# 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 stuart.batten@sci.monash.edu.au _publ_contact_author_name 'Stuart Batten' _publ_author_name 'Stuart Batten' data_AC4482.CIF _database_code_depnum_ccdc_archive 'CCDC 884900' #TrackingRef '- 1Er.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Bis(aqua)hexakis(carbamoylcyanonitrosomethanido)bis (dicyanonitrosomethanido)bis(oxo)dimanganese(III)dierbium (III)].undecaacetonitrile.monohydrate ; _chemical_name_common '[Er2Mn2(ccnm)6(dcnm)2(H2O)2(O)2]' _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Er2 Mn2 N24 O18, H2 O1, (C2 H3 N1)11' _chemical_formula_sum 'C46 H51 Er2 Mn2 N35 O19' _chemical_formula_weight 1842.62 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 24.0111(4) _cell_length_b 14.0491(3) _cell_length_c 23.3703(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.147(1) _cell_angle_gamma 90.00 _cell_volume 7804.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 25279 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 2.527 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4918 _exptl_absorpt_correction_T_max 0.6003 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25279 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8902 _reflns_number_gt 6859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. H9OA and H9OB refined in a fixed position. Bond lengths and angles of lattice acetonitrile solvent and water molecules restrained using DFIX and DANG commands. ; _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^)+(0.2000P)^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 none _refine_ls_extinction_expression ? _refine_ls_number_reflns 8902 _refine_ls_number_parameters 494 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Er1 Er 0.132479(8) 0.838128(16) 0.035954(8) 0.01703(9) Uani 1 1 d . . . Mn1 Mn 0.24102(3) 0.79613(6) -0.05315(3) 0.01576(16) Uani 1 1 d . . . O1 O 0.21980(13) 0.8075(3) 0.02043(13) 0.0161(7) Uani 1 1 d . . . O2 O 0.11157(14) 0.7479(3) -0.05066(14) 0.0216(8) Uani 1 1 d . . . O3 O 0.19814(13) 0.9111(3) -0.08201(13) 0.0209(7) Uani 1 1 d . . . O4 O 0.06359(13) 0.9457(3) -0.00428(14) 0.0241(8) Uani 1 1 d . . . O5 O 0.18565(14) 0.6097(3) 0.05059(15) 0.0234(8) Uani 1 1 d . . . O6 O 0.04616(14) 0.7594(3) 0.04056(15) 0.0258(8) Uani 1 1 d . . . O7 O 0.24160(13) 0.7383(3) 0.13145(13) 0.0218(8) Uani 1 1 d . . . O8 O 0.09900(14) 0.8786(3) 0.12363(14) 0.0267(8) Uani 1 1 d . . . O9 O 0.17341(10) 0.98584(14) 0.06660(6) 0.0289(8) Uani 1 1 d D . . O10 O 0.0000 1.0182(4) -0.2500 0.0395(15) Uani 1 2 d SD . . N1 N 0.15165(17) 0.7173(3) -0.07855(16) 0.0210(9) Uani 1 1 d . . . N2 N 0.0476(2) 0.5490(5) -0.1035(3) 0.0570(17) Uani 1 1 d . . . N3 N 0.2078(3) 0.5620(5) -0.1726(3) 0.0611(19) Uani 1 1 d . . . N4 N 0.15566(16) 0.9284(3) -0.05362(16) 0.0184(8) Uani 1 1 d . . . N5 N 0.1432(2) 1.1015(4) -0.1567(2) 0.0383(12) Uani 1 1 d . . . N6 N 0.0369(2) 1.0766(4) -0.0564(2) 0.0407(13) Uani 1 1 d . . . H6B H 0.0062 1.0823 -0.0402 0.049 Uiso 1 1 calc R . . H6A H 0.0441 1.1179 -0.0827 0.049 Uiso 1 1 calc R . . N7 N 0.13966(17) 0.6582(3) 0.05097(18) 0.0197(9) Uani 1 1 d . . . N8 N 0.0906(3) 0.4328(5) 0.0694(4) 0.075(2) Uani 1 1 d . . . N9 N -0.0057(2) 0.6309(4) 0.0552(2) 0.0407(13) Uani 1 1 d . . . H9A H -0.0370 0.6643 0.0520 0.049 Uiso 1 1 calc R . . H9B H -0.0065 0.5693 0.0619 0.049 Uiso 1 1 calc R . . N10 N 0.19413(16) 0.7878(3) 0.12889(16) 0.0191(9) Uani 1 1 d . . . N11 N 0.2377(2) 0.7815(5) 0.2757(2) 0.0503(16) Uani 1 1 d . . . N12 N 0.10308(19) 0.8874(4) 0.22044(18) 0.0330(12) Uani 1 1 d . . . H12B H 0.0701 0.9153 0.2187 0.040 Uiso 1 1 calc R . . H12A H 0.1229 0.8748 0.2542 0.040 Uiso 1 1 calc R . . N13 N 0.0215(3) 0.8853(5) -0.1568(3) 0.0678(19) Uani 1 1 d . . . N14 N 0.3814(4) 1.2393(6) 0.0466(5) 0.139(5) Uani 1 1 d D . . N15 N 0.3785(5) 1.1155(7) 0.2918(4) 0.094(3) Uani 1 1 d . . . N16 N 0.1564(3) 1.0956(5) 0.1671(3) 0.0587(17) Uani 1 1 d . . . N17 N 0.2470(4) 0.4196(8) -0.0116(4) 0.153(6) Uani 1 1 d D . . N18 N -0.0257(3) 0.7871(8) 0.1627(4) 0.033(2) Uani 0.50 1 d PD A -1 C1 C 0.1394(2) 0.6391(4) -0.1090(2) 0.0291(12) Uani 1 1 d . . . C2 C 0.0880(2) 0.5910(4) -0.1073(2) 0.0347(14) Uani 1 1 d . . . C3 C 0.1792(3) 0.5992(5) -0.1437(3) 0.0375(14) Uani 1 1 d . . . C4 C 0.12234(19) 0.9972(4) -0.07158(19) 0.0183(10) Uani 1 1 d . . . C5 C 0.1330(2) 1.0548(4) -0.1187(2) 0.0220(11) Uani 1 1 d . . . C6 C 0.0717(2) 1.0070(4) -0.0416(2) 0.0232(11) Uani 1 1 d . . . C7 C 0.0928(2) 0.6131(4) 0.0555(2) 0.0238(11) Uani 1 1 d . . . C8 C 0.0922(2) 0.5125(5) 0.0629(3) 0.0410(15) Uani 1 1 d . . . C9 C 0.0424(2) 0.6731(4) 0.0500(2) 0.0260(12) Uani 1 1 d . . . C10 C 0.1786(2) 0.8143(4) 0.1779(2) 0.0241(11) Uani 1 1 d . . . C11 C 0.2114(2) 0.7950(5) 0.2325(2) 0.0346(14) Uani 1 1 d . . . C12 C 0.1232(2) 0.8641(4) 0.1716(2) 0.0270(12) Uani 1 1 d . . . C13 C -0.0016(3) 0.8406(5) -0.1282(3) 0.0492(19) Uani 1 1 d . . . C14 C -0.0313(3) 0.7856(7) -0.0907(3) 0.071(3) Uani 1 1 d . . . H14A H -0.0456 0.7272 -0.1105 0.107 Uiso 1 1 calc R . . H14B H -0.0628 0.8229 -0.0802 0.107 Uiso 1 1 calc R . . H14C H -0.0057 0.7691 -0.0556 0.107 Uiso 1 1 calc R . . C15 C 0.3616(4) 1.2014(9) 0.0876(6) 0.105(5) Uani 1 1 d . . . C16 C 0.3345(6) 1.1536(7) 0.1322(4) 0.099(4) Uani 1 1 d D . . H16A H 0.2975 1.1823 0.1338 0.149 Uiso 1 1 calc R . . H16B H 0.3580 1.1607 0.1698 0.149 Uiso 1 1 calc R . . H16C H 0.3299 1.0858 0.1228 0.149 Uiso 1 1 calc R . . C17 C 0.3414(5) 1.0708(7) 0.2992(4) 0.073(3) Uani 1 1 d . . . C18 C 0.2926(5) 1.0133(7) 0.3092(4) 0.090(3) Uani 1 1 d . . . H18A H 0.2580 1.0491 0.2969 0.135 Uiso 1 1 calc R . . H18B H 0.2952 0.9983 0.3505 0.135 Uiso 1 1 calc R . . H18C H 0.2921 0.9540 0.2870 0.135 Uiso 1 1 calc R . . C19 C 0.1510(3) 1.1248(5) 0.2111(3) 0.0438(16) Uani 1 1 d . . . C20 C 0.1449(4) 1.1634(6) 0.2680(3) 0.069(3) Uani 1 1 d . . . H20A H 0.1209 1.2201 0.2633 0.103 Uiso 1 1 calc R . . H20B H 0.1820 1.1805 0.2884 0.103 Uiso 1 1 calc R . . H20C H 0.1277 1.1153 0.2903 0.103 Uiso 1 1 calc R . . C21 C 0.2348(4) 0.3687(8) 0.0285(5) 0.085(3) Uani 1 1 d . . . C22 C 0.2105(4) 0.3131(8) 0.0728(4) 0.086(3) Uani 1 1 d D . . H22A H 0.1808 0.3504 0.0871 0.129 Uiso 1 1 calc R . . H22B H 0.2400 0.2984 0.1050 0.129 Uiso 1 1 calc R . . H22C H 0.1945 0.2537 0.0557 0.129 Uiso 1 1 calc R . . C23 C -0.0086(5) 0.7604(9) 0.2089(4) 0.063(6) Uani 0.50 1 d PD A -1 C24 C 0.0136(12) 0.7235(17) 0.2699(6) 0.133(16) Uani 0.50 1 d PD A -1 H24A H 0.0305 0.6604 0.2670 0.199 Uiso 0.50 1 calc PR A -1 H24B H -0.0175 0.7190 0.2927 0.199 Uiso 0.50 1 calc PR A -1 H24C H 0.0421 0.7675 0.2888 0.199 Uiso 0.50 1 calc PR A -1 H9OA H 0.1985 1.0219 0.0550 0.098 Uiso 1 1 d D . . H9OB H 0.1674 1.0043 0.1003 0.128 Uiso 1 1 d D . . H10O H 0.003(3) 0.986(4) -0.2184(14) 0.04(2) 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 Er1 0.01291(13) 0.02249(15) 0.01721(13) 0.00067(8) 0.00734(8) 0.00270(9) Mn1 0.0120(3) 0.0216(4) 0.0149(3) 0.0004(3) 0.0063(3) 0.0034(3) O1 0.0119(15) 0.0241(18) 0.0140(14) 0.0014(13) 0.0075(12) 0.0028(14) O2 0.0152(16) 0.030(2) 0.0200(16) -0.0025(15) 0.0053(13) 0.0012(15) O3 0.0166(16) 0.028(2) 0.0205(16) 0.0028(14) 0.0096(13) 0.0063(15) O4 0.0143(16) 0.032(2) 0.0277(17) 0.0092(16) 0.0107(14) 0.0083(16) O5 0.0167(16) 0.022(2) 0.0327(19) 0.0030(15) 0.0081(14) 0.0015(15) O6 0.0163(17) 0.033(2) 0.0305(19) 0.0032(17) 0.0117(14) -0.0005(17) O7 0.0158(16) 0.032(2) 0.0198(16) 0.0002(15) 0.0086(13) 0.0061(15) O8 0.0205(17) 0.039(2) 0.0223(17) 0.0014(17) 0.0104(14) 0.0073(17) O9 0.032(2) 0.026(2) 0.0296(18) -0.0040(16) 0.0094(16) -0.0014(18) O10 0.032(3) 0.035(4) 0.054(4) 0.000 0.016(3) 0.000 N1 0.018(2) 0.031(3) 0.0155(18) -0.0002(17) 0.0059(16) -0.0005(19) N2 0.039(3) 0.051(4) 0.086(4) -0.018(3) 0.023(3) -0.021(3) N3 0.056(4) 0.056(4) 0.080(4) -0.039(3) 0.040(3) -0.022(3) N4 0.0164(19) 0.023(2) 0.0171(18) -0.0013(16) 0.0071(15) 0.0022(18) N5 0.034(3) 0.044(3) 0.037(3) 0.010(2) 0.006(2) 0.004(3) N6 0.037(3) 0.035(3) 0.057(3) 0.022(3) 0.030(3) 0.018(2) N7 0.0145(19) 0.027(2) 0.0188(18) 0.0015(16) 0.0073(16) 0.0035(17) N8 0.042(4) 0.030(4) 0.155(7) 0.008(4) 0.019(4) 0.001(3) N9 0.021(2) 0.041(3) 0.064(3) -0.008(3) 0.017(2) -0.006(2) N10 0.0138(18) 0.025(2) 0.0201(19) 0.0001(17) 0.0068(15) 0.0039(18) N11 0.043(3) 0.083(5) 0.025(2) -0.007(3) 0.003(2) 0.022(3) N12 0.030(2) 0.052(3) 0.020(2) 0.000(2) 0.0121(19) 0.010(2) N13 0.075(5) 0.067(5) 0.061(4) 0.017(4) 0.006(4) -0.015(4) N14 0.079(6) 0.070(6) 0.297(15) -0.054(8) 0.126(8) -0.028(5) N15 0.116(8) 0.079(7) 0.087(6) 0.005(5) 0.014(6) 0.011(6) N16 0.063(4) 0.058(4) 0.057(4) -0.029(3) 0.016(3) -0.009(3) N17 0.163(10) 0.219(13) 0.101(7) -0.101(8) 0.101(7) -0.144(10) N18 0.027(5) 0.042(6) 0.032(5) 0.008(5) 0.008(4) 0.013(5) C1 0.026(3) 0.037(3) 0.026(3) -0.005(2) 0.011(2) -0.008(3) C2 0.034(3) 0.035(3) 0.038(3) -0.009(3) 0.012(3) -0.003(3) C3 0.037(3) 0.034(3) 0.044(3) -0.015(3) 0.012(3) -0.010(3) C4 0.017(2) 0.020(3) 0.020(2) -0.0001(19) 0.0077(18) 0.002(2) C5 0.021(2) 0.025(3) 0.021(2) 0.002(2) 0.0082(19) 0.005(2) C6 0.019(2) 0.022(3) 0.030(3) 0.003(2) 0.009(2) 0.004(2) C7 0.020(2) 0.025(3) 0.028(3) 0.001(2) 0.010(2) -0.002(2) C8 0.024(3) 0.029(3) 0.071(4) 0.000(3) 0.010(3) -0.001(3) C9 0.015(2) 0.037(3) 0.027(3) -0.001(2) 0.007(2) -0.003(2) C10 0.021(2) 0.030(3) 0.023(2) -0.006(2) 0.011(2) 0.003(2) C11 0.028(3) 0.052(4) 0.027(3) -0.005(3) 0.014(2) 0.012(3) C12 0.022(2) 0.033(3) 0.028(3) 0.001(2) 0.011(2) 0.002(2) C13 0.045(4) 0.049(5) 0.049(4) 0.007(3) -0.006(3) -0.009(3) C14 0.046(4) 0.093(7) 0.069(5) 0.039(5) -0.012(4) -0.024(5) C15 0.042(5) 0.081(8) 0.183(13) -0.059(9) -0.018(6) 0.014(5) C16 0.151(12) 0.073(7) 0.083(7) 0.004(5) 0.047(8) -0.012(7) C17 0.120(9) 0.048(5) 0.051(5) -0.005(4) 0.010(5) 0.009(6) C18 0.138(10) 0.073(7) 0.058(5) -0.021(5) 0.010(6) -0.008(7) C19 0.042(4) 0.043(4) 0.048(4) -0.012(3) 0.013(3) -0.010(3) C20 0.076(6) 0.081(7) 0.055(5) -0.022(4) 0.030(4) -0.023(5) C21 0.064(6) 0.096(8) 0.086(7) -0.041(6) -0.015(5) 0.021(6) C22 0.060(6) 0.131(9) 0.070(6) 0.020(6) 0.019(5) 0.023(6) C23 0.015(7) 0.049(11) 0.127(16) -0.018(11) 0.017(10) -0.009(8) C24 0.06(2) 0.13(2) 0.22(5) 0.11(3) 0.07(2) 0.062(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.220(3) . ? Er1 O4 2.338(3) . ? Er1 O9 2.3634(6) . ? Er1 O6 2.365(3) . ? Er1 O8 2.374(3) . ? Er1 O2 2.381(3) . ? Er1 N10 2.549(4) . ? Er1 N7 2.555(4) . ? Er1 N4 2.575(4) . ? Er1 Mn1 3.5495(7) 7_565 ? Mn1 O1 1.840(3) 7_565 ? Mn1 O1 1.868(3) . ? Mn1 O3 1.982(3) . ? Mn1 O7 1.993(3) 7_565 ? Mn1 O5 2.197(3) 7_565 ? Mn1 N1 2.413(4) . ? Mn1 Mn1 2.7811(14) 7_565 ? Mn1 Er1 3.5495(7) 7_565 ? O1 Mn1 1.840(3) 7_565 ? O2 N1 1.309(5) . ? O3 N4 1.316(5) . ? O4 C6 1.260(6) . ? O5 N7 1.299(5) . ? O5 Mn1 2.197(3) 7_565 ? O6 C9 1.239(6) . ? O7 N10 1.330(5) . ? O7 Mn1 1.993(3) 7_565 ? O8 C12 1.205(6) . ? N1 C1 1.320(7) . ? N2 C2 1.150(8) . ? N3 C3 1.155(7) . ? N4 C4 1.287(6) . ? N5 C5 1.157(7) . ? N6 C6 1.299(7) . ? N7 C7 1.309(6) . ? N8 C8 1.132(9) . ? N9 C9 1.320(7) . ? N10 C10 1.308(6) . ? N11 C11 1.127(7) . ? N12 C12 1.341(6) . ? N13 C13 1.119(9) . ? N14 C15 1.248(16) . ? N15 C17 1.122(13) . ? N16 C19 1.133(8) . ? N17 C21 1.245(14) . ? N18 C23 1.16002(10) . ? C1 C2 1.413(8) . ? C1 C3 1.449(8) . ? C4 C5 1.419(7) . ? C4 C6 1.494(6) . ? C7 C8 1.424(8) . ? C7 C9 1.465(7) . ? C10 C11 1.428(8) . ? C10 C12 1.493(7) . ? C13 C14 1.433(10) . ? C15 C16 1.467(15) . ? C17 C18 1.470(15) . ? C19 C20 1.461(9) . ? C21 C22 1.483(14) . ? C23 C24 1.54002(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O4 133.67(11) . . ? O1 Er1 O9 81.85(11) . . ? O4 Er1 O9 78.12(12) . . ? O1 Er1 O6 140.42(13) . . ? O4 Er1 O6 75.28(12) . . ? O9 Er1 O6 136.57(10) . . ? O1 Er1 O8 129.10(12) . . ? O4 Er1 O8 83.43(12) . . ? O9 Er1 O8 72.87(10) . . ? O6 Er1 O8 70.52(13) . . ? O1 Er1 O2 81.25(11) . . ? O4 Er1 O2 87.17(12) . . ? O9 Er1 O2 138.92(9) . . ? O6 Er1 O2 73.09(11) . . ? O8 Er1 O2 143.60(12) . . ? O1 Er1 N10 68.75(11) . . ? O4 Er1 N10 144.53(12) . . ? O9 Er1 N10 79.56(12) . . ? O6 Er1 N10 103.80(12) . . ? O8 Er1 N10 63.74(12) . . ? O2 Er1 N10 127.14(12) . . ? O1 Er1 N7 77.50(12) . . ? O4 Er1 N7 136.50(13) . . ? O9 Er1 N7 144.11(12) . . ? O6 Er1 N7 64.76(13) . . ? O8 Er1 N7 98.20(13) . . ? O2 Er1 N7 65.90(13) . . ? N10 Er1 N7 65.73(14) . . ? O1 Er1 N4 69.18(12) . . ? O4 Er1 N4 64.96(11) . . ? O9 Er1 N4 71.67(10) . . ? O6 Er1 N4 123.99(12) . . ? O8 Er1 N4 136.28(13) . . ? O2 Er1 N4 67.35(12) . . ? N10 Er1 N4 131.52(12) . . ? N7 Er1 N4 125.50(13) . . ? O1 Er1 Mn1 26.18(9) . 7_565 ? O4 Er1 Mn1 159.16(8) . 7_565 ? O9 Er1 Mn1 96.89(7) . 7_565 ? O6 Er1 Mn1 119.20(9) . 7_565 ? O8 Er1 Mn1 114.74(9) . 7_565 ? O2 Er1 Mn1 83.52(8) . 7_565 ? N10 Er1 Mn1 51.09(8) . 7_565 ? N7 Er1 Mn1 54.45(9) . 7_565 ? N4 Er1 Mn1 94.22(9) . 7_565 ? O1 Mn1 O1 82.81(15) 7_565 . ? O1 Mn1 O3 175.38(13) 7_565 . ? O1 Mn1 O3 92.72(14) . . ? O1 Mn1 O7 91.64(14) 7_565 7_565 ? O1 Mn1 O7 170.26(16) . 7_565 ? O3 Mn1 O7 92.95(13) . 7_565 ? O1 Mn1 O5 96.00(14) 7_565 7_565 ? O1 Mn1 O5 104.23(14) . 7_565 ? O3 Mn1 O5 83.92(13) . 7_565 ? O7 Mn1 O5 84.25(14) 7_565 7_565 ? O1 Mn1 N1 97.12(15) 7_565 . ? O1 Mn1 N1 85.20(13) . . ? O3 Mn1 N1 83.63(14) . . ? O7 Mn1 N1 87.57(13) 7_565 . ? O5 Mn1 N1 164.71(14) 7_565 . ? O1 Mn1 Mn1 41.80(9) 7_565 7_565 ? O1 Mn1 Mn1 41.02(10) . 7_565 ? O3 Mn1 Mn1 133.72(9) . 7_565 ? O7 Mn1 Mn1 132.92(11) 7_565 7_565 ? O5 Mn1 Mn1 103.55(10) 7_565 7_565 ? N1 Mn1 Mn1 91.48(10) . 7_565 ? O1 Mn1 Er1 32.17(9) 7_565 7_565 ? O1 Mn1 Er1 106.36(10) . 7_565 ? O3 Mn1 Er1 150.07(9) . 7_565 ? O7 Mn1 Er1 71.82(10) 7_565 7_565 ? O5 Mn1 Er1 69.35(9) 7_565 7_565 ? N1 Mn1 Er1 120.07(11) . 7_565 ? Mn1 Mn1 Er1 68.25(3) 7_565 7_565 ? Mn1 O1 Mn1 97.19(15) 7_565 . ? Mn1 O1 Er1 121.65(15) 7_565 . ? Mn1 O1 Er1 123.65(16) . . ? N1 O2 Er1 121.1(3) . . ? N4 O3 Mn1 112.4(3) . . ? C6 O4 Er1 123.4(3) . . ? N7 O5 Mn1 111.3(3) . 7_565 ? C9 O6 Er1 123.5(3) . . ? N10 O7 Mn1 112.0(3) . 7_565 ? C12 O8 Er1 125.9(3) . . ? O2 N1 C1 114.7(4) . . ? O2 N1 Mn1 114.7(3) . . ? C1 N1 Mn1 129.6(3) . . ? C4 N4 O3 117.7(4) . . ? C4 N4 Er1 116.0(3) . . ? O3 N4 Er1 126.3(3) . . ? O5 N7 C7 119.2(4) . . ? O5 N7 Er1 124.0(3) . . ? C7 N7 Er1 116.6(3) . . ? C10 N10 O7 117.3(4) . . ? C10 N10 Er1 117.7(3) . . ? O7 N10 Er1 125.0(3) . . ? N1 C1 C2 120.8(5) . . ? N1 C1 C3 120.6(5) . . ? C2 C1 C3 118.6(5) . . ? N2 C2 C1 176.4(7) . . ? N3 C3 C1 174.7(6) . . ? N4 C4 C5 120.6(4) . . ? N4 C4 C6 115.2(4) . . ? C5 C4 C6 124.0(4) . . ? N5 C5 C4 178.1(6) . . ? O4 C6 N6 122.8(4) . . ? O4 C6 C4 118.5(4) . . ? N6 C6 C4 118.6(4) . . ? N7 C7 C8 120.8(5) . . ? N7 C7 C9 115.1(5) . . ? C8 C7 C9 124.0(5) . . ? N8 C8 C7 178.2(7) . . ? O6 C9 N9 122.9(5) . . ? O6 C9 C7 119.9(5) . . ? N9 C9 C7 117.1(5) . . ? N10 C10 C11 122.7(5) . . ? N10 C10 C12 114.1(4) . . ? C11 C10 C12 123.2(4) . . ? N11 C11 C10 178.6(8) . . ? O8 C12 N12 124.6(5) . . ? O8 C12 C10 118.4(5) . . ? N12 C12 C10 117.0(5) . . ? N13 C13 C14 178.5(10) . . ? N14 C15 C16 175.1(12) . . ? N15 C17 C18 179.3(12) . . ? N16 C19 C20 179.0(8) . . ? N17 C21 C22 170.4(11) . . ? N18 C23 C24 179.2(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N12 H12B O10 0.88 2.14 2.975(5) 157.6 5_575 N12 H12A N5 0.88 2.10 2.901(7) 151.5 6_576 N6 H6B O4 0.88 2.13 2.984(5) 163.6 5_575 N6 H6A N18 0.88 2.29 3.119(10) 157.0 5_575 O9 H9OA N17 0.86 1.95 2.787(7) 164.8 7_565 N9 H9B N2 0.88 2.22 2.998(8) 146.6 5_565 O10 H10O N13 0.86 2.023(18) 2.859(8) 164(6) . O9 H9OB N16 0.86 2.07 2.886(6) 159.2 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.230 _refine_diff_density_min -1.673 _refine_diff_density_rms 0.190 # Attachment '- 1Gd.CIF' data_C:\GdMn\P-1NEW2.CIF _database_code_depnum_ccdc_archive 'CCDC 884901' #TrackingRef '- 1Gd.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Bis(aqua)hexakis(carbamoylcyanonitrosomethanide)bis (dicyanonitrosomethanide)bis(oxo)dimanganese(III)digadolinium (III)].trihydrate.octaacetonitrile ; _chemical_name_common '[Gd2Mn2(O)2(ccnm)6(dcnm)2(H2O)2].3H2O.8MeCN' _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Gd2 Mn2 N24 O18, 3(H2 O), 8(C2 H3 N)' _chemical_formula_sum 'C40 H46 Gd2 Mn2 N32 O21' _chemical_formula_weight 1735.47 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0873(10) _cell_length_b 13.5327(12) _cell_length_c 13.5370(11) _cell_angle_alpha 89.992(4) _cell_angle_beta 112.274(4) _cell_angle_gamma 90.175(4) _cell_volume 2049.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 23496 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.974 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4386 _exptl_absorpt_correction_T_max 0.6936 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23496 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9268 _reflns_number_gt 8284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. Hydrogen atoms of full occupancy water molecules located from the Fourier map, with bond lengths of the hydrogen atoms restrained using DFIX and DANG commands. One lattice water molecule was refined at 50 % occupancy. Bond lengths and angles of lattice acetonitrile solvent and water molecules restrained using DFIX and DANG commands. Two lattice unique acetonitrile molecules were each disordered over two poisitions and refine at 50 % occupancy. One disordered position of one lattice acetonitrile molecule was refined isotropically. ISOR command used in refinement of O12 C21 C22 C23 C24 N17 N18 ; _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^)+(0.2000P)^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 ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9268 _refine_ls_number_parameters 497 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.232 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.02250(2) 0.144365(16) 0.309162(18) 0.01013(10) Uani 1 1 d . . . Mn1 Mn 0.08485(7) -0.06366(5) 0.48918(6) 0.00990(16) Uani 1 1 d . . . O1 O 0.0396(3) 0.0674(2) 0.4624(3) 0.0111(7) Uani 1 1 d . . . O2 O -0.0294(4) -0.0236(3) 0.2400(3) 0.0149(7) Uani 1 1 d . . . O3 O 0.2185(3) -0.0515(3) 0.4385(3) 0.0147(7) Uani 1 1 d . . . O4 O 0.1560(4) 0.1525(3) 0.2162(3) 0.0184(8) Uani 1 1 d . . . O5 O -0.2260(3) 0.0473(3) 0.3503(3) 0.0165(8) Uani 1 1 d . . . O6 O -0.1230(3) 0.1556(3) 0.1292(3) 0.0157(7) Uani 1 1 d . . . O7 O -0.1122(3) 0.2070(3) 0.4927(3) 0.0142(7) Uani 1 1 d . . . O10 O 0.30844(18) 0.14912(6) 0.6361(3) 0.0327(11) Uani 1 1 d D . . O8 O -0.0133(4) 0.3171(3) 0.2674(3) 0.0166(8) Uani 1 1 d . . . O9 O 0.1895(3) 0.2287(3) 0.4396(3) 0.0219(8) Uani 1 1 d D . . O12 O 0.3905(14) 0.4016(17) 0.649(2) 0.137(11) Uani 0.50 1 d PU . . N1 N -0.0308(4) -0.0966(3) 0.3017(4) 0.0135(8) Uani 1 1 d . . . N2 N -0.2091(7) -0.1752(5) 0.0498(5) 0.0471(18) Uani 1 1 d . . . N3 N -0.1133(5) -0.3293(4) 0.3540(4) 0.0226(10) Uani 1 1 d . . . N4 N 0.2016(4) 0.0197(3) 0.3682(3) 0.0129(8) Uani 1 1 d . . . N5 N 0.4615(6) -0.0854(6) 0.3634(6) 0.0479(19) Uani 1 1 d . . . N6 N 0.3141(5) 0.1060(4) 0.1782(4) 0.0234(11) Uani 1 1 d . . . H6A H 0.2960 0.1478 0.1247 0.028 Uiso 1 1 calc R . . H6B H 0.3773 0.0678 0.1939 0.028 Uiso 1 1 calc R . . N7 N -0.1953(4) 0.0861(3) 0.2764(3) 0.0136(8) Uani 1 1 d . . . N8 N -0.4787(5) 0.0028(5) 0.1305(5) 0.0368(14) Uani 1 1 d . . . N9 N -0.2970(5) 0.1189(5) -0.0028(4) 0.0283(12) Uani 1 1 d . . . H9A H -0.2722 0.1419 -0.0517 0.034 Uiso 1 1 calc R . . H9B H -0.3695 0.0941 -0.0217 0.034 Uiso 1 1 calc R . . N10 N -0.0775(4) 0.2449(3) 0.4184(3) 0.0135(8) Uani 1 1 d . . . N11 N -0.1766(7) 0.4545(4) 0.5059(5) 0.0391(15) Uani 1 1 d . . . N12 N -0.0651(5) 0.4710(4) 0.2945(4) 0.0251(11) Uani 1 1 d . . . H12A H -0.0447 0.4954 0.2435 0.030 Uiso 1 1 calc R . . H12B H -0.0936 0.5102 0.3310 0.030 Uiso 1 1 calc R . . N14 N -0.0132(9) 0.5750(6) 0.1243(7) 0.059(2) Uani 1 1 d . . . N16 N -0.1368(5) 0.1231(8) -0.1345(9) 0.036(3) Uiso 0.50 1 d PD A -1 N17 N -0.1849(13) 0.1680(10) -0.1652(9) 0.041(4) Uani 0.440(14) 1 d PDU A 1 N18 N -0.3308(4) 0.323(2) -0.1686(12) 0.131(12) Uani 0.560(14) 1 d PDU A 2 C1 C -0.0937(5) -0.1740(4) 0.2534(4) 0.0156(10) Uani 1 1 d . . . C2 C -0.1586(6) -0.1747(4) 0.1399(5) 0.0264(13) Uani 1 1 d . . . C3 C -0.1024(5) -0.2586(4) 0.3130(4) 0.0176(11) Uani 1 1 d . . . C4 C 0.2776(5) 0.0258(4) 0.3218(4) 0.0173(10) Uani 1 1 d . . . C5 C 0.3786(6) -0.0373(5) 0.3458(5) 0.0271(13) Uani 1 1 d . . . C6 C 0.2462(5) 0.1004(4) 0.2351(4) 0.0162(10) Uani 1 1 d . . . C7 C -0.2706(5) 0.0821(4) 0.1785(4) 0.0165(10) Uani 1 1 d . . . C8 C -0.3862(5) 0.0376(5) 0.1515(4) 0.0215(12) Uani 1 1 d . . . C9 C -0.2255(5) 0.1216(4) 0.0987(4) 0.0160(10) Uani 1 1 d . . . C10 C -0.0904(5) 0.3388(4) 0.4018(4) 0.0169(10) Uani 1 1 d . . . C11 C -0.1387(6) 0.4017(4) 0.4597(5) 0.0238(12) Uani 1 1 d . . . C12 C -0.0530(5) 0.3763(4) 0.3161(4) 0.0163(10) Uani 1 1 d . . . C15 C -0.0091(8) 0.6199(6) 0.0548(6) 0.0403(18) Uani 1 1 d . . . C16 C -0.0020(12) 0.6764(7) -0.0322(7) 0.064(3) Uani 1 1 d . . . H16A H -0.0206 0.6338 -0.0950 0.097 Uiso 1 1 calc R . . H16B H 0.0791 0.7032 -0.0121 0.097 Uiso 1 1 calc R . . H16C H -0.0594 0.7309 -0.0488 0.097 Uiso 1 1 calc R . . C13 C 0.4950(9) 0.2402(8) 0.3988(8) 0.056(2) Uani 1 1 d . . . C17 C 0.3049(4) 0.3889(8) 0.2069(9) 0.046(4) Uani 0.50 1 d PD B 1 C18 C 0.2545(5) 0.4361(10) 0.2846(10) 0.046(4) Uani 0.50 1 d PD B 1 H18D H 0.2919 0.5009 0.3075 0.069 Uiso 0.50 1 calc PR B 1 H18E H 0.2716 0.3933 0.3470 0.069 Uiso 0.50 1 calc PR B 1 H18F H 0.1678 0.4442 0.2486 0.069 Uiso 0.50 1 calc PR B 1 C19 C -0.0698(5) 0.0695(8) -0.0747(9) 0.027(3) Uiso 0.50 1 d PD A -1 N13 N 0.4120(9) 0.2489(9) 0.4208(9) 0.079(3) Uani 1 1 d . . . C14 C 0.5932(10) 0.2294(13) 0.3651(14) 0.106(6) Uani 1 1 d . . . H14A H 0.6203 0.1606 0.3747 0.159 Uiso 1 1 calc R . . H14B H 0.6589 0.2728 0.4079 0.159 Uiso 1 1 calc R . . H14C H 0.5675 0.2474 0.2896 0.159 Uiso 1 1 calc R . . C20 C 0.0173(10) -0.0030(10) 0.0047(11) 0.020(2) Uiso 0.50 1 d PD A -1 H20A H 0.0073 0.0004 0.0732 0.030 Uiso 0.50 1 calc PR A -1 H20B H 0.0996 0.0149 0.0152 0.030 Uiso 0.50 1 calc PR A -1 H20C H 0.0002 -0.0703 -0.0237 0.030 Uiso 0.50 1 calc PR A -1 H10B H 0.3752 0.1477 0.6271 0.148 Uiso 1 1 d D . . H10A H 0.2773 0.0909 0.6264 0.047 Uiso 1 1 d D . . C21 C -0.2037(12) 0.2217(9) -0.2365(8) 0.030(4) Uani 0.440(14) 1 d PDU A 1 C22 C -0.230(2) 0.2918(16) -0.3322(15) 0.038(6) Uani 0.440(14) 1 d PDU A 1 H22A H -0.1649 0.2876 -0.3587 0.057 Uiso 0.50 1 calc PR A 1 H22B H -0.2358 0.3597 -0.3098 0.057 Uiso 0.50 1 calc PR A 1 H22C H -0.3054 0.2726 -0.3892 0.057 Uiso 0.50 1 calc PR A 1 C23 C -0.2912(4) 0.3088(14) -0.2330(13) 0.075(6) Uani 0.560(14) 1 d PDU A 2 C24 C -0.237(2) 0.291(2) -0.3173(17) 0.087(13) Uani 0.560(14) 1 d PDU A 2 H24A H -0.1642 0.3309 -0.3004 0.130 Uiso 0.50 1 calc PR A 2 H24B H -0.2946 0.3087 -0.3880 0.130 Uiso 0.50 1 calc PR A 2 H24C H -0.2161 0.2205 -0.3172 0.130 Uiso 0.50 1 calc PR A 2 H9OA H 0.2382(8) 0.239(7) 0.4080(18) 0.09(4) Uiso 1 1 d D . . H9OB H 0.226(4) 0.196(7) 0.498(5) 0.08(4) Uiso 1 1 d D . . N15 N 0.3424(18) 0.3516(13) 0.1491(14) 0.072(5) Uani 0.50 1 d PD B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01444(14) 0.00937(14) 0.00847(13) 0.00267(8) 0.00644(10) 0.00119(9) Mn1 0.0132(4) 0.0100(3) 0.0091(3) 0.0035(3) 0.0072(3) 0.0030(3) O1 0.0143(17) 0.0093(16) 0.0109(16) 0.0025(13) 0.0062(14) 0.0015(13) O2 0.022(2) 0.0113(17) 0.0118(17) 0.0045(13) 0.0074(15) 0.0019(14) O3 0.0139(18) 0.0178(18) 0.0155(18) 0.0079(14) 0.0091(15) 0.0046(14) O4 0.021(2) 0.025(2) 0.0147(18) 0.0090(15) 0.0125(16) 0.0047(16) O5 0.0180(19) 0.0234(19) 0.0113(17) 0.0047(14) 0.0093(15) -0.0010(15) O6 0.0181(19) 0.0193(18) 0.0101(17) 0.0048(14) 0.0058(15) -0.0011(15) O7 0.0192(19) 0.0139(17) 0.0134(17) 0.0050(13) 0.0105(15) 0.0041(14) O10 0.028(2) 0.032(2) 0.037(3) 0.002(2) 0.011(2) 0.002(2) O8 0.027(2) 0.0074(16) 0.0180(18) 0.0037(13) 0.0120(16) 0.0010(15) O9 0.022(2) 0.024(2) 0.019(2) 0.0021(16) 0.0077(17) -0.0023(17) O12 0.034(8) 0.141(18) 0.21(2) 0.131(18) 0.015(11) -0.003(9) N1 0.019(2) 0.0105(19) 0.013(2) 0.0023(15) 0.0085(18) 0.0033(17) N2 0.069(5) 0.040(4) 0.018(3) 0.008(2) 0.001(3) -0.019(3) N3 0.033(3) 0.014(2) 0.023(2) 0.0017(18) 0.013(2) 0.001(2) N4 0.015(2) 0.014(2) 0.0102(19) 0.0039(15) 0.0058(17) 0.0018(16) N5 0.039(4) 0.056(4) 0.064(5) 0.032(4) 0.036(4) 0.027(3) N6 0.023(3) 0.032(3) 0.021(2) 0.013(2) 0.016(2) 0.006(2) N7 0.013(2) 0.018(2) 0.011(2) 0.0038(16) 0.0062(17) 0.0029(17) N8 0.023(3) 0.065(4) 0.021(3) 0.005(3) 0.007(2) -0.009(3) N9 0.021(3) 0.052(4) 0.010(2) 0.006(2) 0.005(2) -0.009(2) N10 0.018(2) 0.013(2) 0.0094(19) 0.0047(15) 0.0056(17) 0.0017(17) N11 0.066(5) 0.023(3) 0.043(4) 0.007(2) 0.037(3) 0.017(3) N12 0.046(3) 0.014(2) 0.024(3) 0.0050(19) 0.023(2) 0.004(2) N14 0.100(7) 0.043(4) 0.059(5) 0.026(4) 0.057(5) 0.007(4) N17 0.065(11) 0.040(8) 0.026(7) 0.005(6) 0.024(7) -0.008(8) N18 0.092(16) 0.23(3) 0.087(16) 0.099(18) 0.055(13) 0.040(17) C1 0.022(3) 0.011(2) 0.015(2) 0.0017(19) 0.009(2) 0.002(2) C2 0.037(4) 0.019(3) 0.019(3) 0.001(2) 0.007(3) -0.007(3) C3 0.023(3) 0.016(3) 0.015(2) -0.002(2) 0.008(2) 0.002(2) C4 0.019(3) 0.022(3) 0.015(2) 0.005(2) 0.010(2) 0.001(2) C5 0.026(3) 0.036(3) 0.027(3) 0.014(3) 0.019(3) 0.006(3) C6 0.019(3) 0.017(2) 0.014(2) 0.0034(19) 0.008(2) 0.001(2) C7 0.014(3) 0.022(3) 0.014(2) 0.003(2) 0.005(2) 0.001(2) C8 0.017(3) 0.038(3) 0.009(2) 0.003(2) 0.004(2) -0.003(2) C9 0.019(3) 0.017(2) 0.013(2) 0.0012(19) 0.007(2) 0.002(2) C10 0.020(3) 0.016(2) 0.015(2) 0.0024(19) 0.007(2) 0.002(2) C11 0.034(3) 0.015(3) 0.031(3) 0.009(2) 0.021(3) 0.008(2) C12 0.025(3) 0.013(2) 0.011(2) 0.0031(18) 0.007(2) 0.002(2) C15 0.063(5) 0.032(4) 0.034(4) 0.007(3) 0.027(4) -0.006(3) C16 0.120(10) 0.048(5) 0.036(5) 0.010(4) 0.041(6) -0.013(6) C13 0.047(5) 0.065(6) 0.053(5) -0.002(5) 0.018(4) -0.005(5) C17 0.025(7) 0.044(9) 0.060(11) 0.018(8) 0.007(7) 0.006(6) C18 0.049(10) 0.026(7) 0.071(12) 0.013(7) 0.031(9) 0.008(7) N13 0.051(5) 0.103(8) 0.091(8) -0.004(6) 0.038(5) -0.005(5) C14 0.034(6) 0.134(13) 0.138(14) -0.047(11) 0.018(7) 0.018(7) C21 0.037(9) 0.038(8) 0.024(7) -0.003(6) 0.022(7) -0.008(7) C22 0.050(10) 0.043(11) 0.029(9) 0.005(7) 0.024(8) 0.009(8) C23 0.071(14) 0.063(12) 0.084(15) 0.029(11) 0.022(12) 0.003(10) C24 0.16(3) 0.083(19) 0.030(10) 0.012(10) 0.047(14) -0.043(18) N15 0.075(13) 0.086(14) 0.063(12) -0.001(10) 0.034(10) 0.009(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.260(3) . ? Gd1 O4 2.395(4) . ? Gd1 O9 2.404(4) . ? Gd1 O8 2.406(4) . ? Gd1 O6 2.409(4) . ? Gd1 O2 2.446(4) . ? Gd1 N7 2.618(4) . ? Gd1 N10 2.620(4) . ? Gd1 N4 2.623(4) . ? Gd1 Mn1 3.6061(8) 2_556 ? Gd1 Mn1 3.6125(8) . ? Mn1 O1 1.852(4) . ? Mn1 O1 1.854(4) 2_556 ? Mn1 O7 1.968(4) 2_556 ? Mn1 O3 1.987(4) . ? Mn1 O5 2.207(4) 2_556 ? Mn1 N1 2.429(5) . ? Mn1 Mn1 2.7819(15) 2_556 ? Mn1 Gd1 3.6061(8) 2_556 ? O1 Mn1 1.854(4) 2_556 ? O2 N1 1.299(5) . ? O3 N4 1.314(5) . ? O4 C6 1.244(7) . ? O5 N7 1.301(6) . ? O5 Mn1 2.207(4) 2_556 ? O6 C9 1.236(7) . ? O7 N10 1.330(5) . ? O7 Mn1 1.968(4) 2_556 ? O8 C12 1.245(7) . ? N1 C1 1.311(7) . ? N2 C2 1.138(9) . ? N3 C3 1.138(8) . ? N4 C4 1.298(7) . ? N5 C5 1.143(9) . ? N6 C6 1.323(7) . ? N7 C7 1.294(7) . ? N8 C8 1.144(8) . ? N9 C9 1.317(7) . ? N10 C10 1.290(7) . ? N11 C11 1.153(8) . ? N12 C12 1.311(7) . ? N14 C15 1.136(10) . ? N16 N17 0.835(14) . ? N16 C19 1.16004(14) . ? N16 C21 1.870(13) . ? N17 C21 1.16002(15) . ? N18 C23 1.16003(15) . ? C1 C3 1.427(7) . ? C1 C2 1.437(8) . ? C4 C5 1.425(8) . ? C4 C6 1.484(7) . ? C7 C8 1.434(8) . ? C7 C9 1.481(7) . ? C10 C11 1.424(8) . ? C10 C12 1.484(7) . ? C15 C16 1.434(10) . ? C13 N13 1.156(13) . ? C13 C14 1.431(16) . ? C17 N15 1.16006(14) . ? C17 C18 1.54006(15) . ? C19 C20 1.54004(16) . ? C21 C22 1.54002(16) . ? C23 C24 1.54003(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O4 131.09(13) . . ? O1 Gd1 O9 77.55(13) . . ? O4 Gd1 O9 79.60(14) . . ? O1 Gd1 O8 127.54(13) . . ? O4 Gd1 O8 86.04(13) . . ? O9 Gd1 O8 74.93(13) . . ? O1 Gd1 O6 137.39(13) . . ? O4 Gd1 O6 81.08(13) . . ? O9 Gd1 O6 143.10(13) . . ? O8 Gd1 O6 72.64(13) . . ? O1 Gd1 O2 81.05(12) . . ? O4 Gd1 O2 88.05(13) . . ? O9 Gd1 O2 137.88(13) . . ? O8 Gd1 O2 144.60(13) . . ? O6 Gd1 O2 71.97(13) . . ? O1 Gd1 N7 75.76(13) . . ? O4 Gd1 N7 139.35(14) . . ? O9 Gd1 N7 140.89(13) . . ? O8 Gd1 N7 99.80(14) . . ? O6 Gd1 N7 63.02(13) . . ? O2 Gd1 N7 64.06(13) . . ? O1 Gd1 N10 67.85(13) . . ? O4 Gd1 N10 145.13(14) . . ? O9 Gd1 N10 77.20(13) . . ? O8 Gd1 N10 63.00(13) . . ? O6 Gd1 N10 102.74(13) . . ? O2 Gd1 N10 126.39(13) . . ? N7 Gd1 N10 66.50(14) . . ? O1 Gd1 N4 69.19(13) . . ? O4 Gd1 N4 63.02(13) . . ? O9 Gd1 N4 73.43(13) . . ? O8 Gd1 N4 138.89(14) . . ? O6 Gd1 N4 123.52(13) . . ? O2 Gd1 N4 65.13(13) . . ? N7 Gd1 N4 121.31(14) . . ? N10 Gd1 N4 131.92(13) . . ? O1 Gd1 Mn1 25.82(9) . 2_556 ? O4 Gd1 Mn1 156.67(9) . 2_556 ? O9 Gd1 Mn1 91.69(10) . 2_556 ? O8 Gd1 Mn1 112.74(9) . 2_556 ? O6 Gd1 Mn1 116.80(9) . 2_556 ? O2 Gd1 Mn1 84.04(9) . 2_556 ? N7 Gd1 Mn1 53.91(10) . 2_556 ? N10 Gd1 Mn1 49.79(9) . 2_556 ? N4 Gd1 Mn1 93.81(9) . 2_556 ? O1 Gd1 Mn1 25.60(9) . . ? O4 Gd1 Mn1 112.26(9) . . ? O9 Gd1 Mn1 88.30(10) . . ? O8 Gd1 Mn1 152.78(9) . . ? O6 Gd1 Mn1 128.23(9) . . ? O2 Gd1 Mn1 59.47(8) . . ? N7 Gd1 Mn1 79.69(10) . . ? N10 Gd1 Mn1 92.76(9) . . ? N4 Gd1 Mn1 49.74(9) . . ? Mn1 Gd1 Mn1 45.33(2) 2_556 . ? O1 Mn1 O1 82.73(16) . 2_556 ? O1 Mn1 O7 172.94(17) . 2_556 ? O1 Mn1 O7 93.00(15) 2_556 2_556 ? O1 Mn1 O3 94.26(15) . . ? O1 Mn1 O3 176.78(16) 2_556 . ? O7 Mn1 O3 90.11(15) 2_556 . ? O1 Mn1 O5 99.17(15) . 2_556 ? O1 Mn1 O5 94.73(15) 2_556 2_556 ? O7 Mn1 O5 86.74(15) 2_556 2_556 ? O3 Mn1 O5 84.60(15) . 2_556 ? O1 Mn1 N1 87.70(15) . . ? O1 Mn1 N1 98.14(15) 2_556 . ? O7 Mn1 N1 87.35(15) 2_556 . ? O3 Mn1 N1 82.84(16) . . ? O5 Mn1 N1 166.10(15) 2_556 . ? O1 Mn1 Mn1 41.39(11) . 2_556 ? O1 Mn1 Mn1 41.34(11) 2_556 2_556 ? O7 Mn1 Mn1 134.08(12) 2_556 2_556 ? O3 Mn1 Mn1 135.64(12) . 2_556 ? O5 Mn1 Mn1 99.27(11) 2_556 2_556 ? N1 Mn1 Mn1 93.88(11) . 2_556 ? O1 Mn1 Gd1 105.81(11) . 2_556 ? O1 Mn1 Gd1 32.07(11) 2_556 2_556 ? O7 Mn1 Gd1 72.54(10) 2_556 2_556 ? O3 Mn1 Gd1 149.18(11) . 2_556 ? O5 Mn1 Gd1 69.50(10) 2_556 2_556 ? N1 Mn1 Gd1 120.40(11) . 2_556 ? Mn1 Mn1 Gd1 67.45(3) 2_556 2_556 ? O1 Mn1 Gd1 31.82(11) . . ? O1 Mn1 Gd1 105.53(11) 2_556 . ? O7 Mn1 Gd1 146.63(11) 2_556 . ? O3 Mn1 Gd1 72.14(11) . . ? O5 Mn1 Gd1 118.27(10) 2_556 . ? N1 Mn1 Gd1 63.06(10) . . ? Mn1 Mn1 Gd1 67.21(3) 2_556 . ? Gd1 Mn1 Gd1 134.67(2) 2_556 . ? Mn1 O1 Mn1 97.27(16) . 2_556 ? Mn1 O1 Gd1 122.58(17) . . ? Mn1 O1 Gd1 122.11(17) 2_556 . ? N1 O2 Gd1 121.6(3) . . ? N4 O3 Mn1 112.6(3) . . ? C6 O4 Gd1 125.4(3) . . ? N7 O5 Mn1 112.2(3) . 2_556 ? C9 O6 Gd1 124.7(3) . . ? N10 O7 Mn1 112.8(3) . 2_556 ? C12 O8 Gd1 125.0(3) . . ? O2 N1 C1 115.6(4) . . ? O2 N1 Mn1 113.0(3) . . ? C1 N1 Mn1 131.4(3) . . ? C4 N4 O3 116.8(4) . . ? C4 N4 Gd1 117.8(3) . . ? O3 N4 Gd1 125.3(3) . . ? C7 N7 O5 118.5(5) . . ? C7 N7 Gd1 117.2(3) . . ? O5 N7 Gd1 123.5(3) . . ? C10 N10 O7 117.3(4) . . ? C10 N10 Gd1 117.8(4) . . ? O7 N10 Gd1 124.9(3) . . ? N17 N16 C19 167(2) . . ? N17 N16 C21 24.2(11) . . ? C19 N16 C21 162.9(8) . . ? N16 N17 C21 139(2) . . ? N1 C1 C3 120.7(5) . . ? N1 C1 C2 121.0(5) . . ? C3 C1 C2 118.3(5) . . ? N2 C2 C1 179.5(8) . . ? N3 C3 C1 175.3(6) . . ? N4 C4 C5 123.7(5) . . ? N4 C4 C6 114.2(5) . . ? C5 C4 C6 122.0(5) . . ? N5 C5 C4 177.5(7) . . ? O4 C6 N6 122.5(5) . . ? O4 C6 C4 119.5(5) . . ? N6 C6 C4 118.0(5) . . ? N7 C7 C8 121.1(5) . . ? N7 C7 C9 115.0(5) . . ? C8 C7 C9 123.8(5) . . ? N8 C8 C7 179.3(8) . . ? O6 C9 N9 122.5(5) . . ? O6 C9 C7 119.2(5) . . ? N9 C9 C7 118.3(5) . . ? N10 C10 C11 122.8(5) . . ? N10 C10 C12 114.8(5) . . ? C11 C10 C12 122.4(5) . . ? N11 C11 C10 178.4(7) . . ? O8 C12 N12 123.1(5) . . ? O8 C12 C10 119.1(5) . . ? N12 C12 C10 117.8(5) . . ? N14 C15 C16 179.1(12) . . ? N13 C13 C14 176.7(13) . . ? N15 C17 C18 178.7(7) . . ? N16 C19 C20 178.9(7) . . ? N17 C21 C22 179.1(11) . . ? N17 C21 N16 17.2(9) . . ? C22 C21 N16 162.8(14) . . ? N18 C23 C24 179.0(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6A N2 0.88 2.22 3.009(8) 148.6 2 N12 H12A N14 0.88 2.09 2.962(8) 170.0 . N12 H12B N3 0.88 2.22 2.943(7) 139.1 1_565 N9 H9A N17 0.88 2.20 3.059(13) 166.6 . N9 H9B N8 0.88 2.28 3.078(8) 150.9 2_455 O9 H9OB O10 0.86 1.87(2) 2.722(6) 169(11) . O9 H9OA N13 0.86 2.045(11) 2.808(10) 147.4(12) . O10 H10A O5 0.86 2.03 2.866(4) 163.6 2_556 O10 H10B N5 0.86 2.11 2.911(6) 155.2 2_656 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.169 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.201 # Attachment '- 1Tb.CIF' data_C:\TbMn\P-1.CIF _database_code_depnum_ccdc_archive 'CCDC 884902' #TrackingRef '- 1Tb.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Bis(aqua)hexakis(carbamoylcyanonitrosomethanide)bis (dicyanonitrosomethanide)bis(oxo)dimanganese(III)diterbium (III)].trihydrate.octaacetonitrile ; _chemical_name_common '[Tb2Mn2(O)2(ccnm)6(dcnm)2(H2O)2].3H2O.8MeCN' _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Gd2 Mn2 N24 O18, 3(H2 O), 8(C2 H3 N)' _chemical_formula_sum 'C40 H46 Mn2 N32 O21 Tb2' _chemical_formula_weight 1738.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0839(5) _cell_length_b 13.5201(6) _cell_length_c 13.5658(6) _cell_angle_alpha 90.072(2) _cell_angle_beta 112.601(2) _cell_angle_gamma 90.587(2) _cell_volume 2045.97(15) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 29515 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 2.084 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4222 _exptl_absorpt_correction_T_max 0.6806 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29515 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9360 _reflns_number_gt 8515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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.Hydrogen atoms of the partial occupancy water molecule could not be located from the Fourier map.Hydrogen atoms of full occupancy water molecules located from the Fourier map, with bond lengths of the hydrogen atoms restrained using DFIX and DANG commands. One lattice water molecule was refined at 50 % occupancy. Bond lengths and angles of lattice acetonitrile solvent and water molecules restrained using DFIX and DANG commands. Two lattice unique acetonitrile molecules were each disordered over two poisitions and refine at 50 % occupancy. One disordered position of one lattice acetonitrile molecule was refined isotropically. The hydrogen atoms of one acetonitrile molecule could not be modelled. ISOR restraint applied to N15 C17 C18 C14 ; _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^)+(0.2000P)^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 ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9360 _refine_ls_number_parameters 496 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.023261(17) 0.143676(13) 0.310393(14) 0.01276(7) Uani 1 1 d . . . Mn1 Mn 0.08454(5) -0.06389(4) 0.48934(5) 0.01148(12) Uani 1 1 d . . . O1 O 0.0400(3) 0.0673(2) 0.4620(2) 0.0129(5) Uani 1 1 d . . . O2 O -0.0301(3) -0.0241(2) 0.2399(2) 0.0162(6) Uani 1 1 d . . . O3 O 0.2181(3) -0.0510(2) 0.4397(2) 0.0169(6) Uani 1 1 d . . . O4 O 0.1542(3) 0.1523(2) 0.2169(3) 0.0210(6) Uani 1 1 d . . . O5 O -0.2264(3) 0.0469(2) 0.3496(2) 0.0180(6) Uani 1 1 d . . . O6 O -0.1211(3) 0.1549(2) 0.1305(2) 0.0170(6) Uani 1 1 d . . . O7 O -0.1111(3) 0.2073(2) 0.4923(2) 0.0158(6) Uani 1 1 d . . . O10 O 0.30944(15) 0.14907(6) 0.6377(3) 0.0313(8) Uani 1 1 d D . . O8 O -0.0101(3) 0.3153(2) 0.2680(2) 0.0191(6) Uani 1 1 d . . . O9 O 0.1896(2) 0.2278(2) 0.4395(3) 0.0234(7) Uani 1 1 d D . . N1 N -0.0316(3) -0.0970(3) 0.3018(3) 0.0147(6) Uani 1 1 d . . . N2 N -0.2084(6) -0.1784(4) 0.0477(4) 0.0485(14) Uani 1 1 d . . . N3 N -0.1141(4) -0.3307(3) 0.3530(3) 0.0253(8) Uani 1 1 d . . . N4 N 0.2015(3) 0.0197(3) 0.3692(3) 0.0150(7) Uani 1 1 d . . . N5 N 0.4588(5) -0.0858(4) 0.3635(5) 0.0476(14) Uani 1 1 d . . . N6 N 0.3130(4) 0.1072(3) 0.1797(3) 0.0260(9) Uani 1 1 d . . . H6A H 0.2946 0.1490 0.1263 0.031 Uiso 1 1 calc R . . H6B H 0.3765 0.0697 0.1956 0.031 Uiso 1 1 calc R . . N7 N -0.1945(3) 0.0854(3) 0.2769(3) 0.0149(6) Uani 1 1 d . . . N8 N -0.4813(4) 0.0079(5) 0.1302(4) 0.0433(13) Uani 1 1 d . . . N9 N -0.2970(4) 0.1216(4) -0.0021(3) 0.0382(12) Uani 1 1 d . . . H9A H -0.2713 0.1439 -0.0505 0.046 Uiso 1 1 calc R . . H9B H -0.3707 0.0985 -0.0216 0.046 Uiso 1 1 calc R . . N10 N -0.0754(3) 0.2444(3) 0.4193(3) 0.0154(7) Uani 1 1 d . . . N11 N -0.1778(6) 0.4542(4) 0.5016(4) 0.0435(13) Uani 1 1 d . . . N12 N -0.0631(4) 0.4697(3) 0.2930(3) 0.0282(9) Uani 1 1 d . . . H12A H -0.0424 0.4936 0.2421 0.034 Uiso 1 1 calc R . . H12B H -0.0921 0.5092 0.3286 0.034 Uiso 1 1 calc R . . N14 N -0.0174(7) 0.5749(4) 0.1198(6) 0.0644(19) Uani 1 1 d . . . N15 N 0.3475(3) 0.3569(14) 0.1554(11) 0.104(6) Uani 0.50 1 d PDU A 1 N16 N -0.1367(4) 0.1228(7) -0.1340(8) 0.041(2) Uiso 0.50 1 d PD B -1 N17 N -0.1846(10) 0.1684(9) -0.1643(8) 0.060(4) Uani 0.50 1 d PD C 2 N18 N -0.3234(3) 0.3278(18) -0.1642(12) 0.138(11) Uani 0.50 1 d PD D 1 C1 C -0.0946(4) -0.1752(3) 0.2523(3) 0.0175(8) Uani 1 1 d . . . C2 C -0.1577(5) -0.1771(3) 0.1389(4) 0.0274(10) Uani 1 1 d . . . C3 C -0.1031(4) -0.2595(3) 0.3116(3) 0.0185(8) Uani 1 1 d . . . C4 C 0.2764(4) 0.0265(3) 0.3227(3) 0.0173(8) Uani 1 1 d . . . C5 C 0.3775(4) -0.0369(4) 0.3467(4) 0.0281(10) Uani 1 1 d . . . C6 C 0.2454(4) 0.1008(3) 0.2360(3) 0.0184(8) Uani 1 1 d . . . C7 C -0.2713(4) 0.0831(3) 0.1779(3) 0.0189(8) Uani 1 1 d . . . C8 C -0.3882(4) 0.0413(4) 0.1500(3) 0.0252(10) Uani 1 1 d . . . C9 C -0.2256(4) 0.1230(3) 0.0991(3) 0.0181(8) Uani 1 1 d . . . C10 C -0.0883(4) 0.3383(3) 0.4011(3) 0.0187(8) Uani 1 1 d . . . C11 C -0.1386(5) 0.4018(3) 0.4573(4) 0.0259(10) Uani 1 1 d . . . C12 C -0.0507(4) 0.3753(3) 0.3157(3) 0.0191(8) Uani 1 1 d . . . C15 C -0.0118(8) 0.6186(5) 0.0530(6) 0.0535(18) Uani 1 1 d . . . C16 C -0.0064(11) 0.6750(6) -0.0351(7) 0.079(3) Uani 1 1 d . . . H16A H -0.0637 0.6474 -0.1023 0.118 Uiso 1 1 calc R . . H16B H 0.0748 0.6721 -0.0347 0.118 Uiso 1 1 calc R . . H16C H -0.0265 0.7440 -0.0281 0.118 Uiso 1 1 calc R . . C13 C 0.4974(9) 0.2393(8) 0.4024(8) 0.075(2) Uani 1 1 d . . . C17 C 0.3089(4) 0.3917(10) 0.2135(10) 0.069(4) Uani 0.50 1 d PDU A 1 C18 C 0.2559(16) 0.4361(12) 0.2902(14) 0.071(5) Uani 0.50 1 d PDU A 1 H18A H 0.1682 0.4337 0.2566 0.107 Uiso 0.50 1 calc PR A 1 H18B H 0.2831 0.5050 0.3064 0.107 Uiso 0.50 1 calc PR A 1 H18C H 0.2828 0.3979 0.3565 0.107 Uiso 0.50 1 calc PR A 1 C19 C -0.0706(5) 0.0688(6) -0.0741(7) 0.029(2) Uiso 0.50 1 d PD B -1 N13 N 0.4125(9) 0.2542(9) 0.4236(10) 0.115(4) Uani 1 1 d . . . C14 C 0.5912(10) 0.2209(10) 0.3719(11) 0.109(4) Uani 1 1 d U . . H14A H 0.5730 0.2583 0.3026 0.164 Uiso 1 1 d . . . H14B H 0.6030 0.1553 0.3649 0.164 Uiso 1 1 d . . . H14C H 0.6641 0.2556 0.4248 0.164 Uiso 1 1 d . . . C20 C 0.0154(9) -0.0041(9) 0.0052(10) 0.0242(18) Uiso 0.50 1 d PD B -1 H20A H 0.0000 -0.0053 0.0710 0.036 Uiso 0.50 1 calc PR B -1 H20B H 0.0984 0.0172 0.0216 0.036 Uiso 0.50 1 calc PR B -1 H20C H 0.0025 -0.0704 -0.0267 0.036 Uiso 0.50 1 calc PR B -1 H10B H 0.3752 0.1477 0.6271 0.148 Uiso 1 1 d D . . H10A H 0.2773 0.0909 0.6264 0.047 Uiso 1 1 d D . . C21 C -0.1992(10) 0.2231(8) -0.2339(7) 0.045(3) Uani 0.50 1 d PD C 2 C22 C -0.220(3) 0.2942(13) -0.3277(14) 0.059(7) Uani 0.50 1 d PD C 2 H22A H -0.3054 0.3075 -0.3634 0.088 Uiso 0.50 1 calc PR C 2 H22B H -0.1903 0.2640 -0.3787 0.088 Uiso 0.50 1 calc PR C 2 H22C H -0.1760 0.3564 -0.3007 0.088 Uiso 0.50 1 calc PR C 2 C23 C -0.2870(4) 0.3129(11) -0.2304(12) 0.083(7) Uani 0.50 1 d PD D 1 C24 C -0.237(3) 0.294(2) -0.3173(17) 0.087(13) Uani 0.50 1 d PD D 1 H24A H -0.2536 0.3512 -0.3651 0.130 Uiso 0.50 1 calc PR D 1 H24B H -0.2749 0.2348 -0.3583 0.130 Uiso 0.50 1 calc PR D 1 H24C H -0.1500 0.2847 -0.2836 0.130 Uiso 0.50 1 calc PR D 1 H9OA H 0.2408(7) 0.250(5) 0.415(2) 0.05(2) Uiso 1 1 d D . . H9OB H 0.2275(10) 0.201(5) 0.501(3) 0.06(2) Uiso 1 1 d D . . O12 O 0.3957(12) 0.4032(14) 0.6650(19) 0.152(10) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01523(11) 0.01351(10) 0.01145(10) 0.00249(7) 0.00722(7) 0.00024(7) Mn1 0.0127(3) 0.0132(3) 0.0113(3) 0.0025(2) 0.0076(2) 0.0017(2) O1 0.0152(13) 0.0136(13) 0.0122(13) 0.0012(10) 0.0077(11) 0.0016(10) O2 0.0212(15) 0.0148(13) 0.0140(13) 0.0020(11) 0.0085(12) -0.0015(11) O3 0.0153(14) 0.0207(14) 0.0173(14) 0.0065(11) 0.0092(11) 0.0031(11) O4 0.0216(15) 0.0260(16) 0.0209(15) 0.0093(12) 0.0142(13) 0.0033(12) O5 0.0171(14) 0.0255(15) 0.0135(14) 0.0033(11) 0.0084(11) -0.0025(12) O6 0.0187(14) 0.0203(14) 0.0115(13) 0.0035(11) 0.0054(11) 0.0000(11) O7 0.0197(14) 0.0156(13) 0.0163(14) 0.0037(11) 0.0114(12) 0.0026(11) O10 0.0258(18) 0.0289(18) 0.039(2) -0.0024(15) 0.0127(16) 0.0016(14) O8 0.0279(16) 0.0126(13) 0.0203(15) 0.0023(11) 0.0131(13) 0.0008(12) O9 0.0232(16) 0.0253(16) 0.0226(16) 0.0010(13) 0.0098(13) -0.0057(13) N1 0.0179(17) 0.0144(16) 0.0147(16) 0.0020(12) 0.0094(13) 0.0016(13) N2 0.065(4) 0.045(3) 0.019(2) 0.004(2) -0.002(2) -0.020(3) N3 0.036(2) 0.0172(18) 0.025(2) 0.0017(15) 0.0145(18) 0.0006(16) N4 0.0159(16) 0.0190(17) 0.0111(15) 0.0005(13) 0.0064(13) -0.0010(13) N5 0.035(3) 0.062(3) 0.059(3) 0.027(3) 0.033(3) 0.024(3) N6 0.026(2) 0.035(2) 0.024(2) 0.0121(17) 0.0177(17) 0.0071(17) N7 0.0148(16) 0.0186(16) 0.0131(16) 0.0005(13) 0.0076(13) 0.0003(13) N8 0.023(2) 0.083(4) 0.020(2) 0.000(2) 0.0051(18) -0.017(2) N9 0.025(2) 0.075(4) 0.0130(19) 0.005(2) 0.0060(17) -0.018(2) N10 0.0172(17) 0.0167(16) 0.0115(15) 0.0051(12) 0.0048(13) 0.0000(13) N11 0.069(4) 0.029(2) 0.049(3) 0.010(2) 0.040(3) 0.017(2) N12 0.049(3) 0.0166(18) 0.028(2) 0.0056(15) 0.025(2) 0.0045(17) N14 0.114(6) 0.039(3) 0.069(4) 0.023(3) 0.066(4) 0.009(3) N15 0.108(10) 0.117(10) 0.099(9) -0.004(8) 0.052(8) -0.001(8) N17 0.087(10) 0.067(8) 0.035(6) 0.007(6) 0.035(7) -0.019(7) N18 0.110(16) 0.24(3) 0.099(15) 0.098(18) 0.069(14) 0.083(18) C1 0.021(2) 0.0167(19) 0.0156(19) 0.0014(15) 0.0076(16) 0.0019(15) C2 0.036(3) 0.020(2) 0.022(2) 0.0015(17) 0.006(2) -0.0116(19) C3 0.020(2) 0.018(2) 0.018(2) -0.0035(16) 0.0084(16) 0.0006(16) C4 0.0177(19) 0.022(2) 0.0163(19) 0.0034(16) 0.0105(16) 0.0013(16) C5 0.024(2) 0.039(3) 0.030(2) 0.013(2) 0.021(2) 0.006(2) C6 0.019(2) 0.022(2) 0.0169(19) 0.0022(16) 0.0105(16) -0.0007(16) C7 0.0149(19) 0.028(2) 0.0136(19) -0.0019(16) 0.0052(16) -0.0012(16) C8 0.021(2) 0.044(3) 0.0117(19) -0.0009(18) 0.0068(17) -0.006(2) C9 0.018(2) 0.024(2) 0.0137(19) -0.0012(15) 0.0074(16) -0.0009(16) C10 0.021(2) 0.0169(19) 0.020(2) 0.0007(16) 0.0104(17) 0.0027(16) C11 0.038(3) 0.018(2) 0.028(2) 0.0077(18) 0.019(2) 0.0086(19) C12 0.024(2) 0.0153(19) 0.0163(19) 0.0034(15) 0.0065(17) -0.0004(16) C15 0.085(5) 0.041(3) 0.052(4) 0.009(3) 0.046(4) 0.000(3) C16 0.149(10) 0.053(4) 0.051(5) 0.016(4) 0.057(6) 0.001(5) C13 0.074(6) 0.082(6) 0.068(6) 0.000(5) 0.026(5) 0.001(5) C17 0.060(7) 0.071(8) 0.077(8) 0.007(7) 0.028(6) 0.003(6) C18 0.068(8) 0.058(7) 0.094(9) 0.005(7) 0.037(7) 0.007(6) N13 0.074(6) 0.152(10) 0.145(10) -0.024(8) 0.071(7) -0.014(6) C14 0.058(5) 0.130(8) 0.123(8) -0.035(6) 0.016(5) 0.021(5) C21 0.054(8) 0.052(7) 0.041(7) -0.007(6) 0.031(6) -0.008(6) C22 0.100(17) 0.053(12) 0.048(12) 0.009(9) 0.055(13) 0.022(11) C23 0.058(10) 0.059(10) 0.103(16) 0.036(10) -0.001(10) 0.002(8) C24 0.13(3) 0.10(2) 0.033(10) 0.003(12) 0.038(13) -0.057(19) O12 0.036(7) 0.139(15) 0.24(2) 0.112(16) 0.013(10) -0.017(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 Tb1 O1 2.242(3) . ? Tb1 O9 2.376(3) . ? Tb1 O4 2.380(3) . ? Tb1 O8 2.392(3) . ? Tb1 O6 2.399(3) . ? Tb1 O2 2.443(3) . ? Tb1 N7 2.605(3) . ? Tb1 N10 2.615(4) . ? Tb1 N4 2.615(4) . ? Tb1 Mn1 3.5972(6) 2_556 ? Tb1 Mn1 3.6048(6) . ? Mn1 O1 1.855(3) . ? Mn1 O1 1.861(3) 2_556 ? Mn1 O7 1.969(3) 2_556 ? Mn1 O3 1.980(3) . ? Mn1 O5 2.209(3) 2_556 ? Mn1 N1 2.425(4) . ? Mn1 Mn1 2.7871(11) 2_556 ? Mn1 Tb1 3.5972(6) 2_556 ? O1 Mn1 1.861(3) 2_556 ? O2 N1 1.299(4) . ? O3 N4 1.314(4) . ? O4 C6 1.250(5) . ? O5 N7 1.297(4) . ? O5 Mn1 2.209(3) 2_556 ? O6 C9 1.239(5) . ? O7 N10 1.321(4) . ? O7 Mn1 1.969(3) 2_556 ? O8 C12 1.253(5) . ? N1 C1 1.318(5) . ? N2 C2 1.150(7) . ? N3 C3 1.147(6) . ? N4 C4 1.290(5) . ? N5 C5 1.138(7) . ? N6 C6 1.316(6) . ? N7 C7 1.307(5) . ? N8 C8 1.140(7) . ? N9 C9 1.311(6) . ? N10 C10 1.294(6) . ? N11 C11 1.146(7) . ? N12 C12 1.309(6) . ? N14 C15 1.105(8) . ? N15 C17 1.16005(11) . ? N16 C19 1.16003(10) . ? N17 C21 1.16003(11) . ? N18 C23 1.16003(12) . ? C1 C3 1.422(6) . ? C1 C2 1.431(6) . ? C4 C5 1.431(6) . ? C4 C6 1.485(6) . ? C7 C8 1.424(6) . ? C7 C9 1.480(6) . ? C10 C11 1.432(6) . ? C10 C12 1.482(6) . ? C15 C16 1.441(9) . ? C13 N13 1.185(13) . ? C13 C14 1.373(15) . ? C17 C18 1.54005(11) . ? C19 C20 1.54003(11) . ? C21 C22 1.54003(11) . ? C23 C24 1.54003(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O9 77.77(11) . . ? O1 Tb1 O4 131.64(10) . . ? O9 Tb1 O4 79.95(11) . . ? O1 Tb1 O8 128.15(10) . . ? O9 Tb1 O8 74.81(11) . . ? O4 Tb1 O8 85.15(11) . . ? O1 Tb1 O6 137.74(10) . . ? O9 Tb1 O6 142.64(11) . . ? O4 Tb1 O6 80.06(11) . . ? O8 Tb1 O6 72.32(10) . . ? O1 Tb1 O2 81.26(10) . . ? O9 Tb1 O2 138.07(10) . . ? O4 Tb1 O2 87.74(11) . . ? O8 Tb1 O2 144.17(10) . . ? O6 Tb1 O2 71.87(10) . . ? O1 Tb1 N7 75.75(10) . . ? O9 Tb1 N7 140.98(11) . . ? O4 Tb1 N7 138.87(11) . . ? O8 Tb1 N7 100.15(11) . . ? O6 Tb1 N7 63.43(10) . . ? O2 Tb1 N7 64.20(10) . . ? O1 Tb1 N10 67.95(10) . . ? O9 Tb1 N10 77.15(11) . . ? O4 Tb1 N10 145.01(11) . . ? O8 Tb1 N10 63.54(10) . . ? O6 Tb1 N10 103.04(10) . . ? O2 Tb1 N10 126.70(10) . . ? N7 Tb1 N10 66.58(11) . . ? O1 Tb1 N4 69.28(10) . . ? O9 Tb1 N4 73.46(10) . . ? O4 Tb1 N4 63.40(11) . . ? O8 Tb1 N4 138.39(11) . . ? O6 Tb1 N4 123.27(10) . . ? O2 Tb1 N4 65.23(10) . . ? N7 Tb1 N4 121.45(11) . . ? N10 Tb1 N4 132.00(10) . . ? O1 Tb1 Mn1 25.96(7) . 2_556 ? O9 Tb1 Mn1 91.82(8) . 2_556 ? O4 Tb1 Mn1 157.36(8) . 2_556 ? O8 Tb1 Mn1 113.19(7) . 2_556 ? O6 Tb1 Mn1 117.17(7) . 2_556 ? O2 Tb1 Mn1 84.44(7) . 2_556 ? N7 Tb1 Mn1 53.87(8) . 2_556 ? N10 Tb1 Mn1 49.70(7) . 2_556 ? N4 Tb1 Mn1 94.09(8) . 2_556 ? O1 Tb1 Mn1 25.57(7) . . ? O9 Tb1 Mn1 88.46(8) . . ? O4 Tb1 Mn1 112.68(8) . . ? O8 Tb1 Mn1 153.31(7) . . ? O6 Tb1 Mn1 128.46(7) . . ? O2 Tb1 Mn1 59.71(7) . . ? N7 Tb1 Mn1 79.73(8) . . ? N10 Tb1 Mn1 92.85(7) . . ? N4 Tb1 Mn1 49.84(8) . . ? Mn1 Tb1 Mn1 45.534(17) 2_556 . ? O1 Mn1 O1 82.82(13) . 2_556 ? O1 Mn1 O7 172.95(13) . 2_556 ? O1 Mn1 O7 93.05(12) 2_556 2_556 ? O1 Mn1 O3 93.83(12) . . ? O1 Mn1 O3 176.29(13) 2_556 . ? O7 Mn1 O3 90.44(12) 2_556 . ? O1 Mn1 O5 99.33(12) . 2_556 ? O1 Mn1 O5 94.39(12) 2_556 2_556 ? O7 Mn1 O5 86.65(12) 2_556 2_556 ? O3 Mn1 O5 84.54(12) . 2_556 ? O1 Mn1 N1 87.34(12) . . ? O1 Mn1 N1 98.54(12) 2_556 . ? O7 Mn1 N1 87.63(12) 2_556 . ? O3 Mn1 N1 82.86(12) . . ? O5 Mn1 N1 166.11(12) 2_556 . ? O1 Mn1 Mn1 41.50(9) . 2_556 ? O1 Mn1 Mn1 41.32(9) 2_556 2_556 ? O7 Mn1 Mn1 134.11(9) 2_556 2_556 ? O3 Mn1 Mn1 135.31(9) . 2_556 ? O5 Mn1 Mn1 99.15(9) 2_556 2_556 ? N1 Mn1 Mn1 93.92(9) . 2_556 ? O1 Mn1 Tb1 105.94(9) . 2_556 ? O1 Mn1 Tb1 31.83(9) 2_556 2_556 ? O7 Mn1 Tb1 72.54(8) 2_556 2_556 ? O3 Mn1 Tb1 149.32(9) . 2_556 ? O5 Mn1 Tb1 69.50(8) 2_556 2_556 ? N1 Mn1 Tb1 120.55(8) . 2_556 ? Mn1 Mn1 Tb1 67.38(2) 2_556 2_556 ? O1 Mn1 Tb1 31.45(8) . . ? O1 Mn1 Tb1 105.50(9) 2_556 . ? O7 Mn1 Tb1 146.88(9) 2_556 . ? O3 Mn1 Tb1 72.03(9) . . ? O5 Mn1 Tb1 118.19(8) 2_556 . ? N1 Mn1 Tb1 62.98(8) . . ? Mn1 Mn1 Tb1 67.09(2) 2_556 . ? Tb1 Mn1 Tb1 134.466(17) 2_556 . ? Mn1 O1 Mn1 97.18(13) . 2_556 ? Mn1 O1 Tb1 122.98(13) . . ? Mn1 O1 Tb1 122.21(14) 2_556 . ? N1 O2 Tb1 121.0(2) . . ? N4 O3 Mn1 112.9(2) . . ? C6 O4 Tb1 125.4(3) . . ? N7 O5 Mn1 111.7(2) . 2_556 ? C9 O6 Tb1 124.9(3) . . ? N10 O7 Mn1 112.5(2) . 2_556 ? C12 O8 Tb1 124.9(3) . . ? O2 N1 C1 115.0(3) . . ? O2 N1 Mn1 113.4(2) . . ? C1 N1 Mn1 131.6(3) . . ? C4 N4 O3 117.6(4) . . ? C4 N4 Tb1 117.3(3) . . ? O3 N4 Tb1 125.0(2) . . ? O5 N7 C7 118.2(4) . . ? O5 N7 Tb1 124.1(2) . . ? C7 N7 Tb1 117.1(3) . . ? C10 N10 O7 117.6(4) . . ? C10 N10 Tb1 117.1(3) . . ? O7 N10 Tb1 125.2(2) . . ? N1 C1 C3 120.2(4) . . ? N1 C1 C2 121.4(4) . . ? C3 C1 C2 118.3(4) . . ? N2 C2 C1 179.8(7) . . ? N3 C3 C1 175.4(5) . . ? N4 C4 C5 123.1(4) . . ? N4 C4 C6 114.9(4) . . ? C5 C4 C6 121.8(4) . . ? N5 C5 C4 177.8(5) . . ? O4 C6 N6 122.7(4) . . ? O4 C6 C4 118.9(4) . . ? N6 C6 C4 118.4(4) . . ? N7 C7 C8 121.3(4) . . ? N7 C7 C9 114.9(4) . . ? C8 C7 C9 123.7(4) . . ? N8 C8 C7 178.3(5) . . ? O6 C9 N9 122.4(4) . . ? O6 C9 C7 119.1(4) . . ? N9 C9 C7 118.4(4) . . ? N10 C10 C11 122.4(4) . . ? N10 C10 C12 115.4(4) . . ? C11 C10 C12 122.2(4) . . ? N11 C11 C10 178.6(6) . . ? O8 C12 N12 123.1(4) . . ? O8 C12 C10 118.9(4) . . ? N12 C12 C10 118.0(4) . . ? N14 C15 C16 179.1(11) . . ? N13 C13 C14 176.7(12) . . ? N15 C17 C18 178.8(7) . . ? N16 C19 C20 179.0(6) . . ? N17 C21 C22 179.1(9) . . ? N18 C23 C24 179.0(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6A N2 0.88 2.22 3.013(6) 149.6 2 N12 H12A N14 0.88 2.11 2.974(7) 168.0 . N12 H12B N3 0.88 2.22 2.956(6) 140.6 1_565 N9 H9A N17 0.88 2.20 3.061(10) 167.2 . N9 H9B N8 0.88 2.31 3.096(7) 148.0 2_455 O9 H9OB O10 0.86 1.880(6) 2.739(5) 177(8) . O9 H9OA N13 0.86 2.032(14) 2.804(9) 148.8(19) . O10 H10A O5 0.86 2.02 2.852(3) 161.9 2_556 O10 H10B N5 0.86 2.14 2.943(5) 155.1 2_656 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.516 _refine_diff_density_min -1.626 _refine_diff_density_rms 0.167