Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_[Cu(tn)]3[Cr(CN)6]2.2H2O _database_code_CSD 175842 _audit_creation_date 2-08-01 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Franck Thetiot ' ; UMR CNRS 6521, Universite. de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France). ; 'Smail Triki ' ; UMR CNRS 6521, Universite. de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France). ; 'Pala, Jean-Sala' ; UMR CNRS 6521, Universite. de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France). ; 'Carlos J. Gomez-Garcia' ; Instituto de Ciencia Molecular, Universidad de Valencia, Dr. Moliner 50, 46100 Burjasot (Spain) ; 'Stephane Golhen' ; UMR CNRS 6511, Universite. de Rennes 1, 35042 Rennes Cedex (France). ; _publ_contact_author_name 'Dr Smail Triki' _publ_contact_author_address ; UMR CNRS 6521 Universite de Bretagne Occidentale BP 809 Brest Cedex FRANCE ; _publ_contact_author_phone '33298016146' _publ_contact_author_fax '33298017001' _publ_contact_author_email triki@univ-brest.fr _publ_requested_journal 'ChemComm' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in ChemComm. 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 _publ_section_title ; [Cu(tn)]3]Cr(CN)6]2.2H2O: a unique two-dimensional Cu-Cr cyano-bridged ferromagnet (tn = 1,3-diaminopropane) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. _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. Enraf-Nonius, Cad4-Express Operations Manual, Delft, 1994. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H36 Cr2 Cu3 N18 O3' _chemical_formula_weight 883.30 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.1148(4) _cell_length_b 11.1692(6) _cell_length_c 14.6500(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3782.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 288 _cell_measurement_reflns_used 75495 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description plate _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 2.265 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 288 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19231 _diffrn_reflns_av_R_equivalents 0.1299 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.35 _reflns_number_total 3806 _reflns_number_gt 2337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0911P)^2^+3.7418P] 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 3806 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _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 Cr Cr 0.59295(4) 0.25179(8) 0.06848(7) 0.0392(3) Uani 1 1 d . . . N1 N 0.4601(3) 0.1821(5) 0.0658(4) 0.0607(16) Uani 1 1 d . . . N2 N 0.6134(3) 0.1267(5) 0.2632(4) 0.0617(16) Uani 1 1 d . . . N3 N 0.6221(3) 0.0080(5) -0.0345(4) 0.0620(16) Uani 1 1 d . . . N4 N 0.5434(3) 0.4748(5) 0.1813(4) 0.0628(16) Uani 1 1 d . . . N5 N 0.5763(4) 0.3846(6) -0.1230(5) 0.082(2) Uani 1 1 d . . . N6 N 0.7245(4) 0.3342(11) 0.0850(6) 0.135(4) Uani 1 1 d . . . C1 C 0.5079(3) 0.2012(5) 0.0635(4) 0.0435(14) Uani 1 1 d . . . C2 C 0.6049(3) 0.1660(5) 0.1924(5) 0.0466(15) Uani 1 1 d . . . C3 C 0.6150(3) 0.0973(5) 0.0015(4) 0.0395(13) Uani 1 1 d . . . C4 C 0.5645(3) 0.3980(6) 0.1391(5) 0.0499(16) Uani 1 1 d . . . C5 C 0.5834(3) 0.3393(6) -0.0543(5) 0.0540(17) Uani 1 1 d . . . C6 C 0.6782(4) 0.3076(8) 0.0766(5) 0.069(2) Uani 1 1 d . . . Cu1 Cu 0.37509(3) 0.15822(6) 0.09000(6) 0.0444(3) Uani 1 1 d . . . N7 N 0.3675(3) 0.3409(5) 0.0974(5) 0.0632(17) Uani 1 1 d . . . H7A H 0.4020 0.3704 0.1149 0.076 Uiso 1 1 calc R . . H7B H 0.3607 0.3682 0.0406 0.076 Uiso 1 1 calc R . . N8 N 0.2885(2) 0.1401(5) 0.0966(5) 0.0607(16) Uani 1 1 d . . . H8A H 0.2748 0.1507 0.0397 0.073 Uiso 1 1 calc R . . H8B H 0.2812 0.0636 0.1119 0.073 Uiso 1 1 calc R . . C7 C 0.3226(4) 0.3929(6) 0.1587(7) 0.073(2) Uani 1 1 d . . . H7A' H 0.3233 0.4795 0.1530 0.088 Uiso 1 1 calc R . . H7B' H 0.3320 0.3731 0.2214 0.088 Uiso 1 1 calc R . . C8 C 0.2628(4) 0.3491(7) 0.1380(7) 0.080(3) Uani 1 1 d . . . H8A' H 0.2547 0.3636 0.0740 0.096 Uiso 1 1 calc R . . H8B' H 0.2354 0.3953 0.1736 0.096 Uiso 1 1 calc R . . C9 C 0.2536(4) 0.2166(7) 0.1580(7) 0.079(3) Uani 1 1 d . . . H9A H 0.2641 0.2001 0.2208 0.094 Uiso 1 1 calc R . . H9B H 0.2130 0.1972 0.1505 0.094 Uiso 1 1 calc R . . Cu2 Cu 0.5000 0.60139(9) 0.2500 0.0618(4) Uani 1 2 d S . . N9 N 0.5459(3) 0.7246(5) 0.1820(5) 0.0722(19) Uani 1 1 d . . . H9C H 0.5833 0.7096 0.1948 0.087 Uiso 1 1 calc R A 1 H9D H 0.5412 0.7080 0.1224 0.087 Uiso 1 1 calc R A 1 C10 C 0.5388(7) 0.8511(8) 0.1906(8) 0.143(6) Uani 1 1 d . B 1 H10A H 0.5765 0.8835 0.2059 0.171 Uiso 1 1 calc R B 1 H10B H 0.5293 0.8810 0.1303 0.171 Uiso 1 1 calc R B 1 C11 C 0.5000 0.9019(9) 0.2500 0.104(6) Uani 1 2 d S . 1 H11 H 0.5233 0.9544 0.2879 0.125 Uiso 1 1 calc PR . 1 O1 O 0.3293(5) 0.3470(10) -0.1062(6) 0.161(4) Uani 1 1 d . . . O2 O 0.2774(16) 0.003(3) 0.321(2) 0.33(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0476(6) 0.0297(5) 0.0403(5) -0.0055(4) 0.0034(4) -0.0037(4) N1 0.070(4) 0.042(3) 0.070(4) -0.011(3) 0.012(4) 0.002(3) N2 0.080(4) 0.050(3) 0.055(4) 0.008(3) -0.011(3) -0.012(3) N3 0.067(4) 0.054(4) 0.066(4) -0.007(3) 0.007(3) 0.001(3) N4 0.084(4) 0.043(3) 0.061(4) -0.006(3) 0.014(4) -0.008(3) N5 0.118(6) 0.063(4) 0.065(4) 0.013(4) -0.001(4) -0.010(4) N6 0.088(6) 0.230(13) 0.088(6) -0.026(7) 0.011(5) -0.072(7) C1 0.048(4) 0.035(3) 0.047(4) -0.001(3) 0.007(3) -0.003(3) C2 0.053(4) 0.036(3) 0.050(4) -0.006(3) 0.000(3) -0.008(3) C3 0.048(3) 0.034(3) 0.037(3) -0.007(3) 0.006(3) 0.004(2) C4 0.063(4) 0.038(3) 0.049(4) -0.005(3) 0.004(3) -0.005(3) C5 0.074(5) 0.034(3) 0.054(4) -0.002(3) 0.003(4) -0.008(3) C6 0.058(5) 0.091(6) 0.058(5) -0.017(4) 0.005(4) -0.023(4) Cu1 0.0473(5) 0.0340(4) 0.0521(5) -0.0071(3) -0.0004(4) -0.0008(3) N7 0.058(4) 0.038(3) 0.093(5) -0.001(3) 0.003(3) -0.003(3) N8 0.043(3) 0.046(3) 0.093(5) -0.010(3) -0.004(3) 0.001(2) C7 0.076(5) 0.038(4) 0.105(7) -0.011(4) 0.014(5) 0.008(4) C8 0.072(5) 0.050(4) 0.118(8) -0.001(5) 0.002(5) 0.013(4) C9 0.062(5) 0.066(5) 0.107(7) -0.003(5) 0.019(5) 0.004(4) Cu2 0.1043(11) 0.0260(5) 0.0552(7) 0.000 0.0294(7) 0.000 N9 0.085(5) 0.039(3) 0.093(5) 0.007(3) 0.012(4) -0.010(3) C10 0.276(18) 0.039(5) 0.112(9) -0.008(5) 0.091(11) -0.036(7) C11 0.106(10) 0.024(5) 0.184(17) 0.000 0.013(11) 0.000 O1 0.143(8) 0.225(11) 0.114(7) 0.036(7) 0.004(6) -0.010(7) O2 0.38(4) 0.41(4) 0.22(3) 0.13(3) -0.12(3) -0.33(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 Cr C4 2.042(7) . ? Cr C1 2.047(7) . ? Cr C3 2.049(6) . ? Cr C5 2.059(8) . ? Cr C6 2.070(8) . ? Cr C2 2.071(7) . ? N1 C1 1.126(9) . ? N1 Cu1 2.014(7) . ? N2 C2 1.144(9) . ? N2 Cu1 2.195(7) 3_655 ? N3 C3 1.141(8) . ? N3 Cu1 2.028(6) 5_655 ? N4 C4 1.164(8) . ? N4 Cu2 2.005(6) . ? N5 C5 1.138(10) . ? N6 C6 1.117(11) . ? Cu1 N8 2.013(5) . ? Cu1 N3 2.028(6) 5_655 ? Cu1 N7 2.051(5) . ? Cu1 N2 2.195(7) 3_655 ? N7 C7 1.490(10) . ? N8 C9 1.480(10) . ? C7 C8 1.496(11) . ? C8 C9 1.524(11) . ? Cu2 N9 2.003(6) 3_655 ? Cu2 N9 2.003(6) . ? Cu2 N4 2.005(6) 3_655 ? N9 C10 1.427(10) . ? C10 C11 1.373(12) . ? C11 C10 1.373(12) 3_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 C4 Cr C1 86.0(3) . . ? C4 Cr C3 174.9(3) . . ? C1 Cr C3 89.4(2) . . ? C4 Cr C5 91.6(3) . . ? C1 Cr C5 89.9(3) . . ? C3 Cr C5 90.5(2) . . ? C4 Cr C6 92.1(3) . . ? C1 Cr C6 178.0(3) . . ? C3 Cr C6 92.5(3) . . ? C5 Cr C6 90.5(3) . . ? C4 Cr C2 88.2(3) . . ? C1 Cr C2 91.8(3) . . ? C3 Cr C2 89.8(2) . . ? C5 Cr C2 178.3(3) . . ? C6 Cr C2 87.8(3) . . ? C1 N1 Cu1 171.0(6) . . ? C2 N2 Cu1 147.9(5) . 3_655 ? C3 N3 Cu1 172.2(6) . 5_655 ? C4 N4 Cu2 174.7(6) . . ? N1 C1 Cr 173.6(6) . . ? N2 C2 Cr 174.7(6) . . ? N3 C3 Cr 173.7(6) . . ? N4 C4 Cr 173.3(6) . . ? N5 C5 Cr 177.2(7) . . ? N6 C6 Cr 176.3(10) . . ? N8 Cu1 N1 172.4(3) . . ? N8 Cu1 N3 87.6(2) . 5_655 ? N1 Cu1 N3 91.1(2) . 5_655 ? N8 Cu1 N7 90.7(2) . . ? N1 Cu1 N7 87.7(2) . . ? N3 Cu1 N7 159.2(3) 5_655 . ? N8 Cu1 N2 93.3(3) . 3_655 ? N1 Cu1 N2 94.3(3) . 3_655 ? N3 Cu1 N2 104.0(2) 5_655 3_655 ? N7 Cu1 N2 96.8(3) . 3_655 ? C7 N7 Cu1 118.7(5) . . ? C9 N8 Cu1 120.9(5) . . ? N7 C7 C8 113.2(7) . . ? C7 C8 C9 114.1(7) . . ? N8 C9 C8 111.5(7) . . ? N9 Cu2 N9 93.2(4) 3_655 . ? N9 Cu2 N4 88.3(3) 3_655 3_655 ? N9 Cu2 N4 178.0(3) . 3_655 ? N9 Cu2 N4 178.0(3) 3_655 . ? N9 Cu2 N4 88.3(3) . . ? N4 Cu2 N4 90.3(3) 3_655 . ? C10 N9 Cu2 125.1(6) . . ? C11 C10 N9 122.7(9) . . ? C10 C11 C10 131.2(11) 3_655 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.699 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.125