# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global #===================================================================== _audit_creation_date 6-11-00 _journal_coden_Cambridge 440 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr S Triki' _publ_contact_author_address ; Dr S Triki Chimie, Electrochimie Moleculaires, Chimie Analytique Universite de Bretagne Occidentale BP 809 Brest 29285 Cedex FRANCE ; _publ_contact_author_phone '(33) 2 98 01 61 46' _publ_contact_author_fax '(33) 2 98 01 70 01' _publ_contact_author_email 'triki@univ-brest.fr' _publ_requested_journal 'New Journal of Chemistry' _publ_requested_category FM # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; New Compounds with Bridging Dicyanamide and Bis-Chelating 2,2'-Bipyrimidine Ligands: Syntheses, Structural Characterization and Magnetic Properties of Two-Dimensional Materials [Fe2(dca)4(bpym)].H2O and [Fe2(dca)4(bpym)(H2O)2]. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Triki, Smail' ; UMR CNRS 6521, Chimie, Electrochi;ie Moleculaire et Chimie Analytique, Universite de Bretagne Occidentale, 29285 Brest Cedex, France. ; 'Thetiot, Franck' ; UMR CNRS 6521, Chimie, Electrochi;ie Moleculaire et Chimie Analytique, Universite de Bretagne Occidentale, 29285 Brest Cedex, France. ; 'Galan-Mascaros, Jose-Ramon' ; Department of Chemistry, Texas A&M University, College Station, TX, 77842-3012 USA. ; 'Sala Pala, Jean' ; UMR CNRS 6521, Chimie, Electrochi;ie Moleculaire et Chimie Analytique, Universite de Bretagne Occidentale, 29285 Brest Cedex, France. ; 'Dunbar, R. Kim' ; Department of Chemistry, Texas A&M University, College Station, TX, 77842-3012 USA. ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #===================================================================== data_[Fe2(dca)4(bpym)].H2O (Compound 1) _database_code_CSD 159694 #===================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16H8N16OFe2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16H8N16OFe2' _chemical_formula_weight 552.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Fe ? 0.301 0.845 International_Tables_Vol_IV_Table_2.3.1 # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,-y,1/2+z -x,1/2+y,-z 1/2+x,1/2-y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z +x,1/2-y,+z 1/2-x,1/2+y,1/2+z _cell_length_a 16.203(3) _cell_length_b 13.122(3) _cell_length_c 10.438(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2219(1) _cell_formula_units_z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description needle _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.352 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker CCD _diffrn_measurement_method CCD _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 0 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.250 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4897 _reflns_number_gt 1625 _reflns_threshold_expression >4.0\s(I) _computing_data_collection 'Bruker CCD' _computing_cell_refinement Bruker CCD _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment refxyz_U=1.3_x_bonding_atom _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1625 _refine_ls_number_parameters 172 _refine_ls_number_restraints 22 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.088 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_all 0.147 _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_all ***** _refine_ls_goodness_of_fit_ref 0.724 _refine_ls_shift/su_max 0.142 _refine_ls_shift/esd_mean 0.011 _refine_diff_density_max 1.399 _refine_diff_density_min -0.882 # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol FE 0.64646(4) 0.02521(5) 0.15889(6) 0.0205(3) 1.000 Uij ? ? Fe N1 0.5265(2) 0.0314(3) 0.2429(3) 0.027(2) 1.000 Uij ? ? N N2 0.7737(2) 0.0426(3) 0.1058(3) 0.023(2) 1.000 Uij ? ? N N3 0.4219(2) 0.0780(4) 0.4037(4) 0.039(3) 1.000 Uij ? ? N C1 0.4751(3) 0.0515(4) 0.3148(4) 0.031(3) 1.000 Uij ? ? C C2 0.8431(3) 0.0586(4) 0.1089(4) 0.025(3) 1.000 Uij ? ? C N4 0.6161(2) -0.0850(3) 0.0181(3) 0.023(2) 1.000 Uij ? ? N N5 0.5823(3) -0.2500 -0.0828(5) 0.030(3) 0.500 Uij ? ? N C3 0.6011(3) -0.1638(4) -0.0258(4) 0.023(3) 1.000 Uij ? ? C N6 0.6833(2) -0.0868(3) 0.2919(3) 0.031(2) 1.000 Uij ? ? N N7 0.7116(3) -0.2500 0.4009(5) 0.024(3) 0.500 Uij ? ? N C4 0.6959(3) -0.1649(3) 0.3376(4) 0.023(2) 1.000 Uij ? ? C N8 0.6173(2) 0.1589(3) 0.0381(3) 0.018(2) 1.000 Uij ? ? N N9 0.8292(2) -0.1589(3) -0.2161(3) 0.020(2) 1.000 Uij ? ? N C5 0.6304(3) 0.2500 0.0942(6) 0.015(4) 0.500 Uij ? ? C C6 0.6589(3) 0.2500 0.2281(6) 0.014(3) 0.500 Uij ? ? C C7 0.5891(3) 0.1616(4) -0.0826(4) 0.026(3) 1.000 Uij ? ? C C8 0.5739(4) 0.2500 -0.1486(6) 0.029(4) 0.500 Uij ? ? C C9 0.8046(3) -0.1594(3) -0.0945(4) 0.021(3) 1.000 Uij ? ? C C10 0.7925(4) -0.2500 -0.0291(6) 0.026(4) 0.500 Uij ? ? C O 0.5032(3) 0.2500 0.5597(5) 0.050(3) 0.500 Uij ? ? O H01 0.473(2) 0.197(3) 0.517(3) 0.0507 1.000 Uiso ? ? H H1 0.5790 0.0986 -0.1247 0.0339 1.000 Uiso calc C7 H H2 0.5543 0.2500 -0.2344 0.0374 0.500 Uiso calc C8 H H3 0.7048 0.0966 0.4482 0.0277 1.000 Uiso calc ? H H4 0.7237 0.2500 0.5584 0.0335 0.500 Uiso calc ? H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol FE 0.0197(3) 0.0180(3) 0.0244(3) 0.0003(4) 0.0000(4) 0.0010(4) Fe N1 0.019(2) 0.028(2) 0.038(2) -0.002(2) 0.009(2) -0.003(2) N N2 0.026(2) 0.021(2) 0.024(2) -0.002(2) -0.002(2) -0.003(2) N N3 0.017(2) 0.090(4) 0.039(2) -0.012(2) 0.004(2) -0.024(3) N C1 0.026(3) 0.029(3) 0.039(3) -0.006(2) -0.006(2) -0.005(2) C C2 0.032(3) 0.035(3) 0.014(2) -0.006(2) -0.006(2) -0.001(2) C N4 0.031(2) 0.017(2) 0.025(2) 0.003(2) 0.001(2) -0.000(2) N N5 0.035(4) 0.029(3) 0.026(3) 0.0000 -0.001(3) 0.0000 N C3 0.015(3) 0.028(3) 0.027(3) 0.004(2) 0.003(2) 0.006(3) C N6 0.043(3) 0.025(2) 0.028(2) -0.006(2) -0.002(2) 0.001(2) N N7 0.045(4) 0.012(3) 0.025(3) 0.0000 -0.014(3) 0.0000 N C4 0.025(2) 0.027(2) 0.017(2) -0.005(2) 0.001(2) -0.006(3) C N8 0.018(2) 0.018(2) 0.017(2) -0.001(2) -0.000(2) -0.004(2) N N9 0.024(2) 0.016(2) 0.021(2) -0.003(2) 0.002(2) 0.003(2) N C5 0.009(4) 0.017(3) 0.025(4) 0.0000 0.001(3) 0.0000 C C6 0.011(4) 0.010(3) 0.026(4) 0.0000 0.002(3) 0.0000 C C7 0.023(3) 0.032(3) 0.023(3) -0.012(2) 0.001(2) -0.010(3) C C8 0.032(4) 0.024(4) 0.030(4) 0.0000 -0.000(4) 0.0000 C C9 0.023(3) 0.024(3) 0.017(3) -0.008(2) 0.002(2) -0.006(2) C C10 0.028(4) 0.028(4) 0.022(4) 0.0000 0.007(3) 0.0000 C O 0.050(3) 0.049(3) 0.050(3) 0.0000 -0.023(3) 0.0000 O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag FE N1 2.134(3) . . ? FE N2 2.147(3) . . ? FE N4 2.120(4) . . ? FE N6 2.108(4) . . ? FE N8 2.211(3) . . ? N1 C1 1.152(6) . . ? N2 C2 1.144(6) . . ? N3 C1 1.314(6) . . ? N3 H01 2.13(4) . . ? N4 C3 1.156(6) . . ? N5 C3 1.314(5) . . ? N6 C4 1.149(6) . . ? N7 C4 1.322(5) . . ? N8 C5 1.348(4) . . ? N8 C7 1.341(6) . . ? N8 C8 2.392(7) . . ? N9 C9 1.330(5) . . ? N9 C10 2.365(6) . . ? C5 C6 1.471(8) . . ? C5 C7 2.281(7) . . ? C7 C8 1.372(6) . . ? C9 C10 1.385(5) . . ? O H01 0.96(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 FE N2 167.6(1) . . . ? N1 FE N4 95.7(1) . . . ? N1 FE N6 90.8(1) . . . ? N1 FE N8 90.6(1) . . . ? N2 FE N4 96.7(1) . . . ? N2 FE N6 88.4(1) . . . ? N2 FE N8 88.5(1) . . . ? N4 FE N6 92.7(1) . . . ? N4 FE N8 95.6(1) . . . ? N6 FE N8 171.5(1) . . . ? FE N1 N1 . . . ? FE N1 C1 159.3(4) . . . ? N1 N1 C1 . . . ? FE N2 C2 163.0(3) . . . ? C1 N3 H01 109(1) . . . ? N1 C1 N3 174.6(5) . . . ? N1 C1 C1 . . . ? N3 C1 C1 . . . ? FE N4 C3 159.0(3) . . . ? N4 C3 N5 176.1(5) . . . ? N4 C3 C3 . . . ? N5 C3 C3 . . . ? FE N6 C4 161.0(4) . . . ? N6 C4 N7 174.4(5) . . . ? N6 C4 C4 . . . ? N7 C4 C4 . . . ? FE N8 C5 115.0(3) . . . ? FE N8 C7 129.0(3) . . . ? FE N8 C8 157.5(2) . . . ? C5 N8 C7 116.0(4) . . . ? C5 N8 C8 87.5(3) . . . ? C7 N8 C8 28.5(2) . . . ? C9 N9 C10 30.1(2) . . . ? N8 C5 C6 117.5(3) . . . ? N8 C5 C7 31.9(2) . . . ? C6 C5 C7 149.4(1) . . . ? C5 C6 C6 . . . ? N8 C7 C5 32.1(2) . . . ? N8 C7 C8 123.8(5) . . . ? C5 C7 C8 91.7(3) . . . ? N8 C8 C7 27.8(3) . . . ? N8 C8 C8 . . . ? C7 C8 C8 . . . ? N9 C9 C10 121.1(4) . . . ? N9 C10 C9 28.8(2) . . . ? N9 C10 C10 . . . ? C9 C10 C10 . . . ? N3 H01 O 171(3) . . . ? N3 H01 H01 . . . ? O H01 H01 . . . ? #===END #===================================================================== data_[Fe2(dca)4(bpym)(H2O)2](compound 2) _database_code_CSD 159695 #===================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16H10N16O2Fe2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16H10N16O2Fe2' _chemical_formula_weight 570.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Fe ? 0.301 0.845 International_Tables_Vol_IV_Table_2.3.1 # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.384(2) _cell_length_b 9.223(2) _cell_length_c 13.983(3) _cell_angle_alpha 90 _cell_angle_beta 90.95(3) _cell_angle_gamma 90 _cell_volume 1081.1(7) _cell_formula_units_z 2 _cell_measurement_temperature 110 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.75 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker CCD _diffrn_measurement_method CCD _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 0 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.250 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3128 _reflns_number_gt 1711 _reflns_threshold_expression >4.0\s(I) _computing_data_collection 'Bruker CCD' _computing_cell_refinement Bruker CCD _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1711 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.025 _refine_ls_wR_factor_all 0.076 _refine_ls_wR_factor_ref 0.031 _refine_ls_goodness_of_fit_all 1.973 _refine_ls_goodness_of_fit_ref 0.661 _refine_ls_shift/su_max 0.037 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.488 _refine_diff_density_min -0.453 # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol FE 0.61998(4) 0.26593(4) 0.87308(3) 0.0151(2) Uij ? ? Fe N1 0.5209(2) 0.3670(2) 0.7499(2) 0.019(1) Uij ? ? N N2 0.2142(3) 0.3564(2) 0.4889(2) 0.019(1) Uij ? ? N N3 0.4013(2) 0.4706(2) 0.6033(1) 0.020(1) Uij ? ? N C1 0.4614(3) 0.4084(3) 0.6806(2) 0.016(1) Uij ? ? C C2 0.3034(3) 0.4032(3) 0.5450(2) 0.015(1) Uij ? ? C N4 0.8395(3) 0.2524(2) 0.8048(2) 0.024(1) Uij ? ? N N5 1.2857(3) 0.0951(2) 0.6725(2) 0.024(1) Uij ? ? N N6 1.0439(3) 0.2479(2) 0.6813(2) 0.025(1) Uij ? ? N C3 0.9400(3) 0.2422(2) 0.7494(2) 0.018(1) Uij ? ? C C4 1.1714(3) 0.1626(3) 0.6809(2) 0.018(1) Uij ? ? C N7 0.6862(2) 0.4773(2) 0.9396(1) 0.014(1) Uij ? ? N N8 0.5928(2) 0.6612(2) 1.0455(1) 0.015(1) Uij ? ? N C5 0.5771(3) 0.5385(3) 0.9959(2) 0.013(1) Uij ? ? C C6 0.7353(3) 0.7264(3) 1.0404(2) 0.019(1) Uij ? ? C C7 0.8548(3) 0.6725(3) 0.9847(2) 0.022(1) Uij ? ? C C8 0.8256(3) 0.5483(3) 0.9337(2) 0.020(1) Uij ? ? C H01 0.752(2) 0.806(2) 1.074(1) 0.002(5) Uiso ? ? H H02 0.955(3) 0.718(2) 0.982(2) 0.022(7) Uiso ? ? H H03 0.901(3) 0.505(3) 0.890(2) 0.033(8) Uiso ? ? H O 0.4953(2) 0.0779(2) 0.8290(1) 0.024(1) Uij ? ? O H04 0.499(3) -0.003(3) 0.853(2) 0.049(9) Uiso ? ? H H05 0.432(3) 0.083(3) 0.778(2) 0.07(1) Uiso ? ? H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol FE 0.0170(2) 0.0156(2) 0.0128(1) 0.0017(2) -0.0019(1) -0.0009(2) Fe N1 0.025(1) 0.018(1) 0.016(1) 0.003(1) -0.006(1) -0.002(1) N N2 0.023(1) 0.019(1) 0.015(1) -0.002(1) -0.001(1) 0.0020(9) N N3 0.027(1) 0.014(1) 0.021(1) -0.002(1) -0.011(1) 0.0006(9) N C1 0.018(1) 0.012(1) 0.019(1) -0.002(1) 0.002(1) -0.006(1) C C2 0.020(1) 0.012(1) 0.015(1) 0.006(1) 0.006(1) 0.005(1) C N4 0.028(1) 0.025(1) 0.021(1) 0.009(1) 0.003(1) 0.003(1) N N5 0.020(1) 0.028(1) 0.025(1) -0.005(1) 0.001(1) -0.002(1) N N6 0.028(1) 0.026(1) 0.022(1) 0.005(1) 0.010(1) 0.007(1) N C3 0.023(1) 0.013(1) 0.020(1) -0.000(1) -0.004(1) 0.002(1) C C4 0.026(1) 0.022(1) 0.010(1) -0.012(1) -0.000(1) -0.003(1) C N7 0.012(1) 0.018(1) 0.013(1) -0.0005(9) -0.0010(9) 0.0028(9) N N8 0.018(1) 0.014(1) 0.014(1) -0.0010(9) -0.003(1) 0.0018(9) N C5 0.013(1) 0.014(1) 0.013(1) 0.001(1) -0.002(1) 0.003(1) C C6 0.023(1) 0.013(1) 0.022(1) -0.003(1) -0.004(1) 0.000(1) C C7 0.017(1) 0.022(1) 0.030(2) -0.006(1) -0.001(1) 0.005(1) C C8 0.019(1) 0.021(1) 0.019(1) 0.001(1) 0.003(1) 0.005(1) C O 0.033(1) 0.0177(9) 0.024(1) -0.0001(9) -0.0115(9) -0.0009(8) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag FE N1 2.116(2) . . ? FE N4 2.092(2) . . ? FE N7 2.226(2) . . ? FE O 2.112(2) . . ? N1 C1 1.148(3) . . ? N2 C2 1.158(3) . . ? N3 C1 1.316(3) . . ? N3 C2 1.305(3) . . ? C1 C2 2.295(3) . . ? N4 C3 1.158(3) . . ? N5 C4 1.151(3) . . ? N6 C3 1.302(3) . . ? N6 C4 1.327(3) . . ? C3 C4 2.298(4) . . ? N7 N8 2.392(3) . . ? N7 C5 1.341(3) . . ? N7 C7 2.368(3) . . ? N7 C8 1.344(3) . . ? N7 H03 1.96(2) . . ? N8 C5 1.332(3) . . ? N8 C6 1.341(3) . . ? N8 C7 2.370(3) . . ? N8 H01 1.92(2) . . ? C5 C6 2.264(3) . . ? C5 C8 2.273(3) . . ? C6 C7 1.372(4) . . ? C6 C8 2.354(4) . . ? C6 H01 0.88(2) . . ? C6 H02 2.03(2) . . ? C7 C8 1.370(4) . . ? C7 H01 1.96(2) . . ? C7 H02 0.94(2) . . ? C7 H03 2.07(2) . . ? C8 H02 2.02(2) . . ? C8 H03 0.97(2) . . ? H01 H02 2.30(3) . . ? H02 H03 2.39(3) . . ? O H04 0.82(3) . . ? O H05 0.89(3) . . ? H04 H05 1.43(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 FE N4 89.51(8) . . . ? N1 FE N7 92.64(8) . . . ? N1 FE O 86.45(7) . . . ? N4 FE N7 91.60(8) . . . ? N4 FE O 104.64(8) . . . ? N7 FE O 163.72(7) . . . ? FE N1 N1 . . . ? FE N1 C1 173.2(2) . . . ? N1 N1 C1 . . . ? C1 N3 C2 122.3(2) . . . ? N1 C1 N3 173.3(3) . . . ? N1 C1 C1 . . . ? N1 C1 C2 158.0(2) . . . ? N3 C1 C1 . . . ? N3 C1 C2 28.7(1) . . . ? C1 C1 C2 . . . ? N2 C2 N3 173.2(3) . . . ? N2 C2 C1 157.6(2) . . . ? N2 C2 C2 . . . ? N3 C2 C1 29.0(1) . . . ? N3 C2 C2 . . . ? C1 C2 C2 . . . ? FE N4 C3 165.0(2) . . . ? C3 N6 C4 121.9(2) . . . ? N4 C3 N6 171.5(3) . . . ? N4 C3 C3 . . . ? N4 C3 C4 159.0(2) . . . ? N6 C3 C3 . . . ? N6 C3 C4 29.4(1) . . . ? C3 C3 C4 . . . ? N5 C4 N6 173.5(3) . . . ? N5 C4 C3 157.8(2) . . . ? N5 C4 C4 . . . ? N6 C4 C3 28.7(1) . . . ? N6 C4 C4 . . . ? C3 C4 C4 . . . ? FE N7 N8 142.9(1) . . . ? FE N7 C5 116.5(1) . . . ? FE N7 C7 157.0(1) . . . ? FE N7 C8 127.7(2) . . . ? FE N7 H03 101.0(7) . . . ? N8 N7 C5 26.5(1) . . . ? N8 N7 C7 59.74(9) . . . ? N8 N7 C8 89.3(2) . . . ? N8 N7 H03 116.1(7) . . . ? C5 N7 C7 86.2(1) . . . ? C5 N7 C8 115.7(2) . . . ? C5 N7 H03 142.5(7) . . . ? C7 N7 C8 29.5(1) . . . ? C7 N7 H03 56.4(7) . . . ? C8 N7 H03 26.8(7) . . . ? N7 N8 N8 . . . ? N7 N8 C5 26.6(1) . . . ? N7 N8 C6 89.1(2) . . . ? N7 N8 C7 59.64(9) . . . ? N7 N8 H01 112.8(6) . . . ? N8 N8 C5 . . . ? N8 N8 C6 . . . ? N8 N8 C7 . . . ? N8 N8 H01 . . . ? C5 N8 C6 115.7(2) . . . ? C5 N8 C7 86.3(2) . . . ? C5 N8 H01 139.4(6) . . . ? C6 N8 C7 29.5(1) . . . ? C6 N8 H01 23.7(6) . . . ? C7 N8 H01 53.2(6) . . . ? N7 C5 N8 126.9(2) . . . ? N7 C5 C5 . . . ? N7 C5 C6 94.7(2) . . . ? N7 C5 C8 32.2(1) . . . ? N8 C5 C5 . . . ? N8 C5 C6 32.3(1) . . . ? N8 C5 C8 94.7(2) . . . ? C5 C5 C6 . . . ? C5 C5 C8 . . . ? C6 C5 C8 62.5(1) . . . ? N8 C6 C5 32.0(1) . . . ? N8 C6 C6 . . . ? N8 C6 C7 121.8(2) . . . ? N8 C6 C8 90.9(2) . . . ? N8 C6 H01 118(1) . . . ? N8 C6 H02 145.1(6) . . . ? C5 C6 C6 . . . ? C5 C6 C7 89.8(2) . . . ? C5 C6 C8 58.9(1) . . . ? C5 C6 H01 150(1) . . . ? C5 C6 H02 113.1(6) . . . ? C6 C6 C7 . . . ? C6 C6 C8 . . . ? C6 C6 H01 . . . ? C6 C6 H02 . . . ? C7 C6 C8 30.8(1) . . . ? C7 C6 H01 119(1) . . . ? C7 C6 H02 23.3(6) . . . ? C8 C6 H01 150(1) . . . ? C8 C6 H02 54.2(6) . . . ? H01 C6 H02 96(1) . . . ? N7 C7 N8 60.62(9) . . . ? N7 C7 C6 89.4(2) . . . ? N7 C7 C7 . . . ? N7 C7 C8 28.9(1) . . . ? N7 C7 H01 112.3(6) . . . ? N7 C7 H02 149(1) . . . ? N7 C7 H03 51.7(7) . . . ? N8 C7 C6 28.7(1) . . . ? N8 C7 C7 . . . ? N8 C7 C8 89.5(2) . . . ? N8 C7 H01 51.7(6) . . . ? N8 C7 H02 150(1) . . . ? N8 C7 H03 112.3(7) . . . ? C6 C7 C7 . . . ? C6 C7 C8 118.3(2) . . . ? C6 C7 H01 22.9(6) . . . ? C6 C7 H02 121(1) . . . ? C6 C7 H03 141.0(7) . . . ? C7 C7 C8 . . . ? C7 C7 H01 . . . ? C7 C7 H02 . . . ? C7 C7 H03 . . . ? C8 C7 H01 141.2(6) . . . ? C8 C7 H02 120(1) . . . ? C8 C7 H03 22.8(7) . . . ? H01 C7 H02 98(1) . . . ? H01 C7 H03 163.9(9) . . . ? H02 C7 H03 97(1) . . . ? N7 C8 C5 32.1(1) . . . ? N7 C8 C6 90.7(2) . . . ? N7 C8 C7 121.5(2) . . . ? N7 C8 C8 . . . ? N7 C8 H02 145.2(7) . . . ? N7 C8 H03 114(1) . . . ? C5 C8 C6 58.6(1) . . . ? C5 C8 C7 89.4(2) . . . ? C5 C8 C8 . . . ? C5 C8 H02 113.2(6) . . . ? C5 C8 H03 146(1) . . . ? C6 C8 C7 30.9(1) . . . ? C6 C8 C8 . . . ? C6 C8 H02 54.6(6) . . . ? C6 C8 H03 154(1) . . . ? C7 C8 C8 . . . ? C7 C8 H02 23.7(6) . . . ? C7 C8 H03 124(1) . . . ? C8 C8 H02 . . . ? C8 C8 H03 . . . ? H02 C8 H03 100(1) . . . ? N8 H01 C6 37.8(9) . . . ? N8 H01 C7 75.1(7) . . . ? N8 H01 H02 98(1) . . . ? C6 H01 C7 37.4(9) . . . ? C6 H01 H02 61(1) . . . ? C7 H01 H02 23.9(6) . . . ? C6 H02 C7 35.3(9) . . . ? C6 H02 C8 71.2(7) . . . ? C6 H02 H01 22.4(5) . . . ? C6 H02 H02 . . . ? C6 H02 H03 94(1) . . . ? C7 H02 C8 35.9(9) . . . ? C7 H02 H01 57(1) . . . ? C7 H02 H02 . . . ? C7 H02 H03 59(1) . . . ? C8 H02 H01 93(1) . . . ? C8 H02 H02 . . . ? C8 H02 H03 23.5(6) . . . ? H01 H02 H02 . . . ? H01 H02 H03 117(1) . . . ? H02 H02 H03 . . . ? N7 H03 C7 71.9(8) . . . ? N7 H03 C8 38(1) . . . ? N7 H03 H02 94(1) . . . ? N7 H03 H03 . . . ? C7 H03 C8 33(1) . . . ? C7 H03 H02 23.0(6) . . . ? C7 H03 H03 . . . ? C8 H03 H02 56(1) . . . ? C8 H03 H03 . . . ? H02 H03 H03 . . . ? FE O H04 127(1) . . . ? FE O H05 118(1) . . . ? H04 O H05 113(2) . . . ? O H04 H04 . . . ? O H04 H05 34(1) . . . ? H04 H04 H05 . . . ? O H05 H04 31(1) . . . ? O H05 H05 . . . ? H04 H05 H05 . . . ? #===END