# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sessler, Jonathan' _publ_contact_author_email chemcommun@cm.utexas.edu _publ_section_title ; Multi-Component Self-Assembly: Supramolecular Organic Frameworks Containing Metal-Rotaxane Subunits (RSOFs) ; _publ_author_address ; Department of Chemistry & Biochemistry, 1 University Station A5300, University of Texas at Austin, Austin, Texas, 78712-0165, USA; Department of Chemistry, Yonsei University, Seoul, 120-749, Korea. ; _publ_contact_author_address ; Department of Chemistry & Biochemistry, 1 University Station A5300, University of Texas at Austin, Austin, Texas, 78712-0165, USA; Department of Chemistry, Yonsei University, Seoul, 120-749, Korea. ; loop_ _publ_author_name H.-Y.Gong B.Rambo C.Nelson W.Cho V.Lynch X.Zhu M.Oh J.Sessler # Attachment '- RSOF-Er as CCDC 824440.CIF' data_RSOF-Er _database_code_depnum_ccdc_archive 'CCDC 824440' #TrackingRef '- RSOF-Er as CCDC 824440.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; cyclo(2)(2,6-di(1H-imidazol-1-yl)pyridine)(2)(1,4- dimethylenebenzene) _ 5 terephthalate dianion_ 2 erbium(iii)_8 H2O_ 19 H2O ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H108 Er2 N10 O47' _chemical_formula_weight 2272.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.248(2) _cell_length_b 17.450(4) _cell_length_c 24.160(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.94(3) _cell_angle_gamma 90.00 _cell_volume 4696.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8062 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7214 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37479 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8062 _reflns_number_gt 7372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8062 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.81831(2) 0.694959(16) 0.635889(11) 0.02060(11) Uani 1 1 d . . . O1 O 0.7104(4) 0.7120(3) 0.70992(18) 0.0293(10) Uani 1 1 d . . . O1W O 0.9326(4) 0.6024(3) 0.5962(2) 0.0316(11) Uani 1 1 d . . . O2W O 0.8844(4) 0.6066(2) 0.70753(19) 0.0291(10) Uani 1 1 d . . . O2 O 0.5430(4) 0.7807(3) 0.69126(19) 0.0322(11) Uani 1 1 d . . . O3W O 0.6859(4) 0.7971(3) 0.61366(19) 0.0296(10) Uani 1 1 d . . . O3 O 0.6005(6) 0.6517(4) 0.9832(2) 0.0525(16) Uani 1 1 d . . . O4 O 0.4617(5) 0.7441(3) 0.97198(19) 0.0363(12) Uani 1 1 d . . . O4W O 0.9193(4) 0.7709(3) 0.57724(18) 0.0276(10) Uani 1 1 d . . . O5 O 0.9627(4) 0.7620(2) 0.69244(18) 0.0252(10) Uani 1 1 d . . . O5W O 1.4489(7) 0.9032(4) 0.9838(3) 0.075(2) Uani 1 1 d . . . O6 O 0.9699(4) 0.7188(3) 0.77987(19) 0.0319(11) Uani 1 1 d . . . O6W O 1.0865(8) 0.6507(5) 0.8742(3) 0.091(3) Uani 1 1 d . . . O7 O 1.4353(5) 1.0081(3) 0.7806(3) 0.0620(19) Uani 1 1 d . . . O7W O 0.7150(5) 0.7513(4) 0.4487(2) 0.0587(17) Uani 1 1 d . . . O8 O 1.4009(6) 1.0004(4) 0.8691(4) 0.082(3) Uani 1 1 d . . . O8W O 0.9947(14) 1.0819(5) 0.4140(3) 0.164(6) Uani 1 1 d . . . O9 O 0.6568(4) 0.6081(2) 0.61737(17) 0.0227(9) Uani 1 1 d . . . O9W O 0.5049(9) 0.9420(6) 0.6826(5) 0.121(4) Uani 1 1 d . . . O10 O 0.7130(4) 0.6583(2) 0.54171(18) 0.0238(9) Uani 1 1 d . . . O10W O 0.6361(13) 0.8757(7) 0.5197(4) 0.159(5) Uani 1 1 d . . . O11W O 0.699(3) 0.5090(9) 0.9592(11) 0.170(12) Uani 0.50 1 d P . . O12W O 0.8915(19) 0.5425(10) 0.8817(7) 0.109(7) Uani 0.50 1 d P . . N1 N 0.7161(5) 0.4443(3) 0.7205(2) 0.0248(12) Uani 1 1 d . . . N2 N 0.5710(5) 0.5019(3) 0.7534(2) 0.0237(11) Uani 1 1 d . . . N3 N 0.4338(5) 0.5852(3) 0.7061(2) 0.0225(11) Uani 1 1 d . . . N4 N 0.3094(5) 0.6678(3) 0.6509(2) 0.0239(12) Uani 1 1 d . . . N5 N 0.3346(5) 0.7155(3) 0.5709(2) 0.0291(13) Uani 1 1 d . . . C1 C 0.8031(6) 0.4236(4) 0.6824(3) 0.0261(14) Uani 1 1 d . . . H1A H 0.8629 0.3894 0.7018 0.031 Uiso 1 1 calc R . . H1B H 0.8441 0.4697 0.6729 0.031 Uiso 1 1 calc R . . C2 C 0.6358(5) 0.4996(4) 0.7108(3) 0.0234(13) Uani 1 1 d . . . H2A H 0.6259 0.5315 0.6797 0.028 Uiso 1 1 calc R . . C3 C 0.7044(7) 0.4106(4) 0.7716(3) 0.0360(17) Uani 1 1 d . . . H3A H 0.7503 0.3704 0.7884 0.043 Uiso 1 1 calc R . . C4 C 0.6148(7) 0.4467(4) 0.7923(3) 0.0339(16) Uani 1 1 d . . . H4A H 0.5873 0.4365 0.8261 0.041 Uiso 1 1 calc R . . C5 C 0.4687(6) 0.5506(4) 0.7545(3) 0.0256(14) Uani 1 1 d . . . C6 C 0.4128(6) 0.5589(4) 0.8015(3) 0.0317(15) Uani 1 1 d . . . H6A H 0.4418 0.5347 0.8350 0.038 Uiso 1 1 calc R . . C7 C 0.3120(7) 0.6046(4) 0.7967(3) 0.0339(16) Uani 1 1 d . . . H7A H 0.2697 0.6105 0.8269 0.041 Uiso 1 1 calc R . . C8 C 0.2740(6) 0.6416(4) 0.7471(3) 0.0318(16) Uani 1 1 d . . . H8A H 0.2070 0.6733 0.7432 0.038 Uiso 1 1 calc R . . C9 C 0.3384(6) 0.6299(4) 0.7034(3) 0.0263(14) Uani 1 1 d . . . C10 C 0.3869(6) 0.6763(4) 0.6143(3) 0.0279(15) Uani 1 1 d . . . H10A H 0.4651 0.6576 0.6187 0.033 Uiso 1 1 calc R . . C11 C 0.2028(6) 0.7045(4) 0.6299(3) 0.0329(16) Uani 1 1 d . . . H11A H 0.1336 0.7076 0.6469 0.040 Uiso 1 1 calc R . . C12 C 0.2190(7) 0.7345(5) 0.5806(3) 0.0385(18) Uani 1 1 d . . . H12A H 0.1633 0.7630 0.5571 0.046 Uiso 1 1 calc R . . C13 C 0.3893(6) 0.7363(4) 0.5213(3) 0.0306(15) Uani 1 1 d . . . H13A H 0.4753 0.7282 0.5291 0.037 Uiso 1 1 calc R . . H13B H 0.3759 0.7904 0.5137 0.037 Uiso 1 1 calc R . . C14 C 0.3405(6) 0.6912(4) 0.4699(3) 0.0258(14) Uani 1 1 d . . . C15 C 0.2614(6) 0.6304(4) 0.4703(3) 0.0305(15) Uani 1 1 d . . . H15A H 0.2370 0.6148 0.5038 0.037 Uiso 1 1 calc R . . C16 C 0.2184(6) 0.5926(4) 0.4212(3) 0.0295(15) Uani 1 1 d . . . H16A H 0.1652 0.5519 0.4221 0.035 Uiso 1 1 calc R . . C17 C 0.2536(5) 0.6146(4) 0.3709(3) 0.0240(13) Uani 1 1 d . . . C18 C 0.3353(6) 0.6745(4) 0.3705(3) 0.0283(15) Uani 1 1 d . . . H18A H 0.3611 0.6893 0.3371 0.034 Uiso 1 1 calc R . . C19 C 0.3781(6) 0.7118(4) 0.4195(3) 0.0294(15) Uani 1 1 d . . . H19A H 0.4330 0.7515 0.4188 0.035 Uiso 1 1 calc R . . C20 C 0.6157(5) 0.7405(4) 0.7230(3) 0.0229(13) Uani 1 1 d . . . C21 C 0.5909(6) 0.7268(4) 0.7820(3) 0.0245(14) Uani 1 1 d . . . C22 C 0.4968(6) 0.7641(4) 0.8021(3) 0.0256(14) Uani 1 1 d . . . H22A H 0.4448 0.7949 0.7784 0.031 Uiso 1 1 calc R . . C23 C 0.4803(6) 0.7556(4) 0.8575(3) 0.0278(14) Uani 1 1 d . . . H23A H 0.4184 0.7819 0.8710 0.033 Uiso 1 1 calc R . . C24 C 0.5550(6) 0.7081(4) 0.8931(3) 0.0293(15) Uani 1 1 d . . . C25 C 0.6473(6) 0.6699(4) 0.8721(3) 0.0299(15) Uani 1 1 d . . . H25A H 0.6973 0.6375 0.8954 0.036 Uiso 1 1 calc R . . C26 C 0.6661(6) 0.6794(4) 0.8169(3) 0.0276(15) Uani 1 1 d . . . H26A H 0.7290 0.6541 0.8035 0.033 Uiso 1 1 calc R . . C27 C 0.5389(7) 0.7002(4) 0.9540(3) 0.0337(16) Uani 1 1 d . . . C28 C 1.0027(6) 0.7624(4) 0.7446(3) 0.0260(14) Uani 1 1 d . . . C29 C 1.0989(6) 0.8216(4) 0.7636(3) 0.0267(14) Uani 1 1 d . . . C30 C 1.1311(7) 0.8371(5) 0.8198(3) 0.0388(18) Uani 1 1 d . . . H30A H 1.0928 0.8117 0.8462 0.047 Uiso 1 1 calc R . . C31 C 1.2198(7) 0.8899(5) 0.8370(4) 0.046(2) Uani 1 1 d . . . H31A H 1.2392 0.9009 0.8748 0.055 Uiso 1 1 calc R . . C32 C 1.2797(6) 0.9263(4) 0.7990(4) 0.041(2) Uani 1 1 d . . . C33 C 1.2485(7) 0.9103(4) 0.7422(4) 0.0406(18) Uani 1 1 d . . . H33A H 1.2894 0.9342 0.7161 0.049 Uiso 1 1 calc R . . C34 C 1.1569(6) 0.8590(4) 0.7246(3) 0.0322(16) Uani 1 1 d . . . H34A H 1.1347 0.8497 0.6867 0.039 Uiso 1 1 calc R . . C35 C 1.3785(7) 0.9829(5) 0.8190(5) 0.055(2) Uani 1 1 d . . . C36 C 0.6519(5) 0.6097(3) 0.5645(3) 0.0216(13) Uani 1 1 d . . . C37 C 0.5728(5) 0.5534(3) 0.5308(2) 0.0196(12) Uani 1 1 d . . . C38 C 0.5766(6) 0.5466(3) 0.4740(3) 0.0230(13) Uani 1 1 d . . . H38A H 0.6279 0.5777 0.4568 0.028 Uiso 1 1 calc R . . C39 C 0.5039(6) 0.4936(4) 0.4426(3) 0.0229(13) Uani 1 1 d . . . H39A H 0.5059 0.4892 0.4044 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01787(17) 0.02113(16) 0.02210(16) -0.00098(11) 0.00028(11) -0.00299(11) O1 0.025(3) 0.040(3) 0.024(2) 0.001(2) 0.007(2) 0.003(2) O1W 0.022(3) 0.032(3) 0.040(3) 0.006(2) 0.004(2) 0.0082(19) O2W 0.029(3) 0.024(2) 0.031(2) 0.0043(19) -0.006(2) -0.0009(19) O2 0.029(3) 0.041(3) 0.026(2) 0.000(2) 0.002(2) 0.002(2) O3W 0.034(3) 0.029(2) 0.026(2) -0.0015(19) 0.006(2) 0.012(2) O3 0.062(4) 0.068(4) 0.027(3) 0.004(3) 0.006(3) 0.025(3) O4 0.040(3) 0.044(3) 0.026(2) -0.005(2) 0.007(2) 0.007(2) O4W 0.028(3) 0.032(2) 0.024(2) 0.0007(19) 0.0070(19) -0.009(2) O5 0.023(2) 0.027(2) 0.025(2) -0.0084(18) 0.0004(19) -0.0054(18) O5W 0.096(5) 0.053(4) 0.092(5) -0.030(4) 0.068(4) -0.035(4) O6 0.034(3) 0.038(3) 0.023(2) -0.005(2) 0.002(2) -0.011(2) O6W 0.093(6) 0.105(7) 0.075(5) -0.016(5) 0.007(4) 0.021(5) O7 0.039(4) 0.033(3) 0.102(5) 0.005(3) -0.032(4) -0.006(3) O7W 0.044(4) 0.089(5) 0.041(3) 0.029(3) -0.003(3) -0.005(3) O8 0.049(4) 0.085(5) 0.113(6) -0.069(5) 0.013(4) -0.028(4) O8W 0.357(18) 0.085(6) 0.045(5) -0.003(4) 0.009(7) -0.117(9) O9 0.021(2) 0.027(2) 0.019(2) -0.0016(17) -0.0018(17) -0.0086(18) O9W 0.088(7) 0.098(7) 0.178(10) -0.014(7) 0.025(7) -0.001(6) O10 0.018(2) 0.027(2) 0.025(2) -0.0020(18) 0.0004(18) -0.0054(18) O10W 0.232(14) 0.162(11) 0.075(6) 0.048(7) -0.003(8) 0.059(10) O11W 0.30(3) 0.027(8) 0.20(2) 0.027(11) 0.11(2) 0.046(14) O12W 0.170(19) 0.084(12) 0.077(11) 0.007(9) 0.032(12) 0.058(12) N1 0.027(3) 0.023(3) 0.024(3) -0.002(2) 0.001(2) 0.002(2) N2 0.025(3) 0.024(3) 0.022(3) -0.001(2) 0.002(2) -0.001(2) N3 0.019(3) 0.024(3) 0.024(3) -0.008(2) -0.001(2) -0.001(2) N4 0.017(3) 0.029(3) 0.025(3) -0.009(2) 0.000(2) 0.004(2) N5 0.022(3) 0.035(3) 0.029(3) -0.005(2) -0.002(2) 0.007(2) C1 0.020(3) 0.025(3) 0.033(4) -0.003(3) 0.001(3) 0.003(3) C2 0.019(3) 0.025(3) 0.026(3) -0.003(3) 0.001(3) -0.004(2) C3 0.045(5) 0.031(4) 0.030(4) 0.008(3) 0.000(3) 0.006(3) C4 0.044(5) 0.031(4) 0.026(4) 0.004(3) 0.002(3) 0.005(3) C5 0.026(4) 0.022(3) 0.028(3) -0.008(3) 0.002(3) -0.009(3) C6 0.035(4) 0.032(4) 0.029(4) -0.006(3) 0.007(3) -0.004(3) C7 0.037(4) 0.036(4) 0.030(4) -0.009(3) 0.011(3) -0.004(3) C8 0.021(4) 0.037(4) 0.038(4) -0.009(3) 0.007(3) 0.002(3) C9 0.025(4) 0.029(3) 0.024(3) -0.010(3) 0.002(3) -0.006(3) C10 0.023(4) 0.034(4) 0.025(3) -0.010(3) -0.003(3) -0.001(3) C11 0.022(4) 0.043(4) 0.033(4) -0.010(3) 0.000(3) 0.007(3) C12 0.030(4) 0.047(5) 0.035(4) -0.009(3) -0.006(3) 0.016(3) C13 0.029(4) 0.030(4) 0.032(4) 0.000(3) 0.001(3) 0.003(3) C14 0.022(4) 0.024(3) 0.031(4) 0.001(3) -0.001(3) 0.006(3) C15 0.038(4) 0.028(4) 0.025(3) 0.004(3) 0.004(3) 0.004(3) C16 0.032(4) 0.025(3) 0.031(4) 0.001(3) 0.003(3) -0.001(3) C17 0.017(3) 0.025(3) 0.028(3) -0.002(3) -0.004(3) 0.005(2) C18 0.031(4) 0.026(3) 0.029(4) 0.000(3) 0.007(3) 0.000(3) C19 0.023(4) 0.033(4) 0.031(4) -0.002(3) 0.002(3) -0.004(3) C20 0.017(3) 0.026(3) 0.024(3) -0.006(3) -0.001(3) -0.007(3) C21 0.024(4) 0.027(3) 0.021(3) -0.006(3) -0.001(3) -0.005(3) C22 0.022(3) 0.028(3) 0.025(3) -0.004(3) 0.000(3) -0.003(3) C23 0.030(4) 0.026(3) 0.028(3) -0.009(3) 0.008(3) -0.002(3) C24 0.026(4) 0.036(4) 0.025(3) -0.009(3) 0.001(3) -0.004(3) C25 0.030(4) 0.029(3) 0.029(4) -0.002(3) -0.004(3) 0.001(3) C26 0.022(4) 0.034(4) 0.026(3) -0.008(3) 0.002(3) 0.000(3) C27 0.037(4) 0.039(4) 0.025(4) -0.006(3) 0.003(3) 0.003(3) C28 0.020(3) 0.031(4) 0.026(3) -0.010(3) 0.001(3) 0.000(3) C29 0.015(3) 0.028(3) 0.036(4) -0.009(3) 0.000(3) -0.001(3) C30 0.029(4) 0.046(4) 0.041(4) -0.019(4) 0.003(3) -0.004(3) C31 0.025(4) 0.048(5) 0.062(5) -0.028(4) -0.002(4) -0.002(3) C32 0.019(4) 0.030(4) 0.070(6) -0.023(4) -0.012(4) 0.005(3) C33 0.025(4) 0.026(4) 0.069(6) 0.007(4) 0.000(4) 0.000(3) C34 0.026(4) 0.025(3) 0.043(4) -0.004(3) -0.002(3) 0.002(3) C35 0.027(5) 0.033(4) 0.103(8) -0.008(5) 0.006(5) 0.001(3) C36 0.017(3) 0.022(3) 0.025(3) 0.002(2) -0.002(3) 0.002(2) C37 0.011(3) 0.023(3) 0.024(3) -0.001(2) -0.003(2) -0.001(2) C38 0.021(3) 0.021(3) 0.026(3) 0.000(2) 0.002(3) -0.001(2) C39 0.021(3) 0.027(3) 0.020(3) -0.003(2) 0.002(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O5 2.293(4) . ? Er1 O1 2.315(4) . ? Er1 O3W 2.337(4) . ? Er1 O4W 2.345(4) . ? Er1 O1W 2.349(5) . ? Er1 O2W 2.360(4) . ? Er1 O9 2.361(4) . ? Er1 O10 2.499(4) . ? Er1 C36 2.793(6) . ? O1 C20 1.255(8) . ? O2 C20 1.256(8) . ? O3 C27 1.249(9) . ? O4 C27 1.279(8) . ? O5 C28 1.278(8) . ? O6 C28 1.236(8) . ? O7 C35 1.276(12) . ? O8 C35 1.240(12) . ? O9 C36 1.272(7) . ? O10 C36 1.264(7) . ? N1 C2 1.321(8) . ? N1 C3 1.390(9) . ? N1 C1 1.478(8) . ? N2 C2 1.342(8) . ? N2 C4 1.388(8) . ? N2 C5 1.433(8) . ? N3 C9 1.321(8) . ? N3 C5 1.327(8) . ? N4 C10 1.332(9) . ? N4 C11 1.393(9) . ? N4 C9 1.428(9) . ? N5 C10 1.321(9) . ? N5 C12 1.393(9) . ? N5 C13 1.467(9) . ? C1 C17 1.510(9) 3_666 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 C4 1.342(10) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.380(9) . ? C6 C7 1.378(10) . ? C6 H6A 0.9300 . ? C7 C8 1.376(10) . ? C7 H7A 0.9300 . ? C8 C9 1.375(9) . ? C8 H8A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.336(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.510(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.385(9) . ? C14 C19 1.390(9) . ? C15 C16 1.384(9) . ? C15 H15A 0.9300 . ? C16 C17 1.385(9) . ? C16 H16A 0.9300 . ? C17 C18 1.393(9) . ? C17 C1 1.510(9) 3_666 ? C18 C19 1.379(9) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.508(9) . ? C21 C26 1.383(9) . ? C21 C22 1.388(9) . ? C22 C23 1.383(9) . ? C22 H22A 0.9300 . ? C23 C24 1.391(10) . ? C23 H23A 0.9300 . ? C24 C25 1.387(10) . ? C24 C27 1.512(9) . ? C25 C26 1.388(9) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 C29 1.521(9) . ? C29 C34 1.380(10) . ? C29 C30 1.384(10) . ? C30 C31 1.379(10) . ? C30 H30A 0.9300 . ? C31 C32 1.367(12) . ? C31 H31A 0.9300 . ? C32 C33 1.396(12) . ? C32 C35 1.515(11) . ? C33 C34 1.387(10) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C36 C37 1.490(8) . ? C37 C38 1.384(9) . ? C37 C39 1.408(8) 3_666 ? C38 C39 1.388(9) . ? C38 H38A 0.9300 . ? C39 C37 1.408(8) 3_666 ? C39 H39A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Er1 O1 82.97(16) . . ? O5 Er1 O3W 97.14(16) . . ? O1 Er1 O3W 72.19(16) . . ? O5 Er1 O4W 73.11(15) . . ? O1 Er1 O4W 138.02(16) . . ? O3W Er1 O4W 77.09(17) . . ? O5 Er1 O1W 102.20(16) . . ? O1 Er1 O1W 141.10(16) . . ? O3W Er1 O1W 142.91(16) . . ? O4W Er1 O1W 78.71(17) . . ? O5 Er1 O2W 76.74(16) . . ? O1 Er1 O2W 70.32(16) . . ? O3W Er1 O2W 142.46(16) . . ? O4W Er1 O2W 133.03(16) . . ? O1W Er1 O2W 73.46(16) . . ? O5 Er1 O9 154.61(15) . . ? O1 Er1 O9 75.97(16) . . ? O3W Er1 O9 89.84(17) . . ? O4W Er1 O9 132.27(15) . . ? O1W Er1 O9 86.04(16) . . ? O2W Er1 O9 82.87(15) . . ? O5 Er1 O10 151.72(15) . . ? O1 Er1 O10 120.23(15) . . ? O3W Er1 O10 77.25(15) . . ? O4W Er1 O10 78.63(15) . . ? O1W Er1 O10 70.71(15) . . ? O2W Er1 O10 124.21(15) . . ? O9 Er1 O10 53.66(14) . . ? O5 Er1 C36 177.03(17) . . ? O1 Er1 C36 99.67(17) . . ? O3W Er1 C36 85.01(17) . . ? O4W Er1 C36 105.49(17) . . ? O1W Er1 C36 74.89(17) . . ? O2W Er1 C36 102.80(17) . . ? O9 Er1 C36 26.93(16) . . ? O10 Er1 C36 26.91(16) . . ? C20 O1 Er1 143.1(4) . . ? C28 O5 Er1 135.6(4) . . ? C36 O9 Er1 95.8(4) . . ? C36 O10 Er1 89.6(4) . . ? C2 N1 C3 108.7(6) . . ? C2 N1 C1 124.2(5) . . ? C3 N1 C1 127.1(6) . . ? C2 N2 C4 108.5(6) . . ? C2 N2 C5 123.7(5) . . ? C4 N2 C5 127.6(6) . . ? C9 N3 C5 116.7(6) . . ? C10 N4 C11 108.5(6) . . ? C10 N4 C9 123.4(5) . . ? C11 N4 C9 128.0(6) . . ? C10 N5 C12 108.3(6) . . ? C10 N5 C13 125.9(6) . . ? C12 N5 C13 125.8(6) . . ? N1 C1 C17 113.6(5) . 3_666 ? N1 C1 H1A 108.8 . . ? C17 C1 H1A 108.8 3_666 . ? N1 C1 H1B 108.8 . . ? C17 C1 H1B 108.8 3_666 . ? H1A C1 H1B 107.7 . . ? N1 C2 N2 108.4(6) . . ? N1 C2 H2A 125.8 . . ? N2 C2 H2A 125.8 . . ? C4 C3 N1 107.5(6) . . ? C4 C3 H3A 126.3 . . ? N1 C3 H3A 126.3 . . ? C3 C4 N2 106.8(6) . . ? C3 C4 H4A 126.6 . . ? N2 C4 H4A 126.6 . . ? N3 C5 C6 124.4(6) . . ? N3 C5 N2 113.2(5) . . ? C6 C5 N2 122.4(6) . . ? C7 C6 C5 117.0(7) . . ? C7 C6 H6A 121.5 . . ? C5 C6 H6A 121.5 . . ? C8 C7 C6 119.9(6) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C9 C8 C7 117.8(7) . . ? C9 C8 H8A 121.1 . . ? C7 C8 H8A 121.1 . . ? N3 C9 C8 124.1(6) . . ? N3 C9 N4 113.6(5) . . ? C8 C9 N4 122.2(6) . . ? N5 C10 N4 108.9(6) . . ? N5 C10 H10A 125.6 . . ? N4 C10 H10A 125.6 . . ? C12 C11 N4 106.7(6) . . ? C12 C11 H11A 126.6 . . ? N4 C11 H11A 126.6 . . ? C11 C12 N5 107.6(6) . . ? C11 C12 H12A 126.2 . . ? N5 C12 H12A 126.2 . . ? N5 C13 C14 113.4(6) . . ? N5 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N5 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C19 118.6(6) . . ? C15 C14 C13 123.7(6) . . ? C19 C14 C13 117.7(6) . . ? C16 C15 C14 120.5(6) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C17 C16 C15 120.8(6) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 118.9(6) . . ? C16 C17 C1 119.2(6) . 3_666 ? C18 C17 C1 121.8(6) . 3_666 ? C19 C18 C17 120.0(6) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C14 121.2(6) . . ? C18 C19 H19A 119.4 . . ? C14 C19 H19A 119.4 . . ? O1 C20 O2 124.8(6) . . ? O1 C20 C21 116.7(6) . . ? O2 C20 C21 118.4(6) . . ? C26 C21 C22 119.9(6) . . ? C26 C21 C20 119.6(6) . . ? C22 C21 C20 120.4(6) . . ? C23 C22 C21 119.9(6) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.9(6) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C25 C24 C23 118.5(6) . . ? C25 C24 C27 120.5(6) . . ? C23 C24 C27 120.9(6) . . ? C24 C25 C26 121.0(6) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C21 C26 C25 119.7(6) . . ? C21 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? O3 C27 O4 124.4(7) . . ? O3 C27 C24 118.7(6) . . ? O4 C27 C24 117.0(6) . . ? O6 C28 O5 125.3(6) . . ? O6 C28 C29 118.6(6) . . ? O5 C28 C29 116.1(6) . . ? C34 C29 C30 119.6(6) . . ? C34 C29 C28 119.9(6) . . ? C30 C29 C28 120.5(6) . . ? C31 C30 C29 120.4(8) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C32 C31 C30 120.8(8) . . ? C32 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? C31 C32 C33 119.1(7) . . ? C31 C32 C35 119.7(8) . . ? C33 C32 C35 121.2(9) . . ? C34 C33 C32 120.4(8) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C29 C34 C33 119.8(7) . . ? C29 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? O8 C35 O7 124.8(8) . . ? O8 C35 C32 120.9(9) . . ? O7 C35 C32 114.3(9) . . ? O10 C36 O9 120.1(6) . . ? O10 C36 C37 121.6(5) . . ? O9 C36 C37 118.3(5) . . ? O10 C36 Er1 63.5(3) . . ? O9 C36 Er1 57.2(3) . . ? C37 C36 Er1 170.9(4) . . ? C38 C37 C39 120.5(6) . 3_666 ? C38 C37 C36 120.0(5) . . ? C39 C37 C36 119.6(5) 3_666 . ? C37 C38 C39 120.1(6) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C38 C39 C37 119.4(6) . 3_666 ? C38 C39 H39A 120.3 . . ? C37 C39 H39A 120.3 3_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Er1 O1 C20 120.5(7) . . . . ? O3W Er1 O1 C20 20.6(7) . . . . ? O4W Er1 O1 C20 65.6(8) . . . . ? O1W Er1 O1 C20 -138.8(7) . . . . ? O2W Er1 O1 C20 -161.1(7) . . . . ? O9 Er1 O1 C20 -73.8(7) . . . . ? O10 Er1 O1 C20 -42.3(7) . . . . ? C36 Er1 O1 C20 -60.9(7) . . . . ? O1 Er1 O5 C28 41.0(6) . . . . ? O3W Er1 O5 C28 111.9(6) . . . . ? O4W Er1 O5 C28 -173.9(6) . . . . ? O1W Er1 O5 C28 -99.9(6) . . . . ? O2W Er1 O5 C28 -30.4(6) . . . . ? O9 Er1 O5 C28 7.0(8) . . . . ? O10 Er1 O5 C28 -171.7(5) . . . . ? C36 Er1 O5 C28 -112(3) . . . . ? O5 Er1 O9 C36 -174.3(4) . . . . ? O1 Er1 O9 C36 150.9(4) . . . . ? O3W Er1 O9 C36 79.3(4) . . . . ? O4W Er1 O9 C36 7.0(4) . . . . ? O1W Er1 O9 C36 -63.9(4) . . . . ? O2W Er1 O9 C36 -137.7(4) . . . . ? O10 Er1 O9 C36 5.0(3) . . . . ? O5 Er1 O10 C36 174.3(4) . . . . ? O1 Er1 O10 C36 -44.1(4) . . . . ? O3W Er1 O10 C36 -104.4(4) . . . . ? O4W Er1 O10 C36 176.4(4) . . . . ? O1W Er1 O10 C36 94.6(4) . . . . ? O2W Er1 O10 C36 41.6(4) . . . . ? O9 Er1 O10 C36 -5.0(3) . . . . ? C2 N1 C1 C17 -70.6(8) . . . 3_666 ? C3 N1 C1 C17 109.8(7) . . . 3_666 ? C3 N1 C2 N2 -1.1(7) . . . . ? C1 N1 C2 N2 179.2(5) . . . . ? C4 N2 C2 N1 1.5(7) . . . . ? C5 N2 C2 N1 -174.2(5) . . . . ? C2 N1 C3 C4 0.3(8) . . . . ? C1 N1 C3 C4 -180.0(6) . . . . ? N1 C3 C4 N2 0.6(8) . . . . ? C2 N2 C4 C3 -1.3(8) . . . . ? C5 N2 C4 C3 174.2(6) . . . . ? C9 N3 C5 C6 -0.5(9) . . . . ? C9 N3 C5 N2 178.7(5) . . . . ? C2 N2 C5 N3 9.0(8) . . . . ? C4 N2 C5 N3 -165.9(6) . . . . ? C2 N2 C5 C6 -171.8(6) . . . . ? C4 N2 C5 C6 13.4(10) . . . . ? N3 C5 C6 C7 2.0(10) . . . . ? N2 C5 C6 C7 -177.2(6) . . . . ? C5 C6 C7 C8 -2.2(10) . . . . ? C6 C7 C8 C9 1.1(10) . . . . ? C5 N3 C9 C8 -0.8(9) . . . . ? C5 N3 C9 N4 177.4(5) . . . . ? C7 C8 C9 N3 0.5(10) . . . . ? C7 C8 C9 N4 -177.5(6) . . . . ? C10 N4 C9 N3 -18.8(9) . . . . ? C11 N4 C9 N3 164.6(6) . . . . ? C10 N4 C9 C8 159.4(6) . . . . ? C11 N4 C9 C8 -17.2(10) . . . . ? C12 N5 C10 N4 1.4(8) . . . . ? C13 N5 C10 N4 -179.4(6) . . . . ? C11 N4 C10 N5 -0.9(7) . . . . ? C9 N4 C10 N5 -178.1(5) . . . . ? C10 N4 C11 C12 0.0(8) . . . . ? C9 N4 C11 C12 177.1(6) . . . . ? N4 C11 C12 N5 0.8(8) . . . . ? C10 N5 C12 C11 -1.4(8) . . . . ? C13 N5 C12 C11 179.4(6) . . . . ? C10 N5 C13 C14 107.4(7) . . . . ? C12 N5 C13 C14 -73.5(8) . . . . ? N5 C13 C14 C15 -6.6(9) . . . . ? N5 C13 C14 C19 173.9(6) . . . . ? C19 C14 C15 C16 -1.8(10) . . . . ? C13 C14 C15 C16 178.7(6) . . . . ? C14 C15 C16 C17 0.2(10) . . . . ? C15 C16 C17 C18 1.4(10) . . . . ? C15 C16 C17 C1 -174.9(6) . . . 3_666 ? C16 C17 C18 C19 -1.2(10) . . . . ? C1 C17 C18 C19 175.0(6) 3_666 . . . ? C17 C18 C19 C14 -0.5(10) . . . . ? C15 C14 C19 C18 1.9(10) . . . . ? C13 C14 C19 C18 -178.5(6) . . . . ? Er1 O1 C20 O2 -6.5(11) . . . . ? Er1 O1 C20 C21 175.7(5) . . . . ? O1 C20 C21 C26 -5.3(9) . . . . ? O2 C20 C21 C26 176.7(6) . . . . ? O1 C20 C21 C22 171.7(6) . . . . ? O2 C20 C21 C22 -6.4(9) . . . . ? C26 C21 C22 C23 1.7(9) . . . . ? C20 C21 C22 C23 -175.2(6) . . . . ? C21 C22 C23 C24 -1.8(10) . . . . ? C22 C23 C24 C25 0.6(10) . . . . ? C22 C23 C24 C27 178.5(6) . . . . ? C23 C24 C25 C26 0.8(10) . . . . ? C27 C24 C25 C26 -177.2(6) . . . . ? C22 C21 C26 C25 -0.4(10) . . . . ? C20 C21 C26 C25 176.6(6) . . . . ? C24 C25 C26 C21 -0.9(10) . . . . ? C25 C24 C27 O3 -8.6(11) . . . . ? C23 C24 C27 O3 173.4(7) . . . . ? C25 C24 C27 O4 171.6(7) . . . . ? C23 C24 C27 O4 -6.3(10) . . . . ? Er1 O5 C28 O6 3.1(10) . . . . ? Er1 O5 C28 C29 -177.3(4) . . . . ? O6 C28 C29 C34 165.3(6) . . . . ? O5 C28 C29 C34 -14.3(9) . . . . ? O6 C28 C29 C30 -13.1(10) . . . . ? O5 C28 C29 C30 167.3(6) . . . . ? C34 C29 C30 C31 0.5(11) . . . . ? C28 C29 C30 C31 178.9(7) . . . . ? C29 C30 C31 C32 -1.8(12) . . . . ? C30 C31 C32 C33 1.1(12) . . . . ? C30 C31 C32 C35 -178.7(7) . . . . ? C31 C32 C33 C34 0.9(11) . . . . ? C35 C32 C33 C34 -179.3(7) . . . . ? C30 C29 C34 C33 1.4(10) . . . . ? C28 C29 C34 C33 -177.0(6) . . . . ? C32 C33 C34 C29 -2.1(10) . . . . ? C31 C32 C35 O8 -4.7(12) . . . . ? C33 C32 C35 O8 175.6(8) . . . . ? C31 C32 C35 O7 173.9(7) . . . . ? C33 C32 C35 O7 -5.8(11) . . . . ? Er1 O10 C36 O9 8.7(6) . . . . ? Er1 O10 C36 C37 -171.4(5) . . . . ? Er1 O9 C36 O10 -9.3(6) . . . . ? Er1 O9 C36 C37 170.8(5) . . . . ? O5 Er1 C36 O10 -65(3) . . . . ? O1 Er1 C36 O10 142.4(3) . . . . ? O3W Er1 C36 O10 71.5(3) . . . . ? O4W Er1 C36 O10 -3.6(4) . . . . ? O1W Er1 C36 O10 -77.0(3) . . . . ? O2W Er1 C36 O10 -145.7(3) . . . . ? O9 Er1 C36 O10 171.0(6) . . . . ? O5 Er1 C36 O9 124(3) . . . . ? O1 Er1 C36 O9 -28.6(4) . . . . ? O3W Er1 C36 O9 -99.5(4) . . . . ? O4W Er1 C36 O9 -174.6(3) . . . . ? O1W Er1 C36 O9 111.9(4) . . . . ? O2W Er1 C36 O9 43.3(4) . . . . ? O10 Er1 C36 O9 -171.0(6) . . . . ? O5 Er1 C36 C37 61(5) . . . . ? O1 Er1 C36 C37 -91(3) . . . . ? O3W Er1 C36 C37 -162(3) . . . . ? O4W Er1 C36 C37 123(3) . . . . ? O1W Er1 C36 C37 49(3) . . . . ? O2W Er1 C36 C37 -19(3) . . . . ? O9 Er1 C36 C37 -63(3) . . . . ? O10 Er1 C36 C37 126(3) . . . . ? O10 C36 C37 C38 8.5(9) . . . . ? O9 C36 C37 C38 -171.6(6) . . . . ? Er1 C36 C37 C38 -114(3) . . . . ? O10 C36 C37 C39 -172.7(6) . . . 3_666 ? O9 C36 C37 C39 7.2(9) . . . 3_666 ? Er1 C36 C37 C39 65(3) . . . 3_666 ? C39 C37 C38 C39 0.5(10) 3_666 . . . ? C36 C37 C38 C39 179.3(6) . . . . ? C37 C38 C39 C37 -0.5(10) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.831 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.137 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.205 0.484 0.932 76 25 ' ' 2 0.295 -0.016 0.568 76 25 ' ' 3 0.713 0.017 0.429 73 24 ' ' 4 0.787 0.517 0.071 73 24 ' ' _platon_squeeze_details ; DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group. Number of moved primary input atoms: 89. Number of unusual anisotropic displacement parameters: 2. Total Potential Solvent Accessible Void Vol: 298.9 Ang**3 Electron Count / Cell = 98 - To be included in D(calc), F000 & Mol.Wght. ; _publ_section_references ; ; # start Validation Reply Form _vrf_PUBL018_GLOBAL ; PROBLEM: The author field is longer than 65 characters. RESPONSE: It is the exact author list. ; _vrf_PUBL019_GLOBAL ; PROBLEM: The author field is longer than 8 words. RESPONSE: It is the exact author list. ; _vrf_PUBL021_GLOBAL ; PROBLEM: There is more than one comma in the author field. RESPONSE: It is the exact author list. ; _vrf_PLAT306_I ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O5W RESPONSE: It is because of the disorder of the H-atoms on water solvent. ; data_RSOF-Lu _database_code_depnum_ccdc_archive 'CCDC 824441' #TrackingRef '- RSOF-Lu as CCDC 824441.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; cyclo(2)(2,6-di(1H-imidazol-1-yl)pyridine)(2)(1,4- dimethylenebenzene) _ 5 terephthalate dianion_ 2 lutetium(iii)_8 H2O_22 H2O ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H114 Lu2 N10 O50' _chemical_formula_weight 2341.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.167(2) _cell_length_b 17.820(4) _cell_length_c 24.502(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.33(3) _cell_angle_gamma 90.00 _cell_volume 4811.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8134 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 2.144 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6544 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35963 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8134 _reflns_number_gt 7662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+65.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8134 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1370 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.81136(3) 0.698899(16) 0.634714(11) 0.01741(11) Uani 1 1 d . . . O1 O 0.7046(5) 0.7192(3) 0.70519(19) 0.0245(11) Uani 1 1 d . . . O1W O 0.9316(5) 0.6095(3) 0.6051(2) 0.0263(11) Uani 1 1 d . . . O2W O 0.8801(4) 0.6180(3) 0.71013(18) 0.0217(10) Uani 1 1 d . . . O2 O 0.5449(5) 0.7953(3) 0.6869(2) 0.0341(13) Uani 1 1 d . . . O3W O 0.6772(5) 0.7927(3) 0.6069(2) 0.0301(12) Uani 1 1 d . . . O3 O 0.5753(5) 0.6515(3) 0.9686(2) 0.0348(13) Uani 1 1 d . . . O4 O 0.4582(5) 0.7524(3) 0.9636(2) 0.0270(12) Uani 1 1 d . . . O4W O 0.9088(5) 0.7652(3) 0.57218(19) 0.0247(11) Uani 1 1 d . . . O5 O 0.9569(4) 0.7695(3) 0.68506(19) 0.0228(11) Uani 1 1 d . . . O5W O 1.4755(5) 0.8975(3) 0.9998(2) 0.0311(12) Uani 1 1 d . . . O6 O 0.9659(5) 0.7371(3) 0.77375(19) 0.0254(11) Uani 1 1 d . . . O6W O 1.0963(6) 0.6692(4) 0.8654(2) 0.0465(16) Uani 1 1 d . . . O7 O 1.4437(5) 1.0160(3) 0.7617(2) 0.0292(12) Uani 1 1 d . . . O7W O 0.7117(6) 0.7293(5) 0.4407(3) 0.071(3) Uani 1 1 d . . . O8 O 1.3936(5) 1.0241(3) 0.8450(2) 0.0403(15) Uani 1 1 d . . . O8W O 1.3404(5) 1.0098(3) 0.9477(2) 0.0361(13) Uani 1 1 d . . . O9 O 0.6561(4) 0.6115(3) 0.61552(18) 0.0199(10) Uani 1 1 d . . . O9W O 0.4959(8) 0.9468(6) 0.6701(4) 0.084(3) Uani 1 1 d . . . O10 O 0.7140(4) 0.6561(3) 0.54056(18) 0.0200(10) Uani 1 1 d . . . O10W O 1.0927(6) 0.9879(4) 0.4194(3) 0.0468(16) Uani 1 1 d . . . O11W O 0.6831(10) 1.0867(7) 0.4289(5) 0.109(4) Uani 1 1 d . . . O12W O 0.9529(6) 1.1092(3) 0.4272(2) 0.0444(16) Uani 1 1 d . . . O13W O 0.6221(8) 0.8686(6) 0.5139(3) 0.093(3) Uani 1 1 d . . . O14W O 0.6693(12) 1.0090(8) 0.5196(9) 0.200(9) Uani 1 1 d . . . O15W O 0.5981(16) 1.0559(13) 0.6124(5) 0.252(13) Uani 1 1 d . . . N1 N 0.7167(5) 0.4556(3) 0.7213(2) 0.0226(13) Uani 1 1 d . . . N2 N 0.5696(5) 0.5151(3) 0.7503(2) 0.0196(12) Uani 1 1 d . . . N3 N 0.4342(5) 0.5962(3) 0.6993(2) 0.0209(12) Uani 1 1 d . . . N4 N 0.3105(5) 0.6757(4) 0.6414(2) 0.0232(13) Uani 1 1 d . . . N5 N 0.3376(5) 0.7183(3) 0.5617(2) 0.0237(13) Uani 1 1 d . . . C1 C 0.8035(7) 0.4327(4) 0.6852(3) 0.0256(16) Uani 1 1 d . . . H1A H 0.8638 0.3998 0.7058 0.031 Uiso 1 1 calc R . . H1B H 0.8452 0.4769 0.6748 0.031 Uiso 1 1 calc R . . C2 C 0.6329(6) 0.5086(4) 0.7085(3) 0.0219(15) Uani 1 1 d . . . H2A H 0.6204 0.5364 0.6760 0.026 Uiso 1 1 calc R . . C3 C 0.7075(8) 0.4280(5) 0.7735(3) 0.0327(18) Uani 1 1 d . . . H3A H 0.7551 0.3905 0.7926 0.039 Uiso 1 1 calc R . . C4 C 0.6163(7) 0.4658(5) 0.7914(3) 0.0285(17) Uani 1 1 d . . . H4A H 0.5900 0.4596 0.8252 0.034 Uiso 1 1 calc R . . C5 C 0.4681(6) 0.5641(4) 0.7484(3) 0.0213(15) Uani 1 1 d . . . C6 C 0.4108(7) 0.5749(4) 0.7938(3) 0.0261(16) Uani 1 1 d . . . H6A H 0.4388 0.5522 0.8276 0.031 Uiso 1 1 calc R . . C7 C 0.3100(7) 0.6211(4) 0.7864(3) 0.0293(17) Uani 1 1 d . . . H7A H 0.2678 0.6291 0.8156 0.035 Uiso 1 1 calc R . . C8 C 0.2716(7) 0.6554(4) 0.7361(3) 0.0275(17) Uani 1 1 d . . . H8A H 0.2038 0.6865 0.7304 0.033 Uiso 1 1 calc R . . C9 C 0.3391(6) 0.6410(4) 0.6948(3) 0.0220(15) Uani 1 1 d . . . C10 C 0.3904(6) 0.6820(4) 0.6067(3) 0.0218(15) Uani 1 1 d . . . H10A H 0.4697 0.6640 0.6128 0.026 Uiso 1 1 calc R . . C11 C 0.2020(7) 0.7100(4) 0.6184(3) 0.0265(17) Uani 1 1 d . . . H11A H 0.1318 0.7140 0.6341 0.032 Uiso 1 1 calc R . . C12 C 0.2199(6) 0.7364(5) 0.5685(3) 0.0274(17) Uani 1 1 d . . . H12A H 0.1634 0.7621 0.5433 0.033 Uiso 1 1 calc R . . C13 C 0.3939(7) 0.7353(4) 0.5134(3) 0.0256(16) Uani 1 1 d . . . H13A H 0.4806 0.7268 0.5226 0.031 Uiso 1 1 calc R . . H13B H 0.3815 0.7880 0.5043 0.031 Uiso 1 1 calc R . . C14 C 0.3446(6) 0.6887(4) 0.4629(3) 0.0217(15) Uani 1 1 d . . . C15 C 0.2697(7) 0.6271(4) 0.4651(3) 0.0272(16) Uani 1 1 d . . . H15A H 0.2498 0.6122 0.4989 0.033 Uiso 1 1 calc R . . C16 C 0.2243(7) 0.5876(4) 0.4175(3) 0.0261(16) Uani 1 1 d . . . H16A H 0.1722 0.5474 0.4196 0.031 Uiso 1 1 calc R . . C17 C 0.2557(6) 0.6073(4) 0.3666(3) 0.0223(15) Uani 1 1 d . . . C18 C 0.3336(6) 0.6676(4) 0.3649(3) 0.0230(15) Uani 1 1 d . . . H18A H 0.3570 0.6812 0.3316 0.028 Uiso 1 1 calc R . . C19 C 0.3767(7) 0.7078(4) 0.4124(3) 0.0250(16) Uani 1 1 d . . . H19A H 0.4283 0.7483 0.4103 0.030 Uiso 1 1 calc R . . C20 C 0.6142(6) 0.7524(4) 0.7185(3) 0.0202(15) Uani 1 1 d . . . C21 C 0.5883(6) 0.7401(4) 0.7764(3) 0.0200(14) Uani 1 1 d . . . C22 C 0.4953(6) 0.7777(4) 0.7955(3) 0.0216(15) Uani 1 1 d . . . H22A H 0.4454 0.8097 0.7720 0.026 Uiso 1 1 calc R . . C23 C 0.4760(6) 0.7680(4) 0.8494(3) 0.0218(15) Uani 1 1 d . . . H23A H 0.4146 0.7947 0.8622 0.026 Uiso 1 1 calc R . . C24 C 0.5472(6) 0.7187(4) 0.8847(3) 0.0223(15) Uani 1 1 d . . . C25 C 0.6419(6) 0.6805(4) 0.8653(3) 0.0220(15) Uani 1 1 d . . . H25A H 0.6910 0.6478 0.8886 0.026 Uiso 1 1 calc R . . C26 C 0.6623(6) 0.6911(4) 0.8118(3) 0.0205(15) Uani 1 1 d . . . H26A H 0.7252 0.6658 0.7992 0.025 Uiso 1 1 calc R . . C27 C 0.5250(7) 0.7063(4) 0.9432(3) 0.0229(15) Uani 1 1 d . . . C28 C 0.9987(6) 0.7764(4) 0.7364(3) 0.0197(15) Uani 1 1 d . . . C29 C 1.0948(6) 0.8348(4) 0.7520(3) 0.0196(14) Uani 1 1 d . . . C30 C 1.1291(7) 0.8551(4) 0.8071(3) 0.0260(16) Uani 1 1 d . . . H30A H 1.0918 0.8329 0.8344 0.031 Uiso 1 1 calc R . . C31 C 1.2200(7) 0.9093(4) 0.8217(3) 0.0258(16) Uani 1 1 d . . . H31A H 1.2403 0.9246 0.8584 0.031 Uiso 1 1 calc R . . C32 C 1.2797(6) 0.9402(4) 0.7816(3) 0.0239(16) Uani 1 1 d . . . C33 C 1.2453(7) 0.9189(4) 0.7267(3) 0.0262(16) Uani 1 1 d . . . H33A H 1.2851 0.9393 0.6996 0.031 Uiso 1 1 calc R . . C34 C 1.1527(7) 0.8676(4) 0.7117(3) 0.0235(15) Uani 1 1 d . . . H34A H 1.1291 0.8550 0.6747 0.028 Uiso 1 1 calc R . . C35 C 1.3811(7) 0.9980(4) 0.7970(3) 0.0255(16) Uani 1 1 d . . . C36 C 0.6522(6) 0.6103(4) 0.5634(3) 0.0199(15) Uani 1 1 d . . . C37 C 0.5711(6) 0.5540(4) 0.5299(3) 0.0213(15) Uani 1 1 d . . . C38 C 0.5785(6) 0.5439(4) 0.4744(3) 0.0220(15) Uani 1 1 d . . . H38A H 0.6308 0.5733 0.4576 0.026 Uiso 1 1 calc R . . C39 C 0.5070(6) 0.4896(4) 0.4444(3) 0.0207(15) Uani 1 1 d . . . H39A H 0.5112 0.4824 0.4072 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01578(17) 0.02157(19) 0.01471(15) -0.00144(11) 0.00197(11) -0.00130(12) O1 0.024(3) 0.035(3) 0.016(2) 0.000(2) 0.008(2) 0.006(2) O1W 0.024(3) 0.031(3) 0.024(3) 0.002(2) 0.005(2) 0.008(2) O2W 0.020(3) 0.026(3) 0.019(2) 0.0006(19) 0.0038(19) 0.001(2) O2 0.031(3) 0.047(4) 0.026(3) 0.011(2) 0.010(2) 0.013(3) O3W 0.037(3) 0.030(3) 0.025(3) 0.005(2) 0.011(2) 0.012(2) O3 0.047(4) 0.036(3) 0.024(3) 0.004(2) 0.012(2) 0.008(3) O4 0.029(3) 0.033(3) 0.020(2) -0.002(2) 0.009(2) 0.001(2) O4W 0.027(3) 0.032(3) 0.017(2) 0.001(2) 0.009(2) -0.009(2) O5 0.025(3) 0.025(3) 0.017(2) -0.007(2) 0.001(2) -0.007(2) O5W 0.033(3) 0.037(3) 0.026(3) -0.005(2) 0.011(2) -0.011(3) O6 0.026(3) 0.031(3) 0.020(2) -0.005(2) 0.005(2) -0.008(2) O6W 0.051(4) 0.052(4) 0.037(3) 0.000(3) 0.007(3) 0.005(3) O7 0.024(3) 0.032(3) 0.031(3) -0.002(2) 0.002(2) -0.007(2) O7W 0.035(4) 0.127(7) 0.048(4) 0.051(4) -0.002(3) -0.010(4) O8 0.043(4) 0.050(4) 0.026(3) -0.003(3) 0.003(2) -0.024(3) O8W 0.034(3) 0.043(4) 0.034(3) -0.002(3) 0.014(2) -0.006(3) O9 0.014(2) 0.026(3) 0.020(2) -0.0014(19) 0.0010(18) -0.006(2) O9W 0.074(6) 0.101(7) 0.081(6) 0.001(5) 0.027(5) -0.008(5) O10 0.017(2) 0.026(3) 0.017(2) -0.0017(19) 0.0011(18) -0.007(2) O10W 0.057(4) 0.045(4) 0.040(3) 0.003(3) 0.011(3) 0.002(3) O11W 0.098(8) 0.126(9) 0.102(8) -0.003(7) 0.012(6) 0.008(7) O12W 0.070(5) 0.036(3) 0.029(3) 0.000(2) 0.013(3) 0.004(3) O13W 0.072(6) 0.152(9) 0.061(5) 0.059(6) 0.024(4) 0.033(6) O14W 0.090(9) 0.124(11) 0.40(3) -0.094(14) 0.087(13) -0.026(8) O15W 0.255(18) 0.42(3) 0.062(7) 0.046(11) -0.019(9) -0.28(2) N1 0.024(3) 0.021(3) 0.022(3) -0.003(2) 0.001(2) -0.002(3) N2 0.018(3) 0.022(3) 0.019(3) 0.001(2) 0.003(2) 0.002(2) N3 0.014(3) 0.027(3) 0.021(3) -0.003(2) 0.001(2) -0.003(3) N4 0.020(3) 0.027(3) 0.022(3) -0.004(2) 0.001(2) 0.002(3) N5 0.020(3) 0.026(3) 0.023(3) -0.002(2) -0.001(2) 0.002(3) C1 0.023(4) 0.025(4) 0.029(4) -0.006(3) 0.004(3) 0.002(3) C2 0.019(4) 0.022(4) 0.024(3) -0.001(3) 0.001(3) 0.000(3) C3 0.039(5) 0.031(4) 0.025(4) 0.003(3) -0.003(3) 0.006(4) C4 0.027(4) 0.038(5) 0.020(4) 0.003(3) 0.003(3) 0.004(3) C5 0.021(4) 0.020(4) 0.024(4) -0.005(3) 0.004(3) -0.006(3) C6 0.029(4) 0.026(4) 0.024(4) -0.004(3) 0.006(3) -0.008(3) C7 0.029(4) 0.033(4) 0.029(4) -0.009(3) 0.013(3) -0.005(3) C8 0.024(4) 0.028(4) 0.033(4) -0.009(3) 0.011(3) -0.003(3) C9 0.019(4) 0.024(4) 0.022(3) -0.005(3) -0.001(3) -0.007(3) C10 0.015(3) 0.027(4) 0.024(4) -0.002(3) 0.006(3) 0.001(3) C11 0.013(4) 0.033(4) 0.033(4) -0.007(3) 0.002(3) 0.009(3) C12 0.016(4) 0.038(5) 0.026(4) -0.006(3) 0.000(3) 0.007(3) C13 0.027(4) 0.030(4) 0.020(3) 0.001(3) 0.002(3) 0.002(3) C14 0.011(3) 0.028(4) 0.024(4) 0.001(3) -0.001(3) 0.003(3) C15 0.029(4) 0.029(4) 0.025(4) 0.000(3) 0.008(3) -0.002(3) C16 0.024(4) 0.025(4) 0.031(4) 0.001(3) 0.009(3) -0.003(3) C17 0.017(4) 0.024(4) 0.026(4) 0.002(3) 0.001(3) 0.002(3) C18 0.023(4) 0.025(4) 0.023(3) 0.002(3) 0.007(3) 0.002(3) C19 0.024(4) 0.026(4) 0.025(4) 0.004(3) 0.002(3) 0.002(3) C20 0.019(4) 0.023(4) 0.019(3) -0.003(3) 0.004(3) -0.003(3) C21 0.021(4) 0.018(4) 0.020(3) -0.003(3) 0.002(3) -0.004(3) C22 0.022(4) 0.022(4) 0.020(3) 0.002(3) 0.002(3) -0.001(3) C23 0.019(4) 0.024(4) 0.025(4) -0.004(3) 0.010(3) -0.001(3) C24 0.020(4) 0.027(4) 0.020(3) -0.005(3) 0.003(3) -0.006(3) C25 0.019(4) 0.024(4) 0.022(3) 0.001(3) 0.001(3) -0.004(3) C26 0.015(3) 0.027(4) 0.020(3) -0.006(3) 0.005(3) 0.000(3) C27 0.024(4) 0.024(4) 0.021(3) -0.001(3) 0.004(3) -0.005(3) C28 0.016(3) 0.024(4) 0.019(3) -0.003(3) 0.004(3) 0.002(3) C29 0.014(3) 0.023(4) 0.021(3) -0.005(3) -0.001(3) 0.001(3) C30 0.025(4) 0.028(4) 0.026(4) -0.006(3) 0.005(3) -0.006(3) C31 0.024(4) 0.029(4) 0.023(3) -0.007(3) 0.000(3) -0.003(3) C32 0.017(4) 0.024(4) 0.029(4) -0.001(3) -0.002(3) -0.001(3) C33 0.026(4) 0.028(4) 0.025(4) 0.003(3) 0.004(3) 0.000(3) C34 0.028(4) 0.022(4) 0.020(3) -0.001(3) 0.002(3) -0.005(3) C35 0.023(4) 0.025(4) 0.026(4) -0.003(3) -0.002(3) 0.003(3) C36 0.013(3) 0.026(4) 0.020(3) 0.002(3) 0.002(3) 0.003(3) C37 0.012(3) 0.028(4) 0.022(3) -0.002(3) 0.000(3) 0.005(3) C38 0.018(4) 0.025(4) 0.023(3) 0.002(3) 0.004(3) 0.000(3) C39 0.017(3) 0.025(4) 0.020(3) 0.000(3) 0.002(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O5 2.258(5) . ? Lu1 O3W 2.275(5) . ? Lu1 O1W 2.276(5) . ? Lu1 O1 2.281(5) . ? Lu1 O9 2.322(5) . ? Lu1 O4W 2.339(5) . ? Lu1 O2W 2.371(5) . ? Lu1 O10 2.504(4) . ? Lu1 C36 2.775(7) . ? O1 C20 1.257(9) . ? O2 C20 1.260(9) . ? O3 C27 1.242(9) . ? O4 C27 1.266(9) . ? O5 C28 1.275(8) . ? O6 C28 1.253(9) . ? O7 C35 1.241(9) . ? O8 C35 1.251(9) . ? O9 C36 1.271(8) . ? O10 C36 1.258(8) . ? N1 C2 1.330(9) . ? N1 C3 1.391(10) . ? N1 C1 1.471(9) . ? N2 C2 1.340(9) . ? N2 C4 1.373(9) . ? N2 C5 1.426(9) . ? N3 C9 1.320(9) . ? N3 C5 1.331(9) . ? N4 C10 1.334(9) . ? N4 C11 1.392(9) . ? N4 C9 1.436(9) . ? N5 C10 1.330(9) . ? N5 C12 1.389(9) . ? N5 C13 1.459(9) . ? C1 C17 1.512(10) 3_666 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 C4 1.352(11) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.384(10) . ? C6 C7 1.382(11) . ? C6 H6A 0.9300 . ? C7 C8 1.380(11) . ? C7 H7A 0.9300 . ? C8 C9 1.381(10) . ? C8 H8A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.354(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.517(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.385(10) . ? C14 C15 1.387(11) . ? C15 C16 1.386(10) . ? C15 H15A 0.9300 . ? C16 C17 1.393(10) . ? C16 H16A 0.9300 . ? C17 C18 1.388(10) . ? C17 C1 1.512(10) 3_666 ? C18 C19 1.383(10) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.510(9) . ? C21 C22 1.380(10) . ? C21 C26 1.401(10) . ? C22 C23 1.384(10) . ? C22 H22A 0.9300 . ? C23 C24 1.389(10) . ? C23 H23A 0.9300 . ? C24 C25 1.404(10) . ? C24 C27 1.511(10) . ? C25 C26 1.380(10) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 C29 1.499(10) . ? C29 C30 1.391(10) . ? C29 C34 1.393(10) . ? C30 C31 1.405(10) . ? C30 H30A 0.9300 . ? C31 C32 1.388(11) . ? C31 H31A 0.9300 . ? C32 C33 1.390(10) . ? C32 C35 1.532(10) . ? C33 C34 1.384(10) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C36 C37 1.503(10) . ? C37 C38 1.387(10) . ? C37 C39 1.392(10) 3_666 ? C38 C39 1.388(10) . ? C38 H38A 0.9300 . ? C39 C37 1.392(10) 3_666 ? C39 H39A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Lu1 O3W 97.76(19) . . ? O5 Lu1 O1W 98.87(18) . . ? O3W Lu1 O1W 144.36(17) . . ? O5 Lu1 O1 85.19(18) . . ? O3W Lu1 O1 73.19(18) . . ? O1W Lu1 O1 139.46(18) . . ? O5 Lu1 O9 158.84(17) . . ? O3W Lu1 O9 89.92(19) . . ? O1W Lu1 O9 85.74(18) . . ? O1 Lu1 O9 78.18(18) . . ? O5 Lu1 O4W 72.91(17) . . ? O3W Lu1 O4W 77.61(19) . . ? O1W Lu1 O4W 77.53(18) . . ? O1 Lu1 O4W 140.49(18) . . ? O9 Lu1 O4W 128.16(16) . . ? O5 Lu1 O2W 78.45(17) . . ? O3W Lu1 O2W 142.66(17) . . ? O1W Lu1 O2W 71.90(17) . . ? O1 Lu1 O2W 69.48(17) . . ? O9 Lu1 O2W 83.49(16) . . ? O4W Lu1 O2W 133.77(17) . . ? O5 Lu1 O10 147.08(16) . . ? O3W Lu1 O10 77.34(18) . . ? O1W Lu1 O10 71.59(17) . . ? O1 Lu1 O10 122.94(17) . . ? O9 Lu1 O10 53.90(15) . . ? O4W Lu1 O10 74.26(16) . . ? O2W Lu1 O10 124.76(16) . . ? O5 Lu1 C36 172.85(19) . . ? O3W Lu1 C36 84.6(2) . . ? O1W Lu1 C36 75.65(19) . . ? O1 Lu1 C36 101.96(19) . . ? O9 Lu1 C36 27.06(18) . . ? O4W Lu1 C36 101.15(18) . . ? O2W Lu1 C36 103.79(18) . . ? O10 Lu1 C36 26.94(18) . . ? C20 O1 Lu1 144.2(4) . . ? C28 O5 Lu1 135.2(5) . . ? C36 O9 Lu1 96.7(4) . . ? C36 O10 Lu1 88.6(4) . . ? C2 N1 C3 108.2(6) . . ? C2 N1 C1 124.2(6) . . ? C3 N1 C1 127.5(6) . . ? C2 N2 C4 108.7(6) . . ? C2 N2 C5 122.9(6) . . ? C4 N2 C5 128.4(6) . . ? C9 N3 C5 116.2(6) . . ? C10 N4 C11 109.5(6) . . ? C10 N4 C9 123.0(6) . . ? C11 N4 C9 127.4(6) . . ? C10 N5 C12 108.3(6) . . ? C10 N5 C13 125.5(6) . . ? C12 N5 C13 126.1(6) . . ? N1 C1 C17 113.2(6) . 3_666 ? N1 C1 H1A 108.9 . . ? C17 C1 H1A 108.9 3_666 . ? N1 C1 H1B 108.9 . . ? C17 C1 H1B 108.9 3_666 . ? H1A C1 H1B 107.7 . . ? N1 C2 N2 108.7(6) . . ? N1 C2 H2A 125.7 . . ? N2 C2 H2A 125.7 . . ? C4 C3 N1 107.0(7) . . ? C4 C3 H3A 126.5 . . ? N1 C3 H3A 126.5 . . ? C3 C4 N2 107.4(7) . . ? C3 C4 H4A 126.3 . . ? N2 C4 H4A 126.3 . . ? N3 C5 C6 124.5(7) . . ? N3 C5 N2 113.6(6) . . ? C6 C5 N2 121.8(6) . . ? C7 C6 C5 116.8(7) . . ? C7 C6 H6A 121.6 . . ? C5 C6 H6A 121.6 . . ? C8 C7 C6 120.6(7) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 116.4(7) . . ? C7 C8 H8A 121.8 . . ? C9 C8 H8A 121.8 . . ? N3 C9 C8 125.4(7) . . ? N3 C9 N4 113.1(6) . . ? C8 C9 N4 121.4(7) . . ? N5 C10 N4 108.4(6) . . ? N5 C10 H10A 125.8 . . ? N4 C10 H10A 125.8 . . ? C12 C11 N4 105.7(7) . . ? C12 C11 H11A 127.1 . . ? N4 C11 H11A 127.1 . . ? C11 C12 N5 108.0(6) . . ? C11 C12 H12A 126.0 . . ? N5 C12 H12A 126.0 . . ? N5 C13 C14 113.7(6) . . ? N5 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N5 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C19 C14 C15 118.3(7) . . ? C19 C14 C13 118.9(7) . . ? C15 C14 C13 122.8(7) . . ? C16 C15 C14 120.7(7) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 120.9(7) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C18 C17 C16 118.1(7) . . ? C18 C17 C1 122.1(6) . 3_666 ? C16 C17 C1 119.6(7) . 3_666 ? C19 C18 C17 120.7(7) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C14 121.2(7) . . ? C18 C19 H19A 119.4 . . ? C14 C19 H19A 119.4 . . ? O1 C20 O2 124.4(6) . . ? O1 C20 C21 117.4(6) . . ? O2 C20 C21 118.2(6) . . ? C22 C21 C26 119.5(6) . . ? C22 C21 C20 121.2(6) . . ? C26 C21 C20 119.3(6) . . ? C21 C22 C23 120.4(7) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C24 120.7(7) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C23 C24 C25 118.9(6) . . ? C23 C24 C27 121.2(7) . . ? C25 C24 C27 119.9(6) . . ? C26 C25 C24 120.3(7) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C21 120.2(7) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? O3 C27 O4 124.1(7) . . ? O3 C27 C24 117.4(7) . . ? O4 C27 C24 118.5(6) . . ? O6 C28 O5 124.3(6) . . ? O6 C28 C29 118.9(6) . . ? O5 C28 C29 116.8(6) . . ? C30 C29 C34 119.5(7) . . ? C30 C29 C28 120.1(7) . . ? C34 C29 C28 120.3(6) . . ? C29 C30 C31 120.0(7) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C32 C31 C30 120.1(7) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 119.2(7) . . ? C31 C32 C35 120.8(6) . . ? C33 C32 C35 120.0(7) . . ? C34 C33 C32 120.9(7) . . ? C34 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C33 C34 C29 120.1(6) . . ? C33 C34 H34A 119.9 . . ? C29 C34 H34A 119.9 . . ? O7 C35 O8 124.8(7) . . ? O7 C35 C32 118.6(6) . . ? O8 C35 C32 116.6(7) . . ? O10 C36 O9 120.3(6) . . ? O10 C36 C37 121.1(6) . . ? O9 C36 C37 118.6(6) . . ? O10 C36 Lu1 64.5(3) . . ? O9 C36 Lu1 56.2(3) . . ? C37 C36 Lu1 172.4(5) . . ? C38 C37 C39 120.8(7) . 3_666 ? C38 C37 C36 119.6(7) . . ? C39 C37 C36 119.5(6) 3_666 . ? C37 C38 C39 119.3(7) . . ? C37 C38 H38A 120.3 . . ? C39 C38 H38A 120.3 . . ? C38 C39 C37 119.9(7) . 3_666 ? C38 C39 H39A 120.1 . . ? C37 C39 H39A 120.1 3_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Lu1 O1 C20 110.3(8) . . . . ? O3W Lu1 O1 C20 10.7(8) . . . . ? O1W Lu1 O1 C20 -151.7(7) . . . . ? O9 Lu1 O1 C20 -82.9(8) . . . . ? O4W Lu1 O1 C20 54.7(9) . . . . ? O2W Lu1 O1 C20 -170.3(9) . . . . ? O10 Lu1 O1 C20 -51.4(9) . . . . ? C36 Lu1 O1 C20 -69.8(8) . . . . ? O3W Lu1 O5 C28 110.7(6) . . . . ? O1W Lu1 O5 C28 -100.9(6) . . . . ? O1 Lu1 O5 C28 38.4(6) . . . . ? O9 Lu1 O5 C28 0.3(10) . . . . ? O4W Lu1 O5 C28 -174.9(7) . . . . ? O2W Lu1 O5 C28 -31.6(6) . . . . ? O10 Lu1 O5 C28 -170.6(5) . . . . ? C36 Lu1 O5 C28 -140.6(14) . . . . ? O5 Lu1 O9 C36 -170.1(5) . . . . ? O3W Lu1 O9 C36 78.2(4) . . . . ? O1W Lu1 O9 C36 -66.4(4) . . . . ? O1 Lu1 O9 C36 151.0(4) . . . . ? O4W Lu1 O9 C36 4.1(5) . . . . ? O2W Lu1 O9 C36 -138.6(4) . . . . ? O10 Lu1 O9 C36 3.9(4) . . . . ? O5 Lu1 O10 C36 172.1(4) . . . . ? O3W Lu1 O10 C36 -103.2(4) . . . . ? O1W Lu1 O10 C36 94.5(4) . . . . ? O1 Lu1 O10 C36 -43.1(4) . . . . ? O9 Lu1 O10 C36 -3.9(4) . . . . ? O4W Lu1 O10 C36 176.3(4) . . . . ? O2W Lu1 O10 C36 43.5(4) . . . . ? C2 N1 C1 C17 -68.4(9) . . . 3_666 ? C3 N1 C1 C17 112.5(8) . . . 3_666 ? C3 N1 C2 N2 -0.8(8) . . . . ? C1 N1 C2 N2 179.9(6) . . . . ? C4 N2 C2 N1 1.3(8) . . . . ? C5 N2 C2 N1 -176.3(6) . . . . ? C2 N1 C3 C4 0.0(9) . . . . ? C1 N1 C3 C4 179.3(7) . . . . ? N1 C3 C4 N2 0.7(9) . . . . ? C2 N2 C4 C3 -1.2(9) . . . . ? C5 N2 C4 C3 176.1(7) . . . . ? C9 N3 C5 C6 0.0(10) . . . . ? C9 N3 C5 N2 178.7(6) . . . . ? C2 N2 C5 N3 7.0(9) . . . . ? C4 N2 C5 N3 -170.0(7) . . . . ? C2 N2 C5 C6 -174.2(7) . . . . ? C4 N2 C5 C6 8.8(11) . . . . ? N3 C5 C6 C7 1.4(11) . . . . ? N2 C5 C6 C7 -177.2(6) . . . . ? C5 C6 C7 C8 -1.3(11) . . . . ? C6 C7 C8 C9 -0.2(11) . . . . ? C5 N3 C9 C8 -1.7(10) . . . . ? C5 N3 C9 N4 177.9(6) . . . . ? C7 C8 C9 N3 1.8(11) . . . . ? C7 C8 C9 N4 -177.7(7) . . . . ? C10 N4 C9 N3 -20.3(10) . . . . ? C11 N4 C9 N3 162.6(7) . . . . ? C10 N4 C9 C8 159.3(7) . . . . ? C11 N4 C9 C8 -17.8(11) . . . . ? C12 N5 C10 N4 0.6(8) . . . . ? C13 N5 C10 N4 -178.7(6) . . . . ? C11 N4 C10 N5 -0.7(8) . . . . ? C9 N4 C10 N5 -178.2(6) . . . . ? C10 N4 C11 C12 0.5(8) . . . . ? C9 N4 C11 C12 177.9(7) . . . . ? N4 C11 C12 N5 -0.2(8) . . . . ? C10 N5 C12 C11 -0.2(9) . . . . ? C13 N5 C12 C11 179.0(7) . . . . ? C10 N5 C13 C14 107.9(8) . . . . ? C12 N5 C13 C14 -71.2(9) . . . . ? N5 C13 C14 C19 169.9(6) . . . . ? N5 C13 C14 C15 -11.0(10) . . . . ? C19 C14 C15 C16 -2.6(11) . . . . ? C13 C14 C15 C16 178.2(7) . . . . ? C14 C15 C16 C17 2.0(12) . . . . ? C15 C16 C17 C18 -0.1(11) . . . . ? C15 C16 C17 C1 -174.9(7) . . . 3_666 ? C16 C17 C18 C19 -1.2(11) . . . . ? C1 C17 C18 C19 173.4(7) 3_666 . . . ? C17 C18 C19 C14 0.5(11) . . . . ? C15 C14 C19 C18 1.3(11) . . . . ? C13 C14 C19 C18 -179.5(7) . . . . ? Lu1 O1 C20 O2 -2.6(13) . . . . ? Lu1 O1 C20 C21 178.1(5) . . . . ? O1 C20 C21 C22 176.1(6) . . . . ? O2 C20 C21 C22 -3.3(10) . . . . ? O1 C20 C21 C26 -2.2(10) . . . . ? O2 C20 C21 C26 178.4(7) . . . . ? C26 C21 C22 C23 0.8(10) . . . . ? C20 C21 C22 C23 -177.4(6) . . . . ? C21 C22 C23 C24 -1.9(11) . . . . ? C22 C23 C24 C25 1.9(11) . . . . ? C22 C23 C24 C27 -178.5(7) . . . . ? C23 C24 C25 C26 -0.9(10) . . . . ? C27 C24 C25 C26 179.6(6) . . . . ? C24 C25 C26 C21 -0.2(11) . . . . ? C22 C21 C26 C25 0.2(10) . . . . ? C20 C21 C26 C25 178.5(6) . . . . ? C23 C24 C27 O3 166.2(7) . . . . ? C25 C24 C27 O3 -14.3(10) . . . . ? C23 C24 C27 O4 -14.7(10) . . . . ? C25 C24 C27 O4 164.8(7) . . . . ? Lu1 O5 C28 O6 4.1(11) . . . . ? Lu1 O5 C28 C29 -177.1(4) . . . . ? O6 C28 C29 C30 -12.8(10) . . . . ? O5 C28 C29 C30 168.4(7) . . . . ? O6 C28 C29 C34 165.5(7) . . . . ? O5 C28 C29 C34 -13.3(10) . . . . ? C34 C29 C30 C31 1.1(11) . . . . ? C28 C29 C30 C31 179.4(7) . . . . ? C29 C30 C31 C32 -2.9(11) . . . . ? C30 C31 C32 C33 2.3(11) . . . . ? C30 C31 C32 C35 -178.6(7) . . . . ? C31 C32 C33 C34 0.1(11) . . . . ? C35 C32 C33 C34 -179.0(7) . . . . ? C32 C33 C34 C29 -1.9(11) . . . . ? C30 C29 C34 C33 1.3(11) . . . . ? C28 C29 C34 C33 -177.0(7) . . . . ? C31 C32 C35 O7 169.7(7) . . . . ? C33 C32 C35 O7 -11.3(11) . . . . ? C31 C32 C35 O8 -10.8(11) . . . . ? C33 C32 C35 O8 168.3(7) . . . . ? Lu1 O10 C36 O9 6.6(6) . . . . ? Lu1 O10 C36 C37 -174.2(6) . . . . ? Lu1 O9 C36 O10 -7.2(7) . . . . ? Lu1 O9 C36 C37 173.6(5) . . . . ? O5 Lu1 C36 O10 -37.0(17) . . . . ? O3W Lu1 C36 O10 72.6(4) . . . . ? O1W Lu1 C36 O10 -77.5(4) . . . . ? O1 Lu1 C36 O10 144.1(4) . . . . ? O9 Lu1 C36 O10 173.1(7) . . . . ? O4W Lu1 C36 O10 -3.6(4) . . . . ? O2W Lu1 C36 O10 -144.4(4) . . . . ? O5 Lu1 C36 O9 150.0(14) . . . . ? O3W Lu1 C36 O9 -100.5(4) . . . . ? O1W Lu1 C36 O9 109.4(4) . . . . ? O1 Lu1 C36 O9 -29.0(4) . . . . ? O4W Lu1 C36 O9 -176.7(4) . . . . ? O2W Lu1 C36 O9 42.5(4) . . . . ? O10 Lu1 C36 O9 -173.1(7) . . . . ? O5 Lu1 C36 C37 102(4) . . . . ? O3W Lu1 C36 C37 -148(4) . . . . ? O1W Lu1 C36 C37 61(4) . . . . ? O1 Lu1 C36 C37 -77(4) . . . . ? O9 Lu1 C36 C37 -48(4) . . . . ? O4W Lu1 C36 C37 135(4) . . . . ? O2W Lu1 C36 C37 -5(4) . . . . ? O10 Lu1 C36 C37 139(4) . . . . ? O10 C36 C37 C38 10.4(10) . . . . ? O9 C36 C37 C38 -170.5(6) . . . . ? Lu1 C36 C37 C38 -126(3) . . . . ? O10 C36 C37 C39 -172.3(6) . . . 3_666 ? O9 C36 C37 C39 6.9(10) . . . 3_666 ? Lu1 C36 C37 C39 52(4) . . . 3_666 ? C39 C37 C38 C39 0.0(12) 3_666 . . . ? C36 C37 C38 C39 177.3(6) . . . . ? C37 C38 C39 C37 0.0(11) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 2.576 _refine_diff_density_min -1.776 _refine_diff_density_rms 0.164 # Attachment '- RSOF-Y as CCDC 824442.CIF' data_RSOF-Y _database_code_depnum_ccdc_archive 'CCDC 824442' #TrackingRef '- RSOF-Y as CCDC 824442.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; cyclo(2)(2,6-di(1H-imidazol-1-yl)pyridine)(2)(1,4- dimethylenebenzene)_ 5 terephthalate dianion_ 2 yttrium(iii)_8 H2O_31 H2O ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H132 N10 O59 Y2' _chemical_formula_weight 2331.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.288(5) _cell_length_b 17.608(7) _cell_length_c 24.405(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.315(5) _cell_angle_gamma 90.00 _cell_volume 4800(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8244 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6909 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method dtintegrate.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34857 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8180 _reflns_number_gt 4979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8180 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.2647 _refine_ls_wR_factor_gt 0.2404 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.81401(6) 0.69910(4) 0.63486(3) 0.0398(3) Uani 1 1 d . . . O1 O 0.7060(4) 0.7164(3) 0.70758(19) 0.0475(13) Uani 1 1 d . . . O1W O 0.9317(4) 0.6054(3) 0.5989(2) 0.0560(14) Uani 1 1 d . . . O2W O 0.8833(4) 0.6126(3) 0.70865(19) 0.0488(13) Uani 1 1 d . . . O2 O 0.5413(5) 0.7894(3) 0.6893(2) 0.0559(14) Uani 1 1 d . . . O3W O 0.6785(5) 0.7989(3) 0.6104(2) 0.0514(13) Uani 1 1 d . . . O3 O 0.5939(6) 0.6526(4) 0.9770(2) 0.0791(19) Uani 1 1 d . . . O4 O 0.4608(5) 0.7480(3) 0.9689(2) 0.0600(15) Uani 1 1 d . . . O4W O 0.9151(4) 0.7730(3) 0.5740(2) 0.0510(13) Uani 1 1 d . . . O5 O 0.9613(4) 0.7679(3) 0.68920(19) 0.0499(13) Uani 1 1 d . . . O5W O 1.4625(7) 0.9010(4) 0.9917(3) 0.099(3) Uani 1 1 d . . . O6 O 0.9671(5) 0.7290(3) 0.7773(2) 0.0566(14) Uani 1 1 d . . . O6W O 1.0899(6) 0.6595(4) 0.8691(3) 0.093(2) Uani 1 1 d . . . O7 O 1.4427(6) 1.0118(4) 0.7716(4) 0.091(2) Uani 1 1 d . . . O7W O 0.7155(5) 0.7436(5) 0.4448(2) 0.095(2) Uani 1 1 d . . . O8 O 1.3993(6) 1.0128(5) 0.8575(4) 0.132(4) Uani 1 1 d . . . O8W O 1.3440(9) 1.0082(6) 0.9482(4) 0.151(3) Uiso 1 1 d . . . O9 O 0.6549(4) 0.6106(3) 0.61606(18) 0.0396(11) Uani 1 1 d . . . O10 O 0.7126(4) 0.6577(3) 0.54104(18) 0.0432(12) Uani 1 1 d . . . N1 N 0.7168(5) 0.4495(3) 0.7201(2) 0.0448(15) Uani 1 1 d . . . N2 N 0.5715(5) 0.5085(3) 0.7516(2) 0.0416(14) Uani 1 1 d . . . N3 N 0.4341(5) 0.5895(3) 0.7035(2) 0.0422(14) Uani 1 1 d . . . N4 N 0.3100(5) 0.6702(4) 0.6482(2) 0.0451(15) Uani 1 1 d . . . N5 N 0.3337(5) 0.7169(3) 0.5675(2) 0.0454(15) Uani 1 1 d . . . C1 C 0.8023(6) 0.4296(4) 0.6818(3) 0.0479(18) Uani 1 1 d . . . H1A H 0.8640 0.3972 0.7013 0.058 Uiso 1 1 calc R . . H1B H 0.8407 0.4757 0.6717 0.058 Uiso 1 1 calc R . . C2 C 0.6318(6) 0.5028(4) 0.7089(3) 0.0438(17) Uani 1 1 d . . . H2A H 0.6174 0.5312 0.6764 0.053 Uiso 1 1 calc R . . C3 C 0.7073(8) 0.4192(5) 0.7719(3) 0.067(3) Uani 1 1 d . . . H3A H 0.7545 0.3805 0.7895 0.081 Uiso 1 1 calc R . . C4 C 0.6193(8) 0.4548(5) 0.7919(3) 0.064(2) Uani 1 1 d . . . H4A H 0.5940 0.4462 0.8259 0.077 Uiso 1 1 calc R . . C5 C 0.4685(7) 0.5573(4) 0.7526(3) 0.0482(19) Uani 1 1 d . . . C6 C 0.4132(7) 0.5654(5) 0.7984(3) 0.056(2) Uani 1 1 d . . . H6A H 0.4405 0.5404 0.8315 0.067 Uiso 1 1 calc R . . C7 C 0.3138(7) 0.6128(5) 0.7930(3) 0.053(2) Uani 1 1 d . . . H7A H 0.2743 0.6217 0.8233 0.064 Uiso 1 1 calc R . . C8 C 0.2742(7) 0.6464(5) 0.7437(3) 0.055(2) Uani 1 1 d . . . H8A H 0.2058 0.6765 0.7392 0.067 Uiso 1 1 calc R . . C9 C 0.3385(6) 0.6344(4) 0.7000(3) 0.0453(18) Uani 1 1 d . . . C10 C 0.3880(7) 0.6793(4) 0.6114(3) 0.0469(19) Uani 1 1 d . . . H10A H 0.4667 0.6622 0.6161 0.056 Uiso 1 1 calc R . . C11 C 0.2025(7) 0.7075(5) 0.6252(3) 0.056(2) Uani 1 1 d . . . H11A H 0.1333 0.7119 0.6416 0.067 Uiso 1 1 calc R . . C12 C 0.2188(7) 0.7353(5) 0.5758(3) 0.059(2) Uani 1 1 d . . . H12A H 0.1629 0.7621 0.5515 0.070 Uiso 1 1 calc R . . C13 C 0.3887(7) 0.7380(5) 0.5188(3) 0.0523(19) Uani 1 1 d . . . H13A H 0.4748 0.7321 0.5273 0.063 Uiso 1 1 calc R . . H13B H 0.3719 0.7910 0.5101 0.063 Uiso 1 1 calc R . . C14 C 0.3423(6) 0.6894(4) 0.4679(3) 0.0470(18) Uani 1 1 d . . . C15 C 0.2619(7) 0.6287(4) 0.4692(3) 0.053(2) Uani 1 1 d . . . H15A H 0.2367 0.6146 0.5024 0.063 Uiso 1 1 calc R . . C16 C 0.2207(7) 0.5903(4) 0.4210(3) 0.0506(19) Uani 1 1 d . . . H16A H 0.1695 0.5492 0.4225 0.061 Uiso 1 1 calc R . . C17 C 0.2527(6) 0.6107(4) 0.3710(3) 0.0454(18) Uani 1 1 d . . . C18 C 0.3342(7) 0.6732(4) 0.3687(3) 0.0532(19) Uani 1 1 d . . . H18A H 0.3577 0.6876 0.3352 0.064 Uiso 1 1 calc R . . C19 C 0.3766(7) 0.7111(4) 0.4166(3) 0.0485(19) Uani 1 1 d . . . H19A H 0.4289 0.7517 0.4154 0.058 Uiso 1 1 calc R . . C20 C 0.6130(7) 0.7479(4) 0.7215(3) 0.0455(18) Uani 1 1 d . . . C21 C 0.5887(6) 0.7345(4) 0.7792(3) 0.0401(16) Uani 1 1 d . . . C22 C 0.4943(6) 0.7708(4) 0.7998(3) 0.0477(19) Uani 1 1 d . . . H22A H 0.4426 0.8020 0.7767 0.057 Uiso 1 1 calc R . . C23 C 0.4769(6) 0.7607(4) 0.8543(3) 0.0439(17) Uani 1 1 d . . . H23A H 0.4143 0.7857 0.8676 0.053 Uiso 1 1 calc R . . C24 C 0.5526(7) 0.7132(4) 0.8897(3) 0.0437(18) Uani 1 1 d . . . C25 C 0.6440(6) 0.6751(5) 0.8688(3) 0.0485(19) Uani 1 1 d . . . H25A H 0.6928 0.6419 0.8916 0.058 Uiso 1 1 calc R . . C26 C 0.6638(7) 0.6854(4) 0.8148(3) 0.0461(18) Uani 1 1 d . . . H26A H 0.7265 0.6602 0.8017 0.055 Uiso 1 1 calc R . . C27 C 0.5345(7) 0.7020(5) 0.9496(3) 0.053(2) Uani 1 1 d . . . C28 C 1.0014(7) 0.7712(5) 0.7420(3) 0.0480(18) Uani 1 1 d . . . C29 C 1.0965(6) 0.8281(4) 0.7593(3) 0.0470(18) Uani 1 1 d . . . C30 C 1.1294(7) 0.8468(5) 0.8138(4) 0.067(2) Uani 1 1 d . . . H30A H 1.0898 0.8242 0.8404 0.080 Uiso 1 1 calc R . . C31 C 1.2219(8) 0.8996(5) 0.8310(5) 0.079(3) Uani 1 1 d . . . H31A H 1.2425 0.9115 0.8683 0.095 Uiso 1 1 calc R . . C32 C 1.2831(7) 0.9340(5) 0.7902(5) 0.071(3) Uani 1 1 d . . . C33 C 1.2471(7) 0.9150(5) 0.7357(4) 0.067(2) Uani 1 1 d . . . H33A H 1.2860 0.9377 0.7088 0.080 Uiso 1 1 calc R . . C34 C 1.1559(7) 0.8639(4) 0.7186(4) 0.057(2) Uani 1 1 d . . . H34A H 1.1338 0.8532 0.6812 0.068 Uiso 1 1 calc R . . C35 C 1.3819(8) 0.9921(6) 0.8071(7) 0.092(4) Uani 1 1 d . . . C36 C 0.6498(6) 0.6112(4) 0.5641(3) 0.0383(16) Uani 1 1 d . . . C37 C 0.5716(6) 0.5546(4) 0.5306(3) 0.0397(16) Uani 1 1 d . . . C38 C 0.5779(6) 0.5456(4) 0.4736(3) 0.0458(18) Uani 1 1 d . . . H38A H 0.6291 0.5756 0.4562 0.055 Uiso 1 1 calc R . . C39 C 0.5057(6) 0.4910(4) 0.4440(3) 0.0437(17) Uani 1 1 d . . . H39A H 0.5092 0.4847 0.4064 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0314(4) 0.0449(4) 0.0399(4) 0.0001(3) -0.0051(3) -0.0038(3) O1 0.032(3) 0.066(4) 0.044(3) 0.004(2) 0.005(2) 0.006(2) O1W 0.032(3) 0.068(4) 0.066(3) 0.012(3) 0.000(2) 0.002(3) O2W 0.045(3) 0.046(3) 0.050(3) 0.010(2) -0.012(2) -0.004(2) O2 0.043(3) 0.068(4) 0.055(3) 0.005(3) 0.000(3) 0.010(3) O3W 0.057(3) 0.045(3) 0.051(3) 0.000(2) 0.004(3) 0.007(3) O3 0.088(5) 0.090(5) 0.061(4) 0.003(3) 0.017(3) 0.021(4) O4 0.052(4) 0.080(4) 0.049(3) -0.011(3) 0.011(3) 0.001(3) O4W 0.035(3) 0.063(3) 0.054(3) 0.004(2) 0.004(2) -0.006(2) O5 0.043(3) 0.059(3) 0.044(3) -0.008(2) -0.007(2) -0.015(3) O5W 0.108(6) 0.085(5) 0.121(6) -0.036(4) 0.070(5) -0.040(4) O6 0.047(3) 0.075(4) 0.045(3) -0.004(3) -0.004(2) -0.018(3) O6W 0.086(5) 0.103(6) 0.086(5) -0.015(4) -0.007(4) 0.015(4) O7 0.038(4) 0.070(5) 0.151(7) -0.016(4) -0.030(4) -0.002(3) O7W 0.057(4) 0.164(7) 0.059(4) 0.051(4) -0.007(3) -0.011(4) O8 0.062(5) 0.129(7) 0.201(9) -0.115(7) 0.004(5) -0.027(5) O9 0.035(3) 0.046(3) 0.036(3) -0.004(2) -0.003(2) -0.008(2) O10 0.032(3) 0.056(3) 0.038(2) -0.005(2) -0.009(2) -0.001(2) N1 0.044(4) 0.041(3) 0.046(4) -0.005(3) -0.005(3) 0.004(3) N2 0.041(3) 0.041(3) 0.042(3) 0.003(3) 0.003(3) 0.002(3) N3 0.036(3) 0.039(3) 0.049(3) -0.008(3) -0.002(3) -0.004(3) N4 0.026(3) 0.059(4) 0.048(4) -0.013(3) 0.001(3) -0.004(3) N5 0.028(3) 0.060(4) 0.045(3) -0.011(3) -0.004(3) 0.005(3) C1 0.036(4) 0.057(5) 0.050(4) -0.003(4) 0.004(3) 0.009(4) C2 0.033(4) 0.046(4) 0.049(4) 0.000(3) -0.004(3) -0.005(3) C3 0.078(7) 0.085(7) 0.035(4) 0.018(4) -0.004(4) 0.007(5) C4 0.061(6) 0.093(7) 0.038(4) 0.003(4) 0.010(4) 0.018(5) C5 0.043(4) 0.040(4) 0.057(5) -0.006(3) -0.010(4) -0.008(3) C6 0.052(5) 0.079(6) 0.037(4) -0.013(4) 0.008(4) -0.016(5) C7 0.043(5) 0.065(5) 0.051(5) -0.018(4) 0.004(4) -0.002(4) C8 0.032(4) 0.065(5) 0.069(5) -0.025(4) 0.003(4) -0.013(4) C9 0.032(4) 0.059(5) 0.042(4) -0.011(4) -0.003(3) -0.008(4) C10 0.033(4) 0.053(5) 0.051(4) -0.009(4) -0.008(4) 0.010(3) C11 0.026(4) 0.079(6) 0.059(5) -0.019(4) -0.006(4) 0.017(4) C12 0.042(5) 0.066(6) 0.065(6) 0.000(4) -0.003(4) 0.019(4) C13 0.044(5) 0.056(5) 0.052(4) 0.000(4) -0.010(4) -0.006(4) C14 0.039(4) 0.045(4) 0.053(5) 0.009(3) -0.008(3) 0.006(3) C15 0.067(5) 0.042(4) 0.049(4) 0.004(4) 0.006(4) -0.001(4) C16 0.054(5) 0.046(4) 0.049(4) 0.008(4) -0.005(4) -0.005(4) C17 0.036(4) 0.043(4) 0.053(4) -0.008(3) -0.007(3) 0.003(3) C18 0.046(5) 0.049(5) 0.064(5) 0.002(4) 0.005(4) -0.001(4) C19 0.036(4) 0.047(5) 0.061(5) 0.003(4) 0.001(4) -0.008(3) C20 0.033(4) 0.059(5) 0.043(4) 0.003(4) 0.001(3) -0.007(4) C21 0.028(4) 0.049(4) 0.039(4) -0.013(3) -0.007(3) 0.000(3) C22 0.028(4) 0.057(5) 0.055(5) -0.001(4) -0.004(3) -0.007(4) C23 0.034(4) 0.055(5) 0.042(4) -0.009(3) 0.004(3) 0.004(4) C24 0.045(5) 0.046(4) 0.038(4) -0.009(3) 0.000(3) -0.002(3) C25 0.030(4) 0.062(5) 0.052(5) -0.004(4) 0.002(3) -0.005(4) C26 0.035(4) 0.063(5) 0.040(4) -0.009(3) 0.003(3) -0.005(4) C27 0.044(5) 0.073(6) 0.042(4) -0.012(4) 0.007(4) -0.013(4) C28 0.036(4) 0.056(5) 0.049(5) -0.006(4) -0.005(4) -0.003(4) C29 0.031(4) 0.057(5) 0.050(4) -0.005(4) -0.005(3) 0.007(3) C30 0.038(5) 0.085(7) 0.073(6) -0.028(5) -0.003(4) -0.010(4) C31 0.042(5) 0.072(6) 0.114(8) -0.056(6) -0.023(5) 0.008(5) C32 0.029(5) 0.051(5) 0.127(8) -0.030(5) -0.012(5) -0.011(4) C33 0.034(4) 0.047(5) 0.115(8) -0.006(5) -0.005(5) -0.010(4) C34 0.045(5) 0.046(5) 0.073(5) 0.005(4) -0.010(4) -0.005(4) C35 0.023(5) 0.059(6) 0.181(13) -0.032(8) -0.024(6) 0.010(4) C36 0.032(4) 0.039(4) 0.042(4) -0.001(3) 0.001(3) 0.006(3) C37 0.028(4) 0.042(4) 0.046(4) 0.002(3) -0.003(3) 0.009(3) C38 0.038(4) 0.059(5) 0.036(4) 0.006(3) -0.007(3) -0.006(4) C39 0.038(4) 0.056(5) 0.035(4) -0.003(3) -0.002(3) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O5 2.314(5) . ? Y1 O1 2.314(5) . ? Y1 O3W 2.349(5) . ? Y1 O1W 2.366(5) . ? Y1 O9 2.372(4) . ? Y1 O4W 2.386(5) . ? Y1 O2W 2.401(4) . ? Y1 O10 2.515(4) . ? Y1 C36 2.809(7) . ? O1 C20 1.278(8) . ? O2 C20 1.274(9) . ? O3 C27 1.235(10) . ? O4 C27 1.296(9) . ? O5 C28 1.303(8) . ? O6 C28 1.241(9) . ? O7 C35 1.230(14) . ? O8 C35 1.272(14) . ? O9 C36 1.262(8) . ? O10 C36 1.267(8) . ? N1 C2 1.342(9) . ? N1 C3 1.392(9) . ? N1 C1 1.479(9) . ? N2 C2 1.329(8) . ? N2 C5 1.449(9) . ? N2 C4 1.414(9) . ? N3 C5 1.332(9) . ? N3 C9 1.331(9) . ? N4 C10 1.354(9) . ? N4 C9 1.408(9) . ? N4 C11 1.423(9) . ? N5 C10 1.331(9) . ? N5 C12 1.380(9) . ? N5 C13 1.467(10) . ? C1 C17 1.522(9) 3_666 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 C4 1.326(11) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.366(10) . ? C6 C7 1.390(11) . ? C6 H6A 0.9300 . ? C7 C8 1.357(11) . ? C7 H7A 0.9300 . ? C8 C9 1.390(10) . ? C8 H8A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.339(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.536(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.414(10) . ? C14 C15 1.405(10) . ? C15 C16 1.378(10) . ? C15 H15A 0.9300 . ? C16 C17 1.370(10) . ? C16 H16A 0.9300 . ? C17 C18 1.441(10) . ? C17 C1 1.522(9) 3_666 ? C18 C19 1.372(10) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.490(10) . ? C21 C22 1.398(10) . ? C21 C26 1.417(10) . ? C22 C23 1.383(10) . ? C22 H22A 0.9300 . ? C23 C24 1.401(10) . ? C23 H23A 0.9300 . ? C24 C25 1.388(10) . ? C24 C27 1.519(10) . ? C25 C26 1.380(10) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 C29 1.485(10) . ? C29 C30 1.368(10) . ? C29 C34 1.423(10) . ? C30 C31 1.415(11) . ? C30 H30A 0.9300 . ? C31 C32 1.425(14) . ? C31 H31A 0.9300 . ? C32 C33 1.376(13) . ? C32 C35 1.525(12) . ? C33 C34 1.385(10) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C36 C37 1.494(9) . ? C37 C39 1.395(10) 3_666 ? C37 C38 1.413(9) . ? C38 C39 1.393(10) . ? C38 H38A 0.9300 . ? C39 C37 1.395(10) 3_666 ? C39 H39A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Y1 O1 84.61(17) . . ? O5 Y1 O3W 98.13(19) . . ? O1 Y1 O3W 72.59(17) . . ? O5 Y1 O1W 100.53(18) . . ? O1 Y1 O1W 139.72(17) . . ? O3W Y1 O1W 143.82(17) . . ? O5 Y1 O9 156.38(16) . . ? O1 Y1 O9 76.49(17) . . ? O3W Y1 O9 89.70(18) . . ? O1W Y1 O9 85.44(17) . . ? O5 Y1 O4W 72.68(17) . . ? O1 Y1 O4W 139.30(18) . . ? O3W Y1 O4W 77.65(18) . . ? O1W Y1 O4W 78.73(18) . . ? O9 Y1 O4W 130.91(16) . . ? O5 Y1 O2W 76.90(17) . . ? O1 Y1 O2W 70.04(17) . . ? O3W Y1 O2W 142.59(17) . . ? O1W Y1 O2W 72.35(17) . . ? O9 Y1 O2W 83.34(16) . . ? O4W Y1 O2W 132.82(17) . . ? O5 Y1 O10 150.25(17) . . ? O1 Y1 O10 121.03(16) . . ? O3W Y1 O10 77.95(17) . . ? O1W Y1 O10 70.49(16) . . ? O9 Y1 O10 53.23(15) . . ? O4W Y1 O10 77.71(17) . . ? O2W Y1 O10 123.72(16) . . ? O5 Y1 C36 175.32(19) . . ? O1 Y1 C36 99.81(19) . . ? O3W Y1 C36 84.75(19) . . ? O1W Y1 C36 75.12(18) . . ? O9 Y1 C36 26.51(17) . . ? O4W Y1 C36 104.49(19) . . ? O2W Y1 C36 103.06(18) . . ? O10 Y1 C36 26.81(17) . . ? C20 O1 Y1 143.8(5) . . ? C28 O5 Y1 135.0(5) . . ? C36 O9 Y1 96.5(4) . . ? C36 O10 Y1 89.6(4) . . ? C2 N1 C3 107.9(6) . . ? C2 N1 C1 123.4(6) . . ? C3 N1 C1 128.7(7) . . ? C2 N2 C5 124.1(6) . . ? C2 N2 C4 108.0(6) . . ? C5 N2 C4 127.7(6) . . ? C5 N3 C9 115.9(6) . . ? C10 N4 C9 124.2(6) . . ? C10 N4 C11 106.4(6) . . ? C9 N4 C11 129.2(6) . . ? C10 N5 C12 109.4(6) . . ? C10 N5 C13 125.4(6) . . ? C12 N5 C13 125.2(6) . . ? N1 C1 C17 114.9(6) . 3_666 ? N1 C1 H1A 108.5 . . ? C17 C1 H1A 108.5 3_666 . ? N1 C1 H1B 108.5 . . ? C17 C1 H1B 108.5 3_666 . ? H1A C1 H1B 107.5 . . ? N2 C2 N1 108.9(6) . . ? N2 C2 H2A 125.5 . . ? N1 C2 H2A 125.5 . . ? C4 C3 N1 108.2(8) . . ? C4 C3 H3A 125.9 . . ? N1 C3 H3A 125.9 . . ? C3 C4 N2 106.9(7) . . ? C3 C4 H4A 126.5 . . ? N2 C4 H4A 126.5 . . ? N3 C5 C6 125.8(7) . . ? N3 C5 N2 111.5(6) . . ? C6 C5 N2 122.6(7) . . ? C5 C6 C7 116.3(8) . . ? C5 C6 H6A 121.9 . . ? C7 C6 H6A 121.9 . . ? C8 C7 C6 120.3(7) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C7 C8 C9 118.2(8) . . ? C7 C8 H8A 120.9 . . ? C9 C8 H8A 120.9 . . ? N3 C9 N4 113.6(6) . . ? N3 C9 C8 123.4(7) . . ? N4 C9 C8 123.0(7) . . ? N4 C10 N5 109.0(6) . . ? N4 C10 H10A 125.5 . . ? N5 C10 H10A 125.5 . . ? C12 C11 N4 107.7(7) . . ? C12 C11 H11A 126.2 . . ? N4 C11 H11A 126.2 . . ? C11 C12 N5 107.5(7) . . ? C11 C12 H12A 126.2 . . ? N5 C12 H12A 126.2 . . ? N5 C13 C14 112.3(6) . . ? N5 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N5 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? C19 C14 C15 119.1(7) . . ? C19 C14 C13 117.3(7) . . ? C15 C14 C13 123.4(7) . . ? C16 C15 C14 119.6(7) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C17 C16 C15 122.1(7) . . ? C17 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? C16 C17 C18 119.1(7) . . ? C16 C17 C1 120.3(7) . 3_666 ? C18 C17 C1 120.5(7) . 3_666 ? C19 C18 C17 119.0(7) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C18 C19 C14 121.1(7) . . ? C18 C19 H19A 119.4 . . ? C14 C19 H19A 119.4 . . ? O2 C20 O1 123.9(6) . . ? O2 C20 C21 119.2(7) . . ? O1 C20 C21 117.0(6) . . ? C22 C21 C26 118.5(7) . . ? C22 C21 C20 121.5(7) . . ? C26 C21 C20 120.0(6) . . ? C23 C22 C21 120.7(7) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 120.7(7) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C25 C24 C23 118.8(6) . . ? C25 C24 C27 120.2(7) . . ? C23 C24 C27 121.0(7) . . ? C26 C25 C24 121.3(7) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C21 120.0(7) . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? O3 C27 O4 124.8(7) . . ? O3 C27 C24 118.3(7) . . ? O4 C27 C24 116.8(8) . . ? O6 C28 O5 124.1(7) . . ? O6 C28 C29 119.4(6) . . ? O5 C28 C29 116.5(7) . . ? C30 C29 C34 118.9(8) . . ? C30 C29 C28 121.6(7) . . ? C34 C29 C28 119.6(6) . . ? C29 C30 C31 122.1(9) . . ? C29 C30 H30A 119.0 . . ? C31 C30 H30A 119.0 . . ? C30 C31 C32 118.9(8) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C33 C32 C31 117.8(7) . . ? C33 C32 C35 121.7(11) . . ? C31 C32 C35 120.4(10) . . ? C32 C33 C34 123.4(9) . . ? C32 C33 H33A 118.3 . . ? C34 C33 H33A 118.3 . . ? C29 C34 C33 118.8(8) . . ? C29 C34 H34A 120.6 . . ? C33 C34 H34A 120.6 . . ? O7 C35 O8 125.2(10) . . ? O7 C35 C32 117.4(12) . . ? O8 C35 C32 117.3(12) . . ? O10 C36 O9 120.3(6) . . ? O10 C36 C37 120.9(6) . . ? O9 C36 C37 118.8(6) . . ? O10 C36 Y1 63.6(3) . . ? O9 C36 Y1 57.0(3) . . ? C37 C36 Y1 171.6(5) . . ? C39 C37 C38 119.8(6) 3_666 . ? C39 C37 C36 120.0(6) 3_666 . ? C38 C37 C36 120.2(6) . . ? C39 C38 C37 118.6(7) . . ? C39 C38 H38A 120.7 . . ? C37 C38 H38A 120.7 . . ? C37 C39 C38 121.5(6) 3_666 . ? C37 C39 H39A 119.2 3_666 . ? C38 C39 H39A 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Y1 O1 C20 114.6(8) . . . . ? O3W Y1 O1 C20 14.4(8) . . . . ? O1W Y1 O1 C20 -145.4(7) . . . . ? O9 Y1 O1 C20 -79.6(8) . . . . ? O4W Y1 O1 C20 59.3(9) . . . . ? O2W Y1 O1 C20 -167.4(8) . . . . ? O10 Y1 O1 C20 -49.3(8) . . . . ? C36 Y1 O1 C20 -66.9(8) . . . . ? O1 Y1 O5 C28 38.4(7) . . . . ? O3W Y1 O5 C28 110.0(7) . . . . ? O1W Y1 O5 C28 -101.2(7) . . . . ? O9 Y1 O5 C28 1.7(10) . . . . ? O4W Y1 O5 C28 -175.8(7) . . . . ? O2W Y1 O5 C28 -32.3(7) . . . . ? O10 Y1 O5 C28 -170.1(6) . . . . ? C36 Y1 O5 C28 -122(2) . . . . ? O5 Y1 O9 C36 -171.3(4) . . . . ? O1 Y1 O9 C36 150.9(4) . . . . ? O3W Y1 O9 C36 78.8(4) . . . . ? O1W Y1 O9 C36 -65.3(4) . . . . ? O4W Y1 O9 C36 5.5(5) . . . . ? O2W Y1 O9 C36 -138.1(4) . . . . ? O10 Y1 O9 C36 3.7(4) . . . . ? O5 Y1 O10 C36 172.3(4) . . . . ? O1 Y1 O10 C36 -41.4(4) . . . . ? O3W Y1 O10 C36 -102.4(4) . . . . ? O1W Y1 O10 C36 95.6(4) . . . . ? O9 Y1 O10 C36 -3.6(3) . . . . ? O4W Y1 O10 C36 177.8(4) . . . . ? O2W Y1 O10 C36 44.1(4) . . . . ? C2 N1 C1 C17 -69.0(9) . . . 3_666 ? C3 N1 C1 C17 110.8(8) . . . 3_666 ? C5 N2 C2 N1 -176.2(6) . . . . ? C4 N2 C2 N1 -1.1(8) . . . . ? C3 N1 C2 N2 1.4(8) . . . . ? C1 N1 C2 N2 -178.7(6) . . . . ? C2 N1 C3 C4 -1.2(10) . . . . ? C1 N1 C3 C4 179.0(7) . . . . ? N1 C3 C4 N2 0.5(10) . . . . ? C2 N2 C4 C3 0.3(9) . . . . ? C5 N2 C4 C3 175.3(7) . . . . ? C9 N3 C5 C6 1.4(10) . . . . ? C9 N3 C5 N2 178.8(6) . . . . ? C2 N2 C5 N3 6.7(9) . . . . ? C4 N2 C5 N3 -167.4(7) . . . . ? C2 N2 C5 C6 -175.8(7) . . . . ? C4 N2 C5 C6 10.1(11) . . . . ? N3 C5 C6 C7 -1.5(11) . . . . ? N2 C5 C6 C7 -178.6(7) . . . . ? C5 C6 C7 C8 2.1(11) . . . . ? C6 C7 C8 C9 -2.7(11) . . . . ? C5 N3 C9 N4 176.7(6) . . . . ? C5 N3 C9 C8 -1.9(10) . . . . ? C10 N4 C9 N3 -20.1(10) . . . . ? C11 N4 C9 N3 164.6(7) . . . . ? C10 N4 C9 C8 158.5(7) . . . . ? C11 N4 C9 C8 -16.7(12) . . . . ? C7 C8 C9 N3 2.7(11) . . . . ? C7 C8 C9 N4 -175.9(7) . . . . ? C9 N4 C10 N5 -178.4(6) . . . . ? C11 N4 C10 N5 -2.3(8) . . . . ? C12 N5 C10 N4 2.0(8) . . . . ? C13 N5 C10 N4 179.8(6) . . . . ? C10 N4 C11 C12 1.7(9) . . . . ? C9 N4 C11 C12 177.6(7) . . . . ? N4 C11 C12 N5 -0.5(9) . . . . ? C10 N5 C12 C11 -0.9(9) . . . . ? C13 N5 C12 C11 -178.7(7) . . . . ? C10 N5 C13 C14 106.8(8) . . . . ? C12 N5 C13 C14 -75.7(9) . . . . ? N5 C13 C14 C19 171.8(6) . . . . ? N5 C13 C14 C15 -3.7(10) . . . . ? C19 C14 C15 C16 1.7(11) . . . . ? C13 C14 C15 C16 177.1(7) . . . . ? C14 C15 C16 C17 -2.0(12) . . . . ? C15 C16 C17 C18 1.5(11) . . . . ? C15 C16 C17 C1 -175.4(7) . . . 3_666 ? C16 C17 C18 C19 -0.6(11) . . . . ? C1 C17 C18 C19 176.2(6) 3_666 . . . ? C17 C18 C19 C14 0.4(11) . . . . ? C15 C14 C19 C18 -1.0(11) . . . . ? C13 C14 C19 C18 -176.6(7) . . . . ? Y1 O1 C20 O2 -1.9(13) . . . . ? Y1 O1 C20 C21 178.0(5) . . . . ? O2 C20 C21 C22 -4.8(10) . . . . ? O1 C20 C21 C22 175.3(6) . . . . ? O2 C20 C21 C26 176.7(7) . . . . ? O1 C20 C21 C26 -3.2(10) . . . . ? C26 C21 C22 C23 2.0(10) . . . . ? C20 C21 C22 C23 -176.6(7) . . . . ? C21 C22 C23 C24 -0.8(11) . . . . ? C22 C23 C24 C25 -1.3(11) . . . . ? C22 C23 C24 C27 179.8(7) . . . . ? C23 C24 C25 C26 2.4(11) . . . . ? C27 C24 C25 C26 -178.7(7) . . . . ? C24 C25 C26 C21 -1.3(11) . . . . ? C22 C21 C26 C25 -0.9(10) . . . . ? C20 C21 C26 C25 177.7(6) . . . . ? C25 C24 C27 O3 -7.7(11) . . . . ? C23 C24 C27 O3 171.2(7) . . . . ? C25 C24 C27 O4 169.3(7) . . . . ? C23 C24 C27 O4 -11.9(10) . . . . ? Y1 O5 C28 O6 4.7(12) . . . . ? Y1 O5 C28 C29 -177.2(5) . . . . ? O6 C28 C29 C30 -14.3(12) . . . . ? O5 C28 C29 C30 167.4(7) . . . . ? O6 C28 C29 C34 165.3(7) . . . . ? O5 C28 C29 C34 -13.0(11) . . . . ? C34 C29 C30 C31 -1.2(12) . . . . ? C28 C29 C30 C31 178.4(7) . . . . ? C29 C30 C31 C32 -0.3(13) . . . . ? C30 C31 C32 C33 1.2(12) . . . . ? C30 C31 C32 C35 179.0(8) . . . . ? C31 C32 C33 C34 -0.7(13) . . . . ? C35 C32 C33 C34 -178.4(8) . . . . ? C30 C29 C34 C33 1.7(11) . . . . ? C28 C29 C34 C33 -177.9(7) . . . . ? C32 C33 C34 C29 -0.8(13) . . . . ? C33 C32 C35 O7 -12.4(13) . . . . ? C31 C32 C35 O7 169.9(9) . . . . ? C33 C32 C35 O8 171.7(9) . . . . ? C31 C32 C35 O8 -6.0(13) . . . . ? Y1 O10 C36 O9 6.3(6) . . . . ? Y1 O10 C36 C37 -171.9(5) . . . . ? Y1 O9 C36 O10 -6.7(6) . . . . ? Y1 O9 C36 C37 171.5(5) . . . . ? O5 Y1 C36 O10 -55(2) . . . . ? O1 Y1 C36 O10 144.9(4) . . . . ? O3W Y1 C36 O10 73.6(4) . . . . ? O1W Y1 C36 O10 -76.1(4) . . . . ? O9 Y1 C36 O10 173.5(6) . . . . ? O4W Y1 C36 O10 -2.2(4) . . . . ? O2W Y1 C36 O10 -143.5(4) . . . . ? O5 Y1 C36 O9 132(2) . . . . ? O1 Y1 C36 O9 -28.6(4) . . . . ? O3W Y1 C36 O9 -99.9(4) . . . . ? O1W Y1 C36 O9 110.4(4) . . . . ? O4W Y1 C36 O9 -175.7(4) . . . . ? O2W Y1 C36 O9 43.0(4) . . . . ? O10 Y1 C36 O9 -173.5(6) . . . . ? O5 Y1 C36 C37 70(5) . . . . ? O1 Y1 C36 C37 -91(3) . . . . ? O3W Y1 C36 C37 -162(3) . . . . ? O1W Y1 C36 C37 48(3) . . . . ? O9 Y1 C36 C37 -62(3) . . . . ? O4W Y1 C36 C37 122(3) . . . . ? O2W Y1 C36 C37 -19(3) . . . . ? O10 Y1 C36 C37 124(3) . . . . ? O10 C36 C37 C39 -173.6(6) . . . 3_666 ? O9 C36 C37 C39 8.2(9) . . . 3_666 ? Y1 C36 C37 C39 66(3) . . . 3_666 ? O10 C36 C37 C38 8.1(10) . . . . ? O9 C36 C37 C38 -170.1(6) . . . . ? Y1 C36 C37 C38 -112(3) . . . . ? C39 C37 C38 C39 0.1(11) 3_666 . . . ? C36 C37 C38 C39 178.4(6) . . . . ? C37 C38 C39 C37 -0.1(11) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.793 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.113 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.002 0.000 0.500 456 226 ' ' 2 -0.024 0.500 0.000 456 226 ' ' _platon_squeeze_details ; Number of Isotropic Non-H Atoms: 1. Number of moved primary input atoms: 85. Number of unusual anisotropic displacement parameters: 3. Total Potential Solvent Accessible Void Vol: 914.1 Ang**3. Electron Count / Cell = 452 - To be included in D(calc), F000 & Mol.Wght. ; # end Validation Reply Form data_RSOF-Gd _database_code_depnum_ccdc_archive 'CCDC 838076' #TrackingRef '- RSOF-Gd as CCDC 838076.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; cyclo(2)(2,6-di(1H-imidazol-1-yl)pyridine)(2)(1,4- dimethylenebenzene) _ 5 terephthalate dianion_ 2 gadilinium(iii)_8 H2O_ 22 H2O ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H114 Gd2 N10 O50' _chemical_formula_weight 2306.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.295(2) _cell_length_b 17.674(4) _cell_length_c 24.549(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.66(3) _cell_angle_gamma 90.00 _cell_volume 4844.7(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8425 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8128 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38759 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8425 _reflns_number_gt 7897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8425 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1300 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.81092(2) 0.702741(15) 0.634496(11) 0.01759(10) Uani 1 1 d . . . O1 O 0.7022(4) 0.7238(2) 0.70703(16) 0.0258(9) Uani 1 1 d . . . O1W O 0.9297(4) 0.6066(2) 0.60245(18) 0.0308(10) Uani 1 1 d . . . O2W O 0.8796(4) 0.6179(2) 0.71163(16) 0.0249(9) Uani 1 1 d . . . O2 O 0.5372(4) 0.7942(3) 0.68798(18) 0.0321(10) Uani 1 1 d . . . O3W O 0.6715(4) 0.8013(2) 0.60730(17) 0.0298(10) Uani 1 1 d . . . O3 O 0.5833(5) 0.6531(3) 0.97150(19) 0.0414(12) Uani 1 1 d . . . O4 O 0.4572(4) 0.7506(2) 0.96574(17) 0.0298(10) Uani 1 1 d . . . O4W O 0.9134(4) 0.7734(3) 0.57141(17) 0.0297(10) Uani 1 1 d . . . O5 O 0.9620(4) 0.7727(2) 0.68722(16) 0.0247(9) Uani 1 1 d . . . O5W O 1.4718(5) 0.8983(3) 0.9978(2) 0.0455(13) Uani 1 1 d . . . O6 O 0.9691(4) 0.7372(2) 0.77508(17) 0.0302(10) Uani 1 1 d . . . O6W O 1.0951(5) 0.6660(3) 0.8660(2) 0.0475(13) Uani 1 1 d . . . O7 O 1.4482(4) 1.0147(3) 0.7646(2) 0.0400(12) Uani 1 1 d . . . O7W O 0.7130(5) 0.7365(4) 0.4427(2) 0.0565(16) Uani 1 1 d . . . O8 O 1.3925(5) 1.0260(3) 0.8466(2) 0.0534(14) Uani 1 1 d . . . O8W O 1.3423(5) 1.0102(3) 0.9481(2) 0.0497(13) Uani 1 1 d . . . O9 O 0.6496(3) 0.6128(2) 0.61492(15) 0.0207(8) Uani 1 1 d . . . O9W O 0.4951(7) 0.9472(5) 0.6735(4) 0.098(3) Uani 1 1 d . . . O10 O 0.7098(3) 0.6579(2) 0.54045(15) 0.0206(8) Uani 1 1 d . . . O10W O 0.5846(9) 1.0627(6) 0.6113(4) 0.121(3) Uani 1 1 d . . . O11W O 0.6793(10) 1.0881(6) 0.4248(5) 0.136(4) Uani 1 1 d . . . O12W O 0.9408(6) 1.1027(3) 0.4257(2) 0.0613(16) Uani 1 1 d . . . O13W O 0.6110(7) 0.8632(5) 0.5095(3) 0.088(2) Uani 1 1 d . . . O14W O 1.0953(6) 0.9895(4) 0.4210(3) 0.0668(17) Uani 1 1 d . . . O15W O 0.6739(14) 1.0069(7) 0.5238(5) 0.169(5) Uani 1 1 d . . . N1 N 0.7146(4) 0.4546(3) 0.7201(2) 0.0232(10) Uani 1 1 d . . . N2 N 0.5703(4) 0.5143(3) 0.75020(19) 0.0221(10) Uani 1 1 d . . . N3 N 0.4340(4) 0.5946(3) 0.70059(19) 0.0206(10) Uani 1 1 d . . . N4 N 0.3093(4) 0.6745(3) 0.6439(2) 0.0232(11) Uani 1 1 d . . . N5 N 0.3337(4) 0.7178(3) 0.5641(2) 0.0259(11) Uani 1 1 d . . . C1 C 0.7997(5) 0.4319(3) 0.6833(3) 0.0280(13) Uani 1 1 d . . . H1A H 0.8594 0.3988 0.7035 0.034 Uiso 1 1 calc R . . H1B H 0.8408 0.4767 0.6730 0.034 Uiso 1 1 calc R . . C2 C 0.6306(5) 0.5069(3) 0.7076(2) 0.0216(12) Uani 1 1 d . . . H2A H 0.6161 0.5339 0.6748 0.026 Uiso 1 1 calc R . . C3 C 0.7087(7) 0.4282(4) 0.7728(3) 0.0386(16) Uani 1 1 d . . . H3A H 0.7576 0.3914 0.7915 0.046 Uiso 1 1 calc R . . C4 C 0.6195(6) 0.4654(4) 0.7918(3) 0.0353(15) Uani 1 1 d . . . H4A H 0.5954 0.4596 0.8262 0.042 Uiso 1 1 calc R . . C5 C 0.4691(5) 0.5630(3) 0.7494(2) 0.0223(12) Uani 1 1 d . . . C6 C 0.4130(6) 0.5722(3) 0.7955(2) 0.0277(13) Uani 1 1 d . . . H6A H 0.4414 0.5490 0.8289 0.033 Uiso 1 1 calc R . . C7 C 0.3114(6) 0.6183(3) 0.7890(3) 0.0287(14) Uani 1 1 d . . . H7A H 0.2696 0.6257 0.8184 0.034 Uiso 1 1 calc R . . C8 C 0.2727(5) 0.6532(4) 0.7388(3) 0.0272(13) Uani 1 1 d . . . H8A H 0.2056 0.6843 0.7337 0.033 Uiso 1 1 calc R . . C9 C 0.3385(5) 0.6394(3) 0.6970(2) 0.0224(12) Uani 1 1 d . . . C10 C 0.3871(5) 0.6813(3) 0.6081(2) 0.0214(12) Uani 1 1 d . . . H10A H 0.4654 0.6635 0.6133 0.026 Uiso 1 1 calc R . . C11 C 0.2014(5) 0.7076(3) 0.6210(3) 0.0298(14) Uani 1 1 d . . . H11A H 0.1315 0.7102 0.6367 0.036 Uiso 1 1 calc R . . C12 C 0.2179(6) 0.7348(4) 0.5720(3) 0.0328(15) Uani 1 1 d . . . H12A H 0.1614 0.7608 0.5474 0.039 Uiso 1 1 calc R . . C13 C 0.3889(6) 0.7368(3) 0.5152(2) 0.0280(13) Uani 1 1 d . . . H13A H 0.4749 0.7301 0.5240 0.034 Uiso 1 1 calc R . . H13B H 0.3738 0.7898 0.5063 0.034 Uiso 1 1 calc R . . C14 C 0.3426(5) 0.6891(3) 0.4648(2) 0.0242(13) Uani 1 1 d . . . C15 C 0.2682(6) 0.6272(3) 0.4666(3) 0.0289(14) Uani 1 1 d . . . H15A H 0.2467 0.6121 0.5001 0.035 Uiso 1 1 calc R . . C16 C 0.2253(5) 0.5874(3) 0.4190(3) 0.0273(13) Uani 1 1 d . . . H16A H 0.1748 0.5462 0.4208 0.033 Uiso 1 1 calc R . . C17 C 0.2567(5) 0.6082(3) 0.3687(2) 0.0230(12) Uani 1 1 d . . . C18 C 0.3347(5) 0.6693(3) 0.3668(3) 0.0264(13) Uani 1 1 d . . . H18A H 0.3587 0.6833 0.3336 0.032 Uiso 1 1 calc R . . C19 C 0.3761(5) 0.7089(3) 0.4146(3) 0.0260(13) Uani 1 1 d . . . H19A H 0.4275 0.7497 0.4129 0.031 Uiso 1 1 calc R . . C20 C 0.6090(5) 0.7538(3) 0.7202(2) 0.0216(12) Uani 1 1 d . . . C21 C 0.5847(5) 0.7400(3) 0.7779(2) 0.0208(12) Uani 1 1 d . . . C22 C 0.4918(5) 0.7773(3) 0.7980(2) 0.0225(12) Uani 1 1 d . . . H22A H 0.4414 0.8093 0.7750 0.027 Uiso 1 1 calc R . . C23 C 0.4738(5) 0.7673(3) 0.8519(2) 0.0238(12) Uani 1 1 d . . . H23A H 0.4125 0.7933 0.8651 0.029 Uiso 1 1 calc R . . C24 C 0.5468(5) 0.7184(3) 0.8867(2) 0.0233(12) Uani 1 1 d . . . C25 C 0.6393(5) 0.6808(3) 0.8664(2) 0.0233(12) Uani 1 1 d . . . H25A H 0.6883 0.6479 0.8892 0.028 Uiso 1 1 calc R . . C26 C 0.6590(5) 0.6919(3) 0.8125(2) 0.0218(12) Uani 1 1 d . . . H26A H 0.7219 0.6671 0.7995 0.026 Uiso 1 1 calc R . . C27 C 0.5282(6) 0.7064(3) 0.9454(2) 0.0253(13) Uani 1 1 d . . . C28 C 1.0017(5) 0.7776(3) 0.7385(2) 0.0226(12) Uani 1 1 d . . . C29 C 1.0982(5) 0.8358(3) 0.7549(2) 0.0229(12) Uani 1 1 d . . . C30 C 1.1319(6) 0.8558(4) 0.8103(3) 0.0307(14) Uani 1 1 d . . . H30A H 1.0941 0.8338 0.8375 0.037 Uiso 1 1 calc R . . C31 C 1.2226(6) 0.9088(4) 0.8242(3) 0.0370(16) Uani 1 1 d . . . H31A H 1.2437 0.9231 0.8609 0.044 Uiso 1 1 calc R . . C32 C 1.2826(5) 0.9411(3) 0.7841(3) 0.0314(15) Uani 1 1 d . . . C33 C 1.2485(6) 0.9206(3) 0.7299(3) 0.0305(14) Uani 1 1 d . . . H33A H 1.2879 0.9417 0.7029 0.037 Uiso 1 1 calc R . . C34 C 1.1571(5) 0.8694(3) 0.7149(3) 0.0274(13) Uani 1 1 d . . . H34A H 1.1344 0.8572 0.6780 0.033 Uiso 1 1 calc R . . C35 C 1.3843(7) 0.9986(4) 0.7988(3) 0.0374(17) Uani 1 1 d . . . C36 C 0.6476(5) 0.6118(3) 0.5629(2) 0.0191(11) Uani 1 1 d . . . C37 C 0.5703(5) 0.5546(3) 0.5298(2) 0.0187(11) Uani 1 1 d . . . C38 C 0.5792(5) 0.5439(3) 0.4748(2) 0.0194(11) Uani 1 1 d . . . H38A H 0.6320 0.5732 0.4581 0.023 Uiso 1 1 calc R . . C39 C 0.5093(5) 0.4894(3) 0.4446(2) 0.0205(12) Uani 1 1 d . . . H39A H 0.5150 0.4820 0.4076 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01755(17) 0.01992(16) 0.01448(16) -0.00083(10) -0.00022(11) -0.00199(10) O1 0.027(2) 0.034(2) 0.019(2) 0.0016(17) 0.0090(18) 0.0046(18) O1W 0.024(2) 0.034(2) 0.035(2) 0.0058(19) 0.0034(19) 0.0101(18) O2W 0.026(2) 0.022(2) 0.024(2) 0.0031(17) -0.0022(17) -0.0002(17) O2 0.032(2) 0.043(3) 0.022(2) 0.0038(19) 0.0054(19) 0.011(2) O3W 0.039(3) 0.030(2) 0.022(2) 0.0036(17) 0.0077(19) 0.0122(19) O3 0.058(3) 0.043(3) 0.027(2) 0.005(2) 0.018(2) 0.010(2) O4 0.035(2) 0.034(2) 0.022(2) -0.0050(18) 0.0080(19) 0.0002(19) O4W 0.033(2) 0.040(2) 0.018(2) 0.0023(18) 0.0074(18) -0.0071(19) O5 0.026(2) 0.028(2) 0.019(2) -0.0026(17) 0.0012(17) -0.0085(17) O5W 0.052(3) 0.043(3) 0.048(3) -0.014(2) 0.027(3) -0.019(2) O6 0.034(2) 0.034(2) 0.021(2) -0.0043(18) 0.0006(19) -0.0092(19) O6W 0.051(3) 0.050(3) 0.042(3) -0.002(2) 0.006(2) 0.005(3) O7 0.030(3) 0.035(3) 0.053(3) -0.005(2) -0.001(2) -0.007(2) O7W 0.036(3) 0.090(4) 0.041(3) 0.031(3) -0.003(2) -0.004(3) O8 0.042(3) 0.061(4) 0.056(4) -0.015(3) 0.005(3) -0.019(3) O8W 0.052(3) 0.052(3) 0.048(3) -0.004(3) 0.015(3) -0.013(3) O9 0.019(2) 0.026(2) 0.0156(19) -0.0038(16) -0.0009(16) -0.0041(16) O9W 0.075(5) 0.095(6) 0.128(7) 0.009(5) 0.032(5) -0.005(4) O10 0.022(2) 0.023(2) 0.0159(19) -0.0026(16) 0.0007(16) -0.0032(16) O10W 0.115(7) 0.124(8) 0.127(8) -0.005(6) 0.030(6) -0.005(6) O11W 0.141(9) 0.122(8) 0.150(10) -0.031(7) 0.043(7) -0.023(7) O12W 0.090(5) 0.056(4) 0.035(3) 0.002(3) 0.001(3) -0.002(3) O13W 0.081(5) 0.116(6) 0.069(5) 0.031(4) 0.012(4) 0.017(5) O14W 0.088(5) 0.058(4) 0.059(4) 0.000(3) 0.024(3) 0.003(3) O15W 0.258(16) 0.115(9) 0.144(10) -0.029(8) 0.065(10) -0.023(9) N1 0.026(3) 0.020(2) 0.022(3) 0.0003(19) -0.001(2) 0.002(2) N2 0.025(3) 0.021(2) 0.019(2) 0.0016(19) 0.003(2) 0.000(2) N3 0.017(2) 0.024(2) 0.021(2) -0.0055(19) 0.0019(19) -0.0004(19) N4 0.020(3) 0.026(3) 0.023(3) -0.007(2) -0.001(2) 0.003(2) N5 0.022(3) 0.028(3) 0.026(3) -0.004(2) -0.002(2) 0.003(2) C1 0.027(3) 0.025(3) 0.032(3) -0.004(3) 0.000(3) 0.005(2) C2 0.025(3) 0.019(3) 0.019(3) -0.001(2) -0.002(2) 0.000(2) C3 0.048(4) 0.034(4) 0.031(4) 0.010(3) -0.004(3) 0.011(3) C4 0.042(4) 0.041(4) 0.024(3) 0.008(3) 0.005(3) 0.009(3) C5 0.023(3) 0.022(3) 0.021(3) -0.005(2) 0.001(2) -0.007(2) C6 0.034(4) 0.029(3) 0.020(3) -0.003(2) 0.006(3) -0.010(3) C7 0.031(3) 0.029(3) 0.028(3) -0.011(3) 0.012(3) -0.006(3) C8 0.022(3) 0.031(3) 0.029(3) -0.008(3) 0.005(3) -0.003(2) C9 0.021(3) 0.022(3) 0.024(3) -0.005(2) 0.002(2) -0.005(2) C10 0.018(3) 0.025(3) 0.021(3) -0.004(2) 0.000(2) 0.002(2) C11 0.016(3) 0.033(3) 0.039(4) -0.008(3) -0.002(3) 0.009(2) C12 0.025(3) 0.038(4) 0.034(4) -0.003(3) -0.001(3) 0.011(3) C13 0.031(3) 0.026(3) 0.025(3) 0.002(3) -0.001(3) 0.003(3) C14 0.022(3) 0.026(3) 0.023(3) 0.001(2) -0.002(2) 0.006(2) C15 0.032(3) 0.030(3) 0.026(3) 0.005(3) 0.005(3) -0.001(3) C16 0.026(3) 0.022(3) 0.033(3) 0.000(3) 0.003(3) -0.001(2) C17 0.020(3) 0.022(3) 0.026(3) 0.005(2) -0.001(2) 0.007(2) C18 0.025(3) 0.025(3) 0.030(3) 0.001(3) 0.006(3) 0.003(2) C19 0.020(3) 0.026(3) 0.031(3) 0.000(2) 0.001(3) 0.000(2) C20 0.021(3) 0.023(3) 0.021(3) -0.004(2) 0.002(2) -0.006(2) C21 0.020(3) 0.024(3) 0.018(3) -0.003(2) 0.000(2) -0.004(2) C22 0.020(3) 0.025(3) 0.022(3) -0.004(2) 0.000(2) 0.001(2) C23 0.020(3) 0.026(3) 0.026(3) -0.008(2) 0.007(2) -0.001(2) C24 0.021(3) 0.028(3) 0.021(3) -0.006(2) 0.002(2) -0.009(2) C25 0.023(3) 0.026(3) 0.021(3) -0.001(2) 0.003(2) -0.001(2) C26 0.017(3) 0.028(3) 0.020(3) -0.004(2) 0.002(2) -0.003(2) C27 0.028(3) 0.028(3) 0.020(3) -0.001(2) 0.004(3) -0.006(3) C28 0.022(3) 0.026(3) 0.019(3) -0.003(2) 0.004(2) -0.001(2) C29 0.021(3) 0.022(3) 0.023(3) -0.005(2) -0.006(2) 0.000(2) C30 0.028(3) 0.031(3) 0.032(4) -0.010(3) 0.001(3) -0.004(3) C31 0.034(4) 0.034(4) 0.037(4) -0.020(3) -0.013(3) 0.004(3) C32 0.022(3) 0.018(3) 0.051(4) -0.003(3) -0.001(3) 0.001(2) C33 0.026(3) 0.024(3) 0.039(4) 0.001(3) -0.002(3) -0.003(3) C34 0.029(3) 0.023(3) 0.029(3) 0.001(2) -0.001(3) -0.002(2) C35 0.046(4) 0.024(3) 0.037(4) -0.011(3) -0.012(3) 0.009(3) C36 0.016(3) 0.021(3) 0.019(3) -0.001(2) -0.001(2) 0.004(2) C37 0.014(3) 0.023(3) 0.017(3) -0.002(2) -0.003(2) 0.002(2) C38 0.017(3) 0.022(3) 0.019(3) 0.001(2) 0.005(2) -0.001(2) C39 0.021(3) 0.025(3) 0.014(3) -0.002(2) -0.002(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O5 2.335(4) . ? Gd1 O1 2.340(4) . ? Gd1 O1W 2.371(4) . ? Gd1 O3W 2.376(4) . ? Gd1 O9 2.411(4) . ? Gd1 O4W 2.416(4) . ? Gd1 O2W 2.448(4) . ? Gd1 O10 2.543(4) . ? Gd1 C36 2.846(6) . ? O1 C20 1.264(7) . ? O2 C20 1.265(7) . ? O3 C27 1.252(8) . ? O4 C27 1.274(7) . ? O5 C28 1.274(7) . ? O6 C28 1.246(7) . ? O7 C35 1.221(9) . ? O8 C35 1.259(9) . ? O9 C36 1.274(7) . ? O10 C36 1.256(7) . ? N1 C2 1.326(7) . ? N1 C3 1.386(8) . ? N1 C1 1.470(8) . ? N2 C2 1.337(7) . ? N2 C4 1.388(8) . ? N2 C5 1.429(8) . ? N3 C5 1.328(7) . ? N3 C9 1.330(7) . ? N4 C10 1.339(7) . ? N4 C11 1.392(8) . ? N4 C9 1.435(8) . ? N5 C10 1.322(8) . ? N5 C12 1.384(8) . ? N5 C13 1.473(8) . ? C1 C17 1.514(8) 3_666 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 C4 1.345(10) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.386(8) . ? C6 C7 1.396(9) . ? C6 H6A 0.9300 . ? C7 C8 1.388(9) . ? C7 H7A 0.9300 . ? C8 C9 1.377(8) . ? C8 H8A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.333(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.523(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.385(9) . ? C14 C19 1.388(9) . ? C15 C16 1.389(9) . ? C15 H15A 0.9300 . ? C16 C17 1.385(9) . ? C16 H16A 0.9300 . ? C17 C18 1.399(8) . ? C17 C1 1.514(8) 3_666 ? C18 C19 1.385(9) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.504(8) . ? C21 C26 1.390(8) . ? C21 C22 1.392(8) . ? C22 C23 1.380(8) . ? C22 H22A 0.9300 . ? C23 C24 1.394(9) . ? C23 H23A 0.9300 . ? C24 C25 1.392(8) . ? C24 C27 1.502(8) . ? C25 C26 1.388(8) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 C29 1.508(8) . ? C29 C34 1.398(9) . ? C29 C30 1.401(8) . ? C30 C31 1.393(9) . ? C30 H30A 0.9300 . ? C31 C32 1.399(10) . ? C31 H31A 0.9300 . ? C32 C33 1.375(9) . ? C32 C35 1.537(9) . ? C33 C34 1.381(9) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C36 C37 1.494(8) . ? C37 C38 1.383(8) . ? C37 C39 1.406(8) 3_666 ? C38 C39 1.388(8) . ? C38 H38A 0.9300 . ? C39 C37 1.406(8) 3_666 ? C39 H39A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Gd1 O1 85.27(14) . . ? O5 Gd1 O1W 99.23(15) . . ? O1 Gd1 O1W 138.98(15) . . ? O5 Gd1 O3W 99.53(15) . . ? O1 Gd1 O3W 72.27(14) . . ? O1W Gd1 O3W 144.73(15) . . ? O5 Gd1 O9 157.96(13) . . ? O1 Gd1 O9 77.82(14) . . ? O1W Gd1 O9 84.84(14) . . ? O3W Gd1 O9 88.76(15) . . ? O5 Gd1 O4W 72.59(14) . . ? O1 Gd1 O4W 139.69(15) . . ? O1W Gd1 O4W 78.92(15) . . ? O3W Gd1 O4W 78.60(15) . . ? O9 Gd1 O4W 129.32(14) . . ? O5 Gd1 O2W 77.04(14) . . ? O1 Gd1 O2W 69.54(14) . . ? O1W Gd1 O2W 71.85(14) . . ? O3W Gd1 O2W 141.81(14) . . ? O9 Gd1 O2W 83.81(13) . . ? O4W Gd1 O2W 133.29(14) . . ? O5 Gd1 O10 149.21(13) . . ? O1 Gd1 O10 121.67(14) . . ? O1W Gd1 O10 71.00(14) . . ? O3W Gd1 O10 77.63(14) . . ? O9 Gd1 O10 52.49(12) . . ? O4W Gd1 O10 76.84(13) . . ? O2W Gd1 O10 123.89(13) . . ? O5 Gd1 C36 173.29(15) . . ? O1 Gd1 C36 101.20(15) . . ? O1W Gd1 C36 74.74(15) . . ? O3W Gd1 C36 84.27(16) . . ? O9 Gd1 C36 26.43(14) . . ? O4W Gd1 C36 102.97(15) . . ? O2W Gd1 C36 103.41(15) . . ? O10 Gd1 C36 26.18(14) . . ? C20 O1 Gd1 144.5(4) . . ? C28 O5 Gd1 134.7(4) . . ? C36 O9 Gd1 96.2(3) . . ? C36 O10 Gd1 90.5(3) . . ? C2 N1 C3 108.4(5) . . ? C2 N1 C1 124.1(5) . . ? C3 N1 C1 127.5(5) . . ? C2 N2 C4 108.6(5) . . ? C2 N2 C5 123.3(5) . . ? C4 N2 C5 128.0(5) . . ? C5 N3 C9 116.1(5) . . ? C10 N4 C11 108.5(5) . . ? C10 N4 C9 123.4(5) . . ? C11 N4 C9 128.1(5) . . ? C10 N5 C12 108.5(5) . . ? C10 N5 C13 125.5(5) . . ? C12 N5 C13 126.1(5) . . ? N1 C1 C17 114.5(5) . 3_666 ? N1 C1 H1A 108.6 . . ? C17 C1 H1A 108.6 3_666 . ? N1 C1 H1B 108.6 . . ? C17 C1 H1B 108.6 3_666 . ? H1A C1 H1B 107.6 . . ? N1 C2 N2 108.6(5) . . ? N1 C2 H2A 125.7 . . ? N2 C2 H2A 125.7 . . ? C4 C3 N1 107.7(6) . . ? C4 C3 H3A 126.2 . . ? N1 C3 H3A 126.2 . . ? C3 C4 N2 106.6(6) . . ? C3 C4 H4A 126.7 . . ? N2 C4 H4A 126.7 . . ? N3 C5 C6 125.1(6) . . ? N3 C5 N2 113.3(5) . . ? C6 C5 N2 121.5(5) . . ? C5 C6 C7 116.4(6) . . ? C5 C6 H6A 121.8 . . ? C7 C6 H6A 121.8 . . ? C8 C7 C6 120.2(6) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C9 C8 C7 116.8(6) . . ? C9 C8 H8A 121.6 . . ? C7 C8 H8A 121.6 . . ? N3 C9 C8 125.4(6) . . ? N3 C9 N4 113.0(5) . . ? C8 C9 N4 121.6(5) . . ? N5 C10 N4 108.5(5) . . ? N5 C10 H10A 125.8 . . ? N4 C10 H10A 125.8 . . ? C12 C11 N4 106.5(6) . . ? C12 C11 H11A 126.7 . . ? N4 C11 H11A 126.7 . . ? C11 C12 N5 108.1(6) . . ? C11 C12 H12A 126.0 . . ? N5 C12 H12A 126.0 . . ? N5 C13 C14 113.6(5) . . ? N5 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N5 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C19 118.4(6) . . ? C15 C14 C13 123.2(6) . . ? C19 C14 C13 118.4(5) . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C17 C16 C15 120.8(6) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 118.8(6) . . ? C16 C17 C1 119.7(5) . 3_666 ? C18 C17 C1 121.4(5) . 3_666 ? C19 C18 C17 119.8(6) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C14 121.5(6) . . ? C18 C19 H19A 119.3 . . ? C14 C19 H19A 119.3 . . ? O1 C20 O2 123.9(5) . . ? O1 C20 C21 116.7(5) . . ? O2 C20 C21 119.4(5) . . ? C26 C21 C22 119.5(5) . . ? C26 C21 C20 119.7(5) . . ? C22 C21 C20 120.7(5) . . ? C23 C22 C21 120.4(6) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 120.6(5) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C25 C24 C23 118.8(5) . . ? C25 C24 C27 119.9(6) . . ? C23 C24 C27 121.3(5) . . ? C26 C25 C24 120.7(6) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C25 C26 C21 119.9(5) . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? O3 C27 O4 123.7(6) . . ? O3 C27 C24 117.8(5) . . ? O4 C27 C24 118.5(5) . . ? O6 C28 O5 125.1(5) . . ? O6 C28 C29 118.6(5) . . ? O5 C28 C29 116.3(5) . . ? C34 C29 C30 119.0(6) . . ? C34 C29 C28 120.2(5) . . ? C30 C29 C28 120.7(5) . . ? C31 C30 C29 119.4(6) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C30 C31 C32 121.2(6) . . ? C30 C31 H31A 119.4 . . ? C32 C31 H31A 119.4 . . ? C33 C32 C31 118.7(6) . . ? C33 C32 C35 119.4(6) . . ? C31 C32 C35 121.9(6) . . ? C32 C33 C34 121.3(6) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? C33 C34 C29 120.5(6) . . ? C33 C34 H34A 119.8 . . ? C29 C34 H34A 119.8 . . ? O7 C35 O8 125.7(7) . . ? O7 C35 C32 119.4(6) . . ? O8 C35 C32 114.9(7) . . ? O10 C36 O9 120.3(5) . . ? O10 C36 C37 121.4(5) . . ? O9 C36 C37 118.3(5) . . ? O10 C36 Gd1 63.4(3) . . ? O9 C36 Gd1 57.4(3) . . ? C37 C36 Gd1 171.8(4) . . ? C38 C37 C39 120.4(5) . 3_666 ? C38 C37 C36 120.0(5) . . ? C39 C37 C36 119.5(5) 3_666 . ? C37 C38 C39 119.8(5) . . ? C37 C38 H38A 120.1 . . ? C39 C38 H38A 120.1 . . ? C38 C39 C37 119.8(5) . 3_666 ? C38 C39 H39A 120.1 . . ? C37 C39 H39A 120.1 3_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Gd1 O1 C20 117.9(7) . . . . ? O1W Gd1 O1 C20 -143.5(6) . . . . ? O3W Gd1 O1 C20 16.3(6) . . . . ? O9 Gd1 O1 C20 -76.3(6) . . . . ? O4W Gd1 O1 C20 62.1(7) . . . . ? O2W Gd1 O1 C20 -164.2(7) . . . . ? O10 Gd1 O1 C20 -46.2(7) . . . . ? C36 Gd1 O1 C20 -63.9(7) . . . . ? O1 Gd1 O5 C28 38.1(5) . . . . ? O1W Gd1 O5 C28 -100.8(5) . . . . ? O3W Gd1 O5 C28 109.2(5) . . . . ? O9 Gd1 O5 C28 -1.6(8) . . . . ? O4W Gd1 O5 C28 -176.0(6) . . . . ? O2W Gd1 O5 C28 -31.9(5) . . . . ? O10 Gd1 O5 C28 -169.0(5) . . . . ? C36 Gd1 O5 C28 -126.6(12) . . . . ? O5 Gd1 O9 C36 -167.6(4) . . . . ? O1 Gd1 O9 C36 151.7(3) . . . . ? O1W Gd1 O9 C36 -65.7(3) . . . . ? O3W Gd1 O9 C36 79.6(3) . . . . ? O4W Gd1 O9 C36 5.5(4) . . . . ? O2W Gd1 O9 C36 -137.9(3) . . . . ? O10 Gd1 O9 C36 4.3(3) . . . . ? O5 Gd1 O10 C36 169.7(3) . . . . ? O1 Gd1 O10 C36 -42.5(3) . . . . ? O1W Gd1 O10 C36 94.0(3) . . . . ? O3W Gd1 O10 C36 -102.4(3) . . . . ? O9 Gd1 O10 C36 -4.3(3) . . . . ? O4W Gd1 O10 C36 176.6(3) . . . . ? O2W Gd1 O10 C36 42.9(3) . . . . ? C2 N1 C1 C17 -67.0(7) . . . 3_666 ? C3 N1 C1 C17 114.9(7) . . . 3_666 ? C3 N1 C2 N2 -0.7(7) . . . . ? C1 N1 C2 N2 -179.1(5) . . . . ? C4 N2 C2 N1 1.0(7) . . . . ? C5 N2 C2 N1 -176.3(5) . . . . ? C2 N1 C3 C4 0.1(8) . . . . ? C1 N1 C3 C4 178.5(6) . . . . ? N1 C3 C4 N2 0.5(8) . . . . ? C2 N2 C4 C3 -0.9(7) . . . . ? C5 N2 C4 C3 176.3(6) . . . . ? C9 N3 C5 C6 1.3(8) . . . . ? C9 N3 C5 N2 178.7(5) . . . . ? C2 N2 C5 N3 6.0(8) . . . . ? C4 N2 C5 N3 -170.8(6) . . . . ? C2 N2 C5 C6 -176.5(5) . . . . ? C4 N2 C5 C6 6.7(9) . . . . ? N3 C5 C6 C7 0.3(9) . . . . ? N2 C5 C6 C7 -177.0(5) . . . . ? C5 C6 C7 C8 -1.1(9) . . . . ? C6 C7 C8 C9 0.4(9) . . . . ? C5 N3 C9 C8 -2.2(8) . . . . ? C5 N3 C9 N4 177.0(5) . . . . ? C7 C8 C9 N3 1.4(9) . . . . ? C7 C8 C9 N4 -177.8(5) . . . . ? C10 N4 C9 N3 -19.5(8) . . . . ? C11 N4 C9 N3 161.5(5) . . . . ? C10 N4 C9 C8 159.7(6) . . . . ? C11 N4 C9 C8 -19.2(9) . . . . ? C12 N5 C10 N4 0.0(7) . . . . ? C13 N5 C10 N4 179.9(5) . . . . ? C11 N4 C10 N5 0.7(6) . . . . ? C9 N4 C10 N5 -178.4(5) . . . . ? C10 N4 C11 C12 -1.1(7) . . . . ? C9 N4 C11 C12 177.9(6) . . . . ? N4 C11 C12 N5 1.1(7) . . . . ? C10 N5 C12 C11 -0.7(7) . . . . ? C13 N5 C12 C11 179.4(6) . . . . ? C10 N5 C13 C14 107.2(6) . . . . ? C12 N5 C13 C14 -72.9(7) . . . . ? N5 C13 C14 C15 -8.2(8) . . . . ? N5 C13 C14 C19 171.4(5) . . . . ? C19 C14 C15 C16 -1.9(9) . . . . ? C13 C14 C15 C16 177.7(6) . . . . ? C14 C15 C16 C17 0.5(9) . . . . ? C15 C16 C17 C18 1.4(9) . . . . ? C15 C16 C17 C1 -174.8(5) . . . 3_666 ? C16 C17 C18 C19 -1.9(8) . . . . ? C1 C17 C18 C19 174.2(5) 3_666 . . . ? C17 C18 C19 C14 0.4(9) . . . . ? C15 C14 C19 C18 1.5(9) . . . . ? C13 C14 C19 C18 -178.2(5) . . . . ? Gd1 O1 C20 O2 -5.7(10) . . . . ? Gd1 O1 C20 C21 174.6(4) . . . . ? O1 C20 C21 C26 -4.2(8) . . . . ? O2 C20 C21 C26 176.0(5) . . . . ? O1 C20 C21 C22 172.9(5) . . . . ? O2 C20 C21 C22 -6.8(8) . . . . ? C26 C21 C22 C23 0.5(8) . . . . ? C20 C21 C22 C23 -176.7(5) . . . . ? C21 C22 C23 C24 -1.3(9) . . . . ? C22 C23 C24 C25 0.9(8) . . . . ? C22 C23 C24 C27 -179.6(5) . . . . ? C23 C24 C25 C26 0.3(8) . . . . ? C27 C24 C25 C26 -179.1(5) . . . . ? C24 C25 C26 C21 -1.1(9) . . . . ? C22 C21 C26 C25 0.7(8) . . . . ? C20 C21 C26 C25 177.9(5) . . . . ? C25 C24 C27 O3 -12.1(8) . . . . ? C23 C24 C27 O3 168.5(6) . . . . ? C25 C24 C27 O4 168.2(5) . . . . ? C23 C24 C27 O4 -11.2(8) . . . . ? Gd1 O5 C28 O6 5.8(9) . . . . ? Gd1 O5 C28 C29 -176.0(4) . . . . ? O6 C28 C29 C34 164.9(6) . . . . ? O5 C28 C29 C34 -13.4(8) . . . . ? O6 C28 C29 C30 -13.8(9) . . . . ? O5 C28 C29 C30 167.9(5) . . . . ? C34 C29 C30 C31 0.3(9) . . . . ? C28 C29 C30 C31 179.0(6) . . . . ? C29 C30 C31 C32 -1.6(10) . . . . ? C30 C31 C32 C33 1.4(9) . . . . ? C30 C31 C32 C35 -178.9(6) . . . . ? C31 C32 C33 C34 0.1(9) . . . . ? C35 C32 C33 C34 -179.6(6) . . . . ? C32 C33 C34 C29 -1.4(9) . . . . ? C30 C29 C34 C33 1.2(9) . . . . ? C28 C29 C34 C33 -177.6(6) . . . . ? C33 C32 C35 O7 -13.6(9) . . . . ? C31 C32 C35 O7 166.7(6) . . . . ? C33 C32 C35 O8 165.6(6) . . . . ? C31 C32 C35 O8 -14.1(9) . . . . ? Gd1 O10 C36 O9 7.5(5) . . . . ? Gd1 O10 C36 C37 -172.3(5) . . . . ? Gd1 O9 C36 O10 -8.0(5) . . . . ? Gd1 O9 C36 C37 171.8(4) . . . . ? O5 Gd1 C36 O10 -51.4(14) . . . . ? O1 Gd1 C36 O10 144.1(3) . . . . ? O1W Gd1 C36 O10 -77.9(3) . . . . ? O3W Gd1 C36 O10 73.5(3) . . . . ? O9 Gd1 C36 O10 172.3(5) . . . . ? O4W Gd1 C36 O10 -3.4(3) . . . . ? O2W Gd1 C36 O10 -144.5(3) . . . . ? O5 Gd1 C36 O9 136.3(12) . . . . ? O1 Gd1 C36 O9 -28.2(3) . . . . ? O1W Gd1 C36 O9 109.8(3) . . . . ? O3W Gd1 C36 O9 -98.8(3) . . . . ? O4W Gd1 C36 O9 -175.7(3) . . . . ? O2W Gd1 C36 O9 43.2(3) . . . . ? O10 Gd1 C36 O9 -172.3(5) . . . . ? O5 Gd1 C36 C37 75(3) . . . . ? O1 Gd1 C36 C37 -89(3) . . . . ? O1W Gd1 C36 C37 49(3) . . . . ? O3W Gd1 C36 C37 -160(3) . . . . ? O9 Gd1 C36 C37 -61(3) . . . . ? O4W Gd1 C36 C37 123(3) . . . . ? O2W Gd1 C36 C37 -18(3) . . . . ? O10 Gd1 C36 C37 127(3) . . . . ? O10 C36 C37 C38 9.6(8) . . . . ? O9 C36 C37 C38 -170.2(5) . . . . ? Gd1 C36 C37 C38 -113(3) . . . . ? O10 C36 C37 C39 -172.0(5) . . . 3_666 ? O9 C36 C37 C39 8.2(8) . . . 3_666 ? Gd1 C36 C37 C39 65(3) . . . 3_666 ? C39 C37 C38 C39 0.0(9) 3_666 . . . ? C36 C37 C38 C39 178.4(5) . . . . ? C37 C38 C39 C37 0.0(9) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.258 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.134 # Attachment '- RSOF-Tm as CCDC 838077.CIF' data_RSOF-Tm _database_code_depnum_ccdc_archive 'CCDC 838077' #TrackingRef '- RSOF-Tm as CCDC 838077.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; cyclo(2)(2,6-di(1H-imidazol-1-yl)pyridine)(2)(1,4- dimethylenebenzene) _ 5 terephthalate dianion_ 2 thulium(iii)_8 H2O_32 H2O ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H134 N10 O60 Tm2' _chemical_formula_weight 2509.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.186(2) _cell_length_b 17.851(4) _cell_length_c 24.578(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.16(3) _cell_angle_gamma 90.00 _cell_volume 4845.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8189 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 24.99 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2380 _exptl_absorpt_coefficient_mu 1.923 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6377 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method dtintegrate.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38033 _diffrn_reflns_av_R_equivalents 0.1443 _diffrn_reflns_av_sigmaI/netI 0.1459 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 24.99 _reflns_number_total 8189 _reflns_number_gt 5194 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Sheldrick, G. M. Acta Cryst., 2008, A64, 112-122. ; _publ_section_acknowledgements ; The data were collected using instrumentation purchased with funds provided by the National Science Foundation Grant No. 0741973. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is a solvent channel along x, 1/2, 0 containing several molecules of water. Where possible, these water molecules were refined. However, some regions of diffuse electron density persisted where discrete molecules of water could not be modeled. The utility, Squeeze (Sluis, and Spek, 1990) was used to remove the contributions to the scattering factors due from these diffuse regions of electron density. Squeeze is a component of Platon98 (Spek, 1998) and was used as incorporated in WinGX (Farrugia, 1998). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8189 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1441 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2455 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.81090(5) 0.70075(3) 0.63434(2) 0.0346(2) Uani 1 1 d . . . O1 O 0.7045(8) 0.7214(5) 0.7051(4) 0.041(2) Uani 1 1 d . . . O1W O 0.9337(7) 0.6107(5) 0.6042(4) 0.038(2) Uani 1 1 d . . . O2W O 0.8819(7) 0.6197(5) 0.7112(3) 0.033(2) Uani 1 1 d . . . O2 O 0.5415(8) 0.7967(6) 0.6869(4) 0.047(2) Uani 1 1 d . . . O3W O 0.6718(8) 0.7950(5) 0.6059(4) 0.041(2) Uani 1 1 d . . . O3 O 0.5805(9) 0.6516(6) 0.9699(4) 0.056(3) Uani 1 1 d . . . O4 O 0.4580(8) 0.7510(6) 0.9649(4) 0.043(2) Uani 1 1 d . . . O4W O 0.9103(8) 0.7680(5) 0.5709(4) 0.040(2) Uani 1 1 d . . . O5 O 0.9586(8) 0.7718(5) 0.6844(4) 0.044(2) Uani 1 1 d . . . O5W O 1.4723(8) 0.8967(6) 0.9988(4) 0.048(3) Uani 1 1 d . . . O6 O 0.9685(8) 0.7383(5) 0.7744(4) 0.044(2) Uani 1 1 d . . . O6W O 1.0967(11) 0.6714(8) 0.8661(5) 0.085(4) Uani 1 1 d . . . O7 O 1.4457(8) 1.0182(5) 0.7629(4) 0.046(3) Uani 1 1 d . . . O7W O 0.7124(10) 0.7283(9) 0.4403(5) 0.100(5) Uani 1 1 d . . . O8 O 1.3934(8) 1.0241(6) 0.8453(5) 0.060(3) Uani 1 1 d . . . O8W O 1.3429(9) 1.0086(6) 0.9478(5) 0.062(3) Uani 1 1 d . . . O9 O 0.6551(7) 0.6123(5) 0.6144(4) 0.035(2) Uani 1 1 d . . . O9W O 0.9552(12) 1.1070(6) 0.4282(5) 0.077(4) Uani 1 1 d . . . O10 O 0.7124(8) 0.6566(5) 0.5405(4) 0.037(2) Uani 1 1 d . . . O10W O 1.0978(12) 0.9873(7) 0.4191(5) 0.082(4) Uani 1 1 d . . . N1 N 0.7175(9) 0.4558(6) 0.7209(5) 0.039(3) Uani 1 1 d . . . N2 N 0.5691(9) 0.5162(6) 0.7508(4) 0.031(2) Uani 1 1 d . . . N3 N 0.4335(9) 0.5964(6) 0.6987(4) 0.034(3) Uani 1 1 d . . . N4 N 0.3124(9) 0.6773(6) 0.6416(4) 0.031(3) Uani 1 1 d . . . N5 N 0.3392(9) 0.7193(6) 0.5611(5) 0.039(3) Uani 1 1 d . . . C1 C 0.8031(11) 0.4329(8) 0.6847(6) 0.046(4) Uani 1 1 d . . . H1A H 0.8638 0.4007 0.7053 0.055 Uiso 1 1 calc R . . H1B H 0.8442 0.4773 0.6742 0.055 Uiso 1 1 calc R . . C2 C 0.6311(11) 0.5083(7) 0.7088(6) 0.041(4) Uani 1 1 d . . . H2A H 0.6165 0.5353 0.6761 0.049 Uiso 1 1 calc R . . C3 C 0.7073(13) 0.4296(9) 0.7722(7) 0.049(4) Uani 1 1 d . . . H3A H 0.7564 0.3930 0.7911 0.058 Uiso 1 1 calc R . . C4 C 0.6172(14) 0.4639(9) 0.7910(6) 0.053(4) Uani 1 1 d . . . H4A H 0.5909 0.4551 0.8245 0.064 Uiso 1 1 calc R . . C5 C 0.4650(12) 0.5651(8) 0.7488(6) 0.0428(16) Uani 1 1 d . . . C6 C 0.4092(11) 0.5738(8) 0.7939(6) 0.0428(16) Uani 1 1 d . . . H6A H 0.4362 0.5498 0.8272 0.051 Uiso 1 1 calc R . . C7 C 0.3092(12) 0.6212(8) 0.7868(6) 0.0428(16) Uani 1 1 d . . . H7A H 0.2680 0.6312 0.8160 0.051 Uiso 1 1 calc R . . C8 C 0.2720(12) 0.6529(8) 0.7362(6) 0.0428(16) Uani 1 1 d . . . H8A H 0.2027 0.6825 0.7310 0.051 Uiso 1 1 calc R . . C9 C 0.3350(12) 0.6423(8) 0.6926(6) 0.0428(16) Uani 1 1 d . . . C10 C 0.3886(11) 0.6821(7) 0.6062(5) 0.033(3) Uani 1 1 d . . . H10A H 0.4665 0.6623 0.6118 0.040 Uiso 1 1 calc R . . C11 C 0.2026(12) 0.7096(7) 0.6178(6) 0.042(4) Uani 1 1 d . . . H11A H 0.1312 0.7111 0.6326 0.050 Uiso 1 1 calc R . . C12 C 0.2207(12) 0.7379(9) 0.5689(6) 0.050(4) Uani 1 1 d . . . H12A H 0.1648 0.7650 0.5446 0.061 Uiso 1 1 calc R . . C13 C 0.3955(10) 0.7364(8) 0.5133(5) 0.037(3) Uani 1 1 d . . . H13A H 0.4821 0.7282 0.5224 0.045 Uiso 1 1 calc R . . H13B H 0.3827 0.7890 0.5041 0.045 Uiso 1 1 calc R . . C14 C 0.3448(11) 0.6882(6) 0.4619(6) 0.035(3) Uani 1 1 d . . . C15 C 0.2661(12) 0.6265(8) 0.4643(6) 0.042(4) Uani 1 1 d . . . H15A H 0.2428 0.6135 0.4977 0.051 Uiso 1 1 calc R . . C16 C 0.2243(12) 0.5860(8) 0.4183(6) 0.044(4) Uani 1 1 d . . . H16A H 0.1767 0.5438 0.4207 0.052 Uiso 1 1 calc R . . C17 C 0.2532(11) 0.6081(8) 0.3676(6) 0.042(4) Uani 1 1 d . . . C18 C 0.3318(12) 0.6678(7) 0.3649(6) 0.036(3) Uani 1 1 d . . . H18A H 0.3542 0.6814 0.3314 0.043 Uiso 1 1 calc R . . C19 C 0.3768(12) 0.7073(7) 0.4128(5) 0.036(3) Uani 1 1 d . . . H19A H 0.4293 0.7473 0.4110 0.043 Uiso 1 1 calc R . . C20 C 0.6131(11) 0.7552(9) 0.7180(5) 0.039(4) Uani 1 1 d . . . C21 C 0.5898(11) 0.7400(7) 0.7774(6) 0.0359(13) Uani 1 1 d . . . C22 C 0.4921(11) 0.7773(7) 0.7962(6) 0.0359(13) Uani 1 1 d . . . H22A H 0.4408 0.8083 0.7727 0.043 Uiso 1 1 calc R . . C23 C 0.4744(11) 0.7666(7) 0.8503(5) 0.0359(13) Uani 1 1 d . . . H23A H 0.4128 0.7928 0.8633 0.043 Uiso 1 1 calc R . . C24 C 0.5463(11) 0.7178(7) 0.8859(6) 0.0359(13) Uani 1 1 d . . . C25 C 0.6417(12) 0.6812(7) 0.8657(6) 0.0359(13) Uani 1 1 d . . . H25A H 0.6919 0.6491 0.8888 0.043 Uiso 1 1 calc R . . C26 C 0.6623(11) 0.6923(7) 0.8118(5) 0.0359(13) Uani 1 1 d . . . H26A H 0.7254 0.6672 0.7991 0.043 Uiso 1 1 calc R . . C27 C 0.5279(11) 0.7064(8) 0.9437(6) 0.039(3) Uani 1 1 d . . . C28 C 0.9979(12) 0.7773(7) 0.7355(6) 0.033(3) Uani 1 1 d . . . C29 C 1.0984(11) 0.8350(8) 0.7528(6) 0.038(3) Uani 1 1 d . . . C30 C 1.1311(11) 0.8586(8) 0.8062(6) 0.042(4) Uani 1 1 d . . . H30A H 1.0906 0.8391 0.8332 0.050 Uiso 1 1 calc R . . C31 C 1.2230(11) 0.9109(8) 0.8211(6) 0.047(4) Uani 1 1 d . . . H31A H 1.2440 0.9255 0.8577 0.057 Uiso 1 1 calc R . . C32 C 1.2820(11) 0.9405(7) 0.7812(6) 0.036(3) Uani 1 1 d . . . C33 C 1.2486(11) 0.9203(7) 0.7267(6) 0.038(3) Uani 1 1 d . . . H33A H 1.2890 0.9407 0.6999 0.045 Uiso 1 1 calc R . . C34 C 1.1537(11) 0.8688(7) 0.7115(6) 0.040(3) Uani 1 1 d . . . H34A H 1.1279 0.8573 0.6746 0.048 Uiso 1 1 calc R . . C35 C 1.3817(12) 0.9972(8) 0.7971(6) 0.042(4) Uani 1 1 d . . . C36 C 0.6507(11) 0.6103(8) 0.5626(6) 0.037(3) Uani 1 1 d . . . C37 C 0.5708(11) 0.5518(7) 0.5293(6) 0.035(3) Uani 1 1 d . . . C38 C 0.5806(10) 0.5443(8) 0.4746(6) 0.037(3) Uani 1 1 d . . . H38A H 0.6322 0.5743 0.4579 0.045 Uiso 1 1 calc R . . C39 C 0.5077(10) 0.4884(7) 0.4453(5) 0.032(3) Uani 1 1 d . . . H39A H 0.5134 0.4790 0.4086 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm1 0.0278(3) 0.0404(4) 0.0340(4) -0.0036(3) 0.0007(2) -0.0022(3) O1 0.033(5) 0.054(6) 0.040(6) -0.005(5) 0.023(5) 0.006(4) O1W 0.030(5) 0.035(5) 0.050(6) 0.003(4) 0.010(4) 0.014(4) O2W 0.022(4) 0.036(5) 0.037(5) -0.004(4) -0.003(4) -0.003(4) O2 0.033(5) 0.062(7) 0.042(6) 0.009(5) -0.003(4) 0.011(5) O3W 0.033(5) 0.046(6) 0.044(6) 0.000(5) 0.002(4) 0.013(4) O3 0.059(7) 0.059(7) 0.050(7) 0.009(6) 0.012(5) 0.008(6) O4 0.031(5) 0.060(7) 0.040(6) -0.003(5) 0.009(4) 0.009(5) O4W 0.038(5) 0.057(6) 0.025(5) 0.013(4) 0.007(4) 0.007(4) O5 0.050(6) 0.049(6) 0.036(6) -0.009(5) 0.014(5) -0.013(5) O5W 0.040(5) 0.058(7) 0.047(6) -0.003(5) 0.008(5) -0.011(5) O6 0.045(6) 0.057(6) 0.029(6) -0.020(5) 0.003(4) -0.020(5) O6W 0.082(9) 0.095(10) 0.079(10) 0.006(8) 0.017(7) 0.013(7) O7 0.028(5) 0.051(6) 0.054(7) 0.006(5) -0.009(5) -0.002(4) O7W 0.054(7) 0.173(15) 0.069(9) 0.055(9) 0.001(7) -0.021(8) O8 0.042(6) 0.063(7) 0.074(9) -0.010(6) 0.004(6) -0.017(5) O8W 0.066(7) 0.061(7) 0.064(8) -0.004(6) 0.026(6) -0.014(6) O9 0.025(4) 0.038(5) 0.036(6) 0.001(4) -0.013(4) -0.004(4) O9W 0.119(10) 0.063(8) 0.047(7) 0.002(6) 0.002(7) 0.001(7) O10 0.042(5) 0.025(5) 0.043(6) 0.000(4) 0.009(4) -0.004(4) O10W 0.113(10) 0.071(8) 0.062(9) 0.009(7) 0.014(7) 0.009(8) N1 0.023(6) 0.044(7) 0.048(8) -0.004(6) -0.002(5) -0.005(5) N2 0.031(6) 0.033(6) 0.032(6) 0.003(5) 0.018(5) 0.004(5) N3 0.035(6) 0.033(6) 0.033(6) -0.017(5) 0.006(5) -0.004(5) N4 0.037(6) 0.031(6) 0.025(6) -0.004(5) 0.003(5) -0.001(5) N5 0.019(5) 0.045(7) 0.048(8) 0.011(6) -0.007(5) 0.001(5) C1 0.031(7) 0.034(8) 0.065(11) -0.011(7) -0.016(7) 0.011(6) C2 0.025(7) 0.034(8) 0.058(10) 0.000(7) -0.015(7) 0.002(6) C3 0.040(8) 0.054(10) 0.052(10) -0.010(8) 0.003(8) 0.007(7) C4 0.066(10) 0.072(11) 0.020(8) 0.009(7) 0.001(7) -0.004(9) C5 0.032(3) 0.048(4) 0.052(4) -0.010(3) 0.019(3) -0.013(3) C6 0.032(3) 0.048(4) 0.052(4) -0.010(3) 0.019(3) -0.013(3) C7 0.032(3) 0.048(4) 0.052(4) -0.010(3) 0.019(3) -0.013(3) C8 0.032(3) 0.048(4) 0.052(4) -0.010(3) 0.019(3) -0.013(3) C9 0.032(3) 0.048(4) 0.052(4) -0.010(3) 0.019(3) -0.013(3) C10 0.024(7) 0.039(8) 0.035(8) -0.002(6) -0.002(6) 0.004(5) C11 0.036(8) 0.040(8) 0.049(9) -0.018(7) 0.005(7) 0.012(6) C12 0.038(8) 0.077(11) 0.029(8) 0.008(8) -0.017(7) -0.005(8) C13 0.019(6) 0.064(9) 0.025(7) -0.006(7) -0.005(6) -0.001(6) C14 0.032(7) 0.022(7) 0.043(8) -0.007(6) -0.015(6) 0.009(5) C15 0.041(8) 0.056(10) 0.032(8) 0.001(7) 0.011(6) -0.009(7) C16 0.044(8) 0.039(8) 0.047(10) -0.016(7) 0.006(7) -0.007(7) C17 0.029(7) 0.056(9) 0.034(8) -0.006(7) -0.022(6) 0.018(7) C18 0.043(8) 0.027(7) 0.039(8) 0.012(6) 0.011(7) 0.001(6) C19 0.048(8) 0.026(7) 0.035(8) 0.007(6) 0.010(7) -0.006(6) C20 0.025(7) 0.069(10) 0.019(7) -0.008(7) -0.012(6) -0.017(7) C21 0.033(3) 0.035(3) 0.039(3) -0.006(3) 0.005(3) -0.008(2) C22 0.033(3) 0.035(3) 0.039(3) -0.006(3) 0.005(3) -0.008(2) C23 0.033(3) 0.035(3) 0.039(3) -0.006(3) 0.005(3) -0.008(2) C24 0.033(3) 0.035(3) 0.039(3) -0.006(3) 0.005(3) -0.008(2) C25 0.033(3) 0.035(3) 0.039(3) -0.006(3) 0.005(3) -0.008(2) C26 0.033(3) 0.035(3) 0.039(3) -0.006(3) 0.005(3) -0.008(2) C27 0.022(7) 0.059(10) 0.034(8) 0.005(7) 0.001(6) -0.007(7) C28 0.036(8) 0.035(8) 0.031(8) 0.004(6) 0.013(6) 0.015(6) C29 0.031(7) 0.046(8) 0.037(8) -0.010(7) 0.006(6) 0.001(6) C30 0.022(7) 0.045(9) 0.058(10) -0.006(7) 0.005(7) 0.004(6) C31 0.030(7) 0.059(10) 0.045(9) -0.016(8) -0.017(7) -0.002(7) C32 0.022(6) 0.037(8) 0.051(9) 0.000(7) 0.009(6) -0.012(6) C33 0.041(8) 0.027(7) 0.037(8) -0.010(6) -0.016(6) 0.002(6) C34 0.042(8) 0.041(8) 0.031(8) -0.001(6) -0.010(6) 0.003(6) C35 0.035(8) 0.049(9) 0.036(9) -0.009(7) -0.009(7) 0.002(7) C36 0.027(7) 0.043(8) 0.039(9) -0.005(7) 0.001(6) -0.001(6) C37 0.026(7) 0.032(7) 0.044(9) 0.006(6) -0.006(6) -0.002(6) C38 0.013(6) 0.062(10) 0.036(8) 0.021(7) -0.002(6) -0.004(6) C39 0.020(6) 0.049(8) 0.027(7) 0.009(6) 0.001(5) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O5 2.282(9) . ? Tm1 O1 2.288(8) . ? Tm1 O1W 2.311(8) . ? Tm1 O3W 2.322(8) . ? Tm1 O9 2.345(8) . ? Tm1 O4W 2.378(8) . ? Tm1 O2W 2.411(8) . ? Tm1 O10 2.520(9) . ? Tm1 C36 2.814(13) . ? O1 C20 1.270(15) . ? O2 C20 1.257(16) . ? O3 C27 1.263(16) . ? O4 C27 1.284(16) . ? O5 C28 1.266(15) . ? O6 C28 1.268(15) . ? O7 C35 1.246(17) . ? O8 C35 1.266(16) . ? O9 C36 1.266(15) . ? O10 C36 1.255(15) . ? N1 C2 1.346(15) . ? N1 C3 1.365(18) . ? N1 C1 1.466(18) . ? N2 C2 1.338(17) . ? N2 C4 1.403(17) . ? N2 C5 1.449(16) . ? N3 C5 1.347(17) . ? N3 C9 1.361(17) . ? N4 C10 1.315(15) . ? N4 C9 1.386(17) . ? N4 C11 1.398(16) . ? N5 C10 1.333(16) . ? N5 C13 1.453(17) . ? N5 C12 1.408(17) . ? C1 C17 1.525(18) 3_666 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 C4 1.32(2) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.367(18) . ? C6 C7 1.391(19) . ? C6 H6A 0.9300 . ? C7 C8 1.37(2) . ? C7 H7A 0.9300 . ? C8 C9 1.387(18) . ? C8 H8A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.35(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.559(17) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.355(18) . ? C14 C15 1.417(18) . ? C15 C16 1.360(18) . ? C15 H15A 0.9300 . ? C16 C17 1.392(19) . ? C16 H16A 0.9300 . ? C17 C18 1.391(19) . ? C17 C1 1.525(18) 3_666 ? C18 C19 1.395(18) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.547(18) . ? C21 C26 1.371(18) . ? C21 C22 1.418(17) . ? C22 C23 1.388(18) . ? C22 H22A 0.9300 . ? C23 C24 1.395(18) . ? C23 H23A 0.9300 . ? C24 C25 1.407(18) . ? C24 C27 1.481(19) . ? C25 C26 1.396(18) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 C29 1.534(19) . ? C29 C30 1.371(18) . ? C29 C34 1.406(19) . ? C30 C31 1.394(18) . ? C30 H30A 0.9300 . ? C31 C32 1.372(19) . ? C31 H31A 0.9300 . ? C32 C33 1.380(18) . ? C32 C35 1.512(18) . ? C33 C34 1.409(17) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C36 C37 1.526(17) . ? C37 C39 1.361(17) 3_666 ? C37 C38 1.371(18) . ? C38 C39 1.412(18) . ? C38 H38A 0.9300 . ? C39 C37 1.361(17) 3_666 ? C39 H39A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Tm1 O1 85.4(3) . . ? O5 Tm1 O1W 98.3(3) . . ? O1 Tm1 O1W 139.7(3) . . ? O5 Tm1 O3W 98.8(3) . . ? O1 Tm1 O3W 73.0(3) . . ? O1W Tm1 O3W 144.2(3) . . ? O5 Tm1 O9 159.6(3) . . ? O1 Tm1 O9 78.9(3) . . ? O1W Tm1 O9 85.7(3) . . ? O3W Tm1 O9 89.1(3) . . ? O5 Tm1 O4W 72.5(3) . . ? O1 Tm1 O4W 140.4(3) . . ? O1W Tm1 O4W 77.1(3) . . ? O3W Tm1 O4W 78.4(3) . . ? O9 Tm1 O4W 127.7(3) . . ? O5 Tm1 O2W 78.0(3) . . ? O1 Tm1 O2W 69.3(3) . . ? O1W Tm1 O2W 72.3(3) . . ? O3W Tm1 O2W 142.3(3) . . ? O9 Tm1 O2W 84.3(3) . . ? O4W Tm1 O2W 133.3(3) . . ? O5 Tm1 O10 147.3(3) . . ? O1 Tm1 O10 122.8(3) . . ? O1W Tm1 O10 71.6(3) . . ? O3W Tm1 O10 77.1(3) . . ? O9 Tm1 O10 52.8(3) . . ? O4W Tm1 O10 74.9(3) . . ? O2W Tm1 O10 124.8(3) . . ? O5 Tm1 C36 172.3(4) . . ? O1 Tm1 C36 102.3(4) . . ? O1W Tm1 C36 75.6(3) . . ? O3W Tm1 C36 84.1(4) . . ? O9 Tm1 C36 26.5(3) . . ? O4W Tm1 C36 101.3(4) . . ? O2W Tm1 C36 104.1(3) . . ? O10 Tm1 C36 26.5(3) . . ? C20 O1 Tm1 143.4(9) . . ? C28 O5 Tm1 133.2(9) . . ? C36 O9 Tm1 97.9(8) . . ? C36 O10 Tm1 89.9(8) . . ? C2 N1 C3 106.2(12) . . ? C2 N1 C1 125.1(13) . . ? C3 N1 C1 128.7(12) . . ? C2 N2 C4 106.6(11) . . ? C2 N2 C5 123.2(11) . . ? C4 N2 C5 129.9(12) . . ? C5 N3 C9 116.2(11) . . ? C10 N4 C9 125.7(11) . . ? C10 N4 C11 108.3(11) . . ? C9 N4 C11 125.9(12) . . ? C10 N5 C13 127.0(11) . . ? C10 N5 C12 106.2(12) . . ? C13 N5 C12 126.8(11) . . ? N1 C1 C17 115.1(11) . 3_666 ? N1 C1 H1A 108.5 . . ? C17 C1 H1A 108.5 3_666 . ? N1 C1 H1B 108.5 . . ? C17 C1 H1B 108.5 3_666 . ? H1A C1 H1B 107.5 . . ? N2 C2 N1 110.2(13) . . ? N2 C2 H2A 124.9 . . ? N1 C2 H2A 124.9 . . ? C4 C3 N1 110.2(14) . . ? C4 C3 H3A 124.9 . . ? N1 C3 H3A 124.9 . . ? C3 C4 N2 106.8(13) . . ? C3 C4 H4A 126.6 . . ? N2 C4 H4A 126.6 . . ? N3 C5 C6 127.4(13) . . ? N3 C5 N2 112.0(11) . . ? C6 C5 N2 120.6(14) . . ? C5 C6 C7 115.4(14) . . ? C5 C6 H6A 122.3 . . ? C7 C6 H6A 122.3 . . ? C6 C7 C8 119.2(13) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C7 C8 C9 121.8(14) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? N3 C9 N4 113.5(11) . . ? N3 C9 C8 119.9(14) . . ? N4 C9 C8 126.5(14) . . ? N4 C10 N5 110.9(11) . . ? N4 C10 H10A 124.6 . . ? N5 C10 H10A 124.6 . . ? C12 C11 N4 106.4(12) . . ? C12 C11 H11A 126.8 . . ? N4 C11 H11A 126.8 . . ? C11 C12 N5 108.1(12) . . ? C11 C12 H12A 126.0 . . ? N5 C12 H12A 126.0 . . ? N5 C13 C14 113.0(11) . . ? N5 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N5 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C19 C14 C15 119.1(12) . . ? C19 C14 C13 118.0(12) . . ? C15 C14 C13 122.9(13) . . ? C16 C15 C14 120.8(13) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 119.6(13) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 119.9(12) . . ? C18 C17 C1 120.4(13) . 3_666 ? C16 C17 C1 119.6(13) . 3_666 ? C17 C18 C19 119.5(13) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C14 C19 C18 120.9(12) . . ? C14 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? O1 C20 O2 126.1(12) . . ? O1 C20 C21 114.6(12) . . ? O2 C20 C21 119.3(12) . . ? C26 C21 C22 120.1(13) . . ? C26 C21 C20 121.2(12) . . ? C22 C21 C20 118.7(12) . . ? C23 C22 C21 118.9(13) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 122.0(13) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C25 C24 C23 117.6(13) . . ? C25 C24 C27 120.2(12) . . ? C23 C24 C27 122.2(12) . . ? C26 C25 C24 121.3(13) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C21 120.1(13) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? O3 C27 O4 122.5(13) . . ? O3 C27 C24 118.1(13) . . ? O4 C27 C24 119.4(12) . . ? O5 C28 O6 127.9(13) . . ? O5 C28 C29 116.7(12) . . ? O6 C28 C29 115.3(12) . . ? C30 C29 C34 118.6(13) . . ? C30 C29 C28 122.9(13) . . ? C34 C29 C28 118.4(12) . . ? C29 C30 C31 122.0(14) . . ? C29 C30 H30A 119.0 . . ? C31 C30 H30A 119.0 . . ? C32 C31 C30 119.2(13) . . ? C32 C31 H31A 120.4 . . ? C30 C31 H31A 120.4 . . ? C31 C32 C33 120.4(12) . . ? C31 C32 C35 119.5(13) . . ? C33 C32 C35 120.0(13) . . ? C32 C33 C34 120.3(13) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C29 C34 C33 119.2(13) . . ? C29 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? O7 C35 O8 122.2(13) . . ? O7 C35 C32 120.4(13) . . ? O8 C35 C32 117.3(14) . . ? O10 C36 O9 118.8(12) . . ? O10 C36 C37 122.2(12) . . ? O9 C36 C37 119.0(12) . . ? O10 C36 Tm1 63.6(7) . . ? O9 C36 Tm1 55.6(6) . . ? C37 C36 Tm1 171.6(9) . . ? C39 C37 C38 123.8(12) 3_666 . ? C39 C37 C36 118.7(13) 3_666 . ? C38 C37 C36 117.5(12) . . ? C37 C38 C39 116.0(11) . . ? C37 C38 H38A 122.0 . . ? C39 C38 H38A 122.0 . . ? C37 C39 C38 120.1(12) 3_666 . ? C37 C39 H39A 120.0 3_666 . ? C38 C39 H39A 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Tm1 O1 C20 110.5(15) . . . . ? O1W Tm1 O1 C20 -152.2(13) . . . . ? O3W Tm1 O1 C20 9.8(14) . . . . ? O9 Tm1 O1 C20 -82.7(14) . . . . ? O4W Tm1 O1 C20 55.3(16) . . . . ? O2W Tm1 O1 C20 -170.7(15) . . . . ? O10 Tm1 O1 C20 -51.8(15) . . . . ? C36 Tm1 O1 C20 -70.0(15) . . . . ? O1 Tm1 O5 C28 38.3(11) . . . . ? O1W Tm1 O5 C28 -101.4(11) . . . . ? O3W Tm1 O5 C28 110.2(12) . . . . ? O9 Tm1 O5 C28 -1.5(18) . . . . ? O4W Tm1 O5 C28 -175.0(12) . . . . ? O2W Tm1 O5 C28 -31.6(11) . . . . ? O10 Tm1 O5 C28 -170.0(9) . . . . ? C36 Tm1 O5 C28 -138(3) . . . . ? O5 Tm1 O9 C36 -168.1(9) . . . . ? O1 Tm1 O9 C36 151.4(8) . . . . ? O1W Tm1 O9 C36 -66.0(8) . . . . ? O3W Tm1 O9 C36 78.6(8) . . . . ? O4W Tm1 O9 C36 4.0(9) . . . . ? O2W Tm1 O9 C36 -138.6(8) . . . . ? O10 Tm1 O9 C36 4.1(7) . . . . ? O5 Tm1 O10 C36 170.9(7) . . . . ? O1 Tm1 O10 C36 -43.3(8) . . . . ? O1W Tm1 O10 C36 94.6(8) . . . . ? O3W Tm1 O10 C36 -103.0(8) . . . . ? O9 Tm1 O10 C36 -4.1(7) . . . . ? O4W Tm1 O10 C36 175.8(8) . . . . ? O2W Tm1 O10 C36 43.1(8) . . . . ? C2 N1 C1 C17 -67.7(17) . . . 3_666 ? C3 N1 C1 C17 111.9(15) . . . 3_666 ? C4 N2 C2 N1 -1.7(14) . . . . ? C5 N2 C2 N1 -175.9(11) . . . . ? C3 N1 C2 N2 0.7(14) . . . . ? C1 N1 C2 N2 -179.6(11) . . . . ? C2 N1 C3 C4 0.6(16) . . . . ? C1 N1 C3 C4 -179.0(13) . . . . ? N1 C3 C4 N2 -1.7(17) . . . . ? C2 N2 C4 C3 2.1(16) . . . . ? C5 N2 C4 C3 175.7(13) . . . . ? C9 N3 C5 C6 0(2) . . . . ? C9 N3 C5 N2 178.8(10) . . . . ? C2 N2 C5 N3 4.8(17) . . . . ? C4 N2 C5 N3 -167.8(13) . . . . ? C2 N2 C5 C6 -176.5(12) . . . . ? C4 N2 C5 C6 11(2) . . . . ? N3 C5 C6 C7 -1(2) . . . . ? N2 C5 C6 C7 -179.0(11) . . . . ? C5 C6 C7 C8 2.0(19) . . . . ? C6 C7 C8 C9 -3(2) . . . . ? C5 N3 C9 N4 175.4(11) . . . . ? C5 N3 C9 C8 -1.5(18) . . . . ? C10 N4 C9 N3 -15.1(18) . . . . ? C11 N4 C9 N3 160.7(11) . . . . ? C10 N4 C9 C8 161.5(13) . . . . ? C11 N4 C9 C8 -23(2) . . . . ? C7 C8 C9 N3 3(2) . . . . ? C7 C8 C9 N4 -173.3(13) . . . . ? C9 N4 C10 N5 179.9(12) . . . . ? C11 N4 C10 N5 3.4(14) . . . . ? C13 N5 C10 N4 179.4(11) . . . . ? C12 N5 C10 N4 -1.2(15) . . . . ? C10 N4 C11 C12 -4.3(15) . . . . ? C9 N4 C11 C12 179.3(13) . . . . ? N4 C11 C12 N5 3.5(16) . . . . ? C10 N5 C12 C11 -1.5(16) . . . . ? C13 N5 C12 C11 177.9(12) . . . . ? C10 N5 C13 C14 106.8(14) . . . . ? C12 N5 C13 C14 -72.4(17) . . . . ? N5 C13 C14 C19 169.9(11) . . . . ? N5 C13 C14 C15 -9.2(17) . . . . ? C19 C14 C15 C16 1(2) . . . . ? C13 C14 C15 C16 -179.9(12) . . . . ? C14 C15 C16 C17 -4(2) . . . . ? C15 C16 C17 C18 5(2) . . . . ? C15 C16 C17 C1 -174.4(12) . . . 3_666 ? C16 C17 C18 C19 -2.9(19) . . . . ? C1 C17 C18 C19 176.3(11) 3_666 . . . ? C15 C14 C19 C18 1.0(19) . . . . ? C13 C14 C19 C18 -178.1(11) . . . . ? C17 C18 C19 C14 0(2) . . . . ? Tm1 O1 C20 O2 -1(2) . . . . ? Tm1 O1 C20 C21 177.1(9) . . . . ? O1 C20 C21 C26 -1.4(18) . . . . ? O2 C20 C21 C26 176.9(12) . . . . ? O1 C20 C21 C22 177.9(11) . . . . ? O2 C20 C21 C22 -3.8(18) . . . . ? C26 C21 C22 C23 2.4(18) . . . . ? C20 C21 C22 C23 -176.9(11) . . . . ? C21 C22 C23 C24 -3.0(18) . . . . ? C22 C23 C24 C25 2.3(18) . . . . ? C22 C23 C24 C27 179.9(12) . . . . ? C23 C24 C25 C26 -1.1(18) . . . . ? C27 C24 C25 C26 -178.7(11) . . . . ? C24 C25 C26 C21 0.6(19) . . . . ? C22 C21 C26 C25 -1.2(19) . . . . ? C20 C21 C26 C25 178.1(11) . . . . ? C25 C24 C27 O3 -15.7(18) . . . . ? C23 C24 C27 O3 166.8(12) . . . . ? C25 C24 C27 O4 165.7(11) . . . . ? C23 C24 C27 O4 -11.8(19) . . . . ? Tm1 O5 C28 O6 5(2) . . . . ? Tm1 O5 C28 C29 -178.2(8) . . . . ? O5 C28 C29 C30 165.4(12) . . . . ? O6 C28 C29 C30 -17.7(19) . . . . ? O5 C28 C29 C34 -10.3(18) . . . . ? O6 C28 C29 C34 166.6(12) . . . . ? C34 C29 C30 C31 -5(2) . . . . ? C28 C29 C30 C31 179.7(12) . . . . ? C29 C30 C31 C32 1(2) . . . . ? C30 C31 C32 C33 2(2) . . . . ? C30 C31 C32 C35 179.9(12) . . . . ? C31 C32 C33 C34 0(2) . . . . ? C35 C32 C33 C34 -178.4(11) . . . . ? C30 C29 C34 C33 6.1(19) . . . . ? C28 C29 C34 C33 -178.1(11) . . . . ? C32 C33 C34 C29 -3.7(19) . . . . ? C31 C32 C35 O7 171.7(13) . . . . ? C33 C32 C35 O7 -10(2) . . . . ? C31 C32 C35 O8 -11(2) . . . . ? C33 C32 C35 O8 167.1(13) . . . . ? Tm1 O10 C36 O9 7.0(12) . . . . ? Tm1 O10 C36 C37 -173.0(11) . . . . ? Tm1 O9 C36 O10 -7.6(13) . . . . ? Tm1 O9 C36 C37 172.4(9) . . . . ? O5 Tm1 C36 O10 -40(3) . . . . ? O1 Tm1 C36 O10 143.8(7) . . . . ? O1W Tm1 C36 O10 -77.5(7) . . . . ? O3W Tm1 C36 O10 72.7(7) . . . . ? O9 Tm1 C36 O10 172.6(13) . . . . ? O4W Tm1 C36 O10 -4.2(8) . . . . ? O2W Tm1 C36 O10 -144.7(7) . . . . ? O5 Tm1 C36 O9 147(3) . . . . ? O1 Tm1 C36 O9 -28.7(8) . . . . ? O1W Tm1 C36 O9 109.9(8) . . . . ? O3W Tm1 C36 O9 -99.9(8) . . . . ? O4W Tm1 C36 O9 -176.7(7) . . . . ? O2W Tm1 C36 O9 42.7(8) . . . . ? O10 Tm1 C36 O9 -172.6(13) . . . . ? O5 Tm1 C36 C37 95(7) . . . . ? O1 Tm1 C36 C37 -81(6) . . . . ? O1W Tm1 C36 C37 58(6) . . . . ? O3W Tm1 C36 C37 -152(6) . . . . ? O9 Tm1 C36 C37 -52(6) . . . . ? O4W Tm1 C36 C37 131(6) . . . . ? O2W Tm1 C36 C37 -9(6) . . . . ? O10 Tm1 C36 C37 135(7) . . . . ? O10 C36 C37 C39 -169.6(12) . . . 3_666 ? O9 C36 C37 C39 10.4(18) . . . 3_666 ? Tm1 C36 C37 C39 59(7) . . . 3_666 ? O10 C36 C37 C38 8.7(18) . . . . ? O9 C36 C37 C38 -171.3(11) . . . . ? Tm1 C36 C37 C38 -123(6) . . . . ? C39 C37 C38 C39 -3(2) 3_666 . . . ? C36 C37 C38 C39 178.4(10) . . . . ? C37 C38 C39 C37 3(2) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.532 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.201 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 385 196 ' ' 2 0.500 0.000 0.500 385 196 ' ' _platon_squeeze_details ; Number of moved primary input atoms: 87. Number of unusual anisotropic displacement parameters: 2. Total Potential Solvent Accessible Void Vol: 771.0 Ang**3. Electron Count / Cell = 392 - To be included in D(calc), F000 & Mol.Wght. ;