# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data___TbCu _database_code_depnum_ccdc_archive 'CCDC 881971' #TrackingRef '11255_web_deposit_cif_file_0_TakayukiIshida_1336987557.TbCu_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Cu N5 O14 Tb ' _chemical_formula_moiety 'C24 H30 Cu N5 O14 Tb ' _chemical_formula_weight 835.00 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.616(2) _cell_length_b 19.837(6) _cell_length_c 15.774(8) _cell_angle_alpha 90.0000 _cell_angle_beta 95.295(3) _cell_angle_gamma 90.0000 _cell_volume 2996.2(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 417 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660.00 _exptl_absorpt_coefficient_mu 3.123 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_T_max 0.536 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 51450 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_ambient_temperature 100. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6856 _reflns_number_gt 6292 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0333 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6856 _refine_ls_number_parameters 509 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.80 _refine_diff_density_min -0.92 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 14(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Tb Tb -0.172 4.154 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Tb(1) Tb 0.698200(10) 0.576160(10) 0.744310(10) 0.01203(4) Uani 1.00 1 d . . . Cu(1) Cu 0.79123(4) 0.73877(2) 0.81828(2) 0.01222(8) Uani 1.00 1 d . . . O(1) O 0.7840(2) 0.64584(10) 0.86034(13) 0.0158(5) Uani 1.00 1 d . . . O(2) O 0.6719(2) 0.69468(10) 0.72734(13) 0.0156(5) Uani 1.00 1 d . . . O(3) O 0.7393(2) 0.51778(10) 0.88720(13) 0.0181(5) Uani 1.00 1 d . . . O(4) O 0.5213(2) 0.61414(10) 0.62622(13) 0.0162(5) Uani 1.00 1 d . . . O(5) O 0.4900(2) 0.60136(11) 0.82087(15) 0.0216(5) Uani 1.00 1 d . . . O(6) O 0.4943(2) 0.50446(11) 0.75797(14) 0.0206(5) Uani 1.00 1 d . . . O(7) O 0.3283(2) 0.52718(14) 0.83899(19) 0.0406(8) Uani 1.00 1 d . . . O(8) O 0.6756(2) 0.49517(12) 0.62116(15) 0.0291(6) Uani 1.00 1 d . . . O(9) O 0.7816(2) 0.45549(12) 0.73563(15) 0.0269(6) Uani 1.00 1 d . . . O(10) O 0.7441(2) 0.39010(11) 0.62483(16) 0.0263(6) Uani 1.00 1 d . . . O(11) O 0.9557(2) 0.57161(13) 0.75526(17) 0.0327(7) Uani 1.00 1 d . . . O(12) O 0.8564(2) 0.61234(16) 0.64015(16) 0.0375(7) Uani 1.00 1 d . . . O(13) O 1.0839(2) 0.61380(12) 0.66085(17) 0.0304(6) Uani 1.00 1 d . . . O(14) O 1.0086(2) 0.74460(12) 0.74854(15) 0.0223(5) Uani 1.00 1 d . . . N(1) N 0.8843(2) 0.77125(13) 0.92838(16) 0.0150(6) Uani 1.00 1 d . . . N(2) N 0.7656(2) 0.82801(12) 0.76287(15) 0.0141(6) Uani 1.00 1 d . . . N(3) N 0.4334(2) 0.54427(14) 0.80730(18) 0.0220(7) Uani 1.00 1 d . . . N(4) N 0.7342(2) 0.44519(13) 0.65958(17) 0.0187(6) Uani 1.00 1 d . . . N(5) N 0.9692(2) 0.59964(13) 0.68463(18) 0.0212(7) Uani 1.00 1 d . . . C(1) C 0.8287(3) 0.62193(15) 0.93689(18) 0.0143(7) Uani 1.00 1 d . . . C(2) C 0.8088(3) 0.55309(16) 0.95449(19) 0.0165(7) Uani 1.00 1 d . . . C(3) C 0.8567(3) 0.52453(16) 1.0312(2) 0.0186(7) Uani 1.00 1 d . . . C(4) C 0.9265(3) 0.56481(18) 1.0951(2) 0.0219(8) Uani 1.00 1 d . . . C(5) C 0.9430(3) 0.63199(17) 1.0809(2) 0.0202(8) Uani 1.00 1 d . . . C(6) C 0.8942(3) 0.66204(15) 1.00255(19) 0.0153(7) Uani 1.00 1 d . . . C(7) C 0.9138(3) 0.73362(16) 0.9947(2) 0.0173(7) Uani 1.00 1 d . . . C(8) C 0.6917(4) 0.45073(17) 0.9087(2) 0.0249(9) Uani 1.00 1 d . . . C(9) C 0.9310(3) 0.84214(16) 0.9406(2) 0.0194(7) Uani 1.00 1 d . . . C(10) C 0.8345(3) 0.89369(15) 0.8952(2) 0.0164(7) Uani 1.00 1 d . . . C(11) C 0.8395(3) 0.88758(16) 0.7997(2) 0.0176(7) Uani 1.00 1 d . . . C(12) C 0.8921(3) 0.96329(17) 0.9211(2) 0.0228(8) Uani 1.00 1 d . . . C(13) C 0.6853(3) 0.88668(17) 0.9203(2) 0.0223(8) Uani 1.00 1 d . . . C(14) C 0.6078(2) 0.72300(15) 0.65766(18) 0.0117(6) Uani 1.00 1 d . . . C(15) C 0.5257(3) 0.68065(15) 0.60010(19) 0.0141(7) Uani 1.00 1 d . . . C(16) C 0.4587(3) 0.70516(16) 0.5256(2) 0.0187(7) Uani 1.00 1 d . . . C(17) C 0.4731(3) 0.77346(17) 0.5047(2) 0.0220(8) Uani 1.00 1 d . . . C(18) C 0.5486(3) 0.81562(16) 0.5601(2) 0.0200(8) Uani 1.00 1 d . . . C(19) C 0.6155(3) 0.79111(15) 0.63732(18) 0.0149(7) Uani 1.00 1 d . . . C(20) C 0.6910(3) 0.83944(15) 0.69226(19) 0.0155(7) Uani 1.00 1 d . . . C(21) C 0.4156(3) 0.57283(17) 0.5795(2) 0.0236(9) Uani 1.00 1 d . . . C(22) C 1.1287(3) 0.73059(17) 0.7738(2) 0.0248(8) Uani 1.00 1 d . . . C(23) C 1.1624(3) 0.6889(2) 0.8518(2) 0.0341(10) Uani 1.00 1 d . . . C(24) C 1.2502(4) 0.7552(2) 0.7285(3) 0.0452(13) Uani 1.00 1 d . . . H(1) H 0.843(3) 0.4780(17) 1.044(2) 0.020(9) Uiso 1.00 1 d . . . H(2) H 0.957(3) 0.5451(18) 1.144(2) 0.027(10) Uiso 1.00 1 d . . . H(3) H 0.986(3) 0.6623(19) 1.123(2) 0.037(11) Uiso 1.00 1 d . . . H(4) H 0.956(3) 0.7558(16) 1.049(2) 0.018(8) Uiso 1.00 1 d . . . H(5) H 0.634(3) 0.4349(17) 0.859(2) 0.026(10) Uiso 1.00 1 d . . . H(6) H 0.643(3) 0.4550(19) 0.959(2) 0.034(10) Uiso 1.00 1 d . . . H(7) H 0.773(4) 0.4222(18) 0.920(2) 0.036(11) Uiso 1.00 1 d . . . H(8) H 1.023(3) 0.8450(16) 0.920(2) 0.019(8) Uiso 1.00 1 d . . . H(9) H 0.938(3) 0.8544(18) 1.002(2) 0.027(9) Uiso 1.00 1 d . . . H(10) H 0.941(3) 0.8826(17) 0.788(2) 0.023(9) Uiso 1.00 1 d . . . H(11) H 0.807(3) 0.9263(18) 0.770(2) 0.028(11) Uiso 1.00 1 d . . . H(12) H 0.994(3) 0.9666(15) 0.912(2) 0.014(8) Uiso 1.00 1 d . . . H(13) H 0.886(3) 0.9734(18) 0.979(2) 0.032(10) Uiso 1.00 1 d . . . H(14) H 0.841(3) 1.0004(18) 0.887(2) 0.028(10) Uiso 1.00 1 d . . . H(15) H 0.645(3) 0.8419(16) 0.9076(19) 0.013(8) Uiso 1.00 1 d . . . H(16) H 0.624(3) 0.9154(17) 0.885(2) 0.023(9) Uiso 1.00 1 d . . . H(17) H 0.685(4) 0.895(2) 0.981(2) 0.046(12) Uiso 1.00 1 d . . . H(18) H 0.407(3) 0.6762(15) 0.4865(18) 0.009(7) Uiso 1.00 1 d . . . H(19) H 0.435(3) 0.7902(18) 0.450(2) 0.029(10) Uiso 1.00 1 d . . . H(20) H 0.565(3) 0.8600(17) 0.547(2) 0.022(9) Uiso 1.00 1 d . . . H(21) H 0.684(3) 0.8838(17) 0.670(2) 0.020(9) Uiso 1.00 1 d . . . H(22) H 0.416(3) 0.5315(17) 0.612(2) 0.020(9) Uiso 1.00 1 d . . . H(23) H 0.323(3) 0.5959(19) 0.578(2) 0.033(10) Uiso 1.00 1 d . . . H(24) H 0.438(3) 0.5672(18) 0.520(2) 0.031(10) Uiso 1.00 1 d . . . H(25) H 1.0889 0.6581 0.8592 0.041 Uiso 1.00 1 c R . . H(26) H 1.1756 0.7177 0.9000 0.041 Uiso 1.00 1 c R . . H(27) H 1.2461 0.6646 0.8458 0.041 Uiso 1.00 1 c R . . H(28) H 1.3282 0.7617 0.7692 0.056 Uiso 1.00 1 c R . . H(29) H 1.2270 0.7968 0.7007 0.056 Uiso 1.00 1 c R . . H(30) H 1.2728 0.7228 0.6877 0.056 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tb(1) 0.01408(9) 0.00984(9) 0.01236(9) -0.00117(5) 0.00224(6) -0.00144(5) Cu(1) 0.01449(18) 0.01031(18) 0.01176(18) -0.00122(13) 0.00070(14) -0.00119(13) O(1) 0.0233(11) 0.0120(10) 0.0116(9) -0.0018(8) -0.0015(8) 0.0002(8) O(2) 0.0198(10) 0.0110(10) 0.0154(10) -0.0029(8) -0.0027(8) -0.0007(8) O(3) 0.0272(12) 0.0123(10) 0.0149(10) -0.0032(8) 0.0019(9) 0.0028(8) O(4) 0.0167(10) 0.0127(10) 0.0184(10) -0.0015(8) -0.0026(8) -0.0032(8) O(5) 0.0218(11) 0.0157(11) 0.0287(12) -0.0031(9) 0.0095(9) -0.0052(9) O(6) 0.0200(11) 0.0179(11) 0.0249(12) -0.0025(8) 0.0069(9) -0.0046(9) O(7) 0.0337(14) 0.0346(15) 0.0583(19) -0.0130(12) 0.0301(14) -0.0078(13) O(8) 0.0453(15) 0.0217(12) 0.0191(12) 0.0145(11) -0.0034(10) -0.0049(9) O(9) 0.0365(14) 0.0243(13) 0.0181(11) 0.0084(10) -0.0061(10) -0.0077(10) O(10) 0.0270(12) 0.0188(11) 0.0327(13) 0.0028(9) 0.0011(10) -0.0133(10) O(11) 0.0249(13) 0.0420(16) 0.0312(14) 0.0015(11) 0.0034(11) 0.0131(11) O(12) 0.0203(12) 0.070(2) 0.0223(13) -0.0033(13) 0.0032(10) 0.0112(13) O(13) 0.0215(12) 0.0274(13) 0.0455(16) -0.0082(10) 0.0200(11) -0.0134(11) O(14) 0.0149(10) 0.0252(12) 0.0275(12) 0.0014(9) 0.0062(9) -0.0027(10) N(1) 0.0154(12) 0.0150(12) 0.0149(12) 0.0004(9) 0.0026(9) -0.0028(9) N(2) 0.0165(12) 0.0113(11) 0.0148(12) -0.0015(9) 0.0029(9) -0.0018(9) N(3) 0.0230(14) 0.0201(14) 0.0243(14) -0.0014(11) 0.0094(11) 0.0009(11) N(4) 0.0161(12) 0.0175(13) 0.0231(14) -0.0021(10) 0.0055(10) -0.0065(11) N(5) 0.0226(14) 0.0153(13) 0.0272(15) -0.0026(11) 0.0098(11) -0.0081(11) C(1) 0.0154(14) 0.0163(14) 0.0118(13) 0.0022(11) 0.0041(11) 0.0028(11) C(2) 0.0185(15) 0.0185(15) 0.0129(14) 0.0002(12) 0.0025(11) -0.0026(12) C(3) 0.0233(16) 0.0181(15) 0.0152(15) 0.0053(12) 0.0053(12) 0.0043(12) C(4) 0.0281(18) 0.0254(17) 0.0124(15) 0.0082(14) 0.0034(13) 0.0048(13) C(5) 0.0254(17) 0.0235(16) 0.0118(14) 0.0043(13) 0.0027(12) -0.0036(12) C(6) 0.0167(14) 0.0156(14) 0.0136(14) 0.0025(11) 0.0019(11) -0.0012(11) C(7) 0.0170(14) 0.0195(15) 0.0150(14) 0.0006(12) 0.0000(11) -0.0039(12) C(8) 0.034(2) 0.0163(16) 0.0244(18) -0.0036(14) 0.0032(15) 0.0057(13) C(9) 0.0214(16) 0.0155(15) 0.0211(16) -0.0058(12) 0.0009(13) -0.0029(12) C(10) 0.0181(14) 0.0117(14) 0.0194(15) -0.0043(11) 0.0022(12) -0.0021(11) C(11) 0.0200(15) 0.0142(14) 0.0186(15) -0.0060(12) 0.0021(12) -0.0006(12) C(12) 0.0268(18) 0.0133(15) 0.0291(18) -0.0065(13) 0.0062(14) -0.0051(13) C(13) 0.0225(17) 0.0162(16) 0.0297(19) -0.0035(13) 0.0102(14) -0.0049(14) C(14) 0.0081(12) 0.0164(14) 0.0105(13) 0.0007(10) -0.0001(10) -0.0001(11) C(15) 0.0124(13) 0.0156(14) 0.0146(14) 0.0010(11) 0.0032(11) -0.0006(11) C(16) 0.0164(14) 0.0187(15) 0.0198(15) 0.0021(12) -0.0052(12) -0.0049(12) C(17) 0.0230(16) 0.0232(17) 0.0185(16) 0.0052(13) -0.0050(13) 0.0036(13) C(18) 0.0211(16) 0.0150(15) 0.0233(16) 0.0040(12) -0.0006(13) 0.0042(12) C(19) 0.0122(13) 0.0184(15) 0.0138(14) 0.0003(11) 0.0002(11) -0.0003(11) C(20) 0.0166(14) 0.0126(14) 0.0172(14) -0.0002(11) 0.0011(11) 0.0035(11) C(21) 0.0197(17) 0.0202(17) 0.0299(19) -0.0075(13) -0.0034(14) -0.0051(14) C(22) 0.0193(16) 0.0227(17) 0.0333(19) -0.0023(13) 0.0064(14) -0.0135(14) C(23) 0.0216(18) 0.042(2) 0.038(2) 0.0071(16) 0.0005(15) -0.0061(17) C(24) 0.030(2) 0.045(2) 0.063(3) -0.0021(19) 0.021(2) -0.006(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tb(1) O(1) 2.3797(19) yes . . Tb(1) O(2) 2.3771(19) yes . . Tb(1) O(3) 2.532(2) yes . . Tb(1) O(4) 2.5190(19) yes . . Tb(1) O(5) 2.483(2) yes . . Tb(1) O(6) 2.448(2) yes . . Tb(1) O(8) 2.515(2) yes . . Tb(1) O(9) 2.532(2) yes . . Tb(1) O(11) 2.468(2) yes . . Tb(1) O(12) 2.448(2) yes . . Cu(1) O(1) 1.963(2) yes . . Cu(1) O(2) 1.958(2) yes . . Cu(1) O(14) 2.453(2) yes . . Cu(1) N(1) 1.986(2) yes . . Cu(1) N(2) 1.980(2) yes . . O(1) C(1) 1.331(3) yes . . O(2) C(14) 1.334(3) yes . . O(3) C(2) 1.390(3) yes . . O(3) C(8) 1.457(4) yes . . O(4) C(15) 1.384(3) yes . . O(4) C(21) 1.453(4) yes . . O(5) N(3) 1.266(3) yes . . O(6) N(3) 1.287(3) yes . . O(7) N(3) 1.216(4) yes . . O(8) N(4) 1.267(3) yes . . O(9) N(4) 1.260(3) yes . . O(10) N(4) 1.230(3) yes . . O(11) N(5) 1.263(3) yes . . O(12) N(5) 1.262(3) yes . . O(13) N(5) 1.229(3) yes . . O(14) C(22) 1.218(3) yes . . N(1) C(7) 1.295(4) yes . . N(1) C(9) 1.483(4) yes . . N(2) C(11) 1.471(3) yes . . N(2) C(20) 1.288(3) yes . . C(1) C(2) 1.410(4) yes . . C(1) C(6) 1.408(4) yes . . C(2) C(3) 1.376(4) yes . . C(3) C(4) 1.408(4) yes . . C(4) C(5) 1.363(4) yes . . C(5) C(6) 1.412(4) yes . . C(6) C(7) 1.439(4) yes . . C(9) C(10) 1.515(4) yes . . C(10) C(11) 1.516(4) yes . . C(10) C(12) 1.529(4) yes . . C(10) C(13) 1.529(4) yes . . C(14) C(15) 1.422(3) yes . . C(14) C(19) 1.392(4) yes . . C(15) C(16) 1.376(4) yes . . C(16) C(17) 1.404(4) yes . . C(17) C(18) 1.369(4) yes . . C(18) C(19) 1.411(4) yes . . C(19) C(20) 1.443(4) yes . . C(22) C(23) 1.493(5) yes . . C(22) C(24) 1.506(5) yes . . C(3) H(1) 0.96(3) no . . C(4) H(2) 0.89(3) no . . C(5) H(3) 0.96(3) no . . C(7) H(4) 1.01(3) no . . C(8) H(5) 0.97(3) no . . C(8) H(6) 0.97(4) no . . C(8) H(7) 0.97(3) no . . C(9) H(8) 0.97(3) no . . C(9) H(9) 0.99(3) no . . C(11) H(10) 1.01(3) no . . C(11) H(11) 0.94(3) no . . C(12) H(12) 1.01(3) no . . C(12) H(13) 0.94(3) no . . C(12) H(14) 1.01(3) no . . C(13) H(15) 0.98(3) no . . C(13) H(16) 0.96(3) no . . C(13) H(17) 0.96(4) no . . C(16) H(18) 0.95(2) no . . C(17) H(19) 0.97(3) no . . C(18) H(20) 0.92(3) no . . C(20) H(21) 0.95(3) no . . C(21) H(22) 0.96(3) no . . C(21) H(23) 1.00(3) no . . C(21) H(24) 0.99(4) no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Tb(1) O(2) 62.47(6) yes . . . O(1) Tb(1) O(3) 64.31(6) yes . . . O(1) Tb(1) O(4) 123.89(6) yes . . . O(1) Tb(1) O(5) 75.35(7) yes . . . O(1) Tb(1) O(6) 119.58(7) yes . . . O(1) Tb(1) O(8) 164.65(7) yes . . . O(1) Tb(1) O(9) 120.10(7) yes . . . O(1) Tb(1) O(11) 72.11(8) yes . . . O(1) Tb(1) O(12) 98.80(8) yes . . . O(2) Tb(1) O(3) 123.97(6) yes . . . O(2) Tb(1) O(4) 64.11(6) yes . . . O(2) Tb(1) O(5) 76.91(7) yes . . . O(2) Tb(1) O(6) 120.46(7) yes . . . O(2) Tb(1) O(8) 122.97(7) yes . . . O(2) Tb(1) O(9) 163.70(7) yes . . . O(2) Tb(1) O(11) 98.02(7) yes . . . O(2) Tb(1) O(12) 72.58(8) yes . . . O(3) Tb(1) O(4) 146.54(6) yes . . . O(3) Tb(1) O(5) 74.09(7) yes . . . O(3) Tb(1) O(6) 73.53(6) yes . . . O(3) Tb(1) O(8) 112.99(7) yes . . . O(3) Tb(1) O(9) 65.90(7) yes . . . O(3) Tb(1) O(11) 81.24(7) yes . . . O(3) Tb(1) O(12) 132.52(7) yes . . . O(4) Tb(1) O(5) 77.27(7) yes . . . O(4) Tb(1) O(6) 75.36(6) yes . . . O(4) Tb(1) O(8) 67.38(7) yes . . . O(4) Tb(1) O(9) 116.00(6) yes . . . O(4) Tb(1) O(11) 131.86(7) yes . . . O(4) Tb(1) O(12) 80.50(7) yes . . . O(5) Tb(1) O(6) 52.09(7) yes . . . O(5) Tb(1) O(8) 119.22(7) yes . . . O(5) Tb(1) O(9) 119.36(7) yes . . . O(5) Tb(1) O(11) 145.32(8) yes . . . O(5) Tb(1) O(12) 147.85(8) yes . . . O(6) Tb(1) O(8) 71.57(7) yes . . . O(6) Tb(1) O(9) 73.48(7) yes . . . O(6) Tb(1) O(11) 141.19(7) yes . . . O(6) Tb(1) O(12) 141.45(8) yes . . . O(8) Tb(1) O(9) 50.17(7) yes . . . O(8) Tb(1) O(11) 92.60(8) yes . . . O(8) Tb(1) O(12) 71.56(8) yes . . . O(9) Tb(1) O(11) 69.42(8) yes . . . O(9) Tb(1) O(12) 91.22(9) yes . . . O(11) Tb(1) O(12) 51.38(8) yes . . . O(1) Cu(1) O(2) 77.97(8) yes . . . O(1) Cu(1) O(14) 104.71(8) yes . . . O(1) Cu(1) N(1) 92.07(9) yes . . . O(1) Cu(1) N(2) 169.23(9) yes . . . O(2) Cu(1) O(14) 99.11(8) yes . . . O(2) Cu(1) N(1) 166.29(9) yes . . . O(2) Cu(1) N(2) 92.02(8) yes . . . O(14) Cu(1) N(1) 92.47(9) yes . . . O(14) Cu(1) N(2) 80.59(9) yes . . . N(1) Cu(1) N(2) 97.11(10) yes . . . Tb(1) O(1) Cu(1) 107.83(8) yes . . . Tb(1) O(1) C(1) 123.41(17) yes . . . Cu(1) O(1) C(1) 128.53(18) yes . . . Tb(1) O(2) Cu(1) 108.07(8) yes . . . Tb(1) O(2) C(14) 123.07(17) yes . . . Cu(1) O(2) C(14) 127.63(18) yes . . . Tb(1) O(3) C(2) 118.28(17) yes . . . Tb(1) O(3) C(8) 126.73(18) yes . . . C(2) O(3) C(8) 114.9(2) yes . . . Tb(1) O(4) C(15) 117.93(15) yes . . . Tb(1) O(4) C(21) 126.86(17) yes . . . C(15) O(4) C(21) 115.2(2) yes . . . Tb(1) O(5) N(3) 95.21(17) yes . . . Tb(1) O(6) N(3) 96.28(16) yes . . . Tb(1) O(8) N(4) 97.32(17) yes . . . Tb(1) O(9) N(4) 96.68(17) yes . . . Tb(1) O(11) N(5) 96.11(18) yes . . . Tb(1) O(12) N(5) 97.12(19) yes . . . Cu(1) O(14) C(22) 131.6(2) yes . . . Cu(1) N(1) C(7) 124.5(2) yes . . . Cu(1) N(1) C(9) 121.84(19) yes . . . C(7) N(1) C(9) 113.6(2) yes . . . Cu(1) N(2) C(11) 120.52(18) yes . . . Cu(1) N(2) C(20) 125.2(2) yes . . . C(11) N(2) C(20) 114.2(2) yes . . . O(5) N(3) O(6) 116.0(2) yes . . . O(5) N(3) O(7) 122.7(2) yes . . . O(6) N(3) O(7) 121.3(2) yes . . . O(8) N(4) O(9) 115.7(2) yes . . . O(8) N(4) O(10) 122.1(2) yes . . . O(9) N(4) O(10) 122.2(2) yes . . . O(11) N(5) O(12) 115.2(2) yes . . . O(11) N(5) O(13) 122.6(2) yes . . . O(12) N(5) O(13) 122.3(2) yes . . . O(1) C(1) C(2) 119.0(2) yes . . . O(1) C(1) C(6) 123.4(2) yes . . . C(2) C(1) C(6) 117.5(2) yes . . . O(3) C(2) C(1) 113.7(2) yes . . . O(3) C(2) C(3) 124.2(2) yes . . . C(1) C(2) C(3) 122.1(2) yes . . . C(2) C(3) C(4) 119.7(2) yes . . . C(3) C(4) C(5) 119.5(2) yes . . . C(4) C(5) C(6) 121.5(2) yes . . . C(1) C(6) C(5) 119.7(2) yes . . . C(1) C(6) C(7) 123.2(2) yes . . . C(5) C(6) C(7) 117.1(2) yes . . . N(1) C(7) C(6) 128.1(2) yes . . . N(1) C(9) C(10) 114.4(2) yes . . . C(9) C(10) C(11) 110.0(2) yes . . . C(9) C(10) C(12) 107.0(2) yes . . . C(9) C(10) C(13) 111.4(2) yes . . . C(11) C(10) C(12) 107.0(2) yes . . . C(11) C(10) C(13) 111.5(2) yes . . . C(12) C(10) C(13) 109.8(2) yes . . . N(2) C(11) C(10) 113.5(2) yes . . . O(2) C(14) C(15) 117.7(2) yes . . . O(2) C(14) C(19) 124.6(2) yes . . . C(15) C(14) C(19) 117.7(2) yes . . . O(4) C(15) C(14) 113.8(2) yes . . . O(4) C(15) C(16) 124.5(2) yes . . . C(14) C(15) C(16) 121.7(2) yes . . . C(15) C(16) C(17) 119.6(2) yes . . . C(16) C(17) C(18) 119.8(2) yes . . . C(17) C(18) C(19) 120.9(2) yes . . . C(14) C(19) C(18) 120.3(2) yes . . . C(14) C(19) C(20) 122.8(2) yes . . . C(18) C(19) C(20) 117.0(2) yes . . . N(2) C(20) C(19) 127.7(2) yes . . . O(14) C(22) C(23) 121.6(3) yes . . . O(14) C(22) C(24) 121.6(3) yes . . . C(23) C(22) C(24) 116.8(2) yes . . . C(2) C(3) H(1) 123.1(19) no . . . C(4) C(3) H(1) 117.2(19) no . . . C(3) C(4) H(2) 118(2) no . . . C(5) C(4) H(2) 123(2) no . . . C(4) C(5) H(3) 123(2) no . . . C(6) C(5) H(3) 115(2) no . . . N(1) C(7) H(4) 118.3(18) no . . . C(6) C(7) H(4) 113.6(18) no . . . O(3) C(8) H(5) 106(2) no . . . O(3) C(8) H(6) 107(2) no . . . O(3) C(8) H(7) 108(2) no . . . H(5) C(8) H(6) 114(3) no . . . H(5) C(8) H(7) 111(3) no . . . H(6) C(8) H(7) 110(3) no . . . N(1) C(9) H(8) 106.6(19) no . . . N(1) C(9) H(9) 111(2) no . . . C(10) C(9) H(8) 109.9(19) no . . . C(10) C(9) H(9) 106(2) no . . . H(8) C(9) H(9) 109(2) no . . . N(2) C(11) H(10) 106.5(19) no . . . N(2) C(11) H(11) 110(2) no . . . C(10) C(11) H(10) 108.4(19) no . . . C(10) C(11) H(11) 113(2) no . . . H(10) C(11) H(11) 106(2) no . . . C(10) C(12) H(12) 110.6(18) no . . . C(10) C(12) H(13) 114(2) no . . . C(10) C(12) H(14) 111.7(19) no . . . H(12) C(12) H(13) 106(2) no . . . H(12) C(12) H(14) 108(2) no . . . H(13) C(12) H(14) 107(3) no . . . C(10) C(13) H(15) 113.1(19) no . . . C(10) C(13) H(16) 109(2) no . . . C(10) C(13) H(17) 109(2) no . . . H(15) C(13) H(16) 102(2) no . . . H(15) C(13) H(17) 109(3) no . . . H(16) C(13) H(17) 114(3) no . . . C(15) C(16) H(18) 121.1(18) no . . . C(17) C(16) H(18) 119.2(18) no . . . C(16) C(17) H(19) 120(2) no . . . C(18) C(17) H(19) 120(2) no . . . C(17) C(18) H(20) 122(2) no . . . C(19) C(18) H(20) 117(2) no . . . N(2) C(20) H(21) 119.9(19) no . . . C(19) C(20) H(21) 112.4(19) no . . . O(4) C(21) H(22) 103.8(19) no . . . O(4) C(21) H(23) 109(2) no . . . O(4) C(21) H(24) 110(2) no . . . H(22) C(21) H(23) 111(2) no . . . H(22) C(21) H(24) 114(2) no . . . H(23) C(21) H(24) 108(2) no . . . C(22) C(23) H(25) 110.5 no . . . C(22) C(23) H(26) 109.2 no . . . C(22) C(23) H(27) 108.7 no . . . H(25) C(23) H(26) 109.5 no . . . H(25) C(23) H(27) 109.5 no . . . H(26) C(23) H(27) 109.5 no . . . C(22) C(24) H(28) 108.8 no . . . C(22) C(24) H(29) 109.9 no . . . C(22) C(24) H(30) 109.7 no . . . H(28) C(24) H(29) 109.5 no . . . H(28) C(24) H(30) 109.5 no . . . H(29) C(24) H(30) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Tb(1) O(2) Cu(1) 14.12(8) ? . . . . O(1) Tb(1) O(2) C(14) -177.7(2) ? . . . . O(2) Tb(1) O(1) Cu(1) -14.06(8) ? . . . . O(2) Tb(1) O(1) C(1) 171.0(2) ? . . . . O(1) Tb(1) O(3) C(2) -9.52(19) ? . . . . O(1) Tb(1) O(3) C(8) 167.4(2) ? . . . . O(3) Tb(1) O(1) Cu(1) -175.86(12) ? . . . . O(3) Tb(1) O(1) C(1) 9.2(2) ? . . . . O(1) Tb(1) O(4) C(15) 34.6(2) ? . . . . O(1) Tb(1) O(4) C(21) -147.5(2) ? . . . . O(4) Tb(1) O(1) Cu(1) -33.47(12) ? . . . . O(4) Tb(1) O(1) C(1) 151.6(2) ? . . . . O(1) Tb(1) O(5) N(3) -144.64(17) ? . . . . O(5) Tb(1) O(1) Cu(1) -96.73(10) ? . . . . O(5) Tb(1) O(1) C(1) 88.4(2) ? . . . . O(1) Tb(1) O(6) N(3) 32.30(18) ? . . . . O(6) Tb(1) O(1) Cu(1) -125.26(9) ? . . . . O(6) Tb(1) O(1) C(1) 59.8(2) ? . . . . O(1) Tb(1) O(8) N(4) 56.8(3) ? . . . . O(8) Tb(1) O(1) Cu(1) 100.7(2) ? . . . . O(8) Tb(1) O(1) C(1) -74.2(3) ? . . . . O(1) Tb(1) O(9) N(4) -167.06(16) ? . . . . O(9) Tb(1) O(1) Cu(1) 147.54(8) ? . . . . O(9) Tb(1) O(1) C(1) -27.4(2) ? . . . . O(1) Tb(1) O(11) N(5) -114.94(18) ? . . . . O(11) Tb(1) O(1) Cu(1) 95.42(10) ? . . . . O(11) Tb(1) O(1) C(1) -79.5(2) ? . . . . O(1) Tb(1) O(12) N(5) 55.9(2) ? . . . . O(12) Tb(1) O(1) Cu(1) 50.95(11) ? . . . . O(12) Tb(1) O(1) C(1) -124.0(2) ? . . . . O(2) Tb(1) O(3) C(2) -29.0(2) ? . . . . O(2) Tb(1) O(3) C(8) 147.8(2) ? . . . . O(3) Tb(1) O(2) Cu(1) 33.96(13) ? . . . . O(3) Tb(1) O(2) C(14) -157.82(19) ? . . . . O(2) Tb(1) O(4) C(15) 15.47(18) ? . . . . O(2) Tb(1) O(4) C(21) -166.7(2) ? . . . . O(4) Tb(1) O(2) Cu(1) 176.26(12) ? . . . . O(4) Tb(1) O(2) C(14) -15.52(19) ? . . . . O(2) Tb(1) O(5) N(3) 150.81(17) ? . . . . O(5) Tb(1) O(2) Cu(1) 94.23(10) ? . . . . O(5) Tb(1) O(2) C(14) -97.6(2) ? . . . . O(2) Tb(1) O(6) N(3) -41.28(18) ? . . . . O(6) Tb(1) O(2) Cu(1) 123.95(9) ? . . . . O(6) Tb(1) O(2) C(14) -67.8(2) ? . . . . O(2) Tb(1) O(8) N(4) 163.16(16) ? . . . . O(8) Tb(1) O(2) Cu(1) -149.25(9) ? . . . . O(8) Tb(1) O(2) C(14) 19.0(2) ? . . . . O(2) Tb(1) O(9) N(4) -72.5(3) ? . . . . O(9) Tb(1) O(2) Cu(1) -89.4(2) ? . . . . O(9) Tb(1) O(2) C(14) 78.9(3) ? . . . . O(2) Tb(1) O(11) N(5) -57.34(18) ? . . . . O(11) Tb(1) O(2) Cu(1) -50.84(10) ? . . . . O(11) Tb(1) O(2) C(14) 117.4(2) ? . . . . O(2) Tb(1) O(12) N(5) 113.3(2) ? . . . . O(12) Tb(1) O(2) Cu(1) -96.03(10) ? . . . . O(12) Tb(1) O(2) C(14) 72.2(2) ? . . . . O(3) Tb(1) O(4) C(15) 128.56(19) ? . . . . O(3) Tb(1) O(4) C(21) -53.6(2) ? . . . . O(4) Tb(1) O(3) C(2) -122.8(2) ? . . . . O(4) Tb(1) O(3) C(8) 54.1(2) ? . . . . O(3) Tb(1) O(5) N(3) -77.68(16) ? . . . . O(5) Tb(1) O(3) C(2) -90.6(2) ? . . . . O(5) Tb(1) O(3) C(8) 86.3(2) ? . . . . O(3) Tb(1) O(6) N(3) 78.86(16) ? . . . . O(6) Tb(1) O(3) C(2) -145.0(2) ? . . . . O(6) Tb(1) O(3) C(8) 31.8(2) ? . . . . O(3) Tb(1) O(8) N(4) -19.7(2) ? . . . . O(8) Tb(1) O(3) C(2) 153.88(19) ? . . . . O(8) Tb(1) O(3) C(8) -29.2(2) ? . . . . O(3) Tb(1) O(9) N(4) 156.88(19) ? . . . . O(9) Tb(1) O(3) C(2) 136.1(2) ? . . . . O(9) Tb(1) O(3) C(8) -47.1(2) ? . . . . O(3) Tb(1) O(11) N(5) 179.34(18) ? . . . . O(11) Tb(1) O(3) C(2) 64.8(2) ? . . . . O(11) Tb(1) O(3) C(8) -118.4(2) ? . . . . O(3) Tb(1) O(12) N(5) -7.2(2) ? . . . . O(12) Tb(1) O(3) C(2) 68.3(2) ? . . . . O(12) Tb(1) O(3) C(8) -114.8(2) ? . . . . O(4) Tb(1) O(5) N(3) 84.82(16) ? . . . . O(5) Tb(1) O(4) C(15) 96.93(19) ? . . . . O(5) Tb(1) O(4) C(21) -85.2(2) ? . . . . O(4) Tb(1) O(6) N(3) -88.66(16) ? . . . . O(6) Tb(1) O(4) C(15) 150.6(2) ? . . . . O(6) Tb(1) O(4) C(21) -31.5(2) ? . . . . O(4) Tb(1) O(8) N(4) -163.3(2) ? . . . . O(8) Tb(1) O(4) C(15) -133.6(2) ? . . . . O(8) Tb(1) O(4) C(21) 44.3(2) ? . . . . O(4) Tb(1) O(9) N(4) 13.9(2) ? . . . . O(9) Tb(1) O(4) C(15) -146.39(18) ? . . . . O(9) Tb(1) O(4) C(21) 31.5(2) ? . . . . O(4) Tb(1) O(11) N(5) 4.9(2) ? . . . . O(11) Tb(1) O(4) C(15) -61.4(2) ? . . . . O(11) Tb(1) O(4) C(21) 116.4(2) ? . . . . O(4) Tb(1) O(12) N(5) 179.0(2) ? . . . . O(12) Tb(1) O(4) C(15) -59.7(2) ? . . . . O(12) Tb(1) O(4) C(21) 118.2(2) ? . . . . O(5) Tb(1) O(6) N(3) -3.55(15) ? . . . . O(6) Tb(1) O(5) N(3) 3.60(15) ? . . . . O(5) Tb(1) O(8) N(4) -103.77(18) ? . . . . O(8) Tb(1) O(5) N(3) 30.14(19) ? . . . . O(5) Tb(1) O(9) N(4) 103.48(18) ? . . . . O(9) Tb(1) O(5) N(3) -28.04(19) ? . . . . O(5) Tb(1) O(11) N(5) -135.91(17) ? . . . . O(11) Tb(1) O(5) N(3) -124.02(18) ? . . . . O(5) Tb(1) O(12) N(5) 132.30(18) ? . . . . O(12) Tb(1) O(5) N(3) 132.19(18) ? . . . . O(6) Tb(1) O(8) N(4) -81.95(18) ? . . . . O(8) Tb(1) O(6) N(3) -159.28(17) ? . . . . O(6) Tb(1) O(9) N(4) 77.91(17) ? . . . . O(9) Tb(1) O(6) N(3) 147.98(17) ? . . . . O(6) Tb(1) O(11) N(5) 129.83(17) ? . . . . O(11) Tb(1) O(6) N(3) 130.47(17) ? . . . . O(6) Tb(1) O(12) N(5) -129.41(17) ? . . . . O(12) Tb(1) O(6) N(3) -141.68(17) ? . . . . O(8) Tb(1) O(9) N(4) -1.60(16) ? . . . . O(9) Tb(1) O(8) N(4) 1.60(16) ? . . . . O(8) Tb(1) O(11) N(5) 66.47(18) ? . . . . O(11) Tb(1) O(8) N(4) 61.86(18) ? . . . . O(8) Tb(1) O(12) N(5) -111.8(2) ? . . . . O(12) Tb(1) O(8) N(4) 109.50(19) ? . . . . O(9) Tb(1) O(11) N(5) 111.89(19) ? . . . . O(11) Tb(1) O(9) N(4) -113.71(19) ? . . . . O(9) Tb(1) O(12) N(5) -64.85(19) ? . . . . O(12) Tb(1) O(9) N(4) -66.15(18) ? . . . . O(11) Tb(1) O(12) N(5) -2.69(17) ? . . . . O(12) Tb(1) O(11) N(5) 2.68(16) ? . . . . O(1) Cu(1) O(2) Tb(1) -15.55(9) ? . . . . O(1) Cu(1) O(2) C(14) 176.9(2) ? . . . . O(2) Cu(1) O(1) Tb(1) 15.51(9) ? . . . . O(2) Cu(1) O(1) C(1) -169.9(2) ? . . . . O(1) Cu(1) O(14) C(22) -53.4(3) ? . . . . O(14) Cu(1) O(1) Tb(1) -80.89(9) ? . . . . O(14) Cu(1) O(1) C(1) 93.7(2) ? . . . . O(1) Cu(1) N(1) C(7) -1.6(2) ? . . . . O(1) Cu(1) N(1) C(9) 176.3(2) ? . . . . N(1) Cu(1) O(1) Tb(1) -173.99(10) ? . . . . N(1) Cu(1) O(1) C(1) 0.6(2) ? . . . . O(1) Cu(1) N(2) C(11) 161.7(4) ? . . . . O(1) Cu(1) N(2) C(20) -21.3(6) ? . . . . N(2) Cu(1) O(1) Tb(1) 37.5(5) ? . . . . N(2) Cu(1) O(1) C(1) -147.9(4) ? . . . . O(2) Cu(1) O(14) C(22) -133.2(2) ? . . . . O(14) Cu(1) O(2) Tb(1) 87.67(9) ? . . . . O(14) Cu(1) O(2) C(14) -79.8(2) ? . . . . O(2) Cu(1) N(1) C(7) 41.4(5) ? . . . . O(2) Cu(1) N(1) C(9) -140.7(3) ? . . . . N(1) Cu(1) O(2) Tb(1) -59.7(4) ? . . . . N(1) Cu(1) O(2) C(14) 132.8(3) ? . . . . O(2) Cu(1) N(2) C(11) -176.8(2) ? . . . . O(2) Cu(1) N(2) C(20) 0.2(2) ? . . . . N(2) Cu(1) O(2) Tb(1) 168.47(10) ? . . . . N(2) Cu(1) O(2) C(14) 0.9(2) ? . . . . O(14) Cu(1) N(1) C(7) -106.4(2) ? . . . . O(14) Cu(1) N(1) C(9) 71.5(2) ? . . . . N(1) Cu(1) O(14) C(22) 39.4(3) ? . . . . O(14) Cu(1) N(2) C(11) -77.9(2) ? . . . . O(14) Cu(1) N(2) C(20) 99.1(2) ? . . . . N(2) Cu(1) O(14) C(22) 136.2(3) ? . . . . N(1) Cu(1) N(2) C(11) 13.4(2) ? . . . . N(1) Cu(1) N(2) C(20) -169.6(2) ? . . . . N(2) Cu(1) N(1) C(7) 172.7(2) ? . . . . N(2) Cu(1) N(1) C(9) -9.3(2) ? . . . . Tb(1) O(1) C(1) C(2) -8.3(3) ? . . . . Tb(1) O(1) C(1) C(6) 172.5(2) ? . . . . Cu(1) O(1) C(1) C(2) 177.9(2) ? . . . . Cu(1) O(1) C(1) C(6) -1.4(4) ? . . . . Tb(1) O(2) C(14) C(15) 14.3(3) ? . . . . Tb(1) O(2) C(14) C(19) -165.8(2) ? . . . . Cu(1) O(2) C(14) C(15) -179.91(18) ? . . . . Cu(1) O(2) C(14) C(19) 0.0(3) ? . . . . Tb(1) O(3) C(2) C(1) 9.3(3) ? . . . . Tb(1) O(3) C(2) C(3) -169.6(2) ? . . . . C(8) O(3) C(2) C(1) -167.9(2) ? . . . . C(8) O(3) C(2) C(3) 13.1(4) ? . . . . Tb(1) O(4) C(15) C(14) -14.8(3) ? . . . . Tb(1) O(4) C(15) C(16) 164.9(2) ? . . . . C(21) O(4) C(15) C(14) 167.1(2) ? . . . . C(21) O(4) C(15) C(16) -13.2(4) ? . . . . Tb(1) O(5) N(3) O(6) -6.0(2) ? . . . . Tb(1) O(5) N(3) O(7) 173.5(2) ? . . . . Tb(1) O(6) N(3) O(5) 6.1(2) ? . . . . Tb(1) O(6) N(3) O(7) -173.4(2) ? . . . . Tb(1) O(8) N(4) O(9) -2.7(2) ? . . . . Tb(1) O(8) N(4) O(10) 177.2(2) ? . . . . Tb(1) O(9) N(4) O(8) 2.7(2) ? . . . . Tb(1) O(9) N(4) O(10) -177.2(2) ? . . . . Tb(1) O(11) N(5) O(12) -4.5(2) ? . . . . Tb(1) O(11) N(5) O(13) 175.3(2) ? . . . . Tb(1) O(12) N(5) O(11) 4.5(2) ? . . . . Tb(1) O(12) N(5) O(13) -175.2(2) ? . . . . Cu(1) O(14) C(22) C(23) 15.8(4) ? . . . . Cu(1) O(14) C(22) C(24) -163.4(2) ? . . . . Cu(1) N(1) C(7) C(6) 3.6(4) ? . . . . Cu(1) N(1) C(9) C(10) 36.8(3) ? . . . . C(7) N(1) C(9) C(10) -145.0(2) ? . . . . C(9) N(1) C(7) C(6) -174.4(3) ? . . . . Cu(1) N(2) C(11) C(10) -45.3(3) ? . . . . Cu(1) N(2) C(20) C(19) -2.4(4) ? . . . . C(11) N(2) C(20) C(19) 174.7(2) ? . . . . C(20) N(2) C(11) C(10) 137.4(2) ? . . . . O(1) C(1) C(2) O(3) -1.3(4) ? . . . . O(1) C(1) C(2) C(3) 177.7(2) ? . . . . O(1) C(1) C(6) C(5) -177.7(2) ? . . . . O(1) C(1) C(6) C(7) 2.9(4) ? . . . . C(2) C(1) C(6) C(5) 3.1(4) ? . . . . C(2) C(1) C(6) C(7) -176.4(2) ? . . . . C(6) C(1) C(2) O(3) 178.0(2) ? . . . . C(6) C(1) C(2) C(3) -3.0(4) ? . . . . O(3) C(2) C(3) C(4) 179.7(3) ? . . . . C(1) C(2) C(3) C(4) 0.8(4) ? . . . . C(2) C(3) C(4) C(5) 1.4(5) ? . . . . C(3) C(4) C(5) C(6) -1.3(5) ? . . . . C(4) C(5) C(6) C(1) -1.0(4) ? . . . . C(4) C(5) C(6) C(7) 178.5(3) ? . . . . C(1) C(6) C(7) N(1) -4.3(5) ? . . . . C(5) C(6) C(7) N(1) 176.3(3) ? . . . . N(1) C(9) C(10) C(11) -68.8(3) ? . . . . N(1) C(9) C(10) C(12) 175.2(2) ? . . . . N(1) C(9) C(10) C(13) 55.2(3) ? . . . . C(9) C(10) C(11) N(2) 73.9(3) ? . . . . C(12) C(10) C(11) N(2) -170.2(2) ? . . . . C(13) C(10) C(11) N(2) -50.1(3) ? . . . . O(2) C(14) C(15) O(4) 1.3(3) ? . . . . O(2) C(14) C(15) C(16) -178.3(2) ? . . . . O(2) C(14) C(19) C(18) 177.2(2) ? . . . . O(2) C(14) C(19) C(20) -2.4(4) ? . . . . C(15) C(14) C(19) C(18) -2.8(4) ? . . . . C(15) C(14) C(19) C(20) 177.5(2) ? . . . . C(19) C(14) C(15) O(4) -178.6(2) ? . . . . C(19) C(14) C(15) C(16) 1.7(4) ? . . . . O(4) C(15) C(16) C(17) -178.6(2) ? . . . . C(14) C(15) C(16) C(17) 1.0(4) ? . . . . C(15) C(16) C(17) C(18) -2.7(4) ? . . . . C(16) C(17) C(18) C(19) 1.6(5) ? . . . . C(17) C(18) C(19) C(14) 1.2(4) ? . . . . C(17) C(18) C(19) C(20) -179.1(3) ? . . . . C(14) C(19) C(20) N(2) 3.8(5) ? . . . . C(18) C(19) C(20) N(2) -175.9(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(3) C(4) 3.595(4) ? . 3_767 O(7) C(3) 3.014(4) ? . 3_667 O(7) C(4) 3.299(4) ? . 3_667 O(7) C(23) 3.596(4) ? . 1_455 O(8) C(21) 3.477(4) ? . 3_666 O(10) C(9) 3.512(4) ? . 2_746 O(10) C(16) 3.486(3) ? . 3_666 O(10) C(21) 3.517(4) ? . 3_666 O(10) C(24) 3.534(5) ? . 2_746 O(12) C(9) 3.414(4) ? . 4_564 O(13) C(12) 3.270(4) ? . 2_746 N(2) C(5) 3.562(4) ? . 4_564 N(5) C(12) 3.505(4) ? . 2_746 C(2) C(3) 3.555(4) ? . 3_767 C(2) C(4) 3.596(4) ? . 3_767 C(3) O(7) 3.014(4) ? . 3_667 C(3) C(2) 3.555(4) ? . 3_767 C(3) C(3) 3.164(4) ? . 3_767 C(3) C(4) 3.496(4) ? . 3_767 C(4) O(3) 3.595(4) ? . 3_767 C(4) O(7) 3.299(4) ? . 3_667 C(4) C(2) 3.596(4) ? . 3_767 C(4) C(3) 3.496(4) ? . 3_767 C(4) C(11) 3.537(4) ? . 4_565 C(4) C(20) 3.424(4) ? . 4_565 C(5) N(2) 3.562(4) ? . 4_565 C(5) C(20) 3.172(4) ? . 4_565 C(6) C(18) 3.552(4) ? . 4_565 C(9) O(10) 3.512(4) ? . 2_756 C(9) O(12) 3.414(4) ? . 4_565 C(11) C(4) 3.537(4) ? . 4_564 C(12) O(13) 3.270(4) ? . 2_756 C(12) N(5) 3.505(4) ? . 2_756 C(12) C(12) 3.418(4) ? . 3_777 C(13) C(16) 3.390(4) ? . 4_565 C(16) O(10) 3.486(3) ? . 3_666 C(16) C(13) 3.390(4) ? . 4_564 C(18) C(6) 3.552(4) ? . 4_564 C(20) C(4) 3.424(4) ? . 4_564 C(20) C(5) 3.172(4) ? . 4_564 C(21) O(8) 3.477(4) ? . 3_666 C(21) O(10) 3.517(4) ? . 3_666 C(23) O(7) 3.596(4) ? . 1_655 C(24) O(10) 3.534(5) ? . 2_756 O(3) H(2) 3.25(3) ? . 3_767 O(4) H(17) 2.91(4) ? . 4_564 O(4) H(30) 3.424 ? . 1_455 O(5) H(19) 3.04(3) ? . 4_565 O(5) H(27) 2.720 ? . 1_455 O(5) H(28) 3.600 ? . 1_455 O(6) H(11) 3.28(3) ? . 2_646 O(6) H(16) 3.00(3) ? . 2_646 O(6) H(21) 3.22(3) ? . 2_646 O(7) H(1) 2.58(3) ? . 3_667 O(7) H(2) 3.13(3) ? . 3_667 O(7) H(6) 3.19(3) ? . 3_667 O(7) H(11) 2.87(3) ? . 2_646 O(7) H(21) 2.85(3) ? . 2_646 O(7) H(25) 3.505 ? . 1_455 O(7) H(27) 2.843 ? . 1_455 O(8) H(12) 3.31(3) ? . 2_746 O(8) H(13) 3.23(3) ? . 4_564 O(8) H(16) 3.28(3) ? . 2_646 O(8) H(17) 3.11(4) ? . 4_564 O(8) H(24) 2.69(3) ? . 3_666 O(9) H(2) 3.01(3) ? . 3_767 O(9) H(10) 3.09(3) ? . 2_746 O(9) H(12) 3.32(3) ? . 2_746 O(9) H(29) 3.308 ? . 2_746 O(10) H(8) 2.57(3) ? . 2_746 O(10) H(10) 3.22(3) ? . 2_746 O(10) H(12) 3.04(3) ? . 2_746 O(10) H(16) 3.57(3) ? . 2_646 O(10) H(18) 2.54(2) ? . 3_666 O(10) H(23) 3.22(3) ? . 3_666 O(10) H(24) 2.87(3) ? . 3_666 O(10) H(26) 3.537 ? . 2_746 O(10) H(28) 3.159 ? . 2_746 O(10) H(29) 3.307 ? . 2_746 O(11) H(2) 2.89(3) ? . 3_767 O(11) H(12) 3.42(3) ? . 2_746 O(11) H(14) 3.42(3) ? . 2_746 O(12) H(4) 3.17(3) ? . 4_564 O(12) H(9) 2.48(3) ? . 4_564 O(12) H(12) 3.36(3) ? . 2_746 O(12) H(13) 3.10(3) ? . 4_564 O(12) H(17) 2.88(4) ? . 4_564 O(13) H(4) 3.30(3) ? . 4_564 O(13) H(9) 2.83(3) ? . 4_564 O(13) H(12) 3.20(3) ? . 2_746 O(13) H(13) 3.58(3) ? . 2_746 O(13) H(14) 2.50(3) ? . 2_746 O(13) H(23) 2.77(3) ? . 1_655 O(14) H(3) 2.70(3) ? . 4_564 O(14) H(4) 3.14(3) ? . 4_564 N(2) H(3) 3.21(3) ? . 4_564 N(3) H(11) 3.43(3) ? . 2_646 N(3) H(21) 3.41(3) ? . 2_646 N(3) H(27) 3.084 ? . 1_455 N(4) H(8) 3.40(3) ? . 2_746 N(4) H(10) 3.40(3) ? . 2_746 N(4) H(12) 2.96(3) ? . 2_746 N(4) H(16) 3.51(3) ? . 2_646 N(4) H(18) 3.52(2) ? . 3_666 N(4) H(24) 3.15(3) ? . 3_666 N(5) H(4) 3.57(3) ? . 4_564 N(5) H(9) 3.02(3) ? . 4_564 N(5) H(12) 3.08(3) ? . 2_746 N(5) H(13) 3.58(3) ? . 4_564 N(5) H(14) 2.98(3) ? . 2_746 C(1) H(20) 3.23(3) ? . 4_565 C(2) H(1) 3.41(3) ? . 3_767 C(2) H(2) 3.45(3) ? . 3_767 C(2) H(20) 3.35(3) ? . 4_565 C(3) H(1) 3.23(3) ? . 3_767 C(3) H(21) 3.39(3) ? . 4_565 C(4) H(1) 3.38(3) ? . 3_767 C(4) H(7) 2.93(4) ? . 3_767 C(4) H(10) 3.20(3) ? . 4_565 C(4) H(11) 3.09(3) ? . 4_565 C(4) H(21) 2.89(3) ? . 4_565 C(5) H(7) 2.94(4) ? . 3_767 C(5) H(10) 3.27(3) ? . 4_565 C(5) H(11) 3.56(3) ? . 4_565 C(5) H(21) 2.98(3) ? . 4_565 C(5) H(29) 3.475 ? . 4_565 C(6) H(20) 3.34(3) ? . 4_565 C(6) H(21) 3.58(3) ? . 4_565 C(8) H(2) 3.55(3) ? . 3_767 C(8) H(20) 3.18(3) ? . 2_646 C(11) H(2) 3.10(3) ? . 4_564 C(11) H(3) 3.39(3) ? . 4_564 C(12) H(12) 3.09(3) ? . 3_777 C(12) H(13) 2.83(3) ? . 3_777 C(12) H(22) 3.26(3) ? . 2_656 C(12) H(23) 3.35(3) ? . 2_656 C(13) H(18) 3.21(3) ? . 4_565 C(13) H(22) 3.06(3) ? . 2_656 C(13) H(24) 3.10(3) ? . 4_565 C(14) H(28) 3.434 ? . 1_455 C(14) H(30) 3.299 ? . 1_455 C(15) H(15) 3.37(3) ? . 4_564 C(15) H(17) 2.95(4) ? . 4_564 C(15) H(30) 3.023 ? . 1_455 C(16) H(15) 2.86(3) ? . 4_564 C(16) H(17) 3.08(4) ? . 4_564 C(16) H(26) 3.562 ? . 4_464 C(16) H(30) 3.271 ? . 1_455 C(17) H(15) 3.28(3) ? . 4_564 C(17) H(26) 3.173 ? . 4_464 C(17) H(27) 3.398 ? . 4_464 C(18) H(5) 3.27(3) ? . 2_656 C(18) H(6) 3.32(3) ? . 2_656 C(20) H(2) 3.57(3) ? . 4_564 C(20) H(3) 3.14(3) ? . 4_564 C(21) H(13) 3.56(3) ? . 2_646 C(21) H(14) 2.94(3) ? . 2_646 C(21) H(16) 3.20(3) ? . 2_646 C(21) H(17) 3.21(4) ? . 4_564 C(21) H(24) 3.54(3) ? . 3_666 C(22) H(3) 3.38(3) ? . 4_564 C(23) H(19) 2.95(3) ? . 4_665 C(24) H(3) 3.33(3) ? . 4_564 H(1) O(7) 2.58(3) ? . 3_667 H(1) C(2) 3.41(3) ? . 3_767 H(1) C(3) 3.23(3) ? . 3_767 H(1) C(4) 3.38(3) ? . 3_767 H(1) H(1) 3.56(4) ? . 3_767 H(1) H(25) 3.139 ? . 3_767 H(1) H(27) 3.466 ? . 3_767 H(2) O(3) 3.25(3) ? . 3_767 H(2) O(7) 3.13(3) ? . 3_667 H(2) O(9) 3.01(3) ? . 3_767 H(2) O(11) 2.89(3) ? . 3_767 H(2) C(2) 3.45(3) ? . 3_767 H(2) C(8) 3.55(3) ? . 3_767 H(2) C(11) 3.10(3) ? . 4_565 H(2) C(20) 3.57(3) ? . 4_565 H(2) H(7) 2.94(5) ? . 3_767 H(2) H(10) 2.70(4) ? . 4_565 H(2) H(11) 2.63(5) ? . 4_565 H(2) H(21) 3.04(4) ? . 4_565 H(3) O(14) 2.70(3) ? . 4_565 H(3) N(2) 3.21(3) ? . 4_565 H(3) C(11) 3.39(3) ? . 4_565 H(3) C(20) 3.14(3) ? . 4_565 H(3) C(22) 3.38(3) ? . 4_565 H(3) C(24) 3.33(3) ? . 4_565 H(3) H(7) 2.99(5) ? . 3_767 H(3) H(10) 2.82(5) ? . 4_565 H(3) H(11) 3.49(5) ? . 4_565 H(3) H(21) 3.20(5) ? . 4_565 H(3) H(29) 2.645 ? . 4_565 H(4) O(12) 3.17(3) ? . 4_565 H(4) O(13) 3.30(3) ? . 4_565 H(4) O(14) 3.14(3) ? . 4_565 H(4) N(5) 3.57(3) ? . 4_565 H(4) H(29) 3.530 ? . 4_565 H(5) C(18) 3.27(3) ? . 2_646 H(5) H(20) 2.93(5) ? . 2_646 H(5) H(21) 3.22(4) ? . 2_646 H(5) H(29) 3.227 ? . 2_746 H(6) O(7) 3.19(3) ? . 3_667 H(6) C(18) 3.32(3) ? . 2_646 H(6) H(20) 2.74(5) ? . 2_646 H(7) C(4) 2.93(4) ? . 3_767 H(7) C(5) 2.94(4) ? . 3_767 H(7) H(2) 2.94(5) ? . 3_767 H(7) H(3) 2.99(5) ? . 3_767 H(7) H(20) 3.56(5) ? . 2_646 H(7) H(29) 3.135 ? . 2_746 H(8) O(10) 2.57(3) ? . 2_756 H(8) N(4) 3.40(3) ? . 2_756 H(9) O(12) 2.48(3) ? . 4_565 H(9) O(13) 2.83(3) ? . 4_565 H(9) N(5) 3.02(3) ? . 4_565 H(10) O(9) 3.09(3) ? . 2_756 H(10) O(10) 3.22(3) ? . 2_756 H(10) N(4) 3.40(3) ? . 2_756 H(10) C(4) 3.20(3) ? . 4_564 H(10) C(5) 3.27(3) ? . 4_564 H(10) H(2) 2.70(4) ? . 4_564 H(10) H(3) 2.82(5) ? . 4_564 H(11) O(6) 3.28(3) ? . 2_656 H(11) O(7) 2.87(3) ? . 2_656 H(11) N(3) 3.43(3) ? . 2_656 H(11) C(4) 3.09(3) ? . 4_564 H(11) C(5) 3.56(3) ? . 4_564 H(11) H(2) 2.63(5) ? . 4_564 H(11) H(3) 3.49(5) ? . 4_564 H(12) O(8) 3.31(3) ? . 2_756 H(12) O(9) 3.32(3) ? . 2_756 H(12) O(10) 3.04(3) ? . 2_756 H(12) O(11) 3.42(3) ? . 2_756 H(12) O(12) 3.36(3) ? . 2_756 H(12) O(13) 3.20(3) ? . 2_756 H(12) N(4) 2.96(3) ? . 2_756 H(12) N(5) 3.08(3) ? . 2_756 H(12) C(12) 3.09(3) ? . 3_777 H(12) H(12) 3.08(4) ? . 3_777 H(12) H(13) 2.32(4) ? . 3_777 H(12) H(14) 3.48(4) ? . 3_777 H(13) O(8) 3.23(3) ? . 4_565 H(13) O(12) 3.10(3) ? . 4_565 H(13) O(13) 3.58(3) ? . 2_756 H(13) N(5) 3.58(3) ? . 4_565 H(13) C(12) 2.83(3) ? . 3_777 H(13) C(21) 3.56(3) ? . 2_656 H(13) H(12) 2.32(4) ? . 3_777 H(13) H(13) 2.46(5) ? . 3_777 H(13) H(14) 3.26(4) ? . 3_777 H(13) H(22) 3.33(4) ? . 2_656 H(13) H(23) 3.23(5) ? . 2_656 H(14) O(11) 3.42(3) ? . 2_756 H(14) O(13) 2.50(3) ? . 2_756 H(14) N(5) 2.98(3) ? . 2_756 H(14) C(21) 2.94(3) ? . 2_656 H(14) H(12) 3.48(4) ? . 3_777 H(14) H(13) 3.26(4) ? . 3_777 H(14) H(22) 2.55(4) ? . 2_656 H(14) H(23) 2.55(5) ? . 2_656 H(14) H(24) 3.44(5) ? . 2_656 H(15) C(15) 3.37(3) ? . 4_565 H(15) C(16) 2.86(3) ? . 4_565 H(15) C(17) 3.28(3) ? . 4_565 H(15) H(18) 2.72(4) ? . 4_565 H(15) H(19) 3.41(4) ? . 4_565 H(15) H(24) 3.31(5) ? . 4_565 H(16) O(6) 3.00(3) ? . 2_656 H(16) O(8) 3.28(3) ? . 2_656 H(16) O(10) 3.57(3) ? . 2_656 H(16) N(4) 3.51(3) ? . 2_656 H(16) C(21) 3.20(3) ? . 2_656 H(16) H(18) 3.29(4) ? . 4_565 H(16) H(22) 2.34(4) ? . 2_656 H(16) H(24) 3.44(5) ? . 2_656 H(16) H(24) 2.93(5) ? . 4_565 H(17) O(4) 2.91(4) ? . 4_565 H(17) O(8) 3.11(4) ? . 4_565 H(17) O(12) 2.88(4) ? . 4_565 H(17) C(15) 2.95(4) ? . 4_565 H(17) C(16) 3.08(4) ? . 4_565 H(17) C(21) 3.21(4) ? . 4_565 H(17) H(18) 3.03(5) ? . 4_565 H(17) H(22) 3.18(5) ? . 2_656 H(17) H(24) 2.61(5) ? . 4_565 H(18) O(10) 2.54(2) ? . 3_666 H(18) N(4) 3.52(2) ? . 3_666 H(18) C(13) 3.21(3) ? . 4_564 H(18) H(15) 2.72(4) ? . 4_564 H(18) H(16) 3.29(4) ? . 4_564 H(18) H(17) 3.03(5) ? . 4_564 H(18) H(26) 3.272 ? . 4_464 H(19) O(5) 3.04(3) ? . 4_564 H(19) C(23) 2.95(3) ? . 4_464 H(19) H(15) 3.41(4) ? . 4_564 H(19) H(26) 2.551 ? . 4_464 H(19) H(27) 2.500 ? . 4_464 H(19) H(28) 3.113 ? . 4_464 H(20) C(1) 3.23(3) ? . 4_564 H(20) C(2) 3.35(3) ? . 4_564 H(20) C(6) 3.34(3) ? . 4_564 H(20) C(8) 3.18(3) ? . 2_656 H(20) H(5) 2.93(5) ? . 2_656 H(20) H(6) 2.74(5) ? . 2_656 H(20) H(7) 3.56(5) ? . 2_656 H(21) O(6) 3.22(3) ? . 2_656 H(21) O(7) 2.85(3) ? . 2_656 H(21) N(3) 3.41(3) ? . 2_656 H(21) C(3) 3.39(3) ? . 4_564 H(21) C(4) 2.89(3) ? . 4_564 H(21) C(5) 2.98(3) ? . 4_564 H(21) C(6) 3.58(3) ? . 4_564 H(21) H(2) 3.04(4) ? . 4_564 H(21) H(3) 3.20(5) ? . 4_564 H(21) H(5) 3.22(4) ? . 2_656 H(22) C(12) 3.26(3) ? . 2_646 H(22) C(13) 3.06(3) ? . 2_646 H(22) H(13) 3.33(4) ? . 2_646 H(22) H(14) 2.55(4) ? . 2_646 H(22) H(16) 2.34(4) ? . 2_646 H(22) H(17) 3.18(5) ? . 2_646 H(22) H(24) 3.26(5) ? . 3_666 H(23) O(10) 3.22(3) ? . 3_666 H(23) O(13) 2.77(3) ? . 1_455 H(23) C(12) 3.35(3) ? . 2_646 H(23) H(13) 3.23(5) ? . 2_646 H(23) H(14) 2.55(5) ? . 2_646 H(23) H(30) 3.113 ? . 1_455 H(24) O(8) 2.69(3) ? . 3_666 H(24) O(10) 2.87(3) ? . 3_666 H(24) N(4) 3.15(3) ? . 3_666 H(24) C(13) 3.10(3) ? . 4_564 H(24) C(21) 3.54(3) ? . 3_666 H(24) H(14) 3.44(5) ? . 2_646 H(24) H(15) 3.31(5) ? . 4_564 H(24) H(16) 3.44(5) ? . 2_646 H(24) H(16) 2.93(5) ? . 4_564 H(24) H(17) 2.61(5) ? . 4_564 H(24) H(22) 3.26(5) ? . 3_666 H(24) H(24) 3.01(5) ? . 3_666 H(25) O(7) 3.505 ? . 1_655 H(25) H(1) 3.139 ? . 3_767 H(26) O(10) 3.537 ? . 2_756 H(26) C(16) 3.562 ? . 4_665 H(26) C(17) 3.173 ? . 4_665 H(26) H(18) 3.272 ? . 4_665 H(26) H(19) 2.551 ? . 4_665 H(27) O(5) 2.720 ? . 1_655 H(27) O(7) 2.843 ? . 1_655 H(27) N(3) 3.084 ? . 1_655 H(27) C(17) 3.398 ? . 4_665 H(27) H(1) 3.466 ? . 3_767 H(27) H(19) 2.500 ? . 4_665 H(28) O(5) 3.600 ? . 1_655 H(28) O(10) 3.159 ? . 2_756 H(28) C(14) 3.434 ? . 1_655 H(28) H(19) 3.113 ? . 4_665 H(29) O(9) 3.308 ? . 2_756 H(29) O(10) 3.307 ? . 2_756 H(29) C(5) 3.475 ? . 4_564 H(29) H(3) 2.645 ? . 4_564 H(29) H(4) 3.530 ? . 4_564 H(29) H(5) 3.227 ? . 2_756 H(29) H(7) 3.135 ? . 2_756 H(30) O(4) 3.424 ? . 1_655 H(30) C(14) 3.299 ? . 1_655 H(30) C(15) 3.023 ? . 1_655 H(30) C(16) 3.271 ? . 1_655 H(30) H(23) 3.113 ? . 1_655 Tb(1) Cu(1) 3.5177(18) ? . . data___DyCu _database_code_depnum_ccdc_archive 'CCDC 881972' #TrackingRef '11256_web_deposit_cif_file_1_TakayukiIshida_1336987557.DyCu_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Cu Dy N5 O14 ' _chemical_formula_moiety 'C24 H30 Cu Dy N5 O14 ' _chemical_formula_weight 838.57 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.629(8) _cell_length_b 19.843(18) _cell_length_c 15.730(15) _cell_angle_alpha 90.0000 _cell_angle_beta 95.317(11) _cell_angle_gamma 90.0000 _cell_volume 2993(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 270 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664.00 _exptl_absorpt_coefficient_mu 3.268 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.382 _exptl_absorpt_correction_T_max 0.520 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 50987 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_ambient_temperature 100. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6859 _reflns_number_gt 6196 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0529 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6859 _refine_ls_number_parameters 508 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 2.12 _refine_diff_density_min -1.86 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Dy Dy -0.189 4.410 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Dy(1) Dy 0.69736(2) 0.576130(10) 0.744740(10) 0.01531(6) Uani 1.00 1 d . . . Cu(1) Cu 0.79094(5) 0.73830(2) 0.81846(3) 0.01545(11) Uani 1.00 1 d . . . O(1) O 0.7831(3) 0.64574(13) 0.86047(17) 0.0198(7) Uani 1.00 1 d . . . O(2) O 0.6718(2) 0.69388(14) 0.72758(17) 0.0193(6) Uani 1.00 1 d . . . O(3) O 0.7380(3) 0.51739(14) 0.88746(18) 0.0219(7) Uani 1.00 1 d . . . O(4) O 0.5207(2) 0.61348(14) 0.62670(18) 0.0200(7) Uani 1.00 1 d . . . O(5) O 0.4904(3) 0.60170(15) 0.8211(2) 0.0255(8) Uani 1.00 1 d . . . O(6) O 0.4955(3) 0.50488(15) 0.75819(19) 0.0244(7) Uani 1.00 1 d . . . O(7) O 0.3286(3) 0.52701(18) 0.8386(2) 0.0443(11) Uani 1.00 1 d . . . O(8) O 0.6750(3) 0.49561(16) 0.6222(2) 0.0352(9) Uani 1.00 1 d . . . O(9) O 0.7809(3) 0.45591(17) 0.7362(2) 0.0318(8) Uani 1.00 1 d . . . O(10) O 0.7458(3) 0.39074(15) 0.6249(2) 0.0294(8) Uani 1.00 1 d . . . O(11) O 0.9522(3) 0.57194(17) 0.7561(2) 0.0360(10) Uani 1.00 1 d . . . O(12) O 0.8541(3) 0.6124(2) 0.6409(2) 0.0438(10) Uani 1.00 1 d . . . O(13) O 1.0815(3) 0.61327(16) 0.6607(2) 0.0319(9) Uani 1.00 1 d . . . O(14) O 1.0091(3) 0.74454(16) 0.7485(2) 0.0268(8) Uani 1.00 1 d . . . N(1) N 0.8847(3) 0.77067(16) 0.9293(2) 0.0179(8) Uani 1.00 1 d . . . N(2) N 0.7652(3) 0.82770(17) 0.7629(2) 0.0174(8) Uani 1.00 1 d . . . N(3) N 0.4342(3) 0.54451(18) 0.8076(2) 0.0260(9) Uani 1.00 1 d . . . N(4) N 0.7336(3) 0.44560(18) 0.6595(2) 0.0221(9) Uani 1.00 1 d . . . N(5) N 0.9660(4) 0.59915(19) 0.6847(2) 0.0255(9) Uani 1.00 1 d . . . C(1) C 0.8283(4) 0.6214(2) 0.9375(2) 0.0191(9) Uani 1.00 1 d . . . C(2) C 0.8087(4) 0.5529(2) 0.9548(2) 0.0188(9) Uani 1.00 1 d . . . C(3) C 0.8565(4) 0.5242(2) 1.0313(2) 0.0203(10) Uani 1.00 1 d . . . C(4) C 0.9266(4) 0.5642(2) 1.0954(2) 0.0252(11) Uani 1.00 1 d . . . C(5) C 0.9437(4) 0.6313(2) 1.0817(2) 0.0233(10) Uani 1.00 1 d . . . C(6) C 0.8944(4) 0.6615(2) 1.0026(2) 0.0198(9) Uani 1.00 1 d . . . C(7) C 0.9145(4) 0.7330(2) 0.9954(2) 0.0194(9) Uani 1.00 1 d . . . C(8) C 0.6915(5) 0.4503(2) 0.9089(3) 0.0281(12) Uani 1.00 1 d . . . C(9) C 0.9311(4) 0.8417(2) 0.9414(2) 0.0217(10) Uani 1.00 1 d . . . C(10) C 0.8347(4) 0.89322(19) 0.8955(2) 0.0199(9) Uani 1.00 1 d . . . C(11) C 0.8391(4) 0.8869(2) 0.7992(2) 0.0213(10) Uani 1.00 1 d . . . C(12) C 0.8926(5) 0.9629(2) 0.9212(3) 0.0262(11) Uani 1.00 1 d . . . C(13) C 0.6852(4) 0.8860(2) 0.9198(3) 0.0261(11) Uani 1.00 1 d . . . C(14) C 0.6077(3) 0.72281(19) 0.6580(2) 0.0144(8) Uani 1.00 1 d . . . C(15) C 0.5251(4) 0.6801(2) 0.6000(2) 0.0191(9) Uani 1.00 1 d . . . C(16) C 0.4587(4) 0.7046(2) 0.5255(2) 0.0215(10) Uani 1.00 1 d . . . C(17) C 0.4725(4) 0.7723(2) 0.5042(2) 0.0255(11) Uani 1.00 1 d . . . C(18) C 0.5475(4) 0.8150(2) 0.5596(2) 0.0237(10) Uani 1.00 1 d . . . C(19) C 0.6147(4) 0.7905(2) 0.6371(2) 0.0188(9) Uani 1.00 1 d . . . C(20) C 0.6909(4) 0.8384(2) 0.6914(2) 0.0199(10) Uani 1.00 1 d . . . C(21) C 0.4149(5) 0.5721(2) 0.5802(3) 0.0262(12) Uani 1.00 1 d . . . C(22) C 1.1286(4) 0.7300(2) 0.7745(3) 0.0284(11) Uani 1.00 1 d . . . C(23) C 1.1615(4) 0.6881(2) 0.8526(3) 0.0360(13) Uani 1.00 1 d . . . C(24) C 1.2491(5) 0.7558(3) 0.7288(4) 0.0467(17) Uani 1.00 1 d . . . H(1) H 0.845(4) 0.477(2) 1.044(3) 0.029(12) Uiso 1.00 1 d . . . H(2) H 0.964(4) 0.542(2) 1.147(3) 0.027(12) Uiso 1.00 1 d . . . H(3) H 0.991(6) 0.658(3) 1.121(4) 0.058(19) Uiso 1.00 1 d . . . H(4) H 0.957(4) 0.757(2) 1.050(2) 0.017(10) Uiso 1.00 1 d . . . H(5) H 0.631(5) 0.435(2) 0.859(3) 0.020(11) Uiso 1.00 1 d . . . H(6) H 0.625(6) 0.456(3) 0.960(4) 0.062(18) Uiso 1.00 1 d . . . H(7) H 0.771(4) 0.4215(18) 0.922(2) 0.010(10) Uiso 1.00 1 d . . . H(8) H 1.013(4) 0.8444(19) 0.925(2) 0.010(9) Uiso 1.00 1 d . . . H(9) H 0.930(6) 0.852(3) 1.001(4) 0.07(2) Uiso 1.00 1 d . . . H(10) H 0.928(4) 0.883(2) 0.789(2) 0.013(10) Uiso 1.00 1 d . . . H(11) H 0.793(4) 0.925(2) 0.771(3) 0.021(13) Uiso 1.00 1 d . . . H(12) H 0.999(5) 0.967(2) 0.912(3) 0.034(14) Uiso 1.00 1 d . . . H(13) H 0.894(6) 0.973(2) 0.979(4) 0.045(17) Uiso 1.00 1 d . . . H(14) H 0.846(5) 1.000(2) 0.894(3) 0.033(13) Uiso 1.00 1 d . . . H(15) H 0.652(4) 0.839(2) 0.912(2) 0.018(11) Uiso 1.00 1 d . . . H(16) H 0.617(6) 0.918(2) 0.885(3) 0.043(16) Uiso 1.00 1 d . . . H(17) H 0.686(5) 0.896(2) 0.973(3) 0.033(14) Uiso 1.00 1 d . . . H(18) H 0.402(5) 0.678(2) 0.494(3) 0.030(13) Uiso 1.00 1 d . . . H(19) H 0.432(5) 0.793(2) 0.455(3) 0.039(14) Uiso 1.00 1 d . . . H(20) H 0.562(4) 0.863(2) 0.545(2) 0.021(11) Uiso 1.00 1 d . . . H(21) H 0.689(4) 0.886(2) 0.675(3) 0.023(12) Uiso 1.00 1 d . . . H(22) H 0.424(4) 0.529(2) 0.606(3) 0.030(13) Uiso 1.00 1 d . . . H(23) H 0.324(5) 0.598(2) 0.578(3) 0.028(12) Uiso 1.00 1 d . . . H(24) H 0.444(5) 0.565(2) 0.525(3) 0.031(14) Uiso 1.00 1 d . . . H(25) H 1.0868 0.6577 0.8588 0.043 Uiso 1.00 1 c R . . H(26) H 1.1739 0.7165 0.9013 0.043 Uiso 1.00 1 c R . . H(27) H 1.2447 0.6633 0.8474 0.043 Uiso 1.00 1 c R . . H(28) H 1.3280 0.7624 0.7689 0.057 Uiso 1.00 1 c R . . H(29) H 1.2239 0.7974 0.7016 0.057 Uiso 1.00 1 c R . . H(30) H 1.2713 0.7238 0.6872 0.057 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Dy(1) 0.02005(13) 0.01655(12) 0.00907(12) -0.00117(6) -0.00011(8) -0.00132(6) Cu(1) 0.0209(2) 0.0170(2) 0.0079(2) -0.00122(18) -0.00163(18) -0.00105(17) O(1) 0.0315(15) 0.0171(13) 0.0097(13) -0.0016(11) -0.0049(11) -0.0007(10) O(2) 0.0260(14) 0.0215(14) 0.0092(12) -0.0032(11) -0.0055(11) -0.0025(10) O(3) 0.0348(16) 0.0187(13) 0.0117(14) -0.0022(11) -0.0004(11) -0.0001(10) O(4) 0.0229(14) 0.0202(13) 0.0158(14) -0.0039(11) -0.0044(11) -0.0051(11) O(5) 0.0288(16) 0.0239(15) 0.0244(16) -0.0034(12) 0.0060(13) -0.0044(13) O(6) 0.0268(15) 0.0266(15) 0.0205(15) -0.0010(11) 0.0057(12) -0.0045(12) O(7) 0.044(2) 0.041(2) 0.052(2) -0.0152(16) 0.0273(18) -0.0090(18) O(8) 0.054(2) 0.0318(17) 0.0178(16) 0.0166(15) -0.0054(14) -0.0049(13) O(9) 0.0457(19) 0.0330(18) 0.0147(14) 0.0091(14) -0.0080(13) -0.0056(13) O(10) 0.0320(17) 0.0239(15) 0.0315(18) 0.0025(12) -0.0013(14) -0.0133(13) O(11) 0.0286(19) 0.048(2) 0.032(2) 0.0011(14) 0.0031(15) 0.0141(15) O(12) 0.0246(17) 0.087(3) 0.0194(17) -0.0038(18) 0.0001(13) 0.0153(18) O(13) 0.0302(17) 0.0316(17) 0.0362(19) -0.0081(13) 0.0151(14) -0.0131(14) O(14) 0.0234(15) 0.0317(16) 0.0251(16) 0.0020(12) 0.0021(12) -0.0032(13) N(1) 0.0249(17) 0.0204(16) 0.0080(15) -0.0004(13) -0.0009(13) -0.0032(12) N(2) 0.0230(16) 0.0185(15) 0.0108(15) -0.0013(13) 0.0017(12) -0.0011(12) N(3) 0.0290(19) 0.0265(19) 0.0234(19) -0.0009(15) 0.0074(15) -0.0004(15) N(4) 0.0234(18) 0.0247(17) 0.0182(18) -0.0017(14) 0.0023(14) -0.0052(14) N(5) 0.032(2) 0.0246(18) 0.0206(19) -0.0032(15) 0.0081(15) -0.0083(15) C(1) 0.021(2) 0.028(2) 0.0075(17) 0.0031(15) -0.0004(14) 0.0005(15) C(2) 0.024(2) 0.0222(19) 0.0107(18) 0.0011(15) 0.0019(15) -0.0011(15) C(3) 0.027(2) 0.023(2) 0.0112(19) 0.0070(16) 0.0035(15) 0.0033(15) C(4) 0.031(2) 0.036(2) 0.0095(19) 0.0075(18) 0.0023(17) 0.0054(17) C(5) 0.029(2) 0.031(2) 0.0105(19) 0.0038(18) 0.0021(16) -0.0034(16) C(6) 0.024(2) 0.026(2) 0.0096(18) 0.0036(16) -0.0010(15) -0.0033(15) C(7) 0.0203(19) 0.027(2) 0.0101(18) -0.0005(15) -0.0032(15) -0.0034(15) C(8) 0.038(2) 0.023(2) 0.023(2) -0.0057(19) 0.002(2) 0.0036(18) C(9) 0.025(2) 0.0196(19) 0.020(2) -0.0049(16) 0.0006(17) -0.0018(16) C(10) 0.026(2) 0.0168(18) 0.017(2) -0.0042(15) 0.0016(16) -0.0040(15) C(11) 0.025(2) 0.021(2) 0.017(2) -0.0070(16) 0.0014(16) -0.0010(16) C(12) 0.034(2) 0.018(2) 0.027(2) -0.0069(17) 0.0043(19) -0.0044(17) C(13) 0.028(2) 0.025(2) 0.026(2) -0.0026(17) 0.0072(19) -0.0062(18) C(14) 0.0154(18) 0.0181(17) 0.0087(17) 0.0019(13) -0.0038(13) -0.0000(13) C(15) 0.0217(19) 0.0236(19) 0.0122(18) 0.0009(15) 0.0027(15) 0.0006(15) C(16) 0.020(2) 0.027(2) 0.017(2) -0.0024(16) -0.0060(16) -0.0045(16) C(17) 0.024(2) 0.031(2) 0.019(2) 0.0046(17) -0.0093(17) 0.0013(17) C(18) 0.025(2) 0.025(2) 0.020(2) 0.0040(16) -0.0055(17) 0.0057(16) C(19) 0.024(2) 0.0245(19) 0.0077(17) 0.0032(15) -0.0009(15) 0.0031(15) C(20) 0.025(2) 0.0200(19) 0.0147(19) -0.0001(15) 0.0003(15) 0.0007(15) C(21) 0.028(2) 0.024(2) 0.024(2) -0.0073(17) -0.0102(19) -0.0049(17) C(22) 0.026(2) 0.026(2) 0.033(2) -0.0033(17) 0.0045(19) -0.0131(18) C(23) 0.024(2) 0.050(3) 0.033(2) 0.007(2) -0.0012(19) -0.006(2) C(24) 0.037(3) 0.044(3) 0.062(4) -0.001(2) 0.019(2) -0.001(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Dy(1) O(1) 2.372(2) yes . . Dy(1) O(2) 2.362(2) yes . . Dy(1) O(3) 2.528(2) yes . . Dy(1) O(4) 2.511(2) yes . . Dy(1) O(5) 2.473(3) yes . . Dy(1) O(6) 2.429(2) yes . . Dy(1) O(8) 2.498(3) yes . . Dy(1) O(9) 2.525(3) yes . . Dy(1) O(11) 2.445(3) yes . . Dy(1) O(12) 2.433(3) yes . . Cu(1) O(1) 1.956(2) yes . . Cu(1) O(2) 1.958(2) yes . . Cu(1) O(14) 2.463(3) yes . . Cu(1) N(1) 1.994(3) yes . . Cu(1) N(2) 1.983(3) yes . . O(1) C(1) 1.339(4) yes . . O(2) C(14) 1.336(4) yes . . O(3) C(2) 1.395(4) yes . . O(3) C(8) 1.453(5) yes . . O(4) C(15) 1.388(4) yes . . O(4) C(21) 1.452(5) yes . . O(5) N(3) 1.267(4) yes . . O(6) N(3) 1.287(4) yes . . O(7) N(3) 1.219(5) yes . . O(8) N(4) 1.259(4) yes . . O(9) N(4) 1.267(4) yes . . O(10) N(4) 1.228(4) yes . . O(11) N(5) 1.265(5) yes . . O(12) N(5) 1.252(4) yes . . O(13) N(5) 1.239(5) yes . . O(14) C(22) 1.220(5) yes . . N(1) C(7) 1.291(5) yes . . N(1) C(9) 1.486(5) yes . . N(2) C(11) 1.462(5) yes . . N(2) C(20) 1.294(4) yes . . C(1) C(2) 1.404(5) yes . . C(1) C(6) 1.402(5) yes . . C(2) C(3) 1.373(5) yes . . C(3) C(4) 1.405(5) yes . . C(4) C(5) 1.361(6) yes . . C(5) C(6) 1.423(5) yes . . C(6) C(7) 1.439(5) yes . . C(9) C(10) 1.517(5) yes . . C(10) C(11) 1.524(6) yes . . C(10) C(12) 1.531(5) yes . . C(10) C(13) 1.531(6) yes . . C(14) C(15) 1.432(5) yes . . C(14) C(19) 1.386(5) yes . . C(15) C(16) 1.372(5) yes . . C(16) C(17) 1.395(6) yes . . C(17) C(18) 1.372(6) yes . . C(18) C(19) 1.413(5) yes . . C(19) C(20) 1.433(5) yes . . C(22) C(23) 1.493(7) yes . . C(22) C(24) 1.510(7) yes . . C(3) H(1) 0.97(4) no . . C(4) H(2) 0.96(4) no . . C(5) H(3) 0.91(6) no . . C(7) H(4) 1.03(4) no . . C(8) H(5) 0.98(4) no . . C(8) H(6) 1.07(7) no . . C(8) H(7) 0.96(4) no . . C(9) H(8) 0.85(4) no . . C(9) H(9) 0.96(7) no . . C(11) H(10) 0.89(4) no . . C(11) H(11) 0.97(4) no . . C(12) H(12) 1.05(5) no . . C(12) H(13) 0.93(6) no . . C(12) H(14) 0.95(4) no . . C(13) H(15) 0.98(4) no . . C(13) H(16) 1.03(5) no . . C(13) H(17) 0.86(5) no . . C(16) H(18) 0.89(4) no . . C(17) H(19) 0.93(5) no . . C(18) H(20) 0.98(4) no . . C(20) H(21) 0.98(4) no . . C(21) H(22) 0.95(5) no . . C(21) H(23) 1.02(5) no . . C(21) H(24) 0.94(5) no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Dy(1) O(2) 62.41(8) yes . . . O(1) Dy(1) O(3) 64.69(8) yes . . . O(1) Dy(1) O(4) 124.02(9) yes . . . O(1) Dy(1) O(5) 75.30(9) yes . . . O(1) Dy(1) O(6) 119.77(9) yes . . . O(1) Dy(1) O(8) 164.57(10) yes . . . O(1) Dy(1) O(9) 120.07(9) yes . . . O(1) Dy(1) O(11) 71.83(11) yes . . . O(1) Dy(1) O(12) 98.62(11) yes . . . O(2) Dy(1) O(3) 124.29(9) yes . . . O(2) Dy(1) O(4) 64.36(8) yes . . . O(2) Dy(1) O(5) 76.85(9) yes . . . O(2) Dy(1) O(6) 120.66(9) yes . . . O(2) Dy(1) O(8) 122.94(9) yes . . . O(2) Dy(1) O(9) 163.48(10) yes . . . O(2) Dy(1) O(11) 97.77(10) yes . . . O(2) Dy(1) O(12) 72.27(12) yes . . . O(3) Dy(1) O(4) 146.25(9) yes . . . O(3) Dy(1) O(5) 74.24(9) yes . . . O(3) Dy(1) O(6) 73.35(9) yes . . . O(3) Dy(1) O(8) 112.70(9) yes . . . O(3) Dy(1) O(9) 65.66(9) yes . . . O(3) Dy(1) O(11) 81.24(11) yes . . . O(3) Dy(1) O(12) 132.69(10) yes . . . O(4) Dy(1) O(5) 77.16(9) yes . . . O(4) Dy(1) O(6) 75.14(9) yes . . . O(4) Dy(1) O(8) 67.29(10) yes . . . O(4) Dy(1) O(9) 115.90(9) yes . . . O(4) Dy(1) O(11) 132.10(11) yes . . . O(4) Dy(1) O(12) 80.56(10) yes . . . O(5) Dy(1) O(6) 52.39(9) yes . . . O(5) Dy(1) O(8) 119.39(10) yes . . . O(5) Dy(1) O(9) 119.65(10) yes . . . O(5) Dy(1) O(11) 145.06(11) yes . . . O(5) Dy(1) O(12) 147.50(11) yes . . . O(6) Dy(1) O(8) 71.50(10) yes . . . O(6) Dy(1) O(9) 73.51(10) yes . . . O(6) Dy(1) O(11) 141.23(10) yes . . . O(6) Dy(1) O(12) 141.43(11) yes . . . O(8) Dy(1) O(9) 50.19(10) yes . . . O(8) Dy(1) O(11) 92.79(12) yes . . . O(8) Dy(1) O(12) 71.65(12) yes . . . O(9) Dy(1) O(11) 69.47(11) yes . . . O(9) Dy(1) O(12) 91.32(12) yes . . . O(11) Dy(1) O(12) 51.57(11) yes . . . O(1) Cu(1) O(2) 77.62(11) yes . . . O(1) Cu(1) O(14) 105.05(11) yes . . . O(1) Cu(1) N(1) 92.04(12) yes . . . O(1) Cu(1) N(2) 169.09(12) yes . . . O(2) Cu(1) O(14) 99.36(11) yes . . . O(2) Cu(1) N(1) 166.12(12) yes . . . O(2) Cu(1) N(2) 92.30(12) yes . . . O(14) Cu(1) N(1) 92.21(12) yes . . . O(14) Cu(1) N(2) 80.50(12) yes . . . N(1) Cu(1) N(2) 97.18(12) yes . . . Dy(1) O(1) Cu(1) 108.00(11) yes . . . Dy(1) O(1) C(1) 123.1(2) yes . . . Cu(1) O(1) C(1) 128.6(2) yes . . . Dy(1) O(2) Cu(1) 108.30(11) yes . . . Dy(1) O(2) C(14) 123.7(2) yes . . . Cu(1) O(2) C(14) 126.9(2) yes . . . Dy(1) O(3) C(2) 117.8(2) yes . . . Dy(1) O(3) C(8) 127.0(2) yes . . . C(2) O(3) C(8) 115.2(3) yes . . . Dy(1) O(4) C(15) 117.9(2) yes . . . Dy(1) O(4) C(21) 127.0(2) yes . . . C(15) O(4) C(21) 115.1(3) yes . . . Dy(1) O(5) N(3) 94.9(2) yes . . . Dy(1) O(6) N(3) 96.5(2) yes . . . Dy(1) O(8) N(4) 98.1(2) yes . . . Dy(1) O(9) N(4) 96.6(2) yes . . . Dy(1) O(11) N(5) 96.2(2) yes . . . Dy(1) O(12) N(5) 97.2(2) yes . . . Cu(1) O(14) C(22) 131.0(3) yes . . . Cu(1) N(1) C(7) 124.5(2) yes . . . Cu(1) N(1) C(9) 121.6(2) yes . . . C(7) N(1) C(9) 113.8(3) yes . . . Cu(1) N(2) C(11) 120.7(2) yes . . . Cu(1) N(2) C(20) 124.5(2) yes . . . C(11) N(2) C(20) 114.7(3) yes . . . O(5) N(3) O(6) 115.8(3) yes . . . O(5) N(3) O(7) 123.2(3) yes . . . O(6) N(3) O(7) 120.9(3) yes . . . O(8) N(4) O(9) 115.0(3) yes . . . O(8) N(4) O(10) 123.3(3) yes . . . O(9) N(4) O(10) 121.7(3) yes . . . O(11) N(5) O(12) 115.0(3) yes . . . O(11) N(5) O(13) 122.6(3) yes . . . O(12) N(5) O(13) 122.4(3) yes . . . O(1) C(1) C(2) 119.1(3) yes . . . O(1) C(1) C(6) 123.0(3) yes . . . C(2) C(1) C(6) 117.9(3) yes . . . O(3) C(2) C(1) 114.0(3) yes . . . O(3) C(2) C(3) 123.9(3) yes . . . C(1) C(2) C(3) 122.1(3) yes . . . C(2) C(3) C(4) 119.7(3) yes . . . C(3) C(4) C(5) 119.7(3) yes . . . C(4) C(5) C(6) 121.0(3) yes . . . C(1) C(6) C(5) 119.5(3) yes . . . C(1) C(6) C(7) 123.8(3) yes . . . C(5) C(6) C(7) 116.7(3) yes . . . N(1) C(7) C(6) 127.8(3) yes . . . N(1) C(9) C(10) 114.5(3) yes . . . C(9) C(10) C(11) 110.2(3) yes . . . C(9) C(10) C(12) 106.9(3) yes . . . C(9) C(10) C(13) 111.5(3) yes . . . C(11) C(10) C(12) 107.1(3) yes . . . C(11) C(10) C(13) 110.8(3) yes . . . C(12) C(10) C(13) 110.2(3) yes . . . N(2) C(11) C(10) 113.4(3) yes . . . O(2) C(14) C(15) 117.1(3) yes . . . O(2) C(14) C(19) 125.6(3) yes . . . C(15) C(14) C(19) 117.3(3) yes . . . O(4) C(15) C(14) 113.7(3) yes . . . O(4) C(15) C(16) 124.8(3) yes . . . C(14) C(15) C(16) 121.5(3) yes . . . C(15) C(16) C(17) 120.0(3) yes . . . C(16) C(17) C(18) 119.9(4) yes . . . C(17) C(18) C(19) 120.5(3) yes . . . C(14) C(19) C(18) 120.6(3) yes . . . C(14) C(19) C(20) 122.3(3) yes . . . C(18) C(19) C(20) 117.0(3) yes . . . N(2) C(20) C(19) 128.4(3) yes . . . O(14) C(22) C(23) 122.0(4) yes . . . O(14) C(22) C(24) 120.2(4) yes . . . C(23) C(22) C(24) 117.8(4) yes . . . C(2) C(3) H(1) 123(2) no . . . C(4) C(3) H(1) 117(2) no . . . C(3) C(4) H(2) 118(2) no . . . C(5) C(4) H(2) 122(2) no . . . C(4) C(5) H(3) 122(3) no . . . C(6) C(5) H(3) 117(3) no . . . N(1) C(7) H(4) 116(2) no . . . C(6) C(7) H(4) 116(2) no . . . O(3) C(8) H(5) 106(2) no . . . O(3) C(8) H(6) 107(3) no . . . O(3) C(8) H(7) 110(2) no . . . H(5) C(8) H(6) 106(4) no . . . H(5) C(8) H(7) 113(3) no . . . H(6) C(8) H(7) 115(4) no . . . N(1) C(9) H(8) 107(2) no . . . N(1) C(9) H(9) 107(4) no . . . C(10) C(9) H(8) 111(2) no . . . C(10) C(9) H(9) 105(3) no . . . H(8) C(9) H(9) 113(4) no . . . N(2) C(11) H(10) 108(2) no . . . N(2) C(11) H(11) 105(2) no . . . C(10) C(11) H(10) 107(2) no . . . C(10) C(11) H(11) 110(3) no . . . H(10) C(11) H(11) 114(3) no . . . C(10) C(12) H(12) 111(2) no . . . C(10) C(12) H(13) 115(3) no . . . C(10) C(12) H(14) 116(2) no . . . H(12) C(12) H(13) 101(4) no . . . H(12) C(12) H(14) 108(4) no . . . H(13) C(12) H(14) 104(4) no . . . C(10) C(13) H(15) 111(2) no . . . C(10) C(13) H(16) 112(3) no . . . C(10) C(13) H(17) 107(3) no . . . H(15) C(13) H(16) 109(3) no . . . H(15) C(13) H(17) 109(4) no . . . H(16) C(13) H(17) 109(4) no . . . C(15) C(16) H(18) 119(3) no . . . C(17) C(16) H(18) 121(3) no . . . C(16) C(17) H(19) 126(3) no . . . C(18) C(17) H(19) 114(3) no . . . C(17) C(18) H(20) 122(2) no . . . C(19) C(18) H(20) 118(2) no . . . N(2) C(20) H(21) 113(2) no . . . C(19) C(20) H(21) 119(2) no . . . O(4) C(21) H(22) 105(2) no . . . O(4) C(21) H(23) 107(2) no . . . O(4) C(21) H(24) 107(3) no . . . H(22) C(21) H(23) 122(4) no . . . H(22) C(21) H(24) 104(4) no . . . H(23) C(21) H(24) 111(4) no . . . C(22) C(23) H(25) 109.5 no . . . C(22) C(23) H(26) 109.5 no . . . C(22) C(23) H(27) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . H(25) C(23) H(27) 109.5 no . . . H(26) C(23) H(27) 109.5 no . . . C(22) C(24) H(28) 109.5 no . . . C(22) C(24) H(29) 109.5 no . . . C(22) C(24) H(30) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . H(28) C(24) H(30) 109.5 no . . . H(29) C(24) H(30) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Dy(1) O(2) Cu(1) 14.14(11) ? . . . . O(1) Dy(1) O(2) C(14) -177.5(3) ? . . . . O(2) Dy(1) O(1) Cu(1) -14.13(11) ? . . . . O(2) Dy(1) O(1) C(1) 171.4(3) ? . . . . O(1) Dy(1) O(3) C(2) -10.0(2) ? . . . . O(1) Dy(1) O(3) C(8) 167.8(3) ? . . . . O(3) Dy(1) O(1) Cu(1) -176.00(16) ? . . . . O(3) Dy(1) O(1) C(1) 9.5(2) ? . . . . O(1) Dy(1) O(4) C(15) 34.8(2) ? . . . . O(1) Dy(1) O(4) C(21) -147.4(3) ? . . . . O(4) Dy(1) O(1) Cu(1) -33.77(17) ? . . . . O(4) Dy(1) O(1) C(1) 151.7(2) ? . . . . O(1) Dy(1) O(5) N(3) -144.5(2) ? . . . . O(5) Dy(1) O(1) Cu(1) -96.76(13) ? . . . . O(5) Dy(1) O(1) C(1) 88.7(2) ? . . . . O(1) Dy(1) O(6) N(3) 32.3(2) ? . . . . O(6) Dy(1) O(1) Cu(1) -125.48(12) ? . . . . O(6) Dy(1) O(1) C(1) 60.0(3) ? . . . . O(1) Dy(1) O(8) N(4) 56.8(4) ? . . . . O(8) Dy(1) O(1) Cu(1) 100.3(3) ? . . . . O(8) Dy(1) O(1) C(1) -74.2(4) ? . . . . O(1) Dy(1) O(9) N(4) -166.8(2) ? . . . . O(9) Dy(1) O(1) Cu(1) 147.20(12) ? . . . . O(9) Dy(1) O(1) C(1) -27.3(3) ? . . . . O(1) Dy(1) O(11) N(5) -115.7(2) ? . . . . O(11) Dy(1) O(1) Cu(1) 95.26(14) ? . . . . O(11) Dy(1) O(1) C(1) -79.2(2) ? . . . . O(1) Dy(1) O(12) N(5) 56.6(2) ? . . . . O(12) Dy(1) O(1) Cu(1) 50.61(15) ? . . . . O(12) Dy(1) O(1) C(1) -123.9(2) ? . . . . O(2) Dy(1) O(3) C(2) -29.5(3) ? . . . . O(2) Dy(1) O(3) C(8) 148.4(3) ? . . . . O(3) Dy(1) O(2) Cu(1) 34.04(17) ? . . . . O(3) Dy(1) O(2) C(14) -157.6(2) ? . . . . O(2) Dy(1) O(4) C(15) 15.5(2) ? . . . . O(2) Dy(1) O(4) C(21) -166.7(3) ? . . . . O(4) Dy(1) O(2) Cu(1) 176.13(16) ? . . . . O(4) Dy(1) O(2) C(14) -15.5(2) ? . . . . O(2) Dy(1) O(5) N(3) 151.0(2) ? . . . . O(5) Dy(1) O(2) Cu(1) 94.23(13) ? . . . . O(5) Dy(1) O(2) C(14) -97.4(2) ? . . . . O(2) Dy(1) O(6) N(3) -41.4(2) ? . . . . O(6) Dy(1) O(2) Cu(1) 124.10(12) ? . . . . O(6) Dy(1) O(2) C(14) -67.5(3) ? . . . . O(2) Dy(1) O(8) N(4) 162.7(2) ? . . . . O(8) Dy(1) O(2) Cu(1) -149.08(12) ? . . . . O(8) Dy(1) O(2) C(14) 19.3(3) ? . . . . O(2) Dy(1) O(9) N(4) -72.7(4) ? . . . . O(9) Dy(1) O(2) Cu(1) -89.0(3) ? . . . . O(9) Dy(1) O(2) C(14) 79.4(4) ? . . . . O(2) Dy(1) O(11) N(5) -58.1(2) ? . . . . O(11) Dy(1) O(2) Cu(1) -50.63(15) ? . . . . O(11) Dy(1) O(2) C(14) 117.8(2) ? . . . . O(2) Dy(1) O(12) N(5) 113.9(2) ? . . . . O(12) Dy(1) O(2) Cu(1) -96.02(14) ? . . . . O(12) Dy(1) O(2) C(14) 72.4(2) ? . . . . O(3) Dy(1) O(4) C(15) 129.5(2) ? . . . . O(3) Dy(1) O(4) C(21) -52.7(3) ? . . . . O(4) Dy(1) O(3) C(2) -123.9(2) ? . . . . O(4) Dy(1) O(3) C(8) 53.9(3) ? . . . . O(3) Dy(1) O(5) N(3) -77.2(2) ? . . . . O(5) Dy(1) O(3) C(2) -90.9(2) ? . . . . O(5) Dy(1) O(3) C(8) 87.0(3) ? . . . . O(3) Dy(1) O(6) N(3) 79.0(2) ? . . . . O(6) Dy(1) O(3) C(2) -145.6(2) ? . . . . O(6) Dy(1) O(3) C(8) 32.2(3) ? . . . . O(3) Dy(1) O(8) N(4) -20.1(2) ? . . . . O(8) Dy(1) O(3) C(2) 153.4(2) ? . . . . O(8) Dy(1) O(3) C(8) -28.8(3) ? . . . . O(3) Dy(1) O(9) N(4) 156.8(2) ? . . . . O(9) Dy(1) O(3) C(2) 135.4(2) ? . . . . O(9) Dy(1) O(3) C(8) -46.8(3) ? . . . . O(3) Dy(1) O(11) N(5) 178.2(2) ? . . . . O(11) Dy(1) O(3) C(2) 64.0(2) ? . . . . O(11) Dy(1) O(3) C(8) -118.2(3) ? . . . . O(3) Dy(1) O(12) N(5) -6.7(3) ? . . . . O(12) Dy(1) O(3) C(2) 67.9(3) ? . . . . O(12) Dy(1) O(3) C(8) -114.3(3) ? . . . . O(4) Dy(1) O(5) N(3) 84.7(2) ? . . . . O(5) Dy(1) O(4) C(15) 96.9(2) ? . . . . O(5) Dy(1) O(4) C(21) -85.2(3) ? . . . . O(4) Dy(1) O(6) N(3) -88.7(2) ? . . . . O(6) Dy(1) O(4) C(15) 151.0(2) ? . . . . O(6) Dy(1) O(4) C(21) -31.2(3) ? . . . . O(4) Dy(1) O(8) N(4) -163.4(2) ? . . . . O(8) Dy(1) O(4) C(15) -133.2(2) ? . . . . O(8) Dy(1) O(4) C(21) 44.6(3) ? . . . . O(4) Dy(1) O(9) N(4) 14.2(2) ? . . . . O(9) Dy(1) O(4) C(15) -146.1(2) ? . . . . O(9) Dy(1) O(4) C(21) 31.7(3) ? . . . . O(4) Dy(1) O(11) N(5) 4.1(3) ? . . . . O(11) Dy(1) O(4) C(15) -61.1(3) ? . . . . O(11) Dy(1) O(4) C(21) 116.7(3) ? . . . . O(4) Dy(1) O(12) N(5) 179.89(19) ? . . . . O(12) Dy(1) O(4) C(15) -59.2(2) ? . . . . O(12) Dy(1) O(4) C(21) 118.6(3) ? . . . . O(5) Dy(1) O(6) N(3) -3.6(2) ? . . . . O(6) Dy(1) O(5) N(3) 3.7(2) ? . . . . O(5) Dy(1) O(8) N(4) -104.2(2) ? . . . . O(8) Dy(1) O(5) N(3) 30.3(2) ? . . . . O(5) Dy(1) O(9) N(4) 103.7(2) ? . . . . O(9) Dy(1) O(5) N(3) -28.0(2) ? . . . . O(5) Dy(1) O(11) N(5) -136.3(2) ? . . . . O(11) Dy(1) O(5) N(3) -124.3(2) ? . . . . O(5) Dy(1) O(12) N(5) 132.8(2) ? . . . . O(12) Dy(1) O(5) N(3) 132.6(2) ? . . . . O(6) Dy(1) O(8) N(4) -82.2(2) ? . . . . O(8) Dy(1) O(6) N(3) -159.3(2) ? . . . . O(6) Dy(1) O(9) N(4) 78.0(2) ? . . . . O(9) Dy(1) O(6) N(3) 147.9(2) ? . . . . O(6) Dy(1) O(11) N(5) 129.1(2) ? . . . . O(11) Dy(1) O(6) N(3) 130.3(2) ? . . . . O(6) Dy(1) O(12) N(5) -128.8(2) ? . . . . O(12) Dy(1) O(6) N(3) -141.5(2) ? . . . . O(8) Dy(1) O(9) N(4) -1.4(2) ? . . . . O(9) Dy(1) O(8) N(4) 1.4(2) ? . . . . O(8) Dy(1) O(11) N(5) 65.7(2) ? . . . . O(11) Dy(1) O(8) N(4) 61.6(2) ? . . . . O(8) Dy(1) O(12) N(5) -111.0(2) ? . . . . O(12) Dy(1) O(8) N(4) 109.4(2) ? . . . . O(9) Dy(1) O(11) N(5) 111.0(2) ? . . . . O(11) Dy(1) O(9) N(4) -113.7(2) ? . . . . O(9) Dy(1) O(12) N(5) -64.1(2) ? . . . . O(12) Dy(1) O(9) N(4) -66.0(2) ? . . . . O(11) Dy(1) O(12) N(5) -1.8(2) ? . . . . O(12) Dy(1) O(11) N(5) 1.8(2) ? . . . . O(1) Cu(1) O(2) Dy(1) -15.59(12) ? . . . . O(1) Cu(1) O(2) C(14) 176.5(3) ? . . . . O(2) Cu(1) O(1) Dy(1) 15.50(12) ? . . . . O(2) Cu(1) O(1) C(1) -170.4(3) ? . . . . O(1) Cu(1) O(14) C(22) -52.8(3) ? . . . . O(14) Cu(1) O(1) Dy(1) -81.01(13) ? . . . . O(14) Cu(1) O(1) C(1) 93.1(3) ? . . . . O(1) Cu(1) N(1) C(7) -1.2(3) ? . . . . O(1) Cu(1) N(1) C(9) 176.7(3) ? . . . . N(1) Cu(1) O(1) Dy(1) -173.86(14) ? . . . . N(1) Cu(1) O(1) C(1) 0.2(3) ? . . . . O(1) Cu(1) N(2) C(11) 161.2(5) ? . . . . O(1) Cu(1) N(2) C(20) -22.8(9) ? . . . . N(2) Cu(1) O(1) Dy(1) 38.4(7) ? . . . . N(2) Cu(1) O(1) C(1) -147.5(6) ? . . . . O(2) Cu(1) O(14) C(22) -132.4(3) ? . . . . O(14) Cu(1) O(2) Dy(1) 87.89(12) ? . . . . O(14) Cu(1) O(2) C(14) -80.0(3) ? . . . . O(2) Cu(1) N(1) C(7) 40.2(7) ? . . . . O(2) Cu(1) N(1) C(9) -141.9(4) ? . . . . N(1) Cu(1) O(2) Dy(1) -58.2(5) ? . . . . N(1) Cu(1) O(2) C(14) 133.9(5) ? . . . . O(2) Cu(1) N(2) C(11) -176.5(3) ? . . . . O(2) Cu(1) N(2) C(20) -0.4(3) ? . . . . N(2) Cu(1) O(2) Dy(1) 168.64(13) ? . . . . N(2) Cu(1) O(2) C(14) 0.7(3) ? . . . . O(14) Cu(1) N(1) C(7) -106.4(3) ? . . . . O(14) Cu(1) N(1) C(9) 71.5(3) ? . . . . N(1) Cu(1) O(14) C(22) 39.9(3) ? . . . . O(14) Cu(1) N(2) C(11) -77.4(3) ? . . . . O(14) Cu(1) N(2) C(20) 98.7(3) ? . . . . N(2) Cu(1) O(14) C(22) 136.8(3) ? . . . . N(1) Cu(1) N(2) C(11) 13.7(3) ? . . . . N(1) Cu(1) N(2) C(20) -170.3(3) ? . . . . N(2) Cu(1) N(1) C(7) 173.0(3) ? . . . . N(2) Cu(1) N(1) C(9) -9.2(3) ? . . . . Dy(1) O(1) C(1) C(2) -8.3(5) ? . . . . Dy(1) O(1) C(1) C(6) 172.0(2) ? . . . . Cu(1) O(1) C(1) C(2) 178.4(2) ? . . . . Cu(1) O(1) C(1) C(6) -1.3(5) ? . . . . Dy(1) O(2) C(14) C(15) 13.9(4) ? . . . . Dy(1) O(2) C(14) C(19) -165.8(3) ? . . . . Cu(1) O(2) C(14) C(15) -179.9(2) ? . . . . Cu(1) O(2) C(14) C(19) 0.3(5) ? . . . . Dy(1) O(3) C(2) C(1) 9.9(4) ? . . . . Dy(1) O(3) C(2) C(3) -169.6(3) ? . . . . C(8) O(3) C(2) C(1) -168.1(3) ? . . . . C(8) O(3) C(2) C(3) 12.3(5) ? . . . . Dy(1) O(4) C(15) C(14) -15.0(4) ? . . . . Dy(1) O(4) C(15) C(16) 164.8(3) ? . . . . C(21) O(4) C(15) C(14) 167.0(3) ? . . . . C(21) O(4) C(15) C(16) -13.3(5) ? . . . . Dy(1) O(5) N(3) O(6) -6.1(3) ? . . . . Dy(1) O(5) N(3) O(7) 174.0(3) ? . . . . Dy(1) O(6) N(3) O(5) 6.3(3) ? . . . . Dy(1) O(6) N(3) O(7) -173.9(3) ? . . . . Dy(1) O(8) N(4) O(9) -2.4(3) ? . . . . Dy(1) O(8) N(4) O(10) 178.1(3) ? . . . . Dy(1) O(9) N(4) O(8) 2.4(3) ? . . . . Dy(1) O(9) N(4) O(10) -178.2(3) ? . . . . Dy(1) O(11) N(5) O(12) -3.1(3) ? . . . . Dy(1) O(11) N(5) O(13) 175.2(3) ? . . . . Dy(1) O(12) N(5) O(11) 3.1(4) ? . . . . Dy(1) O(12) N(5) O(13) -175.1(3) ? . . . . Cu(1) O(14) C(22) C(23) 15.3(6) ? . . . . Cu(1) O(14) C(22) C(24) -163.2(3) ? . . . . Cu(1) N(1) C(7) C(6) 3.4(6) ? . . . . Cu(1) N(1) C(9) C(10) 36.4(4) ? . . . . C(7) N(1) C(9) C(10) -145.5(3) ? . . . . C(9) N(1) C(7) C(6) -174.6(4) ? . . . . Cu(1) N(2) C(11) C(10) -45.5(4) ? . . . . Cu(1) N(2) C(20) C(19) -1.0(6) ? . . . . C(11) N(2) C(20) C(19) 175.3(4) ? . . . . C(20) N(2) C(11) C(10) 138.1(3) ? . . . . O(1) C(1) C(2) O(3) -1.7(5) ? . . . . O(1) C(1) C(2) C(3) 177.9(3) ? . . . . O(1) C(1) C(6) C(5) -177.9(3) ? . . . . O(1) C(1) C(6) C(7) 3.1(6) ? . . . . C(2) C(1) C(6) C(5) 2.5(6) ? . . . . C(2) C(1) C(6) C(7) -176.5(3) ? . . . . C(6) C(1) C(2) O(3) 177.9(3) ? . . . . C(6) C(1) C(2) C(3) -2.5(6) ? . . . . O(3) C(2) C(3) C(4) -179.9(3) ? . . . . C(1) C(2) C(3) C(4) 0.5(6) ? . . . . C(2) C(3) C(4) C(5) 1.5(6) ? . . . . C(3) C(4) C(5) C(6) -1.4(7) ? . . . . C(4) C(5) C(6) C(1) -0.6(6) ? . . . . C(4) C(5) C(6) C(7) 178.5(4) ? . . . . C(1) C(6) C(7) N(1) -4.5(7) ? . . . . C(5) C(6) C(7) N(1) 176.5(4) ? . . . . N(1) C(9) C(10) C(11) -68.5(4) ? . . . . N(1) C(9) C(10) C(12) 175.4(3) ? . . . . N(1) C(9) C(10) C(13) 54.9(4) ? . . . . C(9) C(10) C(11) N(2) 74.0(4) ? . . . . C(12) C(10) C(11) N(2) -170.1(3) ? . . . . C(13) C(10) C(11) N(2) -49.9(4) ? . . . . O(2) C(14) C(15) O(4) 1.8(5) ? . . . . O(2) C(14) C(15) C(16) -178.0(3) ? . . . . O(2) C(14) C(19) C(18) 177.1(3) ? . . . . O(2) C(14) C(19) C(20) -2.0(6) ? . . . . C(15) C(14) C(19) C(18) -2.7(5) ? . . . . C(15) C(14) C(19) C(20) 178.2(3) ? . . . . C(19) C(14) C(15) O(4) -178.4(3) ? . . . . C(19) C(14) C(15) C(16) 1.8(6) ? . . . . O(4) C(15) C(16) C(17) -178.8(3) ? . . . . C(14) C(15) C(16) C(17) 0.9(6) ? . . . . C(15) C(16) C(17) C(18) -2.9(6) ? . . . . C(16) C(17) C(18) C(19) 2.0(6) ? . . . . C(17) C(18) C(19) C(14) 0.9(6) ? . . . . C(17) C(18) C(19) C(20) 180.0(3) ? . . . . C(14) C(19) C(20) N(2) 2.4(7) ? . . . . C(18) C(19) C(20) N(2) -176.7(4) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(7) C(3) 3.012(5) ? . 3_667 O(7) C(4) 3.295(6) ? . 3_667 O(7) C(23) 3.594(6) ? . 1_455 O(8) C(21) 3.490(5) ? . 3_666 O(10) C(9) 3.509(5) ? . 2_746 O(10) C(16) 3.490(5) ? . 3_666 O(10) C(21) 3.524(5) ? . 3_666 O(10) C(24) 3.529(6) ? . 2_746 O(12) C(9) 3.416(5) ? . 4_564 O(13) C(12) 3.269(5) ? . 2_746 N(2) C(5) 3.557(5) ? . 4_564 N(5) C(12) 3.516(6) ? . 2_746 C(2) C(3) 3.556(5) ? . 3_767 C(2) C(4) 3.590(6) ? . 3_767 C(3) O(7) 3.012(5) ? . 3_667 C(3) C(2) 3.556(5) ? . 3_767 C(3) C(3) 3.168(6) ? . 3_767 C(3) C(4) 3.490(6) ? . 3_767 C(4) O(7) 3.295(6) ? . 3_667 C(4) C(2) 3.590(6) ? . 3_767 C(4) C(3) 3.490(6) ? . 3_767 C(4) C(11) 3.527(6) ? . 4_565 C(4) C(20) 3.436(6) ? . 4_565 C(5) N(2) 3.557(5) ? . 4_565 C(5) C(20) 3.169(6) ? . 4_565 C(6) C(18) 3.569(6) ? . 4_565 C(9) O(10) 3.509(5) ? . 2_756 C(9) O(12) 3.416(5) ? . 4_565 C(11) C(4) 3.527(6) ? . 4_564 C(12) O(13) 3.269(5) ? . 2_756 C(12) N(5) 3.516(6) ? . 2_756 C(12) C(12) 3.413(6) ? . 3_777 C(13) C(15) 3.597(6) ? . 4_565 C(13) C(16) 3.379(6) ? . 4_565 C(15) C(13) 3.597(6) ? . 4_564 C(16) O(10) 3.490(5) ? . 3_666 C(16) C(13) 3.379(6) ? . 4_564 C(18) C(6) 3.569(6) ? . 4_564 C(20) C(4) 3.436(6) ? . 4_564 C(20) C(5) 3.169(6) ? . 4_564 C(21) O(8) 3.490(5) ? . 3_666 C(21) O(10) 3.524(5) ? . 3_666 C(23) O(7) 3.594(6) ? . 1_655 C(24) O(10) 3.529(6) ? . 2_756 O(3) H(2) 3.20(4) ? . 3_767 O(4) H(17) 3.02(5) ? . 4_564 O(4) H(30) 3.449 ? . 1_455 O(5) H(19) 3.05(5) ? . 4_565 O(5) H(27) 2.728 ? . 1_455 O(6) H(11) 3.19(4) ? . 2_646 O(6) H(16) 2.96(5) ? . 2_646 O(6) H(21) 3.19(4) ? . 2_646 O(7) H(1) 2.61(5) ? . 3_667 O(7) H(2) 3.16(4) ? . 3_667 O(7) H(6) 3.18(6) ? . 3_667 O(7) H(11) 2.84(4) ? . 2_646 O(7) H(21) 2.81(4) ? . 2_646 O(7) H(25) 3.519 ? . 1_455 O(7) H(27) 2.830 ? . 1_455 O(8) H(12) 3.28(5) ? . 2_746 O(8) H(13) 3.28(6) ? . 4_564 O(8) H(16) 3.20(5) ? . 2_646 O(8) H(17) 3.19(5) ? . 4_564 O(8) H(24) 2.77(5) ? . 3_666 O(9) H(2) 2.93(4) ? . 3_767 O(9) H(10) 3.21(4) ? . 2_746 O(9) H(12) 3.30(5) ? . 2_746 O(9) H(29) 3.296 ? . 2_746 O(10) H(8) 2.68(4) ? . 2_746 O(10) H(10) 3.30(4) ? . 2_746 O(10) H(12) 2.98(5) ? . 2_746 O(10) H(16) 3.52(6) ? . 2_646 O(10) H(18) 2.62(4) ? . 3_666 O(10) H(23) 3.20(4) ? . 3_666 O(10) H(24) 2.98(5) ? . 3_666 O(10) H(26) 3.574 ? . 2_746 O(10) H(28) 3.163 ? . 2_746 O(10) H(29) 3.290 ? . 2_746 O(11) H(2) 2.81(4) ? . 3_767 O(11) H(12) 3.44(5) ? . 2_746 O(11) H(14) 3.50(5) ? . 2_746 O(12) H(4) 3.16(4) ? . 4_564 O(12) H(9) 2.49(7) ? . 4_564 O(12) H(12) 3.36(5) ? . 2_746 O(12) H(13) 3.11(6) ? . 4_564 O(12) H(17) 2.97(5) ? . 4_564 O(13) H(4) 3.27(4) ? . 4_564 O(13) H(9) 2.87(6) ? . 4_564 O(13) H(12) 3.20(4) ? . 2_746 O(13) H(13) 3.57(6) ? . 2_746 O(13) H(14) 2.52(5) ? . 2_746 O(13) H(23) 2.80(5) ? . 1_655 O(14) H(3) 2.78(6) ? . 4_564 O(14) H(4) 3.12(4) ? . 4_564 N(2) H(3) 3.28(6) ? . 4_564 N(3) H(11) 3.38(4) ? . 2_646 N(3) H(21) 3.38(4) ? . 2_646 N(3) H(27) 3.081 ? . 1_455 N(4) H(8) 3.51(4) ? . 2_746 N(4) H(10) 3.51(4) ? . 2_746 N(4) H(12) 2.93(5) ? . 2_746 N(4) H(16) 3.43(5) ? . 2_646 N(4) H(18) 3.59(4) ? . 3_666 N(4) H(24) 3.24(5) ? . 3_666 N(5) H(4) 3.55(4) ? . 4_564 N(5) H(9) 3.04(7) ? . 4_564 N(5) H(12) 3.07(5) ? . 2_746 N(5) H(13) 3.55(6) ? . 4_564 N(5) H(14) 3.01(5) ? . 2_746 C(1) H(20) 3.22(4) ? . 4_565 C(2) H(1) 3.38(4) ? . 3_767 C(2) H(2) 3.40(4) ? . 3_767 C(2) H(20) 3.33(4) ? . 4_565 C(3) H(1) 3.21(5) ? . 3_767 C(3) H(21) 3.40(4) ? . 4_565 C(4) H(1) 3.34(5) ? . 3_767 C(4) H(7) 2.96(4) ? . 3_767 C(4) H(10) 3.23(4) ? . 4_565 C(4) H(11) 3.17(5) ? . 4_565 C(4) H(21) 2.88(4) ? . 4_565 C(5) H(7) 2.95(4) ? . 3_767 C(5) H(10) 3.30(4) ? . 4_565 C(5) H(21) 2.99(4) ? . 4_565 C(5) H(29) 3.450 ? . 4_565 C(6) H(20) 3.36(4) ? . 4_565 C(8) H(2) 3.52(4) ? . 3_767 C(8) H(20) 3.14(4) ? . 2_646 C(11) H(2) 3.11(5) ? . 4_564 C(11) H(3) 3.41(6) ? . 4_564 C(12) H(12) 3.07(5) ? . 3_777 C(12) H(13) 2.78(5) ? . 3_777 C(12) H(22) 3.31(4) ? . 2_656 C(12) H(23) 3.40(4) ? . 2_656 C(13) H(18) 3.32(5) ? . 4_565 C(13) H(22) 3.04(5) ? . 2_656 C(13) H(24) 3.13(5) ? . 4_565 C(14) H(28) 3.433 ? . 1_455 C(14) H(30) 3.314 ? . 1_455 C(15) H(15) 3.33(4) ? . 4_564 C(15) H(17) 3.04(5) ? . 4_564 C(15) H(30) 3.038 ? . 1_455 C(16) H(15) 2.84(4) ? . 4_564 C(16) H(17) 3.13(5) ? . 4_564 C(16) H(26) 3.577 ? . 4_464 C(16) H(30) 3.275 ? . 1_455 C(17) H(15) 3.24(4) ? . 4_564 C(17) H(26) 3.174 ? . 4_464 C(17) H(27) 3.395 ? . 4_464 C(18) H(5) 3.27(4) ? . 2_656 C(18) H(6) 3.25(6) ? . 2_656 C(20) H(3) 3.20(6) ? . 4_564 C(21) H(14) 2.95(5) ? . 2_646 C(21) H(16) 3.14(5) ? . 2_646 C(21) H(17) 3.30(5) ? . 4_564 C(21) H(24) 3.53(5) ? . 3_666 C(22) H(3) 3.45(6) ? . 4_564 C(23) H(19) 2.95(5) ? . 4_665 C(24) H(3) 3.34(5) ? . 4_564 H(1) O(7) 2.61(5) ? . 3_667 H(1) C(2) 3.38(4) ? . 3_767 H(1) C(3) 3.21(5) ? . 3_767 H(1) C(4) 3.34(5) ? . 3_767 H(1) H(1) 3.53(7) ? . 3_767 H(1) H(25) 3.115 ? . 3_767 H(1) H(27) 3.416 ? . 3_767 H(2) O(3) 3.20(4) ? . 3_767 H(2) O(7) 3.16(4) ? . 3_667 H(2) O(9) 2.93(4) ? . 3_767 H(2) O(11) 2.81(4) ? . 3_767 H(2) C(2) 3.40(4) ? . 3_767 H(2) C(8) 3.52(4) ? . 3_767 H(2) C(11) 3.11(5) ? . 4_565 H(2) H(7) 2.96(6) ? . 3_767 H(2) H(10) 2.74(6) ? . 4_565 H(2) H(11) 2.75(7) ? . 4_565 H(2) H(21) 3.07(6) ? . 4_565 H(3) O(14) 2.78(6) ? . 4_565 H(3) N(2) 3.28(6) ? . 4_565 H(3) C(11) 3.41(6) ? . 4_565 H(3) C(20) 3.20(6) ? . 4_565 H(3) C(22) 3.45(6) ? . 4_565 H(3) C(24) 3.34(5) ? . 4_565 H(3) H(7) 2.91(7) ? . 3_767 H(3) H(10) 2.89(7) ? . 4_565 H(3) H(11) 3.59(8) ? . 4_565 H(3) H(21) 3.23(7) ? . 4_565 H(3) H(29) 2.623 ? . 4_565 H(4) O(12) 3.16(4) ? . 4_565 H(4) O(13) 3.27(4) ? . 4_565 H(4) O(14) 3.12(4) ? . 4_565 H(4) N(5) 3.55(4) ? . 4_565 H(4) H(29) 3.516 ? . 4_565 H(4) H(30) 3.572 ? . 4_565 H(5) C(18) 3.27(4) ? . 2_646 H(5) H(20) 2.89(6) ? . 2_646 H(5) H(21) 3.22(6) ? . 2_646 H(5) H(29) 3.249 ? . 2_746 H(6) O(7) 3.18(6) ? . 3_667 H(6) C(18) 3.25(6) ? . 2_646 H(6) H(6) 3.33(9) ? . 3_667 H(6) H(19) 3.56(8) ? . 2_646 H(6) H(20) 2.58(7) ? . 2_646 H(7) C(4) 2.96(4) ? . 3_767 H(7) C(5) 2.95(4) ? . 3_767 H(7) H(2) 2.96(6) ? . 3_767 H(7) H(3) 2.91(7) ? . 3_767 H(7) H(20) 3.50(6) ? . 2_646 H(7) H(29) 3.144 ? . 2_746 H(8) O(10) 2.68(4) ? . 2_756 H(8) N(4) 3.51(4) ? . 2_756 H(9) O(12) 2.49(7) ? . 4_565 H(9) O(13) 2.87(6) ? . 4_565 H(9) N(5) 3.04(7) ? . 4_565 H(10) O(9) 3.21(4) ? . 2_756 H(10) O(10) 3.30(4) ? . 2_756 H(10) N(4) 3.51(4) ? . 2_756 H(10) C(4) 3.23(4) ? . 4_564 H(10) C(5) 3.30(4) ? . 4_564 H(10) H(2) 2.74(6) ? . 4_564 H(10) H(3) 2.89(7) ? . 4_564 H(11) O(6) 3.19(4) ? . 2_656 H(11) O(7) 2.84(4) ? . 2_656 H(11) N(3) 3.38(4) ? . 2_656 H(11) C(4) 3.17(5) ? . 4_564 H(11) H(2) 2.75(7) ? . 4_564 H(11) H(3) 3.59(8) ? . 4_564 H(12) O(8) 3.28(5) ? . 2_756 H(12) O(9) 3.30(5) ? . 2_756 H(12) O(10) 2.98(5) ? . 2_756 H(12) O(11) 3.44(5) ? . 2_756 H(12) O(12) 3.36(5) ? . 2_756 H(12) O(13) 3.20(5) ? . 2_756 H(12) N(4) 2.93(5) ? . 2_756 H(12) N(5) 3.07(5) ? . 2_756 H(12) C(12) 3.07(5) ? . 3_777 H(12) H(12) 3.07(7) ? . 3_777 H(12) H(13) 2.26(7) ? . 3_777 H(12) H(14) 3.34(7) ? . 3_777 H(13) O(8) 3.28(6) ? . 4_565 H(13) O(12) 3.11(6) ? . 4_565 H(13) O(13) 3.57(6) ? . 2_756 H(13) N(5) 3.55(6) ? . 4_565 H(13) C(12) 2.78(5) ? . 3_777 H(13) H(12) 2.26(7) ? . 3_777 H(13) H(13) 2.35(8) ? . 3_777 H(13) H(14) 3.10(7) ? . 3_777 H(13) H(22) 3.41(7) ? . 2_656 H(13) H(23) 3.33(7) ? . 2_656 H(14) O(11) 3.50(5) ? . 2_756 H(14) O(13) 2.52(5) ? . 2_756 H(14) N(5) 3.01(5) ? . 2_756 H(14) C(21) 2.95(5) ? . 2_656 H(14) H(12) 3.34(7) ? . 3_777 H(14) H(13) 3.10(7) ? . 3_777 H(14) H(22) 2.66(6) ? . 2_656 H(14) H(23) 2.61(7) ? . 2_656 H(14) H(24) 3.42(7) ? . 2_656 H(15) C(15) 3.33(4) ? . 4_565 H(15) C(16) 2.84(4) ? . 4_565 H(15) C(17) 3.24(4) ? . 4_565 H(15) H(18) 2.86(6) ? . 4_565 H(15) H(19) 3.48(6) ? . 4_565 H(15) H(24) 3.39(7) ? . 4_565 H(16) O(6) 2.96(5) ? . 2_656 H(16) O(8) 3.20(5) ? . 2_656 H(16) O(10) 3.52(6) ? . 2_656 H(16) N(4) 3.43(5) ? . 2_656 H(16) C(21) 3.14(5) ? . 2_656 H(16) H(18) 3.38(7) ? . 4_565 H(16) H(22) 2.25(7) ? . 2_656 H(16) H(24) 3.33(7) ? . 2_656 H(16) H(24) 2.91(8) ? . 4_565 H(17) O(4) 3.02(5) ? . 4_565 H(17) O(8) 3.19(5) ? . 4_565 H(17) O(12) 2.97(5) ? . 4_565 H(17) C(15) 3.04(5) ? . 4_565 H(17) C(16) 3.13(5) ? . 4_565 H(17) C(21) 3.30(5) ? . 4_565 H(17) H(18) 3.15(7) ? . 4_565 H(17) H(22) 3.06(7) ? . 2_656 H(17) H(24) 3.58(7) ? . 2_656 H(17) H(24) 2.66(7) ? . 4_565 H(18) O(10) 2.62(4) ? . 3_666 H(18) N(4) 3.59(4) ? . 3_666 H(18) C(13) 3.32(5) ? . 4_564 H(18) H(15) 2.86(6) ? . 4_564 H(18) H(16) 3.38(7) ? . 4_564 H(18) H(17) 3.15(7) ? . 4_564 H(18) H(26) 3.275 ? . 4_464 H(18) H(30) 3.520 ? . 1_455 H(19) O(5) 3.05(5) ? . 4_564 H(19) C(23) 2.95(5) ? . 4_464 H(19) H(6) 3.56(8) ? . 2_656 H(19) H(15) 3.48(6) ? . 4_564 H(19) H(26) 2.553 ? . 4_464 H(19) H(27) 2.506 ? . 4_464 H(19) H(28) 3.196 ? . 4_464 H(20) C(1) 3.22(4) ? . 4_564 H(20) C(2) 3.33(4) ? . 4_564 H(20) C(6) 3.36(4) ? . 4_564 H(20) C(8) 3.14(4) ? . 2_656 H(20) H(5) 2.89(6) ? . 2_656 H(20) H(6) 2.58(7) ? . 2_656 H(20) H(7) 3.50(6) ? . 2_656 H(21) O(6) 3.19(4) ? . 2_656 H(21) O(7) 2.81(4) ? . 2_656 H(21) N(3) 3.38(4) ? . 2_656 H(21) C(3) 3.40(4) ? . 4_564 H(21) C(4) 2.88(4) ? . 4_564 H(21) C(5) 2.99(4) ? . 4_564 H(21) H(2) 3.07(6) ? . 4_564 H(21) H(3) 3.23(7) ? . 4_564 H(21) H(5) 3.22(6) ? . 2_656 H(22) C(12) 3.31(4) ? . 2_646 H(22) C(13) 3.04(5) ? . 2_646 H(22) H(13) 3.41(7) ? . 2_646 H(22) H(14) 2.66(6) ? . 2_646 H(22) H(16) 2.25(7) ? . 2_646 H(22) H(17) 3.06(7) ? . 2_646 H(22) H(24) 3.14(7) ? . 3_666 H(23) O(10) 3.20(4) ? . 3_666 H(23) O(13) 2.80(5) ? . 1_455 H(23) C(12) 3.40(4) ? . 2_646 H(23) H(13) 3.33(7) ? . 2_646 H(23) H(14) 2.61(7) ? . 2_646 H(23) H(30) 3.098 ? . 1_455 H(24) O(8) 2.77(5) ? . 3_666 H(24) O(10) 2.98(5) ? . 3_666 H(24) N(4) 3.24(5) ? . 3_666 H(24) C(13) 3.13(5) ? . 4_564 H(24) C(21) 3.53(5) ? . 3_666 H(24) H(14) 3.42(7) ? . 2_646 H(24) H(15) 3.39(7) ? . 4_564 H(24) H(16) 3.33(7) ? . 2_646 H(24) H(16) 2.91(8) ? . 4_564 H(24) H(17) 3.58(7) ? . 2_646 H(24) H(17) 2.66(7) ? . 4_564 H(24) H(22) 3.14(7) ? . 3_666 H(24) H(24) 2.94(7) ? . 3_666 H(25) O(7) 3.519 ? . 1_655 H(25) H(1) 3.115 ? . 3_767 H(26) O(10) 3.574 ? . 2_756 H(26) C(16) 3.577 ? . 4_665 H(26) C(17) 3.174 ? . 4_665 H(26) H(18) 3.275 ? . 4_665 H(26) H(19) 2.553 ? . 4_665 H(27) O(5) 2.728 ? . 1_655 H(27) O(7) 2.830 ? . 1_655 H(27) N(3) 3.081 ? . 1_655 H(27) C(17) 3.395 ? . 4_665 H(27) H(1) 3.416 ? . 3_767 H(27) H(19) 2.506 ? . 4_665 H(28) O(10) 3.163 ? . 2_756 H(28) C(14) 3.433 ? . 1_655 H(28) H(19) 3.196 ? . 4_665 H(29) O(9) 3.296 ? . 2_756 H(29) O(10) 3.290 ? . 2_756 H(29) C(5) 3.450 ? . 4_564 H(29) H(3) 2.623 ? . 4_564 H(29) H(4) 3.516 ? . 4_564 H(29) H(5) 3.249 ? . 2_756 H(29) H(7) 3.144 ? . 2_756 H(30) O(4) 3.449 ? . 1_655 H(30) C(14) 3.314 ? . 1_655 H(30) C(15) 3.038 ? . 1_655 H(30) C(16) 3.275 ? . 1_655 H(30) H(4) 3.572 ? . 4_564 H(30) H(18) 3.520 ? . 1_655 H(30) H(23) 3.098 ? . 1_655 Dy(1) Cu(1) 3.510(4) ? . . data___HoCu _database_code_depnum_ccdc_archive 'CCDC 881973' #TrackingRef '11257_web_deposit_cif_file_2_TakayukiIshida_1336987557.HoCu_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Cu Ho N5 O14 ' _chemical_formula_moiety 'C24 H30 Cu Ho N5 O14 ' _chemical_formula_weight 841.00 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.634(3) _cell_length_b 19.842(5) _cell_length_c 15.698(9) _cell_angle_alpha 90.0000 _cell_angle_beta 95.530(4) _cell_angle_gamma 90.0000 _cell_volume 2987(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 391 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668.00 _exptl_absorpt_coefficient_mu 3.422 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.362 _exptl_absorpt_correction_T_max 0.504 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 51234 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_ambient_temperature 100. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6845 _reflns_number_gt 5946 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0354 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6845 _refine_ls_number_parameters 509 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.8000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.99 _refine_diff_density_min -0.76 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 5(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ho Ho -0.218 4.678 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ho(1) Ho 0.69684(2) 0.576210(10) 0.745190(10) 0.01214(4) Uani 1.00 1 d . . . Cu(1) Cu 0.79064(4) 0.73795(2) 0.81868(2) 0.01240(9) Uani 1.00 1 d . . . O(1) O 0.7824(2) 0.64521(11) 0.86081(14) 0.0166(5) Uani 1.00 1 d . . . O(2) O 0.6713(2) 0.69361(11) 0.72767(14) 0.0161(5) Uani 1.00 1 d . . . O(3) O 0.7379(2) 0.51754(12) 0.88768(14) 0.0179(6) Uani 1.00 1 d . . . O(4) O 0.5206(2) 0.61321(11) 0.62719(14) 0.0165(5) Uani 1.00 1 d . . . O(5) O 0.4907(2) 0.60185(12) 0.82156(16) 0.0221(6) Uani 1.00 1 d . . . O(6) O 0.4969(2) 0.50498(12) 0.75815(16) 0.0208(6) Uani 1.00 1 d . . . O(7) O 0.3290(3) 0.52722(15) 0.8382(2) 0.0407(9) Uani 1.00 1 d . . . O(8) O 0.6748(3) 0.49606(14) 0.62165(17) 0.0317(7) Uani 1.00 1 d . . . O(9) O 0.7810(3) 0.45640(14) 0.73667(16) 0.0291(7) Uani 1.00 1 d . . . O(10) O 0.7462(2) 0.39153(13) 0.62470(17) 0.0269(7) Uani 1.00 1 d . . . O(11) O 0.9502(3) 0.57182(14) 0.75692(18) 0.0326(8) Uani 1.00 1 d . . . O(12) O 0.8525(2) 0.61225(18) 0.64146(18) 0.0408(9) Uani 1.00 1 d . . . O(13) O 1.0790(2) 0.61286(13) 0.66120(18) 0.0280(7) Uani 1.00 1 d . . . O(14) O 1.0088(2) 0.74430(13) 0.74881(17) 0.0242(6) Uani 1.00 1 d . . . N(1) N 0.8844(2) 0.77038(14) 0.92962(17) 0.0148(6) Uani 1.00 1 d . . . N(2) N 0.7652(3) 0.82731(14) 0.76256(17) 0.0152(6) Uani 1.00 1 d . . . N(3) N 0.4351(3) 0.54453(15) 0.8070(2) 0.0219(8) Uani 1.00 1 d . . . N(4) N 0.7342(3) 0.44626(15) 0.66011(19) 0.0186(7) Uani 1.00 1 d . . . N(5) N 0.9650(3) 0.59903(15) 0.68557(19) 0.0209(7) Uani 1.00 1 d . . . C(1) C 0.8277(3) 0.62138(17) 0.9375(2) 0.0157(8) Uani 1.00 1 d . . . C(2) C 0.8077(3) 0.55261(17) 0.9546(2) 0.0150(8) Uani 1.00 1 d . . . C(3) C 0.8568(3) 0.52347(18) 1.0316(2) 0.0192(8) Uani 1.00 1 d . . . C(4) C 0.9272(4) 0.5639(2) 1.0957(2) 0.0212(9) Uani 1.00 1 d . . . C(5) C 0.9437(3) 0.63072(19) 1.0819(2) 0.0208(9) Uani 1.00 1 d . . . C(6) C 0.8945(3) 0.66120(17) 1.0033(2) 0.0158(8) Uani 1.00 1 d . . . C(7) C 0.9136(3) 0.73287(18) 0.9954(2) 0.0183(8) Uani 1.00 1 d . . . C(8) C 0.6912(4) 0.4505(2) 0.9084(2) 0.0253(10) Uani 1.00 1 d . . . C(9) C 0.9312(4) 0.84151(18) 0.9416(2) 0.0192(8) Uani 1.00 1 d . . . C(10) C 0.8351(3) 0.89317(17) 0.8956(2) 0.0161(8) Uani 1.00 1 d . . . C(11) C 0.8392(3) 0.88679(17) 0.7991(2) 0.0171(8) Uani 1.00 1 d . . . C(12) C 0.8926(4) 0.96233(19) 0.9214(2) 0.0239(10) Uani 1.00 1 d . . . C(13) C 0.6854(4) 0.88596(19) 0.9197(2) 0.0223(9) Uani 1.00 1 d . . . C(14) C 0.6067(3) 0.72197(16) 0.65792(19) 0.0112(7) Uani 1.00 1 d . . . C(15) C 0.5244(3) 0.67964(17) 0.6006(2) 0.0147(8) Uani 1.00 1 d . . . C(16) C 0.4578(3) 0.70373(18) 0.5254(2) 0.0187(8) Uani 1.00 1 d . . . C(17) C 0.4716(3) 0.77183(19) 0.5039(2) 0.0213(9) Uani 1.00 1 d . . . C(18) C 0.5478(3) 0.81378(18) 0.5587(2) 0.0197(9) Uani 1.00 1 d . . . C(19) C 0.6147(3) 0.78992(17) 0.6371(2) 0.0144(7) Uani 1.00 1 d . . . C(20) C 0.6914(3) 0.83849(17) 0.6915(2) 0.0170(8) Uani 1.00 1 d . . . C(21) C 0.4152(4) 0.57195(19) 0.5806(2) 0.0232(10) Uani 1.00 1 d . . . C(22) C 1.1283(3) 0.72969(19) 0.7743(2) 0.0234(9) Uani 1.00 1 d . . . C(23) C 1.1608(4) 0.6874(2) 0.8528(2) 0.0340(11) Uani 1.00 1 d . . . C(24) C 1.2493(4) 0.7544(2) 0.7296(3) 0.0432(14) Uani 1.00 1 d . . . H(1) H 0.850(3) 0.4763(19) 1.045(2) 0.020(9) Uiso 1.00 1 d . . . H(2) H 0.964(3) 0.5423(17) 1.146(2) 0.013(9) Uiso 1.00 1 d . . . H(3) H 0.989(3) 0.6583(17) 1.121(2) 0.013(9) Uiso 1.00 1 d . . . H(4) H 0.960(3) 0.7540(19) 1.047(2) 0.023(10) Uiso 1.00 1 d . . . H(5) H 0.631(4) 0.437(2) 0.859(2) 0.030(11) Uiso 1.00 1 d . . . H(6) H 0.623(4) 0.454(2) 0.959(3) 0.052(14) Uiso 1.00 1 d . . . H(7) H 0.771(4) 0.4224(18) 0.923(2) 0.022(10) Uiso 1.00 1 d . . . H(8) H 1.023(3) 0.8458(19) 0.922(2) 0.021(10) Uiso 1.00 1 d . . . H(9) H 0.939(4) 0.854(2) 1.002(2) 0.044(13) Uiso 1.00 1 d . . . H(10) H 0.939(3) 0.8821(18) 0.787(2) 0.020(10) Uiso 1.00 1 d . . . H(11) H 0.793(3) 0.9284(19) 0.769(2) 0.023(11) Uiso 1.00 1 d . . . H(12) H 0.991(4) 0.969(2) 0.909(2) 0.030(11) Uiso 1.00 1 d . . . H(13) H 0.890(4) 0.973(2) 0.986(2) 0.047(13) Uiso 1.00 1 d . . . H(14) H 0.846(4) 0.999(2) 0.892(2) 0.031(11) Uiso 1.00 1 d . . . H(15) H 0.650(4) 0.841(2) 0.912(2) 0.035(12) Uiso 1.00 1 d . . . H(16) H 0.619(5) 0.916(2) 0.886(3) 0.061(17) Uiso 1.00 1 d . . . H(17) H 0.681(4) 0.896(2) 0.981(2) 0.027(10) Uiso 1.00 1 d . . . H(18) H 0.401(3) 0.677(2) 0.488(2) 0.028(11) Uiso 1.00 1 d . . . H(19) H 0.431(4) 0.790(2) 0.449(2) 0.033(11) Uiso 1.00 1 d . . . H(20) H 0.563(3) 0.8577(19) 0.546(2) 0.023(10) Uiso 1.00 1 d . . . H(21) H 0.687(3) 0.8843(19) 0.669(2) 0.024(10) Uiso 1.00 1 d . . . H(22) H 0.424(4) 0.526(2) 0.610(2) 0.031(11) Uiso 1.00 1 d . . . H(23) H 0.319(4) 0.594(2) 0.580(2) 0.034(11) Uiso 1.00 1 d . . . H(24) H 0.440(4) 0.565(2) 0.523(2) 0.033(12) Uiso 1.00 1 d . . . H(25) H 1.0859 0.6572 0.8587 0.041 Uiso 1.00 1 c R . . H(26) H 1.1733 0.7157 0.9018 0.041 Uiso 1.00 1 c R . . H(27) H 1.2439 0.6625 0.8478 0.040 Uiso 1.00 1 c R . . H(28) H 1.3280 0.7610 0.7701 0.053 Uiso 1.00 1 c R . . H(29) H 1.2251 0.7959 0.7018 0.053 Uiso 1.00 1 c R . . H(30) H 1.2713 0.7221 0.6883 0.053 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ho(1) 0.01447(9) 0.01029(9) 0.01175(9) -0.00108(5) 0.00177(6) -0.00121(5) Cu(1) 0.0152(2) 0.0106(2) 0.01119(19) -0.00127(15) 0.00037(15) -0.00123(15) O(1) 0.0254(13) 0.0133(11) 0.0104(11) -0.0014(9) -0.0019(9) 0.0002(9) O(2) 0.0195(12) 0.0121(11) 0.0154(11) -0.0032(9) -0.0045(9) -0.0001(9) O(3) 0.0282(13) 0.0131(11) 0.0125(11) -0.0037(10) 0.0024(9) 0.0013(9) O(4) 0.0173(12) 0.0137(11) 0.0174(11) -0.0023(9) -0.0035(9) -0.0025(9) O(5) 0.0243(13) 0.0158(12) 0.0277(14) -0.0039(10) 0.0095(11) -0.0044(10) O(6) 0.0218(13) 0.0166(12) 0.0252(13) -0.0010(10) 0.0082(10) -0.0050(10) O(7) 0.0349(17) 0.0333(17) 0.059(2) -0.0125(13) 0.0296(15) -0.0084(15) O(8) 0.0472(18) 0.0260(15) 0.0210(13) 0.0179(13) -0.0019(12) -0.0041(11) O(9) 0.0428(17) 0.0255(14) 0.0168(12) 0.0110(12) -0.0076(11) -0.0073(11) O(10) 0.0286(14) 0.0180(13) 0.0334(15) 0.0027(11) -0.0004(11) -0.0142(11) O(11) 0.0274(15) 0.0431(18) 0.0275(15) -0.0003(12) 0.0033(12) 0.0156(12) O(12) 0.0193(14) 0.080(2) 0.0236(15) -0.0013(15) 0.0024(11) 0.0173(15) O(13) 0.0217(13) 0.0254(14) 0.0398(16) -0.0068(11) 0.0171(12) -0.0120(12) O(14) 0.0212(13) 0.0239(14) 0.0280(14) 0.0029(11) 0.0048(11) -0.0029(11) N(1) 0.0167(14) 0.0143(14) 0.0131(13) -0.0018(11) 0.0006(11) -0.0025(10) N(2) 0.0190(14) 0.0130(13) 0.0141(13) -0.0019(11) 0.0033(11) -0.0017(10) N(3) 0.0212(16) 0.0200(15) 0.0257(16) -0.0037(12) 0.0088(13) 0.0003(12) N(4) 0.0168(14) 0.0165(14) 0.0226(15) 0.0003(12) 0.0029(12) -0.0046(12) N(5) 0.0230(16) 0.0170(15) 0.0239(16) -0.0050(12) 0.0081(13) -0.0091(12) C(1) 0.0170(16) 0.0177(17) 0.0128(15) 0.0005(13) 0.0040(12) -0.0002(13) C(2) 0.0169(16) 0.0170(16) 0.0114(15) -0.0001(13) 0.0026(12) -0.0023(12) C(3) 0.0230(18) 0.0170(17) 0.0181(17) 0.0062(14) 0.0044(14) 0.0051(13) C(4) 0.0253(19) 0.0271(19) 0.0116(16) 0.0081(15) 0.0043(14) 0.0037(14) C(5) 0.0258(19) 0.0257(19) 0.0108(16) 0.0028(15) 0.0021(14) -0.0041(14) C(6) 0.0197(17) 0.0167(16) 0.0109(15) 0.0060(13) 0.0019(12) -0.0004(12) C(7) 0.0180(17) 0.0204(18) 0.0159(16) -0.0000(14) -0.0014(13) -0.0043(13) C(8) 0.031(2) 0.0177(19) 0.027(2) -0.0065(16) 0.0018(17) 0.0061(15) C(9) 0.0249(19) 0.0160(17) 0.0164(17) -0.0056(14) 0.0012(14) -0.0032(13) C(10) 0.0197(17) 0.0119(16) 0.0170(16) -0.0039(13) 0.0039(13) -0.0032(12) C(11) 0.0208(18) 0.0138(16) 0.0164(16) -0.0082(13) 0.0000(13) -0.0010(13) C(12) 0.031(2) 0.0140(17) 0.027(2) -0.0057(15) 0.0088(17) -0.0037(15) C(13) 0.0196(18) 0.0174(18) 0.031(2) -0.0033(14) 0.0101(16) -0.0057(15) C(14) 0.0085(14) 0.0147(15) 0.0101(14) -0.0008(12) -0.0009(11) 0.0024(12) C(15) 0.0162(16) 0.0140(16) 0.0142(15) 0.0018(13) 0.0020(12) 0.0011(12) C(16) 0.0156(17) 0.0191(17) 0.0204(17) 0.0021(13) -0.0043(13) -0.0044(14) C(17) 0.0220(18) 0.0210(18) 0.0197(18) 0.0042(14) -0.0044(14) 0.0053(14) C(18) 0.0204(18) 0.0150(17) 0.0229(18) 0.0030(14) -0.0019(14) 0.0049(14) C(19) 0.0173(16) 0.0150(16) 0.0109(15) 0.0006(13) 0.0023(12) 0.0006(12) C(20) 0.0169(17) 0.0120(16) 0.0223(17) -0.0013(13) 0.0036(13) 0.0015(13) C(21) 0.0204(19) 0.0189(19) 0.028(2) -0.0082(14) -0.0066(16) -0.0047(15) C(22) 0.0158(17) 0.0211(18) 0.034(2) -0.0033(14) 0.0073(15) -0.0135(16) C(23) 0.022(2) 0.041(2) 0.038(2) 0.0061(18) -0.0017(17) -0.0067(19) C(24) 0.031(2) 0.044(2) 0.059(3) -0.003(2) 0.020(2) -0.004(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ho(1) O(1) 2.358(2) yes . . Ho(1) O(2) 2.356(2) yes . . Ho(1) O(3) 2.519(2) yes . . Ho(1) O(4) 2.500(2) yes . . Ho(1) O(5) 2.470(2) yes . . Ho(1) O(6) 2.414(2) yes . . Ho(1) O(8) 2.501(2) yes . . Ho(1) O(9) 2.519(2) yes . . Ho(1) O(11) 2.432(2) yes . . Ho(1) O(12) 2.425(3) yes . . Cu(1) O(1) 1.960(2) yes . . Cu(1) O(2) 1.955(2) yes . . Cu(1) O(14) 2.466(2) yes . . Cu(1) N(1) 1.990(2) yes . . Cu(1) N(2) 1.984(2) yes . . O(1) C(1) 1.328(3) yes . . O(2) C(14) 1.331(3) yes . . O(3) C(2) 1.380(3) yes . . O(3) C(8) 1.452(4) yes . . O(4) C(15) 1.384(4) yes . . O(4) C(21) 1.446(4) yes . . O(5) N(3) 1.268(3) yes . . O(6) N(3) 1.283(4) yes . . O(7) N(3) 1.224(4) yes . . O(8) N(4) 1.266(3) yes . . O(9) N(4) 1.258(3) yes . . O(10) N(4) 1.231(3) yes . . O(11) N(5) 1.264(4) yes . . O(12) N(5) 1.256(3) yes . . O(13) N(5) 1.228(4) yes . . O(14) C(22) 1.217(4) yes . . N(1) C(7) 1.282(4) yes . . N(1) C(9) 1.488(4) yes . . N(2) C(11) 1.467(4) yes . . N(2) C(20) 1.284(4) yes . . C(1) C(2) 1.407(4) yes . . C(1) C(6) 1.406(4) yes . . C(2) C(3) 1.381(4) yes . . C(3) C(4) 1.409(4) yes . . C(4) C(5) 1.356(5) yes . . C(5) C(6) 1.414(4) yes . . C(6) C(7) 1.441(4) yes . . C(9) C(10) 1.516(4) yes . . C(10) C(11) 1.525(4) yes . . C(10) C(12) 1.520(5) yes . . C(10) C(13) 1.533(5) yes . . C(14) C(15) 1.416(4) yes . . C(14) C(19) 1.391(4) yes . . C(15) C(16) 1.374(4) yes . . C(16) C(17) 1.402(5) yes . . C(17) C(18) 1.360(5) yes . . C(18) C(19) 1.414(4) yes . . C(19) C(20) 1.443(4) yes . . C(22) C(23) 1.499(5) yes . . C(22) C(24) 1.501(6) yes . . C(3) H(1) 0.96(3) no . . C(4) H(2) 0.94(3) no . . C(5) H(3) 0.90(3) no . . C(7) H(4) 0.98(3) no . . C(8) H(5) 0.96(4) no . . C(8) H(6) 1.08(4) no . . C(8) H(7) 0.96(3) no . . C(9) H(8) 0.96(3) no . . C(9) H(9) 0.98(4) no . . C(11) H(10) 1.00(3) no . . C(11) H(11) 1.03(3) no . . C(12) H(12) 1.00(4) no . . C(12) H(13) 1.03(4) no . . C(12) H(14) 0.96(4) no . . C(13) H(15) 0.96(4) no . . C(13) H(16) 0.99(4) no . . C(13) H(17) 0.99(4) no . . C(16) H(18) 0.93(3) no . . C(17) H(19) 0.97(3) no . . C(18) H(20) 0.91(3) no . . C(20) H(21) 0.97(3) no . . C(21) H(22) 1.01(4) no . . C(21) H(23) 1.03(4) no . . C(21) H(24) 0.97(4) no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Ho(1) O(2) 62.64(7) yes . . . O(1) Ho(1) O(3) 64.62(7) yes . . . O(1) Ho(1) O(4) 124.19(7) yes . . . O(1) Ho(1) O(5) 75.19(8) yes . . . O(1) Ho(1) O(6) 119.84(8) yes . . . O(1) Ho(1) O(8) 164.44(9) yes . . . O(1) Ho(1) O(9) 119.90(7) yes . . . O(1) Ho(1) O(11) 71.87(8) yes . . . O(1) Ho(1) O(12) 98.79(9) yes . . . O(2) Ho(1) O(3) 124.50(7) yes . . . O(2) Ho(1) O(4) 64.36(7) yes . . . O(2) Ho(1) O(5) 76.89(8) yes . . . O(2) Ho(1) O(6) 120.90(8) yes . . . O(2) Ho(1) O(8) 122.55(8) yes . . . O(2) Ho(1) O(9) 163.21(8) yes . . . O(2) Ho(1) O(11) 97.87(8) yes . . . O(2) Ho(1) O(12) 72.21(10) yes . . . O(3) Ho(1) O(4) 146.22(7) yes . . . O(3) Ho(1) O(5) 74.28(8) yes . . . O(3) Ho(1) O(6) 73.32(7) yes . . . O(3) Ho(1) O(8) 112.89(8) yes . . . O(3) Ho(1) O(9) 65.62(7) yes . . . O(3) Ho(1) O(11) 81.12(8) yes . . . O(3) Ho(1) O(12) 132.69(8) yes . . . O(4) Ho(1) O(5) 77.20(7) yes . . . O(4) Ho(1) O(6) 75.14(7) yes . . . O(4) Ho(1) O(8) 67.12(8) yes . . . O(4) Ho(1) O(9) 115.90(7) yes . . . O(4) Ho(1) O(11) 132.22(8) yes . . . O(4) Ho(1) O(12) 80.55(8) yes . . . O(5) Ho(1) O(6) 52.69(8) yes . . . O(5) Ho(1) O(8) 119.68(8) yes . . . O(5) Ho(1) O(9) 119.87(8) yes . . . O(5) Ho(1) O(11) 144.98(8) yes . . . O(5) Ho(1) O(12) 147.50(9) yes . . . O(6) Ho(1) O(8) 71.59(9) yes . . . O(6) Ho(1) O(9) 73.47(8) yes . . . O(6) Ho(1) O(11) 140.92(8) yes . . . O(6) Ho(1) O(12) 141.21(9) yes . . . O(8) Ho(1) O(9) 50.40(8) yes . . . O(8) Ho(1) O(11) 92.62(9) yes . . . O(8) Ho(1) O(12) 71.26(10) yes . . . O(9) Ho(1) O(11) 69.18(9) yes . . . O(9) Ho(1) O(12) 91.13(10) yes . . . O(11) Ho(1) O(12) 51.70(9) yes . . . O(1) Cu(1) O(2) 77.51(9) yes . . . O(1) Cu(1) O(14) 105.20(9) yes . . . O(1) Cu(1) N(1) 92.18(10) yes . . . O(1) Cu(1) N(2) 168.96(10) yes . . . O(2) Cu(1) O(14) 99.46(9) yes . . . O(2) Cu(1) N(1) 166.09(10) yes . . . O(2) Cu(1) N(2) 92.23(10) yes . . . O(14) Cu(1) N(1) 92.20(10) yes . . . O(14) Cu(1) N(2) 80.27(10) yes . . . N(1) Cu(1) N(2) 97.23(11) yes . . . Ho(1) O(1) Cu(1) 107.94(9) yes . . . Ho(1) O(1) C(1) 123.46(19) yes . . . Cu(1) O(1) C(1) 128.3(2) yes . . . Ho(1) O(2) Cu(1) 108.20(9) yes . . . Ho(1) O(2) C(14) 123.32(18) yes . . . Cu(1) O(2) C(14) 127.34(19) yes . . . Ho(1) O(3) C(2) 117.79(19) yes . . . Ho(1) O(3) C(8) 126.68(19) yes . . . C(2) O(3) C(8) 115.5(2) yes . . . Ho(1) O(4) C(15) 117.85(17) yes . . . Ho(1) O(4) C(21) 127.01(19) yes . . . C(15) O(4) C(21) 115.1(2) yes . . . Ho(1) O(5) N(3) 94.20(19) yes . . . Ho(1) O(6) N(3) 96.43(18) yes . . . Ho(1) O(8) N(4) 97.23(19) yes . . . Ho(1) O(9) N(4) 96.55(19) yes . . . Ho(1) O(11) N(5) 96.6(2) yes . . . Ho(1) O(12) N(5) 97.2(2) yes . . . Cu(1) O(14) C(22) 131.4(2) yes . . . Cu(1) N(1) C(7) 124.3(2) yes . . . Cu(1) N(1) C(9) 121.6(2) yes . . . C(7) N(1) C(9) 114.1(2) yes . . . Cu(1) N(2) C(11) 120.7(2) yes . . . Cu(1) N(2) C(20) 125.1(2) yes . . . C(11) N(2) C(20) 114.1(2) yes . . . O(5) N(3) O(6) 116.4(2) yes . . . O(5) N(3) O(7) 122.3(3) yes . . . O(6) N(3) O(7) 121.3(2) yes . . . O(8) N(4) O(9) 115.8(2) yes . . . O(8) N(4) O(10) 122.1(2) yes . . . O(9) N(4) O(10) 122.1(2) yes . . . O(11) N(5) O(12) 114.4(3) yes . . . O(11) N(5) O(13) 123.5(2) yes . . . O(12) N(5) O(13) 122.1(3) yes . . . O(1) C(1) C(2) 118.6(2) yes . . . O(1) C(1) C(6) 123.6(2) yes . . . C(2) C(1) C(6) 117.8(2) yes . . . O(3) C(2) C(1) 114.2(2) yes . . . O(3) C(2) C(3) 123.7(3) yes . . . C(1) C(2) C(3) 122.1(3) yes . . . C(2) C(3) C(4) 119.2(3) yes . . . C(3) C(4) C(5) 119.9(3) yes . . . C(4) C(5) C(6) 121.5(3) yes . . . C(1) C(6) C(5) 119.5(3) yes . . . C(1) C(6) C(7) 123.0(2) yes . . . C(5) C(6) C(7) 117.5(2) yes . . . N(1) C(7) C(6) 128.5(3) yes . . . N(1) C(9) C(10) 114.7(2) yes . . . C(9) C(10) C(11) 110.1(2) yes . . . C(9) C(10) C(12) 107.1(2) yes . . . C(9) C(10) C(13) 111.4(2) yes . . . C(11) C(10) C(12) 107.2(2) yes . . . C(11) C(10) C(13) 110.6(2) yes . . . C(12) C(10) C(13) 110.3(3) yes . . . N(2) C(11) C(10) 113.4(2) yes . . . O(2) C(14) C(15) 117.4(2) yes . . . O(2) C(14) C(19) 124.8(2) yes . . . C(15) C(14) C(19) 117.8(2) yes . . . O(4) C(15) C(14) 113.7(2) yes . . . O(4) C(15) C(16) 124.5(2) yes . . . C(14) C(15) C(16) 121.8(3) yes . . . C(15) C(16) C(17) 119.6(3) yes . . . C(16) C(17) C(18) 119.7(3) yes . . . C(17) C(18) C(19) 121.2(3) yes . . . C(14) C(19) C(18) 119.9(2) yes . . . C(14) C(19) C(20) 123.0(2) yes . . . C(18) C(19) C(20) 117.1(3) yes . . . N(2) C(20) C(19) 127.5(3) yes . . . O(14) C(22) C(23) 121.3(3) yes . . . O(14) C(22) C(24) 121.4(3) yes . . . C(23) C(22) C(24) 117.2(3) yes . . . C(2) C(3) H(1) 125(2) no . . . C(4) C(3) H(1) 116(2) no . . . C(3) C(4) H(2) 117(2) no . . . C(5) C(4) H(2) 123(2) no . . . C(4) C(5) H(3) 123(2) no . . . C(6) C(5) H(3) 115(2) no . . . N(1) C(7) H(4) 118(2) no . . . C(6) C(7) H(4) 114(2) no . . . O(3) C(8) H(5) 105(2) no . . . O(3) C(8) H(6) 109(2) no . . . O(3) C(8) H(7) 109(2) no . . . H(5) C(8) H(6) 104(3) no . . . H(5) C(8) H(7) 116(3) no . . . H(6) C(8) H(7) 113(3) no . . . N(1) C(9) H(8) 109(2) no . . . N(1) C(9) H(9) 111(2) no . . . C(10) C(9) H(8) 109(2) no . . . C(10) C(9) H(9) 106(2) no . . . H(8) C(9) H(9) 107(3) no . . . N(2) C(11) H(10) 107(2) no . . . N(2) C(11) H(11) 107(2) no . . . C(10) C(11) H(10) 108(2) no . . . C(10) C(11) H(11) 110(2) no . . . H(10) C(11) H(11) 112(3) no . . . C(10) C(12) H(12) 113(2) no . . . C(10) C(12) H(13) 113(2) no . . . C(10) C(12) H(14) 115(2) no . . . H(12) C(12) H(13) 107(3) no . . . H(12) C(12) H(14) 103(3) no . . . H(13) C(12) H(14) 105(3) no . . . C(10) C(13) H(15) 113(2) no . . . C(10) C(13) H(16) 113(3) no . . . C(10) C(13) H(17) 110(2) no . . . H(15) C(13) H(16) 107(3) no . . . H(15) C(13) H(17) 106(3) no . . . H(16) C(13) H(17) 108(3) no . . . C(15) C(16) H(18) 122(2) no . . . C(17) C(16) H(18) 118(2) no . . . C(16) C(17) H(19) 122(2) no . . . C(18) C(17) H(19) 119(2) no . . . C(17) C(18) H(20) 123(2) no . . . C(19) C(18) H(20) 116(2) no . . . N(2) C(20) H(21) 118(2) no . . . C(19) C(20) H(21) 114(2) no . . . O(4) C(21) H(22) 105(2) no . . . O(4) C(21) H(23) 111(2) no . . . O(4) C(21) H(24) 109(2) no . . . H(22) C(21) H(23) 115(3) no . . . H(22) C(21) H(24) 107(3) no . . . H(23) C(21) H(24) 111(3) no . . . C(22) C(23) H(25) 109.4 no . . . C(22) C(23) H(26) 109.5 no . . . C(22) C(23) H(27) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . H(25) C(23) H(27) 109.5 no . . . H(26) C(23) H(27) 109.5 no . . . C(22) C(24) H(28) 109.7 no . . . C(22) C(24) H(29) 109.3 no . . . C(22) C(24) H(30) 109.4 no . . . H(28) C(24) H(29) 109.5 no . . . H(28) C(24) H(30) 109.5 no . . . H(29) C(24) H(30) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Ho(1) O(2) Cu(1) 14.24(9) ? . . . . O(1) Ho(1) O(2) C(14) -177.1(2) ? . . . . O(2) Ho(1) O(1) Cu(1) -14.18(9) ? . . . . O(2) Ho(1) O(1) C(1) 171.5(2) ? . . . . O(1) Ho(1) O(3) C(2) -9.8(2) ? . . . . O(1) Ho(1) O(3) C(8) 167.9(2) ? . . . . O(3) Ho(1) O(1) Cu(1) -176.21(13) ? . . . . O(3) Ho(1) O(1) C(1) 9.5(2) ? . . . . O(1) Ho(1) O(4) C(15) 34.8(2) ? . . . . O(1) Ho(1) O(4) C(21) -147.3(2) ? . . . . O(4) Ho(1) O(1) Cu(1) -34.03(14) ? . . . . O(4) Ho(1) O(1) C(1) 151.7(2) ? . . . . O(1) Ho(1) O(5) N(3) -144.80(19) ? . . . . O(5) Ho(1) O(1) Cu(1) -96.86(11) ? . . . . O(5) Ho(1) O(1) C(1) 88.8(2) ? . . . . O(1) Ho(1) O(6) N(3) 32.9(2) ? . . . . O(6) Ho(1) O(1) Cu(1) -125.89(10) ? . . . . O(6) Ho(1) O(1) C(1) 59.8(2) ? . . . . O(1) Ho(1) O(8) N(4) 57.4(4) ? . . . . O(8) Ho(1) O(1) Cu(1) 99.4(3) ? . . . . O(8) Ho(1) O(1) C(1) -74.9(4) ? . . . . O(1) Ho(1) O(9) N(4) -166.53(18) ? . . . . O(9) Ho(1) O(1) Cu(1) 146.89(10) ? . . . . O(9) Ho(1) O(1) C(1) -27.4(2) ? . . . . O(1) Ho(1) O(11) N(5) -115.7(2) ? . . . . O(11) Ho(1) O(1) Cu(1) 95.19(12) ? . . . . O(11) Ho(1) O(1) C(1) -79.1(2) ? . . . . O(1) Ho(1) O(12) N(5) 56.5(2) ? . . . . O(12) Ho(1) O(1) Cu(1) 50.47(12) ? . . . . O(12) Ho(1) O(1) C(1) -123.8(2) ? . . . . O(2) Ho(1) O(3) C(2) -29.2(2) ? . . . . O(2) Ho(1) O(3) C(8) 148.4(2) ? . . . . O(3) Ho(1) O(2) Cu(1) 34.01(14) ? . . . . O(3) Ho(1) O(2) C(14) -157.4(2) ? . . . . O(2) Ho(1) O(4) C(15) 15.2(2) ? . . . . O(2) Ho(1) O(4) C(21) -166.8(2) ? . . . . O(4) Ho(1) O(2) Cu(1) 176.09(13) ? . . . . O(4) Ho(1) O(2) C(14) -15.3(2) ? . . . . O(2) Ho(1) O(5) N(3) 150.44(19) ? . . . . O(5) Ho(1) O(2) Cu(1) 94.17(11) ? . . . . O(5) Ho(1) O(2) C(14) -97.2(2) ? . . . . O(2) Ho(1) O(6) N(3) -41.2(2) ? . . . . O(6) Ho(1) O(2) Cu(1) 124.32(10) ? . . . . O(6) Ho(1) O(2) C(14) -67.1(2) ? . . . . O(2) Ho(1) O(8) N(4) 162.48(18) ? . . . . O(8) Ho(1) O(2) Cu(1) -148.81(10) ? . . . . O(8) Ho(1) O(2) C(14) 19.8(2) ? . . . . O(2) Ho(1) O(9) N(4) -72.5(3) ? . . . . O(9) Ho(1) O(2) Cu(1) -88.9(2) ? . . . . O(9) Ho(1) O(2) C(14) 79.7(3) ? . . . . O(2) Ho(1) O(11) N(5) -57.9(2) ? . . . . O(11) Ho(1) O(2) Cu(1) -50.59(11) ? . . . . O(11) Ho(1) O(2) C(14) 118.0(2) ? . . . . O(2) Ho(1) O(12) N(5) 114.0(2) ? . . . . O(12) Ho(1) O(2) Cu(1) -96.05(11) ? . . . . O(12) Ho(1) O(2) C(14) 72.6(2) ? . . . . O(3) Ho(1) O(4) C(15) 129.6(2) ? . . . . O(3) Ho(1) O(4) C(21) -52.5(3) ? . . . . O(4) Ho(1) O(3) C(2) -124.0(2) ? . . . . O(4) Ho(1) O(3) C(8) 53.7(3) ? . . . . O(3) Ho(1) O(5) N(3) -77.51(18) ? . . . . O(5) Ho(1) O(3) C(2) -90.6(2) ? . . . . O(5) Ho(1) O(3) C(8) 87.1(2) ? . . . . O(3) Ho(1) O(6) N(3) 79.46(18) ? . . . . O(6) Ho(1) O(3) C(2) -145.6(2) ? . . . . O(6) Ho(1) O(3) C(8) 32.0(2) ? . . . . O(3) Ho(1) O(8) N(4) -20.0(2) ? . . . . O(8) Ho(1) O(3) C(2) 153.3(2) ? . . . . O(8) Ho(1) O(3) C(8) -29.0(2) ? . . . . O(3) Ho(1) O(9) N(4) 156.9(2) ? . . . . O(9) Ho(1) O(3) C(2) 135.3(2) ? . . . . O(9) Ho(1) O(3) C(8) -47.0(2) ? . . . . O(3) Ho(1) O(11) N(5) 178.2(2) ? . . . . O(11) Ho(1) O(3) C(2) 64.2(2) ? . . . . O(11) Ho(1) O(3) C(8) -118.1(2) ? . . . . O(3) Ho(1) O(12) N(5) -6.9(2) ? . . . . O(12) Ho(1) O(3) C(2) 68.2(2) ? . . . . O(12) Ho(1) O(3) C(8) -114.1(2) ? . . . . O(4) Ho(1) O(5) N(3) 84.19(18) ? . . . . O(5) Ho(1) O(4) C(15) 96.7(2) ? . . . . O(5) Ho(1) O(4) C(21) -85.4(2) ? . . . . O(4) Ho(1) O(6) N(3) -88.30(18) ? . . . . O(6) Ho(1) O(4) C(15) 151.0(2) ? . . . . O(6) Ho(1) O(4) C(21) -31.0(2) ? . . . . O(4) Ho(1) O(8) N(4) -163.3(2) ? . . . . O(8) Ho(1) O(4) C(15) -133.0(2) ? . . . . O(8) Ho(1) O(4) C(21) 44.9(2) ? . . . . O(4) Ho(1) O(9) N(4) 14.3(2) ? . . . . O(9) Ho(1) O(4) C(15) -146.1(2) ? . . . . O(9) Ho(1) O(4) C(21) 31.8(2) ? . . . . O(4) Ho(1) O(11) N(5) 4.4(2) ? . . . . O(11) Ho(1) O(4) C(15) -61.4(2) ? . . . . O(11) Ho(1) O(4) C(21) 116.5(2) ? . . . . O(4) Ho(1) O(12) N(5) 179.93(16) ? . . . . O(12) Ho(1) O(4) C(15) -59.5(2) ? . . . . O(12) Ho(1) O(4) C(21) 118.5(2) ? . . . . O(5) Ho(1) O(6) N(3) -3.23(16) ? . . . . O(6) Ho(1) O(5) N(3) 3.25(16) ? . . . . O(5) Ho(1) O(8) N(4) -104.4(2) ? . . . . O(8) Ho(1) O(5) N(3) 30.2(2) ? . . . . O(5) Ho(1) O(9) N(4) 104.0(2) ? . . . . O(9) Ho(1) O(5) N(3) -28.5(2) ? . . . . O(5) Ho(1) O(11) N(5) -136.30(19) ? . . . . O(11) Ho(1) O(5) N(3) -124.6(2) ? . . . . O(5) Ho(1) O(12) N(5) 132.7(2) ? . . . . O(12) Ho(1) O(5) N(3) 132.1(2) ? . . . . O(6) Ho(1) O(8) N(4) -82.1(2) ? . . . . O(8) Ho(1) O(6) N(3) -158.68(19) ? . . . . O(6) Ho(1) O(9) N(4) 78.1(2) ? . . . . O(9) Ho(1) O(6) N(3) 148.32(19) ? . . . . O(6) Ho(1) O(11) N(5) 129.00(19) ? . . . . O(11) Ho(1) O(6) N(3) 130.80(19) ? . . . . O(6) Ho(1) O(12) N(5) -128.5(2) ? . . . . O(12) Ho(1) O(6) N(3) -141.34(19) ? . . . . O(8) Ho(1) O(9) N(4) -1.39(18) ? . . . . O(9) Ho(1) O(8) N(4) 1.39(18) ? . . . . O(8) Ho(1) O(11) N(5) 65.4(2) ? . . . . O(11) Ho(1) O(8) N(4) 61.4(2) ? . . . . O(8) Ho(1) O(12) N(5) -111.2(2) ? . . . . O(12) Ho(1) O(8) N(4) 109.3(2) ? . . . . O(9) Ho(1) O(11) N(5) 111.0(2) ? . . . . O(11) Ho(1) O(9) N(4) -113.6(2) ? . . . . O(9) Ho(1) O(12) N(5) -64.0(2) ? . . . . O(12) Ho(1) O(9) N(4) -65.7(2) ? . . . . O(11) Ho(1) O(12) N(5) -1.93(19) ? . . . . O(12) Ho(1) O(11) N(5) 1.92(19) ? . . . . O(1) Cu(1) O(2) Ho(1) -15.62(10) ? . . . . O(1) Cu(1) O(2) C(14) 176.4(2) ? . . . . O(2) Cu(1) O(1) Ho(1) 15.58(10) ? . . . . O(2) Cu(1) O(1) C(1) -170.5(2) ? . . . . O(1) Cu(1) O(14) C(22) -52.5(3) ? . . . . O(14) Cu(1) O(1) Ho(1) -80.98(10) ? . . . . O(14) Cu(1) O(1) C(1) 93.0(2) ? . . . . O(1) Cu(1) N(1) C(7) -1.3(3) ? . . . . O(1) Cu(1) N(1) C(9) 176.6(2) ? . . . . N(1) Cu(1) O(1) Ho(1) -173.85(11) ? . . . . N(1) Cu(1) O(1) C(1) 0.1(2) ? . . . . O(1) Cu(1) N(2) C(11) 161.8(4) ? . . . . O(1) Cu(1) N(2) C(20) -21.7(7) ? . . . . N(2) Cu(1) O(1) Ho(1) 37.6(6) ? . . . . N(2) Cu(1) O(1) C(1) -148.4(5) ? . . . . O(2) Cu(1) O(14) C(22) -132.1(3) ? . . . . O(14) Cu(1) O(2) Ho(1) 88.00(10) ? . . . . O(14) Cu(1) O(2) C(14) -80.0(2) ? . . . . O(2) Cu(1) N(1) C(7) 40.5(6) ? . . . . O(2) Cu(1) N(1) C(9) -141.6(4) ? . . . . N(1) Cu(1) O(2) Ho(1) -58.6(4) ? . . . . N(1) Cu(1) O(2) C(14) 133.4(4) ? . . . . O(2) Cu(1) N(2) C(11) -176.7(2) ? . . . . O(2) Cu(1) N(2) C(20) -0.2(3) ? . . . . N(2) Cu(1) O(2) Ho(1) 168.50(11) ? . . . . N(2) Cu(1) O(2) C(14) 0.5(2) ? . . . . O(14) Cu(1) N(1) C(7) -106.6(2) ? . . . . O(14) Cu(1) N(1) C(9) 71.3(2) ? . . . . N(1) Cu(1) O(14) C(22) 40.3(3) ? . . . . O(14) Cu(1) N(2) C(11) -77.5(2) ? . . . . O(14) Cu(1) N(2) C(20) 99.0(3) ? . . . . N(2) Cu(1) O(14) C(22) 137.3(3) ? . . . . N(1) Cu(1) N(2) C(11) 13.5(2) ? . . . . N(1) Cu(1) N(2) C(20) -170.0(2) ? . . . . N(2) Cu(1) N(1) C(7) 172.9(2) ? . . . . N(2) Cu(1) N(1) C(9) -9.2(2) ? . . . . Ho(1) O(1) C(1) C(2) -8.4(4) ? . . . . Ho(1) O(1) C(1) C(6) 171.9(2) ? . . . . Cu(1) O(1) C(1) C(2) 178.5(2) ? . . . . Cu(1) O(1) C(1) C(6) -1.2(4) ? . . . . Ho(1) O(2) C(14) C(15) 14.0(3) ? . . . . Ho(1) O(2) C(14) C(19) -165.6(2) ? . . . . Cu(1) O(2) C(14) C(15) -179.7(2) ? . . . . Cu(1) O(2) C(14) C(19) 0.8(4) ? . . . . Ho(1) O(3) C(2) C(1) 9.7(3) ? . . . . Ho(1) O(3) C(2) C(3) -169.2(2) ? . . . . C(8) O(3) C(2) C(1) -168.2(3) ? . . . . C(8) O(3) C(2) C(3) 12.8(4) ? . . . . Ho(1) O(4) C(15) C(14) -14.6(3) ? . . . . Ho(1) O(4) C(15) C(16) 164.5(2) ? . . . . C(21) O(4) C(15) C(14) 167.2(2) ? . . . . C(21) O(4) C(15) C(16) -13.7(4) ? . . . . Ho(1) O(5) N(3) O(6) -5.4(2) ? . . . . Ho(1) O(5) N(3) O(7) 174.1(2) ? . . . . Ho(1) O(6) N(3) O(5) 5.6(2) ? . . . . Ho(1) O(6) N(3) O(7) -173.9(2) ? . . . . Ho(1) O(8) N(4) O(9) -2.4(3) ? . . . . Ho(1) O(8) N(4) O(10) 178.1(2) ? . . . . Ho(1) O(9) N(4) O(8) 2.4(3) ? . . . . Ho(1) O(9) N(4) O(10) -178.1(2) ? . . . . Ho(1) O(11) N(5) O(12) -3.2(3) ? . . . . Ho(1) O(11) N(5) O(13) 175.5(2) ? . . . . Ho(1) O(12) N(5) O(11) 3.2(3) ? . . . . Ho(1) O(12) N(5) O(13) -175.5(2) ? . . . . Cu(1) O(14) C(22) C(23) 15.1(5) ? . . . . Cu(1) O(14) C(22) C(24) -163.7(2) ? . . . . Cu(1) N(1) C(7) C(6) 3.8(5) ? . . . . Cu(1) N(1) C(9) C(10) 36.6(4) ? . . . . C(7) N(1) C(9) C(10) -145.3(3) ? . . . . C(9) N(1) C(7) C(6) -174.2(3) ? . . . . Cu(1) N(2) C(11) C(10) -45.2(3) ? . . . . Cu(1) N(2) C(20) C(19) -1.3(5) ? . . . . C(11) N(2) C(20) C(19) 175.4(3) ? . . . . C(20) N(2) C(11) C(10) 138.0(3) ? . . . . O(1) C(1) C(2) O(3) -1.6(4) ? . . . . O(1) C(1) C(2) C(3) 177.4(3) ? . . . . O(1) C(1) C(6) C(5) -177.7(3) ? . . . . O(1) C(1) C(6) C(7) 3.5(5) ? . . . . C(2) C(1) C(6) C(5) 2.5(5) ? . . . . C(2) C(1) C(6) C(7) -176.3(3) ? . . . . C(6) C(1) C(2) O(3) 178.2(2) ? . . . . C(6) C(1) C(2) C(3) -2.8(5) ? . . . . O(3) C(2) C(3) C(4) 179.8(3) ? . . . . C(1) C(2) C(3) C(4) 1.0(5) ? . . . . C(2) C(3) C(4) C(5) 1.2(5) ? . . . . C(3) C(4) C(5) C(6) -1.5(5) ? . . . . C(4) C(5) C(6) C(1) -0.4(5) ? . . . . C(4) C(5) C(6) C(7) 178.5(3) ? . . . . C(1) C(6) C(7) N(1) -5.1(6) ? . . . . C(5) C(6) C(7) N(1) 176.1(3) ? . . . . N(1) C(9) C(10) C(11) -68.6(3) ? . . . . N(1) C(9) C(10) C(12) 175.2(3) ? . . . . N(1) C(9) C(10) C(13) 54.6(3) ? . . . . C(9) C(10) C(11) N(2) 73.6(3) ? . . . . C(12) C(10) C(11) N(2) -170.2(2) ? . . . . C(13) C(10) C(11) N(2) -50.0(3) ? . . . . O(2) C(14) C(15) O(4) 1.5(4) ? . . . . O(2) C(14) C(15) C(16) -177.6(3) ? . . . . O(2) C(14) C(19) C(18) 176.4(3) ? . . . . O(2) C(14) C(19) C(20) -2.4(5) ? . . . . C(15) C(14) C(19) C(18) -3.1(4) ? . . . . C(15) C(14) C(19) C(20) 178.0(3) ? . . . . C(19) C(14) C(15) O(4) -179.0(2) ? . . . . C(19) C(14) C(15) C(16) 2.0(5) ? . . . . O(4) C(15) C(16) C(17) -178.5(3) ? . . . . C(14) C(15) C(16) C(17) 0.4(5) ? . . . . C(15) C(16) C(17) C(18) -1.7(5) ? . . . . C(16) C(17) C(18) C(19) 0.5(5) ? . . . . C(17) C(18) C(19) C(14) 2.0(5) ? . . . . C(17) C(18) C(19) C(20) -179.1(3) ? . . . . C(14) C(19) C(20) N(2) 2.8(5) ? . . . . C(18) C(19) C(20) N(2) -176.1(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(3) C(4) 3.595(4) ? . 3_767 O(7) C(3) 3.017(4) ? . 3_667 O(7) C(4) 3.306(5) ? . 3_667 O(7) C(23) 3.585(5) ? . 1_455 O(8) C(21) 3.482(4) ? . 3_666 O(10) C(9) 3.515(4) ? . 2_746 O(10) C(16) 3.477(4) ? . 3_666 O(10) C(21) 3.516(4) ? . 3_666 O(10) C(24) 3.552(5) ? . 2_746 O(12) C(9) 3.422(4) ? . 4_564 O(13) C(12) 3.278(4) ? . 2_746 N(2) C(5) 3.554(4) ? . 4_564 N(5) C(12) 3.536(5) ? . 2_746 C(2) C(3) 3.555(4) ? . 3_767 C(2) C(4) 3.588(5) ? . 3_767 C(3) O(7) 3.017(4) ? . 3_667 C(3) C(2) 3.555(4) ? . 3_767 C(3) C(3) 3.161(5) ? . 3_767 C(3) C(4) 3.483(5) ? . 3_767 C(4) O(3) 3.595(4) ? . 3_767 C(4) O(7) 3.306(5) ? . 3_667 C(4) C(2) 3.588(5) ? . 3_767 C(4) C(3) 3.483(5) ? . 3_767 C(4) C(11) 3.520(5) ? . 4_565 C(4) C(20) 3.440(5) ? . 4_565 C(5) N(2) 3.554(4) ? . 4_565 C(5) C(20) 3.169(5) ? . 4_565 C(6) C(18) 3.566(5) ? . 4_565 C(9) O(10) 3.515(4) ? . 2_756 C(9) O(12) 3.422(4) ? . 4_565 C(11) C(4) 3.520(5) ? . 4_564 C(12) O(13) 3.278(4) ? . 2_756 C(12) N(5) 3.536(5) ? . 2_756 C(12) C(12) 3.410(5) ? . 3_777 C(13) C(16) 3.380(5) ? . 4_565 C(16) O(10) 3.477(4) ? . 3_666 C(16) C(13) 3.380(5) ? . 4_564 C(18) C(6) 3.566(5) ? . 4_564 C(20) C(4) 3.440(5) ? . 4_564 C(20) C(5) 3.169(5) ? . 4_564 C(21) O(8) 3.482(4) ? . 3_666 C(21) O(10) 3.516(4) ? . 3_666 C(23) O(7) 3.585(5) ? . 1_655 C(24) O(10) 3.552(5) ? . 2_756 O(3) H(2) 3.20(3) ? . 3_767 O(4) H(17) 2.90(4) ? . 4_564 O(4) H(30) 3.435 ? . 1_455 O(5) H(19) 3.04(4) ? . 4_565 O(5) H(27) 2.731 ? . 1_455 O(5) H(28) 3.582 ? . 1_455 O(6) H(11) 3.17(3) ? . 2_646 O(6) H(16) 3.00(4) ? . 2_646 O(6) H(21) 3.25(3) ? . 2_646 O(7) H(1) 2.64(3) ? . 3_667 O(7) H(2) 3.17(3) ? . 3_667 O(7) H(6) 3.20(4) ? . 3_667 O(7) H(11) 2.77(3) ? . 2_646 O(7) H(21) 2.84(3) ? . 2_646 O(7) H(25) 3.519 ? . 1_455 O(7) H(27) 2.815 ? . 1_455 O(8) H(12) 3.34(4) ? . 2_746 O(8) H(13) 3.18(4) ? . 4_564 O(8) H(16) 3.23(5) ? . 2_646 O(8) H(17) 3.08(4) ? . 4_564 O(8) H(24) 2.71(4) ? . 3_666 O(9) H(2) 2.93(3) ? . 3_767 O(9) H(10) 3.13(3) ? . 2_746 O(9) H(12) 3.32(4) ? . 2_746 O(9) H(29) 3.330 ? . 2_746 O(10) H(8) 2.58(3) ? . 2_746 O(10) H(10) 3.21(3) ? . 2_746 O(10) H(12) 3.05(4) ? . 2_746 O(10) H(16) 3.54(5) ? . 2_646 O(10) H(18) 2.55(3) ? . 3_666 O(10) H(23) 3.23(4) ? . 3_666 O(10) H(24) 2.92(4) ? . 3_666 O(10) H(28) 3.191 ? . 2_746 O(10) H(29) 3.309 ? . 2_746 O(11) H(2) 2.81(3) ? . 3_767 O(11) H(12) 3.40(4) ? . 2_746 O(11) H(14) 3.50(4) ? . 2_746 O(12) H(4) 3.26(3) ? . 4_564 O(12) H(9) 2.50(4) ? . 4_564 O(12) H(12) 3.35(4) ? . 2_746 O(12) H(13) 3.02(4) ? . 4_564 O(12) H(17) 2.88(3) ? . 4_564 O(13) H(4) 3.33(3) ? . 4_564 O(13) H(9) 2.80(4) ? . 4_564 O(13) H(12) 3.11(3) ? . 2_746 O(13) H(13) 3.58(4) ? . 4_564 O(13) H(14) 2.53(4) ? . 2_746 O(13) H(23) 2.77(4) ? . 1_655 O(14) H(3) 2.78(3) ? . 4_564 O(14) H(4) 3.16(3) ? . 4_564 N(2) H(3) 3.26(3) ? . 4_564 N(3) H(11) 3.32(3) ? . 2_646 N(3) H(21) 3.42(3) ? . 2_646 N(3) H(27) 3.084 ? . 1_455 N(4) H(8) 3.43(3) ? . 2_746 N(4) H(10) 3.42(3) ? . 2_746 N(4) H(12) 2.99(4) ? . 2_746 N(4) H(16) 3.46(5) ? . 2_646 N(4) H(18) 3.53(3) ? . 3_666 N(4) H(24) 3.19(4) ? . 3_666 N(5) H(9) 3.01(4) ? . 4_564 N(5) H(12) 3.03(4) ? . 2_746 N(5) H(13) 3.46(4) ? . 4_564 N(5) H(14) 3.02(4) ? . 2_746 C(1) H(20) 3.23(3) ? . 4_565 C(2) H(1) 3.35(3) ? . 3_767 C(2) H(2) 3.40(3) ? . 3_767 C(2) H(20) 3.38(3) ? . 4_565 C(3) H(1) 3.18(3) ? . 3_767 C(3) H(21) 3.38(3) ? . 4_565 C(4) H(1) 3.32(3) ? . 3_767 C(4) H(7) 2.97(4) ? . 3_767 C(4) H(10) 3.18(3) ? . 4_565 C(4) H(11) 3.12(3) ? . 4_565 C(4) H(21) 2.88(3) ? . 4_565 C(5) H(7) 2.95(4) ? . 3_767 C(5) H(10) 3.23(3) ? . 4_565 C(5) H(11) 3.59(3) ? . 4_565 C(5) H(21) 2.96(3) ? . 4_565 C(5) H(29) 3.468 ? . 4_565 C(6) H(20) 3.34(3) ? . 4_565 C(6) H(21) 3.55(3) ? . 4_565 C(8) H(2) 3.52(3) ? . 3_767 C(8) H(20) 3.20(3) ? . 2_646 C(11) H(2) 3.12(3) ? . 4_564 C(11) H(3) 3.39(3) ? . 4_564 C(12) H(12) 3.11(3) ? . 3_777 C(12) H(13) 2.76(4) ? . 3_777 C(12) H(22) 3.30(3) ? . 2_656 C(12) H(23) 3.31(4) ? . 2_656 C(13) H(18) 3.28(3) ? . 4_565 C(13) H(22) 3.00(4) ? . 2_656 C(13) H(24) 3.14(4) ? . 4_565 C(14) H(28) 3.438 ? . 1_455 C(14) H(30) 3.311 ? . 1_455 C(15) H(15) 3.33(4) ? . 4_564 C(15) H(17) 2.94(4) ? . 4_564 C(15) H(30) 3.033 ? . 1_455 C(16) H(15) 2.83(4) ? . 4_564 C(16) H(17) 3.06(4) ? . 4_564 C(16) H(26) 3.579 ? . 4_464 C(16) H(30) 3.285 ? . 1_455 C(17) H(15) 3.24(4) ? . 4_564 C(17) H(26) 3.163 ? . 4_464 C(17) H(27) 3.388 ? . 4_464 C(18) H(5) 3.32(4) ? . 2_656 C(18) H(6) 3.23(4) ? . 2_656 C(20) H(3) 3.17(3) ? . 4_564 C(21) H(14) 2.97(4) ? . 2_646 C(21) H(16) 3.16(5) ? . 2_646 C(21) H(17) 3.19(4) ? . 4_564 C(21) H(24) 3.52(4) ? . 3_666 C(22) H(3) 3.46(3) ? . 4_564 C(23) H(19) 2.92(3) ? . 4_665 C(24) H(3) 3.38(3) ? . 4_564 H(1) O(7) 2.64(3) ? . 3_667 H(1) C(2) 3.35(3) ? . 3_767 H(1) C(3) 3.18(3) ? . 3_767 H(1) C(4) 3.32(3) ? . 3_767 H(1) H(1) 3.47(5) ? . 3_767 H(1) H(25) 3.084 ? . 3_767 H(1) H(27) 3.396 ? . 3_767 H(2) O(3) 3.20(3) ? . 3_767 H(2) O(7) 3.17(3) ? . 3_667 H(2) O(9) 2.93(3) ? . 3_767 H(2) O(11) 2.81(3) ? . 3_767 H(2) C(2) 3.40(3) ? . 3_767 H(2) C(8) 3.52(3) ? . 3_767 H(2) C(11) 3.12(3) ? . 4_565 H(2) H(7) 2.96(5) ? . 3_767 H(2) H(10) 2.70(5) ? . 4_565 H(2) H(11) 2.71(5) ? . 4_565 H(2) H(21) 3.09(5) ? . 4_565 H(3) O(14) 2.78(3) ? . 4_565 H(3) N(2) 3.26(3) ? . 4_565 H(3) C(11) 3.39(3) ? . 4_565 H(3) C(20) 3.17(3) ? . 4_565 H(3) C(22) 3.46(3) ? . 4_565 H(3) C(24) 3.38(3) ? . 4_565 H(3) H(7) 2.95(5) ? . 3_767 H(3) H(10) 2.82(5) ? . 4_565 H(3) H(11) 3.57(5) ? . 4_565 H(3) H(21) 3.19(5) ? . 4_565 H(3) H(29) 2.663 ? . 4_565 H(4) O(12) 3.26(3) ? . 4_565 H(4) O(13) 3.33(3) ? . 4_565 H(4) O(14) 3.16(3) ? . 4_565 H(4) H(29) 3.496 ? . 4_565 H(4) H(30) 3.587 ? . 4_565 H(5) C(18) 3.32(4) ? . 2_646 H(5) H(20) 2.95(5) ? . 2_646 H(5) H(21) 3.23(5) ? . 2_646 H(5) H(29) 3.310 ? . 2_746 H(6) O(7) 3.20(4) ? . 3_667 H(6) C(18) 3.23(4) ? . 2_646 H(6) H(6) 3.35(6) ? . 3_667 H(6) H(20) 2.62(6) ? . 2_646 H(7) C(4) 2.97(4) ? . 3_767 H(7) C(5) 2.95(4) ? . 3_767 H(7) H(2) 2.96(5) ? . 3_767 H(7) H(3) 2.95(5) ? . 3_767 H(7) H(20) 3.54(5) ? . 2_646 H(7) H(29) 3.186 ? . 2_746 H(8) O(10) 2.58(3) ? . 2_756 H(8) N(4) 3.43(3) ? . 2_756 H(9) O(12) 2.50(4) ? . 4_565 H(9) O(13) 2.80(4) ? . 4_565 H(9) N(5) 3.01(4) ? . 4_565 H(10) O(9) 3.13(3) ? . 2_756 H(10) O(10) 3.21(3) ? . 2_756 H(10) N(4) 3.42(3) ? . 2_756 H(10) C(4) 3.18(3) ? . 4_564 H(10) C(5) 3.23(3) ? . 4_564 H(10) H(2) 2.70(5) ? . 4_564 H(10) H(3) 2.82(5) ? . 4_564 H(11) O(6) 3.17(3) ? . 2_656 H(11) O(7) 2.77(3) ? . 2_656 H(11) N(3) 3.32(3) ? . 2_656 H(11) C(4) 3.12(3) ? . 4_564 H(11) C(5) 3.59(3) ? . 4_564 H(11) H(2) 2.71(5) ? . 4_564 H(11) H(3) 3.57(5) ? . 4_564 H(11) H(22) 3.54(5) ? . 2_656 H(12) O(8) 3.34(4) ? . 2_756 H(12) O(9) 3.32(4) ? . 2_756 H(12) O(10) 3.05(4) ? . 2_756 H(12) O(11) 3.40(4) ? . 2_756 H(12) O(12) 3.35(4) ? . 2_756 H(12) O(13) 3.11(4) ? . 2_756 H(12) N(4) 2.99(4) ? . 2_756 H(12) N(5) 3.03(4) ? . 2_756 H(12) C(12) 3.11(3) ? . 3_777 H(12) H(12) 3.12(5) ? . 3_777 H(12) H(13) 2.25(5) ? . 3_777 H(12) H(14) 3.43(5) ? . 3_777 H(13) O(8) 3.18(4) ? . 4_565 H(13) O(12) 3.02(4) ? . 4_565 H(13) O(13) 3.58(4) ? . 4_565 H(13) N(5) 3.46(4) ? . 4_565 H(13) C(12) 2.76(4) ? . 3_777 H(13) H(12) 2.25(5) ? . 3_777 H(13) H(13) 2.39(6) ? . 3_777 H(13) H(14) 3.09(5) ? . 3_777 H(13) H(22) 3.41(5) ? . 2_656 H(13) H(23) 3.24(6) ? . 2_656 H(14) O(11) 3.50(4) ? . 2_756 H(14) O(13) 2.53(4) ? . 2_756 H(14) N(5) 3.02(4) ? . 2_756 H(14) C(21) 2.97(4) ? . 2_656 H(14) H(12) 3.43(5) ? . 3_777 H(14) H(13) 3.09(5) ? . 3_777 H(14) H(22) 2.65(5) ? . 2_656 H(14) H(23) 2.52(6) ? . 2_656 H(14) H(24) 3.44(6) ? . 2_656 H(15) C(15) 3.33(4) ? . 4_565 H(15) C(16) 2.83(4) ? . 4_565 H(15) C(17) 3.24(4) ? . 4_565 H(15) H(18) 2.80(5) ? . 4_565 H(15) H(19) 3.43(5) ? . 4_565 H(15) H(24) 3.36(6) ? . 4_565 H(16) O(6) 3.00(4) ? . 2_656 H(16) O(8) 3.23(5) ? . 2_656 H(16) O(10) 3.54(5) ? . 2_656 H(16) N(4) 3.46(5) ? . 2_656 H(16) C(21) 3.16(5) ? . 2_656 H(16) H(18) 3.31(6) ? . 4_565 H(16) H(22) 2.23(6) ? . 2_656 H(16) H(24) 3.36(6) ? . 2_656 H(16) H(24) 2.90(7) ? . 4_565 H(17) O(4) 2.90(4) ? . 4_565 H(17) O(8) 3.08(4) ? . 4_565 H(17) O(12) 2.88(3) ? . 4_565 H(17) C(15) 2.94(4) ? . 4_565 H(17) C(16) 3.06(4) ? . 4_565 H(17) C(21) 3.19(4) ? . 4_565 H(17) H(18) 3.07(5) ? . 4_565 H(17) H(22) 3.07(5) ? . 2_656 H(17) H(24) 3.55(5) ? . 2_656 H(17) H(24) 2.59(5) ? . 4_565 H(18) O(10) 2.55(3) ? . 3_666 H(18) N(4) 3.53(3) ? . 3_666 H(18) C(13) 3.28(4) ? . 4_564 H(18) H(15) 2.80(5) ? . 4_564 H(18) H(16) 3.31(6) ? . 4_564 H(18) H(17) 3.07(5) ? . 4_564 H(18) H(26) 3.265 ? . 4_464 H(19) O(5) 3.04(4) ? . 4_564 H(19) C(23) 2.92(3) ? . 4_464 H(19) H(15) 3.43(5) ? . 4_564 H(19) H(26) 2.525 ? . 4_464 H(19) H(27) 2.478 ? . 4_464 H(19) H(28) 3.064 ? . 4_464 H(20) C(1) 3.23(3) ? . 4_564 H(20) C(2) 3.38(3) ? . 4_564 H(20) C(6) 3.34(3) ? . 4_564 H(20) C(8) 3.20(3) ? . 2_656 H(20) H(5) 2.95(5) ? . 2_656 H(20) H(6) 2.62(6) ? . 2_656 H(20) H(7) 3.54(5) ? . 2_656 H(21) O(6) 3.25(3) ? . 2_656 H(21) O(7) 2.84(3) ? . 2_656 H(21) N(3) 3.42(3) ? . 2_656 H(21) C(3) 3.38(3) ? . 4_564 H(21) C(4) 2.88(3) ? . 4_564 H(21) C(5) 2.96(3) ? . 4_564 H(21) C(6) 3.55(3) ? . 4_564 H(21) H(2) 3.09(5) ? . 4_564 H(21) H(3) 3.19(5) ? . 4_564 H(21) H(5) 3.23(5) ? . 2_656 H(22) C(12) 3.30(4) ? . 2_646 H(22) C(13) 3.00(4) ? . 2_646 H(22) H(11) 3.54(5) ? . 2_646 H(22) H(13) 3.41(5) ? . 2_646 H(22) H(14) 2.65(5) ? . 2_646 H(22) H(16) 2.23(6) ? . 2_646 H(22) H(17) 3.07(5) ? . 2_646 H(22) H(24) 3.14(6) ? . 3_666 H(23) O(10) 3.23(4) ? . 3_666 H(23) O(13) 2.77(4) ? . 1_455 H(23) C(12) 3.31(4) ? . 2_646 H(23) H(13) 3.24(6) ? . 2_646 H(23) H(14) 2.52(6) ? . 2_646 H(23) H(30) 3.117 ? . 1_455 H(24) O(8) 2.71(4) ? . 3_666 H(24) O(10) 2.92(4) ? . 3_666 H(24) N(4) 3.19(4) ? . 3_666 H(24) C(13) 3.14(4) ? . 4_564 H(24) C(21) 3.52(4) ? . 3_666 H(24) H(14) 3.44(6) ? . 2_646 H(24) H(15) 3.36(6) ? . 4_564 H(24) H(16) 3.36(6) ? . 2_646 H(24) H(16) 2.90(7) ? . 4_564 H(24) H(17) 3.55(5) ? . 2_646 H(24) H(17) 2.59(5) ? . 4_564 H(24) H(22) 3.14(6) ? . 3_666 H(24) H(24) 2.95(5) ? . 3_666 H(25) O(7) 3.519 ? . 1_655 H(25) H(1) 3.084 ? . 3_767 H(26) C(16) 3.579 ? . 4_665 H(26) C(17) 3.163 ? . 4_665 H(26) H(18) 3.265 ? . 4_665 H(26) H(19) 2.525 ? . 4_665 H(27) O(5) 2.731 ? . 1_655 H(27) O(7) 2.815 ? . 1_655 H(27) N(3) 3.084 ? . 1_655 H(27) C(17) 3.388 ? . 4_665 H(27) H(1) 3.396 ? . 3_767 H(27) H(19) 2.478 ? . 4_665 H(28) O(5) 3.582 ? . 1_655 H(28) O(10) 3.191 ? . 2_756 H(28) C(14) 3.438 ? . 1_655 H(28) H(19) 3.064 ? . 4_665 H(29) O(9) 3.330 ? . 2_756 H(29) O(10) 3.309 ? . 2_756 H(29) C(5) 3.468 ? . 4_564 H(29) H(3) 2.663 ? . 4_564 H(29) H(4) 3.496 ? . 4_564 H(29) H(5) 3.310 ? . 2_756 H(29) H(7) 3.186 ? . 2_756 H(30) O(4) 3.435 ? . 1_655 H(30) C(14) 3.311 ? . 1_655 H(30) C(15) 3.033 ? . 1_655 H(30) C(16) 3.285 ? . 1_655 H(30) H(4) 3.587 ? . 4_564 H(30) H(23) 3.117 ? . 1_655 Ho(1) Cu(1) 3.499(2) ? . . data___ErCu _database_code_depnum_ccdc_archive 'CCDC 881974' #TrackingRef '11258_web_deposit_cif_file_3_TakayukiIshida_1336987557.ErCu_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Cu Er N5 O14 ' _chemical_formula_moiety 'C24 H30 Cu Er N5 O14 ' _chemical_formula_weight 843.33 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.635(5) _cell_length_b 19.833(4) _cell_length_c 15.689(4) _cell_angle_alpha 90.0000 _cell_angle_beta 95.471(2) _cell_angle_gamma 90.0000 _cell_volume 2984.4(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 440 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672.00 _exptl_absorpt_coefficient_mu 3.577 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.207 _exptl_absorpt_correction_T_max 0.489 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 50659 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_ambient_temperature 100. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6831 _reflns_number_gt 6475 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0319 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6831 _refine_ls_number_parameters 509 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.87 _refine_diff_density_min -1.04 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 34(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Er Er -0.259 4.958 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Er(1) Er 0.696380(10) 0.576330(10) 0.745320(10) 0.01179(3) Uani 1.00 1 d . . . Cu(1) Cu 0.79030(3) 0.73775(2) 0.81873(2) 0.01202(7) Uani 1.00 1 d . . . O(1) O 0.7813(2) 0.64508(9) 0.86063(11) 0.0163(4) Uani 1.00 1 d . . . O(2) O 0.6712(2) 0.69334(9) 0.72798(11) 0.0165(4) Uani 1.00 1 d . . . O(3) O 0.7366(2) 0.51725(9) 0.88722(12) 0.0183(4) Uani 1.00 1 d . . . O(4) O 0.52021(19) 0.61289(9) 0.62761(11) 0.0160(4) Uani 1.00 1 d . . . O(5) O 0.4912(2) 0.60220(10) 0.82147(13) 0.0216(5) Uani 1.00 1 d . . . O(6) O 0.4981(2) 0.50555(10) 0.75827(12) 0.0213(5) Uani 1.00 1 d . . . O(7) O 0.3291(2) 0.52775(12) 0.83766(17) 0.0407(7) Uani 1.00 1 d . . . O(8) O 0.6739(2) 0.49625(11) 0.62192(13) 0.0338(6) Uani 1.00 1 d . . . O(9) O 0.7811(2) 0.45721(11) 0.73639(13) 0.0307(6) Uani 1.00 1 d . . . O(10) O 0.7468(2) 0.39201(11) 0.62454(14) 0.0279(5) Uani 1.00 1 d . . . O(11) O 0.9480(2) 0.57206(12) 0.75724(16) 0.0338(6) Uani 1.00 1 d . . . O(12) O 0.8508(2) 0.61135(15) 0.64128(14) 0.0413(7) Uani 1.00 1 d . . . O(13) O 1.0769(2) 0.61240(11) 0.66136(14) 0.0281(5) Uani 1.00 1 d . . . O(14) O 1.0087(2) 0.74421(10) 0.74852(13) 0.0227(5) Uani 1.00 1 d . . . N(1) N 0.8840(2) 0.77030(11) 0.92960(14) 0.0148(5) Uani 1.00 1 d . . . N(2) N 0.7655(2) 0.82714(11) 0.76254(13) 0.0149(5) Uani 1.00 1 d . . . N(3) N 0.4354(2) 0.54496(12) 0.80687(16) 0.0216(6) Uani 1.00 1 d . . . N(4) N 0.7339(2) 0.44663(12) 0.65999(15) 0.0181(5) Uani 1.00 1 d . . . N(5) N 0.9629(2) 0.59874(12) 0.68565(16) 0.0208(6) Uani 1.00 1 d . . . C(1) C 0.8278(2) 0.62097(13) 0.93761(16) 0.0146(6) Uani 1.00 1 d . . . C(2) C 0.8075(2) 0.55254(14) 0.95434(16) 0.0158(6) Uani 1.00 1 d . . . C(3) C 0.8562(3) 0.52334(14) 1.03142(17) 0.0193(6) Uani 1.00 1 d . . . C(4) C 0.9268(3) 0.56325(16) 1.09576(18) 0.0214(7) Uani 1.00 1 d . . . C(5) C 0.9433(3) 0.63040(15) 1.08224(17) 0.0201(7) Uani 1.00 1 d . . . C(6) C 0.8936(2) 0.66083(14) 1.00324(16) 0.0168(6) Uani 1.00 1 d . . . C(7) C 0.9136(3) 0.73250(14) 0.99593(17) 0.0185(6) Uani 1.00 1 d . . . C(8) C 0.6913(3) 0.44988(15) 0.9078(2) 0.0258(8) Uani 1.00 1 d . . . C(9) C 0.9309(3) 0.84125(14) 0.94142(18) 0.0190(6) Uani 1.00 1 d . . . C(10) C 0.8348(2) 0.89287(13) 0.89571(17) 0.0167(6) Uani 1.00 1 d . . . C(11) C 0.8395(3) 0.88658(14) 0.79926(18) 0.0179(6) Uani 1.00 1 d . . . C(12) C 0.8928(3) 0.96233(15) 0.9213(2) 0.0227(7) Uani 1.00 1 d . . . C(13) C 0.6855(3) 0.88581(15) 0.9202(2) 0.0225(7) Uani 1.00 1 d . . . C(14) C 0.6071(2) 0.72146(13) 0.65797(16) 0.0129(5) Uani 1.00 1 d . . . C(15) C 0.5242(2) 0.67936(13) 0.60072(16) 0.0145(6) Uani 1.00 1 d . . . C(16) C 0.4567(2) 0.70341(14) 0.52514(18) 0.0190(6) Uani 1.00 1 d . . . C(17) C 0.4716(3) 0.77170(15) 0.50372(19) 0.0220(7) Uani 1.00 1 d . . . C(18) C 0.5476(3) 0.81374(14) 0.55891(18) 0.0201(7) Uani 1.00 1 d . . . C(19) C 0.6145(2) 0.78968(14) 0.63719(16) 0.0152(6) Uani 1.00 1 d . . . C(20) C 0.6909(2) 0.83815(14) 0.69159(17) 0.0164(6) Uani 1.00 1 d . . . C(21) C 0.4154(3) 0.57135(15) 0.5806(2) 0.0243(8) Uani 1.00 1 d . . . C(22) C 1.1280(3) 0.72987(15) 0.7740(2) 0.0247(7) Uani 1.00 1 d . . . C(23) C 1.1605(3) 0.68771(17) 0.8525(2) 0.0315(8) Uani 1.00 1 d . . . C(24) C 1.2496(3) 0.7543(2) 0.7298(2) 0.0448(11) Uani 1.00 1 d . . . H(1) H 0.850(3) 0.4781(15) 1.0442(18) 0.020(7) Uiso 1.00 1 d . . . H(2) H 0.961(3) 0.5443(16) 1.149(2) 0.026(8) Uiso 1.00 1 d . . . H(3) H 0.990(3) 0.6605(17) 1.123(2) 0.036(9) Uiso 1.00 1 d . . . H(4) H 0.958(3) 0.7549(15) 1.0474(19) 0.021(8) Uiso 1.00 1 d . . . H(5) H 0.637(3) 0.4322(14) 0.860(2) 0.017(8) Uiso 1.00 1 d . . . H(6) H 0.636(3) 0.4541(16) 0.961(2) 0.031(9) Uiso 1.00 1 d . . . H(7) H 0.777(3) 0.4216(15) 0.922(2) 0.032(10) Uiso 1.00 1 d . . . H(8) H 1.020(3) 0.8464(14) 0.9222(18) 0.016(7) Uiso 1.00 1 d . . . H(9) H 0.937(3) 0.8508(17) 0.999(2) 0.032(9) Uiso 1.00 1 d . . . H(10) H 0.933(3) 0.8846(15) 0.7880(18) 0.019(8) Uiso 1.00 1 d . . . H(11) H 0.794(3) 0.9282(15) 0.771(2) 0.024(9) Uiso 1.00 1 d . . . H(12) H 0.994(3) 0.9693(16) 0.906(2) 0.026(8) Uiso 1.00 1 d . . . H(13) H 0.890(3) 0.9684(18) 0.982(2) 0.048(11) Uiso 1.00 1 d . . . H(14) H 0.840(3) 1.0015(18) 0.892(2) 0.039(10) Uiso 1.00 1 d . . . H(15) H 0.650(3) 0.8401(16) 0.9128(18) 0.022(8) Uiso 1.00 1 d . . . H(16) H 0.620(4) 0.915(2) 0.886(2) 0.064(14) Uiso 1.00 1 d . . . H(17) H 0.682(3) 0.8964(15) 0.983(2) 0.021(8) Uiso 1.00 1 d . . . H(18) H 0.403(3) 0.6751(15) 0.4872(19) 0.023(8) Uiso 1.00 1 d . . . H(19) H 0.428(3) 0.7868(15) 0.450(2) 0.026(8) Uiso 1.00 1 d . . . H(20) H 0.563(3) 0.8587(16) 0.547(2) 0.028(8) Uiso 1.00 1 d . . . H(21) H 0.690(2) 0.8794(14) 0.6687(17) 0.011(7) Uiso 1.00 1 d . . . H(22) H 0.425(3) 0.5268(18) 0.610(2) 0.037(10) Uiso 1.00 1 d . . . H(23) H 0.321(3) 0.5946(14) 0.5785(18) 0.014(7) Uiso 1.00 1 d . . . H(24) H 0.440(3) 0.5673(16) 0.520(2) 0.031(9) Uiso 1.00 1 d . . . H(25) H 1.0857 0.6574 0.8585 0.038 Uiso 1.00 1 c R . . H(26) H 1.1729 0.7161 0.9014 0.037 Uiso 1.00 1 c R . . H(27) H 1.2436 0.6628 0.8475 0.037 Uiso 1.00 1 c R . . H(28) H 1.3277 0.7608 0.7707 0.055 Uiso 1.00 1 c R . . H(29) H 1.2263 0.7959 0.7019 0.055 Uiso 1.00 1 c R . . H(30) H 1.2718 0.7219 0.6888 0.055 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er(1) 0.01421(8) 0.01008(8) 0.01114(8) -0.00113(4) 0.00147(5) -0.00120(4) Cu(1) 0.01512(16) 0.01039(16) 0.01030(15) -0.00110(12) -0.00011(12) -0.00117(11) O(1) 0.0238(10) 0.0123(8) 0.0119(8) -0.0012(7) -0.0032(7) 0.0008(7) O(2) 0.0231(9) 0.0119(9) 0.0132(8) -0.0035(7) -0.0049(7) 0.0002(7) O(3) 0.0280(10) 0.0125(9) 0.0144(9) -0.0023(7) 0.0022(7) 0.0009(7) O(4) 0.0178(9) 0.0123(8) 0.0167(9) -0.0024(7) -0.0043(7) -0.0027(7) O(5) 0.0233(10) 0.0164(10) 0.0263(10) -0.0036(8) 0.0088(8) -0.0056(8) O(6) 0.0221(10) 0.0182(10) 0.0244(10) -0.0025(8) 0.0073(8) -0.0045(8) O(7) 0.0335(13) 0.0337(13) 0.0599(16) -0.0130(11) 0.0307(12) -0.0097(12) O(8) 0.0538(15) 0.0280(12) 0.0185(10) 0.0204(11) -0.0018(10) -0.0039(9) O(9) 0.0429(13) 0.0286(12) 0.0185(10) 0.0124(10) -0.0087(9) -0.0086(9) O(10) 0.0291(11) 0.0186(10) 0.0356(12) 0.0020(8) 0.0004(9) -0.0142(9) O(11) 0.0230(12) 0.0498(16) 0.0289(12) 0.0019(10) 0.0038(9) 0.0182(10) O(12) 0.0194(11) 0.082(2) 0.0225(11) 0.0006(12) 0.0037(9) 0.0179(12) O(13) 0.0219(11) 0.0264(11) 0.0387(12) -0.0070(8) 0.0168(9) -0.0115(9) O(14) 0.0193(10) 0.0224(10) 0.0268(10) 0.0019(8) 0.0037(8) -0.0019(8) N(1) 0.0171(11) 0.0143(10) 0.0130(10) -0.0007(8) 0.0012(8) -0.0026(8) N(2) 0.0177(11) 0.0126(10) 0.0144(10) -0.0028(9) 0.0018(8) -0.0007(8) N(3) 0.0197(12) 0.0209(12) 0.0252(12) -0.0034(9) 0.0079(9) 0.0009(10) N(4) 0.0182(11) 0.0153(11) 0.0211(11) -0.0016(9) 0.0036(9) -0.0053(9) N(5) 0.0211(12) 0.0170(11) 0.0253(12) -0.0030(9) 0.0068(10) -0.0092(10) C(1) 0.0152(12) 0.0181(13) 0.0109(11) 0.0035(10) 0.0028(9) 0.0011(9) C(2) 0.0188(13) 0.0177(13) 0.0112(11) 0.0016(10) 0.0033(9) -0.0015(10) C(3) 0.0259(14) 0.0167(13) 0.0160(12) 0.0062(11) 0.0063(10) 0.0040(10) C(4) 0.0260(15) 0.0274(14) 0.0115(12) 0.0097(12) 0.0043(11) 0.0030(11) C(5) 0.0234(14) 0.0254(15) 0.0113(12) 0.0055(12) 0.0005(10) -0.0026(11) C(6) 0.0195(13) 0.0192(13) 0.0116(12) 0.0035(10) 0.0013(10) -0.0008(10) C(7) 0.0207(13) 0.0206(14) 0.0139(12) -0.0002(11) -0.0008(10) -0.0055(10) C(8) 0.0352(18) 0.0175(15) 0.0248(15) -0.0074(13) 0.0033(13) 0.0042(12) C(9) 0.0227(14) 0.0157(13) 0.0182(13) -0.0056(11) 0.0004(11) -0.0042(10) C(10) 0.0206(13) 0.0114(12) 0.0184(12) -0.0037(10) 0.0039(10) -0.0046(10) C(11) 0.0205(14) 0.0134(12) 0.0197(13) -0.0060(10) 0.0013(11) -0.0009(10) C(12) 0.0271(15) 0.0166(14) 0.0253(15) -0.0077(12) 0.0077(12) -0.0073(11) C(13) 0.0231(15) 0.0165(14) 0.0295(16) -0.0015(11) 0.0102(12) -0.0054(12) C(14) 0.0102(11) 0.0173(12) 0.0108(11) -0.0009(9) -0.0004(9) 0.0026(9) C(15) 0.0137(12) 0.0136(12) 0.0161(12) 0.0001(9) 0.0014(9) -0.0019(9) C(16) 0.0171(13) 0.0196(14) 0.0193(13) 0.0026(10) -0.0036(10) -0.0046(11) C(17) 0.0208(14) 0.0234(15) 0.0205(14) 0.0052(11) -0.0040(11) 0.0037(11) C(18) 0.0209(14) 0.0161(13) 0.0229(14) 0.0032(11) -0.0007(11) 0.0057(11) C(19) 0.0141(12) 0.0172(13) 0.0140(12) 0.0007(10) 0.0005(9) 0.0007(10) C(20) 0.0187(13) 0.0117(12) 0.0189(13) -0.0002(10) 0.0027(10) 0.0031(10) C(21) 0.0213(15) 0.0198(15) 0.0293(17) -0.0076(11) -0.0102(13) -0.0039(11) C(22) 0.0191(14) 0.0217(14) 0.0342(16) -0.0031(11) 0.0072(12) -0.0132(12) C(23) 0.0222(15) 0.0413(19) 0.0298(16) 0.0073(14) -0.0031(12) -0.0072(14) C(24) 0.0294(19) 0.045(2) 0.064(2) 0.0009(17) 0.0213(18) -0.0045(19) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Er(1) O(1) 2.3495(17) yes . . Er(1) O(2) 2.3464(17) yes . . Er(1) O(3) 2.5130(18) yes . . Er(1) O(4) 2.4939(17) yes . . Er(1) O(5) 2.460(2) yes . . Er(1) O(6) 2.3952(19) yes . . Er(1) O(8) 2.498(2) yes . . Er(1) O(9) 2.508(2) yes . . Er(1) O(11) 2.415(2) yes . . Er(1) O(12) 2.413(2) yes . . Cu(1) O(1) 1.9566(18) yes . . Cu(1) O(2) 1.9513(17) yes . . Cu(1) O(14) 2.470(2) yes . . Cu(1) N(1) 1.989(2) yes . . Cu(1) N(2) 1.984(2) yes . . O(1) C(1) 1.336(2) yes . . O(2) C(14) 1.330(2) yes . . O(3) C(2) 1.389(3) yes . . O(3) C(8) 1.452(3) yes . . O(4) C(15) 1.386(3) yes . . O(4) C(21) 1.449(3) yes . . O(5) N(3) 1.267(3) yes . . O(6) N(3) 1.282(3) yes . . O(7) N(3) 1.222(3) yes . . O(8) N(4) 1.263(3) yes . . O(9) N(4) 1.258(3) yes . . O(10) N(4) 1.229(3) yes . . O(11) N(5) 1.262(3) yes . . O(12) N(5) 1.253(3) yes . . O(13) N(5) 1.227(3) yes . . O(14) C(22) 1.214(3) yes . . N(1) C(7) 1.292(3) yes . . N(1) C(9) 1.484(3) yes . . N(2) C(11) 1.467(3) yes . . N(2) C(20) 1.285(3) yes . . C(1) C(2) 1.400(3) yes . . C(1) C(6) 1.401(3) yes . . C(2) C(3) 1.382(3) yes . . C(3) C(4) 1.406(3) yes . . C(4) C(5) 1.360(4) yes . . C(5) C(6) 1.420(3) yes . . C(6) C(7) 1.441(3) yes . . C(9) C(10) 1.514(3) yes . . C(10) C(11) 1.523(3) yes . . C(10) C(12) 1.526(3) yes . . C(10) C(13) 1.530(4) yes . . C(14) C(15) 1.416(3) yes . . C(14) C(19) 1.395(3) yes . . C(15) C(16) 1.382(3) yes . . C(16) C(17) 1.406(4) yes . . C(17) C(18) 1.364(3) yes . . C(18) C(19) 1.414(3) yes . . C(19) C(20) 1.440(3) yes . . C(22) C(23) 1.497(4) yes . . C(22) C(24) 1.498(5) yes . . C(3) H(1) 0.92(3) no . . C(4) H(2) 0.95(3) no . . C(5) H(3) 0.95(3) no . . C(7) H(4) 0.98(3) no . . C(8) H(5) 0.94(3) no . . C(8) H(6) 1.03(3) no . . C(8) H(7) 1.01(3) no . . C(9) H(8) 0.95(3) no . . C(9) H(9) 0.92(3) no . . C(11) H(10) 0.93(3) no . . C(11) H(11) 1.02(3) no . . C(12) H(12) 1.03(3) no . . C(12) H(13) 0.96(3) no . . C(12) H(14) 1.01(3) no . . C(13) H(15) 0.97(3) no . . C(13) H(16) 0.97(4) no . . C(13) H(17) 1.01(3) no . . C(16) H(18) 0.94(2) no . . C(17) H(19) 0.96(3) no . . C(18) H(20) 0.93(3) no . . C(20) H(21) 0.89(2) no . . C(21) H(22) 1.00(3) no . . C(21) H(23) 1.01(3) no . . C(21) H(24) 1.00(3) no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Er(1) O(2) 62.60(5) yes . . . O(1) Er(1) O(3) 64.88(5) yes . . . O(1) Er(1) O(4) 124.34(6) yes . . . O(1) Er(1) O(5) 75.06(6) yes . . . O(1) Er(1) O(6) 119.80(6) yes . . . O(1) Er(1) O(8) 164.60(7) yes . . . O(1) Er(1) O(9) 119.89(6) yes . . . O(1) Er(1) O(11) 71.77(7) yes . . . O(1) Er(1) O(12) 99.31(7) yes . . . O(2) Er(1) O(3) 124.71(5) yes . . . O(2) Er(1) O(4) 64.60(5) yes . . . O(2) Er(1) O(5) 76.77(6) yes . . . O(2) Er(1) O(6) 121.00(6) yes . . . O(2) Er(1) O(8) 122.59(6) yes . . . O(2) Er(1) O(9) 162.90(7) yes . . . O(2) Er(1) O(11) 97.79(7) yes . . . O(2) Er(1) O(12) 72.57(8) yes . . . O(3) Er(1) O(4) 145.91(6) yes . . . O(3) Er(1) O(5) 74.35(6) yes . . . O(3) Er(1) O(6) 73.05(6) yes . . . O(3) Er(1) O(8) 112.64(6) yes . . . O(3) Er(1) O(9) 65.59(6) yes . . . O(3) Er(1) O(11) 81.15(7) yes . . . O(3) Er(1) O(12) 132.88(7) yes . . . O(4) Er(1) O(5) 77.13(6) yes . . . O(4) Er(1) O(6) 74.99(6) yes . . . O(4) Er(1) O(8) 66.93(6) yes . . . O(4) Er(1) O(9) 115.77(6) yes . . . O(4) Er(1) O(11) 132.44(7) yes . . . O(4) Er(1) O(12) 80.53(6) yes . . . O(5) Er(1) O(6) 52.87(6) yes . . . O(5) Er(1) O(8) 119.65(7) yes . . . O(5) Er(1) O(9) 120.31(7) yes . . . O(5) Er(1) O(11) 144.80(7) yes . . . O(5) Er(1) O(12) 147.62(8) yes . . . O(6) Er(1) O(8) 71.46(7) yes . . . O(6) Er(1) O(9) 73.69(7) yes . . . O(6) Er(1) O(11) 140.89(7) yes . . . O(6) Er(1) O(12) 140.75(7) yes . . . O(8) Er(1) O(9) 50.38(6) yes . . . O(8) Er(1) O(11) 92.87(8) yes . . . O(8) Er(1) O(12) 70.87(8) yes . . . O(9) Er(1) O(11) 69.00(7) yes . . . O(9) Er(1) O(12) 90.48(8) yes . . . O(11) Er(1) O(12) 51.93(7) yes . . . O(1) Cu(1) O(2) 77.26(7) yes . . . O(1) Cu(1) O(14) 105.39(7) yes . . . O(1) Cu(1) N(1) 92.40(8) yes . . . O(1) Cu(1) N(2) 168.88(8) yes . . . O(2) Cu(1) O(14) 99.47(7) yes . . . O(2) Cu(1) N(1) 166.08(8) yes . . . O(2) Cu(1) N(2) 92.38(7) yes . . . O(14) Cu(1) N(1) 92.20(8) yes . . . O(14) Cu(1) N(2) 80.05(8) yes . . . N(1) Cu(1) N(2) 97.12(8) yes . . . Er(1) O(1) Cu(1) 108.04(7) yes . . . Er(1) O(1) C(1) 123.40(15) yes . . . Cu(1) O(1) C(1) 128.19(15) yes . . . Er(1) O(2) Cu(1) 108.35(7) yes . . . Er(1) O(2) C(14) 123.03(15) yes . . . Cu(1) O(2) C(14) 127.43(16) yes . . . Er(1) O(3) C(2) 117.39(15) yes . . . Er(1) O(3) C(8) 127.03(16) yes . . . C(2) O(3) C(8) 115.6(2) yes . . . Er(1) O(4) C(15) 117.72(13) yes . . . Er(1) O(4) C(21) 127.11(15) yes . . . C(15) O(4) C(21) 115.12(19) yes . . . Er(1) O(5) N(3) 94.11(15) yes . . . Er(1) O(6) N(3) 96.76(14) yes . . . Er(1) O(8) N(4) 97.29(15) yes . . . Er(1) O(9) N(4) 96.91(15) yes . . . Er(1) O(11) N(5) 96.58(16) yes . . . Er(1) O(12) N(5) 96.94(17) yes . . . Cu(1) O(14) C(22) 131.4(2) yes . . . Cu(1) N(1) C(7) 124.26(18) yes . . . Cu(1) N(1) C(9) 121.62(16) yes . . . C(7) N(1) C(9) 114.1(2) yes . . . Cu(1) N(2) C(11) 120.66(16) yes . . . Cu(1) N(2) C(20) 124.79(18) yes . . . C(11) N(2) C(20) 114.5(2) yes . . . O(5) N(3) O(6) 116.0(2) yes . . . O(5) N(3) O(7) 122.4(2) yes . . . O(6) N(3) O(7) 121.6(2) yes . . . O(8) N(4) O(9) 115.4(2) yes . . . O(8) N(4) O(10) 122.3(2) yes . . . O(9) N(4) O(10) 122.3(2) yes . . . O(11) N(5) O(12) 114.4(2) yes . . . O(11) N(5) O(13) 123.4(2) yes . . . O(12) N(5) O(13) 122.2(2) yes . . . O(1) C(1) C(2) 118.4(2) yes . . . O(1) C(1) C(6) 123.5(2) yes . . . C(2) C(1) C(6) 118.1(2) yes . . . O(3) C(2) C(1) 114.5(2) yes . . . O(3) C(2) C(3) 123.6(2) yes . . . C(1) C(2) C(3) 121.9(2) yes . . . C(2) C(3) C(4) 119.5(2) yes . . . C(3) C(4) C(5) 119.7(2) yes . . . C(4) C(5) C(6) 121.2(2) yes . . . C(1) C(6) C(5) 119.5(2) yes . . . C(1) C(6) C(7) 123.6(2) yes . . . C(5) C(6) C(7) 116.9(2) yes . . . N(1) C(7) C(6) 128.0(2) yes . . . N(1) C(9) C(10) 114.6(2) yes . . . C(9) C(10) C(11) 109.9(2) yes . . . C(9) C(10) C(12) 107.1(2) yes . . . C(9) C(10) C(13) 111.5(2) yes . . . C(11) C(10) C(12) 106.9(2) yes . . . C(11) C(10) C(13) 111.1(2) yes . . . C(12) C(10) C(13) 110.2(2) yes . . . N(2) C(11) C(10) 113.4(2) yes . . . O(2) C(14) C(15) 117.8(2) yes . . . O(2) C(14) C(19) 124.7(2) yes . . . C(15) C(14) C(19) 117.5(2) yes . . . O(4) C(15) C(14) 113.5(2) yes . . . O(4) C(15) C(16) 124.4(2) yes . . . C(14) C(15) C(16) 122.1(2) yes . . . C(15) C(16) C(17) 119.2(2) yes . . . C(16) C(17) C(18) 119.9(2) yes . . . C(17) C(18) C(19) 121.2(2) yes . . . C(14) C(19) C(18) 120.1(2) yes . . . C(14) C(19) C(20) 122.9(2) yes . . . C(18) C(19) C(20) 117.0(2) yes . . . N(2) C(20) C(19) 127.7(2) yes . . . O(14) C(22) C(23) 121.3(2) yes . . . O(14) C(22) C(24) 122.0(2) yes . . . C(23) C(22) C(24) 116.7(2) yes . . . C(2) C(3) H(1) 125.1(17) no . . . C(4) C(3) H(1) 115.3(17) no . . . C(3) C(4) H(2) 121.1(19) no . . . C(5) C(4) H(2) 119.2(19) no . . . C(4) C(5) H(3) 124(2) no . . . C(6) C(5) H(3) 114(2) no . . . N(1) C(7) H(4) 116.4(17) no . . . C(6) C(7) H(4) 115.6(17) no . . . O(3) C(8) H(5) 108.9(18) no . . . O(3) C(8) H(6) 107.1(18) no . . . O(3) C(8) H(7) 107.8(19) no . . . H(5) C(8) H(6) 112(2) no . . . H(5) C(8) H(7) 111(2) no . . . H(6) C(8) H(7) 110(2) no . . . N(1) C(9) H(8) 109.8(17) no . . . N(1) C(9) H(9) 108(2) no . . . C(10) C(9) H(8) 108.1(17) no . . . C(10) C(9) H(9) 108(2) no . . . H(8) C(9) H(9) 108(2) no . . . N(2) C(11) H(10) 109.5(18) no . . . N(2) C(11) H(11) 108.0(17) no . . . C(10) C(11) H(10) 108.2(17) no . . . C(10) C(11) H(11) 108.4(18) no . . . H(10) C(11) H(11) 109(2) no . . . C(10) C(12) H(12) 113.0(17) no . . . C(10) C(12) H(13) 109(2) no . . . C(10) C(12) H(14) 114.6(19) no . . . H(12) C(12) H(13) 109(2) no . . . H(12) C(12) H(14) 104(2) no . . . H(13) C(12) H(14) 107(3) no . . . C(10) C(13) H(15) 112.5(18) no . . . C(10) C(13) H(16) 112(2) no . . . C(10) C(13) H(17) 109.9(17) no . . . H(15) C(13) H(16) 106(3) no . . . H(15) C(13) H(17) 106(2) no . . . H(16) C(13) H(17) 110(3) no . . . C(15) C(16) H(18) 121.7(19) no . . . C(17) C(16) H(18) 119.2(19) no . . . C(16) C(17) H(19) 117.8(18) no . . . C(18) C(17) H(19) 122.3(18) no . . . C(17) C(18) H(20) 123.1(19) no . . . C(19) C(18) H(20) 115.7(19) no . . . N(2) C(20) H(21) 119.2(17) no . . . C(19) C(20) H(21) 112.8(17) no . . . O(4) C(21) H(22) 103.8(19) no . . . O(4) C(21) H(23) 109.6(16) no . . . O(4) C(21) H(24) 108.1(19) no . . . H(22) C(21) H(23) 117(2) no . . . H(22) C(21) H(24) 110(2) no . . . H(23) C(21) H(24) 107(2) no . . . C(22) C(23) H(25) 109.5 no . . . C(22) C(23) H(26) 109.5 no . . . C(22) C(23) H(27) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . H(25) C(23) H(27) 109.5 no . . . H(26) C(23) H(27) 109.5 no . . . C(22) C(24) H(28) 109.6 no . . . C(22) C(24) H(29) 109.5 no . . . C(22) C(24) H(30) 109.3 no . . . H(28) C(24) H(29) 109.5 no . . . H(28) C(24) H(30) 109.5 no . . . H(29) C(24) H(30) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Er(1) O(2) Cu(1) 14.35(7) ? . . . . O(1) Er(1) O(2) C(14) -177.3(2) ? . . . . O(2) Er(1) O(1) Cu(1) -14.28(7) ? . . . . O(2) Er(1) O(1) C(1) 172.1(2) ? . . . . O(1) Er(1) O(3) C(2) -10.17(16) ? . . . . O(1) Er(1) O(3) C(8) 168.6(2) ? . . . . O(3) Er(1) O(1) Cu(1) -176.34(11) ? . . . . O(3) Er(1) O(1) C(1) 10.06(18) ? . . . . O(1) Er(1) O(4) C(15) 35.13(19) ? . . . . O(1) Er(1) O(4) C(21) -147.6(2) ? . . . . O(4) Er(1) O(1) Cu(1) -34.39(11) ? . . . . O(4) Er(1) O(1) C(1) 152.01(17) ? . . . . O(1) Er(1) O(5) N(3) -144.86(15) ? . . . . O(5) Er(1) O(1) Cu(1) -96.90(9) ? . . . . O(5) Er(1) O(1) C(1) 89.50(19) ? . . . . O(1) Er(1) O(6) N(3) 33.21(16) ? . . . . O(6) Er(1) O(1) Cu(1) -126.10(8) ? . . . . O(6) Er(1) O(1) C(1) 60.3(2) ? . . . . O(1) Er(1) O(8) N(4) 56.7(3) ? . . . . O(8) Er(1) O(1) Cu(1) 99.5(2) ? . . . . O(8) Er(1) O(1) C(1) -74.1(3) ? . . . . O(1) Er(1) O(9) N(4) -166.81(14) ? . . . . O(9) Er(1) O(1) Cu(1) 146.42(8) ? . . . . O(9) Er(1) O(1) C(1) -27.2(2) ? . . . . O(1) Er(1) O(11) N(5) -116.23(17) ? . . . . O(11) Er(1) O(1) Cu(1) 95.07(10) ? . . . . O(11) Er(1) O(1) C(1) -78.53(19) ? . . . . O(1) Er(1) O(12) N(5) 55.83(19) ? . . . . O(12) Er(1) O(1) Cu(1) 50.45(10) ? . . . . O(12) Er(1) O(1) C(1) -123.15(19) ? . . . . O(2) Er(1) O(3) C(2) -29.6(2) ? . . . . O(2) Er(1) O(3) C(8) 149.1(2) ? . . . . O(3) Er(1) O(2) Cu(1) 34.18(11) ? . . . . O(3) Er(1) O(2) C(14) -157.50(17) ? . . . . O(2) Er(1) O(4) C(15) 15.38(16) ? . . . . O(2) Er(1) O(4) C(21) -167.4(2) ? . . . . O(4) Er(1) O(2) Cu(1) 176.03(10) ? . . . . O(4) Er(1) O(2) C(14) -15.65(17) ? . . . . O(2) Er(1) O(5) N(3) 150.38(15) ? . . . . O(5) Er(1) O(2) Cu(1) 94.18(8) ? . . . . O(5) Er(1) O(2) C(14) -97.50(19) ? . . . . O(2) Er(1) O(6) N(3) -40.86(16) ? . . . . O(6) Er(1) O(2) Cu(1) 124.33(8) ? . . . . O(6) Er(1) O(2) C(14) -67.4(2) ? . . . . O(2) Er(1) O(8) N(4) 162.04(15) ? . . . . O(8) Er(1) O(2) Cu(1) -148.89(8) ? . . . . O(8) Er(1) O(2) C(14) 19.4(2) ? . . . . O(2) Er(1) O(9) N(4) -73.2(2) ? . . . . O(9) Er(1) O(2) Cu(1) -88.6(2) ? . . . . O(9) Er(1) O(2) C(14) 79.7(2) ? . . . . O(2) Er(1) O(11) N(5) -58.51(16) ? . . . . O(11) Er(1) O(2) Cu(1) -50.41(10) ? . . . . O(11) Er(1) O(2) C(14) 117.90(19) ? . . . . O(2) Er(1) O(12) N(5) 113.14(18) ? . . . . O(12) Er(1) O(2) Cu(1) -96.36(9) ? . . . . O(12) Er(1) O(2) C(14) 71.95(19) ? . . . . O(3) Er(1) O(4) C(15) 130.41(16) ? . . . . O(3) Er(1) O(4) C(21) -52.3(2) ? . . . . O(4) Er(1) O(3) C(2) -124.93(17) ? . . . . O(4) Er(1) O(3) C(8) 53.8(2) ? . . . . O(3) Er(1) O(5) N(3) -77.29(14) ? . . . . O(5) Er(1) O(3) C(2) -90.71(18) ? . . . . O(5) Er(1) O(3) C(8) 88.0(2) ? . . . . O(3) Er(1) O(6) N(3) 79.89(14) ? . . . . O(6) Er(1) O(3) C(2) -145.97(18) ? . . . . O(6) Er(1) O(3) C(8) 32.8(2) ? . . . . O(3) Er(1) O(8) N(4) -20.70(18) ? . . . . O(8) Er(1) O(3) C(2) 153.19(17) ? . . . . O(8) Er(1) O(3) C(8) -28.1(2) ? . . . . O(3) Er(1) O(9) N(4) 156.19(18) ? . . . . O(9) Er(1) O(3) C(2) 134.64(19) ? . . . . O(9) Er(1) O(3) C(8) -46.6(2) ? . . . . O(3) Er(1) O(11) N(5) 177.42(17) ? . . . . O(11) Er(1) O(3) C(2) 63.77(18) ? . . . . O(11) Er(1) O(3) C(8) -117.5(2) ? . . . . O(3) Er(1) O(12) N(5) -8.4(2) ? . . . . O(12) Er(1) O(3) C(2) 68.8(2) ? . . . . O(12) Er(1) O(3) C(8) -112.5(2) ? . . . . O(4) Er(1) O(5) N(3) 83.85(14) ? . . . . O(5) Er(1) O(4) C(15) 96.67(17) ? . . . . O(5) Er(1) O(4) C(21) -86.1(2) ? . . . . O(4) Er(1) O(6) N(3) -88.08(14) ? . . . . O(6) Er(1) O(4) C(15) 151.24(17) ? . . . . O(6) Er(1) O(4) C(21) -31.5(2) ? . . . . O(4) Er(1) O(8) N(4) -163.61(18) ? . . . . O(8) Er(1) O(4) C(15) -132.87(18) ? . . . . O(8) Er(1) O(4) C(21) 44.4(2) ? . . . . O(4) Er(1) O(9) N(4) 13.93(18) ? . . . . O(9) Er(1) O(4) C(15) -145.65(16) ? . . . . O(9) Er(1) O(4) C(21) 31.6(2) ? . . . . O(4) Er(1) O(11) N(5) 4.0(2) ? . . . . O(11) Er(1) O(4) C(15) -61.27(19) ? . . . . O(11) Er(1) O(4) C(21) 116.0(2) ? . . . . O(4) Er(1) O(12) N(5) 179.35(19) ? . . . . O(12) Er(1) O(4) C(15) -59.73(17) ? . . . . O(12) Er(1) O(4) C(21) 117.5(2) ? . . . . O(5) Er(1) O(6) N(3) -3.04(13) ? . . . . O(6) Er(1) O(5) N(3) 3.06(13) ? . . . . O(5) Er(1) O(8) N(4) -105.02(16) ? . . . . O(8) Er(1) O(5) N(3) 30.19(16) ? . . . . O(5) Er(1) O(9) N(4) 103.67(16) ? . . . . O(9) Er(1) O(5) N(3) -28.66(16) ? . . . . O(5) Er(1) O(11) N(5) -136.56(16) ? . . . . O(11) Er(1) O(5) N(3) -124.89(16) ? . . . . O(5) Er(1) O(12) N(5) 132.57(17) ? . . . . O(12) Er(1) O(5) N(3) 131.35(16) ? . . . . O(6) Er(1) O(8) N(4) -82.47(16) ? . . . . O(8) Er(1) O(6) N(3) -158.33(15) ? . . . . O(6) Er(1) O(9) N(4) 77.77(16) ? . . . . O(9) Er(1) O(6) N(3) 148.73(15) ? . . . . O(6) Er(1) O(11) N(5) 128.65(15) ? . . . . O(11) Er(1) O(6) N(3) 130.86(15) ? . . . . O(6) Er(1) O(12) N(5) -128.89(16) ? . . . . O(12) Er(1) O(6) N(3) -141.41(15) ? . . . . O(8) Er(1) O(9) N(4) -1.40(14) ? . . . . O(9) Er(1) O(8) N(4) 1.39(14) ? . . . . O(8) Er(1) O(11) N(5) 64.94(16) ? . . . . O(11) Er(1) O(8) N(4) 60.91(17) ? . . . . O(8) Er(1) O(12) N(5) -111.91(19) ? . . . . O(12) Er(1) O(8) N(4) 108.77(18) ? . . . . O(9) Er(1) O(11) N(5) 110.26(17) ? . . . . O(11) Er(1) O(9) N(4) -114.19(17) ? . . . . O(9) Er(1) O(12) N(5) -64.59(18) ? . . . . O(12) Er(1) O(9) N(4) -65.78(16) ? . . . . O(11) Er(1) O(12) N(5) -2.10(15) ? . . . . O(12) Er(1) O(11) N(5) 2.08(15) ? . . . . O(1) Cu(1) O(2) Er(1) -15.71(8) ? . . . . O(1) Cu(1) O(2) C(14) 176.6(2) ? . . . . O(2) Cu(1) O(1) Er(1) 15.66(8) ? . . . . O(2) Cu(1) O(1) C(1) -171.1(2) ? . . . . O(1) Cu(1) O(14) C(22) -53.0(2) ? . . . . O(14) Cu(1) O(1) Er(1) -80.81(8) ? . . . . O(14) Cu(1) O(1) C(1) 92.4(2) ? . . . . O(1) Cu(1) N(1) C(7) -1.1(2) ? . . . . O(1) Cu(1) N(1) C(9) 176.6(2) ? . . . . N(1) Cu(1) O(1) Er(1) -173.76(9) ? . . . . N(1) Cu(1) O(1) C(1) -0.6(2) ? . . . . O(1) Cu(1) N(2) C(11) 162.1(3) ? . . . . O(1) Cu(1) N(2) C(20) -20.8(5) ? . . . . N(2) Cu(1) O(1) Er(1) 37.3(4) ? . . . . N(2) Cu(1) O(1) C(1) -149.5(4) ? . . . . O(2) Cu(1) O(14) C(22) -132.3(2) ? . . . . O(14) Cu(1) O(2) Er(1) 88.06(8) ? . . . . O(14) Cu(1) O(2) C(14) -79.6(2) ? . . . . O(2) Cu(1) N(1) C(7) 40.5(4) ? . . . . O(2) Cu(1) N(1) C(9) -141.8(3) ? . . . . N(1) Cu(1) O(2) Er(1) -58.5(3) ? . . . . N(1) Cu(1) O(2) C(14) 133.8(3) ? . . . . O(2) Cu(1) N(2) C(11) -176.8(2) ? . . . . O(2) Cu(1) N(2) C(20) 0.3(2) ? . . . . N(2) Cu(1) O(2) Er(1) 168.37(9) ? . . . . N(2) Cu(1) O(2) C(14) 0.7(2) ? . . . . O(14) Cu(1) N(1) C(7) -106.6(2) ? . . . . O(14) Cu(1) N(1) C(9) 71.1(2) ? . . . . N(1) Cu(1) O(14) C(22) 40.1(2) ? . . . . O(14) Cu(1) N(2) C(11) -77.6(2) ? . . . . O(14) Cu(1) N(2) C(20) 99.5(2) ? . . . . N(2) Cu(1) O(14) C(22) 137.0(2) ? . . . . N(1) Cu(1) N(2) C(11) 13.4(2) ? . . . . N(1) Cu(1) N(2) C(20) -169.5(2) ? . . . . N(2) Cu(1) N(1) C(7) 173.2(2) ? . . . . N(2) Cu(1) N(1) C(9) -9.2(2) ? . . . . Er(1) O(1) C(1) C(2) -9.1(3) ? . . . . Er(1) O(1) C(1) C(6) 172.17(19) ? . . . . Cu(1) O(1) C(1) C(2) 178.67(18) ? . . . . Cu(1) O(1) C(1) C(6) -0.1(2) ? . . . . Er(1) O(2) C(14) C(15) 14.6(3) ? . . . . Er(1) O(2) C(14) C(19) -166.0(2) ? . . . . Cu(1) O(2) C(14) C(15) -179.46(17) ? . . . . Cu(1) O(2) C(14) C(19) -0.0(2) ? . . . . Er(1) O(3) C(2) C(1) 9.9(2) ? . . . . Er(1) O(3) C(2) C(3) -169.4(2) ? . . . . C(8) O(3) C(2) C(1) -169.0(2) ? . . . . C(8) O(3) C(2) C(3) 11.7(3) ? . . . . Er(1) O(4) C(15) C(14) -14.4(2) ? . . . . Er(1) O(4) C(15) C(16) 164.7(2) ? . . . . C(21) O(4) C(15) C(14) 168.0(2) ? . . . . C(21) O(4) C(15) C(16) -12.9(3) ? . . . . Er(1) O(5) N(3) O(6) -5.1(2) ? . . . . Er(1) O(5) N(3) O(7) 174.3(2) ? . . . . Er(1) O(6) N(3) O(5) 5.2(2) ? . . . . Er(1) O(6) N(3) O(7) -174.1(2) ? . . . . Er(1) O(8) N(4) O(9) -2.4(2) ? . . . . Er(1) O(8) N(4) O(10) 178.4(2) ? . . . . Er(1) O(9) N(4) O(8) 2.4(2) ? . . . . Er(1) O(9) N(4) O(10) -178.5(2) ? . . . . Er(1) O(11) N(5) O(12) -3.5(2) ? . . . . Er(1) O(11) N(5) O(13) 175.5(2) ? . . . . Er(1) O(12) N(5) O(11) 3.5(2) ? . . . . Er(1) O(12) N(5) O(13) -175.5(2) ? . . . . Cu(1) O(14) C(22) C(23) 15.3(4) ? . . . . Cu(1) O(14) C(22) C(24) -163.5(2) ? . . . . Cu(1) N(1) C(7) C(6) 3.5(4) ? . . . . Cu(1) N(1) C(9) C(10) 36.9(3) ? . . . . C(7) N(1) C(9) C(10) -145.2(2) ? . . . . C(9) N(1) C(7) C(6) -174.3(2) ? . . . . Cu(1) N(2) C(11) C(10) -45.2(2) ? . . . . Cu(1) N(2) C(20) C(19) -2.0(4) ? . . . . C(11) N(2) C(20) C(19) 175.2(2) ? . . . . C(20) N(2) C(11) C(10) 137.4(2) ? . . . . O(1) C(1) C(2) O(3) -1.3(3) ? . . . . O(1) C(1) C(2) C(3) 178.0(2) ? . . . . O(1) C(1) C(6) C(5) -178.2(2) ? . . . . O(1) C(1) C(6) C(7) 2.4(4) ? . . . . C(2) C(1) C(6) C(5) 3.1(3) ? . . . . C(2) C(1) C(6) C(7) -176.4(2) ? . . . . C(6) C(1) C(2) O(3) 177.5(2) ? . . . . C(6) C(1) C(2) C(3) -3.2(4) ? . . . . O(3) C(2) C(3) C(4) -179.9(2) ? . . . . C(1) C(2) C(3) C(4) 0.8(4) ? . . . . C(2) C(3) C(4) C(5) 1.6(4) ? . . . . C(3) C(4) C(5) C(6) -1.7(4) ? . . . . C(4) C(5) C(6) C(1) -0.7(4) ? . . . . C(4) C(5) C(6) C(7) 178.8(2) ? . . . . C(1) C(6) C(7) N(1) -4.4(4) ? . . . . C(5) C(6) C(7) N(1) 176.1(2) ? . . . . N(1) C(9) C(10) C(11) -69.0(3) ? . . . . N(1) C(9) C(10) C(12) 175.2(2) ? . . . . N(1) C(9) C(10) C(13) 54.6(3) ? . . . . C(9) C(10) C(11) N(2) 73.9(2) ? . . . . C(12) C(10) C(11) N(2) -170.2(2) ? . . . . C(13) C(10) C(11) N(2) -50.0(3) ? . . . . O(2) C(14) C(15) O(4) 1.0(3) ? . . . . O(2) C(14) C(15) C(16) -178.1(2) ? . . . . O(2) C(14) C(19) C(18) 176.9(2) ? . . . . O(2) C(14) C(19) C(20) -1.8(4) ? . . . . C(15) C(14) C(19) C(18) -3.7(3) ? . . . . C(15) C(14) C(19) C(20) 177.6(2) ? . . . . C(19) C(14) C(15) O(4) -178.4(2) ? . . . . C(19) C(14) C(15) C(16) 2.4(3) ? . . . . O(4) C(15) C(16) C(17) -178.4(2) ? . . . . C(14) C(15) C(16) C(17) 0.7(4) ? . . . . C(15) C(16) C(17) C(18) -2.5(4) ? . . . . C(16) C(17) C(18) C(19) 1.2(4) ? . . . . C(17) C(18) C(19) C(14) 2.0(4) ? . . . . C(17) C(18) C(19) C(20) -179.3(2) ? . . . . C(14) C(19) C(20) N(2) 3.0(4) ? . . . . C(18) C(19) C(20) N(2) -175.7(2) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(7) C(3) 3.022(3) ? . 3_667 O(7) C(4) 3.304(4) ? . 3_667 O(7) C(23) 3.582(4) ? . 1_455 O(8) C(21) 3.481(3) ? . 3_666 O(10) C(9) 3.513(3) ? . 2_746 O(10) C(16) 3.473(3) ? . 3_666 O(10) C(21) 3.518(3) ? . 3_666 O(10) C(24) 3.558(4) ? . 2_746 O(12) C(9) 3.431(3) ? . 4_564 O(13) C(12) 3.271(3) ? . 2_746 N(2) C(5) 3.545(3) ? . 4_564 N(5) C(12) 3.538(3) ? . 2_746 C(2) C(3) 3.560(4) ? . 3_767 C(2) C(4) 3.582(4) ? . 3_767 C(3) O(7) 3.022(3) ? . 3_667 C(3) C(2) 3.560(4) ? . 3_767 C(3) C(3) 3.167(4) ? . 3_767 C(3) C(4) 3.478(4) ? . 3_767 C(4) O(7) 3.304(4) ? . 3_667 C(4) C(2) 3.582(4) ? . 3_767 C(4) C(3) 3.478(4) ? . 3_767 C(4) C(11) 3.522(4) ? . 4_565 C(4) C(20) 3.450(4) ? . 4_565 C(5) N(2) 3.545(3) ? . 4_565 C(5) C(20) 3.169(4) ? . 4_565 C(6) C(18) 3.561(4) ? . 4_565 C(9) O(10) 3.513(3) ? . 2_756 C(9) O(12) 3.431(3) ? . 4_565 C(11) C(4) 3.522(4) ? . 4_564 C(12) O(13) 3.271(3) ? . 2_756 C(12) N(5) 3.538(3) ? . 2_756 C(12) C(12) 3.410(4) ? . 3_777 C(13) C(15) 3.598(4) ? . 4_565 C(13) C(16) 3.376(4) ? . 4_565 C(15) C(13) 3.598(4) ? . 4_564 C(16) O(10) 3.473(3) ? . 3_666 C(16) C(13) 3.376(4) ? . 4_564 C(18) C(6) 3.561(4) ? . 4_564 C(20) C(4) 3.450(4) ? . 4_564 C(20) C(5) 3.169(4) ? . 4_564 C(21) O(8) 3.481(3) ? . 3_666 C(21) O(10) 3.518(3) ? . 3_666 C(23) O(7) 3.582(4) ? . 1_655 C(24) O(10) 3.558(4) ? . 2_756 O(3) H(2) 3.26(3) ? . 3_767 O(4) H(17) 2.88(3) ? . 4_564 O(4) H(30) 3.429 ? . 1_455 O(5) H(19) 3.08(3) ? . 4_565 O(5) H(27) 2.736 ? . 1_455 O(5) H(28) 3.573 ? . 1_455 O(6) H(11) 3.20(3) ? . 2_646 O(6) H(16) 3.03(4) ? . 2_646 O(6) H(21) 3.35(2) ? . 2_646 O(7) H(1) 2.65(3) ? . 3_667 O(7) H(2) 3.16(3) ? . 3_667 O(7) H(6) 3.17(3) ? . 3_667 O(7) H(11) 2.80(3) ? . 2_646 O(7) H(21) 2.95(2) ? . 2_646 O(7) H(25) 3.517 ? . 1_455 O(7) H(27) 2.811 ? . 1_455 O(8) H(12) 3.32(3) ? . 2_746 O(8) H(13) 3.24(4) ? . 4_564 O(8) H(16) 3.25(4) ? . 2_646 O(8) H(17) 3.06(3) ? . 4_564 O(8) H(24) 2.70(3) ? . 3_666 O(9) H(2) 2.92(3) ? . 3_767 O(9) H(10) 3.16(3) ? . 2_746 O(9) H(12) 3.27(3) ? . 2_746 O(9) H(29) 3.346 ? . 2_746 O(10) H(8) 2.59(3) ? . 2_746 O(10) H(10) 3.26(3) ? . 2_746 O(10) H(12) 3.01(3) ? . 2_746 O(10) H(16) 3.55(4) ? . 2_646 O(10) H(18) 2.54(2) ? . 3_666 O(10) H(23) 3.20(2) ? . 3_666 O(10) H(24) 2.88(3) ? . 3_666 O(10) H(28) 3.196 ? . 2_746 O(10) H(29) 3.315 ? . 2_746 O(11) H(2) 2.83(3) ? . 3_767 O(11) H(12) 3.37(3) ? . 2_746 O(11) H(14) 3.54(3) ? . 2_746 O(12) H(4) 3.25(3) ? . 4_564 O(12) H(9) 2.57(3) ? . 4_564 O(12) H(12) 3.31(3) ? . 2_746 O(12) H(13) 3.01(3) ? . 4_564 O(12) H(17) 2.84(3) ? . 4_564 O(13) H(4) 3.32(3) ? . 4_564 O(13) H(9) 2.86(3) ? . 4_564 O(13) H(12) 3.08(3) ? . 2_746 O(13) H(13) 3.57(3) ? . 4_564 O(13) H(14) 2.51(3) ? . 2_746 O(13) H(23) 2.82(3) ? . 1_655 O(14) H(3) 2.73(3) ? . 4_564 O(14) H(4) 3.15(3) ? . 4_564 N(2) H(3) 3.24(3) ? . 4_564 N(3) H(11) 3.35(3) ? . 2_646 N(3) H(21) 3.53(2) ? . 2_646 N(3) H(27) 3.084 ? . 1_455 N(4) H(8) 3.43(3) ? . 2_746 N(4) H(10) 3.46(3) ? . 2_746 N(4) H(12) 2.95(3) ? . 2_746 N(4) H(16) 3.48(4) ? . 2_646 N(4) H(18) 3.51(2) ? . 3_666 N(4) H(24) 3.16(3) ? . 3_666 N(5) H(9) 3.08(3) ? . 4_564 N(5) H(12) 2.99(3) ? . 2_746 N(5) H(13) 3.47(3) ? . 4_564 N(5) H(14) 3.04(3) ? . 2_746 C(1) H(20) 3.23(3) ? . 4_565 C(2) H(1) 3.35(3) ? . 3_767 C(2) H(2) 3.46(3) ? . 3_767 C(2) H(20) 3.38(3) ? . 4_565 C(3) H(1) 3.17(3) ? . 3_767 C(3) H(21) 3.40(2) ? . 4_565 C(4) H(1) 3.32(3) ? . 3_767 C(4) H(7) 2.91(3) ? . 3_767 C(4) H(10) 3.18(2) ? . 4_565 C(4) H(11) 3.14(3) ? . 4_565 C(4) H(21) 2.88(2) ? . 4_565 C(5) H(7) 2.89(3) ? . 3_767 C(5) H(10) 3.25(2) ? . 4_565 C(5) H(21) 2.91(2) ? . 4_565 C(5) H(29) 3.481 ? . 4_565 C(6) H(20) 3.34(3) ? . 4_565 C(6) H(21) 3.49(2) ? . 4_565 C(8) H(2) 3.55(3) ? . 3_767 C(8) H(20) 3.18(3) ? . 2_646 C(11) H(2) 3.05(3) ? . 4_564 C(11) H(3) 3.38(3) ? . 4_564 C(12) H(12) 3.13(3) ? . 3_777 C(12) H(13) 2.82(3) ? . 3_777 C(12) H(22) 3.31(3) ? . 2_656 C(12) H(23) 3.34(2) ? . 2_656 C(13) H(18) 3.24(3) ? . 4_565 C(13) H(22) 3.01(3) ? . 2_656 C(13) H(24) 3.11(3) ? . 4_565 C(14) H(28) 3.448 ? . 1_455 C(14) H(30) 3.311 ? . 1_455 C(15) H(15) 3.32(3) ? . 4_564 C(15) H(17) 2.92(3) ? . 4_564 C(15) H(30) 3.029 ? . 1_455 C(16) H(15) 2.82(3) ? . 4_564 C(16) H(17) 3.06(3) ? . 4_564 C(16) H(26) 3.575 ? . 4_464 C(16) H(30) 3.282 ? . 1_455 C(17) H(15) 3.22(3) ? . 4_564 C(17) H(26) 3.168 ? . 4_464 C(17) H(27) 3.391 ? . 4_464 C(18) H(5) 3.27(3) ? . 2_656 C(18) H(6) 3.30(3) ? . 2_656 C(20) H(3) 3.17(3) ? . 4_564 C(21) H(14) 2.89(3) ? . 2_646 C(21) H(16) 3.18(4) ? . 2_646 C(21) H(17) 3.18(3) ? . 4_564 C(21) H(24) 3.53(3) ? . 3_666 C(22) H(3) 3.40(3) ? . 4_564 C(23) H(19) 2.91(3) ? . 4_665 C(24) H(3) 3.34(3) ? . 4_564 H(1) O(7) 2.65(3) ? . 3_667 H(1) C(2) 3.35(3) ? . 3_767 H(1) C(3) 3.17(3) ? . 3_767 H(1) C(4) 3.32(3) ? . 3_767 H(1) H(1) 3.43(4) ? . 3_767 H(1) H(25) 3.123 ? . 3_767 H(1) H(27) 3.436 ? . 3_767 H(2) O(3) 3.26(3) ? . 3_767 H(2) O(7) 3.16(3) ? . 3_667 H(2) O(9) 2.92(3) ? . 3_767 H(2) O(11) 2.83(3) ? . 3_767 H(2) C(2) 3.46(3) ? . 3_767 H(2) C(8) 3.55(3) ? . 3_767 H(2) C(11) 3.05(3) ? . 4_565 H(2) H(7) 2.94(4) ? . 3_767 H(2) H(10) 2.63(4) ? . 4_565 H(2) H(11) 2.66(4) ? . 4_565 H(2) H(21) 3.06(4) ? . 4_565 H(3) O(14) 2.73(3) ? . 4_565 H(3) N(2) 3.24(3) ? . 4_565 H(3) C(11) 3.38(3) ? . 4_565 H(3) C(20) 3.17(3) ? . 4_565 H(3) C(22) 3.40(3) ? . 4_565 H(3) C(24) 3.34(3) ? . 4_565 H(3) H(7) 2.91(4) ? . 3_767 H(3) H(10) 2.85(4) ? . 4_565 H(3) H(11) 3.59(4) ? . 4_565 H(3) H(21) 3.15(4) ? . 4_565 H(3) H(29) 2.634 ? . 4_565 H(4) O(12) 3.25(3) ? . 4_565 H(4) O(13) 3.32(3) ? . 4_565 H(4) O(14) 3.15(3) ? . 4_565 H(4) H(29) 3.519 ? . 4_565 H(5) C(18) 3.27(3) ? . 2_646 H(5) H(20) 2.91(4) ? . 2_646 H(5) H(21) 3.31(4) ? . 2_646 H(5) H(29) 3.202 ? . 2_746 H(6) O(7) 3.17(3) ? . 3_667 H(6) C(18) 3.30(3) ? . 2_646 H(6) H(6) 3.50(4) ? . 3_667 H(6) H(20) 2.69(4) ? . 2_646 H(7) C(4) 2.91(3) ? . 3_767 H(7) C(5) 2.89(3) ? . 3_767 H(7) H(2) 2.94(4) ? . 3_767 H(7) H(3) 2.91(4) ? . 3_767 H(7) H(20) 3.58(4) ? . 2_646 H(7) H(29) 3.159 ? . 2_746 H(8) O(10) 2.59(3) ? . 2_756 H(8) N(4) 3.43(3) ? . 2_756 H(9) O(12) 2.57(3) ? . 4_565 H(9) O(13) 2.86(3) ? . 4_565 H(9) N(5) 3.08(3) ? . 4_565 H(10) O(9) 3.16(3) ? . 2_756 H(10) O(10) 3.26(3) ? . 2_756 H(10) N(4) 3.46(3) ? . 2_756 H(10) C(4) 3.18(2) ? . 4_564 H(10) C(5) 3.25(2) ? . 4_564 H(10) H(2) 2.63(4) ? . 4_564 H(10) H(3) 2.85(4) ? . 4_564 H(11) O(6) 3.20(3) ? . 2_656 H(11) O(7) 2.80(3) ? . 2_656 H(11) N(3) 3.35(3) ? . 2_656 H(11) C(4) 3.14(3) ? . 4_564 H(11) H(2) 2.66(4) ? . 4_564 H(11) H(3) 3.59(4) ? . 4_564 H(11) H(22) 3.53(4) ? . 2_656 H(12) O(8) 3.32(3) ? . 2_756 H(12) O(9) 3.27(3) ? . 2_756 H(12) O(10) 3.01(3) ? . 2_756 H(12) O(11) 3.37(3) ? . 2_756 H(12) O(12) 3.31(3) ? . 2_756 H(12) O(13) 3.08(3) ? . 2_756 H(12) N(4) 2.95(3) ? . 2_756 H(12) N(5) 2.99(3) ? . 2_756 H(12) C(12) 3.13(3) ? . 3_777 H(12) H(12) 3.17(4) ? . 3_777 H(12) H(13) 2.33(4) ? . 3_777 H(12) H(14) 3.45(4) ? . 3_777 H(13) O(8) 3.24(4) ? . 4_565 H(13) O(12) 3.01(3) ? . 4_565 H(13) O(13) 3.57(3) ? . 4_565 H(13) N(5) 3.47(3) ? . 4_565 H(13) C(12) 2.82(3) ? . 3_777 H(13) H(12) 2.33(4) ? . 3_777 H(13) H(13) 2.47(5) ? . 3_777 H(13) H(14) 3.17(4) ? . 3_777 H(13) H(22) 3.44(4) ? . 2_656 H(13) H(23) 3.31(4) ? . 2_656 H(14) O(11) 3.54(3) ? . 2_756 H(14) O(13) 2.51(3) ? . 2_756 H(14) N(5) 3.04(3) ? . 2_756 H(14) C(21) 2.89(3) ? . 2_656 H(14) H(12) 3.45(4) ? . 3_777 H(14) H(13) 3.17(4) ? . 3_777 H(14) H(22) 2.60(4) ? . 2_656 H(14) H(23) 2.49(4) ? . 2_656 H(14) H(24) 3.40(5) ? . 2_656 H(15) C(15) 3.32(3) ? . 4_565 H(15) C(16) 2.82(3) ? . 4_565 H(15) C(17) 3.22(3) ? . 4_565 H(15) H(18) 2.76(4) ? . 4_565 H(15) H(19) 3.39(4) ? . 4_565 H(15) H(24) 3.31(4) ? . 4_565 H(16) O(6) 3.03(4) ? . 2_656 H(16) O(8) 3.25(4) ? . 2_656 H(16) O(10) 3.55(4) ? . 2_656 H(16) N(4) 3.48(4) ? . 2_656 H(16) C(21) 3.18(4) ? . 2_656 H(16) H(18) 3.27(5) ? . 4_565 H(16) H(22) 2.27(5) ? . 2_656 H(16) H(24) 3.44(5) ? . 2_656 H(16) H(24) 2.88(6) ? . 4_565 H(17) O(4) 2.88(3) ? . 4_565 H(17) O(8) 3.06(3) ? . 4_565 H(17) O(12) 2.84(3) ? . 4_565 H(17) C(15) 2.92(3) ? . 4_565 H(17) C(16) 3.06(3) ? . 4_565 H(17) C(21) 3.18(3) ? . 4_565 H(17) H(18) 3.05(4) ? . 4_565 H(17) H(22) 3.10(4) ? . 2_656 H(17) H(24) 3.59(4) ? . 2_656 H(17) H(24) 2.57(4) ? . 4_565 H(18) O(10) 2.54(2) ? . 3_666 H(18) N(4) 3.51(3) ? . 3_666 H(18) C(13) 3.24(3) ? . 4_564 H(18) H(15) 2.76(4) ? . 4_564 H(18) H(16) 3.27(5) ? . 4_564 H(18) H(17) 3.05(4) ? . 4_564 H(18) H(26) 3.290 ? . 4_464 H(19) O(5) 3.08(3) ? . 4_564 H(19) C(23) 2.91(3) ? . 4_464 H(19) H(15) 3.39(4) ? . 4_564 H(19) H(26) 2.502 ? . 4_464 H(19) H(27) 2.487 ? . 4_464 H(19) H(28) 3.032 ? . 4_464 H(20) C(1) 3.23(3) ? . 4_564 H(20) C(2) 3.38(3) ? . 4_564 H(20) C(6) 3.34(3) ? . 4_564 H(20) C(8) 3.18(3) ? . 2_656 H(20) H(5) 2.91(4) ? . 2_656 H(20) H(6) 2.69(4) ? . 2_656 H(20) H(7) 3.58(4) ? . 2_656 H(21) O(6) 3.35(2) ? . 2_656 H(21) O(7) 2.95(2) ? . 2_656 H(21) N(3) 3.53(2) ? . 2_656 H(21) C(3) 3.40(2) ? . 4_564 H(21) C(4) 2.88(2) ? . 4_564 H(21) C(5) 2.91(2) ? . 4_564 H(21) C(6) 3.49(2) ? . 4_564 H(21) H(2) 3.06(4) ? . 4_564 H(21) H(3) 3.15(4) ? . 4_564 H(21) H(5) 3.31(4) ? . 2_656 H(22) C(12) 3.31(3) ? . 2_646 H(22) C(13) 3.01(3) ? . 2_646 H(22) H(11) 3.53(4) ? . 2_646 H(22) H(13) 3.44(4) ? . 2_646 H(22) H(14) 2.60(4) ? . 2_646 H(22) H(16) 2.27(5) ? . 2_646 H(22) H(17) 3.10(4) ? . 2_646 H(22) H(24) 3.15(5) ? . 3_666 H(23) O(10) 3.20(2) ? . 3_666 H(23) O(13) 2.82(3) ? . 1_455 H(23) C(12) 3.34(2) ? . 2_646 H(23) H(13) 3.31(4) ? . 2_646 H(23) H(14) 2.49(4) ? . 2_646 H(23) H(30) 3.122 ? . 1_455 H(24) O(8) 2.70(3) ? . 3_666 H(24) O(10) 2.88(3) ? . 3_666 H(24) N(4) 3.16(3) ? . 3_666 H(24) C(13) 3.11(3) ? . 4_564 H(24) C(21) 3.53(3) ? . 3_666 H(24) H(14) 3.40(5) ? . 2_646 H(24) H(15) 3.31(4) ? . 4_564 H(24) H(16) 3.44(5) ? . 2_646 H(24) H(16) 2.88(6) ? . 4_564 H(24) H(17) 3.59(4) ? . 2_646 H(24) H(17) 2.57(4) ? . 4_564 H(24) H(22) 3.15(5) ? . 3_666 H(24) H(24) 3.00(4) ? . 3_666 H(25) O(7) 3.517 ? . 1_655 H(25) H(1) 3.123 ? . 3_767 H(26) C(16) 3.575 ? . 4_665 H(26) C(17) 3.168 ? . 4_665 H(26) H(18) 3.290 ? . 4_665 H(26) H(19) 2.502 ? . 4_665 H(27) O(5) 2.736 ? . 1_655 H(27) O(7) 2.811 ? . 1_655 H(27) N(3) 3.084 ? . 1_655 H(27) C(17) 3.391 ? . 4_665 H(27) H(1) 3.436 ? . 3_767 H(27) H(19) 2.487 ? . 4_665 H(28) O(5) 3.573 ? . 1_655 H(28) O(10) 3.196 ? . 2_756 H(28) C(14) 3.448 ? . 1_655 H(28) H(19) 3.032 ? . 4_665 H(29) O(9) 3.346 ? . 2_756 H(29) O(10) 3.315 ? . 2_756 H(29) C(5) 3.481 ? . 4_564 H(29) H(3) 2.634 ? . 4_564 H(29) H(4) 3.519 ? . 4_564 H(29) H(5) 3.202 ? . 2_756 H(29) H(7) 3.159 ? . 2_756 H(30) O(4) 3.429 ? . 1_655 H(30) C(14) 3.311 ? . 1_655 H(30) C(15) 3.029 ? . 1_655 H(30) C(16) 3.282 ? . 1_655 H(30) H(23) 3.122 ? . 1_655 Er(1) Cu(1) 3.4923(19) ? . . data___TbVO _database_code_depnum_ccdc_archive 'CCDC 881975' #TrackingRef '11259_web_deposit_cif_file_4_TakayukiIshida_1336987557.TbV_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 N5 O15 Tb V ' _chemical_formula_moiety 'C24 H30 N5 O15 Tb V ' _chemical_formula_weight 838.39 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.911(3) _cell_length_b 17.547(4) _cell_length_c 18.243(9) _cell_angle_alpha 90.0000 _cell_angle_beta 105.524(4) _cell_angle_gamma 90.0000 _cell_volume 3056.6(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 394 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 90. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668.00 _exptl_absorpt_coefficient_mu 2.675 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_T_max 0.852 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 52235 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_ambient_temperature 90. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6994 _reflns_number_gt 6425 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0350 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6994 _refine_ls_number_parameters 517 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.96 _refine_diff_density_min -0.89 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Tb Tb -0.172 4.154 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; V V 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Tb(1) Tb 0.927240(10) 0.573450(10) 0.203540(10) 0.01040(3) Uani 1.00 1 d . . . V(1) V 0.83766(5) 0.46975(3) 0.34700(3) 0.01072(11) Uani 1.00 1 d . . . O(1) O 0.8769(2) 0.57723(11) 0.32530(12) 0.0122(5) Uani 1.00 1 d . . . O(2) O 0.8121(2) 0.46342(12) 0.23531(12) 0.0130(4) Uani 1.00 1 d . . . O(3) O 0.9291(2) 0.70517(12) 0.26609(12) 0.0153(5) Uani 1.00 1 d . . . O(4) O 0.7855(2) 0.49347(12) 0.09357(12) 0.0147(5) Uani 1.00 1 d . . . O(5) O 1.1175(2) 0.65750(15) 0.18431(14) 0.0265(6) Uani 1.00 1 d . . . O(6) O 1.0394(2) 0.57444(14) 0.09761(16) 0.0279(7) Uani 1.00 1 d . . . O(7) O 1.2018(2) 0.65374(14) 0.08595(16) 0.0319(7) Uani 1.00 1 d . . . O(8) O 1.1427(2) 0.54682(14) 0.30225(14) 0.0244(6) Uani 1.00 1 d . . . O(9) O 1.0856(2) 0.46149(14) 0.21529(15) 0.0257(6) Uani 1.00 1 d . . . O(10) O 1.2650(2) 0.44230(16) 0.31353(17) 0.0338(7) Uani 1.00 1 d . . . O(11) O 0.7967(2) 0.66524(12) 0.10752(12) 0.0173(5) Uani 1.00 1 d . . . O(12) O 0.6851(2) 0.61630(13) 0.18280(12) 0.0164(5) Uani 1.00 1 d . . . O(13) O 0.5894(2) 0.70850(14) 0.10662(14) 0.0270(6) Uani 1.00 1 d . . . O(14) O 0.6054(2) 0.51348(13) 0.30114(12) 0.0171(5) Uani 1.00 1 d . . . O(15) O 0.9869(2) 0.43155(12) 0.38064(13) 0.0158(5) Uani 1.00 1 d . . . N(1) N 0.8050(2) 0.50184(14) 0.45009(14) 0.0121(5) Uani 1.00 1 d . . . N(2) N 0.7280(2) 0.36934(14) 0.34509(14) 0.0124(5) Uani 1.00 1 d . . . N(3) N 1.1218(2) 0.62978(15) 0.12098(16) 0.0193(6) Uani 1.00 1 d . . . N(4) N 1.1680(2) 0.48209(16) 0.27834(16) 0.0197(6) Uani 1.00 1 d . . . N(5) N 0.6865(2) 0.66475(15) 0.13130(14) 0.0159(6) Uani 1.00 1 d . . . C(1) C 0.8601(2) 0.64023(17) 0.36298(17) 0.0126(6) Uani 1.00 1 d . . . C(2) C 0.8882(3) 0.71075(17) 0.33325(17) 0.0132(6) Uani 1.00 1 d . . . C(3) C 0.8760(3) 0.77866(18) 0.36929(19) 0.0180(7) Uani 1.00 1 d . . . C(4) C 0.8369(3) 0.77739(19) 0.4375(2) 0.0224(8) Uani 1.00 1 d . . . C(5) C 0.8090(3) 0.70951(19) 0.46756(18) 0.0182(7) Uani 1.00 1 d . . . C(6) C 0.8200(2) 0.63996(17) 0.43141(17) 0.0131(6) Uani 1.00 1 d . . . C(7) C 0.7976(3) 0.57111(17) 0.47158(17) 0.0135(7) Uani 1.00 1 d . . . C(8) C 0.9537(3) 0.77758(19) 0.2333(2) 0.0222(8) Uani 1.00 1 d . . . C(9) C 0.8039(3) 0.44230(19) 0.50744(17) 0.0159(7) Uani 1.00 1 d . . . C(10) C 0.7035(3) 0.37592(18) 0.47988(17) 0.0160(7) Uani 1.00 1 d . . . C(11) C 0.7414(3) 0.32883(18) 0.41730(19) 0.0174(7) Uani 1.00 1 d . . . C(12) C 0.7187(3) 0.42135(16) 0.18573(17) 0.0131(7) Uani 1.00 1 d . . . C(13) C 0.6998(3) 0.43629(17) 0.10789(17) 0.0145(7) Uani 1.00 1 d . . . C(14) C 0.6012(3) 0.39785(19) 0.05293(18) 0.0169(7) Uani 1.00 1 d . . . C(15) C 0.5180(3) 0.34216(19) 0.07363(19) 0.0195(7) Uani 1.00 1 d . . . C(16) C 0.5367(3) 0.32452(18) 0.14926(19) 0.0184(7) Uani 1.00 1 d . . . C(17) C 0.6380(3) 0.36317(18) 0.20650(18) 0.0165(7) Uani 1.00 1 d . . . C(18) C 0.6544(3) 0.33791(18) 0.28428(18) 0.0164(7) Uani 1.00 1 d . . . C(19) C 0.7704(4) 0.5098(2) 0.01372(19) 0.0221(8) Uani 1.00 1 d . . . C(20) C 0.7223(4) 0.3219(2) 0.5480(2) 0.0234(8) Uani 1.00 1 d . . . C(21) C 0.5510(3) 0.4030(2) 0.4531(2) 0.0208(8) Uani 1.00 1 d . . . C(22) C 0.5057(3) 0.54961(18) 0.26419(17) 0.0156(7) Uani 1.00 1 d . . . C(23) C 0.4170(3) 0.5221(2) 0.18885(19) 0.0264(9) Uani 1.00 1 d . . . C(24) C 0.4674(3) 0.6246(2) 0.2909(2) 0.0282(9) Uani 1.00 1 d . . . H(1) H 0.893(3) 0.823(2) 0.3499(19) 0.014(8) Uiso 1.00 1 d . . . H(2) H 0.834(3) 0.8244(19) 0.4640(19) 0.014(8) Uiso 1.00 1 d . . . H(3) H 0.779(3) 0.7068(19) 0.511(2) 0.015(8) Uiso 1.00 1 d . . . H(4) H 0.782(3) 0.5792(16) 0.5217(18) 0.011(7) Uiso 1.00 1 d . . . H(5) H 0.867(3) 0.809(2) 0.2243(19) 0.015(8) Uiso 1.00 1 d . . . H(6) H 0.981(4) 0.769(2) 0.187(2) 0.049(13) Uiso 1.00 1 d . . . H(7) H 1.046(3) 0.799(2) 0.277(2) 0.028(10) Uiso 1.00 1 d . . . H(8) H 0.788(4) 0.465(2) 0.554(2) 0.030(10) Uiso 1.00 1 d . . . H(9) H 0.901(3) 0.4232(19) 0.521(2) 0.019(9) Uiso 1.00 1 d . . . H(10) H 0.686(3) 0.2848(19) 0.4078(19) 0.013(8) Uiso 1.00 1 d . . . H(11) H 0.835(3) 0.3128(18) 0.4337(18) 0.011(8) Uiso 1.00 1 d . . . H(12) H 0.584(3) 0.407(2) 0.004(2) 0.019(9) Uiso 1.00 1 d . . . H(13) H 0.450(3) 0.313(2) 0.036(2) 0.028(10) Uiso 1.00 1 d . . . H(14) H 0.481(3) 0.285(2) 0.1648(19) 0.017(9) Uiso 1.00 1 d . . . H(15) H 0.601(3) 0.291(2) 0.2869(19) 0.015(8) Uiso 1.00 1 d . . . H(16) H 0.829(4) 0.551(2) 0.010(2) 0.032(11) Uiso 1.00 1 d . . . H(17) H 0.680(4) 0.528(2) -0.012(2) 0.038(12) Uiso 1.00 1 d . . . H(18) H 0.787(4) 0.465(2) -0.011(2) 0.030(10) Uiso 1.00 1 d . . . H(19) H 0.700(4) 0.344(2) 0.591(2) 0.040(12) Uiso 1.00 1 d . . . H(20) H 0.659(4) 0.277(2) 0.534(2) 0.038(11) Uiso 1.00 1 d . . . H(21) H 0.815(4) 0.304(2) 0.562(2) 0.028(10) Uiso 1.00 1 d . . . H(22) H 0.527(4) 0.429(2) 0.496(2) 0.038(12) Uiso 1.00 1 d . . . H(23) H 0.493(3) 0.359(2) 0.438(2) 0.027(10) Uiso 1.00 1 d . . . H(24) H 0.535(4) 0.439(2) 0.411(2) 0.031(11) Uiso 1.00 1 d . . . H(25) H 0.4443 0.4805 0.1702 0.031 Uiso 1.00 1 c R . . H(26) H 0.4200 0.5597 0.1488 0.031 Uiso 1.00 1 c R . . H(27) H 0.3247 0.5240 0.1897 0.031 Uiso 1.00 1 c R . . H(28) H 0.3774 0.6276 0.2879 0.034 Uiso 1.00 1 c R . . H(29) H 0.4765 0.6638 0.2547 0.034 Uiso 1.00 1 c R . . H(30) H 0.5238 0.6377 0.3408 0.033 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tb(1) 0.01146(8) 0.01025(8) 0.01019(8) 0.00027(5) 0.00413(5) 0.00052(5) V(1) 0.0117(2) 0.0104(2) 0.0094(2) -0.00072(18) 0.00178(18) 0.00031(18) O(1) 0.0168(10) 0.0089(9) 0.0122(10) -0.0001(7) 0.0060(8) -0.0020(7) O(2) 0.0132(9) 0.0144(10) 0.0110(9) -0.0039(8) 0.0025(7) -0.0019(7) O(3) 0.0226(11) 0.0110(10) 0.0149(10) -0.0019(8) 0.0097(8) 0.0002(8) O(4) 0.0157(10) 0.0172(10) 0.0108(10) -0.0018(8) 0.0030(8) 0.0002(8) O(5) 0.0223(12) 0.0336(14) 0.0266(13) -0.0062(10) 0.0116(10) -0.0058(10) O(6) 0.0318(14) 0.0257(13) 0.0349(14) -0.0114(10) 0.0238(12) -0.0095(10) O(7) 0.0400(15) 0.0210(12) 0.0482(16) -0.0025(11) 0.0354(13) 0.0061(11) O(8) 0.0215(12) 0.0289(13) 0.0209(12) 0.0043(10) 0.0020(9) -0.0009(10) O(9) 0.0179(11) 0.0217(12) 0.0330(14) 0.0062(9) -0.0012(10) -0.0075(10) O(10) 0.0162(12) 0.0375(15) 0.0446(17) 0.0093(11) 0.0029(11) 0.0162(13) O(11) 0.0230(11) 0.0171(11) 0.0142(10) 0.0019(9) 0.0092(8) 0.0025(8) O(12) 0.0158(10) 0.0198(11) 0.0150(10) 0.0026(8) 0.0065(8) 0.0045(8) O(13) 0.0267(12) 0.0273(13) 0.0246(12) 0.0167(10) 0.0026(10) 0.0067(10) O(14) 0.0133(10) 0.0198(11) 0.0179(11) 0.0030(8) 0.0035(8) 0.0062(8) O(15) 0.0139(10) 0.0158(10) 0.0169(10) 0.0013(8) 0.0029(8) 0.0033(8) N(1) 0.0111(11) 0.0144(12) 0.0099(11) -0.0013(9) 0.0011(9) 0.0016(9) N(2) 0.0132(11) 0.0092(11) 0.0153(12) -0.0003(9) 0.0045(9) 0.0003(9) N(3) 0.0218(13) 0.0132(12) 0.0264(14) 0.0051(10) 0.0127(11) 0.0028(10) N(4) 0.0137(12) 0.0221(14) 0.0252(14) 0.0021(10) 0.0084(11) 0.0094(11) N(5) 0.0188(12) 0.0164(12) 0.0118(12) 0.0017(10) 0.0032(10) -0.0013(9) C(1) 0.0056(12) 0.0151(14) 0.0157(14) 0.0005(10) 0.0004(10) -0.0018(11) C(2) 0.0133(13) 0.0136(14) 0.0124(13) 0.0014(10) 0.0030(10) 0.0001(11) C(3) 0.0221(15) 0.0110(14) 0.0217(16) -0.0001(12) 0.0072(12) -0.0008(12) C(4) 0.0278(17) 0.0152(15) 0.0250(17) 0.0019(13) 0.0084(14) -0.0061(13) C(5) 0.0212(15) 0.0189(15) 0.0155(14) 0.0040(12) 0.0066(12) -0.0046(12) C(6) 0.0101(13) 0.0141(14) 0.0145(14) 0.0007(10) 0.0024(10) -0.0001(11) C(7) 0.0113(13) 0.0198(15) 0.0090(13) -0.0011(11) 0.0021(10) 0.0008(11) C(8) 0.0349(19) 0.0122(15) 0.0236(17) -0.0025(13) 0.0151(15) 0.0053(12) C(9) 0.0167(15) 0.0191(15) 0.0110(14) -0.0041(12) 0.0020(11) 0.0036(11) C(10) 0.0186(15) 0.0147(14) 0.0144(14) -0.0049(11) 0.0038(11) 0.0022(11) C(11) 0.0190(15) 0.0144(14) 0.0202(15) 0.0010(12) 0.0077(12) 0.0047(12) C(12) 0.0124(13) 0.0135(14) 0.0136(14) 0.0029(10) 0.0039(11) -0.0031(10) C(13) 0.0167(14) 0.0157(14) 0.0123(14) 0.0040(11) 0.0061(11) -0.0008(11) C(14) 0.0174(15) 0.0196(15) 0.0115(14) 0.0018(12) -0.0001(11) -0.0013(11) C(15) 0.0201(15) 0.0168(15) 0.0199(16) 0.0003(12) 0.0026(12) -0.0070(12) C(16) 0.0214(15) 0.0146(14) 0.0195(15) -0.0042(12) 0.0061(12) -0.0071(12) C(17) 0.0156(14) 0.0162(15) 0.0178(15) 0.0006(11) 0.0045(11) -0.0028(11) C(18) 0.0167(14) 0.0132(14) 0.0205(15) -0.0035(11) 0.0072(12) 0.0015(11) C(19) 0.0323(19) 0.0231(17) 0.0113(15) -0.0006(14) 0.0069(13) 0.0001(12) C(20) 0.0284(18) 0.0250(18) 0.0186(16) -0.0034(14) 0.0093(14) 0.0062(13) C(21) 0.0168(15) 0.0231(17) 0.0241(17) -0.0043(13) 0.0081(13) -0.0004(14) C(22) 0.0156(14) 0.0186(15) 0.0146(14) -0.0005(12) 0.0076(11) 0.0017(11) C(23) 0.0186(16) 0.041(2) 0.0190(16) 0.0040(14) 0.0033(13) -0.0078(15) C(24) 0.0226(17) 0.0285(19) 0.032(2) 0.0064(14) 0.0053(14) -0.0019(15) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tb(1) O(1) 2.404(2) yes . . Tb(1) O(2) 2.391(2) yes . . Tb(1) O(3) 2.575(2) yes . . Tb(1) O(4) 2.5415(19) yes . . Tb(1) O(5) 2.492(2) yes . . Tb(1) O(6) 2.474(3) yes . . Tb(1) O(8) 2.442(2) yes . . Tb(1) O(9) 2.488(2) yes . . Tb(1) O(11) 2.474(2) yes . . Tb(1) O(12) 2.446(2) yes . . V(1) O(1) 1.987(2) yes . . V(1) O(2) 1.988(2) yes . . V(1) O(14) 2.357(2) yes . . V(1) O(15) 1.590(2) yes . . V(1) N(1) 2.070(2) yes . . V(1) N(2) 2.066(2) yes . . O(1) C(1) 1.335(3) yes . . O(2) C(12) 1.331(3) yes . . O(3) C(2) 1.393(4) yes . . O(3) C(8) 1.452(4) yes . . O(4) C(13) 1.383(3) yes . . O(4) C(19) 1.452(4) yes . . O(5) N(3) 1.265(3) yes . . O(6) N(3) 1.267(3) yes . . O(7) N(3) 1.219(4) yes . . O(8) N(4) 1.266(3) yes . . O(9) N(4) 1.272(3) yes . . O(10) N(4) 1.222(3) yes . . O(11) N(5) 1.278(3) yes . . O(12) N(5) 1.270(3) yes . . O(13) N(5) 1.219(3) yes . . O(14) C(22) 1.215(3) yes . . N(1) C(7) 1.285(3) yes . . N(1) C(9) 1.481(4) yes . . N(2) C(11) 1.471(4) yes . . N(2) C(18) 1.278(3) yes . . C(1) C(2) 1.408(4) yes . . C(1) C(6) 1.408(4) yes . . C(2) C(3) 1.382(4) yes . . C(3) C(4) 1.399(5) yes . . C(4) C(5) 1.370(4) yes . . C(5) C(6) 1.405(4) yes . . C(6) C(7) 1.460(4) yes . . C(9) C(10) 1.527(4) yes . . C(10) C(11) 1.535(4) yes . . C(10) C(20) 1.534(4) yes . . C(10) C(21) 1.535(4) yes . . C(12) C(13) 1.406(4) yes . . C(12) C(17) 1.410(4) yes . . C(13) C(14) 1.375(4) yes . . C(14) C(15) 1.394(4) yes . . C(15) C(16) 1.377(4) yes . . C(16) C(17) 1.413(4) yes . . C(17) C(18) 1.454(4) yes . . C(22) C(23) 1.499(4) yes . . C(22) C(24) 1.488(5) yes . . C(3) H(1) 0.89(3) no . . C(4) H(2) 0.96(3) no . . C(5) H(3) 0.92(3) no . . C(7) H(4) 0.98(3) no . . C(8) H(5) 0.99(3) no . . C(8) H(6) 0.96(5) no . . C(8) H(7) 1.11(3) no . . C(9) H(8) 0.99(4) no . . C(9) H(9) 0.99(3) no . . C(11) H(10) 0.94(3) no . . C(11) H(11) 0.94(3) no . . C(14) H(12) 0.88(3) no . . C(15) H(13) 0.97(3) no . . C(16) H(14) 0.98(3) no . . C(18) H(15) 0.99(3) no . . C(19) H(16) 0.94(4) no . . C(19) H(17) 0.95(4) no . . C(19) H(18) 0.94(4) no . . C(20) H(19) 0.95(4) no . . C(20) H(20) 1.01(4) no . . C(20) H(21) 0.94(4) no . . C(21) H(22) 0.99(4) no . . C(21) H(23) 0.95(3) no . . C(21) H(24) 0.97(4) no . . C(23) H(25) 0.877 no . . C(23) H(26) 0.992 no . . C(23) H(27) 0.919 no . . C(24) H(28) 0.880 no . . C(24) H(29) 0.973 no . . C(24) H(30) 0.959 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Tb(1) O(2) 64.40(7) yes . . . O(1) Tb(1) O(3) 62.91(6) yes . . . O(1) Tb(1) O(4) 122.47(7) yes . . . O(1) Tb(1) O(5) 117.76(7) yes . . . O(1) Tb(1) O(6) 165.75(7) yes . . . O(1) Tb(1) O(8) 71.38(8) yes . . . O(1) Tb(1) O(9) 102.97(8) yes . . . O(1) Tb(1) O(11) 115.95(7) yes . . . O(1) Tb(1) O(12) 72.34(7) yes . . . O(2) Tb(1) O(3) 124.37(7) yes . . . O(2) Tb(1) O(4) 63.04(7) yes . . . O(2) Tb(1) O(5) 160.07(7) yes . . . O(2) Tb(1) O(6) 122.56(7) yes . . . O(2) Tb(1) O(8) 92.66(7) yes . . . O(2) Tb(1) O(9) 70.88(7) yes . . . O(2) Tb(1) O(11) 120.28(6) yes . . . O(2) Tb(1) O(12) 76.92(7) yes . . . O(3) Tb(1) O(4) 141.46(6) yes . . . O(3) Tb(1) O(5) 67.36(8) yes . . . O(3) Tb(1) O(6) 112.85(7) yes . . . O(3) Tb(1) O(8) 86.77(7) yes . . . O(3) Tb(1) O(9) 137.81(6) yes . . . O(3) Tb(1) O(11) 70.73(6) yes . . . O(3) Tb(1) O(12) 71.53(7) yes . . . O(4) Tb(1) O(5) 119.67(7) yes . . . O(4) Tb(1) O(6) 69.90(7) yes . . . O(4) Tb(1) O(8) 131.76(7) yes . . . O(4) Tb(1) O(9) 80.49(7) yes . . . O(4) Tb(1) O(11) 74.15(6) yes . . . O(4) Tb(1) O(12) 74.66(7) yes . . . O(5) Tb(1) O(6) 51.00(8) yes . . . O(5) Tb(1) O(8) 70.84(8) yes . . . O(5) Tb(1) O(9) 89.75(8) yes . . . O(5) Tb(1) O(11) 77.70(7) yes . . . O(5) Tb(1) O(12) 122.99(7) yes . . . O(6) Tb(1) O(8) 95.19(8) yes . . . O(6) Tb(1) O(9) 70.60(8) yes . . . O(6) Tb(1) O(11) 72.63(8) yes . . . O(6) Tb(1) O(12) 120.30(7) yes . . . O(8) Tb(1) O(9) 51.56(8) yes . . . O(8) Tb(1) O(11) 146.61(7) yes . . . O(8) Tb(1) O(12) 143.23(8) yes . . . O(9) Tb(1) O(11) 140.65(8) yes . . . O(9) Tb(1) O(12) 145.73(7) yes . . . O(11) Tb(1) O(12) 52.05(7) yes . . . O(1) V(1) O(2) 80.03(8) yes . . . O(1) V(1) O(14) 81.07(8) yes . . . O(1) V(1) O(15) 105.42(10) yes . . . O(1) V(1) N(1) 90.53(9) yes . . . O(1) V(1) N(2) 159.46(8) yes . . . O(2) V(1) O(14) 79.05(8) yes . . . O(2) V(1) O(15) 102.84(11) yes . . . O(2) V(1) N(1) 159.80(9) yes . . . O(2) V(1) N(2) 90.75(9) yes . . . O(14) V(1) O(15) 173.43(10) yes . . . O(14) V(1) N(1) 81.88(8) yes . . . O(14) V(1) N(2) 79.17(8) yes . . . O(15) V(1) N(1) 96.85(11) yes . . . O(15) V(1) N(2) 94.47(10) yes . . . N(1) V(1) N(2) 92.17(10) yes . . . Tb(1) O(1) V(1) 104.95(8) yes . . . Tb(1) O(1) C(1) 125.70(18) yes . . . V(1) O(1) C(1) 128.7(2) yes . . . Tb(1) O(2) V(1) 105.38(8) yes . . . Tb(1) O(2) C(12) 124.97(18) yes . . . V(1) O(2) C(12) 127.0(2) yes . . . Tb(1) O(3) C(2) 118.90(17) yes . . . Tb(1) O(3) C(8) 125.8(2) yes . . . C(2) O(3) C(8) 114.9(2) yes . . . Tb(1) O(4) C(13) 119.27(17) yes . . . Tb(1) O(4) C(19) 124.73(18) yes . . . C(13) O(4) C(19) 115.4(2) yes . . . Tb(1) O(5) N(3) 96.46(18) yes . . . Tb(1) O(6) N(3) 97.3(2) yes . . . Tb(1) O(8) N(4) 97.61(16) yes . . . Tb(1) O(9) N(4) 95.22(18) yes . . . Tb(1) O(11) N(5) 95.02(15) yes . . . Tb(1) O(12) N(5) 96.63(17) yes . . . V(1) O(14) C(22) 159.8(2) yes . . . V(1) N(1) C(7) 124.7(2) yes . . . V(1) N(1) C(9) 118.86(19) yes . . . C(7) N(1) C(9) 116.1(2) yes . . . V(1) N(2) C(11) 118.41(17) yes . . . V(1) N(2) C(18) 123.9(2) yes . . . C(11) N(2) C(18) 117.6(2) yes . . . O(5) N(3) O(6) 115.2(3) yes . . . O(5) N(3) O(7) 122.1(2) yes . . . O(6) N(3) O(7) 122.6(3) yes . . . O(8) N(4) O(9) 115.4(2) yes . . . O(8) N(4) O(10) 122.2(2) yes . . . O(9) N(4) O(10) 122.5(2) yes . . . O(11) N(5) O(12) 115.8(2) yes . . . O(11) N(5) O(13) 122.2(2) yes . . . O(12) N(5) O(13) 122.0(2) yes . . . O(1) C(1) C(2) 117.7(2) yes . . . O(1) C(1) C(6) 123.9(2) yes . . . C(2) C(1) C(6) 118.4(2) yes . . . O(3) C(2) C(1) 114.3(2) yes . . . O(3) C(2) C(3) 124.2(2) yes . . . C(1) C(2) C(3) 121.5(3) yes . . . C(2) C(3) C(4) 119.3(3) yes . . . C(3) C(4) C(5) 120.2(3) yes . . . C(4) C(5) C(6) 121.2(3) yes . . . C(1) C(6) C(5) 119.3(2) yes . . . C(1) C(6) C(7) 124.4(2) yes . . . C(5) C(6) C(7) 116.2(2) yes . . . N(1) C(7) C(6) 126.9(3) yes . . . N(1) C(9) C(10) 115.7(2) yes . . . C(9) C(10) C(11) 112.8(2) yes . . . C(9) C(10) C(20) 106.1(2) yes . . . C(9) C(10) C(21) 111.6(2) yes . . . C(11) C(10) C(20) 105.6(2) yes . . . C(11) C(10) C(21) 110.2(2) yes . . . C(20) C(10) C(21) 110.2(3) yes . . . N(2) C(11) C(10) 115.1(2) yes . . . O(2) C(12) C(13) 117.6(2) yes . . . O(2) C(12) C(17) 124.1(2) yes . . . C(13) C(12) C(17) 118.3(2) yes . . . O(4) C(13) C(12) 113.8(2) yes . . . O(4) C(13) C(14) 124.8(2) yes . . . C(12) C(13) C(14) 121.4(3) yes . . . C(13) C(14) C(15) 120.2(3) yes . . . C(14) C(15) C(16) 119.9(2) yes . . . C(15) C(16) C(17) 120.7(3) yes . . . C(12) C(17) C(16) 119.4(2) yes . . . C(12) C(17) C(18) 124.1(2) yes . . . C(16) C(17) C(18) 116.5(2) yes . . . N(2) C(18) C(17) 127.2(2) yes . . . O(14) C(22) C(23) 122.0(3) yes . . . O(14) C(22) C(24) 121.4(2) yes . . . C(23) C(22) C(24) 116.6(2) yes . . . C(2) C(3) H(1) 121(2) no . . . C(4) C(3) H(1) 120(2) no . . . C(3) C(4) H(2) 119(2) no . . . C(5) C(4) H(2) 121(2) no . . . C(4) C(5) H(3) 122(2) no . . . C(6) C(5) H(3) 116(2) no . . . N(1) C(7) H(4) 117.3(17) no . . . C(6) C(7) H(4) 115.7(17) no . . . O(3) C(8) H(5) 109(2) no . . . O(3) C(8) H(6) 110(2) no . . . O(3) C(8) H(7) 101(2) no . . . H(5) C(8) H(6) 112(3) no . . . H(5) C(8) H(7) 116(2) no . . . H(6) C(8) H(7) 108(3) no . . . N(1) C(9) H(8) 111(2) no . . . N(1) C(9) H(9) 103(2) no . . . C(10) C(9) H(8) 111(2) no . . . C(10) C(9) H(9) 109.3(19) no . . . H(8) C(9) H(9) 107(3) no . . . N(2) C(11) H(10) 109(2) no . . . N(2) C(11) H(11) 106(2) no . . . C(10) C(11) H(10) 110(2) no . . . C(10) C(11) H(11) 110(2) no . . . H(10) C(11) H(11) 107(2) no . . . C(13) C(14) H(12) 124(2) no . . . C(15) C(14) H(12) 116(2) no . . . C(14) C(15) H(13) 121(2) no . . . C(16) C(15) H(13) 119(2) no . . . C(15) C(16) H(14) 121.1(18) no . . . C(17) C(16) H(14) 118.2(19) no . . . N(2) C(18) H(15) 120.4(19) no . . . C(17) C(18) H(15) 112.4(19) no . . . O(4) C(19) H(16) 108(2) no . . . O(4) C(19) H(17) 113(3) no . . . O(4) C(19) H(18) 110(2) no . . . H(16) C(19) H(17) 103(3) no . . . H(16) C(19) H(18) 114(3) no . . . H(17) C(19) H(18) 108(3) no . . . C(10) C(20) H(19) 114(2) no . . . C(10) C(20) H(20) 111(2) no . . . C(10) C(20) H(21) 109(2) no . . . H(19) C(20) H(20) 105(3) no . . . H(19) C(20) H(21) 110(3) no . . . H(20) C(20) H(21) 108(3) no . . . C(10) C(21) H(22) 108(2) no . . . C(10) C(21) H(23) 108(2) no . . . C(10) C(21) H(24) 113(2) no . . . H(22) C(21) H(23) 110(3) no . . . H(22) C(21) H(24) 107(3) no . . . H(23) C(21) H(24) 110(3) no . . . C(22) C(23) H(25) 117.2 no . . . C(22) C(23) H(26) 109.6 no . . . C(22) C(23) H(27) 108.3 no . . . H(25) C(23) H(26) 101.2 no . . . H(25) C(23) H(27) 116.6 no . . . H(26) C(23) H(27) 102.4 no . . . C(22) C(24) H(28) 112.0 no . . . C(22) C(24) H(29) 108.9 no . . . C(22) C(24) H(30) 112.7 no . . . H(28) C(24) H(29) 101.1 no . . . H(28) C(24) H(30) 111.6 no . . . H(29) C(24) H(30) 109.8 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Tb(1) O(2) V(1) -16.69(7) ? . . . . O(1) Tb(1) O(2) C(12) 145.9(2) ? . . . . O(2) Tb(1) O(1) V(1) 16.67(7) ? . . . . O(2) Tb(1) O(1) C(1) -154.8(2) ? . . . . O(1) Tb(1) O(3) C(2) -5.74(16) ? . . . . O(1) Tb(1) O(3) C(8) -178.0(2) ? . . . . O(3) Tb(1) O(1) V(1) 178.15(11) ? . . . . O(3) Tb(1) O(1) C(1) 6.69(18) ? . . . . O(1) Tb(1) O(4) C(13) -16.3(2) ? . . . . O(1) Tb(1) O(4) C(19) 154.2(2) ? . . . . O(4) Tb(1) O(1) V(1) 42.43(11) ? . . . . O(4) Tb(1) O(1) C(1) -129.03(19) ? . . . . O(1) Tb(1) O(5) N(3) 170.88(15) ? . . . . O(5) Tb(1) O(1) V(1) -141.12(8) ? . . . . O(5) Tb(1) O(1) C(1) 47.4(2) ? . . . . O(1) Tb(1) O(6) N(3) -42.5(3) ? . . . . O(6) Tb(1) O(1) V(1) -105.9(2) ? . . . . O(6) Tb(1) O(1) C(1) 82.7(3) ? . . . . O(1) Tb(1) O(8) N(4) 121.8(2) ? . . . . O(8) Tb(1) O(1) V(1) -85.79(9) ? . . . . O(8) Tb(1) O(1) C(1) 102.8(2) ? . . . . O(1) Tb(1) O(9) N(4) -50.1(2) ? . . . . O(9) Tb(1) O(1) V(1) -44.45(9) ? . . . . O(9) Tb(1) O(1) C(1) 144.10(19) ? . . . . O(1) Tb(1) O(11) N(5) -32.07(16) ? . . . . O(11) Tb(1) O(1) V(1) 129.54(8) ? . . . . O(11) Tb(1) O(1) C(1) -41.9(2) ? . . . . O(1) Tb(1) O(12) N(5) 142.03(17) ? . . . . O(12) Tb(1) O(1) V(1) 100.31(9) ? . . . . O(12) Tb(1) O(1) C(1) -71.15(19) ? . . . . O(2) Tb(1) O(3) C(2) 14.6(2) ? . . . . O(2) Tb(1) O(3) C(8) -157.7(2) ? . . . . O(3) Tb(1) O(2) V(1) -36.74(11) ? . . . . O(3) Tb(1) O(2) C(12) 125.9(2) ? . . . . O(2) Tb(1) O(4) C(13) 9.79(18) ? . . . . O(2) Tb(1) O(4) C(19) -179.7(2) ? . . . . O(4) Tb(1) O(2) V(1) -172.41(11) ? . . . . O(4) Tb(1) O(2) C(12) -9.8(2) ? . . . . O(2) Tb(1) O(5) N(3) 79.8(2) ? . . . . O(5) Tb(1) O(2) V(1) 84.5(2) ? . . . . O(5) Tb(1) O(2) C(12) -112.9(2) ? . . . . O(2) Tb(1) O(6) N(3) -158.07(15) ? . . . . O(6) Tb(1) O(2) V(1) 149.05(8) ? . . . . O(6) Tb(1) O(2) C(12) -48.3(2) ? . . . . O(2) Tb(1) O(8) N(4) 60.0(2) ? . . . . O(8) Tb(1) O(2) V(1) 51.18(10) ? . . . . O(8) Tb(1) O(2) C(12) -146.2(2) ? . . . . O(2) Tb(1) O(9) N(4) -106.8(2) ? . . . . O(9) Tb(1) O(2) V(1) 98.74(9) ? . . . . O(9) Tb(1) O(2) C(12) -98.6(2) ? . . . . O(2) Tb(1) O(11) N(5) 42.13(17) ? . . . . O(11) Tb(1) O(2) V(1) -123.08(8) ? . . . . O(11) Tb(1) O(2) C(12) 39.5(2) ? . . . . O(2) Tb(1) O(12) N(5) -151.02(16) ? . . . . O(12) Tb(1) O(2) V(1) -93.16(9) ? . . . . O(12) Tb(1) O(2) C(12) 69.5(2) ? . . . . O(3) Tb(1) O(4) C(13) -102.4(2) ? . . . . O(3) Tb(1) O(4) C(19) 68.1(2) ? . . . . O(4) Tb(1) O(3) C(2) 103.27(19) ? . . . . O(4) Tb(1) O(3) C(8) -69.0(2) ? . . . . O(3) Tb(1) O(5) N(3) -150.12(18) ? . . . . O(5) Tb(1) O(3) C(2) -147.02(19) ? . . . . O(5) Tb(1) O(3) C(8) 40.8(2) ? . . . . O(3) Tb(1) O(6) N(3) 27.11(18) ? . . . . O(6) Tb(1) O(3) C(2) -170.72(17) ? . . . . O(6) Tb(1) O(3) C(8) 17.0(2) ? . . . . O(3) Tb(1) O(8) N(4) -175.8(2) ? . . . . O(8) Tb(1) O(3) C(2) -76.45(18) ? . . . . O(8) Tb(1) O(3) C(8) 111.3(2) ? . . . . O(3) Tb(1) O(9) N(4) 13.7(2) ? . . . . O(9) Tb(1) O(3) C(2) -84.9(2) ? . . . . O(9) Tb(1) O(3) C(8) 102.9(2) ? . . . . O(3) Tb(1) O(11) N(5) -77.11(15) ? . . . . O(11) Tb(1) O(3) C(2) 128.65(19) ? . . . . O(11) Tb(1) O(3) C(8) -43.6(2) ? . . . . O(3) Tb(1) O(12) N(5) 75.45(16) ? . . . . O(12) Tb(1) O(3) C(2) 73.40(18) ? . . . . O(12) Tb(1) O(3) C(8) -98.8(2) ? . . . . O(4) Tb(1) O(5) N(3) -12.57(19) ? . . . . O(5) Tb(1) O(4) C(13) 167.33(19) ? . . . . O(5) Tb(1) O(4) C(19) -22.2(2) ? . . . . O(4) Tb(1) O(6) N(3) 165.67(18) ? . . . . O(6) Tb(1) O(4) C(13) 155.8(2) ? . . . . O(6) Tb(1) O(4) C(19) -33.7(2) ? . . . . O(4) Tb(1) O(8) N(4) 4.5(2) ? . . . . O(8) Tb(1) O(4) C(13) 77.2(2) ? . . . . O(8) Tb(1) O(4) C(19) -112.3(2) ? . . . . O(4) Tb(1) O(9) N(4) -171.5(2) ? . . . . O(9) Tb(1) O(4) C(13) 83.1(2) ? . . . . O(9) Tb(1) O(4) C(19) -106.4(2) ? . . . . O(4) Tb(1) O(11) N(5) 86.77(15) ? . . . . O(11) Tb(1) O(4) C(13) -127.3(2) ? . . . . O(11) Tb(1) O(4) C(19) 43.2(2) ? . . . . O(4) Tb(1) O(12) N(5) -85.78(16) ? . . . . O(12) Tb(1) O(4) C(13) -73.1(2) ? . . . . O(12) Tb(1) O(4) C(19) 97.4(2) ? . . . . O(5) Tb(1) O(6) N(3) -1.41(15) ? . . . . O(6) Tb(1) O(5) N(3) 1.41(15) ? . . . . O(5) Tb(1) O(8) N(4) -108.6(2) ? . . . . O(8) Tb(1) O(5) N(3) 115.27(18) ? . . . . O(5) Tb(1) O(9) N(4) 68.36(19) ? . . . . O(9) Tb(1) O(5) N(3) 66.32(17) ? . . . . O(5) Tb(1) O(11) N(5) -147.17(16) ? . . . . O(11) Tb(1) O(5) N(3) -76.08(16) ? . . . . O(5) Tb(1) O(12) N(5) 29.93(18) ? . . . . O(12) Tb(1) O(5) N(3) -102.96(17) ? . . . . O(6) Tb(1) O(8) N(4) -63.1(2) ? . . . . O(8) Tb(1) O(6) N(3) -61.57(17) ? . . . . O(6) Tb(1) O(9) N(4) 116.6(2) ? . . . . O(9) Tb(1) O(6) N(3) -107.64(18) ? . . . . O(6) Tb(1) O(11) N(5) 160.19(16) ? . . . . O(11) Tb(1) O(6) N(3) 86.65(17) ? . . . . O(6) Tb(1) O(12) N(5) -30.74(18) ? . . . . O(12) Tb(1) O(6) N(3) 108.37(17) ? . . . . O(8) Tb(1) O(9) N(4) 2.92(17) ? . . . . O(9) Tb(1) O(8) N(4) -2.95(18) ? . . . . O(8) Tb(1) O(11) N(5) -127.41(18) ? . . . . O(11) Tb(1) O(8) N(4) -129.08(19) ? . . . . O(8) Tb(1) O(12) N(5) 132.35(16) ? . . . . O(12) Tb(1) O(8) N(4) 131.52(19) ? . . . . O(9) Tb(1) O(11) N(5) 138.66(15) ? . . . . O(11) Tb(1) O(9) N(4) 138.41(18) ? . . . . O(9) Tb(1) O(12) N(5) -130.78(18) ? . . . . O(12) Tb(1) O(9) N(4) -127.73(18) ? . . . . O(11) Tb(1) O(12) N(5) -4.13(14) ? . . . . O(12) Tb(1) O(11) N(5) 4.09(14) ? . . . . O(1) V(1) O(2) Tb(1) 18.56(8) ? . . . . O(1) V(1) O(2) C(12) -143.6(2) ? . . . . O(2) V(1) O(1) Tb(1) -18.42(8) ? . . . . O(2) V(1) O(1) C(1) 152.7(2) ? . . . . O(1) V(1) O(14) C(22) 32.6(6) ? . . . . O(14) V(1) O(1) Tb(1) -98.78(8) ? . . . . O(14) V(1) O(1) C(1) 72.3(2) ? . . . . O(15) V(1) O(1) Tb(1) 82.27(11) ? . . . . O(15) V(1) O(1) C(1) -106.6(2) ? . . . . O(1) V(1) N(1) C(7) 8.7(2) ? . . . . O(1) V(1) N(1) C(9) -164.8(2) ? . . . . N(1) V(1) O(1) Tb(1) 179.53(9) ? . . . . N(1) V(1) O(1) C(1) -9.4(2) ? . . . . O(1) V(1) N(2) C(11) -134.4(2) ? . . . . O(1) V(1) N(2) C(18) 49.4(4) ? . . . . N(2) V(1) O(1) Tb(1) -82.8(3) ? . . . . N(2) V(1) O(1) C(1) 88.3(3) ? . . . . O(2) V(1) O(14) C(22) -48.8(6) ? . . . . O(14) V(1) O(2) Tb(1) 101.30(9) ? . . . . O(14) V(1) O(2) C(12) -60.9(2) ? . . . . O(15) V(1) O(2) Tb(1) -85.13(10) ? . . . . O(15) V(1) O(2) C(12) 112.7(2) ? . . . . O(2) V(1) N(1) C(7) -52.8(4) ? . . . . O(2) V(1) N(1) C(9) 133.7(2) ? . . . . N(1) V(1) O(2) Tb(1) 81.8(2) ? . . . . N(1) V(1) O(2) C(12) -80.4(3) ? . . . . O(2) V(1) N(2) C(11) 162.9(2) ? . . . . O(2) V(1) N(2) C(18) -13.3(2) ? . . . . N(2) V(1) O(2) Tb(1) -179.89(9) ? . . . . N(2) V(1) O(2) C(12) 18.0(2) ? . . . . O(14) V(1) N(1) C(7) -72.2(2) ? . . . . O(14) V(1) N(1) C(9) 114.3(2) ? . . . . N(1) V(1) O(14) C(22) 124.5(6) ? . . . . O(14) V(1) N(2) C(11) -118.4(2) ? . . . . O(14) V(1) N(2) C(18) 65.4(2) ? . . . . N(2) V(1) O(14) C(22) -141.7(6) ? . . . . O(15) V(1) N(1) C(7) 114.3(2) ? . . . . O(15) V(1) N(1) C(9) -59.2(2) ? . . . . O(15) V(1) N(2) C(11) 60.0(2) ? . . . . O(15) V(1) N(2) C(18) -116.2(2) ? . . . . N(1) V(1) N(2) C(11) -37.1(2) ? . . . . N(1) V(1) N(2) C(18) 146.7(2) ? . . . . N(2) V(1) N(1) C(7) -150.9(2) ? . . . . N(2) V(1) N(1) C(9) 35.6(2) ? . . . . Tb(1) O(1) C(1) C(2) -7.0(3) ? . . . . Tb(1) O(1) C(1) C(6) 174.86(18) ? . . . . V(1) O(1) C(1) C(2) -176.38(17) ? . . . . V(1) O(1) C(1) C(6) 5.5(3) ? . . . . Tb(1) O(2) C(12) C(13) 8.9(3) ? . . . . Tb(1) O(2) C(12) C(17) -171.0(2) ? . . . . V(1) O(2) C(12) C(13) 167.8(2) ? . . . . V(1) O(2) C(12) C(17) -12.1(4) ? . . . . Tb(1) O(3) C(2) C(1) 4.9(2) ? . . . . Tb(1) O(3) C(2) C(3) -175.5(2) ? . . . . C(8) O(3) C(2) C(1) 177.9(2) ? . . . . C(8) O(3) C(2) C(3) -2.5(3) ? . . . . Tb(1) O(4) C(13) C(12) -9.5(3) ? . . . . Tb(1) O(4) C(13) C(14) 168.6(2) ? . . . . C(19) O(4) C(13) C(12) 179.1(2) ? . . . . C(19) O(4) C(13) C(14) -2.8(4) ? . . . . Tb(1) O(5) N(3) O(6) -2.4(2) ? . . . . Tb(1) O(5) N(3) O(7) 179.2(2) ? . . . . Tb(1) O(6) N(3) O(5) 2.4(2) ? . . . . Tb(1) O(6) N(3) O(7) -179.2(2) ? . . . . Tb(1) O(8) N(4) O(9) 5.0(3) ? . . . . Tb(1) O(8) N(4) O(10) -175.0(2) ? . . . . Tb(1) O(9) N(4) O(8) -4.9(3) ? . . . . Tb(1) O(9) N(4) O(10) 175.1(3) ? . . . . Tb(1) O(11) N(5) O(12) -6.9(2) ? . . . . Tb(1) O(11) N(5) O(13) 172.4(2) ? . . . . Tb(1) O(12) N(5) O(11) 7.0(2) ? . . . . Tb(1) O(12) N(5) O(13) -172.3(2) ? . . . . V(1) O(14) C(22) C(23) 89.9(6) ? . . . . V(1) O(14) C(22) C(24) -88.7(6) ? . . . . V(1) N(1) C(7) C(6) -4.6(4) ? . . . . V(1) N(1) C(9) C(10) -53.5(3) ? . . . . C(7) N(1) C(9) C(10) 132.4(2) ? . . . . C(9) N(1) C(7) C(6) 169.1(2) ? . . . . V(1) N(2) C(11) C(10) 56.4(3) ? . . . . V(1) N(2) C(18) C(17) 2.9(4) ? . . . . C(11) N(2) C(18) C(17) -173.3(3) ? . . . . C(18) N(2) C(11) C(10) -127.2(3) ? . . . . O(1) C(1) C(2) O(3) 0.8(3) ? . . . . O(1) C(1) C(2) C(3) -178.8(2) ? . . . . O(1) C(1) C(6) C(5) 178.3(2) ? . . . . O(1) C(1) C(6) C(7) 2.8(4) ? . . . . C(2) C(1) C(6) C(5) 0.1(3) ? . . . . C(2) C(1) C(6) C(7) -175.3(2) ? . . . . C(6) C(1) C(2) O(3) 179.1(2) ? . . . . C(6) C(1) C(2) C(3) -0.6(3) ? . . . . O(3) C(2) C(3) C(4) -178.6(2) ? . . . . C(1) C(2) C(3) C(4) 1.0(4) ? . . . . C(2) C(3) C(4) C(5) -1.0(4) ? . . . . C(3) C(4) C(5) C(6) 0.6(4) ? . . . . C(4) C(5) C(6) C(1) -0.1(3) ? . . . . C(4) C(5) C(6) C(7) 175.7(2) ? . . . . C(1) C(6) C(7) N(1) -3.1(4) ? . . . . C(5) C(6) C(7) N(1) -178.6(2) ? . . . . N(1) C(9) C(10) C(11) 64.0(3) ? . . . . N(1) C(9) C(10) C(20) 179.3(2) ? . . . . N(1) C(9) C(10) C(21) -60.7(3) ? . . . . C(9) C(10) C(11) N(2) -65.7(3) ? . . . . C(20) C(10) C(11) N(2) 178.8(2) ? . . . . C(21) C(10) C(11) N(2) 59.8(3) ? . . . . O(2) C(12) C(13) O(4) 1.1(4) ? . . . . O(2) C(12) C(13) C(14) -177.1(2) ? . . . . O(2) C(12) C(17) C(16) 176.8(2) ? . . . . O(2) C(12) C(17) C(18) -5.0(5) ? . . . . C(13) C(12) C(17) C(16) -3.1(4) ? . . . . C(13) C(12) C(17) C(18) 175.1(3) ? . . . . C(17) C(12) C(13) O(4) -179.0(2) ? . . . . C(17) C(12) C(13) C(14) 2.8(4) ? . . . . O(4) C(13) C(14) C(15) -178.6(3) ? . . . . C(12) C(13) C(14) C(15) -0.6(5) ? . . . . C(13) C(14) C(15) C(16) -1.3(5) ? . . . . C(14) C(15) C(16) C(17) 1.0(5) ? . . . . C(15) C(16) C(17) C(12) 1.2(4) ? . . . . C(15) C(16) C(17) C(18) -177.1(3) ? . . . . C(12) C(17) C(18) N(2) 9.7(5) ? . . . . C(16) C(17) C(18) N(2) -172.0(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(5) C(24) 3.540(3) ? . 1_655 O(6) C(19) 3.451(5) ? . 3_765 O(7) C(11) 3.127(4) ? . 2_755 O(7) C(19) 3.447(4) ? . 3_765 O(7) C(23) 3.357(4) ? . 1_655 O(8) C(9) 3.374(4) ? . 3_766 O(8) C(20) 3.549(4) ? . 3_766 O(8) C(24) 3.552(4) ? . 1_655 O(9) C(8) 3.412(4) ? . 2_745 O(10) C(8) 3.576(4) ? . 2_745 O(10) C(21) 3.336(3) ? . 1_655 O(10) C(22) 3.346(4) ? . 1_655 O(10) C(23) 3.352(5) ? . 1_655 O(11) C(4) 3.385(4) ? . 4_564 O(11) C(5) 3.396(4) ? . 4_564 O(13) C(14) 3.547(3) ? . 3_665 O(13) C(15) 3.296(4) ? . 3_665 O(15) N(1) 3.427(3) ? . 3_766 O(15) C(7) 2.958(3) ? . 3_766 O(15) C(8) 3.553(4) ? . 2_745 O(15) C(9) 3.332(3) ? . 3_766 N(1) O(15) 3.427(3) ? . 3_766 N(3) C(23) 3.425(4) ? . 1_655 N(4) C(23) 3.377(4) ? . 1_655 C(4) O(11) 3.385(4) ? . 4_565 C(5) O(11) 3.396(4) ? . 4_565 C(7) O(15) 2.958(3) ? . 3_766 C(8) O(9) 3.412(4) ? . 2_755 C(8) O(10) 3.576(4) ? . 2_755 C(8) O(15) 3.553(4) ? . 2_755 C(9) O(8) 3.374(4) ? . 3_766 C(9) O(15) 3.332(3) ? . 3_766 C(11) O(7) 3.127(4) ? . 2_745 C(14) O(13) 3.547(3) ? . 3_665 C(15) O(13) 3.296(4) ? . 3_665 C(19) O(6) 3.451(5) ? . 3_765 C(19) O(7) 3.447(4) ? . 3_765 C(20) O(8) 3.549(4) ? . 3_766 C(21) O(10) 3.336(3) ? . 1_455 C(22) O(10) 3.346(4) ? . 1_455 C(23) O(7) 3.357(4) ? . 1_455 C(23) O(10) 3.352(5) ? . 1_455 C(23) N(3) 3.425(4) ? . 1_455 C(23) N(4) 3.377(4) ? . 1_455 C(24) O(5) 3.540(3) ? . 1_455 C(24) O(8) 3.552(4) ? . 1_455 V(1) H(9) 3.56(3) ? . 3_766 O(1) H(8) 3.53(3) ? . 3_766 O(1) H(9) 3.06(3) ? . 3_766 O(2) H(7) 3.24(4) ? . 2_745 O(3) H(21) 3.47(3) ? . 3_766 O(5) H(11) 3.58(3) ? . 2_755 O(5) H(15) 3.56(3) ? . 2_755 O(5) H(27) 3.100 ? . 1_655 O(5) H(28) 2.806 ? . 1_655 O(5) H(29) 3.446 ? . 1_655 O(6) H(2) 3.25(3) ? . 4_564 O(6) H(16) 3.43(4) ? . 3_765 O(6) H(18) 2.71(4) ? . 3_765 O(6) H(27) 3.010 ? . 1_655 O(7) H(10) 2.54(3) ? . 2_755 O(7) H(11) 2.83(3) ? . 2_755 O(7) H(12) 3.19(4) ? . 3_765 O(7) H(15) 3.54(3) ? . 2_755 O(7) H(18) 2.51(4) ? . 3_765 O(7) H(26) 2.718 ? . 1_655 O(7) H(27) 3.003 ? . 1_655 O(7) H(29) 3.526 ? . 1_655 O(8) H(8) 2.53(4) ? . 3_766 O(8) H(9) 3.41(4) ? . 3_766 O(8) H(19) 2.88(4) ? . 3_766 O(8) H(21) 3.55(4) ? . 3_766 O(8) H(27) 3.101 ? . 1_655 O(8) H(28) 2.795 ? . 1_655 O(9) H(1) 2.74(3) ? . 2_745 O(9) H(5) 2.89(3) ? . 2_745 O(9) H(7) 3.16(4) ? . 2_745 O(9) H(27) 2.762 ? . 1_655 O(10) H(4) 3.18(3) ? . 3_766 O(10) H(5) 2.68(3) ? . 2_745 O(10) H(8) 3.07(4) ? . 3_766 O(10) H(23) 3.11(3) ? . 1_655 O(10) H(24) 2.79(3) ? . 1_655 O(10) H(25) 3.597 ? . 1_655 O(10) H(27) 2.868 ? . 1_655 O(10) H(28) 3.509 ? . 1_655 O(11) H(2) 2.75(3) ? . 4_564 O(11) H(3) 2.83(3) ? . 4_564 O(11) H(13) 3.09(3) ? . 3_665 O(13) H(3) 3.24(3) ? . 4_564 O(13) H(10) 2.99(3) ? . 2_655 O(13) H(12) 3.05(3) ? . 3_665 O(13) H(13) 2.55(4) ? . 3_665 O(13) H(15) 3.38(3) ? . 2_655 O(13) H(20) 3.27(3) ? . 2_655 O(13) H(23) 2.83(3) ? . 2_655 O(15) H(3) 3.57(3) ? . 3_766 O(15) H(4) 2.51(2) ? . 3_766 O(15) H(5) 3.45(3) ? . 2_745 O(15) H(6) 3.16(4) ? . 2_745 O(15) H(8) 2.87(3) ? . 3_766 O(15) H(9) 3.14(3) ? . 3_766 N(1) H(9) 3.11(3) ? . 3_766 N(2) H(6) 3.56(4) ? . 2_745 N(3) H(2) 3.55(3) ? . 4_564 N(3) H(10) 3.44(3) ? . 2_755 N(3) H(11) 3.42(3) ? . 2_755 N(3) H(18) 2.93(4) ? . 3_765 N(3) H(26) 3.115 ? . 1_655 N(3) H(27) 2.777 ? . 1_655 N(3) H(28) 3.401 ? . 1_655 N(4) H(1) 3.59(3) ? . 2_745 N(4) H(5) 3.06(3) ? . 2_745 N(4) H(8) 3.11(4) ? . 3_766 N(4) H(27) 2.629 ? . 1_655 N(4) H(28) 3.265 ? . 1_655 N(5) H(3) 3.43(3) ? . 4_564 N(5) H(12) 3.36(3) ? . 3_665 N(5) H(13) 3.01(3) ? . 3_665 C(1) H(9) 2.94(3) ? . 3_766 C(1) H(21) 3.30(3) ? . 3_766 C(2) H(21) 3.06(3) ? . 3_766 C(3) H(14) 3.43(3) ? . 2_655 C(3) H(21) 3.32(3) ? . 3_766 C(4) H(13) 3.08(4) ? . 2_655 C(4) H(14) 3.21(3) ? . 2_655 C(4) H(16) 3.31(4) ? . 4_565 C(5) H(11) 3.52(3) ? . 3_766 C(5) H(13) 3.13(4) ? . 2_655 C(5) H(14) 3.48(3) ? . 2_655 C(6) H(9) 2.88(3) ? . 3_766 C(7) H(9) 2.95(4) ? . 3_766 C(7) H(22) 3.43(4) ? . 3_666 C(12) H(7) 3.10(3) ? . 2_745 C(14) H(17) 2.98(4) ? . 3_665 C(14) H(20) 3.15(4) ? . 4_554 C(15) H(2) 3.39(3) ? . 2_645 C(15) H(17) 3.01(4) ? . 3_665 C(15) H(20) 2.71(4) ? . 4_554 C(16) H(20) 3.22(4) ? . 4_554 C(16) H(29) 3.341 ? . 2_645 C(16) H(30) 3.347 ? . 2_645 C(17) H(7) 3.26(4) ? . 2_745 C(18) H(7) 3.51(4) ? . 2_745 C(18) H(29) 3.321 ? . 2_645 C(19) H(2) 3.16(3) ? . 4_564 C(19) H(25) 3.463 ? . 3_665 C(19) H(26) 3.293 ? . 3_665 C(20) H(13) 3.55(3) ? . 4_555 C(20) H(28) 3.507 ? . 3_666 C(21) H(4) 3.46(3) ? . 3_666 C(21) H(22) 3.24(4) ? . 3_666 C(23) H(17) 3.23(4) ? . 3_665 C(23) H(18) 3.34(3) ? . 3_665 C(24) H(14) 2.93(3) ? . 2_655 C(24) H(15) 3.23(3) ? . 2_655 C(24) H(19) 3.10(5) ? . 3_666 H(1) O(9) 2.74(3) ? . 2_755 H(1) N(4) 3.59(3) ? . 2_755 H(2) O(6) 3.25(3) ? . 4_565 H(2) O(11) 2.75(3) ? . 4_565 H(2) N(3) 3.55(3) ? . 4_565 H(2) C(15) 3.39(3) ? . 2_655 H(2) C(19) 3.16(3) ? . 4_565 H(2) H(13) 2.83(5) ? . 2_655 H(2) H(14) 3.44(4) ? . 2_655 H(2) H(16) 2.36(5) ? . 4_565 H(2) H(17) 3.09(5) ? . 4_565 H(3) O(11) 2.83(3) ? . 4_565 H(3) O(13) 3.24(3) ? . 4_565 H(3) O(15) 3.57(3) ? . 3_766 H(3) N(5) 3.43(3) ? . 4_565 H(3) H(6) 3.32(5) ? . 4_565 H(3) H(13) 2.88(5) ? . 2_655 H(3) H(23) 3.28(5) ? . 3_666 H(4) O(10) 3.18(3) ? . 3_766 H(4) O(15) 2.51(2) ? . 3_766 H(4) C(21) 3.46(3) ? . 3_666 H(4) H(9) 3.43(5) ? . 3_766 H(4) H(22) 2.99(5) ? . 3_666 H(4) H(23) 3.19(5) ? . 3_666 H(5) O(9) 2.89(3) ? . 2_755 H(5) O(10) 2.68(3) ? . 2_755 H(5) O(15) 3.45(3) ? . 2_755 H(5) N(4) 3.06(3) ? . 2_755 H(6) O(15) 3.16(4) ? . 2_755 H(6) N(2) 3.56(4) ? . 2_755 H(6) H(3) 3.32(5) ? . 4_564 H(6) H(11) 3.30(6) ? . 2_755 H(7) O(2) 3.24(4) ? . 2_755 H(7) O(9) 3.16(4) ? . 2_755 H(7) C(12) 3.10(3) ? . 2_755 H(7) C(17) 3.26(4) ? . 2_755 H(7) C(18) 3.51(4) ? . 2_755 H(7) H(21) 3.40(5) ? . 3_766 H(8) O(1) 3.53(3) ? . 3_766 H(8) O(8) 2.53(4) ? . 3_766 H(8) O(10) 3.07(4) ? . 3_766 H(8) O(15) 2.87(3) ? . 3_766 H(8) N(4) 3.11(4) ? . 3_766 H(8) H(22) 3.54(5) ? . 3_666 H(9) V(1) 3.56(3) ? . 3_766 H(9) O(1) 3.06(3) ? . 3_766 H(9) O(8) 3.41(4) ? . 3_766 H(9) O(15) 3.14(3) ? . 3_766 H(9) N(1) 3.11(3) ? . 3_766 H(9) C(1) 2.94(3) ? . 3_766 H(9) C(6) 2.88(3) ? . 3_766 H(9) C(7) 2.95(4) ? . 3_766 H(9) H(4) 3.43(5) ? . 3_766 H(9) H(9) 3.53(5) ? . 3_766 H(10) O(7) 2.54(3) ? . 2_745 H(10) O(13) 2.99(3) ? . 2_645 H(10) N(3) 3.44(3) ? . 2_745 H(11) O(5) 3.58(3) ? . 2_745 H(11) O(7) 2.83(3) ? . 2_745 H(11) N(3) 3.42(3) ? . 2_745 H(11) C(5) 3.52(3) ? . 3_766 H(11) H(6) 3.30(6) ? . 2_745 H(12) O(7) 3.19(4) ? . 3_765 H(12) O(13) 3.05(3) ? . 3_665 H(12) N(5) 3.36(3) ? . 3_665 H(12) H(17) 2.89(6) ? . 3_665 H(12) H(20) 3.32(5) ? . 4_554 H(12) H(26) 2.832 ? . 3_665 H(13) O(11) 3.09(3) ? . 3_665 H(13) O(13) 2.55(4) ? . 3_665 H(13) N(5) 3.01(3) ? . 3_665 H(13) C(4) 3.08(4) ? . 2_645 H(13) C(5) 3.13(4) ? . 2_645 H(13) C(20) 3.55(3) ? . 4_554 H(13) H(2) 2.83(5) ? . 2_645 H(13) H(3) 2.88(5) ? . 2_645 H(13) H(16) 3.58(5) ? . 3_665 H(13) H(17) 3.04(5) ? . 3_665 H(13) H(20) 2.60(6) ? . 4_554 H(13) H(23) 3.59(5) ? . 4_554 H(14) C(3) 3.43(3) ? . 2_645 H(14) C(4) 3.21(3) ? . 2_645 H(14) C(5) 3.48(3) ? . 2_645 H(14) C(24) 2.93(3) ? . 2_645 H(14) H(2) 3.44(4) ? . 2_645 H(14) H(20) 3.49(6) ? . 4_554 H(14) H(28) 3.107 ? . 2_645 H(14) H(29) 2.549 ? . 2_645 H(14) H(30) 2.580 ? . 2_645 H(15) O(5) 3.56(3) ? . 2_745 H(15) O(7) 3.54(3) ? . 2_745 H(15) O(13) 3.38(3) ? . 2_645 H(15) C(24) 3.23(3) ? . 2_645 H(15) H(28) 3.201 ? . 2_645 H(15) H(29) 2.412 ? . 2_645 H(15) H(30) 3.554 ? . 2_645 H(16) O(6) 3.43(4) ? . 3_765 H(16) C(4) 3.31(4) ? . 4_564 H(16) H(2) 2.36(5) ? . 4_564 H(16) H(13) 3.58(5) ? . 3_665 H(17) C(14) 2.98(4) ? . 3_665 H(17) C(15) 3.01(4) ? . 3_665 H(17) C(23) 3.23(4) ? . 3_665 H(17) H(2) 3.09(5) ? . 4_564 H(17) H(12) 2.89(6) ? . 3_665 H(17) H(13) 3.04(5) ? . 3_665 H(17) H(25) 2.821 ? . 3_665 H(17) H(26) 2.876 ? . 3_665 H(17) H(27) 3.358 ? . 3_665 H(18) O(6) 2.71(4) ? . 3_765 H(18) O(7) 2.51(4) ? . 3_765 H(18) N(3) 2.93(4) ? . 3_765 H(18) C(23) 3.34(3) ? . 3_665 H(18) H(25) 3.318 ? . 3_665 H(18) H(26) 2.818 ? . 3_665 H(18) H(27) 3.150 ? . 3_665 H(19) O(8) 2.88(4) ? . 3_766 H(19) C(24) 3.10(5) ? . 3_666 H(19) H(28) 2.575 ? . 3_666 H(19) H(30) 2.837 ? . 3_666 H(20) O(13) 3.27(3) ? . 2_645 H(20) C(14) 3.15(4) ? . 4_555 H(20) C(15) 2.71(4) ? . 4_555 H(20) C(16) 3.22(4) ? . 4_555 H(20) H(12) 3.32(5) ? . 4_555 H(20) H(13) 2.60(6) ? . 4_555 H(20) H(14) 3.49(6) ? . 4_555 H(21) O(3) 3.47(3) ? . 3_766 H(21) O(8) 3.55(3) ? . 3_766 H(21) C(1) 3.30(3) ? . 3_766 H(21) C(2) 3.06(3) ? . 3_766 H(21) C(3) 3.32(3) ? . 3_766 H(21) H(7) 3.40(5) ? . 3_766 H(22) C(7) 3.43(4) ? . 3_666 H(22) C(21) 3.24(4) ? . 3_666 H(22) H(4) 2.99(5) ? . 3_666 H(22) H(8) 3.54(5) ? . 3_666 H(22) H(22) 2.55(5) ? . 3_666 H(22) H(24) 3.02(6) ? . 3_666 H(22) H(30) 3.358 ? . 3_666 H(23) O(10) 3.11(3) ? . 1_455 H(23) O(13) 2.83(4) ? . 2_645 H(23) H(3) 3.28(5) ? . 3_666 H(23) H(4) 3.19(5) ? . 3_666 H(23) H(13) 3.59(5) ? . 4_555 H(24) O(10) 2.79(3) ? . 1_455 H(24) H(22) 3.02(6) ? . 3_666 H(25) O(10) 3.597 ? . 1_455 H(25) C(19) 3.463 ? . 3_665 H(25) H(17) 2.821 ? . 3_665 H(25) H(18) 3.318 ? . 3_665 H(26) O(7) 2.718 ? . 1_455 H(26) N(3) 3.115 ? . 1_455 H(26) C(19) 3.293 ? . 3_665 H(26) H(12) 2.832 ? . 3_665 H(26) H(17) 2.876 ? . 3_665 H(26) H(18) 2.818 ? . 3_665 H(27) O(5) 3.100 ? . 1_455 H(27) O(6) 3.010 ? . 1_455 H(27) O(7) 3.003 ? . 1_455 H(27) O(8) 3.101 ? . 1_455 H(27) O(9) 2.762 ? . 1_455 H(27) O(10) 2.868 ? . 1_455 H(27) N(3) 2.777 ? . 1_455 H(27) N(4) 2.629 ? . 1_455 H(27) H(17) 3.358 ? . 3_665 H(27) H(18) 3.150 ? . 3_665 H(28) O(5) 2.806 ? . 1_455 H(28) O(8) 2.795 ? . 1_455 H(28) O(10) 3.509 ? . 1_455 H(28) N(3) 3.401 ? . 1_455 H(28) N(4) 3.265 ? . 1_455 H(28) C(20) 3.507 ? . 3_666 H(28) H(14) 3.107 ? . 2_655 H(28) H(15) 3.201 ? . 2_655 H(28) H(19) 2.575 ? . 3_666 H(29) O(5) 3.446 ? . 1_455 H(29) O(7) 3.526 ? . 1_455 H(29) C(16) 3.341 ? . 2_655 H(29) C(18) 3.321 ? . 2_655 H(29) H(14) 2.549 ? . 2_655 H(29) H(15) 2.412 ? . 2_655 H(30) C(16) 3.347 ? . 2_655 H(30) H(14) 2.580 ? . 2_655 H(30) H(15) 3.554 ? . 2_655 H(30) H(19) 2.837 ? . 3_666 H(30) H(22) 3.358 ? . 3_666 Tb(1) V(1) 3.4918(18) ? . . data___DyVO _database_code_depnum_ccdc_archive 'CCDC 881976' #TrackingRef '11260_web_deposit_cif_file_5_TakayukiIshida_1336987557.DyV_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Dy N5 O15 V ' _chemical_formula_moiety 'C24 H30 Dy N5 O15 V ' _chemical_formula_weight 841.97 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.909(3) _cell_length_b 17.535(3) _cell_length_c 18.241(9) _cell_angle_alpha 90.0000 _cell_angle_beta 105.490(4) _cell_angle_gamma 90.0000 _cell_volume 3054.4(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 447 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 90. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672.00 _exptl_absorpt_coefficient_mu 2.816 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.192 _exptl_absorpt_correction_T_max 0.655 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 47413 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_ambient_temperature 90. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6939 _reflns_number_gt 6727 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0453 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6939 _refine_ls_number_parameters 517 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.69 _refine_diff_density_min -1.46 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Dy Dy -0.189 4.410 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; V V 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Dy(1) Dy 0.926770(10) 0.573340(10) 0.203540(10) 0.00958(4) Uani 1.00 1 d . . . V(1) V 0.83822(4) 0.46957(2) 0.34707(2) 0.00986(10) Uani 1.00 1 d . . . O(1) O 0.8764(2) 0.57709(9) 0.32472(12) 0.0119(4) Uani 1.00 1 d . . . O(2) O 0.81308(19) 0.46338(10) 0.23529(10) 0.0121(4) Uani 1.00 1 d . . . O(3) O 0.9283(2) 0.70489(11) 0.26549(10) 0.0152(4) Uani 1.00 1 d . . . O(4) O 0.78639(19) 0.49404(11) 0.09369(10) 0.0138(4) Uani 1.00 1 d . . . O(5) O 1.1170(2) 0.65726(14) 0.18503(13) 0.0267(5) Uani 1.00 1 d . . . O(6) O 1.0390(2) 0.57449(12) 0.09779(17) 0.0278(7) Uani 1.00 1 d . . . O(7) O 1.2025(2) 0.65317(13) 0.08702(15) 0.0312(6) Uani 1.00 1 d . . . O(8) O 1.1402(2) 0.54690(14) 0.30228(12) 0.0236(5) Uani 1.00 1 d . . . O(9) O 1.0855(2) 0.46169(13) 0.21517(13) 0.0252(5) Uani 1.00 1 d . . . O(10) O 1.2645(2) 0.44296(16) 0.31298(16) 0.0339(6) Uani 1.00 1 d . . . O(11) O 0.7980(2) 0.66442(12) 0.10801(11) 0.0172(4) Uani 1.00 1 d . . . O(12) O 0.68479(19) 0.61579(11) 0.18289(11) 0.0163(4) Uani 1.00 1 d . . . O(13) O 0.5904(2) 0.70823(13) 0.10649(12) 0.0263(5) Uani 1.00 1 d . . . O(14) O 0.6051(2) 0.51272(12) 0.30048(11) 0.0163(4) Uani 1.00 1 d . . . O(15) O 0.9879(2) 0.43164(10) 0.38123(12) 0.0156(5) Uani 1.00 1 d . . . N(1) N 0.8050(2) 0.50174(13) 0.45016(12) 0.0123(5) Uani 1.00 1 d . . . N(2) N 0.7287(2) 0.36906(12) 0.34514(12) 0.0125(5) Uani 1.00 1 d . . . N(3) N 1.1215(2) 0.62982(13) 0.12157(14) 0.0192(5) Uani 1.00 1 d . . . N(4) N 1.1666(2) 0.48251(15) 0.27794(14) 0.0204(6) Uani 1.00 1 d . . . N(5) N 0.6873(2) 0.66416(13) 0.13160(12) 0.0151(5) Uani 1.00 1 d . . . C(1) C 0.8597(2) 0.64010(15) 0.36224(14) 0.0111(5) Uani 1.00 1 d . . . C(2) C 0.8875(2) 0.71088(15) 0.33265(15) 0.0127(5) Uani 1.00 1 d . . . C(3) C 0.8756(3) 0.77878(15) 0.36883(16) 0.0172(6) Uani 1.00 1 d . . . C(4) C 0.8364(3) 0.77771(16) 0.43682(18) 0.0227(7) Uani 1.00 1 d . . . C(5) C 0.8089(2) 0.70966(17) 0.46736(16) 0.0175(6) Uani 1.00 1 d . . . C(6) C 0.8196(2) 0.63998(16) 0.43117(15) 0.0136(5) Uani 1.00 1 d . . . C(7) C 0.7972(2) 0.57126(14) 0.47125(16) 0.0131(6) Uani 1.00 1 d . . . C(8) C 0.9535(3) 0.77744(16) 0.23263(18) 0.0215(7) Uani 1.00 1 d . . . C(9) C 0.8039(2) 0.44266(18) 0.50750(16) 0.0151(6) Uani 1.00 1 d . . . C(10) C 0.7034(2) 0.37581(16) 0.47969(15) 0.0156(6) Uani 1.00 1 d . . . C(11) C 0.7426(3) 0.32850(16) 0.41723(16) 0.0171(6) Uani 1.00 1 d . . . C(12) C 0.7197(3) 0.42069(14) 0.18606(16) 0.0124(6) Uani 1.00 1 d . . . C(13) C 0.7004(3) 0.43655(15) 0.10781(16) 0.0134(6) Uani 1.00 1 d . . . C(14) C 0.6021(2) 0.39799(17) 0.05260(15) 0.0165(6) Uani 1.00 1 d . . . C(15) C 0.5184(2) 0.34219(16) 0.07374(16) 0.0185(6) Uani 1.00 1 d . . . C(16) C 0.5377(2) 0.32465(16) 0.14892(16) 0.0180(6) Uani 1.00 1 d . . . C(17) C 0.6398(2) 0.36273(15) 0.20661(15) 0.0140(6) Uani 1.00 1 d . . . C(18) C 0.6560(2) 0.33723(15) 0.28420(16) 0.0158(6) Uani 1.00 1 d . . . C(19) C 0.7708(3) 0.50947(19) 0.01398(16) 0.0212(7) Uani 1.00 1 d . . . C(20) C 0.7230(3) 0.32196(19) 0.54822(18) 0.0242(7) Uani 1.00 1 d . . . C(21) C 0.5510(3) 0.40278(19) 0.45294(18) 0.0205(7) Uani 1.00 1 d . . . C(22) C 0.5057(2) 0.54833(16) 0.26366(15) 0.0140(6) Uani 1.00 1 d . . . C(23) C 0.4176(2) 0.5213(2) 0.18861(18) 0.0250(7) Uani 1.00 1 d . . . C(24) C 0.4659(3) 0.62423(19) 0.29064(19) 0.0279(8) Uani 1.00 1 d . . . H(1) H 0.893(2) 0.8236(16) 0.3496(16) 0.008(6) Uiso 1.00 1 d . . . H(2) H 0.834(3) 0.8266(17) 0.4636(17) 0.008(7) Uiso 1.00 1 d . . . H(3) H 0.788(3) 0.7052(19) 0.513(2) 0.020(8) Uiso 1.00 1 d . . . H(4) H 0.780(3) 0.5776(16) 0.517(2) 0.016(8) Uiso 1.00 1 d . . . H(5) H 0.868(3) 0.810(2) 0.229(2) 0.021(8) Uiso 1.00 1 d . . . H(6) H 0.983(4) 0.770(2) 0.187(2) 0.045(12) Uiso 1.00 1 d . . . H(7) H 1.041(3) 0.794(2) 0.277(2) 0.026(9) Uiso 1.00 1 d . . . H(8) H 0.787(3) 0.4638(19) 0.552(2) 0.019(8) Uiso 1.00 1 d . . . H(9) H 0.897(4) 0.4235(17) 0.521(2) 0.017(9) Uiso 1.00 1 d . . . H(10) H 0.685(3) 0.2830(17) 0.4082(17) 0.008(7) Uiso 1.00 1 d . . . H(11) H 0.832(3) 0.3105(16) 0.4308(16) 0.008(6) Uiso 1.00 1 d . . . H(12) H 0.581(3) 0.4130(19) -0.003(2) 0.021(8) Uiso 1.00 1 d . . . H(13) H 0.449(4) 0.310(2) 0.034(2) 0.035(10) Uiso 1.00 1 d . . . H(14) H 0.488(3) 0.286(2) 0.164(2) 0.023(9) Uiso 1.00 1 d . . . H(15) H 0.602(3) 0.288(2) 0.2906(18) 0.019(8) Uiso 1.00 1 d . . . H(16) H 0.822(3) 0.544(2) 0.0120(17) 0.009(7) Uiso 1.00 1 d . . . H(17) H 0.678(5) 0.526(2) -0.012(2) 0.050(14) Uiso 1.00 1 d . . . H(18) H 0.786(4) 0.462(2) -0.011(2) 0.034(10) Uiso 1.00 1 d . . . H(19) H 0.704(4) 0.346(2) 0.592(2) 0.034(10) Uiso 1.00 1 d . . . H(20) H 0.660(3) 0.275(2) 0.533(2) 0.023(8) Uiso 1.00 1 d . . . H(21) H 0.821(5) 0.303(2) 0.561(2) 0.048(14) Uiso 1.00 1 d . . . H(22) H 0.525(4) 0.4309(19) 0.496(2) 0.035(12) Uiso 1.00 1 d . . . H(23) H 0.492(3) 0.360(2) 0.436(2) 0.024(8) Uiso 1.00 1 d . . . H(24) H 0.533(3) 0.4341(18) 0.408(2) 0.020(9) Uiso 1.00 1 d . . . H(25) H 0.4544 0.5405 0.1492 0.029 Uiso 1.00 1 c R . . H(26) H 0.3244 0.5391 0.1813 0.029 Uiso 1.00 1 c R . . H(27) H 0.4179 0.4671 0.1875 0.029 Uiso 1.00 1 c R . . H(28) H 0.4026 0.6164 0.3210 0.033 Uiso 1.00 1 c R . . H(29) H 0.4224 0.6549 0.2480 0.033 Uiso 1.00 1 c R . . H(30) H 0.5476 0.6492 0.3200 0.033 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Dy(1) 0.01093(9) 0.00948(10) 0.00841(9) 0.00021(3) 0.00273(6) 0.00061(3) V(1) 0.0108(2) 0.0098(2) 0.0080(2) -0.00073(15) 0.00061(16) 0.00039(15) O(1) 0.0156(9) 0.0104(9) 0.0100(9) -0.0008(6) 0.0039(7) -0.0012(6) O(2) 0.0132(8) 0.0120(9) 0.0097(8) -0.0014(6) 0.0008(6) -0.0007(6) O(3) 0.0215(9) 0.0131(9) 0.0125(8) -0.0023(7) 0.0073(7) 0.0015(7) O(4) 0.0158(8) 0.0159(9) 0.0089(8) -0.0012(7) 0.0021(6) 0.0006(7) O(5) 0.0227(10) 0.0365(13) 0.0244(11) -0.0085(9) 0.0120(9) -0.0060(9) O(6) 0.0304(14) 0.0258(13) 0.0353(15) -0.0105(8) 0.0232(12) -0.0082(8) O(7) 0.0385(13) 0.0199(11) 0.0483(14) -0.0033(9) 0.0343(11) 0.0044(10) O(8) 0.0203(10) 0.0308(12) 0.0163(10) 0.0050(9) -0.0011(8) -0.0000(9) O(9) 0.0189(10) 0.0204(11) 0.0318(12) 0.0055(8) -0.0010(8) -0.0062(9) O(10) 0.0165(10) 0.0407(13) 0.0409(14) 0.0103(10) 0.0016(10) 0.0184(12) O(11) 0.0225(9) 0.0182(10) 0.0128(9) 0.0031(7) 0.0078(7) 0.0025(7) O(12) 0.0155(8) 0.0206(10) 0.0134(8) 0.0012(7) 0.0045(7) 0.0053(7) O(13) 0.0266(11) 0.0279(11) 0.0214(10) 0.0154(9) 0.0014(8) 0.0053(8) O(14) 0.0148(8) 0.0167(10) 0.0169(9) 0.0020(7) 0.0031(7) 0.0050(7) O(15) 0.0140(9) 0.0177(10) 0.0141(9) 0.0006(6) 0.0021(8) 0.0032(6) N(1) 0.0103(9) 0.0165(11) 0.0095(9) -0.0016(8) 0.0019(8) 0.0026(8) N(2) 0.0136(9) 0.0105(10) 0.0132(10) -0.0012(7) 0.0035(8) 0.0002(8) N(3) 0.0228(11) 0.0132(11) 0.0252(12) 0.0057(9) 0.0128(10) 0.0050(9) N(4) 0.0134(10) 0.0249(13) 0.0250(12) -0.0006(9) 0.0088(9) 0.0080(10) N(5) 0.0192(10) 0.0157(11) 0.0093(9) 0.0015(8) 0.0020(8) 0.0003(8) C(1) 0.0100(10) 0.0122(12) 0.0100(11) 0.0006(8) 0.0007(8) -0.0014(9) C(2) 0.0122(11) 0.0146(12) 0.0104(11) 0.0025(9) 0.0014(9) 0.0012(9) C(3) 0.0221(13) 0.0095(12) 0.0205(13) -0.0001(10) 0.0066(11) 0.0003(10) C(4) 0.0306(15) 0.0138(14) 0.0252(15) -0.0002(11) 0.0101(12) -0.0066(11) C(5) 0.0191(12) 0.0196(14) 0.0145(12) 0.0031(10) 0.0058(10) -0.0032(10) C(6) 0.0102(11) 0.0183(13) 0.0107(11) 0.0019(9) 0.0000(9) 0.0008(9) C(7) 0.0098(12) 0.0203(15) 0.0083(12) -0.0001(8) 0.0009(10) -0.0001(8) C(8) 0.0355(16) 0.0096(13) 0.0240(15) -0.0038(11) 0.0159(13) 0.0045(11) C(9) 0.0158(13) 0.0187(12) 0.0092(12) -0.0033(10) 0.0008(10) 0.0040(10) C(10) 0.0169(12) 0.0158(13) 0.0139(12) -0.0042(9) 0.0037(9) 0.0026(10) C(11) 0.0203(13) 0.0158(13) 0.0151(12) 0.0000(10) 0.0044(10) 0.0045(10) C(12) 0.0125(12) 0.0124(13) 0.0112(12) 0.0030(8) 0.0014(10) -0.0013(8) C(13) 0.0156(12) 0.0132(12) 0.0117(12) 0.0023(9) 0.0038(10) -0.0014(9) C(14) 0.0180(12) 0.0180(14) 0.0117(12) 0.0033(10) 0.0005(10) -0.0021(10) C(15) 0.0165(12) 0.0173(13) 0.0187(13) -0.0028(10) -0.0007(10) -0.0090(10) C(16) 0.0196(13) 0.0150(13) 0.0193(13) -0.0041(10) 0.0052(10) -0.0047(10) C(17) 0.0143(11) 0.0101(12) 0.0165(12) 0.0016(9) 0.0021(9) -0.0023(9) C(18) 0.0175(12) 0.0118(12) 0.0190(13) -0.0011(9) 0.0065(10) 0.0028(10) C(19) 0.0342(16) 0.0202(15) 0.0096(12) -0.0056(13) 0.0064(11) 0.0006(10) C(20) 0.0319(16) 0.0238(15) 0.0182(14) -0.0038(12) 0.0090(12) 0.0056(12) C(21) 0.0170(13) 0.0210(14) 0.0238(14) -0.0067(11) 0.0057(11) -0.0017(12) C(22) 0.0120(11) 0.0181(13) 0.0124(11) -0.0002(10) 0.0039(9) 0.0033(10) C(23) 0.0170(13) 0.0364(19) 0.0188(13) 0.0035(11) 0.0003(11) -0.0055(13) C(24) 0.0230(14) 0.0286(17) 0.0306(16) 0.0067(12) 0.0043(12) -0.0056(13) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Dy(1) O(1) 2.393(2) yes . . Dy(1) O(2) 2.3813(18) yes . . Dy(1) O(3) 2.5669(19) yes . . Dy(1) O(4) 2.5288(17) yes . . Dy(1) O(5) 2.484(2) yes . . Dy(1) O(6) 2.471(3) yes . . Dy(1) O(8) 2.4281(19) yes . . Dy(1) O(9) 2.485(2) yes . . Dy(1) O(11) 2.4550(19) yes . . Dy(1) O(12) 2.4420(18) yes . . V(1) O(1) 1.9866(17) yes . . V(1) O(2) 1.9900(18) yes . . V(1) O(14) 2.3627(19) yes . . V(1) O(15) 1.593(2) yes . . V(1) N(1) 2.072(2) yes . . V(1) N(2) 2.065(2) yes . . O(1) C(1) 1.333(3) yes . . O(2) C(12) 1.334(2) yes . . O(3) C(2) 1.393(3) yes . . O(3) C(8) 1.456(3) yes . . O(4) C(13) 1.388(3) yes . . O(4) C(19) 1.446(3) yes . . O(5) N(3) 1.265(3) yes . . O(6) N(3) 1.268(3) yes . . O(7) N(3) 1.216(3) yes . . O(8) N(4) 1.266(3) yes . . O(9) N(4) 1.264(3) yes . . O(10) N(4) 1.225(3) yes . . O(11) N(5) 1.282(3) yes . . O(12) N(5) 1.268(3) yes . . O(13) N(5) 1.222(3) yes . . O(14) C(22) 1.208(3) yes . . N(1) C(7) 1.287(3) yes . . N(1) C(9) 1.474(3) yes . . N(2) C(11) 1.469(3) yes . . N(2) C(18) 1.280(3) yes . . C(1) C(2) 1.410(3) yes . . C(1) C(6) 1.417(4) yes . . C(2) C(3) 1.382(3) yes . . C(3) C(4) 1.395(4) yes . . C(4) C(5) 1.375(4) yes . . C(5) C(6) 1.406(4) yes . . C(6) C(7) 1.457(3) yes . . C(9) C(10) 1.534(3) yes . . C(10) C(11) 1.541(4) yes . . C(10) C(20) 1.537(4) yes . . C(10) C(21) 1.533(3) yes . . C(12) C(13) 1.416(4) yes . . C(12) C(17) 1.399(4) yes . . C(13) C(14) 1.377(3) yes . . C(14) C(15) 1.402(4) yes . . C(15) C(16) 1.368(4) yes . . C(16) C(17) 1.417(3) yes . . C(17) C(18) 1.452(3) yes . . C(22) C(23) 1.491(3) yes . . C(22) C(24) 1.507(4) yes . . C(3) H(1) 0.90(3) no . . C(4) H(2) 0.99(3) no . . C(5) H(3) 0.92(4) no . . C(7) H(4) 0.90(4) no . . C(8) H(5) 1.01(3) no . . C(8) H(6) 0.96(5) no . . C(8) H(7) 1.05(3) no . . C(9) H(8) 0.96(3) no . . C(9) H(9) 0.95(4) no . . C(11) H(10) 0.97(3) no . . C(11) H(11) 0.91(2) no . . C(14) H(12) 1.01(3) no . . C(15) H(13) 1.03(3) no . . C(16) H(14) 0.92(3) no . . C(18) H(15) 1.03(3) no . . C(19) H(16) 0.80(3) no . . C(19) H(17) 0.96(4) no . . C(19) H(18) 0.97(4) no . . C(20) H(19) 0.96(4) no . . C(20) H(20) 1.02(3) no . . C(20) H(21) 0.99(5) no . . C(21) H(22) 1.02(4) no . . C(21) H(23) 0.95(3) no . . C(21) H(24) 0.96(3) no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Dy(1) O(2) 64.46(5) yes . . . O(1) Dy(1) O(3) 63.06(5) yes . . . O(1) Dy(1) O(4) 122.73(6) yes . . . O(1) Dy(1) O(5) 117.52(6) yes . . . O(1) Dy(1) O(6) 165.73(7) yes . . . O(1) Dy(1) O(8) 71.04(7) yes . . . O(1) Dy(1) O(9) 103.07(7) yes . . . O(1) Dy(1) O(11) 116.15(6) yes . . . O(1) Dy(1) O(12) 72.29(6) yes . . . O(2) Dy(1) O(3) 124.61(6) yes . . . O(2) Dy(1) O(4) 63.36(6) yes . . . O(2) Dy(1) O(5) 159.72(6) yes . . . O(2) Dy(1) O(6) 122.50(6) yes . . . O(2) Dy(1) O(8) 92.28(6) yes . . . O(2) Dy(1) O(9) 70.81(7) yes . . . O(2) Dy(1) O(11) 120.63(6) yes . . . O(2) Dy(1) O(12) 77.02(6) yes . . . O(3) Dy(1) O(4) 141.29(5) yes . . . O(3) Dy(1) O(5) 67.18(7) yes . . . O(3) Dy(1) O(6) 112.67(6) yes . . . O(3) Dy(1) O(8) 86.76(6) yes . . . O(3) Dy(1) O(9) 137.84(6) yes . . . O(3) Dy(1) O(11) 70.66(6) yes . . . O(3) Dy(1) O(12) 71.58(6) yes . . . O(4) Dy(1) O(5) 119.65(7) yes . . . O(4) Dy(1) O(6) 69.69(7) yes . . . O(4) Dy(1) O(8) 131.96(7) yes . . . O(4) Dy(1) O(9) 80.57(6) yes . . . O(4) Dy(1) O(11) 73.96(6) yes . . . O(4) Dy(1) O(12) 74.67(6) yes . . . O(5) Dy(1) O(6) 51.17(7) yes . . . O(5) Dy(1) O(8) 70.85(7) yes . . . O(5) Dy(1) O(9) 89.55(7) yes . . . O(5) Dy(1) O(11) 77.73(7) yes . . . O(5) Dy(1) O(12) 123.22(7) yes . . . O(6) Dy(1) O(8) 95.53(8) yes . . . O(6) Dy(1) O(9) 70.51(7) yes . . . O(6) Dy(1) O(11) 72.39(7) yes . . . O(6) Dy(1) O(12) 120.35(7) yes . . . O(8) Dy(1) O(9) 51.70(7) yes . . . O(8) Dy(1) O(11) 146.64(7) yes . . . O(8) Dy(1) O(12) 142.87(7) yes . . . O(9) Dy(1) O(11) 140.37(7) yes . . . O(9) Dy(1) O(12) 145.75(6) yes . . . O(11) Dy(1) O(12) 52.38(7) yes . . . O(1) V(1) O(2) 79.63(8) yes . . . O(1) V(1) O(14) 81.02(7) yes . . . O(1) V(1) O(15) 105.54(9) yes . . . O(1) V(1) N(1) 90.75(9) yes . . . O(1) V(1) N(2) 159.16(7) yes . . . O(2) V(1) O(14) 78.82(7) yes . . . O(2) V(1) O(15) 103.11(10) yes . . . O(2) V(1) N(1) 159.72(7) yes . . . O(2) V(1) N(2) 90.83(8) yes . . . O(14) V(1) O(15) 173.36(9) yes . . . O(14) V(1) N(1) 82.09(7) yes . . . O(14) V(1) N(2) 78.95(7) yes . . . O(15) V(1) N(1) 96.63(9) yes . . . O(15) V(1) N(2) 94.61(8) yes . . . N(1) V(1) N(2) 92.16(9) yes . . . Dy(1) O(1) V(1) 105.17(8) yes . . . Dy(1) O(1) C(1) 125.60(16) yes . . . V(1) O(1) C(1) 128.65(19) yes . . . Dy(1) O(2) V(1) 105.49(7) yes . . . Dy(1) O(2) C(12) 125.37(16) yes . . . V(1) O(2) C(12) 126.50(18) yes . . . Dy(1) O(3) C(2) 119.08(15) yes . . . Dy(1) O(3) C(8) 125.83(17) yes . . . C(2) O(3) C(8) 114.7(2) yes . . . Dy(1) O(4) C(13) 119.17(15) yes . . . Dy(1) O(4) C(19) 125.62(17) yes . . . C(13) O(4) C(19) 114.6(2) yes . . . Dy(1) O(5) N(3) 96.47(16) yes . . . Dy(1) O(6) N(3) 97.1(2) yes . . . Dy(1) O(8) N(4) 97.53(14) yes . . . Dy(1) O(9) N(4) 94.85(17) yes . . . Dy(1) O(11) N(5) 95.08(14) yes . . . Dy(1) O(12) N(5) 96.08(15) yes . . . V(1) O(14) C(22) 160.0(2) yes . . . V(1) N(1) C(7) 124.5(2) yes . . . V(1) N(1) C(9) 119.05(18) yes . . . C(7) N(1) C(9) 116.2(2) yes . . . V(1) N(2) C(11) 118.35(15) yes . . . V(1) N(2) C(18) 123.95(19) yes . . . C(11) N(2) C(18) 117.6(2) yes . . . O(5) N(3) O(6) 115.2(2) yes . . . O(5) N(3) O(7) 122.4(2) yes . . . O(6) N(3) O(7) 122.3(2) yes . . . O(8) N(4) O(9) 115.7(2) yes . . . O(8) N(4) O(10) 122.1(2) yes . . . O(9) N(4) O(10) 122.2(2) yes . . . O(11) N(5) O(12) 115.9(2) yes . . . O(11) N(5) O(13) 122.0(2) yes . . . O(12) N(5) O(13) 122.1(2) yes . . . O(1) C(1) C(2) 118.0(2) yes . . . O(1) C(1) C(6) 123.9(2) yes . . . C(2) C(1) C(6) 118.1(2) yes . . . O(3) C(2) C(1) 113.7(2) yes . . . O(3) C(2) C(3) 124.6(2) yes . . . C(1) C(2) C(3) 121.7(2) yes . . . C(2) C(3) C(4) 119.5(2) yes . . . C(3) C(4) C(5) 120.3(2) yes . . . C(4) C(5) C(6) 121.1(2) yes . . . C(1) C(6) C(5) 119.3(2) yes . . . C(1) C(6) C(7) 124.3(2) yes . . . C(5) C(6) C(7) 116.3(2) yes . . . N(1) C(7) C(6) 127.2(2) yes . . . N(1) C(9) C(10) 115.4(2) yes . . . C(9) C(10) C(11) 112.7(2) yes . . . C(9) C(10) C(20) 105.7(2) yes . . . C(9) C(10) C(21) 111.5(2) yes . . . C(11) C(10) C(20) 105.6(2) yes . . . C(11) C(10) C(21) 110.6(2) yes . . . C(20) C(10) C(21) 110.4(2) yes . . . N(2) C(11) C(10) 114.8(2) yes . . . O(2) C(12) C(13) 116.8(2) yes . . . O(2) C(12) C(17) 124.6(2) yes . . . C(13) C(12) C(17) 118.6(2) yes . . . O(4) C(13) C(12) 113.9(2) yes . . . O(4) C(13) C(14) 124.8(2) yes . . . C(12) C(13) C(14) 121.3(2) yes . . . C(13) C(14) C(15) 119.8(2) yes . . . C(14) C(15) C(16) 119.9(2) yes . . . C(15) C(16) C(17) 121.3(2) yes . . . C(12) C(17) C(16) 119.1(2) yes . . . C(12) C(17) C(18) 124.2(2) yes . . . C(16) C(17) C(18) 116.7(2) yes . . . N(2) C(18) C(17) 127.0(2) yes . . . O(14) C(22) C(23) 122.5(2) yes . . . O(14) C(22) C(24) 121.4(2) yes . . . C(23) C(22) C(24) 116.1(2) yes . . . C(2) C(3) H(1) 121(2) no . . . C(4) C(3) H(1) 119(2) no . . . C(3) C(4) H(2) 118.4(19) no . . . C(5) C(4) H(2) 121.2(19) no . . . C(4) C(5) H(3) 124(2) no . . . C(6) C(5) H(3) 115(2) no . . . N(1) C(7) H(4) 115.8(18) no . . . C(6) C(7) H(4) 117.0(18) no . . . O(3) C(8) H(5) 106(2) no . . . O(3) C(8) H(6) 111(2) no . . . O(3) C(8) H(7) 97(2) no . . . H(5) C(8) H(6) 118(3) no . . . H(5) C(8) H(7) 114(2) no . . . H(6) C(8) H(7) 109(3) no . . . N(1) C(9) H(8) 112(2) no . . . N(1) C(9) H(9) 104(2) no . . . C(10) C(9) H(8) 109(2) no . . . C(10) C(9) H(9) 108.4(19) no . . . H(8) C(9) H(9) 107(3) no . . . N(2) C(11) H(10) 109.7(18) no . . . N(2) C(11) H(11) 105.2(19) no . . . C(10) C(11) H(10) 108(2) no . . . C(10) C(11) H(11) 113.9(18) no . . . H(10) C(11) H(11) 104(2) no . . . C(13) C(14) H(12) 121.3(19) no . . . C(15) C(14) H(12) 118.6(19) no . . . C(14) C(15) H(13) 122(2) no . . . C(16) C(15) H(13) 118(2) no . . . C(15) C(16) H(14) 121(2) no . . . C(17) C(16) H(14) 117(2) no . . . N(2) C(18) H(15) 116.9(17) no . . . C(17) C(18) H(15) 116.1(17) no . . . O(4) C(19) H(16) 107(2) no . . . O(4) C(19) H(17) 113(3) no . . . O(4) C(19) H(18) 108(2) no . . . H(16) C(19) H(17) 107(3) no . . . H(16) C(19) H(18) 116(3) no . . . H(17) C(19) H(18) 106(3) no . . . C(10) C(20) H(19) 113(2) no . . . C(10) C(20) H(20) 109.8(19) no . . . C(10) C(20) H(21) 107(3) no . . . H(19) C(20) H(20) 109(3) no . . . H(19) C(20) H(21) 110(3) no . . . H(20) C(20) H(21) 107(3) no . . . C(10) C(21) H(22) 110(2) no . . . C(10) C(21) H(23) 109(2) no . . . C(10) C(21) H(24) 113(2) no . . . H(22) C(21) H(23) 112(3) no . . . H(22) C(21) H(24) 111(3) no . . . H(23) C(21) H(24) 103(2) no . . . C(22) C(23) H(25) 109.5 no . . . C(22) C(23) H(26) 109.5 no . . . C(22) C(23) H(27) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . H(25) C(23) H(27) 109.5 no . . . H(26) C(23) H(27) 109.5 no . . . C(22) C(24) H(28) 109.5 no . . . C(22) C(24) H(29) 109.5 no . . . C(22) C(24) H(30) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . H(28) C(24) H(30) 109.5 no . . . H(29) C(24) H(30) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Dy(1) O(2) V(1) -16.72(6) ? . . . . O(1) Dy(1) O(2) C(12) 145.8(2) ? . . . . O(2) Dy(1) O(1) V(1) 16.72(6) ? . . . . O(2) Dy(1) O(1) C(1) -155.10(19) ? . . . . O(1) Dy(1) O(3) C(2) -5.66(14) ? . . . . O(1) Dy(1) O(3) C(8) -178.3(2) ? . . . . O(3) Dy(1) O(1) V(1) 178.38(10) ? . . . . O(3) Dy(1) O(1) C(1) 6.56(16) ? . . . . O(1) Dy(1) O(4) C(13) -16.34(19) ? . . . . O(1) Dy(1) O(4) C(19) 154.2(2) ? . . . . O(4) Dy(1) O(1) V(1) 42.84(10) ? . . . . O(4) Dy(1) O(1) C(1) -128.99(17) ? . . . . O(1) Dy(1) O(5) N(3) 170.99(13) ? . . . . O(5) Dy(1) O(1) V(1) -140.69(8) ? . . . . O(5) Dy(1) O(1) C(1) 47.5(2) ? . . . . O(1) Dy(1) O(6) N(3) -42.1(3) ? . . . . O(6) Dy(1) O(1) V(1) -105.8(2) ? . . . . O(6) Dy(1) O(1) C(1) 82.4(3) ? . . . . O(1) Dy(1) O(8) N(4) 122.57(18) ? . . . . O(8) Dy(1) O(1) V(1) -85.45(9) ? . . . . O(8) Dy(1) O(1) C(1) 102.73(19) ? . . . . O(1) Dy(1) O(9) N(4) -49.93(18) ? . . . . O(9) Dy(1) O(1) V(1) -44.26(9) ? . . . . O(9) Dy(1) O(1) C(1) 143.92(18) ? . . . . O(1) Dy(1) O(11) N(5) -32.08(15) ? . . . . O(11) Dy(1) O(1) V(1) 129.95(7) ? . . . . O(11) Dy(1) O(1) C(1) -41.87(19) ? . . . . O(1) Dy(1) O(12) N(5) 141.88(14) ? . . . . O(12) Dy(1) O(1) V(1) 100.49(8) ? . . . . O(12) Dy(1) O(1) C(1) -71.34(18) ? . . . . O(2) Dy(1) O(3) C(2) 14.52(17) ? . . . . O(2) Dy(1) O(3) C(8) -158.16(18) ? . . . . O(3) Dy(1) O(2) V(1) -36.65(10) ? . . . . O(3) Dy(1) O(2) C(12) 125.9(2) ? . . . . O(2) Dy(1) O(4) C(13) 10.04(16) ? . . . . O(2) Dy(1) O(4) C(19) -179.4(2) ? . . . . O(4) Dy(1) O(2) V(1) -172.25(10) ? . . . . O(4) Dy(1) O(2) C(12) -9.74(19) ? . . . . O(2) Dy(1) O(5) N(3) 80.6(2) ? . . . . O(5) Dy(1) O(2) V(1) 83.9(2) ? . . . . O(5) Dy(1) O(2) C(12) -113.6(2) ? . . . . O(2) Dy(1) O(6) N(3) -157.61(13) ? . . . . O(6) Dy(1) O(2) V(1) 149.01(8) ? . . . . O(6) Dy(1) O(2) C(12) -48.5(2) ? . . . . O(2) Dy(1) O(8) N(4) 60.60(18) ? . . . . O(8) Dy(1) O(2) V(1) 50.98(9) ? . . . . O(8) Dy(1) O(2) C(12) -146.5(2) ? . . . . O(2) Dy(1) O(9) N(4) -106.59(18) ? . . . . O(9) Dy(1) O(2) V(1) 98.86(8) ? . . . . O(9) Dy(1) O(2) C(12) -98.6(2) ? . . . . O(2) Dy(1) O(11) N(5) 42.40(16) ? . . . . O(11) Dy(1) O(2) V(1) -123.27(8) ? . . . . O(11) Dy(1) O(2) C(12) 39.2(2) ? . . . . O(2) Dy(1) O(12) N(5) -151.13(14) ? . . . . O(12) Dy(1) O(2) V(1) -93.08(8) ? . . . . O(12) Dy(1) O(2) C(12) 69.4(2) ? . . . . O(3) Dy(1) O(4) C(13) -102.94(18) ? . . . . O(3) Dy(1) O(4) C(19) 67.6(2) ? . . . . O(4) Dy(1) O(3) C(2) 103.96(16) ? . . . . O(4) Dy(1) O(3) C(8) -68.7(2) ? . . . . O(3) Dy(1) O(5) N(3) -149.69(16) ? . . . . O(5) Dy(1) O(3) C(2) -146.58(16) ? . . . . O(5) Dy(1) O(3) C(8) 40.74(19) ? . . . . O(3) Dy(1) O(6) N(3) 27.44(17) ? . . . . O(6) Dy(1) O(3) C(2) -170.65(15) ? . . . . O(6) Dy(1) O(3) C(8) 16.7(2) ? . . . . O(3) Dy(1) O(8) N(4) -174.85(18) ? . . . . O(8) Dy(1) O(3) C(2) -76.01(16) ? . . . . O(8) Dy(1) O(3) C(8) 111.3(2) ? . . . . O(3) Dy(1) O(9) N(4) 14.2(2) ? . . . . O(9) Dy(1) O(3) C(2) -85.09(18) ? . . . . O(9) Dy(1) O(3) C(8) 102.2(2) ? . . . . O(3) Dy(1) O(11) N(5) -77.06(14) ? . . . . O(11) Dy(1) O(3) C(2) 128.97(16) ? . . . . O(11) Dy(1) O(3) C(8) -43.72(19) ? . . . . O(3) Dy(1) O(12) N(5) 75.15(13) ? . . . . O(12) Dy(1) O(3) C(2) 73.37(15) ? . . . . O(12) Dy(1) O(3) C(8) -99.3(2) ? . . . . O(4) Dy(1) O(5) N(3) -12.42(17) ? . . . . O(5) Dy(1) O(4) C(13) 167.26(17) ? . . . . O(5) Dy(1) O(4) C(19) -22.2(2) ? . . . . O(4) Dy(1) O(6) N(3) 165.78(17) ? . . . . O(6) Dy(1) O(4) C(13) 155.79(19) ? . . . . O(6) Dy(1) O(4) C(19) -33.6(2) ? . . . . O(4) Dy(1) O(8) N(4) 5.2(2) ? . . . . O(8) Dy(1) O(4) C(13) 77.0(2) ? . . . . O(8) Dy(1) O(4) C(19) -112.4(2) ? . . . . O(4) Dy(1) O(9) N(4) -171.54(18) ? . . . . O(9) Dy(1) O(4) C(13) 83.20(18) ? . . . . O(9) Dy(1) O(4) C(19) -106.2(2) ? . . . . O(4) Dy(1) O(11) N(5) 86.97(14) ? . . . . O(11) Dy(1) O(4) C(13) -127.46(18) ? . . . . O(11) Dy(1) O(4) C(19) 43.1(2) ? . . . . O(4) Dy(1) O(12) N(5) -85.58(14) ? . . . . O(12) Dy(1) O(4) C(13) -72.90(18) ? . . . . O(12) Dy(1) O(4) C(19) 97.7(2) ? . . . . O(5) Dy(1) O(6) N(3) -1.42(13) ? . . . . O(6) Dy(1) O(5) N(3) 1.42(13) ? . . . . O(5) Dy(1) O(8) N(4) -107.90(18) ? . . . . O(8) Dy(1) O(5) N(3) 115.65(16) ? . . . . O(5) Dy(1) O(9) N(4) 68.27(17) ? . . . . O(9) Dy(1) O(5) N(3) 66.45(15) ? . . . . O(5) Dy(1) O(11) N(5) -146.92(15) ? . . . . O(11) Dy(1) O(5) N(3) -75.73(15) ? . . . . O(5) Dy(1) O(12) N(5) 30.13(16) ? . . . . O(12) Dy(1) O(5) N(3) -102.96(16) ? . . . . O(6) Dy(1) O(8) N(4) -62.37(18) ? . . . . O(8) Dy(1) O(6) N(3) -61.35(16) ? . . . . O(6) Dy(1) O(9) N(4) 116.79(18) ? . . . . O(9) Dy(1) O(6) N(3) -107.33(16) ? . . . . O(6) Dy(1) O(11) N(5) 160.25(15) ? . . . . O(11) Dy(1) O(6) N(3) 86.83(15) ? . . . . O(6) Dy(1) O(12) N(5) -30.86(16) ? . . . . O(12) Dy(1) O(6) N(3) 108.69(16) ? . . . . O(8) Dy(1) O(9) N(4) 2.60(16) ? . . . . O(9) Dy(1) O(8) N(4) -2.61(16) ? . . . . O(8) Dy(1) O(11) N(5) -127.11(16) ? . . . . O(11) Dy(1) O(8) N(4) -128.42(18) ? . . . . O(8) Dy(1) O(12) N(5) 132.56(15) ? . . . . O(12) Dy(1) O(8) N(4) 131.96(17) ? . . . . O(9) Dy(1) O(11) N(5) 139.05(14) ? . . . . O(11) Dy(1) O(9) N(4) 138.23(16) ? . . . . O(9) Dy(1) O(12) N(5) -130.81(15) ? . . . . O(12) Dy(1) O(9) N(4) -127.58(17) ? . . . . O(11) Dy(1) O(12) N(5) -4.24(12) ? . . . . O(12) Dy(1) O(11) N(5) 4.18(12) ? . . . . O(1) V(1) O(2) Dy(1) 18.54(7) ? . . . . O(1) V(1) O(2) C(12) -143.7(2) ? . . . . O(2) V(1) O(1) Dy(1) -18.41(7) ? . . . . O(2) V(1) O(1) C(1) 153.1(2) ? . . . . O(1) V(1) O(14) C(22) 32.0(5) ? . . . . O(14) V(1) O(1) Dy(1) -98.58(8) ? . . . . O(14) V(1) O(1) C(1) 72.90(19) ? . . . . O(15) V(1) O(1) Dy(1) 82.45(10) ? . . . . O(15) V(1) O(1) C(1) -106.1(2) ? . . . . O(1) V(1) N(1) C(7) 8.6(2) ? . . . . O(1) V(1) N(1) C(9) -164.93(17) ? . . . . N(1) V(1) O(1) Dy(1) 179.55(8) ? . . . . N(1) V(1) O(1) C(1) -8.97(19) ? . . . . O(1) V(1) N(2) C(11) -135.2(2) ? . . . . O(1) V(1) N(2) C(18) 49.3(4) ? . . . . N(2) V(1) O(1) Dy(1) -82.4(2) ? . . . . N(2) V(1) O(1) C(1) 89.1(3) ? . . . . O(2) V(1) O(14) C(22) -49.1(5) ? . . . . O(14) V(1) O(2) Dy(1) 101.32(8) ? . . . . O(14) V(1) O(2) C(12) -60.9(2) ? . . . . O(15) V(1) O(2) Dy(1) -85.18(9) ? . . . . O(15) V(1) O(2) C(12) 112.6(2) ? . . . . O(2) V(1) N(1) C(7) -52.5(3) ? . . . . O(2) V(1) N(1) C(9) 134.0(2) ? . . . . N(1) V(1) O(2) Dy(1) 81.4(2) ? . . . . N(1) V(1) O(2) C(12) -80.9(3) ? . . . . O(2) V(1) N(2) C(11) 162.7(2) ? . . . . O(2) V(1) N(2) C(18) -12.8(2) ? . . . . N(2) V(1) O(2) Dy(1) 179.89(8) ? . . . . N(2) V(1) O(2) C(12) 17.6(2) ? . . . . O(14) V(1) N(1) C(7) -72.2(2) ? . . . . O(14) V(1) N(1) C(9) 114.24(18) ? . . . . N(1) V(1) O(14) C(22) 124.1(5) ? . . . . O(14) V(1) N(2) C(11) -118.9(2) ? . . . . O(14) V(1) N(2) C(18) 65.7(2) ? . . . . N(2) V(1) O(14) C(22) -142.2(5) ? . . . . O(15) V(1) N(1) C(7) 114.3(2) ? . . . . O(15) V(1) N(1) C(9) -59.19(18) ? . . . . O(15) V(1) N(2) C(11) 59.5(2) ? . . . . O(15) V(1) N(2) C(18) -116.0(2) ? . . . . N(1) V(1) N(2) C(11) -37.4(2) ? . . . . N(1) V(1) N(2) C(18) 147.2(2) ? . . . . N(2) V(1) N(1) C(7) -150.8(2) ? . . . . N(2) V(1) N(1) C(9) 35.71(18) ? . . . . Dy(1) O(1) C(1) C(2) -6.8(2) ? . . . . Dy(1) O(1) C(1) C(6) 175.02(16) ? . . . . V(1) O(1) C(1) C(2) -176.72(15) ? . . . . V(1) O(1) C(1) C(6) 5.1(3) ? . . . . Dy(1) O(2) C(12) C(13) 8.5(3) ? . . . . Dy(1) O(2) C(12) C(17) -170.8(2) ? . . . . V(1) O(2) C(12) C(13) 167.35(19) ? . . . . V(1) O(2) C(12) C(17) -12.0(3) ? . . . . Dy(1) O(3) C(2) C(1) 4.8(2) ? . . . . Dy(1) O(3) C(2) C(3) -175.79(18) ? . . . . C(8) O(3) C(2) C(1) 178.2(2) ? . . . . C(8) O(3) C(2) C(3) -2.3(3) ? . . . . Dy(1) O(4) C(13) C(12) -10.1(3) ? . . . . Dy(1) O(4) C(13) C(14) 168.8(2) ? . . . . C(19) O(4) C(13) C(12) 178.3(2) ? . . . . C(19) O(4) C(13) C(14) -2.8(3) ? . . . . Dy(1) O(5) N(3) O(6) -2.4(2) ? . . . . Dy(1) O(5) N(3) O(7) 179.93(17) ? . . . . Dy(1) O(6) N(3) O(5) 2.4(2) ? . . . . Dy(1) O(6) N(3) O(7) -179.92(18) ? . . . . Dy(1) O(8) N(4) O(9) 4.5(2) ? . . . . Dy(1) O(8) N(4) O(10) -175.6(2) ? . . . . Dy(1) O(9) N(4) O(8) -4.3(2) ? . . . . Dy(1) O(9) N(4) O(10) 175.7(2) ? . . . . Dy(1) O(11) N(5) O(12) -7.1(2) ? . . . . Dy(1) O(11) N(5) O(13) 172.4(2) ? . . . . Dy(1) O(12) N(5) O(11) 7.2(2) ? . . . . Dy(1) O(12) N(5) O(13) -172.4(2) ? . . . . V(1) O(14) C(22) C(23) 90.0(5) ? . . . . V(1) O(14) C(22) C(24) -88.4(6) ? . . . . V(1) N(1) C(7) C(6) -4.8(3) ? . . . . V(1) N(1) C(9) C(10) -53.5(2) ? . . . . C(7) N(1) C(9) C(10) 132.5(2) ? . . . . C(9) N(1) C(7) C(6) 168.9(2) ? . . . . V(1) N(2) C(11) C(10) 56.9(2) ? . . . . V(1) N(2) C(18) C(17) 2.2(4) ? . . . . C(11) N(2) C(18) C(17) -173.3(2) ? . . . . C(18) N(2) C(11) C(10) -127.3(2) ? . . . . O(1) C(1) C(2) O(3) 0.8(3) ? . . . . O(1) C(1) C(2) C(3) -178.7(2) ? . . . . O(1) C(1) C(6) C(5) 178.1(2) ? . . . . O(1) C(1) C(6) C(7) 2.7(3) ? . . . . C(2) C(1) C(6) C(5) -0.0(3) ? . . . . C(2) C(1) C(6) C(7) -175.5(2) ? . . . . C(6) C(1) C(2) O(3) 179.03(19) ? . . . . C(6) C(1) C(2) C(3) -0.4(3) ? . . . . O(3) C(2) C(3) C(4) -178.7(2) ? . . . . C(1) C(2) C(3) C(4) 0.7(3) ? . . . . C(2) C(3) C(4) C(5) -0.5(4) ? . . . . C(3) C(4) C(5) C(6) 0.1(3) ? . . . . C(4) C(5) C(6) C(1) 0.2(3) ? . . . . C(4) C(5) C(6) C(7) 176.0(2) ? . . . . C(1) C(6) C(7) N(1) -2.6(4) ? . . . . C(5) C(6) C(7) N(1) -178.2(2) ? . . . . N(1) C(9) C(10) C(11) 64.2(3) ? . . . . N(1) C(9) C(10) C(20) 179.0(2) ? . . . . N(1) C(9) C(10) C(21) -61.0(3) ? . . . . C(9) C(10) C(11) N(2) -66.2(2) ? . . . . C(20) C(10) C(11) N(2) 179.0(2) ? . . . . C(21) C(10) C(11) N(2) 59.5(3) ? . . . . O(2) C(12) C(13) O(4) 1.8(3) ? . . . . O(2) C(12) C(13) C(14) -177.2(2) ? . . . . O(2) C(12) C(17) C(16) 176.1(2) ? . . . . O(2) C(12) C(17) C(18) -5.1(4) ? . . . . C(13) C(12) C(17) C(16) -3.2(4) ? . . . . C(13) C(12) C(17) C(18) 175.6(2) ? . . . . C(17) C(12) C(13) O(4) -178.9(2) ? . . . . C(17) C(12) C(13) C(14) 2.2(4) ? . . . . O(4) C(13) C(14) C(15) -178.4(2) ? . . . . C(12) C(13) C(14) C(15) 0.4(4) ? . . . . C(13) C(14) C(15) C(16) -2.0(4) ? . . . . C(14) C(15) C(16) C(17) 1.0(4) ? . . . . C(15) C(16) C(17) C(12) 1.7(4) ? . . . . C(15) C(16) C(17) C(18) -177.2(2) ? . . . . C(12) C(17) C(18) N(2) 10.2(4) ? . . . . C(16) C(17) C(18) N(2) -171.0(2) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(5) C(24) 3.528(3) ? . 1_655 O(6) C(19) 3.454(4) ? . 3_765 O(7) C(11) 3.127(3) ? . 2_755 O(7) C(19) 3.444(4) ? . 3_765 O(7) C(23) 3.349(3) ? . 1_655 O(8) C(9) 3.370(3) ? . 3_766 O(8) C(20) 3.548(3) ? . 3_766 O(8) C(24) 3.559(4) ? . 1_655 O(9) C(8) 3.419(3) ? . 2_745 O(10) C(8) 3.581(3) ? . 2_745 O(10) C(21) 3.347(3) ? . 1_655 O(10) C(22) 3.329(4) ? . 1_655 O(10) C(23) 3.342(4) ? . 1_655 O(11) C(4) 3.400(4) ? . 4_564 O(11) C(5) 3.408(3) ? . 4_564 O(13) C(14) 3.546(3) ? . 3_665 O(13) C(15) 3.295(3) ? . 3_665 O(15) N(1) 3.415(2) ? . 3_766 O(15) C(7) 2.953(3) ? . 3_766 O(15) C(8) 3.551(3) ? . 2_745 O(15) C(9) 3.316(3) ? . 3_766 N(1) O(15) 3.415(2) ? . 3_766 N(3) C(23) 3.436(3) ? . 1_655 N(4) C(23) 3.386(4) ? . 1_655 C(4) O(11) 3.400(4) ? . 4_565 C(5) O(11) 3.408(3) ? . 4_565 C(7) O(15) 2.953(3) ? . 3_766 C(8) O(9) 3.419(3) ? . 2_755 C(8) O(10) 3.581(3) ? . 2_755 C(8) O(15) 3.551(3) ? . 2_755 C(9) O(8) 3.370(3) ? . 3_766 C(9) O(15) 3.316(3) ? . 3_766 C(11) O(7) 3.127(3) ? . 2_745 C(14) O(13) 3.546(3) ? . 3_665 C(15) O(13) 3.295(3) ? . 3_665 C(19) O(6) 3.454(4) ? . 3_765 C(19) O(7) 3.444(4) ? . 3_765 C(20) O(8) 3.548(3) ? . 3_766 C(21) O(10) 3.347(3) ? . 1_455 C(22) O(10) 3.329(4) ? . 1_455 C(23) O(7) 3.349(3) ? . 1_455 C(23) O(10) 3.342(4) ? . 1_455 C(23) N(3) 3.436(3) ? . 1_455 C(23) N(4) 3.386(4) ? . 1_455 C(24) O(5) 3.528(3) ? . 1_455 C(24) O(8) 3.559(4) ? . 1_455 V(1) H(9) 3.58(3) ? . 3_766 O(1) H(8) 3.56(3) ? . 3_766 O(1) H(9) 3.09(3) ? . 3_766 O(2) H(7) 3.34(3) ? . 2_745 O(3) H(21) 3.46(4) ? . 3_766 O(5) H(11) 3.54(3) ? . 2_755 O(5) H(15) 3.55(3) ? . 2_755 O(5) H(26) 2.932 ? . 1_655 O(5) H(28) 3.305 ? . 1_655 O(5) H(29) 2.937 ? . 1_655 O(6) H(2) 3.24(2) ? . 4_564 O(6) H(16) 3.41(3) ? . 3_765 O(6) H(18) 2.72(4) ? . 3_765 O(6) H(26) 2.898 ? . 1_655 O(7) H(10) 2.52(3) ? . 2_755 O(7) H(11) 2.79(2) ? . 2_755 O(7) H(12) 3.17(4) ? . 3_765 O(7) H(15) 3.47(3) ? . 2_755 O(7) H(18) 2.47(4) ? . 3_765 O(7) H(20) 3.59(3) ? . 2_755 O(7) H(25) 3.148 ? . 1_655 O(7) H(26) 2.704 ? . 1_655 O(7) H(29) 3.155 ? . 1_655 O(8) H(8) 2.56(3) ? . 3_766 O(8) H(9) 3.37(4) ? . 3_766 O(8) H(19) 2.85(3) ? . 3_766 O(8) H(21) 3.56(4) ? . 3_766 O(8) H(26) 3.220 ? . 1_655 O(8) H(28) 2.810 ? . 1_655 O(9) H(1) 2.73(3) ? . 2_745 O(9) H(5) 2.85(3) ? . 2_745 O(9) H(7) 3.22(3) ? . 2_745 O(9) H(26) 2.933 ? . 1_655 O(9) H(27) 3.464 ? . 1_655 O(10) H(4) 3.27(4) ? . 3_766 O(10) H(5) 2.69(3) ? . 2_745 O(10) H(8) 3.10(3) ? . 3_766 O(10) H(23) 3.09(3) ? . 1_655 O(10) H(24) 2.77(3) ? . 1_655 O(10) H(26) 3.118 ? . 1_655 O(10) H(27) 3.096 ? . 1_655 O(10) H(28) 3.322 ? . 1_655 O(11) H(2) 2.76(3) ? . 4_564 O(11) H(3) 2.85(3) ? . 4_564 O(11) H(13) 3.08(3) ? . 3_665 O(13) H(3) 3.29(3) ? . 4_564 O(13) H(10) 2.98(3) ? . 2_655 O(13) H(12) 3.04(3) ? . 3_665 O(13) H(13) 2.51(4) ? . 3_665 O(13) H(15) 3.32(3) ? . 2_655 O(13) H(20) 3.26(3) ? . 2_655 O(13) H(23) 2.83(3) ? . 2_655 O(15) H(3) 3.48(3) ? . 3_766 O(15) H(4) 2.55(3) ? . 3_766 O(15) H(5) 3.49(3) ? . 2_745 O(15) H(6) 3.14(4) ? . 2_745 O(15) H(8) 2.89(3) ? . 3_766 O(15) H(9) 3.14(3) ? . 3_766 N(1) H(9) 3.15(4) ? . 3_766 N(2) H(6) 3.52(4) ? . 2_745 N(3) H(2) 3.55(2) ? . 4_564 N(3) H(10) 3.42(3) ? . 2_755 N(3) H(11) 3.38(2) ? . 2_755 N(3) H(18) 2.92(4) ? . 3_765 N(3) H(25) 3.564 ? . 1_655 N(3) H(26) 2.567 ? . 1_655 N(3) H(29) 3.275 ? . 1_655 N(4) H(1) 3.58(2) ? . 2_745 N(4) H(5) 3.05(3) ? . 2_745 N(4) H(8) 3.15(3) ? . 3_766 N(4) H(26) 2.830 ? . 1_655 N(4) H(27) 3.345 ? . 1_655 N(4) H(28) 3.259 ? . 1_655 N(5) H(3) 3.47(3) ? . 4_564 N(5) H(12) 3.33(3) ? . 3_665 N(5) H(13) 3.00(3) ? . 3_665 C(1) H(9) 2.97(3) ? . 3_766 C(1) H(21) 3.25(4) ? . 3_766 C(2) H(21) 3.03(4) ? . 3_766 C(3) H(14) 3.49(3) ? . 2_655 C(3) H(21) 3.27(4) ? . 3_766 C(4) H(13) 3.07(4) ? . 2_655 C(4) H(14) 3.25(3) ? . 2_655 C(4) H(16) 3.43(3) ? . 4_565 C(5) H(11) 3.56(2) ? . 3_766 C(5) H(13) 3.10(4) ? . 2_655 C(5) H(14) 3.52(3) ? . 2_655 C(6) H(9) 2.93(4) ? . 3_766 C(7) H(9) 3.00(4) ? . 3_766 C(7) H(22) 3.40(5) ? . 3_666 C(12) H(7) 3.20(3) ? . 2_745 C(14) H(17) 2.99(5) ? . 3_665 C(14) H(20) 3.13(3) ? . 4_554 C(15) H(2) 3.38(3) ? . 2_645 C(15) H(17) 3.04(4) ? . 3_665 C(15) H(20) 2.70(3) ? . 4_554 C(16) H(20) 3.22(3) ? . 4_554 C(16) H(29) 3.486 ? . 2_645 C(16) H(30) 3.280 ? . 2_645 C(17) H(7) 3.33(3) ? . 2_745 C(18) H(7) 3.56(4) ? . 2_745 C(18) H(29) 3.305 ? . 2_645 C(19) H(2) 3.13(3) ? . 4_564 C(19) H(25) 3.325 ? . 3_665 C(19) H(26) 3.537 ? . 3_665 C(20) H(13) 3.52(4) ? . 4_555 C(20) H(28) 3.163 ? . 3_666 C(21) H(4) 3.49(4) ? . 3_666 C(21) H(22) 3.21(3) ? . 3_666 C(23) H(12) 3.58(4) ? . 3_665 C(23) H(17) 3.21(4) ? . 3_665 C(23) H(18) 3.35(3) ? . 3_665 C(24) H(14) 2.96(3) ? . 2_655 C(24) H(15) 3.23(3) ? . 2_655 C(24) H(19) 3.11(4) ? . 3_666 H(1) O(9) 2.73(3) ? . 2_755 H(1) N(4) 3.58(2) ? . 2_755 H(2) O(6) 3.24(2) ? . 4_565 H(2) O(11) 2.76(3) ? . 4_565 H(2) N(3) 3.55(2) ? . 4_565 H(2) C(15) 3.38(3) ? . 2_655 H(2) C(19) 3.13(3) ? . 4_565 H(2) H(13) 2.83(5) ? . 2_655 H(2) H(14) 3.48(4) ? . 2_655 H(2) H(16) 2.45(4) ? . 4_565 H(2) H(17) 3.10(6) ? . 4_565 H(3) O(11) 2.85(3) ? . 4_565 H(3) O(13) 3.29(3) ? . 4_565 H(3) O(15) 3.48(3) ? . 3_766 H(3) N(5) 3.47(3) ? . 4_565 H(3) H(6) 3.27(5) ? . 4_565 H(3) H(13) 2.92(5) ? . 2_655 H(3) H(23) 3.35(5) ? . 3_666 H(4) O(10) 3.27(4) ? . 3_766 H(4) O(15) 2.55(3) ? . 3_766 H(4) C(21) 3.49(4) ? . 3_666 H(4) H(9) 3.45(6) ? . 3_766 H(4) H(22) 2.97(6) ? . 3_666 H(4) H(23) 3.23(5) ? . 3_666 H(5) O(9) 2.85(3) ? . 2_755 H(5) O(10) 2.69(3) ? . 2_755 H(5) O(15) 3.49(3) ? . 2_755 H(5) N(4) 3.05(3) ? . 2_755 H(6) O(15) 3.14(4) ? . 2_755 H(6) N(2) 3.52(4) ? . 2_755 H(6) H(3) 3.27(5) ? . 4_564 H(6) H(11) 3.25(6) ? . 2_755 H(7) O(2) 3.34(3) ? . 2_755 H(7) O(9) 3.22(3) ? . 2_755 H(7) C(12) 3.20(3) ? . 2_755 H(7) C(17) 3.33(3) ? . 2_755 H(7) C(18) 3.56(4) ? . 2_755 H(7) H(21) 3.37(6) ? . 3_766 H(8) O(1) 3.56(3) ? . 3_766 H(8) O(8) 2.56(3) ? . 3_766 H(8) O(10) 3.10(3) ? . 3_766 H(8) O(15) 2.89(3) ? . 3_766 H(8) N(4) 3.15(3) ? . 3_766 H(8) H(22) 3.50(5) ? . 3_666 H(9) V(1) 3.58(3) ? . 3_766 H(9) O(1) 3.09(3) ? . 3_766 H(9) O(8) 3.37(4) ? . 3_766 H(9) O(15) 3.14(3) ? . 3_766 H(9) N(1) 3.15(4) ? . 3_766 H(9) C(1) 2.97(3) ? . 3_766 H(9) C(6) 2.93(4) ? . 3_766 H(9) C(7) 3.00(4) ? . 3_766 H(9) H(4) 3.45(6) ? . 3_766 H(9) H(9) 3.58(5) ? . 3_766 H(10) O(7) 2.52(3) ? . 2_745 H(10) O(13) 2.98(3) ? . 2_645 H(10) N(3) 3.42(3) ? . 2_745 H(10) H(29) 3.560 ? . 2_645 H(11) O(5) 3.54(3) ? . 2_745 H(11) O(7) 2.79(2) ? . 2_745 H(11) N(3) 3.38(2) ? . 2_745 H(11) C(5) 3.56(2) ? . 3_766 H(11) H(6) 3.25(6) ? . 2_745 H(12) O(7) 3.17(4) ? . 3_765 H(12) O(13) 3.04(3) ? . 3_665 H(12) N(5) 3.33(3) ? . 3_665 H(12) C(23) 3.58(4) ? . 3_665 H(12) H(12) 3.46(5) ? . 3_665 H(12) H(17) 2.86(6) ? . 3_665 H(12) H(20) 3.42(4) ? . 4_554 H(12) H(25) 2.723 ? . 3_665 H(13) O(11) 3.08(3) ? . 3_665 H(13) O(13) 2.51(4) ? . 3_665 H(13) N(5) 3.00(3) ? . 3_665 H(13) C(4) 3.07(4) ? . 2_645 H(13) C(5) 3.10(4) ? . 2_645 H(13) C(20) 3.52(4) ? . 4_554 H(13) H(2) 2.83(5) ? . 2_645 H(13) H(3) 2.92(5) ? . 2_645 H(13) H(17) 3.13(6) ? . 3_665 H(13) H(20) 2.57(5) ? . 4_554 H(13) H(23) 3.55(5) ? . 4_554 H(14) C(3) 3.49(3) ? . 2_645 H(14) C(4) 3.25(3) ? . 2_645 H(14) C(5) 3.52(3) ? . 2_645 H(14) C(24) 2.96(3) ? . 2_645 H(14) H(2) 3.48(4) ? . 2_645 H(14) H(20) 3.45(5) ? . 4_554 H(14) H(28) 3.158 ? . 2_645 H(14) H(29) 2.817 ? . 2_645 H(14) H(30) 2.460 ? . 2_645 H(15) O(5) 3.55(3) ? . 2_745 H(15) O(7) 3.47(3) ? . 2_745 H(15) O(13) 3.32(3) ? . 2_645 H(15) C(24) 3.23(3) ? . 2_645 H(15) H(29) 2.438 ? . 2_645 H(15) H(30) 3.250 ? . 2_645 H(16) O(6) 3.41(3) ? . 3_765 H(16) C(4) 3.43(3) ? . 4_564 H(16) H(2) 2.45(4) ? . 4_564 H(17) C(14) 2.99(5) ? . 3_665 H(17) C(15) 3.04(4) ? . 3_665 H(17) C(23) 3.21(4) ? . 3_665 H(17) H(2) 3.10(6) ? . 4_564 H(17) H(12) 2.86(6) ? . 3_665 H(17) H(13) 3.13(6) ? . 3_665 H(17) H(25) 2.760 ? . 3_665 H(17) H(26) 3.290 ? . 3_665 H(17) H(27) 3.081 ? . 3_665 H(18) O(6) 2.72(4) ? . 3_765 H(18) O(7) 2.47(4) ? . 3_765 H(18) N(3) 2.92(4) ? . 3_765 H(18) C(23) 3.35(3) ? . 3_665 H(18) H(25) 2.976 ? . 3_665 H(18) H(26) 3.011 ? . 3_665 H(18) H(27) 3.542 ? . 3_665 H(19) O(8) 2.85(3) ? . 3_766 H(19) C(24) 3.11(4) ? . 3_666 H(19) H(28) 2.235 ? . 3_666 H(19) H(29) 3.475 ? . 3_666 H(19) H(30) 3.308 ? . 3_666 H(20) O(7) 3.59(3) ? . 2_745 H(20) O(13) 3.26(3) ? . 2_645 H(20) C(14) 3.13(3) ? . 4_555 H(20) C(15) 2.70(3) ? . 4_555 H(20) C(16) 3.22(3) ? . 4_555 H(20) H(12) 3.42(4) ? . 4_555 H(20) H(13) 2.57(5) ? . 4_555 H(20) H(14) 3.45(5) ? . 4_555 H(20) H(28) 3.452 ? . 3_666 H(21) O(3) 3.46(4) ? . 3_766 H(21) O(8) 3.56(4) ? . 3_766 H(21) C(1) 3.25(4) ? . 3_766 H(21) C(2) 3.03(4) ? . 3_766 H(21) C(3) 3.27(4) ? . 3_766 H(21) H(7) 3.37(6) ? . 3_766 H(22) C(7) 3.40(5) ? . 3_666 H(22) C(21) 3.21(3) ? . 3_666 H(22) H(4) 2.97(6) ? . 3_666 H(22) H(8) 3.50(5) ? . 3_666 H(22) H(22) 2.48(5) ? . 3_666 H(22) H(24) 3.09(5) ? . 3_666 H(22) H(28) 3.325 ? . 3_666 H(23) O(10) 3.09(3) ? . 1_455 H(23) O(13) 2.83(3) ? . 2_645 H(23) H(3) 3.35(5) ? . 3_666 H(23) H(4) 3.23(5) ? . 3_666 H(23) H(13) 3.55(5) ? . 4_555 H(24) O(10) 2.77(3) ? . 1_455 H(24) H(22) 3.09(5) ? . 3_666 H(25) O(7) 3.148 ? . 1_455 H(25) N(3) 3.564 ? . 1_455 H(25) C(19) 3.325 ? . 3_665 H(25) H(12) 2.723 ? . 3_665 H(25) H(17) 2.760 ? . 3_665 H(25) H(18) 2.976 ? . 3_665 H(26) O(5) 2.932 ? . 1_455 H(26) O(6) 2.898 ? . 1_455 H(26) O(7) 2.704 ? . 1_455 H(26) O(8) 3.220 ? . 1_455 H(26) O(9) 2.933 ? . 1_455 H(26) O(10) 3.118 ? . 1_455 H(26) N(3) 2.567 ? . 1_455 H(26) N(4) 2.830 ? . 1_455 H(26) C(19) 3.537 ? . 3_665 H(26) H(17) 3.290 ? . 3_665 H(26) H(18) 3.011 ? . 3_665 H(27) O(9) 3.464 ? . 1_455 H(27) O(10) 3.096 ? . 1_455 H(27) N(4) 3.345 ? . 1_455 H(27) H(17) 3.081 ? . 3_665 H(27) H(18) 3.542 ? . 3_665 H(28) O(5) 3.305 ? . 1_455 H(28) O(8) 2.810 ? . 1_455 H(28) O(10) 3.322 ? . 1_455 H(28) N(4) 3.259 ? . 1_455 H(28) C(20) 3.163 ? . 3_666 H(28) H(14) 3.158 ? . 2_655 H(28) H(19) 2.235 ? . 3_666 H(28) H(20) 3.452 ? . 3_666 H(28) H(22) 3.325 ? . 3_666 H(29) O(5) 2.937 ? . 1_455 H(29) O(7) 3.155 ? . 1_455 H(29) N(3) 3.275 ? . 1_455 H(29) C(16) 3.486 ? . 2_655 H(29) C(18) 3.305 ? . 2_655 H(29) H(10) 3.560 ? . 2_655 H(29) H(14) 2.817 ? . 2_655 H(29) H(15) 2.438 ? . 2_655 H(29) H(19) 3.475 ? . 3_666 H(30) C(16) 3.280 ? . 2_655 H(30) H(14) 2.460 ? . 2_655 H(30) H(15) 3.250 ? . 2_655 H(30) H(19) 3.308 ? . 3_666 Dy(1) V(1) 3.4875(18) ? . . data___HoVO _database_code_depnum_ccdc_archive 'CCDC 881977' #TrackingRef '11261_web_deposit_cif_file_6_TakayukiIshida_1336987557.HoV_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Ho N5 O15 V ' _chemical_formula_moiety 'C24 H30 Ho N5 O15 V ' _chemical_formula_weight 844.40 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.911(2) _cell_length_b 17.521(7) _cell_length_c 18.250(5) _cell_angle_alpha 90.0000 _cell_angle_beta 105.498(4) _cell_angle_gamma 90.0000 _cell_volume 3053.8(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 450 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 90. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676.00 _exptl_absorpt_coefficient_mu 2.961 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.444 _exptl_absorpt_correction_T_max 0.641 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 51412 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_ambient_temperature 90. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6946 _reflns_number_gt 6355 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0691 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6946 _refine_ls_number_parameters 518 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0003Fo^2^ + 3.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.21 _refine_diff_density_min -1.43 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 4(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ho Ho -0.218 4.678 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; V V 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ho(1) Ho 0.92653(3) 0.573190(10) 0.203800(10) 0.01152(8) Uani 1.00 1 d . . . V(1) V 0.83853(10) 0.46971(6) 0.34704(5) 0.0120(2) Uani 1.00 1 d . . . O(1) O 0.8763(4) 0.5771(2) 0.3245(2) 0.0135(10) Uani 1.00 1 d . . . O(2) O 0.8144(4) 0.4633(2) 0.2357(2) 0.0138(9) Uani 1.00 1 d . . . O(3) O 0.9275(4) 0.7051(2) 0.2649(2) 0.0172(10) Uani 1.00 1 d . . . O(4) O 0.7870(4) 0.4940(2) 0.0940(2) 0.0180(10) Uani 1.00 1 d . . . O(5) O 1.1145(4) 0.6575(2) 0.1852(2) 0.0276(12) Uani 1.00 1 d . . . O(6) O 1.0382(5) 0.5735(2) 0.0990(3) 0.0287(14) Uani 1.00 1 d . . . O(7) O 1.2015(5) 0.6527(2) 0.0874(3) 0.0364(15) Uani 1.00 1 d . . . O(8) O 1.1383(4) 0.5474(2) 0.3020(2) 0.0245(12) Uani 1.00 1 d . . . O(9) O 1.0844(4) 0.4620(2) 0.2155(2) 0.0252(12) Uani 1.00 1 d . . . O(10) O 1.2639(4) 0.4438(3) 0.3132(3) 0.0338(14) Uani 1.00 1 d . . . O(11) O 0.8000(4) 0.6637(2) 0.1085(2) 0.0170(10) Uani 1.00 1 d . . . O(12) O 0.6856(4) 0.6154(2) 0.1829(2) 0.0199(11) Uani 1.00 1 d . . . O(13) O 0.5911(5) 0.7072(2) 0.1060(2) 0.0291(13) Uani 1.00 1 d . . . O(14) O 0.6056(4) 0.5123(2) 0.3006(2) 0.0190(11) Uani 1.00 1 d . . . O(15) O 0.9883(4) 0.4316(2) 0.3813(2) 0.0151(10) Uani 1.00 1 d . . . N(1) N 0.8051(5) 0.5019(3) 0.4500(2) 0.0167(12) Uani 1.00 1 d . . . N(2) N 0.7296(5) 0.3688(2) 0.3453(2) 0.0147(12) Uani 1.00 1 d . . . N(3) N 1.1221(5) 0.6294(3) 0.1229(3) 0.0209(13) Uani 1.00 1 d . . . N(4) N 1.1663(5) 0.4825(3) 0.2782(3) 0.0220(14) Uani 1.00 1 d . . . N(5) N 0.6881(5) 0.6644(3) 0.1316(2) 0.0181(12) Uani 1.00 1 d . . . C(1) C 0.8598(5) 0.6409(3) 0.3620(3) 0.0115(12) Uani 1.00 1 d . . . C(2) C 0.8878(5) 0.7115(3) 0.3326(3) 0.0132(13) Uani 1.00 1 d . . . C(3) C 0.8746(6) 0.7791(3) 0.3681(3) 0.0192(15) Uani 1.00 1 d . . . C(4) C 0.8363(7) 0.7775(3) 0.4367(3) 0.0219(16) Uani 1.00 1 d . . . C(5) C 0.8083(6) 0.7095(3) 0.4666(3) 0.0182(14) Uani 1.00 1 d . . . C(6) C 0.8209(5) 0.6395(3) 0.4310(3) 0.0157(14) Uani 1.00 1 d . . . C(7) C 0.7984(6) 0.5709(3) 0.4712(3) 0.0147(14) Uani 1.00 1 d . . . C(8) C 0.9522(7) 0.7777(3) 0.2321(3) 0.0240(17) Uani 1.00 1 d . . . C(9) C 0.8032(6) 0.4428(3) 0.5070(3) 0.0162(14) Uani 1.00 1 d . . . C(10) C 0.7035(6) 0.3752(3) 0.4800(3) 0.0167(14) Uani 1.00 1 d . . . C(11) C 0.7449(6) 0.3288(3) 0.4185(3) 0.0182(15) Uani 1.00 1 d . . . C(12) C 0.7204(6) 0.4214(3) 0.1857(3) 0.0127(13) Uani 1.00 1 d . . . C(13) C 0.7012(6) 0.4362(3) 0.1081(3) 0.0135(13) Uani 1.00 1 d . . . C(14) C 0.6029(6) 0.3982(4) 0.0527(3) 0.0211(16) Uani 1.00 1 d . . . C(15) C 0.5202(6) 0.3423(3) 0.0740(3) 0.0182(14) Uani 1.00 1 d . . . C(16) C 0.5379(6) 0.3245(3) 0.1488(3) 0.0190(15) Uani 1.00 1 d . . . C(17) C 0.6406(6) 0.3626(3) 0.2067(3) 0.0163(14) Uani 1.00 1 d . . . C(18) C 0.6571(6) 0.3373(3) 0.2847(3) 0.0169(14) Uani 1.00 1 d . . . C(19) C 0.7712(7) 0.5105(4) 0.0142(3) 0.0224(17) Uani 1.00 1 d . . . C(20) C 0.7232(8) 0.3218(4) 0.5482(4) 0.0280(19) Uani 1.00 1 d . . . C(21) C 0.5517(6) 0.4029(4) 0.4532(3) 0.0213(16) Uani 1.00 1 d . . . C(22) C 0.5051(5) 0.5481(3) 0.2636(3) 0.0149(14) Uani 1.00 1 d . . . C(23) C 0.4174(6) 0.5195(4) 0.1883(3) 0.0300(19) Uani 1.00 1 d . . . C(24) C 0.4658(7) 0.6229(4) 0.2901(3) 0.0285(18) Uani 1.00 1 d . . . H(1) H 0.901(5) 0.824(3) 0.351(3) 0.006(13) Uiso 1.00 1 d . . . H(2) H 0.831(7) 0.827(4) 0.463(4) 0.03(2) Uiso 1.00 1 d . . . H(3) H 0.782(8) 0.702(4) 0.510(4) 0.04(2) Uiso 1.00 1 d . . . H(4) H 0.780(6) 0.579(3) 0.519(3) 0.008(15) Uiso 1.00 1 d . . . H(5) H 0.868(6) 0.810(3) 0.220(3) 0.010(15) Uiso 1.00 1 d . . . H(6) H 0.974(8) 0.763(4) 0.184(4) 0.04(2) Uiso 1.00 1 d . . . H(7) H 1.053(6) 0.792(3) 0.281(3) 0.012(16) Uiso 1.00 1 d . . . H(8) H 0.780(6) 0.463(3) 0.553(3) 0.012(15) Uiso 1.00 1 d . . . H(9) H 0.896(6) 0.424(2) 0.526(3) 0.006(14) Uiso 1.00 1 d . . . H(10) H 0.687(5) 0.286(3) 0.407(3) 0.008(13) Uiso 1.00 1 d . . . H(11) H 0.842(6) 0.306(3) 0.434(3) 0.019(17) Uiso 1.00 1 d . . . H(12) H 0.590(8) 0.414(4) 0.001(4) 0.04(2) Uiso 1.00 1 d . . . H(13) H 0.456(7) 0.314(3) 0.037(3) 0.024(18) Uiso 1.00 1 d . . . H(14) H 0.486(7) 0.285(4) 0.166(3) 0.026(19) Uiso 1.00 1 d . . . H(15) H 0.603(6) 0.288(3) 0.290(3) 0.016(16) Uiso 1.00 1 d . . . H(16) H 0.829(6) 0.551(3) 0.010(3) 0.008(14) Uiso 1.00 1 d . . . H(17) H 0.671(7) 0.533(4) -0.012(3) 0.025(19) Uiso 1.00 1 d . . . H(18) H 0.795(5) 0.469(3) -0.005(3) 0.006(13) Uiso 1.00 1 d . . . H(19) H 0.709(6) 0.345(3) 0.591(3) 0.016(17) Uiso 1.00 1 d . . . H(20) H 0.653(8) 0.277(4) 0.536(4) 0.04(2) Uiso 1.00 1 d . . . H(21) H 0.820(7) 0.301(4) 0.565(4) 0.028(19) Uiso 1.00 1 d . . . H(22) H 0.515(8) 0.433(3) 0.492(4) 0.03(2) Uiso 1.00 1 d . . . H(23) H 0.487(7) 0.356(4) 0.439(4) 0.04(2) Uiso 1.00 1 d . . . H(24) H 0.531(7) 0.440(3) 0.410(4) 0.021(18) Uiso 1.00 1 d . . . H(25) H 0.4543 0.5383 0.1487 0.036 Uiso 1.00 1 c R . . H(26) H 0.3239 0.5370 0.1805 0.036 Uiso 1.00 1 c R . . H(27) H 0.4185 0.4653 0.1879 0.036 Uiso 1.00 1 c R . . H(28) H 0.4025 0.6150 0.3204 0.033 Uiso 1.00 1 c R . . H(29) H 0.4224 0.6537 0.2475 0.033 Uiso 1.00 1 c R . . H(30) H 0.5475 0.6477 0.3195 0.033 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ho(1) 0.01263(17) 0.01279(17) 0.01013(17) 0.00036(9) 0.00476(11) 0.00055(9) V(1) 0.0124(4) 0.0133(4) 0.0099(4) 0.0000(3) 0.0026(3) 0.0008(3) O(1) 0.019(2) 0.011(2) 0.013(2) -0.0019(15) 0.0089(17) -0.0028(14) O(2) 0.0141(19) 0.016(2) 0.0116(19) -0.0014(16) 0.0035(15) 0.0005(15) O(3) 0.027(2) 0.013(2) 0.015(2) -0.0050(17) 0.0105(17) -0.0024(16) O(4) 0.021(2) 0.023(2) 0.0116(19) -0.0031(18) 0.0073(16) -0.0001(17) O(5) 0.027(2) 0.037(2) 0.024(2) -0.007(2) 0.014(2) -0.003(2) O(6) 0.032(2) 0.027(2) 0.036(3) -0.012(2) 0.024(2) -0.010(2) O(7) 0.047(3) 0.028(2) 0.051(3) -0.001(2) 0.043(2) 0.008(2) O(8) 0.018(2) 0.034(2) 0.016(2) 0.008(2) -0.0041(17) 0.0038(19) O(9) 0.015(2) 0.018(2) 0.036(2) 0.0018(17) -0.0038(19) -0.007(2) O(10) 0.012(2) 0.042(3) 0.042(3) 0.011(2) -0.001(2) 0.020(2) O(11) 0.021(2) 0.017(2) 0.015(2) -0.0038(17) 0.0069(16) -0.0006(16) O(12) 0.022(2) 0.024(2) 0.016(2) 0.0045(18) 0.0095(17) 0.0045(17) O(13) 0.031(2) 0.032(2) 0.023(2) 0.020(2) 0.006(2) 0.012(2) O(14) 0.018(2) 0.022(2) 0.019(2) 0.0064(18) 0.0079(17) 0.0082(17) O(15) 0.011(2) 0.018(2) 0.014(2) -0.0000(15) -0.0005(16) 0.0018(15) N(1) 0.021(2) 0.020(2) 0.011(2) -0.003(2) 0.009(2) -0.002(2) N(2) 0.016(2) 0.015(2) 0.014(2) 0.0017(19) 0.0052(19) 0.0033(19) N(3) 0.018(2) 0.019(2) 0.028(2) 0.009(2) 0.011(2) 0.008(2) N(4) 0.013(2) 0.024(2) 0.031(3) -0.001(2) 0.010(2) 0.009(2) N(5) 0.021(2) 0.021(2) 0.011(2) -0.001(2) 0.003(2) 0.001(2) C(1) 0.009(2) 0.013(2) 0.011(2) -0.001(2) 0.001(2) -0.000(2) C(2) 0.012(2) 0.014(2) 0.012(2) 0.000(2) 0.000(2) 0.002(2) C(3) 0.020(3) 0.016(3) 0.021(3) -0.009(2) 0.005(2) -0.006(2) C(4) 0.030(3) 0.015(3) 0.019(3) 0.011(2) 0.004(2) 0.000(2) C(5) 0.018(2) 0.022(3) 0.013(2) 0.010(2) -0.000(2) 0.004(2) C(6) 0.013(2) 0.022(3) 0.012(2) -0.001(2) 0.004(2) -0.000(2) C(7) 0.011(2) 0.026(3) 0.005(2) 0.001(2) -0.001(2) 0.000(2) C(8) 0.042(4) 0.016(3) 0.017(3) 0.003(2) 0.014(3) 0.006(2) C(9) 0.011(2) 0.025(3) 0.011(2) -0.005(2) -0.000(2) 0.005(2) C(10) 0.018(2) 0.022(3) 0.009(2) -0.005(2) 0.002(2) 0.002(2) C(11) 0.022(3) 0.018(3) 0.014(2) 0.001(2) 0.003(2) 0.009(2) C(12) 0.012(2) 0.013(2) 0.012(2) 0.001(2) 0.002(2) -0.005(2) C(13) 0.016(2) 0.014(2) 0.010(2) 0.005(2) 0.003(2) 0.002(2) C(14) 0.020(3) 0.028(3) 0.015(3) 0.003(2) 0.006(2) -0.002(2) C(15) 0.017(2) 0.021(3) 0.012(2) 0.002(2) -0.003(2) -0.006(2) C(16) 0.017(2) 0.019(3) 0.019(3) 0.004(2) 0.002(2) 0.000(2) C(17) 0.015(2) 0.019(3) 0.015(2) 0.003(2) 0.004(2) -0.001(2) C(18) 0.018(2) 0.012(2) 0.022(3) -0.001(2) 0.008(2) -0.001(2) C(19) 0.034(3) 0.021(3) 0.012(2) 0.003(3) 0.006(2) 0.004(2) C(20) 0.036(4) 0.029(3) 0.022(3) 0.001(3) 0.013(3) 0.009(2) C(21) 0.015(2) 0.026(3) 0.022(3) -0.001(2) 0.004(2) 0.004(2) C(22) 0.011(2) 0.020(3) 0.015(2) -0.001(2) 0.006(2) -0.001(2) C(23) 0.021(3) 0.044(4) 0.025(3) -0.005(3) 0.008(2) -0.013(3) C(24) 0.027(3) 0.029(3) 0.028(3) -0.003(2) 0.003(2) -0.013(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ho(1) O(1) 2.385(4) yes . . Ho(1) O(2) 2.373(4) yes . . Ho(1) O(3) 2.564(4) yes . . Ho(1) O(4) 2.524(3) yes . . Ho(1) O(5) 2.471(5) yes . . Ho(1) O(6) 2.452(6) yes . . Ho(1) O(8) 2.411(3) yes . . Ho(1) O(9) 2.472(4) yes . . Ho(1) O(11) 2.439(3) yes . . Ho(1) O(12) 2.431(4) yes . . V(1) O(1) 1.983(3) yes . . V(1) O(2) 1.984(4) yes . . V(1) O(14) 2.358(4) yes . . V(1) O(15) 1.596(3) yes . . V(1) N(1) 2.071(5) yes . . V(1) N(2) 2.068(5) yes . . O(1) C(1) 1.344(7) yes . . O(2) C(12) 1.337(6) yes . . O(3) C(2) 1.399(7) yes . . O(3) C(8) 1.454(8) yes . . O(4) C(13) 1.390(7) yes . . O(4) C(19) 1.452(7) yes . . O(5) N(3) 1.260(7) yes . . O(6) N(3) 1.283(6) yes . . O(7) N(3) 1.217(8) yes . . O(8) N(4) 1.273(7) yes . . O(9) N(4) 1.266(6) yes . . O(10) N(4) 1.215(6) yes . . O(11) N(5) 1.287(7) yes . . O(12) N(5) 1.275(6) yes . . O(13) N(5) 1.210(6) yes . . O(14) C(22) 1.217(6) yes . . N(1) C(7) 1.276(7) yes . . N(1) C(9) 1.472(8) yes . . N(2) C(11) 1.481(7) yes . . N(2) C(18) 1.273(7) yes . . C(1) C(2) 1.404(8) yes . . C(1) C(6) 1.412(8) yes . . C(2) C(3) 1.373(8) yes . . C(3) C(4) 1.401(10) yes . . C(4) C(5) 1.369(9) yes . . C(5) C(6) 1.408(9) yes . . C(6) C(7) 1.456(8) yes . . C(9) C(10) 1.537(8) yes . . C(10) C(11) 1.527(9) yes . . C(10) C(20) 1.528(9) yes . . C(10) C(21) 1.531(8) yes . . C(12) C(13) 1.401(8) yes . . C(12) C(17) 1.413(8) yes . . C(13) C(14) 1.374(7) yes . . C(14) C(15) 1.396(9) yes . . C(15) C(16) 1.365(8) yes . . C(16) C(17) 1.422(7) yes . . C(17) C(18) 1.457(8) yes . . C(22) C(23) 1.502(8) yes . . C(22) C(24) 1.484(9) yes . . C(3) H(1) 0.91(5) no . . C(4) H(2) 1.00(7) no . . C(5) H(3) 0.91(9) no . . C(7) H(4) 0.94(7) no . . C(8) H(5) 0.99(6) no . . C(8) H(6) 1.00(9) no . . C(8) H(7) 1.17(5) no . . C(9) H(8) 0.99(7) no . . C(9) H(9) 0.95(5) no . . C(11) H(10) 0.94(5) no . . C(11) H(11) 1.01(6) no . . C(14) H(12) 0.96(8) no . . C(15) H(13) 0.94(6) no . . C(16) H(14) 0.96(7) no . . C(18) H(15) 1.04(6) no . . C(19) H(16) 0.93(6) no . . C(19) H(17) 1.06(6) no . . C(19) H(18) 0.87(6) no . . C(20) H(19) 0.92(7) no . . C(20) H(20) 1.03(8) no . . C(20) H(21) 0.99(7) no . . C(21) H(22) 1.02(8) no . . C(21) H(23) 1.03(7) no . . C(21) H(24) 0.99(7) no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Ho(1) O(2) 64.49(13) yes . . . O(1) Ho(1) O(3) 63.28(13) yes . . . O(1) Ho(1) O(4) 122.92(14) yes . . . O(1) Ho(1) O(5) 117.42(14) yes . . . O(1) Ho(1) O(6) 165.72(14) yes . . . O(1) Ho(1) O(8) 70.99(15) yes . . . O(1) Ho(1) O(9) 103.10(15) yes . . . O(1) Ho(1) O(11) 116.44(14) yes . . . O(1) Ho(1) O(12) 72.41(13) yes . . . O(2) Ho(1) O(3) 124.90(14) yes . . . O(2) Ho(1) O(4) 63.63(13) yes . . . O(2) Ho(1) O(5) 159.85(14) yes . . . O(2) Ho(1) O(6) 122.16(14) yes . . . O(2) Ho(1) O(8) 92.14(14) yes . . . O(2) Ho(1) O(9) 70.52(14) yes . . . O(2) Ho(1) O(11) 121.16(13) yes . . . O(2) Ho(1) O(12) 77.33(14) yes . . . O(3) Ho(1) O(4) 141.06(12) yes . . . O(3) Ho(1) O(5) 66.76(16) yes . . . O(3) Ho(1) O(6) 112.75(15) yes . . . O(3) Ho(1) O(8) 86.81(14) yes . . . O(3) Ho(1) O(9) 138.07(13) yes . . . O(3) Ho(1) O(11) 70.46(12) yes . . . O(3) Ho(1) O(12) 71.55(13) yes . . . O(4) Ho(1) O(5) 119.54(15) yes . . . O(4) Ho(1) O(6) 69.39(15) yes . . . O(4) Ho(1) O(8) 132.13(15) yes . . . O(4) Ho(1) O(9) 80.52(13) yes . . . O(4) Ho(1) O(11) 73.91(13) yes . . . O(4) Ho(1) O(12) 74.67(14) yes . . . O(5) Ho(1) O(6) 51.51(15) yes . . . O(5) Ho(1) O(8) 71.04(15) yes . . . O(5) Ho(1) O(9) 89.99(15) yes . . . O(5) Ho(1) O(11) 77.09(14) yes . . . O(5) Ho(1) O(12) 122.79(15) yes . . . O(6) Ho(1) O(8) 95.47(16) yes . . . O(6) Ho(1) O(9) 70.23(16) yes . . . O(6) Ho(1) O(11) 72.29(15) yes . . . O(6) Ho(1) O(12) 120.38(14) yes . . . O(8) Ho(1) O(9) 51.90(15) yes . . . O(8) Ho(1) O(11) 146.29(15) yes . . . O(8) Ho(1) O(12) 142.91(15) yes . . . O(9) Ho(1) O(11) 140.09(16) yes . . . O(9) Ho(1) O(12) 145.70(14) yes . . . O(11) Ho(1) O(12) 52.64(15) yes . . . O(1) V(1) O(2) 79.57(17) yes . . . O(1) V(1) O(14) 81.15(16) yes . . . O(1) V(1) O(15) 105.75(19) yes . . . O(1) V(1) N(1) 90.85(19) yes . . . O(1) V(1) N(2) 159.21(17) yes . . . O(2) V(1) O(14) 79.12(15) yes . . . O(2) V(1) O(15) 102.9(2) yes . . . O(2) V(1) N(1) 159.94(18) yes . . . O(2) V(1) N(2) 90.92(18) yes . . . O(14) V(1) O(15) 173.03(19) yes . . . O(14) V(1) N(1) 82.03(17) yes . . . O(14) V(1) N(2) 78.92(17) yes . . . O(15) V(1) N(1) 96.7(2) yes . . . O(15) V(1) N(2) 94.32(19) yes . . . N(1) V(1) N(2) 92.2(2) yes . . . Ho(1) O(1) V(1) 105.20(17) yes . . . Ho(1) O(1) C(1) 125.4(3) yes . . . V(1) O(1) C(1) 128.9(3) yes . . . Ho(1) O(2) V(1) 105.62(16) yes . . . Ho(1) O(2) C(12) 124.4(3) yes . . . V(1) O(2) C(12) 127.0(3) yes . . . Ho(1) O(3) C(2) 119.1(3) yes . . . Ho(1) O(3) C(8) 126.2(3) yes . . . C(2) O(3) C(8) 114.3(4) yes . . . Ho(1) O(4) C(13) 119.1(3) yes . . . Ho(1) O(4) C(19) 125.2(3) yes . . . C(13) O(4) C(19) 115.1(4) yes . . . Ho(1) O(5) N(3) 96.8(3) yes . . . Ho(1) O(6) N(3) 97.1(4) yes . . . Ho(1) O(8) N(4) 98.0(3) yes . . . Ho(1) O(9) N(4) 95.3(3) yes . . . Ho(1) O(11) N(5) 95.6(3) yes . . . Ho(1) O(12) N(5) 96.3(3) yes . . . V(1) O(14) C(22) 160.0(4) yes . . . V(1) N(1) C(7) 124.5(4) yes . . . V(1) N(1) C(9) 119.0(4) yes . . . C(7) N(1) C(9) 116.1(5) yes . . . V(1) N(2) C(11) 117.6(3) yes . . . V(1) N(2) C(18) 123.7(4) yes . . . C(11) N(2) C(18) 118.5(5) yes . . . O(5) N(3) O(6) 114.6(5) yes . . . O(5) N(3) O(7) 123.5(5) yes . . . O(6) N(3) O(7) 121.9(5) yes . . . O(8) N(4) O(9) 114.6(4) yes . . . O(8) N(4) O(10) 122.4(5) yes . . . O(9) N(4) O(10) 123.0(5) yes . . . O(11) N(5) O(12) 114.9(4) yes . . . O(11) N(5) O(13) 123.0(5) yes . . . O(12) N(5) O(13) 122.1(5) yes . . . O(1) C(1) C(2) 118.3(5) yes . . . O(1) C(1) C(6) 122.7(5) yes . . . C(2) C(1) C(6) 119.0(5) yes . . . O(3) C(2) C(1) 113.5(4) yes . . . O(3) C(2) C(3) 124.9(5) yes . . . C(1) C(2) C(3) 121.6(5) yes . . . C(2) C(3) C(4) 119.2(5) yes . . . C(3) C(4) C(5) 120.4(6) yes . . . C(4) C(5) C(6) 121.4(6) yes . . . C(1) C(6) C(5) 118.4(5) yes . . . C(1) C(6) C(7) 125.3(5) yes . . . C(5) C(6) C(7) 116.3(5) yes . . . N(1) C(7) C(6) 127.1(6) yes . . . N(1) C(9) C(10) 116.3(4) yes . . . C(9) C(10) C(11) 111.7(5) yes . . . C(9) C(10) C(20) 106.2(4) yes . . . C(9) C(10) C(21) 110.5(5) yes . . . C(11) C(10) C(20) 105.8(5) yes . . . C(11) C(10) C(21) 111.6(4) yes . . . C(20) C(10) C(21) 110.8(5) yes . . . N(2) C(11) C(10) 115.4(5) yes . . . O(2) C(12) C(13) 118.1(5) yes . . . O(2) C(12) C(17) 123.6(5) yes . . . C(13) C(12) C(17) 118.3(4) yes . . . O(4) C(13) C(12) 113.4(4) yes . . . O(4) C(13) C(14) 124.4(5) yes . . . C(12) C(13) C(14) 122.1(5) yes . . . C(13) C(14) C(15) 119.2(5) yes . . . C(14) C(15) C(16) 120.7(5) yes . . . C(15) C(16) C(17) 120.7(5) yes . . . C(12) C(17) C(16) 118.8(5) yes . . . C(12) C(17) C(18) 124.2(4) yes . . . C(16) C(17) C(18) 117.0(5) yes . . . N(2) C(18) C(17) 127.4(5) yes . . . O(14) C(22) C(23) 121.6(5) yes . . . O(14) C(22) C(24) 121.4(5) yes . . . C(23) C(22) C(24) 117.0(5) yes . . . C(2) C(3) H(1) 120(3) no . . . C(4) C(3) H(1) 120(3) no . . . C(3) C(4) H(2) 118(4) no . . . C(5) C(4) H(2) 121(4) no . . . C(4) C(5) H(3) 128(5) no . . . C(6) C(5) H(3) 111(5) no . . . N(1) C(7) H(4) 117(3) no . . . C(6) C(7) H(4) 116(3) no . . . O(3) C(8) H(5) 112(3) no . . . O(3) C(8) H(6) 104(4) no . . . O(3) C(8) H(7) 94(3) no . . . H(5) C(8) H(6) 109(5) no . . . H(5) C(8) H(7) 123(4) no . . . H(6) C(8) H(7) 113(5) no . . . N(1) C(9) H(8) 114(3) no . . . N(1) C(9) H(9) 108(3) no . . . C(10) C(9) H(8) 105(3) no . . . C(10) C(9) H(9) 109(3) no . . . H(8) C(9) H(9) 104(5) no . . . N(2) C(11) H(10) 106(3) no . . . N(2) C(11) H(11) 108(4) no . . . C(10) C(11) H(10) 109(4) no . . . C(10) C(11) H(11) 115(3) no . . . H(10) C(11) H(11) 103(5) no . . . C(13) C(14) H(12) 118(4) no . . . C(15) C(14) H(12) 123(4) no . . . C(14) C(15) H(13) 120(4) no . . . C(16) C(15) H(13) 119(4) no . . . C(15) C(16) H(14) 124(3) no . . . C(17) C(16) H(14) 116(3) no . . . N(2) C(18) H(15) 118(3) no . . . C(17) C(18) H(15) 115(3) no . . . O(4) C(19) H(16) 110(3) no . . . O(4) C(19) H(17) 112(4) no . . . O(4) C(19) H(18) 105(4) no . . . H(16) C(19) H(17) 102(5) no . . . H(16) C(19) H(18) 112(5) no . . . H(17) C(19) H(18) 117(5) no . . . C(10) C(20) H(19) 114(3) no . . . C(10) C(20) H(20) 111(4) no . . . C(10) C(20) H(21) 113(4) no . . . H(19) C(20) H(20) 105(6) no . . . H(19) C(20) H(21) 104(5) no . . . H(20) C(20) H(21) 109(6) no . . . C(10) C(21) H(22) 116(4) no . . . C(10) C(21) H(23) 109(4) no . . . C(10) C(21) H(24) 116(4) no . . . H(22) C(21) H(23) 106(6) no . . . H(22) C(21) H(24) 100(5) no . . . H(23) C(21) H(24) 109(5) no . . . C(22) C(23) H(25) 109.5 no . . . C(22) C(23) H(26) 109.4 no . . . C(22) C(23) H(27) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . H(25) C(23) H(27) 109.5 no . . . H(26) C(23) H(27) 109.5 no . . . C(22) C(24) H(28) 109.4 no . . . C(22) C(24) H(29) 109.7 no . . . C(22) C(24) H(30) 109.3 no . . . H(28) C(24) H(29) 109.5 no . . . H(28) C(24) H(30) 109.5 no . . . H(29) C(24) H(30) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Ho(1) O(2) V(1) -16.55(15) ? . . . . O(1) Ho(1) O(2) C(12) 145.0(4) ? . . . . O(2) Ho(1) O(1) V(1) 16.52(14) ? . . . . O(2) Ho(1) O(1) C(1) -155.6(4) ? . . . . O(1) Ho(1) O(3) C(2) -5.1(3) ? . . . . O(1) Ho(1) O(3) C(8) -178.3(4) ? . . . . O(3) Ho(1) O(1) V(1) 178.3(2) ? . . . . O(3) Ho(1) O(1) C(1) 6.2(3) ? . . . . O(1) Ho(1) O(4) C(13) -16.6(4) ? . . . . O(1) Ho(1) O(4) C(19) 153.6(4) ? . . . . O(4) Ho(1) O(1) V(1) 43.0(2) ? . . . . O(4) Ho(1) O(1) C(1) -129.1(3) ? . . . . O(1) Ho(1) O(5) N(3) 169.8(3) ? . . . . O(5) Ho(1) O(1) V(1) -141.03(16) ? . . . . O(5) Ho(1) O(1) C(1) 46.9(4) ? . . . . O(1) Ho(1) O(6) N(3) -43.0(7) ? . . . . O(6) Ho(1) O(1) V(1) -104.5(5) ? . . . . O(6) Ho(1) O(1) C(1) 83.4(6) ? . . . . O(1) Ho(1) O(8) N(4) 122.6(4) ? . . . . O(8) Ho(1) O(1) V(1) -85.49(19) ? . . . . O(8) Ho(1) O(1) C(1) 102.4(4) ? . . . . O(1) Ho(1) O(9) N(4) -50.1(3) ? . . . . O(9) Ho(1) O(1) V(1) -44.11(19) ? . . . . O(9) Ho(1) O(1) C(1) 143.8(3) ? . . . . O(1) Ho(1) O(11) N(5) -31.9(3) ? . . . . O(11) Ho(1) O(1) V(1) 130.29(16) ? . . . . O(11) Ho(1) O(1) C(1) -41.8(4) ? . . . . O(1) Ho(1) O(12) N(5) 141.5(3) ? . . . . O(12) Ho(1) O(1) V(1) 100.58(19) ? . . . . O(12) Ho(1) O(1) C(1) -71.5(3) ? . . . . O(2) Ho(1) O(3) C(2) 15.0(3) ? . . . . O(2) Ho(1) O(3) C(8) -158.2(4) ? . . . . O(3) Ho(1) O(2) V(1) -36.4(2) ? . . . . O(3) Ho(1) O(2) C(12) 125.2(4) ? . . . . O(2) Ho(1) O(4) C(13) 10.1(3) ? . . . . O(2) Ho(1) O(4) C(19) -179.8(4) ? . . . . O(4) Ho(1) O(2) V(1) -171.9(2) ? . . . . O(4) Ho(1) O(2) C(12) -10.3(4) ? . . . . O(2) Ho(1) O(5) N(3) 79.5(5) ? . . . . O(5) Ho(1) O(2) V(1) 83.9(4) ? . . . . O(5) Ho(1) O(2) C(12) -114.6(5) ? . . . . O(2) Ho(1) O(6) N(3) -157.1(2) ? . . . . O(6) Ho(1) O(2) V(1) 149.00(16) ? . . . . O(6) Ho(1) O(2) C(12) -49.4(4) ? . . . . O(2) Ho(1) O(8) N(4) 60.5(3) ? . . . . O(8) Ho(1) O(2) V(1) 51.17(19) ? . . . . O(8) Ho(1) O(2) C(12) -147.2(4) ? . . . . O(2) Ho(1) O(9) N(4) -106.6(3) ? . . . . O(9) Ho(1) O(2) V(1) 99.25(18) ? . . . . O(9) Ho(1) O(2) C(12) -99.2(4) ? . . . . O(2) Ho(1) O(11) N(5) 42.9(3) ? . . . . O(11) Ho(1) O(2) V(1) -123.28(17) ? . . . . O(11) Ho(1) O(2) C(12) 38.3(4) ? . . . . O(2) Ho(1) O(12) N(5) -151.6(3) ? . . . . O(12) Ho(1) O(2) V(1) -92.90(18) ? . . . . O(12) Ho(1) O(2) C(12) 68.7(4) ? . . . . O(3) Ho(1) O(4) C(13) -103.7(4) ? . . . . O(3) Ho(1) O(4) C(19) 66.5(5) ? . . . . O(4) Ho(1) O(3) C(2) 105.1(3) ? . . . . O(4) Ho(1) O(3) C(8) -68.1(5) ? . . . . O(3) Ho(1) O(5) N(3) -150.9(3) ? . . . . O(5) Ho(1) O(3) C(2) -146.1(3) ? . . . . O(5) Ho(1) O(3) C(8) 40.7(4) ? . . . . O(3) Ho(1) O(6) N(3) 27.8(3) ? . . . . O(6) Ho(1) O(3) C(2) -170.0(3) ? . . . . O(6) Ho(1) O(3) C(8) 16.8(4) ? . . . . O(3) Ho(1) O(8) N(4) -174.6(3) ? . . . . O(8) Ho(1) O(3) C(2) -75.4(3) ? . . . . O(8) Ho(1) O(3) C(8) 111.4(4) ? . . . . O(3) Ho(1) O(9) N(4) 14.3(4) ? . . . . O(9) Ho(1) O(3) C(2) -84.7(4) ? . . . . O(9) Ho(1) O(3) C(8) 102.1(4) ? . . . . O(3) Ho(1) O(11) N(5) -76.7(3) ? . . . . O(11) Ho(1) O(3) C(2) 129.9(3) ? . . . . O(11) Ho(1) O(3) C(8) -43.3(4) ? . . . . O(3) Ho(1) O(12) N(5) 74.5(3) ? . . . . O(12) Ho(1) O(3) C(2) 74.0(3) ? . . . . O(12) Ho(1) O(3) C(8) -99.2(4) ? . . . . O(4) Ho(1) O(5) N(3) -14.1(3) ? . . . . O(5) Ho(1) O(4) C(13) 167.5(3) ? . . . . O(5) Ho(1) O(4) C(19) -22.4(5) ? . . . . O(4) Ho(1) O(6) N(3) 165.8(3) ? . . . . O(6) Ho(1) O(4) C(13) 155.3(4) ? . . . . O(6) Ho(1) O(4) C(19) -34.6(4) ? . . . . O(4) Ho(1) O(8) N(4) 5.0(4) ? . . . . O(8) Ho(1) O(4) C(13) 77.0(4) ? . . . . O(8) Ho(1) O(4) C(19) -112.9(4) ? . . . . O(4) Ho(1) O(9) N(4) -171.9(3) ? . . . . O(9) Ho(1) O(4) C(13) 82.9(3) ? . . . . O(9) Ho(1) O(4) C(19) -106.9(4) ? . . . . O(4) Ho(1) O(11) N(5) 87.3(3) ? . . . . O(11) Ho(1) O(4) C(13) -128.0(4) ? . . . . O(11) Ho(1) O(4) C(19) 42.1(4) ? . . . . O(4) Ho(1) O(12) N(5) -85.8(3) ? . . . . O(12) Ho(1) O(4) C(13) -73.2(3) ? . . . . O(12) Ho(1) O(4) C(19) 97.0(4) ? . . . . O(5) Ho(1) O(6) N(3) -0.6(2) ? . . . . O(6) Ho(1) O(5) N(3) 0.6(3) ? . . . . O(5) Ho(1) O(8) N(4) -108.1(4) ? . . . . O(8) Ho(1) O(5) N(3) 114.3(3) ? . . . . O(5) Ho(1) O(9) N(4) 68.1(3) ? . . . . O(9) Ho(1) O(5) N(3) 65.0(3) ? . . . . O(5) Ho(1) O(11) N(5) -146.4(3) ? . . . . O(11) Ho(1) O(5) N(3) -76.9(3) ? . . . . O(5) Ho(1) O(12) N(5) 29.7(3) ? . . . . O(12) Ho(1) O(5) N(3) -104.3(3) ? . . . . O(6) Ho(1) O(8) N(4) -62.1(3) ? . . . . O(8) Ho(1) O(6) N(3) -61.1(3) ? . . . . O(6) Ho(1) O(9) N(4) 116.7(3) ? . . . . O(9) Ho(1) O(6) N(3) -107.2(3) ? . . . . O(6) Ho(1) O(11) N(5) 160.3(3) ? . . . . O(11) Ho(1) O(6) N(3) 86.8(3) ? . . . . O(6) Ho(1) O(12) N(5) -31.6(3) ? . . . . O(12) Ho(1) O(6) N(3) 109.0(3) ? . . . . O(8) Ho(1) O(9) N(4) 2.5(3) ? . . . . O(9) Ho(1) O(8) N(4) -2.5(3) ? . . . . O(8) Ho(1) O(11) N(5) -127.1(3) ? . . . . O(11) Ho(1) O(8) N(4) -128.0(3) ? . . . . O(8) Ho(1) O(12) N(5) 131.9(3) ? . . . . O(12) Ho(1) O(8) N(4) 132.2(3) ? . . . . O(9) Ho(1) O(11) N(5) 139.6(3) ? . . . . O(11) Ho(1) O(9) N(4) 137.8(3) ? . . . . O(9) Ho(1) O(12) N(5) -131.0(3) ? . . . . O(12) Ho(1) O(9) N(4) -128.0(3) ? . . . . O(11) Ho(1) O(12) N(5) -4.6(2) ? . . . . O(12) Ho(1) O(11) N(5) 4.5(2) ? . . . . O(1) V(1) O(2) Ho(1) 18.32(17) ? . . . . O(1) V(1) O(2) C(12) -142.6(4) ? . . . . O(2) V(1) O(1) Ho(1) -18.19(16) ? . . . . O(2) V(1) O(1) C(1) 153.5(4) ? . . . . O(1) V(1) O(14) C(22) 31.6(12) ? . . . . O(14) V(1) O(1) Ho(1) -98.66(16) ? . . . . O(14) V(1) O(1) C(1) 73.0(4) ? . . . . O(15) V(1) O(1) Ho(1) 82.4(2) ? . . . . O(15) V(1) O(1) C(1) -105.9(4) ? . . . . O(1) V(1) N(1) C(7) 7.9(4) ? . . . . O(1) V(1) N(1) C(9) -165.4(3) ? . . . . N(1) V(1) O(1) Ho(1) 179.54(18) ? . . . . N(1) V(1) O(1) C(1) -8.8(4) ? . . . . O(1) V(1) N(2) C(11) -135.3(5) ? . . . . O(1) V(1) N(2) C(18) 48.8(8) ? . . . . N(2) V(1) O(1) Ho(1) -82.1(6) ? . . . . N(2) V(1) O(1) C(1) 89.6(6) ? . . . . O(2) V(1) O(14) C(22) -49.4(12) ? . . . . O(14) V(1) O(2) Ho(1) 101.20(17) ? . . . . O(14) V(1) O(2) C(12) -59.7(4) ? . . . . O(15) V(1) O(2) Ho(1) -85.6(2) ? . . . . O(15) V(1) O(2) C(12) 113.4(4) ? . . . . O(2) V(1) N(1) C(7) -52.9(8) ? . . . . O(2) V(1) N(1) C(9) 133.8(5) ? . . . . N(1) V(1) O(2) Ho(1) 80.9(5) ? . . . . N(1) V(1) O(2) C(12) -80.0(7) ? . . . . O(2) V(1) N(2) C(11) 162.6(4) ? . . . . O(2) V(1) N(2) C(18) -13.3(5) ? . . . . N(2) V(1) O(2) Ho(1) 179.73(18) ? . . . . N(2) V(1) O(2) C(12) 18.8(4) ? . . . . O(14) V(1) N(1) C(7) -73.1(4) ? . . . . O(14) V(1) N(1) C(9) 113.7(4) ? . . . . N(1) V(1) O(14) C(22) 123.7(12) ? . . . . O(14) V(1) N(2) C(11) -118.7(4) ? . . . . O(14) V(1) N(2) C(18) 65.4(5) ? . . . . N(2) V(1) O(14) C(22) -142.5(12) ? . . . . O(15) V(1) N(1) C(7) 113.8(4) ? . . . . O(15) V(1) N(1) C(9) -59.4(4) ? . . . . O(15) V(1) N(2) C(11) 59.6(4) ? . . . . O(15) V(1) N(2) C(18) -116.3(5) ? . . . . N(1) V(1) N(2) C(11) -37.2(4) ? . . . . N(1) V(1) N(2) C(18) 146.9(5) ? . . . . N(2) V(1) N(1) C(7) -151.6(4) ? . . . . N(2) V(1) N(1) C(9) 35.2(4) ? . . . . Ho(1) O(1) C(1) C(2) -6.9(6) ? . . . . Ho(1) O(1) C(1) C(6) 175.7(3) ? . . . . V(1) O(1) C(1) C(2) -177.0(3) ? . . . . V(1) O(1) C(1) C(6) 5.5(7) ? . . . . Ho(1) O(2) C(12) C(13) 9.7(7) ? . . . . Ho(1) O(2) C(12) C(17) -171.1(4) ? . . . . V(1) O(2) C(12) C(13) 167.3(4) ? . . . . V(1) O(2) C(12) C(17) -13.5(8) ? . . . . Ho(1) O(3) C(2) C(1) 4.0(5) ? . . . . Ho(1) O(3) C(2) C(3) -175.3(4) ? . . . . C(8) O(3) C(2) C(1) 177.9(4) ? . . . . C(8) O(3) C(2) C(3) -1.3(7) ? . . . . Ho(1) O(4) C(13) C(12) -9.4(6) ? . . . . Ho(1) O(4) C(13) C(14) 168.3(5) ? . . . . C(19) O(4) C(13) C(12) 179.4(5) ? . . . . C(19) O(4) C(13) C(14) -2.8(8) ? . . . . Ho(1) O(5) N(3) O(6) -1.0(4) ? . . . . Ho(1) O(5) N(3) O(7) 178.8(4) ? . . . . Ho(1) O(6) N(3) O(5) 1.0(4) ? . . . . Ho(1) O(6) N(3) O(7) -178.8(4) ? . . . . Ho(1) O(8) N(4) O(9) 4.2(5) ? . . . . Ho(1) O(8) N(4) O(10) -175.7(5) ? . . . . Ho(1) O(9) N(4) O(8) -4.1(5) ? . . . . Ho(1) O(9) N(4) O(10) 175.8(5) ? . . . . Ho(1) O(11) N(5) O(12) -7.6(4) ? . . . . Ho(1) O(11) N(5) O(13) 173.7(4) ? . . . . Ho(1) O(12) N(5) O(11) 7.6(4) ? . . . . Ho(1) O(12) N(5) O(13) -173.6(4) ? . . . . V(1) O(14) C(22) C(23) 90.6(12) ? . . . . V(1) O(14) C(22) C(24) -87.9(13) ? . . . . V(1) N(1) C(7) C(6) -4.1(8) ? . . . . V(1) N(1) C(9) C(10) -53.0(6) ? . . . . C(7) N(1) C(9) C(10) 133.2(5) ? . . . . C(9) N(1) C(7) C(6) 169.3(5) ? . . . . V(1) N(2) C(11) C(10) 58.1(6) ? . . . . V(1) N(2) C(18) C(17) 2.6(9) ? . . . . C(11) N(2) C(18) C(17) -173.2(6) ? . . . . C(18) N(2) C(11) C(10) -125.8(6) ? . . . . O(1) C(1) C(2) O(3) 1.3(6) ? . . . . O(1) C(1) C(2) C(3) -179.4(4) ? . . . . O(1) C(1) C(6) C(5) 179.1(4) ? . . . . O(1) C(1) C(6) C(7) 2.0(8) ? . . . . C(2) C(1) C(6) C(5) 1.6(7) ? . . . . C(2) C(1) C(6) C(7) -175.4(4) ? . . . . C(6) C(1) C(2) O(3) 178.9(4) ? . . . . C(6) C(1) C(2) C(3) -1.8(7) ? . . . . O(3) C(2) C(3) C(4) -178.8(5) ? . . . . C(1) C(2) C(3) C(4) 2.0(8) ? . . . . C(2) C(3) C(4) C(5) -2.0(8) ? . . . . C(3) C(4) C(5) C(6) 1.9(8) ? . . . . C(4) C(5) C(6) C(1) -1.7(8) ? . . . . C(4) C(5) C(6) C(7) 175.6(5) ? . . . . C(1) C(6) C(7) N(1) -2.5(9) ? . . . . C(5) C(6) C(7) N(1) -179.6(5) ? . . . . N(1) C(9) C(10) C(11) 63.9(6) ? . . . . N(1) C(9) C(10) C(20) 178.8(5) ? . . . . N(1) C(9) C(10) C(21) -61.0(7) ? . . . . C(9) C(10) C(11) N(2) -66.8(6) ? . . . . C(20) C(10) C(11) N(2) 178.1(5) ? . . . . C(21) C(10) C(11) N(2) 57.5(7) ? . . . . O(2) C(12) C(13) O(4) 0.5(7) ? . . . . O(2) C(12) C(13) C(14) -177.2(5) ? . . . . O(2) C(12) C(17) C(16) 176.5(5) ? . . . . O(2) C(12) C(17) C(18) -4.0(9) ? . . . . C(13) C(12) C(17) C(16) -4.2(8) ? . . . . C(13) C(12) C(17) C(18) 175.2(5) ? . . . . C(17) C(12) C(13) O(4) -178.7(5) ? . . . . C(17) C(12) C(13) C(14) 3.5(9) ? . . . . O(4) C(13) C(14) C(15) -178.4(5) ? . . . . C(12) C(13) C(14) C(15) -0.9(9) ? . . . . C(13) C(14) C(15) C(16) -1.0(9) ? . . . . C(14) C(15) C(16) C(17) 0.2(7) ? . . . . C(15) C(16) C(17) C(12) 2.5(9) ? . . . . C(15) C(16) C(17) C(18) -177.0(5) ? . . . . C(12) C(17) C(18) N(2) 9.6(10) ? . . . . C(16) C(17) C(18) N(2) -170.9(6) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(5) C(24) 3.548(7) ? . 1_655 O(6) C(19) 3.477(9) ? . 3_765 O(7) C(11) 3.137(8) ? . 2_755 O(7) C(19) 3.459(8) ? . 3_765 O(7) C(23) 3.363(8) ? . 1_655 O(8) C(9) 3.381(7) ? . 3_766 O(8) C(20) 3.550(8) ? . 3_766 O(8) C(24) 3.564(8) ? . 1_655 O(9) C(8) 3.416(8) ? . 2_745 O(10) C(8) 3.577(8) ? . 2_745 O(10) C(21) 3.358(7) ? . 1_655 O(10) C(22) 3.321(8) ? . 1_655 O(10) C(23) 3.336(9) ? . 1_655 O(11) C(4) 3.410(8) ? . 4_564 O(11) C(5) 3.430(7) ? . 4_564 O(13) C(14) 3.538(7) ? . 3_665 O(13) C(15) 3.289(7) ? . 3_665 O(15) N(1) 3.414(5) ? . 3_766 O(15) C(7) 2.945(6) ? . 3_766 O(15) C(8) 3.543(8) ? . 2_745 O(15) C(9) 3.319(6) ? . 3_766 N(1) O(15) 3.414(5) ? . 3_766 N(3) C(23) 3.439(8) ? . 1_655 N(4) C(23) 3.390(9) ? . 1_655 C(4) O(11) 3.410(8) ? . 4_565 C(5) O(11) 3.430(7) ? . 4_565 C(7) O(15) 2.945(6) ? . 3_766 C(8) O(9) 3.416(8) ? . 2_755 C(8) O(10) 3.577(8) ? . 2_755 C(8) O(15) 3.543(8) ? . 2_755 C(9) O(8) 3.381(7) ? . 3_766 C(9) O(15) 3.319(6) ? . 3_766 C(11) O(7) 3.137(8) ? . 2_745 C(14) O(13) 3.538(7) ? . 3_665 C(15) O(13) 3.289(7) ? . 3_665 C(19) O(6) 3.477(9) ? . 3_765 C(19) O(7) 3.459(8) ? . 3_765 C(20) O(8) 3.550(8) ? . 3_766 C(21) O(10) 3.358(7) ? . 1_455 C(22) O(10) 3.321(8) ? . 1_455 C(23) O(7) 3.363(8) ? . 1_455 C(23) O(10) 3.336(9) ? . 1_455 C(23) N(3) 3.439(8) ? . 1_455 C(23) N(4) 3.390(9) ? . 1_455 C(24) O(5) 3.548(7) ? . 1_455 C(24) O(8) 3.564(8) ? . 1_455 V(1) H(9) 3.54(5) ? . 3_766 O(1) H(9) 3.05(5) ? . 3_766 O(2) H(7) 3.33(6) ? . 2_745 O(3) H(21) 3.43(6) ? . 3_766 O(5) H(11) 3.50(6) ? . 2_755 O(5) H(15) 3.54(6) ? . 2_755 O(5) H(26) 2.978 ? . 1_655 O(5) H(28) 3.320 ? . 1_655 O(5) H(29) 2.958 ? . 1_655 O(6) H(2) 3.27(6) ? . 4_564 O(6) H(16) 3.44(6) ? . 3_765 O(6) H(18) 2.79(6) ? . 3_765 O(6) H(26) 2.896 ? . 1_655 O(7) H(10) 2.57(5) ? . 2_755 O(7) H(11) 2.74(6) ? . 2_755 O(7) H(12) 3.16(9) ? . 3_765 O(7) H(15) 3.47(6) ? . 2_755 O(7) H(18) 2.62(6) ? . 3_765 O(7) H(25) 3.170 ? . 1_655 O(7) H(26) 2.715 ? . 1_655 O(7) H(29) 3.148 ? . 1_655 O(8) H(8) 2.56(6) ? . 3_766 O(8) H(9) 3.29(6) ? . 3_766 O(8) H(19) 2.85(6) ? . 3_766 O(8) H(21) 3.55(7) ? . 3_766 O(8) H(26) 3.242 ? . 1_655 O(8) H(28) 2.811 ? . 1_655 O(9) H(1) 2.73(5) ? . 2_745 O(9) H(5) 2.90(6) ? . 2_745 O(9) H(7) 3.28(6) ? . 2_745 O(9) H(26) 2.929 ? . 1_655 O(9) H(27) 3.480 ? . 1_655 O(10) H(4) 3.23(7) ? . 3_766 O(10) H(5) 2.67(6) ? . 2_745 O(10) H(8) 3.07(6) ? . 3_766 O(10) H(22) 3.54(7) ? . 1_655 O(10) H(23) 3.13(7) ? . 1_655 O(10) H(24) 2.76(6) ? . 1_655 O(10) H(26) 3.108 ? . 1_655 O(10) H(27) 3.097 ? . 1_655 O(10) H(28) 3.287 ? . 1_655 O(11) H(2) 2.76(8) ? . 4_564 O(11) H(3) 2.94(8) ? . 4_564 O(11) H(13) 3.16(6) ? . 3_665 O(13) H(3) 3.31(9) ? . 4_564 O(13) H(10) 3.03(5) ? . 2_655 O(13) H(12) 3.11(7) ? . 3_665 O(13) H(13) 2.54(7) ? . 3_665 O(13) H(15) 3.35(7) ? . 2_655 O(13) H(20) 3.28(7) ? . 2_655 O(13) H(23) 2.78(7) ? . 2_655 O(15) H(3) 3.48(8) ? . 3_766 O(15) H(4) 2.53(5) ? . 3_766 O(15) H(5) 3.38(6) ? . 2_745 O(15) H(6) 3.23(8) ? . 2_745 O(15) H(8) 2.95(6) ? . 3_766 O(15) H(9) 3.09(5) ? . 3_766 N(1) H(9) 3.16(6) ? . 3_766 N(3) H(2) 3.59(6) ? . 4_564 N(3) H(10) 3.46(6) ? . 2_755 N(3) H(11) 3.32(6) ? . 2_755 N(3) H(18) 3.04(6) ? . 3_765 N(3) H(25) 3.575 ? . 1_655 N(3) H(26) 2.569 ? . 1_655 N(3) H(29) 3.255 ? . 1_655 N(4) H(1) 3.59(5) ? . 2_745 N(4) H(5) 3.04(6) ? . 2_745 N(4) H(8) 3.13(6) ? . 3_766 N(4) H(26) 2.831 ? . 1_655 N(4) H(27) 3.354 ? . 1_655 N(4) H(28) 3.239 ? . 1_655 N(5) H(3) 3.52(9) ? . 4_564 N(5) H(12) 3.43(7) ? . 3_665 N(5) H(13) 3.04(6) ? . 3_665 C(1) H(9) 2.95(5) ? . 3_766 C(1) H(21) 3.26(7) ? . 3_766 C(2) H(21) 3.01(6) ? . 3_766 C(3) H(14) 3.46(7) ? . 2_655 C(3) H(21) 3.26(7) ? . 3_766 C(4) H(13) 3.13(7) ? . 2_655 C(4) H(14) 3.24(6) ? . 2_655 C(4) H(16) 3.30(6) ? . 4_565 C(5) H(11) 3.47(6) ? . 3_766 C(5) H(13) 3.18(7) ? . 2_655 C(5) H(14) 3.51(6) ? . 2_655 C(6) H(9) 2.92(5) ? . 3_766 C(7) H(9) 3.02(6) ? . 3_766 C(7) H(22) 3.36(9) ? . 3_666 C(12) H(7) 3.14(6) ? . 2_745 C(14) H(17) 2.88(7) ? . 3_665 C(14) H(20) 3.14(8) ? . 4_554 C(15) H(2) 3.38(7) ? . 2_645 C(15) H(17) 2.92(6) ? . 3_665 C(15) H(20) 2.65(9) ? . 4_554 C(16) H(20) 3.15(9) ? . 4_554 C(16) H(29) 3.506 ? . 2_645 C(16) H(30) 3.303 ? . 2_645 C(17) H(7) 3.24(6) ? . 2_745 C(18) H(7) 3.49(6) ? . 2_745 C(18) H(29) 3.326 ? . 2_645 C(19) H(2) 3.10(7) ? . 4_564 C(19) H(25) 3.319 ? . 3_665 C(19) H(26) 3.524 ? . 3_665 C(20) H(13) 3.52(7) ? . 4_555 C(20) H(28) 3.183 ? . 3_666 C(21) H(4) 3.48(6) ? . 3_666 C(21) H(22) 3.17(7) ? . 3_666 C(23) H(17) 3.23(6) ? . 3_665 C(23) H(18) 3.46(5) ? . 3_665 C(24) H(14) 2.96(7) ? . 2_655 C(24) H(15) 3.23(6) ? . 2_655 C(24) H(19) 3.17(7) ? . 3_666 H(1) O(9) 2.73(5) ? . 2_755 H(1) N(4) 3.59(5) ? . 2_755 H(1) H(21) 3.53(8) ? . 3_766 H(2) O(6) 3.27(6) ? . 4_565 H(2) O(11) 2.76(8) ? . 4_565 H(2) N(3) 3.59(6) ? . 4_565 H(2) C(15) 3.38(7) ? . 2_655 H(2) C(19) 3.10(7) ? . 4_565 H(2) H(13) 2.86(10) ? . 2_655 H(2) H(14) 3.46(9) ? . 2_655 H(2) H(16) 2.30(9) ? . 4_565 H(2) H(17) 3.03(10) ? . 4_565 H(3) O(11) 2.94(8) ? . 4_565 H(3) O(13) 3.31(9) ? . 4_565 H(3) O(15) 3.48(7) ? . 3_766 H(3) N(5) 3.52(9) ? . 4_565 H(3) H(6) 3.29(11) ? . 4_565 H(3) H(11) 3.60(10) ? . 3_766 H(3) H(13) 3.01(10) ? . 2_655 H(3) H(23) 3.22(12) ? . 3_666 H(4) O(10) 3.23(7) ? . 3_766 H(4) O(15) 2.53(5) ? . 3_766 H(4) C(21) 3.48(6) ? . 3_666 H(4) H(9) 3.52(9) ? . 3_766 H(4) H(22) 2.89(10) ? . 3_666 H(4) H(23) 3.17(10) ? . 3_666 H(5) O(9) 2.90(6) ? . 2_755 H(5) O(10) 2.67(6) ? . 2_755 H(5) O(15) 3.38(6) ? . 2_755 H(5) N(4) 3.04(6) ? . 2_755 H(6) O(15) 3.23(8) ? . 2_755 H(6) H(3) 3.29(11) ? . 4_564 H(6) H(11) 3.26(12) ? . 2_755 H(7) O(2) 3.33(6) ? . 2_755 H(7) O(9) 3.28(6) ? . 2_755 H(7) C(12) 3.14(6) ? . 2_755 H(7) C(17) 3.24(6) ? . 2_755 H(7) C(18) 3.49(6) ? . 2_755 H(7) H(21) 3.19(9) ? . 3_766 H(8) O(8) 2.56(6) ? . 3_766 H(8) O(10) 3.07(6) ? . 3_766 H(8) O(15) 2.95(5) ? . 3_766 H(8) N(4) 3.13(6) ? . 3_766 H(8) H(22) 3.36(9) ? . 3_666 H(8) H(28) 3.560 ? . 3_666 H(9) V(1) 3.54(5) ? . 3_766 H(9) O(1) 3.05(5) ? . 3_766 H(9) O(8) 3.29(6) ? . 3_766 H(9) O(15) 3.09(5) ? . 3_766 H(9) N(1) 3.16(6) ? . 3_766 H(9) C(1) 2.95(5) ? . 3_766 H(9) C(6) 2.92(5) ? . 3_766 H(9) C(7) 3.02(6) ? . 3_766 H(9) H(4) 3.52(9) ? . 3_766 H(10) O(7) 2.57(5) ? . 2_745 H(10) O(13) 3.03(5) ? . 2_645 H(10) N(3) 3.46(6) ? . 2_745 H(10) H(29) 3.583 ? . 2_645 H(11) O(5) 3.50(6) ? . 2_745 H(11) O(7) 2.74(6) ? . 2_745 H(11) N(3) 3.32(6) ? . 2_745 H(11) C(5) 3.47(6) ? . 3_766 H(11) H(3) 3.60(10) ? . 3_766 H(11) H(6) 3.26(12) ? . 2_745 H(12) O(7) 3.16(9) ? . 3_765 H(12) O(13) 3.11(7) ? . 3_665 H(12) N(5) 3.43(7) ? . 3_665 H(12) H(12) 3.51(11) ? . 3_665 H(12) H(17) 2.81(11) ? . 3_665 H(12) H(20) 3.43(11) ? . 4_554 H(12) H(25) 2.779 ? . 3_665 H(13) O(11) 3.16(6) ? . 3_665 H(13) O(13) 2.54(7) ? . 3_665 H(13) N(5) 3.04(6) ? . 3_665 H(13) C(4) 3.13(7) ? . 2_645 H(13) C(5) 3.18(7) ? . 2_645 H(13) C(20) 3.52(7) ? . 4_554 H(13) H(2) 2.86(10) ? . 2_645 H(13) H(3) 3.01(10) ? . 2_645 H(13) H(17) 2.95(9) ? . 3_665 H(13) H(20) 2.52(11) ? . 4_554 H(13) H(23) 3.53(10) ? . 4_554 H(14) C(3) 3.46(7) ? . 2_645 H(14) C(4) 3.24(6) ? . 2_645 H(14) C(5) 3.51(6) ? . 2_645 H(14) C(24) 2.96(7) ? . 2_645 H(14) H(2) 3.46(9) ? . 2_645 H(14) H(20) 3.41(12) ? . 4_554 H(14) H(28) 3.169 ? . 2_645 H(14) H(29) 2.803 ? . 2_645 H(14) H(30) 2.454 ? . 2_645 H(15) O(5) 3.54(6) ? . 2_745 H(15) O(7) 3.47(6) ? . 2_745 H(15) O(13) 3.35(7) ? . 2_645 H(15) C(24) 3.23(6) ? . 2_645 H(15) H(29) 2.438 ? . 2_645 H(15) H(30) 3.262 ? . 2_645 H(16) O(6) 3.44(6) ? . 3_765 H(16) C(4) 3.30(6) ? . 4_564 H(16) H(2) 2.30(9) ? . 4_564 H(17) C(14) 2.88(7) ? . 3_665 H(17) C(15) 2.92(6) ? . 3_665 H(17) C(23) 3.23(6) ? . 3_665 H(17) H(2) 3.03(10) ? . 4_564 H(17) H(12) 2.81(11) ? . 3_665 H(17) H(13) 2.95(9) ? . 3_665 H(17) H(25) 2.764 ? . 3_665 H(17) H(26) 3.318 ? . 3_665 H(17) H(27) 3.091 ? . 3_665 H(18) O(6) 2.79(6) ? . 3_765 H(18) O(7) 2.62(6) ? . 3_765 H(18) N(3) 3.04(6) ? . 3_765 H(18) C(23) 3.46(5) ? . 3_665 H(18) H(25) 3.094 ? . 3_665 H(18) H(26) 3.112 ? . 3_665 H(19) O(8) 2.85(6) ? . 3_766 H(19) C(24) 3.17(7) ? . 3_666 H(19) H(28) 2.302 ? . 3_666 H(19) H(29) 3.527 ? . 3_666 H(19) H(30) 3.373 ? . 3_666 H(20) O(13) 3.28(7) ? . 2_645 H(20) C(14) 3.14(8) ? . 4_555 H(20) C(15) 2.65(9) ? . 4_555 H(20) C(16) 3.15(9) ? . 4_555 H(20) H(12) 3.43(11) ? . 4_555 H(20) H(13) 2.52(11) ? . 4_555 H(20) H(14) 3.41(12) ? . 4_555 H(20) H(28) 3.389 ? . 3_666 H(21) O(3) 3.43(6) ? . 3_766 H(21) O(8) 3.55(7) ? . 3_766 H(21) C(1) 3.26(7) ? . 3_766 H(21) C(2) 3.01(6) ? . 3_766 H(21) C(3) 3.26(7) ? . 3_766 H(21) H(1) 3.53(8) ? . 3_766 H(21) H(7) 3.19(9) ? . 3_766 H(22) O(10) 3.54(7) ? . 1_455 H(22) C(7) 3.36(8) ? . 3_666 H(22) C(21) 3.17(7) ? . 3_666 H(22) H(4) 2.89(10) ? . 3_666 H(22) H(8) 3.36(9) ? . 3_666 H(22) H(22) 2.39(10) ? . 3_666 H(22) H(24) 2.97(10) ? . 3_666 H(22) H(28) 3.414 ? . 3_666 H(23) O(10) 3.13(7) ? . 1_455 H(23) O(13) 2.78(7) ? . 2_645 H(23) H(3) 3.22(12) ? . 3_666 H(23) H(4) 3.17(10) ? . 3_666 H(23) H(13) 3.53(10) ? . 4_555 H(24) O(10) 2.76(6) ? . 1_455 H(24) H(22) 2.97(10) ? . 3_666 H(25) O(7) 3.170 ? . 1_455 H(25) N(3) 3.575 ? . 1_455 H(25) C(19) 3.319 ? . 3_665 H(25) H(12) 2.779 ? . 3_665 H(25) H(17) 2.764 ? . 3_665 H(25) H(18) 3.094 ? . 3_665 H(26) O(5) 2.978 ? . 1_455 H(26) O(6) 2.896 ? . 1_455 H(26) O(7) 2.715 ? . 1_455 H(26) O(8) 3.242 ? . 1_455 H(26) O(9) 2.929 ? . 1_455 H(26) O(10) 3.108 ? . 1_455 H(26) N(3) 2.569 ? . 1_455 H(26) N(4) 2.831 ? . 1_455 H(26) C(19) 3.524 ? . 3_665 H(26) H(17) 3.318 ? . 3_665 H(26) H(18) 3.112 ? . 3_665 H(27) O(9) 3.480 ? . 1_455 H(27) O(10) 3.097 ? . 1_455 H(27) N(4) 3.354 ? . 1_455 H(27) H(17) 3.091 ? . 3_665 H(28) O(5) 3.320 ? . 1_455 H(28) O(8) 2.811 ? . 1_455 H(28) O(10) 3.287 ? . 1_455 H(28) N(4) 3.239 ? . 1_455 H(28) C(20) 3.183 ? . 3_666 H(28) H(8) 3.560 ? . 3_666 H(28) H(14) 3.169 ? . 2_655 H(28) H(19) 2.302 ? . 3_666 H(28) H(20) 3.389 ? . 3_666 H(28) H(22) 3.414 ? . 3_666 H(29) O(5) 2.958 ? . 1_455 H(29) O(7) 3.148 ? . 1_455 H(29) N(3) 3.255 ? . 1_455 H(29) C(16) 3.506 ? . 2_655 H(29) C(18) 3.326 ? . 2_655 H(29) H(10) 3.583 ? . 2_655 H(29) H(14) 2.803 ? . 2_655 H(29) H(15) 2.438 ? . 2_655 H(29) H(19) 3.527 ? . 3_666 H(30) C(16) 3.303 ? . 2_655 H(30) H(14) 2.454 ? . 2_655 H(30) H(15) 3.262 ? . 2_655 H(30) H(19) 3.373 ? . 3_666 Ho(1) V(1) 3.4785(10) ? . . data___ErVO _database_code_depnum_ccdc_archive 'CCDC 881978' #TrackingRef '11262_web_deposit_cif_file_7_TakayukiIshida_1336987557.ErV_CIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 Er N5 O15 V ' _chemical_formula_moiety 'C24 H30 Er N5 O15 V ' _chemical_formula_weight 846.73 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.903(3) _cell_length_b 17.515(4) _cell_length_c 18.236(8) _cell_angle_alpha 90.0000 _cell_angle_beta 105.452(4) _cell_angle_gamma 90.0000 _cell_volume 3048.8(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 412 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 90. #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680.00 _exptl_absorpt_coefficient_mu 3.115 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 0.536 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 51925 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_ambient_temperature 90. #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6981 _reflns_number_gt 6525 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0292 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6981 _refine_ls_number_parameters 517 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.93 _refine_diff_density_min -0.68 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Er Er -0.259 4.958 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; V V 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Er(1) Er 0.926370(10) 0.573110(10) 0.203740(10) 0.01028(3) Uani 1.00 1 d . . . V(1) V 0.83853(5) 0.46958(3) 0.34706(3) 0.00934(10) Uani 1.00 1 d . . . O(1) O 0.87634(19) 0.57709(10) 0.32450(11) 0.0104(4) Uani 1.00 1 d . . . O(2) O 0.81416(19) 0.46337(10) 0.23545(10) 0.0114(4) Uani 1.00 1 d . . . O(3) O 0.9275(2) 0.70495(11) 0.26511(11) 0.0138(4) Uani 1.00 1 d . . . O(4) O 0.78705(19) 0.49385(11) 0.09403(10) 0.0127(4) Uani 1.00 1 d . . . O(5) O 1.1153(2) 0.65688(13) 0.18573(12) 0.0237(5) Uani 1.00 1 d . . . O(6) O 1.0379(2) 0.57374(12) 0.09855(14) 0.0265(6) Uani 1.00 1 d . . . O(7) O 1.2018(2) 0.65273(13) 0.08777(14) 0.0296(6) Uani 1.00 1 d . . . O(8) O 1.1390(2) 0.54758(13) 0.30232(12) 0.0228(5) Uani 1.00 1 d . . . O(9) O 1.0848(2) 0.46222(12) 0.21518(13) 0.0236(5) Uani 1.00 1 d . . . O(10) O 1.2644(2) 0.44385(14) 0.31370(15) 0.0317(6) Uani 1.00 1 d . . . O(11) O 0.7992(2) 0.66373(11) 0.10816(11) 0.0152(4) Uani 1.00 1 d . . . O(12) O 0.68541(19) 0.61521(11) 0.18286(11) 0.0149(4) Uani 1.00 1 d . . . O(13) O 0.5913(2) 0.70775(13) 0.10575(12) 0.0255(5) Uani 1.00 1 d . . . O(14) O 0.6055(2) 0.51242(11) 0.30041(11) 0.0149(4) Uani 1.00 1 d . . . O(15) O 0.9879(2) 0.43141(11) 0.38129(11) 0.0144(4) Uani 1.00 1 d . . . N(1) N 0.8048(2) 0.50188(13) 0.45000(12) 0.0106(5) Uani 1.00 1 d . . . N(2) N 0.7293(2) 0.36883(13) 0.34529(13) 0.0117(5) Uani 1.00 1 d . . . N(3) N 1.1209(2) 0.62895(14) 0.12266(15) 0.0180(6) Uani 1.00 1 d . . . N(4) N 1.1661(2) 0.48280(15) 0.27831(15) 0.0195(6) Uani 1.00 1 d . . . N(5) N 0.6881(2) 0.66372(14) 0.13125(13) 0.0161(5) Uani 1.00 1 d . . . C(1) C 0.8599(2) 0.64035(15) 0.36208(15) 0.0108(6) Uani 1.00 1 d . . . C(2) C 0.8869(2) 0.71100(16) 0.33200(15) 0.0125(6) Uani 1.00 1 d . . . C(3) C 0.8750(3) 0.77891(16) 0.36811(18) 0.0173(7) Uani 1.00 1 d . . . C(4) C 0.8363(3) 0.77821(17) 0.43639(18) 0.0203(7) Uani 1.00 1 d . . . C(5) C 0.8082(3) 0.71026(17) 0.46669(17) 0.0162(7) Uani 1.00 1 d . . . C(6) C 0.8195(2) 0.64006(15) 0.43085(15) 0.0118(6) Uani 1.00 1 d . . . C(7) C 0.7972(2) 0.57144(16) 0.47090(16) 0.0123(6) Uani 1.00 1 d . . . C(8) C 0.9512(3) 0.77777(17) 0.23178(19) 0.0199(7) Uani 1.00 1 d . . . C(9) C 0.8035(3) 0.44260(17) 0.50719(16) 0.0145(6) Uani 1.00 1 d . . . C(10) C 0.7039(2) 0.37546(16) 0.47968(16) 0.0140(6) Uani 1.00 1 d . . . C(11) C 0.7430(3) 0.32869(16) 0.41787(17) 0.0155(6) Uani 1.00 1 d . . . C(12) C 0.7203(2) 0.42092(15) 0.18601(16) 0.0114(6) Uani 1.00 1 d . . . C(13) C 0.7013(2) 0.43644(15) 0.10826(16) 0.0124(6) Uani 1.00 1 d . . . C(14) C 0.6024(2) 0.39774(17) 0.05289(17) 0.0158(6) Uani 1.00 1 d . . . C(15) C 0.5194(2) 0.34212(17) 0.07404(17) 0.0172(7) Uani 1.00 1 d . . . C(16) C 0.5387(3) 0.32432(17) 0.14928(17) 0.0176(7) Uani 1.00 1 d . . . C(17) C 0.6403(2) 0.36228(15) 0.20679(16) 0.0139(6) Uani 1.00 1 d . . . C(18) C 0.6569(2) 0.33704(16) 0.28434(17) 0.0149(6) Uani 1.00 1 d . . . C(19) C 0.7716(3) 0.50989(19) 0.01397(17) 0.0199(7) Uani 1.00 1 d . . . C(20) C 0.7228(3) 0.32184(19) 0.54827(18) 0.0225(8) Uani 1.00 1 d . . . C(21) C 0.5517(3) 0.40244(19) 0.45321(19) 0.0191(7) Uani 1.00 1 d . . . C(22) C 0.5047(2) 0.54813(17) 0.26367(16) 0.0141(6) Uani 1.00 1 d . . . C(23) C 0.4169(3) 0.5206(2) 0.18834(17) 0.0240(8) Uani 1.00 1 d . . . C(24) C 0.4660(3) 0.62320(18) 0.29068(19) 0.0256(8) Uani 1.00 1 d . . . H(1) H 0.891(2) 0.8218(17) 0.3491(16) 0.010(7) Uiso 1.00 1 d . . . H(2) H 0.832(3) 0.8265(18) 0.4610(18) 0.021(8) Uiso 1.00 1 d . . . H(3) H 0.784(3) 0.7067(18) 0.5110(18) 0.022(8) Uiso 1.00 1 d . . . H(4) H 0.782(2) 0.5784(15) 0.5182(17) 0.010(7) Uiso 1.00 1 d . . . H(5) H 0.865(3) 0.8093(16) 0.2235(16) 0.011(7) Uiso 1.00 1 d . . . H(6) H 0.978(4) 0.765(2) 0.189(2) 0.046(12) Uiso 1.00 1 d . . . H(7) H 1.039(3) 0.798(2) 0.272(2) 0.033(10) Uiso 1.00 1 d . . . H(8) H 0.782(3) 0.4671(18) 0.5501(18) 0.019(8) Uiso 1.00 1 d . . . H(9) H 0.891(3) 0.4235(15) 0.5224(17) 0.010(7) Uiso 1.00 1 d . . . H(10) H 0.690(3) 0.2835(17) 0.4086(16) 0.010(7) Uiso 1.00 1 d . . . H(11) H 0.839(3) 0.3123(18) 0.4339(18) 0.024(9) Uiso 1.00 1 d . . . H(12) H 0.590(3) 0.4073(19) 0.005(2) 0.026(9) Uiso 1.00 1 d . . . H(13) H 0.455(3) 0.3169(18) 0.0399(18) 0.022(8) Uiso 1.00 1 d . . . H(14) H 0.487(3) 0.2858(17) 0.1614(17) 0.015(8) Uiso 1.00 1 d . . . H(15) H 0.608(3) 0.2919(18) 0.2878(17) 0.017(8) Uiso 1.00 1 d . . . H(16) H 0.834(3) 0.5471(19) 0.0134(17) 0.016(8) Uiso 1.00 1 d . . . H(17) H 0.678(4) 0.528(2) -0.010(2) 0.043(11) Uiso 1.00 1 d . . . H(18) H 0.786(3) 0.463(2) -0.013(2) 0.034(10) Uiso 1.00 1 d . . . H(19) H 0.709(3) 0.347(2) 0.592(2) 0.040(11) Uiso 1.00 1 d . . . H(20) H 0.661(3) 0.278(2) 0.535(2) 0.036(10) Uiso 1.00 1 d . . . H(21) H 0.817(3) 0.301(2) 0.564(2) 0.031(10) Uiso 1.00 1 d . . . H(22) H 0.524(3) 0.4297(19) 0.495(2) 0.033(10) Uiso 1.00 1 d . . . H(23) H 0.496(3) 0.3624(19) 0.4390(18) 0.021(8) Uiso 1.00 1 d . . . H(24) H 0.533(3) 0.436(2) 0.412(2) 0.033(10) Uiso 1.00 1 d . . . H(25) H 0.4442 0.4791 0.1697 0.029 Uiso 1.00 1 c R . . H(26) H 0.4199 0.5583 0.1483 0.029 Uiso 1.00 1 c R . . H(27) H 0.3247 0.5225 0.1892 0.028 Uiso 1.00 1 c R . . H(28) H 0.3760 0.6262 0.2877 0.030 Uiso 1.00 1 c R . . H(29) H 0.4751 0.6623 0.2545 0.030 Uiso 1.00 1 c R . . H(30) H 0.5225 0.6362 0.3406 0.030 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er(1) 0.01120(7) 0.01042(7) 0.00975(7) 0.00013(4) 0.00371(5) 0.00054(4) V(1) 0.0097(2) 0.0095(2) 0.0083(2) -0.00064(16) 0.00144(17) 0.00032(17) O(1) 0.0141(9) 0.0086(9) 0.0095(9) -0.0010(6) 0.0048(7) -0.0009(6) O(2) 0.0124(8) 0.0112(9) 0.0102(9) -0.0021(7) 0.0022(7) -0.0009(7) O(3) 0.0199(9) 0.0105(9) 0.0129(9) -0.0004(7) 0.0079(8) 0.0008(7) O(4) 0.0144(9) 0.0148(9) 0.0086(9) -0.0026(7) 0.0026(7) -0.0006(7) O(5) 0.0190(10) 0.0317(12) 0.0230(11) -0.0062(9) 0.0103(9) -0.0054(9) O(6) 0.0308(13) 0.0236(12) 0.0332(13) -0.0085(9) 0.0226(11) -0.0079(9) O(7) 0.0360(13) 0.0205(11) 0.0456(15) -0.0014(10) 0.0340(12) 0.0076(10) O(8) 0.0192(10) 0.0295(12) 0.0170(11) 0.0051(9) 0.0002(8) -0.0006(9) O(9) 0.0149(10) 0.0209(11) 0.0316(12) 0.0052(8) 0.0000(9) -0.0058(9) O(10) 0.0146(10) 0.0355(13) 0.0422(15) 0.0092(10) 0.0027(10) 0.0174(11) O(11) 0.0185(9) 0.0161(10) 0.0122(9) 0.0012(8) 0.0061(7) 0.0023(7) O(12) 0.0150(9) 0.0184(10) 0.0116(9) 0.0016(7) 0.0038(7) 0.0044(8) O(13) 0.0263(11) 0.0274(12) 0.0209(11) 0.0169(9) 0.0029(9) 0.0056(9) O(14) 0.0128(9) 0.0165(10) 0.0154(10) 0.0027(7) 0.0035(7) 0.0060(7) O(15) 0.0114(9) 0.0168(10) 0.0141(10) 0.0008(7) 0.0017(7) 0.0028(7) N(1) 0.0093(10) 0.0139(11) 0.0080(10) -0.0019(8) 0.0012(8) 0.0009(8) N(2) 0.0123(10) 0.0098(10) 0.0141(11) 0.0001(8) 0.0053(8) 0.0015(8) N(3) 0.0199(12) 0.0121(11) 0.0251(13) 0.0057(9) 0.0112(10) 0.0063(10) N(4) 0.0117(11) 0.0231(13) 0.0262(14) 0.0021(9) 0.0092(10) 0.0102(11) N(5) 0.0199(12) 0.0153(12) 0.0121(11) 0.0015(9) 0.0028(9) -0.0010(9) C(1) 0.0085(11) 0.0131(12) 0.0095(12) -0.0001(9) -0.0001(9) -0.0028(10) C(2) 0.0113(12) 0.0143(13) 0.0118(13) 0.0003(10) 0.0028(10) -0.0002(10) C(3) 0.0211(14) 0.0089(13) 0.0229(15) -0.0013(11) 0.0075(12) -0.0003(11) C(4) 0.0278(16) 0.0137(14) 0.0222(16) 0.0032(12) 0.0115(13) -0.0041(11) C(5) 0.0175(13) 0.0181(14) 0.0142(14) 0.0035(11) 0.0063(11) -0.0034(11) C(6) 0.0088(11) 0.0139(13) 0.0114(12) 0.0015(9) 0.0005(9) -0.0008(10) C(7) 0.0077(12) 0.0204(14) 0.0080(12) -0.0004(9) 0.0009(10) 0.0005(10) C(8) 0.0317(17) 0.0125(14) 0.0191(15) -0.0030(12) 0.0128(13) 0.0019(11) C(9) 0.0146(13) 0.0179(13) 0.0109(13) -0.0011(11) 0.0030(11) 0.0038(11) C(10) 0.0153(13) 0.0150(13) 0.0122(13) -0.0032(10) 0.0044(10) 0.0038(10) C(11) 0.0186(14) 0.0124(13) 0.0160(14) -0.0003(11) 0.0055(11) 0.0053(11) C(12) 0.0114(12) 0.0123(12) 0.0104(13) 0.0029(9) 0.0027(10) -0.0023(9) C(13) 0.0131(12) 0.0127(12) 0.0122(13) 0.0030(10) 0.0050(10) -0.0003(10) C(14) 0.0166(13) 0.0187(14) 0.0112(13) 0.0034(11) 0.0020(11) -0.0030(11) C(15) 0.0148(13) 0.0191(14) 0.0166(14) -0.0018(11) 0.0023(11) -0.0079(11) C(16) 0.0170(13) 0.0162(14) 0.0189(15) -0.0042(11) 0.0037(11) -0.0043(11) C(17) 0.0147(12) 0.0111(12) 0.0159(13) -0.0002(10) 0.0040(10) -0.0019(10) C(18) 0.0161(13) 0.0117(13) 0.0187(14) -0.0039(10) 0.0075(11) 0.0009(11) C(19) 0.0293(17) 0.0208(15) 0.0100(13) -0.0014(13) 0.0058(12) 0.0012(11) C(20) 0.0310(17) 0.0212(16) 0.0167(15) -0.0033(13) 0.0085(13) 0.0059(12) C(21) 0.0148(14) 0.0199(15) 0.0228(16) -0.0044(12) 0.0055(12) -0.0002(13) C(22) 0.0118(12) 0.0185(14) 0.0134(13) -0.0008(10) 0.0057(10) 0.0036(11) C(23) 0.0160(14) 0.0361(19) 0.0187(15) 0.0041(12) 0.0022(12) -0.0086(13) C(24) 0.0200(15) 0.0253(16) 0.0293(18) 0.0071(12) 0.0029(13) -0.0053(14) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Er(1) O(1) 2.384(2) yes . . Er(1) O(2) 2.3677(18) yes . . Er(1) O(3) 2.5649(19) yes . . Er(1) O(4) 2.5224(17) yes . . Er(1) O(5) 2.467(2) yes . . Er(1) O(6) 2.455(2) yes . . Er(1) O(8) 2.4183(18) yes . . Er(1) O(9) 2.471(2) yes . . Er(1) O(11) 2.4441(18) yes . . Er(1) O(12) 2.4287(18) yes . . V(1) O(1) 1.9843(18) yes . . V(1) O(2) 1.9877(19) yes . . V(1) O(14) 2.3594(19) yes . . V(1) O(15) 1.5914(19) yes . . V(1) N(1) 2.071(2) yes . . V(1) N(2) 2.066(2) yes . . O(1) C(1) 1.336(3) yes . . O(2) C(12) 1.335(2) yes . . O(3) C(2) 1.386(3) yes . . O(3) C(8) 1.459(3) yes . . O(4) C(13) 1.385(3) yes . . O(4) C(19) 1.454(3) yes . . O(5) N(3) 1.265(3) yes . . O(6) N(3) 1.270(3) yes . . O(7) N(3) 1.221(3) yes . . O(8) N(4) 1.270(3) yes . . O(9) N(4) 1.268(3) yes . . O(10) N(4) 1.223(3) yes . . O(11) N(5) 1.279(3) yes . . O(12) N(5) 1.273(3) yes . . O(13) N(5) 1.222(3) yes . . O(14) C(22) 1.216(3) yes . . N(1) C(7) 1.285(3) yes . . N(1) C(9) 1.474(3) yes . . N(2) C(11) 1.473(3) yes . . N(2) C(18) 1.279(3) yes . . C(1) C(2) 1.408(3) yes . . C(1) C(6) 1.414(4) yes . . C(2) C(3) 1.380(4) yes . . C(3) C(4) 1.397(5) yes . . C(4) C(5) 1.372(4) yes . . C(5) C(6) 1.411(4) yes . . C(6) C(7) 1.454(3) yes . . C(9) C(10) 1.531(3) yes . . C(10) C(11) 1.525(4) yes . . C(10) C(20) 1.535(4) yes . . C(10) C(21) 1.530(3) yes . . C(12) C(13) 1.406(4) yes . . C(12) C(17) 1.409(4) yes . . C(13) C(14) 1.382(3) yes . . C(14) C(15) 1.394(4) yes . . C(15) C(16) 1.370(4) yes . . C(16) C(17) 1.412(3) yes . . C(17) C(18) 1.449(4) yes . . C(22) C(23) 1.496(3) yes . . C(22) C(24) 1.490(4) yes . . C(3) H(1) 0.86(3) no . . C(4) H(2) 0.96(3) no . . C(5) H(3) 0.90(3) no . . C(7) H(4) 0.92(3) no . . C(8) H(5) 0.99(2) no . . C(8) H(6) 0.92(4) no . . C(8) H(7) 1.03(3) no . . C(9) H(8) 0.97(3) no . . C(9) H(9) 0.90(2) no . . C(11) H(10) 0.94(2) no . . C(11) H(11) 0.96(3) no . . C(14) H(12) 0.86(3) no . . C(15) H(13) 0.88(2) no . . C(16) H(14) 0.91(3) no . . C(18) H(15) 0.94(3) no . . C(19) H(16) 0.90(3) no . . C(19) H(17) 0.96(3) no . . C(19) H(18) 0.98(3) no . . C(20) H(19) 0.96(4) no . . C(20) H(20) 0.97(3) no . . C(20) H(21) 0.97(3) no . . C(21) H(22) 1.00(4) no . . C(21) H(23) 0.89(3) no . . C(21) H(24) 0.93(3) no . . C(23) H(25) 0.876 no . . C(23) H(26) 0.991 no . . C(23) H(27) 0.919 no . . C(24) H(28) 0.880 no . . C(24) H(29) 0.972 no . . C(24) H(30) 0.959 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Er(1) O(2) 64.63(6) yes . . . O(1) Er(1) O(3) 63.15(6) yes . . . O(1) Er(1) O(4) 122.99(6) yes . . . O(1) Er(1) O(5) 117.21(6) yes . . . O(1) Er(1) O(6) 165.74(6) yes . . . O(1) Er(1) O(8) 70.90(7) yes . . . O(1) Er(1) O(9) 103.22(7) yes . . . O(1) Er(1) O(11) 116.45(6) yes . . . O(1) Er(1) O(12) 72.46(6) yes . . . O(2) Er(1) O(3) 124.89(6) yes . . . O(2) Er(1) O(4) 63.50(6) yes . . . O(2) Er(1) O(5) 159.57(6) yes . . . O(2) Er(1) O(6) 122.18(6) yes . . . O(2) Er(1) O(8) 92.33(6) yes . . . O(2) Er(1) O(9) 70.74(6) yes . . . O(2) Er(1) O(11) 121.01(6) yes . . . O(2) Er(1) O(12) 77.25(6) yes . . . O(3) Er(1) O(4) 141.21(5) yes . . . O(3) Er(1) O(5) 66.89(7) yes . . . O(3) Er(1) O(6) 112.73(6) yes . . . O(3) Er(1) O(8) 86.59(6) yes . . . O(3) Er(1) O(9) 137.92(6) yes . . . O(3) Er(1) O(11) 70.61(6) yes . . . O(3) Er(1) O(12) 71.63(6) yes . . . O(4) Er(1) O(5) 119.71(6) yes . . . O(4) Er(1) O(6) 69.37(6) yes . . . O(4) Er(1) O(8) 132.20(6) yes . . . O(4) Er(1) O(9) 80.52(6) yes . . . O(4) Er(1) O(11) 73.90(6) yes . . . O(4) Er(1) O(12) 74.68(6) yes . . . O(5) Er(1) O(6) 51.58(7) yes . . . O(5) Er(1) O(8) 70.61(7) yes . . . O(5) Er(1) O(9) 89.52(7) yes . . . O(5) Er(1) O(11) 77.51(6) yes . . . O(5) Er(1) O(12) 123.14(6) yes . . . O(6) Er(1) O(8) 95.62(7) yes . . . O(6) Er(1) O(9) 70.23(7) yes . . . O(6) Er(1) O(11) 72.15(7) yes . . . O(6) Er(1) O(12) 120.25(6) yes . . . O(8) Er(1) O(9) 51.99(7) yes . . . O(8) Er(1) O(11) 146.24(7) yes . . . O(8) Er(1) O(12) 142.86(7) yes . . . O(9) Er(1) O(11) 139.97(7) yes . . . O(9) Er(1) O(12) 145.83(6) yes . . . O(11) Er(1) O(12) 52.63(7) yes . . . O(1) V(1) O(2) 79.50(7) yes . . . O(1) V(1) O(14) 81.02(7) yes . . . O(1) V(1) O(15) 105.84(9) yes . . . O(1) V(1) N(1) 90.78(9) yes . . . O(1) V(1) N(2) 159.14(7) yes . . . O(2) V(1) O(14) 78.93(7) yes . . . O(2) V(1) O(15) 103.02(9) yes . . . O(2) V(1) N(1) 159.74(8) yes . . . O(2) V(1) N(2) 90.98(8) yes . . . O(14) V(1) O(15) 173.07(9) yes . . . O(14) V(1) N(1) 82.04(7) yes . . . O(14) V(1) N(2) 78.94(7) yes . . . O(15) V(1) N(1) 96.70(9) yes . . . O(15) V(1) N(2) 94.32(9) yes . . . N(1) V(1) N(2) 92.14(9) yes . . . Er(1) O(1) V(1) 105.13(8) yes . . . Er(1) O(1) C(1) 125.61(16) yes . . . V(1) O(1) C(1) 128.71(18) yes . . . Er(1) O(2) V(1) 105.59(7) yes . . . Er(1) O(2) C(12) 125.07(16) yes . . . V(1) O(2) C(12) 126.49(18) yes . . . Er(1) O(3) C(2) 118.96(16) yes . . . Er(1) O(3) C(8) 126.00(18) yes . . . C(2) O(3) C(8) 114.6(2) yes . . . Er(1) O(4) C(13) 118.96(15) yes . . . Er(1) O(4) C(19) 125.38(16) yes . . . C(13) O(4) C(19) 115.0(2) yes . . . Er(1) O(5) N(3) 96.31(16) yes . . . Er(1) O(6) N(3) 96.75(19) yes . . . Er(1) O(8) N(4) 97.52(14) yes . . . Er(1) O(9) N(4) 95.06(16) yes . . . Er(1) O(11) N(5) 95.17(14) yes . . . Er(1) O(12) N(5) 96.04(15) yes . . . V(1) O(14) C(22) 160.4(2) yes . . . V(1) N(1) C(7) 124.3(2) yes . . . V(1) N(1) C(9) 118.86(17) yes . . . C(7) N(1) C(9) 116.5(2) yes . . . V(1) N(2) C(11) 118.11(16) yes . . . V(1) N(2) C(18) 123.8(2) yes . . . C(11) N(2) C(18) 118.0(2) yes . . . O(5) N(3) O(6) 115.3(2) yes . . . O(5) N(3) O(7) 122.4(2) yes . . . O(6) N(3) O(7) 122.2(2) yes . . . O(8) N(4) O(9) 115.2(2) yes . . . O(8) N(4) O(10) 121.9(2) yes . . . O(9) N(4) O(10) 122.9(2) yes . . . O(11) N(5) O(12) 115.6(2) yes . . . O(11) N(5) O(13) 122.1(2) yes . . . O(12) N(5) O(13) 122.3(2) yes . . . O(1) C(1) C(2) 117.9(2) yes . . . O(1) C(1) C(6) 123.7(2) yes . . . C(2) C(1) C(6) 118.5(2) yes . . . O(3) C(2) C(1) 113.9(2) yes . . . O(3) C(2) C(3) 124.6(2) yes . . . C(1) C(2) C(3) 121.5(2) yes . . . C(2) C(3) C(4) 119.8(2) yes . . . C(3) C(4) C(5) 120.0(2) yes . . . C(4) C(5) C(6) 121.3(3) yes . . . C(1) C(6) C(5) 118.9(2) yes . . . C(1) C(6) C(7) 124.4(2) yes . . . C(5) C(6) C(7) 116.5(2) yes . . . N(1) C(7) C(6) 127.3(2) yes . . . N(1) C(9) C(10) 115.8(2) yes . . . C(9) C(10) C(11) 112.7(2) yes . . . C(9) C(10) C(20) 106.0(2) yes . . . C(9) C(10) C(21) 111.1(2) yes . . . C(11) C(10) C(20) 105.9(2) yes . . . C(11) C(10) C(21) 110.8(2) yes . . . C(20) C(10) C(21) 110.0(2) yes . . . N(2) C(11) C(10) 115.3(2) yes . . . O(2) C(12) C(13) 117.1(2) yes . . . O(2) C(12) C(17) 124.3(2) yes . . . C(13) C(12) C(17) 118.6(2) yes . . . O(4) C(13) C(12) 113.9(2) yes . . . O(4) C(13) C(14) 124.7(2) yes . . . C(12) C(13) C(14) 121.4(2) yes . . . C(13) C(14) C(15) 119.7(2) yes . . . C(14) C(15) C(16) 120.1(2) yes . . . C(15) C(16) C(17) 121.2(2) yes . . . C(12) C(17) C(16) 119.0(2) yes . . . C(12) C(17) C(18) 124.0(2) yes . . . C(16) C(17) C(18) 117.0(2) yes . . . N(2) C(18) C(17) 127.4(2) yes . . . O(14) C(22) C(23) 122.1(2) yes . . . O(14) C(22) C(24) 121.2(2) yes . . . C(23) C(22) C(24) 116.7(2) yes . . . C(2) C(3) H(1) 121(2) no . . . C(4) C(3) H(1) 120(2) no . . . C(3) C(4) H(2) 118(2) no . . . C(5) C(4) H(2) 122(2) no . . . C(4) C(5) H(3) 123(2) no . . . C(6) C(5) H(3) 115(2) no . . . N(1) C(7) H(4) 116.1(17) no . . . C(6) C(7) H(4) 116.4(17) no . . . O(3) C(8) H(5) 108.9(18) no . . . O(3) C(8) H(6) 105(2) no . . . O(3) C(8) H(7) 101(2) no . . . H(5) C(8) H(6) 116(2) no . . . H(5) C(8) H(7) 116(2) no . . . H(6) C(8) H(7) 108(3) no . . . N(1) C(9) H(8) 107.9(18) no . . . N(1) C(9) H(9) 107(2) no . . . C(10) C(9) H(8) 110.1(19) no . . . C(10) C(9) H(9) 107.3(17) no . . . H(8) C(9) H(9) 108(2) no . . . N(2) C(11) H(10) 109.1(17) no . . . N(2) C(11) H(11) 105(2) no . . . C(10) C(11) H(10) 110(2) no . . . C(10) C(11) H(11) 111(2) no . . . H(10) C(11) H(11) 105(2) no . . . C(13) C(14) H(12) 122(2) no . . . C(15) C(14) H(12) 119(2) no . . . C(14) C(15) H(13) 122(2) no . . . C(16) C(15) H(13) 118(2) no . . . C(15) C(16) H(14) 118.4(18) no . . . C(17) C(16) H(14) 120.4(18) no . . . N(2) C(18) H(15) 119.3(18) no . . . C(17) C(18) H(15) 113.3(18) no . . . O(4) C(19) H(16) 105(2) no . . . O(4) C(19) H(17) 110(2) no . . . O(4) C(19) H(18) 110(2) no . . . H(16) C(19) H(17) 110(3) no . . . H(16) C(19) H(18) 114(3) no . . . H(17) C(19) H(18) 107(2) no . . . C(10) C(20) H(19) 113(2) no . . . C(10) C(20) H(20) 111(2) no . . . C(10) C(20) H(21) 112(2) no . . . H(19) C(20) H(20) 110(3) no . . . H(19) C(20) H(21) 105(2) no . . . H(20) C(20) H(21) 105(3) no . . . C(10) C(21) H(22) 110.7(19) no . . . C(10) C(21) H(23) 110(2) no . . . C(10) C(21) H(24) 115(2) no . . . H(22) C(21) H(23) 109(3) no . . . H(22) C(21) H(24) 106(3) no . . . H(23) C(21) H(24) 107(2) no . . . C(22) C(23) H(25) 117.4 no . . . C(22) C(23) H(26) 109.8 no . . . C(22) C(23) H(27) 108.1 no . . . H(25) C(23) H(26) 101.1 no . . . H(25) C(23) H(27) 116.6 no . . . H(26) C(23) H(27) 102.3 no . . . C(22) C(24) H(28) 112.2 no . . . C(22) C(24) H(29) 108.6 no . . . C(22) C(24) H(30) 112.8 no . . . H(28) C(24) H(29) 101.1 no . . . H(28) C(24) H(30) 111.7 no . . . H(29) C(24) H(30) 109.9 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Er(1) O(2) V(1) -16.59(6) ? . . . . O(1) Er(1) O(2) C(12) 145.3(2) ? . . . . O(2) Er(1) O(1) V(1) 16.58(6) ? . . . . O(2) Er(1) O(1) C(1) -155.46(19) ? . . . . O(1) Er(1) O(3) C(2) -5.64(14) ? . . . . O(1) Er(1) O(3) C(8) -177.8(2) ? . . . . O(3) Er(1) O(1) V(1) 178.34(9) ? . . . . O(3) Er(1) O(1) C(1) 6.29(16) ? . . . . O(1) Er(1) O(4) C(13) -16.28(19) ? . . . . O(1) Er(1) O(4) C(19) 154.0(2) ? . . . . O(4) Er(1) O(1) V(1) 42.87(9) ? . . . . O(4) Er(1) O(1) C(1) -129.18(17) ? . . . . O(1) Er(1) O(5) N(3) 170.45(13) ? . . . . O(5) Er(1) O(1) V(1) -140.69(7) ? . . . . O(5) Er(1) O(1) C(1) 47.27(19) ? . . . . O(1) Er(1) O(6) N(3) -42.2(3) ? . . . . O(6) Er(1) O(1) V(1) -105.2(2) ? . . . . O(6) Er(1) O(1) C(1) 82.8(3) ? . . . . O(1) Er(1) O(8) N(4) 122.43(18) ? . . . . O(8) Er(1) O(1) V(1) -85.65(8) ? . . . . O(8) Er(1) O(1) C(1) 102.31(18) ? . . . . O(1) Er(1) O(9) N(4) -49.54(18) ? . . . . O(9) Er(1) O(1) V(1) -44.31(8) ? . . . . O(9) Er(1) O(1) C(1) 143.65(17) ? . . . . O(1) Er(1) O(11) N(5) -32.34(15) ? . . . . O(11) Er(1) O(1) V(1) 130.22(7) ? . . . . O(11) Er(1) O(1) C(1) -41.82(19) ? . . . . O(1) Er(1) O(12) N(5) 141.83(15) ? . . . . O(12) Er(1) O(1) V(1) 100.48(8) ? . . . . O(12) Er(1) O(1) C(1) -71.56(17) ? . . . . O(2) Er(1) O(3) C(2) 14.53(18) ? . . . . O(2) Er(1) O(3) C(8) -157.64(18) ? . . . . O(3) Er(1) O(2) V(1) -36.50(10) ? . . . . O(3) Er(1) O(2) C(12) 125.37(19) ? . . . . O(2) Er(1) O(4) C(13) 10.27(16) ? . . . . O(2) Er(1) O(4) C(19) -179.5(2) ? . . . . O(4) Er(1) O(2) V(1) -172.07(10) ? . . . . O(4) Er(1) O(2) C(12) -10.20(19) ? . . . . O(2) Er(1) O(5) N(3) 80.5(2) ? . . . . O(5) Er(1) O(2) V(1) 83.6(2) ? . . . . O(5) Er(1) O(2) C(12) -114.6(2) ? . . . . O(2) Er(1) O(6) N(3) -157.04(13) ? . . . . O(6) Er(1) O(2) V(1) 149.09(7) ? . . . . O(6) Er(1) O(2) C(12) -49.0(2) ? . . . . O(2) Er(1) O(8) N(4) 60.33(18) ? . . . . O(8) Er(1) O(2) V(1) 50.96(9) ? . . . . O(8) Er(1) O(2) C(12) -147.2(2) ? . . . . O(2) Er(1) O(9) N(4) -106.28(18) ? . . . . O(9) Er(1) O(2) V(1) 99.12(8) ? . . . . O(9) Er(1) O(2) C(12) -99.0(2) ? . . . . O(2) Er(1) O(11) N(5) 42.63(16) ? . . . . O(11) Er(1) O(2) V(1) -123.46(7) ? . . . . O(11) Er(1) O(2) C(12) 38.4(2) ? . . . . O(2) Er(1) O(12) N(5) -151.08(15) ? . . . . O(12) Er(1) O(2) V(1) -93.02(8) ? . . . . O(12) Er(1) O(2) C(12) 68.9(2) ? . . . . O(3) Er(1) O(4) C(13) -103.31(18) ? . . . . O(3) Er(1) O(4) C(19) 66.9(2) ? . . . . O(4) Er(1) O(3) C(2) 104.50(17) ? . . . . O(4) Er(1) O(3) C(8) -67.7(2) ? . . . . O(3) Er(1) O(5) N(3) -150.05(16) ? . . . . O(5) Er(1) O(3) C(2) -146.29(17) ? . . . . O(5) Er(1) O(3) C(8) 41.54(19) ? . . . . O(3) Er(1) O(6) N(3) 27.93(16) ? . . . . O(6) Er(1) O(3) C(2) -170.59(15) ? . . . . O(6) Er(1) O(3) C(8) 17.2(2) ? . . . . O(3) Er(1) O(8) N(4) -174.84(18) ? . . . . O(8) Er(1) O(3) C(2) -75.93(16) ? . . . . O(8) Er(1) O(3) C(8) 111.9(2) ? . . . . O(3) Er(1) O(9) N(4) 14.9(2) ? . . . . O(9) Er(1) O(3) C(2) -85.38(19) ? . . . . O(9) Er(1) O(3) C(8) 102.5(2) ? . . . . O(3) Er(1) O(11) N(5) -77.10(14) ? . . . . O(11) Er(1) O(3) C(2) 129.39(17) ? . . . . O(11) Er(1) O(3) C(8) -42.78(19) ? . . . . O(3) Er(1) O(12) N(5) 75.05(14) ? . . . . O(12) Er(1) O(3) C(2) 73.53(16) ? . . . . O(12) Er(1) O(3) C(8) -98.6(2) ? . . . . O(4) Er(1) O(5) N(3) -12.98(17) ? . . . . O(5) Er(1) O(4) C(13) 167.35(16) ? . . . . O(5) Er(1) O(4) C(19) -22.4(2) ? . . . . O(4) Er(1) O(6) N(3) 166.11(16) ? . . . . O(6) Er(1) O(4) C(13) 155.71(18) ? . . . . O(6) Er(1) O(4) C(19) -34.1(2) ? . . . . O(4) Er(1) O(8) N(4) 4.8(2) ? . . . . O(8) Er(1) O(4) C(13) 77.27(19) ? . . . . O(8) Er(1) O(4) C(19) -112.5(2) ? . . . . O(4) Er(1) O(9) N(4) -171.39(18) ? . . . . O(9) Er(1) O(4) C(13) 83.39(17) ? . . . . O(9) Er(1) O(4) C(19) -106.4(2) ? . . . . O(4) Er(1) O(11) N(5) 86.96(14) ? . . . . O(11) Er(1) O(4) C(13) -127.72(18) ? . . . . O(11) Er(1) O(4) C(19) 42.5(2) ? . . . . O(4) Er(1) O(12) N(5) -85.43(14) ? . . . . O(12) Er(1) O(4) C(13) -72.89(17) ? . . . . O(12) Er(1) O(4) C(19) 97.3(2) ? . . . . O(5) Er(1) O(6) N(3) -0.96(13) ? . . . . O(6) Er(1) O(5) N(3) 0.96(13) ? . . . . O(5) Er(1) O(8) N(4) -108.16(18) ? . . . . O(8) Er(1) O(5) N(3) 115.27(16) ? . . . . O(5) Er(1) O(9) N(4) 68.35(17) ? . . . . O(9) Er(1) O(5) N(3) 65.80(15) ? . . . . O(5) Er(1) O(11) N(5) -146.72(15) ? . . . . O(11) Er(1) O(5) N(3) -76.03(15) ? . . . . O(5) Er(1) O(12) N(5) 30.35(16) ? . . . . O(12) Er(1) O(5) N(3) -103.52(15) ? . . . . O(6) Er(1) O(8) N(4) -62.32(18) ? . . . . O(8) Er(1) O(6) N(3) -60.71(15) ? . . . . O(6) Er(1) O(9) N(4) 117.25(18) ? . . . . O(9) Er(1) O(6) N(3) -106.86(15) ? . . . . O(6) Er(1) O(11) N(5) 159.96(15) ? . . . . O(11) Er(1) O(6) N(3) 87.06(15) ? . . . . O(6) Er(1) O(12) N(5) -31.07(16) ? . . . . O(12) Er(1) O(6) N(3) 109.23(15) ? . . . . O(8) Er(1) O(9) N(4) 2.86(16) ? . . . . O(9) Er(1) O(8) N(4) -2.87(16) ? . . . . O(8) Er(1) O(11) N(5) -127.31(16) ? . . . . O(11) Er(1) O(8) N(4) -128.29(18) ? . . . . O(8) Er(1) O(12) N(5) 132.20(15) ? . . . . O(12) Er(1) O(8) N(4) 132.15(17) ? . . . . O(9) Er(1) O(11) N(5) 139.36(14) ? . . . . O(11) Er(1) O(9) N(4) 138.10(16) ? . . . . O(9) Er(1) O(12) N(5) -130.38(16) ? . . . . O(12) Er(1) O(9) N(4) -127.69(17) ? . . . . O(11) Er(1) O(12) N(5) -4.20(13) ? . . . . O(12) Er(1) O(11) N(5) 4.18(13) ? . . . . O(1) V(1) O(2) Er(1) 18.37(7) ? . . . . O(1) V(1) O(2) C(12) -143.2(2) ? . . . . O(2) V(1) O(1) Er(1) -18.20(7) ? . . . . O(2) V(1) O(1) C(1) 153.50(19) ? . . . . O(1) V(1) O(14) C(22) 31.3(5) ? . . . . O(14) V(1) O(1) Er(1) -98.51(7) ? . . . . O(14) V(1) O(1) C(1) 73.20(18) ? . . . . O(15) V(1) O(1) Er(1) 82.49(10) ? . . . . O(15) V(1) O(1) C(1) -105.80(19) ? . . . . O(1) V(1) N(1) C(7) 8.3(2) ? . . . . O(1) V(1) N(1) C(9) -165.09(17) ? . . . . N(1) V(1) O(1) Er(1) 179.68(7) ? . . . . N(1) V(1) O(1) C(1) -8.61(19) ? . . . . O(1) V(1) N(2) C(11) -134.9(2) ? . . . . O(1) V(1) N(2) C(18) 49.3(4) ? . . . . N(2) V(1) O(1) Er(1) -82.2(2) ? . . . . N(2) V(1) O(1) C(1) 89.5(3) ? . . . . O(2) V(1) O(14) C(22) -49.6(5) ? . . . . O(14) V(1) O(2) Er(1) 101.16(7) ? . . . . O(14) V(1) O(2) C(12) -60.37(19) ? . . . . O(15) V(1) O(2) Er(1) -85.64(9) ? . . . . O(15) V(1) O(2) C(12) 112.8(2) ? . . . . O(2) V(1) N(1) C(7) -52.4(3) ? . . . . O(2) V(1) N(1) C(9) 134.2(2) ? . . . . N(1) V(1) O(2) Er(1) 80.8(2) ? . . . . N(1) V(1) O(2) C(12) -80.7(3) ? . . . . O(2) V(1) N(2) C(11) 162.9(2) ? . . . . O(2) V(1) N(2) C(18) -12.9(2) ? . . . . N(2) V(1) O(2) Er(1) 179.70(8) ? . . . . N(2) V(1) O(2) C(12) 18.2(2) ? . . . . O(14) V(1) N(1) C(7) -72.5(2) ? . . . . O(14) V(1) N(1) C(9) 114.09(18) ? . . . . N(1) V(1) O(14) C(22) 123.4(5) ? . . . . O(14) V(1) N(2) C(11) -118.5(2) ? . . . . O(14) V(1) N(2) C(18) 65.6(2) ? . . . . N(2) V(1) O(14) C(22) -142.8(5) ? . . . . O(15) V(1) N(1) C(7) 114.3(2) ? . . . . O(15) V(1) N(1) C(9) -59.03(19) ? . . . . O(15) V(1) N(2) C(11) 59.8(2) ? . . . . O(15) V(1) N(2) C(18) -116.0(2) ? . . . . N(1) V(1) N(2) C(11) -37.1(2) ? . . . . N(1) V(1) N(2) C(18) 147.1(2) ? . . . . N(2) V(1) N(1) C(7) -151.1(2) ? . . . . N(2) V(1) N(1) C(9) 35.57(18) ? . . . . Er(1) O(1) C(1) C(2) -6.4(2) ? . . . . Er(1) O(1) C(1) C(6) 174.88(16) ? . . . . V(1) O(1) C(1) C(2) -176.52(15) ? . . . . V(1) O(1) C(1) C(6) 4.7(3) ? . . . . Er(1) O(2) C(12) C(13) 9.2(3) ? . . . . Er(1) O(2) C(12) C(17) -170.8(2) ? . . . . V(1) O(2) C(12) C(13) 167.27(18) ? . . . . V(1) O(2) C(12) C(17) -12.7(3) ? . . . . Er(1) O(3) C(2) C(1) 4.9(2) ? . . . . Er(1) O(3) C(2) C(3) -175.98(19) ? . . . . C(8) O(3) C(2) C(1) 178.0(2) ? . . . . C(8) O(3) C(2) C(3) -2.9(3) ? . . . . Er(1) O(4) C(13) C(12) -10.0(2) ? . . . . Er(1) O(4) C(13) C(14) 168.5(2) ? . . . . C(19) O(4) C(13) C(12) 178.7(2) ? . . . . C(19) O(4) C(13) C(14) -2.7(3) ? . . . . Er(1) O(5) N(3) O(6) -1.6(2) ? . . . . Er(1) O(5) N(3) O(7) 179.2(2) ? . . . . Er(1) O(6) N(3) O(5) 1.6(2) ? . . . . Er(1) O(6) N(3) O(7) -179.2(2) ? . . . . Er(1) O(8) N(4) O(9) 4.9(2) ? . . . . Er(1) O(8) N(4) O(10) -175.7(2) ? . . . . Er(1) O(9) N(4) O(8) -4.7(2) ? . . . . Er(1) O(9) N(4) O(10) 175.8(2) ? . . . . Er(1) O(11) N(5) O(12) -7.0(2) ? . . . . Er(1) O(11) N(5) O(13) 172.5(2) ? . . . . Er(1) O(12) N(5) O(11) 7.1(2) ? . . . . Er(1) O(12) N(5) O(13) -172.5(2) ? . . . . V(1) O(14) C(22) C(23) 90.4(6) ? . . . . V(1) O(14) C(22) C(24) -87.4(6) ? . . . . V(1) N(1) C(7) C(6) -4.5(3) ? . . . . V(1) N(1) C(9) C(10) -53.3(3) ? . . . . C(7) N(1) C(9) C(10) 132.8(2) ? . . . . C(9) N(1) C(7) C(6) 169.0(2) ? . . . . V(1) N(2) C(11) C(10) 56.8(2) ? . . . . V(1) N(2) C(18) C(17) 2.2(4) ? . . . . C(11) N(2) C(18) C(17) -173.7(2) ? . . . . C(18) N(2) C(11) C(10) -127.1(2) ? . . . . O(1) C(1) C(2) O(3) 0.4(3) ? . . . . O(1) C(1) C(2) C(3) -178.7(2) ? . . . . O(1) C(1) C(6) C(5) 178.6(2) ? . . . . O(1) C(1) C(6) C(7) 2.9(3) ? . . . . C(2) C(1) C(6) C(5) -0.1(2) ? . . . . C(2) C(1) C(6) C(7) -175.8(2) ? . . . . C(6) C(1) C(2) O(3) 179.2(2) ? . . . . C(6) C(1) C(2) C(3) 0.1(2) ? . . . . O(3) C(2) C(3) C(4) -178.5(2) ? . . . . C(1) C(2) C(3) C(4) 0.5(3) ? . . . . C(2) C(3) C(4) C(5) -1.0(4) ? . . . . C(3) C(4) C(5) C(6) 1.0(4) ? . . . . C(4) C(5) C(6) C(1) -0.4(3) ? . . . . C(4) C(5) C(6) C(7) 175.6(2) ? . . . . C(1) C(6) C(7) N(1) -2.8(4) ? . . . . C(5) C(6) C(7) N(1) -178.6(2) ? . . . . N(1) C(9) C(10) C(11) 63.9(3) ? . . . . N(1) C(9) C(10) C(20) 179.3(2) ? . . . . N(1) C(9) C(10) C(21) -61.2(3) ? . . . . C(9) C(10) C(11) N(2) -65.9(2) ? . . . . C(20) C(10) C(11) N(2) 178.6(2) ? . . . . C(21) C(10) C(11) N(2) 59.4(3) ? . . . . O(2) C(12) C(13) O(4) 1.3(3) ? . . . . O(2) C(12) C(13) C(14) -177.3(2) ? . . . . O(2) C(12) C(17) C(16) 176.4(2) ? . . . . O(2) C(12) C(17) C(18) -4.5(4) ? . . . . C(13) C(12) C(17) C(16) -3.6(4) ? . . . . C(13) C(12) C(17) C(18) 175.5(2) ? . . . . C(17) C(12) C(13) O(4) -178.7(2) ? . . . . C(17) C(12) C(13) C(14) 2.7(4) ? . . . . O(4) C(13) C(14) C(15) -178.4(2) ? . . . . C(12) C(13) C(14) C(15) 0.0(3) ? . . . . C(13) C(14) C(15) C(16) -1.9(4) ? . . . . C(14) C(15) C(16) C(17) 1.0(4) ? . . . . C(15) C(16) C(17) C(12) 1.7(4) ? . . . . C(15) C(16) C(17) C(18) -177.4(2) ? . . . . C(12) C(17) C(18) N(2) 10.1(4) ? . . . . C(16) C(17) C(18) N(2) -170.9(2) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(5) C(24) 3.540(3) ? . 1_655 O(6) C(19) 3.461(4) ? . 3_765 O(7) C(11) 3.137(3) ? . 2_755 O(7) C(19) 3.448(4) ? . 3_765 O(7) C(23) 3.343(3) ? . 1_655 O(8) C(9) 3.372(3) ? . 3_766 O(8) C(20) 3.541(3) ? . 3_766 O(8) C(24) 3.557(4) ? . 1_655 O(9) C(8) 3.418(3) ? . 2_745 O(9) C(23) 3.600(3) ? . 1_655 O(10) C(8) 3.573(3) ? . 2_745 O(10) C(21) 3.352(3) ? . 1_655 O(10) C(22) 3.315(4) ? . 1_655 O(10) C(23) 3.340(4) ? . 1_655 O(11) C(4) 3.405(4) ? . 4_564 O(11) C(5) 3.414(3) ? . 4_564 O(13) C(14) 3.536(3) ? . 3_665 O(13) C(15) 3.286(3) ? . 3_665 O(15) N(1) 3.418(2) ? . 3_766 O(15) C(7) 2.956(3) ? . 3_766 O(15) C(8) 3.538(3) ? . 2_745 O(15) C(9) 3.322(3) ? . 3_766 N(1) O(15) 3.418(2) ? . 3_766 N(3) C(23) 3.429(3) ? . 1_655 N(4) C(23) 3.387(4) ? . 1_655 C(4) O(11) 3.405(4) ? . 4_565 C(5) O(11) 3.414(3) ? . 4_565 C(7) O(15) 2.956(3) ? . 3_766 C(8) O(9) 3.418(3) ? . 2_755 C(8) O(10) 3.573(3) ? . 2_755 C(8) O(15) 3.538(3) ? . 2_755 C(9) O(8) 3.372(3) ? . 3_766 C(9) O(15) 3.322(3) ? . 3_766 C(11) O(7) 3.137(3) ? . 2_745 C(14) O(13) 3.536(3) ? . 3_665 C(15) O(13) 3.286(3) ? . 3_665 C(19) O(6) 3.461(4) ? . 3_765 C(19) O(7) 3.448(4) ? . 3_765 C(20) O(8) 3.541(3) ? . 3_766 C(21) O(10) 3.352(3) ? . 1_455 C(22) O(10) 3.315(4) ? . 1_455 C(23) O(7) 3.343(3) ? . 1_455 C(23) O(9) 3.600(3) ? . 1_455 C(23) O(10) 3.340(4) ? . 1_455 C(23) N(3) 3.429(3) ? . 1_455 C(23) N(4) 3.387(4) ? . 1_455 C(24) O(5) 3.540(3) ? . 1_455 C(24) O(8) 3.557(4) ? . 1_455 V(1) H(9) 3.60(2) ? . 3_766 O(1) H(9) 3.11(2) ? . 3_766 O(2) H(7) 3.27(3) ? . 2_745 O(3) H(21) 3.45(3) ? . 3_766 O(5) H(11) 3.59(3) ? . 2_755 O(5) H(15) 3.55(3) ? . 2_755 O(5) H(27) 3.126 ? . 1_655 O(5) H(28) 2.803 ? . 1_655 O(5) H(29) 3.450 ? . 1_655 O(6) H(2) 3.28(2) ? . 4_564 O(6) H(16) 3.41(3) ? . 3_765 O(6) H(18) 2.72(4) ? . 3_765 O(6) H(27) 3.017 ? . 1_655 O(7) H(10) 2.52(3) ? . 2_755 O(7) H(11) 2.84(3) ? . 2_755 O(7) H(12) 3.18(3) ? . 3_765 O(7) H(15) 3.52(2) ? . 2_755 O(7) H(18) 2.47(3) ? . 3_765 O(7) H(26) 2.712 ? . 1_655 O(7) H(27) 2.984 ? . 1_655 O(7) H(29) 3.495 ? . 1_655 O(8) H(8) 2.61(3) ? . 3_766 O(8) H(9) 3.33(3) ? . 3_766 O(8) H(19) 2.80(3) ? . 3_766 O(8) H(21) 3.55(3) ? . 3_766 O(8) H(27) 3.138 ? . 1_655 O(8) H(28) 2.795 ? . 1_655 O(9) H(1) 2.76(3) ? . 2_745 O(9) H(5) 2.89(2) ? . 2_745 O(9) H(7) 3.17(3) ? . 2_745 O(9) H(27) 2.753 ? . 1_655 O(10) H(4) 3.24(3) ? . 3_766 O(10) H(5) 2.68(2) ? . 2_745 O(10) H(8) 3.07(3) ? . 3_766 O(10) H(23) 3.12(2) ? . 1_655 O(10) H(24) 2.79(3) ? . 1_655 O(10) H(25) 3.598 ? . 1_655 O(10) H(27) 2.852 ? . 1_655 O(10) H(28) 3.453 ? . 1_655 O(11) H(2) 2.79(3) ? . 4_564 O(11) H(3) 2.86(3) ? . 4_564 O(11) H(13) 3.18(2) ? . 3_665 O(13) H(3) 3.26(3) ? . 4_564 O(13) H(10) 3.03(3) ? . 2_655 O(13) H(12) 3.07(3) ? . 3_665 O(13) H(13) 2.61(3) ? . 3_665 O(13) H(15) 3.45(3) ? . 2_655 O(13) H(20) 3.31(3) ? . 2_655 O(13) H(23) 2.89(3) ? . 2_655 O(15) H(3) 3.53(3) ? . 3_766 O(15) H(4) 2.52(2) ? . 3_766 O(15) H(5) 3.44(3) ? . 2_745 O(15) H(6) 3.24(4) ? . 2_745 O(15) H(7) 3.60(3) ? . 2_745 O(15) H(8) 2.90(2) ? . 3_766 O(15) H(9) 3.14(2) ? . 3_766 N(1) H(9) 3.20(3) ? . 3_766 N(3) H(10) 3.42(3) ? . 2_755 N(3) H(11) 3.43(3) ? . 2_755 N(3) H(18) 2.91(4) ? . 3_765 N(3) H(26) 3.128 ? . 1_655 N(3) H(27) 2.777 ? . 1_655 N(3) H(28) 3.375 ? . 1_655 N(4) H(5) 3.05(2) ? . 2_745 N(4) H(8) 3.16(3) ? . 3_766 N(4) H(27) 2.637 ? . 1_655 N(4) H(28) 3.235 ? . 1_655 N(5) H(3) 3.46(3) ? . 4_564 N(5) H(12) 3.41(3) ? . 3_665 N(5) H(13) 3.08(3) ? . 3_665 C(1) H(9) 3.00(2) ? . 3_766 C(1) H(21) 3.29(3) ? . 3_766 C(2) H(21) 3.04(3) ? . 3_766 C(3) H(14) 3.48(3) ? . 2_655 C(3) H(21) 3.28(3) ? . 3_766 C(4) H(13) 3.10(3) ? . 2_655 C(4) H(14) 3.23(2) ? . 2_655 C(4) H(16) 3.37(3) ? . 4_565 C(5) H(11) 3.50(3) ? . 3_766 C(5) H(13) 3.18(3) ? . 2_655 C(5) H(14) 3.48(2) ? . 2_655 C(6) H(9) 2.98(2) ? . 3_766 C(7) H(9) 3.06(3) ? . 3_766 C(7) H(22) 3.40(4) ? . 3_666 C(12) H(7) 3.16(3) ? . 2_745 C(14) H(17) 2.98(3) ? . 3_665 C(14) H(20) 3.17(3) ? . 4_554 C(15) H(2) 3.37(3) ? . 2_645 C(15) H(17) 3.03(3) ? . 3_665 C(15) H(20) 2.72(3) ? . 4_554 C(16) H(20) 3.21(4) ? . 4_554 C(16) H(29) 3.358 ? . 2_645 C(16) H(30) 3.364 ? . 2_645 C(17) H(7) 3.30(3) ? . 2_745 C(18) H(7) 3.50(4) ? . 2_745 C(18) H(29) 3.329 ? . 2_645 C(19) H(2) 3.13(3) ? . 4_564 C(19) H(25) 3.465 ? . 3_665 C(19) H(26) 3.284 ? . 3_665 C(20) H(13) 3.57(3) ? . 4_555 C(20) H(28) 3.507 ? . 3_666 C(21) H(4) 3.50(3) ? . 3_666 C(21) H(22) 3.24(3) ? . 3_666 C(23) H(17) 3.25(3) ? . 3_665 C(23) H(18) 3.31(3) ? . 3_665 C(24) H(14) 2.98(3) ? . 2_655 C(24) H(15) 3.28(3) ? . 2_655 C(24) H(19) 3.13(4) ? . 3_666 H(1) O(9) 2.76(3) ? . 2_755 H(2) O(6) 3.28(2) ? . 4_565 H(2) O(11) 2.79(3) ? . 4_565 H(2) C(15) 3.37(3) ? . 2_655 H(2) C(19) 3.13(3) ? . 4_565 H(2) H(13) 2.84(4) ? . 2_655 H(2) H(14) 3.42(3) ? . 2_655 H(2) H(16) 2.41(4) ? . 4_565 H(2) H(17) 3.09(5) ? . 4_565 H(3) O(11) 2.86(3) ? . 4_565 H(3) O(13) 3.26(3) ? . 4_565 H(3) O(15) 3.53(3) ? . 3_766 H(3) N(5) 3.46(3) ? . 4_565 H(3) H(6) 3.34(4) ? . 4_565 H(3) H(13) 3.00(4) ? . 2_655 H(3) H(23) 3.36(5) ? . 3_666 H(4) O(10) 3.24(3) ? . 3_766 H(4) O(15) 2.52(2) ? . 3_766 H(4) C(21) 3.50(3) ? . 3_666 H(4) H(9) 3.51(4) ? . 3_766 H(4) H(22) 2.98(4) ? . 3_666 H(4) H(23) 3.22(4) ? . 3_666 H(5) O(9) 2.89(2) ? . 2_755 H(5) O(10) 2.68(2) ? . 2_755 H(5) O(15) 3.44(3) ? . 2_755 H(5) N(4) 3.05(2) ? . 2_755 H(6) O(15) 3.24(4) ? . 2_755 H(6) H(3) 3.34(4) ? . 4_564 H(6) H(11) 3.34(5) ? . 2_755 H(7) O(2) 3.27(3) ? . 2_755 H(7) O(9) 3.17(3) ? . 2_755 H(7) O(15) 3.60(3) ? . 2_755 H(7) C(12) 3.16(3) ? . 2_755 H(7) C(17) 3.30(3) ? . 2_755 H(7) C(18) 3.50(4) ? . 2_755 H(7) H(21) 3.42(4) ? . 3_766 H(8) O(8) 2.61(3) ? . 3_766 H(8) O(10) 3.07(3) ? . 3_766 H(8) O(15) 2.90(2) ? . 3_766 H(8) N(4) 3.16(3) ? . 3_766 H(8) H(22) 3.44(4) ? . 3_666 H(9) V(1) 3.60(2) ? . 3_766 H(9) O(1) 3.11(2) ? . 3_766 H(9) O(8) 3.33(3) ? . 3_766 H(9) O(15) 3.14(2) ? . 3_766 H(9) N(1) 3.20(3) ? . 3_766 H(9) C(1) 3.00(2) ? . 3_766 H(9) C(6) 2.98(2) ? . 3_766 H(9) C(7) 3.06(3) ? . 3_766 H(9) H(4) 3.51(4) ? . 3_766 H(10) O(7) 2.52(3) ? . 2_745 H(10) O(13) 3.03(3) ? . 2_645 H(10) N(3) 3.42(3) ? . 2_745 H(11) O(5) 3.59(3) ? . 2_745 H(11) O(7) 2.84(3) ? . 2_745 H(11) N(3) 3.43(3) ? . 2_745 H(11) C(5) 3.50(3) ? . 3_766 H(11) H(6) 3.34(5) ? . 2_745 H(12) O(7) 3.18(3) ? . 3_765 H(12) O(13) 3.07(3) ? . 3_665 H(12) N(5) 3.41(3) ? . 3_665 H(12) H(17) 2.91(5) ? . 3_665 H(12) H(20) 3.34(5) ? . 4_554 H(12) H(26) 2.836 ? . 3_665 H(13) O(11) 3.18(2) ? . 3_665 H(13) O(13) 2.61(3) ? . 3_665 H(13) N(5) 3.08(3) ? . 3_665 H(13) C(4) 3.10(3) ? . 2_645 H(13) C(5) 3.18(3) ? . 2_645 H(13) C(20) 3.57(3) ? . 4_554 H(13) H(2) 2.84(4) ? . 2_645 H(13) H(3) 3.00(4) ? . 2_645 H(13) H(17) 3.01(5) ? . 3_665 H(13) H(20) 2.65(5) ? . 4_554 H(14) C(3) 3.48(3) ? . 2_645 H(14) C(4) 3.23(2) ? . 2_645 H(14) C(5) 3.48(2) ? . 2_645 H(14) C(24) 2.98(3) ? . 2_645 H(14) H(2) 3.42(3) ? . 2_645 H(14) H(20) 3.41(5) ? . 4_554 H(14) H(28) 3.139 ? . 2_645 H(14) H(29) 2.621 ? . 2_645 H(14) H(30) 2.622 ? . 2_645 H(15) O(5) 3.55(3) ? . 2_745 H(15) O(7) 3.52(2) ? . 2_745 H(15) O(13) 3.45(3) ? . 2_645 H(15) C(24) 3.28(3) ? . 2_645 H(15) H(28) 3.234 ? . 2_645 H(15) H(29) 2.466 ? . 2_645 H(16) O(6) 3.41(3) ? . 3_765 H(16) C(4) 3.37(3) ? . 4_564 H(16) H(2) 2.41(4) ? . 4_564 H(17) C(14) 2.98(3) ? . 3_665 H(17) C(15) 3.03(3) ? . 3_665 H(17) C(23) 3.25(3) ? . 3_665 H(17) H(2) 3.09(5) ? . 4_564 H(17) H(12) 2.91(5) ? . 3_665 H(17) H(13) 3.01(5) ? . 3_665 H(17) H(25) 2.841 ? . 3_665 H(17) H(26) 2.872 ? . 3_665 H(17) H(27) 3.376 ? . 3_665 H(18) O(6) 2.72(4) ? . 3_765 H(18) O(7) 2.47(3) ? . 3_765 H(18) N(3) 2.91(4) ? . 3_765 H(18) C(23) 3.31(3) ? . 3_665 H(18) H(25) 3.306 ? . 3_665 H(18) H(26) 2.781 ? . 3_665 H(18) H(27) 3.123 ? . 3_665 H(19) O(8) 2.80(3) ? . 3_766 H(19) C(24) 3.13(4) ? . 3_666 H(19) H(28) 2.591 ? . 3_666 H(19) H(30) 2.888 ? . 3_666 H(20) O(13) 3.31(3) ? . 2_645 H(20) C(14) 3.17(3) ? . 4_555 H(20) C(15) 2.72(3) ? . 4_555 H(20) C(16) 3.21(4) ? . 4_555 H(20) H(12) 3.34(5) ? . 4_555 H(20) H(13) 2.65(5) ? . 4_555 H(20) H(14) 3.41(5) ? . 4_555 H(20) H(30) 3.586 ? . 3_666 H(21) O(3) 3.45(3) ? . 3_766 H(21) O(8) 3.55(3) ? . 3_766 H(21) C(1) 3.29(3) ? . 3_766 H(21) C(2) 3.04(3) ? . 3_766 H(21) C(3) 3.28(3) ? . 3_766 H(21) H(7) 3.42(4) ? . 3_766 H(22) C(7) 3.40(4) ? . 3_666 H(22) C(21) 3.24(3) ? . 3_666 H(22) H(4) 2.98(4) ? . 3_666 H(22) H(8) 3.44(4) ? . 3_666 H(22) H(22) 2.52(4) ? . 3_666 H(22) H(24) 3.03(5) ? . 3_666 H(22) H(30) 3.356 ? . 3_666 H(23) O(10) 3.12(2) ? . 1_455 H(23) O(13) 2.89(3) ? . 2_645 H(23) H(3) 3.36(5) ? . 3_666 H(23) H(4) 3.22(4) ? . 3_666 H(24) O(10) 2.79(3) ? . 1_455 H(24) H(22) 3.03(5) ? . 3_666 H(25) O(10) 3.598 ? . 1_455 H(25) C(19) 3.465 ? . 3_665 H(25) H(17) 2.841 ? . 3_665 H(25) H(18) 3.306 ? . 3_665 H(26) O(7) 2.712 ? . 1_455 H(26) N(3) 3.128 ? . 1_455 H(26) C(19) 3.284 ? . 3_665 H(26) H(12) 2.836 ? . 3_665 H(26) H(17) 2.872 ? . 3_665 H(26) H(18) 2.781 ? . 3_665 H(27) O(5) 3.126 ? . 1_455 H(27) O(6) 3.017 ? . 1_455 H(27) O(7) 2.984 ? . 1_455 H(27) O(8) 3.138 ? . 1_455 H(27) O(9) 2.753 ? . 1_455 H(27) O(10) 2.852 ? . 1_455 H(27) N(3) 2.777 ? . 1_455 H(27) N(4) 2.637 ? . 1_455 H(27) H(17) 3.376 ? . 3_665 H(27) H(18) 3.123 ? . 3_665 H(28) O(5) 2.803 ? . 1_455 H(28) O(8) 2.795 ? . 1_455 H(28) O(10) 3.453 ? . 1_455 H(28) N(3) 3.375 ? . 1_455 H(28) N(4) 3.235 ? . 1_455 H(28) C(20) 3.507 ? . 3_666 H(28) H(14) 3.139 ? . 2_655 H(28) H(15) 3.234 ? . 2_655 H(28) H(19) 2.591 ? . 3_666 H(29) O(5) 3.450 ? . 1_455 H(29) O(7) 3.495 ? . 1_455 H(29) C(16) 3.358 ? . 2_655 H(29) C(18) 3.329 ? . 2_655 H(29) H(14) 2.621 ? . 2_655 H(29) H(15) 2.466 ? . 2_655 H(30) C(16) 3.364 ? . 2_655 H(30) H(14) 2.622 ? . 2_655 H(30) H(19) 2.888 ? . 3_666 H(30) H(20) 3.586 ? . 3_666 H(30) H(22) 3.356 ? . 3_666 Er(1) V(1) 3.4767(16) ? . . #============================================================================== # End of CIF #==============================================================================