# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email yaguangsun@yahoo.com.cn _publ_contact_author_phone ? _publ_contact_author_name 'Yaguang Sun' _publ_author_name 'Yaguang Sun' data_5 _database_code_depnum_ccdc_archive 'CCDC 888131' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co Dy2 N4 O24 S2' _chemical_formula_weight 1128.46 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.461(4) _cell_length_b 8.7532(18) _cell_length_c 15.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.78(3) _cell_angle_gamma 90.00 _cell_volume 2966.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2618 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.01 _exptl_crystal_description 0 _exptl_crystal_colour 0 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 5.792 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3904 _exptl_absorpt_correction_T_max 0.3904 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11586 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2618 _reflns_number_gt 2262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0380P)^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 NONE _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2618 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.003 _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 Co1 Co 0.5000 0.70534(10) 0.2500 0.0362(2) Uani 1 2 d S . . S5 S 0.85029(5) 0.54534(12) 1.08636(7) 0.0315(2) Uani 1 1 d . . . Dy1 Dy 0.747566(9) 0.64039(2) 0.883256(12) 0.02847(10) Uani 1 1 d . . . O1 O 0.69063(16) 0.6518(3) 1.1376(2) 0.0393(8) Uani 1 1 d . . . O2 O 0.70432(14) 0.6138(3) 1.0030(2) 0.0370(7) Uani 1 1 d . . . O3 O 0.71370(14) 0.6837(4) 0.7234(2) 0.0426(8) Uani 1 1 d . . . O4 O 0.64859(16) 0.5593(4) 0.7816(2) 0.0517(9) Uani 1 1 d . . . O5 O 0.83468(13) 0.5789(4) 0.99053(19) 0.0396(7) Uani 1 1 d . . . O6 O 0.83088(17) 0.3923(4) 1.1030(3) 0.0534(10) Uani 1 1 d . . . O7 O 0.82017(17) 0.6549(4) 1.1345(2) 0.0471(9) Uani 1 1 d . . . O8 O 0.91642(13) 0.5587(4) 1.1179(2) 0.0502(9) Uani 1 1 d . . . O9 O 0.81835(15) 0.5287(4) 0.8017(2) 0.0519(9) Uani 1 1 d . . . H9A H 0.8084 0.5360 0.7456 0.062 Uiso 1 1 d R . . H9B H 0.8350 0.4413 0.8151 0.062 Uiso 1 1 d R . . O10 O 0.74216(19) 0.3681(4) 0.8982(3) 0.0721(14) Uani 1 1 d . . . H10A H 0.7520 0.3018 0.8641 0.087 Uiso 1 1 d R . . H10B H 0.7196 0.3298 0.9294 0.087 Uiso 1 1 d R . . O11 O 0.5000 0.4601(6) 0.2500 0.0763(18) Uani 1 2 d S . . H11 H 0.4691 0.4069 0.2504 0.092 Uiso 1 1 d R . . O12 O 0.40433(14) 0.7177(4) 0.2253(2) 0.0451(8) Uani 1 1 d . . . H12A H 0.3831 0.6364 0.2196 0.068 Uiso 1 1 d R . . H12B H 0.3913 0.7751 0.1808 0.068 Uiso 1 1 d R . . O13 O 0.5000 0.9445(5) 0.2500 0.0641(17) Uani 1 2 d S . . H13 H 0.5218 0.9909 0.2933 0.077 Uiso 1 1 d R . . N1 N 0.50073(16) 0.7040(4) 0.3865(2) 0.0374(9) Uani 1 1 d . . . N2 N 0.47887(18) 0.8152(5) 0.5048(3) 0.0419(10) Uani 1 1 d . . . H2 H 0.4603 0.8707 0.5365 0.050 Uiso 1 1 d R . . C1 C 0.4624(2) 0.7923(6) 0.4178(3) 0.0427(11) Uani 1 1 d . . . H1 H 0.4274 0.8343 0.3823 0.051 Uiso 1 1 calc R . . C2 C 0.5451(2) 0.6626(5) 0.4603(3) 0.0340(10) Uani 1 1 d . . . C3 C 0.59452(19) 0.5639(5) 0.4698(3) 0.0349(10) Uani 1 1 d . . . H3 H 0.6028 0.5137 0.4208 0.042 Uiso 1 1 calc R . . C4 C 0.63073(19) 0.5418(5) 0.5521(3) 0.0321(9) Uani 1 1 d . . . C5 C 0.6194(2) 0.6231(5) 0.6268(3) 0.0312(10) Uani 1 1 d . . . C6 C 0.57006(19) 0.7187(5) 0.6185(3) 0.0361(10) Uani 1 1 d . . . H6 H 0.5622 0.7720 0.6668 0.043 Uiso 1 1 calc R . . C7 C 0.53265(19) 0.7322(5) 0.5349(3) 0.0341(10) Uani 1 1 d . . . C8 C 0.6629(2) 0.6182(5) 0.7153(3) 0.0336(10) Uani 1 1 d . . . C9 C 0.67870(19) 0.5796(5) 1.0645(3) 0.0316(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0389(5) 0.0340(5) 0.0317(5) 0.000 -0.0008(4) 0.000 S5 0.0289(5) 0.0337(6) 0.0303(6) 0.0041(4) 0.0032(4) 0.0016(4) Dy1 0.03025(15) 0.02916(14) 0.02482(14) 0.00023(7) 0.00359(10) -0.00095(8) O1 0.050(2) 0.0354(18) 0.0309(18) -0.0048(13) 0.0051(15) -0.0111(14) O2 0.0355(17) 0.0410(17) 0.0344(17) 0.0067(13) 0.0074(14) -0.0026(14) O3 0.0368(19) 0.057(2) 0.0336(18) -0.0027(15) 0.0063(14) -0.0026(16) O4 0.071(2) 0.052(2) 0.0291(17) 0.0032(15) 0.0046(16) -0.0271(19) O5 0.0379(17) 0.0488(18) 0.0304(16) 0.0033(15) 0.0036(14) 0.0052(15) O6 0.053(2) 0.0408(19) 0.062(2) 0.0145(17) 0.0030(19) -0.0042(16) O7 0.054(2) 0.052(2) 0.0314(18) -0.0035(14) 0.0007(16) 0.0182(16) O8 0.0312(17) 0.078(3) 0.0370(19) 0.0178(17) -0.0020(14) 0.0005(17) O9 0.066(2) 0.050(2) 0.0397(19) 0.0018(16) 0.0120(17) 0.0205(18) O10 0.072(3) 0.036(2) 0.122(4) -0.003(2) 0.051(3) -0.0056(17) O11 0.132(5) 0.034(3) 0.075(4) 0.000 0.048(4) 0.000 O12 0.0446(18) 0.0426(18) 0.0423(19) 0.0070(15) -0.0027(15) -0.0096(15) O13 0.075(4) 0.033(3) 0.061(3) 0.000 -0.036(3) 0.000 N1 0.036(2) 0.041(2) 0.032(2) -0.0024(17) 0.0007(16) 0.0099(17) N2 0.040(2) 0.046(2) 0.040(2) -0.0008(18) 0.0093(18) 0.0119(19) C1 0.038(3) 0.050(3) 0.035(3) 0.002(2) -0.001(2) 0.009(2) C2 0.036(2) 0.036(2) 0.028(2) 0.0000(18) 0.0023(19) 0.0005(19) C3 0.040(3) 0.035(2) 0.028(2) -0.0047(18) 0.0044(19) 0.006(2) C4 0.036(2) 0.031(2) 0.028(2) -0.0011(17) 0.0035(18) 0.0028(19) C5 0.032(2) 0.032(2) 0.029(2) 0.0014(17) 0.0056(19) -0.0018(17) C6 0.040(3) 0.036(2) 0.034(2) -0.0024(19) 0.012(2) 0.005(2) C7 0.033(2) 0.034(2) 0.035(2) -0.0004(19) 0.008(2) 0.0055(19) C8 0.042(3) 0.031(2) 0.026(2) -0.0032(18) 0.004(2) -0.0004(19) C9 0.033(2) 0.032(2) 0.027(2) 0.0058(19) 0.0007(19) 0.0008(19) _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 Co1 O13 2.093(5) . ? Co1 O12 2.100(3) . ? Co1 O12 2.100(3) 2_655 ? Co1 N1 2.108(4) . ? Co1 N1 2.108(4) 2_655 ? Co1 O11 2.147(5) . ? S5 O6 1.449(3) . ? S5 O8 1.462(3) . ? S5 O7 1.468(3) . ? S5 O5 1.475(3) . ? Dy1 O2 2.286(3) . ? Dy1 O7 2.328(3) 7_667 ? Dy1 O5 2.332(3) . ? Dy1 O1 2.353(3) 7_667 ? Dy1 O10 2.400(3) . ? Dy1 O9 2.442(3) . ? Dy1 O3 2.451(3) . ? Dy1 O4 2.525(3) . ? Dy1 O2 2.838(3) 7_667 ? Dy1 C8 2.867(5) . ? Dy1 C9 2.969(4) 7_667 ? O1 C9 1.271(5) . ? O1 Dy1 2.353(3) 7_667 ? O2 C9 1.252(5) . ? O2 Dy1 2.838(3) 7_667 ? O3 C8 1.258(6) . ? O4 C8 1.251(6) . ? O7 Dy1 2.328(3) 7_667 ? O9 H9A 0.8487 . ? O9 H9B 0.8567 . ? O10 H10A 0.8459 . ? O10 H10B 0.8425 . ? O11 H11 0.8377 . ? O12 H12A 0.8502 . ? O12 H12B 0.8505 . ? O13 H13 0.8420 . ? N1 C1 1.325(6) . ? N1 C2 1.387(5) . ? N2 C1 1.330(6) . ? N2 C7 1.398(5) . ? N2 H2 0.8601 . ? C1 H1 0.9300 . ? C2 C7 1.388(6) . ? C2 C3 1.388(6) . ? C3 C4 1.364(6) . ? C3 H3 0.9300 . ? C4 C5 1.428(6) . ? C4 C9 1.495(6) 6_565 ? C5 C6 1.371(6) . ? C5 C8 1.496(6) . ? C6 C7 1.382(6) . ? C6 H6 0.9300 . ? C9 C4 1.495(6) 6_566 ? C9 Dy1 2.969(4) 7_667 ? 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 O13 Co1 O12 87.05(9) . . ? O13 Co1 O12 87.05(9) . 2_655 ? O12 Co1 O12 174.10(18) . 2_655 ? O13 Co1 N1 90.31(11) . . ? O12 Co1 N1 87.90(14) . . ? O12 Co1 N1 92.13(14) 2_655 . ? O13 Co1 N1 90.31(11) . 2_655 ? O12 Co1 N1 92.13(14) . 2_655 ? O12 Co1 N1 87.90(14) 2_655 2_655 ? N1 Co1 N1 179.4(2) . 2_655 ? O13 Co1 O11 180.000(1) . . ? O12 Co1 O11 92.95(9) . . ? O12 Co1 O11 92.95(9) 2_655 . ? N1 Co1 O11 89.69(11) . . ? N1 Co1 O11 89.69(11) 2_655 . ? O6 S5 O8 109.7(2) . . ? O6 S5 O7 108.9(2) . . ? O8 S5 O7 109.1(2) . . ? O6 S5 O5 110.4(2) . . ? O8 S5 O5 108.50(19) . . ? O7 S5 O5 110.24(19) . . ? O2 Dy1 O7 77.89(12) . 7_667 ? O2 Dy1 O5 80.78(11) . . ? O7 Dy1 O5 133.27(12) 7_667 . ? O2 Dy1 O1 123.99(11) . 7_667 ? O7 Dy1 O1 77.21(13) 7_667 7_667 ? O5 Dy1 O1 81.28(12) . 7_667 ? O2 Dy1 O10 77.37(14) . . ? O7 Dy1 O10 136.91(13) 7_667 . ? O5 Dy1 O10 75.80(14) . . ? O1 Dy1 O10 145.56(13) 7_667 . ? O2 Dy1 O9 145.07(11) . . ? O7 Dy1 O9 136.94(12) 7_667 . ? O5 Dy1 O9 74.68(11) . . ? O1 Dy1 O9 76.56(11) 7_667 . ? O10 Dy1 O9 72.82(13) . . ? O2 Dy1 O3 137.81(11) . . ? O7 Dy1 O3 73.33(12) 7_667 . ? O5 Dy1 O3 141.10(11) . . ? O1 Dy1 O3 78.64(11) 7_667 . ? O10 Dy1 O3 103.86(14) . . ? O9 Dy1 O3 68.44(11) . . ? O2 Dy1 O4 90.17(11) . . ? O7 Dy1 O4 71.36(12) 7_667 . ? O5 Dy1 O4 149.70(12) . . ? O1 Dy1 O4 126.64(11) 7_667 . ? O10 Dy1 O4 74.01(13) . . ? O9 Dy1 O4 98.60(12) . . ? O3 Dy1 O4 51.74(11) . . ? O2 Dy1 O2 75.32(11) . 7_667 ? O7 Dy1 O2 68.81(11) 7_667 7_667 ? O5 Dy1 O2 65.75(10) . 7_667 ? O1 Dy1 O2 48.96(10) 7_667 7_667 ? O10 Dy1 O2 135.55(13) . 7_667 ? O9 Dy1 O2 114.96(11) . 7_667 ? O3 Dy1 O2 119.93(10) . 7_667 ? O4 Dy1 O2 139.60(11) . 7_667 ? O2 Dy1 C8 114.33(12) . . ? O7 Dy1 C8 70.12(12) 7_667 . ? O5 Dy1 C8 156.00(12) . . ? O1 Dy1 C8 102.79(12) 7_667 . ? O10 Dy1 C8 88.99(14) . . ? O9 Dy1 C8 83.20(12) . . ? O3 Dy1 C8 25.89(12) . . ? O4 Dy1 C8 25.85(12) . . ? O2 Dy1 C8 134.30(10) 7_667 . ? O2 Dy1 C9 100.07(12) . 7_667 ? O7 Dy1 C9 72.97(13) 7_667 7_667 ? O5 Dy1 C9 70.55(11) . 7_667 ? O1 Dy1 C9 24.30(11) 7_667 7_667 ? O10 Dy1 C9 146.18(13) . 7_667 ? O9 Dy1 C9 94.80(12) . 7_667 ? O3 Dy1 C9 100.20(11) . 7_667 ? O4 Dy1 C9 139.74(11) . 7_667 ? O2 Dy1 C9 24.77(10) 7_667 7_667 ? C8 Dy1 C9 121.39(12) . 7_667 ? C9 O1 Dy1 106.1(3) . 7_667 ? C9 O2 Dy1 171.5(3) . . ? C9 O2 Dy1 83.5(3) . 7_667 ? Dy1 O2 Dy1 104.68(11) . 7_667 ? C8 O3 Dy1 95.9(3) . . ? C8 O4 Dy1 92.6(3) . . ? S5 O5 Dy1 137.45(19) . . ? S5 O7 Dy1 143.7(2) . 7_667 ? Dy1 O9 H9A 116.3 . . ? Dy1 O9 H9B 122.2 . . ? H9A O9 H9B 108.4 . . ? Dy1 O10 H10A 126.6 . . ? Dy1 O10 H10B 120.0 . . ? H10A O10 H10B 110.9 . . ? Co1 O11 H11 123.8 . . ? Co1 O12 H12A 120.2 . . ? Co1 O12 H12B 109.5 . . ? H12A O12 H12B 109.0 . . ? Co1 O13 H13 118.9 . . ? C1 N1 C2 104.9(4) . . ? C1 N1 Co1 120.1(3) . . ? C2 N1 Co1 132.1(3) . . ? C1 N2 C7 106.6(4) . . ? C1 N2 H2 126.9 . . ? C7 N2 H2 126.5 . . ? N1 C1 N2 113.6(4) . . ? N1 C1 H1 123.2 . . ? N2 C1 H1 123.2 . . ? N1 C2 C7 109.2(4) . . ? N1 C2 C3 131.4(4) . . ? C7 C2 C3 119.3(4) . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 C9 119.0(4) . 6_565 ? C5 C4 C9 120.2(4) . 6_565 ? C6 C5 C4 120.9(4) . . ? C6 C5 C8 117.0(4) . . ? C4 C5 C8 121.9(4) . . ? C5 C6 C7 116.8(4) . . ? C5 C6 H6 121.6 . . ? C7 C6 H6 121.6 . . ? C6 C7 C2 123.2(4) . . ? C6 C7 N2 131.1(4) . . ? C2 C7 N2 105.6(4) . . ? O4 C8 O3 119.8(4) . . ? O4 C8 C5 121.8(4) . . ? O3 C8 C5 118.2(4) . . ? O4 C8 Dy1 61.6(2) . . ? O3 C8 Dy1 58.2(2) . . ? C5 C8 Dy1 174.4(3) . . ? O2 C9 O1 121.0(4) . . ? O2 C9 C4 120.8(4) . 6_566 ? O1 C9 C4 118.1(4) . 6_566 ? O2 C9 Dy1 71.8(2) . 7_667 ? O1 C9 Dy1 49.6(2) . 7_667 ? C4 C9 Dy1 164.7(3) 6_566 7_667 ? 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 O7 Dy1 O2 Dy1 -70.98(12) 7_667 . . 7_667 ? O5 Dy1 O2 Dy1 67.19(11) . . . 7_667 ? O1 Dy1 O2 Dy1 -5.67(16) 7_667 . . 7_667 ? O10 Dy1 O2 Dy1 144.58(14) . . . 7_667 ? O9 Dy1 O2 Dy1 112.75(18) . . . 7_667 ? O3 Dy1 O2 Dy1 -118.63(15) . . . 7_667 ? O4 Dy1 O2 Dy1 -141.86(12) . . . 7_667 ? O2 Dy1 O2 Dy1 0.0 7_667 . . 7_667 ? C8 Dy1 O2 Dy1 -132.37(11) . . . 7_667 ? C9 Dy1 O2 Dy1 -1.00(12) 7_667 . . 7_667 ? O2 Dy1 O3 C8 -29.7(3) . . . . ? O7 Dy1 O3 C8 -78.7(3) 7_667 . . . ? O5 Dy1 O3 C8 141.1(3) . . . . ? O1 Dy1 O3 C8 -158.6(3) 7_667 . . . ? O10 Dy1 O3 C8 56.6(3) . . . . ? O9 Dy1 O3 C8 121.5(3) . . . . ? O4 Dy1 O3 C8 0.4(3) . . . . ? O2 Dy1 O3 C8 -131.3(3) 7_667 . . . ? C9 Dy1 O3 C8 -147.3(3) 7_667 . . . ? O2 Dy1 O4 C8 159.9(3) . . . . ? O7 Dy1 O4 C8 82.7(3) 7_667 . . . ? O5 Dy1 O4 C8 -128.4(3) . . . . ? O1 Dy1 O4 C8 25.5(3) 7_667 . . . ? O10 Dy1 O4 C8 -123.3(3) . . . . ? O9 Dy1 O4 C8 -54.1(3) . . . . ? O3 Dy1 O4 C8 -0.4(3) . . . . ? O2 Dy1 O4 C8 92.7(3) 7_667 . . . ? C9 Dy1 O4 C8 54.0(4) 7_667 . . . ? O6 S5 O5 Dy1 75.9(3) . . . . ? O8 S5 O5 Dy1 -163.8(3) . . . . ? O7 S5 O5 Dy1 -44.4(4) . . . . ? O2 Dy1 O5 S5 -1.4(3) . . . . ? O7 Dy1 O5 S5 62.2(4) 7_667 . . . ? O1 Dy1 O5 S5 125.4(3) 7_667 . . . ? O10 Dy1 O5 S5 -80.6(3) . . . . ? O9 Dy1 O5 S5 -156.3(3) . . . . ? O3 Dy1 O5 S5 -175.1(2) . . . . ? O4 Dy1 O5 S5 -75.6(4) . . . . ? O2 Dy1 O5 S5 76.6(3) 7_667 . . . ? C8 Dy1 O5 S5 -132.8(3) . . . . ? C9 Dy1 O5 S5 102.8(3) 7_667 . . . ? O6 S5 O7 Dy1 -117.4(4) . . . 7_667 ? O8 S5 O7 Dy1 122.9(4) . . . 7_667 ? O5 S5 O7 Dy1 3.8(5) . . . 7_667 ? O13 Co1 N1 C1 47.4(4) . . . . ? O12 Co1 N1 C1 -39.6(4) . . . . ? O12 Co1 N1 C1 134.5(4) 2_655 . . . ? O11 Co1 N1 C1 -132.6(4) . . . . ? O13 Co1 N1 C2 -110.4(4) . . . . ? O12 Co1 N1 C2 162.6(4) . . . . ? O12 Co1 N1 C2 -23.3(4) 2_655 . . . ? O11 Co1 N1 C2 69.6(4) . . . . ? C2 N1 C1 N2 1.8(6) . . . . ? Co1 N1 C1 N2 -161.3(3) . . . . ? C7 N2 C1 N1 -1.2(6) . . . . ? C1 N1 C2 C7 -1.7(5) . . . . ? Co1 N1 C2 C7 158.5(3) . . . . ? C1 N1 C2 C3 175.3(5) . . . . ? Co1 N1 C2 C3 -24.6(8) . . . . ? N1 C2 C3 C4 -178.7(5) . . . . ? C7 C2 C3 C4 -2.0(7) . . . . ? C2 C3 C4 C5 -2.3(7) . . . . ? C2 C3 C4 C9 171.9(4) . . . 6_565 ? C3 C4 C5 C6 3.5(7) . . . . ? C9 C4 C5 C6 -170.6(4) 6_565 . . . ? C3 C4 C5 C8 -171.4(4) . . . . ? C9 C4 C5 C8 14.5(6) 6_565 . . . ? C4 C5 C6 C7 -0.2(6) . . . . ? C8 C5 C6 C7 175.0(4) . . . . ? C5 C6 C7 C2 -4.3(7) . . . . ? C5 C6 C7 N2 178.1(4) . . . . ? N1 C2 C7 C6 -177.1(4) . . . . ? C3 C2 C7 C6 5.5(7) . . . . ? N1 C2 C7 N2 1.0(5) . . . . ? C3 C2 C7 N2 -176.3(4) . . . . ? C1 N2 C7 C6 177.9(5) . . . . ? C1 N2 C7 C2 0.0(5) . . . . ? Dy1 O4 C8 O3 0.7(4) . . . . ? Dy1 O4 C8 C5 -174.9(4) . . . . ? Dy1 O3 C8 O4 -0.8(5) . . . . ? Dy1 O3 C8 C5 175.1(3) . . . . ? C6 C5 C8 O4 70.0(6) . . . . ? C4 C5 C8 O4 -114.9(5) . . . . ? C6 C5 C8 O3 -105.7(5) . . . . ? C4 C5 C8 O3 69.4(6) . . . . ? O2 Dy1 C8 O4 -22.2(3) . . . . ? O7 Dy1 C8 O4 -88.1(3) 7_667 . . . ? O5 Dy1 C8 O4 103.5(4) . . . . ? O1 Dy1 C8 O4 -159.2(3) 7_667 . . . ? O10 Dy1 C8 O4 53.4(3) . . . . ? O9 Dy1 C8 O4 126.3(3) . . . . ? O3 Dy1 C8 O4 179.2(5) . . . . ? O2 Dy1 C8 O4 -115.2(3) 7_667 . . . ? C9 Dy1 C8 O4 -142.2(3) 7_667 . . . ? O2 Dy1 C8 O3 158.6(2) . . . . ? O7 Dy1 C8 O3 92.7(3) 7_667 . . . ? O5 Dy1 C8 O3 -75.8(4) . . . . ? O1 Dy1 C8 O3 21.5(3) 7_667 . . . ? O10 Dy1 C8 O3 -125.8(3) . . . . ? O9 Dy1 C8 O3 -53.0(3) . . . . ? O4 Dy1 C8 O3 -179.2(5) . . . . ? O2 Dy1 C8 O3 65.5(3) 7_667 . . . ? C9 Dy1 C8 O3 38.5(3) 7_667 . . . ? Dy1 O2 C9 C4 170.3(4) 7_667 . . 6_566 ? Dy1 O2 C9 Dy1 164.3(19) . . . 7_667 ? Dy1 O1 C9 O2 7.9(5) 7_667 . . . ? Dy1 O1 C9 C4 -168.8(3) 7_667 . . 6_566 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.752 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.137 data_7 _database_code_depnum_ccdc_archive 'CCDC 888132' #TrackingRef '- CIF.cif' _audit_creation_date 2012-09-08 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 Co Er2 N4 O24 S2' _chemical_formula_sum 'C18 H24 Co Er2 N4 O24 S2' _chemical_formula_weight 1137.98 _chemical_melting_point ? 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' Co Co 0.3494 0.9721 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 15.418(3) _cell_length_b 8.6000(17) _cell_length_c 24.421(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.58(2) _cell_angle_gamma 90.00 _cell_volume 2920.7(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5137 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.01 _cell_measurement_theta_min 1.80 _exptl_absorpt_coefficient_mu 6.513 _exptl_absorpt_correction_T_max 0.4417 _exptl_absorpt_correction_T_min 0.2374 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details SADABS _exptl_crystal_colour 0 _exptl_crystal_density_diffrn 2.588 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 0 _exptl_crystal_F_000 2188 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 19268 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 1.80 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _reflns_number_gt 4374 _reflns_number_total 5137 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.973 _refine_diff_density_min -1.207 _refine_diff_density_rms 0.167 _refine_ls_extinction_coef 0.00155(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 462 _refine_ls_number_reflns 5137 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0275 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.0618 _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. PLATON was used to correct the space group, but it had no effect. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.641585(14) 0.35619(2) 0.257301(9) 0.00644(8) Uani 1 1 d . . . Er2 Er 0.871213(13) 0.13372(2) 0.252287(9) 0.00638(8) Uani 1 1 d . . . Co1 Co 0.74476(4) 0.70887(7) 0.49942(3) 0.00992(15) Uani 1 1 d . . . S1 S 0.76593(8) 0.03271(12) 0.35139(5) 0.0077(2) Uani 1 1 d . . . S3 S 0.74128(8) 0.44755(12) 0.15502(5) 0.0079(2) Uani 1 1 d . . . O1 O 0.8068(2) 0.3649(3) 0.29798(14) 0.0088(7) Uani 1 1 d . . . O2 O 0.9589(2) 0.3356(3) 0.31762(15) 0.0111(7) Uani 1 1 d . . . O3 O 1.0140(2) 0.6536(3) 0.28748(14) 0.0108(7) Uani 1 1 d . . . O4 O 1.1457(2) 0.5693(3) 0.36372(15) 0.0133(7) Uani 1 1 d . . . O5 O 0.5140(2) 0.2900(3) 0.28814(14) 0.0111(7) Uani 1 1 d . . . O6 O 0.6233(2) 0.4586(3) 0.34214(15) 0.0127(7) Uani 1 1 d . . . O7 O 0.5693(2) 0.1393(3) 0.19988(15) 0.0120(7) Uani 1 1 d . . . O8 O 0.7139(2) 0.0864(3) 0.20614(14) 0.0110(7) Uani 1 1 d . . . O9 O 0.7009(2) 0.1669(3) 0.33043(15) 0.0138(7) Uani 1 1 d . . . O10 O 0.8454(2) 0.0476(3) 0.33327(15) 0.0125(7) Uani 1 1 d . . . O11 O 0.8089(2) 0.0283(3) 0.41850(14) 0.0136(7) Uani 1 1 d . . . O12 O 0.7101(2) -0.1098(3) 0.32678(16) 0.0160(8) Uani 1 1 d . . . O13 O 0.6620(2) 0.3956(3) 0.16899(14) 0.0097(7) Uani 1 1 d . . . O14 O 0.8293(2) 0.3552(3) 0.18976(14) 0.0102(7) Uani 1 1 d . . . O15 O 0.7612(2) 0.6131(3) 0.17129(16) 0.0143(7) Uani 1 1 d . . . O16 O 0.7138(2) 0.4281(3) 0.08959(15) 0.0144(7) Uani 1 1 d . . . O17 O 0.4963(2) 0.4763(3) 0.19230(15) 0.0149(8) Uani 1 1 d . . . H17A H 0.4991 0.5760 0.1996 0.022 Uiso 1 1 d R . . H17B H 0.4456 0.4450 0.1868 0.022 Uiso 1 1 d R . . O18 O 0.6775(2) 0.6243(3) 0.25556(16) 0.0170(8) Uani 1 1 d . . . H18A H 0.7096 0.6389 0.2343 0.026 Uiso 1 1 d R . . H18B H 0.7119 0.6575 0.2922 0.026 Uiso 1 1 d R . . O19 O 0.8732(2) -0.1350(3) 0.23755(15) 0.0150(8) Uani 1 1 d . . . H19A H 0.8162 -0.1708 0.2239 0.023 Uiso 1 1 d R . . H19B H 0.9079 -0.1785 0.2714 0.023 Uiso 1 1 d R . . O20 O 1.0249(2) 0.0326(3) 0.32581(15) 0.0147(7) Uani 1 1 d . . . H20A H 1.0671 0.1079 0.3423 0.022 Uiso 1 1 d R . . H20B H 1.0491 -0.0322 0.3081 0.022 Uiso 1 1 d R . . O21 O 0.8191(2) 0.7359(3) 0.59579(15) 0.0132(7) Uani 1 1 d . . . H21A H 0.8485 0.6516 0.6114 0.020 Uiso 1 1 d R . . H21B H 0.7876 0.7687 0.6142 0.016 Uiso 1 1 d R . . O22 O 0.7501(2) 0.4615(3) 0.51017(15) 0.0182(8) Uani 1 1 d . . . H22A H 0.6933 0.4249 0.4963 0.027 Uiso 1 1 d R . . H22B H 0.7799 0.4400 0.5477 0.027 Uiso 1 1 d R . . O23 O 0.7352(2) 0.9528(4) 0.49463(15) 0.0196(8) Uani 1 1 d . . . H23A H 0.7607 0.9997 0.4747 0.029 Uiso 1 1 d R . . H23B H 0.7381 1.0096 0.5237 0.029 Uiso 1 1 d R . . O24 O 0.6737(2) 0.7142(3) 0.40640(14) 0.0136(7) Uani 1 1 d . . . H24A H 0.6538 0.6226 0.3926 0.020 Uiso 1 1 d R . . H24B H 0.6974 0.7696 0.3889 0.020 Uiso 1 1 d R . . N1 N 1.0217(3) 0.8218(4) 0.52028(18) 0.0122(9) Uani 1 1 d . . . H1 H 1.0722 0.8779 0.5390 0.015 Uiso 1 1 calc R . . N2 N 0.8809(3) 0.7066(4) 0.49844(18) 0.0118(8) Uani 1 1 d . . . N3 N 0.5345(3) 0.1856(4) 0.52199(18) 0.0131(9) Uani 1 1 d . . . H3 H 0.5864 0.1330 0.5411 0.016 Uiso 1 1 calc R . . N4 N 0.3918(3) 0.2913(4) 0.49997(18) 0.0115(9) Uani 1 1 d . . . C1 C 1.0585(3) 0.6103(5) 0.3425(2) 0.0092(10) Uani 1 1 d . . . C2 C 1.0090(3) 0.6197(5) 0.3833(2) 0.0087(10) Uani 1 1 d . . . C3 C 1.0482(3) 0.7201(5) 0.4321(2) 0.0095(10) Uani 1 1 d . . . H3A H 1.1046 0.7746 0.4405 0.011 Uiso 1 1 calc R . . C4 C 0.9995(3) 0.7359(5) 0.4679(2) 0.0099(10) Uani 1 1 d . . . C5 C 0.9495(3) 0.8008(5) 0.5361(2) 0.0131(10) Uani 1 1 d . . . H5 H 0.9474 0.8472 0.5699 0.016 Uiso 1 1 calc R . . C6 C 0.9116(3) 0.6616(5) 0.4550(2) 0.0102(10) Uani 1 1 d . . . C7 C 0.8736(3) 0.5592(5) 0.4062(2) 0.0078(9) Uani 1 1 d . . . H7 H 0.8161 0.5074 0.3974 0.009 Uiso 1 1 calc R . . C8 C 0.9226(3) 0.5352(4) 0.3707(2) 0.0082(10) Uani 1 1 d . . . C9 C 0.8936(3) 0.4075(5) 0.3258(2) 0.0091(10) Uani 1 1 d . . . C10 C 0.5495(3) 0.3774(5) 0.3336(2) 0.0079(10) Uani 1 1 d . . . C11 C 0.5079(3) 0.3740(4) 0.3787(2) 0.0077(10) Uani 1 1 d . . . C12 C 0.5526(3) 0.2795(5) 0.4292(2) 0.0102(10) Uani 1 1 d . . . H12 H 0.6097 0.2280 0.4367 0.012 Uiso 1 1 calc R . . C13 C 0.5087(3) 0.2648(5) 0.4679(2) 0.0111(10) Uani 1 1 d . . . C14 C 0.4637(3) 0.2060(5) 0.5390(2) 0.0127(10) Uani 1 1 d . . . H14 H 0.4647 0.1647 0.5744 0.015 Uiso 1 1 calc R . . C15 C 0.4196(3) 0.3324(5) 0.4551(2) 0.0087(10) Uani 1 1 d . . . C16 C 0.3745(3) 0.4255(5) 0.4046(2) 0.0091(10) Uani 1 1 d . . . H16 H 0.3154 0.4711 0.3961 0.011 Uiso 1 1 calc R . . C17 C 0.4194(3) 0.4494(4) 0.3668(2) 0.0081(10) Uani 1 1 d . . . C18 C 0.6239(3) 0.0633(5) 0.1835(2) 0.0079(9) Uani 1 1 d U . . 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 0.00601(12) 0.00688(12) 0.00662(13) -0.00059(8) 0.00290(10) -0.00061(7) Er2 0.00555(12) 0.00707(12) 0.00649(13) -0.00015(8) 0.00257(9) -0.00030(7) Co1 0.0112(3) 0.0110(3) 0.0089(4) -0.0007(2) 0.0057(3) 0.0000(2) S1 0.0081(5) 0.0093(5) 0.0061(6) 0.0001(4) 0.0033(5) -0.0009(4) S3 0.0069(5) 0.0088(6) 0.0073(6) 0.0010(4) 0.0025(5) -0.0005(4) O1 0.0059(15) 0.0120(16) 0.0064(18) -0.0005(13) 0.0006(14) -0.0037(12) O2 0.0096(16) 0.0097(15) 0.0137(19) -0.0017(13) 0.0045(15) 0.0007(13) O3 0.0100(16) 0.0154(16) 0.0065(19) -0.0002(13) 0.0031(15) -0.0044(13) O4 0.0067(16) 0.0130(16) 0.020(2) 0.0010(14) 0.0051(15) 0.0026(13) O5 0.0088(16) 0.0130(16) 0.010(2) -0.0038(14) 0.0030(15) 0.0000(13) O6 0.0116(17) 0.0115(16) 0.017(2) -0.0043(14) 0.0079(16) -0.0039(13) O7 0.0148(17) 0.0086(16) 0.015(2) -0.0042(13) 0.0085(16) -0.0025(13) O8 0.0063(15) 0.0152(16) 0.0079(19) 0.0008(13) -0.0002(14) -0.0030(13) O9 0.0129(17) 0.0157(16) 0.017(2) 0.0067(14) 0.0100(16) 0.0058(13) O10 0.0091(16) 0.0146(17) 0.016(2) 0.0023(14) 0.0075(15) 0.0008(13) O11 0.0138(17) 0.0225(17) 0.0055(19) 0.0009(14) 0.0051(15) -0.0036(13) O12 0.0194(18) 0.0149(16) 0.015(2) -0.0062(14) 0.0083(17) -0.0097(14) O13 0.0095(16) 0.0112(15) 0.0092(19) 0.0015(13) 0.0048(15) -0.0030(13) O14 0.0075(16) 0.0125(16) 0.0092(19) 0.0038(13) 0.0022(14) 0.0023(12) O15 0.0171(17) 0.0087(16) 0.018(2) -0.0026(13) 0.0089(16) -0.0028(13) O16 0.0126(17) 0.0242(17) 0.0059(19) -0.0006(14) 0.0034(15) -0.0058(14) O17 0.0119(17) 0.0122(16) 0.022(2) 0.0030(14) 0.0085(16) 0.0030(13) O18 0.0224(19) 0.0142(17) 0.014(2) -0.0022(14) 0.0077(16) -0.0039(14) O19 0.0191(18) 0.0106(17) 0.013(2) 0.0026(13) 0.0043(16) 0.0021(13) O20 0.0096(16) 0.0214(17) 0.010(2) -0.0022(14) 0.0014(15) 0.0032(13) O21 0.0145(17) 0.0128(16) 0.015(2) 0.0021(13) 0.0083(16) 0.0044(13) O22 0.0160(19) 0.0143(19) 0.021(2) 0.0001(14) 0.0053(17) -0.0012(13) O23 0.037(2) 0.0135(19) 0.022(2) 0.0000(14) 0.026(2) 0.0010(14) O24 0.0200(18) 0.0111(17) 0.012(2) -0.0035(13) 0.0090(16) -0.0064(14) N1 0.013(2) 0.014(2) 0.010(2) -0.0045(16) 0.0044(18) -0.0022(16) N2 0.012(2) 0.0147(19) 0.009(2) 0.0009(16) 0.0050(18) 0.0010(16) N3 0.014(2) 0.015(2) 0.010(2) 0.0052(16) 0.0038(19) 0.0028(16) N4 0.012(2) 0.0127(19) 0.009(2) 0.0049(16) 0.0042(19) 0.0009(16) C1 0.011(2) 0.005(2) 0.013(3) -0.0030(18) 0.006(2) -0.0035(18) C2 0.006(2) 0.009(2) 0.010(3) 0.0029(18) 0.002(2) 0.0007(17) C3 0.010(2) 0.009(2) 0.011(3) -0.0022(18) 0.005(2) -0.0042(18) C4 0.010(2) 0.009(2) 0.008(3) 0.0000(18) 0.002(2) 0.0011(18) C5 0.016(3) 0.014(2) 0.009(3) -0.0025(19) 0.006(2) -0.002(2) C6 0.010(2) 0.012(2) 0.009(3) 0.0012(19) 0.005(2) 0.0015(19) C7 0.006(2) 0.009(2) 0.006(3) 0.0003(18) 0.001(2) -0.0023(18) C8 0.007(2) 0.004(2) 0.011(3) 0.0021(18) 0.002(2) 0.0000(17) C9 0.011(2) 0.009(2) 0.008(3) 0.0024(18) 0.004(2) -0.0005(19) C10 0.006(2) 0.007(2) 0.009(3) 0.0032(18) 0.002(2) 0.0037(17) C11 0.003(2) 0.008(2) 0.008(3) 0.0007(18) -0.001(2) -0.0006(17) C12 0.005(2) 0.010(2) 0.015(3) 0.0015(19) 0.004(2) 0.0019(18) C13 0.009(2) 0.011(2) 0.010(3) 0.0043(19) 0.001(2) 0.0012(18) C14 0.012(2) 0.018(2) 0.009(3) 0.005(2) 0.005(2) 0.002(2) C15 0.009(2) 0.008(2) 0.010(3) -0.0031(18) 0.005(2) -0.0014(18) C16 0.009(2) 0.011(2) 0.010(3) -0.0008(18) 0.006(2) 0.0001(19) C17 0.009(2) 0.005(2) 0.012(3) -0.0038(18) 0.005(2) -0.0018(17) C18 0.0087(12) 0.0077(12) 0.0076(13) 0.0012(9) 0.0038(9) -0.0007(9) _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 O1 2.301(3) . ? Er1 O5 2.458(3) . ? Er1 O6 2.378(3) . ? Er1 O7 2.311(3) . ? Er1 O9 2.295(3) . ? Er1 O13 2.335(3) . ? Er1 O17 2.352(3) . ? Er1 O18 2.376(3) . ? Er2 O1 2.672(3) . ? Er2 O2 2.351(3) . ? Er2 O3 2.364(3) 2_745 ? Er2 O4 2.786(3) 2_745 ? Er2 O8 2.226(3) . ? Er2 O10 2.302(3) . ? Er2 O14 2.350(3) . ? Er2 O19 2.341(3) . ? Er2 O20 2.433(3) . ? Er2 C1 2.955(5) 2_745 ? Co1 O21 2.140(3) . ? Co1 O22 2.141(3) . ? Co1 O23 2.103(3) . ? Co1 O24 2.053(3) . ? Co1 N2 2.109(4) . ? Co1 N4 2.112(4) 3_666 ? S1 O9 1.469(3) . ? S1 O10 1.477(3) . ? S1 O11 1.479(3) . ? S1 O12 1.469(3) . ? S3 O13 1.473(3) . ? S3 O14 1.483(3) . ? S3 O15 1.474(3) . ? S3 O16 1.475(3) . ? O1 C9 1.267(5) . ? O2 C9 1.269(5) . ? O3 Er2 2.364(3) 2_755 ? O3 C1 1.271(5) . ? O4 Er2 2.786(3) 2_755 ? O4 C1 1.264(5) . ? O5 C10 1.254(5) . ? O6 C10 1.272(5) . ? O7 C18 1.261(5) . ? O8 C18 1.268(5) . ? O17 H17A 0.8723 . ? O17 H17B 0.7819 . ? O18 H18A 0.8678 . ? O18 H18B 0.8679 . ? O19 H19A 0.8524 . ? O19 H19B 0.8522 . ? O20 H20A 0.8827 . ? O20 H20B 0.8808 . ? O21 H21A 0.8530 . ? O21 H21B 0.8403 . ? O22 H22A 0.8500 . ? O22 H22B 0.8499 . ? O23 H23A 0.8476 . ? O23 H23B 0.8474 . ? O24 H24A 0.8594 . ? O24 H24B 0.8240 . ? N1 H1 0.8600 . ? N1 C4 1.385(6) . ? N1 C5 1.338(6) . ? N2 C5 1.335(6) . ? N2 C6 1.391(6) . ? N3 H3 0.8600 . ? N3 C13 1.383(6) . ? N3 C14 1.336(6) . ? N4 Co1 2.112(4) 3_666 ? N4 C14 1.328(6) . ? N4 C15 1.383(6) . ? C1 Er2 2.955(5) 2_755 ? C1 C2 1.497(6) . ? C2 C3 1.381(6) . ? C2 C8 1.430(6) . ? C3 H3A 0.9300 . ? C3 C4 1.384(6) . ? C4 C6 1.405(6) . ? C5 H5 0.9300 . ? C6 C7 1.392(6) . ? C7 H7 0.9300 . ? C7 C8 1.389(6) . ? C8 C9 1.478(6) . ? C10 C11 1.497(6) . ? C11 C12 1.386(6) . ? C11 C17 1.423(6) . ? C12 H12 0.9300 . ? C12 C13 1.388(6) . ? C13 C15 1.397(6) . ? C14 H14 0.9300 . ? C15 C16 1.381(6) . ? C16 H16 0.9300 . ? C16 C17 1.389(6) . ? C17 C18 1.484(6) 2_655 ? C18 C17 1.484(6) 2_645 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O5 139.32(11) . . ? O1 Er1 O6 97.90(11) . . ? O1 Er1 O7 116.26(10) . . ? O1 Er1 O13 80.12(11) . . ? O1 Er1 O17 146.21(10) . . ? O1 Er1 O18 75.71(10) . . ? O6 Er1 O5 53.62(10) . . ? O7 Er1 O5 76.03(11) . . ? O7 Er1 O6 128.33(10) . . ? O7 Er1 O13 77.23(11) . . ? O7 Er1 O17 82.86(11) . . ? O7 Er1 O18 145.87(12) . . ? O9 Er1 O1 72.08(11) . . ? O9 Er1 O5 72.52(10) . . ? O9 Er1 O6 75.04(11) . . ? O9 Er1 O7 79.93(11) . . ? O9 Er1 O13 130.89(10) . . ? O9 Er1 O17 141.26(11) . . ? O9 Er1 O18 133.22(12) . . ? O13 Er1 O5 139.62(10) . . ? O13 Er1 O6 149.90(10) . . ? O13 Er1 O17 77.40(11) . . ? O13 Er1 O18 73.57(11) . . ? O17 Er1 O5 69.73(11) . . ? O17 Er1 O6 89.34(11) . . ? O17 Er1 O18 73.93(11) . . ? O18 Er1 O5 116.99(10) . . ? O18 Er1 O6 76.84(11) . . ? O1 Er2 O4 133.16(9) . 2_745 ? O1 Er2 C1 134.89(10) . 2_745 ? O2 Er2 O1 51.37(10) . . ? O2 Er2 O3 84.97(10) . 2_745 ? O2 Er2 O4 127.67(10) . 2_745 ? O2 Er2 O20 70.83(10) . . ? O2 Er2 C1 106.50(11) . 2_745 ? O3 Er2 O1 126.67(9) 2_745 . ? O3 Er2 O4 49.82(10) 2_745 2_745 ? O3 Er2 O20 70.46(11) 2_745 . ? O3 Er2 C1 24.60(11) 2_745 2_745 ? O4 Er2 C1 25.23(10) 2_745 2_745 ? O8 Er2 O1 80.05(10) . . ? O8 Er2 O2 131.32(11) . . ? O8 Er2 O3 130.57(11) . 2_745 ? O8 Er2 O4 81.11(10) . 2_745 ? O8 Er2 O10 79.71(11) . . ? O8 Er2 O14 83.44(11) . . ? O8 Er2 O19 79.95(11) . . ? O8 Er2 O20 144.00(11) . . ? O8 Er2 C1 106.18(12) . 2_745 ? O10 Er2 O1 69.33(9) . . ? O10 Er2 O2 85.22(11) . . ? O10 Er2 O3 144.49(10) . 2_745 ? O10 Er2 O4 146.57(9) . 2_745 ? O10 Er2 O14 135.89(10) . . ? O10 Er2 O19 80.40(11) . . ? O10 Er2 O20 74.08(11) . . ? O10 Er2 C1 155.33(10) . 2_745 ? O14 Er2 O1 67.74(10) . . ? O14 Er2 O2 76.03(11) . . ? O14 Er2 O3 73.68(10) . 2_745 ? O14 Er2 O4 67.77(10) . 2_745 ? O14 Er2 O20 132.51(10) . . ? O14 Er2 C1 68.73(11) . 2_745 ? O19 Er2 O1 146.14(10) . . ? O19 Er2 O2 142.33(11) . . ? O19 Er2 O3 86.91(11) . 2_745 ? O19 Er2 O4 69.45(10) . 2_745 ? O19 Er2 O14 135.90(11) . . ? O19 Er2 O20 71.78(10) . . ? O19 Er2 C1 77.21(11) . 2_745 ? O20 Er2 O1 112.14(10) . . ? O20 Er2 O4 108.25(10) . 2_745 ? O20 Er2 C1 89.09(12) . 2_745 ? O21 Co1 O22 89.95(12) . . ? O23 Co1 O21 86.79(12) . . ? O23 Co1 O22 175.08(13) . . ? O23 Co1 N2 93.13(13) . . ? O23 Co1 N4 87.42(13) . 3_666 ? O24 Co1 O21 172.47(12) . . ? O24 Co1 O22 97.58(12) . . ? O24 Co1 O23 85.70(13) . . ? O24 Co1 N2 92.65(14) . . ? O24 Co1 N4 87.15(14) . 3_666 ? N2 Co1 O21 87.17(14) . . ? N2 Co1 O22 90.39(13) . . ? N2 Co1 N4 179.39(16) . 3_666 ? N4 Co1 O21 93.11(14) 3_666 . ? N4 Co1 O22 89.07(13) 3_666 . ? O9 S1 O10 110.96(18) . . ? O9 S1 O11 108.56(19) . . ? O9 S1 O12 108.74(19) . . ? O10 S1 O11 107.53(18) . . ? O12 S1 O10 111.42(19) . . ? O12 S1 O11 109.58(19) . . ? O13 S3 O14 110.56(17) . . ? O13 S3 O15 109.15(18) . . ? O13 S3 O16 109.73(18) . . ? O15 S3 O14 109.28(18) . . ? O15 S3 O16 109.27(19) . . ? O16 S3 O14 108.83(18) . . ? Er1 O1 Er2 109.72(11) . . ? C9 O1 Er1 163.3(3) . . ? C9 O1 Er2 86.7(2) . . ? C9 O2 Er2 101.8(3) . . ? C1 O3 Er2 104.7(3) . 2_755 ? C1 O4 Er2 84.9(3) . 2_755 ? C10 O5 Er1 91.7(3) . . ? C10 O6 Er1 95.0(3) . . ? C18 O7 Er1 113.4(3) . . ? C18 O8 Er2 175.6(3) . . ? S1 O9 Er1 144.2(2) . . ? S1 O10 Er2 139.37(19) . . ? S3 O13 Er1 135.58(19) . . ? S3 O14 Er2 137.09(18) . . ? Er1 O17 H17A 110.2 . . ? Er1 O17 H17B 123.7 . . ? H17A O17 H17B 109.3 . . ? Er1 O18 H18A 110.4 . . ? Er1 O18 H18B 110.1 . . ? H18A O18 H18B 108.5 . . ? Er2 O19 H19A 109.7 . . ? Er2 O19 H19B 109.2 . . ? H19A O19 H19B 109.3 . . ? Er2 O20 H20A 111.5 . . ? Er2 O20 H20B 110.4 . . ? H20A O20 H20B 107.6 . . ? Co1 O21 H21A 109.2 . . ? Co1 O21 H21B 117.8 . . ? H21A O21 H21B 111.4 . . ? Co1 O22 H22A 109.9 . . ? Co1 O22 H22B 108.8 . . ? H22A O22 H22B 109.5 . . ? Co1 O23 H23A 117.9 . . ? Co1 O23 H23B 123.4 . . ? H23A O23 H23B 109.8 . . ? Co1 O24 H24A 110.0 . . ? Co1 O24 H24B 116.3 . . ? H24A O24 H24B 119.3 . . ? C4 N1 H1 126.6 . . ? C5 N1 H1 126.6 . . ? C5 N1 C4 106.8(4) . . ? C5 N2 Co1 118.9(3) . . ? C5 N2 C6 105.4(4) . . ? C6 N2 Co1 132.8(3) . . ? C13 N3 H3 126.4 . . ? C14 N3 H3 126.4 . . ? C14 N3 C13 107.1(4) . . ? C14 N4 Co1 121.4(3) . 3_666 ? C14 N4 C15 105.1(4) . . ? C15 N4 Co1 131.0(3) . 3_666 ? O3 C1 Er2 50.7(2) . 2_755 ? O3 C1 C2 119.3(4) . . ? O4 C1 Er2 69.9(3) . 2_755 ? O4 C1 O3 120.6(4) . . ? O4 C1 C2 119.9(4) . . ? C2 C1 Er2 169.3(3) . 2_755 ? C3 C2 C1 116.8(4) . . ? C3 C2 C8 121.5(4) . . ? C8 C2 C1 121.6(4) . . ? C2 C3 H3A 121.5 . . ? C2 C3 C4 116.9(4) . . ? C4 C3 H3A 121.5 . . ? N1 C4 C6 106.4(4) . . ? C3 C4 N1 130.5(4) . . ? C3 C4 C6 123.1(4) . . ? N1 C5 H5 123.4 . . ? N2 C5 N1 113.2(4) . . ? N2 C5 H5 123.4 . . ? N2 C6 C4 108.3(4) . . ? N2 C6 C7 132.3(4) . . ? C7 C6 C4 119.3(4) . . ? C6 C7 H7 120.4 . . ? C8 C7 C6 119.1(4) . . ? C8 C7 H7 120.4 . . ? C2 C8 C9 119.5(4) . . ? C7 C8 C2 119.9(4) . . ? C7 C8 C9 120.0(4) . . ? O1 C9 O2 120.1(4) . . ? O1 C9 C8 121.6(4) . . ? O2 C9 C8 118.2(4) . . ? O5 C10 O6 119.5(4) . . ? O5 C10 C11 118.5(4) . . ? O6 C10 C11 121.8(4) . . ? C12 C11 C10 117.3(4) . . ? C12 C11 C17 121.0(4) . . ? C17 C11 C10 121.2(4) . . ? C11 C12 H12 121.4 . . ? C11 C12 C13 117.2(4) . . ? C13 C12 H12 121.4 . . ? N3 C13 C12 132.2(4) . . ? N3 C13 C15 105.6(4) . . ? C12 C13 C15 122.2(4) . . ? N3 C14 H14 123.5 . . ? N4 C14 N3 113.0(4) . . ? N4 C14 H14 123.5 . . ? N4 C15 C13 109.1(4) . . ? C16 C15 N4 130.3(4) . . ? C16 C15 C13 120.5(4) . . ? C15 C16 H16 120.7 . . ? C15 C16 C17 118.5(4) . . ? C17 C16 H16 120.7 . . ? C11 C17 C18 121.3(4) . 2_655 ? C16 C17 C11 120.3(4) . . ? C16 C17 C18 118.2(4) . 2_655 ? O7 C18 O8 122.4(4) . . ? O7 C18 C17 118.7(4) . 2_645 ? O8 C18 C17 118.8(4) . 2_645 ? 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 Er1 O1 C9 O2 -166.7(8) . . . . ? Er1 O1 C9 C8 16.5(13) . . . . ? Er1 O5 C10 O6 3.1(4) . . . . ? Er1 O5 C10 C11 -172.4(3) . . . . ? Er1 O6 C10 O5 -3.2(4) . . . . ? Er1 O6 C10 C11 172.1(3) . . . . ? Er1 O7 C18 O8 13.1(5) . . . . ? Er1 O7 C18 C17 -163.2(3) . . . 2_645 ? Er2 O1 C9 O2 3.0(4) . . . . ? Er2 O1 C9 C8 -173.8(4) . . . . ? Er2 O2 C9 O1 -3.5(5) . . . . ? Er2 O2 C9 C8 173.4(3) . . . . ? Er2 O3 C1 O4 0.0(4) 2_755 . . . ? Er2 O3 C1 C2 175.4(3) 2_755 . . . ? Er2 O4 C1 O3 0.0(4) 2_755 . . . ? Er2 O4 C1 C2 -175.4(4) 2_755 . . . ? Er2 O8 C18 O7 25(4) . . . . ? Er2 O8 C18 C17 -159(4) . . . 2_645 ? Er2 C1 C2 C3 -96.6(16) 2_755 . . . ? Er2 C1 C2 C8 80.1(16) 2_755 . . . ? Co1 N2 C5 N1 -162.4(3) . . . . ? Co1 N2 C6 C4 158.3(3) . . . . ? Co1 N2 C6 C7 -24.1(8) . . . . ? Co1 N4 C14 N3 162.4(3) 3_666 . . . ? Co1 N4 C15 C13 -160.1(3) 3_666 . . . ? Co1 N4 C15 C16 21.0(7) 3_666 . . . ? O1 Er1 O5 C10 51.7(3) . . . . ? O1 Er1 O6 C10 -146.3(2) . . . . ? O1 Er1 O7 C18 -16.5(3) . . . . ? O1 Er1 O9 S1 -52.6(3) . . . . ? O1 Er1 O13 S3 -16.3(2) . . . . ? O1 Er2 O2 C9 1.8(2) . . . . ? O1 Er2 O8 C18 -33(4) . . . . ? O1 Er2 O10 S1 60.6(3) . . . . ? O1 Er2 O14 S3 -62.0(3) . . . . ? O2 Er2 O1 Er1 175.08(18) . . . . ? O2 Er2 O1 C9 -1.8(2) . . . . ? O2 Er2 O8 C18 -37(4) . . . . ? O2 Er2 O10 S1 111.0(3) . . . . ? O2 Er2 O14 S3 -115.6(3) . . . . ? O3 Er2 O1 Er1 132.38(12) 2_745 . . . ? O3 Er2 O1 C9 -44.5(3) 2_745 . . . ? O3 Er2 O2 C9 148.7(3) 2_745 . . . ? O3 Er2 O8 C18 -163(4) 2_745 . . . ? O3 Er2 O10 S1 -174.6(2) 2_745 . . . ? O3 Er2 O14 S3 155.6(3) 2_745 . . . ? O3 C1 C2 C3 -116.1(5) . . . . ? O3 C1 C2 C8 60.6(6) . . . . ? O4 Er2 O1 Er1 66.23(15) 2_745 . . . ? O4 Er2 O1 C9 -110.6(3) 2_745 . . . ? O4 Er2 O2 C9 121.1(3) 2_745 . . . ? O4 Er2 O8 C18 -170(4) 2_745 . . . ? O4 Er2 O10 S1 -78.5(3) 2_745 . . . ? O4 Er2 O14 S3 103.0(3) 2_745 . . . ? O4 C1 C2 C3 59.3(6) . . . . ? O4 C1 C2 C8 -123.9(4) . . . . ? O5 Er1 O1 Er2 108.13(15) . . . . ? O5 Er1 O1 C9 -82.8(11) . . . . ? O5 Er1 O6 C10 1.8(2) . . . . ? O5 Er1 O7 C18 -155.0(3) . . . . ? O5 Er1 O9 S1 147.8(4) . . . . ? O5 Er1 O13 S3 174.12(18) . . . . ? O5 C10 C11 C12 95.5(5) . . . . ? O5 C10 C11 C17 -76.9(5) . . . . ? O6 Er1 O1 Er2 148.92(11) . . . . ? O6 Er1 O1 C9 -42.0(11) . . . . ? O6 Er1 O5 C10 -1.8(2) . . . . ? O6 Er1 O7 C18 -142.3(3) . . . . ? O6 Er1 O9 S1 -156.3(4) . . . . ? O6 Er1 O13 S3 72.4(3) . . . . ? O6 C10 C11 C12 -79.9(5) . . . . ? O6 C10 C11 C17 107.7(5) . . . . ? O7 Er1 O1 Er2 8.87(16) . . . . ? O7 Er1 O1 C9 177.9(10) . . . . ? O7 Er1 O5 C10 165.9(3) . . . . ? O7 Er1 O6 C10 -13.5(3) . . . . ? O7 Er1 O9 S1 69.4(3) . . . . ? O7 Er1 O13 S3 -136.3(3) . . . . ? O8 Er2 O1 Er1 -1.46(12) . . . . ? O8 Er2 O1 C9 -178.3(3) . . . . ? O8 Er2 O2 C9 6.4(3) . . . . ? O8 Er2 O10 S1 -22.5(3) . . . . ? O8 Er2 O14 S3 19.9(3) . . . . ? O9 Er1 O1 Er2 77.50(12) . . . . ? O9 Er1 O1 C9 -113.5(11) . . . . ? O9 Er1 O5 C10 82.2(3) . . . . ? O9 Er1 O6 C10 -77.3(2) . . . . ? O9 Er1 O7 C18 -80.6(3) . . . . ? O9 Er1 O13 S3 -72.0(3) . . . . ? O9 S1 O10 Er2 -38.1(3) . . . . ? O10 Er2 O1 Er1 -84.12(13) . . . . ? O10 Er2 O1 C9 99.0(3) . . . . ? O10 Er2 O2 C9 -65.4(3) . . . . ? O10 Er2 O8 C18 38(4) . . . . ? O10 Er2 O14 S3 -47.9(3) . . . . ? O10 S1 O9 Er1 28.1(4) . . . . ? O11 S1 O9 Er1 146.0(3) . . . . ? O11 S1 O10 Er2 -156.7(2) . . . . ? O12 S1 O9 Er1 -94.8(3) . . . . ? O12 S1 O10 Er2 83.2(3) . . . . ? O13 Er1 O1 Er2 -61.49(11) . . . . ? O13 Er1 O1 C9 107.6(11) . . . . ? O13 Er1 O5 C10 -144.2(2) . . . . ? O13 Er1 O6 C10 129.8(3) . . . . ? O13 Er1 O7 C18 55.6(3) . . . . ? O13 Er1 O9 S1 6.2(4) . . . . ? O13 S3 O14 Er2 8.2(3) . . . . ? O14 Er2 O1 Er1 85.47(13) . . . . ? O14 Er2 O1 C9 -91.4(3) . . . . ? O14 Er2 O2 C9 74.3(3) . . . . ? O14 Er2 O8 C18 -101(4) . . . . ? O14 Er2 O10 S1 46.7(3) . . . . ? O14 S3 O13 Er1 52.2(3) . . . . ? O15 S3 O13 Er1 -68.0(3) . . . . ? O15 S3 O14 Er2 128.3(3) . . . . ? O16 S3 O13 Er1 172.3(2) . . . . ? O16 S3 O14 Er2 -112.4(3) . . . . ? O17 Er1 O1 Er2 -110.33(18) . . . . ? O17 Er1 O1 C9 58.7(11) . . . . ? O17 Er1 O5 C10 -106.7(3) . . . . ? O17 Er1 O6 C10 66.8(3) . . . . ? O17 Er1 O7 C18 134.2(3) . . . . ? O17 Er1 O9 S1 134.3(3) . . . . ? O17 Er1 O13 S3 138.3(2) . . . . ? O18 Er1 O1 Er2 -136.90(14) . . . . ? O18 Er1 O1 C9 32.1(10) . . . . ? O18 Er1 O5 C10 -48.0(3) . . . . ? O18 Er1 O6 C10 140.5(3) . . . . ? O18 Er1 O7 C18 87.2(3) . . . . ? O18 Er1 O9 S1 -101.3(3) . . . . ? O18 Er1 O13 S3 61.6(2) . . . . ? O19 Er2 O1 Er1 -56.0(2) . . . . ? O19 Er2 O1 C9 127.1(3) . . . . ? O19 Er2 O2 C9 -133.0(3) . . . . ? O19 Er2 O8 C18 120(4) . . . . ? O19 Er2 O10 S1 -104.0(3) . . . . ? O19 Er2 O14 S3 88.1(3) . . . . ? O20 Er2 O1 Er1 -146.09(11) . . . . ? O20 Er2 O1 C9 37.0(3) . . . . ? O20 Er2 O2 C9 -140.2(3) . . . . ? O20 Er2 O8 C18 81(4) . . . . ? O20 Er2 O10 S1 -177.6(3) . . . . ? O20 Er2 O14 S3 -162.2(2) . . . . ? O21 Co1 N2 C5 -38.0(3) . . . . ? O21 Co1 N2 C6 164.5(4) . . . . ? O22 Co1 N2 C5 -128.0(3) . . . . ? O22 Co1 N2 C6 74.6(4) . . . . ? O23 Co1 N2 C5 48.6(4) . . . . ? O23 Co1 N2 C6 -108.9(4) . . . . ? O24 Co1 N2 C5 134.4(3) . . . . ? O24 Co1 N2 C6 -23.0(4) . . . . ? N1 C4 C6 N2 1.5(5) . . . . ? N1 C4 C6 C7 -176.4(4) . . . . ? N2 C6 C7 C8 -178.6(4) . . . . ? N3 C13 C15 N4 -1.3(5) . . . . ? N3 C13 C15 C16 177.7(4) . . . . ? N4 Co1 N2 C5 -155(15) 3_666 . . . ? N4 Co1 N2 C6 47(15) 3_666 . . . ? N4 C15 C16 C17 179.2(4) . . . . ? C1 Er2 O1 Er1 101.52(16) 2_745 . . . ? C1 Er2 O1 C9 -75.4(3) 2_745 . . . ? C1 Er2 O2 C9 136.7(3) 2_745 . . . ? C1 Er2 O8 C18 -167(4) 2_745 . . . ? C1 Er2 O10 S1 -129.0(3) 2_745 . . . ? C1 Er2 O14 S3 130.1(3) 2_745 . . . ? C1 C2 C3 C4 176.4(4) . . . . ? C1 C2 C8 C7 -173.4(4) . . . . ? C1 C2 C8 C9 15.2(6) . . . . ? C2 C3 C4 N1 177.5(4) . . . . ? C2 C3 C4 C6 -3.3(7) . . . . ? C2 C8 C9 O1 -155.7(4) . . . . ? C2 C8 C9 O2 27.4(6) . . . . ? C3 C2 C8 C7 3.2(6) . . . . ? C3 C2 C8 C9 -168.2(4) . . . . ? C3 C4 C6 N2 -177.8(4) . . . . ? C3 C4 C6 C7 4.2(7) . . . . ? C4 N1 C5 N2 0.4(5) . . . . ? C4 C6 C7 C8 -1.2(6) . . . . ? C5 N1 C4 C3 178.1(5) . . . . ? C5 N1 C4 C6 -1.2(5) . . . . ? C5 N2 C6 C4 -1.3(5) . . . . ? C5 N2 C6 C7 176.3(5) . . . . ? C6 N2 C5 N1 0.6(5) . . . . ? C6 C7 C8 C2 -2.3(6) . . . . ? C6 C7 C8 C9 169.1(4) . . . . ? C7 C8 C9 O1 32.9(6) . . . . ? C7 C8 C9 O2 -144.0(4) . . . . ? C8 C2 C3 C4 -0.4(6) . . . . ? C10 C11 C12 C13 -174.0(4) . . . . ? C10 C11 C17 C16 170.1(4) . . . . ? C10 C11 C17 C18 -14.2(6) . . . 2_655 ? C11 C12 C13 N3 -177.8(4) . . . . ? C11 C12 C13 C15 4.6(7) . . . . ? C12 C11 C17 C16 -2.1(6) . . . . ? C12 C11 C17 C18 173.7(4) . . . 2_655 ? C12 C13 C15 N4 176.8(4) . . . . ? C12 C13 C15 C16 -4.1(7) . . . . ? C13 N3 C14 N4 0.8(5) . . . . ? C13 C15 C16 C17 0.4(7) . . . . ? C14 N3 C13 C12 -177.5(5) . . . . ? C14 N3 C13 C15 0.4(5) . . . . ? C14 N4 C15 C13 1.8(5) . . . . ? C14 N4 C15 C16 -177.1(5) . . . . ? C15 N4 C14 N3 -1.6(5) . . . . ? C15 C16 C17 C11 2.6(6) . . . . ? C15 C16 C17 C18 -173.3(4) . . . 2_655 ? C17 C11 C12 C13 -1.5(6) . . . . ? data_2 _database_code_depnum_ccdc_archive 'CCDC 888133' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co Eu2 N4 O24 S2' _chemical_formula_weight 1107.38 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.434(19) _cell_length_b 8.783(7) _cell_length_c 15.504(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.989(16) _cell_angle_gamma 90.00 _cell_volume 2988(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3522 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.88 _exptl_crystal_description 0 _exptl_crystal_colour 0 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 4.947 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3093 _exptl_absorpt_correction_T_max 0.4378 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14562 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3522 _reflns_number_gt 2687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0247P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3522 _refine_ls_number_parameters 271 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.904 _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 Eu1 Eu 0.747067(8) -0.14374(2) 0.383139(13) 0.02897(7) Uani 1 1 d U . . Co2 Co 0.5000 0.19972(8) 0.2500 0.02801(16) Uani 1 2 d SU . . S3 S 0.85034(4) -0.03513(11) 0.58621(6) 0.0316(2) Uani 1 1 d U . . O4 O 0.68810(14) -0.1476(3) 0.64209(19) 0.0472(8) Uani 1 1 d U . . O12 O 0.59502(11) 0.2139(3) 0.27355(17) 0.0363(6) Uani 1 1 d U . . H12A H 0.6057 0.3063 0.2830 0.054 Uiso 1 1 d R . . H12B H 0.6074 0.1814 0.2286 0.054 Uiso 1 1 d R . . O1 O 0.64651(13) 0.0694(3) 0.78293(18) 0.0477(8) Uani 1 1 d U . . O3 O 0.70284(12) -0.1212(3) 0.50635(19) 0.0468(8) Uani 1 1 d U . . O7' O 0.9134(5) -0.075(3) 0.6264(10) 0.028(3) Uani 0.47(5) 1 d PU A 2 C1 C 0.46234(16) 0.2922(4) 0.4174(2) 0.0301(8) Uani 1 1 d U . . H1 H 0.4277 0.3344 0.3819 0.036 Uiso 1 1 d R . . O5' O 0.8343(5) -0.100(3) 0.4942(7) 0.027(3) Uani 0.51(6) 1 d PU A 2 N2 N 0.47873(13) 0.3174(3) 0.5049(2) 0.0308(7) Uani 1 1 d U . . H2 H 0.4597 0.3732 0.5360 0.037 Uiso 1 1 d R . . O8 O 0.83102(13) 0.1171(3) 0.6029(2) 0.0496(8) Uani 1 1 d U A . O2 O 0.71292(12) 0.1827(4) 0.72274(19) 0.0565(9) Uani 1 1 d U . . N1 N 0.50032(13) 0.2019(3) 0.3866(2) 0.0287(7) Uani 1 1 d U . . C2 C 0.53186(15) 0.2359(4) 0.5354(2) 0.0274(8) Uani 1 1 d U . . C3 C 0.54461(16) 0.1621(4) 0.4615(2) 0.0274(8) Uani 1 1 d U A . C6 C 0.61838(16) 0.1252(4) 0.6279(2) 0.0268(8) Uani 1 1 d U . . C9 C 0.67703(18) -0.0805(5) 0.5688(3) 0.0371(9) Uani 1 1 d U . . O6' O 0.8102(9) -0.1332(14) 0.6418(9) 0.029(2) Uani 0.47(5) 1 d PU . 2 C4 C 0.59403(16) 0.0622(4) 0.4705(2) 0.0309(8) Uani 1 1 d U . . H4 H 0.6025 0.0101 0.4222 0.037 Uiso 1 1 d R A . C5 C 0.63011(15) 0.0427(4) 0.5546(2) 0.0282(8) Uani 1 1 d U A . C8 C 0.66190(17) 0.1227(4) 0.7163(3) 0.0290(8) Uani 1 1 d U . . O9 O 0.81846(14) -0.0205(3) 0.30396(18) 0.0499(8) Uani 1 1 d U A . H9A H 0.8148 0.0792 0.3049 0.075 Uiso 1 1 d R . . H9B H 0.8110 -0.0498 0.2485 0.075 Uiso 1 1 d R . . C7 C 0.56880(15) 0.2229(4) 0.6187(2) 0.0275(8) Uani 1 1 d U . . H7 H 0.5607 0.2773 0.6665 0.033 Uiso 1 1 d R . . O10' O 0.7328(3) 0.1354(6) 0.3713(4) 0.0327(15) Uani 0.499(5) 1 d PU A 1 H10' H 0.7596 0.1732 0.3462 0.049 Uiso 0.499(5) 1 d PR A 1 H10 H 0.7363 0.1741 0.4225 0.049 Uiso 0.499(5) 1 d PR A 1 O10 O 0.7437(3) 0.1188(7) 0.4245(4) 0.0404(18) Uani 0.499(5) 1 d PU A 2 H10B H 0.7186 0.1361 0.4638 0.061 Uiso 0.499(5) 1 d PR A 2 H10A H 0.7296 0.1819 0.3770 0.061 Uiso 0.499(5) 1 d PR A 2 O5 O 0.8337(5) -0.038(4) 0.4873(7) 0.026(3) Uani 0.49(6) 1 d PU A 1 O7 O 0.9197(5) -0.020(3) 0.6082(10) 0.031(3) Uani 0.53(5) 1 d PU A 1 O6 O 0.8290(9) -0.1525(15) 0.6283(8) 0.029(3) Uani 0.53(5) 1 d PU . 1 O13 O 0.5000 -0.0407(5) 0.2500 0.0717(15) Uani 1 2 d SU . . H13A H 0.4647 -0.0769 0.2376 0.086 Uiso 1 1 d R . . O11 O 0.5000 0.4389(4) 0.2500 0.0489(11) Uani 1 2 d SU . . H11A H 0.4792 0.4947 0.2122 0.059 Uiso 1 1 d 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 Eu1 0.02965(11) 0.03043(10) 0.02440(11) -0.00342(8) 0.00002(8) 0.00583(8) Co2 0.0280(4) 0.0276(3) 0.0269(4) 0.000 0.0023(3) 0.000 S3 0.0266(4) 0.0406(5) 0.0259(5) -0.0060(4) 0.0017(4) 0.0043(4) O4 0.065(2) 0.0424(16) 0.0280(16) -0.0060(13) -0.0056(15) 0.0290(14) O12 0.0331(14) 0.0430(15) 0.0327(16) 0.0026(13) 0.0064(12) 0.0038(12) O1 0.0609(19) 0.0531(18) 0.0257(15) 0.0047(14) 0.0012(14) -0.0272(15) O3 0.0333(15) 0.067(2) 0.0368(17) -0.0208(15) -0.0006(13) 0.0144(13) O7' 0.023(3) 0.033(6) 0.027(4) -0.003(4) 0.004(3) -0.001(3) C1 0.0266(18) 0.0336(19) 0.027(2) 0.0011(16) -0.0009(16) 0.0020(15) O5' 0.030(3) 0.025(8) 0.025(3) -0.003(4) 0.003(2) 0.005(4) N2 0.0290(16) 0.0309(16) 0.0305(18) -0.0014(14) 0.0016(14) 0.0052(13) O8 0.0386(16) 0.0299(15) 0.069(2) -0.0019(14) -0.0142(15) 0.0018(12) O2 0.0302(15) 0.113(3) 0.0255(16) 0.0071(17) 0.0036(13) -0.0167(16) N1 0.0264(15) 0.0310(15) 0.0266(17) -0.0006(13) 0.0005(13) 0.0020(13) C2 0.0260(18) 0.0266(18) 0.029(2) 0.0012(15) 0.0044(15) 0.0016(14) C3 0.0244(17) 0.0301(19) 0.0271(19) 0.0020(15) 0.0038(15) -0.0015(14) C6 0.0262(17) 0.0285(18) 0.0252(19) 0.0025(15) 0.0045(15) -0.0013(14) C9 0.036(2) 0.042(2) 0.028(2) -0.0119(19) -0.0040(17) 0.0088(18) O6' 0.030(5) 0.031(4) 0.028(4) 0.000(3) 0.013(4) -0.004(3) C4 0.0323(19) 0.034(2) 0.027(2) 0.0009(16) 0.0064(16) 0.0045(16) C5 0.0281(18) 0.0314(19) 0.0245(19) 0.0004(15) 0.0039(16) 0.0029(15) C8 0.0320(19) 0.0270(18) 0.029(2) -0.0025(15) 0.0087(16) 0.0061(15) O9 0.082(2) 0.0393(16) 0.0304(16) 0.0047(13) 0.0167(16) 0.0070(16) C7 0.0265(17) 0.0292(19) 0.027(2) -0.0024(15) 0.0057(15) -0.0006(14) O10' 0.041(3) 0.024(3) 0.031(3) -0.002(3) 0.003(3) -0.008(2) O10 0.040(3) 0.031(3) 0.050(4) 0.000(3) 0.007(3) 0.005(2) O5 0.028(3) 0.025(8) 0.022(3) -0.004(4) -0.001(3) -0.004(4) O7 0.028(3) 0.036(6) 0.029(4) -0.003(4) 0.003(3) 0.000(3) O6 0.032(6) 0.035(4) 0.019(4) -0.001(3) 0.003(3) -0.012(4) O13 0.126(4) 0.035(2) 0.070(3) 0.000 0.060(3) 0.000 O11 0.060(3) 0.029(2) 0.044(3) 0.000 -0.022(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6' 2.331(12) 7_646 ? Eu1 O3 2.337(3) . ? Eu1 O5' 2.355(10) . ? Eu1 O10 2.399(6) . ? Eu1 O4 2.421(3) 7_646 ? Eu1 O5 2.438(11) . ? Eu1 O6 2.454(12) 7_646 ? Eu1 O9 2.462(3) . ? Eu1 O2 2.469(3) 6 ? Eu1 O10' 2.474(6) . ? Eu1 O1 2.544(3) 6 ? Eu1 O3 2.768(3) 7_646 ? Co2 O12 2.090(3) . ? Co2 O12 2.090(3) 2_655 ? Co2 O11 2.101(4) . ? Co2 O13 2.112(4) . ? Co2 N1 2.117(3) 2_655 ? Co2 N1 2.117(3) . ? S3 O6 1.359(12) . ? S3 O8 1.446(3) . ? S3 O7' 1.466(10) . ? S3 O5 1.501(11) . ? S3 O5' 1.508(11) . ? S3 O7 1.528(12) . ? S3 O6' 1.618(18) . ? O4 C9 1.258(5) . ? O4 Eu1 2.421(3) 7_646 ? O1 C8 1.246(4) . ? O1 Eu1 2.544(3) 6_556 ? O3 C9 1.278(5) . ? O3 Eu1 2.768(3) 7_646 ? C1 N1 1.323(4) . ? C1 N2 1.348(5) . ? N2 C2 1.386(4) . ? O2 C8 1.245(5) . ? O2 Eu1 2.469(3) 6_556 ? N1 C3 1.406(5) . ? C2 C7 1.387(5) . ? C2 C3 1.397(5) . ? C3 C4 1.398(5) . ? C6 C7 1.388(5) . ? C6 C5 1.419(5) . ? C6 C8 1.508(5) . ? C9 C5 1.493(5) . ? C9 Eu1 2.965(4) 7_646 ? O6' Eu1 2.331(12) 7_646 ? C4 C5 1.395(5) . ? C8 Eu1 2.885(4) 6_556 ? O6 Eu1 2.454(12) 7_646 ? 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 O3 83.9(5) 7_646 . ? O6' Eu1 O5' 127.2(8) 7_646 . ? O3 Eu1 O5' 79.5(3) . . ? O6' Eu1 O10 143.6(6) 7_646 . ? O3 Eu1 O10 69.99(18) . . ? O5' Eu1 O10 73.5(7) . . ? O6' Eu1 O4 70.5(6) 7_646 7_646 ? O3 Eu1 O4 124.57(10) . 7_646 ? O5' Eu1 O4 78.8(5) . 7_646 ? O10 Eu1 O4 145.49(17) . 7_646 ? O6' Eu1 O5 140.0(8) 7_646 . ? O3 Eu1 O5 80.9(2) . . ? O5' Eu1 O5 13.19(19) . . ? O10 Eu1 O5 61.4(7) . . ? O4 Eu1 O5 88.4(6) 7_646 . ? O6' Eu1 O6 12.5(2) 7_646 7_646 ? O3 Eu1 O6 73.3(5) . 7_646 ? O5' Eu1 O6 129.2(7) . 7_646 ? O10 Eu1 O6 131.3(6) . 7_646 ? O4 Eu1 O6 82.5(6) 7_646 7_646 ? O5 Eu1 O6 140.6(6) . 7_646 ? O6' Eu1 O9 132.9(5) 7_646 . ? O3 Eu1 O9 143.25(10) . . ? O5' Eu1 O9 76.4(5) . . ? O10 Eu1 O9 76.74(18) . . ? O4 Eu1 O9 77.13(11) 7_646 . ? O5 Eu1 O9 69.6(4) . . ? O6 Eu1 O9 143.1(5) 7_646 . ? O6' Eu1 O2 70.8(4) 7_646 6 ? O3 Eu1 O2 137.69(10) . 6 ? O5' Eu1 O2 142.8(3) . 6 ? O10 Eu1 O2 112.46(18) . 6 ? O4 Eu1 O2 78.66(10) 7_646 6 ? O5 Eu1 O2 139.3(3) . 6 ? O6 Eu1 O2 76.2(3) 7_646 6 ? O9 Eu1 O2 69.91(11) . 6 ? O6' Eu1 O10' 139.6(5) 7_646 . ? O3 Eu1 O10' 84.61(16) . . ? O5' Eu1 O10' 88.2(7) . . ? O10 Eu1 O10' 19.35(18) . . ? O4 Eu1 O10' 144.19(17) 7_646 . ? O5 Eu1 O10' 75.2(8) . . ? O6 Eu1 O10' 129.8(5) 7_646 . ? O9 Eu1 O10' 67.38(16) . . ? O2 Eu1 O10' 93.13(16) 6 . ? O6' Eu1 O1 74.1(4) 7_646 6 ? O3 Eu1 O1 90.25(11) . 6 ? O5' Eu1 O1 154.4(7) . 6 ? O10 Eu1 O1 80.99(17) . 6 ? O4 Eu1 O1 125.57(10) 7_646 6 ? O5 Eu1 O1 142.2(7) . 6 ? O6 Eu1 O1 68.1(4) 7_646 6 ? O9 Eu1 O1 99.72(11) . 6 ? O2 Eu1 O1 50.97(9) 6 6 ? O10' Eu1 O1 67.40(15) . 6 ? O6' Eu1 O3 67.4(3) 7_646 7_646 ? O3 Eu1 O3 75.15(10) . 7_646 ? O5' Eu1 O3 60.0(8) . 7_646 ? O10 Eu1 O3 125.65(17) . 7_646 ? O4 Eu1 O3 49.85(10) 7_646 7_646 ? O5 Eu1 O3 73.1(7) . 7_646 ? O6 Eu1 O3 71.8(3) 7_646 7_646 ? O9 Eu1 O3 114.46(10) . 7_646 ? O2 Eu1 O3 121.41(10) 6 7_646 ? O10' Eu1 O3 144.54(15) . 7_646 ? O1 Eu1 O3 139.81(10) 6 7_646 ? O12 Co2 O12 173.17(15) . 2_655 ? O12 Co2 O11 86.58(8) . . ? O12 Co2 O11 86.58(8) 2_655 . ? O12 Co2 O13 93.42(8) . . ? O12 Co2 O13 93.42(8) 2_655 . ? O11 Co2 O13 180.000(1) . . ? O12 Co2 N1 88.03(11) . 2_655 ? O12 Co2 N1 91.91(11) 2_655 2_655 ? O11 Co2 N1 89.48(8) . 2_655 ? O13 Co2 N1 90.52(8) . 2_655 ? O12 Co2 N1 91.91(11) . . ? O12 Co2 N1 88.03(11) 2_655 . ? O11 Co2 N1 89.48(8) . . ? O13 Co2 N1 90.52(8) . . ? N1 Co2 N1 178.97(17) 2_655 . ? O6 S3 O8 117.9(11) . . ? O6 S3 O7' 91.0(5) . . ? O8 S3 O7' 116.4(7) . . ? O6 S3 O5 116.1(11) . . ? O8 S3 O5 100.3(12) . . ? O7' S3 O5 116.3(8) . . ? O6 S3 O5' 97.3(13) . . ? O8 S3 O5' 119.9(10) . . ? O7' S3 O5' 109.3(6) . . ? O5 S3 O5' 21.3(3) . . ? O6 S3 O7 113.6(5) . . ? O8 S3 O7 102.2(7) . . ? O7' S3 O7 22.6(3) . . ? O5 S3 O7 104.7(7) . . ? O5' S3 O7 105.9(5) . . ? O6 S3 O6' 18.2(7) . . ? O8 S3 O6' 100.1(7) . . ? O7' S3 O6' 103.9(7) . . ? O5 S3 O6' 119.2(8) . . ? O5' S3 O6' 104.6(11) . . ? O7 S3 O6' 125.4(7) . . ? C9 O4 Eu1 102.8(2) . 7_646 ? C8 O1 Eu1 92.7(2) . 6_556 ? C9 O3 Eu1 168.3(3) . . ? C9 O3 Eu1 86.0(2) . 7_646 ? Eu1 O3 Eu1 104.85(10) . 7_646 ? N1 C1 N2 113.6(3) . . ? S3 O5' Eu1 138.7(6) . . ? C1 N2 C2 107.1(3) . . ? C8 O2 Eu1 96.3(2) . 6_556 ? C1 N1 C3 104.4(3) . . ? C1 N1 Co2 119.9(3) . . ? C3 N1 Co2 132.7(2) . . ? N2 C2 C7 131.7(3) . . ? N2 C2 C3 105.6(3) . . ? C7 C2 C3 122.8(3) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 N1 109.4(3) . . ? C4 C3 N1 130.4(3) . . ? C7 C6 C5 120.7(3) . . ? C7 C6 C8 117.2(3) . . ? C5 C6 C8 121.8(3) . . ? O4 C9 O3 121.2(4) . . ? O4 C9 C5 118.3(3) . . ? O3 C9 C5 120.5(4) . . ? O4 C9 Eu1 52.77(19) . 7_646 ? O3 C9 Eu1 68.6(2) . 7_646 ? C5 C9 Eu1 168.2(3) . 7_646 ? S3 O6' Eu1 135.0(9) . 7_646 ? C5 C4 C3 117.7(3) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 C9 118.8(3) . . ? C6 C5 C9 119.6(3) . . ? O2 C8 O1 120.1(4) . . ? O2 C8 C6 118.5(3) . . ? O1 C8 C6 121.3(3) . . ? O2 C8 Eu1 58.3(2) . 6_556 ? O1 C8 Eu1 61.8(2) . 6_556 ? C6 C8 Eu1 175.3(2) . 6_556 ? C2 C7 C6 117.3(3) . . ? S3 O5 Eu1 132.6(9) . . ? S3 O6 Eu1 145.8(6) . 7_646 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.824 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.123 data_3 _database_code_depnum_ccdc_archive 'CCDC 888134' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co Gd2 N4 O24 S2' _chemical_formula_weight 1117.96 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' Co Co 0.3494 0.9721 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.527(4) _cell_length_b 8.7652(18) _cell_length_c 15.549(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.57(3) _cell_angle_gamma 90.00 _cell_volume 2996.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2639 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 25.00 _exptl_crystal_description 0 _exptl_crystal_colour 0 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2156 _exptl_absorpt_coefficient_mu 5.173 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2722 _exptl_absorpt_correction_T_max 0.4734 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8304 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2639 _reflns_number_gt 2176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0186P)^2^+13.7408P] 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 NONE _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2639 _refine_ls_number_parameters 232 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.163 _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 O4 O 0.70377(16) -0.1150(5) 0.5041(2) 0.0375(11) Uani 1 1 d . . . O3 O 0.68944(17) -0.1494(5) 0.6393(2) 0.0383(11) Uani 1 1 d . . . C9 C 0.6781(2) -0.0770(6) 0.5657(3) 0.0292(15) Uani 1 1 d . . . Gd1 Gd 0.747347(12) 0.14123(3) 0.883282(17) 0.02754(7) Uani 1 1 d . . . Co Co 0.5000 0.20357(14) 0.2500 0.0368(3) Uani 1 2 d S . . S1 S 0.64867(6) 0.45747(17) 0.91371(9) 0.0308(4) Uani 1 1 d . . . O1 O 0.64709(19) 0.0624(5) 0.7809(2) 0.0492(13) Uani 1 1 d . . . O2 O 0.71295(17) 0.1834(5) 0.7228(2) 0.0395(12) Uani 1 1 d . . . O5 O 0.67977(18) 0.3501(5) 0.8668(2) 0.0462(12) Uani 1 1 d . . . O8 O 0.66460(17) 0.4241(5) 1.0088(2) 0.0368(11) Uani 1 1 d . . . O6 O 0.66753(19) 0.6118(5) 0.8967(3) 0.0522(14) Uani 1 1 d . . . O7 O 0.58269(17) 0.4423(5) 0.8827(3) 0.0473(13) Uani 1 1 d . . . O9 O 0.59439(18) 0.2183(5) 0.2733(2) 0.0447(12) Uani 1 1 d D . . H9B H 0.6019 0.1234 0.2718 0.054 Uiso 1 1 d RD . . H9A H 0.6204 0.2626 0.3128 0.054 Uiso 1 1 d RD . . O10 O 0.5000 0.4428(7) 0.2500 0.064(2) Uani 1 2 d S . . H10 H 0.4736 0.4939 0.2116 0.076 Uiso 1 1 d R . . N1 N 0.5005(2) 0.2031(6) 0.3860(3) 0.0385(14) Uani 1 1 d . . . N2 N 0.4796(2) 0.3157(5) 0.5045(3) 0.0365(14) Uani 1 1 d . . . H2 H 0.4610 0.3715 0.5357 0.044 Uiso 1 1 calc R . . C1 C 0.4628(3) 0.2919(7) 0.4167(4) 0.0406(17) Uani 1 1 d . . . H1 H 0.4281 0.3342 0.3814 0.049 Uiso 1 1 calc R . . C2 C 0.5314(2) 0.2347(7) 0.5339(4) 0.0359(16) Uani 1 1 d . . . C3 C 0.5442(3) 0.1612(7) 0.4596(3) 0.0343(16) Uani 1 1 d . . . C4 C 0.5946(3) 0.0644(7) 0.4695(4) 0.0360(16) Uani 1 1 d . . . H4 H 0.6036 0.0152 0.4208 0.043 Uiso 1 1 calc R . . C5 C 0.5694(2) 0.2202(7) 0.6173(3) 0.0336(15) Uani 1 1 d . . . H5 H 0.5617 0.2738 0.6653 0.040 Uiso 1 1 calc R . . C6 C 0.6189(2) 0.1236(7) 0.6263(3) 0.0299(14) Uani 1 1 d . . . C7 C 0.6308(2) 0.0426(6) 0.5527(3) 0.0258(14) Uani 1 1 d . . . C8 C 0.6622(3) 0.1193(6) 0.7152(4) 0.0331(15) Uani 1 1 d . . . O11 O 0.5000 -0.0397(8) 0.2500 0.079(2) Uani 1 2 d SD . . H11 H 0.5316 -0.0940 0.2634 0.094 Uiso 1 1 d RD . . O12 O 0.81797(19) 0.0281(5) 0.7994(3) 0.0500(13) Uani 1 1 d D . . H12A H 0.8317 0.0635 0.7568 0.060 Uiso 1 1 d RD . . H12B H 0.8469 -0.0090 0.8382 0.060 Uiso 1 1 d RD . . O13 O 0.74024(19) -0.1327(5) 0.8938(3) 0.0649(15) Uani 1 1 d . . . H13A H 0.7560 -0.1831 0.8694 0.078 Uiso 1 1 d R . . H13B H 0.7248 -0.1706 0.9303 0.078 Uiso 1 1 d 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 O4 0.033(2) 0.050(3) 0.0302(19) -0.0023(19) 0.0095(16) 0.0056(19) O3 0.050(2) 0.037(2) 0.0257(18) 0.0010(19) 0.0027(17) 0.012(2) C9 0.027(3) 0.029(3) 0.029(3) -0.005(3) 0.001(2) -0.005(3) Gd1 0.02861(13) 0.03055(14) 0.02272(12) 0.00026(14) 0.00398(10) -0.00119(15) Co 0.0387(6) 0.0391(7) 0.0288(6) 0.000 -0.0005(5) 0.000 S1 0.0291(7) 0.0337(8) 0.0284(7) 0.0040(6) 0.0038(6) 0.0000(7) O1 0.060(3) 0.061(3) 0.026(2) 0.001(2) 0.007(2) -0.020(2) O2 0.035(2) 0.059(3) 0.0229(18) -0.0045(19) 0.0029(17) -0.002(2) O5 0.047(2) 0.057(3) 0.030(2) -0.007(2) -0.0025(19) 0.016(2) O8 0.037(2) 0.047(2) 0.0254(19) 0.0031(18) 0.0048(17) 0.004(2) O6 0.055(3) 0.036(3) 0.057(3) 0.011(2) -0.005(2) -0.008(2) O7 0.030(2) 0.069(3) 0.040(2) 0.016(2) -0.0006(19) -0.003(2) O9 0.045(2) 0.043(3) 0.041(2) -0.005(2) -0.004(2) 0.002(2) O10 0.081(5) 0.034(4) 0.053(4) 0.000 -0.036(4) 0.000 N1 0.034(3) 0.052(3) 0.028(2) 0.000(2) 0.004(2) 0.007(3) N2 0.034(2) 0.041(3) 0.035(2) -0.007(2) 0.008(2) 0.011(2) C1 0.039(3) 0.045(4) 0.035(3) 0.006(3) 0.001(3) 0.007(3) C2 0.032(3) 0.036(4) 0.039(3) -0.003(3) 0.006(3) 0.006(3) C3 0.037(3) 0.035(4) 0.028(3) -0.004(3) 0.001(2) 0.001(3) C4 0.043(3) 0.037(4) 0.028(3) 0.000(3) 0.008(3) 0.007(3) C5 0.034(3) 0.040(4) 0.029(3) -0.006(3) 0.011(2) 0.012(3) C6 0.030(3) 0.034(3) 0.024(3) 0.000(3) 0.003(2) -0.002(3) C7 0.026(3) 0.026(3) 0.027(3) 0.002(2) 0.008(2) 0.002(2) C8 0.041(3) 0.026(3) 0.032(3) -0.009(3) 0.008(3) 0.008(3) O11 0.118(6) 0.047(4) 0.083(5) 0.000 0.048(4) 0.000 O12 0.065(3) 0.053(3) 0.031(2) 0.001(2) 0.009(2) 0.018(2) O13 0.065(3) 0.033(2) 0.106(4) 0.000(3) 0.038(3) 0.005(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 O4 C9 1.266(6) . ? O4 Gd1 2.313(4) 6 ? O4 Gd1 2.829(4) 4_646 ? O3 C9 1.285(6) . ? O3 Gd1 2.395(4) 4_646 ? C9 C7 1.476(7) . ? C9 Gd1 2.995(6) 4_646 ? Gd1 O4 2.313(4) 6_556 ? Gd1 O5 2.359(4) . ? Gd1 O8 2.373(4) 7_657 ? Gd1 O3 2.395(4) 4_656 ? Gd1 O13 2.414(4) . ? Gd1 O12 2.473(4) . ? Gd1 O2 2.475(3) . ? Gd1 O1 2.559(4) . ? Gd1 O4 2.829(4) 4_656 ? Gd1 C9 2.995(6) 4_656 ? Gd1 Gd1 4.0787(8) 7_657 ? Co O9 2.082(4) . ? Co O9 2.082(4) 2_655 ? Co O10 2.097(6) . ? Co N1 2.112(4) 2_655 ? Co N1 2.112(4) . ? Co O11 2.133(7) . ? S1 O6 1.459(4) . ? S1 O5 1.460(4) . ? S1 O7 1.466(4) . ? S1 O8 1.472(4) . ? O1 C8 1.248(7) . ? O2 C8 1.256(7) . ? O8 Gd1 2.373(4) 7_657 ? O9 H9B 0.8501 . ? O9 H9A 0.8452 . ? O10 H10 0.8694 . ? N1 C1 1.316(8) . ? N1 C3 1.387(7) . ? N2 C1 1.351(7) . ? N2 C2 1.358(7) . ? N2 H2 0.8600 . ? C1 H1 0.9300 . ? C2 C5 1.396(7) . ? C2 C3 1.407(8) . ? C3 C4 1.398(8) . ? C4 C7 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.382(8) . ? C5 H5 0.9300 . ? C6 C7 1.422(7) . ? C6 C8 1.510(7) . ? O11 H11 0.8442 . ? O12 H12A 0.8488 . ? O12 H12B 0.8502 . ? O13 H13A 0.7244 . ? O13 H13B 0.7987 . ? 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 C9 O4 Gd1 170.0(4) . 6 ? C9 O4 Gd1 84.9(3) . 4_646 ? Gd1 O4 Gd1 104.52(13) 6 4_646 ? C9 O3 Gd1 104.9(3) . 4_646 ? O4 C9 O3 120.5(5) . . ? O4 C9 C7 121.1(5) . . ? O3 C9 C7 118.1(5) . . ? O4 C9 Gd1 70.2(3) . 4_646 ? O3 C9 Gd1 50.6(3) . 4_646 ? C7 C9 Gd1 165.5(4) . 4_646 ? O4 Gd1 O5 77.75(14) 6_556 . ? O4 Gd1 O8 80.71(13) 6_556 7_657 ? O5 Gd1 O8 133.20(13) . 7_657 ? O4 Gd1 O3 124.49(13) 6_556 4_656 ? O5 Gd1 O3 77.27(14) . 4_656 ? O8 Gd1 O3 81.74(13) 7_657 4_656 ? O4 Gd1 O13 78.45(15) 6_556 . ? O5 Gd1 O13 136.76(15) . . ? O8 Gd1 O13 76.68(14) 7_657 . ? O3 Gd1 O13 145.31(14) 4_656 . ? O4 Gd1 O12 145.46(14) 6_556 . ? O5 Gd1 O12 136.69(14) . . ? O8 Gd1 O12 75.02(13) 7_657 . ? O3 Gd1 O12 76.03(14) 4_656 . ? O13 Gd1 O12 72.35(15) . . ? O4 Gd1 O2 137.65(12) 6_556 . ? O5 Gd1 O2 73.82(13) . . ? O8 Gd1 O2 141.22(13) 7_657 . ? O3 Gd1 O2 78.66(12) 4_656 . ? O13 Gd1 O2 101.90(15) . . ? O12 Gd1 O2 67.94(13) . . ? O4 Gd1 O1 90.32(13) 6_556 . ? O5 Gd1 O1 71.39(14) . . ? O8 Gd1 O1 149.73(14) 7_657 . ? O3 Gd1 O1 126.03(13) 4_656 . ? O13 Gd1 O1 73.20(14) . . ? O12 Gd1 O1 98.37(14) . . ? O2 Gd1 O1 51.14(13) . . ? O4 Gd1 O4 75.48(14) 6_556 4_656 ? O5 Gd1 O4 68.66(12) . 4_656 ? O8 Gd1 O4 65.91(12) 7_657 4_656 ? O3 Gd1 O4 49.32(11) 4_656 4_656 ? O13 Gd1 O4 137.04(14) . 4_656 ? O12 Gd1 O4 114.87(12) . 4_656 ? O2 Gd1 O4 120.36(12) . 4_656 ? O1 Gd1 O4 139.55(13) . 4_656 ? O4 Gd1 C9 100.35(14) 6_556 4_656 ? O5 Gd1 C9 72.55(15) . 4_656 ? O8 Gd1 C9 71.18(14) 7_657 4_656 ? O3 Gd1 C9 24.48(13) 4_656 4_656 ? O13 Gd1 C9 147.54(14) . 4_656 ? O12 Gd1 C9 94.71(15) . 4_656 ? O2 Gd1 C9 100.27(14) . 4_656 ? O1 Gd1 C9 139.08(14) . 4_656 ? O4 Gd1 C9 24.91(12) 4_656 4_656 ? O4 Gd1 Gd1 42.19(10) 6_556 7_657 ? O5 Gd1 Gd1 68.11(9) . 7_657 ? O8 Gd1 Gd1 67.99(9) 7_657 7_657 ? O3 Gd1 Gd1 82.47(9) 4_656 7_657 ? O13 Gd1 Gd1 113.21(12) . 7_657 ? O12 Gd1 Gd1 139.37(10) . 7_657 ? O2 Gd1 Gd1 140.33(10) . 7_657 ? O1 Gd1 Gd1 122.08(10) . 7_657 ? O4 Gd1 Gd1 33.30(7) 4_656 7_657 ? C9 Gd1 Gd1 58.18(11) 4_656 7_657 ? O9 Co O9 172.9(2) . 2_655 ? O9 Co O10 86.45(12) . . ? O9 Co O10 86.45(12) 2_655 . ? O9 Co N1 87.55(17) . 2_655 ? O9 Co N1 92.46(17) 2_655 2_655 ? O10 Co N1 90.11(14) . 2_655 ? O9 Co N1 92.46(17) . . ? O9 Co N1 87.55(17) 2_655 . ? O10 Co N1 90.11(14) . . ? N1 Co N1 179.8(3) 2_655 . ? O9 Co O11 93.55(12) . . ? O9 Co O11 93.55(12) 2_655 . ? O10 Co O11 180.000(1) . . ? N1 Co O11 89.89(14) 2_655 . ? N1 Co O11 89.89(14) . . ? O6 S1 O5 108.5(3) . . ? O6 S1 O7 109.8(3) . . ? O5 S1 O7 109.9(3) . . ? O6 S1 O8 110.4(2) . . ? O5 S1 O8 109.6(2) . . ? O7 S1 O8 108.7(2) . . ? C8 O1 Gd1 92.3(3) . . ? C8 O2 Gd1 96.1(3) . . ? S1 O5 Gd1 144.5(2) . . ? S1 O8 Gd1 137.9(2) . 7_657 ? Co O9 H9B 97.9 . . ? Co O9 H9A 132.5 . . ? H9B O9 H9A 111.0 . . ? Co O10 H10 121.0 . . ? C1 N1 C3 104.8(5) . . ? C1 N1 Co 119.9(4) . . ? C3 N1 Co 132.4(4) . . ? C1 N2 C2 106.9(5) . . ? C1 N2 H2 126.5 . . ? C2 N2 H2 126.5 . . ? N1 C1 N2 113.4(5) . . ? N1 C1 H1 123.3 . . ? N2 C1 H1 123.3 . . ? N2 C2 C5 132.0(5) . . ? N2 C2 C3 106.1(5) . . ? C5 C2 C3 121.9(5) . . ? N1 C3 C4 131.7(5) . . ? N1 C3 C2 108.7(5) . . ? C4 C3 C2 119.6(5) . . ? C7 C4 C3 119.1(5) . . ? C7 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C2 117.9(5) . . ? C6 C5 H5 121.1 . . ? C2 C5 H5 121.1 . . ? C5 C6 C7 120.9(5) . . ? C5 C6 C8 117.0(5) . . ? C7 C6 C8 121.8(5) . . ? C4 C7 C6 120.5(5) . . ? C4 C7 C9 119.2(5) . . ? C6 C7 C9 120.1(4) . . ? O1 C8 O2 120.5(5) . . ? O1 C8 C6 121.4(5) . . ? O2 C8 C6 117.9(5) . . ? Co O11 H11 124.3 . . ? Gd1 O12 H12A 130.6 . . ? Gd1 O12 H12B 105.2 . . ? H12A O12 H12B 109.8 . . ? Gd1 O13 H13A 121.6 . . ? Gd1 O13 H13B 120.5 . . ? H13A O13 H13B 117.2 . . ? 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 Gd1 O4 C9 O3 -156.2(16) 6 . . . ? Gd1 O4 C9 O3 5.0(5) 4_646 . . . ? Gd1 O4 C9 C7 29(2) 6 . . . ? Gd1 O4 C9 C7 -169.9(5) 4_646 . . . ? Gd1 O4 C9 Gd1 -161(2) 6 . . 4_646 ? Gd1 O3 C9 O4 -6.1(6) 4_646 . . . ? Gd1 O3 C9 C7 169.0(4) 4_646 . . . ? O4 Gd1 O1 C8 160.8(3) 6_556 . . . ? O5 Gd1 O1 C8 83.8(3) . . . . ? O8 Gd1 O1 C8 -127.3(4) 7_657 . . . ? O3 Gd1 O1 C8 26.0(4) 4_656 . . . ? O13 Gd1 O1 C8 -121.4(4) . . . . ? O12 Gd1 O1 C8 -52.8(4) . . . . ? O2 Gd1 O1 C8 -0.1(3) . . . . ? O4 Gd1 O1 C8 93.1(4) 4_656 . . . ? C9 Gd1 O1 C8 54.5(4) 4_656 . . . ? Gd1 Gd1 O1 C8 131.3(3) 7_657 . . . ? O4 Gd1 O2 C8 -29.1(4) 6_556 . . . ? O5 Gd1 O2 C8 -78.8(3) . . . . ? O8 Gd1 O2 C8 140.2(3) 7_657 . . . ? O3 Gd1 O2 C8 -158.7(3) 4_656 . . . ? O13 Gd1 O2 C8 56.8(3) . . . . ? O12 Gd1 O2 C8 122.0(4) . . . . ? O1 Gd1 O2 C8 0.1(3) . . . . ? O4 Gd1 O2 C8 -131.3(3) 4_656 . . . ? C9 Gd1 O2 C8 -147.1(3) 4_656 . . . ? Gd1 Gd1 O2 C8 -95.5(3) 7_657 . . . ? O6 S1 O5 Gd1 120.0(4) . . . . ? O7 S1 O5 Gd1 -120.0(4) . . . . ? O8 S1 O5 Gd1 -0.6(5) . . . . ? O4 Gd1 O5 S1 27.3(4) 6_556 . . . ? O8 Gd1 O5 S1 -37.2(6) 7_657 . . . ? O3 Gd1 O5 S1 -102.7(5) 4_656 . . . ? O13 Gd1 O5 S1 85.3(5) . . . . ? O12 Gd1 O5 S1 -155.8(4) . . . . ? O2 Gd1 O5 S1 175.6(5) . . . . ? O1 Gd1 O5 S1 121.9(5) . . . . ? O4 Gd1 O5 S1 -51.7(4) 4_656 . . . ? C9 Gd1 O5 S1 -77.8(5) 4_656 . . . ? Gd1 Gd1 O5 S1 -15.8(4) 7_657 . . . ? O6 S1 O8 Gd1 -77.3(4) . . . 7_657 ? O5 S1 O8 Gd1 42.1(4) . . . 7_657 ? O7 S1 O8 Gd1 162.2(3) . . . 7_657 ? O9 Co N1 C1 133.3(5) . . . . ? O9 Co N1 C1 -39.6(5) 2_655 . . . ? O10 Co N1 C1 46.8(5) . . . . ? N1 Co N1 C1 -133.2(5) 2_655 . . . ? O11 Co N1 C1 -133.2(5) . . . . ? O9 Co N1 C3 -24.5(6) . . . . ? O9 Co N1 C3 162.7(5) 2_655 . . . ? O10 Co N1 C3 -110.9(5) . . . . ? N1 Co N1 C3 69.1(7) 2_655 . . . ? O11 Co N1 C3 69.1(5) . . . . ? C3 N1 C1 N2 2.1(7) . . . . ? Co N1 C1 N2 -161.1(4) . . . . ? C2 N2 C1 N1 -1.1(7) . . . . ? C1 N2 C2 C5 178.0(7) . . . . ? C1 N2 C2 C3 -0.4(7) . . . . ? C1 N1 C3 C4 177.4(7) . . . . ? Co N1 C3 C4 -22.4(10) . . . . ? C1 N1 C3 C2 -2.3(7) . . . . ? Co N1 C3 C2 157.9(4) . . . . ? N2 C2 C3 N1 1.7(7) . . . . ? C5 C2 C3 N1 -176.9(6) . . . . ? N2 C2 C3 C4 -178.1(5) . . . . ? C5 C2 C3 C4 3.3(9) . . . . ? N1 C3 C4 C7 -179.6(6) . . . . ? C2 C3 C4 C7 0.1(9) . . . . ? N2 C2 C5 C6 178.2(6) . . . . ? C3 C2 C5 C6 -3.6(9) . . . . ? C2 C5 C6 C7 0.5(9) . . . . ? C2 C5 C6 C8 175.1(5) . . . . ? C3 C4 C7 C6 -3.1(9) . . . . ? C3 C4 C7 C9 170.6(5) . . . . ? C5 C6 C7 C4 2.9(9) . . . . ? C8 C6 C7 C4 -171.5(5) . . . . ? C5 C6 C7 C9 -170.8(5) . . . . ? C8 C6 C7 C9 14.9(8) . . . . ? O4 C9 C7 C4 29.8(8) . . . . ? O3 C9 C7 C4 -145.3(5) . . . . ? Gd1 C9 C7 C4 -109.2(14) 4_646 . . . ? O4 C9 C7 C6 -156.4(5) . . . . ? O3 C9 C7 C6 28.5(8) . . . . ? Gd1 C9 C7 C6 64.6(16) 4_646 . . . ? Gd1 O1 C8 O2 0.1(6) . . . . ? Gd1 O1 C8 C6 -175.4(5) . . . . ? Gd1 O2 C8 O1 -0.1(6) . . . . ? Gd1 O2 C8 C6 175.5(4) . . . . ? C5 C6 C8 O1 69.5(8) . . . . ? C7 C6 C8 O1 -116.0(6) . . . . ? C5 C6 C8 O2 -106.2(6) . . . . ? C7 C6 C8 O2 68.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.832 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.144 data_6 _database_code_depnum_ccdc_archive 'CCDC 888135' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co Ho2 N4 O24 S2' _chemical_formula_weight 1133.32 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.4616(18) _cell_length_b 8.7319(7) _cell_length_c 15.4580(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.7840(10) _cell_angle_gamma 90.00 _cell_volume 2956.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2937 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.10 _exptl_crystal_description 0 _exptl_crystal_colour 0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2180 _exptl_absorpt_coefficient_mu 6.109 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3218 _exptl_absorpt_correction_T_max 0.4610 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7989 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.10 _reflns_number_total 2937 _reflns_number_gt 2681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0250P)^2^+0.6932P] 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 NONE _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2937 _refine_ls_number_parameters 243 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0458 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.004 _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 O2 O 0.69051(12) 0.3474(3) 0.63675(16) 0.0302(6) Uani 1 1 d . . . O1 O 0.70453(11) 0.3877(3) 0.50192(16) 0.0290(6) Uani 1 1 d . . . C9 C 0.67885(15) 0.4212(4) 0.5644(2) 0.0224(7) Uani 1 1 d . . . Co2 Co 0.5000 0.70589(8) 0.2500 0.02705(16) Uani 1 2 d S . . Ho1 Ho 0.747696(7) 0.639800(17) 0.883190(9) 0.01978(6) Uani 1 1 d . . . S5 S 0.65010(4) 0.95333(10) 0.91349(5) 0.02285(18) Uani 1 1 d . . . O3 O 0.71408(11) 0.6838(3) 0.72378(15) 0.0328(6) Uani 1 1 d . . . O5 O 0.68017(13) 0.8437(3) 0.86531(17) 0.0387(7) Uani 1 1 d . . . O6 O 0.66550(10) 0.9205(3) 1.00916(15) 0.0296(6) Uani 1 1 d . . . O7 O 0.66950(14) 1.1072(3) 0.8967(2) 0.0463(8) Uani 1 1 d . . . O8 O 0.58392(11) 0.9407(3) 0.88181(16) 0.0415(7) Uani 1 1 d . . . O9 O 0.81824(14) 0.5291(3) 0.80229(18) 0.0430(7) Uani 1 1 d D . . H9B H 0.8311(19) 0.439(2) 0.816(2) 0.050 Uiso 1 1 d D . . H9A H 0.8091(19) 0.537(4) 0.7463(8) 0.050 Uiso 1 1 d D . . O10 O 0.74148(15) 0.3683(3) 0.8964(3) 0.0614(10) Uani 1 1 d . . . H10A H 0.7627 0.3394 0.9478 0.092 Uiso 1 1 d R . . H10B H 0.7560 0.3230 0.8554 0.092 Uiso 1 1 d R . . O11 O 0.59555(11) 0.7193(3) 0.27447(16) 0.0355(6) Uani 1 1 d . . . H11A H 0.6123 0.6279 0.2788 0.053 Uiso 1 1 d R . . H11B H 0.6101 0.7679 0.3243 0.053 Uiso 1 1 d R . . O12 O 0.5000 0.4599(5) 0.2500 0.0692(15) Uani 1 2 d SD . . H12 H 0.4650 0.4215 0.2320 0.104 Uiso 1 1 d RD . . O13 O 0.5000 0.9446(4) 0.2500 0.0556(13) Uani 1 2 d SD . . H13 H 0.5194(17) 1.004(4) 0.289(2) 0.050 Uiso 1 1 d D . . N1 N 0.50045(13) 0.7045(4) 0.38616(19) 0.0297(7) Uani 1 1 d . . . N2 N 0.47934(14) 0.8147(4) 0.5052(2) 0.0323(7) Uani 1 1 d . . . H2 H 0.4603 0.8689 0.5369 0.039 Uiso 1 1 calc R . . C1 C 0.46304(17) 0.7938(5) 0.4182(2) 0.0349(9) Uani 1 1 d . . . H1 H 0.4284 0.8381 0.3830 0.042 Uiso 1 1 calc R . . C2 C 0.53242(15) 0.7335(4) 0.5354(2) 0.0258(7) Uani 1 1 d . . . C3 C 0.54519(16) 0.6624(4) 0.4603(2) 0.0249(7) Uani 1 1 d . . . C4 C 0.59479(15) 0.5653(4) 0.4690(2) 0.0241(7) Uani 1 1 d . . . H4 H 0.6034 0.5168 0.4196 0.029 Uiso 1 1 calc R . . C5 C 0.57022(15) 0.7188(4) 0.6188(2) 0.0268(8) Uani 1 1 d . . . H5 H 0.5626 0.7720 0.6673 0.032 Uiso 1 1 calc R . . C6 C 0.61989(15) 0.6218(4) 0.6270(2) 0.0225(7) Uani 1 1 d . . . C7 C 0.63142(14) 0.5418(4) 0.5527(2) 0.0213(7) Uani 1 1 d . . . O4 O 0.64927(14) 0.5568(3) 0.78182(16) 0.0455(8) Uani 1 1 d . . . C8 C 0.66393(16) 0.6167(4) 0.7155(2) 0.0243(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0385(15) 0.0271(14) 0.0234(13) 0.0038(10) 0.0031(11) 0.0084(11) O1 0.0259(13) 0.0362(15) 0.0250(13) -0.0083(11) 0.0056(10) 0.0009(11) C9 0.0227(16) 0.0246(17) 0.0184(17) -0.0053(14) 0.0014(13) -0.0025(14) Co2 0.0302(4) 0.0264(4) 0.0206(3) 0.000 -0.0030(3) 0.000 Ho1 0.02187(9) 0.02150(10) 0.01441(9) 0.00029(6) 0.00064(6) -0.00083(6) S5 0.0214(4) 0.0258(5) 0.0196(4) 0.0035(3) 0.0009(3) 0.0019(3) O3 0.0279(14) 0.0486(16) 0.0195(13) -0.0031(12) 0.0003(10) -0.0039(12) O5 0.0445(16) 0.0484(17) 0.0196(13) -0.0056(12) -0.0003(12) 0.0201(13) O6 0.0277(13) 0.0394(14) 0.0189(12) 0.0029(11) -0.0011(10) 0.0044(11) O7 0.0466(17) 0.0308(15) 0.0557(19) 0.0145(14) -0.0012(14) -0.0087(13) O8 0.0230(13) 0.067(2) 0.0307(14) 0.0181(14) -0.0027(11) -0.0017(13) O9 0.0567(18) 0.0436(17) 0.0281(14) 0.0000(13) 0.0082(13) 0.0200(15) O10 0.062(2) 0.0273(18) 0.104(3) 0.0003(16) 0.038(2) -0.0017(14) O11 0.0383(15) 0.0311(15) 0.0308(14) -0.0067(12) -0.0055(12) 0.0082(12) O12 0.119(4) 0.035(3) 0.065(3) 0.000 0.046(3) 0.000 O13 0.064(3) 0.025(2) 0.053(3) 0.000 -0.041(2) 0.000 N1 0.0275(16) 0.0384(17) 0.0192(15) 0.0003(13) -0.0032(12) 0.0095(14) N2 0.0303(17) 0.0389(18) 0.0262(16) -0.0021(14) 0.0030(13) 0.0137(14) C1 0.029(2) 0.041(2) 0.032(2) 0.0027(18) 0.0002(16) 0.0079(17) C2 0.0244(17) 0.0286(19) 0.0238(18) -0.0017(15) 0.0041(14) 0.0050(15) C3 0.0255(18) 0.0272(19) 0.0197(17) 0.0014(14) -0.0002(14) 0.0020(14) C4 0.0299(18) 0.0274(19) 0.0146(16) -0.0017(14) 0.0041(13) 0.0040(15) C5 0.0309(19) 0.0276(19) 0.0225(18) -0.0045(15) 0.0070(15) 0.0024(15) C6 0.0257(18) 0.0228(18) 0.0177(17) -0.0006(13) 0.0021(14) -0.0016(13) C7 0.0243(17) 0.0228(18) 0.0157(16) 0.0005(13) 0.0021(13) 0.0020(14) O4 0.0671(19) 0.0470(18) 0.0181(13) 0.0032(12) -0.0001(13) -0.0289(15) C8 0.033(2) 0.0216(18) 0.0174(17) -0.0017(13) 0.0034(14) 0.0026(14) _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 O2 C9 1.267(4) . ? O2 Ho1 2.344(2) 4_646 ? O1 C9 1.264(4) . ? O1 Ho1 2.270(2) 6_565 ? O1 Ho1 2.855(2) 4_646 ? C9 C7 1.480(4) . ? C9 Ho1 2.970(3) 4_646 ? Co2 O13 2.084(4) . ? Co2 O11 2.099(2) . ? Co2 O11 2.099(2) 2_655 ? Co2 N1 2.103(3) 2_655 ? Co2 N1 2.103(3) . ? Co2 O12 2.148(4) . ? Ho1 O1 2.270(2) 6_566 ? Ho1 O5 2.316(2) . ? Ho1 O6 2.326(2) 7_667 ? Ho1 O2 2.344(2) 4_656 ? Ho1 O10 2.386(3) . ? Ho1 O9 2.426(3) . ? Ho1 O3 2.443(2) . ? Ho1 O4 2.517(3) . ? Ho1 O1 2.855(2) 4_656 ? Ho1 C9 2.970(3) 4_656 ? S5 O7 1.454(3) . ? S5 O8 1.463(2) . ? S5 O5 1.466(3) . ? S5 O6 1.471(2) . ? O3 C8 1.251(4) . ? O6 Ho1 2.326(2) 7_667 ? O9 H9B 0.847(10) . ? O9 H9A 0.847(10) . ? O10 H10A 0.8686 . ? O10 H10B 0.8693 . ? O11 H11A 0.8784 . ? O11 H11B 0.8773 . ? O12 H12 0.8425 . ? O13 H13 0.840(11) . ? N1 C1 1.321(5) . ? N1 C3 1.396(4) . ? N2 C1 1.325(5) . ? N2 C2 1.377(4) . ? N2 H2 0.8600 . ? C1 H1 0.9300 . ? C2 C5 1.384(4) . ? C2 C3 1.400(5) . ? C3 C4 1.382(5) . ? C4 C7 1.386(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(5) . ? C5 H5 0.9300 . ? C6 C7 1.417(4) . ? C6 C8 1.501(5) . ? O4 C8 1.257(4) . ? 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 C9 O2 Ho1 106.9(2) . 4_646 ? C9 O1 Ho1 172.3(2) . 6_565 ? C9 O1 Ho1 82.7(2) . 4_646 ? Ho1 O1 Ho1 104.70(8) 6_565 4_646 ? O1 C9 O2 121.1(3) . . ? O1 C9 C7 120.6(3) . . ? O2 C9 C7 118.2(3) . . ? O1 C9 Ho1 72.39(19) . 4_646 ? O2 C9 Ho1 49.06(16) . 4_646 ? C7 C9 Ho1 164.4(2) . 4_646 ? O13 Co2 O11 86.79(7) . . ? O13 Co2 O11 86.79(7) . 2_655 ? O11 Co2 O11 173.59(15) . 2_655 ? O13 Co2 N1 90.34(9) . 2_655 ? O11 Co2 N1 87.65(10) . 2_655 ? O11 Co2 N1 92.39(10) 2_655 2_655 ? O13 Co2 N1 90.34(9) . . ? O11 Co2 N1 92.39(10) . . ? O11 Co2 N1 87.65(10) 2_655 . ? N1 Co2 N1 179.32(18) 2_655 . ? O13 Co2 O12 180.000(1) . . ? O11 Co2 O12 93.21(7) . . ? O11 Co2 O12 93.21(7) 2_655 . ? N1 Co2 O12 89.66(9) 2_655 . ? N1 Co2 O12 89.66(9) . . ? O1 Ho1 O5 78.01(9) 6_566 . ? O1 Ho1 O6 80.68(8) 6_566 7_667 ? O5 Ho1 O6 133.04(9) . 7_667 ? O1 Ho1 O2 124.01(9) 6_566 4_656 ? O5 Ho1 O2 77.35(10) . 4_656 ? O6 Ho1 O2 80.92(9) 7_667 4_656 ? O1 Ho1 O10 77.41(11) 6_566 . ? O5 Ho1 O10 136.47(11) . . ? O6 Ho1 O10 76.68(11) 7_667 . ? O2 Ho1 O10 145.79(10) 4_656 . ? O1 Ho1 O9 144.99(9) 6_566 . ? O5 Ho1 O9 136.90(10) . . ? O6 Ho1 O9 74.87(9) 7_667 . ? O2 Ho1 O9 76.53(10) 4_656 . ? O10 Ho1 O9 72.87(11) . . ? O1 Ho1 O3 137.75(8) 6_566 . ? O5 Ho1 O3 73.18(9) . . ? O6 Ho1 O3 141.28(8) 7_667 . ? O2 Ho1 O3 78.80(9) 4_656 . ? O10 Ho1 O3 103.39(12) . . ? O9 Ho1 O3 68.53(9) . . ? O1 Ho1 O4 89.97(9) 6_566 . ? O5 Ho1 O4 71.65(10) . . ? O6 Ho1 O4 149.53(10) 7_667 . ? O2 Ho1 O4 127.21(8) 4_656 . ? O10 Ho1 O4 72.98(11) . . ? O9 Ho1 O4 98.53(10) . . ? O3 Ho1 O4 52.00(8) . . ? O1 Ho1 O1 75.30(8) 6_566 4_656 ? O5 Ho1 O1 68.73(8) . 4_656 ? O6 Ho1 O1 65.57(8) 7_667 4_656 ? O2 Ho1 O1 48.96(8) 4_656 4_656 ? O10 Ho1 O1 136.16(11) . 4_656 ? O9 Ho1 O1 115.11(9) . 4_656 ? O3 Ho1 O1 119.88(8) . 4_656 ? O4 Ho1 O1 139.74(9) . 4_656 ? O1 Ho1 C9 100.25(9) 6_566 4_656 ? O5 Ho1 C9 72.91(10) . 4_656 ? O6 Ho1 C9 70.43(9) 7_667 4_656 ? O2 Ho1 C9 24.09(8) 4_656 4_656 ? O10 Ho1 C9 146.92(11) . 4_656 ? O9 Ho1 C9 94.78(10) . 4_656 ? O3 Ho1 C9 100.03(9) . 4_656 ? O4 Ho1 C9 140.02(9) . 4_656 ? O1 Ho1 C9 24.96(7) 4_656 4_656 ? O7 S5 O8 109.40(17) . . ? O7 S5 O5 108.81(18) . . ? O8 S5 O5 109.21(17) . . ? O7 S5 O6 110.32(17) . . ? O8 S5 O6 108.52(14) . . ? O5 S5 O6 110.56(15) . . ? C8 O3 Ho1 95.7(2) . . ? S5 O5 Ho1 143.57(16) . . ? S5 O6 Ho1 137.47(14) . 7_667 ? Ho1 O9 H9B 118(3) . . ? Ho1 O9 H9A 117(3) . . ? H9B O9 H9A 109.1(17) . . ? Ho1 O10 H10A 109.7 . . ? Ho1 O10 H10B 110.6 . . ? H10A O10 H10B 108.4 . . ? Co2 O11 H11A 111.4 . . ? Co2 O11 H11B 110.7 . . ? H11A O11 H11B 107.6 . . ? Co2 O12 H12 113.4 . . ? Co2 O13 H13 128(3) . . ? C1 N1 C3 104.4(3) . . ? C1 N1 Co2 120.6(2) . . ? C3 N1 Co2 131.8(2) . . ? C1 N2 C2 107.3(3) . . ? C1 N2 H2 126.4 . . ? C2 N2 H2 126.4 . . ? N1 C1 N2 114.0(3) . . ? N1 C1 H1 123.0 . . ? N2 C1 H1 123.0 . . ? N2 C2 C5 132.1(3) . . ? N2 C2 C3 105.6(3) . . ? C5 C2 C3 122.3(3) . . ? C4 C3 N1 131.2(3) . . ? C4 C3 C2 120.0(3) . . ? N1 C3 C2 108.7(3) . . ? C3 C4 C7 118.7(3) . . ? C3 C4 H4 120.7 . . ? C7 C4 H4 120.7 . . ? C2 C5 C6 117.3(3) . . ? C2 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? C5 C6 C7 121.0(3) . . ? C5 C6 C8 117.2(3) . . ? C7 C6 C8 121.5(3) . . ? C4 C7 C6 120.4(3) . . ? C4 C7 C9 118.8(3) . . ? C6 C7 C9 120.5(3) . . ? C8 O4 Ho1 92.0(2) . . ? O3 C8 O4 120.3(3) . . ? O3 C8 C6 118.4(3) . . ? O4 C8 C6 121.1(3) . . ? 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 Ho1 O1 C9 O2 -157.6(14) 6_565 . . . ? Ho1 O1 C9 O2 5.8(3) 4_646 . . . ? Ho1 O1 C9 C7 26.2(18) 6_565 . . . ? Ho1 O1 C9 C7 -170.4(3) 4_646 . . . ? Ho1 O1 C9 Ho1 -163.4(16) 6_565 . . 4_646 ? Ho1 O2 C9 O1 -7.3(4) 4_646 . . . ? Ho1 O2 C9 C7 169.0(2) 4_646 . . . ? O1 Ho1 O3 C8 -30.4(3) 6_566 . . . ? O5 Ho1 O3 C8 -79.4(2) . . . . ? O6 Ho1 O3 C8 140.8(2) 7_667 . . . ? O2 Ho1 O3 C8 -159.4(2) 4_656 . . . ? O10 Ho1 O3 C8 55.5(2) . . . . ? O9 Ho1 O3 C8 120.8(2) . . . . ? O4 Ho1 O3 C8 0.1(2) . . . . ? O1 Ho1 O3 C8 -131.8(2) 4_656 . . . ? C9 Ho1 O3 C8 -148.0(2) 4_656 . . . ? O7 S5 O5 Ho1 117.4(3) . . . . ? O8 S5 O5 Ho1 -123.3(3) . . . . ? O6 S5 O5 Ho1 -3.9(4) . . . . ? O1 Ho1 O5 S5 30.3(3) 6_566 . . . ? O6 Ho1 O5 S5 -34.6(4) 7_667 . . . ? O2 Ho1 O5 S5 -99.0(3) 4_656 . . . ? O10 Ho1 O5 S5 87.1(3) . . . . ? O9 Ho1 O5 S5 -152.9(3) . . . . ? O3 Ho1 O5 S5 179.0(3) . . . . ? O4 Ho1 O5 S5 124.3(3) . . . . ? O1 Ho1 O5 S5 -48.4(3) 4_656 . . . ? C9 Ho1 O5 S5 -74.5(3) 4_656 . . . ? O7 S5 O6 Ho1 -75.8(3) . . . 7_667 ? O8 S5 O6 Ho1 164.4(2) . . . 7_667 ? O5 S5 O6 Ho1 44.6(3) . . . 7_667 ? O13 Co2 N1 C1 46.4(3) . . . . ? O11 Co2 N1 C1 133.2(3) . . . . ? O11 Co2 N1 C1 -40.4(3) 2_655 . . . ? N1 Co2 N1 C1 -133.6(3) 2_655 . . . ? O12 Co2 N1 C1 -133.6(3) . . . . ? O13 Co2 N1 C3 -110.4(3) . . . . ? O11 Co2 N1 C3 -23.6(3) . . . . ? O11 Co2 N1 C3 162.9(3) 2_655 . . . ? N1 Co2 N1 C3 69.6(4) 2_655 . . . ? O12 Co2 N1 C3 69.6(3) . . . . ? C3 N1 C1 N2 0.6(5) . . . . ? Co2 N1 C1 N2 -161.7(3) . . . . ? C2 N2 C1 N1 0.2(5) . . . . ? C1 N2 C2 C5 177.4(4) . . . . ? C1 N2 C2 C3 -0.9(4) . . . . ? C1 N1 C3 C4 176.9(4) . . . . ? Co2 N1 C3 C4 -23.6(6) . . . . ? C1 N1 C3 C2 -1.2(4) . . . . ? Co2 N1 C3 C2 158.3(3) . . . . ? N2 C2 C3 C4 -177.0(3) . . . . ? C5 C2 C3 C4 4.4(5) . . . . ? N2 C2 C3 N1 1.3(4) . . . . ? C5 C2 C3 N1 -177.3(3) . . . . ? N1 C3 C4 C7 -178.5(3) . . . . ? C2 C3 C4 C7 -0.6(5) . . . . ? N2 C2 C5 C6 177.7(4) . . . . ? C3 C2 C5 C6 -4.2(5) . . . . ? C2 C5 C6 C7 0.3(5) . . . . ? C2 C5 C6 C8 174.7(3) . . . . ? C3 C4 C7 C6 -3.2(5) . . . . ? C3 C4 C7 C9 171.0(3) . . . . ? C5 C6 C7 C4 3.3(5) . . . . ? C8 C6 C7 C4 -170.7(3) . . . . ? C5 C6 C7 C9 -170.7(3) . . . . ? C8 C6 C7 C9 15.2(5) . . . . ? O1 C9 C7 C4 30.9(5) . . . . ? O2 C9 C7 C4 -145.4(3) . . . . ? Ho1 C9 C7 C4 -112.9(8) 4_646 . . . ? O1 C9 C7 C6 -154.9(3) . . . . ? O2 C9 C7 C6 28.8(5) . . . . ? Ho1 C9 C7 C6 61.3(9) 4_646 . . . ? O1 Ho1 O4 C8 159.9(2) 6_566 . . . ? O5 Ho1 O4 C8 82.6(2) . . . . ? O6 Ho1 O4 C8 -128.8(2) 7_667 . . . ? O2 Ho1 O4 C8 25.3(3) 4_656 . . . ? O10 Ho1 O4 C8 -123.2(2) . . . . ? O9 Ho1 O4 C8 -54.2(2) . . . . ? O3 Ho1 O4 C8 -0.1(2) . . . . ? O1 Ho1 O4 C8 93.1(2) 4_656 . . . ? C9 Ho1 O4 C8 53.9(3) 4_656 . . . ? Ho1 O3 C8 O4 -0.2(4) . . . . ? Ho1 O3 C8 C6 174.4(3) . . . . ? Ho1 O4 C8 O3 0.2(3) . . . . ? Ho1 O4 C8 C6 -174.3(3) . . . . ? C5 C6 C8 O3 -104.4(4) . . . . ? C7 C6 C8 O3 69.9(4) . . . . ? C5 C6 C8 O4 70.2(4) . . . . ? C7 C6 C8 O4 -115.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.584 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.093 data_1 _database_code_depnum_ccdc_archive 'CCDC 888136' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co N4 O24 Pr2 S2' _chemical_formula_weight 1085.28 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' Co Co 0.3494 0.9721 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.799(15) _cell_length_b 8.68(2) _cell_length_c 15.656(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.364(7) _cell_angle_gamma 90.00 _cell_volume 3026(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3607 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 27.86 _exptl_crystal_description 0 _exptl_crystal_colour 0 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 3.959 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3004 _exptl_absorpt_correction_T_max 0.5048 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15471 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.86 _reflns_number_total 3607 _reflns_number_gt 2874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0105P)^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 NONE _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3607 _refine_ls_number_parameters 268 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0442 _refine_ls_wR_factor_gt 0.0432 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _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 Pr1 Pr 0.252979(6) 1.141180(17) 0.617772(8) 0.01320(5) Uani 1 1 d . . . Co1 Co 0.5000 0.79516(7) 0.7500 0.01904(13) Uani 1 2 d S . . S3 S 0.14738(3) 1.03409(8) 0.41527(4) 0.01499(15) Uani 1 1 d . . . O2 O 0.31281(8) 1.1429(2) 0.35904(11) 0.0186(4) Uani 1 1 d . . . O12 O 0.5000 0.5539(4) 0.7500 0.0378(10) Uani 1 2 d S . . H12 H 0.5203(16) 0.511(4) 0.783(2) 0.057 Uiso 1 1 d . . . O9 O 0.26013(10) 0.8586(2) 0.61509(13) 0.0248(5) Uani 1 1 d . . . O7 O 0.16087(9) 0.8709(2) 0.40352(12) 0.0238(5) Uani 1 1 d . . . O1 O 0.29744(8) 1.1125(2) 0.49341(11) 0.0165(4) Uani 1 1 d . . . O4 O 0.35975(8) 0.9275(2) 0.22012(11) 0.0205(4) Uani 1 1 d . . . O11 O 0.40539(9) 0.7817(3) 0.72861(13) 0.0241(5) Uani 1 1 d . . . O8 O 0.08268(8) 1.0623(2) 0.38224(11) 0.0222(5) Uani 1 1 d . . . O5 O 0.16302(8) 1.0754(2) 0.50901(10) 0.0181(4) Uani 1 1 d . . . O3 O 0.29076(8) 0.8178(2) 0.27937(11) 0.0189(4) Uani 1 1 d . . . O10 O 0.17691(10) 1.0444(3) 0.70436(13) 0.0230(5) Uani 1 1 d D . . C7 C 0.40667(12) 0.9339(3) 0.53066(17) 0.0169(6) Uani 1 1 d . . . H7 H 0.3971(12) 0.990(3) 0.5755(16) 0.020 Uiso 1 1 d . . . C9 C 0.34253(12) 0.8762(3) 0.28645(16) 0.0160(6) Uani 1 1 d . . . C3 C 0.46994(12) 0.7626(3) 0.46762(16) 0.0167(6) Uani 1 1 d . . . C2 C 0.45600(12) 0.8356(3) 0.54052(17) 0.0178(6) Uani 1 1 d . . . C5 C 0.38476(12) 0.8733(3) 0.37468(16) 0.0145(6) Uani 1 1 d . . . C8 C 0.32395(12) 1.0747(3) 0.43249(16) 0.0148(6) Uani 1 1 d . . . C6 C 0.37144(11) 0.9539(3) 0.44712(16) 0.0144(6) Uani 1 1 d . . . O6 O 0.18237(8) 1.1308(2) 0.36527(11) 0.0218(5) Uani 1 1 d . . . O13 O 0.5000 1.0403(4) 0.7500 0.0517(11) Uani 1 2 d SD . . H13 H 0.5333(10) 1.082(4) 0.749(3) 0.062 Uiso 1 1 d D . . N1 N 0.49926(10) 0.7939(3) 0.61502(13) 0.0203(5) Uani 1 1 d . . . N2 N 0.52186(11) 0.6803(3) 0.49791(14) 0.0189(5) Uani 1 1 d . . . H2 H 0.5438(13) 0.633(3) 0.4685(18) 0.023 Uiso 1 1 d . . . C1 C 0.53685(13) 0.7034(4) 0.58473(18) 0.0219(7) Uani 1 1 d . . . H1 H 0.5693(13) 0.652(3) 0.6186(17) 0.026 Uiso 1 1 d . . . C4 C 0.43384(12) 0.7758(3) 0.38441(17) 0.0165(6) Uani 1 1 d . . . H4 H 0.4425(12) 0.727(3) 0.3382(16) 0.020 Uiso 1 1 d . . . H9A H 0.2855(12) 0.795(3) 0.5946(17) 0.020 Uiso 1 1 d . . . H11A H 0.3860(12) 0.736(4) 0.6864(17) 0.020 Uiso 1 1 d . . . H10A H 0.1813(13) 0.989(3) 0.7445(16) 0.020 Uiso 1 1 d . . . H11B H 0.3892(13) 0.863(3) 0.7307(18) 0.020 Uiso 1 1 d . . . H9B H 0.2415(13) 0.814(4) 0.6423(18) 0.020 Uiso 1 1 d . . . H10B H 0.1586(11) 1.123(2) 0.7157(18) 0.020 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01632(8) 0.01101(9) 0.01135(8) 0.00004(6) 0.00094(6) 0.00048(6) Co1 0.0251(3) 0.0133(3) 0.0154(3) 0.000 -0.0028(2) 0.000 S3 0.0165(3) 0.0130(4) 0.0143(3) -0.0018(3) 0.0008(3) -0.0004(3) O2 0.0244(10) 0.0149(11) 0.0164(9) 0.0020(8) 0.0044(8) 0.0057(9) O12 0.045(2) 0.018(2) 0.036(2) 0.000 -0.0231(16) 0.000 O9 0.0292(12) 0.0139(12) 0.0340(13) 0.0030(9) 0.0125(10) 0.0032(10) O7 0.0279(11) 0.0140(11) 0.0271(11) -0.0041(9) 0.0003(9) 0.0042(9) O1 0.0187(9) 0.0169(11) 0.0140(9) -0.0003(8) 0.0037(8) 0.0021(9) O4 0.0289(11) 0.0202(11) 0.0119(9) -0.0010(9) 0.0034(8) -0.0063(10) O11 0.0303(12) 0.0187(13) 0.0189(10) -0.0050(9) -0.0048(9) 0.0082(10) O8 0.0152(9) 0.0275(13) 0.0219(10) -0.0089(9) -0.0005(8) 0.0026(9) O5 0.0205(10) 0.0198(11) 0.0135(9) -0.0014(8) 0.0023(8) -0.0020(9) O3 0.0191(9) 0.0232(12) 0.0138(9) 0.0001(8) 0.0020(8) -0.0032(9) O10 0.0275(11) 0.0243(13) 0.0178(10) 0.0037(9) 0.0064(9) -0.0008(10) C7 0.0244(14) 0.0122(15) 0.0140(13) -0.0021(12) 0.0036(11) 0.0027(12) C9 0.0234(14) 0.0096(15) 0.0142(13) -0.0014(11) 0.0025(11) 0.0048(12) C3 0.0178(13) 0.0117(15) 0.0200(14) 0.0006(12) 0.0026(11) 0.0016(12) C2 0.0210(13) 0.0170(16) 0.0139(13) -0.0008(12) 0.0001(11) 0.0014(13) C5 0.0184(13) 0.0124(15) 0.0126(13) 0.0008(11) 0.0028(10) -0.0011(12) C8 0.0185(13) 0.0093(14) 0.0152(13) -0.0033(11) 0.0004(11) -0.0031(12) C6 0.0180(13) 0.0097(14) 0.0157(13) -0.0002(11) 0.0044(11) 0.0001(11) O6 0.0248(10) 0.0261(12) 0.0137(9) 0.0003(8) 0.0022(8) -0.0092(10) O13 0.101(4) 0.016(2) 0.052(2) 0.000 0.048(3) 0.000 N1 0.0220(12) 0.0201(14) 0.0166(11) -0.0001(10) -0.0008(10) 0.0049(11) N2 0.0205(12) 0.0169(14) 0.0181(12) -0.0025(11) 0.0012(10) 0.0051(11) C1 0.0196(14) 0.0205(17) 0.0229(15) -0.0011(13) -0.0012(12) 0.0030(13) C4 0.0209(13) 0.0147(16) 0.0139(13) -0.0027(12) 0.0037(11) 0.0005(12) _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 Pr1 O1 2.393(2) . ? Pr1 O5 2.436(2) . ? Pr1 O6 2.448(4) 7_576 ? Pr1 O9 2.459(6) . ? Pr1 O2 2.475(4) 7_576 ? Pr1 O3 2.517(3) 6_576 ? Pr1 O10 2.561(3) . ? Pr1 O4 2.679(2) 6_576 ? Pr1 O1 2.840(4) 7_576 ? Pr1 C9 2.976(3) 6_576 ? Pr1 C8 3.031(5) 7_576 ? Pr1 Pr1 4.120(4) 7_576 ? Co1 O12 2.094(6) . ? Co1 N1 2.110(3) . ? Co1 N1 2.110(3) 2_656 ? Co1 O11 2.114(3) 2_656 ? Co1 O11 2.114(3) . ? Co1 O13 2.128(6) . ? S3 O7 1.469(4) . ? S3 O8 1.475(2) . ? S3 O5 1.478(2) . ? S3 O6 1.490(2) . ? O2 C8 1.270(3) . ? O2 Pr1 2.475(4) 7_576 ? O1 C8 1.276(3) . ? O1 Pr1 2.840(4) 7_576 ? O4 C9 1.267(3) . ? O4 Pr1 2.679(2) 6_575 ? O3 C9 1.267(3) . ? O3 Pr1 2.517(3) 6_575 ? C7 C6 1.391(3) . ? C7 C2 1.394(4) . ? C9 C5 1.505(3) . ? C9 Pr1 2.976(3) 6_575 ? C3 N2 1.377(3) . ? C3 C4 1.389(3) . ? C3 C2 1.400(4) . ? C2 N1 1.404(3) . ? C5 C4 1.385(4) . ? C5 C6 1.420(4) . ? C8 C6 1.489(4) . ? C8 Pr1 3.031(5) 7_576 ? O6 Pr1 2.448(4) 7_576 ? N1 C1 1.323(4) . ? N2 C1 1.344(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pr1 O5 81.19(8) . . ? O1 Pr1 O6 79.76(8) . 7_576 ? O5 Pr1 O6 131.48(7) . 7_576 ? O1 Pr1 O9 80.86(7) . . ? O5 Pr1 O9 78.66(8) . . ? O6 Pr1 O9 140.14(10) 7_576 . ? O1 Pr1 O2 125.01(7) . 7_576 ? O5 Pr1 O2 80.44(9) . 7_576 ? O6 Pr1 O2 75.03(14) 7_576 7_576 ? O9 Pr1 O2 143.33(9) . 7_576 ? O1 Pr1 O3 135.98(7) . 6_576 ? O5 Pr1 O3 142.31(6) . 6_576 ? O6 Pr1 O3 73.03(6) 7_576 6_576 ? O9 Pr1 O3 98.55(7) . 6_576 ? O2 Pr1 O3 80.40(6) 7_576 6_576 ? O1 Pr1 O10 148.16(8) . . ? O5 Pr1 O10 74.28(9) . . ? O6 Pr1 O10 131.91(7) 7_576 . ? O9 Pr1 O10 74.75(9) . . ? O2 Pr1 O10 70.74(12) 7_576 . ? O3 Pr1 O10 68.85(8) 6_576 . ? O1 Pr1 O4 88.54(8) . 6_576 ? O5 Pr1 O4 152.50(9) . 6_576 ? O6 Pr1 O4 70.50(11) 7_576 6_576 ? O9 Pr1 O4 74.53(7) . 6_576 ? O2 Pr1 O4 125.61(7) 7_576 6_576 ? O3 Pr1 O4 50.12(6) 6_576 6_576 ? O10 Pr1 O4 104.00(9) . 6_576 ? O1 Pr1 O1 76.47(9) . 7_576 ? O5 Pr1 O1 65.06(11) . 7_576 ? O6 Pr1 O1 67.24(12) 7_576 7_576 ? O9 Pr1 O1 139.47(9) . 7_576 ? O2 Pr1 O1 48.81(9) 7_576 7_576 ? O3 Pr1 O1 121.06(10) 6_576 7_576 ? O10 Pr1 O1 109.89(8) . 7_576 ? O4 Pr1 O1 136.95(6) 6_576 7_576 ? O1 Pr1 C9 112.77(9) . 6_576 ? O5 Pr1 C9 157.40(7) . 6_576 ? O6 Pr1 C9 70.25(8) 7_576 6_576 ? O9 Pr1 C9 85.94(7) . 6_576 ? O2 Pr1 C9 103.32(8) 7_576 6_576 ? O3 Pr1 C9 24.93(7) 6_576 6_576 ? O10 Pr1 C9 85.83(9) . 6_576 ? O4 Pr1 C9 25.19(6) 6_576 6_576 ? O1 Pr1 C9 133.85(9) 7_576 6_576 ? O1 Pr1 C8 101.29(7) . 7_576 ? O5 Pr1 C8 69.84(11) . 7_576 ? O6 Pr1 C8 70.84(14) 7_576 7_576 ? O9 Pr1 C8 147.56(9) . 7_576 ? O2 Pr1 C8 24.06(7) 7_576 7_576 ? O3 Pr1 C8 101.55(8) 6_576 7_576 ? O10 Pr1 C8 89.11(11) . 7_576 ? O4 Pr1 C8 137.51(7) 6_576 7_576 ? O1 Pr1 C8 24.84(7) 7_576 7_576 ? C9 Pr1 C8 121.37(8) 6_576 7_576 ? O1 Pr1 Pr1 42.09(7) . 7_576 ? O5 Pr1 Pr1 67.68(7) . 7_576 ? O6 Pr1 Pr1 68.29(7) 7_576 7_576 ? O9 Pr1 Pr1 115.57(8) . 7_576 ? O2 Pr1 Pr1 83.07(9) 7_576 7_576 ? O3 Pr1 Pr1 140.66(8) 6_576 7_576 ? O10 Pr1 Pr1 136.72(5) . 7_576 ? O4 Pr1 Pr1 119.27(5) 6_576 7_576 ? O1 Pr1 Pr1 34.38(4) 7_576 7_576 ? C9 Pr1 Pr1 134.62(7) 6_576 7_576 ? C8 Pr1 Pr1 59.21(7) 7_576 7_576 ? O12 Co1 N1 89.71(7) . . ? O12 Co1 N1 89.71(7) . 2_656 ? N1 Co1 N1 179.43(14) . 2_656 ? O12 Co1 O11 86.83(6) . 2_656 ? N1 Co1 O11 86.98(8) . 2_656 ? N1 Co1 O11 92.98(8) 2_656 2_656 ? O12 Co1 O11 86.83(6) . . ? N1 Co1 O11 92.98(8) . . ? N1 Co1 O11 86.98(8) 2_656 . ? O11 Co1 O11 173.66(13) 2_656 . ? O12 Co1 O13 180.000(2) . . ? N1 Co1 O13 90.29(7) . . ? N1 Co1 O13 90.29(7) 2_656 . ? O11 Co1 O13 93.17(6) 2_656 . ? O11 Co1 O13 93.17(6) . . ? O7 S3 O8 109.65(12) . . ? O7 S3 O5 110.23(11) . . ? O8 S3 O5 108.56(11) . . ? O7 S3 O6 109.11(15) . . ? O8 S3 O6 109.27(13) . . ? O5 S3 O6 110.01(13) . . ? C8 O2 Pr1 103.32(18) . 7_576 ? C8 O1 Pr1 170.25(18) . . ? C8 O1 Pr1 85.98(17) . 7_576 ? Pr1 O1 Pr1 103.53(9) . 7_576 ? C9 O4 Pr1 90.62(16) . 6_575 ? S3 O5 Pr1 137.62(11) . . ? C9 O3 Pr1 98.23(15) . 6_575 ? C6 C7 C2 118.1(3) . . ? O4 C9 O3 121.0(2) . . ? O4 C9 C5 120.6(2) . . ? O3 C9 C5 118.3(2) . . ? O4 C9 Pr1 64.18(14) . 6_575 ? O3 C9 Pr1 56.84(13) . 6_575 ? C5 C9 Pr1 174.80(19) . 6_575 ? N2 C3 C4 131.2(3) . . ? N2 C3 C2 106.4(2) . . ? C4 C3 C2 122.4(3) . . ? C7 C2 C3 120.3(2) . . ? C7 C2 N1 131.0(3) . . ? C3 C2 N1 108.6(2) . . ? C4 C5 C6 121.3(2) . . ? C4 C5 C9 117.0(2) . . ? C6 C5 C9 121.4(2) . . ? O2 C8 O1 121.4(3) . . ? O2 C8 C6 117.7(2) . . ? O1 C8 C6 120.7(2) . . ? O2 C8 Pr1 52.62(14) . 7_576 ? O1 C8 Pr1 69.18(15) . 7_576 ? C6 C8 Pr1 166.91(19) . 7_576 ? C7 C6 C5 120.7(3) . . ? C7 C6 C8 119.1(2) . . ? C5 C6 C8 119.8(2) . . ? S3 O6 Pr1 140.90(11) . 7_576 ? C1 N1 C2 104.4(2) . . ? C1 N1 Co1 119.67(18) . . ? C2 N1 Co1 133.18(19) . . ? C1 N2 C3 106.5(2) . . ? N1 C1 N2 114.0(2) . . ? C5 C4 C3 117.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.540 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.109 data_4 _database_code_depnum_ccdc_archive 'CCDC 888137' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co N4 O24 S2 Tb2' _chemical_formula_weight 1121.30 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' Co Co 0.3494 0.9721 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.805(6) _cell_length_b 8.530(2) _cell_length_c 15.480(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.424(5) _cell_angle_gamma 90.00 _cell_volume 2940.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2596 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 25.01 _exptl_crystal_description 0 _exptl_crystal_colour 0 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 5.571 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4021 _exptl_absorpt_correction_T_max 0.4021 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11724 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2596 _reflns_number_gt 2382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0324P)^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 NONE _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2596 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0527 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.247378(7) 0.138571(17) 0.382487(10) 0.02188(8) Uani 1 1 d . . . Co Co 0.0000 0.20943(8) -0.2500 0.02875(16) Uani 1 2 d S . . S S 0.15044(4) 0.46010(9) 0.41495(5) 0.02355(18) Uani 1 1 d . . . O1 O 0.21160(10) 0.1781(3) 0.22429(15) 0.0280(5) Uani 1 1 d . . . O2 O 0.14278(11) 0.0665(3) 0.28284(14) 0.0328(6) Uani 1 1 d . . . O3 O 0.31025(11) 0.3501(2) 0.36309(16) 0.0279(6) Uani 1 1 d . . . O4 O 0.20391(10) 0.1061(3) 0.50168(15) 0.0261(5) Uani 1 1 d . . . O5 O 0.18491(12) 0.3605(2) 0.36514(16) 0.0312(6) Uani 1 1 d . . . O6 O 0.16588(10) 0.4200(3) 0.51000(14) 0.0278(5) Uani 1 1 d . . . O7 O 0.16437(12) 0.6245(2) 0.40206(18) 0.0339(6) Uani 1 1 d . . . O8 O 0.08587(10) 0.4330(3) 0.38098(15) 0.0341(6) Uani 1 1 d . . . O9 O 0.24118(11) -0.1370(3) 0.38349(17) 0.0374(7) Uani 1 1 d . . . H9A H 0.2237 -0.1921 0.4108 0.056 Uiso 1 1 d R . . H9B H 0.2618 -0.2129 0.3621 0.056 Uiso 1 1 d R . . O10 O 0.32162(10) 0.0401(3) 0.29988(15) 0.0311(5) Uani 1 1 d . . . H10A H 0.3383 0.1089 0.2813 0.047 Uiso 1 1 d R . . H10B H 0.3159 -0.0149 0.2589 0.047 Uiso 1 1 d R . . O11 O 0.0000 -0.0393(4) -0.2500 0.0667(14) Uani 1 2 d S . . H11A H -0.0330 -0.0891 -0.2575 0.100 Uiso 0.50 1 d PR . . H11B H 0.0330 -0.0891 -0.2425 0.100 Uiso 0.50 1 d PR . . O12 O 0.09455(10) 0.2227(3) -0.22904(14) 0.0346(6) Uani 1 1 d . . . H12A H 0.1153 0.1392 -0.2243 0.052 Uiso 1 1 d R . . H12B H 0.1096 0.2816 -0.1852 0.052 Uiso 1 1 d R . . O13 O 0.0000 0.4546(4) -0.2500 0.0494(11) Uani 1 2 d S . . H13 H -0.0174 0.5153 -0.2901 0.074 Uiso 1 1 d R . . N1 N 0.00094(12) 0.2101(3) -0.11345(18) 0.0296(6) Uani 1 1 d . . . N2 N -0.02143(12) 0.3175(3) 0.00577(19) 0.0293(6) Uani 1 1 d . . . H2 H -0.0408 0.3714 0.0375 0.035 Uiso 1 1 d R . . C1 C 0.11711(15) 0.1257(3) 0.1273(2) 0.0243(7) Uani 1 1 d . . . C2 C 0.13002(14) 0.0466(4) 0.0524(2) 0.0238(7) Uani 1 1 d . . . C3 C 0.09422(14) 0.0686(4) -0.0311(2) 0.0262(7) Uani 1 1 d . . . H3 H 0.1031 0.0188 -0.0801 0.031 Uiso 1 1 calc R . . C4 C 0.04504(15) 0.1662(4) -0.0396(2) 0.0270(7) Uani 1 1 d . . . C5 C 0.03139(14) 0.2359(4) 0.0357(2) 0.0262(7) Uani 1 1 d . . . C6 C 0.06764(14) 0.2215(4) 0.1192(2) 0.0254(7) Uani 1 1 d . . . H6 H 0.0590 0.2741 0.1676 0.030 Uiso 1 1 calc R . . C7 C -0.03681(15) 0.2970(4) -0.0819(2) 0.0317(8) Uani 1 1 d . . . H7 H -0.0712 0.3405 -0.1171 0.038 Uiso 1 1 calc R . . C8 C 0.15967(16) 0.1197(4) 0.2162(2) 0.0246(7) Uani 1 1 d . . . C9 C 0.32202(14) 0.4255(4) 0.4360(2) 0.0238(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02284(12) 0.02254(11) 0.02003(11) 0.00051(5) 0.00412(8) -0.00044(5) Co 0.0332(4) 0.0249(4) 0.0248(3) 0.000 -0.0012(3) 0.000 S 0.0228(4) 0.0247(4) 0.0228(4) 0.0014(3) 0.0041(3) -0.0001(3) O1 0.0239(13) 0.0355(13) 0.0243(12) -0.0009(10) 0.0045(10) -0.0014(10) O2 0.0423(15) 0.0331(14) 0.0230(12) -0.0002(10) 0.0073(11) -0.0107(11) O3 0.0342(15) 0.0240(13) 0.0251(13) -0.0012(9) 0.0051(11) -0.0036(9) O4 0.0257(13) 0.0302(13) 0.0229(12) 0.0034(10) 0.0065(10) -0.0021(10) O5 0.0352(15) 0.0340(14) 0.0233(13) -0.0015(9) 0.0040(11) 0.0083(10) O6 0.0258(13) 0.0333(13) 0.0233(12) 0.0034(10) 0.0033(10) 0.0010(10) O7 0.0361(15) 0.0253(13) 0.0380(15) 0.0037(10) 0.0030(12) -0.0023(10) O8 0.0239(13) 0.0455(15) 0.0306(13) 0.0095(11) 0.0010(10) -0.0044(11) O9 0.0364(17) 0.0251(16) 0.054(2) -0.0015(10) 0.0170(15) -0.0009(9) O10 0.0346(14) 0.0325(14) 0.0266(12) -0.0036(10) 0.0076(11) 0.0025(10) O11 0.130(4) 0.023(2) 0.064(3) 0.000 0.059(3) 0.000 O12 0.0395(15) 0.0310(14) 0.0286(13) -0.0046(10) -0.0027(11) 0.0097(11) O13 0.056(2) 0.023(2) 0.053(2) 0.000 -0.025(2) 0.000 N1 0.0296(16) 0.0308(16) 0.0258(14) -0.0010(12) 0.0006(12) 0.0058(13) N2 0.0260(16) 0.0306(15) 0.0304(16) -0.0024(13) 0.0040(13) 0.0062(13) C1 0.0250(19) 0.0251(18) 0.0238(18) 0.0006(12) 0.0073(15) -0.0045(13) C2 0.0233(17) 0.0237(17) 0.0239(17) -0.0010(13) 0.0041(14) -0.0009(13) C3 0.0293(18) 0.0263(18) 0.0232(17) -0.0013(13) 0.0062(14) 0.0028(14) C4 0.0290(19) 0.0257(17) 0.0253(18) 0.0010(13) 0.0038(15) 0.0002(14) C5 0.0245(18) 0.0244(17) 0.0306(18) -0.0008(14) 0.0081(14) -0.0001(13) C6 0.0265(18) 0.0260(18) 0.0247(17) -0.0021(13) 0.0078(14) 0.0008(13) C7 0.0280(19) 0.033(2) 0.0310(19) -0.0022(15) -0.0013(15) 0.0039(15) C8 0.030(2) 0.0228(17) 0.0214(18) -0.0014(12) 0.0070(15) 0.0050(13) C9 0.0232(17) 0.0239(17) 0.0225(17) 0.0018(13) 0.0009(14) 0.0025(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.291(2) . ? Tb1 O6 2.349(2) 7_556 ? Tb1 O5 2.349(2) . ? Tb1 O9 2.355(2) . ? Tb1 O3 2.363(2) . ? Tb1 O1 2.432(2) . ? Tb1 O10 2.478(2) . ? Tb1 O2 2.620(2) . ? Tb1 O4 2.887(2) 7_556 ? Tb1 C8 2.905(3) . ? Tb1 C9 2.994(3) . ? Co O13 2.091(3) . ? Co N1 2.109(3) 2_554 ? Co N1 2.109(3) . ? Co O12 2.113(2) 2_554 ? Co O12 2.113(2) . ? Co O11 2.122(4) . ? S O7 1.461(2) . ? S O8 1.472(2) . ? S O6 1.477(2) . ? S O5 1.482(3) . ? O1 C8 1.266(4) . ? O2 C8 1.261(4) . ? O3 C9 1.276(4) . ? O4 C9 1.265(4) 7_556 ? O4 Tb1 2.887(2) 7_556 ? O6 Tb1 2.349(2) 7_556 ? O9 H9A 0.7946 . ? O9 H9B 0.9048 . ? O10 H10A 0.7873 . ? O10 H10B 0.7771 . ? O11 H11A 0.8500 . ? O11 H11B 0.8500 . ? O12 H12A 0.8500 . ? O12 H12B 0.8550 . ? O13 H13 0.8398 . ? N1 C7 1.308(4) . ? N1 C4 1.402(4) . ? N2 C7 1.338(4) . ? N2 C5 1.382(4) . ? N2 H2 0.8599 . ? C1 C6 1.377(5) . ? C1 C2 1.426(4) . ? C1 C8 1.505(5) . ? C2 C3 1.384(4) . ? C2 C9 1.487(4) 4_545 ? C3 C4 1.380(5) . ? C3 H3 0.9300 . ? C4 C5 1.401(5) . ? C5 C6 1.382(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C9 O4 1.265(4) 7_556 ? C9 C2 1.487(4) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tb1 O6 81.26(8) . 7_556 ? O4 Tb1 O5 80.37(8) . . ? O6 Tb1 O5 130.54(8) 7_556 . ? O4 Tb1 O9 80.63(8) . . ? O6 Tb1 O9 79.95(8) 7_556 . ? O5 Tb1 O9 140.27(9) . . ? O4 Tb1 O3 125.02(8) . . ? O6 Tb1 O3 79.11(8) 7_556 . ? O5 Tb1 O3 74.93(9) . . ? O9 Tb1 O3 143.28(9) . . ? O4 Tb1 O1 135.88(8) . . ? O6 Tb1 O1 142.36(8) 7_556 . ? O5 Tb1 O1 73.10(8) . . ? O9 Tb1 O1 97.91(8) . . ? O3 Tb1 O1 81.22(8) . . ? O4 Tb1 O10 146.79(8) . . ? O6 Tb1 O10 74.26(8) 7_556 . ? O5 Tb1 O10 132.76(8) . . ? O9 Tb1 O10 73.37(8) . . ? O3 Tb1 O10 72.09(8) . . ? O1 Tb1 O10 69.26(7) . . ? O4 Tb1 O2 87.07(8) . . ? O6 Tb1 O2 152.69(8) 7_556 . ? O5 Tb1 O2 70.67(8) . . ? O9 Tb1 O2 73.82(8) . . ? O3 Tb1 O2 127.21(8) . . ? O1 Tb1 O2 51.25(7) . . ? O10 Tb1 O2 104.68(8) . . ? O4 Tb1 O4 76.48(8) . 7_556 ? O6 Tb1 O4 64.38(7) 7_556 7_556 ? O5 Tb1 O4 66.80(8) . 7_556 ? O9 Tb1 O4 139.85(8) . 7_556 ? O3 Tb1 O4 48.72(7) . 7_556 ? O1 Tb1 O4 121.43(7) . 7_556 ? O10 Tb1 O4 111.21(7) . 7_556 ? O2 Tb1 O4 136.27(7) . 7_556 ? O4 Tb1 C8 111.85(9) . . ? O6 Tb1 C8 158.52(8) 7_556 . ? O5 Tb1 C8 70.03(9) . . ? O9 Tb1 C8 85.39(9) . . ? O3 Tb1 C8 104.52(9) . . ? O1 Tb1 C8 25.53(9) . . ? O10 Tb1 C8 86.59(9) . . ? O2 Tb1 C8 25.72(8) . . ? O4 Tb1 C8 133.78(7) 7_556 . ? O4 Tb1 C9 101.23(8) . . ? O6 Tb1 C9 68.65(8) 7_556 . ? O5 Tb1 C9 70.60(9) . . ? O9 Tb1 C9 147.70(9) . . ? O3 Tb1 C9 24.07(8) . . ? O1 Tb1 C9 102.28(8) . . ? O10 Tb1 C9 90.50(8) . . ? O2 Tb1 C9 138.25(8) . . ? O4 Tb1 C9 24.75(7) 7_556 . ? C8 Tb1 C9 122.18(9) . . ? O13 Co N1 89.85(8) . 2_554 ? O13 Co N1 89.85(8) . . ? N1 Co N1 179.70(17) 2_554 . ? O13 Co O12 86.93(7) . 2_554 ? N1 Co O12 93.20(10) 2_554 2_554 ? N1 Co O12 86.78(10) . 2_554 ? O13 Co O12 86.93(7) . . ? N1 Co O12 86.78(10) 2_554 . ? N1 Co O12 93.20(10) . . ? O12 Co O12 173.86(13) 2_554 . ? O13 Co O11 180.0 . . ? N1 Co O11 90.15(8) 2_554 . ? N1 Co O11 90.15(8) . . ? O12 Co O11 93.07(7) 2_554 . ? O12 Co O11 93.07(7) . . ? O7 S O8 109.41(15) . . ? O7 S O6 110.24(15) . . ? O8 S O6 108.99(13) . . ? O7 S O5 108.91(15) . . ? O8 S O5 109.03(15) . . ? O6 S O5 110.25(14) . . ? C8 O1 Tb1 98.6(2) . . ? C8 O2 Tb1 89.9(2) . . ? C9 O3 Tb1 106.9(2) . . ? C9 O4 Tb1 174.0(2) 7_556 . ? C9 O4 Tb1 82.38(18) 7_556 7_556 ? Tb1 O4 Tb1 103.52(8) . 7_556 ? S O5 Tb1 141.18(15) . . ? S O6 Tb1 137.64(14) . 7_556 ? Tb1 O9 H9A 129.2 . . ? Tb1 O9 H9B 132.5 . . ? H9A O9 H9B 97.6 . . ? Tb1 O10 H10A 112.0 . . ? Tb1 O10 H10B 127.8 . . ? H10A O10 H10B 99.3 . . ? Co O11 H11A 120.0 . . ? Co O11 H11B 120.0 . . ? H11A O11 H11B 120.0 . . ? Co O12 H12A 120.0 . . ? Co O12 H12B 112.0 . . ? H12A O12 H12B 107.7 . . ? Co O13 H13 128.1 . . ? C7 N1 C4 105.1(3) . . ? C7 N1 Co 120.7(2) . . ? C4 N1 Co 131.9(2) . . ? C7 N2 C5 107.0(3) . . ? C7 N2 H2 126.5 . . ? C5 N2 H2 126.5 . . ? C6 C1 C2 121.0(3) . . ? C6 C1 C8 117.3(3) . . ? C2 C1 C8 121.5(3) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 C9 118.5(3) . 4_545 ? C1 C2 C9 120.3(3) . 4_545 ? C4 C3 C2 118.4(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 N1 131.7(3) . . ? C5 C4 N1 108.4(3) . . ? N2 C5 C6 131.4(3) . . ? N2 C5 C4 105.6(3) . . ? C6 C5 C4 123.0(3) . . ? C1 C6 C5 116.8(3) . . ? C1 C6 H6 121.6 . . ? C5 C6 H6 121.6 . . ? N1 C7 N2 113.8(3) . . ? N1 C7 H7 123.1 . . ? N2 C7 H7 123.1 . . ? O2 C8 O1 120.3(3) . . ? O2 C8 C1 120.7(3) . . ? O1 C8 C1 118.8(3) . . ? O2 C8 Tb1 64.43(18) . . ? O1 C8 Tb1 55.91(16) . . ? C1 C8 Tb1 173.9(2) . . ? O4 C9 O3 121.6(3) 7_556 . ? O4 C9 C2 120.5(3) 7_556 4 ? O3 C9 C2 117.8(3) . 4 ? O4 C9 Tb1 72.87(18) 7_556 . ? O3 C9 Tb1 49.05(16) . . ? C2 C9 Tb1 163.9(2) 4 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Tb1 O1 C8 -23.3(2) . . . . ? O6 Tb1 O1 C8 145.14(19) 7_556 . . . ? O5 Tb1 O1 C8 -78.93(19) . . . . ? O9 Tb1 O1 C8 61.37(19) . . . . ? O3 Tb1 O1 C8 -155.7(2) . . . . ? O10 Tb1 O1 C8 130.2(2) . . . . ? O2 Tb1 O1 C8 -0.45(18) . . . . ? O4 Tb1 O1 C8 -126.99(18) 7_556 . . . ? C9 Tb1 O1 C8 -144.00(19) . . . . ? O4 Tb1 O2 C8 164.75(19) . . . . ? O6 Tb1 O2 C8 -130.8(2) 7_556 . . . ? O5 Tb1 O2 C8 83.94(19) . . . . ? O9 Tb1 O2 C8 -114.2(2) . . . . ? O3 Tb1 O2 C8 31.7(2) . . . . ? O1 Tb1 O2 C8 0.45(17) . . . . ? O10 Tb1 O2 C8 -46.7(2) . . . . ? O4 Tb1 O2 C8 97.83(19) 7_556 . . . ? C9 Tb1 O2 C8 61.1(2) . . . . ? O4 Tb1 O3 C9 9.7(2) . . . . ? O6 Tb1 O3 C9 -61.4(2) 7_556 . . . ? O5 Tb1 O3 C9 76.1(2) . . . . ? O9 Tb1 O3 C9 -117.7(2) . . . . ? O1 Tb1 O3 C9 150.8(2) . . . . ? O10 Tb1 O3 C9 -138.2(2) . . . . ? O2 Tb1 O3 C9 126.7(2) . . . . ? O4 Tb1 O3 C9 3.92(18) 7_556 . . . ? C8 Tb1 O3 C9 140.3(2) . . . . ? O6 Tb1 O4 Tb1 65.61(8) 7_556 . . 7_556 ? O5 Tb1 O4 Tb1 -68.27(8) . . . 7_556 ? O9 Tb1 O4 Tb1 146.77(9) . . . 7_556 ? O3 Tb1 O4 Tb1 -4.44(12) . . . 7_556 ? O1 Tb1 O4 Tb1 -121.51(10) . . . 7_556 ? O10 Tb1 O4 Tb1 108.20(13) . . . 7_556 ? O2 Tb1 O4 Tb1 -139.15(8) . . . 7_556 ? O4 Tb1 O4 Tb1 0.0 7_556 . . 7_556 ? C8 Tb1 O4 Tb1 -132.09(8) . . . 7_556 ? C9 Tb1 O4 Tb1 -0.44(9) . . . 7_556 ? O7 S O5 Tb1 131.4(2) . . . . ? O8 S O5 Tb1 -109.3(2) . . . . ? O6 S O5 Tb1 10.3(3) . . . . ? O4 Tb1 O5 S 17.6(2) . . . . ? O6 Tb1 O5 S -52.1(3) 7_556 . . . ? O9 Tb1 O5 S 80.0(3) . . . . ? O3 Tb1 O5 S -112.9(2) . . . . ? O1 Tb1 O5 S 161.9(3) . . . . ? O10 Tb1 O5 S -159.8(2) . . . . ? O2 Tb1 O5 S 107.8(2) . . . . ? O4 Tb1 O5 S -61.8(2) 7_556 . . . ? C8 Tb1 O5 S 135.2(3) . . . . ? C9 Tb1 O5 S -88.0(2) . . . . ? O7 S O6 Tb1 -78.2(2) . . . 7_556 ? O8 S O6 Tb1 161.70(19) . . . 7_556 ? O5 S O6 Tb1 42.1(2) . . . 7_556 ? O13 Co N1 C7 48.9(3) . . . . ? O12 Co N1 C7 -38.0(3) 2_554 . . . ? O12 Co N1 C7 135.8(3) . . . . ? O11 Co N1 C7 -131.1(3) . . . . ? O13 Co N1 C4 -111.2(3) . . . . ? O12 Co N1 C4 161.9(3) 2_554 . . . ? O12 Co N1 C4 -24.2(3) . . . . ? O11 Co N1 C4 68.8(3) . . . . ? C6 C1 C2 C3 2.3(5) . . . . ? C8 C1 C2 C3 -172.1(3) . . . . ? C6 C1 C2 C9 -170.8(3) . . . 4_545 ? C8 C1 C2 C9 14.8(5) . . . 4_545 ? C1 C2 C3 C4 -1.4(5) . . . . ? C9 C2 C3 C4 171.8(3) 4_545 . . . ? C2 C3 C4 C5 -2.1(5) . . . . ? C2 C3 C4 N1 -179.4(3) . . . . ? C7 N1 C4 C3 176.0(4) . . . . ? Co N1 C4 C3 -21.7(6) . . . . ? C7 N1 C4 C5 -1.5(4) . . . . ? Co N1 C4 C5 160.8(2) . . . . ? C7 N2 C5 C6 177.6(4) . . . . ? C7 N2 C5 C4 -0.6(4) . . . . ? C3 C4 C5 N2 -176.6(3) . . . . ? N1 C4 C5 N2 1.3(4) . . . . ? C3 C4 C5 C6 5.0(5) . . . . ? N1 C4 C5 C6 -177.1(3) . . . . ? C2 C1 C6 C5 0.4(5) . . . . ? C8 C1 C6 C5 175.0(3) . . . . ? N2 C5 C6 C1 178.0(3) . . . . ? C4 C5 C6 C1 -4.0(5) . . . . ? C4 N1 C7 N2 1.2(4) . . . . ? Co N1 C7 N2 -163.6(2) . . . . ? C5 N2 C7 N1 -0.4(4) . . . . ? Tb1 O2 C8 O1 -0.8(3) . . . . ? Tb1 O2 C8 C1 -176.2(3) . . . . ? Tb1 O1 C8 O2 0.8(3) . . . . ? Tb1 O1 C8 C1 176.4(2) . . . . ? C6 C1 C8 O2 64.0(4) . . . . ? C2 C1 C8 O2 -121.4(4) . . . . ? C6 C1 C8 O1 -111.5(4) . . . . ? C2 C1 C8 O1 63.2(4) . . . . ? O4 Tb1 C8 O2 -16.4(2) . . . . ? O6 Tb1 C8 O2 108.4(3) 7_556 . . . ? O5 Tb1 C8 O2 -86.71(19) . . . . ? O9 Tb1 C8 O2 61.53(19) . . . . ? O3 Tb1 C8 O2 -154.39(18) . . . . ? O1 Tb1 C8 O2 -179.2(3) . . . . ? O10 Tb1 C8 O2 135.10(19) . . . . ? O4 Tb1 C8 O2 -108.48(19) 7_556 . . . ? C9 Tb1 C8 O2 -136.45(18) . . . . ? O4 Tb1 C8 O1 162.75(18) . . . . ? O6 Tb1 C8 O1 -72.4(3) 7_556 . . . ? O5 Tb1 C8 O1 92.5(2) . . . . ? O9 Tb1 C8 O1 -119.28(19) . . . . ? O3 Tb1 C8 O1 24.8(2) . . . . ? O10 Tb1 C8 O1 -45.71(19) . . . . ? O2 Tb1 C8 O1 179.2(3) . . . . ? O4 Tb1 C8 O1 70.7(2) 7_556 . . . ? C9 Tb1 C8 O1 42.7(2) . . . . ? Tb1 O3 C9 O4 -7.9(4) . . . 7_556 ? Tb1 O3 C9 C2 168.7(2) . . . 4 ? O4 Tb1 C9 O4 1.0(2) . . . 7_556 ? O6 Tb1 C9 O4 -74.86(17) 7_556 . . 7_556 ? O5 Tb1 C9 O4 76.49(18) . . . 7_556 ? O9 Tb1 C9 O4 -89.2(2) . . . 7_556 ? O3 Tb1 C9 O4 173.0(3) . . . 7_556 ? O1 Tb1 C9 O4 143.41(16) . . . 7_556 ? O10 Tb1 C9 O4 -147.72(17) . . . 7_556 ? O2 Tb1 C9 O4 99.31(18) . . . 7_556 ? C8 Tb1 C9 O4 125.99(17) . . . 7_556 ? O4 Tb1 C9 O3 -171.9(2) . . . . ? O6 Tb1 C9 O3 112.2(2) 7_556 . . . ? O5 Tb1 C9 O3 -96.5(2) . . . . ? O9 Tb1 C9 O3 97.9(2) . . . . ? O1 Tb1 C9 O3 -29.5(2) . . . . ? O10 Tb1 C9 O3 39.3(2) . . . . ? O2 Tb1 C9 O3 -73.6(2) . . . . ? O4 Tb1 C9 O3 -173.0(3) 7_556 . . . ? C8 Tb1 C9 O3 -47.0(2) . . . . ? O4 Tb1 C9 C2 149.3(8) . . . 4 ? O6 Tb1 C9 C2 73.4(8) 7_556 . . 4 ? O5 Tb1 C9 C2 -135.2(8) . . . 4 ? O9 Tb1 C9 C2 59.1(8) . . . 4 ? O3 Tb1 C9 C2 -38.7(7) . . . 4 ? O1 Tb1 C9 C2 -68.3(8) . . . 4 ? O10 Tb1 C9 C2 0.6(8) . . . 4 ? O2 Tb1 C9 C2 -112.4(7) . . . 4 ? O4 Tb1 C9 C2 148.3(9) 7_556 . . 4 ? C8 Tb1 C9 C2 -85.7(8) . . . 4 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.614 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.105