Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;A Rational Design by Hydrothermal methods of a Tetrazolate-Bridged Bimetallic Spin-Canted Antiferromagnet. Synthesis, X-ray Structure and Magnetic Properties of [CoNi(pmtz)4] (Hpmtz-=5-(pyrimidyl)tetrazole) ; loop_ _publ_author_name E.Colacio M.A.Palacios A.Rodrguez-Dieguez A.Sironi _publ_contact_author_name 'Prof. E.Colacio' _publ_contact_author_email ECOLACIO@UGR.ES # Attachment 'nico.cif' data_nico _database_code_depnum_ccdc_archive 'CCDC 675631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 Co0.50 N12 Ni0.50' _chemical_formula_weight 353.09 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.2427(16) _cell_length_b 9.2387(18) _cell_length_c 17.919(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1364.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3607 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.09 _exptl_crystal_description prismatic _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Empirical _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 12786 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.16 _reflns_number_total 1364 _reflns_number_gt 1098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0381P)^2^+3.9945P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1364 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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 Ni Ni 1.0000 0.5000 0.0000 0.0168(2) Uani 0.50 2 d SP . . Co Co 1.0000 0.5000 0.0000 0.0168(2) Uani 0.50 2 d SP . . N1 N 0.8517(3) 0.6779(3) 0.01772(16) 0.0197(6) Uani 1 1 d . . . N2 N 0.7426(4) 0.7574(3) -0.01846(16) 0.0229(7) Uani 1 1 d . . . N3 N 0.8096(4) 0.3570(3) 0.02848(17) 0.0212(6) Uani 1 1 d . . . N4 N 0.7627(4) 0.8454(3) 0.09513(16) 0.0232(7) Uani 1 1 d . . . C5 C 0.8620(4) 0.7327(4) 0.08639(19) 0.0195(7) Uani 1 1 d . . . C6 C 0.9708(4) 0.6652(4) 0.1407(2) 0.0212(8) Uani 1 1 d . . . N7 N 1.0442(3) 0.5451(3) 0.11430(17) 0.0187(6) Uani 1 1 d . . . C8 C 1.1419(5) 0.4746(4) 0.1617(2) 0.0255(8) Uani 1 1 d . . . H8 H 1.1961 0.3921 0.1456 0.031 Uiso 1 1 calc R . . C9 C 1.1636(5) 0.5222(4) 0.2340(2) 0.0323(10) Uani 1 1 d . . . H9 H 1.2294 0.4721 0.2673 0.039 Uiso 1 1 calc R . . C10 C 1.0841(5) 0.6463(5) 0.2546(2) 0.0342(10) Uani 1 1 d . . . H10 H 1.0989 0.6810 0.3029 0.041 Uiso 1 1 calc R . . N11 N 0.9865(4) 0.7194(4) 0.20869(18) 0.0289(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 Ni 0.0153(3) 0.0133(3) 0.0218(3) -0.0011(3) -0.0004(3) 0.0001(3) Co 0.0153(3) 0.0133(3) 0.0218(3) -0.0011(3) -0.0004(3) 0.0001(3) N1 0.0171(14) 0.0175(15) 0.0245(15) 0.0009(12) -0.0004(12) 0.0014(12) N2 0.0228(15) 0.0196(15) 0.0264(15) -0.0021(13) -0.0027(14) 0.0044(13) N3 0.0201(15) 0.0169(14) 0.0265(15) -0.0023(12) 0.0017(13) -0.0018(13) N4 0.0229(15) 0.0206(15) 0.0261(15) -0.0035(13) -0.0022(13) 0.0026(13) C5 0.0166(16) 0.0169(17) 0.0251(18) -0.0025(14) 0.0011(14) 0.0019(14) C6 0.0174(17) 0.0199(18) 0.0263(19) 0.0008(15) -0.0001(14) -0.0016(14) N7 0.0148(13) 0.0144(14) 0.0270(16) 0.0013(12) -0.0005(12) -0.0002(11) C8 0.0242(19) 0.0166(18) 0.036(2) 0.0033(15) -0.0036(16) 0.0009(15) C9 0.033(2) 0.029(2) 0.035(2) 0.0066(17) -0.0121(18) -0.0003(18) C10 0.036(2) 0.038(2) 0.028(2) -0.0031(19) -0.0096(18) 0.001(2) N11 0.0304(18) 0.0280(18) 0.0283(18) -0.0058(14) -0.0057(14) 0.0050(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 Ni N1 2.073(3) 5_765 ? Ni N1 2.073(3) . ? Ni N3 2.114(3) . ? Ni N3 2.114(3) 5_765 ? Ni N7 2.122(3) . ? Ni N7 2.122(3) 5_765 ? N1 N2 1.330(4) . ? N1 C5 1.333(4) . ? N2 N3 1.319(4) 8_765 ? N3 N2 1.319(4) 8_755 ? N3 N4 1.339(4) 8_755 ? N4 C5 1.333(5) . ? N4 N3 1.339(4) 8_765 ? C5 C6 1.463(5) . ? C6 N11 1.324(5) . ? C6 N7 1.349(5) . ? N7 C8 1.340(5) . ? C8 C9 1.378(6) . ? C9 C10 1.371(6) . ? C10 N11 1.335(5) . ? Co N1 2.073(3) 5_765 ? Co N1 2.073(3) . ? Co N3 2.114(3) . ? Co N3 2.114(3) 5_765 ? Co N7 2.122(3) . ? Co N7 2.122(3) 5_765 ? N1 N2 1.330(4) . ? N1 C5 1.333(4) . ? N2 N3 1.319(4) 8_765 ? N3 N2 1.319(4) 8_755 ? N3 N4 1.339(4) 8_755 ? N4 C5 1.333(5) . ? N4 N3 1.339(4) 8_765 ? C5 C6 1.463(5) . ? C6 N11 1.324(5) . ? C6 N7 1.349(5) . ? N7 C8 1.340(5) . ? C8 C9 1.378(6) . ? C9 C10 1.371(6) . ? C10 N11 1.335(5) . ? 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 N1 Ni N1 180.00(16) 5_765 . ? N1 Ni N3 88.81(11) 5_765 . ? N1 Ni N3 91.19(11) . . ? N1 Ni N3 91.19(11) 5_765 5_765 ? N1 Ni N3 88.81(11) . 5_765 ? N3 Ni N3 180.00(16) . 5_765 ? N1 Ni N7 101.68(11) 5_765 . ? N1 Ni N7 78.32(11) . . ? N3 Ni N7 90.98(11) . . ? N3 Ni N7 89.02(11) 5_765 . ? N1 Ni N7 78.32(11) 5_765 5_765 ? N1 Ni N7 101.68(11) . 5_765 ? N3 Ni N7 89.02(11) . 5_765 ? N3 Ni N7 90.98(11) 5_765 5_765 ? N7 Ni N7 180.0 . 5_765 ? N2 N1 C5 106.4(3) . . ? N2 N1 Ni 139.7(2) . . ? C5 N1 Ni 113.9(2) . . ? N3 N2 N1 107.2(3) 8_765 . ? N2 N3 N4 111.6(3) 8_755 8_755 ? N2 N3 Ni 121.6(2) 8_755 . ? N4 N3 Ni 126.6(2) 8_755 . ? C5 N4 N3 103.4(3) . 8_765 ? N1 C5 N4 111.5(3) . . ? N1 C5 C6 119.4(3) . . ? N4 C5 C6 129.1(3) . . ? N11 C6 N7 126.2(3) . . ? N11 C6 C5 120.7(3) . . ? N7 C6 C5 113.1(3) . . ? C8 N7 C6 116.5(3) . . ? C8 N7 Ni 128.3(3) . . ? C6 N7 Ni 115.0(2) . . ? N7 C8 C9 121.3(4) . . ? C10 C9 C8 117.2(4) . . ? N11 C10 C9 123.0(4) . . ? C6 N11 C10 115.8(3) . . ? N1 Co N1 180.00(16) 5_765 . ? N1 Co N3 88.81(11) 5_765 . ? N1 Co N3 91.19(11) . . ? N1 Co N3 91.19(11) 5_765 5_765 ? N1 Co N3 88.81(11) . 5_765 ? N3 Co N3 180.00(16) . 5_765 ? N1 Co N7 101.68(11) 5_765 . ? N1 Co N7 78.32(11) . . ? N3 Co N7 90.98(11) . . ? N3 Co N7 89.02(11) 5_765 . ? N1 Co N7 78.32(11) 5_765 5_765 ? N1 Co N7 101.68(11) . 5_765 ? N3 Co N7 89.02(11) . 5_765 ? N3 Co N7 90.98(11) 5_765 5_765 ? N7 Co N7 180.0 . 5_765 ? N2 N1 C5 106.4(3) . . ? N2 N1 Co 139.7(2) . . ? C5 N1 Co 113.9(2) . . ? N3 N2 N1 107.2(3) 8_765 . ? N2 N3 N4 111.6(3) 8_755 8_755 ? N2 N3 Co 121.6(2) 8_755 . ? N4 N3 Co 126.6(2) 8_755 . ? C5 N4 N3 103.4(3) . 8_765 ? N1 C5 N4 111.5(3) . . ? N1 C5 C6 119.4(3) . . ? N4 C5 C6 129.1(3) . . ? N11 C6 N7 126.2(3) . . ? N11 C6 C5 120.7(3) . . ? N7 C6 C5 113.1(3) . . ? C8 N7 C6 116.5(3) . . ? C8 N7 Co 128.3(3) . . ? C6 N7 Co 115.0(2) . . ? N7 C8 C9 121.3(4) . . ? C10 C9 C8 117.2(4) . . ? N11 C10 C9 123.0(4) . . ? C6 N11 C10 115.8(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.076 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.092