Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Rina Patel' ;School of Chemistry, University of Southampton, Highfield, Southampton, SO17 1BJ, United Kingdom ; 'Daniel J. Price' ;WestCHEM, Department of Chemistry, University of Glasgow, University Avenue, Glasgow, G12 8QQ, United Kingdom ; 'Mark T. Weller' ;School of Chemistry, University of Southampton, Highfield, Southampton, SO17 1BJ, United Kingdom ; _publ_contact_author_address ;WestCHEM, Department of Chemistry, University of Glasgow, University Avenue, Glasgow, G12 8QQ, United Kingdom ; _publ_contact_author_email d.price@chem.gla.ac.uk _publ_contact_author_fax +44(0)1413304888 #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Dr. Daniel J. Price' #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; Topological ferrimagnetism and superparamagnetic-like behaviour in a disordered homometallic coordination network ; data_coamtrz _database_code_depnum_ccdc_archive 'CCDC 297715' _audit_creation_method SHELXL-97 #------------------ TEXT ----------------------------------------------------# _chemical_name_systematic ; catena-((tris(\m^3^-3-amino-1,2,4-triazolato-N^1^,N^2^,N^4^))- chloro dicobalt(II)) ; _chemical_name_common ; catena-((tris(mu$3!-3-amino-1,2,4-triazolato-N$1!,N$2!,N$4!))- chloro dicobalt(ii)) ; _chemical_melting_point 'not available' _chemical_formula_moiety 'C6 H9 Cl1 Co2 N12' _chemical_formula_sum 'C6 H9 Cl1 Co2 N12' _chemical_formula_weight 402.54 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P63/mmc _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 9.9655(7) _cell_length_b 9.9655(7) _cell_length_c 7.7523(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 666.74(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min 7.86 _cell_measurement_theta_max 27.40 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 2.702 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4634 _diffrn_reflns_av_R_equivalents 0.1103 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.40 _reflns_number_total 320 _reflns_number_gt 264 _reflns_threshold_expression 4sigma(I) _computing_data_collection 'COLLECT (Hooft, 1988)' _computing_cell_refinement 'DENZO (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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. All H atoms are fixed in idealised geometries and refined in riding mode, with isostropic thermal parameters fixed at 1.2 times thar of the parent atom. The orientation of the triazole is orienatationally dissordered over two sites. ; _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^)+(0.0000P)^2^+5.2804P] 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 320 _refine_ls_number_parameters 31 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.257 _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 Co1 Co 0.0000 0.0000 0.0000 0.0204(7) Uani 1 12 d S . . Co2 Co -0.3333 -0.6667 0.1603(4) 0.0205(8) Uani 0.50 6 d SP . . Cl1 Cl -0.3333 -0.6667 -0.1350(8) 0.0339(17) Uani 0.50 6 d SP . . N1 N -0.1000(4) -0.2000(7) 0.1602(7) 0.0266(15) Uani 1 2 d S . . C1A C -0.1738(6) -0.3476(11) 0.1172(11) 0.051(3) Uani 1 2 d S . . H1 H -0.1907 -0.3815 0.0033 0.061 Uiso 0.50 2 calc SPR A 1 N2 N -0.2216(6) -0.4433(12) 0.2500 0.064(4) Uani 1 4 d S . . N3 N -0.2151(8) -0.4303(16) -0.0286(16) 0.053(5) Uani 0.50 2 d SP B 2 H3A H -0.1920 -0.3839 -0.1268 0.063 Uiso 0.50 2 calc SPR B 2 H3B H -0.2649 -0.5299 -0.0243 0.063 Uiso 0.50 2 calc SPR B 2 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 Co1 0.0239(9) 0.0239(9) 0.0134(10) 0.000 0.000 0.0120(4) Co2 0.0182(11) 0.0182(11) 0.0252(17) 0.000 0.000 0.0091(5) Cl1 0.040(3) 0.040(3) 0.021(3) 0.000 0.000 0.0201(13) N1 0.034(3) 0.022(3) 0.021(3) -0.002(3) -0.0011(13) 0.0108(16) C1A 0.066(5) 0.029(5) 0.047(5) -0.024(4) -0.012(2) 0.014(3) N2 0.072(8) 0.004(5) 0.093(9) 0.000 0.000 0.002(2) N3 0.094(11) 0.014(7) 0.023(7) 0.001(6) 0.000(3) 0.007(3) _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 Co1 N1 2.126(6) 16 ? Co1 N1 2.126(6) 4 ? Co1 N1 2.126(6) 20 ? Co1 N1 2.126(6) 8 ? Co1 N1 2.126(6) . ? Co1 N1 2.126(6) 13 ? Co2 Co2 1.390(7) 14_556 ? Co2 N2 2.049(10) 7_545 ? Co2 N2 2.049(10) . ? Co2 N2 2.049(10) 3_445 ? Co2 Cl1 2.289(7) . ? Cl1 Cl1 1.784(12) 14 ? N1 C1A 1.317(10) . ? N1 N1 1.393(10) 14_556 ? C1A N2 1.320(11) . ? C1A N3 1.337(14) . ? C1A H1 0.9300 . ? N2 C1A 1.320(11) 14_556 ? N2 Co2 2.049(10) 14_556 ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? 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 Co1 N1 180 16 4 ? N1 Co1 N1 89.3(2) 16 20 ? N1 Co1 N1 90.7(2) 4 20 ? N1 Co1 N1 90.7(2) 16 8 ? N1 Co1 N1 89.3(2) 4 8 ? N1 Co1 N1 180 20 8 ? N1 Co1 N1 89.3(2) 16 . ? N1 Co1 N1 90.7(2) 4 . ? N1 Co1 N1 89.3(2) 20 . ? N1 Co1 N1 90.7(2) 8 . ? N1 Co1 N1 90.7(2) 16 13 ? N1 Co1 N1 89.3(2) 4 13 ? N1 Co1 N1 90.7(2) 20 13 ? N1 Co1 N1 89.3(2) 8 13 ? N1 Co1 N1 180 . 13 ? Co2 Co2 N2 70.17(13) 14_556 7_545 ? Co2 Co2 N2 70.17(13) 14_556 . ? N2 Co2 N2 109.11(13) 7_545 . ? Co2 Co2 N2 70.17(13) 14_556 3_445 ? N2 Co2 N2 109.11(13) 7_545 3_445 ? N2 Co2 N2 109.11(13) . 3_445 ? Co2 Co2 Cl1 180 14_556 . ? N2 Co2 Cl1 109.83(13) 7_545 . ? N2 Co2 Cl1 109.83(13) . . ? N2 Co2 Cl1 109.83(13) 3_445 . ? Cl1 Cl1 Co2 180 14 . ? C1A N1 N1 104.7(5) . 14_556 ? C1A N1 Co1 129.6(5) . . ? N1 N1 Co1 125.72(15) 14_556 . ? N1 C1A N2 114.1(8) . . ? N1 C1A N3 136.9(10) . . ? N2 C1A N3 109.0(9) . . ? N1 C1A H1 123.0 . . ? N2 C1A H1 123.0 . . ? C1A N2 C1A 102.6(10) 14_556 . ? C1A N2 Co2 148.5(6) 14_556 . ? C1A N2 Co2 108.9(4) . . ? C1A N2 Co2 108.9(4) 14_556 14_556 ? C1A N2 Co2 148.5(6) . 14_556 ? C1A N3 H3A 120.0 . . ? C1A N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.592 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.117