Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Julve, M.' 'Andruh, Marius' 'Lescouezec, R.' 'Lloret, F.' 'Toma, Luminita M.' 'Toma, Liviu' 'Vaissermann, Jacqueline' _publ_contact_author_name 'Prof M Julve' _publ_contact_author_address ; Department de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica de la Universitat de Valencia Dr Moliner 50 Burjassot 46100 SPAIN ; _publ_contact_author_phone ' 0034 386 4856' _publ_contact_author_fax ' 0034 398 3001' _publ_contact_author_email ' miguel.julve@uv.es' _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ' ? ' _publ_contact_letter ; ; #============================================================================= # TITLE AND AUTHOR LIST _publ_section_title ; [Mn2(bipym)(H20)8]4+ and [Fe(bipy)(CN4]- as building blocks in designing novel bipym- and cyanide-bridged heterobimetallic complexes (bipym = 2,2'-bipyrimidine and bipy = 2,2'- bipyridine) ; #============================================================================== _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; data_compound1 _database_code_CSD 174231 _audit_creation_date 01-06-25 _audit_creation_method CRYSTALS _chemical_melting_point ? _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Enraf-nonius CAD4' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary 'Direct_Methods' _atom_sites_solution_hydrogens 'Geometric' _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle, one overall isotropic thermal parameter refined. ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 10.052(2) _cell_angle_alpha 90 _cell_length_b 12.345(2) _cell_angle_beta 90.13(1) _cell_length_c 12.886(2) _cell_angle_gamma 90 _cell_volume 1599.0(5) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'K ' 0.1790 0.2500 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International_Tables_Vol_IV_Table_2.2B' 'Fe ' 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C14 H10 Fe1 K1 N6 O1 ' _chemical_formula_moiety ' C14 H8 Fe1 N6 1-, K 1+, H2O ' _chemical_compound_source ; ? ; _chemical_formula_weight 373.22 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 295 _cell_formula_units_Z 4 _exptl_crystal_description 'stick' _exptl_crystal_colour 'red' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.8 _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_meas ? _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.21 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_process_details 'refined from delta-F' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600 _diffrn_standards_number 2 _diffrn_standards_decay_% 'none' _diffrn_ambient_temperature 295 _diffrn_reflns_number 3127 _reflns_number_total 2800 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 1684 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.31 _refine_diff_density_max 0.27 _refine_ls_number_reflns 1684 _refine_ls_number_parameters 210 _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_obs 0.0446 _refine_ls_goodness_of_fit_obs 1.1238 _refine_ls_shift/esd_max 0.001758 _refine_ls_structure_factor_coef 'F' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type FE1 0.15660(6) 0.27398(5) 0.04240(4) 0.0302 1.0000 Uani N1 -0.1340(4) 0.2711(4) -0.0353(3) 0.0526 1.0000 Uani N2 0.2325(4) 0.4646(4) -0.0972(3) 0.0540 1.0000 Uani N3 0.2184(5) 0.1223(4) -0.1375(3) 0.0582 1.0000 Uani N4 0.4574(4) 0.2654(3) 0.0952(3) 0.0498 1.0000 Uani N11 0.1112(3) 0.3698(3) 0.1615(2) 0.0315 1.0000 Uani N12 0.1158(3) 0.1603(3) 0.1471(3) 0.0349 1.0000 Uani C1 -0.0273(4) 0.2733(4) -0.0068(3) 0.0381 1.0000 Uani C2 0.2022(4) 0.3917(4) -0.0474(3) 0.0396 1.0000 Uani C3 0.1966(4) 0.1778(4) -0.0708(3) 0.0379 1.0000 Uani C4 0.3454(4) 0.2671(3) 0.0795(3) 0.0348 1.0000 Uani C11 0.1009(4) 0.4781(3) 0.1586(3) 0.0386 1.0000 Uani C12 0.0712(5) 0.5382(4) 0.2452(4) 0.0455 1.0000 Uani C13 0.0509(5) 0.4857(4) 0.3374(4) 0.0484 1.0000 Uani C14 0.0591(5) 0.3745(4) 0.3412(3) 0.0479 1.0000 Uani C15 0.0893(4) 0.3181(4) 0.2520(3) 0.0351 1.0000 Uani C16 0.0926(4) 0.1997(3) 0.2442(3) 0.0346 1.0000 Uani C17 0.0686(5) 0.1305(4) 0.3269(4) 0.0460 1.0000 Uani C18 0.0680(5) 0.0213(4) 0.3102(4) 0.0514 1.0000 Uani C19 0.0893(5) -0.0185(4) 0.2113(4) 0.0460 1.0000 Uani C20 0.1132(4) 0.0533(3) 0.1315(4) 0.0404 1.0000 Uani K1 0.2181(1) 0.18135(8) 0.64910(8) 0.0467 1.0000 Uani O1 0.7695(4) 0.1159(3) 0.1887(3) 0.0671 1.0000 Uani H1 0.7725 0.0733 0.2475 0.068(5) 1.0000 Uiso H2 0.7656 0.0588 0.1487 0.068(5) 1.0000 Uiso H111 0.1154 0.5164 0.0910 0.068(5) 1.0000 Uiso H121 0.0638 0.6190 0.2412 0.068(5) 1.0000 Uiso H131 0.0306 0.5279 0.4018 0.068(5) 1.0000 Uiso H141 0.0438 0.3351 0.4081 0.068(5) 1.0000 Uiso H171 0.0515 0.1603 0.3979 0.068(5) 1.0000 Uiso H181 0.0519 -0.0300 0.3691 0.068(5) 1.0000 Uiso H191 0.0877 -0.0983 0.1979 0.068(5) 1.0000 Uiso H201 0.1291 0.0245 0.0599 0.068(5) 1.0000 Uiso 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 FE1 0.0317(3) 0.0310(3) 0.0282(3) 0.0003(2) 0.0006(2) 0.0002(2) N1 0.041(2) 0.071(3) 0.052(2) 0.005(2) -0.009(2) 0.002(2) N2 0.072(3) 0.052(3) 0.048(2) 0.012(2) 0.015(2) 0.000(2) N3 0.070(3) 0.062(3) 0.050(2) -0.016(2) 0.005(2) 0.005(2) N4 0.039(2) 0.047(2) 0.068(3) 0.001(2) -0.007(2) -0.002(2) N11 0.029(2) 0.035(2) 0.032(2) 0.002(1) 0.001(1) 0.003(1) N12 0.033(2) 0.037(2) 0.036(2) 0.003(2) -0.000(1) -0.005(1) C1 0.040(2) 0.041(2) 0.035(2) 0.004(2) 0.000(2) 0.003(2) C2 0.040(2) 0.047(3) 0.034(2) -0.004(2) -0.001(2) 0.004(2) C3 0.045(2) 0.038(2) 0.033(2) -0.006(2) -0.002(2) 0.001(2) C4 0.047(3) 0.029(2) 0.031(2) -0.002(2) -0.001(2) -0.000(2) C11 0.039(2) 0.036(2) 0.042(2) 0.002(2) 0.003(2) 0.002(2) C12 0.049(3) 0.041(3) 0.049(3) -0.006(2) -0.001(2) 0.006(2) C13 0.061(3) 0.049(3) 0.044(3) -0.014(2) 0.009(2) 0.002(2) C14 0.059(3) 0.055(3) 0.037(2) 0.001(2) 0.012(2) -0.005(2) C15 0.032(2) 0.042(2) 0.033(2) 0.001(2) 0.003(2) -0.003(2) C16 0.030(2) 0.037(2) 0.038(2) 0.005(2) 0.001(2) -0.001(2) C17 0.048(3) 0.052(3) 0.043(2) 0.014(2) 0.003(2) -0.003(2) C18 0.051(3) 0.052(3) 0.058(3) 0.018(2) 0.001(2) -0.003(2) C19 0.044(3) 0.033(2) 0.075(4) 0.013(2) -0.007(2) -0.004(2) C20 0.042(2) 0.030(2) 0.054(3) 0.002(2) -0.003(2) 0.001(2) K1 0.0439(6) 0.0450(6) 0.0524(6) -0.0052(5) -0.0018(5) 0.0033(5) O1 0.090(3) 0.055(2) 0.064(2) 0.010(2) 0.005(2) 0.008(2) _refine_ls_extinction_coef 'none' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag FE1 . N11 . 1.991(3) yes FE1 . N12 . 1.990(3) yes FE1 . C1 . 1.952(4) yes FE1 . C2 . 1.914(5) yes FE1 . C3 . 1.924(4) yes FE1 . C4 . 1.958(5) yes N1 . C1 . 1.134(5) yes N2 . C2 . 1.147(6) yes N3 . C3 . 1.122(6) yes N4 . C4 . 1.143(5) yes N11 . C11 . 1.342(5) yes N11 . C15 . 1.347(5) yes N12 . C16 . 1.363(5) yes N12 . C20 . 1.337(5) yes C11 . C12 . 1.374(6) yes C11 . H111 . 1.002 no C12 . C13 . 1.368(7) yes C12 . H121 . 1.002 no C13 . C14 . 1.376(7) yes C13 . H131 . 1.001 no C14 . C15 . 1.379(6) yes C14 . H141 . 1.001 no C15 . C16 . 1.466(6) yes C16 . C17 . 1.387(6) yes C17 . C18 . 1.365(7) yes C17 . H171 . 1.002 no C18 . C19 . 1.383(7) yes C18 . H181 . 1.002 no C19 . C20 . 1.380(6) yes C19 . H191 . 1.000 no C20 . H201 . 1.002 no O1 . H1 . 0.923 no O1 . H2 . 0.874 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N11 . FE1 . N12 . 81.3(1) no N11 . FE1 . C1 . 92.0(2) no N12 . FE1 . C1 . 91.2(2) no N11 . FE1 . C2 . 94.1(2) no N12 . FE1 . C2 . 174.4(2) no C1 . FE1 . C2 . 92.0(2) no N11 . FE1 . C3 . 178.1(2) no N12 . FE1 . C3 . 97.0(2) no C1 . FE1 . C3 . 87.2(2) no C2 . FE1 . C3 . 87.7(2) no N11 . FE1 . C4 . 93.5(1) no N12 . FE1 . C4 . 90.3(2) no C1 . FE1 . C4 . 174.5(2) no C2 . FE1 . C4 . 87.0(2) no C3 . FE1 . C4 . 87.4(2) no FE1 . N11 . C11 . 126.0(3) no FE1 . N11 . C15 . 115.1(3) no C11 . N11 . C15 . 118.9(4) no FE1 . N12 . C16 . 114.0(3) no FE1 . N12 . C20 . 126.8(3) no C16 . N12 . C20 . 119.2(4) no FE1 . C1 . N1 . 178.9(4) no FE1 . C2 . N2 . 176.7(4) no FE1 . C3 . N3 . 179.0(4) no FE1 . C4 . N4 . 175.8(4) no N11 . C11 . C12 . 122.2(4) no N11 . C11 . H111 . 118.9 no C12 . C11 . H111 . 118.9 no C11 . C12 . C13 . 118.8(4) no C11 . C12 . H121 . 120.7 no C13 . C12 . H121 . 120.4 no C12 . C13 . C14 . 119.6(4) no C12 . C13 . H131 . 120.3 no C14 . C13 . H131 . 120.1 no C13 . C14 . C15 . 119.1(4) no C13 . C14 . H141 . 120.4 no C15 . C14 . H141 . 120.5 no N11 . C15 . C14 . 121.3(4) no N11 . C15 . C16 . 114.2(3) no C14 . C15 . C16 . 124.4(4) no N12 . C16 . C15 . 114.9(3) no N12 . C16 . C17 . 121.1(4) no C15 . C16 . C17 . 123.9(4) no C16 . C17 . C18 . 119.2(5) no C16 . C17 . H171 . 120.4 no C18 . C17 . H171 . 120.4 no C17 . C18 . C19 . 119.7(4) no C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 119.9 no C18 . C19 . C20 . 119.1(4) no C18 . C19 . H191 . 120.4 no C20 . C19 . H191 . 120.5 no N12 . C20 . C19 . 121.7(4) no N12 . C20 . H201 . 119.2 no C19 . C20 . H201 . 119.1 no H1 . O1 . H2 . 91.4 no data_compound2 _database_code_CSD 174232 _audit_creation_date 01-06-26 _audit_creation_method CRYSTALS #**************************************************************************** #Compound 2 #**************************************************************************** #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator ' graphite ' _diffrn_measurement_device ' Enraf-nonius CAD4 ' _refine_ls_matrix_type ' full ' _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary ' Direct_Methods' _atom_sites_solution_hydrogens ' Geometric' _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle one overall isotropic thermal parameter refined ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 13.624(3) _cell_angle_alpha 90 _cell_length_b 14.927(2) _cell_angle_beta 107.30(2) _cell_length_c 21.767(5) _cell_angle_gamma 90 _cell_volume 4226(1) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Mn ' 0.2950 0.7290 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International_Tables_Vol_IV_Table_2.2B' 'Fe ' 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C64 H74 Fe4 Mn2 N28 O18 ' _chemical_formula_moiety ' C36 H34 Fe2 Mn2 N16 O6 2+, (C14 H8 Fe N6 2+)2, (H2 O)12 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1856.7 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 295 _cell_formula_units_Z 2 _exptl_crystal_description ' stick ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.46 _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.02 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_process_details 'refined from delta-F' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600 _diffrn_standards_number 2 _diffrn_standards_decay_% 7.68 _diffrn_ambient_temperature 295 _diffrn_reflns_number 8086 _reflns_number_total 7415 _diffrn_reflns_av_R_equivalents 0.08 _reflns_number_observed 1527 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.42 _refine_diff_density_max 1.28 _refine_ls_number_reflns 1527 _refine_ls_number_parameters 234 _refine_ls_R_factor_obs 0.0671 _refine_ls_wR_factor_obs 0.0803 _refine_ls_goodness_of_fit_obs 1.1038 _refine_ls_shift/esd_max 0.215185 _refine_ls_structure_factor_coef 'F' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type FE1 0.7148(2) 0.3535(2) 0.1546(1) 0.0303(8) 1.0000 Uiso FE2 0.7838(2) 0.6365(2) -0.1646(1) 0.0283(8) 1.0000 Uiso MN1 0.8275(2) 0.1155(2) 0.0221(1) 0.0330(8) 1.0000 Uiso O1 0.779(1) 0.007(1) 0.0716(7) 0.056(4) 1.0000 Uiso O2 0.675(1) 0.121(1) -0.0401(7) 0.067(5) 1.0000 Uiso O3 0.883(1) 0.2209(9) -0.0304(6) 0.045(4) 1.0000 Uiso N1 0.821(1) 0.209(1) 0.0979(8) 0.050(5) 1.0000 Uiso N2 0.629(1) 0.201(1) 0.2150(9) 0.060(5) 1.0000 Uiso N3 0.892(1) 0.366(1) 0.2808(9) 0.061(6) 1.0000 Uiso N4 0.525(1) 0.339(1) 0.0345(8) 0.043(5) 1.0000 Uiso N5 0.867(1) 0.767(1) -0.2441(8) 0.040(4) 1.0000 Uiso N6 0.688(1) 0.792(1) -0.1106(9) 0.055(5) 1.0000 Uiso N7 0.974(1) 0.658(1) -0.0468(8) 0.044(5) 1.0000 Uiso N8 0.598(1) 0.631(1) -0.2851(9) 0.054(5) 1.0000 Uiso N9 0.994(1) 0.070(1) 0.0649(7) 0.026(4) 1.0000 Uiso N10 1.131(1) -0.014(1) 0.0488(7) 0.028(4) 1.0000 Uiso N11 0.648(1) 0.453(1) 0.1874(7) 0.027(4) 1.0000 Uiso N12 0.774(1) 0.457(1) 0.1190(7) 0.031(4) 1.0000 Uiso N21 0.724(1) 0.542(1) -0.1229(7) 0.036(5) 1.0000 Uiso N22 0.848(1) 0.528(1) -0.1911(7) 0.031(4) 1.0000 Uiso C1 0.783(2) 0.262(1) 0.120(1) 0.041(6) 1.0000 Uiso C2 0.660(2) 0.264(1) 0.192(1) 0.041(6) 1.0000 Uiso C3 0.829(1) 0.360(1) 0.2343(9) 0.031(5) 1.0000 Uiso C4 0.594(2) 0.347(1) 0.080(1) 0.040(6) 1.0000 Uiso C5 0.840(2) 0.721(1) -0.214(1) 0.039(5) 1.0000 Uiso C6 0.726(2) 0.737(1) -0.132(1) 0.041(6) 1.0000 Uiso C7 0.903(2) 0.652(1) -0.0896(9) 0.031(5) 1.0000 Uiso C8 0.670(2) 0.629(1) -0.240(1) 0.044(6) 1.0000 Uiso C11 0.580(2) 0.450(1) 0.2231(9) 0.032(5) 1.0000 Uiso C12 0.545(1) 0.523(1) 0.2435(9) 0.036(5) 1.0000 Uiso C13 0.570(2) 0.604(2) 0.228(1) 0.050(6) 1.0000 Uiso C14 0.640(2) 0.615(2) 0.189(1) 0.061(7) 1.0000 Uiso C15 0.675(2) 0.534(1) 0.170(1) 0.040(6) 1.0000 Uiso C16 0.746(2) 0.540(2) 0.132(1) 0.048(6) 1.0000 Uiso C17 0.784(2) 0.613(2) 0.109(1) 0.049(6) 1.0000 Uiso C18 0.848(1) 0.609(1) 0.0729(9) 0.039(5) 1.0000 Uiso C19 0.873(2) 0.521(2) 0.061(1) 0.044(6) 1.0000 Uiso C20 0.838(1) 0.445(1) 0.0833(9) 0.031(5) 1.0000 Uiso C21 0.659(2) 0.555(1) -0.0886(9) 0.042(6) 1.0000 Uiso C22 0.619(2) 0.484(2) -0.062(1) 0.051(7) 1.0000 Uiso C23 0.654(1) 0.399(1) -0.0670(9) 0.038(5) 1.0000 Uiso C24 0.722(2) 0.386(2) -0.1032(9) 0.041(5) 1.0000 Uiso C25 0.758(1) 0.460(1) -0.1303(8) 0.019(4) 1.0000 Uiso C26 0.827(1) 0.450(1) -0.1690(9) 0.032(5) 1.0000 Uiso C27 0.869(1) 0.371(1) -0.1820(8) 0.030(4) 1.0000 Uiso C28 0.932(1) 0.370(1) -0.2193(9) 0.038(5) 1.0000 Uiso C29 0.957(2) 0.448(2) -0.241(1) 0.053(7) 1.0000 Uiso C30 0.916(2) 0.531(2) -0.226(1) 0.041(6) 1.0000 Uiso C31 1.052(1) 0.097(1) 0.1236(9) 0.035(5) 1.0000 Uiso C32 1.153(1) 0.064(1) 0.1470(9) 0.037(5) 1.0000 Uiso C33 1.191(2) 0.010(1) 0.107(1) 0.043(6) 1.0000 Uiso C34 1.035(1) 0.013(1) 0.0321(7) 0.019(4) 1.0000 Uiso O10 0.763(1) 0.830(1) 0.0281(7) 0.068(5) 1.0000 Uiso O11 0.978(1) 0.836(1) 0.0865(7) 0.064(4) 1.0000 Uiso O12 0.422(1) 0.795(1) 0.1468(8) 0.090(6) 1.0000 Uiso O13 0.661(1) 0.027(1) 0.1543(9) 0.097(6) 1.0000 Uiso O14 0.599(1) 0.771(1) 0.0623(8) 0.089(6) 1.0000 Uiso O15 0.448(2) 0.070(2) 0.083(1) 0.18(1) 1.0000 Uiso H111 0.5550 0.3864 0.2343 0.05(1) 1.0000 Uiso H121 0.5000 0.5155 0.2726 0.05(1) 1.0000 Uiso H131 0.5345 0.6554 0.2417 0.05(1) 1.0000 Uiso H141 0.6623 0.6727 0.1779 0.05(1) 1.0000 Uiso H171 0.7552 0.6801 0.1195 0.05(1) 1.0000 Uiso H181 0.8762 0.6643 0.0520 0.05(1) 1.0000 Uiso H191 0.9291 0.5166 0.0375 0.05(1) 1.0000 Uiso H201 0.8588 0.3843 0.0707 0.05(1) 1.0000 Uiso H211 0.6394 0.6206 -0.0811 0.05(1) 1.0000 Uiso H221 0.5647 0.4969 -0.0419 0.05(1) 1.0000 Uiso H231 0.6334 0.3494 -0.0429 0.05(1) 1.0000 Uiso H241 0.7495 0.3266 -0.1090 0.05(1) 1.0000 Uiso H271 0.8521 0.3132 -0.1632 0.05(1) 1.0000 Uiso H281 0.9622 0.3109 -0.2311 0.05(1) 1.0000 Uiso H291 1.0090 0.4491 -0.2652 0.05(1) 1.0000 Uiso H301 0.9294 0.5932 -0.2438 0.05(1) 1.0000 Uiso H311 1.0314 0.1475 0.1498 0.05(1) 1.0000 Uiso H321 1.1985 0.0780 0.1921 0.05(1) 1.0000 Uiso H331 1.2654 -0.0097 0.1241 0.05(1) 1.0000 Uiso _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag FE1 . N11 . 1.99(2) yes FE1 . N12 . 2.00(2) yes FE1 . C1 . 1.92(2) yes FE1 . C2 . 1.83(2) yes FE1 . C3 . 1.95(2) yes FE1 . C4 . 1.94(2) yes FE2 . N21 . 1.98(2) yes FE2 . N22 . 2.00(2) yes FE2 . C5 . 1.95(2) yes FE2 . C6 . 1.93(2) yes FE2 . C7 . 1.94(2) yes FE2 . C8 . 1.89(2) yes MN1 . O1 . 2.16(1) yes MN1 . O2 . 2.12(2) yes MN1 . O3 . 2.21(1) yes MN1 . N1 . 2.19(2) yes MN1 . N9 . 2.29(1) yes MN1 . N10 2_755 2.35(1) yes N1 . C1 . 1.13(2) yes N2 . C2 . 1.20(2) yes N3 . C3 . 1.12(2) yes N4 . C4 . 1.16(2) yes N5 . C5 . 1.09(2) yes N6 . C6 . 1.14(2) yes N7 . C7 . 1.13(2) yes N8 . C8 . 1.18(2) yes N9 . C31 . 1.35(2) yes N9 . C34 . 1.33(2) yes N10 . C33 . 1.34(2) yes N10 . C34 . 1.31(2) yes N11 . C11 . 1.37(2) yes N11 . C15 . 1.35(2) yes N12 . C16 . 1.36(3) yes N12 . C20 . 1.34(2) yes N21 . C21 . 1.33(2) yes N21 . C25 . 1.33(2) yes N22 . C26 . 1.32(2) yes N22 . C30 . 1.36(2) yes C11 . C12 . 1.32(3) yes C11 . H111 . 1.06 no C12 . C13 . 1.35(3) yes C12 . H121 . 1.00 no C13 . C14 . 1.45(3) yes C13 . H131 . 1.00 no C14 . C15 . 1.41(3) yes C14 . H141 . 0.96 no C15 . C16 . 1.46(3) yes C16 . C17 . 1.35(3) yes C17 . C18 . 1.34(3) yes C17 . H171 . 1.12 no C18 . C19 . 1.40(3) yes C18 . H181 . 1.07 no C19 . C20 . 1.38(3) yes C19 . H191 . 1.03 no C20 . H201 . 1.01 no C21 . C22 . 1.38(3) yes C21 . H211 . 1.04 no C22 . C23 . 1.38(3) yes C22 . H221 . 0.99 no C23 . C24 . 1.39(2) yes C23 . H231 . 0.99 no C24 . C25 . 1.41(3) yes C24 . H241 . 0.99 no C25 . C26 . 1.45(2) yes C26 . C27 . 1.37(2) yes C27 . C28 . 1.35(2) yes C27 . H271 . 1.02 no C28 . C29 . 1.33(3) yes C28 . H281 . 1.04 no C29 . C30 . 1.44(3) yes C29 . H291 . 1.00 no C30 . H301 . 1.05 no C31 . C32 . 1.40(2) yes C31 . H311 . 1.04 no C32 . C33 . 1.39(2) yes C32 . H321 . 1.01 no C33 . H331 . 1.01 no C34 . C34 2_755 1.49(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N11 . FE1 . N12 . 81.0(6) no N11 . FE1 . C1 . 176.9(8) no N12 . FE1 . C1 . 95.9(7) no N11 . FE1 . C2 . 95.6(7) no N12 . FE1 . C2 . 176.0(8) no C1 . FE1 . C2 . 87.5(9) no N11 . FE1 . C3 . 88.6(7) no N12 . FE1 . C3 . 90.1(7) no C1 . FE1 . C3 . 91.9(8) no C2 . FE1 . C3 . 87.7(9) no N11 . FE1 . C4 . 88.3(8) no N12 . FE1 . C4 . 93.4(8) no C1 . FE1 . C4 . 91.5(9) no C2 . FE1 . C4 . 88.6(9) no C3 . FE1 . C4 . 174.9(7) no N21 . FE2 . N22 . 80.3(6) no N21 . FE2 . C5 . 174.0(8) no N22 . FE2 . C5 . 95.2(7) no N21 . FE2 . C6 . 96.6(7) no N22 . FE2 . C6 . 175.1(8) no C5 . FE2 . C6 . 88.1(9) no N21 . FE2 . C7 . 93.1(7) no N22 . FE2 . C7 . 90.7(7) no C5 . FE2 . C7 . 91.1(8) no C6 . FE2 . C7 . 85.7(8) no N21 . FE2 . C8 . 90.5(8) no N22 . FE2 . C8 . 91.0(8) no C5 . FE2 . C8 . 85.5(9) no C6 . FE2 . C8 . 92.8(9) no C7 . FE2 . C8 . 176.3(9) no O1 . MN1 . O2 . 87.9(6) no O1 . MN1 . O3 . 176.4(6) no O2 . MN1 . O3 . 93.6(6) no O1 . MN1 . N1 . 90.9(6) no O2 . MN1 . N1 . 101.7(6) no O3 . MN1 . N1 . 92.0(6) no O1 . MN1 . N9 . 89.4(5) no O2 . MN1 . N9 . 160.0(6) no O3 . MN1 . N9 . 88.1(5) no N1 . MN1 . N9 . 98.1(6) no O1 . MN1 . N10 2_755 90.8(5) no O2 . MN1 . N10 2_755 89.3(6) no O3 . MN1 . N10 2_755 85.9(5) no N1 . MN1 . N10 2_755 168.9(6) no N9 . MN1 . N10 2_755 70.9(5) no MN1 . N1 . C1 . 154.1(18) no MN1 . N9 . C31 . 122.4(12) no MN1 . N9 . C34 . 119.3(11) no C31 . N9 . C34 . 118.3(15) no MN1 2_755 N10 . C33 . 126.3(12) no MN1 2_755 N10 . C34 . 115.8(11) no C33 . N10 . C34 . 117.4(15) no FE1 . N11 . C11 . 129.3(13) no FE1 . N11 . C15 . 112.2(12) no C11 . N11 . C15 . 118.5(17) no FE1 . N12 . C16 . 117.4(13) no FE1 . N12 . C20 . 122.2(13) no C16 . N12 . C20 . 120.5(17) no FE2 . N21 . C21 . 126.0(15) no FE2 . N21 . C25 . 113.0(12) no C21 . N21 . C25 . 120.9(17) no FE2 . N22 . C26 . 116.6(12) no FE2 . N22 . C30 . 124.3(15) no C26 . N22 . C30 . 118.9(17) no FE1 . C1 . N1 . 177.5(21) no FE1 . C2 . N2 . 175.4(19) no FE1 . C3 . N3 . 177.2(19) no FE1 . C4 . N4 . 175.7(18) no FE2 . C5 . N5 . 175.9(20) no FE2 . C6 . N6 . 175.3(20) no FE2 . C7 . N7 . 177.1(18) no FE2 . C8 . N8 . 174.3(21) no N11 . C11 . C12 . 122.4(19) no N11 . C11 . H111 . 118.9 no C12 . C11 . H111 . 118.7 no C11 . C12 . C13 . 120.8(18) no C11 . C12 . H121 . 118.5 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 121.1(22) no C12 . C13 . H131 . 115.1 no C14 . C13 . H131 . 123.6 no C13 . C14 . C15 . 114.3(23) no C13 . C14 . H141 . 124.0 no C15 . C14 . H141 . 121.7 no N11 . C15 . C14 . 122.9(18) no N11 . C15 . C16 . 119.9(21) no C14 . C15 . C16 . 117.2(21) no N12 . C16 . C15 . 109.5(21) no N12 . C16 . C17 . 120.2(20) no C15 . C16 . C17 . 130.3(23) no C16 . C17 . C18 . 124.1(24) no C16 . C17 . H171 . 116.7 no C18 . C17 . H171 . 119.0 no C17 . C18 . C19 . 113.5(21) no C17 . C18 . H181 . 126.5 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 124.6(18) no C18 . C19 . H191 . 114.8 no C20 . C19 . H191 . 120.2 no N12 . C20 . C19 . 117.2(18) no N12 . C20 . H201 . 123.7 no C19 . C20 . H201 . 119.1 no N21 . C21 . C22 . 122.0(20) no N21 . C21 . H211 . 118.0 no C22 . C21 . H211 . 120.0 no C21 . C22 . C23 . 119.3(20) no C21 . C22 . H221 . 118.8 no C23 . C22 . H221 . 121.9 no C22 . C23 . C24 . 117.7(20) no C22 . C23 . H231 . 119.3 no C24 . C23 . H231 . 123.0 no C23 . C24 . C25 . 120.3(20) no C23 . C24 . H241 . 122.2 no C25 . C24 . H241 . 117.5 no N21 . C25 . C24 . 119.5(16) no N21 . C25 . C26 . 118.6(17) no C24 . C25 . C26 . 121.9(18) no N22 . C26 . C25 . 111.4(17) no N22 . C26 . C27 . 122.2(16) no C25 . C26 . C27 . 126.4(18) no C26 . C27 . C28 . 121.0(19) no C26 . C27 . H271 . 119.5 no C28 . C27 . H271 . 119.5 no C27 . C28 . C29 . 118.5(20) no C27 . C28 . H281 . 121.8 no C29 . C28 . H281 . 119.7 no C28 . C29 . C30 . 121.0(19) no C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 118.9 no N22 . C30 . C29 . 118.4(20) no N22 . C30 . H301 . 117.1 no C29 . C30 . H301 . 124.3 no N9 . C31 . C32 . 118.7(16) no N9 . C31 . H311 . 123.5 no C32 . C31 . H311 . 117.1 no C31 . C32 . C33 . 118.9(18) no C31 . C32 . H321 . 121.8 no C33 . C32 . H321 . 119.3 no N10 . C33 . C32 . 120.3(18) no N10 . C33 . H331 . 122.4 no C32 . C33 . H331 . 117.3 no N9 . C34 . N10 . 126.0(15) no N9 . C34 . C34 2_755 115.0(18) no N10 . C34 . C34 2_755 118.7(18) no