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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ming-Hua Zeng' _publ_contact_author_email ZMH@MAILBOX.GXNU.EDU.CN _publ_section_title ; A Unique 2D Framework Containing Linear Trimeric Cobalt(II) of Mixed Td-Oh-Td Geometries Linked by Two Different Single-carboxylate-aromatic amine Ligands: Structure and Magnetic Properties ; loop_ _publ_author_name 'Ming-Hua Zeng.' 'Yan-Ling Zhou.' 'Hong Liang.' 'Min-Xia Yao.' ; Hua-Hong Zou ; # Attachment 'revised co3cif.cif' data_CO _database_code_depnum_ccdc_archive 'CCDC 669902' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 Co3 N6 O10' _chemical_formula_sum 'C32 H28 Co3 N6 O10' _chemical_formula_weight 833.41 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' O O 0.0106 0.0060 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.209(4) _cell_length_b 10.023(4) _cell_length_c 10.459(5) _cell_angle_alpha 89.260(8) _cell_angle_beta 87.753(8) _cell_angle_gamma 68.912(7) _cell_volume 802.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour darkpurple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 423 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7723 _exptl_absorpt_correction_T_max 0.9242 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ? _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6823 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.13 _reflns_number_total 3455 _reflns_number_gt 2450 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0319P)^2^+0.5387P] 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 3455 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.5000 0.0000 0.0000 0.01864(15) Uani 1 2 d S . . Co2 Co 0.85990(5) -0.08221(4) -0.19508(4) 0.02108(13) Uani 1 1 d . . . O1 O 0.7250(3) 0.0234(2) -0.05465(19) 0.0253(5) Uani 1 1 d . . . H1 H 0.7644 0.0782 -0.0151 0.030 Uiso 1 1 d R . . O2 O 0.4578(3) -0.0585(2) -0.18858(19) 0.0267(5) Uani 1 1 d . . . O3 O 0.6779(3) -0.0740(2) -0.3276(2) 0.0282(5) Uani 1 1 d . . . O4 O 0.9675(3) -0.2932(2) -0.1992(2) 0.0371(6) Uani 1 1 d . . . O5 O 1.1332(3) -0.2375(3) -0.0646(3) 0.0446(7) Uani 1 1 d . . . N1 N -0.0159(3) 0.0332(3) -0.2935(2) 0.0226(6) Uani 1 1 d . . . N2 N 0.1470(3) 0.0984(3) -0.4372(2) 0.0248(6) Uani 1 1 d . . . H2 H 0.2343 0.0932 -0.4877 0.030 Uiso 1 1 calc R . . N3 N 1.3550(3) -0.7725(3) -0.0395(3) 0.0264(6) Uani 1 1 d . . . C1 C 0.5337(4) -0.0890(3) -0.2943(3) 0.0194(6) Uani 1 1 d . . . C2 C 0.4564(4) -0.1570(3) -0.3924(3) 0.0229(7) Uani 1 1 d . . . H2A H 0.5326 -0.2559 -0.4044 0.027 Uiso 1 1 calc R . . H2B H 0.4533 -0.1083 -0.4736 0.027 Uiso 1 1 calc R . . C3 C 0.2724(4) -0.1525(3) -0.3560(3) 0.0245(7) Uani 1 1 d . . . H3A H 0.2428 -0.2149 -0.4135 0.029 Uiso 1 1 calc R . . H3B H 0.2726 -0.1902 -0.2701 0.029 Uiso 1 1 calc R . . C4 C 0.1341(4) -0.0070(3) -0.3606(3) 0.0207(6) Uani 1 1 d . . . C5 C -0.0050(4) 0.2159(3) -0.4202(3) 0.0242(7) Uani 1 1 d . . . C6 C -0.0634(5) 0.3492(3) -0.4788(3) 0.0330(8) Uani 1 1 d . . . H6A H 0.0049 0.3755 -0.5398 0.040 Uiso 1 1 calc R . . C7 C -0.2272(5) 0.4397(4) -0.4414(4) 0.0406(9) Uani 1 1 d . . . H7A H -0.2713 0.5299 -0.4785 0.049 Uiso 1 1 calc R . . C8 C -0.3307(5) 0.4013(4) -0.3495(4) 0.0446(10) Uani 1 1 d . . . H8A H -0.4408 0.4666 -0.3265 0.054 Uiso 1 1 calc R . . C9 C -0.2727(5) 0.2686(4) -0.2922(4) 0.0369(9) Uani 1 1 d . . . H9A H -0.3416 0.2428 -0.2313 0.044 Uiso 1 1 calc R . . C10 C -0.1076(4) 0.1752(3) -0.3292(3) 0.0236(7) Uani 1 1 d . . . C11 C 1.0886(4) -0.3265(3) -0.1194(3) 0.0297(8) Uani 1 1 d . . . C12 C 1.1803(4) -0.4840(3) -0.0929(3) 0.0264(7) Uani 1 1 d . . . C13 C 1.3066(5) -0.5271(4) -0.0034(3) 0.0352(8) Uani 1 1 d . . . H13A H 1.3344 -0.4595 0.0421 0.042 Uiso 1 1 calc R . . C14 C 1.3923(4) -0.6709(4) 0.0191(3) 0.0350(8) Uani 1 1 d . . . H14A H 1.4803 -0.6979 0.0781 0.042 Uiso 1 1 calc R . . C15 C 1.2289(5) -0.7307(4) -0.1241(3) 0.0348(8) Uani 1 1 d . . . H15A H 1.1989 -0.8004 -0.1645 0.042 Uiso 1 1 calc R . . C16 C 1.1402(4) -0.5885(3) -0.1549(3) 0.0337(8) Uani 1 1 d . . . H16A H 1.0553 -0.5640 -0.2162 0.040 Uiso 1 1 calc R . . 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 0.0176(3) 0.0201(3) 0.0178(3) 0.0004(2) 0.0011(2) -0.0064(2) Co2 0.0189(2) 0.0228(2) 0.0212(2) 0.00259(17) 0.00050(17) -0.00734(18) O1 0.0242(11) 0.0311(13) 0.0242(12) -0.0066(10) 0.0053(9) -0.0149(10) O2 0.0251(12) 0.0391(14) 0.0193(11) -0.0044(10) 0.0021(9) -0.0159(10) O3 0.0213(12) 0.0444(14) 0.0222(12) 0.0043(10) -0.0021(9) -0.0157(11) O4 0.0374(14) 0.0254(13) 0.0415(15) 0.0062(11) -0.0053(12) -0.0027(11) O5 0.0564(17) 0.0252(14) 0.0540(17) 0.0025(12) -0.0057(14) -0.0165(12) N1 0.0197(13) 0.0256(14) 0.0238(14) 0.0018(11) -0.0003(11) -0.0099(11) N2 0.0198(14) 0.0319(16) 0.0258(14) 0.0016(12) 0.0032(11) -0.0135(12) N3 0.0230(14) 0.0221(14) 0.0318(15) 0.0012(12) -0.0012(12) -0.0054(12) C1 0.0158(15) 0.0183(15) 0.0206(16) 0.0043(12) -0.0032(12) -0.0018(12) C2 0.0200(16) 0.0266(17) 0.0201(16) -0.0038(13) 0.0010(13) -0.0060(13) C3 0.0210(16) 0.0244(17) 0.0288(17) -0.0015(14) 0.0000(14) -0.0091(14) C4 0.0193(15) 0.0263(17) 0.0200(15) 0.0004(13) -0.0023(12) -0.0124(13) C5 0.0250(17) 0.0268(18) 0.0248(17) -0.0037(14) -0.0033(14) -0.0139(14) C6 0.046(2) 0.0255(18) 0.0327(19) 0.0032(15) -0.0022(17) -0.0188(17) C7 0.053(2) 0.0233(19) 0.043(2) 0.0046(16) -0.0035(19) -0.0101(18) C8 0.038(2) 0.030(2) 0.057(3) -0.0039(18) 0.0048(19) -0.0016(17) C9 0.031(2) 0.032(2) 0.042(2) 0.0023(17) 0.0083(16) -0.0064(16) C10 0.0258(17) 0.0252(17) 0.0213(16) -0.0022(13) 0.0013(13) -0.0113(14) C11 0.0303(19) 0.0223(18) 0.0313(19) 0.0051(15) 0.0091(15) -0.0043(15) C12 0.0255(17) 0.0242(17) 0.0271(17) 0.0024(14) 0.0022(14) -0.0064(14) C13 0.040(2) 0.0251(19) 0.043(2) 0.0004(16) -0.0094(17) -0.0137(16) C14 0.034(2) 0.0289(19) 0.044(2) 0.0086(17) -0.0178(17) -0.0122(16) C15 0.039(2) 0.0243(19) 0.040(2) -0.0034(16) -0.0120(17) -0.0091(16) C16 0.036(2) 0.0258(19) 0.0333(19) 0.0013(15) -0.0124(16) -0.0024(16) _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 O1 2.005(2) . ? Co1 O1 2.005(2) 2_655 ? Co1 O2 2.141(2) . ? Co1 O2 2.141(2) 2_655 ? Co1 N3 2.202(3) 2_745 ? Co1 N3 2.202(3) 1_465 ? Co2 O1 1.890(2) . ? Co2 O4 1.977(2) . ? Co2 N1 2.043(3) 1_655 ? Co2 O3 2.057(2) . ? O1 H1 0.8501 . ? O2 C1 1.234(3) . ? O3 C1 1.280(3) . ? O4 C11 1.271(4) . ? O5 C11 1.234(4) . ? N1 C4 1.324(4) . ? N1 C10 1.404(4) . ? N1 Co2 2.043(3) 1_455 ? N2 C4 1.349(4) . ? N2 C5 1.381(4) . ? N2 H2 0.8600 . ? N3 C14 1.327(4) . ? N3 C15 1.335(4) . ? N3 Co1 2.202(3) 1_645 ? C1 C2 1.518(4) . ? C2 C3 1.528(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.493(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.390(4) . ? C5 C10 1.398(4) . ? C6 C7 1.369(5) . ? C6 H6A 0.9300 . ? C7 C8 1.398(5) . ? C7 H7A 0.9300 . ? C8 C9 1.379(5) . ? C8 H8A 0.9300 . ? C9 C10 1.385(4) . ? C9 H9A 0.9300 . ? C11 C12 1.512(4) . ? C12 C13 1.372(4) . ? C12 C16 1.382(5) . ? C13 C14 1.379(5) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.388(5) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? 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 O1 Co1 O1 180.00(11) . 2_655 ? O1 Co1 O2 92.75(8) . . ? O1 Co1 O2 87.25(8) 2_655 . ? O1 Co1 O2 87.25(8) . 2_655 ? O1 Co1 O2 92.75(8) 2_655 2_655 ? O2 Co1 O2 180.00(12) . 2_655 ? O1 Co1 N3 89.56(9) . 2_745 ? O1 Co1 N3 90.44(9) 2_655 2_745 ? O2 Co1 N3 88.78(9) . 2_745 ? O2 Co1 N3 91.22(9) 2_655 2_745 ? O1 Co1 N3 90.44(9) . 1_465 ? O1 Co1 N3 89.56(9) 2_655 1_465 ? O2 Co1 N3 91.22(9) . 1_465 ? O2 Co1 N3 88.78(9) 2_655 1_465 ? N3 Co1 N3 180.00(18) 2_745 1_465 ? O1 Co2 O4 123.99(10) . . ? O1 Co2 N1 110.92(10) . 1_655 ? O4 Co2 N1 118.35(10) . 1_655 ? O1 Co2 O3 103.97(9) . . ? O4 Co2 O3 93.92(10) . . ? N1 Co2 O3 98.35(9) 1_655 . ? Co2 O1 Co1 120.08(11) . . ? Co2 O1 H1 117.9 . . ? Co1 O1 H1 122.0 . . ? C1 O2 Co1 140.3(2) . . ? C1 O3 Co2 121.23(19) . . ? C11 O4 Co2 105.9(2) . . ? C4 N1 C10 105.8(2) . . ? C4 N1 Co2 131.5(2) . 1_455 ? C10 N1 Co2 120.69(19) . 1_455 ? C4 N2 C5 107.8(3) . . ? C4 N2 H2 126.1 . . ? C5 N2 H2 126.1 . . ? C14 N3 C15 117.3(3) . . ? C14 N3 Co1 120.8(2) . 1_645 ? C15 N3 Co1 121.9(2) . 1_645 ? O2 C1 O3 125.7(3) . . ? O2 C1 C2 118.0(3) . . ? O3 C1 C2 116.2(3) . . ? C1 C2 C3 114.0(2) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 114.4(3) . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N1 C4 N2 112.1(3) . . ? N1 C4 C3 124.7(3) . . ? N2 C4 C3 123.2(3) . . ? N2 C5 C6 131.9(3) . . ? N2 C5 C10 105.8(3) . . ? C6 C5 C10 122.2(3) . . ? C7 C6 C5 116.2(3) . . ? C7 C6 H6A 121.9 . . ? C5 C6 H6A 121.9 . . ? C6 C7 C8 122.3(3) . . ? C6 C7 H7A 118.8 . . ? C8 C7 H7A 118.8 . . ? C9 C8 C7 121.4(3) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 117.2(3) . . ? C8 C9 H9A 121.4 . . ? C10 C9 H9A 121.4 . . ? C9 C10 C5 120.7(3) . . ? C9 C10 N1 130.8(3) . . ? C5 C10 N1 108.4(3) . . ? O5 C11 O4 123.3(3) . . ? O5 C11 C12 119.8(3) . . ? O4 C11 C12 116.9(3) . . ? C13 C12 C16 117.8(3) . . ? C13 C12 C11 119.9(3) . . ? C16 C12 C11 122.3(3) . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? N3 C14 C13 123.0(3) . . ? N3 C14 H14A 118.5 . . ? C13 C14 H14A 118.5 . . ? N3 C15 C16 123.2(3) . . ? N3 C15 H15A 118.4 . . ? C16 C15 H15A 118.4 . . ? C12 C16 C15 118.8(3) . . ? C12 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O5 0.85 2.24 3.082(3) 172.5 2_755 N2 H2 O3 0.86 2.02 2.768(3) 144.5 2_654 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.595 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.089