3 C2 128.0(2) 4_465 . . . ? O5 Ce1 O3 C2 63.7(2) 4_465 . . . ? N11 Ce1 O3 C2 -9.3(2) . . . . ? O4 Ce1 N11 C16 131.65(19) 2_655 . . . ? O7 Ce1 N11 C16 24.8(2) 4_465 . . . ? O9 Ce1 N11 C16 79.2(2) . . . . ? O3 Ce1 N11 C16 -3.30(18) . . . . ? O1 Ce1 N11 C16 179.6(2) . . . . ? O1 Ce1 N11 C16 -142.89(19) 3_665 . . . ? N21 Ce1 N11 C16 -50.0(2) 4_465 . . . ? O5 Ce1 N11 C16 -88.0(2) 4_465 . . . ? O4 Ce1 N11 C12 -39.8(2) 2_655 . . . ? O7 Ce1 N11 C12 -146.58(18) 4_465 . . . ? O9 Ce1 N11 C12 -92.2(2) . . . . ? O3 Ce1 N11 C12 -174.7(2) . . . . ? O1 Ce1 N11 C12 8.23(18) . . . . ? O1 Ce1 N11 C12 45.7(2) 3_665 . . . ? N21 Ce1 N11 C12 138.57(19) 4_465 . . . ? O5 Ce1 N11 C12 100.6(2) 4_465 . . . ? Ce1 O1 C1 O2 167.2(2) . . . . ? Ce1 O1 C1 O2 24.2(3) 3_665 . . . ? Ce1 O1 C1 C12 -9.4(3) . . . . ? Ce1 O1 C1 C12 -152.35(18) 3_665 . . . ? Ce1 O4 C2 O3 106.0(4) 2_645 . . . ? Ce1 O4 C2 C16 -74.2(4) 2_645 . . . ? Ce1 O3 C2 O4 -161.4(2) . . . . ? Ce1 O3 C2 C16 18.9(3) . . . . ? Ce1 O5 C3 O6 -143.4(3) 4_666 . . . ? Ce1 O5 C3 C22 35.2(3) 4_666 . . . ? Ce1 O7 C4 O8 175.9(2) 4_666 . . . ? Ce1 O7 C4 C26 -3.6(3) 4_666 . . . ? C16 N11 C12 C13 -5.4(4) . . . . ? Ce1 N11 C12 C13 166.3(2) . . . . ? C16 N11 C12 C1 172.6(2) . . . . ? Ce1 N11 C12 C1 -15.7(3) . . . . ? O2 C1 C12 N11 -160.6(3) . . . . ? O1 C1 C12 N11 16.1(4) . . . . ? O2 C1 C12 C13 17.4(4) . . . . ? O1 C1 C12 C13 -165.9(3) . . . . ? N11 C12 C13 C14 1.4(4) . . . . ? C1 C12 C13 C14 -176.4(3) . . . . ? C12 C13 C14 C15 3.5(4) . . . . ? C12 C13 C14 C24 -175.0(3) . . . . ? C13 C14 C15 C16 -4.4(4) . . . . ? C24 C14 C15 C16 174.1(3) . . . . ? C12 N11 C16 C15 4.5(4) . . . . ? Ce1 N11 C16 C15 -167.2(2) . . . . ? C12 N11 C16 C2 -175.7(2) . . . . ? Ce1 N11 C16 C2 12.7(3) . . . . ? C14 C15 C16 N11 0.4(4) . . . . ? C14 C15 C16 C2 -179.4(2) . . . . ? O4 C2 C16 N11 160.7(3) . . . . ? O3 C2 C16 N11 -19.5(3) . . . . ? O4 C2 C16 C15 -19.4(4) . . . . ? O3 C2 C16 C15 160.4(3) . . . . ? C26 N21 C22 C23 1.0(4) . . . . ? Ce1 N21 C22 C23 160.1(2) 4_666 . . . ? C26 N21 C22 C3 -177.3(2) . . . . ? Ce1 N21 C22 C3 -18.3(3) 4_666 . . . ? O5 C3 C22 N21 -12.1(4) . . . . ? O6 C3 C22 N21 166.6(3) . . . . ? O5 C3 C22 C23 169.5(3) . . . . ? O6 C3 C22 C23 -11.7(4) . . . . ? N21 C22 C23 C24 1.3(5) . . . . ? C3 C22 C23 C24 179.5(3) . . . . ? C22 C23 C24 C25 -2.1(4) . . . . ? C22 C23 C24 C14 176.8(3) . . . . ? C13 C14 C24 C25 169.6(3) . . . . ? C15 C14 C24 C25 -8.9(4) . . . . ? C13 C14 C24 C23 -9.3(4) . . . . ? C15 C14 C24 C23 172.3(3) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C14 C24 C25 C26 -178.3(3) . . . . ? C22 N21 C26 C25 -2.6(4) . . . . ? Ce1 N21 C26 C25 -161.1(2) 4_666 . . . ? C22 N21 C26 C4 175.4(2) . . . . ? Ce1 N21 C26 C4 16.9(3) 4_666 . . . ? C24 C25 C26 N21 1.8(4) . . . . ? C24 C25 C26 C4 -176.0(3) . . . . ? O8 C4 C26 N21 171.5(3) . . . . ? O7 C4 C26 N21 -9.0(4) . . . . ? O8 C4 C26 C25 -10.6(4) . . . . ? O7 C4 C26 C25 169.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.567 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.106 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 702668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H7 N2 O9 Sm, 3(H2 O)' _chemical_formula_sum 'C14 H13 N2 O12 Sm' _chemical_formula_weight 551.61 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' Sm Sm -0.1638 3.4418 '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 ' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.0648(12) _cell_length_b 12.5148(13) _cell_length_c 12.3787(13) _cell_angle_alpha 90.00 _cell_angle_beta 115.069(2) _cell_angle_gamma 90.00 _cell_volume 1693.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3456 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 3.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _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 'Bruker Smart Apex. CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8284 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2974 _reflns_number_gt 2763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart (Bruker,2000)' _computing_cell_refinement 'Saintplus (Bruker.2000)' _computing_data_reduction 'Saintplus (Bruker.2000)' _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^)+(0.0715P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2974 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Sm1 Sm -0.04033(2) 0.449250(19) 0.64517(2) 0.01209(14) Uani 1 1 d . . . O1 O 0.1187(3) 0.4953(3) 0.5708(3) 0.0175(8) Uani 1 1 d . . . O2 O 0.2947(4) 0.4595(3) 0.5611(4) 0.0248(9) Uani 1 1 d . . . O3 O -0.0211(3) 0.2960(3) 0.7805(3) 0.0194(8) Uani 1 1 d . . . O4 O 0.0613(3) 0.1402(3) 0.8643(3) 0.0212(8) Uani 1 1 d . . . O5 O 0.9391(3) 0.2148(3) 1.0155(3) 0.0193(8) Uani 1 1 d . . . O6 O 0.8075(3) 0.2682(4) 0.8351(4) 0.0386(11) Uani 1 1 d . . . H1 H 0.8704 0.2824 0.8278 0.058 Uiso 1 1 calc R . . O7 O 0.8186(3) 0.0123(3) 1.2369(3) 0.0180(7) Uani 1 1 d . . . O8 O 0.6337(4) 0.0222(4) 1.2386(4) 0.0338(10) Uani 1 1 d . . . O9 O 0.0929(4) 0.5182(3) 0.8445(3) 0.0308(9) Uani 1 1 d . . . H2 H 0.1098 0.4621 0.9021 0.037 Uiso 1 1 d R . . H3 H 0.1682 0.5431 0.8447 0.037 Uiso 1 1 d R . . O10 O 0.5803(7) 0.9045(7) 0.3957(7) 0.109(3) Uani 1 1 d . . . H4 H 0.6244 0.9513 0.4448 0.131 Uiso 1 1 d R . . H5 H 0.5441 0.9324 0.3269 0.131 Uiso 1 1 d R . . O11 O 0.8696(5) 0.8953(4) 0.4541(4) 0.0515(13) Uani 1 1 d . . . H6 H 0.8689 0.9369 0.3995 0.062 Uiso 1 1 d R . . H7 H 0.8919 0.8331 0.4437 0.062 Uiso 1 1 d R . . O12 O 0.3370(17) 0.555(4) 0.914(3) 0.054(9) Uani 0.45(9) 1 d P A 1 O12' O 0.326(2) 0.592(3) 0.860(6) 0.094(12) Uani 0.55(9) 1 d P A 2 N11 N 0.1588(4) 0.3398(3) 0.7272(3) 0.0157(9) Uani 1 1 d . . . N21 N 0.7572(4) 0.1482(3) 1.0631(3) 0.0143(9) Uani 1 1 d . . . C1 C 0.2242(5) 0.4477(4) 0.6063(5) 0.0173(12) Uani 1 1 d . . . C2 C 0.0649(4) 0.2272(4) 0.8201(4) 0.0130(10) Uani 1 1 d . . . C3 C 0.8355(5) 0.2311(4) 0.9408(5) 0.0193(11) Uani 1 1 d . . . C4 C 0.7084(5) 0.0446(4) 1.1993(5) 0.0180(12) Uani 1 1 d . . . C12 C 0.2531(4) 0.3706(4) 0.7052(4) 0.0154(10) Uani 1 1 d . . . C13 C 0.3699(5) 0.3298(4) 0.7678(4) 0.0199(11) Uani 1 1 d . . . H10 H 0.4337 0.3544 0.7512 0.024 Uiso 1 1 calc R . . C14 C 0.3922(4) 0.2531(4) 0.8546(4) 0.0174(11) Uani 1 1 d . . . C15 C 0.2913(5) 0.2159(4) 0.8708(4) 0.0169(11) Uani 1 1 d . . . H11 H 0.3005 0.1615 0.9251 0.020 Uiso 1 1 calc R . . C16 C 0.1785(4) 0.2603(4) 0.8061(4) 0.0158(10) Uani 1 1 d . . . C22 C 0.7281(4) 0.2078(4) 0.9665(4) 0.0174(11) Uani 1 1 d . . . C23 C 0.6114(5) 0.2415(4) 0.8955(5) 0.0210(12) Uani 1 1 d . . . H12 H 0.5955 0.2823 0.8277 0.025 Uiso 1 1 calc R . . C24 C 0.5178(5) 0.2139(4) 0.9267(4) 0.0187(11) Uani 1 1 d . . . C25 C 0.5481(4) 0.1507(4) 1.0283(4) 0.0169(11) Uani 1 1 d . . . H13 H 0.4879 0.1299 1.0522 0.020 Uiso 1 1 calc R . . C26 C 0.6677(5) 0.1193(4) 1.0929(4) 0.0149(11) 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 Sm1 0.01018(19) 0.0136(2) 0.01241(19) 0.00012(9) 0.00469(13) -0.00037(9) O1 0.0133(19) 0.021(2) 0.0172(18) 0.0057(15) 0.0051(15) 0.0051(15) O2 0.025(2) 0.031(2) 0.027(2) 0.0060(15) 0.018(2) 0.0049(16) O3 0.0128(18) 0.025(2) 0.0239(19) 0.0089(15) 0.0116(16) 0.0009(15) O4 0.0175(19) 0.020(2) 0.029(2) 0.0057(15) 0.0127(17) 0.0027(15) O5 0.0116(19) 0.022(2) 0.025(2) 0.0028(15) 0.0076(16) 0.0010(14) O6 0.017(2) 0.064(3) 0.040(3) 0.031(2) 0.016(2) 0.011(2) O7 0.0128(19) 0.0239(19) 0.0165(18) 0.0048(15) 0.0054(15) 0.0013(15) O8 0.027(2) 0.047(3) 0.036(3) 0.020(2) 0.021(2) 0.007(2) O9 0.031(2) 0.034(2) 0.024(2) -0.0052(18) 0.0093(19) -0.0041(19) O10 0.124(7) 0.134(6) 0.090(5) 0.053(5) 0.066(5) -0.005(6) O11 0.075(4) 0.056(3) 0.024(2) 0.015(2) 0.022(2) 0.017(3) O12 0.032(10) 0.068(15) 0.064(15) -0.011(10) 0.023(9) -0.022(7) O12' 0.104(13) 0.061(15) 0.14(3) -0.036(17) 0.070(14) -0.026(10) N11 0.014(2) 0.017(2) 0.015(2) 0.0033(17) 0.0048(18) -0.0017(17) N21 0.013(2) 0.017(2) 0.017(2) 0.0049(17) 0.0091(18) 0.0007(17) C1 0.018(3) 0.016(3) 0.015(3) -0.0043(19) 0.005(2) -0.0052(19) C2 0.011(2) 0.017(3) 0.010(2) -0.003(2) 0.004(2) 0.0024(19) C3 0.018(3) 0.018(3) 0.024(3) 0.010(2) 0.011(2) 0.004(2) C4 0.019(3) 0.023(3) 0.015(3) 0.0002(19) 0.009(2) 0.003(2) C12 0.011(3) 0.016(3) 0.018(3) -0.003(2) 0.005(2) 0.0026(19) C13 0.013(3) 0.025(3) 0.026(3) 0.009(2) 0.013(2) 0.003(2) C14 0.012(3) 0.019(3) 0.024(3) 0.001(2) 0.010(2) 0.001(2) C15 0.016(3) 0.015(3) 0.020(3) 0.005(2) 0.007(2) 0.002(2) C16 0.015(3) 0.016(3) 0.018(3) 0.002(2) 0.008(2) -0.001(2) C22 0.014(3) 0.022(3) 0.017(3) 0.005(2) 0.008(2) 0.004(2) C23 0.019(3) 0.024(3) 0.022(3) 0.010(2) 0.011(2) 0.006(2) C24 0.017(3) 0.019(3) 0.019(3) 0.004(2) 0.007(2) 0.006(2) C25 0.015(3) 0.018(3) 0.018(3) 0.002(2) 0.008(2) -0.003(2) C26 0.014(3) 0.015(3) 0.016(3) 0.000(2) 0.007(2) 0.002(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 Sm1 O4 2.401(4) 2_556 ? Sm1 O9 2.461(4) . ? Sm1 O7 2.461(3) 4_465 ? Sm1 O3 2.493(3) . ? Sm1 O1 2.521(3) . ? Sm1 O1 2.526(3) 3_566 ? Sm1 N21 2.526(4) 4_465 ? Sm1 O5 2.552(3) 4_465 ? Sm1 N11 2.572(4) . ? O1 C1 1.301(6) . ? O1 Sm1 2.526(3) 3_566 ? O2 C1 1.209(7) . ? O3 C2 1.275(6) . ? O4 C2 1.228(6) . ? O4 Sm1 2.401(4) 2_546 ? O5 C3 1.217(6) . ? O5 Sm1 2.552(3) 4_666 ? O6 C3 1.291(6) . ? O6 H1 0.8200 . ? O7 C4 1.274(7) . ? O7 Sm1 2.461(3) 4_666 ? O8 C4 1.224(7) . ? O9 H2 0.9600 . ? O9 H3 0.9599 . ? O10 H4 0.8501 . ? O10 H5 0.8499 . ? O11 H6 0.8501 . ? O11 H7 0.8500 . ? N11 C12 1.333(6) . ? N11 C16 1.344(6) . ? N21 C22 1.325(6) . ? N21 C26 1.331(6) . ? N21 Sm1 2.526(4) 4_666 ? C1 C12 1.480(7) . ? C2 C16 1.509(6) . ? C3 C22 1.487(6) . ? C4 C26 1.518(7) . ? C12 C13 1.386(7) . ? C13 C14 1.380(7) . ? C13 H10 0.9300 . ? C14 C15 1.396(7) . ? C14 C24 1.479(7) . ? C15 C16 1.371(7) . ? C15 H11 0.9300 . ? C22 C23 1.374(7) . ? C23 C24 1.383(7) . ? C23 H12 0.9300 . ? C24 C25 1.396(7) . ? C25 C26 1.378(7) . ? C25 H13 0.9300 . ? 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 O4 Sm1 O9 73.16(13) 2_556 . ? O4 Sm1 O7 75.45(11) 2_556 4_465 ? O9 Sm1 O7 75.78(12) . 4_465 ? O4 Sm1 O3 140.97(11) 2_556 . ? O9 Sm1 O3 76.16(13) . . ? O7 Sm1 O3 74.08(11) 4_465 . ? O4 Sm1 O1 80.53(11) 2_556 . ? O9 Sm1 O1 90.64(13) . . ? O7 Sm1 O1 154.94(13) 4_465 . ? O3 Sm1 O1 123.57(11) . . ? O4 Sm1 O1 71.96(11) 2_556 3_566 ? O9 Sm1 O1 139.21(13) . 3_566 ? O7 Sm1 O1 114.39(11) 4_465 3_566 ? O3 Sm1 O1 144.06(12) . 3_566 ? O1 Sm1 O1 63.39(13) . 3_566 ? O4 Sm1 N21 113.41(12) 2_556 4_465 ? O9 Sm1 N21 133.00(13) . 4_465 ? O7 Sm1 N21 62.63(11) 4_465 4_465 ? O3 Sm1 N21 72.37(12) . 4_465 ? O1 Sm1 N21 135.98(12) . 4_465 ? O1 Sm1 N21 80.97(12) 3_566 4_465 ? O4 Sm1 O5 142.16(11) 2_556 4_465 ? O9 Sm1 O5 139.54(12) . 4_465 ? O7 Sm1 O5 123.07(11) 4_465 4_465 ? O3 Sm1 O5 76.14(12) . 4_465 ? O1 Sm1 O5 80.81(11) . 4_465 ? O1 Sm1 O5 70.27(11) 3_566 4_465 ? N21 Sm1 O5 62.54(11) 4_465 4_465 ? O4 Sm1 N11 127.66(12) 2_556 . ? O9 Sm1 N11 71.76(13) . . ? O7 Sm1 N11 129.44(12) 4_465 . ? O3 Sm1 N11 61.29(11) . . ? O1 Sm1 N11 62.45(11) . . ? O1 Sm1 N11 115.60(11) 3_566 . ? N21 Sm1 N11 118.93(14) 4_465 . ? O5 Sm1 N11 69.24(12) 4_465 . ? C1 O1 Sm1 124.0(3) . . ? C1 O1 Sm1 110.9(3) . 3_566 ? Sm1 O1 Sm1 116.61(13) . 3_566 ? C2 O3 Sm1 127.3(3) . . ? C2 O4 Sm1 152.1(3) . 2_546 ? C3 O5 Sm1 114.1(3) . 4_666 ? C3 O6 H1 109.5 . . ? C4 O7 Sm1 126.0(3) . 4_666 ? Sm1 O9 H2 109.4 . . ? Sm1 O9 H3 109.4 . . ? H2 O9 H3 109.5 . . ? H4 O10 H5 109.5 . . ? H6 O11 H7 109.8 . . ? C12 N11 C16 117.4(4) . . ? C12 N11 Sm1 120.0(3) . . ? C16 N11 Sm1 121.9(3) . . ? C22 N21 C26 117.9(4) . . ? C22 N21 Sm1 118.4(3) . 4_666 ? C26 N21 Sm1 121.1(3) . 4_666 ? O2 C1 O1 124.6(5) . . ? O2 C1 C12 119.8(5) . . ? O1 C1 C12 115.5(5) . . ? O4 C2 O3 126.3(4) . . ? O4 C2 C16 120.0(4) . . ? O3 C2 C16 113.7(4) . . ? O5 C3 O6 125.0(5) . . ? O5 C3 C22 120.8(4) . . ? O6 C3 C22 114.2(4) . . ? O8 C4 O7 127.8(5) . . ? O8 C4 C26 117.6(5) . . ? O7 C4 C26 114.6(5) . . ? N11 C12 C13 122.1(5) . . ? N11 C12 C1 115.8(4) . . ? C13 C12 C1 122.0(5) . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H10 119.7 . . ? C12 C13 H10 119.7 . . ? C13 C14 C15 116.7(5) . . ? C13 C14 C24 120.9(5) . . ? C15 C14 C24 122.4(5) . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H11 120.3 . . ? C14 C15 H11 120.3 . . ? N11 C16 C15 123.4(5) . . ? N11 C16 C2 113.4(4) . . ? C15 C16 C2 123.1(4) . . ? N21 C22 C23 123.9(4) . . ? N21 C22 C3 112.5(4) . . ? C23 C22 C3 123.6(4) . . ? C22 C23 C24 118.8(5) . . ? C22 C23 H12 120.6 . . ? C24 C23 H12 120.6 . . ? C23 C24 C25 117.4(5) . . ? C23 C24 C14 119.8(5) . . ? C25 C24 C14 122.8(5) . . ? C26 C25 C24 119.7(4) . . ? C26 C25 H13 120.2 . . ? C24 C25 H13 120.2 . . ? N21 C26 C25 122.3(5) . . ? N21 C26 C4 114.0(4) . . ? C25 C26 C4 123.6(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.021 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.126 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 702669' _audit_creation_date 'Sun Aug 19 14:29:10 2007' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Tb4(BPTCA)3(OH2)8] ; _chemical_name_common (Tb4(BPTCA)3(OH2)8) _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 N6 O32 Tb4 ' _chemical_formula_sum 'C42 H28 N6 O32 Tb4' _chemical_formula_weight 1764.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tb Tb -0.1723 4.1537 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 12.130(4) _cell_length_b 22.320(7) _cell_length_c 21.819(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.325(12) _cell_angle_gamma 90.00 _cell_volume 5697(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 11328 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 5.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 20483 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5015 _reflns_number_gt 3700 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.1299P)^2^+538.9194P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5015 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1343 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.2811 _refine_ls_wR_factor_gt 0.2550 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.0000 0.21250(6) 0.2500 0.0428(4) Uani 1 2 d S . . Tb2 Tb 0.5000 0.25299(6) 0.2500 0.0404(4) Uani 1 2 d S . . Tb3 Tb 0.13779(9) 0.63047(8) 0.52555(5) 0.0737(5) Uani 1 1 d U . . O1 O 0.6439(13) 0.3245(8) 0.3017(6) 0.057(4) Uani 1 1 d . . . O2 O 0.7148(11) 0.3889(6) 0.3817(6) 0.041(3) Uani 1 1 d . . . O3 O 0.3261(13) 0.2262(6) 0.2762(6) 0.046(3) Uani 1 1 d . . . O4 O 0.1784(13) 0.2532(6) 0.3125(7) 0.050(4) Uani 1 1 d . . . O5 O 0.3042(19) 0.6565(8) 0.4894(10) 0.089(4) Uani 1 1 d . . . O6 O 0.408(3) 0.6372(16) 0.4225(17) 0.172(9) Uani 1 1 d U . . O7 O 0.0559(18) 0.5419(8) 0.5338(10) 0.089(4) Uani 1 1 d D . . O8 O 0.166(3) 0.4502(14) 0.5827(15) 0.172(9) Uani 1 1 d D . . O9 O 0.0436(15) 0.2629(8) 0.1583(7) 0.060(4) Uani 1 1 d . . . O10 O 0.0365(15) 0.3445(9) 0.0978(7) 0.078(6) Uani 1 1 d . . . O11 O 0.0760(14) 0.7052(7) 0.3525(6) 0.055(4) Uani 1 1 d . . . O12 O 0.0888(17) 0.6229(8) 0.4131(7) 0.076(5) Uani 1 1 d . . . O13 O 0.1483(15) 0.1550(8) 0.2171(9) 0.072(5) Uani 1 1 d . . . O14 O 0.0765(16) 0.1414(8) 0.3364(9) 0.077(5) Uani 1 1 d . . . O15 O 0.198(3) 0.7280(9) 0.5662(13) 0.128(10) Uani 1 1 d U . . O16 O -0.052(4) 0.666(2) 0.4728(19) 0.220(18) Uani 1 1 d U . . N11 N 0.4500(14) 0.3161(7) 0.3313(7) 0.038(4) Uani 1 1 d . . . N21 N 0.2448(15) 0.5446(9) 0.4940(7) 0.051(4) Uani 1 1 d . . . C5 C 0.0374(19) 0.3158(13) 0.1496(11) 0.059(6) Uani 1 1 d . . . C6 C 0.0689(19) 0.6502(12) 0.3605(10) 0.058(6) Uani 1 1 d . . . C1 C 0.6371(17) 0.3590(9) 0.3471(9) 0.042(5) Uani 1 1 d D . . C12 C 0.5192(15) 0.3604(8) 0.3607(8) 0.041(5) Uani 1 1 d D . . C13 C 0.4850(15) 0.4041(8) 0.3955(8) 0.039(4) Uani 1 1 d D . . H1 H 0.5367 0.4347 0.4151 0.047 Uiso 1 1 calc R . . C14 C 0.3735(16) 0.4034(8) 0.4021(9) 0.045(5) Uani 1 1 d D . . C15 C 0.3050(18) 0.3550(9) 0.3768(9) 0.050(5) Uani 1 1 d D . . H2 H 0.2308 0.3510 0.3832 0.060 Uiso 1 1 calc R . . C16 C 0.3464(16) 0.3123(8) 0.3420(8) 0.042(5) Uani 1 1 d D . . C2 C 0.2767(19) 0.2584(9) 0.3065(8) 0.047(5) Uani 1 1 d D . . C3 C 0.344(4) 0.6219(12) 0.456(2) 0.120(9) Uani 1 1 d D . . C22 C 0.317(2) 0.5552(10) 0.4595(12) 0.069(5) Uani 1 1 d D . . C23 C 0.363(2) 0.5107(9) 0.4311(12) 0.066(5) Uani 1 1 d D . . H3 H 0.4162 0.5201 0.4075 0.079 Uiso 1 1 calc R . . C24 C 0.3311(17) 0.4512(9) 0.4369(9) 0.052(6) Uani 1 1 d D . . C25 C 0.251(2) 0.4430(9) 0.4715(12) 0.066(5) Uani 1 1 d D . . H4 H 0.2236 0.4038 0.4756 0.079 Uiso 1 1 calc R . . C26 C 0.211(2) 0.4905(10) 0.5002(13) 0.069(5) Uani 1 1 d D . . C4 C 0.1297(17) 0.4971(9) 0.5446(11) 0.120(9) Uani 1 1 d DU . . N31 N 0.0000 0.3263(10) 0.2500 0.047(6) Uani 1 2 d SD . . C32 C 0.017(2) 0.3572(9) 0.2011(10) 0.053(5) Uani 1 1 d D . . C33 C 0.018(2) 0.4180(9) 0.1991(12) 0.076(8) Uani 1 1 d D . . H5 H 0.0303 0.4380 0.1631 0.092 Uiso 1 1 calc R . . C34 C 0.0000 0.4510(11) 0.2500 0.059(9) Uani 1 2 d SD . . N41 N 0.0000 0.6413(10) 0.2500 0.052(6) Uani 1 2 d SD . . C42 C 0.031(2) 0.6092(8) 0.3029(9) 0.062(7) Uani 1 1 d D . . C43 C 0.033(2) 0.5486(10) 0.3055(10) 0.069(7) Uani 1 1 d D . . H6 H 0.0559 0.5289 0.3454 0.083 Uiso 1 1 calc R . . C44 C 0.0000 0.5153(16) 0.2500 0.092(14) Uani 1 2 d SD . . 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 0.0563(9) 0.0447(8) 0.0381(7) 0.000 0.0313(6) 0.000 Tb2 0.0503(8) 0.0518(8) 0.0213(6) 0.000 0.0133(5) 0.000 Tb3 0.0428(6) 0.1495(14) 0.0315(6) -0.0382(7) 0.0148(5) 0.0074(7) O1 0.067(10) 0.090(11) 0.024(7) -0.002(7) 0.028(7) 0.002(9) O2 0.045(8) 0.045(7) 0.035(7) 0.003(6) 0.016(6) -0.002(6) O3 0.063(9) 0.053(8) 0.022(6) -0.010(6) 0.011(6) -0.008(7) O4 0.055(9) 0.057(9) 0.047(8) -0.010(7) 0.030(7) -0.017(7) O5 0.120(12) 0.071(8) 0.105(11) -0.011(8) 0.082(10) 0.010(8) O6 0.215(17) 0.187(16) 0.152(14) -0.024(13) 0.116(14) -0.009(14) O7 0.120(12) 0.071(8) 0.105(11) -0.011(8) 0.082(10) 0.010(8) O8 0.215(17) 0.187(16) 0.152(14) -0.024(13) 0.116(14) -0.009(14) O9 0.088(12) 0.061(10) 0.050(9) -0.007(8) 0.052(9) -0.007(9) O10 0.074(11) 0.130(16) 0.040(9) 0.024(10) 0.031(8) -0.023(11) O11 0.076(11) 0.047(9) 0.035(8) 0.007(6) -0.001(7) -0.009(8) O12 0.095(14) 0.083(12) 0.038(9) 0.012(8) -0.002(9) -0.016(10) O13 0.066(11) 0.079(12) 0.077(12) -0.037(10) 0.029(9) 0.002(9) O14 0.076(12) 0.069(11) 0.085(13) 0.017(10) 0.018(10) 0.006(10) O15 0.21(3) 0.069(12) 0.16(2) 0.050(13) 0.15(2) 0.063(15) O16 0.21(3) 0.27(4) 0.17(3) -0.04(3) 0.03(2) 0.14(3) N11 0.045(9) 0.038(8) 0.028(8) 0.002(6) 0.010(7) -0.001(7) N21 0.053(10) 0.076(12) 0.032(9) -0.013(8) 0.026(8) -0.005(9) C5 0.049(13) 0.089(19) 0.050(13) -0.025(13) 0.032(11) -0.027(13) C6 0.048(13) 0.081(18) 0.039(12) -0.001(11) -0.001(10) -0.005(12) C1 0.044(11) 0.056(12) 0.030(10) 0.010(9) 0.018(9) 0.006(10) C12 0.044(11) 0.057(12) 0.026(9) 0.003(8) 0.015(8) -0.003(10) C13 0.043(11) 0.046(11) 0.028(9) -0.002(8) 0.007(8) -0.001(9) C14 0.064(13) 0.045(11) 0.034(10) -0.005(9) 0.025(9) -0.016(10) C15 0.071(15) 0.053(12) 0.030(10) -0.010(9) 0.021(10) -0.007(11) C16 0.051(12) 0.050(11) 0.028(9) -0.006(8) 0.017(8) -0.013(9) C2 0.064(14) 0.058(13) 0.024(9) -0.002(9) 0.019(9) -0.010(11) C3 0.125(16) 0.118(15) 0.143(17) 0.055(13) 0.081(14) 0.005(13) C22 0.080(12) 0.078(12) 0.073(12) -0.007(10) 0.060(11) -0.007(10) C23 0.095(13) 0.056(9) 0.069(11) -0.002(8) 0.059(11) -0.014(9) C24 0.048(12) 0.076(15) 0.040(11) -0.024(11) 0.023(9) -0.015(11) C25 0.095(13) 0.056(9) 0.069(11) -0.002(8) 0.059(11) -0.014(9) C26 0.080(12) 0.078(12) 0.073(12) -0.007(10) 0.060(11) -0.007(10) C4 0.125(16) 0.118(15) 0.143(17) 0.055(13) 0.081(14) 0.005(13) N31 0.057(15) 0.050(14) 0.044(13) 0.000 0.031(12) 0.000 C32 0.060(14) 0.052(12) 0.053(13) 0.002(10) 0.026(11) -0.012(11) C33 0.09(2) 0.055(15) 0.083(19) 0.008(13) 0.019(16) -0.030(14) C34 0.09(3) 0.021(13) 0.07(2) 0.000 0.026(19) 0.000 N41 0.062(16) 0.047(14) 0.039(14) 0.000 0.001(12) 0.000 C42 0.089(18) 0.035(11) 0.047(12) -0.004(9) -0.011(12) -0.004(12) C43 0.070(16) 0.067(16) 0.052(14) -0.003(12) -0.017(12) 0.000(13) C44 0.07(3) 0.11(4) 0.09(3) 0.000 0.00(2) 0.000 _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 O4 2.410(14) . ? Tb1 O4 2.410(14) 2 ? Tb1 O14 2.450(18) 2 ? Tb1 O14 2.450(18) . ? Tb1 O13 2.465(15) . ? Tb1 O13 2.465(15) 2 ? Tb1 O9 2.472(14) 2 ? Tb1 O9 2.472(14) . ? Tb1 N31 2.54(2) . ? Tb2 O3 2.403(15) 2_655 ? Tb2 O3 2.403(15) . ? Tb2 O1 2.413(16) . ? Tb2 O1 2.413(16) 2_655 ? Tb2 O11 2.428(13) 3_545 ? Tb2 O11 2.428(13) 4_545 ? Tb2 N11 2.464(15) 2_655 ? Tb2 N11 2.464(15) . ? Tb2 N41 2.49(2) 3_545 ? Tb3 O7 2.24(2) . ? Tb3 O10 2.309(14) 6_566 ? Tb3 O2 2.359(13) 5_666 ? Tb3 O12 2.374(16) . ? Tb3 O15 2.39(3) . ? Tb3 O16 2.42(4) . ? Tb3 O5 2.423(19) . ? Tb3 N21 2.510(18) . ? Tb3 C4 3.01(2) . ? O1 C1 1.27(2) . ? O2 C1 1.24(2) . ? O2 Tb3 2.359(13) 5_666 ? O3 C2 1.23(2) . ? O4 C2 1.24(2) . ? O5 C3 1.24(4) . ? O6 C3 1.25(4) . ? O7 C4 1.323(18) . ? O8 C4 1.34(4) . ? O9 C5 1.20(3) . ? O10 C5 1.30(3) . ? O10 Tb3 2.309(14) 6_565 ? O11 C6 1.25(3) . ? O11 Tb2 2.428(13) 3_455 ? O12 C6 1.26(3) . ? N11 C16 1.34(2) . ? N11 C12 1.34(2) . ? N21 C26 1.29(3) . ? N21 C22 1.32(2) . ? C5 C32 1.52(3) . ? C6 C42 1.53(3) . ? C1 C12 1.53(2) . ? C12 C13 1.37(2) . ? C13 C14 1.40(2) . ? C13 H1 0.9500 . ? C14 C15 1.39(2) . ? C14 C24 1.48(3) . ? C15 C16 1.39(2) . ? C15 H2 0.9500 . ? C16 C2 1.55(2) . ? C3 C22 1.53(3) . ? C22 C23 1.36(2) . ? C23 C24 1.40(2) . ? C23 H3 0.9500 . ? C24 C25 1.39(2) . ? C25 C26 1.38(2) . ? C25 H4 0.9500 . ? C26 C4 1.57(2) . ? N31 C32 1.332(19) . ? N31 C32 1.332(19) 2 ? C32 C33 1.36(2) . ? C33 C34 1.40(2) . ? C33 H5 0.9500 . ? C34 C33 1.40(2) 2 ? C34 C44 1.44(5) . ? N41 C42 1.33(2) . ? N41 C42 1.33(2) 2 ? N41 Tb2 2.49(2) 3_455 ? C42 C43 1.35(2) . ? C43 C44 1.39(2) . ? C43 H6 0.9500 . ? C44 C43 1.39(2) 2 ? 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 O4 Tb1 O4 135.7(7) . 2 ? O4 Tb1 O14 141.3(6) . 2 ? O4 Tb1 O14 73.0(6) 2 2 ? O4 Tb1 O14 73.0(6) . . ? O4 Tb1 O14 141.3(6) 2 . ? O14 Tb1 O14 99.3(9) 2 . ? O4 Tb1 O13 75.3(5) . . ? O4 Tb1 O13 130.3(5) 2 . ? O14 Tb1 O13 66.2(6) 2 . ? O14 Tb1 O13 74.3(7) . . ? O4 Tb1 O13 130.3(5) . 2 ? O4 Tb1 O13 75.3(5) 2 2 ? O14 Tb1 O13 74.3(7) 2 2 ? O14 Tb1 O13 66.2(6) . 2 ? O13 Tb1 O13 117.3(9) . 2 ? O4 Tb1 O9 73.9(5) . 2 ? O4 Tb1 O9 86.2(5) 2 2 ? O14 Tb1 O9 143.0(6) 2 2 ? O14 Tb1 O9 77.9(6) . 2 ? O13 Tb1 O9 143.3(6) . 2 ? O13 Tb1 O9 70.9(6) 2 2 ? O4 Tb1 O9 86.2(5) . . ? O4 Tb1 O9 73.9(5) 2 . ? O14 Tb1 O9 77.9(6) 2 . ? O14 Tb1 O9 143.0(6) . . ? O13 Tb1 O9 70.9(6) . . ? O13 Tb1 O9 143.3(6) 2 . ? O9 Tb1 O9 125.8(7) 2 . ? O4 Tb1 N31 67.9(4) . . ? O4 Tb1 N31 67.9(4) 2 . ? O14 Tb1 N31 130.3(5) 2 . ? O14 Tb1 N31 130.3(5) . . ? O13 Tb1 N31 121.3(4) . . ? O13 Tb1 N31 121.3(4) 2 . ? O9 Tb1 N31 62.9(4) 2 . ? O9 Tb1 N31 62.9(4) . . ? O3 Tb2 O3 151.2(7) 2_655 . ? O3 Tb2 O1 72.8(5) 2_655 . ? O3 Tb2 O1 128.7(4) . . ? O3 Tb2 O1 128.7(4) 2_655 2_655 ? O3 Tb2 O1 72.8(5) . 2_655 ? O1 Tb2 O1 97.2(8) . 2_655 ? O3 Tb2 O11 88.1(5) 2_655 3_545 ? O3 Tb2 O11 79.3(5) . 3_545 ? O1 Tb2 O11 79.0(5) . 3_545 ? O1 Tb2 O11 140.6(5) 2_655 3_545 ? O3 Tb2 O11 79.3(5) 2_655 4_545 ? O3 Tb2 O11 88.1(5) . 4_545 ? O1 Tb2 O11 140.6(5) . 4_545 ? O1 Tb2 O11 79.0(5) 2_655 4_545 ? O11 Tb2 O11 127.9(7) 3_545 4_545 ? O3 Tb2 N11 64.7(5) 2_655 2_655 ? O3 Tb2 N11 135.5(5) . 2_655 ? O1 Tb2 N11 70.9(5) . 2_655 ? O1 Tb2 N11 64.6(5) 2_655 2_655 ? O11 Tb2 N11 143.9(5) 3_545 2_655 ? O11 Tb2 N11 72.2(5) 4_545 2_655 ? O3 Tb2 N11 135.5(5) 2_655 . ? O3 Tb2 N11 64.7(5) . . ? O1 Tb2 N11 64.6(5) . . ? O1 Tb2 N11 70.9(5) 2_655 . ? O11 Tb2 N11 72.2(5) 3_545 . ? O11 Tb2 N11 143.9(5) 4_545 . ? N11 Tb2 N11 110.3(7) 2_655 . ? O3 Tb2 N41 75.6(3) 2_655 3_545 ? O3 Tb2 N41 75.6(3) . 3_545 ? O1 Tb2 N41 131.4(4) . 3_545 ? O1 Tb2 N41 131.4(4) 2_655 3_545 ? O11 Tb2 N41 63.9(3) 3_545 3_545 ? O11 Tb2 N41 63.9(3) 4_545 3_545 ? N11 Tb2 N41 124.9(3) 2_655 3_545 ? N11 Tb2 N41 124.9(3) . 3_545 ? O7 Tb3 O10 80.3(7) . 6_566 ? O7 Tb3 O2 91.2(7) . 5_666 ? O10 Tb3 O2 83.0(5) 6_566 5_666 ? O7 Tb3 O12 91.4(7) . . ? O10 Tb3 O12 133.7(7) 6_566 . ? O2 Tb3 O12 143.1(6) 5_666 . ? O7 Tb3 O15 150.7(7) . . ? O10 Tb3 O15 72.1(7) 6_566 . ? O2 Tb3 O15 76.1(8) 5_666 . ? O12 Tb3 O15 114.6(7) . . ? O7 Tb3 O16 86.6(15) . . ? O10 Tb3 O16 68.6(10) 6_566 . ? O2 Tb3 O16 151.5(10) 5_666 . ? O12 Tb3 O16 65.4(10) . . ? O15 Tb3 O16 92.2(13) . . ? O7 Tb3 O5 131.5(6) . . ? O10 Tb3 O5 143.4(7) 6_566 . ? O2 Tb3 O5 79.4(6) 5_666 . ? O12 Tb3 O5 71.5(7) . . ? O15 Tb3 O5 72.7(7) . . ? O16 Tb3 O5 122.4(14) . . ? O7 Tb3 N21 67.7(6) . . ? O10 Tb3 N21 141.2(7) 6_566 . ? O2 Tb3 N21 76.5(5) 5_666 . ? O12 Tb3 N21 70.6(6) . . ? O15 Tb3 N21 131.8(8) . . ? O16 Tb3 N21 127.9(10) . . ? O5 Tb3 N21 63.8(6) . . ? O7 Tb3 C4 23.9(5) . . ? O10 Tb3 C4 95.9(7) 6_566 . ? O2 Tb3 C4 75.3(5) 5_666 . ? O12 Tb3 C4 93.6(6) . . ? O15 Tb3 C4 150.1(8) . . ? O16 Tb3 C4 109.1(13) . . ? O5 Tb3 C4 110.0(6) . . ? N21 Tb3 C4 47.3(6) . . ? C1 O1 Tb2 125.1(13) . . ? C1 O2 Tb3 135.0(12) . 5_666 ? C2 O3 Tb2 124.4(13) . . ? C2 O4 Tb1 136.1(12) . . ? C3 O5 Tb3 122(2) . . ? C4 O7 Tb3 112.8(13) . . ? C5 O9 Tb1 124.1(13) . . ? C5 O10 Tb3 146.3(17) . 6_565 ? C6 O11 Tb2 122.6(13) . 3_455 ? C6 O12 Tb3 147.0(17) . . ? C16 N11 C12 117.4(15) . . ? C16 N11 Tb2 120.6(11) . . ? C12 N11 Tb2 121.4(12) . . ? C26 N21 C22 120.0(18) . . ? C26 N21 Tb3 119.1(13) . . ? C22 N21 Tb3 119.4(15) . . ? O9 C5 O10 128(2) . . ? O9 C5 C32 120(2) . . ? O10 C5 C32 112(2) . . ? O11 C6 O12 127(2) . . ? O11 C6 C42 119.5(19) . . ? O12 C6 C42 114(2) . . ? O2 C1 O1 127.2(18) . . ? O2 C1 C12 118.0(16) . . ? O1 C1 C12 114.7(18) . . ? N11 C12 C13 123.1(16) . . ? N11 C12 C1 112.9(16) . . ? C13 C12 C1 123.9(16) . . ? C12 C13 C14 119.6(16) . . ? C12 C13 H1 120.2 . . ? C14 C13 H1 120.2 . . ? C15 C14 C13 117.5(17) . . ? C15 C14 C24 120.9(15) . . ? C13 C14 C24 121.5(14) . . ? C14 C15 C16 119.0(18) . . ? C14 C15 H2 120.5 . . ? C16 C15 H2 120.5 . . ? N11 C16 C15 122.8(16) . . ? N11 C16 C2 112.0(15) . . ? C15 C16 C2 125.0(17) . . ? O3 C2 O4 128.3(18) . . ? O3 C2 C16 116.1(18) . . ? O4 C2 C16 115.6(17) . . ? O5 C3 O6 125(3) . . ? O5 C3 C22 117(2) . . ? O6 C3 C22 118(3) . . ? N21 C22 C23 123(2) . . ? N21 C22 C3 113(2) . . ? C23 C22 C3 125(2) . . ? C22 C23 C24 119.7(17) . . ? C22 C23 H3 120.2 . . ? C24 C23 H3 120.2 . . ? C25 C24 C23 115.1(17) . . ? C25 C24 C14 124.8(16) . . ? C23 C24 C14 119.8(14) . . ? C26 C25 C24 121.5(19) . . ? C26 C25 H4 119.2 . . ? C24 C25 H4 119.2 . . ? N21 C26 C25 120.9(17) . . ? N21 C26 C4 104.1(17) . . ? C25 C26 C4 135.0(19) . . ? O7 C4 O8 143(3) . . ? O7 C4 C26 118(2) . . ? O8 C4 C26 99(2) . . ? O8 C4 Tb3 147.4(11) . . ? C26 C4 Tb3 87.6(13) . . ? C32 N31 C32 118(2) . 2 ? C32 N31 Tb1 121.2(12) . . ? C32 N31 Tb1 121.2(12) 2 . ? N31 C32 C33 123(2) . . ? N31 C32 C5 111.5(18) . . ? C33 C32 C5 125.3(19) . . ? C32 C33 C34 120(2) . . ? C32 C33 H5 120.1 . . ? C34 C33 H5 120.1 . . ? C33 C34 C33 116(2) . 2 ? C33 C34 C44 121.8(12) . . ? C33 C34 C44 121.8(12) 2 . ? C42 N41 C42 115(2) . 2 ? C42 N41 Tb2 122.7(12) . 3_455 ? C42 N41 Tb2 122.7(12) 2 3_455 ? N41 C42 C43 125(2) . . ? N41 C42 C6 110.3(17) . . ? C43 C42 C6 124.6(19) . . ? C42 C43 C44 120(2) . . ? C42 C43 H6 119.9 . . ? C44 C43 H6 119.9 . . ? C43 C44 C43 115(3) 2 . ? C43 C44 C34 122.5(16) 2 . ? C43 C44 C34 122.5(16) . . ? 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 O3 Tb2 O1 C1 -163.0(16) 2_655 . . . ? O3 Tb2 O1 C1 -5.0(18) . . . . ? O1 Tb2 O1 C1 68.7(15) 2_655 . . . ? O11 Tb2 O1 C1 -71.6(16) 3_545 . . . ? O11 Tb2 O1 C1 150.0(14) 4_545 . . . ? N11 Tb2 O1 C1 128.6(16) 2_655 . . . ? N11 Tb2 O1 C1 3.8(15) . . . . ? N41 Tb2 O1 C1 -111.3(15) 3_545 . . . ? O3 Tb2 O3 C2 154.7(16) 2_655 . . . ? O1 Tb2 O3 C2 22.7(18) . . . . ? O1 Tb2 O3 C2 -62.7(15) 2_655 . . . ? O11 Tb2 O3 C2 89.1(15) 3_545 . . . ? O11 Tb2 O3 C2 -141.7(16) 4_545 . . . ? N11 Tb2 O3 C2 -79.8(16) 2_655 . . . ? N11 Tb2 O3 C2 13.9(15) . . . . ? N41 Tb2 O3 C2 154.7(16) 3_545 . . . ? O4 Tb1 O4 C2 -106(2) 2 . . . ? O14 Tb1 O4 C2 21(2) 2 . . . ? O14 Tb1 O4 C2 105(2) . . . . ? O13 Tb1 O4 C2 27(2) . . . . ? O13 Tb1 O4 C2 140.9(19) 2 . . . ? O9 Tb1 O4 C2 -173(2) 2 . . . ? O9 Tb1 O4 C2 -44(2) . . . . ? N31 Tb1 O4 C2 -106(2) . . . . ? O7 Tb3 O5 C3 19(3) . . . . ? O10 Tb3 O5 C3 163(3) 6_566 . . . ? O2 Tb3 O5 C3 101(3) 5_666 . . . ? O12 Tb3 O5 C3 -56(3) . . . . ? O15 Tb3 O5 C3 180(3) . . . . ? O16 Tb3 O5 C3 -99(3) . . . . ? N21 Tb3 O5 C3 21(3) . . . . ? C4 Tb3 O5 C3 31(3) . . . . ? O10 Tb3 O7 C4 -130.1(16) 6_566 . . . ? O2 Tb3 O7 C4 -47.4(15) 5_666 . . . ? O12 Tb3 O7 C4 95.8(15) . . . . ? O15 Tb3 O7 C4 -110(2) . . . . ? O16 Tb3 O7 C4 161.0(17) . . . . ? O5 Tb3 O7 C4 29.4(19) . . . . ? N21 Tb3 O7 C4 27.4(14) . . . . ? O4 Tb1 O9 C5 -73(2) . . . . ? O4 Tb1 O9 C5 67(2) 2 . . . ? O14 Tb1 O9 C5 142(2) 2 . . . ? O14 Tb1 O9 C5 -128.4(19) . . . . ? O13 Tb1 O9 C5 -149(2) . . . . ? O13 Tb1 O9 C5 101(2) 2 . . . ? O9 Tb1 O9 C5 -6.4(18) 2 . . . ? N31 Tb1 O9 C5 -6.4(18) . . . . ? O7 Tb3 O12 C6 155(3) . . . . ? O10 Tb3 O12 C6 78(3) 6_566 . . . ? O2 Tb3 O12 C6 -111(3) 5_666 . . . ? O15 Tb3 O12 C6 -11(3) . . . . ? O16 Tb3 O12 C6 70(3) . . . . ? O5 Tb3 O12 C6 -71(3) . . . . ? N21 Tb3 O12 C6 -139(3) . . . . ? C4 Tb3 O12 C6 179(3) . . . . ? O3 Tb2 N11 C16 -165.8(12) 2_655 . . . ? O3 Tb2 N11 C16 -11.6(13) . . . . ? O1 Tb2 N11 C16 176.0(15) . . . . ? O1 Tb2 N11 C16 67.9(14) 2_655 . . . ? O11 Tb2 N11 C16 -98.0(14) 3_545 . . . ? O11 Tb2 N11 C16 32.9(18) 4_545 . . . ? N11 Tb2 N11 C16 120.2(15) 2_655 . . . ? N41 Tb2 N11 C16 -59.8(15) 3_545 . . . ? O3 Tb2 N11 C12 22.6(16) 2_655 . . . ? O3 Tb2 N11 C12 176.9(15) . . . . ? O1 Tb2 N11 C12 4.5(13) . . . . ? O1 Tb2 N11 C12 -103.7(14) 2_655 . . . ? O11 Tb2 N11 C12 90.5(14) 3_545 . . . ? O11 Tb2 N11 C12 -138.7(13) 4_545 . . . ? N11 Tb2 N11 C12 -51.4(12) 2_655 . . . ? N41 Tb2 N11 C12 128.6(12) 3_545 . . . ? O7 Tb3 N21 C26 -4.3(19) . . . . ? O10 Tb3 N21 C26 33(2) 6_566 . . . ? O2 Tb3 N21 C26 92.7(19) 5_666 . . . ? O12 Tb3 N21 C26 -104(2) . . . . ? O15 Tb3 N21 C26 149.6(19) . . . . ? O16 Tb3 N21 C26 -71(3) . . . . ? O5 Tb3 N21 C26 177(2) . . . . ? C4 Tb3 N21 C26 10.4(17) . . . . ? O7 Tb3 N21 C22 162(2) . . . . ? O10 Tb3 N21 C22 -161.5(18) 6_566 . . . ? O2 Tb3 N21 C22 -101.4(19) 5_666 . . . ? O12 Tb3 N21 C22 61.7(19) . . . . ? O15 Tb3 N21 C22 -44(2) . . . . ? O16 Tb3 N21 C22 95(2) . . . . ? O5 Tb3 N21 C22 -16.8(19) . . . . ? C4 Tb3 N21 C22 176(2) . . . . ? Tb1 O9 C5 O10 -165.2(17) . . . . ? Tb1 O9 C5 C32 9(3) . . . . ? Tb3 O10 C5 O9 -65(4) 6_565 . . . ? Tb3 O10 C5 C32 121(3) 6_565 . . . ? Tb2 O11 C6 O12 -167.7(19) 3_455 . . . ? Tb2 O11 C6 C42 11(3) 3_455 . . . ? Tb3 O12 C6 O11 4(5) . . . . ? Tb3 O12 C6 C42 -175(2) . . . . ? Tb3 O2 C1 O1 -84(2) 5_666 . . . ? Tb3 O2 C1 C12 94(2) 5_666 . . . ? Tb2 O1 C1 O2 167.2(14) . . . . ? Tb2 O1 C1 C12 -10(2) . . . . ? C16 N11 C12 C13 -6(3) . . . . ? Tb2 N11 C12 C13 165.7(14) . . . . ? C16 N11 C12 C1 177.8(16) . . . . ? Tb2 N11 C12 C1 -10(2) . . . . ? O2 C1 C12 N11 -164.8(16) . . . . ? O1 C1 C12 N11 13(2) . . . . ? O2 C1 C12 C13 19(3) . . . . ? O1 C1 C12 C13 -163.1(18) . . . . ? N11 C12 C13 C14 1(3) . . . . ? C1 C12 C13 C14 176.2(17) . . . . ? C12 C13 C14 C15 5(3) . . . . ? C12 C13 C14 C24 -177.2(19) . . . . ? C13 C14 C15 C16 -5(3) . . . . ? C24 C14 C15 C16 177.2(19) . . . . ? C12 N11 C16 C15 6(3) . . . . ? Tb2 N11 C16 C15 -165.8(15) . . . . ? C12 N11 C16 C2 -178.6(16) . . . . ? Tb2 N11 C16 C2 9(2) . . . . ? C14 C15 C16 N11 0(3) . . . . ? C14 C15 C16 C2 -175.1(19) . . . . ? Tb2 O3 C2 O4 166.1(16) . . . . ? Tb2 O3 C2 C16 -14(2) . . . . ? Tb1 O4 C2 O3 -28(4) . . . . ? Tb1 O4 C2 C16 151.9(13) . . . . ? N11 C16 C2 O3 2(3) . . . . ? C15 C16 C2 O3 177.6(19) . . . . ? N11 C16 C2 O4 -177.8(17) . . . . ? C15 C16 C2 O4 -3(3) . . . . ? Tb3 O5 C3 O6 160(4) . . . . ? Tb3 O5 C3 C22 -23(5) . . . . ? C26 N21 C22 C23 -2(4) . . . . ? Tb3 N21 C22 C23 -168(2) . . . . ? C26 N21 C22 C3 178(3) . . . . ? Tb3 N21 C22 C3 13(3) . . . . ? O5 C3 C22 N21 6(5) . . . . ? O6 C3 C22 N21 -177(4) . . . . ? O5 C3 C22 C23 -174(3) . . . . ? O6 C3 C22 C23 4(6) . . . . ? N21 C22 C23 C24 1(5) . . . . ? C3 C22 C23 C24 -179(3) . . . . ? C22 C23 C24 C25 1(4) . . . . ? C22 C23 C24 C14 175(2) . . . . ? C15 C14 C24 C25 30(4) . . . . ? C13 C14 C24 C25 -148(2) . . . . ? C15 C14 C24 C23 -144(2) . . . . ? C13 C14 C24 C23 39(3) . . . . ? C23 C24 C25 C26 -3(4) . . . . ? C14 C24 C25 C26 -177(3) . . . . ? C22 N21 C26 C25 0(4) . . . . ? Tb3 N21 C26 C25 166(2) . . . . ? C22 N21 C26 C4 179(2) . . . . ? Tb3 N21 C26 C4 -15(3) . . . . ? C24 C25 C26 N21 2(5) . . . . ? C24 C25 C26 C4 -176(3) . . . . ? Tb3 O7 C4 O8 129.3(17) . . . . ? Tb3 O7 C4 C26 -50.6(16) . . . . ? N21 C26 C4 O7 43(2) . . . . ? C25 C26 C4 O7 -139(3) . . . . ? N21 C26 C4 O8 -137(2) . . . . ? C25 C26 C4 O8 41(3) . . . . ? N21 C26 C4 Tb3 11.1(19) . . . . ? C25 C26 C4 Tb3 -171(3) . . . . ? O10 Tb3 C4 O7 49.3(15) 6_566 . . . ? O2 Tb3 C4 O7 130.5(16) 5_666 . . . ? O12 Tb3 C4 O7 -85.3(15) . . . . ? O15 Tb3 C4 O7 113.2(17) . . . . ? O16 Tb3 C4 O7 -20.1(18) . . . . ? O5 Tb3 C4 O7 -156.9(15) . . . . ? N21 Tb3 C4 O7 -144.5(17) . . . . ? O7 Tb3 C4 O8 -120(4) . . . . ? O10 Tb3 C4 O8 -71(4) 6_566 . . . ? O2 Tb3 C4 O8 10(3) 5_666 . . . ? O12 Tb3 C4 O8 155(4) . . . . ? O15 Tb3 C4 O8 -7(4) . . . . ? O16 Tb3 C4 O8 -140(4) . . . . ? O5 Tb3 C4 O8 83(4) . . . . ? N21 Tb3 C4 O8 95(4) . . . . ? O7 Tb3 C4 C26 137.0(19) . . . . ? O10 Tb3 C4 C26 -173.7(13) 6_566 . . . ? O2 Tb3 C4 C26 -92.6(13) 5_666 . . . ? O12 Tb3 C4 C26 51.7(13) . . . . ? O15 Tb3 C4 C26 -109.8(18) . . . . ? O16 Tb3 C4 C26 116.9(15) . . . . ? O5 Tb3 C4 C26 -20.0(14) . . . . ? N21 Tb3 C4 C26 -7.5(12) . . . . ? O4 Tb1 N31 C32 100.7(12) . . . . ? O4 Tb1 N31 C32 -79.3(12) 2 . . . ? O14 Tb1 N31 C32 -38.8(13) 2 . . . ? O14 Tb1 N31 C32 141.2(13) . . . . ? O13 Tb1 N31 C32 45.4(13) . . . . ? O13 Tb1 N31 C32 -134.6(13) 2 . . . ? O9 Tb1 N31 C32 -176.7(13) 2 . . . ? O9 Tb1 N31 C32 3.3(13) . . . . ? O4 Tb1 N31 C32 -79.3(12) . . . 2 ? O4 Tb1 N31 C32 100.7(12) 2 . . 2 ? O14 Tb1 N31 C32 141.2(13) 2 . . 2 ? O14 Tb1 N31 C32 -38.8(13) . . . 2 ? O13 Tb1 N31 C32 -134.6(13) . . . 2 ? O13 Tb1 N31 C32 45.4(13) 2 . . 2 ? O9 Tb1 N31 C32 3.3(13) 2 . . 2 ? O9 Tb1 N31 C32 -176.7(13) . . . 2 ? C32 N31 C32 C33 0.0(19) 2 . . . ? Tb1 N31 C32 C33 180.0(19) . . . . ? C32 N31 C32 C5 179(2) 2 . . . ? Tb1 N31 C32 C5 -1(2) . . . . ? O9 C5 C32 N31 -5(3) . . . . ? O10 C5 C32 N31 170.0(17) . . . . ? O9 C5 C32 C33 174(3) . . . . ? O10 C5 C32 C33 -11(3) . . . . ? N31 C32 C33 C34 0(4) . . . . ? C5 C32 C33 C34 -179(2) . . . . ? C32 C33 C34 C33 0.0(18) . . . 2 ? C32 C33 C34 C44 180.0(18) . . . . ? C42 N41 C42 C43 0(2) 2 . . . ? Tb2 N41 C42 C43 180(2) 3_455 . . . ? C42 N41 C42 C6 178(3) 2 . . . ? Tb2 N41 C42 C6 -2(3) 3_455 . . . ? O11 C6 C42 N41 -6(3) . . . . ? O12 C6 C42 N41 173(2) . . . . ? O11 C6 C42 C43 172(3) . . . . ? O12 C6 C42 C43 -9(4) . . . . ? N41 C42 C43 C44 0(4) . . . . ? C6 C42 C43 C44 -178(2) . . . . ? C42 C43 C44 C43 0(2) . . . 2 ? C42 C43 C44 C34 180(2) . . . . ? C33 C34 C44 C43 29.1(19) . . . 2 ? C33 C34 C44 C43 -150.9(19) 2 . . 2 ? C33 C34 C44 C43 -150.9(19) . . . . ? C33 C34 C44 C43 29.1(19) 2 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.505 _refine_diff_density_min -5.057 _refine_diff_density_rms 0.330 #====END data_5 _database_code_depnum_ccdc_archive 'CCDC 702670' _audit_creation_date 'Sun Aug 19 12:37:04 2007' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Dy4(BPTCA)3(OH2)8] ; _chemical_name_common (Dy4(BPTCA)3(OH2)8) _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 Dy4 N6 O32 ' _chemical_formula_sum 'C42 H28 Dy4 N6 O32' _chemical_formula_weight 1778.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Dy Dy -0.1892 4.4098 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 12.1025(16) _cell_length_b 22.287(4) _cell_length_c 21.695(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.315(8) _cell_angle_gamma 90.00 _cell_volume 5644.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 15753 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 5.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 21653 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4967 _reflns_number_gt 4172 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.1097P)^2^+661.8397P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4967 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.2624 _refine_ls_wR_factor_gt 0.2482 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.005 _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 Dy1 Dy 0.5000 0.74692(5) 0.2500 0.0351(3) Uani 1 2 d S . . Dy2 Dy 0.0000 0.78666(5) 0.2500 0.0379(4) Uani 1 2 d S . . Dy3 Dy 0.13864(8) 0.36984(7) 0.52572(5) 0.0710(5) Uani 1 1 d U . . O1 O 0.6440(12) 0.6756(6) 0.3017(6) 0.045(3) Uani 1 1 d . . . O2 O 0.7146(10) 0.6109(5) 0.3815(6) 0.035(3) Uani 1 1 d . . . O3 O 0.3260(11) 0.7741(6) 0.2753(6) 0.041(3) Uani 1 1 d . . . O4 O 0.1764(12) 0.7469(6) 0.3110(7) 0.047(3) Uani 1 1 d . . . O5 O 0.304(2) 0.3427(10) 0.4898(13) 0.119(7) Uani 1 1 d . . . O6 O 0.411(3) 0.3625(11) 0.4234(16) 0.158(10) Uani 1 1 d . . . O7 O 0.116(2) 0.4729(10) 0.5695(12) 0.119(7) Uani 1 1 d D . . O8 O 0.016(3) 0.5525(10) 0.5027(14) 0.158(10) Uani 1 1 d DU . . O9 O -0.0427(14) 0.7373(7) 0.3422(7) 0.054(4) Uani 1 1 d . . . O10 O -0.0367(14) 0.6549(9) 0.4029(7) 0.071(5) Uani 1 1 d U . . O11 O 0.0765(13) 0.2942(6) 0.3524(6) 0.049(4) Uani 1 1 d . . . O12 O 0.0885(17) 0.3759(8) 0.4134(8) 0.077(5) Uani 1 1 d . . . O13 O 0.1478(13) 0.8445(7) 0.2181(9) 0.069(5) Uani 1 1 d . . . O14 O 0.0765(16) 0.8576(8) 0.3370(10) 0.077(5) Uani 1 1 d . . . O15 O 0.195(3) 0.2715(10) 0.5654(14) 0.131(10) Uani 1 1 d U . . O16 O -0.047(4) 0.330(2) 0.4715(19) 0.226(19) Uani 1 1 d U . . N11 N 0.4493(13) 0.6837(6) 0.3316(7) 0.035(3) Uani 1 1 d . . . N21 N 0.2436(15) 0.4560(9) 0.4937(8) 0.049(4) Uani 1 1 d . . . C5 C -0.0351(18) 0.6823(12) 0.3519(10) 0.054(6) Uani 1 1 d . . . C6 C 0.0680(19) 0.3492(11) 0.3623(10) 0.058(6) Uani 1 1 d . . . C1 C 0.6359(14) 0.6421(7) 0.3470(8) 0.032(4) Uani 1 1 d D . . C12 C 0.5181(14) 0.6393(7) 0.3595(8) 0.033(4) Uani 1 1 d D . . C13 C 0.4847(14) 0.5956(8) 0.3952(8) 0.038(4) Uani 1 1 d D . . H1 H 0.5363 0.5647 0.4148 0.045 Uiso 1 1 calc R . . C14 C 0.3724(14) 0.5973(7) 0.4021(8) 0.039(4) Uani 1 1 d D . . C15 C 0.3027(16) 0.6461(7) 0.3750(9) 0.040(4) Uani 1 1 d D . . H2 H 0.2277 0.6504 0.3804 0.048 Uiso 1 1 calc R . . C16 C 0.3456(16) 0.6877(7) 0.3403(8) 0.037(4) Uani 1 1 d D . . C2 C 0.2760(16) 0.7405(8) 0.3064(8) 0.037(4) Uani 1 1 d D . . C3 C 0.345(4) 0.3784(10) 0.456(2) 0.121(11) Uani 1 1 d D . . C22 C 0.316(2) 0.4445(9) 0.4586(12) 0.064(5) Uani 1 1 d D . . C23 C 0.363(2) 0.4890(8) 0.4305(12) 0.062(5) Uani 1 1 d D . . H3 H 0.4164 0.4795 0.4071 0.075 Uiso 1 1 calc R . . C24 C 0.3306(16) 0.5487(8) 0.4364(9) 0.044(5) Uani 1 1 d D . . C25 C 0.254(2) 0.5581(9) 0.4737(12) 0.062(5) Uani 1 1 d D . . H4 H 0.2327 0.5978 0.4820 0.075 Uiso 1 1 calc R . . C26 C 0.208(2) 0.5099(9) 0.4982(12) 0.064(5) Uani 1 1 d D . . C4 C 0.1029(19) 0.5137(8) 0.5241(9) 0.121(11) Uani 1 1 d D . . N31 N 0.0000 0.6725(9) 0.2500 0.044(5) Uani 1 2 d SD . . C32 C -0.017(2) 0.6429(8) 0.2998(9) 0.049(5) Uani 1 1 d D . . C33 C -0.0194(19) 0.5807(9) 0.3009(11) 0.060(6) Uani 1 1 d D . . H5 H -0.0341 0.5600 0.3362 0.072 Uiso 1 1 calc R . . C34 C 0.0000 0.5491(11) 0.2500 0.068(10) Uani 1 2 d SD . . N41 N 0.0000 0.3583(10) 0.2500 0.053(6) Uani 1 2 d SD . . C42 C 0.029(2) 0.3895(7) 0.3041(9) 0.056(6) Uani 1 1 d D . . C43 C 0.032(2) 0.4512(9) 0.3056(11) 0.072(8) Uani 1 1 d D . . H6 H 0.0556 0.4714 0.3454 0.086 Uiso 1 1 calc R . . C44 C 0.0000 0.4841(14) 0.2500 0.075(11) Uani 1 2 d SD . . 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 Dy1 0.0452(7) 0.0391(7) 0.0217(6) 0.000 0.0101(5) 0.000 Dy2 0.0501(7) 0.0332(6) 0.0405(7) 0.000 0.0295(6) 0.000 Dy3 0.0361(6) 0.1448(13) 0.0349(6) 0.0396(6) 0.0142(4) -0.0095(6) O1 0.050(8) 0.057(8) 0.033(7) 0.012(6) 0.019(6) 0.004(6) O2 0.039(7) 0.034(6) 0.033(6) -0.003(5) 0.009(5) -0.004(5) O3 0.051(8) 0.042(7) 0.031(6) 0.007(5) 0.014(6) 0.007(6) O4 0.049(8) 0.053(8) 0.046(8) 0.016(6) 0.024(6) 0.022(6) O5 0.159(16) 0.093(11) 0.156(16) 0.048(11) 0.134(15) 0.034(10) O6 0.27(2) 0.085(11) 0.201(19) 0.034(12) 0.20(2) 0.050(13) O7 0.159(16) 0.093(11) 0.156(16) 0.048(11) 0.134(15) 0.034(10) O8 0.27(2) 0.085(11) 0.201(19) 0.034(12) 0.20(2) 0.050(13) O9 0.077(11) 0.053(9) 0.047(8) -0.007(7) 0.042(8) -0.003(8) O10 0.064(10) 0.110(13) 0.049(9) 0.030(9) 0.034(8) -0.018(9) O11 0.069(9) 0.032(7) 0.031(7) -0.007(5) -0.013(6) 0.015(6) O12 0.100(14) 0.074(11) 0.045(9) -0.025(8) -0.003(9) 0.014(10) O13 0.050(9) 0.056(9) 0.100(13) 0.041(9) 0.018(9) -0.002(7) O14 0.076(12) 0.059(10) 0.095(14) -0.029(9) 0.018(10) 0.001(9) O15 0.21(3) 0.072(13) 0.17(2) -0.032(14) 0.15(2) -0.053(15) O16 0.22(3) 0.28(4) 0.16(3) 0.07(3) 0.01(2) -0.15(3) N11 0.044(8) 0.037(8) 0.027(7) 0.001(6) 0.013(6) 0.011(7) N21 0.055(10) 0.066(11) 0.037(9) 0.015(8) 0.031(8) 0.013(9) C5 0.047(12) 0.079(17) 0.049(12) -0.005(11) 0.034(10) -0.009(11) C6 0.054(13) 0.070(15) 0.037(11) -0.009(10) -0.011(9) 0.012(11) C1 0.040(9) 0.034(9) 0.026(8) -0.006(7) 0.015(7) 0.000(7) C12 0.041(9) 0.036(9) 0.026(8) 0.000(7) 0.014(7) -0.002(7) C13 0.039(10) 0.040(10) 0.033(9) 0.009(8) 0.007(7) 0.006(8) C14 0.044(10) 0.037(9) 0.035(9) 0.000(8) 0.010(8) 0.004(8) C15 0.051(11) 0.036(9) 0.042(10) 0.004(8) 0.027(9) 0.002(8) C16 0.060(12) 0.035(9) 0.023(8) 0.004(7) 0.021(8) 0.012(8) C2 0.050(11) 0.045(10) 0.021(8) -0.006(7) 0.016(8) 0.013(8) C3 0.19(3) 0.065(13) 0.18(3) 0.012(14) 0.16(2) 0.017(15) C22 0.088(12) 0.059(10) 0.070(11) 0.011(8) 0.065(10) 0.016(9) C23 0.091(12) 0.049(9) 0.072(11) 0.012(8) 0.064(10) 0.014(8) C24 0.043(10) 0.056(12) 0.039(10) 0.018(9) 0.020(8) 0.006(9) C25 0.091(12) 0.049(9) 0.072(11) 0.012(8) 0.064(10) 0.014(8) C26 0.088(12) 0.059(10) 0.070(11) 0.011(8) 0.065(10) 0.016(9) C4 0.19(3) 0.065(13) 0.18(3) 0.012(14) 0.16(2) 0.017(15) N31 0.062(15) 0.038(12) 0.041(12) 0.000 0.029(11) 0.000 C32 0.070(14) 0.045(11) 0.046(11) 0.005(9) 0.040(10) -0.012(10) C33 0.055(13) 0.051(13) 0.073(15) 0.017(11) 0.019(12) -0.009(10) C34 0.10(3) 0.018(13) 0.09(3) 0.000 0.03(2) 0.000 N41 0.065(16) 0.043(13) 0.042(14) 0.000 -0.002(12) 0.000 C42 0.069(14) 0.027(9) 0.062(14) 0.003(9) 0.001(11) 0.005(9) C43 0.071(16) 0.046(13) 0.078(17) -0.007(12) -0.015(13) 0.010(12) C44 0.047(19) 0.08(3) 0.08(3) 0.000 -0.017(18) 0.000 _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 Dy1 O3 2.390(13) . ? Dy1 O3 2.390(13) 2_655 ? Dy1 O1 2.406(13) . ? Dy1 O1 2.406(13) 2_655 ? Dy1 O11 2.411(12) 4 ? Dy1 O11 2.411(12) 3 ? Dy1 N11 2.463(14) 2_655 ? Dy1 N11 2.463(14) . ? Dy1 N41 2.48(2) 3 ? Dy2 O4 2.366(13) 2 ? Dy2 O4 2.366(13) . ? Dy2 O13 2.448(14) . ? Dy2 O13 2.448(14) 2 ? Dy2 O14 2.450(17) . ? Dy2 O14 2.450(17) 2 ? Dy2 O9 2.454(14) 2 ? Dy2 O9 2.454(14) . ? Dy2 N31 2.54(2) . ? Dy3 O10 2.287(13) 5_566 ? Dy3 O2 2.347(12) 5_666 ? Dy3 O12 2.353(16) . ? Dy3 O15 2.39(3) . ? Dy3 O5 2.409(19) . ? Dy3 O16 2.41(4) . ? Dy3 N21 2.500(18) . ? Dy3 O8 2.51(2) 5_566 ? Dy3 O7 2.53(2) . ? O1 C1 1.26(2) . ? O2 C1 1.25(2) . ? O2 Dy3 2.347(12) 5_666 ? O3 C2 1.26(2) . ? O4 C2 1.24(2) . ? O5 C3 1.27(3) . ? O6 C3 1.25(3) . ? O7 C4 1.318(18) . ? O8 C4 1.35(4) . ? O8 Dy3 2.51(2) 5_566 ? O9 C5 1.24(3) . ? O10 C5 1.27(3) . ? O10 Dy3 2.287(13) 5_566 ? O11 C6 1.25(3) . ? O11 Dy1 2.411(12) 3_445 ? O12 C6 1.23(3) . ? N11 C16 1.32(2) . ? N11 C12 1.33(2) . ? N21 C26 1.29(3) . ? N21 C22 1.33(2) . ? C5 C32 1.49(3) . ? C6 C42 1.52(3) . ? C1 C12 1.52(2) . ? C12 C13 1.37(2) . ? C13 C14 1.41(2) . ? C13 H1 0.9500 . ? C14 C15 1.41(2) . ? C14 C24 1.48(3) . ? C15 C16 1.38(2) . ? C15 H2 0.9500 . ? C16 C2 1.52(2) . ? C3 C22 1.52(2) . ? C22 C23 1.36(2) . ? C23 C24 1.40(2) . ? C23 H3 0.9500 . ? C24 C25 1.40(2) . ? C25 C26 1.37(2) . ? C25 H4 0.9500 . ? C26 C4 1.53(2) . ? N31 C32 1.328(18) 2 ? N31 C32 1.328(18) . ? C32 C33 1.39(2) . ? C33 C34 1.38(2) . ? C33 H5 0.9500 . ? C34 C33 1.38(2) 2 ? C34 C44 1.45(5) . ? N41 C42 1.329(19) 2 ? N41 C42 1.329(19) . ? N41 Dy1 2.48(2) 3_445 ? C42 C43 1.38(2) . ? C43 C44 1.38(2) . ? C43 H6 0.9500 . ? C44 C43 1.38(2) 2 ? 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 O3 Dy1 O3 150.6(6) . 2_655 ? O3 Dy1 O1 129.3(4) . . ? O3 Dy1 O1 72.6(4) 2_655 . ? O3 Dy1 O1 72.6(4) . 2_655 ? O3 Dy1 O1 129.4(4) 2_655 2_655 ? O1 Dy1 O1 97.3(7) . 2_655 ? O3 Dy1 O11 87.3(5) . 4 ? O3 Dy1 O11 79.9(5) 2_655 4 ? O1 Dy1 O11 140.6(5) . 4 ? O1 Dy1 O11 78.8(4) 2_655 4 ? O3 Dy1 O11 79.9(5) . 3 ? O3 Dy1 O11 87.4(5) 2_655 3 ? O1 Dy1 O11 78.8(4) . 3 ? O1 Dy1 O11 140.6(5) 2_655 3 ? O11 Dy1 O11 128.2(6) 4 3 ? O3 Dy1 N11 135.4(5) . 2_655 ? O3 Dy1 N11 65.0(4) 2_655 2_655 ? O1 Dy1 N11 70.7(5) . 2_655 ? O1 Dy1 N11 64.8(4) 2_655 2_655 ? O11 Dy1 N11 72.3(5) 4 2_655 ? O11 Dy1 N11 143.5(5) 3 2_655 ? O3 Dy1 N11 65.0(4) . . ? O3 Dy1 N11 135.4(5) 2_655 . ? O1 Dy1 N11 64.8(4) . . ? O1 Dy1 N11 70.7(5) 2_655 . ? O11 Dy1 N11 143.5(5) 4 . ? O11 Dy1 N11 72.3(5) 3 . ? N11 Dy1 N11 110.2(6) 2_655 . ? O3 Dy1 N41 75.3(3) . 3 ? O3 Dy1 N41 75.3(3) 2_655 3 ? O1 Dy1 N41 131.4(3) . 3 ? O1 Dy1 N41 131.4(3) 2_655 3 ? O11 Dy1 N41 64.1(3) 4 3 ? O11 Dy1 N41 64.1(3) 3 3 ? N11 Dy1 N41 124.9(3) 2_655 3 ? N11 Dy1 N41 124.9(3) . 3 ? O4 Dy2 O4 136.1(7) 2 . ? O4 Dy2 O13 131.1(5) 2 . ? O4 Dy2 O13 74.7(5) . . ? O4 Dy2 O13 74.7(5) 2 2 ? O4 Dy2 O13 131.1(5) . 2 ? O13 Dy2 O13 116.5(8) . 2 ? O4 Dy2 O14 140.7(5) 2 . ? O4 Dy2 O14 73.1(6) . . ? O13 Dy2 O14 73.9(7) . . ? O13 Dy2 O14 66.3(6) 2 . ? O4 Dy2 O14 73.1(6) 2 2 ? O4 Dy2 O14 140.7(6) . 2 ? O13 Dy2 O14 66.3(6) . 2 ? O13 Dy2 O14 73.9(7) 2 2 ? O14 Dy2 O14 99.6(9) . 2 ? O4 Dy2 O9 74.3(5) 2 2 ? O4 Dy2 O9 86.3(5) . 2 ? O13 Dy2 O9 71.3(6) . 2 ? O13 Dy2 O9 142.5(6) 2 2 ? O14 Dy2 O9 143.1(6) . 2 ? O14 Dy2 O9 77.2(6) 2 2 ? O4 Dy2 O9 86.3(5) 2 . ? O4 Dy2 O9 74.3(5) . . ? O13 Dy2 O9 142.5(6) . . ? O13 Dy2 O9 71.3(6) 2 . ? O14 Dy2 O9 77.2(6) . . ? O14 Dy2 O9 143.1(6) 2 . ? O9 Dy2 O9 126.8(7) 2 . ? O4 Dy2 N31 68.0(4) 2 . ? O4 Dy2 N31 68.0(4) . . ? O13 Dy2 N31 121.8(4) . . ? O13 Dy2 N31 121.8(4) 2 . ? O14 Dy2 N31 130.2(5) . . ? O14 Dy2 N31 130.2(5) 2 . ? O9 Dy2 N31 63.4(3) 2 . ? O9 Dy2 N31 63.4(3) . . ? O10 Dy3 O2 83.4(5) 5_566 5_666 ? O10 Dy3 O12 132.6(7) 5_566 . ? O2 Dy3 O12 143.9(6) 5_666 . ? O10 Dy3 O15 71.9(7) 5_566 . ? O2 Dy3 O15 77.2(8) 5_666 . ? O12 Dy3 O15 113.4(8) . . ? O10 Dy3 O5 143.2(7) 5_566 . ? O2 Dy3 O5 79.5(8) 5_666 . ? O12 Dy3 O5 71.9(8) . . ? O15 Dy3 O5 72.7(7) . . ? O10 Dy3 O16 69.0(11) 5_566 . ? O2 Dy3 O16 151.9(9) 5_666 . ? O12 Dy3 O16 64.2(10) . . ? O15 Dy3 O16 88.9(14) . . ? O5 Dy3 O16 119.8(16) . . ? O10 Dy3 N21 141.1(6) 5_566 . ? O2 Dy3 N21 76.9(5) 5_666 . ? O12 Dy3 N21 71.3(6) . . ? O15 Dy3 N21 133.3(7) . . ? O5 Dy3 N21 64.9(6) . . ? O16 Dy3 N21 128.5(9) . . ? O10 Dy3 O8 80.3(7) 5_566 5_566 ? O2 Dy3 O8 115.6(8) 5_666 5_566 ? O12 Dy3 O8 74.6(8) . 5_566 ? O15 Dy3 O8 148.0(8) . 5_566 ? O5 Dy3 O8 136.5(7) . 5_566 ? O16 Dy3 O8 66.0(15) . 5_566 ? N21 Dy3 O8 78.6(7) . 5_566 ? O10 Dy3 O7 80.4(6) 5_566 . ? O2 Dy3 O7 69.2(7) 5_666 . ? O12 Dy3 O7 108.2(7) . . ? O15 Dy3 O7 138.4(8) . . ? O5 Dy3 O7 122.1(8) . . ? O16 Dy3 O7 109.6(16) . . ? N21 Dy3 O7 61.3(6) . . ? O8 Dy3 O7 46.8(9) 5_566 . ? C1 O1 Dy1 124.0(11) . . ? C1 O2 Dy3 133.9(11) . 5_666 ? C2 O3 Dy1 123.2(11) . . ? C2 O4 Dy2 138.5(11) . . ? C3 O5 Dy3 120.8(19) . . ? C4 O7 Dy3 110.4(13) . . ? C4 O8 Dy3 173.8(18) . 5_566 ? C5 O9 Dy2 123.9(12) . . ? C5 O10 Dy3 147.4(16) . 5_566 ? C6 O11 Dy1 123.9(12) . 3_445 ? C6 O12 Dy3 147.5(17) . . ? C16 N11 C12 119.2(14) . . ? C16 N11 Dy1 119.4(10) . . ? C12 N11 Dy1 120.5(11) . . ? C26 N21 C22 120.4(17) . . ? C26 N21 Dy3 119.5(12) . . ? C22 N21 Dy3 118.0(14) . . ? O9 C5 O10 127(2) . . ? O9 C5 C32 118.2(18) . . ? O10 C5 C32 115(2) . . ? O12 C6 O11 129(2) . . ? O12 C6 C42 114(2) . . ? O11 C6 C42 117.1(17) . . ? O2 C1 O1 126.2(15) . . ? O2 C1 C12 118.0(14) . . ? O1 C1 C12 115.8(15) . . ? N11 C12 C13 123.0(15) . . ? N11 C12 C1 112.9(14) . . ? C13 C12 C1 124.1(14) . . ? C12 C13 C14 118.6(14) . . ? C12 C13 H1 120.7 . . ? C14 C13 H1 120.7 . . ? C13 C14 C15 117.7(15) . . ? C13 C14 C24 120.2(13) . . ? C15 C14 C24 122.1(14) . . ? C16 C15 C14 118.6(15) . . ? C16 C15 H2 120.7 . . ? C14 C15 H2 120.7 . . ? N11 C16 C15 122.9(15) . . ? N11 C16 C2 114.1(14) . . ? C15 C16 C2 123.0(15) . . ? O4 C2 O3 125.9(16) . . ? O4 C2 C16 118.4(16) . . ? O3 C2 C16 115.8(15) . . ? O6 C3 O5 124(2) . . ? O6 C3 C22 119(2) . . ? O5 C3 C22 117(2) . . ? N21 C22 C23 122.0(18) . . ? N21 C22 C3 113.8(17) . . ? C23 C22 C3 124.1(17) . . ? C22 C23 C24 119.5(16) . . ? C22 C23 H3 120.2 . . ? C24 C23 H3 120.2 . . ? C23 C24 C25 115.8(15) . . ? C23 C24 C14 120.7(13) . . ? C25 C24 C14 123.3(14) . . ? C26 C25 C24 120.0(17) . . ? C26 C25 H4 120.0 . . ? C24 C25 H4 120.0 . . ? N21 C26 C25 121.7(16) . . ? N21 C26 C4 113.9(16) . . ? C25 C26 C4 123.9(17) . . ? O7 C4 O8 129(2) . . ? O7 C4 C26 107.0(18) . . ? O8 C4 C26 124.0(19) . . ? C32 N31 C32 120(2) 2 . ? C32 N31 Dy2 119.8(11) 2 . ? C32 N31 Dy2 119.8(11) . . ? N31 C32 C33 121.2(18) . . ? N31 C32 C5 114.1(17) . . ? C33 C32 C5 124.7(17) . . ? C34 C33 C32 119.2(19) . . ? C34 C33 H5 120.4 . . ? C32 C33 H5 120.4 . . ? C33 C34 C33 119(2) . 2 ? C33 C34 C44 120.6(12) . . ? C33 C34 C44 120.6(12) 2 . ? C42 N41 C42 117(2) 2 . ? C42 N41 Dy1 121.5(11) 2 3_445 ? C42 N41 Dy1 121.5(11) . 3_445 ? N41 C42 C43 123(2) . . ? N41 C42 C6 112.1(16) . . ? C43 C42 C6 124.9(18) . . ? C44 C43 C42 121(2) . . ? C44 C43 H6 119.6 . . ? C42 C43 H6 119.6 . . ? C43 C44 C43 116(3) 2 . ? C43 C44 C34 122.1(15) 2 . ? C43 C44 C34 122.1(15) . . ? 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 O3 Dy1 O1 C1 4.4(16) . . . . ? O3 Dy1 O1 C1 161.9(15) 2_655 . . . ? O1 Dy1 O1 C1 -69.0(13) 2_655 . . . ? O11 Dy1 O1 C1 -150.2(12) 4 . . . ? O11 Dy1 O1 C1 71.2(14) 3 . . . ? N11 Dy1 O1 C1 -129.1(15) 2_655 . . . ? N11 Dy1 O1 C1 -4.4(13) . . . . ? N41 Dy1 O1 C1 111.0(13) 3 . . . ? O3 Dy1 O3 C2 -154.6(14) 2_655 . . . ? O1 Dy1 O3 C2 -22.6(16) . . . . ? O1 Dy1 O3 C2 62.5(13) 2_655 . . . ? O11 Dy1 O3 C2 141.5(13) 4 . . . ? O11 Dy1 O3 C2 -88.9(13) 3 . . . ? N11 Dy1 O3 C2 80.2(14) 2_655 . . . ? N11 Dy1 O3 C2 -13.9(13) . . . . ? N41 Dy1 O3 C2 -154.6(14) 3 . . . ? O4 Dy2 O4 C2 105.6(19) 2 . . . ? O13 Dy2 O4 C2 -28.8(19) . . . . ? O13 Dy2 O4 C2 -140.8(18) 2 . . . ? O14 Dy2 O4 C2 -106(2) . . . . ? O14 Dy2 O4 C2 -22(2) 2 . . . ? O9 Dy2 O4 C2 42.8(19) 2 . . . ? O9 Dy2 O4 C2 173(2) . . . . ? N31 Dy2 O4 C2 105.6(19) . . . . ? O10 Dy3 O5 C3 -164(3) 5_566 . . . ? O2 Dy3 O5 C3 -101(4) 5_666 . . . ? O12 Dy3 O5 C3 57(3) . . . . ? O15 Dy3 O5 C3 180(4) . . . . ? O16 Dy3 O5 C3 101(4) . . . . ? N21 Dy3 O5 C3 -20(3) . . . . ? O8 Dy3 O5 C3 16(4) 5_566 . . . ? O7 Dy3 O5 C3 -44(4) . . . . ? O10 Dy3 O7 C4 -144.4(19) 5_566 . . . ? O2 Dy3 O7 C4 129.1(18) 5_666 . . . ? O12 Dy3 O7 C4 -13(2) . . . . ? O15 Dy3 O7 C4 167.2(16) . . . . ? O5 Dy3 O7 C4 67(2) . . . . ? O16 Dy3 O7 C4 -80.9(19) . . . . ? N21 Dy3 O7 C4 43.0(16) . . . . ? O8 Dy3 O7 C4 -58.8(18) 5_566 . . . ? O4 Dy2 O9 C5 74.4(18) 2 . . . ? O4 Dy2 O9 C5 -65.7(18) . . . . ? O13 Dy2 O9 C5 -101.2(19) . . . . ? O13 Dy2 O9 C5 149.5(19) 2 . . . ? O14 Dy2 O9 C5 -141.5(19) . . . . ? O14 Dy2 O9 C5 129.5(18) 2 . . . ? O9 Dy2 O9 C5 7.2(16) 2 . . . ? N31 Dy2 O9 C5 7.2(16) . . . . ? O10 Dy3 O12 C6 -76(4) 5_566 . . . ? O2 Dy3 O12 C6 111(3) 5_666 . . . ? O15 Dy3 O12 C6 10(4) . . . . ? O5 Dy3 O12 C6 71(3) . . . . ? O16 Dy3 O12 C6 -67(4) . . . . ? N21 Dy3 O12 C6 140(4) . . . . ? O8 Dy3 O12 C6 -137(4) 5_566 . . . ? O7 Dy3 O12 C6 -170(3) . . . . ? O3 Dy1 N11 C16 12.5(12) . . . . ? O3 Dy1 N11 C16 166.3(11) 2_655 . . . ? O1 Dy1 N11 C16 -174.9(14) . . . . ? O1 Dy1 N11 C16 -66.7(13) 2_655 . . . ? O11 Dy1 N11 C16 -31.9(17) 4 . . . ? O11 Dy1 N11 C16 99.4(13) 3 . . . ? N11 Dy1 N11 C16 -119.2(14) 2_655 . . . ? N41 Dy1 N11 C16 60.8(14) 3 . . . ? O3 Dy1 N11 C12 -178.1(14) . . . . ? O3 Dy1 N11 C12 -24.3(16) 2_655 . . . ? O1 Dy1 N11 C12 -5.6(12) . . . . ? O1 Dy1 N11 C12 102.6(13) 2_655 . . . ? O11 Dy1 N11 C12 137.5(12) 4 . . . ? O11 Dy1 N11 C12 -91.3(13) 3 . . . ? N11 Dy1 N11 C12 50.2(11) 2_655 . . . ? N41 Dy1 N11 C12 -129.8(11) 3 . . . ? O10 Dy3 N21 C26 -33(2) 5_566 . . . ? O2 Dy3 N21 C26 -94.6(19) 5_666 . . . ? O12 Dy3 N21 C26 102.8(19) . . . . ? O15 Dy3 N21 C26 -152.3(19) . . . . ? O5 Dy3 N21 C26 -179(2) . . . . ? O16 Dy3 N21 C26 72(3) . . . . ? O8 Dy3 N21 C26 25.4(19) 5_566 . . . ? O7 Dy3 N21 C26 -21.4(19) . . . . ? O10 Dy3 N21 C22 163.0(17) 5_566 . . . ? O2 Dy3 N21 C22 101.5(18) 5_666 . . . ? O12 Dy3 N21 C22 -61.2(18) . . . . ? O15 Dy3 N21 C22 44(2) . . . . ? O5 Dy3 N21 C22 17.0(19) . . . . ? O16 Dy3 N21 C22 -92(3) . . . . ? O8 Dy3 N21 C22 -139(2) 5_566 . . . ? O7 Dy3 N21 C22 175(2) . . . . ? Dy2 O9 C5 O10 167.2(16) . . . . ? Dy2 O9 C5 C32 -10(3) . . . . ? Dy3 O10 C5 O9 64(4) 5_566 . . . ? Dy3 O10 C5 C32 -118(3) 5_566 . . . ? Dy3 O12 C6 O11 -6(6) . . . . ? Dy3 O12 C6 C42 175(2) . . . . ? Dy1 O11 C6 O12 168(2) 3_445 . . . ? Dy1 O11 C6 C42 -13(3) 3_445 . . . ? Dy3 O2 C1 O1 86(2) 5_666 . . . ? Dy3 O2 C1 C12 -95.5(17) 5_666 . . . ? Dy1 O1 C1 O2 -168.8(12) . . . . ? Dy1 O1 C1 C12 12(2) . . . . ? C16 N11 C12 C13 3(3) . . . . ? Dy1 N11 C12 C13 -166.5(13) . . . . ? C16 N11 C12 C1 -177.8(15) . . . . ? Dy1 N11 C12 C1 12.8(19) . . . . ? O2 C1 C12 N11 165.0(15) . . . . ? O1 C1 C12 N11 -16(2) . . . . ? O2 C1 C12 C13 -16(3) . . . . ? O1 C1 C12 C13 163.4(17) . . . . ? N11 C12 C13 C14 1(3) . . . . ? C1 C12 C13 C14 -178.7(16) . . . . ? C12 C13 C14 C15 -4(3) . . . . ? C12 C13 C14 C24 175.8(17) . . . . ? C13 C14 C15 C16 3(3) . . . . ? C24 C14 C15 C16 -176.0(17) . . . . ? C12 N11 C16 C15 -3(3) . . . . ? Dy1 N11 C16 C15 166.4(14) . . . . ? C12 N11 C16 C2 179.5(15) . . . . ? Dy1 N11 C16 C2 -11.0(19) . . . . ? C14 C15 C16 N11 0(3) . . . . ? C14 C15 C16 C2 177.1(16) . . . . ? Dy2 O4 C2 O3 29(3) . . . . ? Dy2 O4 C2 C16 -150.4(14) . . . . ? Dy1 O3 C2 O4 -166.0(14) . . . . ? Dy1 O3 C2 C16 14(2) . . . . ? N11 C16 C2 O4 178.5(16) . . . . ? C15 C16 C2 O4 1(3) . . . . ? N11 C16 C2 O3 -1(2) . . . . ? C15 C16 C2 O3 -178.5(17) . . . . ? Dy3 O5 C3 O6 -162(4) . . . . ? Dy3 O5 C3 C22 22(6) . . . . ? C26 N21 C22 C23 6(4) . . . . ? Dy3 N21 C22 C23 169(2) . . . . ? C26 N21 C22 C3 -177(3) . . . . ? Dy3 N21 C22 C3 -14(4) . . . . ? O6 C3 C22 N21 179(4) . . . . ? O5 C3 C22 N21 -4(6) . . . . ? O6 C3 C22 C23 -4(7) . . . . ? O5 C3 C22 C23 173(4) . . . . ? N21 C22 C23 C24 -3(4) . . . . ? C3 C22 C23 C24 -179(3) . . . . ? C22 C23 C24 C25 2(4) . . . . ? C22 C23 C24 C14 -175(2) . . . . ? C13 C14 C24 C23 -37(3) . . . . ? C15 C14 C24 C23 142(2) . . . . ? C13 C14 C24 C25 146(2) . . . . ? C15 C14 C24 C25 -35(3) . . . . ? C23 C24 C25 C26 -4(4) . . . . ? C14 C24 C25 C26 172(2) . . . . ? C22 N21 C26 C25 -8(4) . . . . ? Dy3 N21 C26 C25 -172(2) . . . . ? C22 N21 C26 C4 164(2) . . . . ? Dy3 N21 C26 C4 1(3) . . . . ? C24 C25 C26 N21 8(4) . . . . ? C24 C25 C26 C4 -164(2) . . . . ? Dy3 O7 C4 O8 122.1(16) . . . . ? Dy3 O7 C4 C26 -58.0(16) . . . . ? N21 C26 C4 O7 39(2) . . . . ? C25 C26 C4 O7 -149(3) . . . . ? N21 C26 C4 O8 -141(2) . . . . ? C25 C26 C4 O8 30(3) . . . . ? O4 Dy2 N31 C32 79.7(12) 2 . . 2 ? O4 Dy2 N31 C32 -100.3(12) . . . 2 ? O13 Dy2 N31 C32 -46.0(13) . . . 2 ? O13 Dy2 N31 C32 134.0(13) 2 . . 2 ? O14 Dy2 N31 C32 -141.5(13) . . . 2 ? O14 Dy2 N31 C32 38.5(13) 2 . . 2 ? O9 Dy2 N31 C32 -3.2(12) 2 . . 2 ? O9 Dy2 N31 C32 176.8(12) . . . 2 ? O4 Dy2 N31 C32 -100.3(12) 2 . . . ? O4 Dy2 N31 C32 79.7(12) . . . . ? O13 Dy2 N31 C32 134.0(13) . . . . ? O13 Dy2 N31 C32 -46.0(13) 2 . . . ? O14 Dy2 N31 C32 38.5(13) . . . . ? O14 Dy2 N31 C32 -141.5(13) 2 . . . ? O9 Dy2 N31 C32 176.8(12) 2 . . . ? O9 Dy2 N31 C32 -3.2(12) . . . . ? C32 N31 C32 C33 -1.0(17) 2 . . . ? Dy2 N31 C32 C33 179.0(17) . . . . ? C32 N31 C32 C5 -180(2) 2 . . . ? Dy2 N31 C32 C5 0(2) . . . . ? O9 C5 C32 N31 6(3) . . . . ? O10 C5 C32 N31 -171.3(17) . . . . ? O9 C5 C32 C33 -173(2) . . . . ? O10 C5 C32 C33 10(3) . . . . ? N31 C32 C33 C34 2(3) . . . . ? C5 C32 C33 C34 -179.2(18) . . . . ? C32 C33 C34 C33 -1.0(16) . . . 2 ? C32 C33 C34 C44 179.0(16) . . . . ? C42 N41 C42 C43 -1(2) 2 . . . ? Dy1 N41 C42 C43 179.0(19) 3_445 . . . ? C42 N41 C42 C6 -177(2) 2 . . . ? Dy1 N41 C42 C6 3(2) 3_445 . . . ? O12 C6 C42 N41 -175(2) . . . . ? O11 C6 C42 N41 6(3) . . . . ? O12 C6 C42 C43 9(4) . . . . ? O11 C6 C42 C43 -170(3) . . . . ? N41 C42 C43 C44 2(4) . . . . ? C6 C42 C43 C44 177(2) . . . . ? C42 C43 C44 C43 -0.9(19) . . . 2 ? C42 C43 C44 C34 179.1(19) . . . . ? C33 C34 C44 C43 150.5(18) . . . 2 ? C33 C34 C44 C43 -29.5(18) 2 . . 2 ? C33 C34 C44 C43 -29.5(18) . . . . ? C33 C34 C44 C43 150.5(18) 2 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.554 _refine_diff_density_min -7.301 _refine_diff_density_rms 0.354 #====END data_6 _database_code_depnum_ccdc_archive 'CCDC 702671' _audit_creation_date 'Sun Aug 19 14:03:30 2007' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Ho4(BPTCA)3(OH2)8] ; _chemical_name_common (Ho4(BPTCA)3(OH2)8) _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 Ho4 N6 O32 ' _chemical_formula_sum 'C42 H28 Ho4 N6 O32' _chemical_formula_weight 1788.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ho Ho -0.2175 4.6783 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 12.126(2) _cell_length_b 22.270(5) _cell_length_c 21.568(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.283(10) _cell_angle_gamma 90.00 _cell_volume 5618(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 12352 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 5.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 21062 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4942 _reflns_number_gt 3837 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0823P)^2^+1248.3945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4942 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1489 _refine_ls_R_factor_gt 0.1206 _refine_ls_wR_factor_ref 0.2918 _refine_ls_wR_factor_gt 0.2702 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.0000 0.21489(7) 0.2500 0.0389(5) Uani 1 2 d S . . Ho2 Ho 0.5000 0.25311(7) 0.2500 0.0358(4) Uani 1 2 d S . . Ho3 Ho 0.13963(11) 0.63036(10) 0.52568(6) 0.0786(7) Uani 1 1 d U . . O1 O 0.6443(15) 0.3244(8) 0.3021(8) 0.046(4) Uani 1 1 d . . . O2 O 0.7156(13) 0.3886(7) 0.3820(7) 0.033(3) Uani 1 1 d . . . O3 O 0.326(2) 0.2259(10) 0.2743(12) 0.078(5) Uani 1 1 d . . . O4 O 0.176(3) 0.2546(15) 0.3099(13) 0.118(8) Uani 1 1 d . . . O5 O 0.3010(15) 0.6572(9) 0.4888(9) 0.050(5) Uani 1 1 d . . . O6 O 0.408(4) 0.6389(11) 0.4226(17) 0.143(17) Uani 1 1 d . . . O7 O 0.052(2) 0.5447(10) 0.5315(11) 0.078(5) Uani 1 1 d D . . O8 O 0.158(3) 0.4562(13) 0.5804(12) 0.118(8) Uani 1 1 d D . . O9 O -0.0430(18) 0.2633(10) 0.3423(9) 0.058(5) Uani 1 1 d . . . O10 O -0.0366(18) 0.3455(12) 0.4038(9) 0.075(7) Uani 1 1 d . . . O11 O 0.0749(17) 0.7070(8) 0.3524(8) 0.056(5) Uani 1 1 d . . . O12 O 0.088(2) 0.6248(10) 0.4144(11) 0.080(7) Uani 1 1 d . . . O13 O 0.1471(19) 0.1569(10) 0.2172(13) 0.080(7) Uani 1 1 d . . . O14 O 0.078(2) 0.1445(10) 0.3366(12) 0.078(7) Uani 1 1 d . . . O15 O 0.192(4) 0.7274(13) 0.5634(18) 0.141(14) Uani 1 1 d U . . O16 O -0.053(5) 0.664(3) 0.469(3) 0.24(3) Uani 1 1 d U . . N11 N 0.4492(16) 0.3162(8) 0.3306(8) 0.033(4) Uani 1 1 d . . . N21 N 0.2442(18) 0.5443(11) 0.4938(9) 0.045(5) Uani 1 1 d . . . C5 C -0.037(3) 0.3175(16) 0.3521(14) 0.058(8) Uani 1 1 d . . . C6 C 0.069(2) 0.6522(13) 0.3613(13) 0.055(8) Uani 1 1 d . . . C1 C 0.6365(19) 0.3582(10) 0.3480(10) 0.032(5) Uani 1 1 d D . . C12 C 0.5176(17) 0.3604(9) 0.3597(10) 0.033(5) Uani 1 1 d D . . C13 C 0.4839(17) 0.4043(10) 0.3949(10) 0.034(5) Uani 1 1 d D . . H1 H 0.5362 0.4347 0.4148 0.034 Uiso 1 1 calc R . . C14 C 0.3728(18) 0.4045(10) 0.4015(10) 0.037(5) Uani 1 1 d D . . C15 C 0.304(2) 0.3547(9) 0.3746(10) 0.037(5) Uani 1 1 d D . . H2 H 0.2295 0.3505 0.3806 0.037 Uiso 1 1 calc R . . C16 C 0.344(2) 0.3126(9) 0.3400(10) 0.037(6) Uani 1 1 d D . . C2 C 0.279(2) 0.2587(10) 0.3041(11) 0.039(5) Uani 1 1 d DU . . C3 C 0.347(4) 0.6228(13) 0.456(2) 0.101(9) Uani 1 1 d DU . . C22 C 0.317(3) 0.5564(12) 0.4587(15) 0.065(6) Uani 1 1 d D . . C23 C 0.362(3) 0.5117(10) 0.4298(15) 0.061(6) Uani 1 1 d D . . H3 H 0.4152 0.5211 0.4056 0.061 Uiso 1 1 calc R . . C24 C 0.331(2) 0.4524(11) 0.4357(12) 0.047(6) Uani 1 1 d D . . C25 C 0.252(3) 0.4432(11) 0.4729(15) 0.061(6) Uani 1 1 d D . . H4 H 0.2283 0.4036 0.4798 0.061 Uiso 1 1 calc R . . C26 C 0.210(3) 0.4906(13) 0.4986(15) 0.065(6) Uani 1 1 d D . . C4 C 0.1271(18) 0.5012(10) 0.5397(12) 0.101(9) Uani 1 1 d D . . N31 N 0.0000 0.3272(12) 0.2500 0.045(7) Uani 1 2 d SD . . C32 C -0.016(2) 0.3576(10) 0.2997(11) 0.046(6) Uani 1 1 d D . . C33 C -0.018(3) 0.4189(11) 0.3009(15) 0.067(9) Uani 1 1 d D . . H5 H -0.0321 0.4394 0.3367 0.067 Uiso 1 1 calc R . . C34 C 0.0000 0.4509(15) 0.2500 0.064(12) Uani 1 2 d SD . . N41 N 0.0000 0.6425(11) 0.2500 0.054(9) Uani 1 2 d SD . . C42 C 0.031(3) 0.6115(10) 0.3042(12) 0.060(8) Uani 1 1 d D . . C43 C 0.030(3) 0.5502(11) 0.3066(14) 0.075(11) Uani 1 1 d D . . H6 H 0.0498 0.5299 0.3467 0.075 Uiso 1 1 calc R . . C44 C 0.0000 0.5185(14) 0.2500 0.070(14) Uani 1 2 d SD . . 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 Ho1 0.0513(10) 0.0337(8) 0.0416(9) 0.000 0.0299(8) 0.000 Ho2 0.0463(9) 0.0387(9) 0.0204(7) 0.000 0.0051(6) 0.000 Ho3 0.0316(7) 0.1685(19) 0.0373(7) -0.0470(9) 0.0118(5) 0.0091(8) O1 0.050(10) 0.063(12) 0.031(9) -0.007(8) 0.020(8) -0.001(9) O2 0.042(9) 0.031(8) 0.027(8) 0.006(7) 0.008(7) 0.006(7) O3 0.106(13) 0.062(10) 0.089(12) -0.001(9) 0.067(11) 0.006(9) O4 0.17(2) 0.127(18) 0.073(13) -0.041(13) 0.051(14) -0.039(17) O5 0.054(11) 0.059(11) 0.051(11) 0.006(9) 0.036(9) 0.024(9) O6 0.29(4) 0.058(15) 0.17(3) 0.022(17) 0.20(3) 0.01(2) O7 0.106(13) 0.062(10) 0.089(12) -0.001(9) 0.067(11) 0.006(9) O8 0.17(2) 0.127(18) 0.073(13) -0.041(13) 0.051(14) -0.039(17) O9 0.079(14) 0.064(13) 0.050(11) 0.003(10) 0.050(11) 0.002(11) O10 0.059(12) 0.14(2) 0.039(11) -0.026(12) 0.031(10) 0.012(13) O11 0.076(13) 0.044(11) 0.033(9) 0.016(8) -0.013(9) -0.016(10) O12 0.096(18) 0.068(14) 0.058(13) 0.020(12) -0.013(12) -0.024(13) O13 0.061(13) 0.069(14) 0.110(19) -0.044(14) 0.022(13) 0.006(12) O14 0.075(15) 0.063(14) 0.095(18) 0.019(13) 0.022(13) 0.001(12) O15 0.23(3) 0.086(18) 0.17(3) 0.042(18) 0.16(3) 0.07(2) O16 0.25(4) 0.27(4) 0.19(4) -0.05(3) 0.05(3) 0.10(4) N11 0.043(11) 0.038(10) 0.015(8) -0.006(8) 0.002(8) -0.014(9) N21 0.042(11) 0.068(15) 0.032(11) -0.021(10) 0.023(9) -0.012(11) C5 0.056(18) 0.08(2) 0.050(17) 0.019(16) 0.032(14) 0.013(16) C6 0.051(16) 0.055(18) 0.045(16) 0.012(14) -0.015(13) -0.009(14) C1 0.042(13) 0.038(12) 0.019(10) 0.005(9) 0.015(9) 0.004(11) C12 0.036(12) 0.034(12) 0.028(11) 0.007(9) 0.008(9) 0.016(10) C13 0.035(12) 0.033(12) 0.032(12) 0.005(10) 0.004(10) -0.002(10) C14 0.040(13) 0.041(13) 0.028(11) -0.005(10) 0.006(10) -0.003(11) C15 0.052(15) 0.031(12) 0.032(12) -0.003(10) 0.018(11) -0.003(11) C16 0.060(16) 0.034(12) 0.018(10) -0.001(9) 0.012(10) -0.014(11) C2 0.044(9) 0.043(9) 0.034(9) 0.016(7) 0.014(7) -0.009(8) C3 0.110(16) 0.097(16) 0.120(17) 0.042(14) 0.071(14) 0.013(13) C22 0.077(15) 0.075(15) 0.060(13) -0.004(11) 0.050(12) -0.015(13) C23 0.083(15) 0.047(11) 0.075(14) 0.003(10) 0.061(13) -0.007(11) C24 0.039(13) 0.071(19) 0.035(13) -0.013(13) 0.016(11) -0.007(13) C25 0.083(15) 0.047(11) 0.075(14) 0.003(10) 0.061(13) -0.007(11) C26 0.077(15) 0.075(15) 0.060(13) -0.004(11) 0.050(12) -0.015(13) C4 0.110(16) 0.097(16) 0.120(17) 0.042(14) 0.071(14) 0.013(13) N31 0.056(19) 0.046(18) 0.042(17) 0.000 0.029(15) 0.000 C32 0.063(17) 0.044(15) 0.043(14) -0.005(12) 0.034(13) 0.009(13) C33 0.062(19) 0.049(18) 0.09(2) -0.019(17) 0.020(18) 0.011(15) C34 0.07(3) 0.025(19) 0.11(4) 0.000 0.04(3) 0.000 N41 0.07(2) 0.022(15) 0.06(2) 0.000 -0.001(17) 0.000 C42 0.08(2) 0.031(14) 0.054(17) 0.007(12) -0.014(15) -0.006(14) C43 0.07(2) 0.042(16) 0.08(2) 0.019(16) -0.029(18) -0.009(15) C44 0.07(3) 0.023(18) 0.09(3) 0.000 -0.02(3) 0.000 _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 Ho1 O4 2.36(3) 2 ? Ho1 O4 2.36(3) . ? Ho1 O14 2.43(2) . ? Ho1 O14 2.43(2) 2 ? Ho1 O9 2.438(18) . ? Ho1 O9 2.438(18) 2 ? Ho1 O13 2.45(2) . ? Ho1 O13 2.45(2) 2 ? Ho1 N31 2.50(3) . ? Ho2 O3 2.38(2) . ? Ho2 O3 2.38(2) 2_655 ? Ho2 O11 2.387(16) 3_545 ? Ho2 O11 2.387(16) 4_545 ? Ho2 O1 2.410(18) 2_655 ? Ho2 O1 2.410(18) . ? Ho2 N11 2.436(18) . ? Ho2 N11 2.436(18) 2_655 ? Ho2 N41 2.46(3) 3_545 ? Ho3 O7 2.21(2) . ? Ho3 O10 2.272(17) 5_566 ? Ho3 O12 2.32(2) . ? Ho3 O2 2.320(15) 5_666 ? Ho3 O15 2.34(4) . ? Ho3 O5 2.375(17) . ? Ho3 O16 2.45(6) . ? Ho3 N21 2.49(2) . ? Ho3 C4 2.90(2) . ? O1 C1 1.27(3) . ? O2 C1 1.24(3) . ? O2 Ho3 2.320(15) 5_666 ? O3 C2 1.21(3) . ? O4 C2 1.29(4) . ? O5 C3 1.26(4) . ? O6 C3 1.22(4) . ? O7 C4 1.312(18) . ? O8 C4 1.32(4) . ? O9 C5 1.23(4) . ? O10 C5 1.28(4) . ? O10 Ho3 2.273(17) 5_566 ? O11 C6 1.24(3) . ? O11 Ho2 2.387(16) 3_455 ? O12 C6 1.27(3) . ? N11 C12 1.33(3) . ? N11 C16 1.34(3) . ? N21 C26 1.28(3) . ? N21 C22 1.33(3) . ? C5 C32 1.51(4) . ? C6 C42 1.50(4) . ? C1 C12 1.53(3) . ? C12 C13 1.36(3) . ? C13 C14 1.39(3) . ? C13 H1 0.9500 . ? C14 C15 1.42(2) . ? C14 C24 1.46(3) . ? C15 C16 1.37(3) . ? C15 H2 0.9500 . ? C16 C2 1.53(3) . ? C3 C22 1.53(3) . ? C22 C23 1.36(3) . ? C23 C24 1.39(3) . ? C23 H3 0.9500 . ? C24 C25 1.42(3) . ? C25 C26 1.35(3) . ? C25 H4 0.9500 . ? C26 C4 1.52(3) . ? N31 C32 1.32(2) 2 ? N31 C32 1.32(2) . ? C32 C33 1.37(3) . ? C33 C34 1.37(3) . ? C33 H5 0.9500 . ? C34 C33 1.37(3) 2 ? C34 C44 1.51(5) . ? N41 C42 1.33(2) . ? N41 C42 1.33(2) 2 ? N41 Ho2 2.46(3) 3_455 ? C42 C43 1.37(3) . ? C43 C44 1.37(3) . ? C43 H6 0.9500 . ? C44 C43 1.37(3) 2 ? 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 O4 Ho1 O4 136.0(18) 2 . ? O4 Ho1 O14 140.7(9) 2 . ? O4 Ho1 O14 73.1(10) . . ? O4 Ho1 O14 73.1(10) 2 2 ? O4 Ho1 O14 140.7(9) . 2 ? O14 Ho1 O14 99.7(12) . 2 ? O4 Ho1 O9 85.6(9) 2 . ? O4 Ho1 O9 75.3(9) . . ? O14 Ho1 O9 77.3(8) . . ? O14 Ho1 O9 142.2(8) 2 . ? O4 Ho1 O9 75.3(9) 2 2 ? O4 Ho1 O9 85.6(9) . 2 ? O14 Ho1 O9 142.2(8) . 2 ? O14 Ho1 O9 77.3(8) 2 2 ? O9 Ho1 O9 127.5(10) . 2 ? O4 Ho1 O13 131.5(9) 2 . ? O4 Ho1 O13 74.4(9) . . ? O14 Ho1 O13 73.7(9) . . ? O14 Ho1 O13 66.6(8) 2 . ? O9 Ho1 O13 142.8(8) . . ? O9 Ho1 O13 70.7(8) 2 . ? O4 Ho1 O13 74.4(9) 2 2 ? O4 Ho1 O13 131.5(9) . 2 ? O14 Ho1 O13 66.6(8) . 2 ? O14 Ho1 O13 73.7(9) 2 2 ? O9 Ho1 O13 70.7(8) . 2 ? O9 Ho1 O13 142.8(8) 2 2 ? O13 Ho1 O13 116.5(12) . 2 ? O4 Ho1 N31 68.0(9) 2 . ? O4 Ho1 N31 68.0(9) . . ? O14 Ho1 N31 130.2(6) . . ? O14 Ho1 N31 130.2(6) 2 . ? O9 Ho1 N31 63.8(5) . . ? O9 Ho1 N31 63.8(5) 2 . ? O13 Ho1 N31 121.8(6) . . ? O13 Ho1 N31 121.8(6) 2 . ? O3 Ho2 O3 150.5(11) . 2_655 ? O3 Ho2 O11 80.2(8) . 3_545 ? O3 Ho2 O11 87.2(8) 2_655 3_545 ? O3 Ho2 O11 87.2(8) . 4_545 ? O3 Ho2 O11 80.2(8) 2_655 4_545 ? O11 Ho2 O11 129.1(9) 3_545 4_545 ? O3 Ho2 O1 72.2(7) . 2_655 ? O3 Ho2 O1 129.9(7) 2_655 2_655 ? O11 Ho2 O1 140.1(7) 3_545 2_655 ? O11 Ho2 O1 78.4(6) 4_545 2_655 ? O3 Ho2 O1 129.9(7) . . ? O3 Ho2 O1 72.2(7) 2_655 . ? O11 Ho2 O1 78.4(6) 3_545 . ? O11 Ho2 O1 140.1(7) 4_545 . ? O1 Ho2 O1 97.6(9) 2_655 . ? O3 Ho2 N11 65.4(7) . . ? O3 Ho2 N11 135.1(8) 2_655 . ? O11 Ho2 N11 72.2(7) 3_545 . ? O11 Ho2 N11 143.3(6) 4_545 . ? O1 Ho2 N11 70.3(6) 2_655 . ? O1 Ho2 N11 65.0(6) . . ? O3 Ho2 N11 135.1(8) . 2_655 ? O3 Ho2 N11 65.5(7) 2_655 2_655 ? O11 Ho2 N11 143.3(7) 3_545 2_655 ? O11 Ho2 N11 72.2(7) 4_545 2_655 ? O1 Ho2 N11 65.0(6) 2_655 2_655 ? O1 Ho2 N11 70.3(6) . 2_655 ? N11 Ho2 N11 109.6(9) . 2_655 ? O3 Ho2 N41 75.3(5) . 3_545 ? O3 Ho2 N41 75.3(5) 2_655 3_545 ? O11 Ho2 N41 64.5(5) 3_545 3_545 ? O11 Ho2 N41 64.5(5) 4_545 3_545 ? O1 Ho2 N41 131.2(4) 2_655 3_545 ? O1 Ho2 N41 131.2(4) . 3_545 ? N11 Ho2 N41 125.2(4) . 3_545 ? N11 Ho2 N41 125.2(4) 2_655 3_545 ? O7 Ho3 O10 78.9(9) . 5_566 ? O7 Ho3 O12 90.5(8) . . ? O10 Ho3 O12 131.1(9) 5_566 . ? O7 Ho3 O2 93.5(8) . 5_666 ? O10 Ho3 O2 83.9(7) 5_566 5_666 ? O12 Ho3 O2 144.8(8) . 5_666 ? O7 Ho3 O15 150.5(8) . . ? O10 Ho3 O15 72.2(9) 5_566 . ? O12 Ho3 O15 112.7(10) . . ? O2 Ho3 O15 78.2(11) 5_666 . ? O7 Ho3 O5 133.6(7) . . ? O10 Ho3 O5 144.3(8) 5_566 . ? O12 Ho3 O5 72.0(8) . . ? O2 Ho3 O5 80.2(6) 5_666 . ? O15 Ho3 O5 73.3(8) . . ? O7 Ho3 O16 83.0(18) . . ? O10 Ho3 O16 69.0(14) 5_566 . ? O12 Ho3 O16 62.4(14) . . ? O2 Ho3 O16 152.8(13) 5_666 . ? O15 Ho3 O16 91.6(18) . . ? O5 Ho3 O16 121.3(17) . . ? O7 Ho3 N21 68.9(7) . . ? O10 Ho3 N21 140.9(9) 5_566 . ? O12 Ho3 N21 72.1(8) . . ? O2 Ho3 N21 76.8(6) 5_666 . ? O15 Ho3 N21 134.1(10) . . ? O5 Ho3 N21 64.9(7) . . ? O16 Ho3 N21 125.7(14) . . ? O7 Ho3 C4 25.4(5) . . ? O10 Ho3 C4 96.4(9) 5_566 . ? O12 Ho3 C4 92.7(7) . . ? O2 Ho3 C4 77.2(6) 5_666 . ? O15 Ho3 C4 153.8(10) . . ? O5 Ho3 C4 110.8(7) . . ? O16 Ho3 C4 106.4(17) . . ? N21 Ho3 C4 46.5(7) . . ? C1 O1 Ho2 124.1(15) . . ? C1 O2 Ho3 134.3(14) . 5_666 ? C2 O3 Ho2 122.3(19) . . ? C2 O4 Ho1 137(2) . . ? C3 O5 Ho3 124(2) . . ? C4 O7 Ho3 108.3(15) . . ? C5 O9 Ho1 124.0(17) . . ? C5 O10 Ho3 146(2) . 5_566 ? C6 O11 Ho2 122.9(17) . 3_455 ? C6 O12 Ho3 148(2) . . ? C12 N11 C16 117.9(18) . . ? C12 N11 Ho2 121.3(14) . . ? C16 N11 Ho2 120.2(13) . . ? C26 N21 C22 121(2) . . ? C26 N21 Ho3 119.7(16) . . ? C22 N21 Ho3 117.5(18) . . ? O9 C5 O10 128(3) . . ? O9 C5 C32 118(3) . . ? O10 C5 C32 114(3) . . ? O11 C6 O12 128(3) . . ? O11 C6 C42 119(2) . . ? O12 C6 C42 113(2) . . ? O2 C1 O1 125(2) . . ? O2 C1 C12 120.0(18) . . ? O1 C1 C12 115(2) . . ? N11 C12 C13 123.4(19) . . ? N11 C12 C1 113.2(18) . . ? C13 C12 C1 123.3(19) . . ? C12 C13 C14 119.9(19) . . ? C12 C13 H1 120.0 . . ? C14 C13 H1 120.0 . . ? C13 C14 C15 116.0(18) . . ? C13 C14 C24 121.9(17) . . ? C15 C14 C24 122.1(17) . . ? C16 C15 C14 120(2) . . ? C16 C15 H2 119.9 . . ? C14 C15 H2 119.9 . . ? N11 C16 C15 122.3(18) . . ? N11 C16 C2 110.7(18) . . ? C15 C16 C2 127(2) . . ? O3 C2 O4 128(3) . . ? O3 C2 C16 119(2) . . ? O4 C2 C16 113(2) . . ? O6 C3 O5 125(3) . . ? O6 C3 C22 119(3) . . ? O5 C3 C22 115(3) . . ? N21 C22 C23 121(2) . . ? N21 C22 C3 114(2) . . ? C23 C22 C3 124(2) . . ? C22 C23 C24 120(2) . . ? C22 C23 H3 120.1 . . ? C24 C23 H3 120.1 . . ? C23 C24 C25 116(2) . . ? C23 C24 C14 120.4(17) . . ? C25 C24 C14 123.8(19) . . ? C26 C25 C24 120(2) . . ? C26 C25 H4 119.9 . . ? C24 C25 H4 119.9 . . ? N21 C26 C25 122(2) . . ? N21 C26 C4 100(2) . . ? C25 C26 C4 138(2) . . ? O7 C4 O8 136(3) . . ? O7 C4 C26 125(3) . . ? O8 C4 C26 99(2) . . ? O7 C4 Ho3 46.2(12) . . ? O8 C4 Ho3 144.1(12) . . ? C26 C4 Ho3 91.9(15) . . ? C32 N31 C32 119(3) 2 . ? C32 N31 Ho1 120.7(14) 2 . ? C32 N31 Ho1 120.7(14) . . ? N31 C32 C33 122(2) . . ? N31 C32 C5 113(2) . . ? C33 C32 C5 125(2) . . ? C32 C33 C34 120(3) . . ? C32 C33 H5 120.2 . . ? C34 C33 H5 120.2 . . ? C33 C34 C33 118(3) . 2 ? C33 C34 C44 121.2(16) . . ? C33 C34 C44 121.2(16) 2 . ? C42 N41 C42 117(3) . 2 ? C42 N41 Ho2 121.5(14) . 3_455 ? C42 N41 Ho2 121.5(14) 2 3_455 ? N41 C42 C43 123(2) . . ? N41 C42 C6 111(2) . . ? C43 C42 C6 125(2) . . ? C42 C43 C44 119(3) . . ? C42 C43 H6 120.5 . . ? C44 C43 H6 120.5 . . ? C43 C44 C43 118(3) . 2 ? C43 C44 C34 121.0(15) . . ? C43 C44 C34 121.0(15) 2 . ? 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 O3 Ho2 O1 C1 -4(2) . . . . ? O3 Ho2 O1 C1 -161.6(19) 2_655 . . . ? O11 Ho2 O1 C1 -70.8(18) 3_545 . . . ? O11 Ho2 O1 C1 149.9(16) 4_545 . . . ? O1 Ho2 O1 C1 68.9(17) 2_655 . . . ? N11 Ho2 O1 C1 4.8(17) . . . . ? N11 Ho2 O1 C1 128.8(19) 2_655 . . . ? N41 Ho2 O1 C1 -111.1(17) 3_545 . . . ? O3 Ho2 O3 C2 154(2) 2_655 . . . ? O11 Ho2 O3 C2 88(2) 3_545 . . . ? O11 Ho2 O3 C2 -141(2) 4_545 . . . ? O1 Ho2 O3 C2 -62(2) 2_655 . . . ? O1 Ho2 O3 C2 23(3) . . . . ? N11 Ho2 O3 C2 14(2) . . . . ? N11 Ho2 O3 C2 -80(3) 2_655 . . . ? N41 Ho2 O3 C2 154(2) 3_545 . . . ? O4 Ho1 O4 C2 -109(4) 2 . . . ? O14 Ho1 O4 C2 103(4) . . . . ? O14 Ho1 O4 C2 18(5) 2 . . . ? O9 Ho1 O4 C2 -176(4) . . . . ? O9 Ho1 O4 C2 -46(4) 2 . . . ? O13 Ho1 O4 C2 26(4) . . . . ? O13 Ho1 O4 C2 137(3) 2 . . . ? N31 Ho1 O4 C2 -109(4) . . . . ? O7 Ho3 O5 C3 13(3) . . . . ? O10 Ho3 O5 C3 163(3) 5_566 . . . ? O12 Ho3 O5 C3 -60(3) . . . . ? O2 Ho3 O5 C3 98(3) 5_666 . . . ? O15 Ho3 O5 C3 179(3) . . . . ? O16 Ho3 O5 C3 -100(3) . . . . ? N21 Ho3 O5 C3 18(3) . . . . ? C4 Ho3 O5 C3 26(3) . . . . ? O10 Ho3 O7 C4 -132.7(17) 5_566 . . . ? O12 Ho3 O7 C4 95.3(17) . . . . ? O2 Ho3 O7 C4 -49.6(16) 5_666 . . . ? O15 Ho3 O7 C4 -122(3) . . . . ? O5 Ho3 O7 C4 30(2) . . . . ? O16 Ho3 O7 C4 157(2) . . . . ? N21 Ho3 O7 C4 24.8(15) . . . . ? O4 Ho1 O9 C5 -74(3) 2 . . . ? O4 Ho1 O9 C5 66(3) . . . . ? O14 Ho1 O9 C5 142(3) . . . . ? O14 Ho1 O9 C5 -129(2) 2 . . . ? O9 Ho1 O9 C5 -6(2) 2 . . . ? O13 Ho1 O9 C5 102(3) . . . . ? O13 Ho1 O9 C5 -149(3) 2 . . . ? N31 Ho1 O9 C5 -6(2) . . . . ? O7 Ho3 O12 C6 157(4) . . . . ? O10 Ho3 O12 C6 81(5) 5_566 . . . ? O2 Ho3 O12 C6 -106(4) 5_666 . . . ? O15 Ho3 O12 C6 -4(5) . . . . ? O5 Ho3 O12 C6 -67(4) . . . . ? O16 Ho3 O12 C6 75(5) . . . . ? N21 Ho3 O12 C6 -135(5) . . . . ? C4 Ho3 O12 C6 -178(4) . . . . ? O3 Ho2 N11 C12 177.4(19) . . . . ? O3 Ho2 N11 C12 24(2) 2_655 . . . ? O11 Ho2 N11 C12 90.2(17) 3_545 . . . ? O11 Ho2 N11 C12 -137.2(16) 4_545 . . . ? O1 Ho2 N11 C12 -103.8(17) 2_655 . . . ? O1 Ho2 N11 C12 5.0(15) . . . . ? N11 Ho2 N11 C12 -51.0(15) 2_655 . . . ? N41 Ho2 N11 C12 129.0(15) 3_545 . . . ? O3 Ho2 N11 C16 -12.1(16) . . . . ? O3 Ho2 N11 C16 -166.0(16) 2_655 . . . ? O11 Ho2 N11 C16 -99.2(17) 3_545 . . . ? O11 Ho2 N11 C16 33(2) 4_545 . . . ? O1 Ho2 N11 C16 66.7(16) 2_655 . . . ? O1 Ho2 N11 C16 175.5(18) . . . . ? N11 Ho2 N11 C16 119.6(17) 2_655 . . . ? N41 Ho2 N11 C16 -60.4(17) 3_545 . . . ? O7 Ho3 N21 C26 -5(2) . . . . ? O10 Ho3 N21 C26 32(3) 5_566 . . . ? O12 Ho3 N21 C26 -103(2) . . . . ? O2 Ho3 N21 C26 94(2) 5_666 . . . ? O15 Ho3 N21 C26 153(2) . . . . ? O5 Ho3 N21 C26 179(2) . . . . ? O16 Ho3 N21 C26 -69(3) . . . . ? C4 Ho3 N21 C26 9(2) . . . . ? O7 Ho3 N21 C22 160(2) . . . . ? O10 Ho3 N21 C22 -163(2) 5_566 . . . ? O12 Ho3 N21 C22 62(2) . . . . ? O2 Ho3 N21 C22 -101(2) 5_666 . . . ? O15 Ho3 N21 C22 -42(3) . . . . ? O5 Ho3 N21 C22 -16(2) . . . . ? O16 Ho3 N21 C22 96(3) . . . . ? C4 Ho3 N21 C22 174(3) . . . . ? Ho1 O9 C5 O10 -166(2) . . . . ? Ho1 O9 C5 C32 8(4) . . . . ? Ho3 O10 C5 O9 -66(5) 5_566 . . . ? Ho3 O10 C5 C32 120(4) 5_566 . . . ? Ho2 O11 C6 O12 -167(3) 3_455 . . . ? Ho2 O11 C6 C42 10(4) 3_455 . . . ? Ho3 O12 C6 O11 -2(7) . . . . ? Ho3 O12 C6 C42 -178(3) . . . . ? Ho3 O2 C1 O1 -86(3) 5_666 . . . ? Ho3 O2 C1 C12 95(2) 5_666 . . . ? Ho2 O1 C1 O2 168.6(16) . . . . ? Ho2 O1 C1 C12 -12(3) . . . . ? C16 N11 C12 C13 -4(3) . . . . ? Ho2 N11 C12 C13 166.2(17) . . . . ? C16 N11 C12 C1 177.2(18) . . . . ? Ho2 N11 C12 C1 -12(2) . . . . ? O2 C1 C12 N11 -165.5(19) . . . . ? O1 C1 C12 N11 15(3) . . . . ? O2 C1 C12 C13 16(3) . . . . ? O1 C1 C12 C13 -163(2) . . . . ? N11 C12 C13 C14 0(3) . . . . ? C1 C12 C13 C14 178(2) . . . . ? C12 C13 C14 C15 5(3) . . . . ? C12 C13 C14 C24 -177(2) . . . . ? C13 C14 C15 C16 -5(3) . . . . ? C24 C14 C15 C16 176(2) . . . . ? C12 N11 C16 C15 4(3) . . . . ? Ho2 N11 C16 C15 -166.5(17) . . . . ? C12 N11 C16 C2 -178.9(18) . . . . ? Ho2 N11 C16 C2 10(2) . . . . ? C14 C15 C16 N11 1(3) . . . . ? C14 C15 C16 C2 -176(2) . . . . ? Ho2 O3 C2 O4 166(3) . . . . ? Ho2 O3 C2 C16 -14(3) . . . . ? Ho1 O4 C2 O3 -26(6) . . . . ? Ho1 O4 C2 C16 153(3) . . . . ? N11 C16 C2 O3 2(3) . . . . ? C15 C16 C2 O3 178(2) . . . . ? N11 C16 C2 O4 -178(2) . . . . ? C15 C16 C2 O4 -1(4) . . . . ? Ho3 O5 C3 O6 159(4) . . . . ? Ho3 O5 C3 C22 -18(5) . . . . ? C26 N21 C22 C23 -4(5) . . . . ? Ho3 N21 C22 C23 -168(3) . . . . ? C26 N21 C22 C3 178(3) . . . . ? Ho3 N21 C22 C3 14(4) . . . . ? O6 C3 C22 N21 -176(4) . . . . ? O5 C3 C22 N21 2(6) . . . . ? O6 C3 C22 C23 6(7) . . . . ? O5 C3 C22 C23 -176(4) . . . . ? N21 C22 C23 C24 1(5) . . . . ? C3 C22 C23 C24 179(4) . . . . ? C22 C23 C24 C25 0(5) . . . . ? C22 C23 C24 C14 176(3) . . . . ? C13 C14 C24 C23 39(4) . . . . ? C15 C14 C24 C23 -143(3) . . . . ? C13 C14 C24 C25 -145(3) . . . . ? C15 C14 C24 C25 33(4) . . . . ? C23 C24 C25 C26 2(5) . . . . ? C14 C24 C25 C26 -174(3) . . . . ? C22 N21 C26 C25 5(5) . . . . ? Ho3 N21 C26 C25 170(3) . . . . ? C22 N21 C26 C4 -178(3) . . . . ? Ho3 N21 C26 C4 -13(3) . . . . ? C24 C25 C26 N21 -4(5) . . . . ? C24 C25 C26 C4 180(3) . . . . ? Ho3 O7 C4 O8 128.6(16) . . . . ? Ho3 O7 C4 C26 -51.3(16) . . . . ? N21 C26 C4 O7 44(3) . . . . ? C25 C26 C4 O7 -139(4) . . . . ? N21 C26 C4 O8 -136(3) . . . . ? C25 C26 C4 O8 41(4) . . . . ? N21 C26 C4 Ho3 10(2) . . . . ? C25 C26 C4 Ho3 -174(4) . . . . ? O10 Ho3 C4 O7 46.5(17) 5_566 . . . ? O12 Ho3 C4 O7 -85.4(18) . . . . ? O2 Ho3 C4 O7 128.8(17) 5_666 . . . ? O15 Ho3 C4 O7 108(2) . . . . ? O5 Ho3 C4 O7 -157.1(16) . . . . ? O16 Ho3 C4 O7 -23(2) . . . . ? N21 Ho3 C4 O7 -147.3(19) . . . . ? O7 Ho3 C4 O8 -112(5) . . . . ? O10 Ho3 C4 O8 -65(4) 5_566 . . . ? O12 Ho3 C4 O8 163(4) . . . . ? O2 Ho3 C4 O8 17(3) 5_666 . . . ? O15 Ho3 C4 O8 -3(5) . . . . ? O5 Ho3 C4 O8 91(4) . . . . ? O16 Ho3 C4 O8 -135(4) . . . . ? N21 Ho3 C4 O8 101(4) . . . . ? O7 Ho3 C4 C26 140(2) . . . . ? O10 Ho3 C4 C26 -173.0(15) 5_566 . . . ? O12 Ho3 C4 C26 55.1(15) . . . . ? O2 Ho3 C4 C26 -90.8(14) 5_666 . . . ? O15 Ho3 C4 C26 -111(2) . . . . ? O5 Ho3 C4 C26 -16.6(15) . . . . ? O16 Ho3 C4 C26 117.0(19) . . . . ? N21 Ho3 C4 C26 -6.9(15) . . . . ? O4 Ho1 N31 C32 -79.9(16) 2 . . 2 ? O4 Ho1 N31 C32 100.1(16) . . . 2 ? O14 Ho1 N31 C32 141.4(16) . . . 2 ? O14 Ho1 N31 C32 -38.6(16) 2 . . 2 ? O9 Ho1 N31 C32 -176.0(16) . . . 2 ? O9 Ho1 N31 C32 4.0(16) 2 . . 2 ? O13 Ho1 N31 C32 46.3(16) . . . 2 ? O13 Ho1 N31 C32 -133.7(16) 2 . . 2 ? O4 Ho1 N31 C32 100.1(16) 2 . . . ? O4 Ho1 N31 C32 -79.9(16) . . . . ? O14 Ho1 N31 C32 -38.6(16) . . . . ? O14 Ho1 N31 C32 141.4(16) 2 . . . ? O9 Ho1 N31 C32 4.0(16) . . . . ? O9 Ho1 N31 C32 -176.0(16) 2 . . . ? O13 Ho1 N31 C32 -133.7(16) . . . . ? O13 Ho1 N31 C32 46.3(16) 2 . . . ? C32 N31 C32 C33 1(2) 2 . . . ? Ho1 N31 C32 C33 -179(2) . . . . ? C32 N31 C32 C5 178(3) 2 . . . ? Ho1 N31 C32 C5 -2(3) . . . . ? O9 C5 C32 N31 -4(4) . . . . ? O10 C5 C32 N31 171(2) . . . . ? O9 C5 C32 C33 173(3) . . . . ? O10 C5 C32 C33 -12(4) . . . . ? N31 C32 C33 C34 -2(4) . . . . ? C5 C32 C33 C34 -179(2) . . . . ? C32 C33 C34 C33 1(2) . . . 2 ? C32 C33 C34 C44 -179(2) . . . . ? C42 N41 C42 C43 -1(3) 2 . . . ? Ho2 N41 C42 C43 179(3) 3_455 . . . ? C42 N41 C42 C6 177(3) 2 . . . ? Ho2 N41 C42 C6 -3(3) 3_455 . . . ? O11 C6 C42 N41 -4(4) . . . . ? O12 C6 C42 N41 173(3) . . . . ? O11 C6 C42 C43 174(3) . . . . ? O12 C6 C42 C43 -9(5) . . . . ? N41 C42 C43 C44 3(5) . . . . ? C6 C42 C43 C44 -175(3) . . . . ? C42 C43 C44 C43 -1(2) . . . 2 ? C42 C43 C44 C34 179(2) . . . . ? C33 C34 C44 C43 28(2) . . . . ? C33 C34 C44 C43 -152(2) 2 . . . ? C33 C34 C44 C43 -152(2) . . . 2 ? C33 C34 C44 C43 28(2) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 7.002 _refine_diff_density_min -8.689 _refine_diff_density_rms 0.414 #====END data_4-sq _database_code_depnum_ccdc_archive 'CCDC 713721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Tb4(BPTCA)3(OH2)8] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 N6 O32 Tb4 ' _chemical_formula_sum 'C42 H28 N6 O32 Tb4' _chemical_formula_weight 1764.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tb Tb -0.1723 4.1537 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 12.130(4) _cell_length_b 22.320(7) _cell_length_c 21.819(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.325(12) _cell_angle_gamma 90.00 _cell_volume 5697(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11328 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 5.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20483 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5015 _reflns_number_gt 3727 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. At first, the unit cell was found as F-centered orthorhombic symmetry but the intensity of the reflections showed C-centered monoclinic space group. The pseudo-symmetry resulted unusual thermal factors which were constrained by EADP instruction in SHELXL. The structure has a solvent-accessible large void space. Some intense peaks remained, which were to close to the framework to locate a reasonable molecule. The disordered solvent region was treated with SQUEEZE subroutine in PLATON software suite: Spek, A. L. J. Appl. Cryst. 2003. 36. 7-13. The sum total of 285 electrons were accounted for in the void space of 968.7 A^3^ ; _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^)+(0.1142P)^2^+318.3914P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5015 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2480 _refine_ls_wR_factor_gt 0.2309 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.0000 0.21250(5) 0.2500 0.0429(4) Uani 1 2 d S . . Tb2 Tb 0.5000 0.25298(5) 0.2500 0.0405(3) Uani 1 2 d S . . Tb3 Tb 0.13781(8) 0.63045(7) 0.52556(4) 0.0735(5) Uani 1 1 d U . . O1 O 0.6434(12) 0.3246(7) 0.3016(5) 0.058(4) Uani 1 1 d . . . O2 O 0.7149(10) 0.3891(5) 0.3816(5) 0.041(3) Uani 1 1 d . . . O3 O 0.3262(11) 0.2260(5) 0.2761(5) 0.047(3) Uani 1 1 d . . . O4 O 0.1784(11) 0.2533(5) 0.3126(6) 0.050(3) Uani 1 1 d . . . O5 O 0.3049(17) 0.6569(7) 0.4898(9) 0.091(4) Uani 1 1 d . . . O6 O 0.409(3) 0.6375(14) 0.4229(14) 0.172(8) Uani 1 1 d U . . O7 O 0.0596(16) 0.5412(7) 0.5354(9) 0.091(4) Uani 1 1 d D . . O8 O 0.170(3) 0.4459(12) 0.5850(13) 0.172(8) Uani 1 1 d D . . O9 O 0.0433(13) 0.2630(7) 0.1582(6) 0.062(4) Uani 1 1 d . . . O10 O 0.0359(13) 0.3449(8) 0.0978(6) 0.078(5) Uani 1 1 d . . . O11 O 0.0757(12) 0.7052(6) 0.3524(6) 0.054(3) Uani 1 1 d . . . O12 O 0.0884(14) 0.6230(7) 0.4134(6) 0.075(4) Uani 1 1 d . . . O13 O 0.1484(12) 0.1549(7) 0.2170(7) 0.071(4) Uani 1 1 d . . . O14 O 0.0771(14) 0.1414(7) 0.3366(8) 0.078(4) Uani 1 1 d . . . O15 O 0.198(2) 0.7281(8) 0.5656(12) 0.136(10) Uani 1 1 d U . . O16 O -0.052(3) 0.6669(19) 0.4735(16) 0.233(17) Uani 1 1 d U . . N11 N 0.4494(12) 0.3163(6) 0.3314(6) 0.038(3) Uani 1 1 d . . . N21 N 0.2446(13) 0.5449(8) 0.4939(6) 0.051(4) Uani 1 1 d . . . C5 C 0.0370(17) 0.3165(11) 0.1494(9) 0.058(5) Uani 1 1 d . . . C6 C 0.0685(17) 0.6501(11) 0.3609(9) 0.061(5) Uani 1 1 d . . . C1 C 0.6374(15) 0.3592(8) 0.3470(8) 0.043(4) Uani 1 1 d D . . C12 C 0.5192(13) 0.3603(7) 0.3608(7) 0.040(4) Uani 1 1 d D . . C13 C 0.4857(13) 0.4042(7) 0.3954(7) 0.039(4) Uani 1 1 d D . . H1 H 0.5371 0.4352 0.4145 0.047 Uiso 1 1 calc R . . C14 C 0.3740(15) 0.4030(7) 0.4024(8) 0.047(4) Uani 1 1 d D . . C15 C 0.3057(17) 0.3550(8) 0.3773(8) 0.053(5) Uani 1 1 d D . . H2 H 0.2315 0.3510 0.3838 0.064 Uiso 1 1 calc R . . C16 C 0.3470(14) 0.3124(7) 0.3423(7) 0.040(4) Uani 1 1 d D . . C2 C 0.2763(17) 0.2589(8) 0.3065(8) 0.048(4) Uani 1 1 d D . . C3 C 0.344(3) 0.6223(11) 0.4556(18) 0.123(8) Uani 1 1 d D . . C22 C 0.317(2) 0.5552(8) 0.4592(11) 0.070(4) Uani 1 1 d D . . C23 C 0.363(2) 0.5106(8) 0.4308(11) 0.067(4) Uani 1 1 d D . . H3 H 0.4164 0.5200 0.4071 0.081 Uiso 1 1 calc R . . C24 C 0.3316(15) 0.4507(8) 0.4370(8) 0.052(5) Uani 1 1 d D . . C25 C 0.2528(19) 0.4427(8) 0.4718(10) 0.067(4) Uani 1 1 d D . . H4 H 0.2251 0.4036 0.4759 0.081 Uiso 1 1 calc R . . C26 C 0.213(2) 0.4902(9) 0.5010(11) 0.070(4) Uani 1 1 d D . . C4 C 0.1329(16) 0.4947(8) 0.5472(10) 0.123(8) Uani 1 1 d DU . . N31 N 0.0000 0.3265(9) 0.2500 0.048(5) Uani 1 2 d SD . . C32 C 0.0168(17) 0.3573(7) 0.2008(8) 0.052(5) Uani 1 1 d D . . C33 C 0.017(2) 0.4179(8) 0.1988(10) 0.074(7) Uani 1 1 d D . . H5 H 0.0288 0.4380 0.1627 0.089 Uiso 1 1 calc R . . C34 C 0.0000 0.4509(9) 0.2500 0.057(7) Uani 1 2 d SD . . N41 N 0.0000 0.6414(9) 0.2500 0.053(6) Uani 1 2 d SD . . C42 C 0.0318(19) 0.6093(7) 0.3028(8) 0.058(5) Uani 1 1 d D . . C43 C 0.0319(19) 0.5488(8) 0.3055(9) 0.070(6) Uani 1 1 d D . . H6 H 0.0538 0.5291 0.3455 0.084 Uiso 1 1 calc R . . C44 C 0.0000 0.5154(15) 0.2500 0.097(13) Uani 1 2 d SD . . 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 0.0563(8) 0.0448(7) 0.0383(7) 0.000 0.0314(6) 0.000 Tb2 0.0505(7) 0.0520(7) 0.0214(5) 0.000 0.0135(5) 0.000 Tb3 0.0429(6) 0.1490(12) 0.0314(5) -0.0380(6) 0.0147(4) 0.0076(6) O1 0.070(9) 0.091(10) 0.024(6) -0.003(6) 0.029(6) 0.006(8) O2 0.044(7) 0.046(6) 0.036(6) 0.004(5) 0.015(5) -0.003(6) O3 0.063(8) 0.056(7) 0.021(5) -0.011(5) 0.012(5) -0.007(6) O4 0.055(8) 0.057(7) 0.048(7) -0.011(6) 0.032(6) -0.017(6) O5 0.123(10) 0.071(7) 0.109(10) -0.009(7) 0.086(9) 0.010(7) O6 0.221(16) 0.187(14) 0.153(13) -0.026(11) 0.129(13) -0.011(13) O7 0.123(10) 0.071(7) 0.109(10) -0.009(7) 0.086(9) 0.010(7) O8 0.221(16) 0.187(14) 0.153(13) -0.026(11) 0.129(13) -0.011(13) O9 0.088(11) 0.064(9) 0.053(8) -0.008(7) 0.054(8) -0.006(8) O10 0.075(10) 0.127(14) 0.042(8) 0.024(8) 0.032(7) -0.022(10) O11 0.072(9) 0.045(7) 0.035(7) 0.005(5) -0.003(6) -0.010(7) O12 0.090(11) 0.083(10) 0.040(8) 0.011(7) -0.001(7) -0.013(9) O13 0.063(9) 0.081(10) 0.074(10) -0.035(8) 0.027(8) 0.002(8) O14 0.072(10) 0.068(9) 0.092(12) 0.015(9) 0.018(9) 0.006(8) O15 0.24(2) 0.068(10) 0.165(19) 0.054(12) 0.163(19) 0.070(13) O16 0.23(3) 0.29(3) 0.15(2) -0.04(2) 0.01(2) 0.16(3) N11 0.047(8) 0.036(7) 0.030(7) 0.002(6) 0.009(6) 0.000(6) N21 0.054(9) 0.077(11) 0.032(8) -0.011(7) 0.028(7) -0.008(8) C5 0.051(11) 0.085(16) 0.046(11) -0.022(11) 0.030(9) -0.024(11) C6 0.048(11) 0.086(16) 0.041(11) -0.005(11) -0.002(9) -0.003(11) C1 0.045(10) 0.055(10) 0.034(9) 0.012(8) 0.018(8) 0.005(9) C12 0.046(10) 0.052(10) 0.025(8) 0.002(7) 0.014(7) -0.002(8) C13 0.045(10) 0.042(9) 0.027(8) -0.003(7) 0.006(7) -0.004(8) C14 0.064(12) 0.046(10) 0.039(9) -0.010(8) 0.027(9) -0.015(9) C15 0.078(14) 0.055(11) 0.034(9) -0.008(8) 0.028(9) -0.008(10) C16 0.049(10) 0.045(9) 0.029(8) -0.008(7) 0.016(7) -0.013(8) C2 0.062(12) 0.060(11) 0.027(8) -0.001(8) 0.019(8) -0.012(10) C3 0.127(15) 0.118(14) 0.154(16) 0.060(12) 0.088(13) 0.002(11) C22 0.077(10) 0.082(11) 0.072(10) -0.005(8) 0.059(9) -0.006(9) C23 0.093(12) 0.059(9) 0.072(10) -0.001(7) 0.060(9) -0.011(8) C24 0.047(10) 0.074(13) 0.041(10) -0.025(9) 0.023(8) -0.017(10) C25 0.093(12) 0.059(9) 0.072(10) -0.001(7) 0.060(9) -0.011(8) C26 0.077(10) 0.082(11) 0.072(10) -0.005(8) 0.059(9) -0.006(9) C4 0.127(15) 0.118(14) 0.154(16) 0.060(12) 0.088(13) 0.002(11) N31 0.055(13) 0.052(12) 0.048(12) 0.000 0.031(10) 0.000 C32 0.059(12) 0.053(11) 0.052(11) 0.002(9) 0.028(9) -0.013(9) C33 0.096(18) 0.050(12) 0.077(15) 0.002(11) 0.025(13) -0.031(12) C34 0.09(2) 0.014(10) 0.069(18) 0.000 0.023(16) 0.000 N41 0.062(14) 0.047(12) 0.044(13) 0.000 0.004(11) 0.000 C42 0.078(14) 0.038(10) 0.045(10) -0.004(8) -0.006(10) -0.004(10) C43 0.075(15) 0.063(13) 0.052(12) 0.000(10) -0.018(11) 0.004(12) C44 0.08(3) 0.12(3) 0.08(3) 0.000 -0.01(2) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.412(13) . ? Tb1 O4 2.411(12) 2 ? Tb1 O14 2.455(15) 2 ? Tb1 O14 2.455(15) . ? Tb1 O13 2.469(13) 2 ? Tb1 O13 2.469(13) . ? Tb1 O9 2.472(13) . ? Tb1 O9 2.472(13) 2 ? Tb1 N31 2.55(2) . ? Tb2 O3 2.402(13) 2_655 ? Tb2 O3 2.402(13) . ? Tb2 O1 2.411(14) . ? Tb2 O1 2.411(14) 2_655 ? Tb2 O11 2.427(12) 4_545 ? Tb2 O11 2.427(12) 3_545 ? Tb2 N11 2.470(13) . ? Tb2 N11 2.470(13) 2_655 ? Tb2 N41 2.49(2) 3_545 ? Tb3 O7 2.240(17) . ? Tb3 O10 2.312(12) 6_566 ? Tb3 O2 2.361(12) 5_666 ? Tb3 O12 2.367(14) . ? Tb3 O15 2.39(2) . ? Tb3 O16 2.42(3) . ? Tb3 O5 2.429(17) . ? Tb3 N21 2.504(16) . ? O1 C1 1.27(2) . ? O2 C1 1.24(2) . ? O2 Tb3 2.361(11) 5_666 ? O3 C2 1.25(2) . ? O4 C2 1.24(2) . ? O5 C3 1.25(3) . ? O6 C3 1.24(3) . ? O7 C4 1.347(17) . ? O8 C4 1.369(18) . ? O9 C5 1.21(3) . ? O10 C5 1.29(2) . ? O10 Tb3 2.312(12) 6_565 ? O11 C6 1.25(3) . ? O11 Tb2 2.427(12) 3_455 ? O12 C6 1.26(2) . ? N11 C16 1.33(2) . ? N11 C12 1.34(2) . ? N21 C26 1.30(3) . ? N21 C22 1.32(2) . ? C5 C32 1.51(3) . ? C6 C42 1.53(3) . ? C1 C12 1.54(2) . ? C12 C13 1.364(19) . ? C13 C14 1.40(2) . ? C13 H1 0.9500 . ? C14 C15 1.38(2) . ? C14 C24 1.47(2) . ? C15 C16 1.39(2) . ? C15 H2 0.9500 . ? C16 C2 1.55(2) . ? C3 C22 1.54(2) . ? C22 C23 1.37(2) . ? C23 C24 1.41(2) . ? C23 H3 0.9500 . ? C24 C25 1.380(19) . ? C25 C26 1.39(2) . ? C25 H4 0.9500 . ? C26 C4 1.58(2) . ? N31 C32 1.335(17) . ? N31 C32 1.335(17) 2 ? C32 C33 1.35(2) . ? C33 C34 1.40(2) . ? C33 H5 0.9500 . ? C34 C33 1.40(2) 2 ? C34 C44 1.44(4) . ? N41 C42 1.325(17) 2 ? N41 C42 1.325(17) . ? N41 Tb2 2.49(2) 3_455 ? C42 C43 1.35(2) . ? C43 C44 1.39(2) . ? C43 H6 0.9500 . ? C44 C43 1.39(2) 2 ? 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 O4 Tb1 O4 135.6(6) . 2 ? O4 Tb1 O14 141.5(5) . 2 ? O4 Tb1 O14 72.9(5) 2 2 ? O4 Tb1 O14 72.9(5) . . ? O4 Tb1 O14 141.5(5) 2 . ? O14 Tb1 O14 99.5(8) 2 . ? O4 Tb1 O13 130.2(5) . 2 ? O4 Tb1 O13 75.4(4) 2 2 ? O14 Tb1 O13 74.3(6) 2 2 ? O14 Tb1 O13 66.3(5) . 2 ? O4 Tb1 O13 75.4(4) . . ? O4 Tb1 O13 130.2(5) 2 . ? O14 Tb1 O13 66.3(5) 2 . ? O14 Tb1 O13 74.3(6) . . ? O13 Tb1 O13 117.2(8) 2 . ? O4 Tb1 O9 86.3(5) . . ? O4 Tb1 O9 73.7(5) 2 . ? O14 Tb1 O9 77.9(5) 2 . ? O14 Tb1 O9 143.0(5) . . ? O13 Tb1 O9 143.2(5) 2 . ? O13 Tb1 O9 70.9(5) . . ? O4 Tb1 O9 73.7(5) . 2 ? O4 Tb1 O9 86.3(5) 2 2 ? O14 Tb1 O9 143.0(5) 2 2 ? O14 Tb1 O9 77.9(5) . 2 ? O13 Tb1 O9 70.9(5) 2 2 ? O13 Tb1 O9 143.2(5) . 2 ? O9 Tb1 O9 125.8(6) . 2 ? O4 Tb1 N31 67.8(3) . . ? O4 Tb1 N31 67.8(3) 2 . ? O14 Tb1 N31 130.3(4) 2 . ? O14 Tb1 N31 130.3(4) . . ? O13 Tb1 N31 121.4(4) 2 . ? O13 Tb1 N31 121.4(4) . . ? O9 Tb1 N31 62.9(3) . . ? O9 Tb1 N31 62.9(3) 2 . ? O3 Tb2 O3 150.9(6) 2_655 . ? O3 Tb2 O1 73.0(4) 2_655 . ? O3 Tb2 O1 128.8(4) . . ? O3 Tb2 O1 128.8(4) 2_655 2_655 ? O3 Tb2 O1 73.0(4) . 2_655 ? O1 Tb2 O1 97.0(7) . 2_655 ? O3 Tb2 O11 79.3(4) 2_655 4_545 ? O3 Tb2 O11 88.0(4) . 4_545 ? O1 Tb2 O11 140.5(4) . 4_545 ? O1 Tb2 O11 79.1(4) 2_655 4_545 ? O3 Tb2 O11 88.0(4) 2_655 3_545 ? O3 Tb2 O11 79.3(4) . 3_545 ? O1 Tb2 O11 79.1(4) . 3_545 ? O1 Tb2 O11 140.5(4) 2_655 3_545 ? O11 Tb2 O11 127.9(6) 4_545 3_545 ? O3 Tb2 N11 135.6(4) 2_655 . ? O3 Tb2 N11 64.7(4) . . ? O1 Tb2 N11 64.6(4) . . ? O1 Tb2 N11 70.8(4) 2_655 . ? O11 Tb2 N11 143.9(5) 4_545 . ? O11 Tb2 N11 72.2(4) 3_545 . ? O3 Tb2 N11 64.7(4) 2_655 2_655 ? O3 Tb2 N11 135.6(4) . 2_655 ? O1 Tb2 N11 70.8(4) . 2_655 ? O1 Tb2 N11 64.6(4) 2_655 2_655 ? O11 Tb2 N11 72.2(4) 4_545 2_655 ? O11 Tb2 N11 143.9(5) 3_545 2_655 ? N11 Tb2 N11 110.2(6) . 2_655 ? O3 Tb2 N41 75.5(3) 2_655 3_545 ? O3 Tb2 N41 75.5(3) . 3_545 ? O1 Tb2 N41 131.5(3) . 3_545 ? O1 Tb2 N41 131.5(3) 2_655 3_545 ? O11 Tb2 N41 63.9(3) 4_545 3_545 ? O11 Tb2 N41 63.9(3) 3_545 3_545 ? N11 Tb2 N41 124.9(3) . 3_545 ? N11 Tb2 N41 124.9(3) 2_655 3_545 ? O7 Tb3 O10 80.2(6) . 6_566 ? O7 Tb3 O2 89.8(6) . 5_666 ? O10 Tb3 O2 83.0(5) 6_566 5_666 ? O7 Tb3 O12 92.2(6) . . ? O10 Tb3 O12 133.4(6) 6_566 . ? O2 Tb3 O12 143.3(5) 5_666 . ? O7 Tb3 O15 150.7(6) . . ? O10 Tb3 O15 72.6(6) 6_566 . ? O2 Tb3 O15 76.4(7) 5_666 . ? O12 Tb3 O15 114.3(6) . . ? O7 Tb3 O16 88.3(13) . . ? O10 Tb3 O16 68.1(9) 6_566 . ? O2 Tb3 O16 150.9(8) 5_666 . ? O12 Tb3 O16 65.7(9) . . ? O15 Tb3 O16 91.5(12) . . ? O7 Tb3 O5 131.1(5) . . ? O10 Tb3 O5 143.4(6) 6_566 . ? O2 Tb3 O5 79.3(6) 5_666 . ? O12 Tb3 O5 71.9(6) . . ? O15 Tb3 O5 72.2(6) . . ? O16 Tb3 O5 122.5(12) . . ? O7 Tb3 N21 67.2(5) . . ? O10 Tb3 N21 141.1(6) 6_566 . ? O2 Tb3 N21 76.5(4) 5_666 . ? O12 Tb3 N21 70.7(5) . . ? O15 Tb3 N21 131.7(7) . . ? O16 Tb3 N21 128.6(9) . . ? O5 Tb3 N21 63.9(5) . . ? C1 O1 Tb2 125.6(11) . . ? C1 O2 Tb3 134.9(11) . 5_666 ? C2 O3 Tb2 123.8(11) . . ? C2 O4 Tb1 136.2(11) . . ? C3 O5 Tb3 121.6(17) . . ? C4 O7 Tb3 115.4(12) . . ? C5 O9 Tb1 124.1(11) . . ? C5 O10 Tb3 146.0(15) . 6_565 ? C6 O11 Tb2 122.9(11) . 3_455 ? C6 O12 Tb3 147.3(15) . . ? C16 N11 C12 117.6(13) . . ? C16 N11 Tb2 120.9(10) . . ? C12 N11 Tb2 121.1(10) . . ? C26 N21 C22 119.5(16) . . ? C26 N21 Tb3 119.5(11) . . ? C22 N21 Tb3 119.7(13) . . ? O9 C5 O10 127.6(18) . . ? O9 C5 C32 119.5(17) . . ? O10 C5 C32 113(2) . . ? O11 C6 O12 126.9(19) . . ? O11 C6 C42 118.7(17) . . ? O12 C6 C42 114(2) . . ? O2 C1 O1 127.8(16) . . ? O2 C1 C12 118.0(14) . . ? O1 C1 C12 114.2(15) . . ? N11 C12 C13 123.2(14) . . ? N11 C12 C1 113.4(14) . . ? C13 C12 C1 123.2(14) . . ? C12 C13 C14 118.9(14) . . ? C12 C13 H1 120.5 . . ? C14 C13 H1 120.5 . . ? C15 C14 C13 118.0(15) . . ? C15 C14 C24 120.8(14) . . ? C13 C14 C24 121.2(12) . . ? C14 C15 C16 118.9(16) . . ? C14 C15 H2 120.5 . . ? C16 C15 H2 120.5 . . ? N11 C16 C15 122.9(14) . . ? N11 C16 C2 112.2(13) . . ? C15 C16 C2 124.6(15) . . ? O4 C2 O3 127.7(16) . . ? O4 C2 C16 116.3(15) . . ? O3 C2 C16 116.0(15) . . ? O6 C3 O5 125(3) . . ? O6 C3 C22 118(3) . . ? O5 C3 C22 117(2) . . ? N21 C22 C23 123.1(17) . . ? N21 C22 C3 112.5(18) . . ? C23 C22 C3 124.4(18) . . ? C22 C23 C24 119.5(15) . . ? C22 C23 H3 120.2 . . ? C24 C23 H3 120.2 . . ? C25 C24 C23 115.0(15) . . ? C25 C24 C14 125.0(14) . . ? C23 C24 C14 119.8(13) . . ? C24 C25 C26 122.0(17) . . ? C24 C25 H4 119.0 . . ? C26 C25 H4 119.0 . . ? N21 C26 C25 120.8(15) . . ? N21 C26 C4 105.5(15) . . ? C25 C26 C4 133.6(17) . . ? O7 C4 O8 146(2) . . ? O7 C4 C26 114.4(18) . . ? O8 C4 C26 100.0(18) . . ? C32 N31 C32 118(2) . 2 ? C32 N31 Tb1 120.9(11) . . ? C32 N31 Tb1 120.9(11) 2 . ? N31 C32 C33 122.8(17) . . ? N31 C32 C5 112.1(16) . . ? C33 C32 C5 125.1(17) . . ? C32 C33 C34 119.9(18) . . ? C32 C33 H5 120.1 . . ? C34 C33 H5 120.1 . . ? C33 C34 C33 117(2) . 2 ? C33 C34 C44 121.7(10) . . ? C33 C34 C44 121.7(10) 2 . ? C42 N41 C42 115(2) 2 . ? C42 N41 Tb2 122.7(10) 2 3_455 ? C42 N41 Tb2 122.7(10) . 3_455 ? N41 C42 C43 125.0(17) . . ? N41 C42 C6 110.7(15) . . ? C43 C42 C6 124.3(17) . . ? C42 C43 C44 120(2) . . ? C42 C43 H6 119.9 . . ? C44 C43 H6 119.9 . . ? C43 C44 C43 115(3) . 2 ? C43 C44 C34 122.5(14) . . ? C43 C44 C34 122.5(14) 2 . ? 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 O3 Tb2 O1 C1 -162.7(14) 2_655 . . . ? O3 Tb2 O1 C1 -4.9(16) . . . . ? O1 Tb2 O1 C1 68.8(13) 2_655 . . . ? O11 Tb2 O1 C1 150.1(12) 4_545 . . . ? O11 Tb2 O1 C1 -71.4(14) 3_545 . . . ? N11 Tb2 O1 C1 3.9(13) . . . . ? N11 Tb2 O1 C1 128.8(14) 2_655 . . . ? N41 Tb2 O1 C1 -111.2(13) 3_545 . . . ? O3 Tb2 O3 C2 155.1(13) 2_655 . . . ? O1 Tb2 O3 C2 23.0(15) . . . . ? O1 Tb2 O3 C2 -62.2(13) 2_655 . . . ? O11 Tb2 O3 C2 -141.4(13) 4_545 . . . ? O11 Tb2 O3 C2 89.4(13) 3_545 . . . ? N11 Tb2 O3 C2 14.1(13) . . . . ? N11 Tb2 O3 C2 -79.5(14) 2_655 . . . ? N41 Tb2 O3 C2 155.1(13) 3_545 . . . ? O4 Tb1 O4 C2 -105.4(18) 2 . . . ? O14 Tb1 O4 C2 22(2) 2 . . . ? O14 Tb1 O4 C2 105.7(18) . . . . ? O13 Tb1 O4 C2 141.5(17) 2 . . . ? O13 Tb1 O4 C2 28.0(18) . . . . ? O9 Tb1 O4 C2 -43.3(18) . . . . ? O9 Tb1 O4 C2 -172.2(18) 2 . . . ? N31 Tb1 O4 C2 -105.4(18) . . . . ? O7 Tb3 O5 C3 22(3) . . . . ? O10 Tb3 O5 C3 164(2) 6_566 . . . ? O2 Tb3 O5 C3 102(3) 5_666 . . . ? O12 Tb3 O5 C3 -55(3) . . . . ? O15 Tb3 O5 C3 -179(3) . . . . ? O16 Tb3 O5 C3 -99(3) . . . . ? N21 Tb3 O5 C3 22(2) . . . . ? O10 Tb3 O7 C4 -129.9(14) 6_566 . . . ? O2 Tb3 O7 C4 -47.0(13) 5_666 . . . ? O12 Tb3 O7 C4 96.4(13) . . . . ? O15 Tb3 O7 C4 -108.0(18) . . . . ? O16 Tb3 O7 C4 162.0(15) . . . . ? O5 Tb3 O7 C4 28.6(17) . . . . ? N21 Tb3 O7 C4 28.4(12) . . . . ? O4 Tb1 O9 C5 -73.3(17) . . . . ? O4 Tb1 O9 C5 66.6(17) 2 . . . ? O14 Tb1 O9 C5 142.1(18) 2 . . . ? O14 Tb1 O9 C5 -128.2(17) . . . . ? O13 Tb1 O9 C5 100.6(18) 2 . . . ? O13 Tb1 O9 C5 -149.1(18) . . . . ? O9 Tb1 O9 C5 -6.4(16) 2 . . . ? N31 Tb1 O9 C5 -6.4(16) . . . . ? O7 Tb3 O12 C6 157(3) . . . . ? O10 Tb3 O12 C6 78(3) 6_566 . . . ? O2 Tb3 O12 C6 -111(3) 5_666 . . . ? O15 Tb3 O12 C6 -11(3) . . . . ? O16 Tb3 O12 C6 70(3) . . . . ? O5 Tb3 O12 C6 -71(3) . . . . ? N21 Tb3 O12 C6 -138(3) . . . . ? O3 Tb2 N11 C16 -165.2(11) 2_655 . . . ? O3 Tb2 N11 C16 -11.2(11) . . . . ? O1 Tb2 N11 C16 176.4(13) . . . . ? O1 Tb2 N11 C16 68.5(12) 2_655 . . . ? O11 Tb2 N11 C16 33.4(16) 4_545 . . . ? O11 Tb2 N11 C16 -97.5(12) 3_545 . . . ? N11 Tb2 N11 C16 120.7(13) 2_655 . . . ? N41 Tb2 N11 C16 -59.3(13) 3_545 . . . ? O3 Tb2 N11 C12 22.3(14) 2_655 . . . ? O3 Tb2 N11 C12 176.3(13) . . . . ? O1 Tb2 N11 C12 4.0(11) . . . . ? O1 Tb2 N11 C12 -103.9(12) 2_655 . . . ? O11 Tb2 N11 C12 -139.1(11) 4_545 . . . ? O11 Tb2 N11 C12 90.1(12) 3_545 . . . ? N11 Tb2 N11 C12 -51.7(11) 2_655 . . . ? N41 Tb2 N11 C12 128.3(11) 3_545 . . . ? O7 Tb3 N21 C26 -4.2(16) . . . . ? O10 Tb3 N21 C26 31(2) 6_566 . . . ? O2 Tb3 N21 C26 91.4(17) 5_666 . . . ? O12 Tb3 N21 C26 -105.3(17) . . . . ? O15 Tb3 N21 C26 148.9(17) . . . . ? O16 Tb3 N21 C26 -72(2) . . . . ? O5 Tb3 N21 C26 175.9(18) . . . . ? O7 Tb3 N21 C22 162.6(18) . . . . ? O10 Tb3 N21 C22 -162.0(15) 6_566 . . . ? O2 Tb3 N21 C22 -101.8(16) 5_666 . . . ? O12 Tb3 N21 C22 61.5(16) . . . . ? O15 Tb3 N21 C22 -44.3(19) . . . . ? O16 Tb3 N21 C22 95(2) . . . . ? O5 Tb3 N21 C22 -17.3(16) . . . . ? Tb1 O9 C5 O10 -165.1(15) . . . . ? Tb1 O9 C5 C32 8(3) . . . . ? Tb3 O10 C5 O9 -65(4) 6_565 . . . ? Tb3 O10 C5 C32 121(2) 6_565 . . . ? Tb2 O11 C6 O12 -167.8(17) 3_455 . . . ? Tb2 O11 C6 C42 12(3) 3_455 . . . ? Tb3 O12 C6 O11 4(4) . . . . ? Tb3 O12 C6 C42 -176.4(19) . . . . ? Tb3 O2 C1 O1 -84(2) 5_666 . . . ? Tb3 O2 C1 C12 93.2(18) 5_666 . . . ? Tb2 O1 C1 O2 167.0(13) . . . . ? Tb2 O1 C1 C12 -10(2) . . . . ? C16 N11 C12 C13 -7(2) . . . . ? Tb2 N11 C12 C13 165.5(12) . . . . ? C16 N11 C12 C1 177.6(14) . . . . ? Tb2 N11 C12 C1 -9.7(17) . . . . ? O2 C1 C12 N11 -165.0(14) . . . . ? O1 C1 C12 N11 12(2) . . . . ? O2 C1 C12 C13 20(2) . . . . ? O1 C1 C12 C13 -162.9(16) . . . . ? N11 C12 C13 C14 2(2) . . . . ? C1 C12 C13 C14 176.5(15) . . . . ? C12 C13 C14 C15 4(3) . . . . ? C12 C13 C14 C24 -177.4(16) . . . . ? C13 C14 C15 C16 -5(3) . . . . ? C24 C14 C15 C16 176.9(17) . . . . ? C12 N11 C16 C15 7(2) . . . . ? Tb2 N11 C16 C15 -166.0(13) . . . . ? C12 N11 C16 C2 -178.8(14) . . . . ? Tb2 N11 C16 C2 8.5(18) . . . . ? C14 C15 C16 N11 -1(3) . . . . ? C14 C15 C16 C2 -174.6(17) . . . . ? Tb1 O4 C2 O3 -30(3) . . . . ? Tb1 O4 C2 C16 152.1(12) . . . . ? Tb2 O3 C2 O4 166.6(14) . . . . ? Tb2 O3 C2 C16 -15(2) . . . . ? N11 C16 C2 O4 -177.8(15) . . . . ? C15 C16 C2 O4 -3(3) . . . . ? N11 C16 C2 O3 4(2) . . . . ? C15 C16 C2 O3 178.1(16) . . . . ? Tb3 O5 C3 O6 161(3) . . . . ? Tb3 O5 C3 C22 -24(4) . . . . ? C26 N21 C22 C23 -2(4) . . . . ? Tb3 N21 C22 C23 -168(2) . . . . ? C26 N21 C22 C3 180(2) . . . . ? Tb3 N21 C22 C3 13(3) . . . . ? O6 C3 C22 N21 -178(3) . . . . ? O5 C3 C22 N21 7(4) . . . . ? O6 C3 C22 C23 3(5) . . . . ? O5 C3 C22 C23 -172(3) . . . . ? N21 C22 C23 C24 2(4) . . . . ? C3 C22 C23 C24 -180(3) . . . . ? C22 C23 C24 C25 1(3) . . . . ? C22 C23 C24 C14 175(2) . . . . ? C15 C14 C24 C25 30(3) . . . . ? C13 C14 C24 C25 -148(2) . . . . ? C15 C14 C24 C23 -143(2) . . . . ? C13 C14 C24 C23 38(3) . . . . ? C23 C24 C25 C26 -3(3) . . . . ? C14 C24 C25 C26 -177(2) . . . . ? C22 N21 C26 C25 -1(4) . . . . ? Tb3 N21 C26 C25 165.9(18) . . . . ? C22 N21 C26 C4 177.3(19) . . . . ? Tb3 N21 C26 C4 -16(2) . . . . ? C24 C25 C26 N21 3(4) . . . . ? C24 C25 C26 C4 -174(2) . . . . ? Tb3 O7 C4 O8 130.1(15) . . . . ? Tb3 O7 C4 C26 -49.8(14) . . . . ? N21 C26 C4 O7 42(2) . . . . ? C25 C26 C4 O7 -141(3) . . . . ? N21 C26 C4 O8 -138(2) . . . . ? C25 C26 C4 O8 39(3) . . . . ? O4 Tb1 N31 C32 101.0(11) . . . . ? O4 Tb1 N31 C32 -79.0(11) 2 . . . ? O14 Tb1 N31 C32 -38.7(11) 2 . . . ? O14 Tb1 N31 C32 141.3(11) . . . . ? O13 Tb1 N31 C32 -134.5(11) 2 . . . ? O13 Tb1 N31 C32 45.5(11) . . . . ? O9 Tb1 N31 C32 3.4(11) . . . . ? O9 Tb1 N31 C32 -176.6(11) 2 . . . ? O4 Tb1 N31 C32 -79.0(11) . . . 2 ? O4 Tb1 N31 C32 101.0(11) 2 . . 2 ? O14 Tb1 N31 C32 141.3(11) 2 . . 2 ? O14 Tb1 N31 C32 -38.7(11) . . . 2 ? O13 Tb1 N31 C32 45.5(11) 2 . . 2 ? O13 Tb1 N31 C32 -134.5(11) . . . 2 ? O9 Tb1 N31 C32 -176.6(11) . . . 2 ? O9 Tb1 N31 C32 3.4(11) 2 . . 2 ? C32 N31 C32 C33 -0.2(17) 2 . . . ? Tb1 N31 C32 C33 179.8(17) . . . . ? C32 N31 C32 C5 178.8(19) 2 . . . ? Tb1 N31 C32 C5 -1.2(19) . . . . ? O9 C5 C32 N31 -4(3) . . . . ? O10 C5 C32 N31 170.0(15) . . . . ? O9 C5 C32 C33 175(2) . . . . ? O10 C5 C32 C33 -11(3) . . . . ? N31 C32 C33 C34 0(3) . . . . ? C5 C32 C33 C34 -178.4(18) . . . . ? C32 C33 C34 C33 -0.2(15) . . . 2 ? C32 C33 C34 C44 179.8(15) . . . . ? C42 N41 C42 C43 -1.0(19) 2 . . . ? Tb2 N41 C42 C43 179.0(19) 3_455 . . . ? C42 N41 C42 C6 179(2) 2 . . . ? Tb2 N41 C42 C6 -1(2) 3_455 . . . ? O11 C6 C42 N41 -7(3) . . . . ? O12 C6 C42 N41 172.9(18) . . . . ? O11 C6 C42 C43 173(2) . . . . ? O12 C6 C42 C43 -7(3) . . . . ? N41 C42 C43 C44 2(4) . . . . ? C6 C42 C43 C44 -178.3(18) . . . . ? C42 C43 C44 C43 -0.9(17) . . . 2 ? C42 C43 C44 C34 179.1(17) . . . . ? C33 C34 C44 C43 -151.8(17) . . . . ? C33 C34 C44 C43 28.2(17) 2 . . . ? C33 C34 C44 C43 28.2(17) . . . 2 ? C33 C34 C44 C43 -151.8(17) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.370 _refine_diff_density_min -4.776 _refine_diff_density_rms 0.285 #====END data_5-sq _database_code_depnum_ccdc_archive 'CCDC 713722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Dy4(BPTCA)3(OH2)8] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 Dy4 N6 O32 ' _chemical_formula_sum 'C42 H28 Dy4 N6 O32' _chemical_formula_weight 1778.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Dy Dy -0.1892 4.4098 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 12.1025(16) _cell_length_b 22.287(4) _cell_length_c 21.695(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.315(8) _cell_angle_gamma 90.00 _cell_volume 5644.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 15753 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 5.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21653 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4967 _reflns_number_gt 4187 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. At first, the unit cell was found as F-centered orthorhombic symmetry but the intensity of the reflections showed C-centered monoclinic space group. The pseudo-symmetry resulted unusual thermal factors which were constrained by EADP instruction in SHELXL. The structure has a solvent-accessible large void space. Some intense peaks remained, which were to close to the framework to locate a reasonable molecule. The disordered solvent region was treated with SQUEEZE subroutine in PLATON software suite: Spek, A. L. J. Appl. Cryst. 2003. 36. 7-13. The sum total of 268 electrons were accounted for in the void space of 1057.7 A^3^ ; _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^)+(0.0709P)^2^+467.9748P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4967 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2144 _refine_ls_wR_factor_gt 0.2069 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.102 _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 Dy1 Dy 0.5000 0.74694(5) 0.2500 0.0350(3) Uani 1 2 d S . . Dy2 Dy 0.0000 0.78664(5) 0.2500 0.0380(3) Uani 1 2 d S . . Dy3 Dy 0.13866(7) 0.36983(6) 0.52571(4) 0.0708(4) Uani 1 1 d U . . O1 O 0.6438(10) 0.6752(5) 0.3016(5) 0.045(3) Uani 1 1 d . . . O2 O 0.7149(9) 0.6109(4) 0.3813(5) 0.035(2) Uani 1 1 d . . . O3 O 0.3260(10) 0.7742(5) 0.2753(5) 0.041(3) Uani 1 1 d . . . O4 O 0.1767(10) 0.7469(5) 0.3109(5) 0.047(3) Uani 1 1 d . . . O5 O 0.3044(18) 0.3426(8) 0.4899(10) 0.108(5) Uani 1 1 d . . . O6 O 0.410(3) 0.3625(9) 0.4231(14) 0.172(9) Uani 1 1 d . . . O7 O 0.1267(18) 0.4768(8) 0.5751(10) 0.108(5) Uani 1 1 d D . . O8 O 0.014(2) 0.5524(9) 0.5020(12) 0.172(9) Uani 1 1 d DU . . O9 O -0.0427(12) 0.7373(6) 0.3422(6) 0.056(3) Uani 1 1 d . . . O10 O -0.0366(12) 0.6548(7) 0.4029(6) 0.072(4) Uani 1 1 d U . . O11 O 0.0766(11) 0.2940(5) 0.3525(5) 0.049(3) Uani 1 1 d . . . O12 O 0.0884(14) 0.3759(7) 0.4141(7) 0.075(4) Uani 1 1 d . . . O13 O 0.1483(11) 0.8446(6) 0.2183(8) 0.067(4) Uani 1 1 d . . . O14 O 0.0772(13) 0.8577(6) 0.3370(8) 0.076(4) Uani 1 1 d . . . O15 O 0.194(2) 0.2714(8) 0.5651(12) 0.133(9) Uani 1 1 d U . . O16 O -0.047(3) 0.3299(19) 0.4713(14) 0.239(18) Uani 1 1 d U . . N11 N 0.4493(11) 0.6837(5) 0.3315(6) 0.035(3) Uani 1 1 d . . . N21 N 0.2435(12) 0.4558(7) 0.4936(6) 0.049(4) Uani 1 1 d . . . C5 C -0.0350(15) 0.6814(10) 0.3521(9) 0.053(5) Uani 1 1 d . . . C6 C 0.0681(16) 0.3496(9) 0.3618(8) 0.056(5) Uani 1 1 d . . . C1 C 0.6357(12) 0.6422(6) 0.3469(7) 0.032(3) Uani 1 1 d D . . C12 C 0.5179(12) 0.6391(6) 0.3592(6) 0.033(3) Uani 1 1 d D . . C13 C 0.4844(12) 0.5953(7) 0.3952(7) 0.037(3) Uani 1 1 d D . . H1 H 0.5356 0.5643 0.4147 0.045 Uiso 1 1 calc R . . C14 C 0.3723(12) 0.5975(6) 0.4024(7) 0.039(3) Uani 1 1 d D . . C15 C 0.3036(13) 0.6460(6) 0.3754(7) 0.039(4) Uani 1 1 d D . . H2 H 0.2290 0.6503 0.3813 0.047 Uiso 1 1 calc R . . C16 C 0.3452(13) 0.6874(6) 0.3402(7) 0.037(3) Uani 1 1 d D . . C2 C 0.2763(13) 0.7404(7) 0.3065(6) 0.037(4) Uani 1 1 d D . . C3 C 0.346(3) 0.3785(9) 0.456(2) 0.140(12) Uani 1 1 d D . . C22 C 0.3161(19) 0.4442(7) 0.4590(10) 0.063(4) Uani 1 1 d D . . C23 C 0.3616(18) 0.4891(7) 0.4300(10) 0.062(4) Uani 1 1 d D . . H3 H 0.4139 0.4797 0.4055 0.074 Uiso 1 1 calc R . . C24 C 0.3306(13) 0.5487(7) 0.4365(8) 0.046(4) Uani 1 1 d D . . C25 C 0.2545(18) 0.5582(8) 0.4736(10) 0.062(4) Uani 1 1 d D . . H4 H 0.2335 0.5980 0.4815 0.074 Uiso 1 1 calc R . . C26 C 0.2094(18) 0.5104(8) 0.4990(10) 0.063(4) Uani 1 1 d D . . C4 C 0.1053(17) 0.5151(7) 0.5262(9) 0.140(12) Uani 1 1 d D . . N31 N 0.0000 0.6724(8) 0.2500 0.043(4) Uani 1 2 d SD . . C32 C -0.0165(16) 0.6428(7) 0.2998(8) 0.048(4) Uani 1 1 d D . . C33 C -0.0182(17) 0.5806(7) 0.3018(9) 0.060(5) Uani 1 1 d D . . H5 H -0.0315 0.5601 0.3376 0.072 Uiso 1 1 calc R . . C34 C 0.0000 0.5490(9) 0.2500 0.067(8) Uani 1 2 d SD . . N41 N 0.0000 0.3581(8) 0.2500 0.051(5) Uani 1 2 d SD . . C42 C 0.0301(17) 0.3890(6) 0.3040(8) 0.051(4) Uani 1 1 d D . . C43 C 0.0316(19) 0.4509(7) 0.3063(9) 0.071(6) Uani 1 1 d D . . H6 H 0.0542 0.4711 0.3462 0.086 Uiso 1 1 calc R . . C44 C 0.0000 0.4835(12) 0.2500 0.073(9) Uani 1 2 d SD . . 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 Dy1 0.0450(6) 0.0389(6) 0.0218(5) 0.000 0.0101(4) 0.000 Dy2 0.0499(6) 0.0334(6) 0.0407(6) 0.000 0.0295(5) 0.000 Dy3 0.0362(5) 0.1442(11) 0.0348(5) 0.0393(6) 0.0143(4) -0.0096(5) O1 0.050(7) 0.057(7) 0.031(6) 0.010(5) 0.018(5) 0.003(6) O2 0.039(6) 0.034(5) 0.033(5) -0.003(4) 0.009(5) -0.004(5) O3 0.051(7) 0.043(6) 0.031(5) 0.005(5) 0.014(5) 0.006(5) O4 0.051(7) 0.052(7) 0.046(7) 0.015(5) 0.025(6) 0.021(6) O5 0.137(12) 0.094(9) 0.131(12) 0.034(8) 0.105(10) 0.025(8) O6 0.30(2) 0.081(9) 0.230(18) 0.044(11) 0.235(19) 0.059(12) O7 0.137(12) 0.094(9) 0.131(12) 0.034(8) 0.105(10) 0.025(8) O8 0.30(2) 0.081(9) 0.230(18) 0.044(11) 0.235(19) 0.059(12) O9 0.077(9) 0.057(8) 0.048(7) -0.008(6) 0.044(7) 0.000(7) O10 0.067(9) 0.112(12) 0.050(8) 0.030(8) 0.038(7) -0.018(8) O11 0.069(8) 0.032(6) 0.032(6) -0.006(5) -0.011(5) 0.015(5) O12 0.094(11) 0.069(9) 0.049(8) -0.022(7) -0.003(7) 0.013(8) O13 0.051(8) 0.056(8) 0.095(11) 0.038(8) 0.019(7) -0.004(6) O14 0.075(10) 0.057(9) 0.094(12) -0.025(8) 0.018(9) 0.001(7) O15 0.23(2) 0.065(10) 0.171(19) -0.034(11) 0.161(19) -0.052(13) O16 0.24(3) 0.31(3) 0.14(2) 0.06(2) 0.00(2) -0.19(3) N11 0.046(7) 0.035(7) 0.026(6) 0.001(5) 0.011(5) 0.011(6) N21 0.054(8) 0.069(10) 0.036(7) 0.014(7) 0.032(7) 0.012(7) C5 0.049(10) 0.073(13) 0.048(10) -0.004(9) 0.033(9) -0.008(9) C6 0.054(11) 0.066(13) 0.037(9) -0.010(9) -0.010(8) 0.011(9) C1 0.041(8) 0.032(7) 0.026(7) -0.005(6) 0.014(6) 0.000(6) C12 0.042(8) 0.036(8) 0.022(7) -0.001(6) 0.013(6) -0.003(6) C13 0.039(8) 0.038(8) 0.033(8) 0.007(7) 0.007(6) 0.007(7) C14 0.043(9) 0.038(8) 0.035(8) 0.003(7) 0.011(7) 0.001(7) C15 0.049(9) 0.036(8) 0.039(8) 0.003(7) 0.025(7) 0.005(7) C16 0.057(10) 0.035(8) 0.025(7) 0.003(6) 0.021(7) 0.011(7) C2 0.048(9) 0.048(9) 0.020(7) -0.009(6) 0.016(6) 0.011(7) C3 0.22(3) 0.068(12) 0.21(3) 0.034(14) 0.19(2) 0.030(14) C22 0.085(10) 0.059(8) 0.071(9) 0.008(7) 0.064(9) 0.015(7) C23 0.087(10) 0.049(7) 0.073(9) 0.012(7) 0.062(9) 0.017(7) C24 0.040(9) 0.062(11) 0.039(9) 0.023(8) 0.017(7) 0.006(8) C25 0.087(10) 0.049(7) 0.073(9) 0.012(7) 0.062(9) 0.017(7) C26 0.085(10) 0.059(8) 0.071(9) 0.008(7) 0.064(9) 0.015(7) C4 0.22(3) 0.068(12) 0.21(3) 0.034(14) 0.19(2) 0.030(14) N31 0.055(12) 0.040(10) 0.042(11) 0.000 0.028(9) 0.000 C32 0.064(11) 0.048(10) 0.045(10) 0.005(8) 0.035(9) -0.009(8) C33 0.059(12) 0.049(11) 0.071(13) 0.018(10) 0.016(10) -0.010(9) C34 0.09(2) 0.011(10) 0.10(2) 0.000 0.026(18) 0.000 N41 0.057(13) 0.043(11) 0.045(12) 0.000 0.001(10) 0.000 C42 0.063(11) 0.026(8) 0.057(11) 0.005(7) 0.001(9) 0.004(8) C43 0.076(14) 0.043(11) 0.075(14) -0.008(10) -0.016(11) 0.012(10) C44 0.048(16) 0.08(2) 0.08(2) 0.000 -0.014(15) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Dy1 O3 2.391(11) 2_655 ? Dy1 O3 2.391(11) . ? Dy1 O1 2.410(11) 2_655 ? Dy1 O1 2.410(11) . ? Dy1 O11 2.411(10) 3 ? Dy1 O11 2.411(10) 4 ? Dy1 N11 2.462(12) 2_655 ? Dy1 N11 2.462(12) . ? Dy1 N41 2.479(19) 3 ? Dy2 O4 2.369(11) . ? Dy2 O4 2.369(11) 2 ? Dy2 O14 2.451(14) . ? Dy2 O14 2.451(14) 2 ? Dy2 O13 2.454(12) . ? Dy2 O13 2.454(12) 2 ? Dy2 O9 2.454(12) 2 ? Dy2 O9 2.454(12) . ? Dy2 N31 2.546(18) . ? Dy3 O10 2.289(11) 5_566 ? Dy3 O12 2.339(14) . ? Dy3 O2 2.347(10) 5_666 ? Dy3 O15 2.39(2) . ? Dy3 O5 2.412(16) . ? Dy3 O16 2.42(3) . ? Dy3 O8 2.49(2) 5_566 ? Dy3 N21 2.497(15) . ? Dy3 O7 2.63(2) . ? O1 C1 1.252(17) . ? O2 C1 1.258(18) . ? O2 Dy3 2.347(10) 5_666 ? O3 C2 1.266(19) . ? O4 C2 1.244(19) . ? O5 C3 1.27(3) . ? O6 C3 1.24(3) . ? O7 C4 1.333(17) . ? O8 C4 1.375(18) . ? O8 Dy3 2.49(2) 5_566 ? O9 C5 1.26(2) . ? O10 C5 1.26(2) . ? O10 Dy3 2.289(11) 5_566 ? O11 C6 1.26(2) . ? O11 Dy1 2.411(10) 3_445 ? O12 C6 1.24(2) . ? N11 C16 1.324(19) . ? N11 C12 1.332(18) . ? N21 C26 1.30(2) . ? N21 C22 1.323(19) . ? C5 C32 1.49(2) . ? C6 C42 1.50(2) . ? C1 C12 1.520(18) . ? C12 C13 1.377(17) . ? C13 C14 1.406(18) . ? C13 H1 0.9500 . ? C14 C15 1.394(18) . ? C14 C24 1.48(2) . ? C15 C16 1.376(18) . ? C15 H2 0.9500 . ? C16 C2 1.517(18) . ? C3 C22 1.51(2) . ? C22 C23 1.373(19) . ? C23 C24 1.398(19) . ? C23 H3 0.9500 . ? C24 C25 1.390(18) . ? C25 C26 1.377(19) . ? C25 H4 0.9500 . ? C26 C4 1.53(2) . ? N31 C32 1.325(15) 2 ? N31 C32 1.325(15) . ? C32 C33 1.39(2) . ? C33 C34 1.39(2) . ? C33 H5 0.9500 . ? C34 C33 1.39(2) 2 ? C34 C44 1.46(4) . ? N41 C42 1.324(17) . ? N41 C42 1.324(16) 2 ? N41 Dy1 2.479(19) 3_445 ? C42 C43 1.38(2) . ? C43 C44 1.38(2) . ? C43 H6 0.9500 . ? C44 C43 1.38(2) 2 ? 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 O3 Dy1 O3 150.5(5) 2_655 . ? O3 Dy1 O1 129.3(3) 2_655 2_655 ? O3 Dy1 O1 72.8(4) . 2_655 ? O3 Dy1 O1 72.8(4) 2_655 . ? O3 Dy1 O1 129.3(4) . . ? O1 Dy1 O1 96.9(6) 2_655 . ? O3 Dy1 O11 87.3(4) 2_655 3 ? O3 Dy1 O11 79.9(4) . 3 ? O1 Dy1 O11 140.5(4) 2_655 3 ? O1 Dy1 O11 78.8(4) . 3 ? O3 Dy1 O11 79.9(4) 2_655 4 ? O3 Dy1 O11 87.3(4) . 4 ? O1 Dy1 O11 78.8(4) 2_655 4 ? O1 Dy1 O11 140.5(4) . 4 ? O11 Dy1 O11 128.4(5) 3 4 ? O3 Dy1 N11 65.1(4) 2_655 2_655 ? O3 Dy1 N11 135.4(4) . 2_655 ? O1 Dy1 N11 64.7(4) 2_655 2_655 ? O1 Dy1 N11 70.6(4) . 2_655 ? O11 Dy1 N11 143.4(4) 3 2_655 ? O11 Dy1 N11 72.2(4) 4 2_655 ? O3 Dy1 N11 135.4(4) 2_655 . ? O3 Dy1 N11 65.1(4) . . ? O1 Dy1 N11 70.6(4) 2_655 . ? O1 Dy1 N11 64.7(4) . . ? O11 Dy1 N11 72.2(4) 3 . ? O11 Dy1 N11 143.4(4) 4 . ? N11 Dy1 N11 110.2(6) 2_655 . ? O3 Dy1 N41 75.3(3) 2_655 3 ? O3 Dy1 N41 75.3(3) . 3 ? O1 Dy1 N41 131.5(3) 2_655 3 ? O1 Dy1 N41 131.5(3) . 3 ? O11 Dy1 N41 64.2(3) 3 3 ? O11 Dy1 N41 64.2(3) 4 3 ? N11 Dy1 N41 124.9(3) 2_655 3 ? N11 Dy1 N41 124.9(3) . 3 ? O4 Dy2 O4 136.1(6) . 2 ? O4 Dy2 O14 73.0(5) . . ? O4 Dy2 O14 140.9(5) 2 . ? O4 Dy2 O14 140.9(5) . 2 ? O4 Dy2 O14 73.0(5) 2 2 ? O14 Dy2 O14 99.5(8) . 2 ? O4 Dy2 O13 74.6(4) . . ? O4 Dy2 O13 131.3(5) 2 . ? O14 Dy2 O13 73.6(6) . . ? O14 Dy2 O13 66.6(5) 2 . ? O4 Dy2 O13 131.3(5) . 2 ? O4 Dy2 O13 74.6(4) 2 2 ? O14 Dy2 O13 66.6(5) . 2 ? O14 Dy2 O13 73.6(6) 2 2 ? O13 Dy2 O13 116.4(7) . 2 ? O4 Dy2 O9 86.2(4) . 2 ? O4 Dy2 O9 74.4(4) 2 2 ? O14 Dy2 O9 142.9(5) . 2 ? O14 Dy2 O9 77.4(5) 2 2 ? O13 Dy2 O9 71.4(5) . 2 ? O13 Dy2 O9 142.4(5) 2 2 ? O4 Dy2 O9 74.4(4) . . ? O4 Dy2 O9 86.2(4) 2 . ? O14 Dy2 O9 77.4(5) . . ? O14 Dy2 O9 142.9(5) 2 . ? O13 Dy2 O9 142.4(5) . . ? O13 Dy2 O9 71.4(5) 2 . ? O9 Dy2 O9 126.8(6) 2 . ? O4 Dy2 N31 68.1(3) . . ? O4 Dy2 N31 68.1(3) 2 . ? O14 Dy2 N31 130.2(4) . . ? O14 Dy2 N31 130.2(4) 2 . ? O13 Dy2 N31 121.8(3) . . ? O13 Dy2 N31 121.8(3) 2 . ? O9 Dy2 N31 63.4(3) 2 . ? O9 Dy2 N31 63.4(3) . . ? O10 Dy3 O12 132.5(6) 5_566 . ? O10 Dy3 O2 83.2(5) 5_566 5_666 ? O12 Dy3 O2 144.1(5) . 5_666 ? O10 Dy3 O15 71.9(6) 5_566 . ? O12 Dy3 O15 113.3(6) . . ? O2 Dy3 O15 77.4(7) 5_666 . ? O10 Dy3 O5 143.3(6) 5_566 . ? O12 Dy3 O5 72.1(7) . . ? O2 Dy3 O5 79.6(6) 5_666 . ? O15 Dy3 O5 72.7(6) . . ? O10 Dy3 O16 69.1(9) 5_566 . ? O12 Dy3 O16 64.0(8) . . ? O2 Dy3 O16 151.8(7) 5_666 . ? O15 Dy3 O16 88.6(12) . . ? O5 Dy3 O16 119.8(13) . . ? O10 Dy3 O8 80.3(6) 5_566 5_566 ? O12 Dy3 O8 74.7(7) . 5_566 ? O2 Dy3 O8 115.1(7) 5_666 5_566 ? O15 Dy3 O8 148.1(7) . 5_566 ? O5 Dy3 O8 136.4(6) . 5_566 ? O16 Dy3 O8 66.6(13) . 5_566 ? O10 Dy3 N21 141.0(5) 5_566 . ? O12 Dy3 N21 71.3(5) . . ? O2 Dy3 N21 77.0(4) 5_666 . ? O15 Dy3 N21 133.5(6) . . ? O5 Dy3 N21 64.9(5) . . ? O16 Dy3 N21 128.5(8) . . ? O8 Dy3 N21 78.3(6) 5_566 . ? O10 Dy3 O7 81.0(5) 5_566 . ? O12 Dy3 O7 109.9(5) . . ? O2 Dy3 O7 66.1(5) 5_666 . ? O15 Dy3 O7 136.7(7) . . ? O5 Dy3 O7 119.9(7) . . ? O16 Dy3 O7 112.8(13) . . ? O8 Dy3 O7 49.5(8) 5_566 . ? N21 Dy3 O7 60.4(5) . . ? C1 O1 Dy1 124.0(10) . . ? C1 O2 Dy3 133.8(9) . 5_666 ? C2 O3 Dy1 122.9(9) . . ? C2 O4 Dy2 138.7(10) . . ? C3 O5 Dy3 121.1(16) . . ? C4 O7 Dy3 106.1(10) . . ? C4 O8 Dy3 170.4(15) . 5_566 ? C5 O9 Dy2 124.0(10) . . ? C5 O10 Dy3 147.5(13) . 5_566 ? C6 O11 Dy1 123.1(10) . 3_445 ? C6 O12 Dy3 148.4(14) . . ? C16 N11 C12 119.0(12) . . ? C16 N11 Dy1 119.6(9) . . ? C12 N11 Dy1 120.5(9) . . ? C26 N21 C22 120.6(15) . . ? C26 N21 Dy3 119.7(10) . . ? C22 N21 Dy3 118.0(12) . . ? O10 C5 O9 126.7(18) . . ? O10 C5 C32 115.9(18) . . ? O9 C5 C32 117.3(15) . . ? O12 C6 O11 127.2(18) . . ? O12 C6 C42 115.4(17) . . ? O11 C6 C42 117.4(15) . . ? O1 C1 O2 125.9(13) . . ? O1 C1 C12 115.8(13) . . ? O2 C1 C12 118.3(12) . . ? N11 C12 C13 122.9(13) . . ? N11 C12 C1 112.9(12) . . ? C13 C12 C1 124.2(13) . . ? C12 C13 C14 118.4(13) . . ? C12 C13 H1 120.8 . . ? C14 C13 H1 120.8 . . ? C15 C14 C13 117.8(13) . . ? C15 C14 C24 122.4(12) . . ? C13 C14 C24 119.8(11) . . ? C16 C15 C14 119.2(13) . . ? C16 C15 H2 120.4 . . ? C14 C15 H2 120.4 . . ? N11 C16 C15 122.6(13) . . ? N11 C16 C2 113.7(12) . . ? C15 C16 C2 123.7(13) . . ? O4 C2 O3 125.4(14) . . ? O4 C2 C16 118.3(14) . . ? O3 C2 C16 116.3(13) . . ? O6 C3 O5 124(2) . . ? O6 C3 C22 119.7(19) . . ? O5 C3 C22 116.6(18) . . ? N21 C22 C23 121.6(15) . . ? N21 C22 C3 114.6(15) . . ? C23 C22 C3 123.8(15) . . ? C22 C23 C24 119.7(14) . . ? C22 C23 H3 120.2 . . ? C24 C23 H3 120.2 . . ? C25 C24 C23 116.1(13) . . ? C25 C24 C14 123.0(13) . . ? C23 C24 C14 120.8(12) . . ? C26 C25 C24 120.5(15) . . ? C26 C25 H4 119.7 . . ? C24 C25 H4 119.7 . . ? N21 C26 C25 121.2(14) . . ? N21 C26 C4 114.4(14) . . ? C25 C26 C4 123.8(14) . . ? O7 C4 O8 131.3(18) . . ? O7 C4 C26 104.9(16) . . ? O8 C4 C26 123.8(17) . . ? C32 N31 C32 120.3(19) 2 . ? C32 N31 Dy2 119.9(10) 2 . ? C32 N31 Dy2 119.9(10) . . ? N31 C32 C33 122.0(16) . . ? N31 C32 C5 114.8(14) . . ? C33 C32 C5 123.2(15) . . ? C32 C33 C34 118.3(16) . . ? C32 C33 H5 120.9 . . ? C34 C33 H5 120.9 . . ? C33 C34 C33 119(2) 2 . ? C33 C34 C44 120.4(10) 2 . ? C33 C34 C44 120.4(10) . . ? C42 N41 C42 117.5(19) . 2 ? C42 N41 Dy1 121.3(10) . 3_445 ? C42 N41 Dy1 121.3(10) 2 3_445 ? N41 C42 C43 123.2(16) . . ? N41 C42 C6 112.8(13) . . ? C43 C42 C6 123.9(16) . . ? C42 C43 C44 119.7(19) . . ? C42 C43 H6 120.2 . . ? C44 C43 H6 120.2 . . ? C43 C44 C43 117(2) . 2 ? C43 C44 C34 121.6(12) . . ? C43 C44 C34 121.6(12) 2 . ? 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 O3 Dy1 O1 C1 161.5(12) 2_655 . . . ? O3 Dy1 O1 C1 3.9(14) . . . . ? O1 Dy1 O1 C1 -69.4(11) 2_655 . . . ? O11 Dy1 O1 C1 70.8(12) 3 . . . ? O11 Dy1 O1 C1 -150.1(10) 4 . . . ? N11 Dy1 O1 C1 -129.5(12) 2_655 . . . ? N11 Dy1 O1 C1 -4.7(11) . . . . ? N41 Dy1 O1 C1 110.6(11) 3 . . . ? O3 Dy1 O3 C2 -154.6(11) 2_655 . . . ? O1 Dy1 O3 C2 62.3(11) 2_655 . . . ? O1 Dy1 O3 C2 -22.5(13) . . . . ? O11 Dy1 O3 C2 -88.8(11) 3 . . . ? O11 Dy1 O3 C2 141.3(11) 4 . . . ? N11 Dy1 O3 C2 80.2(12) 2_655 . . . ? N11 Dy1 O3 C2 -13.9(11) . . . . ? N41 Dy1 O3 C2 -154.6(11) 3 . . . ? O4 Dy2 O4 C2 105.5(17) 2 . . . ? O14 Dy2 O4 C2 -106.1(17) . . . . ? O14 Dy2 O4 C2 -22(2) 2 . . . ? O13 Dy2 O4 C2 -29.0(16) . . . . ? O13 Dy2 O4 C2 -140.8(16) 2 . . . ? O9 Dy2 O4 C2 42.7(16) 2 . . . ? O9 Dy2 O4 C2 172.6(17) . . . . ? N31 Dy2 O4 C2 105.5(17) . . . . ? O10 Dy3 O5 C3 -164(3) 5_566 . . . ? O12 Dy3 O5 C3 57(3) . . . . ? O2 Dy3 O5 C3 -100(3) 5_666 . . . ? O15 Dy3 O5 C3 180(3) . . . . ? O16 Dy3 O5 C3 102(3) . . . . ? O8 Dy3 O5 C3 15(4) 5_566 . . . ? N21 Dy3 O5 C3 -20(3) . . . . ? O7 Dy3 O5 C3 -46(3) . . . . ? O10 Dy3 O7 C4 -138.4(14) 5_566 . . . ? O12 Dy3 O7 C4 -6.3(15) . . . . ? O2 Dy3 O7 C4 135.1(14) 5_666 . . . ? O15 Dy3 O7 C4 170.4(13) . . . . ? O5 Dy3 O7 C4 74.0(15) . . . . ? O16 Dy3 O7 C4 -75.7(15) . . . . ? O8 Dy3 O7 C4 -53.5(13) 5_566 . . . ? N21 Dy3 O7 C4 46.9(12) . . . . ? O4 Dy2 O9 C5 -65.7(15) . . . . ? O4 Dy2 O9 C5 74.5(15) 2 . . . ? O14 Dy2 O9 C5 -141.3(16) . . . . ? O14 Dy2 O9 C5 129.5(15) 2 . . . ? O13 Dy2 O9 C5 -101.2(16) . . . . ? O13 Dy2 O9 C5 149.5(16) 2 . . . ? O9 Dy2 O9 C5 7.2(14) 2 . . . ? N31 Dy2 O9 C5 7.2(14) . . . . ? O10 Dy3 O12 C6 -78(3) 5_566 . . . ? O2 Dy3 O12 C6 110(3) 5_666 . . . ? O15 Dy3 O12 C6 9(3) . . . . ? O5 Dy3 O12 C6 70(3) . . . . ? O16 Dy3 O12 C6 -68(3) . . . . ? O8 Dy3 O12 C6 -139(3) 5_566 . . . ? N21 Dy3 O12 C6 139(3) . . . . ? O7 Dy3 O12 C6 -174(3) . . . . ? O3 Dy1 N11 C16 166.6(10) 2_655 . . . ? O3 Dy1 N11 C16 12.9(10) . . . . ? O1 Dy1 N11 C16 -66.6(11) 2_655 . . . ? O1 Dy1 N11 C16 -174.4(12) . . . . ? O11 Dy1 N11 C16 99.8(11) 3 . . . ? O11 Dy1 N11 C16 -31.7(14) 4 . . . ? N11 Dy1 N11 C16 -118.8(12) 2_655 . . . ? N41 Dy1 N11 C16 61.2(12) 3 . . . ? O3 Dy1 N11 C12 -24.7(13) 2_655 . . . ? O3 Dy1 N11 C12 -178.4(12) . . . . ? O1 Dy1 N11 C12 102.1(11) 2_655 . . . ? O1 Dy1 N11 C12 -5.7(10) . . . . ? O11 Dy1 N11 C12 -91.5(11) 3 . . . ? O11 Dy1 N11 C12 137.0(10) 4 . . . ? N11 Dy1 N11 C12 49.9(10) 2_655 . . . ? N41 Dy1 N11 C12 -130.1(10) 3 . . . ? O10 Dy3 N21 C26 -31.8(19) 5_566 . . . ? O12 Dy3 N21 C26 103.8(16) . . . . ? O2 Dy3 N21 C26 -93.3(16) 5_666 . . . ? O15 Dy3 N21 C26 -151.5(16) . . . . ? O5 Dy3 N21 C26 -177.7(18) . . . . ? O16 Dy3 N21 C26 73(2) . . . . ? O8 Dy3 N21 C26 26.2(16) 5_566 . . . ? O7 Dy3 N21 C26 -23.6(16) . . . . ? O10 Dy3 N21 C22 162.5(14) 5_566 . . . ? O12 Dy3 N21 C22 -61.9(15) . . . . ? O2 Dy3 N21 C22 101.1(15) 5_666 . . . ? O15 Dy3 N21 C22 42.9(18) . . . . ? O5 Dy3 N21 C22 16.6(16) . . . . ? O16 Dy3 N21 C22 -93(2) . . . . ? O8 Dy3 N21 C22 -139.5(17) 5_566 . . . ? O7 Dy3 N21 C22 170.8(17) . . . . ? Dy3 O10 C5 O9 65(4) 5_566 . . . ? Dy3 O10 C5 C32 -118(2) 5_566 . . . ? Dy2 O9 C5 O10 167.0(14) . . . . ? Dy2 O9 C5 C32 -10(2) . . . . ? Dy3 O12 C6 O11 -4(5) . . . . ? Dy3 O12 C6 C42 176.0(19) . . . . ? Dy1 O11 C6 O12 167.7(17) 3_445 . . . ? Dy1 O11 C6 C42 -13(3) 3_445 . . . ? Dy1 O1 C1 O2 -168.7(11) . . . . ? Dy1 O1 C1 C12 13.0(17) . . . . ? Dy3 O2 C1 O1 86.4(18) 5_666 . . . ? Dy3 O2 C1 C12 -95.4(15) 5_666 . . . ? C16 N11 C12 C13 2(2) . . . . ? Dy1 N11 C12 C13 -166.8(11) . . . . ? C16 N11 C12 C1 -177.9(13) . . . . ? Dy1 N11 C12 C1 13.3(16) . . . . ? O1 C1 C12 N11 -16.8(18) . . . . ? O2 C1 C12 N11 164.8(13) . . . . ? O1 C1 C12 C13 163.3(14) . . . . ? O2 C1 C12 C13 -15(2) . . . . ? N11 C12 C13 C14 1(2) . . . . ? C1 C12 C13 C14 -179.5(13) . . . . ? C12 C13 C14 C15 -3(2) . . . . ? C12 C13 C14 C24 175.3(14) . . . . ? C13 C14 C15 C16 4(2) . . . . ? C24 C14 C15 C16 -175.1(15) . . . . ? C12 N11 C16 C15 -2(2) . . . . ? Dy1 N11 C16 C15 167.1(12) . . . . ? C12 N11 C16 C2 179.6(12) . . . . ? Dy1 N11 C16 C2 -11.6(17) . . . . ? C14 C15 C16 N11 -1(2) . . . . ? C14 C15 C16 C2 177.4(14) . . . . ? Dy2 O4 C2 O3 29(3) . . . . ? Dy2 O4 C2 C16 -150.1(12) . . . . ? Dy1 O3 C2 O4 -166.0(12) . . . . ? Dy1 O3 C2 C16 13.4(17) . . . . ? N11 C16 C2 O4 178.8(14) . . . . ? C15 C16 C2 O4 0(2) . . . . ? N11 C16 C2 O3 -0.6(19) . . . . ? C15 C16 C2 O3 -179.3(14) . . . . ? Dy3 O5 C3 O6 -161(4) . . . . ? Dy3 O5 C3 C22 21(5) . . . . ? C26 N21 C22 C23 3(4) . . . . ? Dy3 N21 C22 C23 168.3(18) . . . . ? C26 N21 C22 C3 -179(3) . . . . ? Dy3 N21 C22 C3 -13(3) . . . . ? O6 C3 C22 N21 177(4) . . . . ? O5 C3 C22 N21 -4(5) . . . . ? O6 C3 C22 C23 -4(6) . . . . ? O5 C3 C22 C23 174(3) . . . . ? N21 C22 C23 C24 0(4) . . . . ? C3 C22 C23 C24 -179(3) . . . . ? C22 C23 C24 C25 1(3) . . . . ? C22 C23 C24 C14 -176(2) . . . . ? C15 C14 C24 C25 -35(3) . . . . ? C13 C14 C24 C25 146.2(19) . . . . ? C15 C14 C24 C23 141.2(19) . . . . ? C13 C14 C24 C23 -37(3) . . . . ? C23 C24 C25 C26 -3(3) . . . . ? C14 C24 C25 C26 173(2) . . . . ? C22 N21 C26 C25 -5(3) . . . . ? Dy3 N21 C26 C25 -170.7(17) . . . . ? C22 N21 C26 C4 165.9(19) . . . . ? Dy3 N21 C26 C4 1(2) . . . . ? C24 C25 C26 N21 6(4) . . . . ? C24 C25 C26 C4 -164.7(18) . . . . ? Dy3 O7 C4 O8 117.7(12) . . . . ? Dy3 O7 C4 C26 -62.5(11) . . . . ? Dy3 O8 C4 O7 73(8) 5_566 . . . ? Dy3 O8 C4 C26 -107(8) 5_566 . . . ? N21 C26 C4 O7 44.0(19) . . . . ? C25 C26 C4 O7 -145(2) . . . . ? N21 C26 C4 O8 -136.1(19) . . . . ? C25 C26 C4 O8 35(2) . . . . ? O4 Dy2 N31 C32 -100.5(10) . . . 2 ? O4 Dy2 N31 C32 79.5(10) 2 . . 2 ? O14 Dy2 N31 C32 -141.5(11) . . . 2 ? O14 Dy2 N31 C32 38.5(11) 2 . . 2 ? O13 Dy2 N31 C32 -46.5(11) . . . 2 ? O13 Dy2 N31 C32 133.5(11) 2 . . 2 ? O9 Dy2 N31 C32 -3.5(10) 2 . . 2 ? O9 Dy2 N31 C32 176.5(10) . . . 2 ? O4 Dy2 N31 C32 79.5(10) . . . . ? O4 Dy2 N31 C32 -100.5(10) 2 . . . ? O14 Dy2 N31 C32 38.5(11) . . . . ? O14 Dy2 N31 C32 -141.5(11) 2 . . . ? O13 Dy2 N31 C32 133.5(11) . . . . ? O13 Dy2 N31 C32 -46.5(11) 2 . . . ? O9 Dy2 N31 C32 176.5(10) 2 . . . ? O9 Dy2 N31 C32 -3.5(10) . . . . ? C32 N31 C32 C33 -0.6(14) 2 . . . ? Dy2 N31 C32 C33 179.4(14) . . . . ? C32 N31 C32 C5 -179.5(19) 2 . . . ? Dy2 N31 C32 C5 0.5(19) . . . . ? O10 C5 C32 N31 -171.5(15) . . . . ? O9 C5 C32 N31 6(2) . . . . ? O10 C5 C32 C33 10(3) . . . . ? O9 C5 C32 C33 -173.2(19) . . . . ? N31 C32 C33 C34 1(3) . . . . ? C5 C32 C33 C34 179.9(15) . . . . ? C32 C33 C34 C33 -0.5(13) . . . 2 ? C32 C33 C34 C44 179.5(13) . . . . ? C42 N41 C42 C43 -0.2(16) 2 . . . ? Dy1 N41 C42 C43 179.8(16) 3_445 . . . ? C42 N41 C42 C6 -177(2) 2 . . . ? Dy1 N41 C42 C6 3(2) 3_445 . . . ? O12 C6 C42 N41 -174.4(17) . . . . ? O11 C6 C42 N41 6(3) . . . . ? O12 C6 C42 C43 9(3) . . . . ? O11 C6 C42 C43 -171(2) . . . . ? N41 C42 C43 C44 0(3) . . . . ? C6 C42 C43 C44 176.9(17) . . . . ? C42 C43 C44 C43 -0.1(15) . . . 2 ? C42 C43 C44 C34 179.9(15) . . . . ? C33 C34 C44 C43 151.6(15) 2 . . . ? C33 C34 C44 C43 -28.4(15) . . . . ? C33 C34 C44 C43 -28.4(15) 2 . . 2 ? C33 C34 C44 C43 151.6(15) . . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.141 _refine_diff_density_min -7.031 _refine_diff_density_rms 0.298 #====END data_6-sq _database_code_depnum_ccdc_archive 'CCDC 713723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ho4(BPTCA)3(OH2)8] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 Ho4 N6 O32 ' _chemical_formula_sum 'C42 H28 Ho4 N6 O32' _chemical_formula_weight 1788.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ho Ho -0.2175 4.6783 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 12.126(2) _cell_length_b 22.270(5) _cell_length_c 21.568(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.283(10) _cell_angle_gamma 90.00 _cell_volume 5618(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 12352 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 5.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21062 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4942 _reflns_number_gt 3838 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. At first, the unit cell was found as F-centered orthorhombic symmetry but the intensity of the reflections showed C-centered monoclinic space group. The pseudo-symmetry resulted unusual thermal factors which were constrained by EADP instruction in SHELXL. The structure has a solvent-accessible large void space. Some intense peaks remained, which were to close to the framework to locate a reasonable molecule. The disordered solvent region was treated with SQUEEZE subroutine in PLATON software suite: Spek, A. L. J. Appl. Cryst. 2003. 36. 7-13. The sum total of 318 electrons were accounted for in the void space of 978.4 A^3^ ; _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^)+(0.0868P)^2^+843.9507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4942 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.1114 _refine_ls_wR_factor_ref 0.2720 _refine_ls_wR_factor_gt 0.2562 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.0000 0.21487(6) 0.2500 0.0388(4) Uani 1 2 d S . . Ho2 Ho 0.5000 0.25307(6) 0.2500 0.0358(4) Uani 1 2 d S . . Ho3 Ho 0.13960(10) 0.63041(9) 0.52566(6) 0.0785(6) Uani 1 1 d U . . O1 O 0.6440(13) 0.3248(8) 0.3020(7) 0.046(4) Uani 1 1 d . . . O2 O 0.7154(12) 0.3885(6) 0.3819(6) 0.035(3) Uani 1 1 d . . . O3 O 0.326(2) 0.2257(9) 0.2743(11) 0.077(4) Uani 1 1 d . . . O4 O 0.176(3) 0.2548(14) 0.3100(12) 0.122(8) Uani 1 1 d . . . O5 O 0.3012(14) 0.6573(8) 0.4893(8) 0.050(4) Uani 1 1 d . . . O6 O 0.408(3) 0.6393(10) 0.4230(15) 0.145(15) Uani 1 1 d . . . O7 O 0.0565(19) 0.5453(9) 0.5336(10) 0.077(4) Uani 1 1 d D . . O8 O 0.160(3) 0.4533(12) 0.5815(11) 0.122(8) Uani 1 1 d D . . O9 O -0.0423(17) 0.2634(9) 0.3426(8) 0.060(5) Uani 1 1 d . . . O10 O -0.0358(16) 0.3453(11) 0.4041(8) 0.075(6) Uani 1 1 d . . . O11 O 0.0749(15) 0.7070(7) 0.3525(7) 0.055(5) Uani 1 1 d . . . O12 O 0.0871(19) 0.6252(9) 0.4148(10) 0.081(7) Uani 1 1 d . . . O13 O 0.1473(17) 0.1565(9) 0.2173(11) 0.081(7) Uani 1 1 d . . . O14 O 0.0781(18) 0.1443(9) 0.3367(11) 0.078(6) Uani 1 1 d . . . O15 O 0.190(3) 0.7269(12) 0.5622(16) 0.146(13) Uani 1 1 d U . . O16 O -0.057(5) 0.662(3) 0.470(2) 0.24(2) Uani 1 1 d U . . N11 N 0.4492(15) 0.3164(7) 0.3307(7) 0.033(4) Uani 1 1 d . . . N21 N 0.2446(16) 0.5446(10) 0.4938(8) 0.045(5) Uani 1 1 d . . . C5 C -0.036(2) 0.3187(14) 0.3523(12) 0.057(7) Uani 1 1 d . . . C6 C 0.069(2) 0.6523(12) 0.3614(12) 0.058(7) Uani 1 1 d . . . C1 C 0.6368(16) 0.3585(9) 0.3478(9) 0.031(4) Uani 1 1 d D . . C12 C 0.5179(16) 0.3605(8) 0.3599(9) 0.033(5) Uani 1 1 d D . . C13 C 0.4840(16) 0.4044(8) 0.3948(9) 0.035(5) Uani 1 1 d D . . H1 H 0.5361 0.4350 0.4144 0.035 Uiso 1 1 calc R . . C14 C 0.3728(16) 0.4044(9) 0.4016(9) 0.036(5) Uani 1 1 d D . . C15 C 0.3036(18) 0.3551(8) 0.3747(10) 0.038(5) Uani 1 1 d D . . H2 H 0.2289 0.3511 0.3804 0.038 Uiso 1 1 calc R . . C16 C 0.3450(18) 0.3129(8) 0.3403(9) 0.036(5) Uani 1 1 d D . . C2 C 0.2790(19) 0.2588(9) 0.3044(10) 0.040(5) Uani 1 1 d DU . . C3 C 0.348(3) 0.6233(12) 0.457(2) 0.103(9) Uani 1 1 d DU . . C22 C 0.317(2) 0.5567(11) 0.4586(14) 0.067(6) Uani 1 1 d D . . C23 C 0.362(2) 0.5118(9) 0.4297(14) 0.061(5) Uani 1 1 d D . . H3 H 0.4147 0.5211 0.4052 0.061 Uiso 1 1 calc R . . C24 C 0.3313(18) 0.4521(10) 0.4360(10) 0.047(6) Uani 1 1 d D . . C25 C 0.253(2) 0.4426(10) 0.4734(13) 0.061(5) Uani 1 1 d D . . H4 H 0.2308 0.4030 0.4810 0.061 Uiso 1 1 calc R . . C26 C 0.210(2) 0.4907(12) 0.4985(14) 0.067(6) Uani 1 1 d D . . C4 C 0.1296(17) 0.5000(9) 0.5418(11) 0.103(9) Uani 1 1 d D . . N31 N 0.0000 0.3274(11) 0.2500 0.044(6) Uani 1 2 d SD . . C32 C -0.016(2) 0.3579(9) 0.2993(10) 0.046(6) Uani 1 1 d D . . C33 C -0.019(2) 0.4189(10) 0.3000(14) 0.068(8) Uani 1 1 d D . . H5 H -0.0339 0.4392 0.3356 0.068 Uiso 1 1 calc R . . C34 C 0.0000 0.4512(12) 0.2500 0.061(11) Uani 1 2 d SD . . N41 N 0.0000 0.6424(10) 0.2500 0.052(8) Uani 1 2 d SD . . C42 C 0.030(2) 0.6114(9) 0.3039(11) 0.057(7) Uani 1 1 d D . . C43 C 0.030(3) 0.5506(10) 0.3059(13) 0.075(10) Uani 1 1 d D . . H6 H 0.0515 0.5303 0.3461 0.075 Uiso 1 1 calc R . . C44 C 0.0000 0.5188(13) 0.2500 0.074(14) Uani 1 2 d SD . . 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 Ho1 0.0512(9) 0.0336(8) 0.0416(8) 0.000 0.0298(7) 0.000 Ho2 0.0463(8) 0.0387(8) 0.0205(6) 0.000 0.0051(6) 0.000 Ho3 0.0316(6) 0.1682(17) 0.0373(7) -0.0471(8) 0.0116(5) 0.0093(8) O1 0.050(9) 0.063(10) 0.031(8) -0.006(7) 0.020(7) -0.001(8) O2 0.043(8) 0.035(8) 0.027(7) 0.006(6) 0.008(6) 0.006(7) O3 0.104(12) 0.062(9) 0.087(11) 0.001(8) 0.066(10) 0.007(8) O4 0.17(2) 0.140(17) 0.074(12) -0.046(12) 0.059(13) -0.050(16) O5 0.054(10) 0.057(10) 0.051(10) 0.010(8) 0.037(8) 0.026(8) O6 0.29(4) 0.053(13) 0.17(3) 0.022(15) 0.21(3) 0.013(18) O7 0.104(12) 0.062(9) 0.087(11) 0.001(8) 0.066(10) 0.007(8) O8 0.17(2) 0.140(17) 0.074(12) -0.046(12) 0.059(13) -0.050(16) O9 0.080(13) 0.068(12) 0.049(10) 0.003(9) 0.050(10) 0.004(10) O10 0.062(11) 0.133(19) 0.040(10) -0.026(11) 0.034(9) 0.013(12) O11 0.073(12) 0.043(9) 0.033(8) 0.016(7) -0.013(8) -0.016(8) O12 0.095(16) 0.067(13) 0.060(12) 0.021(11) -0.014(11) -0.024(12) O13 0.063(12) 0.069(13) 0.110(17) -0.044(13) 0.020(12) 0.011(10) O14 0.074(14) 0.062(12) 0.097(16) 0.017(11) 0.022(12) -0.002(11) O15 0.25(3) 0.090(17) 0.17(2) 0.048(17) 0.17(2) 0.081(19) O16 0.25(4) 0.26(4) 0.19(3) -0.03(3) 0.04(3) 0.11(3) N11 0.043(10) 0.034(9) 0.015(7) -0.004(7) -0.001(7) -0.012(8) N21 0.046(11) 0.066(13) 0.031(9) -0.018(9) 0.025(8) -0.013(10) C5 0.057(16) 0.08(2) 0.048(15) 0.017(14) 0.032(13) 0.012(14) C6 0.051(15) 0.060(17) 0.045(14) 0.010(13) -0.019(12) -0.009(13) C1 0.037(11) 0.040(11) 0.019(9) 0.004(8) 0.014(8) 0.004(9) C12 0.040(11) 0.033(11) 0.027(10) 0.007(8) 0.008(9) 0.016(9) C13 0.037(11) 0.030(10) 0.035(11) 0.002(9) 0.006(9) -0.002(9) C14 0.041(12) 0.038(11) 0.026(10) -0.008(9) 0.004(9) -0.001(10) C15 0.052(13) 0.034(11) 0.033(11) -0.003(9) 0.018(10) -0.002(10) C16 0.056(14) 0.032(11) 0.022(10) -0.005(8) 0.014(9) -0.010(10) C2 0.046(9) 0.044(9) 0.033(8) 0.019(7) 0.014(7) -0.007(7) C3 0.112(16) 0.091(14) 0.131(16) 0.048(13) 0.076(14) 0.008(12) C22 0.077(13) 0.079(14) 0.063(12) -0.001(11) 0.052(11) -0.010(12) C23 0.085(14) 0.046(10) 0.076(13) 0.005(9) 0.063(12) -0.008(10) C24 0.035(11) 0.075(17) 0.032(11) -0.015(11) 0.012(9) -0.009(12) C25 0.085(14) 0.046(10) 0.076(13) 0.005(9) 0.063(12) -0.008(10) C26 0.077(13) 0.079(14) 0.063(12) -0.001(11) 0.052(11) -0.010(12) C4 0.112(16) 0.091(14) 0.131(16) 0.048(13) 0.076(14) 0.008(12) N31 0.051(16) 0.048(16) 0.042(15) 0.000 0.029(13) 0.000 C32 0.061(15) 0.044(13) 0.043(13) -0.003(10) 0.032(12) 0.005(11) C33 0.064(18) 0.048(16) 0.09(2) -0.019(15) 0.022(16) 0.013(14) C34 0.07(2) 0.013(15) 0.11(3) 0.000 0.03(2) 0.000 N41 0.07(2) 0.019(12) 0.057(18) 0.000 -0.003(15) 0.000 C42 0.070(17) 0.030(12) 0.057(15) 0.002(11) -0.010(13) -0.002(12) C43 0.08(2) 0.039(14) 0.08(2) 0.012(14) -0.031(16) -0.008(14) C44 0.08(3) 0.024(17) 0.09(3) 0.000 -0.02(2) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ho1 O4 2.36(3) . ? Ho1 O4 2.36(3) 2 ? Ho1 O14 2.44(2) 2 ? Ho1 O14 2.44(2) . ? Ho1 O9 2.441(16) 2 ? Ho1 O9 2.441(16) . ? Ho1 O13 2.458(18) . ? Ho1 O13 2.458(18) 2 ? Ho1 N31 2.51(2) . ? Ho2 O3 2.38(2) . ? Ho2 O3 2.38(2) 2_655 ? Ho2 O11 2.388(14) 4_545 ? Ho2 O11 2.388(14) 3_545 ? Ho2 O1 2.414(16) 2_655 ? Ho2 O1 2.414(16) . ? Ho2 N11 2.443(16) 2_655 ? Ho2 N11 2.443(16) . ? Ho2 N41 2.47(2) 3_545 ? Ho3 O7 2.17(2) . ? Ho3 O10 2.275(15) 5_566 ? Ho3 O12 2.31(2) . ? Ho3 O15 2.32(3) . ? Ho3 O2 2.322(14) 5_666 ? Ho3 O5 2.371(15) . ? Ho3 O16 2.47(5) . ? Ho3 N21 2.49(2) . ? Ho3 C4 2.93(2) . ? O1 C1 1.26(2) . ? O2 C1 1.24(2) . ? O2 Ho3 2.322(14) 5_666 ? O3 C2 1.22(3) . ? O4 C2 1.28(4) . ? O5 C3 1.26(4) . ? O6 C3 1.21(4) . ? O7 C4 1.324(18) . ? O8 C4 1.335(19) . ? O9 C5 1.25(3) . ? O10 C5 1.26(3) . ? O10 Ho3 2.275(15) 5_566 ? O11 C6 1.24(3) . ? O11 Ho2 2.388(14) 3_455 ? O12 C6 1.27(3) . ? N11 C12 1.33(2) . ? N11 C16 1.33(3) . ? N21 C26 1.28(3) . ? N21 C22 1.34(3) . ? C5 C32 1.51(3) . ? C6 C42 1.51(3) . ? C1 C12 1.53(2) . ? C12 C13 1.36(2) . ? C13 C14 1.40(2) . ? C13 H1 0.9500 . ? C14 C15 1.41(2) . ? C14 C24 1.46(3) . ? C15 C16 1.37(2) . ? C15 H2 0.9500 . ? C16 C2 1.54(2) . ? C3 C22 1.53(3) . ? C22 C23 1.36(3) . ? C23 C24 1.40(2) . ? C23 H3 0.9500 . ? C24 C25 1.41(2) . ? C25 C26 1.36(3) . ? C25 H4 0.9500 . ? C26 C4 1.53(3) . ? N31 C32 1.32(2) 2 ? N31 C32 1.32(2) . ? C32 C33 1.36(3) . ? C33 C34 1.36(3) . ? C33 H5 0.9500 . ? C34 C33 1.36(3) 2 ? C34 C44 1.51(4) . ? N41 C42 1.32(2) 2 ? N41 C42 1.32(2) . ? N41 Ho2 2.47(2) 3_455 ? C42 C43 1.36(3) . ? C43 C44 1.36(3) . ? C43 H6 0.9500 . ? C44 C43 1.36(3) 2 ? 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 O4 Ho1 O4 135.8(17) . 2 ? O4 Ho1 O14 140.9(9) . 2 ? O4 Ho1 O14 73.1(9) 2 2 ? O4 Ho1 O14 73.1(9) . . ? O4 Ho1 O14 140.9(9) 2 . ? O14 Ho1 O14 99.6(11) 2 . ? O4 Ho1 O9 85.8(8) . 2 ? O4 Ho1 O9 74.9(8) 2 2 ? O14 Ho1 O9 77.3(7) 2 2 ? O14 Ho1 O9 142.3(7) . 2 ? O4 Ho1 O9 74.9(8) . . ? O4 Ho1 O9 85.8(8) 2 . ? O14 Ho1 O9 142.3(7) 2 . ? O14 Ho1 O9 77.3(7) . . ? O9 Ho1 O9 127.4(9) 2 . ? O4 Ho1 O13 74.6(9) . . ? O4 Ho1 O13 131.6(8) 2 . ? O14 Ho1 O13 66.6(7) 2 . ? O14 Ho1 O13 73.4(8) . . ? O9 Ho1 O13 71.0(7) 2 . ? O9 Ho1 O13 142.6(7) . . ? O4 Ho1 O13 131.6(8) . 2 ? O4 Ho1 O13 74.6(9) 2 2 ? O14 Ho1 O13 73.4(8) 2 2 ? O14 Ho1 O13 66.6(7) . 2 ? O9 Ho1 O13 142.6(7) 2 2 ? O9 Ho1 O13 71.0(8) . 2 ? O13 Ho1 O13 116.2(11) . 2 ? O4 Ho1 N31 67.9(8) . . ? O4 Ho1 N31 67.9(8) 2 . ? O14 Ho1 N31 130.2(5) 2 . ? O14 Ho1 N31 130.2(5) . . ? O9 Ho1 N31 63.7(4) 2 . ? O9 Ho1 N31 63.7(4) . . ? O13 Ho1 N31 121.9(5) . . ? O13 Ho1 N31 121.9(5) 2 . ? O3 Ho2 O3 150.4(10) . 2_655 ? O3 Ho2 O11 87.2(7) . 4_545 ? O3 Ho2 O11 80.2(7) 2_655 4_545 ? O3 Ho2 O11 80.2(7) . 3_545 ? O3 Ho2 O11 87.2(7) 2_655 3_545 ? O11 Ho2 O11 129.1(8) 4_545 3_545 ? O3 Ho2 O1 72.4(6) . 2_655 ? O3 Ho2 O1 129.8(6) 2_655 2_655 ? O11 Ho2 O1 78.6(5) 4_545 2_655 ? O11 Ho2 O1 140.0(6) 3_545 2_655 ? O3 Ho2 O1 129.8(6) . . ? O3 Ho2 O1 72.4(6) 2_655 . ? O11 Ho2 O1 140.0(6) 4_545 . ? O11 Ho2 O1 78.6(5) 3_545 . ? O1 Ho2 O1 97.1(8) 2_655 . ? O3 Ho2 N11 135.1(7) . 2_655 ? O3 Ho2 N11 65.6(6) 2_655 2_655 ? O11 Ho2 N11 72.2(6) 4_545 2_655 ? O11 Ho2 N11 143.3(6) 3_545 2_655 ? O1 Ho2 N11 64.8(5) 2_655 2_655 ? O1 Ho2 N11 70.2(5) . 2_655 ? O3 Ho2 N11 65.6(6) . . ? O3 Ho2 N11 135.1(7) 2_655 . ? O11 Ho2 N11 143.3(6) 4_545 . ? O11 Ho2 N11 72.2(6) 3_545 . ? O1 Ho2 N11 70.2(5) 2_655 . ? O1 Ho2 N11 64.8(5) . . ? N11 Ho2 N11 109.4(8) 2_655 . ? O3 Ho2 N41 75.2(5) . 3_545 ? O3 Ho2 N41 75.2(5) 2_655 3_545 ? O11 Ho2 N41 64.6(4) 4_545 3_545 ? O11 Ho2 N41 64.6(4) 3_545 3_545 ? O1 Ho2 N41 131.4(4) 2_655 3_545 ? O1 Ho2 N41 131.4(4) . 3_545 ? N11 Ho2 N41 125.3(4) 2_655 3_545 ? N11 Ho2 N41 125.3(4) . 3_545 ? O7 Ho3 O10 78.8(8) . 5_566 ? O7 Ho3 O12 91.7(8) . . ? O10 Ho3 O12 130.7(8) 5_566 . ? O7 Ho3 O15 150.3(7) . . ? O10 Ho3 O15 72.2(8) 5_566 . ? O12 Ho3 O15 112.0(9) . . ? O7 Ho3 O2 92.1(7) . 5_666 ? O10 Ho3 O2 84.2(6) 5_566 5_666 ? O12 Ho3 O2 145.0(7) . 5_666 ? O15 Ho3 O2 78.7(10) . 5_666 ? O7 Ho3 O5 133.3(6) . . ? O10 Ho3 O5 144.2(7) 5_566 . ? O12 Ho3 O5 72.3(7) . . ? O15 Ho3 O5 73.3(7) . . ? O2 Ho3 O5 79.9(5) 5_666 . ? O7 Ho3 O16 82.9(16) . . ? O10 Ho3 O16 67.8(12) 5_566 . ? O12 Ho3 O16 62.9(13) . . ? O15 Ho3 O16 92.1(16) . . ? O2 Ho3 O16 152.0(12) 5_666 . ? O5 Ho3 O16 123.0(15) . . ? O7 Ho3 N21 68.5(7) . . ? O10 Ho3 N21 141.2(8) 5_566 . ? O12 Ho3 N21 72.3(7) . . ? O15 Ho3 N21 134.3(9) . . ? O2 Ho3 N21 76.8(6) 5_666 . ? O5 Ho3 N21 64.9(6) . . ? O16 Ho3 N21 125.5(12) . . ? O7 Ho3 C4 24.8(5) . . ? O10 Ho3 C4 96.3(8) 5_566 . ? O12 Ho3 C4 93.7(7) . . ? O15 Ho3 C4 153.5(9) . . ? O2 Ho3 C4 76.3(5) 5_666 . ? O5 Ho3 C4 110.7(6) . . ? O16 Ho3 C4 105.8(15) . . ? N21 Ho3 C4 46.6(6) . . ? C1 O1 Ho2 124.5(13) . . ? C1 O2 Ho3 134.8(13) . 5_666 ? C2 O3 Ho2 121.9(17) . . ? C2 O4 Ho1 137.3(18) . . ? C3 O5 Ho3 124.3(18) . . ? C4 O7 Ho3 111.5(13) . . ? C5 O9 Ho1 124.1(15) . . ? C5 O10 Ho3 145.7(19) . 5_566 ? C6 O11 Ho2 122.9(15) . 3_455 ? C6 O12 Ho3 148.3(19) . . ? C12 N11 C16 118.0(16) . . ? C12 N11 Ho2 121.2(13) . . ? C16 N11 Ho2 120.1(11) . . ? C26 N21 C22 121(2) . . ? C26 N21 Ho3 119.7(14) . . ? C22 N21 Ho3 117.7(16) . . ? O9 C5 O10 127(2) . . ? O9 C5 C32 117(2) . . ? O10 C5 C32 116(3) . . ? O11 C6 O12 127(3) . . ? O11 C6 C42 119(2) . . ? O12 C6 C42 114(2) . . ? O2 C1 O1 125.9(18) . . ? O2 C1 C12 119.7(16) . . ? O1 C1 C12 114.4(17) . . ? N11 C12 C13 123.2(18) . . ? N11 C12 C1 113.4(16) . . ? C13 C12 C1 123.3(17) . . ? C12 C13 C14 120.0(17) . . ? C12 C13 H1 120.0 . . ? C14 C13 H1 120.0 . . ? C13 C14 C15 116.3(17) . . ? C13 C14 C24 121.8(15) . . ? C15 C14 C24 121.9(16) . . ? C16 C15 C14 119.5(18) . . ? C16 C15 H2 120.2 . . ? C14 C15 H2 120.2 . . ? N11 C16 C15 122.6(17) . . ? N11 C16 C2 111.0(16) . . ? C15 C16 C2 126.3(18) . . ? O3 C2 O4 128(2) . . ? O3 C2 C16 119(2) . . ? O4 C2 C16 113(2) . . ? O6 C3 O5 126(3) . . ? O6 C3 C22 119(3) . . ? O5 C3 C22 115(2) . . ? N21 C22 C23 121(2) . . ? N21 C22 C3 114(2) . . ? C23 C22 C3 125(2) . . ? C22 C23 C24 120.2(18) . . ? C22 C23 H3 119.9 . . ? C24 C23 H3 119.9 . . ? C23 C24 C25 115.9(18) . . ? C23 C24 C14 120.4(16) . . ? C25 C24 C14 123.6(17) . . ? C26 C25 C24 119.5(19) . . ? C26 C25 H4 120.3 . . ? C24 C25 H4 120.3 . . ? N21 C26 C25 122.4(19) . . ? N21 C26 C4 101.2(18) . . ? C25 C26 C4 136(2) . . ? O7 C4 O8 138(3) . . ? O7 C4 C26 122(2) . . ? O8 C4 C26 100(2) . . ? O7 C4 Ho3 43.6(10) . . ? O8 C4 Ho3 146.6(11) . . ? C26 C4 Ho3 90.5(14) . . ? C32 N31 C32 118(3) 2 . ? C32 N31 Ho1 121.0(13) 2 . ? C32 N31 Ho1 121.0(13) . . ? N31 C32 C33 122(2) . . ? N31 C32 C5 114(2) . . ? C33 C32 C5 124(2) . . ? C32 C33 C34 121(2) . . ? C32 C33 H5 119.7 . . ? C34 C33 H5 119.7 . . ? C33 C34 C33 116(3) . 2 ? C33 C34 C44 121.8(14) . . ? C33 C34 C44 121.8(14) 2 . ? C42 N41 C42 117(2) 2 . ? C42 N41 Ho2 121.6(12) 2 3_455 ? C42 N41 Ho2 121.6(12) . 3_455 ? N41 C42 C43 123(2) . . ? N41 C42 C6 111.3(18) . . ? C43 C42 C6 125(2) . . ? C42 C43 C44 119(2) . . ? C42 C43 H6 120.3 . . ? C44 C43 H6 120.3 . . ? C43 C44 C43 117(3) 2 . ? C43 C44 C34 121.3(14) 2 . ? C43 C44 C34 121.3(14) . . ? 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 O3 Ho2 O1 C1 -4(2) . . . . ? O3 Ho2 O1 C1 -161.3(17) 2_655 . . . ? O11 Ho2 O1 C1 149.8(14) 4_545 . . . ? O11 Ho2 O1 C1 -70.6(16) 3_545 . . . ? O1 Ho2 O1 C1 69.1(15) 2_655 . . . ? N11 Ho2 O1 C1 129.0(17) 2_655 . . . ? N11 Ho2 O1 C1 5.0(15) . . . . ? N41 Ho2 O1 C1 -110.9(15) 3_545 . . . ? O3 Ho2 O3 C2 154(2) 2_655 . . . ? O11 Ho2 O3 C2 -141(2) 4_545 . . . ? O11 Ho2 O3 C2 88(2) 3_545 . . . ? O1 Ho2 O3 C2 -62(2) 2_655 . . . ? O1 Ho2 O3 C2 22(2) . . . . ? N11 Ho2 O3 C2 -80(2) 2_655 . . . ? N11 Ho2 O3 C2 13.5(19) . . . . ? N41 Ho2 O3 C2 154(2) 3_545 . . . ? O4 Ho1 O4 C2 -109(4) 2 . . . ? O14 Ho1 O4 C2 18(4) 2 . . . ? O14 Ho1 O4 C2 102(4) . . . . ? O9 Ho1 O4 C2 -46(3) 2 . . . ? O9 Ho1 O4 C2 -177(4) . . . . ? O13 Ho1 O4 C2 26(3) . . . . ? O13 Ho1 O4 C2 137(3) 2 . . . ? N31 Ho1 O4 C2 -109(4) . . . . ? O7 Ho3 O5 C3 15(3) . . . . ? O10 Ho3 O5 C3 163(3) 5_566 . . . ? O12 Ho3 O5 C3 -60(3) . . . . ? O15 Ho3 O5 C3 180(3) . . . . ? O2 Ho3 O5 C3 98(3) 5_666 . . . ? O16 Ho3 O5 C3 -99(3) . . . . ? N21 Ho3 O5 C3 18(3) . . . . ? C4 Ho3 O5 C3 27(3) . . . . ? O10 Ho3 O7 C4 -133.8(16) 5_566 . . . ? O12 Ho3 O7 C4 95.1(16) . . . . ? O15 Ho3 O7 C4 -121(2) . . . . ? O2 Ho3 O7 C4 -50.1(15) 5_666 . . . ? O5 Ho3 O7 C4 28.0(19) . . . . ? O16 Ho3 O7 C4 157.5(18) . . . . ? N21 Ho3 O7 C4 24.8(14) . . . . ? O4 Ho1 O9 C5 66(2) . . . . ? O4 Ho1 O9 C5 -74(2) 2 . . . ? O14 Ho1 O9 C5 -129(2) 2 . . . ? O14 Ho1 O9 C5 142(2) . . . . ? O9 Ho1 O9 C5 -6(2) 2 . . . ? O13 Ho1 O9 C5 103(2) . . . . ? O13 Ho1 O9 C5 -149(2) 2 . . . ? N31 Ho1 O9 C5 -6(2) . . . . ? O7 Ho3 O12 C6 158(4) . . . . ? O10 Ho3 O12 C6 82(4) 5_566 . . . ? O15 Ho3 O12 C6 -3(4) . . . . ? O2 Ho3 O12 C6 -106(4) 5_666 . . . ? O5 Ho3 O12 C6 -66(4) . . . . ? O16 Ho3 O12 C6 77(4) . . . . ? N21 Ho3 O12 C6 -135(4) . . . . ? C4 Ho3 O12 C6 -177(4) . . . . ? O3 Ho2 N11 C12 177.0(16) . . . . ? O3 Ho2 N11 C12 23.2(18) 2_655 . . . ? O11 Ho2 N11 C12 -137.4(14) 4_545 . . . ? O11 Ho2 N11 C12 89.9(15) 3_545 . . . ? O1 Ho2 N11 C12 -103.9(15) 2_655 . . . ? O1 Ho2 N11 C12 4.4(13) . . . . ? N11 Ho2 N11 C12 -51.3(13) 2_655 . . . ? N41 Ho2 N11 C12 128.7(13) 3_545 . . . ? O3 Ho2 N11 C16 -12.0(15) . . . . ? O3 Ho2 N11 C16 -165.8(14) 2_655 . . . ? O11 Ho2 N11 C16 33.7(19) 4_545 . . . ? O11 Ho2 N11 C16 -99.0(15) 3_545 . . . ? O1 Ho2 N11 C16 67.1(15) 2_655 . . . ? O1 Ho2 N11 C16 175.5(16) . . . . ? N11 Ho2 N11 C16 119.7(16) 2_655 . . . ? N41 Ho2 N11 C16 -60.3(16) 3_545 . . . ? O7 Ho3 N21 C26 -3(2) . . . . ? O10 Ho3 N21 C26 32(3) 5_566 . . . ? O12 Ho3 N21 C26 -102(2) . . . . ? O15 Ho3 N21 C26 154(2) . . . . ? O2 Ho3 N21 C26 94(2) 5_666 . . . ? O5 Ho3 N21 C26 179(2) . . . . ? O16 Ho3 N21 C26 -67(3) . . . . ? C4 Ho3 N21 C26 10.8(18) . . . . ? O7 Ho3 N21 C22 161(2) . . . . ? O10 Ho3 N21 C22 -163.8(19) 5_566 . . . ? O12 Ho3 N21 C22 62(2) . . . . ? O15 Ho3 N21 C22 -42(2) . . . . ? O2 Ho3 N21 C22 -101(2) 5_666 . . . ? O5 Ho3 N21 C22 -16.1(19) . . . . ? O16 Ho3 N21 C22 98(3) . . . . ? C4 Ho3 N21 C22 175(2) . . . . ? Ho1 O9 C5 O10 -166(2) . . . . ? Ho1 O9 C5 C32 8(3) . . . . ? Ho3 O10 C5 O9 -69(5) 5_566 . . . ? Ho3 O10 C5 C32 118(3) 5_566 . . . ? Ho2 O11 C6 O12 -167(2) 3_455 . . . ? Ho2 O11 C6 C42 10(4) 3_455 . . . ? Ho3 O12 C6 O11 -2(6) . . . . ? Ho3 O12 C6 C42 -179(3) . . . . ? Ho3 O2 C1 O1 -86(2) 5_666 . . . ? Ho3 O2 C1 C12 94(2) 5_666 . . . ? Ho2 O1 C1 O2 167.8(15) . . . . ? Ho2 O1 C1 C12 -12(2) . . . . ? C16 N11 C12 C13 -5(3) . . . . ? Ho2 N11 C12 C13 166.0(15) . . . . ? C16 N11 C12 C1 177.5(17) . . . . ? Ho2 N11 C12 C1 -11(2) . . . . ? O2 C1 C12 N11 -165.2(17) . . . . ? O1 C1 C12 N11 15(2) . . . . ? O2 C1 C12 C13 18(3) . . . . ? O1 C1 C12 C13 -162.5(19) . . . . ? N11 C12 C13 C14 1(3) . . . . ? C1 C12 C13 C14 177.5(18) . . . . ? C12 C13 C14 C15 4(3) . . . . ? C12 C13 C14 C24 -177.1(19) . . . . ? C13 C14 C15 C16 -4(3) . . . . ? C24 C14 C15 C16 177(2) . . . . ? C12 N11 C16 C15 5(3) . . . . ? Ho2 N11 C16 C15 -166.3(16) . . . . ? C12 N11 C16 C2 -178.6(16) . . . . ? Ho2 N11 C16 C2 10(2) . . . . ? C14 C15 C16 N11 0(3) . . . . ? C14 C15 C16 C2 -176.0(19) . . . . ? Ho2 O3 C2 O4 166(2) . . . . ? Ho2 O3 C2 C16 -14(3) . . . . ? Ho1 O4 C2 O3 -26(5) . . . . ? Ho1 O4 C2 C16 153(2) . . . . ? N11 C16 C2 O3 2(3) . . . . ? C15 C16 C2 O3 178(2) . . . . ? N11 C16 C2 O4 -177(2) . . . . ? C15 C16 C2 O4 -1(3) . . . . ? Ho3 O5 C3 O6 159(4) . . . . ? Ho3 O5 C3 C22 -18(5) . . . . ? C26 N21 C22 C23 -4(5) . . . . ? Ho3 N21 C22 C23 -168(2) . . . . ? C26 N21 C22 C3 179(3) . . . . ? Ho3 N21 C22 C3 14(4) . . . . ? O6 C3 C22 N21 -176(4) . . . . ? O5 C3 C22 N21 1(5) . . . . ? O6 C3 C22 C23 7(6) . . . . ? O5 C3 C22 C23 -177(3) . . . . ? N21 C22 C23 C24 1(5) . . . . ? C3 C22 C23 C24 178(3) . . . . ? C22 C23 C24 C25 0(4) . . . . ? C22 C23 C24 C14 176(3) . . . . ? C13 C14 C24 C23 39(3) . . . . ? C15 C14 C24 C23 -142(2) . . . . ? C13 C14 C24 C25 -145(2) . . . . ? C15 C14 C24 C25 33(4) . . . . ? C23 C24 C25 C26 2(4) . . . . ? C14 C24 C25 C26 -173(3) . . . . ? C22 N21 C26 C25 6(5) . . . . ? Ho3 N21 C26 C25 170(2) . . . . ? C22 N21 C26 C4 -179(2) . . . . ? Ho3 N21 C26 C4 -15(3) . . . . ? C24 C25 C26 N21 -6(5) . . . . ? C24 C25 C26 C4 -178(3) . . . . ? Ho3 O7 C4 O8 130.1(15) . . . . ? Ho3 O7 C4 C26 -49.8(15) . . . . ? N21 C26 C4 O7 43(2) . . . . ? C25 C26 C4 O7 -144(4) . . . . ? N21 C26 C4 O8 -137(2) . . . . ? C25 C26 C4 O8 36(4) . . . . ? N21 C26 C4 Ho3 11(2) . . . . ? C25 C26 C4 Ho3 -176(4) . . . . ? O10 Ho3 C4 O7 45.5(16) 5_566 . . . ? O12 Ho3 C4 O7 -86.1(16) . . . . ? O15 Ho3 C4 O7 108(2) . . . . ? O2 Ho3 C4 O7 127.9(16) 5_666 . . . ? O5 Ho3 C4 O7 -158.6(15) . . . . ? O16 Ho3 C4 O7 -23.2(19) . . . . ? N21 Ho3 C4 O7 -147.5(17) . . . . ? O7 Ho3 C4 O8 -111(4) . . . . ? O10 Ho3 C4 O8 -66(3) 5_566 . . . ? O12 Ho3 C4 O8 163(3) . . . . ? O15 Ho3 C4 O8 -4(4) . . . . ? O2 Ho3 C4 O8 17(3) 5_666 . . . ? O5 Ho3 C4 O8 90(3) . . . . ? O16 Ho3 C4 O8 -134(3) . . . . ? N21 Ho3 C4 O8 101(3) . . . . ? O7 Ho3 C4 C26 139.7(19) . . . . ? O10 Ho3 C4 C26 -174.8(13) 5_566 . . . ? O12 Ho3 C4 C26 53.6(14) . . . . ? O15 Ho3 C4 C26 -113(2) . . . . ? O2 Ho3 C4 C26 -92.4(13) 5_666 . . . ? O5 Ho3 C4 C26 -18.9(14) . . . . ? O16 Ho3 C4 C26 116.5(17) . . . . ? N21 Ho3 C4 C26 -7.8(13) . . . . ? O4 Ho1 N31 C32 100.2(15) . . . 2 ? O4 Ho1 N31 C32 -79.8(15) 2 . . 2 ? O14 Ho1 N31 C32 -38.7(15) 2 . . 2 ? O14 Ho1 N31 C32 141.3(15) . . . 2 ? O9 Ho1 N31 C32 3.7(14) 2 . . 2 ? O9 Ho1 N31 C32 -176.3(14) . . . 2 ? O13 Ho1 N31 C32 46.4(15) . . . 2 ? O13 Ho1 N31 C32 -133.6(15) 2 . . 2 ? O4 Ho1 N31 C32 -79.8(15) . . . . ? O4 Ho1 N31 C32 100.2(15) 2 . . . ? O14 Ho1 N31 C32 141.3(15) 2 . . . ? O14 Ho1 N31 C32 -38.7(15) . . . . ? O9 Ho1 N31 C32 -176.3(14) 2 . . . ? O9 Ho1 N31 C32 3.7(14) . . . . ? O13 Ho1 N31 C32 -133.6(15) . . . . ? O13 Ho1 N31 C32 46.4(15) 2 . . . ? C32 N31 C32 C33 2(2) 2 . . . ? Ho1 N31 C32 C33 -178(2) . . . . ? C32 N31 C32 C5 178(3) 2 . . . ? Ho1 N31 C32 C5 -2(3) . . . . ? O9 C5 C32 N31 -4(3) . . . . ? O10 C5 C32 N31 170(2) . . . . ? O9 C5 C32 C33 173(3) . . . . ? O10 C5 C32 C33 -13(4) . . . . ? N31 C32 C33 C34 -3(4) . . . . ? C5 C32 C33 C34 -179(2) . . . . ? C32 C33 C34 C33 1.5(19) . . . 2 ? C32 C33 C34 C44 -178.5(19) . . . . ? C42 N41 C42 C43 -1(2) 2 . . . ? Ho2 N41 C42 C43 179(2) 3_455 . . . ? C42 N41 C42 C6 177(3) 2 . . . ? Ho2 N41 C42 C6 -3(3) 3_455 . . . ? O11 C6 C42 N41 -4(4) . . . . ? O12 C6 C42 N41 173(2) . . . . ? O11 C6 C42 C43 173(3) . . . . ? O12 C6 C42 C43 -10(5) . . . . ? N41 C42 C43 C44 1(5) . . . . ? C6 C42 C43 C44 -176(2) . . . . ? C42 C43 C44 C43 -1(2) . . . 2 ? C42 C43 C44 C34 179(2) . . . . ? C33 C34 C44 C43 -151(2) . . . 2 ? C33 C34 C44 C43 29(2) 2 . . 2 ? C33 C34 C44 C43 29(2) . . . . ? C33 C34 C44 C43 -151(2) 2 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 6.499 _refine_diff_density_min -8.333 _refine_diff_density_rms 0.377 #====END