Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Lanthanide-3d Cyanometalate Chains with the Tridentate Ligand 2,4,6-tri(2-pyridyl)-1,3,5-triazine (tptz): Evidence for Ferromagnetic Interactions for the Sm(III)-M(III) compounds (M = Fe, Cr) ; _publ_contact_author_name 'Prof. Kim Dunbar' _publ_contact_author_email DUNBAR@MAIL.CHEM.TAMU.EDU loop_ _publ_author_name 'Hanhua Zhao.' 'Nazario Lopez' 'Andrey Prosvirin' 'Helen Chifotides' 'Kim R. Dunbar' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 296493' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-iron(iii)-praseodimiun(iii) octahydrate ; _chemical_formula_moiety '[Pr(tptz)(H2O)4Fe(CN)6]8H2O' _chemical_formula_sum 'C24 H36 Fe N12 O12 Pr' _chemical_formula_weight 881.41 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.036(3) _cell_length_b 14.195(3) _cell_length_c 31.549(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.22(3) _cell_angle_gamma 90.00 _cell_volume 6991(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 934 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 1.867 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20562 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7923 _reflns_number_gt 6579 _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^)+(0.0528P)^2^+64.4429P] 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 0.0000(15) _refine_ls_number_reflns 7923 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.760 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.464368(18) 0.30786(2) 0.103496(10) 0.01825(10) Uani 1 1 d . . . Fe1 Fe 0.75690(5) 0.49533(6) 0.10842(2) 0.01847(18) Uani 1 1 d . . . N9 N 0.5338(3) 0.2096(3) 0.17462(16) 0.0238(10) Uani 1 1 d . . . N8 N 0.5231(3) 0.4009(3) 0.17670(14) 0.0186(9) Uani 1 1 d . . . C1 C 0.6773(3) 0.3992(4) 0.11630(17) 0.0202(11) Uani 1 1 d . . . N10 N 0.5615(3) 0.5445(3) 0.21320(15) 0.0225(10) Uani 1 1 d . . . C14 C 0.5675(4) 0.3567(4) 0.21270(18) 0.0203(11) Uani 1 1 d . . . C15 C 0.5711(4) 0.2530(4) 0.2125(2) 0.0256(13) Uani 1 1 d . . . C2 C 0.8317(4) 0.5958(4) 0.10044(18) 0.0232(12) Uani 1 1 d . . . N11 N 0.6104(3) 0.4013(3) 0.24816(15) 0.0229(10) Uani 1 1 d . . . C12 C 0.5231(3) 0.4948(4) 0.17879(18) 0.0204(11) Uani 1 1 d . . . N1 N 0.6251(3) 0.3450(4) 0.11855(16) 0.0244(11) Uani 1 1 d . . . C16 C 0.6110(4) 0.2038(5) 0.2497(3) 0.0414(18) Uani 1 1 d . . . H16 H 0.6364 0.2361 0.2758 0.050 Uiso 1 1 calc R . . N7 N 0.4451(3) 0.4956(4) 0.10402(16) 0.0271(11) Uani 1 1 d . . . C3 C 0.6646(4) 0.5513(5) 0.06538(19) 0.0270(13) Uani 1 1 d . . . C4 C 0.7883(4) 0.4214(5) 0.0628(2) 0.0297(13) Uani 1 1 d . . . C13 C 0.6054(4) 0.4945(4) 0.24692(18) 0.0221(12) Uani 1 1 d . . . C19 C 0.5377(4) 0.1150(5) 0.1744(2) 0.0348(15) Uani 1 1 d . . . H19 H 0.5127 0.0830 0.1481 0.042 Uiso 1 1 calc R . . C6 C 0.7259(4) 0.5767(5) 0.15177(19) 0.0307(14) Uani 1 1 d . . . C20 C 0.6553(4) 0.5487(5) 0.28433(19) 0.0269(13) Uani 1 1 d . . . C10 C 0.4721(4) 0.6440(5) 0.1406(2) 0.0364(16) Uani 1 1 d . . . H10 H 0.4965 0.6784 0.1663 0.044 Uiso 1 1 calc R . . C5 C 0.8493(4) 0.4377(5) 0.1511(2) 0.0301(14) Uani 1 1 d . . . C11 C 0.4785(4) 0.5472(4) 0.13958(19) 0.0226(12) Uani 1 1 d . . . C18 C 0.5757(5) 0.0615(5) 0.2100(3) 0.055(2) Uani 1 1 d . . . H18 H 0.5762 -0.0053 0.2084 0.066 Uiso 1 1 calc R . . C9 C 0.4291(5) 0.6898(5) 0.1031(3) 0.050(2) Uani 1 1 d . . . H9 H 0.4234 0.7564 0.1027 0.060 Uiso 1 1 calc R . . C17 C 0.6126(5) 0.1069(6) 0.2477(3) 0.062(3) Uani 1 1 d . . . H17 H 0.6396 0.0716 0.2726 0.074 Uiso 1 1 calc R . . C8 C 0.3952(5) 0.6378(6) 0.0669(3) 0.049(2) Uani 1 1 d . . . H8 H 0.3653 0.6678 0.0409 0.059 Uiso 1 1 calc R . . C7 C 0.4049(4) 0.5420(5) 0.0684(2) 0.0375(16) Uani 1 1 d . . . H7 H 0.3818 0.5067 0.0428 0.045 Uiso 1 1 calc R . . O1 O 0.3368(3) 0.3315(4) 0.04241(18) 0.0496(14) Uani 1 1 d . . . O2 O 0.5318(4) 0.1768(4) 0.07126(19) 0.0522(15) Uani 1 1 d . . . O3 O 0.3459(3) 0.3314(4) 0.14254(16) 0.0396(12) Uani 1 1 d . . . N2 N 0.8750(3) 0.6591(4) 0.09747(17) 0.0318(12) Uani 1 1 d . . . N4 N 0.8061(5) 0.3776(5) 0.0357(2) 0.0516(17) Uani 1 1 d . . . N3 N 0.6094(4) 0.5827(5) 0.03983(19) 0.0475(16) Uani 1 1 d . . . O4 O 0.5054(3) 0.3678(5) 0.03544(15) 0.0595(18) Uani 1 1 d . . . N12 N 0.6900(4) 0.4991(5) 0.32143(18) 0.0397(14) Uani 1 1 d . . . N5 N 0.9038(4) 0.4028(5) 0.1758(2) 0.0503(17) Uani 1 1 d . . . C22 C 0.7177(5) 0.6939(6) 0.3155(2) 0.0441(18) Uani 1 1 d . . . H22 H 0.7264 0.7600 0.3141 0.053 Uiso 1 1 calc R . . C24 C 0.7380(5) 0.5475(6) 0.3539(2) 0.0428(18) Uani 1 1 d . . . H24 H 0.7623 0.5147 0.3801 0.051 Uiso 1 1 calc R . . C21 C 0.6671(4) 0.6450(5) 0.2808(2) 0.0321(14) Uani 1 1 d . . . H21 H 0.6408 0.6773 0.2548 0.039 Uiso 1 1 calc R . . C23 C 0.7549(5) 0.6425(6) 0.3522(2) 0.0456(19) Uani 1 1 d . . . H23 H 0.7919 0.6726 0.3762 0.055 Uiso 1 1 calc R . . N6 N 0.7090(4) 0.6320(6) 0.1753(2) 0.0558(19) Uani 1 1 d . . . O6 O 0.6610(4) 0.2236(4) 0.03475(19) 0.0603(17) Uani 1 1 d . . . O5 O 0.1693(6) 0.3013(8) 0.0270(6) 0.194(7) Uani 1 1 d . . . O11 O 0.4183(8) 0.0456(8) 0.0081(3) 0.145(4) Uani 1 1 d . . . O7 O 0.5385(9) 0.8190(10) 0.2382(6) 0.203(7) Uani 1 1 d . . . O10 O 0.6681(7) 0.7812(9) 0.1028(7) 0.218(8) Uani 1 1 d . . . O8 O 0.6781(9) 0.8231(7) 0.1999(4) 0.172(6) Uani 1 1 d . . . O9 O 0.5700(10) 0.8840(10) 0.1375(6) 0.218(7) Uani 1 1 d . . . O12 O 0.5144(14) -0.0148(15) 0.0642(7) 0.281(9) Uiso 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 Pr1 0.01490(15) 0.02140(16) 0.01796(16) -0.00157(12) 0.00274(11) -0.00531(12) Fe1 0.0158(4) 0.0240(4) 0.0151(4) 0.0007(3) 0.0025(3) -0.0074(3) N9 0.020(2) 0.018(3) 0.032(3) 0.004(2) 0.004(2) -0.0047(19) N8 0.018(2) 0.024(3) 0.014(2) 0.0004(18) 0.0028(18) -0.0042(18) C1 0.015(3) 0.028(3) 0.015(3) 0.002(2) -0.001(2) -0.005(2) N10 0.022(2) 0.024(3) 0.022(2) -0.0021(19) 0.007(2) -0.003(2) C14 0.022(3) 0.020(3) 0.019(3) 0.005(2) 0.005(2) -0.004(2) C15 0.024(3) 0.021(3) 0.029(3) 0.008(2) 0.001(2) -0.008(2) C2 0.024(3) 0.027(3) 0.017(3) -0.005(2) 0.004(2) -0.012(2) N11 0.022(2) 0.026(3) 0.020(2) -0.0028(19) 0.0021(19) -0.005(2) C12 0.018(3) 0.022(3) 0.022(3) 0.002(2) 0.006(2) -0.002(2) N1 0.020(2) 0.027(3) 0.024(3) 0.007(2) 0.000(2) -0.005(2) C16 0.036(4) 0.031(4) 0.046(4) 0.014(3) -0.013(3) -0.010(3) N7 0.025(3) 0.029(3) 0.025(3) 0.008(2) 0.002(2) 0.006(2) C3 0.026(3) 0.033(3) 0.021(3) 0.000(2) 0.004(2) -0.007(3) C4 0.032(3) 0.030(3) 0.026(3) 0.001(3) 0.005(3) -0.006(3) C13 0.018(3) 0.028(3) 0.021(3) -0.006(2) 0.006(2) -0.006(2) C19 0.030(3) 0.022(3) 0.051(4) 0.003(3) 0.006(3) -0.005(3) C6 0.022(3) 0.051(4) 0.018(3) -0.001(3) 0.002(2) -0.008(3) C20 0.020(3) 0.037(4) 0.025(3) -0.012(3) 0.007(2) -0.008(2) C10 0.035(4) 0.022(3) 0.047(4) 0.004(3) -0.002(3) 0.001(3) C5 0.023(3) 0.034(4) 0.029(3) 0.004(3) -0.002(3) -0.008(3) C11 0.022(3) 0.020(3) 0.025(3) 0.004(2) 0.005(2) -0.004(2) C18 0.038(4) 0.018(4) 0.095(7) 0.014(4) -0.014(4) -0.005(3) C9 0.042(4) 0.029(4) 0.074(6) 0.019(4) 0.001(4) 0.000(3) C17 0.046(5) 0.037(4) 0.082(6) 0.028(4) -0.030(4) -0.013(4) C8 0.046(4) 0.046(5) 0.046(4) 0.030(4) -0.009(4) 0.003(4) C7 0.039(4) 0.041(4) 0.029(3) 0.013(3) -0.001(3) 0.002(3) O1 0.032(3) 0.048(3) 0.055(3) 0.008(3) -0.019(2) -0.007(2) O2 0.053(3) 0.051(3) 0.066(4) -0.026(3) 0.040(3) -0.016(3) O3 0.024(2) 0.051(3) 0.046(3) -0.019(2) 0.014(2) -0.008(2) N2 0.030(3) 0.038(3) 0.029(3) -0.007(2) 0.010(2) -0.016(2) N4 0.065(5) 0.052(4) 0.042(4) -0.011(3) 0.020(3) 0.002(4) N3 0.044(4) 0.064(5) 0.030(3) 0.006(3) 0.000(3) 0.011(3) O4 0.031(3) 0.122(6) 0.025(3) 0.031(3) 0.005(2) 0.015(3) N12 0.036(3) 0.056(4) 0.025(3) -0.006(3) 0.001(2) -0.008(3) N5 0.040(4) 0.043(4) 0.055(4) 0.011(3) -0.016(3) -0.012(3) C22 0.043(4) 0.041(4) 0.046(4) -0.023(4) 0.007(3) -0.011(3) C24 0.036(4) 0.058(5) 0.030(4) -0.015(3) 0.000(3) -0.005(3) C21 0.036(4) 0.032(4) 0.029(3) -0.007(3) 0.007(3) -0.006(3) C23 0.036(4) 0.056(5) 0.041(4) -0.023(4) -0.001(3) -0.005(4) N6 0.044(4) 0.086(6) 0.036(4) -0.023(4) 0.007(3) 0.004(4) O6 0.064(4) 0.070(4) 0.062(4) -0.026(3) 0.044(3) -0.022(3) O5 0.066(6) 0.145(11) 0.324(19) 0.070(11) -0.052(9) -0.041(6) O11 0.215(12) 0.132(9) 0.123(8) -0.024(7) 0.109(9) 0.003(8) O7 0.186(17) 0.168(12) 0.238(19) 0.012(11) 0.011(13) 0.063(10) O10 0.087(8) 0.109(9) 0.45(3) -0.071(13) 0.037(11) -0.003(7) O8 0.260(15) 0.088(7) 0.232(13) 0.054(8) 0.185(12) 0.054(8) O9 0.197(14) 0.121(11) 0.31(2) -0.046(12) 0.012(14) -0.029(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O2 2.484(5) . ? Pr1 O1 2.492(5) . ? Pr1 O3 2.512(4) . ? Pr1 O4 2.533(5) . ? Pr1 N2 2.535(5) 3_445 ? Pr1 N1 2.566(5) . ? Pr1 N8 2.640(4) . ? Pr1 N9 2.660(5) . ? Pr1 N7 2.683(5) . ? Fe1 C2 1.917(6) . ? Fe1 C1 1.923(6) . ? Fe1 C3 1.935(6) . ? Fe1 C4 1.938(7) . ? Fe1 C5 1.941(6) . ? Fe1 C6 1.939(7) . ? N9 C19 1.345(8) . ? N9 C15 1.356(8) . ? N8 C12 1.335(7) . ? N8 C14 1.349(7) . ? C1 N1 1.151(7) . ? N10 C12 1.323(7) . ? N10 C13 1.337(8) . ? C14 N11 1.332(7) . ? C14 C15 1.473(8) . ? C15 C16 1.390(9) . ? C2 N2 1.151(7) . ? N11 C13 1.325(8) . ? C12 C11 1.480(8) . ? C16 C17 1.377(10) . ? N7 C7 1.335(8) . ? N7 C11 1.344(8) . ? C3 N3 1.143(8) . ? C4 N4 1.144(9) . ? C13 C20 1.481(8) . ? C19 C18 1.377(10) . ? C6 N6 1.154(9) . ? C20 N12 1.371(9) . ? C20 C21 1.388(9) . ? C10 C11 1.379(8) . ? C10 C9 1.388(10) . ? C5 N5 1.142(8) . ? C18 C17 1.361(12) . ? C9 C8 1.365(12) . ? C8 C7 1.368(11) . ? N2 Pr1 2.535(5) 3 ? N12 C24 1.325(8) . ? C22 C23 1.384(11) . ? C22 C21 1.391(9) . ? C24 C23 1.379(11) . ? O7 O7 1.58(3) 2_655 ? 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 O2 Pr1 O1 98.2(2) . . ? O2 Pr1 O3 138.52(16) . . ? O1 Pr1 O3 77.40(18) . . ? O2 Pr1 O4 71.5(2) . . ? O1 Pr1 O4 68.03(17) . . ? O3 Pr1 O4 138.03(17) . . ? O2 Pr1 N2 68.70(17) . 3_445 ? O1 Pr1 N2 72.79(18) . 3_445 ? O3 Pr1 N2 70.68(17) . 3_445 ? O4 Pr1 N2 117.9(2) . 3_445 ? O2 Pr1 N1 73.55(17) . . ? O1 Pr1 N1 136.70(17) . . ? O3 Pr1 N1 136.24(15) . . ? O4 Pr1 N1 69.09(16) . . ? N2 Pr1 N1 135.37(18) 3_445 . ? O2 Pr1 N8 129.15(18) . . ? O1 Pr1 N8 132.42(17) . . ? O3 Pr1 N8 70.32(14) . . ? O4 Pr1 N8 117.61(18) . . ? N2 Pr1 N8 124.40(15) 3_445 . ? N1 Pr1 N8 65.99(15) . . ? O2 Pr1 N9 79.34(18) . . ? O1 Pr1 N9 146.53(16) . . ? O3 Pr1 N9 82.74(16) . . ? O4 Pr1 N9 138.72(15) . . ? N2 Pr1 N9 75.34(16) 3_445 . ? N1 Pr1 N9 75.09(15) . . ? N8 Pr1 N9 61.82(15) . . ? O2 Pr1 N7 143.92(17) . . ? O1 Pr1 N7 78.19(16) . . ? O3 Pr1 N7 76.34(16) . . ? O4 Pr1 N7 73.98(19) . . ? N2 Pr1 N7 139.80(17) 3_445 . ? N1 Pr1 N7 84.68(16) . . ? N8 Pr1 N7 61.07(15) . . ? N9 Pr1 N7 122.83(15) . . ? C2 Fe1 C1 177.1(3) . . ? C2 Fe1 C3 90.2(3) . . ? C1 Fe1 C3 87.6(2) . . ? C2 Fe1 C4 91.6(3) . . ? C1 Fe1 C4 90.3(3) . . ? C3 Fe1 C4 89.3(3) . . ? C2 Fe1 C5 90.2(3) . . ? C1 Fe1 C5 92.0(2) . . ? C3 Fe1 C5 179.2(3) . . ? C4 Fe1 C5 90.0(3) . . ? C2 Fe1 C6 85.3(3) . . ? C1 Fe1 C6 92.7(3) . . ? C3 Fe1 C6 88.4(3) . . ? C4 Fe1 C6 176.2(3) . . ? C5 Fe1 C6 92.3(3) . . ? C19 N9 C15 116.5(5) . . ? C19 N9 Pr1 122.1(4) . . ? C15 N9 Pr1 121.4(4) . . ? C12 N8 C14 115.4(5) . . ? C12 N8 Pr1 122.6(4) . . ? C14 N8 Pr1 121.2(4) . . ? N1 C1 Fe1 174.8(5) . . ? C12 N10 C13 115.6(5) . . ? N11 C14 N8 123.9(5) . . ? N11 C14 C15 117.8(5) . . ? N8 C14 C15 118.3(5) . . ? N9 C15 C16 122.8(6) . . ? N9 C15 C14 116.6(5) . . ? C16 C15 C14 120.6(6) . . ? N2 C2 Fe1 176.0(5) . . ? C13 N11 C14 115.7(5) . . ? N10 C12 N8 124.6(5) . . ? N10 C12 C11 117.6(5) . . ? N8 C12 C11 117.7(5) . . ? C1 N1 Pr1 147.1(4) . . ? C17 C16 C15 118.2(7) . . ? C7 N7 C11 117.2(6) . . ? C7 N7 Pr1 121.3(5) . . ? C11 N7 Pr1 121.4(4) . . ? N3 C3 Fe1 178.7(7) . . ? N4 C4 Fe1 179.4(7) . . ? N11 C13 N10 124.8(5) . . ? N11 C13 C20 118.5(5) . . ? N10 C13 C20 116.6(5) . . ? N9 C19 C18 124.0(7) . . ? N6 C6 Fe1 173.7(7) . . ? N12 C20 C21 122.6(6) . . ? N12 C20 C13 116.9(6) . . ? C21 C20 C13 120.4(6) . . ? C11 C10 C9 118.1(7) . . ? N5 C5 Fe1 179.0(7) . . ? N7 C11 C10 123.1(6) . . ? N7 C11 C12 116.6(5) . . ? C10 C11 C12 120.3(6) . . ? C17 C18 C19 118.3(7) . . ? C8 C9 C10 119.1(7) . . ? C18 C17 C16 120.3(7) . . ? C9 C8 C7 119.2(7) . . ? N7 C7 C8 123.3(7) . . ? C2 N2 Pr1 169.9(5) . 3 ? C24 N12 C20 116.4(7) . . ? C23 C22 C21 117.3(7) . . ? N12 C24 C23 124.2(8) . . ? C20 C21 C22 119.6(7) . . ? C22 C23 C24 119.9(7) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.298 _refine_diff_density_min -2.125 _refine_diff_density_rms 0.151 # Attachment 'compound2.txt' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 296494' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-iron(iii)-Neodymium(iii) octahydrate ; _chemical_formula_moiety '[Nd(tptz)(H2O)4Fe(CN)6]8H2O' _chemical_formula_sum 'C24 H36 Fe N12 O12 Nd' _chemical_formula_weight 884.71 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 15.927(3) _cell_length_b 14.139(3) _cell_length_c 31.462(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.18(3) _cell_angle_gamma 90.00 _cell_volume 6898(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 1.985 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19961 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7903 _reflns_number_gt 6564 _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^)+(0.0680P)^2^+105.3367P] 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 0.0000(15) _refine_ls_number_reflns 7903 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 1.259 _refine_ls_shift/su_mean 0.034 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 Nd1 Nd 0.46453(2) 0.30853(3) 0.103806(12) 0.01940(13) Uani 1 1 d . . . Fe1 Fe 0.75698(6) 0.49617(7) 0.10836(3) 0.0195(2) Uani 1 1 d . . . N9 N 0.5343(4) 0.2098(4) 0.1739(2) 0.0256(14) Uani 1 1 d . . . N8 N 0.5232(4) 0.4008(4) 0.17662(19) 0.0195(12) Uani 1 1 d . . . C1 C 0.6765(5) 0.3995(5) 0.1159(2) 0.0227(15) Uani 1 1 d . . . N10 N 0.5612(4) 0.5450(5) 0.2132(2) 0.0259(13) Uani 1 1 d . . . C14 C 0.5676(5) 0.3567(5) 0.2123(2) 0.0220(14) Uani 1 1 d . . . C15 C 0.5710(5) 0.2525(5) 0.2120(3) 0.0273(16) Uani 1 1 d . . . C2 C 0.8319(5) 0.5972(5) 0.1007(2) 0.0256(16) Uani 1 1 d . . . N11 N 0.6102(4) 0.4007(4) 0.2481(2) 0.0248(13) Uani 1 1 d . . . C12 C 0.5231(4) 0.4954(5) 0.1785(2) 0.0200(14) Uani 1 1 d . . . N1 N 0.6246(4) 0.3457(5) 0.1183(2) 0.0250(13) Uani 1 1 d . . . C16 C 0.6107(6) 0.2026(7) 0.2491(3) 0.045(2) Uani 1 1 d . . . H16 H 0.6367 0.2354 0.2751 0.054 Uiso 1 1 calc R . . N7 N 0.4445(4) 0.4951(5) 0.1040(2) 0.0298(15) Uani 1 1 d . . . C3 C 0.6644(5) 0.5523(6) 0.0655(3) 0.0280(16) Uani 1 1 d . . . C4 C 0.7877(5) 0.4218(6) 0.0624(3) 0.0291(16) Uani 1 1 d . . . C13 C 0.6052(5) 0.4943(5) 0.2467(2) 0.0237(15) Uani 1 1 d . . . C19 C 0.5390(5) 0.1147(6) 0.1735(3) 0.038(2) Uani 1 1 d . . . H19 H 0.5160 0.0824 0.1469 0.045 Uiso 1 1 calc R . . C6 C 0.7266(5) 0.5767(7) 0.1519(3) 0.0322(18) Uani 1 1 d . . . C20 C 0.6550(5) 0.5491(6) 0.2842(3) 0.0274(16) Uani 1 1 d . . . C10 C 0.4728(6) 0.6443(6) 0.1402(3) 0.037(2) Uani 1 1 d . . . H10 H 0.4978 0.6788 0.1659 0.045 Uiso 1 1 calc R . . C5 C 0.8504(5) 0.4370(6) 0.1508(3) 0.0328(18) Uani 1 1 d . . . C11 C 0.4786(5) 0.5472(5) 0.1395(3) 0.0237(15) Uani 1 1 d . . . C18 C 0.5752(6) 0.0625(6) 0.2094(4) 0.054(3) Uani 1 1 d . . . H18 H 0.5748 -0.0046 0.2076 0.065 Uiso 1 1 calc R . . C9 C 0.4297(7) 0.6907(7) 0.1027(4) 0.051(3) Uani 1 1 d . . . H9 H 0.4237 0.7575 0.1022 0.061 Uiso 1 1 calc R . . C17 C 0.6122(7) 0.1057(7) 0.2480(4) 0.064(4) Uani 1 1 d . . . H17 H 0.6380 0.0699 0.2731 0.076 Uiso 1 1 calc R . . C8 C 0.3963(7) 0.6378(7) 0.0667(4) 0.053(3) Uani 1 1 d . . . H8 H 0.3669 0.6678 0.0405 0.063 Uiso 1 1 calc R . . C7 C 0.4050(6) 0.5416(7) 0.0682(3) 0.037(2) Uani 1 1 d . . . H7 H 0.3817 0.5062 0.0425 0.044 Uiso 1 1 calc R . . O1 O 0.3366(4) 0.3314(5) 0.0434(2) 0.0497(18) Uani 1 1 d . . . O2 O 0.5317(5) 0.1783(5) 0.0717(3) 0.053(2) Uani 1 1 d . . . O3 O 0.3467(4) 0.3310(5) 0.1426(2) 0.0400(15) Uani 1 1 d . . . N2 N 0.8754(5) 0.6605(5) 0.0979(2) 0.0339(16) Uani 1 1 d . . . N4 N 0.8051(6) 0.3786(6) 0.0354(3) 0.052(2) Uani 1 1 d . . . N3 N 0.6090(6) 0.5847(7) 0.0398(3) 0.051(2) Uani 1 1 d . . . O4 O 0.5050(4) 0.3695(7) 0.0360(2) 0.059(2) Uani 1 1 d . . . N12 N 0.6905(5) 0.4981(7) 0.3212(2) 0.047(2) Uani 1 1 d . . . N5 N 0.9052(5) 0.4024(6) 0.1750(3) 0.052(2) Uani 1 1 d . . . C22 C 0.7174(6) 0.6935(8) 0.3155(3) 0.047(2) Uani 1 1 d . . . H22 H 0.7259 0.7597 0.3138 0.056 Uiso 1 1 calc R . . C24 C 0.7377(6) 0.5481(8) 0.3538(3) 0.043(2) Uani 1 1 d . . . H24 H 0.7618 0.5154 0.3801 0.052 Uiso 1 1 calc R . . C21 C 0.6667(6) 0.6442(6) 0.2807(3) 0.0346(19) Uani 1 1 d . . . H21 H 0.6405 0.6766 0.2545 0.042 Uiso 1 1 calc R . . C23 C 0.7547(6) 0.6433(8) 0.3525(3) 0.048(3) Uani 1 1 d . . . H23 H 0.7914 0.6738 0.3767 0.058 Uiso 1 1 calc R . . N6 N 0.7099(6) 0.6323(7) 0.1757(3) 0.056(2) Uani 1 1 d . . . O6 O 0.6613(5) 0.2236(6) 0.0352(3) 0.059(2) Uani 1 1 d . . . O11 O 0.4173(11) 0.0445(9) 0.0075(5) 0.130(5) Uani 1 1 d . . . O7 O 0.5382(12) 0.8190(12) 0.2389(7) 0.173(7) Uani 1 1 d . . . O10 O 0.6686(8) 0.7811(10) 0.1017(8) 0.179(9) Uani 1 1 d . . . O8 O 0.6796(11) 0.8229(8) 0.2017(5) 0.141(6) Uani 1 1 d . . . O9 O 0.5702(11) 0.8866(11) 0.1369(7) 0.180(8) Uani 1 1 d . . . O12 O 0.517(3) -0.0113(19) 0.0634(13) 0.39(3) Uani 1 1 d . . . O5 O 0.6684(8) 0.8012(11) 0.0255(7) 0.179(8) 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 Nd1 0.01800(19) 0.0210(2) 0.0191(2) -0.00193(15) 0.00402(13) -0.00540(15) Fe1 0.0195(5) 0.0226(5) 0.0162(5) 0.0009(4) 0.0038(4) -0.0071(4) N9 0.025(3) 0.015(3) 0.037(4) 0.001(3) 0.007(3) -0.006(2) N8 0.020(3) 0.019(3) 0.019(3) 0.003(2) 0.005(2) -0.001(2) C1 0.023(4) 0.028(4) 0.017(3) -0.001(3) 0.004(3) -0.004(3) N10 0.029(3) 0.026(3) 0.023(3) -0.005(3) 0.006(3) -0.006(3) C14 0.026(4) 0.016(3) 0.024(4) 0.005(3) 0.006(3) -0.003(3) C15 0.024(4) 0.024(4) 0.031(4) 0.008(3) 0.002(3) -0.008(3) C2 0.025(4) 0.029(4) 0.023(4) -0.002(3) 0.005(3) -0.010(3) N11 0.026(3) 0.026(3) 0.022(3) -0.002(2) 0.006(2) -0.008(3) C12 0.018(3) 0.015(3) 0.027(4) 0.001(3) 0.005(3) -0.005(3) N1 0.021(3) 0.028(3) 0.025(3) 0.008(3) 0.002(2) -0.005(3) C16 0.040(5) 0.035(5) 0.048(6) 0.016(4) -0.014(4) -0.014(4) N7 0.030(4) 0.031(4) 0.028(4) 0.010(3) 0.006(3) 0.010(3) C3 0.031(4) 0.027(4) 0.025(4) -0.005(3) 0.003(3) -0.005(3) C4 0.032(4) 0.028(4) 0.029(4) -0.003(3) 0.011(3) -0.001(3) C13 0.021(4) 0.030(4) 0.021(4) -0.007(3) 0.008(3) -0.009(3) C19 0.026(4) 0.024(4) 0.061(6) 0.001(4) 0.004(4) -0.006(3) C6 0.026(4) 0.046(5) 0.024(4) -0.005(4) 0.004(3) -0.008(4) C20 0.031(4) 0.027(4) 0.026(4) -0.013(3) 0.009(3) -0.009(3) C10 0.035(5) 0.019(4) 0.054(6) 0.007(4) 0.002(4) 0.003(3) C5 0.032(4) 0.033(4) 0.031(4) 0.005(3) 0.002(3) -0.009(3) C11 0.021(4) 0.017(3) 0.032(4) 0.006(3) 0.004(3) 0.001(3) C18 0.038(5) 0.014(4) 0.099(9) 0.014(5) -0.005(5) -0.006(4) C9 0.039(5) 0.033(5) 0.074(8) 0.019(5) -0.001(5) 0.001(4) C17 0.055(6) 0.035(5) 0.079(8) 0.033(5) -0.031(6) -0.010(5) C8 0.052(6) 0.046(6) 0.055(7) 0.034(5) 0.001(5) 0.011(5) C7 0.038(5) 0.042(5) 0.028(4) 0.012(4) 0.002(3) 0.000(4) O1 0.033(3) 0.047(4) 0.055(4) 0.003(3) -0.019(3) -0.006(3) O2 0.059(4) 0.048(4) 0.066(5) -0.026(4) 0.041(4) -0.017(3) O3 0.025(3) 0.050(4) 0.046(4) -0.019(3) 0.011(3) -0.009(3) N2 0.036(4) 0.039(4) 0.028(4) -0.007(3) 0.011(3) -0.013(3) N4 0.064(6) 0.055(5) 0.043(5) -0.006(4) 0.025(4) 0.000(4) N3 0.051(5) 0.065(6) 0.032(4) 0.001(4) 0.000(4) 0.015(4) O4 0.036(4) 0.113(7) 0.028(4) 0.027(4) 0.005(3) 0.015(4) N12 0.039(4) 0.072(6) 0.025(4) -0.005(4) 0.000(3) -0.006(4) N5 0.043(5) 0.043(5) 0.056(5) 0.016(4) -0.016(4) -0.011(4) C22 0.049(6) 0.049(6) 0.043(6) -0.028(5) 0.012(4) -0.013(5) C24 0.038(5) 0.060(6) 0.028(5) -0.013(4) 0.003(4) -0.004(4) C21 0.040(5) 0.028(4) 0.035(5) -0.010(4) 0.009(4) -0.008(4) C23 0.039(5) 0.054(6) 0.050(6) -0.029(5) 0.006(4) -0.014(5) N6 0.047(5) 0.079(7) 0.042(5) -0.026(5) 0.007(4) 0.004(5) O6 0.067(5) 0.064(5) 0.059(5) -0.024(4) 0.045(4) -0.021(4) O11 0.211(15) 0.103(9) 0.109(10) -0.006(7) 0.105(10) 0.027(9) O7 0.164(18) 0.174(15) 0.165(18) 0.001(12) 0.004(13) 0.055(12) O10 0.079(8) 0.093(9) 0.36(3) -0.085(14) 0.034(12) -0.010(7) O8 0.217(16) 0.093(8) 0.158(13) 0.048(8) 0.138(13) 0.051(9) O9 0.152(14) 0.104(11) 0.26(2) -0.030(12) -0.012(13) -0.014(10) O12 0.68(7) 0.20(3) 0.42(5) -0.06(3) 0.40(5) -0.08(3) O5 0.062(8) 0.138(13) 0.30(2) 0.069(12) -0.042(10) -0.032(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 Nd1 O2 2.459(6) . ? Nd1 O1 2.470(6) . ? Nd1 O3 2.481(6) . ? Nd1 N2 2.512(7) 3_445 ? Nd1 O4 2.518(6) . ? Nd1 N1 2.541(6) . ? Nd1 N8 2.616(6) . ? Nd1 N9 2.632(7) . ? Nd1 N7 2.657(7) . ? Fe1 C2 1.911(7) . ? Fe1 C1 1.925(7) . ? Fe1 C6 1.926(9) . ? Fe1 C3 1.927(8) . ? Fe1 C4 1.938(8) . ? Fe1 C5 1.947(9) . ? N9 C19 1.347(10) . ? N9 C15 1.352(10) . ? N8 C14 1.336(9) . ? N8 C12 1.339(9) . ? C1 N1 1.138(9) . ? N10 C12 1.323(9) . ? N10 C13 1.333(10) . ? C14 N11 1.330(9) . ? C14 C15 1.474(10) . ? C15 C16 1.386(11) . ? C2 N2 1.148(10) . ? N11 C13 1.326(10) . ? C12 C11 1.466(10) . ? C16 C17 1.371(13) . ? N7 C7 1.331(10) . ? N7 C11 1.346(10) . ? C3 N3 1.148(11) . ? C4 N4 1.131(11) . ? C13 C20 1.481(10) . ? C19 C18 1.363(14) . ? C6 N6 1.158(11) . ? C20 C21 1.365(11) . ? C20 N12 1.378(12) . ? C10 C11 1.376(10) . ? C10 C9 1.386(13) . ? C5 N5 1.132(11) . ? C18 C17 1.366(16) . ? C9 C8 1.361(16) . ? C8 C7 1.368(14) . ? N2 Nd1 2.512(7) 3 ? N12 C24 1.328(12) . ? C22 C23 1.377(16) . ? C22 C21 1.391(12) . ? C24 C23 1.375(14) . ? O7 O7 1.53(4) 2_655 ? 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 O2 Nd1 O1 98.2(3) . . ? O2 Nd1 O3 138.3(2) . . ? O1 Nd1 O3 77.2(2) . . ? O2 Nd1 N2 68.7(2) . 3_445 ? O1 Nd1 N2 72.5(2) . 3_445 ? O3 Nd1 N2 70.5(2) . 3_445 ? O2 Nd1 O4 71.9(3) . . ? O1 Nd1 O4 68.2(2) . . ? O3 Nd1 O4 137.8(2) . . ? N2 Nd1 O4 118.2(3) 3_445 . ? O2 Nd1 N1 73.5(2) . . ? O1 Nd1 N1 136.8(2) . . ? O3 Nd1 N1 136.5(2) . . ? N2 Nd1 N1 135.5(2) 3_445 . ? O4 Nd1 N1 68.9(2) . . ? O2 Nd1 N8 129.1(2) . . ? O1 Nd1 N8 132.5(2) . . ? O3 Nd1 N8 70.42(19) . . ? N2 Nd1 N8 124.3(2) 3_445 . ? O4 Nd1 N8 117.5(2) . . ? N1 Nd1 N8 66.2(2) . . ? O2 Nd1 N9 78.8(2) . . ? O1 Nd1 N9 146.2(2) . . ? O3 Nd1 N9 83.0(2) . . ? N2 Nd1 N9 75.2(2) 3_445 . ? O4 Nd1 N9 138.6(2) . . ? N1 Nd1 N9 75.19(19) . . ? N8 Nd1 N9 62.14(18) . . ? O2 Nd1 N7 143.9(2) . . ? O1 Nd1 N7 78.0(2) . . ? O3 Nd1 N7 76.5(2) . . ? N2 Nd1 N7 139.6(2) 3_445 . ? O4 Nd1 N7 73.5(3) . . ? N1 Nd1 N7 84.9(2) . . ? N8 Nd1 N7 61.49(19) . . ? N9 Nd1 N7 123.6(2) . . ? C2 Fe1 C1 176.8(3) . . ? C2 Fe1 C6 85.0(3) . . ? C1 Fe1 C6 92.8(3) . . ? C2 Fe1 C3 90.2(3) . . ? C1 Fe1 C3 87.4(3) . . ? C6 Fe1 C3 88.7(3) . . ? C2 Fe1 C4 92.3(3) . . ? C1 Fe1 C4 89.7(3) . . ? C6 Fe1 C4 176.6(4) . . ? C3 Fe1 C4 89.1(3) . . ? C2 Fe1 C5 90.3(3) . . ? C1 Fe1 C5 92.1(3) . . ? C6 Fe1 C5 92.5(4) . . ? C3 Fe1 C5 178.7(4) . . ? C4 Fe1 C5 89.7(4) . . ? C19 N9 C15 116.1(7) . . ? C19 N9 Nd1 122.4(6) . . ? C15 N9 Nd1 121.4(5) . . ? C14 N8 C12 115.8(6) . . ? C14 N8 Nd1 121.2(5) . . ? C12 N8 Nd1 122.2(5) . . ? N1 C1 Fe1 175.2(7) . . ? C12 N10 C13 115.3(6) . . ? N11 C14 N8 124.3(7) . . ? N11 C14 C15 117.4(7) . . ? N8 C14 C15 118.3(7) . . ? N9 C15 C16 122.8(8) . . ? N9 C15 C14 116.3(7) . . ? C16 C15 C14 120.9(8) . . ? N2 C2 Fe1 176.3(7) . . ? C13 N11 C14 115.1(7) . . ? N10 C12 N8 124.1(7) . . ? N10 C12 C11 118.0(6) . . ? N8 C12 C11 117.9(6) . . ? C1 N1 Nd1 147.2(6) . . ? C17 C16 C15 119.6(9) . . ? C7 N7 C11 117.1(7) . . ? C7 N7 Nd1 121.5(6) . . ? C11 N7 Nd1 121.3(5) . . ? N3 C3 Fe1 179.2(8) . . ? N4 C4 Fe1 179.5(10) . . ? N11 C13 N10 125.4(7) . . ? N11 C13 C20 118.6(7) . . ? N10 C13 C20 115.9(7) . . ? N9 C19 C18 123.1(9) . . ? N6 C6 Fe1 173.4(9) . . ? C21 C20 N12 123.2(8) . . ? C21 C20 C13 120.6(8) . . ? N12 C20 C13 116.2(7) . . ? C11 C10 C9 118.7(9) . . ? N5 C5 Fe1 179.1(9) . . ? N7 C11 C10 123.0(7) . . ? N7 C11 C12 116.6(6) . . ? C10 C11 C12 120.5(7) . . ? C19 C18 C17 120.7(9) . . ? C8 C9 C10 118.2(9) . . ? C18 C17 C16 117.6(9) . . ? C9 C8 C7 120.0(9) . . ? N7 C7 C8 123.0(9) . . ? C2 N2 Nd1 170.0(6) . 3 ? C24 N12 C20 115.1(9) . . ? C23 C22 C21 118.0(9) . . ? N12 C24 C23 125.4(10) . . ? C20 C21 C22 119.6(9) . . ? C24 C23 C22 118.6(9) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 2.780 _refine_diff_density_min -2.921 _refine_diff_density_rms 0.195 # Attachment 'compound3.txt' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 296495' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-iron(iii)-samarium(iii) octahydrate ; _chemical_formula_moiety '[Sm(tptz)(H2O)4Fe(CN)6]8H2O' _chemical_formula_sum 'C24 H36 Fe N12 O12 Sm' _chemical_formula_weight 890.85 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 15.897(3) _cell_length_b 14.130(3) _cell_length_c 31.522(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.19(3) _cell_angle_gamma 90.00 _cell_volume 6894(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20560 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7815 _reflns_number_gt 6122 _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^)+(0.0720P)^2^+75.6801P] 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 7815 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.364 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.464487(19) 0.30963(2) 0.104021(10) 0.01888(12) Uani 1 1 d . . . Fe1 Fe 0.75704(5) 0.49743(6) 0.10843(3) 0.0186(2) Uani 1 1 d . . . N9 N 0.5337(3) 0.2093(4) 0.17338(19) 0.0232(11) Uani 1 1 d . . . N8 N 0.5229(3) 0.3999(4) 0.17614(17) 0.0209(11) Uani 1 1 d . . . C1 C 0.6767(4) 0.4004(4) 0.11637(19) 0.0197(12) Uani 1 1 d . . . N10 N 0.5608(3) 0.5456(4) 0.21312(18) 0.0228(11) Uani 1 1 d . . . C14 C 0.5671(4) 0.3564(4) 0.2124(2) 0.0197(12) Uani 1 1 d . . . C15 C 0.5706(4) 0.2520(4) 0.2115(2) 0.0239(13) Uani 1 1 d . . . C2 C 0.8328(4) 0.5987(5) 0.1008(2) 0.0252(14) Uani 1 1 d . . . N11 N 0.6101(4) 0.4004(4) 0.24830(17) 0.0239(11) Uani 1 1 d . . . C12 C 0.5226(4) 0.4956(4) 0.1781(2) 0.0197(12) Uani 1 1 d . . . N1 N 0.6235(3) 0.3467(4) 0.11828(18) 0.0242(11) Uani 1 1 d . . . C16 C 0.6099(5) 0.2021(5) 0.2488(3) 0.039(2) Uani 1 1 d . . . H16 H 0.6350 0.2345 0.2750 0.047 Uiso 1 1 calc R . . N7 N 0.4450(4) 0.4950(4) 0.10336(18) 0.0275(12) Uani 1 1 d . . . C3 C 0.6636(4) 0.5551(5) 0.0657(2) 0.0263(14) Uani 1 1 d . . . C4 C 0.7866(4) 0.4240(5) 0.0617(2) 0.0266(14) Uani 1 1 d . . . C13 C 0.6055(4) 0.4961(5) 0.2468(2) 0.0227(13) Uani 1 1 d . . . C19 C 0.5380(5) 0.1145(5) 0.1723(3) 0.0348(17) Uani 1 1 d . . . H19 H 0.5140 0.0827 0.1458 0.042 Uiso 1 1 calc R . . C6 C 0.7269(4) 0.5779(6) 0.1526(2) 0.0313(16) Uani 1 1 d . . . C20 C 0.6546(4) 0.5495(5) 0.2841(2) 0.0271(14) Uani 1 1 d . . . C10 C 0.4723(5) 0.6450(5) 0.1391(3) 0.0364(17) Uani 1 1 d . . . H10 H 0.4967 0.6801 0.1647 0.044 Uiso 1 1 calc R . . C5 C 0.8513(5) 0.4372(5) 0.1497(2) 0.0301(15) Uani 1 1 d . . . C11 C 0.4781(4) 0.5477(4) 0.1390(2) 0.0244(13) Uani 1 1 d . . . C18 C 0.5761(5) 0.0609(5) 0.2085(3) 0.051(3) Uani 1 1 d . . . H18 H 0.5773 -0.0061 0.2065 0.061 Uiso 1 1 calc R . . C9 C 0.4301(6) 0.6909(5) 0.1013(3) 0.043(2) Uani 1 1 d . . . H9 H 0.4256 0.7580 0.1002 0.051 Uiso 1 1 calc R . . C17 C 0.6117(6) 0.1041(6) 0.2468(4) 0.062(3) Uani 1 1 d . . . H17 H 0.6373 0.0679 0.2719 0.074 Uiso 1 1 calc R . . C8 C 0.3955(5) 0.6374(6) 0.0657(3) 0.044(2) Uani 1 1 d . . . H8 H 0.3658 0.6670 0.0396 0.052 Uiso 1 1 calc R . . C7 C 0.4034(5) 0.5408(5) 0.0675(3) 0.0342(17) Uani 1 1 d . . . H7 H 0.3784 0.5049 0.0423 0.041 Uiso 1 1 calc R . . O1 O 0.3376(4) 0.3314(4) 0.0438(2) 0.0465(15) Uani 1 1 d . . . O2 O 0.5304(4) 0.1815(4) 0.0718(2) 0.0508(17) Uani 1 1 d . . . O3 O 0.3471(3) 0.3311(4) 0.14197(19) 0.0398(13) Uani 1 1 d . . . N2 N 0.8753(4) 0.6622(4) 0.09760(19) 0.0286(13) Uani 1 1 d . . . N4 N 0.8040(5) 0.3806(5) 0.0341(2) 0.0421(16) Uani 1 1 d . . . N3 N 0.6081(5) 0.5881(5) 0.0405(2) 0.0455(17) Uani 1 1 d . . . O4 O 0.5053(4) 0.3697(6) 0.03676(18) 0.060(2) Uani 1 1 d . . . N12 N 0.6893(4) 0.4998(5) 0.32063(19) 0.0326(14) Uani 1 1 d . . . N5 N 0.9069(5) 0.4012(5) 0.1736(3) 0.050(2) Uani 1 1 d . . . C22 C 0.7173(5) 0.6930(6) 0.3163(3) 0.042(2) Uani 1 1 d . . . H22 H 0.7258 0.7594 0.3150 0.050 Uiso 1 1 calc R . . C24 C 0.7392(5) 0.5481(7) 0.3542(3) 0.043(2) Uani 1 1 d . . . H24 H 0.7645 0.5147 0.3802 0.052 Uiso 1 1 calc R . . C21 C 0.6662(5) 0.6457(5) 0.2810(2) 0.0327(16) Uani 1 1 d . . . H21 H 0.6397 0.6792 0.2553 0.039 Uiso 1 1 calc R . . C23 C 0.7548(5) 0.6437(7) 0.3523(3) 0.047(2) Uani 1 1 d . . . H23 H 0.7917 0.6747 0.3762 0.056 Uiso 1 1 calc R . . N6 N 0.7114(5) 0.6337(6) 0.1766(2) 0.053(2) Uani 1 1 d . . . O6 O 0.6618(4) 0.2235(5) 0.0356(2) 0.0525(16) Uani 1 1 d . . . O5 O 0.1659(7) 0.3052(8) 0.0308(8) 0.257(13) Uani 1 1 d . . . O7 O 0.5346(8) 0.8164(8) 0.2397(4) 0.124(4) Uani 1 1 d . . . O10 O 0.6710(6) 0.7799(7) 0.1057(4) 0.098(3) Uani 1 1 d . . . O8 O 0.6811(7) 0.8221(6) 0.2026(3) 0.102(4) Uani 1 1 d . . . O9 O 0.5719(8) 0.8865(8) 0.1353(5) 0.146(5) Uani 1 1 d . . . O11 O 0.0821(8) 0.4564(7) -0.0084(3) 0.109(4) Uani 1 1 d . . . O12 O 0.530(2) -0.0050(17) 0.0696(12) 0.335(15) 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 Sm1 0.01493(18) 0.02112(18) 0.02002(19) -0.00153(12) 0.00278(12) -0.00304(11) Fe1 0.0155(4) 0.0229(4) 0.0165(4) 0.0009(3) 0.0020(3) -0.0054(3) N9 0.016(2) 0.016(2) 0.036(3) 0.005(2) 0.003(2) -0.0028(19) N8 0.021(3) 0.023(3) 0.019(3) 0.000(2) 0.004(2) -0.004(2) C1 0.018(3) 0.028(3) 0.013(3) 0.004(2) 0.002(2) 0.001(2) N10 0.022(3) 0.021(3) 0.026(3) -0.004(2) 0.006(2) -0.005(2) C14 0.020(3) 0.022(3) 0.018(3) 0.003(2) 0.005(2) -0.005(2) C15 0.018(3) 0.019(3) 0.031(4) 0.010(2) -0.003(3) -0.007(2) C2 0.026(3) 0.030(3) 0.017(3) 0.000(2) 0.000(3) -0.007(3) N11 0.026(3) 0.028(3) 0.017(3) 0.000(2) 0.004(2) -0.006(2) C12 0.016(3) 0.017(3) 0.026(3) 0.000(2) 0.005(2) -0.002(2) N1 0.017(3) 0.027(3) 0.026(3) 0.006(2) 0.000(2) -0.006(2) C16 0.031(4) 0.033(4) 0.043(5) 0.021(3) -0.015(3) -0.015(3) N7 0.028(3) 0.031(3) 0.022(3) 0.008(2) 0.002(2) -0.001(2) C3 0.026(3) 0.025(3) 0.027(3) -0.004(3) 0.004(3) -0.003(3) C4 0.024(3) 0.025(3) 0.032(4) 0.005(3) 0.009(3) -0.002(3) C13 0.015(3) 0.032(3) 0.022(3) -0.004(3) 0.007(2) -0.005(2) C19 0.026(3) 0.020(3) 0.057(5) -0.002(3) 0.005(3) -0.004(3) C6 0.020(3) 0.049(4) 0.022(3) -0.005(3) 0.000(3) -0.014(3) C20 0.020(3) 0.037(4) 0.027(4) -0.011(3) 0.010(3) -0.008(3) C10 0.028(4) 0.024(4) 0.052(5) 0.009(3) -0.001(3) -0.002(3) C5 0.029(4) 0.036(4) 0.023(3) 0.008(3) 0.001(3) -0.010(3) C11 0.027(3) 0.020(3) 0.026(3) 0.004(2) 0.003(3) 0.000(2) C18 0.031(4) 0.016(3) 0.093(7) 0.017(4) -0.012(4) -0.003(3) C9 0.037(4) 0.023(4) 0.064(6) 0.024(4) 0.002(4) 0.002(3) C17 0.041(5) 0.039(5) 0.083(7) 0.037(5) -0.034(5) -0.017(4) C8 0.037(4) 0.041(5) 0.050(5) 0.029(4) 0.004(4) 0.004(3) C7 0.028(4) 0.036(4) 0.037(4) 0.019(3) 0.004(3) 0.002(3) O1 0.029(3) 0.043(3) 0.056(4) 0.009(3) -0.015(3) -0.003(2) O2 0.050(4) 0.050(4) 0.064(4) -0.027(3) 0.038(3) -0.015(3) O3 0.021(2) 0.052(3) 0.046(3) -0.020(3) 0.008(2) -0.007(2) N2 0.028(3) 0.033(3) 0.027(3) -0.007(2) 0.010(2) -0.016(2) N4 0.060(4) 0.040(4) 0.032(4) -0.002(3) 0.022(3) 0.008(3) N3 0.043(4) 0.061(5) 0.031(4) 0.002(3) 0.003(3) 0.020(3) O4 0.027(3) 0.124(6) 0.026(3) 0.028(3) 0.002(2) 0.016(3) N12 0.026(3) 0.047(4) 0.025(3) -0.008(3) 0.007(2) -0.006(3) N5 0.042(4) 0.040(4) 0.055(5) 0.022(3) -0.013(3) -0.012(3) C22 0.037(4) 0.047(5) 0.045(5) -0.025(4) 0.018(4) -0.010(3) C24 0.034(4) 0.069(6) 0.023(4) -0.018(4) 0.001(3) -0.004(4) C21 0.031(4) 0.037(4) 0.032(4) -0.012(3) 0.011(3) -0.008(3) C23 0.031(4) 0.066(6) 0.041(5) -0.027(4) 0.004(4) -0.011(4) N6 0.041(4) 0.080(6) 0.037(4) -0.023(4) 0.004(3) -0.002(4) O6 0.060(4) 0.053(4) 0.059(4) -0.020(3) 0.044(3) -0.012(3) O5 0.055(6) 0.100(9) 0.53(3) 0.118(13) -0.109(12) -0.042(6) O7 0.120(11) 0.129(10) 0.122(11) -0.004(7) 0.024(8) 0.021(7) O10 0.067(5) 0.073(5) 0.151(9) -0.019(6) 0.018(6) -0.002(5) O8 0.148(9) 0.076(6) 0.112(8) 0.045(5) 0.095(7) 0.052(6) O9 0.112(9) 0.078(7) 0.227(15) -0.025(8) -0.007(9) -0.018(6) O11 0.179(11) 0.081(6) 0.103(7) -0.020(5) 0.105(8) 0.010(6) O12 0.33(3) 0.19(2) 0.50(5) -0.03(2) 0.14(3) 0.03(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 Sm1 O2 2.428(5) . ? Sm1 O1 2.453(5) . ? Sm1 O3 2.454(5) . ? Sm1 N2 2.501(5) 3_445 ? Sm1 O4 2.503(6) . ? Sm1 N1 2.519(5) . ? Sm1 N8 2.587(5) . ? Sm1 N9 2.627(5) . ? Sm1 N7 2.637(6) . ? Fe1 C2 1.921(7) . ? Fe1 C1 1.929(6) . ? Fe1 C6 1.940(8) . ? Fe1 C3 1.942(7) . ? Fe1 C5 1.942(7) . ? Fe1 C4 1.945(7) . ? N9 C19 1.343(8) . ? N9 C15 1.354(9) . ? N8 C14 1.346(8) . ? N8 C12 1.353(8) . ? C1 N1 1.148(8) . ? N10 C13 1.333(9) . ? N10 C12 1.336(8) . ? C14 N11 1.335(8) . ? C14 C15 1.476(9) . ? C15 C16 1.390(9) . ? C2 N2 1.142(8) . ? N11 C13 1.354(8) . ? C12 C11 1.470(9) . ? C16 C17 1.387(11) . ? N7 C7 1.338(8) . ? N7 C11 1.350(9) . ? C3 N3 1.144(9) . ? C4 N4 1.147(9) . ? C13 C20 1.464(9) . ? C19 C18 1.388(11) . ? C6 N6 1.157(10) . ? C20 N12 1.355(10) . ? C20 C21 1.378(10) . ? C10 C11 1.378(9) . ? C10 C9 1.389(11) . ? C5 N5 1.141(9) . ? C18 C17 1.356(14) . ? C9 C8 1.359(13) . ? C8 C7 1.371(11) . ? N2 Sm1 2.501(5) 3 ? N12 C24 1.354(9) . ? C22 C23 1.350(13) . ? C22 C21 1.388(10) . ? C24 C23 1.376(13) . ? O7 O7 1.40(2) 2_655 ? 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 O2 Sm1 O1 97.3(2) . . ? O2 Sm1 O3 138.16(19) . . ? O1 Sm1 O3 77.2(2) . . ? O2 Sm1 N2 68.67(19) . 3_445 ? O1 Sm1 N2 72.0(2) . 3_445 ? O3 Sm1 N2 70.27(19) . 3_445 ? O2 Sm1 O4 71.2(2) . . ? O1 Sm1 O4 68.2(2) . . ? O3 Sm1 O4 138.1(2) . . ? N2 Sm1 O4 117.7(2) 3_445 . ? O2 Sm1 N1 73.6(2) . . ? O1 Sm1 N1 136.58(19) . . ? O3 Sm1 N1 136.95(18) . . ? N2 Sm1 N1 135.61(19) 3_445 . ? O4 Sm1 N1 68.73(18) . . ? O2 Sm1 N8 129.2(2) . . ? O1 Sm1 N8 133.24(19) . . ? O3 Sm1 N8 70.82(17) . . ? N2 Sm1 N8 124.39(18) 3_445 . ? O4 Sm1 N8 117.8(2) . . ? N1 Sm1 N8 66.17(18) . . ? O2 Sm1 N9 78.9(2) . . ? O1 Sm1 N9 145.66(18) . . ? O3 Sm1 N9 83.19(19) . . ? N2 Sm1 N9 74.94(18) 3_445 . ? O4 Sm1 N9 138.40(18) . . ? N1 Sm1 N9 75.59(17) . . ? N8 Sm1 N9 62.38(17) . . ? O2 Sm1 N7 142.96(19) . . ? O1 Sm1 N7 78.18(18) . . ? O3 Sm1 N7 77.31(19) . . ? N2 Sm1 N7 139.74(19) 3_445 . ? O4 Sm1 N7 73.1(2) . . ? N1 Sm1 N7 84.60(18) . . ? N8 Sm1 N7 62.30(17) . . ? N9 Sm1 N7 124.65(17) . . ? C2 Fe1 C1 177.1(3) . . ? C2 Fe1 C6 85.3(3) . . ? C1 Fe1 C6 92.5(3) . . ? C2 Fe1 C3 90.2(3) . . ? C1 Fe1 C3 87.9(3) . . ? C6 Fe1 C3 88.6(3) . . ? C2 Fe1 C5 90.0(3) . . ? C1 Fe1 C5 92.0(3) . . ? C6 Fe1 C5 93.2(3) . . ? C3 Fe1 C5 178.2(3) . . ? C2 Fe1 C4 92.0(3) . . ? C1 Fe1 C4 90.1(3) . . ? C6 Fe1 C4 176.2(3) . . ? C3 Fe1 C4 88.7(3) . . ? C5 Fe1 C4 89.5(3) . . ? C19 N9 C15 116.9(6) . . ? C19 N9 Sm1 122.1(5) . . ? C15 N9 Sm1 120.9(4) . . ? C14 N8 C12 115.2(5) . . ? C14 N8 Sm1 122.3(4) . . ? C12 N8 Sm1 121.8(4) . . ? N1 C1 Fe1 173.9(5) . . ? C13 N10 C12 116.1(5) . . ? N11 C14 N8 125.0(6) . . ? N11 C14 C15 117.9(5) . . ? N8 C14 C15 117.1(5) . . ? N9 C15 C16 123.0(6) . . ? N9 C15 C14 116.8(5) . . ? C16 C15 C14 120.2(6) . . ? N2 C2 Fe1 175.9(6) . . ? C14 N11 C13 115.0(5) . . ? N10 C12 N8 124.0(6) . . ? N10 C12 C11 118.0(5) . . ? N8 C12 C11 118.0(5) . . ? C1 N1 Sm1 148.1(5) . . ? C17 C16 C15 118.7(8) . . ? C7 N7 C11 117.3(6) . . ? C7 N7 Sm1 121.4(5) . . ? C11 N7 Sm1 121.2(4) . . ? N3 C3 Fe1 179.2(7) . . ? N4 C4 Fe1 179.9(8) . . ? N10 C13 N11 124.6(6) . . ? N10 C13 C20 117.2(6) . . ? N11 C13 C20 118.2(6) . . ? N9 C19 C18 122.6(7) . . ? N6 C6 Fe1 172.9(8) . . ? N12 C20 C21 122.3(6) . . ? N12 C20 C13 117.0(6) . . ? C21 C20 C13 120.6(7) . . ? C11 C10 C9 118.9(8) . . ? N5 C5 Fe1 179.3(8) . . ? N7 C11 C10 122.7(6) . . ? N7 C11 C12 116.2(5) . . ? C10 C11 C12 121.1(6) . . ? C17 C18 C19 120.2(7) . . ? C8 C9 C10 118.2(7) . . ? C18 C17 C16 118.7(7) . . ? C9 C8 C7 120.3(7) . . ? N7 C7 C8 122.6(8) . . ? C2 N2 Sm1 169.6(5) . 3 ? C24 N12 C20 117.2(7) . . ? C23 C22 C21 119.4(8) . . ? N12 C24 C23 122.7(8) . . ? C20 C21 C22 118.9(8) . . ? C22 C23 C24 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 2.244 _refine_diff_density_min -1.535 _refine_diff_density_rms 0.214 # Attachment 'compound4.txt' data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 296496' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-iron(iii)-europium(iii) hexahydrate ; _chemical_formula_moiety '[Eu(tptz)(H2O)4Fe(CN)6]6H2O' _chemical_formula_sum 'C24 H32 Eu Fe N12 O10' _chemical_formula_weight 856.43 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 16.067(3) _cell_length_b 14.056(3) _cell_length_c 31.350(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.34(3) _cell_angle_gamma 90.00 _cell_volume 6889(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 2.293 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27567 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.40 _reflns_number_total 7986 _reflns_number_gt 6893 _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^)+(0.0547P)^2^+88.5325P] 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 7986 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.432 _refine_ls_shift/su_mean 0.018 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 0.46465(2) 0.29977(2) 0.104120(10) 0.02025(11) Uani 1 1 d . . . Fe1 Fe 0.75439(6) 0.49065(6) 0.10853(3) 0.0198(2) Uani 1 1 d . . . N9 N 0.5332(4) 0.2003(4) 0.17354(19) 0.0267(12) Uani 1 1 d . . . C1 C 0.6729(4) 0.3948(5) 0.1155(2) 0.0238(13) Uani 1 1 d . . . C19 C 0.5663(4) 0.3480(5) 0.2122(2) 0.0225(13) Uani 1 1 d . . . C20 C 0.5707(4) 0.2432(5) 0.2119(2) 0.0238(14) Uani 1 1 d . . . N1 N 0.6204(4) 0.3415(4) 0.11756(18) 0.0235(12) Uani 1 1 d . . . C12 C 0.5217(4) 0.4865(4) 0.1782(2) 0.0211(13) Uani 1 1 d . . . N11 N 0.5602(4) 0.5367(4) 0.21246(19) 0.0253(12) Uani 1 1 d . . . O1 O 0.3485(3) 0.3235(4) 0.14215(18) 0.0365(12) Uani 1 1 d . . . C21 C 0.6112(5) 0.1928(5) 0.2488(3) 0.0388(19) Uani 1 1 d . . . H21 H 0.6371 0.2256 0.2750 0.047 Uiso 1 1 calc R . . C2 C 0.8308(4) 0.5910(5) 0.1013(2) 0.0234(13) Uani 1 1 d . . . C23 C 0.5755(5) 0.0508(5) 0.2091(3) 0.044(2) Uani 1 1 d . . . H23 H 0.5750 -0.0167 0.2073 0.053 Uiso 1 1 calc R . . C13 C 0.6054(4) 0.4872(5) 0.2464(2) 0.0239(13) Uani 1 1 d . . . C4 C 0.6637(5) 0.5475(5) 0.0646(2) 0.0293(15) Uani 1 1 d . . . N10 N 0.6097(4) 0.3924(4) 0.24816(18) 0.0252(12) Uani 1 1 d . . . C5 C 0.7870(5) 0.4150(5) 0.0636(2) 0.0322(16) Uani 1 1 d . . . C22 C 0.6135(6) 0.0954(6) 0.2474(3) 0.051(2) Uani 1 1 d . . . H22 H 0.6409 0.0597 0.2724 0.061 Uiso 1 1 calc R . . C10 C 0.4669(6) 0.6350(5) 0.1397(3) 0.043(2) Uani 1 1 d . . . H10 H 0.4908 0.6703 0.1655 0.052 Uiso 1 1 calc R . . C3 C 0.7236(5) 0.5736(6) 0.1514(2) 0.0307(16) Uani 1 1 d . . . O3 O 0.3411(4) 0.3188(4) 0.0433(2) 0.0468(15) Uani 1 1 d . . . N8 N 0.5226(3) 0.3911(3) 0.17613(17) 0.0189(10) Uani 1 1 d . . . N7 N 0.4434(4) 0.4847(4) 0.10323(18) 0.0257(12) Uani 1 1 d . . . C6 C 0.8446(5) 0.4311(5) 0.1523(2) 0.0307(16) Uani 1 1 d . . . C24 C 0.5379(5) 0.1054(5) 0.1728(3) 0.0361(17) Uani 1 1 d . . . H24 H 0.5141 0.0735 0.1461 0.043 Uiso 1 1 calc R . . C11 C 0.4757(4) 0.5378(5) 0.1388(2) 0.0260(14) Uani 1 1 d . . . N6 N 0.8980(5) 0.3948(5) 0.1776(2) 0.0491(19) Uani 1 1 d . . . O4 O 0.5032(4) 0.3572(6) 0.03664(19) 0.0560(19) Uani 1 1 d . . . C7 C 0.4002(5) 0.5297(6) 0.0673(3) 0.0383(18) Uani 1 1 d . . . H7 H 0.3772 0.4933 0.0418 0.046 Uiso 1 1 calc R . . C8 C 0.3877(6) 0.6269(7) 0.0657(3) 0.054(3) Uani 1 1 d . . . H8 H 0.3557 0.6566 0.0399 0.065 Uiso 1 1 calc R . . N5 N 0.8069(6) 0.3711(6) 0.0366(3) 0.060(2) Uani 1 1 d . . . N4 N 0.6092(5) 0.5795(7) 0.0388(2) 0.056(2) Uani 1 1 d . . . O2 O 0.5305(4) 0.1703(4) 0.0726(2) 0.0464(15) Uani 1 1 d . . . N12 N 0.6906(4) 0.4908(5) 0.3214(2) 0.0355(14) Uani 1 1 d . . . N2 N 0.8760(4) 0.6536(4) 0.0998(2) 0.0308(13) Uani 1 1 d . . . C14 C 0.6558(5) 0.5419(5) 0.2842(2) 0.0290(15) Uani 1 1 d . . . C15 C 0.6688(5) 0.6375(5) 0.2801(3) 0.0346(17) Uani 1 1 d . . . H15 H 0.6420 0.6704 0.2541 0.041 Uiso 1 1 calc R . . N3 N 0.7080(5) 0.6296(7) 0.1753(3) 0.058(2) Uani 1 1 d . . . C9 C 0.4225(7) 0.6796(6) 0.1024(4) 0.055(3) Uani 1 1 d . . . H9 H 0.4159 0.7468 0.1020 0.066 Uiso 1 1 calc R . . C18 C 0.7391(6) 0.5406(7) 0.3540(3) 0.044(2) Uani 1 1 d . . . H18 H 0.7624 0.5080 0.3807 0.053 Uiso 1 1 calc R . . C17 C 0.7581(6) 0.6358(7) 0.3519(3) 0.049(2) Uani 1 1 d . . . H17 H 0.7955 0.6666 0.3758 0.059 Uiso 1 1 calc R . . C16 C 0.7216(3) 0.6851(3) 0.31452(17) 0.044(2) Uani 1 1 d . . . H16 H 0.7326 0.7511 0.3123 0.052 Uiso 1 1 calc R . . O5 O 0.6555(3) 0.2234(3) 0.03488(17) 0.073(2) Uani 1 1 d R . . O7 O 0.5294(3) 0.8055(3) 0.23638(17) 0.180(7) Uani 1 1 d R . . O6 O 0.1734(3) 0.3059(3) 0.02748(17) 0.168(7) Uani 1 1 d R . . O8 O 0.4201(17) 0.0547(13) 0.0052(7) 0.251(11) Uani 1 1 d . . . O9 O 0.4976(13) -0.0299(13) 0.0630(7) 0.214(8) Uani 1 1 d . . . O10 O 0.6530(18) 0.8214(9) 0.1862(9) 0.351(19) 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 Eu1 0.01870(17) 0.02330(17) 0.01776(17) 0.00054(12) 0.00218(12) -0.00675(13) Fe1 0.0199(5) 0.0227(4) 0.0161(4) -0.0004(3) 0.0028(4) -0.0082(4) N9 0.028(3) 0.022(3) 0.030(3) -0.001(2) 0.005(2) -0.006(2) C1 0.022(3) 0.030(3) 0.017(3) 0.003(3) 0.000(3) -0.008(3) C19 0.025(3) 0.025(3) 0.018(3) 0.001(2) 0.007(3) -0.007(3) C20 0.020(3) 0.025(3) 0.025(3) 0.007(3) 0.001(3) -0.003(3) N1 0.022(3) 0.027(3) 0.019(3) 0.002(2) 0.001(2) -0.009(2) C12 0.019(3) 0.023(3) 0.022(3) 0.000(2) 0.006(3) -0.003(2) N11 0.028(3) 0.020(3) 0.028(3) -0.003(2) 0.006(2) -0.004(2) O1 0.030(3) 0.042(3) 0.041(3) -0.011(2) 0.013(2) -0.009(2) C21 0.040(5) 0.031(4) 0.038(4) 0.013(3) -0.007(4) -0.003(3) C2 0.020(3) 0.031(3) 0.019(3) -0.004(3) 0.005(3) -0.004(3) C23 0.039(5) 0.020(3) 0.066(6) 0.011(4) -0.004(4) -0.001(3) C13 0.023(3) 0.028(3) 0.021(3) -0.005(3) 0.006(3) -0.007(3) C4 0.024(4) 0.042(4) 0.019(3) 0.002(3) 0.002(3) -0.007(3) N10 0.026(3) 0.026(3) 0.023(3) -0.001(2) 0.006(2) -0.003(2) C5 0.039(4) 0.028(3) 0.027(4) -0.005(3) 0.003(3) -0.004(3) C22 0.043(5) 0.036(4) 0.057(6) 0.020(4) -0.020(4) -0.007(4) C10 0.045(5) 0.025(4) 0.054(5) 0.009(3) 0.000(4) -0.004(3) C3 0.021(3) 0.048(4) 0.023(4) -0.006(3) 0.005(3) -0.002(3) O3 0.033(3) 0.056(4) 0.043(3) 0.012(3) -0.010(3) -0.011(3) N8 0.021(3) 0.017(2) 0.019(3) 0.0007(19) 0.006(2) -0.005(2) N7 0.028(3) 0.024(3) 0.024(3) 0.007(2) 0.003(2) 0.000(2) C6 0.035(4) 0.026(3) 0.027(4) -0.001(3) -0.001(3) -0.013(3) C24 0.037(4) 0.021(3) 0.048(5) -0.004(3) 0.004(4) -0.002(3) C11 0.025(3) 0.019(3) 0.033(4) 0.005(3) 0.004(3) -0.005(3) N6 0.047(4) 0.038(4) 0.048(4) 0.007(3) -0.017(4) -0.010(3) O4 0.035(3) 0.105(6) 0.029(3) 0.026(3) 0.010(3) 0.019(3) C7 0.038(4) 0.040(4) 0.034(4) 0.014(3) 0.002(3) 0.001(4) C8 0.058(6) 0.045(5) 0.052(6) 0.029(4) -0.004(5) 0.001(4) N5 0.075(6) 0.059(5) 0.039(4) -0.017(4) 0.002(4) 0.023(4) N4 0.044(5) 0.085(6) 0.034(4) 0.013(4) -0.002(3) 0.010(4) O2 0.051(4) 0.038(3) 0.060(4) -0.020(3) 0.033(3) -0.018(3) N12 0.034(4) 0.040(3) 0.028(3) -0.005(3) -0.001(3) -0.001(3) N2 0.028(3) 0.033(3) 0.031(3) 0.000(3) 0.007(3) -0.012(3) C14 0.024(4) 0.036(4) 0.029(4) -0.012(3) 0.009(3) -0.002(3) C15 0.038(4) 0.031(4) 0.034(4) -0.011(3) 0.008(3) -0.007(3) N3 0.045(5) 0.087(6) 0.042(4) -0.024(4) 0.007(4) 0.011(4) C9 0.062(6) 0.019(4) 0.074(7) 0.019(4) -0.004(5) 0.003(4) C18 0.040(5) 0.053(5) 0.036(5) -0.015(4) 0.003(4) -0.007(4) C17 0.035(5) 0.058(6) 0.052(6) -0.030(4) 0.004(4) -0.010(4) C16 0.045(5) 0.039(4) 0.045(5) -0.018(4) 0.007(4) -0.010(4) O5 0.080(5) 0.088(5) 0.064(5) -0.037(4) 0.043(4) -0.035(4) O7 0.25(2) 0.166(13) 0.129(14) 0.018(9) 0.044(11) 0.086(13) O6 0.045(6) 0.169(13) 0.266(18) -0.046(12) -0.013(8) -0.010(7) O8 0.44(3) 0.169(15) 0.203(18) -0.102(14) 0.19(2) -0.105(19) O9 0.224(19) 0.195(17) 0.26(2) -0.073(16) 0.135(17) -0.038(14) O10 0.57(4) 0.068(8) 0.60(4) -0.060(14) 0.53(4) -0.053(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2 2.427(6) . ? Eu1 O3 2.430(6) . ? Eu1 O1 2.458(5) . ? Eu1 O4 2.473(6) . ? Eu1 N2 2.486(6) 3_445 ? Eu1 N1 2.509(5) . ? Eu1 N8 2.577(5) . ? Eu1 N9 2.608(6) . ? Eu1 N7 2.621(6) . ? Fe1 C2 1.918(7) . ? Fe1 C1 1.926(6) . ? Fe1 C5 1.931(7) . ? Fe1 C3 1.929(7) . ? Fe1 C4 1.931(7) . ? Fe1 C6 1.940(8) . ? N9 C24 1.337(8) . ? N9 C20 1.356(9) . ? C1 N1 1.142(8) . ? C19 N10 1.336(8) . ? C19 N8 1.330(8) . ? C19 C20 1.474(9) . ? C20 C21 1.385(10) . ? C12 N11 1.314(8) . ? C12 N8 1.343(8) . ? C12 C11 1.475(9) . ? N11 C13 1.337(9) . ? C21 C22 1.371(11) . ? C2 N2 1.148(9) . ? C23 C22 1.367(13) . ? C23 C24 1.389(11) . ? C13 N10 1.335(9) . ? C13 C14 1.486(9) . ? C4 N4 1.140(10) . ? C5 N5 1.151(10) . ? C10 C11 1.374(10) . ? C10 C9 1.373(12) . ? C3 N3 1.152(10) . ? N7 C7 1.338(9) . ? N7 C11 1.342(9) . ? C6 N6 1.146(10) . ? C7 C8 1.380(12) . ? C8 C9 1.374(14) . ? N12 C18 1.332(10) . ? N12 C14 1.374(10) . ? N2 Eu1 2.486(6) 3 ? C14 C15 1.371(10) . ? C15 C16 1.381(9) . ? C18 C17 1.378(13) . ? C17 C16 1.371(12) . ? O7 O7 1.413(9) 2_655 ? 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 O2 Eu1 O3 96.7(2) . . ? O2 Eu1 O1 138.61(18) . . ? O3 Eu1 O1 77.9(2) . . ? O2 Eu1 O4 71.2(2) . . ? O3 Eu1 O4 67.3(2) . . ? O1 Eu1 O4 137.6(2) . . ? O2 Eu1 N2 69.9(2) . 3_445 ? O3 Eu1 N2 72.2(2) . 3_445 ? O1 Eu1 N2 69.45(19) . 3_445 ? O4 Eu1 N2 118.4(2) . 3_445 ? O2 Eu1 N1 74.47(19) . . ? O3 Eu1 N1 135.13(19) . . ? O1 Eu1 N1 136.58(18) . . ? O4 Eu1 N1 68.30(19) . . ? N2 Eu1 N1 137.6(2) 3_445 . ? O2 Eu1 N8 128.8(2) . . ? O3 Eu1 N8 134.2(2) . . ? O1 Eu1 N8 70.68(17) . . ? O4 Eu1 N8 118.4(2) . . ? N2 Eu1 N8 123.12(18) 3_445 . ? N1 Eu1 N8 65.90(17) . . ? O2 Eu1 N9 78.4(2) . . ? O3 Eu1 N9 145.62(18) . . ? O1 Eu1 N9 83.66(19) . . ? O4 Eu1 N9 138.43(19) . . ? N2 Eu1 N9 74.26(19) 3_445 . ? N1 Eu1 N9 76.86(18) . . ? N8 Eu1 N9 62.50(17) . . ? O2 Eu1 N7 143.84(19) . . ? O3 Eu1 N7 78.53(19) . . ? O1 Eu1 N7 76.05(18) . . ? O4 Eu1 N7 74.1(2) . . ? N2 Eu1 N7 138.4(2) 3_445 . ? N1 Eu1 N7 83.85(18) . . ? N8 Eu1 N7 62.32(17) . . ? N9 Eu1 N7 124.74(17) . . ? C2 Fe1 C1 177.0(3) . . ? C2 Fe1 C5 91.8(3) . . ? C1 Fe1 C5 90.2(3) . . ? C2 Fe1 C3 84.9(3) . . ? C1 Fe1 C3 93.1(3) . . ? C5 Fe1 C3 176.2(3) . . ? C2 Fe1 C4 90.6(3) . . ? C1 Fe1 C4 87.1(3) . . ? C5 Fe1 C4 89.7(3) . . ? C3 Fe1 C4 88.5(3) . . ? C2 Fe1 C6 90.4(3) . . ? C1 Fe1 C6 92.0(3) . . ? C5 Fe1 C6 89.7(3) . . ? C3 Fe1 C6 92.1(3) . . ? C4 Fe1 C6 178.9(3) . . ? C24 N9 C20 116.4(6) . . ? C24 N9 Eu1 122.4(5) . . ? C20 N9 Eu1 121.1(4) . . ? N1 C1 Fe1 175.2(6) . . ? N10 C19 N8 125.1(6) . . ? N10 C19 C20 117.1(6) . . ? N8 C19 C20 117.8(6) . . ? N9 C20 C21 122.7(6) . . ? N9 C20 C19 116.0(6) . . ? C21 C20 C19 121.3(7) . . ? C1 N1 Eu1 149.9(5) . . ? N11 C12 N8 124.6(6) . . ? N11 C12 C11 118.2(6) . . ? N8 C12 C11 117.2(6) . . ? C12 N11 C13 115.9(6) . . ? C22 C21 C20 119.7(8) . . ? N2 C2 Fe1 175.3(6) . . ? C22 C23 C24 119.2(7) . . ? N10 C13 N11 124.5(6) . . ? N10 C13 C14 118.0(6) . . ? N11 C13 C14 117.5(6) . . ? N4 C4 Fe1 178.6(8) . . ? C13 N10 C19 114.8(6) . . ? N5 C5 Fe1 179.0(8) . . ? C21 C22 C23 118.5(8) . . ? C11 C10 C9 118.1(8) . . ? N3 C3 Fe1 174.0(8) . . ? C12 N8 C19 115.0(5) . . ? C12 N8 Eu1 122.3(4) . . ? C19 N8 Eu1 122.1(4) . . ? C7 N7 C11 117.5(6) . . ? C7 N7 Eu1 121.3(5) . . ? C11 N7 Eu1 121.2(4) . . ? N6 C6 Fe1 178.8(8) . . ? N9 C24 C23 123.6(8) . . ? N7 C11 C10 123.3(7) . . ? N7 C11 C12 116.5(6) . . ? C10 C11 C12 120.1(7) . . ? N7 C7 C8 122.7(8) . . ? C7 C8 C9 118.5(8) . . ? C18 N12 C14 115.3(7) . . ? C2 N2 Eu1 172.0(6) . 3 ? N12 C14 C15 123.4(7) . . ? N12 C14 C13 116.5(6) . . ? C15 C14 C13 120.0(7) . . ? C14 C15 C16 118.8(7) . . ? C10 C9 C8 119.9(8) . . ? N12 C18 C17 124.8(9) . . ? C18 C17 C16 118.5(7) . . ? C15 C16 C17 119.1(6) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 2.528 _refine_diff_density_min -2.303 _refine_diff_density_rms 0.185 # Attachment 'compound5.txt' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 296497' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-iron(iii)-gadolinium(iii) hexahydrate ; _chemical_formula_moiety '[Gd(tptz)(H2O)4Fe(CN)6]6H2O' _chemical_formula_sum 'C24 H32 Fe Gd N12 O10' _chemical_formula_weight 861.72 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' Fe Fe 0.3463 0.8444 '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 ? _symmetry_space_group_name_H-M ? 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 16.074(3) _cell_length_b 14.072(3) _cell_length_c 31.417(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.38(3) _cell_angle_gamma 90.00 _cell_volume 6913(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20278 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1440 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7671 _reflns_number_gt 4676 _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^)+(0.0909P)^2^+11.6746P] 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 7671 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.010 _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 Gd1 Gd 0.46455(3) 0.30058(3) 0.104141(15) 0.02048(16) Uani 1 1 d . . . Fe1 Fe 0.75442(8) 0.49140(9) 0.10856(4) 0.0200(3) Uani 1 1 d . . . N9 N 0.5340(5) 0.2011(5) 0.1734(3) 0.0263(18) Uani 1 1 d . . . N8 N 0.5232(5) 0.3914(5) 0.1759(3) 0.0198(17) Uani 1 1 d . . . C1 C 0.6722(6) 0.3956(7) 0.1158(3) 0.023(2) Uani 1 1 d . . . N10 N 0.5607(5) 0.5368(5) 0.2131(3) 0.0229(18) Uani 1 1 d . . . C14 C 0.5664(6) 0.3490(6) 0.2120(3) 0.022(2) Uani 1 1 d . . . C15 C 0.5695(6) 0.2441(7) 0.2114(3) 0.024(2) Uani 1 1 d . . . C2 C 0.8304(6) 0.5921(7) 0.1018(3) 0.021(2) Uani 1 1 d . . . N11 N 0.6097(5) 0.3931(5) 0.2483(3) 0.0223(17) Uani 1 1 d . . . C12 C 0.5207(5) 0.4880(6) 0.1780(3) 0.019(2) Uani 1 1 d . . . N1 N 0.6195(5) 0.3420(6) 0.1173(3) 0.0228(18) Uani 1 1 d . . . C16 C 0.6117(7) 0.1939(8) 0.2488(4) 0.040(3) Uani 1 1 d . . . H16 H 0.6385 0.2265 0.2748 0.048 Uiso 1 1 calc R . . N7 N 0.4434(5) 0.4855(6) 0.1029(3) 0.0255(19) Uani 1 1 d . . . C3 C 0.6635(6) 0.5501(8) 0.0651(3) 0.028(2) Uani 1 1 d . . . C4 C 0.7875(7) 0.4159(7) 0.0635(4) 0.032(2) Uani 1 1 d . . . C13 C 0.6049(6) 0.4878(7) 0.2462(3) 0.021(2) Uani 1 1 d . . . C19 C 0.5389(6) 0.1062(7) 0.1727(4) 0.034(3) Uani 1 1 d . . . H19 H 0.5157 0.0747 0.1458 0.041 Uiso 1 1 calc R . . C6 C 0.7239(6) 0.5736(8) 0.1519(3) 0.029(2) Uani 1 1 d . . . C20 C 0.6566(6) 0.5410(8) 0.2843(3) 0.028(2) Uani 1 1 d . . . C10 C 0.4670(7) 0.6358(7) 0.1389(4) 0.041(3) Uani 1 1 d . . . H10 H 0.4911 0.6711 0.1646 0.049 Uiso 1 1 calc R . . C5 C 0.8464(6) 0.4315(7) 0.1530(3) 0.027(2) Uani 1 1 d . . . C11 C 0.4749(6) 0.5385(7) 0.1385(3) 0.028(2) Uani 1 1 d . . . C18 C 0.5759(7) 0.0503(8) 0.2091(5) 0.045(3) Uani 1 1 d . . . H18 H 0.5746 -0.0171 0.2074 0.054 Uiso 1 1 calc R . . C9 C 0.4236(8) 0.6810(7) 0.1017(4) 0.049(4) Uani 1 1 d . . . H9 H 0.4189 0.7483 0.1010 0.059 Uiso 1 1 calc R . . C17 C 0.6135(7) 0.0949(8) 0.2467(4) 0.046(3) Uani 1 1 d . . . H17 H 0.6411 0.0590 0.2716 0.055 Uiso 1 1 calc R . . C8 C 0.3872(8) 0.6282(9) 0.0654(5) 0.053(4) Uani 1 1 d . . . H8 H 0.3541 0.6579 0.0399 0.064 Uiso 1 1 calc R . . C7 C 0.3996(7) 0.5306(8) 0.0667(4) 0.039(3) Uani 1 1 d . . . H7 H 0.3765 0.4942 0.0412 0.047 Uiso 1 1 calc R . . O1 O 0.3408(4) 0.3197(5) 0.0439(3) 0.045(2) Uani 1 1 d . . . O2 O 0.5300(5) 0.1709(5) 0.0726(3) 0.045(2) Uani 1 1 d . . . O3 O 0.3484(4) 0.3252(5) 0.1419(2) 0.0299(17) Uani 1 1 d . . . N2 N 0.8753(5) 0.6551(6) 0.0995(3) 0.032(2) Uani 1 1 d . . . N4 N 0.8063(7) 0.3724(7) 0.0356(3) 0.053(3) Uani 1 1 d . . . N3 N 0.6092(6) 0.5804(8) 0.0391(3) 0.052(3) Uani 1 1 d . . . O4 O 0.5030(5) 0.3590(7) 0.0369(3) 0.052(2) Uani 1 1 d . . . N12 N 0.6896(5) 0.4927(6) 0.3213(3) 0.032(2) Uani 1 1 d . . . N5 N 0.8984(6) 0.3950(7) 0.1770(3) 0.046(3) Uani 1 1 d . . . C22 C 0.7206(7) 0.6861(8) 0.3148(4) 0.042(3) Uani 1 1 d . . . H22 H 0.7308 0.7522 0.3127 0.050 Uiso 1 1 calc R . . C24 C 0.7395(7) 0.5410(9) 0.3540(4) 0.042(3) Uani 1 1 d . . . H24 H 0.7643 0.5075 0.3801 0.050 Uiso 1 1 calc R . . C21 C 0.6681(7) 0.6385(8) 0.2802(4) 0.034(3) Uani 1 1 d . . . H21 H 0.6407 0.6713 0.2543 0.041 Uiso 1 1 calc R . . C23 C 0.7576(7) 0.6377(9) 0.3521(4) 0.043(3) Uani 1 1 d . . . H23 H 0.7945 0.6689 0.3761 0.051 Uiso 1 1 calc R . . N6 N 0.7085(6) 0.6301(8) 0.1758(3) 0.050(3) Uani 1 1 d . . . O8 O 0.6560(6) 0.2223(7) 0.0348(3) 0.068(3) Uani 1 1 d . . . O5 O 0.5349(15) 0.8072(12) 0.2355(7) 0.202(10) Uani 1 1 d . . . O7 O 0.6704(7) 0.8002(11) 0.0457(15) 0.47(3) Uani 1 1 d . . . O6 O 0.636(3) 0.8329(16) 0.1761(15) 0.56(4) Uani 1 1 d . . . O9 O 0.4180(16) 0.0542(15) 0.0057(7) 0.223(11) Uani 1 1 d . . . O10 O 0.4964(15) -0.0285(14) 0.0612(8) 0.199(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0199(2) 0.0241(3) 0.0174(3) 0.0004(2) 0.00411(18) -0.0060(2) Fe1 0.0212(7) 0.0227(7) 0.0161(7) -0.0009(6) 0.0047(6) -0.0084(6) N9 0.029(4) 0.022(4) 0.028(5) -0.004(4) 0.008(4) -0.007(4) N8 0.021(4) 0.015(4) 0.023(4) 0.003(3) 0.004(3) 0.001(3) C1 0.022(5) 0.024(5) 0.021(5) 0.003(4) 0.004(4) -0.007(4) N10 0.023(4) 0.022(4) 0.025(5) -0.003(4) 0.008(4) -0.005(3) C14 0.027(5) 0.019(5) 0.021(5) -0.002(4) 0.008(4) -0.010(4) C15 0.015(5) 0.031(5) 0.025(6) 0.002(5) 0.000(4) -0.011(4) C2 0.020(4) 0.031(5) 0.013(5) -0.001(4) 0.005(4) -0.003(4) N11 0.030(4) 0.018(4) 0.018(4) 0.002(3) 0.004(4) -0.001(3) C12 0.018(4) 0.012(4) 0.032(6) -0.001(4) 0.012(4) -0.004(4) N1 0.023(4) 0.028(4) 0.017(5) 0.001(4) 0.005(4) -0.006(4) C16 0.037(6) 0.036(6) 0.037(7) 0.017(6) -0.011(5) -0.011(5) N7 0.023(4) 0.027(4) 0.026(5) 0.011(4) 0.005(4) -0.008(3) C3 0.025(5) 0.040(6) 0.021(6) 0.001(5) 0.009(5) -0.008(5) C4 0.035(6) 0.028(6) 0.031(6) -0.005(5) 0.002(5) -0.006(5) C13 0.019(5) 0.026(5) 0.020(5) -0.005(4) 0.010(4) -0.005(4) C19 0.031(6) 0.024(5) 0.045(7) -0.009(5) 0.006(5) -0.002(5) C6 0.021(5) 0.047(7) 0.021(6) -0.012(5) 0.007(4) -0.007(5) C20 0.022(5) 0.042(6) 0.025(6) -0.010(5) 0.012(4) 0.001(5) C10 0.037(6) 0.027(6) 0.053(8) 0.010(6) -0.003(6) -0.006(5) C5 0.032(6) 0.019(5) 0.025(6) -0.002(4) -0.006(5) -0.008(4) C11 0.027(5) 0.034(6) 0.022(6) 0.006(5) 0.005(5) -0.005(5) C18 0.040(6) 0.022(6) 0.069(10) 0.002(6) 0.005(7) -0.006(5) C9 0.055(7) 0.017(6) 0.063(9) 0.021(6) -0.014(7) -0.008(5) C17 0.040(6) 0.023(6) 0.062(9) 0.012(6) -0.017(6) -0.006(5) C8 0.057(8) 0.040(7) 0.052(9) 0.029(7) -0.008(7) 0.005(6) C7 0.035(6) 0.044(7) 0.039(7) 0.018(6) 0.008(5) -0.002(5) O1 0.028(4) 0.054(5) 0.043(5) 0.008(4) -0.015(4) -0.008(4) O2 0.055(5) 0.041(4) 0.048(5) -0.023(4) 0.031(4) -0.020(4) O3 0.024(3) 0.036(4) 0.032(4) -0.003(3) 0.011(3) -0.007(3) N2 0.029(4) 0.038(5) 0.031(5) -0.004(4) 0.010(4) -0.014(4) N4 0.070(7) 0.049(6) 0.038(7) -0.011(5) 0.007(6) 0.008(6) N3 0.043(6) 0.088(8) 0.024(6) 0.001(6) 0.007(5) 0.002(6) O4 0.034(4) 0.100(7) 0.026(5) 0.022(5) 0.014(4) 0.020(4) N12 0.033(5) 0.039(5) 0.022(5) -0.007(4) 0.006(4) -0.009(4) N5 0.047(6) 0.032(5) 0.048(7) 0.004(5) -0.016(5) -0.013(5) C22 0.035(6) 0.040(7) 0.048(8) -0.024(6) 0.007(6) -0.011(5) C24 0.033(6) 0.067(9) 0.019(6) -0.016(6) -0.006(5) 0.002(6) C21 0.036(6) 0.034(6) 0.034(7) -0.018(5) 0.009(5) 0.000(5) C23 0.036(6) 0.054(8) 0.034(7) -0.028(6) -0.001(6) -0.005(6) N6 0.039(5) 0.068(7) 0.043(7) -0.016(6) 0.006(5) 0.001(5) O8 0.073(6) 0.088(7) 0.053(6) -0.036(5) 0.035(5) -0.024(5) O5 0.25(3) 0.182(18) 0.18(2) 0.013(15) 0.058(16) 0.100(16) O7 0.021(6) 0.102(12) 1.19(9) -0.20(3) -0.030(19) -0.003(7) O6 0.90(7) 0.158(18) 0.95(8) -0.30(3) 0.89(7) -0.27(3) O9 0.33(3) 0.199(19) 0.18(2) -0.114(17) 0.13(2) -0.10(2) O10 0.26(2) 0.158(17) 0.22(2) -0.047(16) 0.130(19) -0.021(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 Gd1 O1 2.422(7) . ? Gd1 O2 2.429(7) . ? Gd1 O3 2.456(7) . ? Gd1 O4 2.475(8) . ? Gd1 N2 2.485(8) 3_445 ? Gd1 N1 2.498(7) . ? Gd1 N8 2.572(8) . ? Gd1 N9 2.610(8) . ? Gd1 N7 2.623(8) . ? Fe1 C2 1.914(9) . ? Fe1 C6 1.935(11) . ? Fe1 C1 1.937(9) . ? Fe1 C3 1.939(11) . ? Fe1 C4 1.941(12) . ? Fe1 C5 1.973(10) . ? N9 C19 1.338(12) . ? N9 C15 1.343(12) . ? N8 C14 1.328(12) . ? N8 C12 1.362(11) . ? C1 N1 1.144(11) . ? N10 C13 1.313(12) . ? N10 C12 1.330(12) . ? C14 N11 1.341(11) . ? C14 C15 1.478(13) . ? C15 C16 1.403(14) . ? C2 N2 1.156(12) . ? N11 C13 1.335(12) . ? C12 C11 1.473(13) . ? C16 C17 1.396(14) . ? N7 C11 1.342(12) . ? N7 C7 1.350(13) . ? C3 N3 1.131(13) . ? C4 N4 1.165(14) . ? C13 C20 1.491(13) . ? C19 C18 1.403(16) . ? C6 N6 1.158(13) . ? C20 N12 1.343(13) . ? C20 C21 1.395(15) . ? C10 C9 1.372(15) . ? C10 C11 1.376(14) . ? C5 N5 1.113(12) . ? C18 C17 1.350(16) . ? C9 C8 1.374(17) . ? C8 C7 1.387(16) . ? N2 Gd1 2.485(8) 3 ? N12 C24 1.333(13) . ? C22 C23 1.367(17) . ? C22 C21 1.386(14) . ? C24 C23 1.396(17) . ? O5 O5 1.60(4) 2_655 ? 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 O2 96.9(3) . . ? O1 Gd1 O3 77.5(3) . . ? O2 Gd1 O3 138.7(2) . . ? O1 Gd1 O4 67.5(3) . . ? O2 Gd1 O4 71.6(3) . . ? O3 Gd1 O4 137.1(2) . . ? O1 Gd1 N2 71.8(3) . 3_445 ? O2 Gd1 N2 69.9(3) . 3_445 ? O3 Gd1 N2 69.6(3) . 3_445 ? O4 Gd1 N2 118.6(3) . 3_445 ? O1 Gd1 N1 135.3(3) . . ? O2 Gd1 N1 74.5(3) . . ? O3 Gd1 N1 136.6(2) . . ? O4 Gd1 N1 68.2(3) . . ? N2 Gd1 N1 137.9(3) 3_445 . ? O1 Gd1 N8 134.2(3) . . ? O2 Gd1 N8 128.7(3) . . ? O3 Gd1 N8 70.9(2) . . ? O4 Gd1 N8 118.0(3) . . ? N2 Gd1 N8 123.4(3) 3_445 . ? N1 Gd1 N8 65.8(2) . . ? O1 Gd1 N9 145.7(2) . . ? O2 Gd1 N9 78.1(3) . . ? O3 Gd1 N9 84.3(2) . . ? O4 Gd1 N9 138.3(2) . . ? N2 Gd1 N9 74.7(3) 3_445 . ? N1 Gd1 N9 76.6(2) . . ? N8 Gd1 N9 62.4(2) . . ? O1 Gd1 N7 78.3(3) . . ? O2 Gd1 N7 143.7(3) . . ? O3 Gd1 N7 75.9(2) . . ? O4 Gd1 N7 73.4(3) . . ? N2 Gd1 N7 138.2(3) 3_445 . ? N1 Gd1 N7 83.8(2) . . ? N8 Gd1 N7 62.6(2) . . ? N9 Gd1 N7 125.0(3) . . ? C2 Fe1 C6 84.7(4) . . ? C2 Fe1 C1 176.3(4) . . ? C6 Fe1 C1 92.4(4) . . ? C2 Fe1 C3 90.1(4) . . ? C6 Fe1 C3 88.2(4) . . ? C1 Fe1 C3 87.5(4) . . ? C2 Fe1 C4 92.0(4) . . ? C6 Fe1 C4 176.4(5) . . ? C1 Fe1 C4 90.8(4) . . ? C3 Fe1 C4 90.5(4) . . ? C2 Fe1 C5 90.1(4) . . ? C6 Fe1 C5 91.6(4) . . ? C1 Fe1 C5 92.3(4) . . ? C3 Fe1 C5 179.7(4) . . ? C4 Fe1 C5 89.7(4) . . ? C19 N9 C15 116.7(9) . . ? C19 N9 Gd1 122.5(7) . . ? C15 N9 Gd1 120.8(6) . . ? C14 N8 C12 114.9(8) . . ? C14 N8 Gd1 122.7(6) . . ? C12 N8 Gd1 122.0(6) . . ? N1 C1 Fe1 174.8(9) . . ? C13 N10 C12 117.0(8) . . ? N8 C14 N11 125.8(8) . . ? N8 C14 C15 116.7(8) . . ? N11 C14 C15 117.4(9) . . ? N9 C15 C16 122.8(9) . . ? N9 C15 C14 116.9(9) . . ? C16 C15 C14 120.2(9) . . ? N2 C2 Fe1 176.7(9) . . ? C13 N11 C14 114.1(8) . . ? N10 C12 N8 122.9(8) . . ? N10 C12 C11 120.0(8) . . ? N8 C12 C11 117.0(8) . . ? C1 N1 Gd1 150.1(7) . . ? C17 C16 C15 118.3(11) . . ? C11 N7 C7 117.6(9) . . ? C11 N7 Gd1 121.1(6) . . ? C7 N7 Gd1 121.3(7) . . ? N3 C3 Fe1 176.9(10) . . ? N4 C4 Fe1 178.1(10) . . ? N10 C13 N11 125.3(8) . . ? N10 C13 C20 118.2(9) . . ? N11 C13 C20 116.5(9) . . ? N9 C19 C18 124.2(10) . . ? N6 C6 Fe1 173.3(10) . . ? N12 C20 C21 122.9(10) . . ? N12 C20 C13 118.4(9) . . ? C21 C20 C13 118.7(10) . . ? C9 C10 C11 118.8(11) . . ? N5 C5 Fe1 177.4(10) . . ? N7 C11 C10 123.0(10) . . ? N7 C11 C12 117.0(9) . . ? C10 C11 C12 120.1(10) . . ? C17 C18 C19 118.2(10) . . ? C10 C9 C8 119.5(10) . . ? C18 C17 C16 119.7(11) . . ? C9 C8 C7 118.7(11) . . ? N7 C7 C8 122.3(11) . . ? C2 N2 Gd1 171.3(8) . 3 ? C24 N12 C20 117.0(10) . . ? C23 C22 C21 119.8(11) . . ? N12 C24 C23 124.0(11) . . ? C22 C21 C20 118.2(11) . . ? C22 C23 C24 117.9(10) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 2.119 _refine_diff_density_min -1.319 _refine_diff_density_rms 0.225 # Attachment 'compound6.txt' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 296498' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-iron(iii)-terbium(iii) octahydrate ; _chemical_formula_moiety '[Tb(tptz)(H2O)4Fe(CN)6]8H2O' _chemical_formula_sum 'C24 H36 Fe N12 O12 Tb' _chemical_formula_weight 899.42 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' Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 15.951(4) _cell_length_b 14.086(4) _cell_length_c 31.266(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.017(4) _cell_angle_gamma 90.00 _cell_volume 6844(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 2.550 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8417 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20122 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.61 _reflns_number_total 7611 _reflns_number_gt 6024 _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^)+(0.0555P)^2^+67.3035P] 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 7611 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 1.876 _refine_ls_shift/su_mean 0.029 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 0.46526(2) 0.19606(2) 0.104583(10) 0.01983(9) Uani 1 1 d . . . Fe1 Fe 0.25587(6) 0.50590(7) 0.10833(3) 0.0197(2) Uani 1 1 d . . . N12 N 0.6890(4) 0.0053(5) 0.3216(2) 0.0363(16) Uani 1 1 d . . . N7 N 0.5338(4) 0.2962(4) 0.17293(18) 0.0242(12) Uani 1 1 d . . . C2 C 0.1744(4) 0.6019(5) 0.1155(2) 0.0228(14) Uani 1 1 d . . . C1 C 0.3324(4) 0.4047(5) 0.1010(2) 0.0239(14) Uani 1 1 d . . . C12 C 0.5672(4) 0.1492(5) 0.2119(2) 0.0214(14) Uani 1 1 d . . . N2 N 0.1208(4) 0.6558(4) 0.11722(17) 0.0215(12) Uani 1 1 d . . . C11 C 0.5710(4) 0.2540(4) 0.2119(2) 0.0204(14) Uani 1 1 d . . . O4 O 0.3494(3) 0.1732(4) 0.14250(17) 0.0356(13) Uani 1 1 d . . . C13 C 0.5227(4) 0.0099(4) 0.1779(2) 0.0206(14) Uani 1 1 d . . . C10 C 0.6115(5) 0.3031(5) 0.2483(2) 0.0336(17) Uani 1 1 d . . . H10 H 0.6382 0.2700 0.2743 0.040 Uiso 1 1 calc R . . N10 N 0.6098(4) 0.1035(4) 0.24824(18) 0.0225(12) Uani 1 1 d . . . C19 C 0.6053(4) 0.0100(5) 0.2462(2) 0.0225(14) Uani 1 1 d . . . C6 C 0.2881(5) 0.5805(5) 0.0629(2) 0.0291(16) Uani 1 1 d . . . C24 C 0.7379(5) -0.0433(6) 0.3541(3) 0.041(2) Uani 1 1 d . . . H24 H 0.7624 -0.0103 0.3804 0.049 Uiso 1 1 calc R . . C8 C 0.5764(5) 0.4461(6) 0.2078(3) 0.044(2) Uani 1 1 d . . . H8 H 0.5772 0.5134 0.2055 0.052 Uiso 1 1 calc R . . N11 N 0.5609(4) -0.0407(4) 0.21248(19) 0.0242(13) Uani 1 1 d . . . C5 C 0.1642(5) 0.4484(5) 0.0647(2) 0.0264(16) Uani 1 1 d . . . C3 C 0.3472(5) 0.5656(5) 0.1518(2) 0.0286(16) Uani 1 1 d . . . C9 C 0.6138(5) 0.4019(6) 0.2473(3) 0.043(2) Uani 1 1 d . . . H9 H 0.6398 0.4377 0.2725 0.052 Uiso 1 1 calc R . . N3 N 0.4011(5) 0.6019(5) 0.1772(2) 0.051(2) Uani 1 1 d . . . C4 C 0.2242(5) 0.4229(6) 0.1514(2) 0.0311(17) Uani 1 1 d . . . O3 O 0.3410(4) 0.1767(4) 0.04465(18) 0.0481(16) Uani 1 1 d . . . C14 C 0.4773(4) -0.0409(5) 0.1381(2) 0.0242(15) Uani 1 1 d . . . N6 N 0.3082(5) 0.6243(5) 0.0356(2) 0.0488(19) Uani 1 1 d . . . C20 C 0.6554(4) -0.0455(5) 0.2841(2) 0.0252(15) Uani 1 1 d . . . C21 C 0.6673(5) -0.1426(5) 0.2801(3) 0.0325(17) Uani 1 1 d . . . H21 H 0.6409 -0.1751 0.2539 0.039 Uiso 1 1 calc R . . C23 C 0.7555(5) -0.1397(7) 0.3520(3) 0.047(2) Uani 1 1 d . . . H23 H 0.7930 -0.1700 0.3760 0.056 Uiso 1 1 calc R . . N8 N 0.5229(3) 0.1051(4) 0.17583(17) 0.0173(11) Uani 1 1 d . . . C15 C 0.4698(5) -0.1388(5) 0.1387(3) 0.0373(19) Uani 1 1 d . . . H15 H 0.4940 -0.1743 0.1644 0.045 Uiso 1 1 calc R . . C18 C 0.4011(5) -0.0328(6) 0.0668(3) 0.0376(19) Uani 1 1 d . . . H18 H 0.3767 0.0039 0.0416 0.045 Uiso 1 1 calc R . . O1 O 0.5042(4) 0.1393(6) 0.03708(18) 0.0574(19) Uani 1 1 d . . . C16 C 0.4260(6) -0.1833(6) 0.1008(3) 0.052(3) Uani 1 1 d . . . H16 H 0.4200 -0.2505 0.0999 0.062 Uiso 1 1 calc R . . N9 N 0.4436(4) 0.0119(5) 0.10312(19) 0.0324(15) Uani 1 1 d . . . C22 C 0.7187(5) -0.1913(6) 0.3152(3) 0.0397(19) Uani 1 1 d . . . H22 H 0.7280 -0.2577 0.3137 0.048 Uiso 1 1 calc R . . N5 N 0.1097(5) 0.4167(6) 0.0389(2) 0.053(2) Uani 1 1 d . . . C7 C 0.5383(5) 0.3921(5) 0.1721(3) 0.0312(17) Uani 1 1 d . . . H7 H 0.5137 0.4237 0.1454 0.037 Uiso 1 1 calc R . . C17 C 0.3917(6) -0.1301(6) 0.0648(3) 0.050(2) Uani 1 1 d . . . H17 H 0.3614 -0.1597 0.0386 0.060 Uiso 1 1 calc R . . N4 N 0.2083(5) 0.3662(7) 0.1749(2) 0.060(2) Uani 1 1 d . . . N1 N 0.3764(4) 0.3415(4) 0.09944(19) 0.0284(13) Uani 1 1 d . . . O2 O 0.5294(4) 0.3233(4) 0.0723(2) 0.0486(16) Uani 1 1 d . . . O10 O 0.5353(11) -0.3135(10) 0.2383(6) 0.196(8) Uani 1 1 d . . . O5 O 0.4336(13) 0.4562(15) 0.0151(8) 0.420(12) Uani 1 1 d . . . O11 O 0.6708(14) -0.3208(11) 0.2007(6) 0.238(9) Uani 1 1 d . . . O9 O 0.862(3) 0.1592(19) 0.3373(11) 0.85(2) Uani 1 1 d . . . O7 O 0.1697(14) 0.2193(17) 0.1041(12) 0.351(17) Uani 1 1 d . . . O8 O 0.6572(4) 0.2751(5) 0.0348(2) 0.0593(19) Uani 1 1 d . . . O6 O 0.1720(7) 0.2001(10) 0.0312(6) 0.173(7) Uani 1 1 d . . . O12 O 0.549(3) -0.425(3) 0.094(2) 0.79(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01805(15) 0.02327(15) 0.01765(15) -0.00025(14) 0.00295(11) 0.00587(14) Fe1 0.0199(5) 0.0230(5) 0.0156(4) 0.0000(4) 0.0030(4) 0.0082(4) N12 0.034(4) 0.042(4) 0.029(3) 0.005(3) 0.001(3) 0.002(3) N7 0.024(3) 0.024(3) 0.025(3) 0.000(2) 0.006(2) 0.005(2) C2 0.022(3) 0.028(3) 0.017(3) -0.001(3) 0.002(3) 0.001(3) C1 0.024(3) 0.027(3) 0.021(3) 0.000(3) 0.006(3) 0.010(3) C12 0.021(3) 0.023(3) 0.022(3) 0.001(3) 0.009(3) 0.009(3) N2 0.023(3) 0.024(3) 0.018(3) 0.000(2) 0.005(2) 0.007(2) C11 0.021(3) 0.015(3) 0.025(3) -0.004(3) 0.003(3) 0.003(3) O4 0.024(3) 0.048(3) 0.037(3) 0.006(2) 0.012(2) 0.006(2) C13 0.015(3) 0.018(3) 0.029(3) -0.002(3) 0.008(3) 0.005(3) C10 0.034(4) 0.031(4) 0.031(4) 0.000(3) -0.003(3) 0.003(3) N10 0.023(3) 0.022(3) 0.022(3) 0.001(2) 0.005(2) 0.004(2) C19 0.018(3) 0.025(3) 0.027(3) 0.011(3) 0.009(3) 0.005(3) C6 0.030(4) 0.029(4) 0.028(4) 0.005(3) 0.007(3) 0.004(3) C24 0.034(4) 0.054(5) 0.030(4) 0.015(4) -0.002(3) 0.004(4) C8 0.037(5) 0.026(4) 0.062(6) -0.001(4) -0.004(4) 0.006(3) N11 0.025(3) 0.016(3) 0.031(3) 0.002(2) 0.005(3) 0.001(2) C5 0.025(4) 0.036(4) 0.015(3) 0.000(3) -0.001(3) 0.005(3) C3 0.032(4) 0.025(3) 0.023(3) -0.001(3) -0.006(3) 0.013(3) C9 0.034(4) 0.035(4) 0.052(5) -0.020(4) -0.008(4) 0.006(4) N3 0.048(4) 0.036(4) 0.056(5) -0.003(3) -0.020(4) 0.015(3) C4 0.024(4) 0.045(4) 0.024(4) 0.008(3) 0.005(3) 0.009(3) O3 0.040(3) 0.056(4) 0.038(3) -0.009(3) -0.013(3) 0.014(3) C14 0.018(3) 0.023(3) 0.032(4) -0.009(3) 0.008(3) 0.005(3) N6 0.054(5) 0.054(5) 0.035(4) 0.011(3) 0.003(3) -0.006(4) C20 0.020(3) 0.029(3) 0.029(4) 0.015(3) 0.009(3) 0.004(3) C21 0.027(4) 0.033(4) 0.038(4) 0.013(3) 0.008(3) 0.005(3) C23 0.029(4) 0.060(6) 0.051(5) 0.033(5) 0.008(4) 0.013(4) N8 0.015(2) 0.015(2) 0.022(3) 0.000(2) 0.004(2) 0.002(2) C15 0.035(4) 0.021(3) 0.053(5) -0.008(3) 0.006(4) 0.003(3) C18 0.038(4) 0.042(4) 0.031(4) -0.016(3) 0.005(3) 0.000(4) O1 0.033(3) 0.112(6) 0.027(3) -0.026(3) 0.007(2) -0.023(4) C16 0.043(5) 0.027(4) 0.076(7) -0.026(4) -0.005(5) 0.002(4) N9 0.025(3) 0.043(4) 0.028(3) -0.010(3) 0.005(3) -0.004(3) C22 0.038(4) 0.038(4) 0.041(4) 0.020(4) 0.004(4) 0.012(4) N5 0.045(4) 0.076(6) 0.032(4) 0.003(4) 0.000(3) -0.009(4) C7 0.028(4) 0.023(3) 0.041(4) 0.004(3) 0.002(3) 0.004(3) C17 0.046(5) 0.045(5) 0.054(6) -0.031(4) 0.000(4) -0.006(4) N4 0.048(5) 0.090(6) 0.042(4) 0.031(4) 0.010(4) -0.002(4) N1 0.025(3) 0.034(3) 0.026(3) 0.001(3) 0.005(3) 0.004(3) O2 0.049(3) 0.048(3) 0.060(4) 0.031(3) 0.036(3) 0.026(3) O10 0.193(19) 0.170(13) 0.203(19) -0.045(12) 0.001(13) -0.048(11) O5 0.403(18) 0.372(18) 0.65(3) 0.444(18) 0.464(18) 0.320(15) O11 0.44(2) 0.138(12) 0.220(15) -0.054(11) 0.251(17) -0.079(14) O9 2.00(6) 0.294(19) 0.64(3) -0.296(12) 1.10(3) -0.517 O7 0.185(19) 0.25(2) 0.58(5) 0.20(3) 0.00(2) 0.037(17) O8 0.066(4) 0.070(4) 0.053(4) 0.028(3) 0.036(3) 0.028(4) O6 0.066(7) 0.145(11) 0.276(18) 0.029(11) -0.025(9) 0.027(7) O12 0.52(5) 0.69(6) 1.29(12) 0.78(7) 0.50(6) 0.44(5) _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 O2 2.396(6) . ? Tb1 O3 2.417(5) . ? Tb1 O4 2.431(5) . ? Tb1 O1 2.464(6) . ? Tb1 N1 2.475(6) . ? Tb1 N2 2.488(5) 3_545 ? Tb1 N8 2.554(5) . ? Tb1 N7 2.588(6) . ? Tb1 N9 2.616(7) . ? Fe1 C2 1.923(7) . ? Fe1 C1 1.924(7) . ? Fe1 C6 1.929(7) . ? Fe1 C4 1.934(8) . ? Fe1 C5 1.937(7) . ? Fe1 C3 1.945(7) . ? N12 C24 1.323(9) . ? N12 C20 1.375(9) . ? N7 C7 1.353(9) . ? N7 C11 1.365(8) . ? C2 N2 1.154(8) . ? C1 N1 1.142(9) . ? C12 N8 1.341(8) . ? C12 N10 1.349(8) . ? C12 C11 1.477(9) . ? N2 Tb1 2.488(5) 3_455 ? C11 C10 1.364(9) . ? C13 N11 1.324(8) . ? C13 N8 1.343(8) . ? C13 C14 1.476(9) . ? C10 C9 1.392(11) . ? N10 C19 1.320(8) . ? C19 N11 1.336(9) . ? C19 C20 1.492(9) . ? C6 N6 1.153(10) . ? C24 C23 1.392(12) . ? C8 C7 1.373(11) . ? C8 C9 1.392(12) . ? C5 N5 1.136(9) . ? C3 N3 1.151(9) . ? C4 N4 1.151(10) . ? C14 N9 1.331(9) . ? C14 C15 1.385(10) . ? C20 C21 1.390(10) . ? C21 C22 1.393(10) . ? C23 C22 1.375(12) . ? C15 C16 1.382(11) . ? C18 N9 1.341(9) . ? C18 C17 1.378(12) . ? C16 C17 1.361(13) . ? O10 O10 1.48(3) 2_655 ? O11 O9 1.22(5) 4_645 ? O9 O11 1.22(5) 4_655 ? 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 O2 Tb1 O3 96.4(2) . . ? O2 Tb1 O4 138.39(18) . . ? O3 Tb1 O4 77.4(2) . . ? O2 Tb1 O1 70.6(2) . . ? O3 Tb1 O1 67.7(2) . . ? O4 Tb1 O1 137.80(19) . . ? O2 Tb1 N1 69.26(19) . . ? O3 Tb1 N1 71.7(2) . . ? O4 Tb1 N1 69.78(19) . . ? O1 Tb1 N1 117.6(2) . . ? O2 Tb1 N2 74.49(18) . 3_545 ? O3 Tb1 N2 135.35(19) . 3_545 ? O4 Tb1 N2 137.11(17) . 3_545 ? O1 Tb1 N2 68.11(18) . 3_545 ? N1 Tb1 N2 137.28(19) . 3_545 ? O2 Tb1 N8 129.69(19) . . ? O3 Tb1 N8 133.67(19) . . ? O4 Tb1 N8 70.85(17) . . ? O1 Tb1 N8 118.3(2) . . ? N1 Tb1 N8 124.05(18) . . ? N2 Tb1 N8 66.25(17) 3_545 . ? O2 Tb1 N7 78.4(2) . . ? O3 Tb1 N7 145.28(18) . . ? O4 Tb1 N7 84.01(18) . . ? O1 Tb1 N7 137.98(18) . . ? N1 Tb1 N7 74.45(18) . . ? N2 Tb1 N7 76.85(17) 3_545 . ? N8 Tb1 N7 63.32(17) . . ? O2 Tb1 N9 143.3(2) . . ? O3 Tb1 N9 78.02(19) . . ? O4 Tb1 N9 76.43(19) . . ? O1 Tb1 N9 73.8(2) . . ? N1 Tb1 N9 138.43(19) . . ? N2 Tb1 N9 84.24(18) 3_545 . ? N8 Tb1 N9 62.49(17) . . ? N7 Tb1 N9 125.75(18) . . ? C2 Fe1 C1 176.9(3) . . ? C2 Fe1 C6 90.1(3) . . ? C1 Fe1 C6 91.9(3) . . ? C2 Fe1 C4 93.2(3) . . ? C1 Fe1 C4 84.7(3) . . ? C6 Fe1 C4 175.8(3) . . ? C2 Fe1 C5 87.3(3) . . ? C1 Fe1 C5 90.3(3) . . ? C6 Fe1 C5 89.6(3) . . ? C4 Fe1 C5 87.9(3) . . ? C2 Fe1 C3 92.0(3) . . ? C1 Fe1 C3 90.5(3) . . ? C6 Fe1 C3 89.8(3) . . ? C4 Fe1 C3 92.7(3) . . ? C5 Fe1 C3 179.1(3) . . ? C24 N12 C20 115.8(7) . . ? C7 N7 C11 115.9(6) . . ? C7 N7 Tb1 122.9(5) . . ? C11 N7 Tb1 121.2(4) . . ? N2 C2 Fe1 174.6(6) . . ? N1 C1 Fe1 174.6(6) . . ? N8 C12 N10 123.9(6) . . ? N8 C12 C11 118.5(6) . . ? N10 C12 C11 117.7(6) . . ? C2 N2 Tb1 149.9(5) . 3_455 ? C10 C11 N7 123.5(6) . . ? C10 C11 C12 121.3(6) . . ? N7 C11 C12 115.2(6) . . ? N11 C13 N8 124.8(6) . . ? N11 C13 C14 118.4(6) . . ? N8 C13 C14 116.7(6) . . ? C11 C10 C9 119.9(7) . . ? C19 N10 C12 115.1(6) . . ? N10 C19 N11 125.8(6) . . ? N10 C19 C20 118.0(6) . . ? N11 C19 C20 116.2(6) . . ? N6 C6 Fe1 179.1(8) . . ? N12 C24 C23 124.0(8) . . ? C7 C8 C9 119.6(7) . . ? C13 N11 C19 114.9(6) . . ? N5 C5 Fe1 178.5(7) . . ? N3 C3 Fe1 179.2(7) . . ? C8 C9 C10 117.4(7) . . ? N4 C4 Fe1 173.2(8) . . ? N9 C14 C15 123.2(7) . . ? N9 C14 C13 116.9(6) . . ? C15 C14 C13 119.9(7) . . ? N12 C20 C21 123.6(6) . . ? N12 C20 C19 116.2(6) . . ? C21 C20 C19 120.2(7) . . ? C20 C21 C22 118.8(8) . . ? C22 C23 C24 120.1(7) . . ? C12 N8 C13 115.4(5) . . ? C12 N8 Tb1 121.3(4) . . ? C13 N8 Tb1 122.6(4) . . ? C16 C15 C14 117.9(8) . . ? N9 C18 C17 122.3(8) . . ? C17 C16 C15 119.3(8) . . ? C14 N9 C18 117.8(7) . . ? C14 N9 Tb1 120.8(4) . . ? C18 N9 Tb1 121.3(5) . . ? C23 C22 C21 117.6(8) . . ? N7 C7 C8 123.7(7) . . ? C16 C17 C18 119.5(8) . . ? C1 N1 Tb1 172.4(6) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.830 _refine_diff_density_min -2.146 _refine_diff_density_rms 0.164 # Attachment 'compound7.txt' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 296499' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tetra-agua-(2,4,6-tri(2-pyridyl)-1,3,5- triazine)-tetracyano-cobalt(iii)-samarium(iii) octahydrate ; _chemical_formula_moiety '[Sm(tptz)(H2O)4Co(CN)6]8H2O' _chemical_formula_sum 'C24 H36 Co N12 O12 Sm' _chemical_formula_weight 893.93 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 15.813(3) _cell_length_b 14.070(3) _cell_length_c 31.523(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.31(3) _cell_angle_gamma 90.00 _cell_volume 6825(2) _cell_formula_units_Z 6 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2694 _exptl_absorpt_coefficient_mu 1.700 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20483 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.37 _reflns_number_total 7758 _reflns_number_gt 5905 _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^)+(0.0582P)^2^+56.0429P] 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 7758 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 1.555 _refine_ls_shift/su_mean 0.020 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.465205(19) 0.30814(2) 0.103967(10) 0.01559(10) Uani 1 1 d . . . Co1 Co 0.25708(5) -0.00293(6) 0.10748(2) 0.01509(18) Uani 1 1 d . . . N12 N 0.6896(4) 0.4983(5) 0.32152(19) 0.0360(15) Uani 1 1 d . . . N7 N 0.5351(3) 0.2076(4) 0.17287(18) 0.0214(12) Uani 1 1 d . . . C1 C 0.3323(4) 0.0962(5) 0.10014(19) 0.0194(13) Uani 1 1 d . . . N8 N 0.5234(3) 0.3984(4) 0.17602(15) 0.0152(10) Uani 1 1 d . . . C13 C 0.5232(4) 0.4939(4) 0.17831(19) 0.0163(12) Uani 1 1 d . . . C11 C 0.5710(4) 0.2501(5) 0.2114(2) 0.0235(14) Uani 1 1 d . . . C12 C 0.5675(4) 0.3545(4) 0.21216(19) 0.0172(12) Uani 1 1 d . . . N11 N 0.5610(3) 0.5440(4) 0.21294(17) 0.0197(11) Uani 1 1 d . . . C2 C 0.1775(4) -0.0969(5) 0.11557(18) 0.0195(13) Uani 1 1 d . . . C5 C 0.1666(4) 0.0534(5) 0.0657(2) 0.0218(14) Uani 1 1 d . . . N9 N 0.4449(3) 0.4935(4) 0.10323(17) 0.0230(12) Uani 1 1 d . . . N1 N 0.3760(4) 0.1603(4) 0.09757(18) 0.0268(13) Uani 1 1 d . . . N2 N 0.6244(3) 0.3479(4) 0.11755(16) 0.0212(11) Uani 1 1 d . . . O1 O 0.5319(4) 0.1807(4) 0.0718(2) 0.0468(15) Uani 1 1 d . . . C19 C 0.6056(4) 0.4940(5) 0.24653(19) 0.0197(13) Uani 1 1 d . . . O4 O 0.3475(3) 0.3300(4) 0.14231(16) 0.0377(13) Uani 1 1 d . . . C10 C 0.6108(5) 0.2000(6) 0.2489(3) 0.040(2) Uani 1 1 d . . . H10 H 0.6360 0.2323 0.2752 0.048 Uiso 1 1 calc R . . C7 C 0.5395(4) 0.1126(5) 0.1720(3) 0.0330(17) Uani 1 1 d . . . H7 H 0.5159 0.0808 0.1453 0.040 Uiso 1 1 calc R . . N10 N 0.6108(3) 0.3994(4) 0.24831(16) 0.0219(12) Uani 1 1 d . . . N3 N 0.4033(4) -0.0966(5) 0.1737(2) 0.0418(17) Uani 1 1 d . . . C14 C 0.4789(4) 0.5463(4) 0.1387(2) 0.0196(13) Uani 1 1 d . . . C6 C 0.2265(4) 0.0749(5) 0.1507(2) 0.0247(15) Uani 1 1 d . . . C4 C 0.2880(4) -0.0749(5) 0.0628(2) 0.0228(14) Uani 1 1 d . . . N4 N 0.3055(5) -0.1187(5) 0.0354(2) 0.0416(16) Uani 1 1 d . . . O2 O 0.5047(3) 0.3680(5) 0.03646(16) 0.0569(19) Uani 1 1 d . . . C22 C 0.7169(5) 0.6944(6) 0.3165(3) 0.0396(19) Uani 1 1 d . . . H22 H 0.7253 0.7610 0.3150 0.048 Uiso 1 1 calc R . . N5 N 0.1112(4) 0.0859(5) 0.0400(2) 0.0433(17) Uani 1 1 d . . . C3 C 0.3478(4) -0.0613(5) 0.1487(2) 0.0255(15) Uani 1 1 d . . . C20 C 0.6551(4) 0.5488(5) 0.2845(2) 0.0228(14) Uani 1 1 d . . . C24 C 0.7387(5) 0.5469(7) 0.3544(2) 0.040(2) Uani 1 1 d . . . H24 H 0.7646 0.5132 0.3802 0.047 Uiso 1 1 calc R . . C9 C 0.6127(5) 0.1026(6) 0.2465(3) 0.056(3) Uani 1 1 d . . . H9 H 0.6387 0.0661 0.2714 0.068 Uiso 1 1 calc R . . C8 C 0.5767(5) 0.0590(5) 0.2080(3) 0.048(2) Uani 1 1 d . . . H8 H 0.5772 -0.0084 0.2060 0.058 Uiso 1 1 calc R . . C15 C 0.4728(4) 0.6446(5) 0.1393(3) 0.0336(17) Uani 1 1 d . . . H15 H 0.4972 0.6798 0.1649 0.040 Uiso 1 1 calc R . . C21 C 0.6662(5) 0.6441(5) 0.2816(2) 0.0315(16) Uani 1 1 d . . . H21 H 0.6393 0.6767 0.2556 0.038 Uiso 1 1 calc R . . C16 C 0.4299(5) 0.6897(6) 0.1013(3) 0.044(2) Uani 1 1 d . . . H16 H 0.4246 0.7570 0.1003 0.053 Uiso 1 1 calc R . . C17 C 0.3955(5) 0.6364(6) 0.0655(3) 0.042(2) Uani 1 1 d . . . H17 H 0.3654 0.6662 0.0394 0.050 Uiso 1 1 calc R . . C18 C 0.4043(5) 0.5396(6) 0.0672(2) 0.0320(17) Uani 1 1 d . . . H18 H 0.3805 0.5037 0.0418 0.038 Uiso 1 1 calc R . . C23 C 0.7542(5) 0.6430(7) 0.3532(3) 0.044(2) Uani 1 1 d . . . H23 H 0.7904 0.6737 0.3776 0.052 Uiso 1 1 calc R . . O5 O 0.6625(4) 0.2230(4) 0.03486(19) 0.0487(16) Uani 1 1 d . . . O3 O 0.3375(3) 0.3305(4) 0.04386(19) 0.0466(15) Uani 1 1 d . . . N6 N 0.2106(4) 0.1281(6) 0.1754(2) 0.0477(19) Uani 1 1 d . . . O9 O 0.8203(7) 0.3185(6) 0.2990(3) 0.106(3) Uani 1 1 d . . . O6 O 0.4194(7) 0.0444(7) 0.0091(3) 0.117(4) Uani 1 1 d . . . O8 O 0.1665(6) 0.2818(7) 0.1005(6) 0.169(7) Uani 1 1 d . . . O11 O 0.5344(8) -0.1801(9) 0.2399(4) 0.149(5) Uani 1 1 d . . . O10 O 0.5694(8) -0.1167(8) 0.1351(5) 0.156(5) Uani 1 1 d . . . O7 O 0.1673(6) 0.3038(8) 0.0254(6) 0.186(7) Uani 1 1 d . . . O12 O 0.5247(19) -0.0084(19) 0.0662(9) 0.359(13) Uiso 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 Sm1 0.01214(15) 0.01839(17) 0.01646(16) -0.00191(14) 0.00376(10) -0.00365(13) Co1 0.0125(4) 0.0197(4) 0.0133(4) 0.0003(3) 0.0035(3) -0.0058(3) N12 0.029(3) 0.055(4) 0.022(3) -0.009(3) 0.001(2) -0.003(3) N7 0.017(3) 0.013(3) 0.033(3) 0.002(2) 0.004(2) -0.003(2) C1 0.019(3) 0.022(3) 0.017(3) -0.003(3) 0.004(2) -0.010(3) N8 0.013(2) 0.016(3) 0.016(2) 0.001(2) 0.0035(19) -0.003(2) C13 0.013(3) 0.019(3) 0.019(3) -0.001(2) 0.007(2) -0.002(2) C11 0.018(3) 0.019(3) 0.031(4) 0.011(3) 0.001(3) -0.004(3) C12 0.019(3) 0.016(3) 0.017(3) 0.002(2) 0.005(2) -0.002(2) N11 0.018(3) 0.019(3) 0.023(3) -0.001(2) 0.007(2) -0.001(2) C2 0.017(3) 0.028(4) 0.012(3) 0.000(3) 0.000(2) 0.000(3) C5 0.024(3) 0.021(3) 0.020(3) -0.006(3) 0.005(3) -0.008(3) N9 0.021(3) 0.026(3) 0.021(3) 0.007(2) 0.002(2) 0.004(2) N1 0.028(3) 0.035(3) 0.020(3) -0.003(2) 0.010(2) -0.015(3) N2 0.020(3) 0.024(3) 0.019(3) 0.000(2) 0.002(2) -0.007(2) O1 0.047(3) 0.045(4) 0.063(4) -0.024(3) 0.043(3) -0.014(3) C19 0.017(3) 0.031(4) 0.013(3) -0.004(3) 0.007(2) -0.006(3) O4 0.023(2) 0.055(4) 0.038(3) -0.024(3) 0.013(2) -0.011(2) C10 0.036(4) 0.034(4) 0.039(4) 0.012(4) -0.016(3) -0.015(4) C7 0.021(3) 0.018(4) 0.056(5) 0.002(3) 0.001(3) -0.005(3) N10 0.024(3) 0.026(3) 0.015(3) 0.000(2) 0.002(2) -0.003(2) N3 0.035(4) 0.036(4) 0.046(4) 0.010(3) -0.009(3) -0.008(3) C14 0.014(3) 0.017(3) 0.028(3) 0.008(3) 0.004(2) 0.000(2) C6 0.016(3) 0.039(4) 0.019(3) -0.004(3) 0.003(2) -0.009(3) C4 0.021(3) 0.025(4) 0.024(3) 0.002(3) 0.007(3) -0.003(3) N4 0.055(4) 0.039(4) 0.034(4) -0.004(3) 0.017(3) 0.005(3) O2 0.027(3) 0.120(6) 0.022(3) 0.026(3) 0.005(2) 0.022(3) C22 0.033(4) 0.045(5) 0.041(4) -0.023(4) 0.009(3) -0.012(4) N5 0.038(4) 0.056(5) 0.029(3) 0.005(3) -0.006(3) 0.009(3) C3 0.021(3) 0.029(4) 0.024(3) 0.006(3) 0.001(3) -0.011(3) C20 0.021(3) 0.028(4) 0.020(3) -0.011(3) 0.007(3) -0.003(3) C24 0.027(4) 0.064(6) 0.024(4) -0.014(4) -0.001(3) 0.000(4) C9 0.041(5) 0.034(5) 0.073(6) 0.035(5) -0.031(4) -0.014(4) C8 0.031(4) 0.013(4) 0.088(7) 0.018(4) -0.011(4) -0.006(3) C15 0.025(4) 0.022(4) 0.051(5) 0.009(3) 0.003(3) -0.002(3) C21 0.029(4) 0.033(4) 0.034(4) -0.013(3) 0.011(3) -0.002(3) C16 0.030(4) 0.025(4) 0.074(6) 0.025(4) 0.004(4) -0.003(3) C17 0.037(4) 0.030(4) 0.053(5) 0.027(4) -0.002(4) 0.003(3) C18 0.030(4) 0.039(4) 0.026(4) 0.011(3) 0.004(3) 0.002(3) C23 0.030(4) 0.056(6) 0.041(5) -0.030(4) 0.002(3) -0.013(4) O5 0.054(4) 0.051(4) 0.055(4) -0.021(3) 0.041(3) -0.020(3) O3 0.031(3) 0.041(3) 0.052(3) 0.007(3) -0.022(2) -0.002(2) N6 0.038(4) 0.073(6) 0.031(4) -0.027(4) 0.006(3) -0.002(4) O9 0.155(9) 0.078(6) 0.120(7) -0.039(5) 0.100(7) -0.047(6) O6 0.169(10) 0.108(8) 0.110(7) -0.023(6) 0.104(7) 0.005(7) O8 0.065(6) 0.088(7) 0.36(2) -0.089(10) 0.064(9) -0.016(5) O11 0.141(12) 0.165(12) 0.152(11) -0.007(9) 0.056(9) 0.018(8) O10 0.129(9) 0.091(8) 0.225(14) -0.020(9) -0.008(9) -0.005(7) O7 0.062(6) 0.138(10) 0.308(18) 0.094(11) -0.057(8) -0.044(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.419(5) . ? Sm1 O3 2.451(5) . ? Sm1 O4 2.461(5) . ? Sm1 N1 2.495(6) . ? Sm1 O2 2.498(5) . ? Sm1 N2 2.517(5) . ? Sm1 N8 2.580(5) . ? Sm1 N7 2.614(5) . ? Sm1 N9 2.627(6) . ? Co1 C1 1.881(6) . ? Co1 C5 1.882(7) . ? Co1 C2 1.882(6) . ? Co1 C3 1.888(7) . ? Co1 C4 1.888(7) . ? Co1 C6 1.895(7) . ? N12 C24 1.332(9) . ? N12 C20 1.366(9) . ? N7 C7 1.339(8) . ? N7 C11 1.355(8) . ? C1 N1 1.151(8) . ? N8 C12 1.342(7) . ? N8 C13 1.346(8) . ? C13 N11 1.320(8) . ? C13 C14 1.480(8) . ? C11 C10 1.395(9) . ? C11 C12 1.469(9) . ? C12 N10 1.344(8) . ? N11 C19 1.330(8) . ? C2 N2 1.157(8) 3_445 ? C5 N5 1.143(8) . ? N9 C18 1.336(8) . ? N9 C14 1.347(8) . ? N2 C2 1.157(8) 3 ? C19 N10 1.333(8) . ? C19 C20 1.487(8) . ? C10 C9 1.373(11) . ? C7 C8 1.377(10) . ? N3 C3 1.149(9) . ? C14 C15 1.387(9) . ? C6 N6 1.149(9) . ? C4 N4 1.145(9) . ? C22 C23 1.377(12) . ? C22 C21 1.397(10) . ? C20 C21 1.358(10) . ? C24 C23 1.376(12) . ? C9 C8 1.362(12) . ? C15 C16 1.386(10) . ? C16 C17 1.360(12) . ? C17 C18 1.368(11) . ? O11 O11 1.38(2) 2_655 ? 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 Sm1 O3 97.6(2) . . ? O1 Sm1 O4 138.65(18) . . ? O3 Sm1 O4 77.4(2) . . ? O1 Sm1 N1 68.97(18) . . ? O3 Sm1 N1 72.20(19) . . ? O4 Sm1 N1 70.50(18) . . ? O1 Sm1 O2 71.0(2) . . ? O3 Sm1 O2 67.76(19) . . ? O4 Sm1 O2 137.92(19) . . ? N1 Sm1 O2 117.4(2) . . ? O1 Sm1 N2 73.78(18) . . ? O3 Sm1 N2 135.80(19) . . ? O4 Sm1 N2 136.75(16) . . ? N1 Sm1 N2 136.37(19) . . ? O2 Sm1 N2 68.49(17) . . ? O1 Sm1 N8 129.25(19) . . ? O3 Sm1 N8 132.91(18) . . ? O4 Sm1 N8 70.29(15) . . ? N1 Sm1 N8 124.18(16) . . ? O2 Sm1 N8 118.4(2) . . ? N2 Sm1 N8 66.48(16) . . ? O1 Sm1 N7 78.77(19) . . ? O3 Sm1 N7 145.83(17) . . ? O4 Sm1 N7 83.26(18) . . ? N1 Sm1 N7 74.90(17) . . ? O2 Sm1 N7 138.51(16) . . ? N2 Sm1 N7 76.33(16) . . ? N8 Sm1 N7 62.48(16) . . ? O1 Sm1 N9 142.81(18) . . ? O3 Sm1 N9 77.80(17) . . ? O4 Sm1 N9 77.04(17) . . ? N1 Sm1 N9 139.56(18) . . ? O2 Sm1 N9 73.3(2) . . ? N2 Sm1 N9 84.04(17) . . ? N8 Sm1 N9 62.43(16) . . ? N7 Sm1 N9 124.87(16) . . ? C1 Co1 C5 90.1(3) . . ? C1 Co1 C2 176.8(3) . . ? C5 Co1 C2 88.0(3) . . ? C1 Co1 C3 90.3(3) . . ? C5 Co1 C3 179.0(3) . . ? C2 Co1 C3 91.5(3) . . ? C1 Co1 C4 91.5(3) . . ? C5 Co1 C4 89.4(3) . . ? C2 Co1 C4 91.1(3) . . ? C3 Co1 C4 89.7(3) . . ? C1 Co1 C6 86.2(3) . . ? C5 Co1 C6 88.9(3) . . ? C2 Co1 C6 91.1(3) . . ? C3 Co1 C6 92.0(3) . . ? C4 Co1 C6 177.2(3) . . ? C24 N12 C20 116.4(7) . . ? C7 N7 C11 116.5(6) . . ? C7 N7 Sm1 122.5(5) . . ? C11 N7 Sm1 121.0(4) . . ? N1 C1 Co1 175.4(6) . . ? C12 N8 C13 114.9(5) . . ? C12 N8 Sm1 122.1(4) . . ? C13 N8 Sm1 122.3(4) . . ? N11 C13 N8 124.8(6) . . ? N11 C13 C14 117.9(6) . . ? N8 C13 C14 117.3(5) . . ? N7 C11 C10 123.3(6) . . ? N7 C11 C12 116.5(5) . . ? C10 C11 C12 120.2(6) . . ? N8 C12 N10 124.5(6) . . ? N8 C12 C11 117.4(5) . . ? N10 C12 C11 118.0(5) . . ? C13 N11 C19 115.6(5) . . ? N2 C2 Co1 174.6(5) 3_445 . ? N5 C5 Co1 178.7(7) . . ? C18 N9 C14 117.3(6) . . ? C18 N9 Sm1 121.6(5) . . ? C14 N9 Sm1 121.0(4) . . ? C1 N1 Sm1 170.3(5) . . ? C2 N2 Sm1 148.3(5) 3 . ? N11 C19 N10 125.3(6) . . ? N11 C19 C20 116.8(6) . . ? N10 C19 C20 117.9(6) . . ? C9 C10 C11 118.0(7) . . ? N7 C7 C8 123.0(7) . . ? C19 N10 C12 114.8(5) . . ? N9 C14 C15 123.0(6) . . ? N9 C14 C13 116.6(5) . . ? C15 C14 C13 120.4(6) . . ? N6 C6 Co1 174.5(7) . . ? N4 C4 Co1 179.0(7) . . ? C23 C22 C21 117.0(8) . . ? N3 C3 Co1 179.7(7) . . ? C21 C20 N12 122.6(6) . . ? C21 C20 C19 120.6(6) . . ? N12 C20 C19 116.8(6) . . ? N12 C24 C23 124.0(8) . . ? C8 C9 C10 119.3(7) . . ? C9 C8 C7 119.9(7) . . ? C16 C15 C14 117.8(7) . . ? C20 C21 C22 120.4(7) . . ? C17 C16 C15 119.1(7) . . ? C16 C17 C18 119.9(7) . . ? N9 C18 C17 122.8(7) . . ? C22 C23 C24 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 1.716 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.175 # Attachment 'compound8.txt' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 296500' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-N,N-dimethyl-formamide-tri-agua-(2,4,6- tri(2-pyridyl)-1,3,5-triazine)-tetracyano-iron(iii)-lanthamium(iii) pentahydrate ; _chemical_formula_moiety '[La(tptz)(DMF)(H2O)3Fe(CN)6]5H2O' _chemical_formula_sum 'C27 H35 Fe La N13 O9' _chemical_formula_weight 880.44 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 16.069(3) _cell_length_b 14.390(3) _cell_length_c 32.076(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.45(3) _cell_angle_gamma 90.00 _cell_volume 7243(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3544 _exptl_absorpt_coefficient_mu 1.631 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40258 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.35 _reflns_number_total 8648 _reflns_number_gt 7157 _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^)+(0.0655P)^2^+89.2252P] 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 8648 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 2.230 _refine_ls_shift/su_mean 0.036 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 La1 La 0.463872(19) 0.30502(2) 0.105635(9) 0.01794(10) Uani 1 1 d . . . Fe1 Fe 0.75974(5) 0.48810(6) 0.10827(2) 0.02204(18) Uani 1 1 d . . . N9 N 0.5360(3) 0.2123(3) 0.17755(16) 0.0262(10) Uani 1 1 d . . . N8 N 0.5262(3) 0.4009(3) 0.17760(14) 0.0220(9) Uani 1 1 d . . . C1 C 0.6797(4) 0.3942(4) 0.11551(17) 0.0243(11) Uani 1 1 d . . . N10 N 0.5621(3) 0.5442(4) 0.21347(16) 0.0305(11) Uani 1 1 d . . . C14 C 0.5684(4) 0.3591(4) 0.21343(18) 0.0265(12) Uani 1 1 d . . . C15 C 0.5730(4) 0.2557(4) 0.21409(19) 0.0288(13) Uani 1 1 d . . . C2 C 0.8354(4) 0.5873(4) 0.10219(19) 0.0275(12) Uani 1 1 d . . . N11 N 0.6090(4) 0.4032(4) 0.24848(16) 0.0326(12) Uani 1 1 d . . . C12 C 0.5256(4) 0.4941(4) 0.17940(18) 0.0247(11) Uani 1 1 d . . . N1 N 0.6264(3) 0.3421(4) 0.11803(16) 0.0286(11) Uani 1 1 d . . . C16 C 0.6136(6) 0.2098(5) 0.2505(2) 0.047(2) Uani 1 1 d . . . H16 H 0.6399 0.2433 0.2753 0.057 Uiso 1 1 calc R . . N7 N 0.4488(3) 0.4942(4) 0.10644(16) 0.0305(11) Uani 1 1 d . . . C3 C 0.6708(4) 0.5349(4) 0.06214(18) 0.0274(12) Uani 1 1 d . . . C4 C 0.7985(4) 0.4096(4) 0.0673(2) 0.0296(13) Uani 1 1 d . . . C13 C 0.6048(4) 0.4958(4) 0.24654(19) 0.0302(13) Uani 1 1 d . . . C19 C 0.5390(5) 0.1189(4) 0.1778(2) 0.0361(15) Uani 1 1 d . . . H19 H 0.5132 0.0864 0.1525 0.043 Uiso 1 1 calc R . . C6 C 0.7223(5) 0.5683(7) 0.1479(2) 0.053(2) Uani 1 1 d . . . C20 C 0.6521(4) 0.5500(5) 0.2835(2) 0.0352(15) Uani 1 1 d . . . C10 C 0.4771(5) 0.6418(4) 0.1415(2) 0.0397(16) Uani 1 1 d . . . H10 H 0.5008 0.6759 0.1666 0.048 Uiso 1 1 calc R . . C5 C 0.8474(5) 0.4367(5) 0.1538(2) 0.0390(16) Uani 1 1 d . . . C11 C 0.4825(4) 0.5453(4) 0.14114(19) 0.0272(12) Uani 1 1 d . . . C18 C 0.5781(6) 0.0681(5) 0.2133(3) 0.050(2) Uani 1 1 d . . . H18 H 0.5792 0.0021 0.2121 0.060 Uiso 1 1 calc R . . C9 C 0.4372(6) 0.6869(5) 0.1050(3) 0.052(2) Uani 1 1 d . . . H9 H 0.4337 0.7528 0.1042 0.062 Uiso 1 1 calc R . . C17 C 0.6151(6) 0.1134(5) 0.2499(2) 0.053(2) Uani 1 1 d . . . H17 H 0.6415 0.0795 0.2747 0.064 Uiso 1 1 calc R . . C8 C 0.4021(5) 0.6350(5) 0.0693(3) 0.0451(18) Uani 1 1 d . . . H8 H 0.3734 0.6647 0.0438 0.054 Uiso 1 1 calc R . . C7 C 0.4093(5) 0.5389(4) 0.0712(2) 0.0362(15) Uani 1 1 d . . . H7 H 0.3851 0.5036 0.0465 0.043 Uiso 1 1 calc R . . O1 O 0.3277(3) 0.3296(3) 0.05256(15) 0.0380(11) Uani 1 1 d . . . O2 O 0.5364(3) 0.1756(3) 0.07336(16) 0.0409(11) Uani 1 1 d . . . O3 O 0.3505(3) 0.3274(4) 0.14945(15) 0.0390(11) Uani 1 1 d . . . N2 N 0.8777(3) 0.6511(4) 0.10083(19) 0.0354(12) Uani 1 1 d . . . N4 N 0.8184(5) 0.3621(4) 0.0421(2) 0.0496(16) Uani 1 1 d . . . N3 N 0.6174(4) 0.5579(4) 0.03448(18) 0.0427(14) Uani 1 1 d . . . O4 O 0.4982(3) 0.3692(4) 0.03620(14) 0.0370(11) Uani 1 1 d . . . N12 N 0.6836(4) 0.4995(5) 0.31948(19) 0.0460(15) Uani 1 1 d . . . N5 N 0.8978(5) 0.4070(5) 0.1809(3) 0.069(2) Uani 1 1 d . . . C22 C 0.7146(6) 0.6904(6) 0.3146(3) 0.053(2) Uani 1 1 d . . . H22 H 0.7248 0.7552 0.3131 0.063 Uiso 1 1 calc R . . C24 C 0.7300(5) 0.5482(6) 0.3523(2) 0.052(2) Uani 1 1 d . . . H24 H 0.7520 0.5159 0.3782 0.062 Uiso 1 1 calc R . . C21 C 0.6655(5) 0.6437(5) 0.2799(2) 0.0433(17) Uani 1 1 d . . . H21 H 0.6418 0.6760 0.2543 0.052 Uiso 1 1 calc R . . C23 C 0.7479(5) 0.6423(6) 0.3508(3) 0.052(2) Uani 1 1 d . . . H23 H 0.7827 0.6726 0.3747 0.063 Uiso 1 1 calc R . . N6 N 0.7014(6) 0.6241(10) 0.1699(3) 0.126(5) Uani 1 1 d . . . N13 N 0.1843(4) 0.3432(4) 0.03484(18) 0.0379(13) Uani 1 1 d . . . C25 C 0.2539(5) 0.2989(5) 0.0507(2) 0.0405(16) Uiso 1 1 d . . . H25 H 0.2488 0.2385 0.0619 0.049 Uiso 1 1 calc R . . C26 C 0.1858(7) 0.4356(7) 0.0169(3) 0.068(3) Uiso 1 1 d . . . H26A H 0.2445 0.4519 0.0157 0.102 Uiso 1 1 calc R . . H26B H 0.1642 0.4806 0.0349 0.102 Uiso 1 1 calc R . . H26C H 0.1499 0.4368 -0.0119 0.102 Uiso 1 1 calc R . . C27 C 0.1011(6) 0.3023(7) 0.0343(3) 0.065(2) Uiso 1 1 d . . . H27A H 0.1085 0.2389 0.0457 0.097 Uiso 1 1 calc R . . H27B H 0.0675 0.3007 0.0049 0.097 Uiso 1 1 calc R . . H27C H 0.0712 0.3399 0.0520 0.097 Uiso 1 1 calc R . . O7 O 0.5021(9) -0.0064(9) 0.0630(4) 0.153(4) Uiso 1 1 d . . . O6 O 1.0000 0.3114(15) 0.2500 0.184(8) Uiso 1 2 d S . . O5 O 0.5421(14) 0.8995(15) 0.1297(7) 0.256(9) Uiso 1 1 d . . . O8 O 0.6687(5) 0.2129(5) 0.0369(2) 0.0719(18) Uiso 1 1 d . . . O9 O 0.1709(18) 0.3086(17) 0.1665(8) 0.301(12) Uiso 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 La1 0.01832(17) 0.01834(15) 0.01627(16) 0.00037(11) 0.00179(11) -0.00489(11) Fe1 0.0193(4) 0.0260(4) 0.0193(4) 0.0005(3) 0.0009(3) -0.0088(3) N9 0.027(3) 0.022(2) 0.027(2) 0.0038(19) 0.001(2) -0.0041(19) N8 0.024(2) 0.025(2) 0.016(2) 0.0004(17) 0.0036(18) -0.0056(19) C1 0.020(3) 0.030(3) 0.021(3) 0.004(2) 0.000(2) -0.007(2) N10 0.035(3) 0.028(2) 0.026(3) -0.007(2) 0.002(2) -0.005(2) C14 0.032(3) 0.027(3) 0.021(3) -0.001(2) 0.006(2) -0.005(2) C15 0.031(3) 0.027(3) 0.025(3) 0.003(2) -0.002(2) -0.007(2) C2 0.021(3) 0.027(3) 0.032(3) -0.002(2) -0.001(2) -0.005(2) N11 0.040(3) 0.035(3) 0.020(2) -0.002(2) 0.000(2) -0.013(2) C12 0.027(3) 0.025(3) 0.023(3) -0.002(2) 0.009(2) -0.003(2) N1 0.024(3) 0.033(3) 0.027(3) 0.004(2) -0.001(2) -0.005(2) C16 0.071(6) 0.033(3) 0.028(3) 0.007(3) -0.012(3) -0.015(3) N7 0.035(3) 0.027(2) 0.027(3) 0.002(2) 0.004(2) 0.001(2) C3 0.029(3) 0.027(3) 0.025(3) 0.001(2) 0.002(2) -0.009(2) C4 0.031(3) 0.023(3) 0.032(3) 0.002(2) 0.004(2) -0.006(2) C13 0.034(3) 0.034(3) 0.023(3) -0.006(2) 0.008(2) -0.010(3) C19 0.046(4) 0.025(3) 0.032(3) 0.002(2) -0.005(3) -0.006(3) C6 0.033(4) 0.087(6) 0.036(4) -0.028(4) 0.002(3) 0.001(4) C20 0.036(4) 0.042(3) 0.027(3) -0.015(3) 0.008(3) -0.016(3) C10 0.039(4) 0.025(3) 0.052(4) -0.004(3) 0.003(3) -0.005(3) C5 0.036(4) 0.039(4) 0.035(4) 0.010(3) -0.007(3) -0.013(3) C11 0.030(3) 0.022(3) 0.030(3) 0.001(2) 0.006(2) -0.002(2) C18 0.063(5) 0.027(3) 0.050(4) 0.009(3) -0.012(4) -0.005(3) C9 0.059(5) 0.025(3) 0.063(5) 0.012(3) -0.004(4) -0.001(3) C17 0.077(6) 0.036(4) 0.034(4) 0.014(3) -0.017(4) -0.005(4) C8 0.049(5) 0.033(3) 0.048(4) 0.018(3) -0.002(3) 0.004(3) C7 0.045(4) 0.030(3) 0.031(3) 0.007(3) 0.002(3) 0.001(3) O1 0.030(3) 0.049(3) 0.030(2) 0.006(2) -0.0048(19) -0.007(2) O2 0.047(3) 0.035(2) 0.045(3) -0.009(2) 0.020(2) -0.004(2) O3 0.026(2) 0.060(3) 0.032(2) -0.005(2) 0.0085(19) 0.002(2) N2 0.026(3) 0.026(3) 0.050(3) 0.004(2) 0.000(2) -0.009(2) N4 0.065(5) 0.042(3) 0.044(4) -0.002(3) 0.015(3) 0.008(3) N3 0.043(4) 0.048(3) 0.031(3) 0.007(3) -0.003(3) 0.001(3) O4 0.026(2) 0.058(3) 0.026(2) 0.012(2) 0.0030(18) 0.000(2) N12 0.042(4) 0.063(4) 0.032(3) -0.010(3) 0.005(3) -0.025(3) N5 0.066(5) 0.051(4) 0.068(5) 0.017(4) -0.032(4) -0.016(4) C22 0.052(5) 0.049(4) 0.056(5) -0.026(4) 0.009(4) -0.018(4) C24 0.051(5) 0.071(5) 0.031(4) -0.021(4) 0.002(3) -0.018(4) C21 0.048(4) 0.040(4) 0.041(4) -0.016(3) 0.008(3) -0.009(3) C23 0.041(4) 0.067(5) 0.046(4) -0.030(4) 0.003(3) -0.016(4) N6 0.057(6) 0.217(14) 0.096(7) -0.106(9) -0.002(5) 0.017(7) N13 0.032(3) 0.044(3) 0.034(3) -0.007(2) -0.002(2) 0.000(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 La1 O1 2.491(5) . ? La1 O2 2.533(5) . ? La1 O3 2.550(4) . ? La1 O4 2.578(4) . ? La1 N2 2.599(5) 3_445 ? La1 N1 2.610(5) . ? La1 N8 2.691(4) . ? La1 N9 2.700(5) . ? La1 N7 2.734(5) . ? Fe1 C6 1.907(7) . ? Fe1 C2 1.912(6) . ? Fe1 C1 1.915(5) . ? Fe1 C4 1.936(6) . ? Fe1 C3 1.942(6) . ? Fe1 C5 1.944(7) . ? N9 C15 1.348(8) . ? N9 C19 1.345(7) . ? N8 C12 1.342(7) . ? N8 C14 1.344(7) . ? C1 N1 1.154(7) . ? N10 C13 1.330(8) . ? N10 C12 1.335(7) . ? C14 N11 1.333(7) . ? C14 C15 1.490(8) . ? C15 C16 1.377(9) . ? C2 N2 1.149(8) . ? N11 C13 1.334(8) . ? C12 C11 1.470(8) . ? C16 C17 1.388(10) . ? N7 C7 1.336(8) . ? N7 C11 1.346(8) . ? C3 N3 1.143(8) . ? C4 N4 1.153(9) . ? C13 C20 1.486(8) . ? C19 C18 1.385(9) . ? C6 N6 1.167(11) . ? C20 N12 1.364(10) . ? C20 C21 1.374(10) . ? C10 C9 1.372(10) . ? C10 C11 1.392(8) . ? C5 N5 1.135(9) . ? C18 C17 1.363(11) . ? C9 C8 1.380(11) . ? C8 C7 1.387(9) . ? O1 C25 1.255(9) . ? N2 La1 2.599(5) 3 ? N12 C24 1.348(9) . ? C22 C23 1.357(13) . ? C22 C21 1.390(10) . ? C24 C23 1.388(12) . ? N13 C25 1.293(9) . ? N13 C26 1.452(11) . ? N13 C27 1.458(11) . ? 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 La1 O2 103.79(17) . . ? O1 La1 O3 74.47(16) . . ? O2 La1 O3 139.85(16) . . ? O1 La1 O4 71.26(15) . . ? O2 La1 O4 72.98(16) . . ? O3 La1 O4 137.92(15) . . ? O1 La1 N2 72.65(17) . 3_445 ? O2 La1 N2 68.62(17) . 3_445 ? O3 La1 N2 72.88(18) . 3_445 ? O4 La1 N2 117.67(17) . 3_445 ? O1 La1 N1 141.04(15) . . ? O2 La1 N1 71.31(17) . . ? O3 La1 N1 134.44(16) . . ? O4 La1 N1 70.43(15) . . ? N2 La1 N1 133.33(17) 3_445 . ? O1 La1 N8 128.56(16) . . ? O2 La1 N8 127.50(16) . . ? O3 La1 N8 68.91(15) . . ? O4 La1 N8 116.63(14) . . ? N2 La1 N8 125.66(16) 3_445 . ? N1 La1 N8 65.75(15) . . ? O1 La1 N9 143.70(15) . . ? O2 La1 N9 80.51(16) . . ? O3 La1 N9 79.51(16) . . ? O4 La1 N9 141.48(15) . . ? N2 La1 N9 75.80(16) 3_445 . ? N1 La1 N9 74.92(15) . . ? N8 La1 N9 60.58(14) . . ? O1 La1 N7 78.40(16) . . ? O2 La1 N7 141.76(15) . . ? O3 La1 N7 78.09(16) . . ? O4 La1 N7 71.79(16) . . ? N2 La1 N7 143.32(17) 3_445 . ? N1 La1 N7 83.25(16) . . ? N8 La1 N7 59.89(15) . . ? N9 La1 N7 120.44(15) . . ? C6 Fe1 C2 85.1(3) . . ? C6 Fe1 C1 91.7(3) . . ? C2 Fe1 C1 176.5(3) . . ? C6 Fe1 C4 178.5(4) . . ? C2 Fe1 C4 93.5(3) . . ? C1 Fe1 C4 89.6(2) . . ? C6 Fe1 C3 90.7(3) . . ? C2 Fe1 C3 92.5(2) . . ? C1 Fe1 C3 86.2(2) . . ? C4 Fe1 C3 88.6(3) . . ? C6 Fe1 C5 90.7(3) . . ? C2 Fe1 C5 89.3(3) . . ? C1 Fe1 C5 92.2(3) . . ? C4 Fe1 C5 90.1(3) . . ? C3 Fe1 C5 177.9(3) . . ? C15 N9 C19 116.7(5) . . ? C15 N9 La1 122.8(4) . . ? C19 N9 La1 120.5(4) . . ? C12 N8 C14 114.7(5) . . ? C12 N8 La1 123.0(4) . . ? C14 N8 La1 122.0(4) . . ? N1 C1 Fe1 174.5(5) . . ? C13 N10 C12 115.4(5) . . ? N11 C14 N8 125.0(5) . . ? N11 C14 C15 116.7(5) . . ? N8 C14 C15 118.3(5) . . ? N9 C15 C16 123.7(6) . . ? N9 C15 C14 116.1(5) . . ? C16 C15 C14 120.3(6) . . ? N2 C2 Fe1 174.3(6) . . ? C13 N11 C14 115.2(5) . . ? N10 C12 N8 124.7(5) . . ? N10 C12 C11 117.2(5) . . ? N8 C12 C11 118.1(5) . . ? C1 N1 La1 148.8(5) . . ? C15 C16 C17 118.4(6) . . ? C7 N7 C11 118.1(5) . . ? C7 N7 La1 119.9(4) . . ? C11 N7 La1 122.0(4) . . ? N3 C3 Fe1 176.6(6) . . ? N4 C4 Fe1 177.4(6) . . ? N10 C13 N11 125.0(6) . . ? N10 C13 C20 116.7(6) . . ? N11 C13 C20 118.4(6) . . ? N9 C19 C18 122.8(6) . . ? N6 C6 Fe1 173.7(11) . . ? N12 C20 C21 123.9(6) . . ? N12 C20 C13 115.3(6) . . ? C21 C20 C13 120.7(6) . . ? C9 C10 C11 118.9(7) . . ? N5 C5 Fe1 178.8(8) . . ? N7 C11 C10 122.4(6) . . ? N7 C11 C12 116.8(5) . . ? C10 C11 C12 120.8(6) . . ? C17 C18 C19 119.5(7) . . ? C10 C9 C8 118.9(6) . . ? C18 C17 C16 118.9(6) . . ? C9 C8 C7 119.2(7) . . ? N7 C7 C8 122.4(7) . . ? C25 O1 La1 131.6(4) . . ? C2 N2 La1 172.3(5) . 3 ? C24 N12 C20 115.2(7) . . ? C23 C22 C21 119.3(8) . . ? N12 C24 C23 124.3(8) . . ? C20 C21 C22 118.6(8) . . ? C22 C23 C24 118.7(7) . . ? C25 N13 C26 121.4(7) . . ? C25 N13 C27 121.3(7) . . ? C26 N13 C27 117.3(7) . . ? O1 C25 N13 125.0(7) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.461 _refine_diff_density_min -1.369 _refine_diff_density_rms 0.171 # Attachment 'compound9.txt' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 296501' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-tri-N,N-dimethyl-formamide-agua- (3,4,7,8-tetramethyl-1,10-phenanthroline)-tetracyano-iron(iii)- samarium(iii) dihydrate ; _chemical_formula_moiety '[Sm(tmphen)(DMF)3(H2O)Fe(CN)6]2H2O' _chemical_formula_sum 'C31 H43 Fe N11 O6 Sm' _chemical_formula_weight 871.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7240(19) _cell_length_b 13.477(3) _cell_length_c 16.552(3) _cell_angle_alpha 74.62(3) _cell_angle_beta 88.44(3) _cell_angle_gamma 81.45(3) _cell_volume 2068.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.807 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12589 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.61 _reflns_number_total 9062 _reflns_number_gt 7392 _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^)+(0.0974P)^2^+2.4090P] 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 9062 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.122 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.13212(3) 0.62950(3) 0.22862(2) 0.01791(12) Uani 1 1 d . . . Fe1 Fe 0.5000 0.5000 0.5000 0.0192(3) Uani 1 2 d S . . Fe2 Fe 0.0000 1.0000 0.0000 0.0208(3) Uani 1 2 d S . . N8 N 0.0033(6) 0.5399(4) 0.1394(3) 0.0180(11) Uani 1 1 d . . . O4 O 0.0537(5) 0.4816(4) 0.3242(3) 0.0270(11) Uiso 1 1 d . . . N7 N 0.2682(6) 0.4664(4) 0.1949(4) 0.0221(12) Uani 1 1 d . . . O1 O 0.3275(5) 0.6823(4) 0.1515(3) 0.0269(11) Uani 1 1 d . . . C3 C 0.6543(8) 0.5423(6) 0.4298(5) 0.0285(16) Uani 1 1 d . . . O2 O -0.0931(5) 0.6859(4) 0.2758(3) 0.0325(12) Uani 1 1 d . . . C13 C -0.0168(7) 0.3830(5) 0.0985(4) 0.0209(13) Uani 1 1 d . . . C2 C 0.0126(7) 0.8578(5) 0.0660(4) 0.0219(14) Uani 1 1 d . . . N2 N 0.0274(6) 0.7734(4) 0.1086(4) 0.0224(12) Uani 1 1 d . . . N1 N 0.3029(6) 0.5719(5) 0.3473(4) 0.0262(13) Uani 1 1 d . . . N11 N -0.0117(7) 0.3550(5) 0.4316(4) 0.0295(14) Uani 1 1 d . . . C16 C -0.1257(7) 0.5769(5) 0.1126(4) 0.0222(14) Uani 1 1 d . . . H16 H -0.1629 0.6448 0.1165 0.027 Uiso 1 1 calc R . . O3 O 0.1660(6) 0.7817(4) 0.2703(4) 0.0396(14) Uani 1 1 d . . . C1 C 0.3760(7) 0.5457(5) 0.4036(4) 0.0223(14) Uani 1 1 d . . . C18 C 0.1993(7) 0.4048(5) 0.1621(4) 0.0193(13) Uani 1 1 d . . . N9 N 0.4944(6) 0.7846(5) 0.1360(4) 0.0319(14) Uani 1 1 d . . . C29 C 0.0563(8) 0.4340(5) 0.3994(4) 0.0260(15) Uani 1 1 d . . . H29 H 0.1109 0.4557 0.4364 0.031 Uiso 1 1 calc R . . N5 N 0.2660(7) 1.0098(5) 0.0943(5) 0.0393(17) Uani 1 1 d . . . C23 C 0.3836(8) 0.7572(6) 0.1118(5) 0.0322(17) Uani 1 1 d . . . H23 H 0.3423 0.7974 0.0598 0.039 Uiso 1 1 calc R . . C5 C 0.1664(8) 1.0087(6) 0.0591(5) 0.0292(16) Uani 1 1 d . . . C15 C -0.2123(7) 0.5219(5) 0.0782(4) 0.0207(13) Uani 1 1 d . . . C14 C -0.1566(7) 0.4235(5) 0.0713(4) 0.0212(13) Uani 1 1 d . . . C6 C -0.1180(7) 1.0437(6) 0.0853(5) 0.0279(16) Uani 1 1 d . . . C17 C 0.0582(7) 0.4442(5) 0.1330(4) 0.0187(13) Uani 1 1 d . . . C4 C 0.5371(8) 0.3611(7) 0.4824(5) 0.0316(17) Uani 1 1 d . . . C22 C -0.3568(7) 0.5726(6) 0.0507(5) 0.0276(15) Uani 1 1 d . . . H22A H -0.3747 0.5660 -0.0054 0.041 Uiso 1 1 calc R . . H22B H -0.3668 0.6465 0.0495 0.041 Uiso 1 1 calc R . . H22C H -0.4235 0.5388 0.0900 0.041 Uiso 1 1 calc R . . C12 C 0.0515(8) 0.2839(6) 0.0915(5) 0.0275(15) Uani 1 1 d . . . H12 H 0.0025 0.2424 0.0677 0.033 Uiso 1 1 calc R . . C7 C 0.3990(7) 0.4306(6) 0.2203(4) 0.0255(15) Uani 1 1 d . . . C11 C 0.1836(8) 0.2485(6) 0.1179(5) 0.0301(16) Uani 1 1 d . . . H11 H 0.2253 0.1827 0.1117 0.036 Uiso 1 1 calc R . . C8 C 0.4709(7) 0.3338(6) 0.2168(5) 0.0272(15) Uani 1 1 d . . . C10 C 0.2635(7) 0.3057(5) 0.1547(5) 0.0250(15) Uani 1 1 d . . . N4 N 0.5554(9) 0.2767(6) 0.4732(5) 0.0456(18) Uani 1 1 d . . . C21 C -0.2425(8) 0.3601(6) 0.0363(5) 0.0307(17) Uani 1 1 d . . . H21A H -0.3414 0.3831 0.0434 0.046 Uiso 1 1 calc R . . H21B H -0.2189 0.2864 0.0661 0.046 Uiso 1 1 calc R . . H21C H -0.2230 0.3694 -0.0234 0.046 Uiso 1 1 calc R . . C19 C 0.6179(8) 0.3037(7) 0.2514(5) 0.0372(18) Uani 1 1 d . . . H19A H 0.6176 0.2564 0.3077 0.056 Uiso 1 1 calc R . . H19B H 0.6554 0.3662 0.2542 0.056 Uiso 1 1 calc R . . H19C H 0.6758 0.2688 0.2147 0.056 Uiso 1 1 calc R . . C9 C 0.4016(8) 0.2696(6) 0.1836(5) 0.0300(16) Uani 1 1 d . . . N3 N 0.7491(7) 0.5701(6) 0.3895(5) 0.0421(17) Uani 1 1 d . . . C20 C 0.4756(9) 0.1641(7) 0.1813(8) 0.053(3) Uani 1 1 d . . . H20A H 0.5643 0.1717 0.1525 0.079 Uiso 1 1 calc R . . H20B H 0.4177 0.1317 0.1512 0.079 Uiso 1 1 calc R . . H20C H 0.4929 0.1203 0.2386 0.079 Uiso 1 1 calc R . . N6 N -0.1868(7) 1.0662(5) 0.1363(5) 0.0396(17) Uani 1 1 d . . . C30 C -0.0991(11) 0.3180(8) 0.3797(6) 0.048(2) Uani 1 1 d . . . H30A H -0.1074 0.3657 0.3234 0.072 Uiso 1 1 calc R . . H30B H -0.1916 0.3147 0.4045 0.072 Uiso 1 1 calc R . . H32C H -0.0574 0.2485 0.3762 0.072 Uiso 1 1 calc R . . C31 C -0.0152(11) 0.3095(8) 0.5209(5) 0.047(2) Uani 1 1 d . . . H31A H 0.0283 0.3515 0.5501 0.070 Uiso 1 1 calc R . . H31B H 0.0357 0.2386 0.5346 0.070 Uiso 1 1 calc R . . H31C H -0.1120 0.3075 0.5387 0.070 Uiso 1 1 calc R . . C25 C 0.5655(10) 0.8676(7) 0.0906(7) 0.055(3) Uani 1 1 d . . . H25A H 0.5221 0.8982 0.0351 0.082 Uiso 1 1 calc R . . H25B H 0.6633 0.8405 0.0843 0.082 Uiso 1 1 calc R . . H25C H 0.5599 0.9210 0.1214 0.082 Uiso 1 1 calc R . . C24 C 0.5530(10) 0.7274(9) 0.2207(6) 0.055(3) Uani 1 1 d . . . H24A H 0.4953 0.6744 0.2476 0.083 Uiso 1 1 calc R . . H24B H 0.5542 0.7765 0.2550 0.083 Uiso 1 1 calc R . . H24C H 0.6481 0.6938 0.2152 0.083 Uiso 1 1 calc R . . O5 O -0.2246(8) 0.8829(6) 0.2695(5) 0.0555(17) Uiso 1 1 d . . . N10 N 0.1642(10) 0.9316(6) 0.3039(6) 0.057(2) Uani 1 1 d . . . C28 C 0.1005(17) 1.0443(9) 0.2875(9) 0.086(4) Uani 1 1 d . . . H28A H 0.0136 1.0560 0.2554 0.129 Uiso 1 1 calc R . . H28B H 0.1654 1.0885 0.2555 0.129 Uiso 1 1 calc R . . H28C H 0.0810 1.0616 0.3410 0.129 Uiso 1 1 calc R . . C27 C 0.2720(17) 0.8887(13) 0.3668(10) 0.102(5) Uani 1 1 d . . . H27A H 0.2792 0.8127 0.3834 0.153 Uiso 1 1 calc R . . H27B H 0.2493 0.9155 0.4158 0.153 Uiso 1 1 calc R . . H27C H 0.3609 0.9087 0.3440 0.153 Uiso 1 1 calc R . . O6 O 0.299(3) 0.186(2) 0.4133(17) 0.266(11) Uiso 1 1 d . . . C26 C 0.1214(9) 0.8718(6) 0.2625(6) 0.0387(19) Uani 1 1 d . . . H26 H 0.0485 0.9022 0.2225 0.046 Uiso 1 1 calc R . . H7 H 0.456(6) 0.482(5) 0.245(4) 0.003(14) Uiso 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 Sm1 0.01484(18) 0.01982(18) 0.01931(18) -0.00409(12) -0.00388(11) -0.00452(12) Fe1 0.0122(6) 0.0302(7) 0.0155(6) -0.0046(5) -0.0018(5) -0.0064(5) Fe2 0.0158(7) 0.0161(6) 0.0291(7) -0.0041(5) -0.0021(5) -0.0005(5) N8 0.017(3) 0.021(3) 0.016(3) -0.005(2) -0.001(2) -0.004(2) N7 0.019(3) 0.025(3) 0.023(3) -0.008(2) -0.004(2) -0.002(2) O1 0.025(3) 0.029(3) 0.027(3) -0.005(2) 0.002(2) -0.011(2) C3 0.022(4) 0.038(4) 0.024(4) -0.001(3) 0.001(3) -0.009(3) O2 0.026(3) 0.032(3) 0.040(3) -0.012(2) 0.007(2) -0.001(2) C13 0.024(3) 0.022(3) 0.019(3) -0.007(3) 0.001(3) -0.007(3) C2 0.015(3) 0.022(3) 0.030(4) -0.010(3) -0.003(3) -0.001(3) N2 0.026(3) 0.019(3) 0.022(3) -0.004(2) -0.003(2) -0.005(2) N1 0.020(3) 0.034(3) 0.024(3) -0.006(3) -0.005(2) -0.006(3) N11 0.034(4) 0.032(3) 0.025(3) -0.006(3) 0.001(3) -0.013(3) C16 0.017(3) 0.023(3) 0.025(3) -0.006(3) -0.002(3) -0.001(3) O3 0.047(4) 0.033(3) 0.044(3) -0.020(3) -0.014(3) -0.003(3) C1 0.017(3) 0.029(4) 0.024(3) -0.011(3) 0.003(3) -0.007(3) C18 0.015(3) 0.017(3) 0.028(3) -0.007(3) 0.003(2) -0.004(2) N9 0.019(3) 0.030(3) 0.048(4) -0.010(3) 0.001(3) -0.007(3) C29 0.028(4) 0.025(3) 0.026(4) -0.004(3) -0.002(3) -0.010(3) N5 0.028(4) 0.033(4) 0.057(5) -0.016(3) -0.011(3) 0.003(3) C23 0.029(4) 0.034(4) 0.032(4) -0.008(3) 0.006(3) -0.001(3) C5 0.024(4) 0.021(3) 0.040(4) -0.005(3) 0.000(3) -0.001(3) C15 0.021(3) 0.023(3) 0.020(3) -0.006(3) -0.001(2) -0.007(3) C14 0.020(3) 0.029(4) 0.017(3) -0.007(3) -0.001(2) -0.010(3) C6 0.018(3) 0.023(3) 0.039(4) -0.003(3) -0.004(3) 0.000(3) C17 0.020(3) 0.019(3) 0.016(3) -0.003(3) 0.001(2) -0.004(3) C4 0.031(4) 0.043(5) 0.022(4) -0.010(3) -0.005(3) -0.005(3) C22 0.014(3) 0.034(4) 0.037(4) -0.015(3) -0.006(3) -0.003(3) C12 0.024(4) 0.024(4) 0.039(4) -0.014(3) -0.001(3) -0.008(3) C7 0.017(3) 0.035(4) 0.025(4) -0.009(3) -0.002(3) -0.003(3) C11 0.031(4) 0.019(3) 0.042(4) -0.014(3) -0.001(3) 0.001(3) C8 0.020(3) 0.033(4) 0.025(4) -0.004(3) -0.003(3) 0.001(3) C10 0.025(4) 0.018(3) 0.032(4) -0.008(3) 0.003(3) -0.001(3) N4 0.050(5) 0.043(4) 0.044(4) -0.012(4) -0.004(3) -0.005(4) C21 0.030(4) 0.035(4) 0.036(4) -0.021(3) -0.004(3) -0.009(3) C19 0.023(4) 0.044(5) 0.041(5) -0.007(4) -0.003(3) 0.000(3) C9 0.023(4) 0.027(4) 0.040(4) -0.012(3) -0.004(3) 0.001(3) N3 0.028(4) 0.052(4) 0.040(4) -0.002(3) 0.008(3) -0.008(3) C20 0.024(4) 0.038(5) 0.094(8) -0.022(5) -0.006(5) 0.011(4) N6 0.031(4) 0.035(4) 0.051(4) -0.013(3) 0.006(3) 0.004(3) C30 0.053(6) 0.056(6) 0.044(5) -0.015(4) -0.006(4) -0.033(5) C31 0.054(6) 0.051(5) 0.029(4) 0.006(4) 0.000(4) -0.018(5) C25 0.037(5) 0.036(5) 0.086(8) -0.006(5) 0.019(5) -0.009(4) C24 0.042(6) 0.073(7) 0.052(6) -0.011(5) -0.009(4) -0.021(5) N10 0.078(6) 0.040(4) 0.057(5) -0.018(4) -0.011(5) -0.010(4) C28 0.119(12) 0.039(6) 0.105(11) -0.031(7) -0.013(9) 0.001(7) C27 0.111(12) 0.109(12) 0.107(12) -0.056(10) -0.053(10) -0.022(10) C26 0.037(5) 0.032(4) 0.048(5) -0.009(4) -0.004(4) -0.010(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 Sm1 O1 2.352(5) . ? Sm1 O2 2.390(5) . ? Sm1 O3 2.399(5) . ? Sm1 O4 2.402(5) . ? Sm1 N1 2.490(6) . ? Sm1 N2 2.495(6) . ? Sm1 N7 2.577(6) . ? Sm1 N8 2.590(5) . ? Fe1 C3 1.932(7) . ? Fe1 C3 1.932(7) 2_666 ? Fe1 C1 1.934(7) 2_666 ? Fe1 C1 1.934(7) . ? Fe1 C4 1.951(8) 2_666 ? Fe1 C4 1.951(8) . ? Fe2 C2 1.926(7) 2_575 ? Fe2 C2 1.926(7) . ? Fe2 C5 1.948(8) 2_575 ? Fe2 C5 1.948(8) . ? Fe2 C6 1.952(8) 2_575 ? Fe2 C6 1.952(8) . ? N8 C16 1.321(9) . ? N8 C17 1.351(8) . ? O4 C29 1.238(9) . ? N7 C7 1.329(9) . ? N7 C18 1.362(8) . ? O1 C23 1.241(9) . ? C3 N3 1.171(10) . ? C13 C17 1.410(9) . ? C13 C14 1.425(10) . ? C13 C12 1.433(10) . ? C2 N2 1.158(9) . ? N1 C1 1.134(9) . ? N11 C29 1.320(9) . ? N11 C31 1.444(10) . ? N11 C30 1.450(10) . ? C16 C15 1.421(9) . ? O3 C26 1.202(10) . ? C18 C10 1.423(9) . ? C18 C17 1.443(9) . ? N9 C23 1.295(10) . ? N9 C25 1.432(11) . ? N9 C24 1.492(12) . ? N5 C5 1.147(10) . ? C15 C14 1.388(10) . ? C15 C22 1.494(9) . ? C14 C21 1.506(9) . ? C6 N6 1.139(10) . ? C4 N4 1.175(11) . ? C12 C11 1.344(11) . ? C7 C8 1.401(10) . ? C11 C10 1.422(10) . ? C8 C9 1.397(11) . ? C8 C19 1.511(10) . ? C10 C9 1.409(10) . ? C9 C20 1.505(11) . ? N10 C26 1.305(11) . ? N10 C27 1.441(16) . ? N10 C28 1.508(13) . ? 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 Sm1 O2 145.40(18) . . ? O1 Sm1 O3 76.9(2) . . ? O2 Sm1 O3 77.2(2) . . ? O1 Sm1 O4 141.94(17) . . ? O2 Sm1 O4 72.25(18) . . ? O3 Sm1 O4 122.31(19) . . ? O1 Sm1 N1 82.86(18) . . ? O2 Sm1 N1 110.6(2) . . ? O3 Sm1 N1 72.9(2) . . ? O4 Sm1 N1 73.97(19) . . ? O1 Sm1 N2 76.96(18) . . ? O2 Sm1 N2 75.39(19) . . ? O3 Sm1 N2 77.52(19) . . ? O4 Sm1 N2 135.71(18) . . ? N1 Sm1 N2 147.26(19) . . ? O1 Sm1 N7 73.25(18) . . ? O2 Sm1 N7 138.98(18) . . ? O3 Sm1 N7 141.64(19) . . ? O4 Sm1 N7 73.25(17) . . ? N1 Sm1 N7 79.89(19) . . ? N2 Sm1 N7 117.53(18) . . ? O1 Sm1 N8 106.49(17) . . ? O2 Sm1 N8 85.95(18) . . ? O3 Sm1 N8 150.58(19) . . ? O4 Sm1 N8 73.35(17) . . ? N1 Sm1 N8 136.21(19) . . ? N2 Sm1 N8 74.98(18) . . ? N7 Sm1 N8 63.29(17) . . ? C3 Fe1 C3 180.0(5) . 2_666 ? C3 Fe1 C1 89.6(3) . 2_666 ? C3 Fe1 C1 90.4(3) 2_666 2_666 ? C3 Fe1 C1 90.4(3) . . ? C3 Fe1 C1 89.6(3) 2_666 . ? C1 Fe1 C1 180.000(1) 2_666 . ? C3 Fe1 C4 89.0(3) . 2_666 ? C3 Fe1 C4 91.0(3) 2_666 2_666 ? C1 Fe1 C4 90.2(3) 2_666 2_666 ? C1 Fe1 C4 89.8(3) . 2_666 ? C3 Fe1 C4 91.0(3) . . ? C3 Fe1 C4 89.0(3) 2_666 . ? C1 Fe1 C4 89.8(3) 2_666 . ? C1 Fe1 C4 90.2(3) . . ? C4 Fe1 C4 180.0(4) 2_666 . ? C2 Fe2 C2 180.0(2) 2_575 . ? C2 Fe2 C5 87.4(3) 2_575 2_575 ? C2 Fe2 C5 92.6(3) . 2_575 ? C2 Fe2 C5 92.6(3) 2_575 . ? C2 Fe2 C5 87.4(3) . . ? C5 Fe2 C5 180.0(4) 2_575 . ? C2 Fe2 C6 89.5(3) 2_575 2_575 ? C2 Fe2 C6 90.5(3) . 2_575 ? C5 Fe2 C6 90.9(3) 2_575 2_575 ? C5 Fe2 C6 89.1(3) . 2_575 ? C2 Fe2 C6 90.5(3) 2_575 . ? C2 Fe2 C6 89.5(3) . . ? C5 Fe2 C6 89.1(3) 2_575 . ? C5 Fe2 C6 90.9(3) . . ? C6 Fe2 C6 180.000(1) 2_575 . ? C16 N8 C17 118.5(6) . . ? C16 N8 Sm1 121.1(4) . . ? C17 N8 Sm1 119.3(4) . . ? C29 O4 Sm1 142.0(5) . . ? C7 N7 C18 117.6(6) . . ? C7 N7 Sm1 122.1(5) . . ? C18 N7 Sm1 119.5(4) . . ? C23 O1 Sm1 145.9(5) . . ? N3 C3 Fe1 177.3(7) . . ? C17 C13 C14 118.2(6) . . ? C17 C13 C12 118.5(6) . . ? C14 C13 C12 123.2(6) . . ? N2 C2 Fe2 175.4(6) . . ? C2 N2 Sm1 154.3(5) . . ? C1 N1 Sm1 177.1(6) . . ? C29 N11 C31 121.5(7) . . ? C29 N11 C30 121.3(7) . . ? C31 N11 C30 116.8(7) . . ? N8 C16 C15 124.2(6) . . ? C26 O3 Sm1 143.9(6) . . ? N1 C1 Fe1 179.5(7) . . ? N7 C18 C10 122.0(6) . . ? N7 C18 C17 117.8(6) . . ? C10 C18 C17 120.2(6) . . ? C23 N9 C25 126.6(8) . . ? C23 N9 C24 117.8(7) . . ? C25 N9 C24 115.5(8) . . ? O4 C29 N11 124.5(7) . . ? O1 C23 N9 124.8(8) . . ? N5 C5 Fe2 177.4(7) . . ? C14 C15 C16 117.6(6) . . ? C14 C15 C22 123.6(6) . . ? C16 C15 C22 118.8(6) . . ? C15 C14 C13 119.0(6) . . ? C15 C14 C21 120.7(6) . . ? C13 C14 C21 120.3(6) . . ? N6 C6 Fe2 178.0(7) . . ? N8 C17 C13 122.4(6) . . ? N8 C17 C18 118.0(6) . . ? C13 C17 C18 119.6(6) . . ? N4 C4 Fe1 177.8(8) . . ? C11 C12 C13 121.3(7) . . ? N7 C7 C8 124.9(7) . . ? C12 C11 C10 122.7(6) . . ? C7 C8 C9 118.2(6) . . ? C7 C8 C19 118.0(7) . . ? C9 C8 C19 123.8(7) . . ? C9 C10 C18 118.8(7) . . ? C9 C10 C11 123.6(6) . . ? C18 C10 C11 117.6(6) . . ? C8 C9 C10 118.5(6) . . ? C8 C9 C20 119.1(7) . . ? C10 C9 C20 122.4(7) . . ? C26 N10 C27 119.4(9) . . ? C26 N10 C28 120.6(10) . . ? C27 N10 C28 120.0(10) . . ? O3 C26 N10 125.7(9) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 2.611 _refine_diff_density_min -2.032 _refine_diff_density_rms 0.197 # Attachment 'compound10.txt' data_compound10 _database_code_depnum_ccdc_archive 'CCDC 296502' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-di-agua-bis-(3,4,7,8-tetramethyl-1,10- phenanthroline)-tetracyano-iron(iii)-samarium(iii) hydrate ; _chemical_formula_moiety '[Sm(tmphen)2(H2O)2Fe(CN)6]MeOH13H2O' _chemical_formula_sum 'C39 H66 Fe N10 O16 Sm' _chemical_formula_weight 1137.22 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 20.322(4) _cell_length_b 19.728(4) _cell_length_c 13.473(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.48(3) _cell_angle_gamma 90.00 _cell_volume 5179.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.475 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22489 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 23.32 _reflns_number_total 7431 _reflns_number_gt 5854 _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^)+(0.0394P)^2^+20.3326P] 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 7431 _refine_ls_number_parameters 636 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.252831(15) 0.602579(14) 0.51167(2) 0.01207(9) Uani 1 1 d . . . Fe1 Fe 0.5000 0.5000 0.5000 0.0127(3) Uani 1 2 d S . . Fe2 Fe 0.0000 0.5000 0.5000 0.0126(3) Uani 1 2 d S . . N8 N 0.2094(2) 0.7044(2) 0.5958(3) 0.0158(11) Uani 1 1 d . . . N9 N 0.2983(2) 0.7097(2) 0.4483(3) 0.0136(11) Uani 1 1 d . . . C18 C 0.3270(3) 0.7196(3) 0.6933(4) 0.0154(13) Uani 1 1 d . . . C34 C 0.2519(3) 0.7578(3) 0.4011(4) 0.0146(13) Uani 1 1 d . . . N10 N 0.1687(2) 0.6684(2) 0.3620(3) 0.0154(11) Uani 1 1 d . . . O1 O 0.2877(2) 0.50521(19) 0.6204(3) 0.0199(10) Uani 1 1 d D . . N4 N 0.4241(3) 0.3658(3) 0.4208(4) 0.0283(14) Uani 1 1 d . . . C11 C 0.3682(3) 0.8314(3) 0.7559(4) 0.0189(14) Uani 1 1 d . . . H11 H 0.4043 0.8603 0.7927 0.023 Uiso 1 1 calc R . . C24 C 0.3846(3) 0.7976(3) 0.4978(4) 0.0169(13) Uani 1 1 d . . . C17 C 0.2597(3) 0.7472(3) 0.6478(4) 0.0168(14) Uani 1 1 d . . . N7 N 0.3357(2) 0.6524(2) 0.6767(3) 0.0158(11) Uani 1 1 d . . . C23 C 0.3626(3) 0.7302(3) 0.4915(4) 0.0168(14) Uani 1 1 d . . . H23 H 0.3959 0.6965 0.5201 0.020 Uiso 1 1 calc R . . N6 N 0.0654(3) 0.3576(3) 0.5441(4) 0.0269(14) Uani 1 1 d . . . C16 C 0.1468(3) 0.7306(3) 0.5569(4) 0.0204(15) Uani 1 1 d . . . H16 H 0.1107 0.7004 0.5248 0.025 Uiso 1 1 calc R . . C13 C 0.2489(3) 0.8169(3) 0.6557(4) 0.0186(14) Uani 1 1 d . . . C26 C 0.2689(3) 0.8269(3) 0.4003(4) 0.0170(14) Uani 1 1 d . . . C31 C 0.0499(3) 0.6912(3) 0.2668(4) 0.0167(14) Uani 1 1 d . . . N1 N 0.3621(3) 0.5691(2) 0.4819(3) 0.0187(12) Uani 1 1 d . . . C15 C 0.1305(3) 0.7989(3) 0.5599(4) 0.0227(15) Uani 1 1 d . . . C8 C 0.4553(3) 0.6625(3) 0.7771(4) 0.0157(13) Uani 1 1 d . . . O2 O 0.2272(2) 0.5199(2) 0.3737(3) 0.0248(10) Uani 1 1 d D . . C33 C 0.1829(3) 0.7349(3) 0.3522(4) 0.0139(13) Uani 1 1 d . . . C35 C 0.4573(3) 0.8140(3) 0.5566(4) 0.0225(15) Uani 1 1 d . . . H35A H 0.4798 0.8370 0.5106 0.034 Uiso 1 1 calc R . . H35B H 0.4819 0.7720 0.5824 0.034 Uiso 1 1 calc R . . H35C H 0.4577 0.8437 0.6150 0.034 Uiso 1 1 calc R . . C7 C 0.3982(3) 0.6259(3) 0.7193(4) 0.0146(13) Uani 1 1 d . . . H7 H 0.4041 0.5789 0.7095 0.017 Uiso 1 1 calc R . . C25 C 0.3362(3) 0.8471(3) 0.4543(4) 0.0206(14) Uani 1 1 d . . . C10 C 0.3815(3) 0.7607(3) 0.7487(4) 0.0163(14) Uani 1 1 d . . . C29 C 0.1322(3) 0.7827(3) 0.3016(4) 0.0159(13) Uani 1 1 d . . . C14 C 0.1824(3) 0.8439(3) 0.6073(4) 0.0239(15) Uani 1 1 d . . . C4 C 0.4539(3) 0.4157(3) 0.4493(4) 0.0195(15) Uani 1 1 d . . . C30 C 0.0631(3) 0.7591(3) 0.2583(4) 0.0171(14) Uani 1 1 d . . . C6 C 0.0406(3) 0.4109(3) 0.5277(4) 0.0164(14) Uani 1 1 d . . . C38 C -0.0218(3) 0.6633(3) 0.2261(4) 0.0223(15) Uani 1 1 d . . . H38A H -0.0514 0.6837 0.2641 0.033 Uiso 1 1 calc R . . H38B H -0.0208 0.6140 0.2353 0.033 Uiso 1 1 calc R . . H38C H -0.0398 0.6741 0.1523 0.033 Uiso 1 1 calc R . . N2 N 0.1423(3) 0.5619(3) 0.5280(4) 0.0203(12) Uani 1 1 d . . . C9 C 0.4477(3) 0.7310(3) 0.7910(4) 0.0177(14) Uani 1 1 d . . . C28 C 0.1521(3) 0.8514(3) 0.2989(4) 0.0199(14) Uani 1 1 d . . . H28 H 0.1191 0.8835 0.2627 0.024 Uiso 1 1 calc R . . C20 C 0.5075(3) 0.7740(3) 0.8492(5) 0.0273(16) Uani 1 1 d . . . H20A H 0.4970 0.7950 0.9087 0.041 Uiso 1 1 calc R . . H20B H 0.5160 0.8093 0.8033 0.041 Uiso 1 1 calc R . . H20C H 0.5484 0.7455 0.8733 0.041 Uiso 1 1 calc R . . C22 C 0.0573(3) 0.8221(3) 0.5066(5) 0.0293(16) Uani 1 1 d . . . H22A H 0.0395 0.8477 0.5557 0.044 Uiso 1 1 calc R . . H22B H 0.0282 0.7824 0.4824 0.044 Uiso 1 1 calc R . . H22C H 0.0573 0.8510 0.4474 0.044 Uiso 1 1 calc R . . C12 C 0.3055(3) 0.8583(3) 0.7118(4) 0.0221(15) Uani 1 1 d . . . H12 H 0.2986 0.9056 0.7180 0.027 Uiso 1 1 calc R . . N3 N 0.4998(3) 0.4575(3) 0.7219(4) 0.0278(13) Uani 1 1 d . . . C27 C 0.2163(3) 0.8725(3) 0.3461(4) 0.0218(15) Uani 1 1 d . . . H27 H 0.2270 0.9192 0.3432 0.026 Uiso 1 1 calc R . . C32 C 0.1037(3) 0.6482(3) 0.3180(4) 0.0167(14) Uani 1 1 d . . . H32 H 0.0935 0.6014 0.3219 0.020 Uiso 1 1 calc R . . C37 C 0.0075(3) 0.8067(3) 0.2056(5) 0.0339(18) Uani 1 1 d . . . H37A H -0.0128 0.7919 0.1340 0.051 Uiso 1 1 calc R . . H37B H 0.0266 0.8523 0.2059 0.051 Uiso 1 1 calc R . . H37C H -0.0279 0.8072 0.2422 0.051 Uiso 1 1 calc R . . C19 C 0.5231(3) 0.6265(3) 0.8175(4) 0.0251(16) Uani 1 1 d . . . H19A H 0.5569 0.6468 0.7871 0.038 Uiso 1 1 calc R . . H19B H 0.5174 0.5784 0.7987 0.038 Uiso 1 1 calc R . . H19C H 0.5390 0.6308 0.8930 0.038 Uiso 1 1 calc R . . C21 C 0.1686(4) 0.9189(3) 0.6051(5) 0.0317(17) Uani 1 1 d . . . H21A H 0.1789 0.9391 0.5447 0.048 Uiso 1 1 calc R . . H21B H 0.1977 0.9398 0.6684 0.048 Uiso 1 1 calc R . . H21C H 0.1202 0.9267 0.6007 0.048 Uiso 1 1 calc R . . C36 C 0.3556(3) 0.9213(3) 0.4652(5) 0.0299(17) Uani 1 1 d . . . H36A H 0.3985 0.9268 0.5207 0.045 Uiso 1 1 calc R . . H36B H 0.3191 0.9472 0.4820 0.045 Uiso 1 1 calc R . . H36C H 0.3619 0.9379 0.3999 0.045 Uiso 1 1 calc R . . C3 C 0.5007(3) 0.4737(3) 0.6398(4) 0.0181(14) Uani 1 1 d . . . C1 C 0.4139(3) 0.5430(3) 0.4855(4) 0.0155(14) Uani 1 1 d . . . C2 C 0.0889(3) 0.5385(3) 0.5198(4) 0.0160(14) Uani 1 1 d . . . O12 O 0.3464(2) 0.3890(2) -0.0756(3) 0.0318(11) Uani 1 1 d . . . O13 O 0.1423(2) 0.3905(2) 0.0736(3) 0.0375(12) Uani 1 1 d . . . O3 O 0.2504(2) 0.4637(2) 0.7855(3) 0.0287(11) Uani 1 1 d D . . O7 O 0.3117(3) 0.3804(2) 0.5381(4) 0.0396(13) Uani 1 1 d . . . O6 O 0.4593(2) 0.4657(2) 0.9129(3) 0.0302(11) Uani 1 1 d . . . O8 O 0.3433(3) 0.2447(2) 0.3539(4) 0.0464(15) Uani 1 1 d . . . O9 O 0.2922(3) 0.2420(2) 0.1401(4) 0.0428(13) Uani 1 1 d . . . O4 O 0.1507(3) 0.2454(3) 0.6287(5) 0.0604(17) Uani 1 1 d . . . N5 N 0.0100(3) 0.5166(3) 0.7319(4) 0.0239(13) Uani 1 1 d . . . O14 O 0.1243(3) 0.4409(3) 0.2565(4) 0.0460(14) Uani 1 1 d . . . O10 O 0.3129(3) 0.4671(3) 0.2651(4) 0.0437(14) Uani 1 1 d . . . O15 O -0.0411(3) 0.5289(3) 0.0522(4) 0.0508(15) Uani 1 1 d . . . O5 O 0.1717(3) 0.3618(3) 0.4257(5) 0.0721(19) Uani 1 1 d . . . O11 O 0.2007(4) 0.2565(4) -0.1564(5) 0.087(2) Uani 1 1 d . . . C5 C 0.0072(3) 0.5109(3) 0.6453(4) 0.0161(14) Uani 1 1 d . . . C39 C 0.1854(4) 0.4349(4) 0.7722(7) 0.061(3) Uani 1 1 d . . . H39A H 0.1683 0.4472 0.8308 0.092 Uiso 1 1 calc R . . H39B H 0.1888 0.3854 0.7686 0.092 Uiso 1 1 calc R . . H39C H 0.1538 0.4518 0.7079 0.092 Uiso 1 1 calc R . . O16 O 0.2850(3) 0.3815(2) 0.0881(3) 0.0385(12) Uani 1 1 d . . . H1A H 0.2694(15) 0.491(2) 0.676(2) 0.05(2) Uiso 1 1 d D . . H1B H 0.308(2) 0.4667(15) 0.596(4) 0.06(2) Uiso 1 1 d D . . H2A H 0.2617(12) 0.505(3) 0.341(3) 0.13(4) Uiso 1 1 d D . . H2B H 0.1906(16) 0.4869(19) 0.360(5) 0.10(4) Uiso 1 1 d D . . H3 H 0.284(3) 0.438(3) 0.837(5) 0.09(3) 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 Sm1 0.00923(15) 0.01057(15) 0.01506(15) 0.00045(13) 0.00127(11) 0.00080(15) Fe1 0.0112(6) 0.0123(6) 0.0140(6) 0.0004(4) 0.0028(5) 0.0023(5) Fe2 0.0099(6) 0.0114(6) 0.0150(6) 0.0007(4) 0.0013(5) -0.0010(5) N8 0.016(3) 0.019(3) 0.016(2) 0.001(2) 0.009(2) 0.001(2) N9 0.017(3) 0.011(2) 0.012(2) -0.0011(19) 0.003(2) -0.001(2) C18 0.022(3) 0.013(3) 0.010(3) 0.001(2) 0.002(2) 0.001(3) C34 0.014(3) 0.020(3) 0.012(3) 0.000(2) 0.009(2) 0.003(3) N10 0.013(3) 0.017(3) 0.015(2) 0.0010(19) 0.002(2) -0.004(2) O1 0.024(2) 0.012(2) 0.022(2) 0.0032(17) 0.0030(19) 0.0008(19) N4 0.035(4) 0.022(3) 0.025(3) -0.003(2) 0.005(3) -0.006(3) C11 0.029(4) 0.013(3) 0.017(3) -0.005(2) 0.010(3) -0.005(3) C24 0.018(3) 0.019(3) 0.016(3) -0.001(2) 0.007(2) -0.008(3) C17 0.025(4) 0.018(3) 0.009(3) -0.001(2) 0.008(3) 0.004(3) N7 0.019(3) 0.013(3) 0.016(2) 0.0026(19) 0.005(2) 0.002(2) C23 0.015(3) 0.020(3) 0.015(3) -0.001(2) 0.003(2) 0.001(3) N6 0.032(3) 0.023(3) 0.020(3) -0.002(2) -0.001(2) 0.007(3) C16 0.023(4) 0.023(4) 0.019(3) 0.001(2) 0.012(3) 0.006(3) C13 0.028(4) 0.017(3) 0.013(3) 0.003(2) 0.010(3) 0.002(3) C26 0.021(3) 0.014(3) 0.019(3) 0.003(2) 0.011(3) -0.003(3) C31 0.018(3) 0.016(3) 0.014(3) 0.001(2) 0.001(2) 0.002(3) N1 0.021(3) 0.013(3) 0.021(3) 0.001(2) 0.003(2) 0.005(2) C15 0.025(4) 0.031(4) 0.014(3) 0.005(3) 0.010(3) 0.016(3) C8 0.014(3) 0.016(3) 0.014(3) 0.000(2) 0.000(2) 0.002(3) O2 0.023(3) 0.019(2) 0.029(2) -0.0055(18) 0.002(2) 0.000(2) C33 0.014(3) 0.017(3) 0.012(3) -0.001(2) 0.005(2) -0.006(3) C35 0.022(4) 0.021(3) 0.026(3) 0.000(3) 0.010(3) -0.005(3) C7 0.016(3) 0.010(3) 0.017(3) 0.001(2) 0.003(2) 0.000(3) C25 0.028(4) 0.014(3) 0.019(3) -0.002(2) 0.008(3) -0.011(3) C10 0.028(4) 0.011(3) 0.012(3) -0.002(2) 0.008(3) -0.001(3) C29 0.018(3) 0.014(3) 0.016(3) 0.001(2) 0.005(2) 0.005(3) C14 0.037(4) 0.018(3) 0.018(3) 0.006(3) 0.011(3) 0.013(3) C4 0.024(4) 0.021(4) 0.015(3) 0.002(2) 0.007(3) 0.007(3) C30 0.018(3) 0.017(3) 0.014(3) 0.003(2) 0.001(2) 0.006(3) C6 0.018(3) 0.015(4) 0.014(3) -0.002(2) 0.001(2) -0.001(3) C38 0.023(4) 0.021(3) 0.021(3) 0.006(3) 0.003(3) 0.001(3) N2 0.020(3) 0.020(3) 0.021(3) 0.003(2) 0.007(2) -0.004(3) C9 0.019(3) 0.023(4) 0.011(3) -0.001(2) 0.003(2) -0.008(3) C28 0.029(4) 0.013(3) 0.017(3) 0.006(2) 0.005(3) 0.001(3) C20 0.021(4) 0.024(4) 0.030(3) -0.004(3) -0.004(3) -0.006(3) C22 0.025(4) 0.033(4) 0.030(4) 0.002(3) 0.007(3) 0.012(3) C12 0.032(4) 0.012(3) 0.023(3) 0.001(3) 0.009(3) 0.002(3) N3 0.041(4) 0.018(3) 0.025(3) 0.004(2) 0.010(3) 0.007(3) C27 0.029(4) 0.008(3) 0.028(3) 0.002(2) 0.009(3) -0.003(3) C32 0.022(4) 0.011(3) 0.018(3) 0.000(2) 0.008(3) -0.001(3) C37 0.026(4) 0.026(4) 0.042(4) 0.006(3) -0.002(3) 0.004(3) C19 0.022(4) 0.028(4) 0.019(3) -0.006(3) -0.003(3) 0.001(3) C21 0.038(4) 0.021(4) 0.033(4) 0.000(3) 0.005(3) 0.017(3) C36 0.027(4) 0.016(3) 0.040(4) -0.001(3) -0.002(3) -0.004(3) C3 0.023(4) 0.014(3) 0.016(3) -0.003(2) 0.004(3) 0.005(3) C1 0.021(4) 0.015(3) 0.011(3) 0.001(2) 0.005(2) -0.001(3) C2 0.018(4) 0.012(3) 0.018(3) 0.004(2) 0.005(3) 0.002(3) O12 0.030(3) 0.031(3) 0.030(2) 0.006(2) 0.002(2) 0.006(2) O13 0.037(3) 0.033(3) 0.042(3) -0.002(2) 0.010(2) 0.001(2) O3 0.027(3) 0.031(3) 0.028(2) 0.007(2) 0.007(2) 0.002(2) O7 0.047(3) 0.025(3) 0.055(3) 0.000(2) 0.028(2) 0.002(2) O6 0.031(3) 0.031(3) 0.033(2) -0.001(2) 0.014(2) 0.004(2) O8 0.057(4) 0.032(3) 0.041(3) -0.003(2) 0.001(3) -0.018(3) O9 0.048(3) 0.034(3) 0.047(3) -0.012(2) 0.013(2) -0.005(3) O4 0.053(4) 0.044(4) 0.080(4) 0.009(3) 0.012(3) 0.013(3) N5 0.029(3) 0.020(3) 0.023(3) -0.003(2) 0.008(2) -0.006(2) O14 0.035(3) 0.056(3) 0.047(3) -0.009(3) 0.011(2) -0.014(3) O10 0.036(3) 0.045(3) 0.044(3) -0.010(2) 0.001(2) 0.014(3) O15 0.060(4) 0.057(4) 0.031(3) 0.007(2) 0.006(3) 0.006(3) O5 0.056(4) 0.089(5) 0.067(4) 0.010(3) 0.011(3) -0.014(4) O11 0.082(5) 0.095(5) 0.081(5) 0.002(4) 0.018(4) 0.012(4) C5 0.015(3) 0.011(3) 0.021(3) 0.003(2) 0.002(3) -0.008(3) C39 0.042(5) 0.054(6) 0.072(6) 0.014(5) -0.007(4) -0.010(5) O16 0.041(3) 0.035(3) 0.039(3) -0.006(2) 0.011(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 Sm1 O1 2.398(4) . ? Sm1 O2 2.416(4) . ? Sm1 N2 2.453(5) . ? Sm1 N1 2.457(5) . ? Sm1 N9 2.549(5) . ? Sm1 N7 2.573(4) . ? Sm1 N8 2.582(5) . ? Sm1 N10 2.593(4) . ? Fe1 C1 1.904(6) . ? Fe1 C1 1.904(6) 3_666 ? Fe1 C4 1.935(6) . ? Fe1 C4 1.935(6) 3_666 ? Fe1 C3 1.950(6) 3_666 ? Fe1 C3 1.950(6) . ? Fe2 C2 1.908(6) . ? Fe2 C2 1.908(6) 3_566 ? Fe2 C6 1.932(6) . ? Fe2 C6 1.932(6) 3_566 ? Fe2 C5 1.933(6) 3_566 ? Fe2 C5 1.933(6) . ? N8 C16 1.336(7) . ? N8 C17 1.357(7) . ? N9 C23 1.333(7) . ? N9 C34 1.362(7) . ? C18 N7 1.364(7) . ? C18 C10 1.405(8) . ? C18 C17 1.437(8) . ? C34 C26 1.407(8) . ? C34 C33 1.441(8) . ? N10 C32 1.346(7) . ? N10 C33 1.357(7) . ? N4 C4 1.164(8) . ? C11 C12 1.353(9) . ? C11 C10 1.430(8) . ? C24 C25 1.391(8) . ? C24 C23 1.397(8) . ? C24 C35 1.501(8) . ? C17 C13 1.401(8) . ? N7 C7 1.343(7) . ? N6 C6 1.160(7) . ? C16 C15 1.390(9) . ? C13 C14 1.428(9) . ? C13 C12 1.438(8) . ? C26 C25 1.413(8) . ? C26 C27 1.430(8) . ? C31 C30 1.377(8) . ? C31 C32 1.401(8) . ? C31 C38 1.507(8) . ? N1 C1 1.160(7) . ? C15 C14 1.388(9) . ? C15 C22 1.527(8) . ? C8 C9 1.380(8) . ? C8 C7 1.400(8) . ? C8 C19 1.507(8) . ? C33 C29 1.419(8) . ? C25 C36 1.511(8) . ? C10 C9 1.430(8) . ? C29 C28 1.418(8) . ? C29 C30 1.437(8) . ? C14 C21 1.504(8) . ? C30 C37 1.486(8) . ? N2 C2 1.154(7) . ? C9 C20 1.506(8) . ? C28 C27 1.345(8) . ? N3 C3 1.156(7) . ? O3 C39 1.401(9) . ? N5 C5 1.158(7) . ? 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 Sm1 O2 83.77(14) . . ? O1 Sm1 N2 78.59(15) . . ? O2 Sm1 N2 81.10(16) . . ? O1 Sm1 N1 76.13(15) . . ? O2 Sm1 N1 72.56(15) . . ? N2 Sm1 N1 145.05(16) . . ? O1 Sm1 N9 142.80(14) . . ? O2 Sm1 N9 108.74(14) . . ? N2 Sm1 N9 136.86(15) . . ? N1 Sm1 N9 74.80(16) . . ? O1 Sm1 N7 76.73(14) . . ? O2 Sm1 N7 150.24(15) . . ? N2 Sm1 N7 116.02(15) . . ? N1 Sm1 N7 81.01(15) . . ? N9 Sm1 N7 76.25(14) . . ? O1 Sm1 N8 115.69(14) . . ? O2 Sm1 N8 146.83(14) . . ? N2 Sm1 N8 77.26(16) . . ? N1 Sm1 N8 135.93(15) . . ? N9 Sm1 N8 72.76(14) . . ? N7 Sm1 N8 62.92(14) . . ? O1 Sm1 N10 153.11(14) . . ? O2 Sm1 N10 77.80(14) . . ? N2 Sm1 N10 79.34(15) . . ? N1 Sm1 N10 115.79(15) . . ? N9 Sm1 N10 63.00(14) . . ? N7 Sm1 N10 127.34(14) . . ? N8 Sm1 N10 73.72(14) . . ? C1 Fe1 C1 180.0(3) . 3_666 ? C1 Fe1 C4 90.5(2) . . ? C1 Fe1 C4 89.5(2) 3_666 . ? C1 Fe1 C4 89.5(2) . 3_666 ? C1 Fe1 C4 90.5(2) 3_666 3_666 ? C4 Fe1 C4 180.000(1) . 3_666 ? C1 Fe1 C3 91.6(2) . 3_666 ? C1 Fe1 C3 88.4(2) 3_666 3_666 ? C4 Fe1 C3 91.0(2) . 3_666 ? C4 Fe1 C3 89.0(2) 3_666 3_666 ? C1 Fe1 C3 88.4(2) . . ? C1 Fe1 C3 91.6(2) 3_666 . ? C4 Fe1 C3 89.0(2) . . ? C4 Fe1 C3 91.0(2) 3_666 . ? C3 Fe1 C3 180.000(1) 3_666 . ? C2 Fe2 C2 180.0(5) . 3_566 ? C2 Fe2 C6 90.0(2) . . ? C2 Fe2 C6 90.0(2) 3_566 . ? C2 Fe2 C6 90.0(2) . 3_566 ? C2 Fe2 C6 90.0(2) 3_566 3_566 ? C6 Fe2 C6 180.000(1) . 3_566 ? C2 Fe2 C5 89.0(2) . 3_566 ? C2 Fe2 C5 91.0(2) 3_566 3_566 ? C6 Fe2 C5 90.0(2) . 3_566 ? C6 Fe2 C5 90.0(2) 3_566 3_566 ? C2 Fe2 C5 91.0(2) . . ? C2 Fe2 C5 89.0(2) 3_566 . ? C6 Fe2 C5 90.0(2) . . ? C6 Fe2 C5 90.0(2) 3_566 . ? C5 Fe2 C5 180.000(1) 3_566 . ? C16 N8 C17 117.1(5) . . ? C16 N8 Sm1 122.4(4) . . ? C17 N8 Sm1 114.2(4) . . ? C23 N9 C34 117.1(5) . . ? C23 N9 Sm1 120.6(3) . . ? C34 N9 Sm1 117.7(4) . . ? N7 C18 C10 121.9(5) . . ? N7 C18 C17 116.8(5) . . ? C10 C18 C17 121.3(5) . . ? N9 C34 C26 122.6(5) . . ? N9 C34 C33 116.8(5) . . ? C26 C34 C33 120.6(5) . . ? C32 N10 C33 117.0(5) . . ? C32 N10 Sm1 122.9(4) . . ? C33 N10 Sm1 116.6(3) . . ? C12 C11 C10 121.7(6) . . ? C25 C24 C23 117.8(5) . . ? C25 C24 C35 123.0(5) . . ? C23 C24 C35 119.1(5) . . ? N8 C17 C13 122.6(5) . . ? N8 C17 C18 118.0(5) . . ? C13 C17 C18 119.3(5) . . ? C7 N7 C18 117.3(5) . . ? C7 N7 Sm1 121.9(4) . . ? C18 N7 Sm1 115.4(3) . . ? N9 C23 C24 124.9(5) . . ? N8 C16 C15 124.9(6) . . ? C17 C13 C14 118.7(6) . . ? C17 C13 C12 118.6(6) . . ? C14 C13 C12 122.7(6) . . ? C34 C26 C25 118.3(5) . . ? C34 C26 C27 117.7(5) . . ? C25 C26 C27 124.0(5) . . ? C30 C31 C32 119.1(5) . . ? C30 C31 C38 121.1(5) . . ? C32 C31 C38 119.8(5) . . ? C1 N1 Sm1 164.5(4) . . ? C14 C15 C16 118.5(6) . . ? C14 C15 C22 122.4(6) . . ? C16 C15 C22 119.0(6) . . ? C9 C8 C7 118.2(5) . . ? C9 C8 C19 122.6(5) . . ? C7 C8 C19 119.1(5) . . ? N10 C33 C29 122.9(5) . . ? N10 C33 C34 117.7(5) . . ? C29 C33 C34 119.4(5) . . ? N7 C7 C8 124.9(5) . . ? C24 C25 C26 118.9(5) . . ? C24 C25 C36 120.3(5) . . ? C26 C25 C36 120.8(6) . . ? C18 C10 C9 119.1(5) . . ? C18 C10 C11 117.6(5) . . ? C9 C10 C11 123.2(5) . . ? C28 C29 C33 118.3(5) . . ? C28 C29 C30 123.5(5) . . ? C33 C29 C30 118.1(5) . . ? C15 C14 C13 117.9(5) . . ? C15 C14 C21 120.6(6) . . ? C13 C14 C21 121.5(6) . . ? N4 C4 Fe1 177.1(6) . . ? C31 C30 C29 118.3(5) . . ? C31 C30 C37 120.9(6) . . ? C29 C30 C37 120.8(5) . . ? N6 C6 Fe2 179.4(6) . . ? C2 N2 Sm1 168.8(4) . . ? C8 C9 C10 118.4(5) . . ? C8 C9 C20 121.2(6) . . ? C10 C9 C20 120.4(5) . . ? C27 C28 C29 122.0(6) . . ? C11 C12 C13 121.4(6) . . ? C28 C27 C26 122.0(6) . . ? N10 C32 C31 124.7(5) . . ? N3 C3 Fe1 178.6(6) . . ? N1 C1 Fe1 176.7(5) . . ? N2 C2 Fe2 177.6(5) . . ? N5 C5 Fe2 178.4(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 O1 Sm1 N8 C16 -121.9(4) . . . . ? O2 Sm1 N8 C16 -0.8(6) . . . . ? N2 Sm1 N8 C16 -51.3(4) . . . . ? N1 Sm1 N8 C16 141.6(4) . . . . ? N9 Sm1 N8 C16 97.2(4) . . . . ? N7 Sm1 N8 C16 -179.7(5) . . . . ? N10 Sm1 N8 C16 31.1(4) . . . . ? O1 Sm1 N8 C17 87.0(4) . . . . ? O2 Sm1 N8 C17 -151.9(3) . . . . ? N2 Sm1 N8 C17 157.5(4) . . . . ? N1 Sm1 N8 C17 -9.5(5) . . . . ? N9 Sm1 N8 C17 -53.9(4) . . . . ? N7 Sm1 N8 C17 29.2(3) . . . . ? N10 Sm1 N8 C17 -120.0(4) . . . . ? O1 Sm1 N9 C23 -10.4(5) . . . . ? O2 Sm1 N9 C23 -115.3(4) . . . . ? N2 Sm1 N9 C23 147.6(4) . . . . ? N1 Sm1 N9 C23 -50.2(4) . . . . ? N7 Sm1 N9 C23 34.1(4) . . . . ? N8 Sm1 N9 C23 99.6(4) . . . . ? N10 Sm1 N9 C23 179.7(5) . . . . ? O1 Sm1 N9 C34 -165.7(3) . . . . ? O2 Sm1 N9 C34 89.4(4) . . . . ? N2 Sm1 N9 C34 -7.6(5) . . . . ? N1 Sm1 N9 C34 154.6(4) . . . . ? N7 Sm1 N9 C34 -121.2(4) . . . . ? N8 Sm1 N9 C34 -55.7(4) . . . . ? N10 Sm1 N9 C34 24.5(3) . . . . ? C23 N9 C34 C26 -2.5(8) . . . . ? Sm1 N9 C34 C26 153.6(4) . . . . ? C23 N9 C34 C33 178.4(5) . . . . ? Sm1 N9 C34 C33 -25.4(6) . . . . ? O1 Sm1 N10 C32 13.5(6) . . . . ? O2 Sm1 N10 C32 61.3(4) . . . . ? N2 Sm1 N10 C32 -21.8(4) . . . . ? N1 Sm1 N10 C32 124.8(4) . . . . ? N9 Sm1 N10 C32 179.9(5) . . . . ? N7 Sm1 N10 C32 -136.5(4) . . . . ? N8 Sm1 N10 C32 -101.5(4) . . . . ? O1 Sm1 N10 C33 171.4(4) . . . . ? O2 Sm1 N10 C33 -140.8(4) . . . . ? N2 Sm1 N10 C33 136.1(4) . . . . ? N1 Sm1 N10 C33 -77.3(4) . . . . ? N9 Sm1 N10 C33 -22.2(4) . . . . ? N7 Sm1 N10 C33 21.4(5) . . . . ? N8 Sm1 N10 C33 56.4(4) . . . . ? C16 N8 C17 C13 -4.0(8) . . . . ? Sm1 N8 C17 C13 148.7(4) . . . . ? C16 N8 C17 C18 178.0(5) . . . . ? Sm1 N8 C17 C18 -29.3(6) . . . . ? N7 C18 C17 N8 2.7(7) . . . . ? C10 C18 C17 N8 -179.6(5) . . . . ? N7 C18 C17 C13 -175.4(5) . . . . ? C10 C18 C17 C13 2.3(8) . . . . ? C10 C18 N7 C7 2.7(8) . . . . ? C17 C18 N7 C7 -179.6(5) . . . . ? C10 C18 N7 Sm1 -152.0(4) . . . . ? C17 C18 N7 Sm1 25.7(6) . . . . ? O1 Sm1 N7 C7 50.0(4) . . . . ? O2 Sm1 N7 C7 -0.4(6) . . . . ? N2 Sm1 N7 C7 120.0(4) . . . . ? N1 Sm1 N7 C7 -27.8(4) . . . . ? N9 Sm1 N7 C7 -104.2(4) . . . . ? N8 Sm1 N7 C7 178.4(5) . . . . ? N10 Sm1 N7 C7 -143.4(4) . . . . ? O1 Sm1 N7 C18 -156.6(4) . . . . ? O2 Sm1 N7 C18 153.0(4) . . . . ? N2 Sm1 N7 C18 -86.5(4) . . . . ? N1 Sm1 N7 C18 125.7(4) . . . . ? N9 Sm1 N7 C18 49.2(4) . . . . ? N8 Sm1 N7 C18 -28.2(4) . . . . ? N10 Sm1 N7 C18 10.0(5) . . . . ? C34 N9 C23 C24 4.5(8) . . . . ? Sm1 N9 C23 C24 -150.9(4) . . . . ? C25 C24 C23 N9 -1.2(8) . . . . ? C35 C24 C23 N9 174.9(5) . . . . ? C17 N8 C16 C15 4.4(8) . . . . ? Sm1 N8 C16 C15 -146.0(5) . . . . ? N8 C17 C13 C14 0.1(8) . . . . ? C18 C17 C13 C14 178.0(5) . . . . ? N8 C17 C13 C12 -179.6(5) . . . . ? C18 C17 C13 C12 -1.6(8) . . . . ? N9 C34 C26 C25 -2.5(8) . . . . ? C33 C34 C26 C25 176.5(5) . . . . ? N9 C34 C26 C27 178.5(5) . . . . ? C33 C34 C26 C27 -2.5(8) . . . . ? O1 Sm1 N1 C1 -6.2(16) . . . . ? O2 Sm1 N1 C1 -93.9(17) . . . . ? N2 Sm1 N1 C1 -51.0(17) . . . . ? N9 Sm1 N1 C1 150.3(17) . . . . ? N7 Sm1 N1 C1 72.3(17) . . . . ? N8 Sm1 N1 C1 106.6(16) . . . . ? N10 Sm1 N1 C1 -160.5(16) . . . . ? N8 C16 C15 C14 -0.5(9) . . . . ? N8 C16 C15 C22 176.5(5) . . . . ? C32 N10 C33 C29 2.1(8) . . . . ? Sm1 N10 C33 C29 -157.1(4) . . . . ? C32 N10 C33 C34 178.5(5) . . . . ? Sm1 N10 C33 C34 19.2(6) . . . . ? N9 C34 C33 N10 3.6(7) . . . . ? C26 C34 C33 N10 -175.4(5) . . . . ? N9 C34 C33 C29 -179.9(5) . . . . ? C26 C34 C33 C29 1.0(8) . . . . ? C18 N7 C7 C8 -1.6(8) . . . . ? Sm1 N7 C7 C8 151.3(4) . . . . ? C9 C8 C7 N7 -0.7(9) . . . . ? C19 C8 C7 N7 -178.1(5) . . . . ? C23 C24 C25 C26 -4.0(8) . . . . ? C35 C24 C25 C26 -180.0(5) . . . . ? C23 C24 C25 C36 175.7(6) . . . . ? C35 C24 C25 C36 -0.3(9) . . . . ? C34 C26 C25 C24 5.7(8) . . . . ? C27 C26 C25 C24 -175.3(6) . . . . ? C34 C26 C25 C36 -174.0(6) . . . . ? C27 C26 C25 C36 5.0(9) . . . . ? N7 C18 C10 C9 -1.4(8) . . . . ? C17 C18 C10 C9 -179.0(5) . . . . ? N7 C18 C10 C11 175.9(5) . . . . ? C17 C18 C10 C11 -1.6(8) . . . . ? C12 C11 C10 C18 0.4(8) . . . . ? C12 C11 C10 C9 177.6(5) . . . . ? N10 C33 C29 C28 177.8(5) . . . . ? C34 C33 C29 C28 1.5(8) . . . . ? N10 C33 C29 C30 -0.5(8) . . . . ? C34 C33 C29 C30 -176.8(5) . . . . ? C16 C15 C14 C13 -3.6(8) . . . . ? C22 C15 C14 C13 179.5(5) . . . . ? C16 C15 C14 C21 175.1(6) . . . . ? C22 C15 C14 C21 -1.8(9) . . . . ? C17 C13 C14 C15 3.8(8) . . . . ? C12 C13 C14 C15 -176.5(5) . . . . ? C17 C13 C14 C21 -174.9(6) . . . . ? C12 C13 C14 C21 4.8(9) . . . . ? C1 Fe1 C4 N4 -33(10) . . . . ? C1 Fe1 C4 N4 147(10) 3_666 . . . ? C4 Fe1 C4 N4 130(100) 3_666 . . . ? C3 Fe1 C4 N4 -124(10) 3_666 . . . ? C3 Fe1 C4 N4 56(10) . . . . ? C32 C31 C30 C29 0.8(8) . . . . ? C38 C31 C30 C29 178.1(5) . . . . ? C32 C31 C30 C37 -179.4(6) . . . . ? C38 C31 C30 C37 -2.0(9) . . . . ? C28 C29 C30 C31 -179.2(5) . . . . ? C33 C29 C30 C31 -1.0(8) . . . . ? C28 C29 C30 C37 1.0(9) . . . . ? C33 C29 C30 C37 179.1(5) . . . . ? C2 Fe2 C6 N6 -24(66) . . . . ? C2 Fe2 C6 N6 156(100) 3_566 . . . ? C6 Fe2 C6 N6 -161(95) 3_566 . . . ? C5 Fe2 C6 N6 65(66) 3_566 . . . ? C5 Fe2 C6 N6 -115(66) . . . . ? O1 Sm1 N2 C2 -102(2) . . . . ? O2 Sm1 N2 C2 -17(2) . . . . ? N1 Sm1 N2 C2 -58(2) . . . . ? N9 Sm1 N2 C2 91(2) . . . . ? N7 Sm1 N2 C2 -171(2) . . . . ? N8 Sm1 N2 C2 138(2) . . . . ? N10 Sm1 N2 C2 62(2) . . . . ? C7 C8 C9 C10 2.0(8) . . . . ? C19 C8 C9 C10 179.3(5) . . . . ? C7 C8 C9 C20 -177.9(5) . . . . ? C19 C8 C9 C20 -0.7(9) . . . . ? C18 C10 C9 C8 -1.0(8) . . . . ? C11 C10 C9 C8 -178.2(5) . . . . ? C18 C10 C9 C20 178.9(5) . . . . ? C11 C10 C9 C20 1.7(8) . . . . ? C33 C29 C28 C27 -2.6(9) . . . . ? C30 C29 C28 C27 175.5(6) . . . . ? C10 C11 C12 C13 0.3(9) . . . . ? C17 C13 C12 C11 0.4(9) . . . . ? C14 C13 C12 C11 -179.3(6) . . . . ? C29 C28 C27 C26 1.1(9) . . . . ? C34 C26 C27 C28 1.5(9) . . . . ? C25 C26 C27 C28 -177.5(6) . . . . ? C33 N10 C32 C31 -2.5(8) . . . . ? Sm1 N10 C32 C31 155.4(4) . . . . ? C30 C31 C32 N10 1.0(9) . . . . ? C38 C31 C32 N10 -176.4(5) . . . . ? C1 Fe1 C3 N3 48(23) . . . . ? C1 Fe1 C3 N3 -132(23) 3_666 . . . ? C4 Fe1 C3 N3 -42(23) . . . . ? C4 Fe1 C3 N3 138(23) 3_666 . . . ? C3 Fe1 C3 N3 101(36) 3_666 . . . ? Sm1 N1 C1 Fe1 -39(10) . . . . ? C1 Fe1 C1 N1 -64(38) 3_666 . . . ? C4 Fe1 C1 N1 106(9) . . . . ? C4 Fe1 C1 N1 -74(9) 3_666 . . . ? C3 Fe1 C1 N1 -163(9) 3_666 . . . ? C3 Fe1 C1 N1 17(9) . . . . ? Sm1 N2 C2 Fe2 -22(15) . . . . ? C2 Fe2 C2 N2 -96(17) 3_566 . . . ? C6 Fe2 C2 N2 99(13) . . . . ? C6 Fe2 C2 N2 -81(13) 3_566 . . . ? C5 Fe2 C2 N2 9(13) 3_566 . . . ? C5 Fe2 C2 N2 -171(13) . . . . ? C2 Fe2 C5 N5 -179(100) . . . . ? C2 Fe2 C5 N5 1(20) 3_566 . . . ? C6 Fe2 C5 N5 -89(20) . . . . ? C6 Fe2 C5 N5 91(20) 3_566 . . . ? C5 Fe2 C5 N5 19(100) 3_566 . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.284 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.106 # Attachment 'compound11.txt' data_compound11 _database_code_depnum_ccdc_archive 'CCDC 296503' _audit_creation_method SHELXL-97 _chemical_name_common ; Catena-(trans-biscyano-di-agua-bis-(3,4,7,8-tetramethyl-1,10- phenanthroline)-tetracyano-chromium(iii)-samarium(iii) nonahydrate ; _chemical_formula_moiety '[Sm(tmphen)2(H2O)2Cr(CN)6]MeOH9H2O' _chemical_formula_sum 'C39 H58 Cr N10 O12 Sm' _chemical_formula_weight 1061.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.214(3) _cell_length_b 13.998(3) _cell_length_c 14.075(3) _cell_angle_alpha 105.38(3) _cell_angle_beta 92.56(3) _cell_angle_gamma 92.76(3) _cell_volume 2502.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10850 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.34 _reflns_number_total 7067 _reflns_number_gt 5299 _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^)+(0.1343P)^2^+7.8940P] 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 7067 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.321 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.24993(6) 0.14620(5) 0.35406(6) 0.0250(3) Uani 1 1 d . . . Cr2 Cr 0.5000 0.5000 0.5000 0.0254(7) Uani 1 2 d S . . Cr1 Cr 0.0000 0.0000 0.0000 0.0259(7) Uani 1 2 d S . . O2 O 0.3350(6) 0.1657(7) 0.2193(7) 0.042(2) Uani 1 1 d . . . O1 O 0.1654(6) 0.2810(6) 0.3355(7) 0.040(2) Uani 1 1 d . . . N9 N 0.3622(6) 0.0773(7) 0.4725(7) 0.027(2) Uani 1 1 d . . . N10 N 0.3189(7) -0.0242(7) 0.2828(8) 0.030(2) Uani 1 1 d . . . N7 N 0.1810(6) 0.2175(7) 0.5235(8) 0.031(2) Uani 1 1 d . . . N8 N 0.1393(6) 0.0265(7) 0.4234(8) 0.029(2) Uani 1 1 d . . . N2 N 0.3829(7) 0.2836(7) 0.4264(7) 0.028(2) Uani 1 1 d . . . C18 C 0.1572(8) 0.1539(9) 0.5793(9) 0.026(3) Uani 1 1 d . . . N1 N 0.1170(7) 0.0738(7) 0.2158(8) 0.030(2) Uani 1 1 d . . . C33 C 0.3438(8) -0.0787(10) 0.3479(10) 0.035(3) Uani 1 1 d . . . C34 C 0.3621(8) -0.0243(9) 0.4486(9) 0.028(3) Uani 1 1 d . . . C17 C 0.1376(8) 0.0532(9) 0.5250(10) 0.035(3) Uani 1 1 d . . . C14 C 0.1026(8) -0.1209(10) 0.5205(12) 0.041(4) Uani 1 1 d . . . C23 C 0.3816(8) 0.1276(10) 0.5659(9) 0.032(3) Uani 1 1 d . . . H23 H 0.3842 0.1981 0.5824 0.039 Uiso 1 1 calc R . . C16 C 0.1185(8) -0.0660(9) 0.3708(11) 0.035(3) Uani 1 1 d . . . H16 H 0.1146 -0.0815 0.3007 0.041 Uiso 1 1 calc R . . C6 C 0.6413(10) 0.4432(9) 0.4861(11) 0.040(3) Uani 1 1 d . . . C25 C 0.3964(8) -0.0207(11) 0.6201(11) 0.042(4) Uani 1 1 d . . . C15 C 0.1014(8) -0.1443(9) 0.4196(12) 0.038(3) Uani 1 1 d . . . C10 C 0.1543(9) 0.1837(10) 0.6827(11) 0.041(3) Uani 1 1 d . . . C7 C 0.1989(8) 0.3119(9) 0.5740(9) 0.028(3) Uani 1 1 d . . . H7 H 0.2154 0.3576 0.5369 0.034 Uiso 1 1 calc R . . C29 C 0.3450(9) -0.1810(10) 0.3163(11) 0.040(3) Uani 1 1 d . . . C2 C 0.4274(8) 0.3598(9) 0.4523(9) 0.026(3) Uani 1 1 d . . . C1 C 0.0716(8) 0.0484(9) 0.1407(9) 0.027(3) Uani 1 1 d . . . C24 C 0.3990(8) 0.0800(13) 0.6439(10) 0.046(4) Uani 1 1 d . . . C27 C 0.3828(9) -0.1824(12) 0.4867(14) 0.048(4) Uani 1 1 d . . . H27 H 0.3962 -0.2190 0.5334 0.058 Uiso 1 1 calc R . . C32 C 0.3014(8) -0.0732(9) 0.1878(10) 0.032(3) Uani 1 1 d . . . H32 H 0.2870 -0.0353 0.1426 0.038 Uiso 1 1 calc R . . C9 C 0.1758(9) 0.2839(12) 0.7323(10) 0.047(4) Uani 1 1 d . . . C13 C 0.1182(8) -0.0195(11) 0.5787(11) 0.040(4) Uani 1 1 d . . . N3 N -0.0024(11) 0.2237(11) -0.0195(11) 0.066(4) Uani 1 1 d . . . C5 C 0.4994(9) 0.5129(10) 0.3552(11) 0.039(3) Uani 1 1 d . . . C12 C 0.1174(9) 0.0142(13) 0.6825(12) 0.047(4) Uani 1 1 d . . . H12 H 0.1051 -0.0336 0.7183 0.057 Uiso 1 1 calc R . . C8 C 0.1960(9) 0.3503(10) 0.6743(11) 0.045(4) Uani 1 1 d . . . C11 C 0.1328(9) 0.1082(13) 0.7326(12) 0.046(4) Uani 1 1 d . . . H11 H 0.1297 0.1263 0.8023 0.055 Uiso 1 1 calc R . . C3 C 0.0003(9) 0.1427(12) -0.0125(10) 0.043(3) Uani 1 1 d . . . C21 C 0.0865(12) -0.2028(11) 0.5723(14) 0.061(5) Uani 1 1 d . . . H21A H 0.0139 -0.2216 0.5701 0.091 Uiso 1 1 calc R . . H21B H 0.1128 -0.1788 0.6413 0.091 Uiso 1 1 calc R . . H21C H 0.1226 -0.2608 0.5390 0.091 Uiso 1 1 calc R . . C28 C 0.3658(9) -0.2307(11) 0.3934(13) 0.047(4) Uani 1 1 d . . . H28 H 0.3671 -0.3010 0.3752 0.056 Uiso 1 1 calc R . . C26 C 0.3820(9) -0.0767(10) 0.5210(11) 0.038(3) Uani 1 1 d . . . C4 C -0.1417(10) 0.0147(11) 0.0573(10) 0.042(3) Uani 1 1 d . . . N5 N 0.5014(10) 0.5210(10) 0.2772(10) 0.060(4) Uani 1 1 d . . . C31 C 0.3028(9) -0.1751(11) 0.1503(10) 0.045(4) Uani 1 1 d . . . C36 C 0.4125(11) -0.0747(14) 0.7015(12) 0.059(5) Uani 1 1 d . . . H36A H 0.4853 -0.0794 0.7144 0.089 Uiso 1 1 calc R . . H36B H 0.3791 -0.1415 0.6798 0.089 Uiso 1 1 calc R . . H36C H 0.3833 -0.0373 0.7621 0.089 Uiso 1 1 calc R . . C30 C 0.3243(10) -0.2310(11) 0.2167(13) 0.053(4) Uani 1 1 d . . . C35 C 0.4119(10) 0.1467(14) 0.7481(10) 0.060(5) Uani 1 1 d . . . H35A H 0.3527 0.1363 0.7845 0.090 Uiso 1 1 calc R . . H35B H 0.4183 0.2162 0.7462 0.090 Uiso 1 1 calc R . . H35C H 0.4732 0.1308 0.7812 0.090 Uiso 1 1 calc R . . C22 C 0.0877(10) -0.2499(10) 0.3496(14) 0.061(5) Uani 1 1 d . . . H22A H 0.1458 -0.2878 0.3601 0.091 Uiso 1 1 calc R . . H22B H 0.0836 -0.2461 0.2810 0.091 Uiso 1 1 calc R . . H22C H 0.0251 -0.2831 0.3632 0.091 Uiso 1 1 calc R . . N4 N -0.2218(10) 0.0196(13) 0.0841(11) 0.076(5) Uani 1 1 d . . . N6 N 0.7233(10) 0.4151(11) 0.4782(13) 0.077(5) Uani 1 1 d . . . C20 C 0.1761(15) 0.3206(15) 0.8402(12) 0.080(6) Uani 1 1 d . . . H20A H 0.2295 0.3738 0.8638 0.119 Uiso 1 1 calc R . . H20B H 0.1890 0.2661 0.8699 0.119 Uiso 1 1 calc R . . H20C H 0.1101 0.3463 0.8588 0.119 Uiso 1 1 calc R . . C37 C 0.3225(16) -0.3422(12) 0.1827(16) 0.087(6) Uani 1 1 d . . . H37A H 0.2801 -0.3659 0.1212 0.130 Uiso 1 1 calc R . . H37B H 0.2946 -0.3704 0.2334 0.130 Uiso 1 1 calc R . . H37C H 0.3918 -0.3628 0.1713 0.130 Uiso 1 1 calc R . . C38 C 0.2810(13) -0.2236(13) 0.0415(12) 0.071(5) Uani 1 1 d . . . H38A H 0.2668 -0.1727 0.0074 0.107 Uiso 1 1 calc R . . H38B H 0.2219 -0.2710 0.0322 0.107 Uiso 1 1 calc R . . H38C H 0.3400 -0.2587 0.0143 0.107 Uiso 1 1 calc R . . C19 C 0.2186(13) 0.4567(13) 0.7239(13) 0.073(5) Uani 1 1 d . . . H19A H 0.2779 0.4645 0.7703 0.110 Uiso 1 1 calc R . . H19B H 0.1600 0.4837 0.7599 0.110 Uiso 1 1 calc R . . H19C H 0.2330 0.4926 0.6744 0.110 Uiso 1 1 calc R . . O5 O 0.5849(17) 0.5790(18) 0.1191(17) 0.154(8) Uani 1 1 d . . . O6 O 0.7478(18) 0.859(3) 0.641(3) 0.32(4) Uani 1 1 d . . . O10 O -0.0835(16) 0.3835(18) -0.0771(19) 0.154(8) Uani 1 1 d . . . O3 O 0.153(3) 0.672(3) 0.718(4) 0.38(3) Uani 1 1 d . . . O4 O 0.337(3) -0.224(5) -0.178(4) 0.49(5) Uani 1 1 d . . . O7 O 0.911(4) 0.450(2) 0.015(2) 0.35(3) Uani 1 1 d . . . O12 O -0.5000 0.0000 0.0000 0.48(7) Uani 1 2 d S . . O11 O 0.1221(19) -0.6065(14) 0.265(2) 0.195(12) Uani 1 1 d . . . O8 O 0.960(5) 0.483(4) 0.458(3) 0.36(3) Uani 1 1 d . . . O9 O 0.6218(18) -0.2357(19) -0.1063(12) 0.188(12) Uani 1 1 d . . . C39 C 0.606(3) 0.496(2) 0.0552(18) 0.158(14) Uani 1 1 d . . . H39A H 0.6372 0.5111 -0.0014 0.237 Uiso 1 1 calc R . . H39B H 0.5439 0.4537 0.0326 0.237 Uiso 1 1 calc R . . H39C H 0.6540 0.4606 0.0871 0.237 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 Sm1 0.0158(4) 0.0281(5) 0.0331(5) 0.0130(3) -0.0015(3) -0.0025(3) Cr2 0.0133(13) 0.0253(14) 0.0385(17) 0.0107(12) 0.0016(11) -0.0004(10) Cr1 0.0151(13) 0.0373(16) 0.0261(15) 0.0100(12) 0.0009(11) 0.0009(11) O2 0.031(5) 0.053(6) 0.050(6) 0.026(5) 0.006(4) -0.005(4) O1 0.031(5) 0.040(5) 0.053(6) 0.021(4) -0.006(4) -0.001(4) N9 0.008(4) 0.042(6) 0.037(6) 0.019(5) 0.001(4) 0.010(4) N10 0.017(5) 0.040(6) 0.039(7) 0.020(5) 0.007(4) 0.007(4) N7 0.009(4) 0.037(6) 0.052(7) 0.020(5) 0.005(4) 0.004(4) N8 0.006(4) 0.036(6) 0.053(7) 0.022(5) 0.013(4) 0.003(4) N2 0.023(5) 0.025(6) 0.037(6) 0.007(5) 0.001(4) 0.005(5) C18 0.009(5) 0.042(8) 0.034(7) 0.020(6) 0.010(5) 0.004(5) N1 0.020(5) 0.035(6) 0.037(6) 0.013(5) 0.004(5) -0.001(4) C33 0.003(5) 0.051(9) 0.055(9) 0.018(7) 0.005(5) 0.007(5) C34 0.010(5) 0.043(8) 0.037(8) 0.020(6) 0.006(5) 0.008(5) C17 0.014(6) 0.042(8) 0.057(9) 0.025(7) 0.010(6) 0.008(5) C14 0.009(6) 0.047(9) 0.079(11) 0.037(8) 0.013(6) 0.004(5) C23 0.012(6) 0.047(8) 0.038(8) 0.010(6) 0.007(5) 0.008(5) C16 0.008(5) 0.025(7) 0.072(10) 0.017(7) 0.003(6) 0.002(5) C6 0.029(7) 0.020(7) 0.074(10) 0.020(7) -0.001(7) -0.006(6) C25 0.013(6) 0.058(10) 0.069(11) 0.042(9) 0.007(6) 0.014(6) C15 0.011(6) 0.033(7) 0.075(11) 0.020(7) 0.018(6) 0.007(5) C10 0.026(7) 0.049(9) 0.055(9) 0.026(8) 0.018(6) 0.008(6) C7 0.014(6) 0.041(8) 0.027(7) 0.005(6) 0.004(5) -0.005(5) C29 0.018(6) 0.042(8) 0.070(10) 0.028(8) 0.016(6) 0.018(6) C2 0.017(6) 0.029(7) 0.032(7) 0.010(5) -0.003(5) 0.002(5) C1 0.012(5) 0.046(8) 0.027(7) 0.014(6) 0.004(5) 0.001(5) C24 0.006(6) 0.095(13) 0.039(8) 0.023(8) -0.002(5) 0.008(6) C27 0.013(6) 0.066(11) 0.089(13) 0.058(10) 0.011(7) 0.007(6) C32 0.011(6) 0.034(7) 0.050(9) 0.009(6) 0.003(5) 0.010(5) C9 0.022(7) 0.080(12) 0.039(8) 0.014(8) 0.019(6) 0.003(7) C13 0.009(6) 0.058(10) 0.065(10) 0.037(8) 0.010(6) 0.013(6) N3 0.069(9) 0.064(10) 0.077(10) 0.035(8) 0.026(8) 0.014(7) C5 0.030(7) 0.037(8) 0.050(10) 0.013(7) 0.004(6) 0.003(6) C12 0.017(6) 0.085(12) 0.062(11) 0.053(10) 0.019(6) 0.019(7) C8 0.024(7) 0.044(8) 0.064(10) 0.008(8) 0.015(7) 0.005(6) C11 0.020(7) 0.073(12) 0.053(9) 0.031(9) 0.011(6) -0.003(7) C3 0.029(7) 0.061(10) 0.045(9) 0.027(8) 0.002(6) 0.000(7) C21 0.049(9) 0.052(10) 0.098(13) 0.051(10) 0.011(9) -0.003(7) C28 0.015(6) 0.039(8) 0.090(13) 0.021(9) 0.003(7) 0.008(6) C26 0.018(6) 0.052(9) 0.057(10) 0.031(8) 0.019(6) 0.008(6) C4 0.028(7) 0.069(10) 0.036(8) 0.023(7) 0.006(6) 0.019(7) N5 0.073(9) 0.070(9) 0.042(8) 0.020(7) 0.011(7) 0.014(7) C31 0.024(7) 0.058(10) 0.048(9) 0.002(7) -0.002(6) 0.020(6) C36 0.037(8) 0.106(14) 0.056(10) 0.059(10) 0.004(7) 0.012(8) C30 0.027(7) 0.044(9) 0.082(12) 0.006(8) -0.006(7) 0.019(6) C35 0.021(7) 0.123(15) 0.037(9) 0.022(9) 0.008(6) 0.016(8) C22 0.024(7) 0.039(9) 0.119(15) 0.020(9) 0.006(8) 0.000(6) N4 0.046(8) 0.139(15) 0.063(9) 0.055(10) 0.021(7) 0.030(8) N6 0.035(8) 0.066(9) 0.149(15) 0.054(10) 0.025(8) 0.019(7) C20 0.080(13) 0.097(15) 0.053(11) 0.003(10) 0.028(10) -0.003(11) C37 0.106(16) 0.043(10) 0.102(15) 0.000(10) -0.013(12) 0.033(10) C38 0.069(11) 0.059(11) 0.067(12) -0.021(9) 0.006(9) 0.029(9) C19 0.067(11) 0.077(13) 0.067(12) -0.001(10) 0.035(9) -0.004(9) O5 0.169(19) 0.17(2) 0.142(18) 0.055(16) 0.063(15) 0.071(16) O6 0.040(14) 0.62(10) 0.46(7) 0.40(7) 0.05(2) 0.09(3) O10 0.144(17) 0.17(2) 0.18(2) 0.093(18) 0.025(15) 0.047(15) O3 0.26(4) 0.34(5) 0.73(9) 0.42(6) 0.26(5) 0.18(3) O4 0.34(5) 0.98(13) 0.39(5) 0.51(8) 0.28(5) 0.44(7) O7 0.75(11) 0.17(3) 0.12(2) 0.011(19) 0.05(4) 0.09(4) O12 0.88(16) 0.44(8) 0.29(6) 0.24(6) 0.44(9) 0.45(10) O11 0.19(2) 0.091(13) 0.29(3) 0.055(16) -0.13(2) -0.014(13) O8 0.51(9) 0.37(5) 0.21(4) 0.03(4) 0.00(4) 0.28(6) O9 0.21(2) 0.26(3) 0.085(12) 0.062(14) -0.021(12) -0.16(2) C39 0.30(5) 0.10(2) 0.068(17) 0.010(15) 0.05(2) 0.00(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 Sm1 O1 2.306(8) . ? Sm1 O2 2.318(8) . ? Sm1 N2 2.509(10) . ? Sm1 N1 2.525(10) . ? Sm1 N7 2.555(10) . ? Sm1 N10 2.559(10) . ? Sm1 N8 2.580(9) . ? Sm1 N9 2.585(9) . ? Cr2 C6 2.062(13) 2_666 ? Cr2 C6 2.062(13) . ? Cr2 C2 2.071(12) 2_666 ? Cr2 C2 2.071(12) . ? Cr2 C5 2.093(15) . ? Cr2 C5 2.093(15) 2_666 ? Cr1 C3 2.051(15) . ? Cr1 C3 2.051(15) 2 ? Cr1 C4 2.069(13) . ? Cr1 C4 2.069(13) 2 ? Cr1 C1 2.082(13) 2 ? Cr1 C1 2.082(13) . ? N9 C23 1.323(16) . ? N9 C34 1.372(15) . ? N10 C32 1.334(16) . ? N10 C33 1.378(15) . ? N7 C7 1.329(15) . ? N7 C18 1.369(14) . ? N8 C16 1.318(16) . ? N8 C17 1.381(17) . ? N2 C2 1.154(14) . ? C18 C10 1.408(18) . ? C18 C17 1.418(18) . ? N1 C1 1.153(15) . ? C33 C29 1.383(18) . ? C33 C34 1.423(18) . ? C34 C26 1.428(17) . ? C17 C13 1.440(17) . ? C14 C15 1.37(2) . ? C14 C13 1.44(2) . ? C14 C21 1.526(17) . ? C23 C24 1.443(19) . ? C16 C15 1.455(17) . ? C6 N6 1.171(17) . ? C25 C24 1.36(2) . ? C25 C26 1.41(2) . ? C25 C36 1.543(18) . ? C15 C22 1.54(2) . ? C10 C9 1.40(2) . ? C10 C11 1.440(19) . ? C7 C8 1.374(18) . ? C29 C30 1.40(2) . ? C29 C28 1.46(2) . ? C24 C35 1.51(2) . ? C27 C28 1.31(2) . ? C27 C26 1.43(2) . ? C32 C31 1.385(19) . ? C9 C8 1.41(2) . ? C9 C20 1.47(2) . ? C13 C12 1.41(2) . ? N3 C3 1.166(18) . ? C5 N5 1.134(17) . ? C12 C11 1.32(2) . ? C8 C19 1.48(2) . ? C4 N4 1.138(17) . ? C31 C30 1.40(2) . ? C31 C38 1.51(2) . ? C30 C37 1.50(2) . ? O5 C39 1.32(3) . ? O10 O7 1.39(3) 1_455 ? O7 O10 1.39(3) 1_655 ? O8 O8 1.52(9) 2_766 ? 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 Sm1 O2 84.0(3) . . ? O1 Sm1 N2 79.7(3) . . ? O2 Sm1 N2 75.7(3) . . ? O1 Sm1 N1 75.6(3) . . ? O2 Sm1 N1 79.2(3) . . ? N2 Sm1 N1 146.3(3) . . ? O1 Sm1 N7 76.3(3) . . ? O2 Sm1 N7 151.1(3) . . ? N2 Sm1 N7 80.0(3) . . ? N1 Sm1 N7 115.2(3) . . ? O1 Sm1 N10 151.2(3) . . ? O2 Sm1 N10 76.4(3) . . ? N2 Sm1 N10 114.8(3) . . ? N1 Sm1 N10 80.1(3) . . ? N7 Sm1 N10 129.0(3) . . ? O1 Sm1 N8 112.9(3) . . ? O2 Sm1 N8 145.5(3) . . ? N2 Sm1 N8 135.0(3) . . ? N1 Sm1 N8 76.7(3) . . ? N7 Sm1 N8 63.1(3) . . ? N10 Sm1 N8 75.4(3) . . ? O1 Sm1 N9 145.3(3) . . ? O2 Sm1 N9 112.5(3) . . ? N2 Sm1 N9 75.7(3) . . ? N1 Sm1 N9 135.7(3) . . ? N7 Sm1 N9 75.7(3) . . ? N10 Sm1 N9 63.1(3) . . ? N8 Sm1 N9 71.1(3) . . ? C6 Cr2 C6 180.000(2) 2_666 . ? C6 Cr2 C2 92.1(4) 2_666 2_666 ? C6 Cr2 C2 87.9(4) . 2_666 ? C6 Cr2 C2 87.9(4) 2_666 . ? C6 Cr2 C2 92.1(4) . . ? C2 Cr2 C2 180.000(1) 2_666 . ? C6 Cr2 C5 89.7(5) 2_666 . ? C6 Cr2 C5 90.3(5) . . ? C2 Cr2 C5 88.8(5) 2_666 . ? C2 Cr2 C5 91.2(5) . . ? C6 Cr2 C5 90.3(5) 2_666 2_666 ? C6 Cr2 C5 89.7(5) . 2_666 ? C2 Cr2 C5 91.2(5) 2_666 2_666 ? C2 Cr2 C5 88.8(5) . 2_666 ? C5 Cr2 C5 180.000(3) . 2_666 ? C3 Cr1 C3 180.0(8) . 2 ? C3 Cr1 C4 89.9(5) . . ? C3 Cr1 C4 90.1(5) 2 . ? C3 Cr1 C4 90.1(5) . 2 ? C3 Cr1 C4 89.9(5) 2 2 ? C4 Cr1 C4 180.000(1) . 2 ? C3 Cr1 C1 88.8(5) . 2 ? C3 Cr1 C1 91.2(5) 2 2 ? C4 Cr1 C1 88.6(5) . 2 ? C4 Cr1 C1 91.4(5) 2 2 ? C3 Cr1 C1 91.2(5) . . ? C3 Cr1 C1 88.8(5) 2 . ? C4 Cr1 C1 91.4(5) . . ? C4 Cr1 C1 88.6(5) 2 . ? C1 Cr1 C1 180.000(1) 2 . ? C23 N9 C34 118.5(10) . . ? C23 N9 Sm1 121.2(8) . . ? C34 N9 Sm1 114.6(7) . . ? C32 N10 C33 117.6(11) . . ? C32 N10 Sm1 121.6(7) . . ? C33 N10 Sm1 117.4(8) . . ? C7 N7 C18 115.0(11) . . ? C7 N7 Sm1 122.5(7) . . ? C18 N7 Sm1 118.5(8) . . ? C16 N8 C17 121.6(10) . . ? C16 N8 Sm1 120.1(8) . . ? C17 N8 Sm1 114.2(7) . . ? C2 N2 Sm1 163.9(8) . . ? N7 C18 C10 123.6(12) . . ? N7 C18 C17 114.8(11) . . ? C10 C18 C17 121.5(11) . . ? C1 N1 Sm1 164.9(9) . . ? N10 C33 C29 120.8(12) . . ? N10 C33 C34 116.2(11) . . ? C29 C33 C34 122.9(12) . . ? N9 C34 C33 118.7(10) . . ? N9 C34 C26 122.1(11) . . ? C33 C34 C26 119.2(12) . . ? N8 C17 C18 120.2(10) . . ? N8 C17 C13 121.4(12) . . ? C18 C17 C13 118.3(12) . . ? C15 C14 C13 120.8(11) . . ? C15 C14 C21 119.9(14) . . ? C13 C14 C21 119.2(14) . . ? N9 C23 C24 122.8(13) . . ? N8 C16 C15 120.2(13) . . ? N6 C6 Cr2 177.0(11) . . ? C24 C25 C26 120.5(12) . . ? C24 C25 C36 120.2(15) . . ? C26 C25 C36 119.3(13) . . ? C14 C15 C16 119.6(12) . . ? C14 C15 C22 125.6(12) . . ? C16 C15 C22 114.7(13) . . ? C9 C10 C18 118.9(11) . . ? C9 C10 C11 123.3(14) . . ? C18 C10 C11 117.8(13) . . ? N7 C7 C8 126.7(12) . . ? C33 C29 C30 120.6(12) . . ? C33 C29 C28 115.6(14) . . ? C30 C29 C28 123.8(13) . . ? N2 C2 Cr2 177.0(10) . . ? N1 C1 Cr1 175.6(10) . . ? C25 C24 C23 118.5(13) . . ? C25 C24 C35 124.5(14) . . ? C23 C24 C35 116.8(14) . . ? C28 C27 C26 122.6(13) . . ? N10 C32 C31 125.0(12) . . ? C10 C9 C8 117.5(13) . . ? C10 C9 C20 122.2(14) . . ? C8 C9 C20 120.4(15) . . ? C12 C13 C14 126.0(12) . . ? C12 C13 C17 117.8(13) . . ? C14 C13 C17 116.1(13) . . ? N5 C5 Cr2 178.4(13) . . ? C11 C12 C13 123.7(13) . . ? C7 C8 C9 118.2(13) . . ? C7 C8 C19 122.6(13) . . ? C9 C8 C19 119.0(14) . . ? C12 C11 C10 120.8(14) . . ? N3 C3 Cr1 178.1(12) . . ? C27 C28 C29 122.7(13) . . ? C25 C26 C27 125.5(12) . . ? C25 C26 C34 117.5(12) . . ? C27 C26 C34 117.0(13) . . ? N4 C4 Cr1 176.3(15) . . ? C32 C31 C30 117.6(13) . . ? C32 C31 C38 120.9(13) . . ? C30 C31 C38 121.5(14) . . ? C29 C30 C31 118.4(13) . . ? C29 C30 C37 120.7(15) . . ? C31 C30 C37 120.9(15) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.375 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.200