# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peng Cheng' _publ_contact_author_email PCHENG@NANKAI.EDU.CN _publ_section_title ; Self-Assembly of Novel 3d-4d-4f- Heterometal-organic Framework Based on Double-stranded Helical Motifs ; loop_ _publ_author_name 'Peng Cheng' 'Dai-Zheng Liao' 'Wei Shi' 'Shi-Ping Yan' 'Bin Zhao' ; Xiao-Qing Zhao ; # Attachment '1.cif' data_r71127d _database_code_depnum_ccdc_archive 'CCDC 693165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cd Co Dy N3 O29' _chemical_formula_sum 'C21 H36 Cd Co Dy N3 O29' _chemical_formula_weight 1128.36 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9449(18) _cell_length_b 24.424(5) _cell_length_c 18.089(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.71(3) _cell_angle_gamma 90.00 _cell_volume 3696.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5628 _cell_measurement_theta_min 2.4342 _cell_measurement_theta_max 27.0983 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 3.122 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8368 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27845 _diffrn_reflns_av_R_equivalents 0.1380 _diffrn_reflns_av_sigmaI/netI 0.1299 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6494 _reflns_number_gt 4820 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _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^)+(0.0369P)^2^+8.0652P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6494 _refine_ls_number_parameters 547 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.97694(6) 0.81231(2) 0.43894(3) 0.01483(16) Uani 1 1 d . . . Cd1 Cd 1.59171(12) 0.91230(4) 0.58530(6) 0.0185(3) Uani 0.75 1 d P . . Co2 Co 1.59171(12) 0.91230(4) 0.58530(6) 0.0185(3) Uani 0.25 1 d P . . Co1 Co 0.52704(15) 0.66395(5) 0.50685(8) 0.0194(3) Uani 0.75 1 d P . . Cd2 Cd 0.52704(15) 0.66395(5) 0.50685(8) 0.0194(3) Uani 0.25 1 d P . . C1 C 0.8562(13) 0.7268(4) 0.5485(7) 0.015(3) Uani 1 1 d . . . C2 C 1.0051(13) 0.7496(4) 0.6093(6) 0.014(2) Uani 1 1 d . . . C3 C 1.0651(13) 0.7306(4) 0.6855(7) 0.015(3) Uani 1 1 d . . . H3A H 1.0121 0.7030 0.7018 0.018 Uiso 1 1 d R . . C4 C 1.2075(14) 0.7528(4) 0.7377(7) 0.019(3) Uani 1 1 d . . . C5 C 1.2801(14) 0.7944(4) 0.7101(7) 0.017(3) Uani 1 1 d . . . H5 H 1.3736 0.8110 0.7430 0.020 Uiso 1 1 d R . . C6 C 1.2098(13) 0.8110(4) 0.6320(7) 0.015(3) Uani 1 1 d . . . C7 C 1.2841(13) 0.8528(4) 0.5934(8) 0.017(3) Uani 1 1 d . . . C8 C 0.7985(14) 0.9209(5) 0.4792(7) 0.020(3) Uani 1 1 d . . . C9 C 0.8697(13) 0.9456(4) 0.4222(7) 0.015(3) Uani 1 1 d . . . C10 C 0.8550(14) 1.0009(5) 0.4035(7) 0.021(3) Uani 1 1 d . . . H10 H 0.7959 1.0244 0.4230 0.026 Uiso 1 1 d R . . C11 C 0.9354(13) 1.0193(4) 0.3531(7) 0.018(3) Uani 1 1 d . . . C12 C 1.0180(13) 0.9828(5) 0.3224(7) 0.020(3) Uani 1 1 d . . . H12 H 1.0675 0.9937 0.2875 0.025 Uiso 1 1 d R . . C13 C 1.0210(13) 0.9284(4) 0.3464(7) 0.017(3) Uani 1 1 d . . . C14 C 1.1078(13) 0.8842(4) 0.3193(7) 0.012(2) Uani 1 1 d . . . C15 C 0.6764(15) 0.7850(5) 0.2709(8) 0.025(3) Uani 1 1 d . . . C16 C 0.7840(12) 0.7340(4) 0.2800(6) 0.011(2) Uani 1 1 d . . . C17 C 0.7402(13) 0.6912(4) 0.2253(7) 0.018(3) Uani 1 1 d . . . H17 H 0.6438 0.6921 0.1829 0.022 Uiso 1 1 d R . . C18 C 0.8441(14) 0.6471(5) 0.2363(7) 0.019(3) Uani 1 1 d . . . C19 C 0.9852(13) 0.6474(5) 0.3035(7) 0.018(3) Uani 1 1 d . . . H19 H 1.0552 0.6179 0.3138 0.022 Uiso 1 1 d R . . C20 C 1.0165(13) 0.6922(4) 0.3532(7) 0.016(3) Uani 1 1 d . . . C21 C 1.1633(15) 0.6968(4) 0.4238(8) 0.021(3) Uani 1 1 d . . . N1 N 1.0728(10) 0.7899(4) 0.5818(5) 0.014(2) Uani 1 1 d . . . N2 N 0.9489(10) 0.9096(4) 0.3950(6) 0.017(2) Uani 1 1 d . . . N3 N 0.9174(10) 0.7352(3) 0.3440(5) 0.012(2) Uani 1 1 d . . . O1 O 0.8134(9) 0.7492(3) 0.4806(5) 0.0181(18) Uani 1 1 d . . . O2 O 0.7821(9) 0.6891(3) 0.5676(5) 0.0223(19) Uani 1 1 d . . . O3 O 1.2783(10) 0.7352(3) 0.8117(5) 0.025(2) Uani 1 1 d . . . H3 H 1.2158 0.7159 0.8241 0.038 Uiso 1 1 d R . . O4 O 1.4131(9) 0.8750(3) 0.6348(5) 0.0208(19) Uani 1 1 d . . . O5 O 1.2094(9) 0.8619(3) 0.5210(4) 0.0163(18) Uani 1 1 d . . . O6 O 0.8233(9) 0.8701(3) 0.4909(5) 0.0160(18) Uani 1 1 d . . . O7 O 0.7250(9) 0.9504(3) 0.5112(5) 0.0199(19) Uani 1 1 d . . . O8 O 0.9298(10) 1.0738(3) 0.3367(5) 0.026(2) Uani 1 1 d . . . H8 H 1.0178 1.0842 0.3379 0.039 Uiso 1 1 d R . . O9 O 1.1721(10) 0.8955(3) 0.2699(5) 0.026(2) Uani 1 1 d . . . O10 O 1.1110(9) 0.8364(3) 0.3506(5) 0.0172(18) Uani 1 1 d . . . O11 O 0.7263(8) 0.8177(3) 0.3304(5) 0.0178(18) Uani 1 1 d . . . O12 O 0.5565(9) 0.7917(3) 0.2123(5) 0.0228(19) Uani 1 1 d . . . O13 O 0.8141(10) 0.6065(3) 0.1838(5) 0.0208(19) Uani 1 1 d . . . O14 O 1.2693(10) 0.6604(3) 0.4383(5) 0.024(2) Uani 1 1 d . . . O15 O 1.1781(9) 0.7405(3) 0.4661(5) 0.0168(18) Uani 1 1 d . . . O16 O 0.5358(10) 0.7047(3) 0.4033(5) 0.031(2) Uani 1 1 d . . . H16A H 0.4688 0.7293 0.3840 0.037 Uiso 1 1 d R . . H16B H 0.6208 0.7281 0.4164 0.037 Uiso 1 1 d R . . O17 O 0.5678(12) 0.5909(4) 0.4613(6) 0.055(3) Uani 1 1 d . . . H17A H 0.5409 0.5611 0.4776 0.066 Uiso 1 1 d R . . H17B H 0.6114 0.5901 0.4265 0.066 Uiso 1 1 d R . . O18 O 0.5164(11) 0.6223(4) 0.6075(6) 0.046(3) Uani 1 1 d . . . H18A H 0.4969 0.6399 0.6436 0.055 Uiso 1 1 d R . . H18B H 0.5319 0.5879 0.6118 0.055 Uiso 1 1 d R . . O19 O 0.4714(9) 0.7396(3) 0.5625(5) 0.0211(19) Uani 1 1 d . . . H19A H 0.5473 0.7598 0.5911 0.025 Uiso 1 1 d R . . H19B H 0.3751 0.7482 0.5550 0.025 Uiso 1 1 d R . . O20 O 1.5608(10) 0.8363(3) 0.5147(5) 0.029(2) Uani 1 1 d . . . H20A H 1.4858 0.8339 0.4701 0.035 Uiso 1 1 d R . . H20B H 1.6240 0.8095 0.5324 0.035 Uiso 1 1 d R . . O21 O 1.3730(10) 0.9425(3) 0.4817(5) 0.0190(19) Uani 1 1 d . . . H21A H 1.350(14) 0.973(5) 0.482(7) 0.023 Uiso 1 1 d . . . H21B H 1.310(14) 0.918(5) 0.483(7) 0.023 Uiso 1 1 d . . . O22 O 1.5895(10) 0.9907(3) 0.6428(5) 0.035(2) Uani 1 1 d . . . H22A H 1.5191 1.0145 0.6199 0.042 Uiso 1 1 d R . . H22B H 1.6587 0.9973 0.6881 0.042 Uiso 1 1 d R . . O23 O 0.5077(11) 0.9003(4) 0.3100(6) 0.048(3) Uani 1 1 d . . . H23A H 0.5894 0.8799 0.3199 0.057 Uiso 1 1 d R . . H23B H 0.4885 0.9133 0.3494 0.057 Uiso 1 1 d R . . O24 O 0.2502(14) 0.5554(4) 0.5718(7) 0.069(4) Uani 1 1 d . . . H24A H 0.2254 0.5473 0.5230 0.082 Uiso 1 1 d R . . H24B H 0.1804 0.5732 0.5842 0.082 Uiso 1 1 d R . . O25 O 0.9827(13) 0.9112(5) 0.1108(7) 0.073(4) Uani 1 1 d . . . H25A H 0.9066 0.8881 0.0987 0.088 Uiso 1 1 d R . . H25B H 1.0658 0.9035 0.1505 0.088 Uiso 1 1 d R . . O26 O 0.3387(14) 0.5489(5) 0.3263(7) 0.076(4) Uani 1 1 d . . . H26A H 0.4146 0.5449 0.3084 0.092 Uiso 1 1 d R . . H26B H 0.2699 0.5736 0.3040 0.092 Uiso 1 1 d R . . O27 O 0.5413(17) 0.0138(5) 0.7814(8) 0.093(5) Uani 1 1 d . . . H27A H 0.5906 0.0059 0.8299 0.112 Uiso 1 1 d R . . H27B H 0.5189 0.0475 0.7707 0.112 Uiso 1 1 d R . . O28 O 0.7577(17) 0.5057(5) 0.5586(9) 0.097(5) Uani 1 1 d . . . H28A H 0.6699 0.4968 0.5640 0.117 Uiso 1 1 d R . . H28B H 0.8247 0.4799 0.5632 0.117 Uiso 1 1 d R . . O29 O 0.779(7) 0.980(2) 0.824(4) 0.095(16) Uani 0.25 1 d PU . . O30 O 0.366(7) 0.026(2) 0.795(4) 0.103(17) Uani 0.25 1 d PU . . O31 O 0.498(7) 0.584(2) 0.292(3) 0.097(16) Uani 0.25 1 d PU . . O32 O 0.939(12) 0.472(4) 0.595(6) 0.07(2) Uani 0.13 1 d PU . . O33 O 0.78(2) 0.593(7) 0.651(10) 0.17(3) Uani 0.13 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0178(3) 0.0113(3) 0.0170(3) -0.0005(2) 0.0083(2) 0.0001(2) Cd1 0.0200(6) 0.0154(5) 0.0216(6) 0.0026(4) 0.0092(5) -0.0003(4) Co2 0.0200(6) 0.0154(5) 0.0216(6) 0.0026(4) 0.0092(5) -0.0003(4) Co1 0.0136(7) 0.0256(7) 0.0191(8) -0.0033(6) 0.0056(6) -0.0033(6) Cd2 0.0136(7) 0.0256(7) 0.0191(8) -0.0033(6) 0.0056(6) -0.0033(6) C1 0.023(7) 0.012(6) 0.017(7) -0.003(5) 0.015(6) -0.005(5) C2 0.022(7) 0.013(6) 0.004(6) -0.003(5) 0.000(5) -0.003(5) C3 0.023(7) 0.012(6) 0.017(7) 0.002(5) 0.016(6) -0.002(5) C4 0.030(7) 0.008(6) 0.028(8) -0.007(5) 0.023(6) -0.005(5) C5 0.023(7) 0.022(6) 0.009(6) -0.006(5) 0.011(5) -0.007(5) C6 0.017(6) 0.011(6) 0.023(7) 0.001(5) 0.013(5) -0.005(5) C7 0.016(6) 0.009(6) 0.035(8) -0.003(5) 0.021(6) -0.002(5) C8 0.026(7) 0.015(6) 0.017(7) 0.006(5) 0.007(6) 0.004(5) C9 0.013(6) 0.014(6) 0.014(6) 0.005(5) 0.001(5) 0.010(5) C10 0.024(7) 0.016(6) 0.031(8) -0.002(5) 0.019(6) 0.001(5) C11 0.017(6) 0.010(6) 0.023(7) 0.000(5) 0.001(5) 0.005(5) C12 0.008(6) 0.026(7) 0.030(8) 0.004(6) 0.010(5) 0.004(5) C13 0.015(6) 0.016(6) 0.016(7) -0.006(5) 0.002(5) -0.003(5) C14 0.014(6) 0.009(6) 0.012(6) 0.003(5) 0.004(5) -0.001(4) C15 0.032(8) 0.013(6) 0.041(9) -0.001(6) 0.027(7) 0.008(6) C16 0.012(6) 0.008(5) 0.011(6) 0.002(4) 0.002(5) 0.005(4) C17 0.019(6) 0.009(6) 0.026(7) 0.000(5) 0.007(5) 0.006(5) C18 0.029(7) 0.017(6) 0.017(7) -0.006(5) 0.017(6) 0.001(5) C19 0.016(6) 0.015(6) 0.019(7) -0.001(5) 0.002(5) 0.002(5) C20 0.022(6) 0.016(6) 0.008(6) -0.002(5) 0.004(5) -0.003(5) C21 0.035(8) 0.006(6) 0.036(8) -0.002(5) 0.029(7) -0.007(5) N1 0.007(5) 0.013(5) 0.020(6) -0.001(4) 0.003(4) -0.001(4) N2 0.012(5) 0.013(5) 0.026(6) -0.004(4) 0.008(5) -0.001(4) N3 0.012(5) 0.011(5) 0.013(5) -0.006(4) 0.004(4) 0.004(4) O1 0.016(4) 0.020(4) 0.017(5) 0.007(4) 0.005(4) 0.002(3) O2 0.024(5) 0.023(5) 0.016(5) 0.000(4) 0.003(4) -0.003(4) O3 0.027(5) 0.032(5) 0.018(5) 0.003(4) 0.011(4) -0.006(4) O4 0.020(5) 0.019(4) 0.023(5) 0.002(4) 0.007(4) -0.004(4) O5 0.026(5) 0.019(4) 0.002(4) 0.001(3) 0.003(4) 0.002(3) O6 0.019(4) 0.012(4) 0.021(5) -0.002(3) 0.014(4) 0.001(3) O7 0.023(5) 0.016(4) 0.028(5) -0.004(4) 0.018(4) 0.004(3) O8 0.028(5) 0.010(4) 0.046(6) 0.007(4) 0.021(5) 0.005(3) O9 0.041(6) 0.022(5) 0.026(5) 0.000(4) 0.026(5) 0.003(4) O10 0.025(5) 0.010(4) 0.019(5) 0.000(3) 0.010(4) -0.001(3) O11 0.015(4) 0.015(4) 0.021(5) -0.002(4) 0.003(4) 0.002(3) O12 0.019(5) 0.023(5) 0.021(5) 0.000(4) 0.000(4) 0.008(4) O13 0.032(5) 0.010(4) 0.023(5) -0.009(4) 0.013(4) -0.004(3) O14 0.032(5) 0.006(4) 0.032(5) -0.003(4) 0.009(4) 0.000(4) O15 0.019(4) 0.009(4) 0.025(5) -0.002(3) 0.011(4) 0.001(3) O16 0.022(5) 0.038(6) 0.029(6) 0.002(4) 0.004(4) -0.005(4) O17 0.052(7) 0.066(8) 0.047(7) -0.011(6) 0.018(6) -0.005(6) O18 0.056(7) 0.025(5) 0.058(8) -0.001(5) 0.021(6) 0.007(5) O19 0.017(4) 0.018(4) 0.021(5) 0.002(4) -0.002(4) -0.002(3) O20 0.025(5) 0.021(5) 0.041(6) 0.004(4) 0.013(4) 0.008(4) O21 0.023(5) 0.017(5) 0.018(5) 0.001(4) 0.008(4) -0.006(4) O22 0.031(6) 0.031(5) 0.032(6) -0.008(4) -0.003(4) 0.007(4) O23 0.031(6) 0.035(6) 0.079(9) -0.003(5) 0.022(6) 0.017(5) O24 0.086(10) 0.048(7) 0.080(10) -0.012(6) 0.040(8) -0.007(6) O25 0.056(8) 0.070(9) 0.072(9) 0.018(7) -0.003(7) 0.000(6) O26 0.061(9) 0.092(10) 0.063(9) -0.011(7) 0.006(7) 0.020(7) O27 0.135(14) 0.064(9) 0.080(11) 0.018(8) 0.038(10) -0.010(8) O28 0.108(12) 0.079(10) 0.110(13) -0.019(9) 0.044(10) -0.007(9) O29 0.095(16) 0.095(16) 0.095(16) 0.0000(10) 0.034(6) 0.0000(10) O30 0.103(17) 0.103(17) 0.103(17) 0.0000(10) 0.036(6) 0.0000(10) O31 0.097(16) 0.097(16) 0.097(16) 0.0000(10) 0.034(6) 0.0000(10) O32 0.07(2) 0.07(2) 0.07(2) 0.0000(10) 0.026(8) 0.0000(10) O33 0.17(3) 0.17(3) 0.17(3) 0.0000(10) 0.062(11) 0.0000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O6 2.383(7) . ? Dy1 O10 2.385(7) . ? Dy1 O11 2.405(7) . ? Dy1 O5 2.410(8) . ? Dy1 O1 2.421(7) . ? Dy1 O15 2.435(7) . ? Dy1 N3 2.477(8) . ? Dy1 N1 2.480(9) . ? Dy1 N2 2.489(9) . ? Cd1 O22 2.182(8) . ? Cd1 O13 2.199(8) 4_676 ? Cd1 O20 2.213(8) . ? Cd1 O4 2.279(8) . ? Cd1 O7 2.283(8) 1_655 ? Cd1 O21 2.300(9) . ? Co1 O17 2.052(10) . ? Co1 O18 2.116(10) . ? Co1 O16 2.147(9) . ? Co1 O14 2.199(8) 1_455 ? Co1 O2 2.240(8) . ? Co1 O19 2.242(8) . ? C1 O2 1.253(12) . ? C1 O1 1.273(13) . ? C1 C2 1.503(15) . ? C2 N1 1.340(13) . ? C2 C3 1.371(15) . ? C3 C4 1.398(16) . ? C3 H3A 0.9299 . ? C4 O3 1.334(14) . ? C4 C5 1.391(14) . ? C5 C6 1.389(15) . ? C5 H5 0.9300 . ? C6 N1 1.344(13) . ? C6 C7 1.516(14) . ? C7 O4 1.255(13) . ? C7 O5 1.262(14) . ? C8 O7 1.247(13) . ? C8 O6 1.265(12) . ? C8 C9 1.516(15) . ? C9 N2 1.329(13) . ? C9 C10 1.388(15) . ? C10 C11 1.417(16) . ? C10 H10 0.9298 . ? C11 O8 1.362(12) . ? C11 C12 1.393(15) . ? C12 C13 1.394(15) . ? C12 H12 0.9300 . ? C13 N2 1.343(14) . ? C13 C14 1.509(15) . ? C14 O9 1.253(12) . ? C14 O10 1.293(12) . ? C15 O12 1.223(14) . ? C15 O11 1.288(14) . ? C15 C16 1.545(14) . ? C16 N3 1.337(13) . ? C16 C17 1.399(15) . ? C17 C18 1.389(15) . ? C17 H17 0.9301 . ? C18 O13 1.334(13) . ? C18 C19 1.409(16) . ? C19 C20 1.380(15) . ? C19 H19 0.9300 . ? C20 N3 1.345(13) . ? C20 C21 1.477(16) . ? C21 O14 1.257(13) . ? C21 O15 1.292(12) . ? O3 H3 0.8201 . ? O7 Co2 2.283(8) 1_455 ? O7 Cd1 2.283(8) 1_455 ? O8 H8 0.8200 . ? O13 Co2 2.199(8) 4_475 ? O13 Cd1 2.199(8) 4_475 ? O14 Cd2 2.199(8) 1_655 ? O14 Co1 2.199(8) 1_655 ? O16 H16A 0.8344 . ? O16 H16B 0.9132 . ? O17 H17A 0.8501 . ? O17 H17B 0.8499 . ? O18 H18A 0.8500 . ? O18 H18B 0.8502 . ? O19 H19A 0.8502 . ? O19 H19B 0.8500 . ? O20 H20A 0.8499 . ? O20 H20B 0.8500 . ? O21 H21A 0.78(12) . ? O21 H21B 0.84(12) . ? O22 H22A 0.8499 . ? O22 H22B 0.8500 . ? O23 H23A 0.8498 . ? O23 H23B 0.8509 . ? O24 H24A 0.8537 . ? O24 H24B 0.8534 . ? O25 H25A 0.8522 . ? O25 H25B 0.8519 . ? O26 H26A 0.8552 . ? O26 H26B 0.8535 . ? O27 H27A 0.8526 . ? O27 H27B 0.8534 . ? O28 H28A 0.8532 . ? O28 H28B 0.8534 . ? 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 O6 Dy1 O10 127.9(2) . . ? O6 Dy1 O11 77.8(3) . . ? O10 Dy1 O11 89.1(3) . . ? O6 Dy1 O5 87.2(2) . . ? O10 Dy1 O5 76.1(3) . . ? O11 Dy1 O5 145.8(2) . . ? O6 Dy1 O1 76.0(2) . . ? O10 Dy1 O1 150.1(3) . . ? O11 Dy1 O1 78.3(3) . . ? O5 Dy1 O1 127.8(3) . . ? O6 Dy1 O15 146.6(3) . . ? O10 Dy1 O15 78.6(2) . . ? O11 Dy1 O15 127.8(3) . . ? O5 Dy1 O15 79.8(2) . . ? O1 Dy1 O15 87.9(2) . . ? O6 Dy1 N3 135.4(3) . . ? O10 Dy1 N3 76.1(3) . . ? O11 Dy1 N3 64.2(3) . . ? O5 Dy1 N3 137.4(3) . . ? O1 Dy1 N3 74.1(3) . . ? O15 Dy1 N3 63.5(3) . . ? O6 Dy1 N1 75.8(3) . . ? O10 Dy1 N1 133.0(3) . . ? O11 Dy1 N1 137.9(3) . . ? O5 Dy1 N1 64.2(3) . . ? O1 Dy1 N1 63.9(3) . . ? O15 Dy1 N1 70.9(3) . . ? N3 Dy1 N1 117.7(3) . . ? O6 Dy1 N2 63.5(3) . . ? O10 Dy1 N2 64.4(3) . . ? O11 Dy1 N2 74.2(3) . . ? O5 Dy1 N2 71.6(3) . . ? O1 Dy1 N2 134.7(3) . . ? O15 Dy1 N2 137.4(3) . . ? N3 Dy1 N2 122.1(3) . . ? N1 Dy1 N2 120.1(3) . . ? O22 Cd1 O13 87.4(3) . 4_676 ? O22 Cd1 O20 171.9(3) . . ? O13 Cd1 O20 100.7(3) 4_676 . ? O22 Cd1 O4 92.2(3) . . ? O13 Cd1 O4 99.1(3) 4_676 . ? O20 Cd1 O4 86.0(3) . . ? O22 Cd1 O7 90.9(3) . 1_655 ? O13 Cd1 O7 92.9(3) 4_676 1_655 ? O20 Cd1 O7 89.3(3) . 1_655 ? O4 Cd1 O7 167.8(3) . 1_655 ? O22 Cd1 O21 87.6(3) . . ? O13 Cd1 O21 172.8(3) 4_676 . ? O20 Cd1 O21 84.4(3) . . ? O4 Cd1 O21 86.3(3) . . ? O7 Cd1 O21 82.0(3) 1_655 . ? O17 Co1 O18 89.7(4) . . ? O17 Co1 O16 89.2(4) . . ? O18 Co1 O16 178.8(3) . . ? O17 Co1 O14 92.3(3) . 1_455 ? O18 Co1 O14 96.3(3) . 1_455 ? O16 Co1 O14 83.1(3) . 1_455 ? O17 Co1 O2 98.1(3) . . ? O18 Co1 O2 93.3(3) . . ? O16 Co1 O2 87.4(3) . . ? O14 Co1 O2 165.9(3) 1_455 . ? O17 Co1 O19 174.9(4) . . ? O18 Co1 O19 85.7(3) . . ? O16 Co1 O19 95.3(3) . . ? O14 Co1 O19 86.0(3) 1_455 . ? O2 Co1 O19 84.4(3) . . ? O2 C1 O1 125.0(11) . . ? O2 C1 C2 119.2(10) . . ? O1 C1 C2 115.8(9) . . ? N1 C2 C3 123.7(10) . . ? N1 C2 C1 113.5(9) . . ? C3 C2 C1 122.8(10) . . ? C2 C3 C4 119.1(10) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.8 . . ? O3 C4 C5 118.6(11) . . ? O3 C4 C3 123.3(10) . . ? C5 C4 C3 118.1(11) . . ? C6 C5 C4 118.6(11) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 121.1 . . ? N1 C6 C5 123.4(10) . . ? N1 C6 C7 113.1(10) . . ? C5 C6 C7 123.4(10) . . ? O4 C7 O5 125.5(10) . . ? O4 C7 C6 118.5(11) . . ? O5 C7 C6 116.0(10) . . ? O7 C8 O6 125.4(11) . . ? O7 C8 C9 120.2(10) . . ? O6 C8 C9 114.4(10) . . ? N2 C9 C10 124.9(11) . . ? N2 C9 C8 113.3(9) . . ? C10 C9 C8 121.8(10) . . ? C9 C10 C11 116.0(10) . . ? C9 C10 H10 121.7 . . ? C11 C10 H10 122.3 . . ? O8 C11 C12 121.5(11) . . ? O8 C11 C10 117.5(10) . . ? C12 C11 C10 121.0(10) . . ? C11 C12 C13 116.1(11) . . ? C11 C12 H12 122.3 . . ? C13 C12 H12 121.6 . . ? N2 C13 C12 124.7(11) . . ? N2 C13 C14 112.9(9) . . ? C12 C13 C14 122.4(10) . . ? O9 C14 O10 124.5(10) . . ? O9 C14 C13 119.5(9) . . ? O10 C14 C13 115.9(9) . . ? O12 C15 O11 125.5(10) . . ? O12 C15 C16 121.5(11) . . ? O11 C15 C16 113.0(11) . . ? N3 C16 C17 124.7(9) . . ? N3 C16 C15 114.0(9) . . ? C17 C16 C15 121.2(10) . . ? C18 C17 C16 118.2(11) . . ? C18 C17 H17 121.1 . . ? C16 C17 H17 120.7 . . ? O13 C18 C17 121.2(11) . . ? O13 C18 C19 120.7(10) . . ? C17 C18 C19 118.0(10) . . ? C20 C19 C18 118.6(10) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 120.2 . . ? N3 C20 C19 124.4(11) . . ? N3 C20 C21 113.2(9) . . ? C19 C20 C21 122.4(10) . . ? O14 C21 O15 123.2(12) . . ? O14 C21 C20 120.1(10) . . ? O15 C21 C20 116.6(10) . . ? C2 N1 C6 117.1(10) . . ? C2 N1 Dy1 121.0(7) . . ? C6 N1 Dy1 121.0(7) . . ? C9 N2 C13 117.3(10) . . ? C9 N2 Dy1 121.4(7) . . ? C13 N2 Dy1 121.2(7) . . ? C16 N3 C20 116.0(9) . . ? C16 N3 Dy1 121.6(6) . . ? C20 N3 Dy1 122.5(7) . . ? C1 O1 Dy1 124.4(7) . . ? C1 O2 Co1 127.8(8) . . ? C4 O3 H3 109.3 . . ? C7 O4 Cd1 124.3(7) . . ? C7 O5 Dy1 125.2(7) . . ? C8 O6 Dy1 127.3(7) . . ? C8 O7 Co2 120.5(7) . 1_455 ? C8 O7 Cd1 120.5(7) . 1_455 ? Co2 O7 Cd1 0.00(6) 1_455 1_455 ? C11 O8 H8 109.7 . . ? C14 O10 Dy1 125.3(7) . . ? C15 O11 Dy1 126.6(7) . . ? C18 O13 Co2 128.9(7) . 4_475 ? C18 O13 Cd1 128.9(7) . 4_475 ? Co2 O13 Cd1 0.00(6) 4_475 4_475 ? C21 O14 Cd2 130.8(8) . 1_655 ? C21 O14 Co1 130.8(8) . 1_655 ? Cd2 O14 Co1 0.00(10) 1_655 1_655 ? C21 O15 Dy1 124.2(8) . . ? Co1 O16 H16A 117.2 . . ? Co1 O16 H16B 110.4 . . ? H16A O16 H16B 93.7 . . ? Co1 O17 H17A 119.4 . . ? Co1 O17 H17B 120.6 . . ? H17A O17 H17B 120.0 . . ? Co1 O18 H18A 120.1 . . ? Co1 O18 H18B 119.9 . . ? H18A O18 H18B 120.0 . . ? Co1 O19 H19A 119.6 . . ? Co1 O19 H19B 120.4 . . ? H19A O19 H19B 120.0 . . ? Cd1 O20 H20A 120.2 . . ? Cd1 O20 H20B 119.8 . . ? H20A O20 H20B 120.0 . . ? Cd1 O21 H21A 117(9) . . ? Cd1 O21 H21B 98(8) . . ? H21A O21 H21B 121(10) . . ? Cd1 O22 H22A 120.0 . . ? Cd1 O22 H22B 120.0 . . ? H22A O22 H22B 120.0 . . ? H23A O23 H23B 117.1 . . ? H24A O24 H24B 116.2 . . ? H25A O25 H25B 116.6 . . ? H26A O26 H26B 116.0 . . ? O30 O27 H27A 93.6 . . ? O30 O27 H27B 73.4 . . ? H27A O27 H27B 116.4 . . ? O32 O28 H28A 128.0 . . ? O32 O28 H28B 23.1 . . ? H28A O28 H28B 116.3 . . ? O28 O32 H28B 19.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.323 _refine_diff_density_min -1.651 _refine_diff_density_rms 0.236 # Attachment '2.cif' data_r70930c _database_code_depnum_ccdc_archive 'CCDC 693166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cd Co Eu N3 O29' _chemical_formula_sum 'C21 H36 Cd Co Eu N3 O29' _chemical_formula_weight 1117.82 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9716(18) _cell_length_b 24.550(5) _cell_length_c 18.082(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.22(3) _cell_angle_gamma 90.00 _cell_volume 3737.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8656 _cell_measurement_theta_min 1.6589 _cell_measurement_theta_max 27.9604 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 2.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8974 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28185 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6583 _reflns_number_gt 6014 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _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^)+(0.0403P)^2^+23.9989P] 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 6583 _refine_ls_number_parameters 669 _refine_ls_number_restraints 270 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.161 _refine_ls_shift/su_mean 0.002 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 Eu1 Eu 0.03394(3) 0.186589(11) 0.566748(16) 0.01106(10) Uani 1 1 d . . . Cd1 Cd -0.58156(5) 0.087385(19) 0.41681(3) 0.01454(13) Uani 0.75 1 d P . . Co2 Co -0.58156(5) 0.087385(19) 0.41681(3) 0.01454(13) Uani 0.25 1 d P . . Co1 Co 0.48596(7) 0.33407(3) 0.50072(4) 0.02142(17) Uani 0.75 1 d P . . Cd2 Cd 0.48596(7) 0.33407(3) 0.50072(4) 0.02142(17) Uani 0.25 1 d P . . C1 C 0.1591(7) 0.2716(2) 0.4553(3) 0.0160(12) Uani 1 1 d . . . C2 C 0.0085(6) 0.2507(2) 0.3948(3) 0.0135(12) Uani 1 1 d . . . C3 C -0.0524(6) 0.2709(2) 0.3195(3) 0.0149(12) Uani 1 1 d . . . H3 H 0.0006 0.2982 0.3028 0.018 Uiso 1 1 calc R . . C4 C -0.1943(6) 0.2499(2) 0.2686(3) 0.0140(12) Uani 1 1 d . . . C5 C -0.2688(6) 0.2079(2) 0.2957(3) 0.0137(12) Uani 1 1 d . . . H5 H -0.3633 0.1926 0.2627 0.016 Uiso 1 1 calc R . . C6 C -0.1985(6) 0.1898(2) 0.3723(3) 0.0121(11) Uani 1 1 d . . . C7 C -0.2729(6) 0.1479(2) 0.4085(3) 0.0115(11) Uani 1 1 d . . . C8 C 0.2101(6) 0.0783(2) 0.5237(3) 0.0140(12) Uani 1 1 d . . . C9 C 0.1358(6) 0.0521(2) 0.5781(3) 0.0130(12) Uani 1 1 d . . . C10 C 0.1432(6) -0.0032(2) 0.5952(3) 0.0135(12) Uani 1 1 d . . . H10 H 0.2044 -0.0265 0.5769 0.016 Uiso 1 1 calc R . . C11 C 0.0575(6) -0.0230(2) 0.6403(3) 0.0156(12) Uani 1 1 d . . . C12 C -0.0239(7) 0.0139(2) 0.6720(4) 0.0167(12) Uani 1 1 d . . . H12 H -0.0789 0.0020 0.7042 0.020 Uiso 1 1 calc R . . C13 C -0.0195(6) 0.0683(2) 0.6538(3) 0.0145(12) Uani 1 1 d . . . C14 C -0.1082(7) 0.1110(2) 0.6826(4) 0.0176(13) Uani 1 1 d . . . C15 C 0.3314(6) 0.2152(2) 0.7330(3) 0.0139(12) Uani 1 1 d . . . C16 C 0.2286(6) 0.2651(2) 0.7257(3) 0.0137(12) Uani 1 1 d . . . C17 C 0.2707(7) 0.3077(2) 0.7791(4) 0.0174(13) Uani 1 1 d . . . H17 H 0.3676 0.3071 0.8204 0.021 Uiso 1 1 calc R . . C18 C 0.1663(6) 0.3522(2) 0.7708(3) 0.0161(12) Uani 1 1 d . . . C19 C 0.0248(7) 0.3506(2) 0.7054(4) 0.0186(13) Uani 1 1 d . . . H19 H -0.0483 0.3789 0.6965 0.022 Uiso 1 1 calc R . . C20 C -0.0053(6) 0.3067(2) 0.6542(4) 0.0151(12) Uani 1 1 d . . . C21 C -0.1545(6) 0.3019(2) 0.5834(3) 0.0155(12) Uani 1 1 d . . . N1 N -0.0619(5) 0.21100(19) 0.4221(3) 0.0127(10) Uani 1 1 d . . . N2 N 0.0565(5) 0.08781(18) 0.6076(3) 0.0121(10) Uani 1 1 d . . . N3 N 0.0931(5) 0.26392(19) 0.6632(3) 0.0138(10) Uani 1 1 d . . . O1 O 0.1969(4) 0.24997(16) 0.5233(2) 0.0171(9) Uani 1 1 d . . . O2 O 0.2379(5) 0.30769(17) 0.4364(2) 0.0208(9) Uani 1 1 d . . . O3 O -0.2651(5) 0.26778(17) 0.1943(2) 0.0188(9) Uani 1 1 d . . . H3A H -0.2125 0.2926 0.1854 0.028 Uiso 1 1 calc R . . O4 O -0.4012(4) 0.12589(16) 0.3668(2) 0.0165(9) Uani 1 1 d . . . O5 O -0.2028(4) 0.13845(16) 0.4811(2) 0.0152(8) Uani 1 1 d . . . O6 O 0.1920(4) 0.12877(15) 0.5150(2) 0.0159(9) Uani 1 1 d . . . O7 O 0.2838(5) 0.04877(16) 0.4906(2) 0.0180(9) Uani 1 1 d . . . O8 O 0.0565(5) -0.07692(16) 0.6530(3) 0.0213(10) Uani 1 1 d . . . H8 H -0.0211 -0.0848 0.6650 0.032 Uiso 1 1 calc R . . O9 O -0.1769(6) 0.09855(19) 0.7285(3) 0.0378(13) Uani 1 1 d . . . O10 O -0.1023(4) 0.15941(15) 0.6566(2) 0.0147(8) Uani 1 1 d . . . O11 O 0.2843(5) 0.18127(16) 0.6764(2) 0.0182(9) Uani 1 1 d . . . O12 O 0.4552(5) 0.20975(17) 0.7920(2) 0.0195(9) Uani 1 1 d . . . O13 O 0.1978(5) 0.39301(17) 0.8205(2) 0.0207(9) Uani 1 1 d . . . O14 O -0.2569(5) 0.33869(17) 0.5703(3) 0.0225(10) Uani 1 1 d . . . O15 O -0.1652(4) 0.25978(16) 0.5414(2) 0.0164(9) Uani 1 1 d . . . O16 O 0.4783(5) 0.28957(19) 0.6031(3) 0.0285(11) Uani 1 1 d . . . H16A H 0.3853 0.2763 0.5909 0.034 Uiso 1 1 d R . . H16B H 0.5554 0.2681 0.6253 0.034 Uiso 1 1 d R . . O17 O 0.4384(10) 0.4031(4) 0.5494(5) 0.055(2) Uani 0.75 1 d PU . . O17' O 0.379(3) 0.3977(11) 0.5601(16) 0.055(2) Uani 0.25 1 d PU . . O18 O 0.5094(10) 0.3760(4) 0.4013(5) 0.052(2) Uani 0.75 1 d PU . . O18' O 0.496(3) 0.3913(11) 0.4247(16) 0.052(2) Uani 0.25 1 d PU . . O19 O 0.5420(5) 0.26049(17) 0.4431(2) 0.0205(9) Uani 1 1 d . . . H19B H 0.6399 0.2542 0.4668 0.025 Uiso 1 1 d R . . H19A H 0.5136 0.2717 0.3959 0.025 Uiso 1 1 d R . . O20 O -0.5482(5) 0.16361(18) 0.4883(3) 0.0274(10) Uani 1 1 d . . . H20A H -0.5259 0.1939 0.4718 0.033 Uiso 1 1 d R . . H20B H -0.6329 0.1625 0.4994 0.033 Uiso 1 1 d R . . O21 O -0.3686(5) 0.05812(17) 0.5195(2) 0.0209(9) Uani 1 1 d . . . H21B H -0.3077 0.0837 0.5157 0.025 Uiso 1 1 d R . . H21A H -0.3417 0.0259 0.5116 0.025 Uiso 1 1 d R . . O22 O -0.5758(6) 0.0098(2) 0.3572(3) 0.0410(13) Uani 1 1 d . . . H22A H -0.5669 -0.0201 0.3819 0.049 Uiso 1 1 d R . . H22B H -0.5990 0.0084 0.3077 0.049 Uiso 1 1 d R . . O23 O 0.5100(9) 0.9058(3) 0.3046(5) 0.078(2) Uani 1 1 d U . . H23A H 0.4952 0.8943 0.3461 0.094 Uiso 1 1 d R . . H23B H 0.4338 0.9012 0.2611 0.094 Uiso 1 1 d R . . O24 O 0.4855(17) 0.5814(6) 0.2885(9) 0.057(3) Uani 0.50 1 d PU . . O25 O 0.7686(16) -0.0193(5) 0.8187(7) 0.060(3) Uani 0.50 1 d PU . . O26 O 0.386(2) 0.0272(7) 0.7967(9) 0.076(3) Uani 0.50 1 d PU . . O27 O 0.7793(19) 0.4380(7) 0.4392(10) 0.086(5) Uani 0.50 1 d PU . . O28 O 0.036(2) 0.4096(7) 0.3929(10) 0.022(4) Uani 0.25 1 d PU . . O29 O 0.703(2) 0.3610(8) 0.3381(11) 0.109(6) Uani 0.50 1 d PU . . O30 O 0.6179(19) 0.0084(6) 0.7875(9) 0.080(3) Uani 0.50 1 d PU . . O31 O 0.104(4) 0.5207(12) 0.3998(18) 0.059(5) Uani 0.25 1 d PU . . O32 O 0.314(3) 0.5585(10) 0.3176(14) 0.050(4) Uani 0.25 1 d PU . . O33 O 0.561(3) 0.5043(10) 0.5363(14) 0.051(6) Uani 0.25 1 d PU . . O34 O 0.150(3) 0.4054(9) 0.3344(14) 0.048(6) Uani 0.25 1 d PU . . O35 O 0.353(4) 0.0768(13) 0.7694(18) 0.075(4) Uani 0.25 1 d PU . . O36 O -0.041(3) 0.4743(11) 0.3667(15) 0.062(5) Uani 0.25 1 d PU . . O37 O 0.411(3) 0.5764(12) 0.2850(17) 0.055(3) Uani 0.25 1 d PU . . O38 O 0.236(5) 0.5145(17) 0.334(2) 0.040(6) Uani 0.13 1 d PU . . O39 O 0.490(8) 0.031(3) 0.812(4) 0.076(3) Uani 0.13 1 d PU . . O40 O 0.196(5) 0.3884(18) 0.582(3) 0.044(8) Uani 0.13 1 d PU . . O42 O 0.179(7) 0.551(2) 0.449(3) 0.058(5) Uani 0.13 1 d PU . . O41 O 0.119(8) 0.537(3) 0.419(4) 0.058(5) Uani 0.13 1 d PU . . O43 O 0.074(5) 0.4222(19) 0.508(3) 0.046(7) Uani 0.13 1 d PU . . O44 O -0.014(6) 0.395(2) 0.483(3) 0.050(8) Uani 0.13 1 d PU . . O45 O 0.557(7) 0.581(2) 0.290(3) 0.056(4) Uani 0.13 1 d PU . . 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 Eu1 0.01102(15) 0.01065(16) 0.01100(16) -0.00075(11) 0.00315(11) -0.00013(10) Cd1 0.0130(2) 0.0147(2) 0.0162(3) 0.00391(19) 0.00544(19) 0.00009(18) Co2 0.0130(2) 0.0147(2) 0.0162(3) 0.00391(19) 0.00544(19) 0.00009(18) Co1 0.0094(3) 0.0357(4) 0.0156(4) -0.0060(3) -0.0002(3) -0.0064(3) Cd2 0.0094(3) 0.0357(4) 0.0156(4) -0.0060(3) -0.0002(3) -0.0064(3) C1 0.015(3) 0.016(3) 0.017(3) 0.000(2) 0.006(2) -0.002(2) C2 0.015(3) 0.011(3) 0.017(3) -0.003(2) 0.009(2) 0.000(2) C3 0.016(3) 0.017(3) 0.013(3) 0.004(2) 0.006(2) 0.000(2) C4 0.013(3) 0.015(3) 0.013(3) -0.003(2) 0.004(2) 0.003(2) C5 0.015(3) 0.015(3) 0.011(3) 0.001(2) 0.005(2) 0.000(2) C6 0.013(3) 0.009(3) 0.014(3) -0.002(2) 0.004(2) -0.002(2) C7 0.013(3) 0.010(3) 0.013(3) 0.000(2) 0.006(2) 0.002(2) C8 0.010(3) 0.016(3) 0.016(3) -0.004(2) 0.004(2) -0.002(2) C9 0.009(2) 0.013(3) 0.015(3) 0.000(2) 0.002(2) 0.000(2) C10 0.012(3) 0.010(3) 0.018(3) -0.003(2) 0.006(2) 0.003(2) C11 0.012(3) 0.011(3) 0.020(3) 0.002(2) 0.001(2) 0.000(2) C12 0.017(3) 0.011(3) 0.022(3) 0.005(2) 0.007(2) 0.001(2) C13 0.017(3) 0.016(3) 0.012(3) 0.002(2) 0.007(2) 0.000(2) C14 0.019(3) 0.016(3) 0.021(3) 0.002(3) 0.010(3) 0.003(2) C15 0.013(3) 0.018(3) 0.011(3) 0.003(2) 0.005(2) 0.000(2) C16 0.010(3) 0.015(3) 0.017(3) 0.000(2) 0.005(2) -0.001(2) C17 0.015(3) 0.019(3) 0.016(3) 0.000(2) 0.003(2) 0.001(2) C18 0.014(3) 0.016(3) 0.021(3) -0.003(3) 0.008(2) -0.001(2) C19 0.016(3) 0.015(3) 0.025(3) 0.000(3) 0.007(3) 0.001(2) C20 0.011(3) 0.016(3) 0.020(3) 0.002(2) 0.007(2) -0.001(2) C21 0.015(3) 0.014(3) 0.018(3) 0.003(2) 0.006(2) -0.002(2) N1 0.010(2) 0.014(2) 0.014(2) -0.003(2) 0.0038(19) 0.0015(19) N2 0.011(2) 0.012(2) 0.014(2) -0.0010(19) 0.0042(19) -0.0005(18) N3 0.014(2) 0.012(2) 0.014(2) -0.002(2) 0.004(2) -0.0013(19) O1 0.0153(19) 0.018(2) 0.016(2) 0.0040(17) 0.0030(16) -0.0037(16) O2 0.019(2) 0.021(2) 0.022(2) 0.0025(18) 0.0057(18) -0.0062(17) O3 0.019(2) 0.020(2) 0.015(2) 0.0069(17) 0.0014(17) -0.0061(17) O4 0.0118(19) 0.020(2) 0.017(2) -0.0014(17) 0.0036(16) -0.0041(16) O5 0.0135(19) 0.017(2) 0.015(2) -0.0018(17) 0.0045(16) -0.0015(16) O6 0.018(2) 0.012(2) 0.021(2) 0.0018(17) 0.0100(17) -0.0003(16) O7 0.019(2) 0.017(2) 0.024(2) -0.0024(18) 0.0140(18) 0.0009(17) O8 0.021(2) 0.012(2) 0.036(3) 0.0077(19) 0.015(2) 0.0020(16) O9 0.055(3) 0.025(3) 0.052(3) 0.014(2) 0.043(3) 0.013(2) O10 0.020(2) 0.012(2) 0.014(2) -0.0026(16) 0.0088(17) 0.0005(16) O11 0.017(2) 0.015(2) 0.018(2) -0.0037(17) 0.0002(17) 0.0053(16) O12 0.017(2) 0.019(2) 0.018(2) -0.0031(18) -0.0011(17) 0.0047(17) O13 0.021(2) 0.017(2) 0.022(2) -0.0108(18) 0.0058(18) -0.0008(17) O14 0.019(2) 0.017(2) 0.026(2) -0.0006(19) 0.0008(18) 0.0033(17) O15 0.0146(19) 0.015(2) 0.016(2) -0.0031(17) 0.0012(16) 0.0018(16) O16 0.013(2) 0.038(3) 0.026(3) 0.006(2) -0.0044(18) -0.0038(19) O17 0.055(2) 0.055(2) 0.054(2) -0.0009(8) 0.0187(11) -0.0001(8) O17' 0.055(2) 0.055(2) 0.054(2) -0.0005(8) 0.0188(11) -0.0001(8) O18 0.053(2) 0.052(2) 0.052(2) 0.0002(8) 0.0175(11) 0.0002(8) O18' 0.052(2) 0.052(2) 0.052(2) 0.0001(8) 0.0179(11) 0.0003(8) O19 0.016(2) 0.025(2) 0.017(2) 0.0026(18) 0.0016(17) -0.0025(17) O20 0.028(2) 0.020(2) 0.044(3) 0.002(2) 0.025(2) -0.0018(19) O21 0.021(2) 0.019(2) 0.024(2) 0.0029(18) 0.0084(18) -0.0013(17) O22 0.040(3) 0.035(3) 0.055(4) -0.010(3) 0.025(3) -0.006(2) O23 0.074(4) 0.065(4) 0.092(4) -0.010(3) 0.026(3) 0.004(3) O24 0.056(5) 0.060(4) 0.054(4) 0.001(3) 0.020(3) 0.000(3) O25 0.067(5) 0.064(5) 0.053(4) -0.005(4) 0.027(4) 0.003(4) O26 0.079(4) 0.074(4) 0.073(4) 0.001(3) 0.024(3) 0.000(3) O27 0.087(6) 0.080(6) 0.090(6) 0.003(4) 0.030(4) -0.004(4) O28 0.025(5) 0.020(5) 0.021(5) -0.005(4) 0.007(4) 0.004(4) O29 0.111(7) 0.111(7) 0.110(7) -0.004(5) 0.043(5) 0.001(5) O30 0.086(4) 0.076(4) 0.075(4) -0.001(3) 0.023(3) -0.001(3) O31 0.060(5) 0.058(5) 0.058(5) 0.003(3) 0.018(3) -0.001(3) O32 0.050(5) 0.051(5) 0.050(5) -0.003(4) 0.017(3) 0.001(4) O33 0.054(7) 0.045(7) 0.052(7) 0.006(5) 0.017(5) -0.003(5) O34 0.047(7) 0.044(7) 0.048(7) 0.005(5) 0.011(5) -0.001(5) O35 0.077(4) 0.074(4) 0.073(4) 0.000(3) 0.024(3) -0.001(3) O36 0.062(6) 0.062(6) 0.059(6) 0.003(4) 0.016(4) -0.004(4) O37 0.055(4) 0.057(4) 0.053(4) -0.001(3) 0.018(3) 0.001(3) O38 0.042(7) 0.041(7) 0.040(7) -0.001(5) 0.016(4) 0.000(5) O39 0.079(4) 0.074(4) 0.074(4) 0.000(3) 0.025(3) -0.001(3) O40 0.045(8) 0.044(8) 0.045(8) 0.001(5) 0.018(5) 0.001(5) O42 0.059(6) 0.057(6) 0.057(6) 0.002(4) 0.019(4) -0.001(4) O41 0.059(6) 0.057(6) 0.057(6) 0.002(4) 0.018(4) 0.000(4) O43 0.046(8) 0.048(8) 0.046(8) 0.000(4) 0.017(5) 0.000(4) O44 0.051(9) 0.049(9) 0.049(9) 0.000(5) 0.017(5) -0.002(5) O45 0.055(5) 0.059(4) 0.055(4) 0.001(3) 0.019(3) 0.000(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 Eu1 O6 2.413(4) . ? Eu1 O11 2.432(4) . ? Eu1 O10 2.440(4) . ? Eu1 O1 2.444(4) . ? Eu1 O5 2.456(4) . ? Eu1 O15 2.463(4) . ? Eu1 N3 2.507(5) . ? Eu1 N2 2.522(5) . ? Eu1 N1 2.526(5) . ? Cd1 O13 2.191(4) 4_465 ? Cd1 O22 2.198(5) . ? Cd1 O20 2.235(5) . ? Cd1 O21 2.272(4) . ? Cd1 O7 2.292(4) 1_455 ? Cd1 O4 2.312(4) . ? Co1 O18' 1.99(3) . ? Co1 O17 2.022(9) . ? Co1 O18 2.144(9) . ? Co1 O16 2.170(5) . ? Co1 O14 2.216(4) 1_655 ? Co1 O2 2.222(4) . ? Co1 O19 2.228(4) . ? Co1 O17' 2.29(3) . ? C1 O2 1.253(7) . ? C1 O1 1.272(7) . ? C1 C2 1.504(8) . ? C2 N1 1.345(7) . ? C2 C3 1.373(8) . ? C3 C4 1.386(8) . ? C3 H3 0.9300 . ? C4 O3 1.345(7) . ? C4 C5 1.406(8) . ? C5 C6 1.383(8) . ? C5 H5 0.9300 . ? C6 N1 1.350(7) . ? C6 C7 1.496(8) . ? C7 O4 1.259(7) . ? C7 O5 1.265(7) . ? C8 O6 1.252(7) . ? C8 O7 1.263(7) . ? C8 C9 1.509(8) . ? C9 N2 1.350(7) . ? C9 C10 1.390(8) . ? C10 C11 1.387(8) . ? C10 H10 0.9300 . ? C11 O8 1.345(7) . ? C11 C12 1.404(8) . ? C12 C13 1.380(8) . ? C12 H12 0.9300 . ? C13 N2 1.337(7) . ? C13 C14 1.512(8) . ? C14 O9 1.231(7) . ? C14 O10 1.286(7) . ? C15 O12 1.253(7) . ? C15 O11 1.274(7) . ? C15 C16 1.510(8) . ? C16 N3 1.344(7) . ? C16 C17 1.386(8) . ? C17 C18 1.412(8) . ? C17 H17 0.9300 . ? C18 O13 1.310(7) . ? C18 C19 1.404(8) . ? C19 C20 1.386(8) . ? C19 H19 0.9300 . ? C20 N3 1.345(7) . ? C20 C21 1.502(8) . ? C21 O14 1.251(7) . ? C21 O15 1.267(7) . ? O3 H3A 0.8200 . ? O7 Co2 2.292(4) 1_655 ? O7 Cd1 2.292(4) 1_655 ? O8 H8 0.8200 . ? O13 Co2 2.191(4) 4_666 ? O13 Cd1 2.191(4) 4_666 ? O14 Cd2 2.216(4) 1_455 ? O14 Co1 2.216(4) 1_455 ? O16 H16A 0.8503 . ? O16 H16B 0.8511 . ? O17 O17' 0.64(3) . ? O18 O18' 0.61(3) . ? O19 H19B 0.8476 . ? O19 H19A 0.8468 . ? O20 H20A 0.8504 . ? O20 H20B 0.8511 . ? O21 H21B 0.8507 . ? O21 H21A 0.8529 . ? O22 H22A 0.8484 . ? O22 H22B 0.8481 . ? O23 H23A 0.8547 . ? O23 H23B 0.8522 . ? 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 O6 Eu1 O11 77.52(13) . . ? O6 Eu1 O10 126.48(13) . . ? O11 Eu1 O10 88.64(14) . . ? O6 Eu1 O1 75.67(14) . . ? O11 Eu1 O1 79.03(13) . . ? O10 Eu1 O1 151.83(13) . . ? O6 Eu1 O5 88.19(13) . . ? O11 Eu1 O5 147.34(13) . . ? O10 Eu1 O5 76.42(13) . . ? O1 Eu1 O5 125.93(13) . . ? O6 Eu1 O15 147.46(13) . . ? O11 Eu1 O15 126.66(13) . . ? O10 Eu1 O15 79.93(13) . . ? O1 Eu1 O15 87.24(13) . . ? O5 Eu1 O15 79.63(13) . . ? O6 Eu1 N3 134.74(14) . . ? O11 Eu1 N3 63.88(14) . . ? O10 Eu1 N3 77.20(14) . . ? O1 Eu1 N3 74.63(15) . . ? O5 Eu1 N3 137.05(14) . . ? O15 Eu1 N3 62.78(14) . . ? O6 Eu1 N2 63.22(14) . . ? O11 Eu1 N2 75.63(14) . . ? O10 Eu1 N2 63.27(14) . . ? O1 Eu1 N2 135.22(14) . . ? O5 Eu1 N2 71.72(14) . . ? O15 Eu1 N2 137.35(14) . . ? N3 Eu1 N2 123.25(15) . . ? O6 Eu1 N1 76.89(14) . . ? O11 Eu1 N1 138.13(14) . . ? O10 Eu1 N1 133.22(14) . . ? O1 Eu1 N1 62.83(14) . . ? O5 Eu1 N1 63.31(14) . . ? O15 Eu1 N1 70.66(14) . . ? N3 Eu1 N1 117.04(15) . . ? N2 Eu1 N1 119.67(15) . . ? O13 Cd1 O22 88.21(19) 4_465 . ? O13 Cd1 O20 100.34(16) 4_465 . ? O22 Cd1 O20 171.13(18) . . ? O13 Cd1 O21 173.06(15) 4_465 . ? O22 Cd1 O21 88.31(18) . . ? O20 Cd1 O21 83.43(16) . . ? O13 Cd1 O7 92.32(15) 4_465 1_455 ? O22 Cd1 O7 91.91(17) . 1_455 ? O20 Cd1 O7 90.11(15) . 1_455 ? O21 Cd1 O7 81.80(15) . 1_455 ? O13 Cd1 O4 99.28(14) 4_465 . ? O22 Cd1 O4 91.38(17) . . ? O20 Cd1 O4 84.95(15) . . ? O21 Cd1 O4 86.81(14) . . ? O7 Cd1 O4 168.04(14) 1_455 . ? O18' Co1 O17 77.1(9) . . ? O18' Co1 O18 16.4(8) . . ? O17 Co1 O18 93.4(3) . . ? O18' Co1 O16 165.3(8) . . ? O17 Co1 O16 88.7(3) . . ? O18 Co1 O16 176.1(3) . . ? O18' Co1 O14 94.0(8) . 1_655 ? O17 Co1 O14 92.6(3) . 1_655 ? O18 Co1 O14 93.8(3) . 1_655 ? O16 Co1 O14 82.83(16) . 1_655 ? O18' Co1 O2 96.9(8) . . ? O17 Co1 O2 98.5(3) . . ? O18 Co1 O2 94.1(3) . . ? O16 Co1 O2 88.78(16) . . ? O14 Co1 O2 165.92(16) 1_655 . ? O18' Co1 O19 100.2(8) . . ? O17 Co1 O19 177.2(3) . . ? O18 Co1 O19 83.9(3) . . ? O16 Co1 O19 93.99(17) . . ? O14 Co1 O19 87.02(15) 1_655 . ? O2 Co1 O19 82.30(15) . . ? O18' Co1 O17' 88.2(11) . . ? O17 Co1 O17' 15.6(7) . . ? O18 Co1 O17' 104.2(7) . . ? O16 Co1 O17' 78.5(7) . . ? O14 Co1 O17' 102.8(7) 1_655 . ? O2 Co1 O17' 86.5(7) . . ? O19 Co1 O17' 166.7(7) . . ? O2 C1 O1 124.9(5) . . ? O2 C1 C2 119.4(5) . . ? O1 C1 C2 115.7(5) . . ? N1 C2 C3 123.3(5) . . ? N1 C2 C1 113.4(5) . . ? C3 C2 C1 123.2(5) . . ? C2 C3 C4 118.9(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? O3 C4 C3 123.4(5) . . ? O3 C4 C5 118.0(5) . . ? C3 C4 C5 118.7(5) . . ? C6 C5 C4 118.5(5) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 122.7(5) . . ? N1 C6 C7 114.4(5) . . ? C5 C6 C7 122.8(5) . . ? O4 C7 O5 124.6(5) . . ? O4 C7 C6 119.1(5) . . ? O5 C7 C6 116.3(5) . . ? O6 C8 O7 125.1(5) . . ? O6 C8 C9 115.9(5) . . ? O7 C8 C9 119.0(5) . . ? N2 C9 C10 122.5(5) . . ? N2 C9 C8 113.1(5) . . ? C10 C9 C8 124.4(5) . . ? C11 C10 C9 118.6(5) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? O8 C11 C10 118.8(5) . . ? O8 C11 C12 122.0(5) . . ? C10 C11 C12 119.2(5) . . ? C13 C12 C11 117.7(5) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? N2 C13 C12 123.9(5) . . ? N2 C13 C14 114.2(5) . . ? C12 C13 C14 121.8(5) . . ? O9 C14 O10 124.7(5) . . ? O9 C14 C13 120.4(5) . . ? O10 C14 C13 114.9(5) . . ? O12 C15 O11 124.3(5) . . ? O12 C15 C16 119.8(5) . . ? O11 C15 C16 115.9(5) . . ? N3 C16 C17 123.5(5) . . ? N3 C16 C15 113.9(5) . . ? C17 C16 C15 122.7(5) . . ? C16 C17 C18 119.9(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? O13 C18 C19 121.1(5) . . ? O13 C18 C17 122.7(5) . . ? C19 C18 C17 116.2(5) . . ? C20 C19 C18 119.7(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? N3 C20 C19 123.9(5) . . ? N3 C20 C21 113.4(5) . . ? C19 C20 C21 122.7(5) . . ? O14 C21 O15 125.2(5) . . ? O14 C21 C20 119.0(5) . . ? O15 C21 C20 115.8(5) . . ? C2 N1 C6 117.9(5) . . ? C2 N1 Eu1 121.1(4) . . ? C6 N1 Eu1 120.4(4) . . ? C13 N2 C9 117.9(5) . . ? C13 N2 Eu1 121.4(4) . . ? C9 N2 Eu1 120.6(4) . . ? C16 N3 C20 116.8(5) . . ? C16 N3 Eu1 120.9(4) . . ? C20 N3 Eu1 122.3(4) . . ? C1 O1 Eu1 125.9(3) . . ? C1 O2 Co1 128.4(4) . . ? C4 O3 H3A 109.5 . . ? C7 O4 Cd1 124.0(4) . . ? C7 O5 Eu1 125.3(3) . . ? C8 O6 Eu1 126.9(4) . . ? C8 O7 Co2 120.4(4) . 1_655 ? C8 O7 Cd1 120.4(4) . 1_655 ? Co2 O7 Cd1 0.00(3) 1_655 1_655 ? C11 O8 H8 109.5 . . ? C14 O10 Eu1 126.1(3) . . ? C15 O11 Eu1 125.2(3) . . ? C18 O13 Co2 129.4(4) . 4_666 ? C18 O13 Cd1 129.4(4) . 4_666 ? Co2 O13 Cd1 0.00(2) 4_666 4_666 ? C21 O14 Cd2 128.5(4) . 1_455 ? C21 O14 Co1 128.5(4) . 1_455 ? Cd2 O14 Co1 0.00(4) 1_455 1_455 ? C21 O15 Eu1 125.7(3) . . ? Co1 O16 H16A 106.8 . . ? Co1 O16 H16B 117.0 . . ? H16A O16 H16B 116.7 . . ? O17' O17 Co1 106(3) . . ? O17 O17' Co1 58(3) . . ? O18' O18 Co1 67(3) . . ? O18 O18' Co1 96(3) . . ? Co1 O19 H19B 105.8 . . ? Co1 O19 H19A 99.8 . . ? H19B O19 H19A 117.9 . . ? Cd1 O20 H20A 122.0 . . ? Cd1 O20 H20B 99.1 . . ? H20A O20 H20B 116.6 . . ? Cd1 O21 H21B 94.8 . . ? Cd1 O21 H21A 111.3 . . ? H21B O21 H21A 116.5 . . ? Cd1 O22 H22A 120.4 . . ? Cd1 O22 H22B 121.0 . . ? H22A O22 H22B 117.7 . . ? H23A O23 H23B 116.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.460 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.149 # Attachment '3.cif' data_r71022b _database_code_depnum_ccdc_archive 'CCDC 693167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cd Co N3 O29 Sm' _chemical_formula_sum 'C21 H36 Cd Co N3 O29 Sm' _chemical_formula_weight 1116.21 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9565(18) _cell_length_b 24.590(5) _cell_length_c 18.107(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.01(3) _cell_angle_gamma 90.00 _cell_volume 3747.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8567 _cell_measurement_theta_min 2.0435 _cell_measurement_theta_max 27.9283 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.0800 _exptl_crystal_size_mid 0.0600 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9325 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28110 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6556 _reflns_number_gt 6174 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _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^)+(0.0000P)^2^+3.2596P] 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 6556 _refine_ls_number_parameters 633 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.96339(5) 0.813757(18) 0.43020(3) 0.01242(13) Uani 1 1 d . . . Cd1 Cd 1.57925(8) 0.91245(3) 0.58238(4) 0.01615(18) Uani 0.75 1 d P . . Co2 Co 1.57925(8) 0.91245(3) 0.58238(4) 0.01615(18) Uani 0.25 1 d P . . Co1 Co 0.51036(12) 0.66726(5) 0.49477(7) 0.0271(3) Uani 0.75 1 d P . . Cd2 Cd 0.51036(12) 0.66726(5) 0.49477(7) 0.0271(3) Uani 0.25 1 d P . . C1 C 0.8355(10) 0.7290(3) 0.5416(5) 0.0150(19) Uani 1 1 d . . . C2 C 0.9873(10) 0.7498(3) 0.6014(6) 0.017(2) Uani 1 1 d . . . C3 C 1.0483(10) 0.7291(4) 0.6769(5) 0.0167(19) Uani 1 1 d . . . H3 H 0.9946 0.7017 0.6930 0.020 Uiso 1 1 calc R . . C4 C 1.1896(10) 0.7494(3) 0.7280(5) 0.0170(19) Uani 1 1 d . . . C5 C 1.2647(10) 0.7909(4) 0.7015(5) 0.0133(18) Uani 1 1 d . . . H5 H 1.3594 0.8060 0.7343 0.016 Uiso 1 1 calc R . . C6 C 1.1935(10) 0.8090(4) 0.6243(5) 0.0147(18) Uani 1 1 d . . . C7 C 1.2700(10) 0.8519(3) 0.5890(5) 0.0130(18) Uani 1 1 d . . . C8 C 0.7868(10) 0.9221(4) 0.4740(5) 0.0147(19) Uani 1 1 d . . . C9 C 0.8624(10) 0.9484(4) 0.4209(5) 0.0139(18) Uani 1 1 d . . . C10 C 0.8587(10) 1.0035(3) 0.4067(5) 0.0156(19) Uani 1 1 d . . . H10 H 0.7994 1.0265 0.4266 0.019 Uiso 1 1 calc R . . C11 C 0.9463(10) 1.0243(4) 0.3615(6) 0.019(2) Uani 1 1 d . . . C12 C 1.0264(10) 0.9874(4) 0.3298(6) 0.020(2) Uani 1 1 d . . . H12 H 1.0829 0.9994 0.2983 0.024 Uiso 1 1 calc R . . C13 C 1.0202(11) 0.9328(4) 0.3459(5) 0.0169(19) Uani 1 1 d . . . C14 C 1.1078(11) 0.8901(4) 0.3161(6) 0.022(2) Uani 1 1 d . . . C15 C 0.6673(10) 0.7850(4) 0.2645(5) 0.0159(19) Uani 1 1 d . . . C16 C 0.7685(10) 0.7350(4) 0.2707(5) 0.0159(19) Uani 1 1 d . . . C17 C 0.7268(10) 0.6926(4) 0.2185(5) 0.0177(19) Uani 1 1 d . . . H17 H 0.6302 0.6933 0.1772 0.021 Uiso 1 1 calc R . . C18 C 0.8303(10) 0.6481(4) 0.2273(5) 0.0169(19) Uani 1 1 d . . . C19 C 0.9701(11) 0.6496(4) 0.2914(6) 0.020(2) Uani 1 1 d . . . H19 H 1.0421 0.6210 0.3001 0.023 Uiso 1 1 calc R . . C20 C 1.0033(11) 0.6933(4) 0.3428(6) 0.019(2) Uani 1 1 d . . . C21 C 1.1522(10) 0.6983(4) 0.4122(6) 0.018(2) Uani 1 1 d . . . N1 N 1.0598(8) 0.7891(3) 0.5751(4) 0.0143(15) Uani 1 1 d . . . N2 N 0.9431(8) 0.9133(3) 0.3918(4) 0.0118(15) Uani 1 1 d . . . N3 N 0.9038(8) 0.7362(3) 0.3333(4) 0.0156(16) Uani 1 1 d . . . O1 O 0.7995(7) 0.7505(2) 0.4741(4) 0.0186(14) Uani 1 1 d . . . O2 O 0.7576(7) 0.6927(3) 0.5604(4) 0.0248(15) Uani 1 1 d . . . O3 O 1.2601(7) 0.7313(3) 0.8012(4) 0.0222(15) Uani 1 1 d . . . H3A H 1.2022 0.7091 0.8120 0.033 Uiso 1 1 calc R . . O4 O 1.3976(7) 0.8738(2) 0.6322(4) 0.0178(14) Uani 1 1 d . . . O5 O 1.2018(7) 0.8618(2) 0.5170(3) 0.0144(13) Uani 1 1 d . . . O6 O 0.8024(7) 0.8709(2) 0.4819(4) 0.0172(14) Uani 1 1 d . . . O7 O 0.7148(7) 0.9511(2) 0.5085(4) 0.0178(14) Uani 1 1 d . . . O8 O 0.9489(8) 1.0780(3) 0.3517(4) 0.0231(15) Uani 1 1 d . . . H8 H 1.0214 1.0859 0.3357 0.035 Uiso 1 1 calc R . . O9 O 1.1805(11) 0.9043(3) 0.2728(5) 0.046(2) Uani 1 1 d . . . O10 O 1.0983(7) 0.8422(2) 0.3394(4) 0.0174(14) Uani 1 1 d . . . O11 O 0.7154(7) 0.8195(2) 0.3194(4) 0.0210(15) Uani 1 1 d . . . O12 O 0.5435(8) 0.7903(3) 0.2053(4) 0.0233(15) Uani 1 1 d . . . O13 O 0.7980(7) 0.6071(2) 0.1781(4) 0.0211(15) Uani 1 1 d . . . O14 O 1.2550(7) 0.6615(3) 0.4256(4) 0.0234(15) Uani 1 1 d . . . O15 O 1.1640(7) 0.7404(3) 0.4557(4) 0.0190(14) Uani 1 1 d . . . O16 O 0.5186(8) 0.7126(3) 0.3951(4) 0.0345(18) Uani 1 1 d . . . H16A H 0.4396 0.7332 0.3732 0.041 Uiso 1 1 d R . . H16B H 0.6104 0.7267 0.4064 0.041 Uiso 1 1 d R . . O17 O 0.5641(19) 0.5989(7) 0.4463(10) 0.068(4) Uani 0.75 1 d PU . . O17' O 0.607(6) 0.608(2) 0.431(3) 0.068(4) Uani 0.25 1 d PU . . O18 O 0.486(2) 0.6214(7) 0.5898(9) 0.066(4) Uani 0.75 1 d PU . . O18' O 0.489(6) 0.609(2) 0.564(3) 0.066(4) Uani 0.25 1 d PU . . O19 O 0.4535(7) 0.7390(3) 0.5537(4) 0.0219(15) Uani 1 1 d . . . H19A H 0.3556 0.7452 0.5290 0.026 Uiso 1 1 d R . . H19B H 0.4804 0.7329 0.6028 0.026 Uiso 1 1 d R . . O20 O 1.5477(8) 0.8368(3) 0.5118(4) 0.0286(17) Uani 1 1 d . . . H20A H 1.6329 0.8368 0.5010 0.034 Uiso 1 1 d R . . H20B H 1.5094 0.8062 0.5174 0.034 Uiso 1 1 d R . . O21 O 1.3676(7) 0.9423(3) 0.4796(4) 0.0230(15) Uani 1 1 d . . . H21A H 1.3025 0.9164 0.4762 0.028 Uiso 1 1 d R . . H21B H 1.3365 0.9742 0.4853 0.028 Uiso 1 1 d R . . O22 O 1.5673(9) 0.9916(3) 0.6377(5) 0.041(2) Uani 1 1 d . . . H22A H 1.5745 1.0240 0.6229 0.050 Uiso 1 1 d R . . H22B H 1.6182 0.9838 0.6854 0.050 Uiso 1 1 d R . . O23 O 0.5091(19) 0.9056(7) 0.3036(10) 0.136(6) Uani 1 1 d U . . H23A H 0.5009 0.8885 0.3430 0.163 Uiso 1 1 d R . . H23B H 0.4795 0.8888 0.2599 0.163 Uiso 1 1 d R . . O24 O 0.445(2) 0.5809(6) 0.2828(9) 0.127(5) Uani 1 1 d U . . H24A H 0.5377 0.5714 0.2840 0.152 Uiso 1 1 d R . . H24B H 0.3665 0.5633 0.2524 0.152 Uiso 1 1 d R . . O25 O 0.613(3) 1.0071(10) 0.7852(15) 0.086(4) Uani 0.50 1 d PU . . O26 O 0.302(3) 0.6350(9) 0.6644(13) 0.071(6) Uani 0.50 1 d PU . . O27 O 0.222(4) 0.5175(14) 0.3341(19) 0.126(5) Uani 0.50 1 d PU . . O28 O 0.767(3) 0.9820(10) 0.8181(15) 0.087(4) Uani 0.50 1 d PU . . O29 O 0.599(3) 0.5284(12) 0.6989(17) 0.102(4) Uani 0.50 1 d PU . . O30 O 0.658(3) 0.5786(12) 0.7257(17) 0.102(4) Uani 0.50 1 d PU . . O31 O 0.981(7) 0.594(2) 0.601(3) 0.102(4) Uani 0.25 1 d PU . . O32 O 0.223(4) 0.5634(14) 0.560(2) 0.045(8) Uani 0.25 1 d PU . . O33 O 0.941(3) 1.0056(10) 0.8659(15) 0.087(4) Uani 0.50 1 d PU . . O34 O 0.650(5) 0.0168(17) 0.009(2) 0.063(7) Uani 0.25 1 d PU . . O35 O 0.869(7) 0.564(2) 0.474(3) 0.101(4) Uani 0.25 1 d PU . . O36 O 0.560(5) -0.0030(17) 0.030(2) 0.063(7) Uani 0.25 1 d PU . . O37 O 0.855(7) 0.593(2) 0.651(3) 0.102(4) Uani 0.25 1 d PU . . O38 O 1.114(6) 0.9689(19) 0.914(3) 0.080(12) Uani 0.25 1 d PU . . O39 O 0.310(8) 0.557(3) 0.319(4) 0.126(5) Uani 0.25 1 d PU . . O40 O 1.026(7) 0.604(2) 0.522(3) 0.102(4) Uani 0.25 1 d PU . . O41 O 0.776(7) 0.596(2) 0.686(3) 0.102(4) Uani 0.25 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0119(2) 0.0112(2) 0.0142(2) -0.00090(18) 0.00453(17) -0.00015(17) Cd1 0.0137(4) 0.0164(4) 0.0185(4) 0.0041(3) 0.0057(3) 0.0004(3) Co2 0.0137(4) 0.0164(4) 0.0185(4) 0.0041(3) 0.0057(3) 0.0004(3) Co1 0.0117(5) 0.0413(7) 0.0261(6) -0.0098(5) 0.0035(5) -0.0054(5) Cd2 0.0117(5) 0.0413(7) 0.0261(6) -0.0098(5) 0.0035(5) -0.0054(5) C1 0.013(4) 0.012(4) 0.024(5) 0.002(4) 0.010(4) -0.002(3) C2 0.017(5) 0.010(4) 0.026(5) -0.004(4) 0.009(4) 0.003(3) C3 0.020(5) 0.018(5) 0.019(5) 0.007(4) 0.014(4) -0.002(4) C4 0.018(5) 0.011(4) 0.020(5) 0.006(4) 0.004(4) 0.003(3) C5 0.014(4) 0.018(4) 0.008(4) 0.001(3) 0.004(3) 0.001(3) C6 0.017(4) 0.014(4) 0.013(4) -0.002(4) 0.004(4) 0.002(4) C7 0.014(4) 0.010(4) 0.014(5) -0.001(3) 0.004(4) 0.001(3) C8 0.008(4) 0.019(5) 0.017(5) 0.001(4) 0.004(4) -0.001(3) C9 0.011(4) 0.018(5) 0.014(4) -0.005(4) 0.006(4) -0.002(3) C10 0.017(4) 0.012(4) 0.018(5) 0.001(4) 0.008(4) 0.002(3) C11 0.012(4) 0.013(4) 0.032(6) 0.010(4) 0.007(4) 0.002(3) C12 0.015(4) 0.019(5) 0.024(5) 0.008(4) 0.005(4) 0.003(4) C13 0.019(5) 0.019(5) 0.016(5) -0.001(4) 0.011(4) -0.007(4) C14 0.021(5) 0.024(5) 0.024(5) -0.001(4) 0.012(4) 0.005(4) C15 0.015(4) 0.020(5) 0.013(5) 0.006(4) 0.005(4) 0.001(4) C16 0.015(4) 0.016(4) 0.018(5) 0.000(4) 0.006(4) 0.002(4) C17 0.014(4) 0.022(5) 0.016(5) -0.007(4) 0.002(4) -0.002(4) C18 0.017(5) 0.021(5) 0.015(5) -0.002(4) 0.007(4) -0.002(4) C19 0.019(5) 0.014(4) 0.026(5) -0.001(4) 0.008(4) 0.004(4) C20 0.017(5) 0.021(5) 0.021(5) 0.002(4) 0.009(4) 0.002(4) C21 0.017(5) 0.016(5) 0.023(5) 0.003(4) 0.009(4) 0.001(4) N1 0.014(4) 0.010(3) 0.018(4) 0.001(3) 0.005(3) 0.004(3) N2 0.014(4) 0.012(4) 0.010(4) -0.004(3) 0.006(3) -0.003(3) N3 0.015(4) 0.012(4) 0.022(4) -0.002(3) 0.009(3) 0.001(3) O1 0.021(3) 0.017(3) 0.019(4) 0.003(3) 0.009(3) -0.006(3) O2 0.019(3) 0.022(4) 0.033(4) 0.002(3) 0.008(3) -0.008(3) O3 0.017(3) 0.026(4) 0.024(4) 0.009(3) 0.008(3) -0.005(3) O4 0.019(3) 0.016(3) 0.018(3) 0.001(3) 0.007(3) -0.002(3) O5 0.014(3) 0.014(3) 0.016(3) -0.002(3) 0.007(3) -0.003(2) O6 0.019(3) 0.012(3) 0.026(4) 0.002(3) 0.014(3) 0.001(2) O7 0.019(3) 0.017(3) 0.022(3) 0.001(3) 0.012(3) 0.002(3) O8 0.022(4) 0.016(3) 0.036(4) 0.000(3) 0.015(3) -0.001(3) O9 0.071(6) 0.028(4) 0.067(6) 0.018(4) 0.060(5) 0.017(4) O10 0.017(3) 0.014(3) 0.023(4) -0.002(3) 0.010(3) -0.001(3) O11 0.015(3) 0.016(3) 0.026(4) -0.010(3) -0.002(3) 0.003(3) O12 0.023(4) 0.019(3) 0.025(4) -0.004(3) 0.004(3) 0.005(3) O13 0.023(3) 0.014(3) 0.027(4) -0.011(3) 0.009(3) -0.001(3) O14 0.017(3) 0.017(3) 0.031(4) -0.004(3) 0.003(3) 0.005(3) O15 0.016(3) 0.019(3) 0.020(3) -0.005(3) 0.003(3) 0.002(3) O16 0.016(3) 0.050(5) 0.032(4) 0.009(4) 0.001(3) -0.005(3) O17 0.068(4) 0.068(4) 0.068(4) -0.0004(8) 0.0231(15) 0.0000(8) O17' 0.068(4) 0.068(4) 0.068(4) -0.0002(8) 0.0232(15) 0.0000(8) O18 0.066(4) 0.066(4) 0.066(4) 0.0003(8) 0.0223(15) 0.0000(8) O18' 0.066(4) 0.066(4) 0.066(4) 0.0001(8) 0.0224(15) 0.0001(8) O19 0.017(3) 0.024(4) 0.021(4) 0.003(3) 0.002(3) 0.000(3) O20 0.023(4) 0.024(4) 0.047(5) -0.001(3) 0.023(4) -0.002(3) O21 0.022(3) 0.020(3) 0.027(4) 0.004(3) 0.009(3) -0.003(3) O22 0.044(5) 0.028(4) 0.060(6) -0.005(4) 0.029(4) -0.002(4) O23 0.136(6) 0.135(6) 0.136(6) -0.0002(10) 0.046(2) 0.0001(10) O24 0.127(5) 0.126(5) 0.126(5) 0.0000(9) 0.0433(18) 0.0001(9) O25 0.086(4) 0.086(4) 0.086(4) 0.0000(9) 0.0297(16) 0.0000(9) O26 0.071(6) 0.071(6) 0.071(6) -0.0002(10) 0.024(2) -0.0002(10) O27 0.126(5) 0.126(5) 0.126(5) 0.0000(9) 0.0431(18) 0.0000(9) O28 0.087(4) 0.087(4) 0.087(4) 0.0000(8) 0.0298(15) 0.0000(8) O29 0.102(4) 0.102(4) 0.102(4) 0.0000(9) 0.0348(16) -0.0001(9) O30 0.102(4) 0.102(4) 0.102(4) 0.0000(8) 0.0347(15) 0.0000(8) O31 0.102(4) 0.102(4) 0.102(4) 0.0000(7) 0.0347(15) 0.0000(7) O32 0.045(8) 0.045(8) 0.045(8) 0.0000(10) 0.015(3) -0.0001(10) O33 0.087(4) 0.088(4) 0.087(4) 0.0000(8) 0.0298(16) 0.0001(8) O34 0.063(7) 0.063(7) 0.063(7) 0.0000(8) 0.022(2) 0.0000(8) O35 0.101(4) 0.101(4) 0.101(4) 0.0000(9) 0.0348(16) 0.0001(9) O36 0.063(7) 0.063(7) 0.063(7) 0.0000(8) 0.022(2) 0.0000(8) O37 0.102(4) 0.102(4) 0.102(4) 0.0000(7) 0.0348(15) 0.0000(7) O38 0.080(12) 0.080(12) 0.080(12) -0.0001(10) 0.027(4) -0.0001(10) O39 0.126(5) 0.126(5) 0.126(5) 0.0000(9) 0.0432(18) 0.0000(9) O40 0.102(4) 0.102(4) 0.102(4) 0.0000(8) 0.0347(15) 0.0000(8) O41 0.102(4) 0.102(4) 0.102(4) 0.0000(7) 0.0348(15) 0.0000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O6 2.421(6) . ? Sm1 O11 2.435(6) . ? Sm1 O1 2.451(6) . ? Sm1 O10 2.452(6) . ? Sm1 O15 2.476(6) . ? Sm1 O5 2.476(6) . ? Sm1 N3 2.521(7) . ? Sm1 N2 2.534(7) . ? Sm1 N1 2.539(7) . ? Cd1 O13 2.180(6) 4_676 ? Cd1 O22 2.207(8) . ? Cd1 O20 2.219(7) . ? Cd1 O21 2.276(6) . ? Cd1 O7 2.297(6) 1_655 ? Cd1 O4 2.317(6) . ? Co1 O18' 1.96(5) . ? Co1 O17 2.030(17) . ? Co1 O18 2.132(16) . ? Co1 O16 2.144(7) . ? Co1 O14 2.205(6) 1_455 ? Co1 O17' 2.21(5) . ? Co1 O19 2.210(7) . ? Co1 O2 2.215(6) . ? C1 O2 1.250(10) . ? C1 O1 1.268(11) . ? C1 C2 1.508(12) . ? C2 N1 1.340(11) . ? C2 C3 1.383(13) . ? C3 C4 1.381(13) . ? C3 H3 0.9300 . ? C4 O3 1.335(11) . ? C4 C5 1.396(12) . ? C5 C6 1.397(12) . ? C5 H5 0.9300 . ? C6 N1 1.318(11) . ? C6 C7 1.512(12) . ? C7 O5 1.260(10) . ? C7 O4 1.263(10) . ? C8 O7 1.262(10) . ? C8 O6 1.268(11) . ? C8 C9 1.499(12) . ? C9 N2 1.344(11) . ? C9 C10 1.376(12) . ? C10 C11 1.409(13) . ? C10 H10 0.9300 . ? C11 O8 1.335(11) . ? C11 C12 1.397(13) . ? C12 C13 1.379(13) . ? C12 H12 0.9300 . ? C13 N2 1.337(11) . ? C13 C14 1.515(13) . ? C14 O9 1.228(12) . ? C14 O10 1.265(11) . ? C15 O12 1.258(11) . ? C15 O11 1.265(11) . ? C15 C16 1.508(12) . ? C16 N3 1.347(11) . ? C16 C17 1.370(12) . ? C17 C18 1.408(13) . ? C17 H17 0.9300 . ? C18 O13 1.311(11) . ? C18 C19 1.387(13) . ? C19 C20 1.384(13) . ? C19 H19 0.9300 . ? C20 N3 1.355(11) . ? C20 C21 1.493(13) . ? C21 O14 1.254(11) . ? C21 O15 1.283(11) . ? O3 H3A 0.8200 . ? O7 Co2 2.297(6) 1_455 ? O7 Cd1 2.297(6) 1_455 ? O8 H8 0.8200 . ? O13 Co2 2.180(6) 4_475 ? O13 Cd1 2.180(6) 4_475 ? O14 Cd2 2.205(6) 1_655 ? O14 Co1 2.205(6) 1_655 ? O16 H16A 0.8510 . ? O16 H16B 0.8506 . ? O17 O17' 0.59(5) . ? O18 O18' 0.57(5) . ? O19 H19A 0.8506 . ? O19 H19B 0.8494 . ? O20 H20A 0.8491 . ? O20 H20B 0.8492 . ? O21 H21A 0.8505 . ? O21 H21B 0.8501 . ? O22 H22A 0.8497 . ? O22 H22B 0.8496 . ? O23 H23A 0.8529 . ? O23 H23B 0.8525 . ? O24 O39 1.67(7) . ? O24 H24A 0.8527 . ? O24 H24B 0.8499 . ? 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 O6 Sm1 O11 77.8(2) . . ? O6 Sm1 O1 75.0(2) . . ? O11 Sm1 O1 79.9(2) . . ? O6 Sm1 O10 126.1(2) . . ? O11 Sm1 O10 87.2(2) . . ? O1 Sm1 O10 152.4(2) . . ? O6 Sm1 O15 147.3(2) . . ? O11 Sm1 O15 126.5(2) . . ? O1 Sm1 O15 87.4(2) . . ? O10 Sm1 O15 80.8(2) . . ? O6 Sm1 O5 88.6(2) . . ? O11 Sm1 O5 147.2(2) . . ? O1 Sm1 O5 125.4(2) . . ? O10 Sm1 O5 76.9(2) . . ? O15 Sm1 O5 79.4(2) . . ? O6 Sm1 N3 134.1(2) . . ? O11 Sm1 N3 63.5(2) . . ? O1 Sm1 N3 74.8(2) . . ? O10 Sm1 N3 77.6(2) . . ? O15 Sm1 N3 63.0(2) . . ? O5 Sm1 N3 137.2(2) . . ? O6 Sm1 N2 63.2(2) . . ? O11 Sm1 N2 76.0(2) . . ? O1 Sm1 N2 135.0(2) . . ? O10 Sm1 N2 63.0(2) . . ? O15 Sm1 N2 137.2(2) . . ? O5 Sm1 N2 71.2(2) . . ? N3 Sm1 N2 124.1(2) . . ? O6 Sm1 N1 77.0(2) . . ? O11 Sm1 N1 139.2(2) . . ? O1 Sm1 N1 62.8(2) . . ? O10 Sm1 N1 133.6(2) . . ? O15 Sm1 N1 70.4(2) . . ? O5 Sm1 N1 62.8(2) . . ? N3 Sm1 N1 117.0(2) . . ? N2 Sm1 N1 118.8(2) . . ? O13 Cd1 O22 90.2(3) 4_676 . ? O13 Cd1 O20 100.1(3) 4_676 . ? O22 Cd1 O20 169.6(3) . . ? O13 Cd1 O21 172.7(2) 4_676 . ? O22 Cd1 O21 86.0(3) . . ? O20 Cd1 O21 83.8(3) . . ? O13 Cd1 O7 92.5(2) 4_676 1_655 ? O22 Cd1 O7 91.0(3) . 1_655 ? O20 Cd1 O7 90.0(2) . 1_655 ? O21 Cd1 O7 81.3(2) . 1_655 ? O13 Cd1 O4 99.2(2) 4_676 . ? O22 Cd1 O4 92.0(3) . . ? O20 Cd1 O4 85.0(2) . . ? O21 Cd1 O4 87.2(2) . . ? O7 Cd1 O4 167.9(2) 1_655 . ? O18' Co1 O17 76.1(15) . . ? O18' Co1 O18 15.1(15) . . ? O17 Co1 O18 90.9(6) . . ? O18' Co1 O16 163.7(15) . . ? O17 Co1 O16 89.2(5) . . ? O18 Co1 O16 176.2(5) . . ? O18' Co1 O14 90.5(15) . 1_455 ? O17 Co1 O14 93.1(5) . 1_455 ? O18 Co1 O14 92.9(5) . 1_455 ? O16 Co1 O14 83.3(3) . 1_455 ? O18' Co1 O17' 89.8(19) . . ? O17 Co1 O17' 15.4(13) . . ? O18 Co1 O17' 104.1(14) . . ? O16 Co1 O17' 76.6(13) . . ? O14 Co1 O17' 100.1(13) 1_455 . ? O18' Co1 O19 100.7(15) . . ? O17 Co1 O19 176.7(5) . . ? O18 Co1 O19 85.9(4) . . ? O16 Co1 O19 94.1(3) . . ? O14 Co1 O19 87.7(2) 1_455 . ? O17' Co1 O19 166.9(13) . . ? O18' Co1 O2 99.2(15) . . ? O17 Co1 O2 97.1(5) . . ? O18 Co1 O2 94.5(5) . . ? O16 Co1 O2 89.3(3) . . ? O14 Co1 O2 167.3(2) 1_455 . ? O17' Co1 O2 88.2(13) . . ? O19 Co1 O2 82.5(2) . . ? O2 C1 O1 125.3(8) . . ? O2 C1 C2 119.8(8) . . ? O1 C1 C2 114.9(7) . . ? N1 C2 C3 122.8(8) . . ? N1 C2 C1 114.6(8) . . ? C3 C2 C1 122.6(8) . . ? C4 C3 C2 119.4(8) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? O3 C4 C3 124.1(8) . . ? O3 C4 C5 117.7(8) . . ? C3 C4 C5 118.2(8) . . ? C4 C5 C6 118.0(8) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? N1 C6 C5 123.7(8) . . ? N1 C6 C7 114.4(8) . . ? C5 C6 C7 121.8(8) . . ? O5 C7 O4 125.0(8) . . ? O5 C7 C6 116.2(7) . . ? O4 C7 C6 118.8(8) . . ? O7 C8 O6 124.0(8) . . ? O7 C8 C9 119.5(8) . . ? O6 C8 C9 116.5(8) . . ? N2 C9 C10 122.8(8) . . ? N2 C9 C8 113.3(7) . . ? C10 C9 C8 123.9(8) . . ? C9 C10 C11 118.9(8) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? O8 C11 C12 123.6(8) . . ? O8 C11 C10 118.4(8) . . ? C12 C11 C10 118.0(8) . . ? C13 C12 C11 118.8(9) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N2 C13 C12 123.2(9) . . ? N2 C13 C14 114.4(8) . . ? C12 C13 C14 122.3(8) . . ? O9 C14 O10 126.1(9) . . ? O9 C14 C13 118.9(9) . . ? O10 C14 C13 115.1(8) . . ? O12 C15 O11 124.2(8) . . ? O12 C15 C16 118.8(8) . . ? O11 C15 C16 117.0(7) . . ? N3 C16 C17 123.5(8) . . ? N3 C16 C15 112.9(8) . . ? C17 C16 C15 123.6(8) . . ? C16 C17 C18 120.0(8) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? O13 C18 C19 121.0(8) . . ? O13 C18 C17 122.5(8) . . ? C19 C18 C17 116.4(8) . . ? C20 C19 C18 120.5(8) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? N3 C20 C19 122.7(8) . . ? N3 C20 C21 113.6(8) . . ? C19 C20 C21 123.7(8) . . ? O14 C21 O15 124.3(8) . . ? O14 C21 C20 119.2(8) . . ? O15 C21 C20 116.5(8) . . ? C6 N1 C2 117.9(8) . . ? C6 N1 Sm1 121.2(6) . . ? C2 N1 Sm1 120.3(6) . . ? C13 N2 C9 118.3(8) . . ? C13 N2 Sm1 120.8(6) . . ? C9 N2 Sm1 120.7(6) . . ? C16 N3 C20 116.9(8) . . ? C16 N3 Sm1 121.2(6) . . ? C20 N3 Sm1 121.9(6) . . ? C1 O1 Sm1 126.5(5) . . ? C1 O2 Co1 127.2(6) . . ? C4 O3 H3A 109.5 . . ? C7 O4 Cd1 122.8(6) . . ? C7 O5 Sm1 124.9(5) . . ? C8 O6 Sm1 126.1(5) . . ? C8 O7 Co2 121.1(5) . 1_455 ? C8 O7 Cd1 121.1(5) . 1_455 ? Co2 O7 Cd1 0.00(4) 1_455 1_455 ? C11 O8 H8 109.5 . . ? C14 O10 Sm1 126.5(6) . . ? C15 O11 Sm1 125.3(5) . . ? C18 O13 Co2 129.8(6) . 4_475 ? C18 O13 Cd1 129.8(6) . 4_475 ? Co2 O13 Cd1 0.00(5) 4_475 4_475 ? C21 O14 Cd2 127.8(6) . 1_655 ? C21 O14 Co1 127.8(6) . 1_655 ? Cd2 O14 Co1 0.00(6) 1_655 1_655 ? C21 O15 Sm1 124.8(5) . . ? Co1 O16 H16A 116.1 . . ? Co1 O16 H16B 108.6 . . ? H16A O16 H16B 116.7 . . ? O17' O17 Co1 100(6) . . ? O17 O17' Co1 65(5) . . ? O18' O18 Co1 65(6) . . ? O18 O18' Co1 100(7) . . ? Co1 O19 H19A 104.8 . . ? Co1 O19 H19B 109.5 . . ? H19A O19 H19B 117.1 . . ? Cd1 O20 H20A 100.7 . . ? Cd1 O20 H20B 130.7 . . ? H20A O20 H20B 117.3 . . ? Cd1 O21 H21A 100.2 . . ? Cd1 O21 H21B 114.4 . . ? H21A O21 H21B 116.9 . . ? Cd1 O22 H22A 131.5 . . ? Cd1 O22 H22B 99.9 . . ? H22A O22 H22B 117.2 . . ? H23A O23 H23B 116.6 . . ? O39 O24 H24A 135.9 . . ? O39 O24 H24B 61.1 . . ? H24A O24 H24B 117.4 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.466 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.185