# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_([Cu(tn)]2[Fe(CN)6]).KCl.5H2O_(1) _database_code_CSD 175834 _audit_creation_date 22-06-01 _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Smail Triki' ; UMR CNRS 6521, Chimie, Electrochimie Moleculaires, Chimie Analytique, Universite de Bretagne Occidentale, BP 809, 29285 Brest Cedex, France. ; 'Franck Thetiot' ; UMR CNRS 6521, Chimie, Electrochimie Moleculaires, Chimie Analytique, Universite de Bretagne Occidentale, BP 809, 29285 Brest Cedex, France. ; 'Pala, Jean-Sala' ; UMR CNRS 6521, Chimie, Electrochimie Moleculaires, Chimie Analytique, Universite de Bretagne Occidentale, BP 809, 29285 Brest Cedex, France. ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr S Triki ' _publ_contact_author_address ; 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 SMAIL.TRIKI@UNIV-BREST.FR _publ_requested_journal 'New Journal of Chemistry' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in 'New Journal of Chemistry'. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM # 3. TITLE AND AUTHOR LIST _publ_section_title ; {[CuII(pn)]2]Fell(CN)6]}. KCI.5H20 (pn = 1,3-diaminopropane): a two-dimensional bimetallic layered material with "Cu4Fe3" defective cubane units ; _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. ; # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12H30N10O5ClKFeCu2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12H30N10O5ClKFeCu2' _chemical_formula_weight 651.92 _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 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 K ? 0.179 0.250 International_Tables_Vol_IV_Table_2.3.1 Fe ? 0.301 0.845 International_Tables_Vol_IV_Table_2.3.1 Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1 # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 15.1478(3) _cell_length_b 14.6941(4) _cell_length_c 12.6533(4) _cell_angle_alpha 90 _cell_angle_beta 109.95(9) _cell_angle_gamma 90 _cell_volume 2647(1) _cell_formula_units_z 4 _cell_measurement_temperature 288 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description plate _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.437 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 288 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method \q/2\q _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 11239 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.333 _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 30.04 _reflns_number_total 6961 _reflns_number_gt 3177 _reflns_threshold_expression 3.0\s(I) _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _diffrn_measurement_method 'CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Direct_methods_(SIR,_Burla_et_al.,_1989)' _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP _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 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 3177 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.103 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_all 0.235 _refine_ls_wR_factor_ref 0.064 _refine_ls_goodness_of_fit_all 6.345 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_shift/su_max 0.034 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.015 _refine_diff_density_min -0.204 # 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 -0.00784(5) 0.13395(4) 0.74533(6) 0.0207(3) 1.000 Uij ? ? Fe N1 0.0833(3) 0.1083(3) 0.5652(4) 0.038(2) 1.000 Uij ? ? N N2 -0.1401(3) -0.0202(3) 0.6254(4) 0.031(2) 1.000 Uij ? ? N N3 -0.1403(3) 0.2822(3) 0.6105(4) 0.034(2) 1.000 Uij ? ? N N4 -0.1006(3) 0.1420(3) 0.9238(4) 0.044(2) 1.000 Uij ? ? N N5 0.1310(3) -0.0123(3) 0.8761(4) 0.035(2) 1.000 Uij ? ? N N6 0.1254(3) 0.2861(3) 0.8673(4) 0.031(2) 1.000 Uij ? ? N C1 0.0493(4) 0.1216(3) 0.6312(4) 0.025(2) 1.000 Uij ? ? C C2 -0.0935(3) 0.0387(3) 0.6721(4) 0.026(2) 1.000 Uij ? ? C C3 -0.0910(3) 0.2250(3) 0.6606(4) 0.024(2) 1.000 Uij ? ? C C4 -0.0653(3) 0.1401(3) 0.8568(4) 0.026(2) 1.000 Uij ? ? C C5 0.0800(4) 0.0433(3) 0.8306(4) 0.027(2) 1.000 Uij ? ? C C6 0.0786(3) 0.2279(3) 0.8211(4) 0.027(2) 1.000 Uij ? ? C CU1 -0.19317(4) 0.38491(4) 0.50367(5) 0.0257(3) 1.000 Uij ? ? Cu N7 -0.2466(3) 0.4792(3) 0.3839(4) 0.040(2) 1.000 Uij ? ? N N8 -0.3252(3) 0.3527(3) 0.4996(4) 0.045(3) 1.000 Uij ? ? N C7 -0.3219(5) 0.5373(4) 0.3921(6) 0.052(4) 1.000 Uij ? ? C C8 -0.4067(4) 0.4843(4) 0.3900(6) 0.052(4) 1.000 Uij ? ? C C9 -0.3925(4) 0.4273(5) 0.4907(6) 0.064(4) 1.000 Uij ? ? C CU2 -0.19234(4) -0.12155(4) 0.51579(5) 0.0247(3) 1.000 Uij ? ? Cu N9 -0.2557(3) -0.2254(3) 0.4150(4) 0.035(2) 1.000 Uij ? ? N N10 -0.2887(3) -0.0338(3) 0.4222(4) 0.041(3) 1.000 Uij ? ? N C10 -0.2912(5) -0.2114(4) 0.2920(5) 0.045(4) 1.000 Uij ? ? C C11 -0.3614(5) -0.1345(5) 0.2580(7) 0.056(4) 1.000 Uij ? ? C C12 -0.3195(5) -0.0430(4) 0.2977(6) 0.054(4) 1.000 Uij ? ? C K 0.9434(1) 0.10818(9) 0.3454(1) 0.0483(3) 1.000 Uiso ? ? K CL 0.3957(2) -0.2750(2) 0.2577(2) 0.105(2) 1.000 Uij ? ? Cl O1 0.1116(3) 0.1318(3) 0.1120(4) 0.057(1) 1.000 Uiso ? ? O O2 0.7917(3) 0.1495(3) 0.4010(4) 0.059(1) 1.000 Uiso ? ? O O3 0.5729(4) -0.2631(4) 0.4783(5) 0.099(2) 1.000 Uiso ? ? O O4 0.3096(6) -0.1259(5) 0.3564(7) 0.147(3) 1.000 Uiso ? ? O O5 0.504(1) 0.143(1) 0.397(1) 0.124(5) 0.500 Uiso ? ? O O6 0.568(1) 0.009(2) 0.534(2) 0.194(8) 0.500 Uiso ? ? O H1 -0.2701 0.4480 0.3140 0.0535 1.000 Uiso calc N7 H H2 -0.1964 0.5178 0.3838 0.0535 1.000 Uiso calc N7 H H3 -0.3393 0.5785 0.3305 0.0742 1.000 Uiso calc C7 H H4 -0.2994 0.5705 0.4605 0.0742 1.000 Uiso calc C7 H H5 -0.4242 0.4457 0.3259 0.0746 1.000 Uiso calc C8 H H6 -0.4561 0.5259 0.3839 0.0746 1.000 Uiso calc C8 H H7 -0.3693 0.4646 0.5557 0.0842 1.000 Uiso calc C9 H H8 -0.4511 0.4018 0.4869 0.0842 1.000 Uiso calc C9 H H9 -0.3189 0.3204 0.5668 0.0598 1.000 Uiso calc N8 H H10 -0.3520 0.3139 0.4367 0.0598 1.000 Uiso calc N8 H H11 -0.3079 -0.2431 0.4358 0.0498 1.000 Uiso calc N9 H H12 -0.2117 -0.2740 0.4299 0.0498 1.000 Uiso calc N9 H H13 -0.3206 -0.2658 0.2565 0.0656 1.000 Uiso calc C10 H H14 -0.2397 -0.1975 0.2680 0.0656 1.000 Uiso calc C10 H H15 -0.4095 -0.1458 0.2887 0.0840 1.000 Uiso calc C11 H H16 -0.3879 -0.1333 0.1783 0.0840 1.000 Uiso calc C11 H H17 -0.2667 -0.0344 0.2745 0.0803 1.000 Uiso calc C12 H H18 -0.3652 0.0025 0.2645 0.0803 1.000 Uiso calc C12 H H19 -0.2636 0.0257 0.4406 0.0595 1.000 Uiso calc N10 H H20 -0.3430 -0.0401 0.4431 0.0595 1.000 Uiso calc N10 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 0.0269(3) 0.0190(3) 0.0172(3) -0.0003(3) 0.0064(2) 0.0001(3) Fe N1 0.035(2) 0.048(2) 0.031(2) -0.002(2) 0.015(2) -0.006(2) N N2 0.041(2) 0.025(2) 0.028(2) -0.004(2) 0.009(2) -0.003(2) N N3 0.031(2) 0.033(2) 0.039(3) 0.004(2) 0.012(2) 0.003(2) N N4 0.044(2) 0.047(2) 0.040(3) -0.011(2) 0.024(2) -0.005(2) N N5 0.044(3) 0.031(2) 0.032(3) 0.010(2) 0.004(2) 0.004(2) N N6 0.035(2) 0.028(2) 0.030(2) -0.007(2) 0.006(2) -0.006(2) N C1 0.032(3) 0.024(2) 0.020(2) -0.000(2) 0.002(2) -0.000(2) C C2 0.031(2) 0.029(2) 0.020(2) 0.011(2) 0.009(2) 0.005(2) C C3 0.028(2) 0.026(2) 0.020(2) 0.002(2) 0.009(2) -0.001(2) C C4 0.031(2) 0.028(2) 0.021(2) -0.002(2) 0.010(2) -0.001(2) C C5 0.036(3) 0.022(2) 0.026(3) -0.007(2) 0.013(2) -0.008(2) C C6 0.032(2) 0.028(2) 0.022(2) 0.008(2) 0.012(2) 0.006(2) C CU1 0.0264(3) 0.0245(3) 0.0262(3) 0.0008(2) 0.0077(2) 0.0025(3) Cu N7 0.040(3) 0.034(2) 0.046(3) 0.004(2) 0.010(2) 0.014(2) N N8 0.034(2) 0.053(3) 0.051(3) -0.002(2) 0.014(2) 0.008(2) N C7 0.052(4) 0.039(3) 0.071(5) 0.013(3) 0.008(3) 0.017(3) C C8 0.035(3) 0.055(3) 0.073(5) 0.012(3) 0.007(3) 0.005(4) C C9 0.041(3) 0.083(5) 0.078(4) 0.018(3) 0.029(3) 0.009(4) C CU2 0.0273(3) 0.0225(3) 0.0247(3) 0.0004(2) 0.0043(2) 0.0004(2) Cu N9 0.039(3) 0.031(2) 0.036(3) -0.002(2) 0.000(2) -0.004(2) N N10 0.052(3) 0.032(2) 0.042(3) 0.007(2) 0.000(2) 0.000(2) N C10 0.058(4) 0.046(3) 0.033(4) -0.004(3) -0.002(3) -0.007(3) C C11 0.062(4) 0.058(4) 0.049(4) -0.004(4) -0.013(4) -0.009(4) C C12 0.068(4) 0.046(3) 0.049(4) 0.009(3) -0.008(4) 0.006(3) C CL 0.100(2) 0.129(2) 0.091(2) -0.037(1) -0.005(1) 0.008(2) Cl # 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 C1 1.929(6) . . ? FE C2 1.918(5) . . ? FE C3 1.899(4) . . ? FE C4 1.895(6) . . ? FE C5 1.931(4) . . ? FE C6 1.919(5) . . ? N1 C1 1.138(8) . . ? N1 CU2 2.230(5) . 3_556 ? N2 C2 1.145(6) . . ? N2 CU2 2.005(4) . . ? N3 C3 1.159(6) . . ? N3 CU1 2.002(4) . . ? N4 C4 1.147(8) . . ? N4 CU1 2.027(6) . 4_555 ? N5 C5 1.137(6) . . ? N5 CU1 2.122(4) . 2_546 ? N6 C6 1.138(6) . . ? N6 CU2 2.008(4) . 2_556 ? CU1 N7 2.009(4) . . ? CU1 N8 2.039(5) . . ? N7 C7 1.456(9) . . ? N8 C9 1.474(9) . . ? C7 C8 1.50(1) . . ? C8 C9 1.48(1) . . ? CU2 N9 2.011(4) . . ? CU2 N10 2.004(4) . . ? N9 C10 1.477(8) . . ? N10 C12 1.489(9) . . ? C10 C11 1.511(9) . . ? C11 C12 1.498(9) . . ? O6 O6 1.97(3) . 3_656 ? 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 C1 FE C2 88.4(2) . . . ? C1 FE C3 91.4(2) . . . ? C1 FE C4 177.3(2) . . . ? C1 FE C5 87.3(2) . . . ? C1 FE C6 92.1(2) . . . ? C2 FE C3 91.8(2) . . . ? C2 FE C4 89.3(2) . . . ? C2 FE C5 89.4(2) . . . ? C2 FE C6 178.9(2) . . . ? C3 FE C4 90.1(2) . . . ? C3 FE C5 178.2(2) . . . ? C3 FE C6 89.1(2) . . . ? C4 FE C5 91.2(2) . . . ? C4 FE C6 90.1(2) . . . ? C5 FE C6 89.7(2) . . . ? C1 N1 CU2 156.0(4) . . 3_556 ? C2 N2 CU2 161.2(5) . . . ? C3 N3 CU1 162.0(5) . . . ? C4 N4 CU1 160.1(4) . . 4_555 ? C5 N5 CU1 159.0(5) . . 2_546 ? C6 N6 CU2 163.0(5) . . 2_556 ? FE C1 N1 175.4(4) . . . ? FE C2 N2 175.3(5) . . . ? FE C3 N3 178.3(4) . . . ? FE C4 N4 178.5(4) . . . ? FE C5 N5 176.7(5) . . . ? FE C6 N6 175.8(5) . . . ? N3 CU1 N4 90.2(2) . . 4_554 ? N3 CU1 N5 94.3(2) . . 2_556 ? N3 CU1 N7 174.2(2) . . . ? N3 CU1 N8 90.3(2) . . . ? N4 CU1 N5 106.4(2) . 4_554 2_556 ? N4 CU1 N7 85.8(2) . 4_554 . ? N4 CU1 N8 141.4(2) . 4_554 . ? N5 CU1 N7 90.9(2) . 2_556 . ? N5 CU1 N8 112.0(2) . 2_556 . ? N7 CU1 N8 90.1(2) . . . ? CU1 N7 C7 118.3(4) . . . ? CU1 N8 C9 118.4(4) . . . ? N7 C7 C8 112.4(5) . . . ? C7 C8 C9 114.1(5) . . . ? N8 C9 C8 112.4(7) . . . ? N1 CU2 N2 94.2(2) . 3_556 . ? N1 CU2 N6 97.5(2) . 3_556 2_546 ? N1 CU2 N9 92.5(2) . 3_556 . ? N1 CU2 N10 100.2(2) . 3_556 . ? N2 CU2 N6 90.7(2) . . 2_546 ? N2 CU2 N9 173.3(2) . . . ? N2 CU2 N10 88.1(2) . . . ? N6 CU2 N9 88.1(2) . 2_546 . ? N6 CU2 N10 162.3(2) . 2_546 . ? N9 CU2 N10 91.1(2) . . . ? CU2 N9 C10 119.0(3) . . . ? CU2 N10 C12 117.9(4) . . . ? N9 C10 C11 111.9(6) . . . ? C10 C11 C12 113.5(6) . . . ? N10 C12 C11 112.3(6) . . . ? #===END