# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email sundi28@126.com loop_ _publ_author_name 'Yaguang Sun' 'Gang Xiong' 'Fu Ding' data_1 _database_code_depnum_ccdc_archive 'CCDC 862562' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N4 Ni O24 Pr2 S2' _chemical_formula_weight 1085.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 22.656(7) _cell_length_b 8.645(2) _cell_length_c 15.634(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.471(6) _cell_angle_gamma 90.00 _cell_volume 2989.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3548 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.88 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 4.082 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4408 _exptl_absorpt_correction_T_max 0.5110 _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 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _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 13327 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0532 _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 -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3548 _reflns_number_gt 3018 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3548 _refine_ls_number_parameters 244 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 3.344 _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 O5 O 0.2914(3) 0.6831(9) 0.7797(5) 0.0154(17) Uani 1 1 d . . . O4 O 0.3599(4) 0.5720(9) 0.7207(5) 0.0179(18) Uani 1 1 d . . . C9 C 0.3434(5) 0.6231(12) 0.7874(8) 0.012(2) Uani 1 1 d . . . O7 O 0.1631(3) 0.4273(9) 1.0092(5) 0.0148(17) Uani 1 1 d . . . S1 S 0.14696(11) 0.4666(3) 0.91512(18) 0.0107(6) Uani 1 1 d . . . C1 C 0.3242(5) 0.4244(12) 0.9325(7) 0.011(2) Uani 1 1 d . . . C2 C 0.3722(5) 0.5451(12) 0.9483(7) 0.011(2) Uani 1 1 d . . . C8 C 0.3855(5) 0.6265(12) 0.8756(7) 0.011(2) Uani 1 1 d . . . C3 C 0.4071(5) 0.5648(12) 1.0322(7) 0.013(2) Uani 1 1 d . . . H3 H 0.3976 0.5142 1.0800 0.015 Uiso 1 1 calc R . . C5 C 0.5372(5) 0.7997(14) 1.0866(8) 0.018(3) Uani 1 1 d . . . H5 H 0.5707 0.8458 1.1224 0.022 Uiso 1 1 calc R . . C6 C 0.4710(5) 0.7372(13) 0.9698(7) 0.013(2) Uani 1 1 d . . . C4 C 0.4571(5) 0.6635(12) 1.0424(8) 0.014(2) Uani 1 1 d . . . N1 N 0.4996(4) 0.7079(11) 1.1167(6) 0.016(2) Uani 1 1 d . . . O12 O 0.3224(3) 0.0452(9) 0.7946(5) 0.0190(18) Uani 1 1 d . . . H12A H 0.3536 0.0986 0.7928 0.023 Uiso 1 1 d R . . H12B H 0.3164 -0.0404 0.7674 0.023 Uiso 1 1 d R . . O9 O 0.5000 0.4648(16) 1.2500 0.038(4) Uani 1 2 d SD . . O1 O 0.1809(4) 0.3684(9) 0.8653(5) 0.020(2) Uani 1 1 d . . . O3 O 0.2979(3) 0.3867(8) 0.9936(5) 0.0128(17) Uani 1 1 d . . . O2 O 0.3129(4) 0.3571(8) 0.8592(5) 0.0147(18) Uani 1 1 d . . . Pr1 Pr 0.24670(2) 0.14147(7) 0.88208(4) 0.0087(2) Uani 1 1 d . . . Ni2 Ni 0.5000 0.7047(3) 1.2500 0.0173(5) Uani 1 2 d S . . O13 O 0.2397(4) -0.1415(8) 0.8845(5) 0.020(2) Uani 1 1 d . . . H13A H 0.2703 -0.1950 0.9087 0.024 Uiso 1 1 d R . . H13B H 0.2067 -0.1862 0.8612 0.024 Uiso 1 1 d R . . O8 O 0.0821(3) 0.4391(10) 0.8829(5) 0.0198(19) Uani 1 1 d . . . N2 N 0.5224(4) 0.8196(11) 1.0005(6) 0.016(2) Uani 1 1 d . . . H2 H 0.5417 0.8745 0.9697 0.019 Uiso 1 1 calc R . . O11 O 0.5000 0.9429(15) 1.2500 0.036(4) Uani 1 2 d SD . . C7 C 0.4351(5) 0.7227(13) 0.8855(7) 0.013(2) Uani 1 1 d . . . H7 H 0.4443 0.7755 0.8382 0.016 Uiso 1 1 calc R . . O10 O 0.4074(4) 0.7157(10) 1.2286(5) 0.022(2) Uani 1 1 d D . . O6 O 0.1606(4) 0.6294(9) 0.9021(6) 0.022(2) Uani 1 1 d . . . H11A H 0.479(5) 1.011(10) 1.219(7) 0.027 Uiso 1 1 d D . . H10A H 0.391(5) 0.628(8) 1.230(8) 0.027 Uiso 1 1 d D . . H10B H 0.394(6) 0.763(11) 1.187(8) 0.027 Uiso 1 1 d D . . H9A H 0.468(3) 0.418(14) 1.227(9) 0.027 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 O5 0.013(4) 0.023(4) 0.009(4) 0.000(4) 0.002(3) 0.002(3) O4 0.025(5) 0.019(4) 0.009(4) -0.001(4) 0.003(3) 0.008(4) C9 0.016(6) 0.008(5) 0.014(6) 0.001(4) 0.005(5) -0.003(4) O7 0.012(4) 0.021(4) 0.010(4) 0.002(4) 0.001(3) 0.002(3) S1 0.0090(13) 0.0117(13) 0.0109(14) 0.0018(11) 0.0011(10) 0.0003(10) C1 0.012(5) 0.009(5) 0.010(6) 0.004(5) 0.000(4) 0.001(4) C2 0.010(5) 0.011(5) 0.014(6) 0.000(5) 0.003(4) -0.002(4) C8 0.012(5) 0.012(6) 0.009(6) -0.001(4) 0.001(4) 0.001(4) C3 0.017(6) 0.012(6) 0.010(6) 0.001(5) 0.004(5) -0.002(4) C5 0.014(6) 0.020(6) 0.019(7) -0.001(5) -0.001(5) -0.002(5) C6 0.010(5) 0.014(6) 0.015(6) 0.003(5) 0.002(4) 0.002(4) C4 0.013(6) 0.015(6) 0.013(6) -0.001(5) 0.002(5) 0.000(4) N1 0.017(5) 0.017(5) 0.011(5) 0.000(4) -0.003(4) -0.004(4) O12 0.018(4) 0.021(4) 0.019(4) -0.007(4) 0.006(3) 0.000(3) O9 0.063(11) 0.020(8) 0.035(9) 0.000 0.022(8) 0.000 O1 0.023(5) 0.023(5) 0.011(4) -0.002(4) 0.001(4) 0.012(3) O3 0.012(4) 0.016(4) 0.011(4) 0.002(3) 0.003(3) -0.002(3) O2 0.020(4) 0.013(4) 0.012(4) -0.004(3) 0.004(3) -0.006(3) Pr1 0.0094(3) 0.0092(4) 0.0072(4) 0.0000(2) 0.0009(3) -0.0007(2) Ni2 0.0210(12) 0.0141(11) 0.0138(12) 0.000 -0.0029(9) 0.000 O13 0.016(4) 0.009(4) 0.035(6) 0.000(3) 0.004(4) 0.000(3) O8 0.007(4) 0.031(5) 0.019(4) 0.010(4) -0.002(3) -0.004(3) N2 0.016(5) 0.015(5) 0.015(5) 0.004(4) 0.001(4) -0.004(4) O11 0.044(9) 0.016(7) 0.034(9) 0.000 -0.026(7) 0.000 C7 0.014(6) 0.015(6) 0.012(6) 0.002(5) 0.003(4) -0.001(4) O10 0.028(5) 0.019(5) 0.014(5) 0.003(4) -0.005(4) -0.010(4) O6 0.024(5) 0.013(4) 0.027(5) 0.007(4) -0.001(4) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O5 C9 1.270(13) . ? O5 Pr1 2.515(7) 4_556 ? O4 C9 1.260(13) . ? O4 Pr1 2.665(7) 4_556 ? C9 C8 1.498(15) . ? C9 Pr1 2.979(11) 4_556 ? O7 S1 1.477(8) . ? O7 Pr1 2.433(7) 7_557 ? S1 O6 1.465(8) . ? S1 O8 1.467(7) . ? S1 O1 1.476(8) . ? C1 O2 1.262(13) . ? C1 O3 1.271(13) . ? C1 C2 1.489(14) . ? C2 C3 1.388(14) . ? C2 C8 1.424(15) . ? C8 C7 1.380(14) . ? C3 C4 1.400(15) . ? C3 H3 0.9300 . ? C5 N1 1.323(14) . ? C5 N2 1.327(14) . ? C5 H5 0.9300 . ? C6 N2 1.362(13) . ? C6 C4 1.396(16) . ? C6 C7 1.396(14) . ? C4 N1 1.393(13) . ? N1 Ni2 2.083(10) . ? O12 Pr1 2.551(8) . ? O12 H12A 0.8502 . ? O12 H12B 0.8499 . ? O9 Ni2 2.074(14) . ? O9 H9A 0.850(4) . ? O1 Pr1 2.443(7) . ? O3 Pr1 2.390(8) 7_557 ? O3 Pr1 2.830(7) . ? O2 Pr1 2.467(7) . ? Pr1 O3 2.390(8) 7_557 ? Pr1 O7 2.433(7) 7_557 ? Pr1 O13 2.453(7) . ? Pr1 O5 2.515(7) 4_546 ? Pr1 O4 2.665(7) 4_546 ? Pr1 C9 2.979(11) 4_546 ? Pr1 Pr1 4.1112(14) 7_557 ? Ni2 O10 2.054(9) 2_657 ? Ni2 O10 2.054(9) . ? Ni2 O11 2.059(13) . ? Ni2 N1 2.083(10) 2_657 ? O13 H13A 0.8500 . ? O13 H13B 0.8499 . ? N2 H2 0.8600 . ? O11 H11A 0.85(3) . ? C7 H7 0.9300 . ? O10 H10A 0.84(3) . ? O10 H10B 0.77(9) . ? 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 O5 Pr1 98.4(7) . 4_556 ? C9 O4 Pr1 91.6(7) . 4_556 ? O4 C9 O5 120.0(10) . . ? O4 C9 C8 121.6(10) . . ? O5 C9 C8 118.2(10) . . ? O4 C9 Pr1 63.4(6) . 4_556 ? O5 C9 Pr1 56.6(5) . 4_556 ? C8 C9 Pr1 174.5(8) . 4_556 ? S1 O7 Pr1 137.9(5) . 7_557 ? O6 S1 O8 109.5(5) . . ? O6 S1 O1 109.2(5) . . ? O8 S1 O1 108.9(5) . . ? O6 S1 O7 110.2(5) . . ? O8 S1 O7 108.6(5) . . ? O1 S1 O7 110.4(5) . . ? O2 C1 O3 121.9(10) . . ? O2 C1 C2 118.1(10) . . ? O3 C1 C2 119.9(10) . . ? C3 C2 C8 121.2(10) . . ? C3 C2 C1 119.3(10) . . ? C8 C2 C1 119.2(9) . . ? C7 C8 C2 121.1(10) . . ? C7 C8 C9 117.2(10) . . ? C2 C8 C9 121.5(10) . . ? C2 C3 C4 117.7(10) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? N1 C5 N2 113.4(10) . . ? N1 C5 H5 123.3 . . ? N2 C5 H5 123.3 . . ? N2 C6 C4 106.2(9) . . ? N2 C6 C7 131.2(11) . . ? C4 C6 C7 122.6(10) . . ? N1 C4 C6 108.4(10) . . ? N1 C4 C3 131.3(11) . . ? C6 C4 C3 120.3(10) . . ? C5 N1 C4 104.5(10) . . ? C5 N1 Ni2 120.0(8) . . ? C4 N1 Ni2 133.2(8) . . ? Pr1 O12 H12A 120.0 . . ? Pr1 O12 H12B 120.0 . . ? H12A O12 H12B 120.0 . . ? Ni2 O9 H9A 119(10) . . ? S1 O1 Pr1 141.3(5) . . ? C1 O3 Pr1 170.3(7) . 7_557 ? C1 O3 Pr1 85.7(6) . . ? Pr1 O3 Pr1 103.6(3) 7_557 . ? C1 O2 Pr1 103.1(7) . . ? O3 Pr1 O7 81.2(2) 7_557 7_557 ? O3 Pr1 O1 79.3(3) 7_557 . ? O7 Pr1 O1 132.2(3) 7_557 . ? O3 Pr1 O13 81.1(3) 7_557 . ? O7 Pr1 O13 78.0(3) 7_557 . ? O1 Pr1 O13 139.7(3) . . ? O3 Pr1 O2 124.9(3) 7_557 . ? O7 Pr1 O2 80.9(3) 7_557 . ? O1 Pr1 O2 75.7(3) . . ? O13 Pr1 O2 143.1(3) . . ? O3 Pr1 O5 136.0(2) 7_557 4_546 ? O7 Pr1 O5 142.3(3) 7_557 4_546 ? O1 Pr1 O5 73.0(3) . 4_546 ? O13 Pr1 O5 98.6(3) . 4_546 ? O2 Pr1 O5 80.4(3) . 4_546 ? O3 Pr1 O12 148.6(2) 7_557 . ? O7 Pr1 O12 74.6(2) 7_557 . ? O1 Pr1 O12 132.0(3) . . ? O13 Pr1 O12 74.7(3) . . ? O2 Pr1 O12 70.7(3) . . ? O5 Pr1 O12 68.4(2) 4_546 . ? O3 Pr1 O4 88.9(2) 7_557 4_546 ? O7 Pr1 O4 151.8(3) 7_557 4_546 ? O1 Pr1 O4 70.3(3) . 4_546 ? O13 Pr1 O4 74.4(2) . 4_546 ? O2 Pr1 O4 125.6(2) . 4_546 ? O5 Pr1 O4 49.9(2) 4_546 4_546 ? O12 Pr1 O4 103.3(2) . 4_546 ? O3 Pr1 O3 76.4(3) 7_557 . ? O7 Pr1 O3 65.3(2) 7_557 . ? O1 Pr1 O3 67.9(2) . . ? O13 Pr1 O3 139.2(2) . . ? O2 Pr1 O3 48.8(2) . . ? O5 Pr1 O3 121.2(2) 4_546 . ? O12 Pr1 O3 109.9(2) . . ? O4 Pr1 O3 137.6(2) 4_546 . ? O3 Pr1 C9 112.9(3) 7_557 4_546 ? O7 Pr1 C9 156.8(3) 7_557 4_546 ? O1 Pr1 C9 70.3(3) . 4_546 ? O13 Pr1 C9 85.8(3) . 4_546 ? O2 Pr1 C9 103.4(3) . 4_546 ? O5 Pr1 C9 24.9(3) 4_546 4_546 ? O12 Pr1 C9 85.2(3) . 4_546 ? O4 Pr1 C9 25.0(3) 4_546 4_546 ? O3 Pr1 C9 134.4(2) . 4_546 ? O3 Pr1 Pr1 41.98(17) 7_557 7_557 ? O7 Pr1 Pr1 67.84(18) 7_557 7_557 ? O1 Pr1 Pr1 68.47(19) . 7_557 ? O13 Pr1 Pr1 115.6(2) . 7_557 ? O2 Pr1 Pr1 83.09(18) . 7_557 ? O5 Pr1 Pr1 140.76(19) 4_546 7_557 ? O12 Pr1 Pr1 136.96(17) . 7_557 ? O4 Pr1 Pr1 119.76(18) 4_546 7_557 ? O3 Pr1 Pr1 34.39(16) . 7_557 ? C9 Pr1 Pr1 135.0(2) 4_546 7_557 ? O10 Ni2 O10 174.7(5) 2_657 . ? O10 Ni2 O11 87.3(3) 2_657 . ? O10 Ni2 O11 87.3(3) . . ? O10 Ni2 O9 92.7(3) 2_657 . ? O10 Ni2 O9 92.7(3) . . ? O11 Ni2 O9 180.000(10) . . ? O10 Ni2 N1 93.0(3) 2_657 2_657 ? O10 Ni2 N1 86.9(3) . 2_657 ? O11 Ni2 N1 89.2(3) . 2_657 ? O9 Ni2 N1 90.8(3) . 2_657 ? O10 Ni2 N1 86.9(3) 2_657 . ? O10 Ni2 N1 93.0(3) . . ? O11 Ni2 N1 89.2(3) . . ? O9 Ni2 N1 90.8(3) . . ? N1 Ni2 N1 178.5(6) 2_657 . ? Pr1 O13 H13A 120.0 . . ? Pr1 O13 H13B 120.0 . . ? H13A O13 H13B 120.0 . . ? C5 N2 C6 107.4(10) . . ? C5 N2 H2 126.3 . . ? C6 N2 H2 126.3 . . ? Ni2 O11 H11A 134(8) . . ? C8 C7 C6 117.0(10) . . ? C8 C7 H7 121.5 . . ? C6 C7 H7 121.5 . . ? Ni2 O10 H10A 113(9) . . ? Ni2 O10 H10B 111(9) . . ? H10A O10 H10B 114(9) . . ? 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 Pr1 O4 C9 O5 -2.2(10) 4_556 . . . ? Pr1 O4 C9 C8 -177.3(9) 4_556 . . . ? Pr1 O5 C9 O4 2.4(11) 4_556 . . . ? Pr1 O5 C9 C8 177.6(8) 4_556 . . . ? Pr1 O7 S1 O6 -81.3(8) 7_557 . . . ? Pr1 O7 S1 O8 158.7(6) 7_557 . . . ? Pr1 O7 S1 O1 39.4(8) 7_557 . . . ? O2 C1 C2 C3 -147.3(10) . . . . ? O3 C1 C2 C3 29.4(15) . . . . ? O2 C1 C2 C8 26.1(15) . . . . ? O3 C1 C2 C8 -157.2(10) . . . . ? C3 C2 C8 C7 2.8(17) . . . . ? C1 C2 C8 C7 -170.5(10) . . . . ? C3 C2 C8 C9 -171.4(10) . . . . ? C1 C2 C8 C9 15.3(16) . . . . ? O4 C9 C8 C7 65.4(14) . . . . ? O5 C9 C8 C7 -109.8(12) . . . . ? Pr1 C9 C8 C7 -89(8) 4_556 . . . ? O4 C9 C8 C2 -120.2(12) . . . . ? O5 C9 C8 C2 64.6(14) . . . . ? Pr1 C9 C8 C2 86(8) 4_556 . . . ? C8 C2 C3 C4 -2.1(16) . . . . ? C1 C2 C3 C4 171.2(10) . . . . ? N2 C6 C4 N1 2.2(12) . . . . ? C7 C6 C4 N1 -176.8(10) . . . . ? N2 C6 C4 C3 -178.0(10) . . . . ? C7 C6 C4 C3 3.0(17) . . . . ? C2 C3 C4 N1 179.1(11) . . . . ? C2 C3 C4 C6 -0.7(16) . . . . ? N2 C5 N1 C4 0.7(14) . . . . ? N2 C5 N1 Ni2 -164.1(8) . . . . ? C6 C4 N1 C5 -1.8(13) . . . . ? C3 C4 N1 C5 178.5(12) . . . . ? C6 C4 N1 Ni2 160.1(8) . . . . ? C3 C4 N1 Ni2 -19.6(19) . . . . ? O6 S1 O1 Pr1 131.0(7) . . . . ? O8 S1 O1 Pr1 -109.4(8) . . . . ? O7 S1 O1 Pr1 9.7(9) . . . . ? O2 C1 O3 Pr1 -159(3) . . . 7_557 ? C2 C1 O3 Pr1 25(5) . . . 7_557 ? O2 C1 O3 Pr1 6.3(10) . . . . ? C2 C1 O3 Pr1 -170.3(9) . . . . ? O3 C1 O2 Pr1 -7.4(12) . . . . ? C2 C1 O2 Pr1 169.3(7) . . . . ? S1 O1 Pr1 O3 17.5(8) . . . 7_557 ? S1 O1 Pr1 O7 -50.0(10) . . . 7_557 ? S1 O1 Pr1 O13 79.7(9) . . . . ? S1 O1 Pr1 O2 -113.0(8) . . . . ? S1 O1 Pr1 O5 162.9(9) . . . 4_546 ? S1 O1 Pr1 O12 -159.5(7) . . . . ? S1 O1 Pr1 O4 110.1(8) . . . 4_546 ? S1 O1 Pr1 O3 -62.0(8) . . . . ? S1 O1 Pr1 C9 136.7(9) . . . 4_546 ? S1 O1 Pr1 Pr1 -24.9(7) . . . 7_557 ? C1 O2 Pr1 O3 11.1(7) . . . 7_557 ? C1 O2 Pr1 O7 -61.3(6) . . . 7_557 ? C1 O2 Pr1 O1 76.7(7) . . . . ? C1 O2 Pr1 O13 -117.0(7) . . . . ? C1 O2 Pr1 O5 151.5(7) . . . 4_546 ? C1 O2 Pr1 O12 -138.1(7) . . . . ? C1 O2 Pr1 O4 129.1(6) . . . 4_546 ? C1 O2 Pr1 O3 3.7(6) . . . . ? C1 O2 Pr1 C9 141.9(7) . . . 4_546 ? C1 O2 Pr1 Pr1 7.2(6) . . . 7_557 ? C1 O3 Pr1 O3 -177.4(7) . . . 7_557 ? Pr1 O3 Pr1 O3 0.0 7_557 . . 7_557 ? C1 O3 Pr1 O7 96.2(6) . . . 7_557 ? Pr1 O3 Pr1 O7 -86.4(3) 7_557 . . 7_557 ? C1 O3 Pr1 O1 -93.7(6) . . . . ? Pr1 O3 Pr1 O1 83.8(3) 7_557 . . . ? C1 O3 Pr1 O13 124.2(6) . . . . ? Pr1 O3 Pr1 O13 -58.4(5) 7_557 . . . ? C1 O3 Pr1 O2 -3.6(6) . . . . ? Pr1 O3 Pr1 O2 173.8(4) 7_557 . . . ? C1 O3 Pr1 O5 -41.5(6) . . . 4_546 ? Pr1 O3 Pr1 O5 135.9(3) 7_557 . . 4_546 ? C1 O3 Pr1 O12 34.7(6) . . . . ? Pr1 O3 Pr1 O12 -147.9(3) 7_557 . . . ? C1 O3 Pr1 O4 -104.6(6) . . . 4_546 ? Pr1 O3 Pr1 O4 72.8(4) 7_557 . . 4_546 ? C1 O3 Pr1 C9 -68.6(7) . . . 4_546 ? Pr1 O3 Pr1 C9 108.8(4) 7_557 . . 4_546 ? C1 O3 Pr1 Pr1 -177.4(7) . . . 7_557 ? C5 N1 Ni2 O10 -40.6(9) . . . 2_657 ? C4 N1 Ni2 O10 159.7(11) . . . 2_657 ? C5 N1 Ni2 O10 134.1(9) . . . . ? C4 N1 Ni2 O10 -25.6(11) . . . . ? C5 N1 Ni2 O11 46.8(9) . . . . ? C4 N1 Ni2 O11 -112.9(10) . . . . ? C5 N1 Ni2 O9 -133.2(9) . . . . ? C4 N1 Ni2 O9 67.1(10) . . . . ? C5 N1 Ni2 N1 46.8(9) . . . 2_657 ? C4 N1 Ni2 N1 -112.9(10) . . . 2_657 ? N1 C5 N2 C6 0.6(14) . . . . ? C4 C6 N2 C5 -1.7(12) . . . . ? C7 C6 N2 C5 177.2(12) . . . . ? C2 C8 C7 C6 -0.5(16) . . . . ? C9 C8 C7 C6 173.9(10) . . . . ? N2 C6 C7 C8 179.0(11) . . . . ? C4 C6 C7 C8 -2.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.046 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.149 data_2 _database_code_depnum_ccdc_archive 'CCDC 862563' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N4 Ni O24 S2 Sm2' _chemical_formula_weight 1103.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 22.704(8) _cell_length_b 8.590(2) _cell_length_c 15.513(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.450(6) _cell_angle_gamma 90.00 _cell_volume 2954.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3522 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 27.88 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 4.808 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3264 _exptl_absorpt_correction_T_max 0.4782 _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 13232 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -28 _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 1.84 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3522 _reflns_number_gt 2833 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3522 _refine_ls_number_parameters 256 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 2.397 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O7 O 0.1831(2) 0.3653(6) -0.1348(4) 0.0172(13) Uani 1 1 d . . . N2 N -0.0220(3) -0.3196(7) 0.0020(5) 0.0155(15) Uani 1 1 d . . . H2 H -0.0412 -0.3745 0.0334 0.019 Uiso 1 1 calc R . . O12 O 0.2597(3) 0.6374(6) 0.1154(4) 0.0198(14) Uani 1 1 d D . . O9 O 0.0926(3) -0.2176(7) -0.2291(4) 0.0224(14) Uani 1 1 d D . . O8 O 0.0836(2) 0.4351(6) -0.1187(4) 0.0185(13) Uani 1 1 d . . . O6 O 0.1620(3) 0.6277(6) -0.0982(4) 0.0194(13) Uani 1 1 d . . . O1 O 0.1415(2) -0.0700(6) 0.2816(3) 0.0178(12) Uani 1 1 d . . . O2 O 0.2102(2) -0.1806(6) 0.2221(4) 0.0151(12) Uani 1 1 d . . . C9 C 0.1582(3) -0.1219(8) 0.2147(5) 0.0118(16) Uani 1 1 d . . . Sm1 Sm 0.252929(17) 0.35901(4) 0.11753(3) 0.00844(13) Uani 1 1 d . . . Ni2 Ni 0.0000 -0.20622(16) -0.2500 0.0162(3) Uani 1 2 d S . . O3 O 0.1879(2) 0.1462(5) 0.1391(4) 0.0127(12) Uani 1 1 d . . . O5 O 0.1645(2) 0.4241(6) 0.0096(3) 0.0133(11) Uani 1 1 d . . . O10 O 0.0000 0.0360(11) -0.2500 0.040(3) Uani 1 2 d SD . . O4 O 0.2029(2) 0.1110(5) 0.0042(3) 0.0117(12) Uani 1 1 d . . . C8 C 0.1158(3) -0.1260(8) 0.1259(5) 0.0111(16) Uani 1 1 d . . . C4 C 0.0437(4) -0.1655(8) -0.0419(5) 0.0140(17) Uani 1 1 d . . . O13 O 0.1782(3) 0.4576(7) 0.2025(4) 0.0191(13) Uani 1 1 d D . . C5 C -0.0375(4) -0.2996(9) -0.0851(6) 0.0191(18) Uani 1 1 d . . . H5 H -0.0716 -0.3442 -0.1206 0.023 Uiso 1 1 calc R . . C6 C 0.0299(3) -0.2372(9) 0.0326(5) 0.0139(17) Uani 1 1 d . . . C3 C 0.0936(3) -0.0659(9) -0.0320(5) 0.0137(17) Uani 1 1 d . . . H3 H 0.1027 -0.0150 -0.0804 0.016 Uiso 1 1 calc R . . N1 N 0.0011(3) -0.2088(7) -0.1162(4) 0.0168(15) Uani 1 1 d . . . C1 C 0.1765(3) 0.0750(8) 0.0660(5) 0.0105(15) Uani 1 1 d U . . C2 C 0.1288(3) -0.0452(8) 0.0519(5) 0.0104(16) Uani 1 1 d . . . C7 C 0.0661(3) -0.2223(9) 0.1165(5) 0.0134(17) Uani 1 1 d . . . H7 H 0.0573 -0.2750 0.1645 0.016 Uiso 1 1 calc R . . O11 O 0.0000 -0.4458(10) -0.2500 0.037(3) Uani 1 2 d SD . . S1 S 0.14848(8) 0.4638(2) -0.08505(13) 0.0101(4) Uani 1 1 d . . . H12A H 0.240(3) 0.677(7) 0.148(4) 0.012 Uiso 1 1 d D . . H11A H 0.023(3) -0.502(7) -0.214(4) 0.012 Uiso 1 1 d D . . H9A H 0.109(3) -0.130(4) -0.231(4) 0.012 Uiso 1 1 d D . . H9B H 0.112(3) -0.262(7) -0.183(3) 0.012 Uiso 1 1 d D . . H12B H 0.280(3) 0.704(6) 0.096(5) 0.012 Uiso 1 1 d D . . H13A H 0.163(3) 0.378(5) 0.221(4) 0.012 Uiso 1 1 d D . . H13B H 0.186(3) 0.519(6) 0.246(3) 0.012 Uiso 1 1 d D . . H10A H 0.0348(19) 0.074(9) -0.238(6) 0.012 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 O7 0.020(3) 0.021(3) 0.009(3) -0.002(2) 0.000(2) 0.011(2) N2 0.015(3) 0.015(3) 0.016(4) 0.003(3) 0.001(3) -0.005(3) O12 0.022(3) 0.010(3) 0.031(4) -0.003(3) 0.013(3) -0.002(2) O9 0.029(4) 0.018(3) 0.015(4) 0.004(3) -0.007(3) -0.010(3) O8 0.009(3) 0.027(3) 0.017(3) 0.008(3) -0.003(2) -0.004(2) O6 0.023(3) 0.012(3) 0.021(3) 0.003(2) -0.001(3) -0.004(2) O1 0.025(3) 0.019(3) 0.010(3) 0.000(3) 0.005(2) 0.008(3) O2 0.015(3) 0.021(3) 0.009(3) 0.000(2) 0.001(2) 0.002(2) C9 0.017(4) 0.008(4) 0.011(4) 0.002(3) 0.005(3) -0.004(3) Sm1 0.0094(2) 0.0092(2) 0.0066(2) 0.00028(16) 0.00161(15) -0.00037(15) Ni2 0.0223(8) 0.0116(7) 0.0110(8) 0.000 -0.0045(6) 0.000 O3 0.017(3) 0.013(3) 0.009(3) -0.002(2) 0.003(2) -0.005(2) O5 0.013(3) 0.019(3) 0.008(3) 0.004(2) 0.002(2) 0.003(2) O10 0.071(8) 0.017(5) 0.040(7) 0.000 0.031(7) 0.000 O4 0.011(3) 0.016(3) 0.009(3) 0.002(2) 0.003(2) -0.001(2) C8 0.013(4) 0.012(4) 0.009(4) 0.001(3) 0.003(3) 0.002(3) C4 0.014(4) 0.014(4) 0.013(4) 0.000(3) 0.000(3) -0.001(3) O13 0.023(3) 0.021(3) 0.014(3) -0.005(3) 0.006(3) 0.001(3) C5 0.015(4) 0.019(4) 0.021(5) 0.002(4) 0.000(4) -0.004(3) C6 0.011(4) 0.014(4) 0.018(5) 0.003(3) 0.005(3) -0.002(3) C3 0.019(4) 0.014(4) 0.009(4) 0.002(3) 0.005(3) -0.003(3) N1 0.018(4) 0.018(3) 0.012(4) 0.001(3) -0.002(3) -0.007(3) C1 0.011(4) 0.010(3) 0.011(4) 0.005(3) 0.001(3) 0.006(3) C2 0.012(4) 0.011(4) 0.009(4) 0.000(3) 0.002(3) -0.001(3) C7 0.014(4) 0.013(4) 0.014(5) 0.000(3) 0.005(3) -0.001(3) O11 0.047(6) 0.009(4) 0.035(6) 0.000 -0.033(5) 0.000 S1 0.0093(9) 0.0111(9) 0.0098(10) 0.0013(8) 0.0016(8) 0.0004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O7 S1 1.479(5) . ? O7 Sm1 2.394(5) 7 ? N2 C5 1.331(10) . ? N2 C6 1.369(9) . ? N2 H2 0.8600 . ? O12 Sm1 2.397(5) . ? O12 H12A 0.82(2) . ? O12 H12B 0.83(2) . ? O9 Ni2 2.059(6) . ? O9 H9A 0.84(2) . ? O9 H9B 0.84(2) . ? O8 S1 1.474(5) . ? O6 S1 1.464(5) . ? O1 C9 1.261(9) . ? O1 Sm1 2.636(6) 4_545 ? O2 C9 1.266(9) . ? O2 Sm1 2.472(5) 4_545 ? C9 C8 1.501(11) . ? C9 Sm1 2.935(8) 4_545 ? Sm1 O4 2.336(5) 7 ? Sm1 O5 2.387(5) . ? Sm1 O7 2.394(5) 7 ? Sm1 O3 2.417(5) . ? Sm1 O2 2.472(5) 4 ? Sm1 O13 2.510(5) . ? Sm1 O1 2.636(6) 4 ? Sm1 O4 2.839(5) . ? Sm1 C9 2.935(8) 4 ? Sm1 Sm1 4.0760(12) 7 ? Ni2 O11 2.058(8) . ? Ni2 O9 2.059(6) 2_554 ? Ni2 N1 2.070(7) 2_554 ? Ni2 N1 2.070(7) . ? Ni2 O10 2.080(9) . ? O3 C1 1.265(9) . ? O5 S1 1.475(5) . ? O10 H10A 0.84(2) . ? O4 C1 1.273(8) . ? O4 Sm1 2.336(5) 7 ? C8 C7 1.380(10) . ? C8 C2 1.426(10) . ? C4 N1 1.387(10) . ? C4 C3 1.401(10) . ? C4 C6 1.404(10) . ? O13 H13A 0.84(2) . ? O13 H13B 0.84(2) . ? C5 N1 1.339(10) . ? C5 H5 0.9300 . ? C6 C7 1.387(10) . ? C3 C2 1.383(10) . ? C3 H3 0.9300 . ? C1 C2 1.479(10) . ? C7 H7 0.9300 . ? O11 H11A 0.83(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 O7 Sm1 141.2(3) . 7 ? C5 N2 C6 107.7(6) . . ? C5 N2 H2 126.1 . . ? C6 N2 H2 126.1 . . ? Sm1 O12 H12A 111(4) . . ? Sm1 O12 H12B 137(4) . . ? H12A O12 H12B 111(4) . . ? Ni2 O9 H9A 113(5) . . ? Ni2 O9 H9B 120(5) . . ? H9A O9 H9B 107(4) . . ? C9 O1 Sm1 90.6(5) . 4_545 ? C9 O2 Sm1 98.3(5) . 4_545 ? O1 C9 O2 120.4(7) . . ? O1 C9 C8 121.1(7) . . ? O2 C9 C8 118.3(7) . . ? O1 C9 Sm1 63.9(4) . 4_545 ? O2 C9 Sm1 56.5(4) . 4_545 ? C8 C9 Sm1 174.2(5) . 4_545 ? O4 Sm1 O5 81.40(17) 7 . ? O4 Sm1 O7 79.80(18) 7 7 ? O5 Sm1 O7 131.73(18) . 7 ? O4 Sm1 O12 80.73(18) 7 . ? O5 Sm1 O12 78.67(19) . . ? O7 Sm1 O12 139.96(19) 7 . ? O4 Sm1 O3 125.22(17) 7 . ? O5 Sm1 O3 80.06(17) . . ? O7 Sm1 O3 75.52(19) 7 . ? O12 Sm1 O3 143.04(18) . . ? O4 Sm1 O2 135.86(18) 7 4 ? O5 Sm1 O2 142.12(17) . 4 ? O7 Sm1 O2 73.20(18) 7 4 ? O12 Sm1 O2 98.18(19) . 4 ? O3 Sm1 O2 80.86(17) . 4 ? O4 Sm1 O13 147.59(18) 7 . ? O5 Sm1 O13 74.17(18) . . ? O7 Sm1 O13 132.54(19) 7 . ? O12 Sm1 O13 73.91(19) . . ? O3 Sm1 O13 71.37(18) . . ? O2 Sm1 O13 68.81(18) 4 . ? O4 Sm1 O1 87.73(17) 7 4 ? O5 Sm1 O1 151.89(17) . 4 ? O7 Sm1 O1 70.58(17) 7 4 ? O12 Sm1 O1 74.02(19) . 4 ? O3 Sm1 O1 126.65(17) . 4 ? O2 Sm1 O1 50.71(16) 4 4 ? O13 Sm1 O1 103.96(18) . 4 ? O4 Sm1 O4 76.50(17) 7 . ? O5 Sm1 O4 65.01(16) . . ? O7 Sm1 O4 67.49(17) 7 . ? O12 Sm1 O4 139.33(19) . . ? O3 Sm1 O4 48.96(16) . . ? O2 Sm1 O4 121.57(15) 4 . ? O13 Sm1 O4 110.67(17) . . ? O1 Sm1 O4 137.10(15) 4 . ? O4 Sm1 C9 112.21(19) 7 4 ? O5 Sm1 C9 157.32(18) . 4 ? O7 Sm1 C9 70.19(19) 7 4 ? O12 Sm1 C9 85.6(2) . 4 ? O3 Sm1 C9 104.08(19) . 4 ? O2 Sm1 C9 25.27(18) 4 4 ? O13 Sm1 C9 85.9(2) . 4 ? O1 Sm1 C9 25.44(17) 4 4 ? O4 Sm1 C9 134.29(17) . 4 ? O4 Sm1 Sm1 42.63(12) 7 7 ? O5 Sm1 Sm1 67.67(12) . 7 ? O7 Sm1 Sm1 68.40(13) 7 7 ? O12 Sm1 Sm1 115.85(15) . 7 ? O3 Sm1 Sm1 82.71(12) . 7 ? O2 Sm1 Sm1 140.89(12) 4 7 ? O13 Sm1 Sm1 136.86(14) . 7 ? O1 Sm1 Sm1 119.18(11) 4 7 ? O4 Sm1 Sm1 33.87(10) . 7 ? C9 Sm1 Sm1 134.66(14) 4 7 ? O11 Ni2 O9 87.27(16) . . ? O11 Ni2 O9 87.27(16) . 2_554 ? O9 Ni2 O9 174.5(3) . 2_554 ? O11 Ni2 N1 89.39(18) . 2_554 ? O9 Ni2 N1 87.1(2) . 2_554 ? O9 Ni2 N1 92.9(2) 2_554 2_554 ? O11 Ni2 N1 89.39(18) . . ? O9 Ni2 N1 92.9(2) . . ? O9 Ni2 N1 87.1(2) 2_554 . ? N1 Ni2 N1 178.8(4) 2_554 . ? O11 Ni2 O10 180.000(1) . . ? O9 Ni2 O10 92.73(16) . . ? O9 Ni2 O10 92.73(16) 2_554 . ? N1 Ni2 O10 90.61(18) 2_554 . ? N1 Ni2 O10 90.61(18) . . ? C1 O3 Sm1 104.8(4) . . ? S1 O5 Sm1 137.8(3) . . ? Ni2 O10 H10A 113(6) . . ? C1 O4 Sm1 171.6(5) . 7 ? C1 O4 Sm1 84.6(4) . . ? Sm1 O4 Sm1 103.50(17) 7 . ? C7 C8 C2 120.9(7) . . ? C7 C8 C9 117.3(7) . . ? C2 C8 C9 121.6(7) . . ? N1 C4 C3 131.2(7) . . ? N1 C4 C6 109.1(7) . . ? C3 C4 C6 119.7(7) . . ? Sm1 O13 H13A 105(5) . . ? Sm1 O13 H13B 125(5) . . ? H13A O13 H13B 106(4) . . ? N2 C5 N1 113.1(7) . . ? N2 C5 H5 123.5 . . ? N1 C5 H5 123.5 . . ? N2 C6 C7 131.7(7) . . ? N2 C6 C4 105.6(7) . . ? C7 C6 C4 122.7(7) . . ? C2 C3 C4 118.1(7) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 N1 C4 104.5(7) . . ? C5 N1 Ni2 120.1(6) . . ? C4 N1 Ni2 133.3(5) . . ? O3 C1 O4 121.3(7) . . ? O3 C1 C2 118.2(6) . . ? O4 C1 C2 120.4(7) . . ? C3 C2 C8 121.1(7) . . ? C3 C2 C1 119.1(7) . . ? C8 C2 C1 119.5(7) . . ? C8 C7 C6 117.4(7) . . ? C8 C7 H7 121.3 . . ? C6 C7 H7 121.3 . . ? Ni2 O11 H11A 125(5) . . ? O6 S1 O8 109.5(3) . . ? O6 S1 O5 110.3(3) . . ? O8 S1 O5 109.0(3) . . ? O6 S1 O7 109.0(3) . . ? O8 S1 O7 108.8(3) . . ? O5 S1 O7 110.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.082 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.144 data_3 _database_code_depnum_ccdc_archive 'CCDC 862564' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Eu2 N4 Ni O24 S2' _chemical_formula_weight 1105.15 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' 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' Ni Ni 0.3393 1.1124 '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 22.477(4) _cell_length_b 8.7351(17) _cell_length_c 15.536(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.85(3) _cell_angle_gamma 90.00 _cell_volume 2973.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3391 _cell_measurement_theta_min 3.53 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 5.046 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4319 _exptl_absorpt_correction_T_max 0.4319 _exptl_absorpt_process_details ? _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 ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10227 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _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 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3391 _reflns_number_gt 2872 _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^)+(0.0190P)^2^+10.5568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3391 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 0.247014(11) 0.85806(3) 0.383038(15) 0.01547(8) Uani 1 1 d . . . Ni2 Ni 0.0000 0.79611(11) -0.2500 0.0233(2) Uani 1 2 d S . . S1 S 0.35183(5) 0.95997(14) 0.58600(8) 0.0178(3) Uani 1 1 d . . . O1 O 0.14536(18) 0.9354(5) 0.2799(2) 0.0345(10) Uani 1 1 d . . . O2 O 0.21209(16) 0.8170(4) 0.2217(2) 0.0263(9) Uani 1 1 d . . . O3 O 0.31100(16) 0.6474(4) 0.3607(2) 0.0260(8) Uani 1 1 d . . . O4 O 0.29696(15) 0.6151(4) 0.4955(2) 0.0223(8) Uani 1 1 d . . . O5 O 0.31893(18) 0.9702(5) 0.2999(2) 0.0377(10) Uani 1 1 d . . . H5A H 0.3513 0.9223 0.2967 0.057 Uiso 1 1 d R . . H5B H 0.3112 1.0566 0.2746 0.057 Uiso 1 1 d R . . O6 O 0.33534(15) 0.9272(4) 0.4906(2) 0.0254(8) Uani 1 1 d . . . O7 O 0.33420(19) 1.1144(4) 0.6033(3) 0.0415(11) Uani 1 1 d . . . O8 O 0.41792(15) 0.9413(5) 0.6169(2) 0.0341(10) Uani 1 1 d . . . O9 O -0.09334(17) 0.7845(4) -0.2727(2) 0.0330(9) Uani 1 1 d . . . H9A H -0.1108 0.8686 -0.2741 0.050 Uiso 1 1 d R . . H9B H -0.1062 0.7274 -0.3146 0.050 Uiso 1 1 d R . . O10 O 0.0000 1.0368(7) -0.2500 0.0541(18) Uani 1 2 d S . . O11 O 0.0000 0.5590(6) -0.2500 0.0461(17) Uani 1 2 d S . . O12 O 0.23956(19) 1.1351(5) 0.3914(3) 0.0507(12) Uani 1 1 d . . . H12A H 0.2694 1.1866 0.4206 0.076 Uiso 1 1 d R . . H12B H 0.2071 1.1805 0.3653 0.076 Uiso 1 1 d R . . O13 O 0.32056(18) 0.8539(5) 0.6341(2) 0.0354(10) Uani 1 1 d . . . N1 N 0.0009(2) 0.7939(5) -0.1161(3) 0.0277(11) Uani 1 1 d . . . N2 N -0.0214(2) 0.6832(5) 0.0009(3) 0.0266(11) Uani 1 1 d . . . H2 H -0.0405 0.6280 0.0318 0.032 Uiso 1 1 d R . . C1 C 0.1610(2) 0.8809(6) 0.2143(3) 0.0214(11) Uani 1 1 d . . . C2 C 0.1177(2) 0.8769(6) 0.1254(3) 0.0187(11) Uani 1 1 d . . . C3 C 0.3225(2) 0.5773(6) 0.4342(3) 0.0186(11) Uani 1 1 d . . . C4 C 0.1298(2) 0.9567(6) 0.0520(3) 0.0171(10) Uani 1 1 d . . . C5 C 0.0942(2) 0.9360(6) -0.0318(3) 0.0209(11) Uani 1 1 d . . . H5 H 0.1030 0.9871 -0.0799 0.025 Uiso 1 1 calc R . . C6 C 0.0442(2) 0.8355(6) -0.0423(3) 0.0205(11) Uani 1 1 d . . . C7 C -0.0373(3) 0.7051(7) -0.0861(3) 0.0289(13) Uani 1 1 d . . . H7 H -0.0719 0.6619 -0.1220 0.035 Uiso 1 1 calc R . . C8 C 0.0310(2) 0.7651(6) 0.0319(3) 0.0226(11) Uani 1 1 d . . . C9 C 0.0681(2) 0.7799(6) 0.1157(3) 0.0231(12) Uani 1 1 d . . . H9 H 0.0598 0.7266 0.1636 0.028 Uiso 1 1 calc R . . H11 H -0.0278 0.5275 -0.2896 0.028 Uiso 0.50 1 d PR . . H10 H 0.0342 0.9317 0.2732 0.028 Uiso 0.50 1 d PR . . 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 0.01780(12) 0.01639(13) 0.01141(12) -0.00014(11) 0.00148(9) 0.00088(11) Ni2 0.0275(5) 0.0211(5) 0.0176(5) 0.000 -0.0029(4) 0.000 S1 0.0169(6) 0.0187(7) 0.0165(6) -0.0039(5) 0.0012(5) -0.0014(5) O1 0.047(2) 0.038(2) 0.0155(18) -0.0004(17) 0.0026(18) 0.018(2) O2 0.0226(19) 0.037(2) 0.0174(17) 0.0025(16) 0.0010(15) 0.0053(17) O3 0.036(2) 0.022(2) 0.0201(18) 0.0032(16) 0.0062(16) 0.0077(17) O4 0.0227(18) 0.026(2) 0.0198(17) -0.0059(15) 0.0076(15) 0.0033(15) O5 0.040(2) 0.039(3) 0.036(2) 0.0123(19) 0.012(2) -0.004(2) O6 0.0239(19) 0.034(2) 0.0159(17) -0.0021(16) -0.0001(15) -0.0053(17) O7 0.048(3) 0.025(2) 0.047(2) -0.0118(19) -0.001(2) 0.0116(19) O8 0.0172(18) 0.056(3) 0.027(2) -0.0171(19) -0.0001(16) 0.0028(19) O9 0.034(2) 0.031(2) 0.029(2) -0.0069(17) -0.0043(18) 0.0077(18) O10 0.086(5) 0.029(4) 0.056(4) 0.000 0.036(4) 0.000 O11 0.057(4) 0.020(3) 0.044(3) 0.000 -0.025(3) 0.000 O12 0.044(3) 0.021(2) 0.090(4) 0.000(2) 0.020(3) 0.003(2) O13 0.043(2) 0.041(2) 0.0202(18) 0.0039(18) 0.0027(17) -0.022(2) N1 0.028(2) 0.034(3) 0.017(2) 0.0003(19) -0.002(2) -0.009(2) N2 0.027(2) 0.031(3) 0.021(2) 0.0040(19) 0.004(2) -0.009(2) C1 0.031(3) 0.015(3) 0.018(2) -0.003(2) 0.005(2) -0.004(2) C2 0.021(2) 0.022(3) 0.013(2) -0.003(2) 0.0024(19) 0.001(2) C3 0.018(2) 0.019(3) 0.018(2) -0.004(2) 0.003(2) -0.005(2) C4 0.020(2) 0.018(3) 0.015(2) 0.001(2) 0.005(2) -0.002(2) C5 0.028(3) 0.022(3) 0.013(2) 0.002(2) 0.005(2) -0.002(2) C6 0.021(2) 0.021(3) 0.018(2) 0.001(2) -0.001(2) -0.001(2) C7 0.027(3) 0.031(3) 0.026(3) -0.003(2) 0.003(2) -0.011(3) C8 0.022(3) 0.021(3) 0.026(3) 0.003(2) 0.007(2) -0.002(2) C9 0.026(3) 0.028(3) 0.017(2) 0.003(2) 0.007(2) -0.006(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 Eu1 O4 2.328(3) 7_566 ? Eu1 O6 2.371(3) . ? Eu1 O13 2.372(4) 7_566 ? Eu1 O3 2.408(4) . ? Eu1 O12 2.432(4) . ? Eu1 O2 2.480(3) . ? Eu1 O5 2.484(4) . ? Eu1 O1 2.572(4) . ? Eu1 O4 2.819(3) . ? Eu1 C1 2.897(5) . ? Eu1 C3 2.988(5) . ? Eu1 Eu1 4.0709(8) 7_566 ? Ni2 O9 2.051(4) . ? Ni2 O9 2.051(4) 2_554 ? Ni2 O11 2.072(6) . ? Ni2 N1 2.075(4) . ? Ni2 N1 2.075(4) 2_554 ? Ni2 O10 2.102(6) . ? S1 O7 1.448(4) . ? S1 O13 1.465(4) . ? S1 O8 1.465(4) . ? S1 O6 1.474(3) . ? O1 C1 1.245(6) . ? O2 C1 1.258(6) . ? O3 C3 1.271(6) . ? O4 C3 1.261(6) . ? O4 Eu1 2.328(3) 7_566 ? O5 H5A 0.8499 . ? O5 H5B 0.8500 . ? O9 H9A 0.8306 . ? O9 H9B 0.8199 . ? O11 H11 0.8205 . ? O12 H12A 0.8497 . ? O12 H12B 0.8502 . ? O13 Eu1 2.372(4) 7_566 ? N1 C7 1.316(7) . ? N1 C6 1.378(6) . ? N2 C7 1.333(6) . ? N2 C8 1.372(6) . ? N2 H2 0.8602 . ? C1 C2 1.503(6) . ? C2 C9 1.383(7) . ? C2 C4 1.413(6) . ? C3 C4 1.484(7) 4_545 ? C4 C5 1.380(6) . ? C4 C3 1.484(7) 4 ? C5 C6 1.406(7) . ? C5 H5 0.9300 . ? C6 C8 1.395(7) . ? C7 H7 0.9300 . ? C8 C9 1.387(7) . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu1 O6 80.97(12) 7_566 . ? O4 Eu1 O13 78.06(13) 7_566 7_566 ? O6 Eu1 O13 133.85(12) . 7_566 ? O4 Eu1 O3 124.67(12) 7_566 . ? O6 Eu1 O3 82.12(12) . . ? O13 Eu1 O3 77.02(14) 7_566 . ? O4 Eu1 O12 79.03(13) 7_566 . ? O6 Eu1 O12 76.45(14) . . ? O13 Eu1 O12 137.14(14) 7_566 . ? O3 Eu1 O12 144.97(13) . . ? O4 Eu1 O2 137.51(12) 7_566 . ? O6 Eu1 O2 140.92(12) . . ? O13 Eu1 O2 73.88(12) 7_566 . ? O3 Eu1 O2 78.96(11) . . ? O12 Eu1 O2 100.84(14) . . ? O4 Eu1 O5 145.52(13) 7_566 . ? O6 Eu1 O5 74.12(12) . . ? O13 Eu1 O5 136.37(13) 7_566 . ? O3 Eu1 O5 75.38(13) . . ? O12 Eu1 O5 72.29(14) . . ? O2 Eu1 O5 68.16(12) . . ? O4 Eu1 O1 90.00(12) 7_566 . ? O6 Eu1 O1 149.40(13) . . ? O13 Eu1 O1 71.16(14) 7_566 . ? O3 Eu1 O1 125.94(11) . . ? O12 Eu1 O1 73.13(14) . . ? O2 Eu1 O1 51.00(11) . . ? O5 Eu1 O1 99.38(13) . . ? O4 Eu1 O4 75.86(12) 7_566 . ? O6 Eu1 O4 66.36(11) . . ? O13 Eu1 O4 68.83(12) 7_566 . ? O3 Eu1 O4 49.15(10) . . ? O12 Eu1 O4 137.63(13) . . ? O2 Eu1 O4 120.70(11) . . ? O5 Eu1 O4 113.82(12) . . ? O1 Eu1 O4 139.47(12) . . ? O4 Eu1 C1 114.10(13) 7_566 . ? O6 Eu1 C1 154.91(13) . . ? O13 Eu1 C1 70.75(13) 7_566 . ? O3 Eu1 C1 102.80(13) . . ? O12 Eu1 C1 86.56(15) . . ? O2 Eu1 C1 25.58(13) . . ? O5 Eu1 C1 83.25(13) . . ? O1 Eu1 C1 25.42(13) . . ? O4 Eu1 C1 134.94(12) . . ? O4 Eu1 C3 100.68(13) 7_566 . ? O6 Eu1 C3 71.60(13) . . ? O13 Eu1 C3 72.59(14) 7_566 . ? O3 Eu1 C3 24.35(12) . . ? O12 Eu1 C3 147.63(14) . . ? O2 Eu1 C3 100.58(12) . . ? O5 Eu1 C3 93.75(14) . . ? O1 Eu1 C3 138.99(13) . . ? O4 Eu1 C3 24.86(11) . . ? C1 Eu1 C3 121.49(13) . . ? O4 Eu1 Eu1 42.18(8) 7_566 7_566 ? O6 Eu1 Eu1 68.45(9) . 7_566 ? O13 Eu1 Eu1 68.39(9) 7_566 7_566 ? O3 Eu1 Eu1 82.67(8) . 7_566 ? O12 Eu1 Eu1 113.75(11) . 7_566 ? O2 Eu1 Eu1 140.82(9) . 7_566 ? O5 Eu1 Eu1 138.68(9) . 7_566 ? O1 Eu1 Eu1 121.76(9) . 7_566 ? O4 Eu1 Eu1 33.68(7) . 7_566 ? C1 Eu1 Eu1 136.27(10) . 7_566 ? C3 Eu1 Eu1 58.52(9) . 7_566 ? O9 Ni2 O9 174.3(2) . 2_554 ? O9 Ni2 O11 87.16(11) . . ? O9 Ni2 O11 87.16(11) 2_554 . ? O9 Ni2 N1 87.30(16) . . ? O9 Ni2 N1 92.65(16) 2_554 . ? O11 Ni2 N1 89.47(13) . . ? O9 Ni2 N1 92.65(16) . 2_554 ? O9 Ni2 N1 87.30(16) 2_554 2_554 ? O11 Ni2 N1 89.47(13) . 2_554 ? N1 Ni2 N1 178.9(3) . 2_554 ? O9 Ni2 O10 92.84(11) . . ? O9 Ni2 O10 92.84(11) 2_554 . ? O11 Ni2 O10 180.0 . . ? N1 Ni2 O10 90.53(13) . . ? N1 Ni2 O10 90.53(13) 2_554 . ? O7 S1 O13 108.2(3) . . ? O7 S1 O8 110.0(2) . . ? O13 S1 O8 109.2(2) . . ? O7 S1 O6 110.5(2) . . ? O13 S1 O6 110.4(2) . . ? O8 S1 O6 108.5(2) . . ? C1 O1 Eu1 92.0(3) . . ? C1 O2 Eu1 96.1(3) . . ? C3 O3 Eu1 104.3(3) . . ? C3 O4 Eu1 170.2(3) . 7_566 ? C3 O4 Eu1 85.1(3) . . ? Eu1 O4 Eu1 104.14(12) 7_566 . ? Eu1 O5 H5A 120.0 . . ? Eu1 O5 H5B 120.0 . . ? H5A O5 H5B 120.0 . . ? S1 O6 Eu1 137.9(2) . . ? Ni2 O9 H9A 114.8 . . ? Ni2 O9 H9B 109.5 . . ? H9A O9 H9B 115.8 . . ? Ni2 O11 H11 109.6 . . ? Eu1 O12 H12A 120.0 . . ? Eu1 O12 H12B 120.0 . . ? H12A O12 H12B 120.0 . . ? S1 O13 Eu1 143.5(2) . 7_566 ? C7 N1 C6 104.8(4) . . ? C7 N1 Ni2 119.9(4) . . ? C6 N1 Ni2 132.7(4) . . ? C7 N2 C8 107.2(4) . . ? C7 N2 H2 126.4 . . ? C8 N2 H2 126.4 . . ? O1 C1 O2 120.9(5) . . ? O1 C1 C2 121.2(5) . . ? O2 C1 C2 117.7(4) . . ? O1 C1 Eu1 62.5(3) . . ? O2 C1 Eu1 58.3(2) . . ? C2 C1 Eu1 174.5(4) . . ? C9 C2 C4 120.7(4) . . ? C9 C2 C1 117.1(4) . . ? C4 C2 C1 121.9(4) . . ? O4 C3 O3 121.1(5) . . ? O4 C3 C4 120.9(4) . 4_545 ? O3 C3 C4 117.9(4) . 4_545 ? O4 C3 Eu1 70.0(3) . . ? O3 C3 Eu1 51.3(2) . . ? C4 C3 Eu1 166.0(3) 4_545 . ? C5 C4 C2 121.4(4) . . ? C5 C4 C3 118.6(4) . 4 ? C2 C4 C3 119.7(4) . 4 ? C4 C5 C6 118.2(4) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? N1 C6 C8 109.3(4) . . ? N1 C6 C5 131.3(5) . . ? C8 C6 C5 119.3(4) . . ? N1 C7 N2 113.3(5) . . ? N1 C7 H7 123.4 . . ? N2 C7 H7 123.4 . . ? N2 C8 C9 131.9(5) . . ? N2 C8 C6 105.3(4) . . ? C9 C8 C6 122.8(5) . . ? C2 C9 C8 117.4(5) . . ? C2 C9 H9 121.3 . . ? C8 C9 H9 121.3 . . ? 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 O4 Eu1 O1 C1 -162.0(3) 7_566 . . . ? O6 Eu1 O1 C1 125.9(3) . . . . ? O13 Eu1 O1 C1 -84.6(3) 7_566 . . . ? O3 Eu1 O1 C1 -27.4(4) . . . . ? O12 Eu1 O1 C1 119.5(3) . . . . ? O2 Eu1 O1 C1 -0.4(3) . . . . ? O5 Eu1 O1 C1 51.3(3) . . . . ? O4 Eu1 O1 C1 -94.1(3) . . . . ? C3 Eu1 O1 C1 -55.6(4) . . . . ? Eu1 Eu1 O1 C1 -132.6(3) 7_566 . . . ? O4 Eu1 O2 C1 28.3(4) 7_566 . . . ? O6 Eu1 O2 C1 -139.0(3) . . . . ? O13 Eu1 O2 C1 79.0(3) 7_566 . . . ? O3 Eu1 O2 C1 158.5(3) . . . . ? O12 Eu1 O2 C1 -57.2(3) . . . . ? O5 Eu1 O2 C1 -123.0(3) . . . . ? O1 Eu1 O2 C1 0.4(3) . . . . ? O4 Eu1 O2 C1 131.5(3) . . . . ? C3 Eu1 O2 C1 147.2(3) . . . . ? Eu1 Eu1 O2 C1 94.9(3) 7_566 . . . ? O4 Eu1 O3 C3 -11.1(4) 7_566 . . . ? O6 Eu1 O3 C3 62.2(3) . . . . ? O13 Eu1 O3 C3 -76.4(3) 7_566 . . . ? O12 Eu1 O3 C3 114.6(3) . . . . ? O2 Eu1 O3 C3 -152.2(3) . . . . ? O5 Eu1 O3 C3 137.7(3) . . . . ? O1 Eu1 O3 C3 -131.2(3) . . . . ? O4 Eu1 O3 C3 -3.3(3) . . . . ? C1 Eu1 O3 C3 -142.9(3) . . . . ? Eu1 Eu1 O3 C3 -7.0(3) 7_566 . . . ? O4 Eu1 O4 C3 176.6(3) 7_566 . . . ? O6 Eu1 O4 C3 -97.2(3) . . . . ? O13 Eu1 O4 C3 94.2(3) 7_566 . . . ? O3 Eu1 O4 C3 3.2(3) . . . . ? O12 Eu1 O4 C3 -127.9(3) . . . . ? O2 Eu1 O4 C3 39.3(3) . . . . ? O5 Eu1 O4 C3 -38.5(3) . . . . ? O1 Eu1 O4 C3 103.8(3) . . . . ? C1 Eu1 O4 C3 66.5(3) . . . . ? Eu1 Eu1 O4 C3 176.6(3) 7_566 . . . ? O4 Eu1 O4 Eu1 0.0 7_566 . . 7_566 ? O6 Eu1 O4 Eu1 86.19(14) . . . 7_566 ? O13 Eu1 O4 Eu1 -82.46(15) 7_566 . . 7_566 ? O3 Eu1 O4 Eu1 -173.4(2) . . . 7_566 ? O12 Eu1 O4 Eu1 55.4(2) . . . 7_566 ? O2 Eu1 O4 Eu1 -137.28(12) . . . 7_566 ? O5 Eu1 O4 Eu1 144.89(13) . . . 7_566 ? O1 Eu1 O4 Eu1 -72.87(19) . . . 7_566 ? C1 Eu1 O4 Eu1 -110.09(18) . . . 7_566 ? C3 Eu1 O4 Eu1 -176.6(3) . . . 7_566 ? O7 S1 O6 Eu1 -79.7(4) . . . . ? O13 S1 O6 Eu1 40.0(4) . . . . ? O8 S1 O6 Eu1 159.6(3) . . . . ? O4 Eu1 O6 S1 3.1(3) 7_566 . . . ? O13 Eu1 O6 S1 -60.5(4) 7_566 . . . ? O3 Eu1 O6 S1 -124.0(3) . . . . ? O12 Eu1 O6 S1 83.9(3) . . . . ? O2 Eu1 O6 S1 174.5(3) . . . . ? O5 Eu1 O6 S1 159.1(4) . . . . ? O1 Eu1 O6 S1 77.6(4) . . . . ? O4 Eu1 O6 S1 -75.3(3) . . . . ? C1 Eu1 O6 S1 132.6(3) . . . . ? C3 Eu1 O6 S1 -101.4(3) . . . . ? Eu1 Eu1 O6 S1 -38.8(3) 7_566 . . . ? O7 S1 O13 Eu1 122.4(4) . . . 7_566 ? O8 S1 O13 Eu1 -117.9(4) . . . 7_566 ? O6 S1 O13 Eu1 1.4(5) . . . 7_566 ? O9 Ni2 N1 C7 39.6(4) . . . . ? O9 Ni2 N1 C7 -134.7(4) 2_554 . . . ? O11 Ni2 N1 C7 -47.6(4) . . . . ? N1 Ni2 N1 C7 -47.6(4) 2_554 . . . ? O10 Ni2 N1 C7 132.4(4) . . . . ? O9 Ni2 N1 C6 -161.3(5) . . . . ? O9 Ni2 N1 C6 24.4(5) 2_554 . . . ? O11 Ni2 N1 C6 111.5(5) . . . . ? N1 Ni2 N1 C6 111.5(5) 2_554 . . . ? O10 Ni2 N1 C6 -68.5(5) . . . . ? Eu1 O1 C1 O2 0.8(5) . . . . ? Eu1 O1 C1 C2 175.4(4) . . . . ? Eu1 O2 C1 O1 -0.8(5) . . . . ? Eu1 O2 C1 C2 -175.6(4) . . . . ? O4 Eu1 C1 O1 19.8(3) 7_566 . . . ? O6 Eu1 C1 O1 -103.6(4) . . . . ? O13 Eu1 C1 O1 86.4(3) 7_566 . . . ? O3 Eu1 C1 O1 157.6(3) . . . . ? O12 Eu1 C1 O1 -56.6(3) . . . . ? O2 Eu1 C1 O1 179.2(5) . . . . ? O5 Eu1 C1 O1 -129.1(3) . . . . ? O4 Eu1 C1 O1 113.7(3) . . . . ? C3 Eu1 C1 O1 140.6(3) . . . . ? Eu1 Eu1 C1 O1 64.8(4) 7_566 . . . ? O4 Eu1 C1 O2 -159.4(3) 7_566 . . . ? O6 Eu1 C1 O2 77.2(4) . . . . ? O13 Eu1 C1 O2 -92.8(3) 7_566 . . . ? O3 Eu1 C1 O2 -21.7(3) . . . . ? O12 Eu1 C1 O2 124.2(3) . . . . ? O5 Eu1 C1 O2 51.6(3) . . . . ? O1 Eu1 C1 O2 -179.2(5) . . . . ? O4 Eu1 C1 O2 -65.5(4) . . . . ? C3 Eu1 C1 O2 -38.6(3) . . . . ? Eu1 Eu1 C1 O2 -114.4(3) 7_566 . . . ? O4 Eu1 C1 C2 -114(4) 7_566 . . . ? O6 Eu1 C1 C2 122(4) . . . . ? O13 Eu1 C1 C2 -48(4) 7_566 . . . ? O3 Eu1 C1 C2 24(4) . . . . ? O12 Eu1 C1 C2 169(4) . . . . ? O2 Eu1 C1 C2 45(4) . . . . ? O5 Eu1 C1 C2 97(4) . . . . ? O1 Eu1 C1 C2 -134(4) . . . . ? O4 Eu1 C1 C2 -20(4) . . . . ? C3 Eu1 C1 C2 7(4) . . . . ? Eu1 Eu1 C1 C2 -69(4) 7_566 . . . ? O1 C1 C2 C9 -68.3(7) . . . . ? O2 C1 C2 C9 106.5(6) . . . . ? Eu1 C1 C2 C9 63(4) . . . . ? O1 C1 C2 C4 117.7(6) . . . . ? O2 C1 C2 C4 -67.5(7) . . . . ? Eu1 C1 C2 C4 -110(4) . . . . ? Eu1 O4 C3 O3 155.0(15) 7_566 . . . ? Eu1 O4 C3 O3 -5.4(4) . . . . ? Eu1 O4 C3 C4 -29(2) 7_566 . . 4_545 ? Eu1 O4 C3 C4 170.3(4) . . . 4_545 ? Eu1 O4 C3 Eu1 160.4(18) 7_566 . . . ? Eu1 O3 C3 O4 6.5(5) . . . . ? Eu1 O3 C3 C4 -169.3(3) . . . 4_545 ? O4 Eu1 C3 O4 -3.3(3) 7_566 . . . ? O6 Eu1 C3 O4 73.3(3) . . . . ? O13 Eu1 C3 O4 -77.1(3) 7_566 . . . ? O3 Eu1 C3 O4 -174.1(5) . . . . ? O12 Eu1 C3 O4 83.0(4) . . . . ? O2 Eu1 C3 O4 -146.3(2) . . . . ? O5 Eu1 C3 O4 145.2(3) . . . . ? O1 Eu1 C3 O4 -105.9(3) . . . . ? C1 Eu1 C3 O4 -130.4(3) . . . . ? Eu1 Eu1 C3 O4 -2.2(2) 7_566 . . . ? O4 Eu1 C3 O3 170.7(3) 7_566 . . . ? O6 Eu1 C3 O3 -112.6(3) . . . . ? O13 Eu1 C3 O3 97.0(3) 7_566 . . . ? O12 Eu1 C3 O3 -102.9(4) . . . . ? O2 Eu1 C3 O3 27.7(3) . . . . ? O5 Eu1 C3 O3 -40.7(3) . . . . ? O1 Eu1 C3 O3 68.2(4) . . . . ? O4 Eu1 C3 O3 174.1(5) . . . . ? C1 Eu1 C3 O3 43.7(3) . . . . ? Eu1 Eu1 C3 O3 171.9(3) 7_566 . . . ? O4 Eu1 C3 C4 -146.4(13) 7_566 . . 4_545 ? O6 Eu1 C3 C4 -69.8(13) . . . 4_545 ? O13 Eu1 C3 C4 139.8(13) 7_566 . . 4_545 ? O3 Eu1 C3 C4 42.8(12) . . . 4_545 ? O12 Eu1 C3 C4 -60.1(14) . . . 4_545 ? O2 Eu1 C3 C4 70.6(13) . . . 4_545 ? O5 Eu1 C3 C4 2.1(13) . . . 4_545 ? O1 Eu1 C3 C4 111.0(13) . . . 4_545 ? O4 Eu1 C3 C4 -143.1(15) . . . 4_545 ? C1 Eu1 C3 C4 86.5(13) . . . 4_545 ? Eu1 Eu1 C3 C4 -145.3(14) 7_566 . . 4_545 ? C9 C2 C4 C5 -2.7(8) . . . . ? C1 C2 C4 C5 171.1(5) . . . . ? C9 C2 C4 C3 170.9(5) . . . 4 ? C1 C2 C4 C3 -15.4(7) . . . 4 ? C2 C4 C5 C6 1.5(8) . . . . ? C3 C4 C5 C6 -172.1(5) 4 . . . ? C7 N1 C6 C8 1.3(6) . . . . ? Ni2 N1 C6 C8 -160.0(4) . . . . ? C7 N1 C6 C5 -175.6(6) . . . . ? Ni2 N1 C6 C5 23.1(9) . . . . ? C4 C5 C6 N1 179.0(5) . . . . ? C4 C5 C6 C8 2.4(8) . . . . ? C6 N1 C7 N2 -1.3(7) . . . . ? Ni2 N1 C7 N2 162.9(4) . . . . ? C8 N2 C7 N1 0.8(7) . . . . ? C7 N2 C8 C9 -177.7(6) . . . . ? C7 N2 C8 C6 0.1(6) . . . . ? N1 C6 C8 N2 -0.9(6) . . . . ? C5 C6 C8 N2 176.4(5) . . . . ? N1 C6 C8 C9 177.2(5) . . . . ? C5 C6 C8 C9 -5.5(8) . . . . ? C4 C2 C9 C8 -0.2(8) . . . . ? C1 C2 C9 C8 -174.3(5) . . . . ? N2 C8 C9 C2 -178.2(5) . . . . ? C6 C8 C9 C2 4.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.720 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.157 data_4 _database_code_depnum_ccdc_archive 'CCDC 862565' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Gd2 N4 Ni O24 S2' _chemical_formula_weight 1115.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 22.339(4) _cell_length_b 8.7332(17) _cell_length_c 15.413(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.23(3) _cell_angle_gamma 90.00 _cell_volume 2938.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3470 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.9 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 5.351 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4141 _exptl_absorpt_correction_T_max 0.4141 _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 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _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 11798 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.90 _reflns_number_total 3470 _reflns_number_gt 3069 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+5.8275P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00132(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3470 _refine_ls_number_parameters 235 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.121 _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 O13 O 0.73804(19) -0.1290(4) 0.8931(4) 0.0788(19) Uani 1 1 d U . . H13A H 0.7145 -0.1778 0.8517 0.095 Uiso 1 1 d R . . H13B H 0.7582 -0.1769 0.9379 0.095 Uiso 1 1 d R . . O4 O 0.68814(17) -0.1485(3) 0.64125(19) 0.0292(8) Uani 1 1 d . . . O3 O 0.70303(13) -0.1201(4) 0.50542(19) 0.0283(8) Uani 1 1 d . . . C1 C 0.67657(18) -0.0795(5) 0.5671(2) 0.0188(8) Uani 1 1 d . . . Gd1 Gd 0.747077(8) 0.14358(2) 0.882898(11) 0.01186(9) Uani 1 1 d . . . S1 S 0.85054(4) 0.03587(11) 1.08618(6) 0.0144(2) Uani 1 1 d . . . O2 O 0.64571(16) 0.0676(4) 0.78218(18) 0.0327(8) Uani 1 1 d . . . N1 N 0.50036(14) 0.2046(4) 0.3841(2) 0.0146(6) Uani 1 1 d . . . C9 C 0.66131(18) 0.1215(4) 0.7154(2) 0.0128(7) Uani 1 1 d . . . O12 O 0.81765(16) 0.0228(4) 0.80282(19) 0.0336(8) Uani 1 1 d . . . H12A H 0.8058 -0.0002 0.7483 0.040 Uiso 1 1 d R . . H12B H 0.8542 0.0038 0.8296 0.040 Uiso 1 1 d R . . O6 O 0.83218(15) -0.1181(4) 1.1024(3) 0.0336(8) Uani 1 1 d . . . C8 C 0.61806(17) 0.1251(4) 0.6272(2) 0.0119(7) Uani 1 1 d . . . C4 C 0.54450(17) 0.1629(4) 0.4589(3) 0.0137(8) Uani 1 1 d . . . O1 O 0.71251(14) 0.1824(5) 0.7225(2) 0.0392(10) Uani 1 1 d . . . O5 O 0.83440(13) 0.0701(5) 0.99054(19) 0.0390(10) Uani 1 1 d . . . C5 C 0.46222(17) 0.2951(5) 0.4150(3) 0.0171(8) Uani 1 1 d . . . H5 H 0.4276 0.3386 0.3792 0.020 Uiso 1 1 calc R . . O7 O 0.81969(19) 0.1436(4) 1.1348(2) 0.0393(10) Uani 1 1 d . . . C6 C 0.53084(16) 0.2357(4) 0.5332(2) 0.0127(7) Uani 1 1 d . . . C2 C 0.62996(16) 0.0430(5) 0.5529(2) 0.0137(8) Uani 1 1 d . . . O8 O 0.91679(13) 0.0503(5) 1.1174(2) 0.0476(12) Uani 1 1 d . . . C3 C 0.59399(17) 0.0631(5) 0.4686(2) 0.0155(8) Uani 1 1 d . . . H2 H 0.6027 0.0113 0.4200 0.019 Uiso 1 1 calc R . . C7 C 0.56809(16) 0.2215(4) 0.6178(2) 0.0126(7) Uani 1 1 d . . . H47 H 0.5596 0.2748 0.6660 0.015 Uiso 1 1 calc R . . Ni1 Ni 0.5000 0.20175(8) 0.2500 0.01241(15) Uani 1 2 d S . . O10 O 0.40659(12) 0.2140(4) 0.22738(18) 0.0207(6) Uani 1 1 d . . . H10A H 0.3854 0.1325 0.2223 0.025 Uiso 1 1 d R . . H10B H 0.3890 0.3008 0.2232 0.025 Uiso 1 1 d R . . O9 O 0.5000 0.4379(5) 0.2500 0.0335(12) Uani 1 2 d S . . H9 H 0.5238 0.4692 0.2944 0.050 Uiso 0.50 1 calc PR . . O11 O 0.5000 -0.0370(5) 0.2500 0.0467(15) Uani 1 2 d S . . H11 H 0.4965 -0.0683 0.1990 0.070 Uiso 0.50 1 calc PR . . N2 N 0.47814(15) 0.3180(4) 0.5027(2) 0.0164(7) Uani 1 1 d . . . H2A H 0.4590 0.3736 0.5340 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O13 0.037(2) 0.021(2) 0.190(6) 0.033(3) 0.051(3) 0.0075(16) O4 0.045(2) 0.0261(18) 0.0105(14) -0.0040(11) -0.0078(13) 0.0236(14) O3 0.0144(14) 0.051(2) 0.0157(15) -0.0176(13) -0.0048(12) 0.0144(14) C1 0.0195(19) 0.022(2) 0.0114(18) -0.0119(16) -0.0033(15) 0.0057(16) Gd1 0.01225(11) 0.01371(12) 0.00778(12) 0.00274(6) -0.00201(7) -0.00502(6) S1 0.0093(4) 0.0221(5) 0.0105(4) 0.0045(3) -0.0009(3) -0.0038(3) O2 0.050(2) 0.035(2) 0.0107(14) 0.0023(13) 0.0007(14) -0.0261(17) N1 0.0132(15) 0.0155(16) 0.0130(15) 0.0024(12) -0.0014(12) 0.0044(12) C9 0.0187(18) 0.0114(19) 0.0094(18) -0.0020(13) 0.0057(14) 0.0050(14) O12 0.053(2) 0.032(2) 0.0160(15) -0.0099(13) 0.0084(14) -0.0033(16) O6 0.0251(17) 0.0148(16) 0.053(2) 0.0041(14) -0.0103(15) -0.0034(13) C8 0.0114(17) 0.0132(19) 0.0117(18) 0.0034(13) 0.0037(14) 0.0002(13) C4 0.0111(17) 0.017(2) 0.0123(18) 0.0036(14) 0.0002(14) 0.0000(14) O1 0.0121(15) 0.094(3) 0.0111(15) 0.0072(16) 0.0015(12) -0.0113(17) O5 0.0105(14) 0.094(3) 0.0115(15) 0.0193(17) -0.0006(11) 0.0046(17) C5 0.0133(17) 0.019(2) 0.0170(19) 0.0004(15) -0.0015(15) 0.0033(15) O7 0.064(3) 0.0274(19) 0.0141(16) -0.0085(12) -0.0186(16) 0.0276(17) C6 0.0116(16) 0.0120(19) 0.0143(18) 0.0019(14) 0.0022(14) 0.0008(14) C2 0.0115(16) 0.019(2) 0.0107(17) 0.0008(14) 0.0036(14) 0.0041(14) O8 0.0120(15) 0.088(3) 0.0356(19) 0.043(2) -0.0116(13) -0.0182(17) C3 0.0144(17) 0.018(2) 0.0138(18) 0.0000(15) 0.0031(14) 0.0033(15) C7 0.0130(17) 0.014(2) 0.0113(17) 0.0001(14) 0.0037(14) 0.0021(14) Ni1 0.0126(3) 0.0110(3) 0.0120(3) 0.000 -0.0011(3) 0.000 O10 0.0147(13) 0.0229(16) 0.0227(15) -0.0056(12) 0.0002(11) -0.0040(12) O9 0.041(3) 0.015(2) 0.030(3) 0.000 -0.026(2) 0.000 O11 0.103(5) 0.011(2) 0.043(3) 0.000 0.053(3) 0.000 N2 0.0157(16) 0.0162(17) 0.0164(16) -0.0020(13) 0.0013(13) 0.0059(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 O13 Gd1 2.397(4) . ? O13 H13A 0.8501 . ? O13 H13B 0.8500 . ? O4 C1 1.269(5) . ? O4 Gd1 2.400(3) 4_646 ? O3 C1 1.272(5) . ? O3 Gd1 2.316(3) 6 ? O3 Gd1 2.766(3) 4_646 ? C1 C2 1.477(5) . ? C1 Gd1 2.966(4) 4_646 ? Gd1 O3 2.316(3) 6_556 ? Gd1 O7 2.362(3) 7_657 ? Gd1 O5 2.366(3) . ? Gd1 O4 2.400(3) 4_656 ? Gd1 O12 2.439(3) . ? Gd1 O1 2.453(3) . ? Gd1 O2 2.547(3) . ? Gd1 O3 2.766(3) 4_656 ? Gd1 C1 2.966(4) 4_656 ? Gd1 Gd1 4.0376(7) 7_657 ? S1 O6 1.443(3) . ? S1 O8 1.461(3) . ? S1 O7 1.463(4) . ? S1 O5 1.472(3) . ? O2 C9 1.246(5) . ? N1 C5 1.323(5) . ? N1 C4 1.398(5) . ? N1 Ni1 2.065(3) . ? C9 O1 1.245(5) . ? C9 C8 1.493(5) . ? O12 H12A 0.8500 . ? O12 H12B 0.8502 . ? C8 C7 1.381(5) . ? C8 C2 1.422(5) . ? C4 C3 1.391(5) . ? C4 C6 1.398(5) . ? C5 N2 1.338(5) . ? C5 H5 0.9300 . ? O7 Gd1 2.362(3) 7_657 ? C6 N2 1.374(5) . ? C6 C7 1.397(5) . ? C2 C3 1.387(5) . ? C3 H2 0.9300 . ? C7 H47 0.9300 . ? Ni1 O10 2.044(3) . ? Ni1 O10 2.044(3) 2_655 ? Ni1 O9 2.063(4) . ? Ni1 N1 2.065(3) 2_655 ? Ni1 O11 2.085(5) . ? O10 H10A 0.8501 . ? O10 H10B 0.8500 . ? O9 H9 0.8200 . ? O11 H11 0.8200 . ? N2 H2A 0.8600 . ? 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 Gd1 O13 H13A 119.7 . . ? Gd1 O13 H13B 120.3 . . ? H13A O13 H13B 120.0 . . ? C1 O4 Gd1 103.6(3) . 4_646 ? C1 O3 Gd1 168.3(3) . 6 ? C1 O3 Gd1 86.1(3) . 4_646 ? Gd1 O3 Gd1 104.88(10) 6 4_646 ? O4 C1 O3 120.1(4) . . ? O4 C1 C2 118.7(3) . . ? O3 C1 C2 121.1(4) . . ? O4 C1 Gd1 51.9(2) . 4_646 ? O3 C1 Gd1 68.5(2) . 4_646 ? C2 C1 Gd1 168.0(3) . 4_646 ? O3 Gd1 O7 78.28(13) 6_556 7_657 ? O3 Gd1 O5 80.43(10) 6_556 . ? O7 Gd1 O5 134.50(13) 7_657 . ? O3 Gd1 O13 78.59(16) 6_556 . ? O7 Gd1 O13 136.80(14) 7_657 . ? O5 Gd1 O13 75.70(17) . . ? O3 Gd1 O4 124.59(11) 6_556 4_656 ? O7 Gd1 O4 76.91(15) 7_657 4_656 ? O5 Gd1 O4 83.06(12) . 4_656 ? O13 Gd1 O4 145.45(14) . 4_656 ? O3 Gd1 O12 143.75(11) 6_556 . ? O7 Gd1 O12 137.90(12) 7_657 . ? O5 Gd1 O12 73.27(11) . . ? O13 Gd1 O12 71.11(14) . . ? O4 Gd1 O12 76.88(12) 4_656 . ? O3 Gd1 O1 137.47(10) 6_556 . ? O7 Gd1 O1 73.66(12) 7_657 . ? O5 Gd1 O1 141.36(11) . . ? O13 Gd1 O1 100.99(18) . . ? O4 Gd1 O1 79.08(11) 4_656 . ? O12 Gd1 O1 69.43(11) . . ? O3 Gd1 O2 89.86(10) 6_556 . ? O7 Gd1 O2 71.12(12) 7_657 . ? O5 Gd1 O2 148.34(14) . . ? O13 Gd1 O2 72.85(15) . . ? O4 Gd1 O2 126.16(10) 4_656 . ? O12 Gd1 O2 99.52(11) . . ? O1 Gd1 O2 51.11(10) . . ? O3 Gd1 O3 75.12(11) 6_556 4_656 ? O7 Gd1 O3 69.28(11) 7_657 4_656 ? O5 Gd1 O3 66.56(12) . 4_656 ? O13 Gd1 O3 136.75(16) . 4_656 ? O4 Gd1 O3 49.86(10) 4_656 4_656 ? O12 Gd1 O3 114.79(11) . 4_656 ? O1 Gd1 O3 121.58(12) . 4_656 ? O2 Gd1 O3 139.69(11) . 4_656 ? O3 Gd1 C1 100.41(11) 6_556 4_656 ? O7 Gd1 C1 72.71(13) 7_657 4_656 ? O5 Gd1 C1 72.28(13) . 4_656 ? O13 Gd1 C1 147.63(14) . 4_656 ? O4 Gd1 C1 24.57(11) 4_656 4_656 ? O12 Gd1 C1 94.95(12) . 4_656 ? O1 Gd1 C1 100.95(12) . 4_656 ? O2 Gd1 C1 139.36(11) . 4_656 ? O3 Gd1 C1 25.35(10) 4_656 4_656 ? O3 Gd1 Gd1 41.46(8) 6_556 7_657 ? O7 Gd1 Gd1 68.97(8) 7_657 7_657 ? O5 Gd1 Gd1 68.42(9) . 7_657 ? O13 Gd1 Gd1 112.68(15) . 7_657 ? O4 Gd1 Gd1 83.34(8) 4_656 7_657 ? O12 Gd1 Gd1 138.57(8) . 7_657 ? O1 Gd1 Gd1 141.38(10) . 7_657 ? O2 Gd1 Gd1 121.40(8) . 7_657 ? O3 Gd1 Gd1 33.67(6) 4_656 7_657 ? C1 Gd1 Gd1 58.97(8) 4_656 7_657 ? O6 S1 O8 109.2(2) . . ? O6 S1 O7 109.2(2) . . ? O8 S1 O7 109.3(2) . . ? O6 S1 O5 110.2(2) . . ? O8 S1 O5 109.15(18) . . ? O7 S1 O5 109.9(2) . . ? C9 O2 Gd1 92.1(2) . . ? C5 N1 C4 104.7(3) . . ? C5 N1 Ni1 120.1(3) . . ? C4 N1 Ni1 132.5(3) . . ? O1 C9 O2 120.1(4) . . ? O1 C9 C8 118.4(3) . . ? O2 C9 C8 121.3(4) . . ? Gd1 O12 H12A 120.2 . . ? Gd1 O12 H12B 119.8 . . ? H12A O12 H12B 120.0 . . ? C7 C8 C2 120.5(3) . . ? C7 C8 C9 117.4(3) . . ? C2 C8 C9 121.8(3) . . ? C3 C4 N1 131.1(4) . . ? C3 C4 C6 120.2(3) . . ? N1 C4 C6 108.6(3) . . ? C9 O1 Gd1 96.7(2) . . ? S1 O5 Gd1 138.41(18) . . ? N1 C5 N2 113.5(3) . . ? N1 C5 H5 123.2 . . ? N2 C5 H5 123.2 . . ? S1 O7 Gd1 143.24(19) . 7_657 ? N2 C6 C7 131.6(3) . . ? N2 C6 C4 106.1(3) . . ? C7 C6 C4 122.3(3) . . ? C3 C2 C8 121.4(3) . . ? C3 C2 C1 118.7(3) . . ? C8 C2 C1 119.5(3) . . ? C2 C3 C4 118.0(4) . . ? C2 C3 H2 121.0 . . ? C4 C3 H2 121.0 . . ? C8 C7 C6 117.4(3) . . ? C8 C7 H47 121.3 . . ? C6 C7 H47 121.3 . . ? O10 Ni1 O10 174.00(18) . 2_655 ? O10 Ni1 O9 87.00(9) . . ? O10 Ni1 O9 87.00(9) 2_655 . ? O10 Ni1 N1 87.57(12) . . ? O10 Ni1 N1 92.36(12) 2_655 . ? O9 Ni1 N1 89.31(10) . . ? O10 Ni1 N1 92.36(12) . 2_655 ? O10 Ni1 N1 87.57(12) 2_655 2_655 ? O9 Ni1 N1 89.31(10) . 2_655 ? N1 Ni1 N1 178.61(19) . 2_655 ? O10 Ni1 O11 93.00(9) . . ? O10 Ni1 O11 93.00(9) 2_655 . ? O9 Ni1 O11 180.000(1) . . ? N1 Ni1 O11 90.69(10) . . ? N1 Ni1 O11 90.69(10) 2_655 . ? Ni1 O10 H10A 120.1 . . ? Ni1 O10 H10B 119.9 . . ? H10A O10 H10B 120.0 . . ? Ni1 O9 H9 109.5 . . ? Ni1 O11 H11 109.5 . . ? C5 N2 C6 107.0(3) . . ? C5 N2 H2A 126.5 . . ? C6 N2 H2A 126.5 . . ? 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 C1 O3 -6.1(5) 4_646 . . . ? Gd1 O4 C1 C2 171.0(3) 4_646 . . . ? Gd1 O3 C1 O4 -155.7(11) 6 . . . ? Gd1 O3 C1 O4 5.2(4) 4_646 . . . ? Gd1 O3 C1 C2 27.2(15) 6 . . . ? Gd1 O3 C1 C2 -171.9(4) 4_646 . . . ? Gd1 O3 C1 Gd1 -160.9(13) 6 . . 4_646 ? O3 Gd1 O2 C9 161.6(3) 6_556 . . . ? O7 Gd1 O2 C9 83.9(3) 7_657 . . . ? O5 Gd1 O2 C9 -127.1(2) . . . . ? O13 Gd1 O2 C9 -120.3(3) . . . . ? O4 Gd1 O2 C9 27.0(3) 4_656 . . . ? O12 Gd1 O2 C9 -53.6(3) . . . . ? O1 Gd1 O2 C9 0.0(2) . . . . ? O3 Gd1 O2 C9 95.1(3) 4_656 . . . ? C1 Gd1 O2 C9 55.6(3) 4_656 . . . ? Gd1 Gd1 O2 C9 133.1(2) 7_657 . . . ? Gd1 O2 C9 O1 0.0(4) . . . . ? Gd1 O2 C9 C8 -175.6(3) . . . . ? O1 C9 C8 C7 -107.7(5) . . . . ? O2 C9 C8 C7 68.0(5) . . . . ? O1 C9 C8 C2 67.1(5) . . . . ? O2 C9 C8 C2 -117.3(4) . . . . ? C5 N1 C4 C3 175.9(4) . . . . ? Ni1 N1 C4 C3 -23.5(6) . . . . ? C5 N1 C4 C6 -1.3(4) . . . . ? Ni1 N1 C4 C6 159.3(3) . . . . ? O2 C9 O1 Gd1 0.0(4) . . . . ? C8 C9 O1 Gd1 175.7(3) . . . . ? O3 Gd1 O1 C9 -27.9(4) 6_556 . . . ? O7 Gd1 O1 C9 -78.7(3) 7_657 . . . ? O5 Gd1 O1 C9 137.9(3) . . . . ? O13 Gd1 O1 C9 57.1(3) . . . . ? O4 Gd1 O1 C9 -158.1(3) 4_656 . . . ? O12 Gd1 O1 C9 122.0(3) . . . . ? O2 Gd1 O1 C9 0.0(2) . . . . ? O3 Gd1 O1 C9 -130.9(3) 4_656 . . . ? C1 Gd1 O1 C9 -146.8(3) 4_656 . . . ? Gd1 Gd1 O1 C9 -93.6(3) 7_657 . . . ? O6 S1 O5 Gd1 80.2(4) . . . . ? O8 S1 O5 Gd1 -159.9(4) . . . . ? O7 S1 O5 Gd1 -40.1(4) . . . . ? O3 Gd1 O5 S1 -2.6(4) 6_556 . . . ? O7 Gd1 O5 S1 60.4(5) 7_657 . . . ? O13 Gd1 O5 S1 -83.1(4) . . . . ? O4 Gd1 O5 S1 124.3(4) 4_656 . . . ? O12 Gd1 O5 S1 -157.3(4) . . . . ? O1 Gd1 O5 S1 -172.9(3) . . . . ? O2 Gd1 O5 S1 -76.4(5) . . . . ? O3 Gd1 O5 S1 75.3(4) 4_656 . . . ? C1 Gd1 O5 S1 101.7(4) 4_656 . . . ? Gd1 Gd1 O5 S1 38.8(4) 7_657 . . . ? C4 N1 C5 N2 1.1(5) . . . . ? Ni1 N1 C5 N2 -162.5(3) . . . . ? O6 S1 O7 Gd1 -121.4(4) . . . 7_657 ? O8 S1 O7 Gd1 119.3(4) . . . 7_657 ? O5 S1 O7 Gd1 -0.5(5) . . . 7_657 ? C3 C4 C6 N2 -176.5(4) . . . . ? N1 C4 C6 N2 1.1(4) . . . . ? C3 C4 C6 C7 5.0(6) . . . . ? N1 C4 C6 C7 -177.4(3) . . . . ? C7 C8 C2 C3 3.4(6) . . . . ? C9 C8 C2 C3 -171.2(4) . . . . ? C7 C8 C2 C1 -169.0(4) . . . . ? C9 C8 C2 C1 16.4(6) . . . . ? O4 C1 C2 C3 -146.3(4) . . . . ? O3 C1 C2 C3 30.8(6) . . . . ? Gd1 C1 C2 C3 -110.2(12) 4_646 . . . ? O4 C1 C2 C8 26.3(6) . . . . ? O3 C1 C2 C8 -156.5(4) . . . . ? Gd1 C1 C2 C8 62.4(13) 4_646 . . . ? C8 C2 C3 C4 -1.9(6) . . . . ? C1 C2 C3 C4 170.6(4) . . . . ? N1 C4 C3 C2 -179.1(4) . . . . ? C6 C4 C3 C2 -2.2(6) . . . . ? C2 C8 C7 C6 -0.7(6) . . . . ? C9 C8 C7 C6 174.1(3) . . . . ? N2 C6 C7 C8 178.5(4) . . . . ? C4 C6 C7 C8 -3.4(6) . . . . ? C5 N1 Ni1 O10 -40.1(3) . . . . ? C4 N1 Ni1 O10 161.6(4) . . . . ? C5 N1 Ni1 O10 133.9(3) . . . 2_655 ? C4 N1 Ni1 O10 -24.4(4) . . . 2_655 ? C5 N1 Ni1 O9 46.9(3) . . . . ? C4 N1 Ni1 O9 -111.4(4) . . . . ? C5 N1 Ni1 N1 46.9(3) . . . 2_655 ? C4 N1 Ni1 N1 -111.4(4) . . . 2_655 ? C5 N1 Ni1 O11 -133.1(3) . . . . ? C4 N1 Ni1 O11 68.6(4) . . . . ? N1 C5 N2 C6 -0.4(5) . . . . ? C7 C6 N2 C5 177.9(4) . . . . ? C4 C6 N2 C5 -0.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.716 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.164 data_5 _database_code_depnum_ccdc_archive 'CCDC 862566' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N4 Ni O24 S2 Tb2' _chemical_formula_weight 1121.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 22.761(9) _cell_length_b 8.521(3) _cell_length_c 15.455(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.513(9) _cell_angle_gamma 90.00 _cell_volume 2926.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3473 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.86 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 5.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3312 _exptl_absorpt_correction_T_max 0.3965 _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 12891 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.86 _reflns_number_total 3473 _reflns_number_gt 2989 _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^)+(0.0221P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3473 _refine_ls_number_parameters 244 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 3.299 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3 O 0.2038(4) 0.6061(10) 0.0016(5) 0.0117(19) Uani 1 1 d . . . O4 O 0.1892(4) 0.6493(9) 0.1366(6) 0.0129(19) Uani 1 1 d . . . C8 C 0.1777(5) 0.5746(14) 0.0644(8) 0.011(3) Uani 1 1 d . . . Tb1 Tb 0.24718(2) 0.36115(7) 0.38230(4) 0.0086(2) Uani 1 1 d . . . Ni2 Ni 0.0000 0.2897(3) -0.2500 0.0172(6) Uani 1 2 d S . . S1 S 0.34993(13) 0.4609(4) 0.5851(2) 0.0101(6) Uani 1 1 d . . . O10 O 0.0000 0.0479(17) -0.2500 0.038(4) Uani 1 2 d SDU . . O2 O 0.1418(4) 0.4326(11) 0.2823(6) 0.018(2) Uani 1 1 d . . . O5 O 0.3341(4) 0.4206(10) 0.4898(5) 0.0130(19) Uani 1 1 d . . . N2 N -0.0217(5) 0.1800(13) 0.0036(7) 0.016(2) Uani 1 1 d . . . H2 H -0.0409 0.1257 0.0354 0.020 Uiso 1 1 calc R . . O7 O 0.3154(4) 0.3619(10) 0.6353(6) 0.016(2) Uani 1 1 d . . . O1 O 0.2109(4) 0.3227(10) 0.2240(6) 0.0148(19) Uani 1 1 d . . . C1 C 0.1584(6) 0.3814(14) 0.2155(8) 0.011(3) Uani 1 1 d . . . O9 O -0.0924(4) 0.2786(12) -0.2704(6) 0.022(2) Uani 1 1 d D . . O12 O 0.3211(4) 0.4565(10) 0.2984(6) 0.017(2) Uani 1 1 d . . . H12A H 0.3100 0.4761 0.2434 0.021 Uiso 1 1 d R . . H12B H 0.3576 0.4697 0.3247 0.021 Uiso 1 1 d R . . C12 C 0.1165(5) 0.3746(14) 0.1265(8) 0.011(3) Uani 1 1 d . . . C3 C 0.0302(5) 0.2627(15) 0.0339(8) 0.013(3) Uani 1 1 d . . . N1 N 0.0011(5) 0.2878(13) -0.1159(7) 0.018(2) Uani 1 1 d . . . C4 C -0.0373(6) 0.1988(15) -0.0840(9) 0.018(3) Uani 1 1 d . . . H4 H -0.0715 0.1541 -0.1193 0.022 Uiso 1 1 calc R . . C6 C 0.0941(5) 0.4311(15) -0.0321(8) 0.013(3) Uani 1 1 d . . . H6 H 0.1036 0.4800 -0.0811 0.016 Uiso 1 1 calc R . . C7 C 0.1295(5) 0.4538(14) 0.0519(8) 0.011(3) Uani 1 1 d . . . C5 C 0.0438(6) 0.3329(15) -0.0417(9) 0.015(3) Uani 1 1 d . . . O11 O 0.0000 0.5329(18) -0.2500 0.044(5) Uani 1 2 d SD . . C2 C 0.0665(5) 0.2795(15) 0.1179(8) 0.013(3) Uani 1 1 d . . . H2A H 0.0575 0.2286 0.1667 0.015 Uiso 1 1 calc R . . O8 O 0.4146(4) 0.4318(11) 0.6193(6) 0.019(2) Uani 1 1 d . . . O6 O 0.3364(4) 0.6270(10) 0.5979(6) 0.017(2) Uani 1 1 d . . . O13 O 0.2413(4) 0.6358(9) 0.3824(6) 0.020(2) Uani 1 1 d . . . H13A H 0.2179 0.6831 0.3401 0.024 Uiso 1 1 d R . . H13B H 0.2625 0.6880 0.4247 0.024 Uiso 1 1 d R . . H9A H -0.107(5) 0.370(7) -0.270(8) 0.024 Uiso 1 1 d D . . H9B H -0.110(5) 0.234(12) -0.317(5) 0.024 Uiso 1 1 d D . . H10A H 0.023(5) -0.006(13) -0.211(6) 0.024 Uiso 1 1 d D . . H11A H 0.027(5) 0.592(14) -0.221(9) 0.024 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 O3 0.012(4) 0.015(5) 0.009(4) 0.003(4) 0.003(4) 0.000(4) O4 0.015(5) 0.011(5) 0.011(5) -0.001(4) 0.001(4) -0.004(3) C8 0.010(6) 0.010(6) 0.010(6) 0.006(5) -0.001(5) 0.003(5) Tb1 0.0087(3) 0.0089(3) 0.0076(4) -0.0004(2) 0.0003(2) 0.0000(2) Ni2 0.0228(13) 0.0114(13) 0.0126(13) 0.000 -0.0065(11) 0.000 S1 0.0086(14) 0.0105(15) 0.0102(16) -0.0012(12) -0.0002(12) -0.0003(12) O10 0.043(10) 0.012(8) 0.040(10) 0.000 -0.034(8) 0.000 O2 0.027(5) 0.019(5) 0.010(5) 0.002(4) 0.003(4) 0.010(4) O5 0.013(4) 0.017(5) 0.008(4) -0.005(4) 0.001(4) -0.002(4) N2 0.015(6) 0.015(6) 0.018(6) 0.005(5) 0.001(5) -0.004(5) O7 0.020(5) 0.018(5) 0.010(5) 0.000(4) 0.000(4) -0.008(4) O1 0.012(4) 0.020(5) 0.011(5) 0.002(4) 0.000(4) 0.001(4) C1 0.013(6) 0.009(6) 0.011(7) 0.002(5) 0.004(5) -0.003(5) O9 0.030(6) 0.019(6) 0.012(5) -0.004(4) -0.008(4) 0.010(5) O12 0.015(5) 0.026(6) 0.009(4) 0.005(4) 0.000(4) -0.004(4) C12 0.012(6) 0.012(6) 0.008(6) -0.001(5) 0.003(5) 0.001(5) C3 0.012(6) 0.012(6) 0.016(7) 0.003(6) 0.004(5) -0.001(5) N1 0.018(6) 0.018(6) 0.013(6) 0.002(5) -0.004(5) -0.006(5) C4 0.013(6) 0.017(7) 0.021(8) 0.003(6) -0.005(6) -0.004(5) C6 0.017(6) 0.013(7) 0.010(6) 0.002(5) 0.002(5) -0.002(5) C7 0.011(6) 0.011(6) 0.011(6) 0.000(5) 0.001(5) -0.001(5) C5 0.015(6) 0.015(7) 0.013(7) 0.000(6) -0.001(6) -0.001(5) O11 0.091(17) 0.014(9) 0.032(11) 0.000 0.025(11) 0.000 C2 0.013(6) 0.014(7) 0.012(7) 0.003(5) 0.003(5) 0.000(5) O8 0.009(4) 0.025(6) 0.020(5) -0.009(4) -0.002(4) 0.003(4) O6 0.020(5) 0.009(5) 0.020(5) -0.003(4) -0.001(4) 0.003(4) O13 0.019(5) 0.008(5) 0.029(6) 0.002(4) -0.002(5) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C8 1.270(13) . ? O3 Tb1 2.290(8) 6_565 ? O3 Tb1 2.885(8) 4 ? O4 C8 1.262(14) . ? O4 Tb1 2.372(8) 4 ? C8 C7 1.487(16) . ? C8 Tb1 2.992(13) 4 ? Tb1 O3 2.290(8) 6_566 ? Tb1 O13 2.344(8) . ? Tb1 O5 2.346(8) . ? Tb1 O7 2.355(8) 7_556 ? Tb1 O4 2.372(8) 4_545 ? Tb1 O1 2.428(9) . ? Tb1 O12 2.473(8) . ? Tb1 O2 2.628(9) . ? Tb1 O3 2.885(8) 4_545 ? Tb1 C8 2.992(13) 4_545 ? Ni2 O10 2.060(15) . ? Ni2 O9 2.060(10) 2_554 ? Ni2 O9 2.060(10) . ? Ni2 N1 2.068(11) . ? Ni2 N1 2.068(11) 2_554 ? Ni2 O11 2.073(15) . ? S1 O6 1.472(8) . ? S1 O8 1.474(9) . ? S1 O5 1.479(8) . ? S1 O7 1.482(9) . ? O10 H10A 0.85(3) . ? O2 C1 1.253(14) . ? N2 C4 1.332(16) . ? N2 C3 1.369(15) . ? N2 H2 0.8600 . ? O7 Tb1 2.355(8) 7_556 ? O1 C1 1.274(14) . ? C1 C12 1.497(17) . ? O9 H9A 0.84(3) . ? O9 H9B 0.84(3) . ? O12 H12A 0.8500 . ? O12 H12B 0.8500 . ? C12 C2 1.380(16) . ? C12 C7 1.421(16) . ? C3 C2 1.387(17) . ? C3 C5 1.405(17) . ? N1 C4 1.329(15) . ? N1 C5 1.388(16) . ? C4 H4 0.9300 . ? C6 C7 1.385(17) . ? C6 C5 1.400(17) . ? C6 H6 0.9300 . ? O11 H11A 0.85(3) . ? C2 H2A 0.9300 . ? O13 H13A 0.8499 . ? O13 H13B 0.8500 . ? 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 C8 O3 Tb1 174.2(8) . 6_565 ? C8 O3 Tb1 82.3(7) . 4 ? Tb1 O3 Tb1 103.4(3) 6_565 4 ? C8 O4 Tb1 106.8(7) . 4 ? O4 C8 O3 121.9(11) . . ? O4 C8 C7 118.0(10) . . ? O3 C8 C7 120.0(11) . . ? O4 C8 Tb1 49.4(6) . 4 ? O3 C8 Tb1 72.8(7) . 4 ? C7 C8 Tb1 164.2(8) . 4 ? O3 Tb1 O13 81.0(3) 6_566 . ? O3 Tb1 O5 81.3(3) 6_566 . ? O13 Tb1 O5 79.8(3) . . ? O3 Tb1 O7 80.5(3) 6_566 7_556 ? O13 Tb1 O7 140.6(3) . 7_556 ? O5 Tb1 O7 130.7(3) . 7_556 ? O3 Tb1 O4 125.0(3) 6_566 4_545 ? O13 Tb1 O4 142.8(3) . 4_545 ? O5 Tb1 O4 78.9(3) . 4_545 ? O7 Tb1 O4 75.0(3) 7_556 4_545 ? O3 Tb1 O1 135.7(3) 6_566 . ? O13 Tb1 O1 97.4(3) . . ? O5 Tb1 O1 142.5(3) . . ? O7 Tb1 O1 73.1(3) 7_556 . ? O4 Tb1 O1 81.8(3) 4_545 . ? O3 Tb1 O12 147.5(3) 6_566 . ? O13 Tb1 O12 73.6(3) . . ? O5 Tb1 O12 74.6(3) . . ? O7 Tb1 O12 131.9(3) 7_556 . ? O4 Tb1 O12 71.5(3) 4_545 . ? O1 Tb1 O12 68.8(3) . . ? O3 Tb1 O2 86.9(3) 6_566 . ? O13 Tb1 O2 74.0(3) . . ? O5 Tb1 O2 152.7(3) . . ? O7 Tb1 O2 70.5(3) 7_556 . ? O4 Tb1 O2 127.5(3) 4_545 . ? O1 Tb1 O2 51.0(3) . . ? O12 Tb1 O2 104.7(3) . . ? O3 Tb1 O3 76.6(3) 6_566 4_545 ? O13 Tb1 O3 140.0(3) . 4_545 ? O5 Tb1 O3 64.5(3) . 4_545 ? O7 Tb1 O3 66.8(3) 7_556 4_545 ? O4 Tb1 O3 48.6(3) 4_545 4_545 ? O1 Tb1 O3 121.8(3) . 4_545 ? O12 Tb1 O3 111.0(3) . 4_545 ? O2 Tb1 O3 136.2(3) . 4_545 ? O3 Tb1 C8 101.4(3) 6_566 4_545 ? O13 Tb1 C8 147.6(3) . 4_545 ? O5 Tb1 C8 68.7(3) . 4_545 ? O7 Tb1 C8 70.6(3) 7_556 4_545 ? O4 Tb1 C8 23.8(3) 4_545 4_545 ? O1 Tb1 C8 102.5(3) . 4_545 ? O12 Tb1 C8 90.0(3) . 4_545 ? O2 Tb1 C8 138.2(3) . 4_545 ? O3 Tb1 C8 24.9(3) 4_545 4_545 ? O10 Ni2 O9 87.4(3) . 2_554 ? O10 Ni2 O9 87.4(3) . . ? O9 Ni2 O9 174.8(6) 2_554 . ? O10 Ni2 N1 89.6(3) . . ? O9 Ni2 N1 93.3(4) 2_554 . ? O9 Ni2 N1 86.7(4) . . ? O10 Ni2 N1 89.6(3) . 2_554 ? O9 Ni2 N1 86.7(4) 2_554 2_554 ? O9 Ni2 N1 93.3(4) . 2_554 ? N1 Ni2 N1 179.1(6) . 2_554 ? O10 Ni2 O11 180.000(1) . . ? O9 Ni2 O11 92.6(3) 2_554 . ? O9 Ni2 O11 92.6(3) . . ? N1 Ni2 O11 90.4(3) . . ? N1 Ni2 O11 90.4(3) 2_554 . ? O6 S1 O8 109.6(6) . . ? O6 S1 O5 110.2(5) . . ? O8 S1 O5 109.1(5) . . ? O6 S1 O7 109.1(5) . . ? O8 S1 O7 108.6(6) . . ? O5 S1 O7 110.3(5) . . ? Ni2 O10 H10A 123(9) . . ? C1 O2 Tb1 90.2(7) . . ? S1 O5 Tb1 137.9(5) . . ? C4 N2 C3 107.8(10) . . ? C4 N2 H2 126.1 . . ? C3 N2 H2 126.1 . . ? S1 O7 Tb1 140.8(5) . 7_556 ? C1 O1 Tb1 99.1(7) . . ? O2 C1 O1 119.7(12) . . ? O2 C1 C12 121.7(11) . . ? O1 C1 C12 118.4(11) . . ? Ni2 O9 H9A 110(9) . . ? Ni2 O9 H9B 116(9) . . ? H9A O9 H9B 107(6) . . ? Tb1 O12 H12A 120.1 . . ? Tb1 O12 H12B 119.9 . . ? H12A O12 H12B 120.0 . . ? C2 C12 C7 120.9(12) . . ? C2 C12 C1 117.3(11) . . ? C7 C12 C1 121.6(11) . . ? N2 C3 C2 131.9(11) . . ? N2 C3 C5 105.3(11) . . ? C2 C3 C5 122.7(11) . . ? C4 N1 C5 104.6(11) . . ? C4 N1 Ni2 120.6(9) . . ? C5 N1 Ni2 132.8(8) . . ? N1 C4 N2 113.2(12) . . ? N1 C4 H4 123.4 . . ? N2 C4 H4 123.4 . . ? C7 C6 C5 118.6(12) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C12 120.9(11) . . ? C6 C7 C8 118.7(11) . . ? C12 C7 C8 120.1(11) . . ? N1 C5 C6 131.6(12) . . ? N1 C5 C3 109.1(11) . . ? C6 C5 C3 119.3(12) . . ? Ni2 O11 H11A 126(10) . . ? C12 C2 C3 117.5(11) . . ? C12 C2 H2A 121.3 . . ? C3 C2 H2A 121.3 . . ? Tb1 O13 H13A 120.0 . . ? Tb1 O13 H13B 120.0 . . ? H13A O13 H13B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tb1 O4 C8 O3 7.4(14) 4 . . . ? Tb1 O4 C8 C7 -168.6(9) 4 . . . ? Tb1 O3 C8 O4 165(7) 6_565 . . . ? Tb1 O3 C8 O4 -5.9(11) 4 . . . ? Tb1 O3 C8 C7 -19(9) 6_565 . . . ? Tb1 O3 C8 C7 170.1(11) 4 . . . ? Tb1 O3 C8 Tb1 171(8) 6_565 . . 4 ? O3 Tb1 O2 C1 -165.4(7) 6_566 . . . ? O13 Tb1 O2 C1 113.1(7) . . . . ? O5 Tb1 O2 C1 130.3(7) . . . . ? O7 Tb1 O2 C1 -84.4(7) 7_556 . . . ? O4 Tb1 O2 C1 -32.4(8) 4_545 . . . ? O1 Tb1 O2 C1 -0.8(7) . . . . ? O12 Tb1 O2 C1 45.3(7) . . . . ? O3 Tb1 O2 C1 -98.5(7) 4_545 . . . ? C8 Tb1 O2 C1 -61.7(8) 4_545 . . . ? O6 S1 O5 Tb1 -78.9(9) . . . . ? O8 S1 O5 Tb1 160.8(7) . . . . ? O7 S1 O5 Tb1 41.6(9) . . . . ? O3 Tb1 O5 S1 -1.0(8) 6_566 . . . ? O13 Tb1 O5 S1 81.3(8) . . . . ? O7 Tb1 O5 S1 -70.4(9) 7_556 . . . ? O4 Tb1 O5 S1 -129.4(8) 4_545 . . . ? O1 Tb1 O5 S1 170.2(6) . . . . ? O12 Tb1 O5 S1 157.0(9) . . . . ? O2 Tb1 O5 S1 64.5(11) . . . . ? O3 Tb1 O5 S1 -80.2(8) 4_545 . . . ? C8 Tb1 O5 S1 -106.9(8) 4_545 . . . ? O6 S1 O7 Tb1 132.0(8) . . . 7_556 ? O8 S1 O7 Tb1 -108.6(9) . . . 7_556 ? O5 S1 O7 Tb1 10.9(10) . . . 7_556 ? O3 Tb1 O1 C1 22.9(9) 6_566 . . . ? O13 Tb1 O1 C1 -61.7(7) . . . . ? O5 Tb1 O1 C1 -144.6(7) . . . . ? O7 Tb1 O1 C1 79.1(7) 7_556 . . . ? O4 Tb1 O1 C1 155.9(7) 4_545 . . . ? O12 Tb1 O1 C1 -130.9(8) . . . . ? O2 Tb1 O1 C1 0.7(7) . . . . ? O3 Tb1 O1 C1 126.9(7) 4_545 . . . ? C8 Tb1 O1 C1 144.1(7) 4_545 . . . ? Tb1 O2 C1 O1 1.3(11) . . . . ? Tb1 O2 C1 C12 176.0(10) . . . . ? Tb1 O1 C1 O2 -1.4(12) . . . . ? Tb1 O1 C1 C12 -176.3(9) . . . . ? O2 C1 C12 C2 -62.6(17) . . . . ? O1 C1 C12 C2 112.2(13) . . . . ? O2 C1 C12 C7 121.7(13) . . . . ? O1 C1 C12 C7 -63.5(16) . . . . ? C4 N2 C3 C2 -177.7(14) . . . . ? C4 N2 C3 C5 0.7(14) . . . . ? O10 Ni2 N1 C4 -48.8(10) . . . . ? O9 Ni2 N1 C4 -136.1(10) 2_554 . . . ? O9 Ni2 N1 C4 38.6(10) . . . . ? N1 Ni2 N1 C4 -48.7(10) 2_554 . . . ? O11 Ni2 N1 C4 131.2(10) . . . . ? O10 Ni2 N1 C5 112.6(12) . . . . ? O9 Ni2 N1 C5 25.2(12) 2_554 . . . ? O9 Ni2 N1 C5 -160.0(12) . . . . ? N1 Ni2 N1 C5 112.6(12) 2_554 . . . ? O11 Ni2 N1 C5 -67.4(12) . . . . ? C5 N1 C4 N2 -1.7(16) . . . . ? Ni2 N1 C4 N2 164.3(9) . . . . ? C3 N2 C4 N1 0.6(16) . . . . ? C5 C6 C7 C12 2.5(19) . . . . ? C5 C6 C7 C8 -171.6(11) . . . . ? C2 C12 C7 C6 -3.5(19) . . . . ? C1 C12 C7 C6 172.1(11) . . . . ? C2 C12 C7 C8 170.4(11) . . . . ? C1 C12 C7 C8 -14.0(18) . . . . ? O4 C8 C7 C6 145.8(12) . . . . ? O3 C8 C7 C6 -30.3(17) . . . . ? Tb1 C8 C7 C6 112(3) 4 . . . ? O4 C8 C7 C12 -28.2(17) . . . . ? O3 C8 C7 C12 155.7(11) . . . . ? Tb1 C8 C7 C12 -62(4) 4 . . . ? C4 N1 C5 C6 -177.5(14) . . . . ? Ni2 N1 C5 C6 19(2) . . . . ? C4 N1 C5 C3 2.0(15) . . . . ? Ni2 N1 C5 C3 -161.5(9) . . . . ? C7 C6 C5 N1 -179.6(13) . . . . ? C7 C6 C5 C3 1.0(19) . . . . ? N2 C3 C5 N1 -1.7(14) . . . . ? C2 C3 C5 N1 176.9(12) . . . . ? N2 C3 C5 C6 177.9(12) . . . . ? C2 C3 C5 C6 -4(2) . . . . ? C7 C12 C2 C3 1.0(18) . . . . ? C1 C12 C2 C3 -174.8(11) . . . . ? N2 C3 C2 C12 -179.3(13) . . . . ? C5 C3 C2 C12 2.6(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.490 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.181 data_6 _database_code_depnum_ccdc_archive 'CCDC 862567' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Dy2 N4 Ni O24 S2' _chemical_formula_weight 1128.24 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' 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' Ni Ni 0.3393 1.1124 '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 22.529(9) _cell_length_b 8.625(3) _cell_length_c 15.467(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.641(8) _cell_angle_gamma 90.00 _cell_volume 2932.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3497 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.91 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 5.935 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3185 _exptl_absorpt_correction_T_max 0.8905 _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 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _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 12934 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0399 _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 -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.91 _reflns_number_total 3497 _reflns_number_gt 2929 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3497 _refine_ls_number_parameters 253 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 3.414 _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 O7 O 0.6667(4) 0.9262(13) 0.5097(5) 0.032(3) Uani 1 1 d . . . O13' O 0.7437(10) 0.376(3) 0.4139(19) 0.030(6) Uani 0.50 1 d PDU . . O13 O 0.7355(10) 0.363(3) 0.3672(11) 0.015(4) Uani 0.50 1 d PD . . C1 C 0.8395(6) 1.1181(14) 0.2844(7) 0.015(3) Uani 1 1 d . . . S1 S 0.65047(12) 0.9607(4) 0.41424(17) 0.0137(6) Uani 1 1 d . . . O6 O 0.6690(4) 1.1177(11) 0.3987(7) 0.033(3) Uani 1 1 d . . . C4 C 0.9691(5) 1.2369(14) 0.4666(7) 0.014(2) Uani 1 1 d . . . O12 O 0.8177(4) 0.5313(12) 0.3010(5) 0.032(2) Uani 1 1 d . . . H12A H 0.8500 0.5804 0.2983 0.038 Uiso 1 1 d R . . H12B H 0.8103 0.4442 0.2752 0.038 Uiso 1 1 d R . . O8 O 0.5847(4) 0.9458(14) 0.3829(6) 0.038(3) Uani 1 1 d . . . O11 O 1.0000 1.4469(18) 0.7500 0.041(4) Uani 1 2 d SD . . H11A H 1.021(6) 1.508(14) 0.786(8) 0.049 Uiso 1 1 d D . . C6 C 0.9558(5) 1.1651(14) 0.5409(7) 0.014(3) Uani 1 1 d . . . O9 O 1.0000 0.9670(19) 0.7500 0.042(4) Uani 1 2 d SD . . O5 O 0.6809(5) 0.8518(11) 0.3655(6) 0.035(3) Uani 1 1 d . . . O4 O 0.7965(4) 0.8870(12) 0.4982(6) 0.029(2) Uani 1 1 d . . . C2 C 0.8823(5) 1.1232(14) 0.3736(7) 0.013(2) Uani 1 1 d . . . C7 C 0.9059(5) 1.0659(15) 0.5322(7) 0.014(2) Uani 1 1 d . . . H7 H 0.8970 1.0164 0.5813 0.016 Uiso 1 1 calc R . . C5 C 1.0377(5) 1.2985(16) 0.5841(8) 0.020(3) Uani 1 1 d . . . H5 H 1.0722 1.3430 0.6196 0.024 Uiso 1 1 calc R . . C8 C 0.8700(5) 1.0434(14) 0.4480(7) 0.012(2) Uani 1 1 d . . . C9 C 0.8224(5) 0.9244(16) 0.4355(7) 0.018(3) Uani 1 1 d . . . C3 C 0.9324(5) 1.2207(15) 0.3820(7) 0.014(3) Uani 1 1 d . . . H3 H 0.9410 1.2727 0.3335 0.017 Uiso 1 1 calc R . . Dy1 Dy 0.74713(2) 0.64028(7) 0.38264(3) 0.0125(2) Uani 1 1 d . . . N1 N 0.9996(4) 1.2090(13) 0.6153(6) 0.016(2) Uani 1 1 d . . . N2 N 1.0216(4) 1.3188(12) 0.4966(7) 0.017(2) Uani 1 1 d . . . H2 H 1.0407 1.3733 0.4648 0.020 Uiso 1 1 calc R . . Ni2 Ni 1.0000 1.2073(3) 0.7500 0.0166(5) Uani 1 2 d S . . O1 O 0.8551(5) 1.0605(12) 0.2185(5) 0.037(3) Uani 1 1 d . . . O2 O 0.7884(4) 1.1812(13) 0.2755(5) 0.032(3) Uani 1 1 d . . . O3 O 0.8102(5) 0.8504(10) 0.3625(5) 0.029(3) Uani 1 1 d . . . O10 O 0.9074(4) 1.2199(11) 0.7278(5) 0.022(2) Uani 1 1 d . . . H10A H 0.8900 1.3079 0.7236 0.027 Uiso 1 1 d R . . H10B H 0.8863 1.1375 0.7227 0.027 Uiso 1 1 d R . . H13A H 0.7731(13) 0.359(15) 0.389(4) 0.027 Uiso 1 1 d D . . H13B H 0.722(5) 0.315(18) 0.414(10) 0.027 Uiso 1 1 d D . . H9A H 1.036(3) 0.936(17) 0.758(10) 0.027 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 O7 0.013(4) 0.073(8) 0.009(4) 0.013(5) -0.001(3) 0.002(5) O13' 0.007(9) 0.018(13) 0.065(15) 0.004(13) 0.004(12) -0.004(8) O13 0.021(11) 0.008(11) 0.010(8) 0.001(8) -0.007(8) -0.002(8) C1 0.021(6) 0.013(7) 0.012(5) 0.001(5) 0.005(5) -0.008(5) S1 0.0113(13) 0.0193(19) 0.0091(12) 0.0028(12) -0.0005(10) -0.0038(12) O6 0.025(5) 0.014(6) 0.051(6) 0.007(5) -0.009(5) -0.008(4) C4 0.008(5) 0.013(7) 0.020(6) 0.000(5) 0.003(4) -0.001(5) O12 0.047(6) 0.026(6) 0.020(4) -0.012(4) 0.002(4) 0.003(5) O8 0.013(5) 0.066(9) 0.028(5) 0.029(5) -0.010(4) -0.016(5) O11 0.050(10) 0.015(9) 0.038(8) 0.000 -0.033(7) 0.000 C6 0.013(6) 0.014(7) 0.013(5) -0.005(5) 0.000(4) -0.001(5) O9 0.065(12) 0.024(10) 0.051(9) 0.000 0.041(10) 0.000 O5 0.059(7) 0.023(7) 0.013(4) -0.007(4) -0.013(4) 0.022(5) O4 0.013(4) 0.051(7) 0.021(4) 0.022(4) 0.000(4) -0.008(4) C2 0.015(6) 0.013(7) 0.011(5) 0.000(5) 0.003(4) -0.001(5) C7 0.014(6) 0.016(7) 0.011(5) 0.000(5) 0.002(4) -0.004(5) C5 0.017(6) 0.021(8) 0.019(6) 0.002(5) -0.004(5) -0.004(5) C8 0.012(5) 0.014(7) 0.011(5) 0.001(5) 0.002(4) -0.002(5) C9 0.020(6) 0.019(8) 0.014(5) 0.012(5) 0.001(5) -0.003(5) C3 0.017(6) 0.013(7) 0.014(5) 0.002(5) 0.006(4) -0.002(5) Dy1 0.0150(3) 0.0129(4) 0.0077(3) 0.0017(2) -0.0015(2) -0.0046(2) N1 0.015(5) 0.015(6) 0.015(5) 0.000(4) -0.004(4) -0.005(4) N2 0.015(5) 0.015(6) 0.019(5) 0.001(4) -0.001(4) -0.007(4) Ni2 0.0156(11) 0.0157(14) 0.0158(10) 0.000 -0.0027(8) 0.000 O1 0.068(8) 0.029(7) 0.010(4) 0.000(4) 0.001(4) 0.026(6) O2 0.013(5) 0.071(8) 0.011(4) -0.001(4) 0.001(3) 0.001(5) O3 0.045(6) 0.022(6) 0.013(4) 0.006(4) -0.009(4) -0.021(4) O10 0.019(5) 0.020(6) 0.025(4) -0.008(4) -0.001(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O7 S1 1.472(8) . ? O7 Dy1 2.336(8) 7_666 ? O13' Dy1 2.33(2) . ? O13' H13A 0.85(2) . ? O13' H13B 0.72(11) . ? O13 Dy1 2.42(2) . ? O13 H13A 0.84(2) . ? O13 H13B 0.94(11) . ? C1 O1 1.251(14) . ? C1 O2 1.254(15) . ? C1 C2 1.501(15) . ? C1 Dy1 2.883(12) 4_655 ? S1 O6 1.452(9) . ? S1 O8 1.460(8) . ? S1 O5 1.464(10) . ? C4 N2 1.369(14) . ? C4 C3 1.393(14) . ? C4 C6 1.393(16) . ? O12 Dy1 2.426(9) . ? O12 H12A 0.8498 . ? O12 H12B 0.8499 . ? O11 Ni2 2.067(16) . ? O11 H11A 0.84(3) . ? C6 N1 1.394(14) . ? C6 C7 1.396(16) . ? O9 Ni2 2.073(17) . ? O9 H9A 0.85(3) . ? O5 Dy1 2.335(9) . ? O4 C9 1.278(13) . ? O4 Dy1 2.283(9) 7_666 ? O4 Dy1 2.844(10) . ? C2 C3 1.390(16) . ? C2 C8 1.420(15) . ? C7 C8 1.387(14) . ? C7 H7 0.9300 . ? C5 N1 1.321(15) . ? C5 N2 1.334(15) . ? C5 H5 0.9300 . ? C8 C9 1.466(16) . ? C9 O3 1.274(15) . ? C3 H3 0.9300 . ? Dy1 O4 2.283(9) 7_666 ? Dy1 O7 2.336(8) 7_666 ? Dy1 O3 2.365(9) . ? Dy1 O2 2.428(8) 4_645 ? Dy1 O1 2.578(9) 4_645 ? Dy1 C1 2.883(12) 4_645 ? Dy1 H13A 2.50(12) . ? N1 Ni2 2.082(9) . ? N2 H2 0.8600 . ? Ni2 O10 2.042(8) 2_756 ? Ni2 O10 2.042(8) . ? Ni2 N1 2.082(9) 2_756 ? O1 Dy1 2.578(9) 4_655 ? O2 Dy1 2.428(8) 4_655 ? O10 H10A 0.8499 . ? O10 H10B 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 O7 Dy1 138.6(5) . 7_666 ? Dy1 O13' H13A 91(9) . . ? Dy1 O13' H13B 141(10) . . ? H13A O13' H13B 118(10) . . ? Dy1 O13 H13A 86(9) . . ? Dy1 O13 H13B 114(10) . . ? H13A O13 H13B 98(8) . . ? O1 C1 O2 119.9(11) . . ? O1 C1 C2 121.4(11) . . ? O2 C1 C2 118.5(11) . . ? O1 C1 Dy1 63.4(6) . 4_655 ? O2 C1 Dy1 56.5(6) . 4_655 ? C2 C1 Dy1 173.9(9) . 4_655 ? O6 S1 O8 109.5(6) . . ? O6 S1 O5 109.2(6) . . ? O8 S1 O5 109.2(6) . . ? O6 S1 O7 109.7(6) . . ? O8 S1 O7 109.0(5) . . ? O5 S1 O7 110.2(6) . . ? N2 C4 C3 131.3(11) . . ? N2 C4 C6 106.0(10) . . ? C3 C4 C6 122.7(10) . . ? Dy1 O12 H12A 119.9 . . ? Dy1 O12 H12B 120.1 . . ? H12A O12 H12B 120.0 . . ? Ni2 O11 H11A 129(10) . . ? C4 C6 N1 108.6(10) . . ? C4 C6 C7 120.4(10) . . ? N1 C6 C7 131.0(11) . . ? Ni2 O9 H9A 108(10) . . ? S1 O5 Dy1 143.3(5) . . ? C9 O4 Dy1 170.9(10) . 7_666 ? C9 O4 Dy1 83.9(8) . . ? Dy1 O4 Dy1 104.6(3) 7_666 . ? C3 C2 C8 121.1(10) . . ? C3 C2 C1 116.7(10) . . ? C8 C2 C1 122.0(10) . . ? C8 C7 C6 117.9(11) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? N1 C5 N2 113.1(11) . . ? N1 C5 H5 123.4 . . ? N2 C5 H5 123.4 . . ? C7 C8 C2 121.0(11) . . ? C7 C8 C9 118.8(10) . . ? C2 C8 C9 119.9(10) . . ? O3 C9 O4 120.0(12) . . ? O3 C9 C8 118.6(10) . . ? O4 C9 C8 121.2(11) . . ? C2 C3 C4 116.8(10) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? O4 Dy1 O13' 72.1(7) 7_666 . ? O4 Dy1 O5 78.1(4) 7_666 . ? O13' Dy1 O5 137.5(6) . . ? O4 Dy1 O7 80.6(3) 7_666 7_666 ? O13' Dy1 O7 70.9(6) . 7_666 ? O5 Dy1 O7 133.1(3) . 7_666 ? O4 Dy1 O3 124.2(3) 7_666 . ? O13' Dy1 O3 145.4(6) . . ? O5 Dy1 O3 76.9(4) . . ? O7 Dy1 O3 81.5(3) 7_666 . ? O4 Dy1 O13 85.5(6) 7_666 . ? O13' Dy1 O13 17.2(7) . . ? O5 Dy1 O13 135.3(6) . . ? O7 Dy1 O13 83.3(5) 7_666 . ? O3 Dy1 O13 143.3(6) . . ? O4 Dy1 O12 145.8(3) 7_666 . ? O13' Dy1 O12 77.6(7) . . ? O5 Dy1 O12 136.0(3) . . ? O7 Dy1 O12 74.8(3) 7_666 . ? O3 Dy1 O12 75.3(4) . . ? O13 Dy1 O12 68.5(6) . . ? O4 Dy1 O2 136.4(3) 7_666 4_645 ? O13' Dy1 O2 109.4(7) . 4_645 ? O5 Dy1 O2 73.2(3) . 4_645 ? O7 Dy1 O2 142.5(3) 7_666 4_645 ? O3 Dy1 O2 80.2(3) . 4_645 ? O13 Dy1 O2 92.3(5) . 4_645 ? O12 Dy1 O2 68.9(3) . 4_645 ? O4 Dy1 O1 88.7(3) 7_666 4_645 ? O13' Dy1 O1 78.4(6) . 4_645 ? O5 Dy1 O1 71.1(3) . 4_645 ? O7 Dy1 O1 149.3(4) 7_666 4_645 ? O3 Dy1 O1 127.4(3) . 4_645 ? O13 Dy1 O1 67.2(5) . 4_645 ? O12 Dy1 O1 100.4(3) . 4_645 ? O2 Dy1 O1 51.2(3) 4_645 4_645 ? O4 Dy1 O4 75.4(3) 7_666 . ? O13' Dy1 O4 128.8(7) . . ? O5 Dy1 O4 68.8(3) . . ? O7 Dy1 O4 65.5(3) 7_666 . ? O3 Dy1 O4 49.2(3) . . ? O13 Dy1 O4 145.4(4) . . ? O12 Dy1 O4 114.0(3) . . ? O2 Dy1 O4 121.4(3) 4_645 . ? O1 Dy1 O4 139.1(3) 4_645 . ? O4 Dy1 C1 113.0(3) 7_666 4_645 ? O13' Dy1 C1 94.3(7) . 4_645 ? O5 Dy1 C1 70.1(3) . 4_645 ? O7 Dy1 C1 156.4(3) 7_666 4_645 ? O3 Dy1 C1 104.0(3) . 4_645 ? O13 Dy1 C1 78.9(5) . 4_645 ? O12 Dy1 C1 84.3(3) . 4_645 ? O2 Dy1 C1 25.5(3) 4_645 4_645 ? O1 Dy1 C1 25.7(3) 4_645 4_645 ? O4 Dy1 C1 135.0(3) . 4_645 ? O4 Dy1 H13A 90.4(14) 7_666 . ? O13' Dy1 H13A 19.9(12) . . ? O5 Dy1 H13A 154.7(11) . . ? O7 Dy1 H13A 65.3(12) 7_666 . ? O3 Dy1 H13A 127.5(12) . . ? O13 Dy1 H13A 19.7(9) . . ? O12 Dy1 H13A 57.9(13) . . ? O2 Dy1 H13A 101.8(14) 4_645 . ? O1 Dy1 H13A 86.3(11) 4_645 . ? O4 Dy1 H13A 130.4(12) . . ? C1 Dy1 H13A 94.4(13) 4_645 . ? C5 N1 C6 104.8(9) . . ? C5 N1 Ni2 120.6(8) . . ? C6 N1 Ni2 132.2(8) . . ? C5 N2 C4 107.4(10) . . ? C5 N2 H2 126.3 . . ? C4 N2 H2 126.3 . . ? O10 Ni2 O10 173.9(6) 2_756 . ? O10 Ni2 O11 87.0(3) 2_756 . ? O10 Ni2 O11 87.0(3) . . ? O10 Ni2 O9 93.0(3) 2_756 . ? O10 Ni2 O9 93.0(3) . . ? O11 Ni2 O9 180.000(9) . . ? O10 Ni2 N1 87.0(3) 2_756 . ? O10 Ni2 N1 92.9(3) . . ? O11 Ni2 N1 89.6(3) . . ? O9 Ni2 N1 90.4(3) . . ? O10 Ni2 N1 92.9(3) 2_756 2_756 ? O10 Ni2 N1 87.0(3) . 2_756 ? O11 Ni2 N1 89.6(3) . 2_756 ? O9 Ni2 N1 90.4(3) . 2_756 ? N1 Ni2 N1 179.2(6) . 2_756 ? C1 O1 Dy1 90.9(8) . 4_655 ? C1 O2 Dy1 98.0(7) . 4_655 ? C9 O3 Dy1 106.7(8) . . ? Ni2 O10 H10A 119.8 . . ? Ni2 O10 H10B 120.2 . . ? H10A O10 H10B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 O7 S1 O6 -77.9(11) 7_666 . . . ? Dy1 O7 S1 O8 162.1(9) 7_666 . . . ? Dy1 O7 S1 O5 42.3(12) 7_666 . . . ? N2 C4 C6 N1 1.9(14) . . . . ? C3 C4 C6 N1 -177.6(11) . . . . ? N2 C4 C6 C7 -177.1(11) . . . . ? C3 C4 C6 C7 3.4(19) . . . . ? O6 S1 O5 Dy1 120.3(11) . . . . ? O8 S1 O5 Dy1 -120.0(11) . . . . ? O7 S1 O5 Dy1 -0.3(14) . . . . ? O1 C1 C2 C3 68.1(17) . . . . ? O2 C1 C2 C3 -107.8(14) . . . . ? Dy1 C1 C2 C3 -73(8) 4_655 . . . ? O1 C1 C2 C8 -117.3(14) . . . . ? O2 C1 C2 C8 66.9(17) . . . . ? Dy1 C1 C2 C8 101(8) 4_655 . . . ? C4 C6 C7 C8 -0.8(18) . . . . ? N1 C6 C7 C8 -179.5(12) . . . . ? C6 C7 C8 C2 -2.3(18) . . . . ? C6 C7 C8 C9 171.9(11) . . . . ? C3 C2 C8 C7 3.0(18) . . . . ? C1 C2 C8 C7 -171.4(11) . . . . ? C3 C2 C8 C9 -171.1(12) . . . . ? C1 C2 C8 C9 14.5(18) . . . . ? Dy1 O4 C9 O3 -154(4) 7_666 . . . ? Dy1 O4 C9 O3 5.2(12) . . . . ? Dy1 O4 C9 C8 31(6) 7_666 . . . ? Dy1 O4 C9 C8 -169.8(12) . . . . ? C7 C8 C9 O3 -146.2(12) . . . . ? C2 C8 C9 O3 28.0(18) . . . . ? C7 C8 C9 O4 28.8(18) . . . . ? C2 C8 C9 O4 -157.0(11) . . . . ? C8 C2 C3 C4 -0.5(18) . . . . ? C1 C2 C3 C4 174.2(11) . . . . ? N2 C4 C3 C2 178.0(13) . . . . ? C6 C4 C3 C2 -2.6(18) . . . . ? S1 O5 Dy1 O4 27.7(11) . . . 7_666 ? S1 O5 Dy1 O13' 73.8(16) . . . . ? S1 O5 Dy1 O7 -37.1(14) . . . 7_666 ? S1 O5 Dy1 O3 -102.0(12) . . . . ? S1 O5 Dy1 O13 98.7(13) . . . . ? S1 O5 Dy1 O12 -154.1(10) . . . . ? S1 O5 Dy1 O2 174.4(13) . . . 4_645 ? S1 O5 Dy1 O1 120.5(13) . . . 4_645 ? S1 O5 Dy1 O4 -51.0(11) . . . . ? S1 O5 Dy1 C1 147.7(13) . . . 4_645 ? C9 O4 Dy1 O4 -176.7(9) . . . 7_666 ? Dy1 O4 Dy1 O4 0.0 7_666 . . 7_666 ? C9 O4 Dy1 O13' 131.4(10) . . . . ? Dy1 O4 Dy1 O13' -51.9(8) 7_666 . . . ? C9 O4 Dy1 O5 -94.0(8) . . . . ? Dy1 O4 Dy1 O5 82.7(4) 7_666 . . . ? C9 O4 Dy1 O7 97.1(7) . . . 7_666 ? Dy1 O4 Dy1 O7 -86.2(4) 7_666 . . 7_666 ? C9 O4 Dy1 O3 -3.2(7) . . . . ? Dy1 O4 Dy1 O3 173.5(5) 7_666 . . . ? C9 O4 Dy1 O13 124.7(12) . . . . ? Dy1 O4 Dy1 O13 -58.6(11) 7_666 . . . ? C9 O4 Dy1 O12 38.2(8) . . . . ? Dy1 O4 Dy1 O12 -145.1(3) 7_666 . . . ? C9 O4 Dy1 O2 -40.9(8) . . . 4_645 ? Dy1 O4 Dy1 O2 135.8(3) 7_666 . . 4_645 ? C9 O4 Dy1 O1 -106.4(7) . . . 4_645 ? Dy1 O4 Dy1 O1 70.4(5) 7_666 . . 4_645 ? C9 O4 Dy1 C1 -68.7(8) . . . 4_645 ? Dy1 O4 Dy1 C1 108.0(4) 7_666 . . 4_645 ? N2 C5 N1 C6 1.3(15) . . . . ? N2 C5 N1 Ni2 -163.0(8) . . . . ? C4 C6 N1 C5 -2.0(14) . . . . ? C7 C6 N1 C5 176.9(13) . . . . ? C4 C6 N1 Ni2 159.8(9) . . . . ? C7 C6 N1 Ni2 -21(2) . . . . ? N1 C5 N2 C4 -0.1(16) . . . . ? C3 C4 N2 C5 178.4(13) . . . . ? C6 C4 N2 C5 -1.1(14) . . . . ? C5 N1 Ni2 O10 -39.4(10) . . . 2_756 ? C6 N1 Ni2 O10 161.2(12) . . . 2_756 ? C5 N1 Ni2 O10 134.5(10) . . . . ? C6 N1 Ni2 O10 -24.9(12) . . . . ? C5 N1 Ni2 O11 47.5(10) . . . . ? C6 N1 Ni2 O11 -111.9(11) . . . . ? C5 N1 Ni2 O9 -132.5(10) . . . . ? C6 N1 Ni2 O9 68.1(11) . . . . ? C5 N1 Ni2 N1 47.5(11) . . . 2_756 ? C6 N1 Ni2 N1 -111.9(10) . . . 2_756 ? O2 C1 O1 Dy1 0.0(13) . . . 4_655 ? C2 C1 O1 Dy1 -175.8(10) . . . 4_655 ? O1 C1 O2 Dy1 0.0(14) . . . 4_655 ? C2 C1 O2 Dy1 175.9(9) . . . 4_655 ? O4 C9 O3 Dy1 -6.5(15) . . . . ? C8 C9 O3 Dy1 168.6(9) . . . . ? O4 Dy1 O3 C9 10.9(10) 7_666 . . . ? O13' Dy1 O3 C9 -98.5(15) . . . . ? O5 Dy1 O3 C9 76.5(9) . . . . ? O7 Dy1 O3 C9 -61.6(9) 7_666 . . . ? O13 Dy1 O3 C9 -128.0(10) . . . . ? O12 Dy1 O3 C9 -138.0(9) . . . . ? O2 Dy1 O3 C9 151.3(9) 4_645 . . . ? O1 Dy1 O3 C9 129.9(8) 4_645 . . . ? O4 Dy1 O3 C9 3.3(8) . . . . ? C1 Dy1 O3 C9 141.8(8) 4_645 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.070 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.161 data_7 _database_code_depnum_ccdc_archive 'CCDC 862568' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Ho2 N4 Ni O24 S2' _chemical_formula_weight 1133.10 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _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 22.488(2) _cell_length_b 8.6668(9) _cell_length_c 15.4291(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.904(2) _cell_angle_gamma 90.00 _cell_volume 2931.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 6.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3684 _exptl_absorpt_correction_T_max 0.3684 _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 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _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 9252 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0559 _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 3.55 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2588 _reflns_number_gt 2180 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+15.3083P] 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 2588 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.752589(16) 0.36047(4) 0.11703(2) 0.01632(12) Uani 1 1 d . . . Ni1 Ni 1.0000 0.29276(17) 0.7500 0.0243(3) Uani 1 2 d S . . C1 C 0.9304(4) 0.2825(9) 0.3826(5) 0.0230(18) Uani 1 1 d . . . H1 H 0.9382 0.2290 0.3340 0.028 Uiso 1 1 calc R . . C2 C 0.8812(3) 0.3795(8) 0.3730(5) 0.0188(17) Uani 1 1 d . . . C3 C 0.8689(3) 0.4578(8) 0.4479(4) 0.0172(17) Uani 1 1 d . . . C4 C 0.9052(4) 0.4341(9) 0.5316(5) 0.0228(18) Uani 1 1 d . . . H4 H 0.8965 0.4838 0.5807 0.027 Uiso 1 1 calc R . . C5 C 0.9551(3) 0.3350(9) 0.5416(5) 0.0212(17) Uani 1 1 d . . . C6 C 0.9683(4) 0.2660(8) 0.4659(5) 0.0224(18) Uani 1 1 d . . . C7 C 1.0376(4) 0.2039(10) 0.5844(5) 0.033(2) Uani 1 1 d . . . H7 H 1.0726 0.1608 0.6197 0.040 Uiso 1 1 calc R . . C8 C 0.8369(4) 0.3847(8) 0.2847(5) 0.0214(18) Uani 1 1 d . . . C9 C 0.8221(3) 0.5771(9) 0.4362(5) 0.0194(17) Uani 1 1 d . . . N1 N 1.0206(3) 0.1845(8) 0.4963(4) 0.0288(17) Uani 1 1 d . . . H1A H 1.0395 0.1300 0.4644 0.035 Uiso 1 1 calc R . . N2 N 0.9990(3) 0.2912(7) 0.6158(4) 0.0280(16) Uani 1 1 d . . . O1 O 0.7867(2) 0.3187(6) 0.2762(3) 0.0284(13) Uani 1 1 d . . . O2 O 0.8528(3) 0.4416(7) 0.2180(3) 0.0412(17) Uani 1 1 d . . . O3 O 0.8101(2) 0.6519(6) 0.3640(3) 0.0281(13) Uani 1 1 d . . . O4 O 0.7959(2) 0.6123(6) 0.4989(3) 0.0236(13) Uani 1 1 d . . . O5 O 0.8192(3) 0.1526(6) 0.1354(3) 0.0327(14) Uani 1 1 d . . . O6 O 0.8341(2) 0.0770(6) -0.0091(3) 0.0242(13) Uani 1 1 d . . . O7 O 0.8323(3) -0.1112(6) 0.1038(4) 0.0411(16) Uani 1 1 d . . . O8 O 0.9158(2) 0.0622(7) 0.1181(4) 0.0361(15) Uani 1 1 d . . . O9 O 0.7585(3) 0.6325(6) 0.1073(5) 0.0523(18) Uani 1 1 d . . . H9A H 0.7813 0.6832 0.1490 0.063 Uiso 1 1 d R . . H9B H 0.7380 0.6794 0.0620 0.063 Uiso 1 1 d R . . O10 O 0.6820(3) 0.4711(6) 0.1982(4) 0.0382(15) Uani 1 1 d . . . H10A H 0.6940 0.4929 0.2530 0.046 Uiso 1 1 d R . . H10B H 0.6452 0.4880 0.1717 0.046 Uiso 1 1 d R . . O11 O 1.0000 0.5337(10) 0.7500 0.054(3) Uani 1 2 d S . . H11A H 0.9665 0.5828 0.7415 0.065 Uiso 0.50 1 d PR . . H11B H 1.0335 0.5828 0.7585 0.065 Uiso 0.50 1 d PR . . O12 O 0.9068(3) 0.2822(6) 0.7265(3) 0.0322(14) Uani 1 1 d . . . H12A H 0.8860 0.3648 0.7212 0.039 Uiso 1 1 d R . . H12B H 0.8890 0.1951 0.7220 0.039 Uiso 1 1 d R . . O13 O 1.0000 0.0569(9) 0.7500 0.051(3) Uani 1 2 d S . . H13B H 0.9728 -0.0076 0.7256 0.061 Uiso 1 1 d R . . S1 S 0.85008(9) 0.0447(2) 0.08651(12) 0.0190(4) 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 Ho1 0.01807(19) 0.01875(18) 0.01128(18) 0.00067(17) 0.00146(13) -0.00082(18) Ni1 0.0265(8) 0.0234(8) 0.0195(8) 0.000 -0.0023(7) 0.000 C1 0.033(5) 0.022(4) 0.015(4) 0.000(3) 0.007(4) 0.007(4) C2 0.020(4) 0.018(4) 0.018(4) 0.002(3) 0.001(3) 0.000(3) C3 0.020(4) 0.021(4) 0.011(4) 0.000(3) 0.004(3) 0.002(3) C4 0.030(5) 0.024(4) 0.016(4) -0.002(4) 0.006(4) 0.003(4) C5 0.020(4) 0.023(4) 0.019(4) -0.001(4) 0.002(3) 0.003(3) C6 0.024(5) 0.014(4) 0.029(5) 0.004(4) 0.006(4) 0.005(3) C7 0.025(5) 0.047(6) 0.024(5) 0.000(4) -0.002(4) 0.010(4) C8 0.036(5) 0.009(4) 0.018(4) 0.000(3) 0.006(4) 0.004(4) C9 0.018(4) 0.029(4) 0.009(4) -0.004(3) -0.001(3) -0.006(3) N1 0.029(4) 0.035(4) 0.021(4) -0.001(3) 0.004(3) 0.019(3) N2 0.028(4) 0.031(4) 0.019(4) 0.003(3) -0.007(3) 0.009(3) O1 0.027(3) 0.040(4) 0.016(3) -0.006(3) -0.001(2) -0.004(3) O2 0.061(4) 0.047(4) 0.012(3) 0.004(3) 0.002(3) -0.026(4) O3 0.035(3) 0.026(3) 0.020(3) 0.003(3) 0.001(2) 0.011(3) O4 0.022(3) 0.031(3) 0.020(3) -0.009(2) 0.008(2) 0.002(2) O5 0.042(4) 0.036(3) 0.016(3) 0.001(3) -0.002(3) 0.022(3) O6 0.025(3) 0.034(3) 0.012(3) 0.006(2) -0.001(2) 0.006(3) O7 0.050(4) 0.025(4) 0.045(4) 0.010(3) 0.002(3) -0.010(3) O8 0.018(3) 0.061(4) 0.027(3) 0.017(3) -0.001(3) -0.003(3) O9 0.046(4) 0.022(3) 0.090(6) -0.006(4) 0.017(4) -0.001(3) O10 0.042(4) 0.047(4) 0.025(3) -0.003(3) 0.005(3) 0.015(3) O11 0.086(8) 0.029(5) 0.055(6) 0.000 0.034(6) 0.000 O12 0.034(4) 0.026(3) 0.033(3) -0.001(3) -0.001(3) 0.004(3) O13 0.057(6) 0.019(5) 0.055(6) 0.000 -0.033(5) 0.000 S1 0.0184(10) 0.0220(11) 0.0153(10) 0.0047(8) 0.0013(8) 0.0012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O4 2.263(4) 6_565 ? Ho1 O5 2.319(5) . ? Ho1 O6 2.328(5) 7_655 ? Ho1 O3 2.350(5) 4_645 ? Ho1 O9 2.368(6) . ? Ho1 O10 2.428(5) . ? Ho1 O1 2.431(5) . ? Ho1 O2 2.537(6) . ? Ho1 O4 2.854(5) 4_645 ? Ho1 C9 2.985(8) 4_645 ? Ni1 O13 2.044(8) . ? Ni1 O12 2.048(6) . ? Ni1 O12 2.048(6) 2_756 ? Ni1 N2 2.066(6) . ? Ni1 N2 2.066(6) 2_756 ? Ni1 O11 2.088(8) . ? C1 C2 1.371(10) . ? C1 C6 1.382(10) . ? C1 H1 0.9300 . ? C2 C3 1.420(9) . ? C2 C8 1.498(10) . ? C3 C4 1.380(10) . ? C3 C9 1.458(10) . ? C4 C5 1.394(10) . ? C4 H4 0.9300 . ? C5 N2 1.386(9) . ? C5 C6 1.402(10) . ? C6 N1 1.363(9) . ? C7 N2 1.321(10) . ? C7 N1 1.338(10) . ? C7 H7 0.9300 . ? C8 O1 1.246(9) . ? C8 O2 1.263(8) . ? C9 O3 1.265(8) . ? C9 O4 1.276(8) . ? C9 Ho1 2.985(8) 4_655 ? N1 H1A 0.8600 . ? O3 Ho1 2.350(5) 4_655 ? O4 Ho1 2.263(4) 6_566 ? O4 Ho1 2.854(5) 4_655 ? O5 S1 1.470(5) . ? O6 S1 1.465(5) . ? O6 Ho1 2.328(5) 7_655 ? O7 S1 1.451(5) . ? O8 S1 1.457(5) . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? O11 H11A 0.8500 . ? O11 H11B 0.8500 . ? O12 H12A 0.8500 . ? O12 H12B 0.8499 . ? O13 H13B 0.8511 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ho1 O5 78.29(18) 6_565 . ? O4 Ho1 O6 80.90(17) 6_565 7_655 ? O5 Ho1 O6 133.08(18) . 7_655 ? O4 Ho1 O3 123.98(18) 6_565 4_645 ? O5 Ho1 O3 77.1(2) . 4_645 ? O6 Ho1 O3 80.72(18) 7_655 4_645 ? O4 Ho1 O9 78.7(2) 6_565 . ? O5 Ho1 O9 137.5(2) . . ? O6 Ho1 O9 76.9(2) 7_655 . ? O3 Ho1 O9 144.8(2) 4_645 . ? O4 Ho1 O10 145.38(18) 6_565 . ? O5 Ho1 O10 136.26(18) . . ? O6 Ho1 O10 74.78(18) 7_655 . ? O3 Ho1 O10 76.11(19) 4_645 . ? O9 Ho1 O10 72.1(2) . . ? O4 Ho1 O1 137.19(18) 6_565 . ? O5 Ho1 O1 73.23(17) . . ? O6 Ho1 O1 141.50(18) 7_655 . ? O3 Ho1 O1 79.76(18) 4_645 . ? O9 Ho1 O1 101.7(2) . . ? O10 Ho1 O1 68.47(19) . . ? O4 Ho1 O2 89.00(18) 6_565 . ? O5 Ho1 O2 71.3(2) . . ? O6 Ho1 O2 149.58(19) 7_655 . ? O3 Ho1 O2 127.72(18) 4_645 . ? O9 Ho1 O2 73.0(2) . . ? O10 Ho1 O2 99.6(2) . . ? O1 Ho1 O2 51.96(17) . . ? O4 Ho1 O4 75.35(17) 6_565 4_645 ? O5 Ho1 O4 68.71(17) . 4_645 ? O6 Ho1 O4 65.50(16) 7_655 4_645 ? O3 Ho1 O4 48.89(15) 4_645 4_645 ? O9 Ho1 O4 136.9(2) . 4_645 ? O10 Ho1 O4 114.73(17) . 4_645 ? O1 Ho1 O4 120.74(16) . 4_645 ? O2 Ho1 O4 139.18(18) . 4_645 ? O4 Ho1 C9 100.45(19) 6_565 4_645 ? O5 Ho1 C9 72.7(2) . 4_645 ? O6 Ho1 C9 70.42(19) 7_655 4_645 ? O3 Ho1 C9 23.85(17) 4_645 4_645 ? O9 Ho1 C9 146.9(2) . 4_645 ? O10 Ho1 C9 94.3(2) . 4_645 ? O1 Ho1 C9 100.77(18) . 4_645 ? O2 Ho1 C9 139.93(19) . 4_645 ? O4 Ho1 C9 25.12(15) 4_645 4_645 ? O13 Ni1 O12 87.43(16) . . ? O13 Ni1 O12 87.43(16) . 2_756 ? O12 Ni1 O12 174.9(3) . 2_756 ? O13 Ni1 N2 89.63(18) . . ? O12 Ni1 N2 92.3(2) . . ? O12 Ni1 N2 87.6(2) 2_756 . ? O13 Ni1 N2 89.63(18) . 2_756 ? O12 Ni1 N2 87.6(2) . 2_756 ? O12 Ni1 N2 92.3(2) 2_756 2_756 ? N2 Ni1 N2 179.3(4) . 2_756 ? O13 Ni1 O11 180.000(3) . . ? O12 Ni1 O11 92.57(16) . . ? O12 Ni1 O11 92.57(16) 2_756 . ? N2 Ni1 O11 90.37(18) . . ? N2 Ni1 O11 90.37(19) 2_756 . ? C2 C1 C6 118.6(7) . . ? C2 C1 H1 120.7 . . ? C6 C1 H1 120.7 . . ? C1 C2 C3 120.3(7) . . ? C1 C2 C8 118.3(6) . . ? C3 C2 C8 121.0(6) . . ? C4 C3 C2 120.6(7) . . ? C4 C3 C9 118.8(6) . . ? C2 C3 C9 120.3(6) . . ? C3 C4 C5 119.3(7) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N2 C5 C4 131.9(7) . . ? N2 C5 C6 109.1(7) . . ? C4 C5 C6 119.0(7) . . ? N1 C6 C1 132.8(7) . . ? N1 C6 C5 105.1(7) . . ? C1 C6 C5 122.1(7) . . ? N2 C7 N1 112.5(7) . . ? N2 C7 H7 123.8 . . ? N1 C7 H7 123.8 . . ? O1 C8 O2 120.5(7) . . ? O1 C8 C2 119.1(6) . . ? O2 C8 C2 120.0(7) . . ? O3 C9 O4 120.1(7) . . ? O3 C9 C3 118.6(6) . . ? O4 C9 C3 121.2(7) . . ? O3 C9 Ho1 48.7(4) . 4_655 ? O4 C9 Ho1 71.7(4) . 4_655 ? C3 C9 Ho1 164.6(5) . 4_655 ? C7 N1 C6 108.3(7) . . ? C7 N1 H1A 125.9 . . ? C6 N1 H1A 125.9 . . ? C7 N2 C5 105.0(6) . . ? C7 N2 Ni1 120.6(5) . . ? C5 N2 Ni1 132.2(5) . . ? C8 O1 Ho1 96.5(4) . . ? C8 O2 Ho1 91.0(5) . . ? C9 O3 Ho1 107.5(4) . 4_655 ? C9 O4 Ho1 171.8(5) . 6_566 ? C9 O4 Ho1 83.2(4) . 4_655 ? Ho1 O4 Ho1 104.65(17) 6_566 4_655 ? S1 O5 Ho1 143.0(3) . . ? S1 O6 Ho1 138.0(3) . 7_655 ? Ho1 O9 H9A 120.0 . . ? Ho1 O9 H9B 120.0 . . ? H9A O9 H9B 120.0 . . ? Ho1 O10 H10A 120.1 . . ? Ho1 O10 H10B 119.9 . . ? H10A O10 H10B 120.0 . . ? Ni1 O11 H11A 120.0 . . ? Ni1 O11 H11B 120.0 . . ? H11A O11 H11B 120.0 . . ? Ni1 O12 H12A 120.0 . . ? Ni1 O12 H12B 120.0 . . ? H12A O12 H12B 120.0 . . ? Ni1 O13 H13B 131.0 . . ? O7 S1 O8 109.6(4) . . ? O7 S1 O6 110.3(3) . . ? O8 S1 O6 108.6(3) . . ? O7 S1 O5 108.5(4) . . ? O8 S1 O5 108.8(4) . . ? O6 S1 O5 110.9(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 C6 C1 C2 C3 -1.6(11) . . . . ? C6 C1 C2 C8 -173.9(7) . . . . ? C1 C2 C3 C4 -1.8(11) . . . . ? C8 C2 C3 C4 170.3(7) . . . . ? C1 C2 C3 C9 171.2(7) . . . . ? C8 C2 C3 C9 -16.7(10) . . . . ? C2 C3 C4 C5 1.4(11) . . . . ? C9 C3 C4 C5 -171.7(7) . . . . ? C3 C4 C5 N2 179.2(8) . . . . ? C3 C4 C5 C6 2.2(11) . . . . ? C2 C1 C6 N1 -177.7(8) . . . . ? C2 C1 C6 C5 5.3(11) . . . . ? N2 C5 C6 N1 -1.1(8) . . . . ? C4 C5 C6 N1 176.6(7) . . . . ? N2 C5 C6 C1 176.6(7) . . . . ? C4 C5 C6 C1 -5.7(11) . . . . ? C1 C2 C8 O1 104.3(8) . . . . ? C3 C2 C8 O1 -68.0(9) . . . . ? C1 C2 C8 O2 -68.6(10) . . . . ? C3 C2 C8 O2 119.2(8) . . . . ? C4 C3 C9 O3 145.6(7) . . . . ? C2 C3 C9 O3 -27.5(10) . . . . ? C4 C3 C9 O4 -30.5(11) . . . . ? C2 C3 C9 O4 156.3(7) . . . . ? C4 C3 C9 Ho1 113.9(18) . . . 4_655 ? C2 C3 C9 Ho1 -59(2) . . . 4_655 ? N2 C7 N1 C6 1.4(10) . . . . ? C1 C6 N1 C7 -177.5(9) . . . . ? C5 C6 N1 C7 -0.1(9) . . . . ? N1 C7 N2 C5 -2.0(10) . . . . ? N1 C7 N2 Ni1 163.2(6) . . . . ? C4 C5 N2 C7 -175.4(9) . . . . ? C6 C5 N2 C7 1.9(9) . . . . ? C4 C5 N2 Ni1 21.8(13) . . . . ? C6 C5 N2 Ni1 -160.9(6) . . . . ? O13 Ni1 N2 C7 -48.6(6) . . . . ? O12 Ni1 N2 C7 -136.0(7) . . . . ? O12 Ni1 N2 C7 38.9(7) 2_756 . . . ? N2 Ni1 N2 C7 -48.6(7) 2_756 . . . ? O11 Ni1 N2 C7 131.4(6) . . . . ? O13 Ni1 N2 C5 112.0(7) . . . . ? O12 Ni1 N2 C5 24.6(7) . . . . ? O12 Ni1 N2 C5 -160.5(7) 2_756 . . . ? N2 Ni1 N2 C5 112.0(7) 2_756 . . . ? O11 Ni1 N2 C5 -68.0(7) . . . . ? O2 C8 O1 Ho1 -1.3(8) . . . . ? C2 C8 O1 Ho1 -174.1(5) . . . . ? O4 Ho1 O1 C8 29.4(6) 6_565 . . . ? O5 Ho1 O1 C8 79.8(4) . . . . ? O6 Ho1 O1 C8 -140.1(4) 7_655 . . . ? O3 Ho1 O1 C8 159.2(5) 4_645 . . . ? O9 Ho1 O1 C8 -56.6(5) . . . . ? O10 Ho1 O1 C8 -121.8(5) . . . . ? O2 Ho1 O1 C8 0.7(4) . . . . ? O4 Ho1 O1 C8 131.4(4) 4_645 . . . ? C9 Ho1 O1 C8 147.9(4) 4_645 . . . ? O1 C8 O2 Ho1 1.2(7) . . . . ? C2 C8 O2 Ho1 174.0(6) . . . . ? O4 Ho1 O2 C8 -161.6(5) 6_565 . . . ? O5 Ho1 O2 C8 -83.7(5) . . . . ? O6 Ho1 O2 C8 128.4(4) 7_655 . . . ? O3 Ho1 O2 C8 -27.8(5) 4_645 . . . ? O9 Ho1 O2 C8 119.8(5) . . . . ? O10 Ho1 O2 C8 52.1(5) . . . . ? O1 Ho1 O2 C8 -0.7(4) . . . . ? O4 Ho1 O2 C8 -95.7(5) 4_645 . . . ? C9 Ho1 O2 C8 -56.5(6) 4_645 . . . ? O4 C9 O3 Ho1 6.9(8) . . . 4_655 ? C3 C9 O3 Ho1 -169.3(5) . . . 4_655 ? O3 C9 O4 Ho1 157(3) . . . 6_566 ? C3 C9 O4 Ho1 -27(4) . . . 6_566 ? Ho1 C9 O4 Ho1 163(3) 4_655 . . 6_566 ? O3 C9 O4 Ho1 -5.4(6) . . . 4_655 ? C3 C9 O4 Ho1 170.7(7) . . . 4_655 ? O4 Ho1 O5 S1 -27.6(6) 6_565 . . . ? O6 Ho1 O5 S1 37.9(7) 7_655 . . . ? O3 Ho1 O5 S1 101.7(6) 4_645 . . . ? O9 Ho1 O5 S1 -86.2(7) . . . . ? O10 Ho1 O5 S1 155.1(5) . . . . ? O1 Ho1 O5 S1 -175.3(7) . . . . ? O2 Ho1 O5 S1 -120.6(6) . . . . ? O4 Ho1 O5 S1 51.1(6) 4_645 . . . ? C9 Ho1 O5 S1 77.4(6) 4_645 . . . ? Ho1 O6 S1 O7 78.0(5) 7_655 . . . ? Ho1 O6 S1 O8 -161.8(5) 7_655 . . . ? Ho1 O6 S1 O5 -42.2(6) 7_655 . . . ? Ho1 O5 S1 O7 -121.2(6) . . . . ? Ho1 O5 S1 O8 119.6(6) . . . . ? Ho1 O5 S1 O6 0.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.805 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.170 data_8 _database_code_depnum_ccdc_archive 'CCDC 862569' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Er2 N4 Ni O24 S2' _chemical_formula_weight 1137.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ni Ni 0.3393 1.1124 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.420(3) _cell_length_b 8.6010(17) _cell_length_c 24.344(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.62(2) _cell_angle_gamma 90.00 _cell_volume 2911.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5123 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 6.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2417 _exptl_absorpt_correction_T_max 0.3515 _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 20675 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5123 _reflns_number_gt 4217 _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^)+(0.0370P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00286(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5123 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.141206(15) 0.64464(2) 0.257103(9) 0.00803(9) Uani 1 1 d . . . Er2 Er 0.370793(15) 0.86647(2) 0.251750(9) 0.00792(9) Uani 1 1 d . . . Ni1 Ni 0.24442(4) 1.20972(8) -0.00071(3) 0.01241(17) Uani 1 1 d . . . S1 S 0.26628(9) 0.96806(14) 0.35166(5) 0.0090(3) Uani 1 1 d . . . S2 S 0.24108(9) 0.55186(14) 0.15449(5) 0.0090(3) Uani 1 1 d . . . O2 O 0.0680(3) 0.8607(4) 0.19911(15) 0.0145(8) Uani 1 1 d . . . O3 O 0.2130(2) 0.9132(4) 0.20546(14) 0.0131(8) Uani 1 1 d . . . O4 O 0.1246(3) 0.5440(4) 0.34377(15) 0.0158(8) Uani 1 1 d . . . O5 O 0.0138(2) 0.7094(4) 0.28809(14) 0.0138(8) Uani 1 1 d . . . O6 O -0.0048(3) 0.5254(4) 0.19183(15) 0.0178(8) Uani 1 1 d . . . H6C H -0.0077 0.4276 0.1851 0.027 Uiso 1 1 d R . . H6D H -0.0564 0.5793 0.1746 0.027 Uiso 1 1 d R . . O7 O 0.1763(3) 0.3770(4) 0.25602(16) 0.0224(9) Uani 1 1 d . . . H7A H 0.1850 0.3618 0.2268 0.034 Uiso 1 1 d R . . H7B H 0.1776 0.3081 0.2747 0.034 Uiso 1 1 d R . . O8 O 0.3718(3) 1.1360(4) 0.23744(15) 0.0177(9) Uani 1 1 d . . . H8C H 0.3868 1.1989 0.2672 0.027 Uiso 1 1 d R . . H8D H 0.3593 1.1737 0.2020 0.027 Uiso 1 1 d R . . O9 O 0.5247(3) 0.9661(4) 0.32488(14) 0.0195(9) Uani 1 1 d . . . H9A H 0.5580 0.9145 0.3569 0.029 Uiso 1 1 d R . . H9B H 0.5453 1.0529 0.3186 0.029 Uiso 1 1 d R . . O10 O 0.3059(2) 0.6347(4) 0.29803(14) 0.0121(8) Uani 1 1 d . . . O11 O 0.4579(2) 0.6652(4) 0.31745(15) 0.0133(8) Uani 1 1 d . . . O12 O 0.5144(3) 0.3471(4) 0.28847(15) 0.0145(8) Uani 1 1 d . . . O13 O 0.6458(2) 0.4319(4) 0.36478(15) 0.0164(8) Uani 1 1 d . . . O14 O 0.3452(2) 0.9527(4) 0.33309(14) 0.0130(8) Uani 1 1 d . . . O15 O 0.1997(3) 0.8356(4) 0.32954(16) 0.0165(8) Uani 1 1 d . . . O16 O 0.3096(2) 0.9691(4) 0.41877(14) 0.0169(8) Uani 1 1 d . . . O17 O 0.2121(3) 1.1126(4) 0.32801(16) 0.0196(9) Uani 1 1 d . . . O18 O 0.3287(2) 0.6453(4) 0.18932(15) 0.0129(8) Uani 1 1 d . . . O19 O 0.1620(2) 0.6034(4) 0.16863(14) 0.0124(8) Uani 1 1 d . . . O20 O 0.2614(3) 0.3863(4) 0.17073(16) 0.0167(8) Uani 1 1 d . . . O21 O 0.2137(3) 0.5721(4) 0.08926(14) 0.0171(8) Uani 1 1 d . . . O22 O 0.2502(2) 0.9669(4) 0.00792(15) 0.0196(9) Uani 1 1 d . . . H22A H 0.1906 0.9449 -0.0090 0.029 Uiso 1 1 d R . . H22B H 0.2745 0.9382 0.0450 0.029 Uiso 1 1 d R . . O23 O 0.3169(2) 1.2348(4) 0.09362(14) 0.0158(8) Uani 1 1 d . . . H23A H 0.2788 1.2719 0.1071 0.024 Uiso 1 1 d R . . H23B H 0.3384 1.1476 0.1104 0.024 Uiso 1 1 d R . . O24 O 0.2344(3) 1.4498(4) -0.00644(14) 0.0217(9) Uani 1 1 d . . . H24A H 0.2415 1.5031 0.0247 0.033 Uiso 1 1 d R . . H24B H 0.2636 1.4936 -0.0249 0.033 Uiso 1 1 d R . . O25 O 0.1743(2) 1.2125(4) -0.09222(14) 0.0150(8) Uani 1 1 d . . . H25A H 0.2093 1.2619 -0.1053 0.022 Uiso 1 1 d R . . H25B H 0.1573 1.1261 -0.1108 0.022 Uiso 1 1 d R . . N1 N 0.1099(3) 1.2112(5) -0.00053(17) 0.0135(9) Uani 1 1 d . . . N2 N -0.0327(3) 1.3160(5) -0.02258(18) 0.0149(10) Uani 1 1 d . . . H2 H -0.0844 1.3688 -0.0419 0.018 Uiso 1 1 d R . . N3 N 0.5191(3) 0.1775(5) 0.52048(17) 0.0126(9) Uani 1 1 d . . . H3A H 0.5694 0.1212 0.5394 0.015 Uiso 1 1 d R . . N4 N 0.3781(3) 0.2898(5) 0.49832(17) 0.0134(9) Uani 1 1 d . . . C1 C 0.1236(3) 0.9370(5) 0.1828(2) 0.0089(10) Uani 1 1 d . . . C2 C 0.0803(3) 1.0511(5) 0.1325(2) 0.0096(11) Uani 1 1 d . . . C3 C 0.1262(4) 1.0743(6) 0.0953(2) 0.0115(11) Uani 1 1 d . . . H3 H 0.1852 1.0280 0.1040 0.014 Uiso 1 1 calc R . . C4 C 0.0814(4) 1.1690(6) 0.0446(2) 0.0117(11) Uani 1 1 d . . . C5 C 0.0387(4) 1.2961(6) -0.0393(2) 0.0175(12) Uani 1 1 d . . . H5 H 0.0380 1.3379 -0.0748 0.021 Uiso 1 1 calc R . . C6 C -0.0081(4) 1.2363(5) 0.0314(2) 0.0119(11) Uani 1 1 d . . . C7 C -0.0525(4) 1.2205(6) 0.0694(2) 0.0120(11) Uani 1 1 d . . . H7 H -0.1102 1.2708 0.0612 0.014 Uiso 1 1 calc R . . C8 C -0.0080(4) 1.1266(5) 0.1206(2) 0.0104(11) Uani 1 1 d . . . C9 C 0.0506(4) 0.6228(5) 0.3343(2) 0.0108(11) Uani 1 1 d . . . C10 C 0.3931(3) 0.5914(6) 0.3259(2) 0.0100(11) Uani 1 1 d . . . C11 C 0.4224(4) 0.4654(5) 0.3717(2) 0.0104(11) Uani 1 1 d . . . C12 C 0.3724(4) 0.4414(5) 0.4067(2) 0.0112(11) Uani 1 1 d . . . H12 H 0.3152 0.4936 0.3981 0.013 Uiso 1 1 calc R . . C13 C 0.4105(4) 0.3367(6) 0.4552(2) 0.0124(11) Uani 1 1 d . . . C14 C 0.4463(4) 0.1966(6) 0.5356(2) 0.0166(12) Uani 1 1 d . . . H14 H 0.4438 0.1488 0.5691 0.020 Uiso 1 1 calc R . . C15 C 0.4986(4) 0.2648(5) 0.4690(2) 0.0122(11) Uani 1 1 d . . . C16 C 0.5481(4) 0.2822(6) 0.4334(2) 0.0119(11) Uani 1 1 d . . . H16 H 0.6052 0.2292 0.4423 0.014 Uiso 1 1 calc R . . C17 C 0.5088(4) 0.3815(5) 0.3842(2) 0.0108(11) Uani 1 1 d . . . C18 C 0.5596(4) 0.3905(5) 0.3439(2) 0.0109(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.00705(15) 0.00849(15) 0.00860(13) 0.00071(8) 0.00344(10) 0.00069(9) Er2 0.00650(15) 0.00831(15) 0.00867(13) 0.00017(8) 0.00301(10) 0.00031(8) Ni1 0.0139(4) 0.0129(4) 0.0121(3) -0.0003(2) 0.0072(3) -0.0001(3) S1 0.0090(7) 0.0098(6) 0.0084(6) -0.0003(5) 0.0040(5) 0.0011(5) S2 0.0083(7) 0.0106(7) 0.0075(6) 0.0001(4) 0.0030(5) 0.0013(5) O2 0.014(2) 0.013(2) 0.0173(19) 0.0067(14) 0.0082(17) 0.0038(15) O3 0.0079(19) 0.0154(19) 0.0134(17) -0.0004(15) 0.0022(15) 0.0021(15) O4 0.015(2) 0.016(2) 0.0200(19) 0.0064(15) 0.0114(17) 0.0045(16) O5 0.0093(19) 0.0173(19) 0.0140(18) 0.0032(15) 0.0042(16) 0.0009(15) O6 0.013(2) 0.016(2) 0.0236(19) -0.0072(15) 0.0077(17) -0.0008(16) O7 0.032(3) 0.014(2) 0.0175(19) 0.0063(15) 0.0072(18) 0.0031(17) O8 0.028(2) 0.014(2) 0.0116(17) -0.0016(14) 0.0086(18) -0.0021(16) O9 0.016(2) 0.026(2) 0.0116(17) 0.0036(15) 0.0018(16) -0.0097(16) O10 0.009(2) 0.016(2) 0.0091(17) 0.0002(13) 0.0023(15) 0.0041(15) O11 0.012(2) 0.0115(19) 0.0162(18) 0.0037(14) 0.0055(16) -0.0005(15) O12 0.012(2) 0.016(2) 0.0163(18) -0.0008(14) 0.0068(16) 0.0001(15) O13 0.012(2) 0.0154(19) 0.0231(19) -0.0016(15) 0.0089(17) -0.0041(16) O14 0.010(2) 0.018(2) 0.0140(17) -0.0033(14) 0.0084(16) -0.0025(15) O15 0.018(2) 0.0136(19) 0.022(2) -0.0102(15) 0.0122(17) -0.0094(16) O16 0.012(2) 0.027(2) 0.0094(17) -0.0007(15) 0.0022(16) 0.0051(16) O17 0.028(2) 0.015(2) 0.0193(19) 0.0060(15) 0.0128(18) 0.0123(17) O18 0.010(2) 0.0127(19) 0.0169(18) -0.0051(14) 0.0072(16) -0.0037(14) O19 0.011(2) 0.0154(19) 0.0119(17) 0.0020(14) 0.0063(15) 0.0036(15) O20 0.019(2) 0.0098(19) 0.0221(19) 0.0015(14) 0.0092(17) 0.0036(15) O21 0.015(2) 0.028(2) 0.0076(16) -0.0005(15) 0.0040(15) 0.0057(17) O22 0.015(2) 0.016(2) 0.022(2) -0.0003(15) 0.0031(17) -0.0010(15) O23 0.022(2) 0.0144(19) 0.0149(18) 0.0034(14) 0.0117(17) 0.0052(16) O24 0.035(3) 0.016(2) 0.023(2) -0.0018(15) 0.021(2) 0.0005(17) O25 0.019(2) 0.0134(19) 0.0152(18) -0.0035(14) 0.0102(17) -0.0048(16) N1 0.016(3) 0.017(2) 0.010(2) 0.0044(17) 0.0083(19) 0.0021(19) N2 0.014(3) 0.020(3) 0.011(2) 0.0056(17) 0.004(2) 0.0025(19) N3 0.013(2) 0.014(2) 0.011(2) 0.0063(17) 0.0062(19) 0.0056(19) N4 0.015(3) 0.016(2) 0.010(2) 0.0031(17) 0.0061(19) 0.0017(19) C1 0.012(3) 0.005(2) 0.010(2) -0.0050(19) 0.005(2) -0.001(2) C2 0.009(3) 0.010(3) 0.009(2) -0.0007(19) 0.003(2) 0.001(2) C3 0.009(3) 0.013(3) 0.013(2) 0.004(2) 0.005(2) 0.005(2) C4 0.012(3) 0.013(3) 0.012(2) -0.002(2) 0.007(2) -0.002(2) C5 0.018(3) 0.020(3) 0.016(3) 0.002(2) 0.010(2) 0.002(2) C6 0.011(3) 0.012(3) 0.009(2) -0.0007(19) 0.000(2) 0.000(2) C7 0.007(3) 0.012(3) 0.016(3) -0.002(2) 0.005(2) 0.000(2) C8 0.010(3) 0.010(3) 0.010(2) 0.0003(18) 0.003(2) 0.000(2) C9 0.006(3) 0.009(3) 0.014(2) -0.0058(19) 0.001(2) -0.004(2) C10 0.011(3) 0.011(3) 0.007(2) -0.0058(19) 0.004(2) 0.002(2) C11 0.009(3) 0.011(3) 0.011(2) -0.0029(19) 0.004(2) -0.002(2) C12 0.009(3) 0.013(3) 0.011(2) 0.001(2) 0.003(2) 0.000(2) C13 0.013(3) 0.014(3) 0.012(2) 0.000(2) 0.007(2) -0.001(2) C14 0.021(3) 0.018(3) 0.012(3) 0.002(2) 0.008(2) 0.002(2) C15 0.015(3) 0.009(3) 0.008(2) 0.0015(19) 0.000(2) 0.004(2) C16 0.009(3) 0.013(3) 0.015(2) -0.003(2) 0.007(2) -0.002(2) C17 0.010(3) 0.012(3) 0.009(2) -0.0013(19) 0.003(2) -0.002(2) C18 0.011(3) 0.006(3) 0.015(3) 0.0030(19) 0.005(2) 0.001(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 Er1 O15 2.290(3) . ? Er1 O10 2.294(3) . ? Er1 O2 2.311(3) . ? Er1 O19 2.338(3) . ? Er1 O6 2.357(3) . ? Er1 O7 2.367(3) . ? Er1 O4 2.394(3) . ? Er1 O5 2.454(3) . ? Er2 O3 2.232(3) . ? Er2 O14 2.303(3) . ? Er2 O18 2.345(3) . ? Er2 O8 2.345(3) . ? Er2 O11 2.346(3) . ? Er2 O12 2.370(3) 2_655 ? Er2 O9 2.426(3) . ? Er2 O10 2.687(3) . ? Er2 O13 2.793(3) 2_655 ? Er2 C10 2.905(5) . ? Er2 C18 2.962(5) 2_655 ? Ni1 O25 2.012(3) . ? Ni1 O24 2.071(4) . ? Ni1 N4 2.072(4) 4_575 ? Ni1 N1 2.077(4) . ? Ni1 O23 2.086(3) . ? Ni1 O22 2.097(4) . ? S1 O17 1.470(3) . ? S1 O15 1.471(3) . ? S1 O16 1.474(3) . ? S1 O14 1.476(3) . ? S2 O21 1.466(3) . ? S2 O19 1.471(3) . ? S2 O20 1.475(3) . ? S2 O18 1.483(3) . ? O2 C1 1.273(6) . ? O3 C1 1.261(6) . ? O4 C9 1.261(6) . ? O5 C9 1.261(6) . ? O6 H6C 0.8542 . ? O6 H6D 0.8576 . ? O7 H7A 0.7903 . ? O7 H7B 0.7427 . ? O8 H8C 0.8529 . ? O8 H8D 0.8621 . ? O9 H9A 0.8501 . ? O9 H9B 0.8500 . ? O10 C10 1.272(6) . ? O11 C10 1.273(6) . ? O12 C18 1.278(6) . ? O12 Er2 2.370(3) 2_645 ? O13 C18 1.251(6) . ? O13 Er2 2.793(3) 2_645 ? O22 H22A 0.8500 . ? O22 H22B 0.8500 . ? O23 H23A 0.8498 . ? O23 H23B 0.8499 . ? O24 H24A 0.8501 . ? O24 H24B 0.8500 . ? O25 H25A 0.8498 . ? O25 H25B 0.8499 . ? N1 C5 1.316(6) . ? N1 C4 1.395(6) . ? N2 C5 1.340(6) . ? N2 C6 1.382(6) . ? N2 H2 0.8599 . ? N3 C14 1.332(6) . ? N3 C15 1.376(6) . ? N3 H3A 0.8601 . ? N4 C14 1.321(6) . ? N4 C13 1.404(6) . ? N4 Ni1 2.072(4) 4_576 ? C1 C2 1.484(6) . ? C2 C3 1.383(7) . ? C2 C8 1.422(7) . ? C3 C4 1.388(7) . ? C3 H3 0.9300 . ? C4 C6 1.399(7) . ? C5 H5 0.9300 . ? C6 C7 1.377(7) . ? C7 C8 1.391(6) . ? C7 H7 0.9300 . ? C8 C9 1.503(7) 2 ? C9 C8 1.503(7) 2_545 ? C10 C11 1.477(7) . ? C11 C12 1.390(7) . ? C11 C17 1.428(7) . ? C12 C13 1.396(7) . ? C12 H12 0.9300 . ? C13 C15 1.394(7) . ? C14 H14 0.9300 . ? C15 C16 1.389(7) . ? C16 C17 1.380(7) . ? C16 H16 0.9300 . ? C17 C18 1.499(7) . ? C18 Er2 2.962(5) 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 O15 Er1 O10 72.48(12) . . ? O15 Er1 O2 79.60(12) . . ? O10 Er1 O2 116.88(12) . . ? O15 Er1 O19 130.77(12) . . ? O10 Er1 O19 80.04(12) . . ? O2 Er1 O19 77.57(12) . . ? O15 Er1 O6 140.77(12) . . ? O10 Er1 O6 146.34(11) . . ? O2 Er1 O6 82.30(12) . . ? O19 Er1 O6 77.56(12) . . ? O15 Er1 O7 133.63(13) . . ? O10 Er1 O7 75.69(12) . . ? O2 Er1 O7 145.95(12) . . ? O19 Er1 O7 73.68(12) . . ? O6 Er1 O7 74.09(13) . . ? O15 Er1 O4 74.77(12) . . ? O10 Er1 O4 97.11(12) . . ? O2 Er1 O4 128.24(12) . . ? O19 Er1 O4 150.04(11) . . ? O6 Er1 O4 90.10(12) . . ? O7 Er1 O4 76.72(12) . . ? O15 Er1 O5 72.64(12) . . ? O10 Er1 O5 139.32(11) . . ? O2 Er1 O5 76.15(12) . . ? O19 Er1 O5 139.89(11) . . ? O6 Er1 O5 69.35(11) . . ? O7 Er1 O5 116.20(12) . . ? O4 Er1 O5 53.59(11) . . ? O3 Er2 O14 79.72(12) . . ? O3 Er2 O18 83.27(12) . . ? O14 Er2 O18 135.75(11) . . ? O3 Er2 O8 79.80(12) . . ? O14 Er2 O8 79.86(12) . . ? O18 Er2 O8 136.35(11) . . ? O3 Er2 O11 130.90(12) . . ? O14 Er2 O11 84.94(12) . . ? O18 Er2 O11 76.08(12) . . ? O8 Er2 O11 142.41(12) . . ? O3 Er2 O12 130.54(12) . 2_655 ? O14 Er2 O12 144.49(12) . 2_655 ? O18 Er2 O12 73.87(12) . 2_655 ? O8 Er2 O12 87.36(12) . 2_655 ? O11 Er2 O12 85.44(12) . 2_655 ? O3 Er2 O9 144.51(12) . . ? O14 Er2 O9 74.46(12) . . ? O18 Er2 O9 132.17(12) . . ? O8 Er2 O9 72.09(12) . . ? O11 Er2 O9 70.76(12) . . ? O12 Er2 O9 70.09(11) 2_655 . ? O3 Er2 O10 79.80(12) . . ? O14 Er2 O10 69.21(10) . . ? O18 Er2 O10 67.71(11) . . ? O8 Er2 O10 145.42(11) . . ? O11 Er2 O10 51.20(11) . . ? O12 Er2 O10 126.94(11) 2_655 . ? O9 Er2 O10 112.21(11) . . ? O3 Er2 O13 81.37(11) . 2_655 ? O14 Er2 O13 146.51(11) . 2_655 ? O18 Er2 O13 68.10(11) . 2_655 ? O8 Er2 O13 69.74(11) . 2_655 ? O11 Er2 O13 127.97(11) . 2_655 ? O12 Er2 O13 49.56(11) 2_655 2_655 ? O9 Er2 O13 107.76(11) . 2_655 ? O10 Er2 O13 133.49(10) . 2_655 ? O3 Er2 C10 105.70(13) . . ? O14 Er2 C10 75.30(12) . . ? O18 Er2 C10 70.56(12) . . ? O8 Er2 C10 152.97(12) . . ? O11 Er2 C10 25.29(12) . . ? O12 Er2 C10 106.90(12) 2_655 . ? O9 Er2 C10 90.93(12) . . ? O10 Er2 C10 25.92(12) . . ? O13 Er2 C10 136.84(11) 2_655 . ? O3 Er2 C18 106.08(13) . 2_655 ? O14 Er2 C18 155.29(12) . 2_655 ? O18 Er2 C18 68.90(12) . 2_655 ? O8 Er2 C18 77.67(12) . 2_655 ? O11 Er2 C18 107.00(13) . 2_655 ? O12 Er2 C18 24.67(13) 2_655 2_655 ? O9 Er2 C18 88.87(12) . 2_655 ? O10 Er2 C18 135.10(11) . 2_655 ? O13 Er2 C18 24.89(11) 2_655 2_655 ? C10 Er2 C18 124.02(13) . 2_655 ? O25 Ni1 O24 85.69(13) . . ? O25 Ni1 N4 92.78(14) . 4_575 ? O24 Ni1 N4 92.46(15) . 4_575 ? O25 Ni1 N1 86.75(15) . . ? O24 Ni1 N1 87.03(15) . . ? N4 Ni1 N1 179.33(17) 4_575 . ? O25 Ni1 O23 173.39(15) . . ? O24 Ni1 O23 87.70(13) . . ? N4 Ni1 O23 87.16(14) 4_575 . ? N1 Ni1 O23 93.26(14) . . ? O25 Ni1 O22 95.86(13) . . ? O24 Ni1 O22 176.84(13) . . ? N4 Ni1 O22 90.22(15) 4_575 . ? N1 Ni1 O22 90.30(15) . . ? O23 Ni1 O22 90.76(13) . . ? O17 S1 O15 108.9(2) . . ? O17 S1 O16 109.7(2) . . ? O15 S1 O16 108.7(2) . . ? O17 S1 O14 111.1(2) . . ? O15 S1 O14 110.9(2) . . ? O16 S1 O14 107.6(2) . . ? O21 S2 O19 109.7(2) . . ? O21 S2 O20 109.5(2) . . ? O19 S2 O20 109.2(2) . . ? O21 S2 O18 108.6(2) . . ? O19 S2 O18 110.19(19) . . ? O20 S2 O18 109.5(2) . . ? C1 O2 Er1 112.8(3) . . ? C1 O3 Er2 176.0(3) . . ? C9 O4 Er1 94.5(3) . . ? C9 O5 Er1 91.7(3) . . ? Er1 O6 H6C 120.8 . . ? Er1 O6 H6D 120.5 . . ? H6C O6 H6D 118.6 . . ? Er1 O7 H7A 107.5 . . ? Er1 O7 H7B 135.7 . . ? H7A O7 H7B 116.7 . . ? Er2 O8 H8C 121.2 . . ? Er2 O8 H8D 120.5 . . ? H8C O8 H8D 118.3 . . ? Er2 O9 H9A 120.0 . . ? Er2 O9 H9B 120.0 . . ? H9A O9 H9B 120.0 . . ? C10 O10 Er1 163.5(3) . . ? C10 O10 Er2 86.7(3) . . ? Er1 O10 Er2 109.46(12) . . ? C10 O11 Er2 102.8(3) . . ? C18 O12 Er2 104.6(3) . 2_645 ? C18 O13 Er2 85.1(3) . 2_645 ? S1 O14 Er2 139.7(2) . . ? S1 O15 Er1 144.8(2) . . ? S2 O18 Er2 137.6(2) . . ? S2 O19 Er1 136.0(2) . . ? Ni1 O22 H22A 100.5 . . ? Ni1 O22 H22B 112.1 . . ? H22A O22 H22B 109.7 . . ? Ni1 O23 H23A 109.5 . . ? Ni1 O23 H23B 110.5 . . ? H23A O23 H23B 109.7 . . ? Ni1 O24 H24A 120.0 . . ? Ni1 O24 H24B 115.8 . . ? H24A O24 H24B 109.7 . . ? Ni1 O25 H25A 107.2 . . ? Ni1 O25 H25B 118.2 . . ? H25A O25 H25B 109.7 . . ? C5 N1 C4 105.1(4) . . ? C5 N1 Ni1 121.7(3) . . ? C4 N1 Ni1 130.9(3) . . ? C5 N2 C6 107.6(4) . . ? C5 N2 H2 126.2 . . ? C6 N2 H2 126.2 . . ? C14 N3 C15 107.1(4) . . ? C14 N3 H3A 126.4 . . ? C15 N3 H3A 126.4 . . ? C14 N4 C13 104.6(4) . . ? C14 N4 Ni1 119.6(3) . 4_576 ? C13 N4 Ni1 133.3(3) . 4_576 ? O3 C1 O2 122.4(4) . . ? O3 C1 C2 119.0(4) . . ? O2 C1 C2 118.4(4) . . ? C3 C2 C8 121.2(4) . . ? C3 C2 C1 117.5(4) . . ? C8 C2 C1 121.3(4) . . ? C4 C3 C2 117.9(5) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 N1 130.4(5) . . ? C3 C4 C6 120.6(5) . . ? N1 C4 C6 109.1(4) . . ? N1 C5 N2 113.0(5) . . ? N1 C5 H5 123.5 . . ? N2 C5 H5 123.5 . . ? C7 C6 N2 132.6(5) . . ? C7 C6 C4 122.2(4) . . ? N2 C6 C4 105.1(4) . . ? C6 C7 C8 117.6(5) . . ? C6 C7 H7 121.2 . . ? C8 C7 H7 121.2 . . ? C7 C8 C2 120.4(5) . . ? C7 C8 C9 117.7(4) . 2 ? C2 C8 C9 121.6(4) . 2 ? O5 C9 O4 120.2(5) . . ? O5 C9 C8 118.0(4) . 2_545 ? O4 C9 C8 121.7(4) . 2_545 ? O11 C10 O10 119.3(4) . . ? O11 C10 C11 118.9(4) . . ? O10 C10 C11 121.7(4) . . ? O11 C10 Er2 51.9(2) . . ? O10 C10 Er2 67.4(3) . . ? C11 C10 Er2 168.9(3) . . ? C12 C11 C17 120.5(4) . . ? C12 C11 C10 120.1(4) . . ? C17 C11 C10 118.9(4) . . ? C13 C12 C11 118.2(5) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C12 C13 C15 120.0(5) . . ? C12 C13 N4 131.5(5) . . ? C15 C13 N4 108.5(4) . . ? N4 C14 N3 113.6(4) . . ? N4 C14 H14 123.2 . . ? N3 C14 H14 123.2 . . ? N3 C15 C16 131.0(5) . . ? N3 C15 C13 106.1(4) . . ? C16 C15 C13 122.8(4) . . ? C17 C16 C15 117.1(5) . . ? C17 C16 H16 121.5 . . ? C15 C16 H16 121.5 . . ? C16 C17 C11 121.1(5) . . ? C16 C17 C18 116.3(4) . . ? C11 C17 C18 122.6(4) . . ? O13 C18 O12 120.7(5) . . ? O13 C18 C17 120.8(4) . . ? O12 C18 C17 118.4(5) . . ? O13 C18 Er2 70.0(3) . 2_645 ? O12 C18 Er2 50.7(2) . 2_645 ? C17 C18 Er2 168.6(3) . 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 O15 Er1 O2 C1 80.2(3) . . . . ? O10 Er1 O2 C1 16.1(3) . . . . ? O19 Er1 O2 C1 -55.8(3) . . . . ? O6 Er1 O2 C1 -134.7(3) . . . . ? O7 Er1 O2 C1 -88.7(4) . . . . ? O4 Er1 O2 C1 141.3(3) . . . . ? O5 Er1 O2 C1 154.7(3) . . . . ? O14 Er2 O3 C1 -31(5) . . . . ? O18 Er2 O3 C1 108(5) . . . . ? O8 Er2 O3 C1 -113(5) . . . . ? O11 Er2 O3 C1 43(5) . . . . ? O12 Er2 O3 C1 170(5) 2_655 . . . ? O9 Er2 O3 C1 -75(5) . . . . ? O10 Er2 O3 C1 39(5) . . . . ? O13 Er2 O3 C1 176(5) 2_655 . . . ? C10 Er2 O3 C1 40(5) . . . . ? C18 Er2 O3 C1 173(5) 2_655 . . . ? O15 Er1 O4 C9 78.0(3) . . . . ? O10 Er1 O4 C9 147.6(3) . . . . ? O2 Er1 O4 C9 14.9(3) . . . . ? O19 Er1 O4 C9 -130.0(3) . . . . ? O6 Er1 O4 C9 -65.4(3) . . . . ? O7 Er1 O4 C9 -139.0(3) . . . . ? O5 Er1 O4 C9 -1.4(3) . . . . ? O15 Er1 O5 C9 -82.2(3) . . . . ? O10 Er1 O5 C9 -50.1(3) . . . . ? O2 Er1 O5 C9 -165.4(3) . . . . ? O19 Er1 O5 C9 144.1(3) . . . . ? O6 Er1 O5 C9 107.7(3) . . . . ? O7 Er1 O5 C9 48.5(3) . . . . ? O4 Er1 O5 C9 1.4(3) . . . . ? O15 Er1 O10 C10 115.0(11) . . . . ? O2 Er1 O10 C10 -176.9(10) . . . . ? O19 Er1 O10 C10 -106.4(10) . . . . ? O6 Er1 O10 C10 -57.5(11) . . . . ? O7 Er1 O10 C10 -30.8(10) . . . . ? O4 Er1 O10 C10 43.5(10) . . . . ? O5 Er1 O10 C10 82.9(11) . . . . ? O15 Er1 O10 Er2 -76.96(13) . . . . ? O2 Er1 O10 Er2 -8.80(16) . . . . ? O19 Er1 O10 Er2 61.69(12) . . . . ? O6 Er1 O10 Er2 110.54(19) . . . . ? O7 Er1 O10 Er2 137.23(14) . . . . ? O4 Er1 O10 Er2 -148.48(12) . . . . ? O5 Er1 O10 Er2 -109.05(16) . . . . ? O3 Er2 O10 C10 178.0(3) . . . . ? O14 Er2 O10 C10 -99.2(3) . . . . ? O18 Er2 O10 C10 91.2(3) . . . . ? O8 Er2 O10 C10 -127.3(3) . . . . ? O11 Er2 O10 C10 1.4(2) . . . . ? O12 Er2 O10 C10 44.3(3) 2_655 . . . ? O9 Er2 O10 C10 -36.9(3) . . . . ? O13 Er2 O10 C10 110.4(3) 2_655 . . . ? C18 Er2 O10 C10 75.4(3) 2_655 . . . ? O3 Er2 O10 Er1 1.40(11) . . . . ? O14 Er2 O10 Er1 84.17(14) . . . . ? O18 Er2 O10 Er1 -85.45(14) . . . . ? O8 Er2 O10 Er1 56.1(2) . . . . ? O11 Er2 O10 Er1 -175.22(19) . . . . ? O12 Er2 O10 Er1 -132.31(13) 2_655 . . . ? O9 Er2 O10 Er1 146.50(12) . . . . ? O13 Er2 O10 Er1 -66.23(17) 2_655 . . . ? C10 Er2 O10 Er1 -176.6(3) . . . . ? C18 Er2 O10 Er1 -101.21(18) 2_655 . . . ? O3 Er2 O11 C10 -5.8(3) . . . . ? O14 Er2 O11 C10 65.9(3) . . . . ? O18 Er2 O11 C10 -73.9(3) . . . . ? O8 Er2 O11 C10 132.0(3) . . . . ? O12 Er2 O11 C10 -148.3(3) 2_655 . . . ? O9 Er2 O11 C10 141.2(3) . . . . ? O10 Er2 O11 C10 -1.4(2) . . . . ? O13 Er2 O11 C10 -120.9(3) 2_655 . . . ? C18 Er2 O11 C10 -136.2(3) 2_655 . . . ? O17 S1 O14 Er2 -84.4(3) . . . . ? O15 S1 O14 Er2 36.8(4) . . . . ? O16 S1 O14 Er2 155.5(3) . . . . ? O3 Er2 O14 S1 22.3(3) . . . . ? O18 Er2 O14 S1 -46.7(4) . . . . ? O8 Er2 O14 S1 103.7(3) . . . . ? O11 Er2 O14 S1 -110.8(3) . . . . ? O12 Er2 O14 S1 174.3(2) 2_655 . . . ? O9 Er2 O14 S1 177.8(3) . . . . ? O10 Er2 O14 S1 -60.6(3) . . . . ? O13 Er2 O14 S1 78.9(4) 2_655 . . . ? C10 Er2 O14 S1 -87.1(3) . . . . ? C18 Er2 O14 S1 128.5(3) 2_655 . . . ? O17 S1 O15 Er1 97.7(4) . . . . ? O16 S1 O15 Er1 -142.8(4) . . . . ? O14 S1 O15 Er1 -24.8(5) . . . . ? O10 Er1 O15 S1 50.3(4) . . . . ? O2 Er1 O15 S1 -72.3(4) . . . . ? O19 Er1 O15 S1 -8.9(5) . . . . ? O6 Er1 O15 S1 -136.2(3) . . . . ? O7 Er1 O15 S1 99.1(4) . . . . ? O4 Er1 O15 S1 153.1(4) . . . . ? O5 Er1 O15 S1 -150.9(4) . . . . ? O21 S2 O18 Er2 112.0(3) . . . . ? O19 S2 O18 Er2 -8.3(4) . . . . ? O20 S2 O18 Er2 -128.5(3) . . . . ? O3 Er2 O18 S2 -19.9(3) . . . . ? O14 Er2 O18 S2 47.9(4) . . . . ? O8 Er2 O18 S2 -87.4(3) . . . . ? O11 Er2 O18 S2 115.2(3) . . . . ? O12 Er2 O18 S2 -155.5(3) 2_655 . . . ? O9 Er2 O18 S2 162.2(2) . . . . ? O10 Er2 O18 S2 61.8(3) . . . . ? O13 Er2 O18 S2 -103.2(3) 2_655 . . . ? C10 Er2 O18 S2 89.4(3) . . . . ? C18 Er2 O18 S2 -130.0(3) 2_655 . . . ? O21 S2 O19 Er1 -171.4(2) . . . . ? O20 S2 O19 Er1 68.6(3) . . . . ? O18 S2 O19 Er1 -51.8(3) . . . . ? O15 Er1 O19 S2 71.9(3) . . . . ? O10 Er1 O19 S2 15.6(3) . . . . ? O2 Er1 O19 S2 136.2(3) . . . . ? O6 Er1 O19 S2 -139.1(3) . . . . ? O7 Er1 O19 S2 -62.3(3) . . . . ? O4 Er1 O19 S2 -71.4(4) . . . . ? O5 Er1 O19 S2 -173.8(2) . . . . ? O25 Ni1 N1 C5 -39.7(4) . . . . ? O24 Ni1 N1 C5 46.2(4) . . . . ? N4 Ni1 N1 C5 5(16) 4_575 . . . ? O23 Ni1 N1 C5 133.7(4) . . . . ? O22 Ni1 N1 C5 -135.5(4) . . . . ? O25 Ni1 N1 C4 160.2(4) . . . . ? O24 Ni1 N1 C4 -114.0(4) . . . . ? N4 Ni1 N1 C4 -155(15) 4_575 . . . ? O23 Ni1 N1 C4 -26.4(4) . . . . ? O22 Ni1 N1 C4 64.4(4) . . . . ? Er2 O3 C1 O2 -32(5) . . . . ? Er2 O3 C1 C2 152(4) . . . . ? Er1 O2 C1 O3 -12.4(5) . . . . ? Er1 O2 C1 C2 163.6(3) . . . . ? O3 C1 C2 C3 27.9(6) . . . . ? O2 C1 C2 C3 -148.3(4) . . . . ? O3 C1 C2 C8 -155.8(4) . . . . ? O2 C1 C2 C8 28.0(7) . . . . ? C8 C2 C3 C4 -2.5(7) . . . . ? C1 C2 C3 C4 173.8(4) . . . . ? C2 C3 C4 N1 -179.3(5) . . . . ? C2 C3 C4 C6 -1.0(7) . . . . ? C5 N1 C4 C3 176.8(5) . . . . ? Ni1 N1 C4 C3 -20.7(8) . . . . ? C5 N1 C4 C6 -1.6(5) . . . . ? Ni1 N1 C4 C6 160.9(3) . . . . ? C4 N1 C5 N2 1.6(6) . . . . ? Ni1 N1 C5 N2 -163.0(3) . . . . ? C6 N2 C5 N1 -0.9(6) . . . . ? C5 N2 C6 C7 177.8(5) . . . . ? C5 N2 C6 C4 -0.2(5) . . . . ? C3 C4 C6 C7 4.2(8) . . . . ? N1 C4 C6 C7 -177.1(4) . . . . ? C3 C4 C6 N2 -177.5(4) . . . . ? N1 C4 C6 N2 1.1(5) . . . . ? N2 C6 C7 C8 178.6(5) . . . . ? C4 C6 C7 C8 -3.7(7) . . . . ? C6 C7 C8 C2 0.2(7) . . . . ? C6 C7 C8 C9 173.5(4) . . . 2 ? C3 C2 C8 C7 2.9(7) . . . . ? C1 C2 C8 C7 -173.2(4) . . . . ? C3 C2 C8 C9 -170.1(4) . . . 2 ? C1 C2 C8 C9 13.7(7) . . . 2 ? Er1 O5 C9 O4 -2.6(5) . . . . ? Er1 O5 C9 C8 172.9(4) . . . 2_545 ? Er1 O4 C9 O5 2.6(5) . . . . ? Er1 O4 C9 C8 -172.6(4) . . . 2_545 ? Er2 O11 C10 O10 2.7(5) . . . . ? Er2 O11 C10 C11 -172.5(3) . . . . ? Er1 O10 C10 O11 166.4(8) . . . . ? Er2 O10 C10 O11 -2.3(4) . . . . ? Er1 O10 C10 C11 -18.5(13) . . . . ? Er2 O10 C10 C11 172.7(4) . . . . ? Er1 O10 C10 Er2 168.7(11) . . . . ? O3 Er2 C10 O11 175.4(3) . . . . ? O14 Er2 C10 O11 -110.0(3) . . . . ? O18 Er2 C10 O11 98.6(3) . . . . ? O8 Er2 C10 O11 -86.2(4) . . . . ? O12 Er2 C10 O11 33.1(3) 2_655 . . . ? O9 Er2 C10 O11 -36.3(3) . . . . ? O10 Er2 C10 O11 177.4(4) . . . . ? O13 Er2 C10 O11 81.3(3) 2_655 . . . ? C18 Er2 C10 O11 52.9(3) 2_655 . . . ? O3 Er2 C10 O10 -2.0(3) . . . . ? O14 Er2 C10 O10 72.6(2) . . . . ? O18 Er2 C10 O10 -78.8(3) . . . . ? O8 Er2 C10 O10 96.4(4) . . . . ? O11 Er2 C10 O10 -177.4(4) . . . . ? O12 Er2 C10 O10 -144.3(2) 2_655 . . . ? O9 Er2 C10 O10 146.2(2) . . . . ? O13 Er2 C10 O10 -96.2(3) 2_655 . . . ? C18 Er2 C10 O10 -124.5(2) 2_655 . . . ? O3 Er2 C10 C11 -148.2(17) . . . . ? O14 Er2 C10 C11 -73.6(17) . . . . ? O18 Er2 C10 C11 135.0(17) . . . . ? O8 Er2 C10 C11 -49.7(18) . . . . ? O11 Er2 C10 C11 36.4(16) . . . . ? O12 Er2 C10 C11 69.6(17) 2_655 . . . ? O9 Er2 C10 C11 0.1(17) . . . . ? O10 Er2 C10 C11 -146.1(18) . . . . ? O13 Er2 C10 C11 117.7(16) 2_655 . . . ? C18 Er2 C10 C11 89.4(17) 2_655 . . . ? O11 C10 C11 C12 144.0(5) . . . . ? O10 C10 C11 C12 -31.1(7) . . . . ? Er2 C10 C11 C12 111.7(16) . . . . ? O11 C10 C11 C17 -28.7(6) . . . . ? O10 C10 C11 C17 156.2(4) . . . . ? Er2 C10 C11 C17 -61.0(18) . . . . ? C17 C11 C12 C13 1.7(7) . . . . ? C10 C11 C12 C13 -170.9(4) . . . . ? C11 C12 C13 C15 2.9(7) . . . . ? C11 C12 C13 N4 179.3(5) . . . . ? C14 N4 C13 C12 -175.9(5) . . . . ? Ni1 N4 C13 C12 22.7(8) 4_576 . . . ? C14 N4 C13 C15 0.9(5) . . . . ? Ni1 N4 C13 C15 -160.6(4) 4_576 . . . ? C13 N4 C14 N3 -0.6(6) . . . . ? Ni1 N4 C14 N3 164.0(3) 4_576 . . . ? C15 N3 C14 N4 0.1(6) . . . . ? C14 N3 C15 C16 -177.4(5) . . . . ? C14 N3 C15 C13 0.5(5) . . . . ? C12 C13 C15 N3 176.4(4) . . . . ? N4 C13 C15 N3 -0.8(5) . . . . ? C12 C13 C15 C16 -5.5(8) . . . . ? N4 C13 C15 C16 177.3(4) . . . . ? N3 C15 C16 C17 -179.2(5) . . . . ? C13 C15 C16 C17 3.2(7) . . . . ? C15 C16 C17 C11 1.6(7) . . . . ? C15 C16 C17 C18 -176.0(4) . . . . ? C12 C11 C17 C16 -4.1(7) . . . . ? C10 C11 C17 C16 168.6(4) . . . . ? C12 C11 C17 C18 173.4(4) . . . . ? C10 C11 C17 C18 -13.9(7) . . . . ? Er2 O13 C18 O12 -0.5(4) 2_645 . . . ? Er2 O13 C18 C17 175.9(4) 2_645 . . . ? Er2 O12 C18 O13 0.6(5) 2_645 . . . ? Er2 O12 C18 C17 -175.9(3) 2_645 . . . ? C16 C17 C18 O13 -59.3(6) . . . . ? C11 C17 C18 O13 123.2(5) . . . . ? C16 C17 C18 O12 117.2(5) . . . . ? C11 C17 C18 O12 -60.4(6) . . . . ? C16 C17 C18 Er2 100.8(16) . . . 2_645 ? C11 C17 C18 Er2 -76.8(17) . . . 2_645 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.021 _refine_diff_density_min -1.499 _refine_diff_density_rms 0.247 data_9 _database_code_depnum_ccdc_archive 'CCDC 862570' #TrackingRef '- 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N4 Ni O24 S2 Yb2' _chemical_formula_weight 1149.32 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.408(3) _cell_length_b 8.5449(13) _cell_length_c 24.386(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.573(9) _cell_angle_gamma 90.00 _cell_volume 2896.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5073 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25.02 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 7.308 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2623 _exptl_absorpt_correction_T_max 0.3227 _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 19310 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5073 _reflns_number_gt 4979 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+5.8298P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5073 _refine_ls_number_parameters 472 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 Yb1 Yb 0.358438(12) 0.35749(2) 0.242104(8) 0.00548(8) Uani 1 1 d . . . Yb2 Yb 0.127243(12) 0.13278(2) 0.246527(8) 0.00557(8) Uani 1 1 d . . . Ni3 Ni 0.74225(3) 0.28605(8) -0.00153(2) 0.00739(14) Uani 1 1 d . . . S1 S 0.23437(6) 0.03395(13) 0.14867(4) 0.0067(2) Uani 1 1 d . . . S2 S 0.25742(6) 0.44619(13) 0.34355(4) 0.0069(2) Uani 1 1 d . . . O1 O 0.37845(19) 0.4622(4) 0.15861(12) 0.0099(6) Uani 1 1 d . . . O2 O 0.48560(18) 0.2883(4) 0.21226(12) 0.0095(6) Uani 1 1 d . . . O3 O 0.4250(2) 0.1388(3) 0.29832(14) 0.0111(7) Uani 1 1 d . . . O4 O 0.28232(19) 0.0796(4) 0.29441(12) 0.0106(6) Uani 1 1 d . . . O5 O 0.19461(19) 0.3664(3) 0.20229(13) 0.0094(7) Uani 1 1 d . . . O6 O 0.0426(2) 0.3338(4) 0.18164(13) 0.0092(6) Uani 1 1 d . . . O7 O -0.0184(2) 0.6496(4) 0.20972(13) 0.0098(7) Uani 1 1 d . . . O8 O -0.14776(19) 0.5632(4) 0.13152(13) 0.0122(6) Uani 1 1 d . . . O10 O 0.2911(2) -0.1091(4) 0.17357(14) 0.0129(7) Uani 1 1 d . . . O11 O 0.19067(19) 0.0290(4) 0.08175(12) 0.0116(6) Uani 1 1 d . . . O12 O 0.15550(18) 0.0475(4) 0.16738(12) 0.0096(6) Uani 1 1 d . . . O13 O 0.2992(2) 0.1696(4) 0.16929(14) 0.0115(6) Uani 1 1 d . . . O14 O 0.33674(19) 0.3934(4) 0.32967(13) 0.0092(6) Uani 1 1 d . . . O15 O 0.1696(2) 0.3516(3) 0.30902(13) 0.0094(7) Uani 1 1 d . . . O16 O 0.2367(2) 0.6127(4) 0.32644(13) 0.0111(7) Uani 1 1 d . . . O17 O 0.28441(19) 0.4285(4) 0.40861(12) 0.0126(7) Uani 1 1 d . . . O18 O 0.8161(2) 0.2597(4) 0.09381(12) 0.0100(6) Uani 1 1 d D . . O19 O 0.7315(2) 0.0443(4) -0.00731(12) 0.0135(7) Uani 1 1 d . . . H19A H 0.7549 -0.0110 0.0248 0.020 Uiso 1 1 d R . . H19B H 0.7035 0.0004 -0.0419 0.020 Uiso 1 1 d R . . O20 O 0.67209(19) 0.2832(4) -0.09313(12) 0.0112(6) Uani 1 1 d . . . H20A H 0.6574 0.1963 -0.1119 0.017 Uiso 1 1 d R . . H20B H 0.6571 0.3686 -0.1129 0.017 Uiso 1 1 d R . . O21 O 0.74800(18) 0.5302(4) 0.00689(12) 0.0129(7) Uani 1 1 d . . . H21A H 0.7747 0.5721 0.0419 0.019 Uiso 1 1 d R . . H21B H 0.7236 0.5873 -0.0247 0.019 Uiso 1 1 d R . . O22 O 0.50269(19) 0.4751(4) 0.30727(12) 0.0132(7) Uani 1 1 d . . . H22A H 0.5187 0.4780 0.3453 0.020 Uiso 1 1 d R . . H22B H 0.5392 0.5151 0.2931 0.020 Uiso 1 1 d R . . O23 O 0.3223(2) 0.6236(4) 0.24459(14) 0.0130(7) Uani 1 1 d . . . H23A H 0.2703 0.6503 0.2461 0.019 Uiso 1 1 d R . . H23B H 0.3614 0.6932 0.2440 0.019 Uiso 1 1 d R . . O24 O 0.1214(2) -0.1352(3) 0.26088(14) 0.0102(7) Uani 1 1 d . . . H24A H 0.1692 -0.1925 0.2656 0.015 Uiso 1 1 d R . . H24B H 0.0714 -0.1758 0.2614 0.015 Uiso 1 1 d R . . O25 O -0.02680(19) 0.0387(4) 0.17471(13) 0.0115(6) Uani 1 1 d D . . N1 N 0.6082(2) 0.2875(5) -0.00079(15) 0.0089(7) Uani 1 1 d . . . N2 N 0.4645(2) 0.1832(5) -0.02227(15) 0.0104(8) Uani 1 1 d . . . H2 H 0.4121 0.1317 -0.0415 0.012 Uiso 1 1 d R . . N3 N 0.1243(2) 0.7147(5) 0.00228(14) 0.0088(7) Uani 1 1 d . . . N4 N -0.0188(2) 0.8243(5) -0.02086(16) 0.0112(8) Uani 1 1 d . . . H4 H -0.0700 0.8787 -0.0403 0.013 Uiso 1 1 d R . . C1 C 0.4511(3) 0.3787(5) 0.16700(19) 0.0072(9) Uani 1 1 d . . . C2 C 0.4930(3) 0.3730(5) 0.12161(19) 0.0073(9) Uani 1 1 d . . . C3 C 0.4471(3) 0.2787(5) 0.07093(18) 0.0087(9) Uani 1 1 d . . . H3 H 0.3894 0.2289 0.0633 0.010 Uiso 1 1 calc R . . C4 C 0.4912(3) 0.2617(5) 0.03176(17) 0.0086(9) Uani 1 1 d . . . C5 C 0.5356(3) 0.2026(6) -0.03963(18) 0.0109(9) Uani 1 1 d . . . H5 H 0.5340 0.1607 -0.0752 0.013 Uiso 1 1 calc R . . C6 C 0.5807(3) 0.3303(5) 0.04433(18) 0.0082(8) Uani 1 1 d . . . C7 C 0.6265(3) 0.4246(5) 0.09553(17) 0.0077(8) Uani 1 1 d . . . H7 H 0.6857 0.4705 0.1041 0.009 Uiso 1 1 calc R . . C8 C 0.5817(3) 0.4481(5) 0.13325(17) 0.0067(8) Uani 1 1 d . . . C9 C 0.3725(3) 0.0613(5) 0.31557(17) 0.0075(8) Uani 1 1 d . . . C10 C 0.1078(3) 0.4075(5) 0.17386(18) 0.0077(8) Uani 1 1 d . . . C11 C 0.0784(3) 0.5367(5) 0.12804(17) 0.0080(8) Uani 1 1 d . . . C12 C 0.1296(3) 0.5610(5) 0.09384(17) 0.0075(8) Uani 1 1 d . . . H12 H 0.1874 0.5093 0.1031 0.009 Uiso 1 1 calc R . . C13 C 0.0913(3) 0.6663(5) 0.04482(18) 0.0078(8) Uani 1 1 d . . . C14 C 0.0554(3) 0.8075(5) -0.03543(18) 0.0097(9) Uani 1 1 d . . . H14 H 0.0582 0.8562 -0.0687 0.012 Uiso 1 1 calc R . . C15 C 0.0025(3) 0.7379(6) 0.03066(17) 0.0099(9) Uani 1 1 d . . . C16 C -0.0479(3) 0.7190(5) 0.06580(17) 0.0084(8) Uani 1 1 d . . . H16 H -0.1052 0.7718 0.0567 0.010 Uiso 1 1 calc R . . C17 C -0.0091(3) 0.6182(5) 0.11481(19) 0.0078(9) Uani 1 1 d . . . C18 C -0.0611(3) 0.6071(5) 0.15445(19) 0.0076(9) Uani 1 1 d U . . H25A H -0.066(2) 0.108(3) 0.1530(17) 0.009 Uiso 1 1 d D . . H25B H -0.061(2) -0.029(3) 0.1823(18) 0.009 Uiso 1 1 d D . . H18B H 0.787(3) 0.216(4) 0.1118(16) 0.009 Uiso 1 1 d D . . H18A H 0.837(3) 0.346(3) 0.1115(17) 0.009 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 Yb1 0.00554(11) 0.00477(14) 0.00668(11) 0.00045(6) 0.00315(8) 0.00049(6) Yb2 0.00513(11) 0.00507(14) 0.00691(11) -0.00014(7) 0.00299(8) 0.00026(6) Ni3 0.0082(3) 0.0076(4) 0.0077(3) 0.0000(2) 0.0046(2) 0.0001(2) S1 0.0070(4) 0.0062(6) 0.0074(4) -0.0001(4) 0.0036(4) 0.0003(4) S2 0.0069(4) 0.0070(5) 0.0071(4) -0.0005(4) 0.0032(4) 0.0005(4) O1 0.0100(13) 0.0078(16) 0.0134(14) 0.0025(13) 0.0064(11) 0.0039(12) O2 0.0095(13) 0.0109(17) 0.0093(13) 0.0032(13) 0.0053(11) 0.0030(12) O3 0.0132(15) 0.0090(17) 0.0128(15) 0.0006(12) 0.0072(13) 0.0014(12) O4 0.0075(13) 0.0122(17) 0.0099(13) 0.0014(13) 0.0017(11) 0.0043(12) O5 0.0062(14) 0.0111(17) 0.0098(14) -0.0003(12) 0.0024(12) 0.0030(11) O6 0.0087(14) 0.0085(16) 0.0098(14) 0.0010(13) 0.0034(11) -0.0003(12) O7 0.0087(14) 0.0135(17) 0.0088(14) 0.0007(12) 0.0052(11) -0.0004(12) O8 0.0080(13) 0.0104(16) 0.0182(14) 0.0010(14) 0.0056(11) 0.0001(13) O10 0.0166(15) 0.0095(16) 0.0147(15) 0.0034(13) 0.0086(13) 0.0067(13) O11 0.0092(13) 0.0151(18) 0.0100(13) -0.0005(13) 0.0037(11) 0.0016(12) O12 0.0090(13) 0.0114(17) 0.0103(13) -0.0028(13) 0.0060(11) -0.0028(12) O13 0.0119(14) 0.0106(16) 0.0150(15) -0.0024(14) 0.0087(12) -0.0044(13) O14 0.0070(13) 0.0110(16) 0.0107(14) 0.0010(13) 0.0047(11) 0.0021(12) O15 0.0066(14) 0.0114(17) 0.0104(14) -0.0014(12) 0.0039(12) -0.0033(12) O16 0.0145(15) 0.0066(16) 0.0137(15) -0.0007(13) 0.0074(12) 0.0013(12) O17 0.0114(13) 0.0178(18) 0.0078(13) -0.0011(14) 0.0036(11) 0.0030(13) O18 0.0137(14) 0.0083(16) 0.0108(14) -0.0014(13) 0.0080(11) -0.0041(13) O19 0.0201(14) 0.012(2) 0.0099(13) 0.0008(13) 0.0076(12) -0.0033(14) O20 0.0144(14) 0.0086(16) 0.0090(13) 0.0010(13) 0.0036(11) 0.0003(13) O21 0.0150(15) 0.009(2) 0.0114(13) 0.0017(13) 0.0028(12) 0.0003(12) O22 0.0104(13) 0.0183(19) 0.0133(14) -0.0025(14) 0.0075(11) -0.0037(13) O23 0.0117(15) 0.0112(17) 0.0188(16) 0.0012(13) 0.0091(13) -0.0009(12) O24 0.0065(14) 0.0098(17) 0.0156(16) 0.0029(12) 0.0061(12) 0.0008(11) O25 0.0077(13) 0.0135(18) 0.0121(14) 0.0030(14) 0.0032(11) -0.0015(13) N1 0.0128(16) 0.0066(19) 0.0086(15) -0.0015(15) 0.0057(13) -0.0001(15) N2 0.0089(16) 0.011(2) 0.0100(17) -0.0052(16) 0.0025(13) -0.0029(16) N3 0.0096(16) 0.010(2) 0.0068(15) -0.0004(15) 0.0033(13) 0.0016(15) N4 0.0092(16) 0.013(2) 0.0124(17) 0.0043(17) 0.0053(14) 0.0034(16) C1 0.0074(19) 0.005(2) 0.0095(19) -0.0018(17) 0.0038(16) -0.0023(16) C2 0.0074(19) 0.006(2) 0.0090(19) 0.0037(17) 0.0039(16) 0.0000(16) C3 0.0062(17) 0.007(2) 0.0123(19) 0.0030(18) 0.0035(15) 0.0006(17) C4 0.0093(18) 0.005(2) 0.0087(18) 0.0011(18) 0.0015(15) 0.0001(17) C5 0.0136(19) 0.014(3) 0.0078(18) -0.0014(19) 0.0072(16) 0.0007(19) C6 0.0071(19) 0.007(2) 0.0105(19) 0.0026(19) 0.0040(16) 0.0011(17) C7 0.0061(17) 0.007(2) 0.0102(18) 0.0007(18) 0.0034(15) 0.0010(17) C8 0.0083(17) 0.004(2) 0.0079(17) -0.0006(17) 0.0030(14) -0.0003(17) C9 0.0099(19) 0.006(2) 0.0069(17) -0.0021(17) 0.0037(15) 0.0032(17) C10 0.0104(19) 0.005(2) 0.0080(18) -0.0030(18) 0.0040(16) 0.0002(17) C11 0.0074(17) 0.009(2) 0.0068(17) 0.0000(18) 0.0022(14) -0.0008(17) C12 0.0058(17) 0.006(2) 0.0090(17) -0.0021(18) 0.0019(14) -0.0012(17) C13 0.0082(19) 0.008(2) 0.0075(18) -0.0010(18) 0.0033(15) -0.0037(17) C14 0.014(2) 0.007(2) 0.0084(18) 0.0043(18) 0.0054(16) 0.0017(18) C15 0.0109(19) 0.008(2) 0.0085(18) 0.0006(18) 0.0018(15) 0.0017(17) C16 0.0091(18) 0.006(2) 0.0112(18) -0.0019(18) 0.0056(15) -0.0022(17) C17 0.0073(19) 0.005(2) 0.0097(19) -0.0030(17) 0.0027(16) -0.0006(16) C18 0.0083(19) 0.002(2) 0.012(2) 0.0026(17) 0.0043(16) 0.0018(16) _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 Yb1 O13 2.272(3) . ? Yb1 O5 2.281(3) . ? Yb1 O3 2.283(3) . ? Yb1 O14 2.320(3) . ? Yb1 O22 2.329(3) . ? Yb1 O23 2.348(3) . ? Yb1 O1 2.363(3) . ? Yb1 O2 2.439(3) . ? Yb2 O4 2.207(3) . ? Yb2 O12 2.274(3) . ? Yb2 O6 2.318(3) . ? Yb2 O15 2.321(3) . ? Yb2 O24 2.324(3) . ? Yb2 O7 2.348(3) 2_545 ? Yb2 O25 2.400(3) . ? Yb2 O5 2.682(3) . ? Yb2 O8 2.913(3) 2_545 ? Yb2 C18 3.008(4) 2_545 ? Ni3 O20 2.018(3) . ? Ni3 N3 2.065(3) 3_665 ? Ni3 O19 2.072(4) . ? Ni3 N1 2.073(3) . ? Ni3 O21 2.094(4) . ? Ni3 O18 2.114(3) . ? S1 O13 1.470(3) . ? S1 O10 1.472(3) . ? S1 O11 1.473(3) . ? S1 O12 1.476(3) . ? S2 O17 1.464(3) . ? S2 O14 1.473(3) . ? S2 O16 1.478(3) . ? S2 O15 1.486(3) . ? O1 C1 1.267(5) . ? O2 C1 1.262(5) . ? O3 C9 1.250(5) . ? O4 C9 1.266(5) . ? O5 C10 1.261(5) . ? O6 C10 1.267(5) . ? O7 C18 1.271(5) . ? O7 Yb2 2.348(3) 2 ? O8 C18 1.262(5) . ? O8 Yb2 2.913(3) 2 ? O18 H18B 0.841(10) . ? O18 H18A 0.846(10) . ? O19 H19A 0.8501 . ? O19 H19B 0.8501 . ? O20 H20A 0.8499 . ? O20 H20B 0.8500 . ? O21 H21A 0.8500 . ? O21 H21B 0.8500 . ? O22 H22A 0.8498 . ? O22 H22B 0.8500 . ? O23 H23A 0.8498 . ? O23 H23B 0.8501 . ? O24 H24A 0.8500 . ? O24 H24B 0.8499 . ? O25 H25A 0.845(10) . ? O25 H25B 0.848(10) . ? N1 C5 1.327(5) . ? N1 C6 1.388(5) . ? N2 C5 1.344(5) . ? N2 C4 1.374(5) . ? N2 H2 0.8600 . ? N3 C14 1.326(5) . ? N3 C13 1.400(5) . ? N3 Ni3 2.065(3) 3_665 ? N4 C14 1.344(5) . ? N4 C15 1.369(5) . ? N4 H4 0.8600 . ? C1 C2 1.505(6) . ? C2 C3 1.386(6) . ? C2 C8 1.422(6) . ? C3 C4 1.398(6) . ? C3 H3 0.9300 . ? C4 C6 1.406(6) . ? C5 H5 0.9300 . ? C6 C7 1.395(6) . ? C7 C8 1.383(6) . ? C7 H7 0.9300 . ? C8 C9 1.494(6) 2_655 ? C9 C8 1.494(6) 2_645 ? C10 C11 1.495(6) . ? C11 C12 1.389(6) . ? C11 C17 1.425(6) . ? C12 C13 1.406(6) . ? C12 H12 0.9300 . ? C13 C15 1.399(6) . ? C14 H14 0.9300 . ? C15 C16 1.392(6) . ? C16 C17 1.382(6) . ? C16 H16 0.9300 . ? C17 C18 1.501(6) . ? C18 Yb2 3.008(4) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Yb1 O5 72.17(10) . . ? O13 Yb1 O3 79.37(11) . . ? O5 Yb1 O3 114.26(10) . . ? O13 Yb1 O14 130.07(11) . . ? O5 Yb1 O14 79.32(10) . . ? O3 Yb1 O14 76.19(11) . . ? O13 Yb1 O22 141.34(10) . . ? O5 Yb1 O22 146.16(10) . . ? O3 Yb1 O22 83.93(11) . . ? O14 Yb1 O22 77.84(10) . . ? O13 Yb1 O23 133.21(11) . . ? O5 Yb1 O23 75.38(10) . . ? O3 Yb1 O23 145.84(11) . . ? O14 Yb1 O23 73.64(10) . . ? O22 Yb1 O23 74.43(11) . . ? O13 Yb1 O1 75.64(11) . . ? O5 Yb1 O1 98.78(10) . . ? O3 Yb1 O1 129.46(10) . . ? O14 Yb1 O1 150.16(10) . . ? O22 Yb1 O1 89.06(10) . . ? O23 Yb1 O1 77.06(10) . . ? O13 Yb1 O2 72.47(10) . . ? O5 Yb1 O2 139.90(10) . . ? O3 Yb1 O2 76.70(10) . . ? O14 Yb1 O2 139.48(9) . . ? O22 Yb1 O2 69.84(10) . . ? O23 Yb1 O2 118.18(10) . . ? O1 Yb1 O2 54.14(9) . . ? O4 Yb2 O12 79.80(10) . . ? O4 Yb2 O6 132.48(11) . . ? O12 Yb2 O6 85.14(11) . . ? O4 Yb2 O15 83.42(11) . . ? O12 Yb2 O15 135.47(10) . . ? O6 Yb2 O15 76.53(11) . . ? O4 Yb2 O24 79.69(11) . . ? O12 Yb2 O24 81.16(11) . . ? O6 Yb2 O24 141.80(10) . . ? O15 Yb2 O24 135.50(11) . . ? O4 Yb2 O7 126.48(10) . 2_545 ? O12 Yb2 O7 147.26(10) . 2_545 ? O6 Yb2 O7 87.89(10) . 2_545 ? O15 Yb2 O7 72.88(10) . 2_545 ? O24 Yb2 O7 84.85(10) . 2_545 ? O4 Yb2 O25 145.19(11) . . ? O12 Yb2 O25 76.39(10) . . ? O6 Yb2 O25 70.25(11) . . ? O15 Yb2 O25 131.16(10) . . ? O24 Yb2 O25 71.91(11) . . ? O7 Yb2 O25 71.15(10) 2_545 . ? O4 Yb2 O5 81.23(10) . . ? O12 Yb2 O5 69.39(10) . . ? O6 Yb2 O5 51.33(9) . . ? O15 Yb2 O5 67.44(10) . . ? O24 Yb2 O5 147.24(10) . . ? O7 Yb2 O5 127.82(10) 2_545 . ? O25 Yb2 O5 112.85(10) . . ? O4 Yb2 O8 78.59(9) . 2_545 ? O12 Yb2 O8 145.58(10) . 2_545 ? O6 Yb2 O8 129.01(9) . 2_545 ? O15 Yb2 O8 67.57(10) . 2_545 ? O24 Yb2 O8 68.85(10) . 2_545 ? O7 Yb2 O8 48.15(9) 2_545 2_545 ? O25 Yb2 O8 108.30(9) . 2_545 ? O5 Yb2 O8 132.25(9) . 2_545 ? O4 Yb2 C18 103.01(11) . 2_545 ? O12 Yb2 C18 156.01(11) . 2_545 ? O6 Yb2 C18 108.45(11) . 2_545 ? O15 Yb2 C18 68.18(11) . 2_545 ? O24 Yb2 C18 76.02(11) . 2_545 ? O7 Yb2 C18 23.60(10) 2_545 2_545 ? O25 Yb2 C18 89.44(10) . 2_545 ? O5 Yb2 C18 134.55(10) . 2_545 ? O8 Yb2 C18 24.55(10) 2_545 2_545 ? O20 Ni3 N3 92.85(12) . 3_665 ? O20 Ni3 O19 85.62(12) . . ? N3 Ni3 O19 92.69(13) 3_665 . ? O20 Ni3 N1 87.14(12) . . ? N3 Ni3 N1 179.82(19) 3_665 . ? O19 Ni3 N1 87.48(13) . . ? O20 Ni3 O21 95.76(12) . . ? N3 Ni3 O21 90.22(13) 3_665 . ? O19 Ni3 O21 176.71(10) . . ? N1 Ni3 O21 89.61(13) . . ? O20 Ni3 O18 173.18(15) . . ? N3 Ni3 O18 86.80(12) 3_665 . ? O19 Ni3 O18 87.59(12) . . ? N1 Ni3 O18 93.23(12) . . ? O21 Ni3 O18 91.05(12) . . ? O13 S1 O10 108.58(18) . . ? O13 S1 O11 108.65(18) . . ? O10 S1 O11 109.83(18) . . ? O13 S1 O12 111.17(18) . . ? O10 S1 O12 111.05(18) . . ? O11 S1 O12 107.53(16) . . ? O17 S2 O14 109.99(16) . . ? O17 S2 O16 109.33(19) . . ? O14 S2 O16 109.23(18) . . ? O17 S2 O15 108.73(18) . . ? O14 S2 O15 110.24(17) . . ? O16 S2 O15 109.30(17) . . ? C1 O1 Yb1 94.7(2) . . ? C1 O2 Yb1 91.3(2) . . ? C9 O3 Yb1 116.6(3) . . ? C9 O4 Yb2 171.2(3) . . ? C10 O5 Yb1 163.5(3) . . ? C10 O5 Yb2 85.7(2) . . ? Yb1 O5 Yb2 110.68(11) . . ? C10 O6 Yb2 102.8(2) . . ? C18 O7 Yb2 108.7(2) . 2 ? C18 O8 Yb2 81.9(2) . 2 ? S1 O12 Yb2 140.59(16) . . ? S1 O13 Yb1 143.96(18) . . ? S2 O14 Yb1 135.70(17) . . ? S2 O15 Yb2 137.65(17) . . ? Ni3 O18 H18B 118(3) . . ? Ni3 O18 H18A 112(3) . . ? H18B O18 H18A 106.6(16) . . ? Ni3 O19 H19A 120.1 . . ? Ni3 O19 H19B 119.9 . . ? H19A O19 H19B 120.0 . . ? Ni3 O20 H20A 119.9 . . ? Ni3 O20 H20B 120.1 . . ? H20A O20 H20B 120.0 . . ? Ni3 O21 H21A 120.0 . . ? Ni3 O21 H21B 120.0 . . ? H21A O21 H21B 120.0 . . ? Yb1 O22 H22A 120.0 . . ? Yb1 O22 H22B 120.0 . . ? H22A O22 H22B 120.0 . . ? Yb1 O23 H23A 120.0 . . ? Yb1 O23 H23B 120.0 . . ? H23A O23 H23B 120.0 . . ? Yb2 O24 H24A 120.1 . . ? Yb2 O24 H24B 119.9 . . ? H24A O24 H24B 120.0 . . ? Yb2 O25 H25A 116(3) . . ? Yb2 O25 H25B 125(3) . . ? H25A O25 H25B 105.9(16) . . ? C5 N1 C6 105.0(3) . . ? C5 N1 Ni3 121.8(3) . . ? C6 N1 Ni3 130.9(3) . . ? C5 N2 C4 107.2(4) . . ? C5 N2 H2 126.4 . . ? C4 N2 H2 126.4 . . ? C14 N3 C13 104.6(3) . . ? C14 N3 Ni3 119.8(3) . 3_665 ? C13 N3 Ni3 133.4(3) . 3_665 ? C14 N4 C15 106.8(4) . . ? C14 N4 H4 126.6 . . ? C15 N4 H4 126.6 . . ? O2 C1 O1 119.7(4) . . ? O2 C1 C2 118.1(4) . . ? O1 C1 C2 122.0(4) . . ? C3 C2 C8 121.1(4) . . ? C3 C2 C1 117.3(4) . . ? C8 C2 C1 121.3(4) . . ? C2 C3 C4 117.3(4) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? N2 C4 C3 132.4(4) . . ? N2 C4 C6 105.7(4) . . ? C3 C4 C6 121.9(4) . . ? N1 C5 N2 113.2(4) . . ? N1 C5 H5 123.4 . . ? N2 C5 H5 123.4 . . ? N1 C6 C7 130.7(4) . . ? N1 C6 C4 108.9(4) . . ? C7 C6 C4 120.3(4) . . ? C8 C7 C6 118.4(4) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C2 120.9(4) . . ? C7 C8 C9 117.3(4) . 2_655 ? C2 C8 C9 121.7(4) . 2_655 ? O3 C9 O4 123.6(4) . . ? O3 C9 C8 118.9(3) . 2_645 ? O4 C9 C8 117.4(4) . 2_645 ? O5 C10 O6 120.0(4) . . ? O5 C10 C11 121.6(4) . . ? O6 C10 C11 118.3(3) . . ? C12 C11 C17 121.2(4) . . ? C12 C11 C10 119.4(4) . . ? C17 C11 C10 118.8(4) . . ? C11 C12 C13 117.9(4) . . ? C11 C12 H12 121.1 . . ? C13 C12 H12 121.1 . . ? N3 C13 C12 131.7(4) . . ? N3 C13 C15 108.4(4) . . ? C12 C13 C15 119.8(4) . . ? N3 C14 N4 113.5(4) . . ? N3 C14 H14 123.3 . . ? N4 C14 H14 123.3 . . ? N4 C15 C16 130.6(4) . . ? N4 C15 C13 106.5(4) . . ? C16 C15 C13 122.9(4) . . ? C17 C16 C15 117.2(4) . . ? C17 C16 H16 121.4 . . ? C15 C16 H16 121.4 . . ? C16 C17 C11 120.9(4) . . ? C16 C17 C18 116.4(4) . . ? C11 C17 C18 122.6(4) . . ? O8 C18 O7 121.2(4) . . ? O8 C18 C17 119.4(4) . . ? O7 C18 C17 119.3(4) . . ? O8 C18 Yb2 73.5(2) . 2 ? O7 C18 Yb2 47.7(2) . 2 ? C17 C18 Yb2 166.5(3) . 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 O13 Yb1 O1 C1 -76.7(2) . . . . ? O5 Yb1 O1 C1 -145.6(2) . . . . ? O3 Yb1 O1 C1 -13.9(3) . . . . ? O14 Yb1 O1 C1 130.6(3) . . . . ? O22 Yb1 O1 C1 67.5(2) . . . . ? O23 Yb1 O1 C1 141.7(3) . . . . ? O2 Yb1 O1 C1 1.9(2) . . . . ? O13 Yb1 O2 C1 82.8(2) . . . . ? O5 Yb1 O2 C1 53.7(3) . . . . ? O3 Yb1 O2 C1 165.7(3) . . . . ? O14 Yb1 O2 C1 -145.2(2) . . . . ? O22 Yb1 O2 C1 -106.0(3) . . . . ? O23 Yb1 O2 C1 -47.4(3) . . . . ? O1 Yb1 O2 C1 -1.9(2) . . . . ? O13 Yb1 O3 C9 -81.6(3) . . . . ? O5 Yb1 O3 C9 -16.8(3) . . . . ? O14 Yb1 O3 C9 54.5(3) . . . . ? O22 Yb1 O3 C9 133.4(3) . . . . ? O23 Yb1 O3 C9 83.0(3) . . . . ? O1 Yb1 O3 C9 -142.8(3) . . . . ? O2 Yb1 O3 C9 -155.9(3) . . . . ? O12 Yb2 O4 C9 49.6(19) . . . . ? O6 Yb2 O4 C9 -24(2) . . . . ? O15 Yb2 O4 C9 -89(2) . . . . ? O24 Yb2 O4 C9 132(2) . . . . ? O7 Yb2 O4 C9 -152.0(19) 2_545 . . . ? O25 Yb2 O4 C9 97(2) . . . . ? O5 Yb2 O4 C9 -20.9(19) . . . . ? O8 Yb2 O4 C9 -157(2) 2_545 . . . ? C18 Yb2 O4 C9 -154.7(19) 2_545 . . . ? O13 Yb1 O5 C10 -108.9(10) . . . . ? O3 Yb1 O5 C10 -178.0(9) . . . . ? O14 Yb1 O5 C10 112.6(10) . . . . ? O22 Yb1 O5 C10 64.3(10) . . . . ? O23 Yb1 O5 C10 36.9(9) . . . . ? O1 Yb1 O5 C10 -37.2(10) . . . . ? O2 Yb1 O5 C10 -79.7(10) . . . . ? O13 Yb1 O5 Yb2 77.15(12) . . . . ? O3 Yb1 O5 Yb2 8.09(15) . . . . ? O14 Yb1 O5 Yb2 -61.34(12) . . . . ? O22 Yb1 O5 Yb2 -109.56(18) . . . . ? O23 Yb1 O5 Yb2 -137.04(13) . . . . ? O1 Yb1 O5 Yb2 148.89(11) . . . . ? O2 Yb1 O5 Yb2 106.35(15) . . . . ? O4 Yb2 O5 C10 -178.9(2) . . . . ? O12 Yb2 O5 C10 98.8(2) . . . . ? O6 Yb2 O5 C10 -1.9(2) . . . . ? O15 Yb2 O5 C10 -92.4(2) . . . . ? O24 Yb2 O5 C10 126.2(2) . . . . ? O7 Yb2 O5 C10 -49.0(3) 2_545 . . . ? O25 Yb2 O5 C10 34.3(2) . . . . ? O8 Yb2 O5 C10 -113.1(2) 2_545 . . . ? C18 Yb2 O5 C10 -79.2(3) 2_545 . . . ? O4 Yb2 O5 Yb1 -0.64(11) . . . . ? O12 Yb2 O5 Yb1 -82.96(12) . . . . ? O6 Yb2 O5 Yb1 176.38(17) . . . . ? O15 Yb2 O5 Yb1 85.83(13) . . . . ? O24 Yb2 O5 Yb1 -55.6(2) . . . . ? O7 Yb2 O5 Yb1 129.29(12) 2_545 . . . ? O25 Yb2 O5 Yb1 -147.41(11) . . . . ? O8 Yb2 O5 Yb1 65.13(15) 2_545 . . . ? C18 Yb2 O5 Yb1 99.02(15) 2_545 . . . ? O4 Yb2 O6 C10 5.9(3) . . . . ? O12 Yb2 O6 C10 -65.5(3) . . . . ? O15 Yb2 O6 C10 73.7(3) . . . . ? O24 Yb2 O6 C10 -134.5(2) . . . . ? O7 Yb2 O6 C10 146.6(3) 2_545 . . . ? O25 Yb2 O6 C10 -142.7(3) . . . . ? O5 Yb2 O6 C10 1.9(2) . . . . ? O8 Yb2 O6 C10 119.3(2) 2_545 . . . ? C18 Yb2 O6 C10 134.8(2) 2_545 . . . ? O13 S1 O12 Yb2 -37.3(3) . . . . ? O10 S1 O12 Yb2 83.7(3) . . . . ? O11 S1 O12 Yb2 -156.1(3) . . . . ? O4 Yb2 O12 S1 -25.5(3) . . . . ? O6 Yb2 O12 S1 109.2(3) . . . . ? O15 Yb2 O12 S1 44.0(4) . . . . ? O24 Yb2 O12 S1 -106.5(3) . . . . ? O7 Yb2 O12 S1 -172.3(2) 2_545 . . . ? O25 Yb2 O12 S1 -179.9(3) . . . . ? O5 Yb2 O12 S1 58.9(3) . . . . ? O8 Yb2 O12 S1 -77.3(4) 2_545 . . . ? C18 Yb2 O12 S1 -124.6(3) 2_545 . . . ? O10 S1 O13 Yb1 -94.1(3) . . . . ? O11 S1 O13 Yb1 146.5(3) . . . . ? O12 S1 O13 Yb1 28.3(4) . . . . ? O5 Yb1 O13 S1 -53.2(3) . . . . ? O3 Yb1 O13 S1 66.8(3) . . . . ? O14 Yb1 O13 S1 5.1(4) . . . . ? O22 Yb1 O13 S1 132.8(3) . . . . ? O23 Yb1 O13 S1 -101.4(3) . . . . ? O1 Yb1 O13 S1 -157.5(3) . . . . ? O2 Yb1 O13 S1 146.0(4) . . . . ? O17 S2 O14 Yb1 174.1(2) . . . . ? O16 S2 O14 Yb1 -65.9(3) . . . . ? O15 S2 O14 Yb1 54.2(3) . . . . ? O13 Yb1 O14 S2 -72.8(3) . . . . ? O5 Yb1 O14 S2 -17.3(3) . . . . ? O3 Yb1 O14 S2 -135.8(3) . . . . ? O22 Yb1 O14 S2 137.6(3) . . . . ? O23 Yb1 O14 S2 60.4(3) . . . . ? O1 Yb1 O14 S2 71.7(3) . . . . ? O2 Yb1 O14 S2 174.9(2) . . . . ? O17 S2 O15 Yb2 -113.9(3) . . . . ? O14 S2 O15 Yb2 6.7(3) . . . . ? O16 S2 O15 Yb2 126.8(3) . . . . ? O4 Yb2 O15 S2 23.0(3) . . . . ? O12 Yb2 O15 S2 -45.2(3) . . . . ? O6 Yb2 O15 S2 -113.6(3) . . . . ? O24 Yb2 O15 S2 91.0(3) . . . . ? O7 Yb2 O15 S2 154.4(3) 2_545 . . . ? O25 Yb2 O15 S2 -161.5(2) . . . . ? O5 Yb2 O15 S2 -60.2(3) . . . . ? O8 Yb2 O15 S2 103.3(3) 2_545 . . . ? C18 Yb2 O15 S2 129.9(3) 2_545 . . . ? O20 Ni3 N1 C5 39.6(3) . . . . ? N3 Ni3 N1 C5 127(41) 3_665 . . . ? O19 Ni3 N1 C5 -46.1(3) . . . . ? O21 Ni3 N1 C5 135.4(3) . . . . ? O18 Ni3 N1 C5 -133.6(3) . . . . ? O20 Ni3 N1 C6 -160.7(4) . . . . ? N3 Ni3 N1 C6 -74(33) 3_665 . . . ? O19 Ni3 N1 C6 113.6(4) . . . . ? O21 Ni3 N1 C6 -64.9(4) . . . . ? O18 Ni3 N1 C6 26.1(4) . . . . ? Yb1 O2 C1 O1 3.3(4) . . . . ? Yb1 O2 C1 C2 -171.5(3) . . . . ? Yb1 O1 C1 O2 -3.4(4) . . . . ? Yb1 O1 C1 C2 171.2(3) . . . . ? O2 C1 C2 C3 95.0(5) . . . . ? O1 C1 C2 C3 -79.7(5) . . . . ? O2 C1 C2 C8 -78.6(5) . . . . ? O1 C1 C2 C8 106.7(5) . . . . ? C8 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 -174.1(4) . . . . ? C5 N2 C4 C3 -178.3(5) . . . . ? C5 N2 C4 C6 1.1(5) . . . . ? C2 C3 C4 N2 -177.6(4) . . . . ? C2 C3 C4 C6 3.1(6) . . . . ? C6 N1 C5 N2 -1.8(5) . . . . ? Ni3 N1 C5 N2 162.4(3) . . . . ? C4 N2 C5 N1 0.5(5) . . . . ? C5 N1 C6 C7 -177.2(5) . . . . ? Ni3 N1 C6 C7 20.6(7) . . . . ? C5 N1 C6 C4 2.4(5) . . . . ? Ni3 N1 C6 C4 -159.8(3) . . . . ? N2 C4 C6 N1 -2.2(5) . . . . ? C3 C4 C6 N1 177.2(4) . . . . ? N2 C4 C6 C7 177.5(4) . . . . ? C3 C4 C6 C7 -3.1(7) . . . . ? N1 C6 C7 C8 179.7(4) . . . . ? C4 C6 C7 C8 0.1(6) . . . . ? C6 C7 C8 C2 2.5(6) . . . . ? C6 C7 C8 C9 -174.4(4) . . . 2_655 ? C3 C2 C8 C7 -2.4(6) . . . . ? C1 C2 C8 C7 171.0(4) . . . . ? C3 C2 C8 C9 174.3(4) . . . 2_655 ? C1 C2 C8 C9 -12.3(6) . . . 2_655 ? Yb1 O3 C9 O4 14.0(5) . . . . ? Yb1 O3 C9 C8 -161.7(3) . . . 2_645 ? Yb2 O4 C9 O3 13(2) . . . . ? Yb2 O4 C9 C8 -171.6(17) . . . 2_645 ? Yb1 O5 C10 O6 -171.2(7) . . . . ? Yb2 O5 C10 O6 3.1(4) . . . . ? Yb1 O5 C10 C11 12.3(12) . . . . ? Yb2 O5 C10 C11 -173.4(4) . . . . ? Yb2 O6 C10 O5 -3.7(4) . . . . ? Yb2 O6 C10 C11 172.9(3) . . . . ? O5 C10 C11 C12 32.2(6) . . . . ? O6 C10 C11 C12 -144.4(4) . . . . ? O5 C10 C11 C17 -156.1(4) . . . . ? O6 C10 C11 C17 27.3(6) . . . . ? C17 C11 C12 C13 -1.4(6) . . . . ? C10 C11 C12 C13 170.1(4) . . . . ? C14 N3 C13 C12 176.1(5) . . . . ? Ni3 N3 C13 C12 -21.1(7) 3_665 . . . ? C14 N3 C13 C15 -1.4(5) . . . . ? Ni3 N3 C13 C15 161.4(3) 3_665 . . . ? C11 C12 C13 N3 -179.6(4) . . . . ? C11 C12 C13 C15 -2.3(6) . . . . ? C13 N3 C14 N4 0.4(5) . . . . ? Ni3 N3 C14 N4 -165.2(3) 3_665 . . . ? C15 N4 C14 N3 0.7(5) . . . . ? C14 N4 C15 C16 177.6(5) . . . . ? C14 N4 C15 C13 -1.6(5) . . . . ? N3 C13 C15 N4 1.9(5) . . . . ? C12 C13 C15 N4 -176.0(4) . . . . ? N3 C13 C15 C16 -177.4(4) . . . . ? C12 C13 C15 C16 4.8(7) . . . . ? N4 C15 C16 C17 177.7(4) . . . . ? C13 C15 C16 C17 -3.2(6) . . . . ? C15 C16 C17 C11 -0.6(6) . . . . ? C15 C16 C17 C18 176.2(4) . . . . ? C12 C11 C17 C16 2.9(6) . . . . ? C10 C11 C17 C16 -168.7(4) . . . . ? C12 C11 C17 C18 -173.7(4) . . . . ? C10 C11 C17 C18 14.7(6) . . . . ? Yb2 O8 C18 O7 0.6(4) 2 . . . ? Yb2 O8 C18 C17 -175.8(4) 2 . . . ? Yb2 O7 C18 O8 -0.8(5) 2 . . . ? Yb2 O7 C18 C17 175.6(3) 2 . . . ? C16 C17 C18 O8 59.5(6) . . . . ? C11 C17 C18 O8 -123.7(5) . . . . ? C16 C17 C18 O7 -116.9(5) . . . . ? C11 C17 C18 O7 59.8(6) . . . . ? C16 C17 C18 Yb2 -102.9(12) . . . 2 ? C11 C17 C18 Yb2 73.8(14) . . . 2 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.243 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.197