Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_mn _database_code_CSD 170949 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Chen, Xiao-Ming' 'Chen, Hong-Ji' 'Gao, Song' 'Mao, Zong-Wan' _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry & Chemical Engineering Zhongshan University Guangzhou 510275 CHINA ; _publ_contact_author_email 'CESCXM@ZSU.EDU.CN' _publ_section_title ; Ferrimagnetic-like ordering in a unique three-dimensional coordination polymer featuring mixed azide/carboxylate-bridged trinuclear manganese(II) clusters as subunits ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 Mn3 N10 O10' _chemical_formula_weight 773.32 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' 'Mn' 'Mn' 0.3368 0.7283 '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 6.771(2) _cell_length_b 10.158(6) _cell_length_c 11.635(4) _cell_angle_alpha 73.210(2) _cell_angle_beta 74.5700(10) _cell_angle_gamma 87.800(2) _cell_volume 737.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 15 _exptl_crystal_description Prismic _exptl_crystal_colour 'Light yellow ' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 389 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.859 _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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% <2 _diffrn_reflns_number 3566 _diffrn_reflns_av_R_equivalents 0.0098 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3553 _reflns_number_gt 3041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-90 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP Version 5.1 (Bruker AXS 1998)' _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 w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.3134P] 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 SHELXL _refine_ls_extinction_coef 0.0098 _refine_ls_number_reflns 3553 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.0000 0.0000 0.02196(14) Uani 1 d S . . Mn2 Mn 0.22860(5) -0.16444(3) -0.18069(3) 0.02399(12) Uani 1 d . . . O1W O 0.0971(3) 0.04000(19) -0.19618(18) 0.0351(4) Uani 1 d . . . H1WA H 0.1359 0.0770 -0.1486 0.080 Uiso 1 d R . . H1WB H -0.0408 0.0259 -0.1755 0.080 Uiso 1 d R . . N3 N 0.6915(3) 0.1747(2) 0.00415(19) 0.0290(4) Uani 1 d . . . N4 N 0.7774(3) 0.2653(2) -0.08763(19) 0.0293(4) Uani 1 d . . . N5 N 0.8615(5) 0.3516(3) -0.1742(2) 0.0497(7) Uani 1 d . . . O1 O -0.0656(3) -0.27368(18) -0.07228(16) 0.0304(4) Uani 1 d . . . O2 O -0.2454(3) -0.13580(17) 0.03355(17) 0.0308(4) Uani 1 d . . . C1 C -0.1983(3) -0.2520(2) 0.0178(2) 0.0242(4) Uani 1 d . . . C2 C -0.3055(4) -0.3782(2) 0.1200(2) 0.0275(5) Uani 1 d . . . C3 C -0.2759(4) -0.5093(3) 0.1035(2) 0.0300(5) Uani 1 d . . . H3B H -0.1955 -0.5162 0.0241 0.080 Uiso 1 d R . . C4 C -0.4711(4) -0.6131(3) 0.3035(3) 0.0374(6) Uani 1 d . . . H4A H -0.5312 -0.6950 0.3678 0.080 Uiso 1 d R . . N1 N -0.3541(4) -0.6258(2) 0.1929(2) 0.0330(5) Uani 1 d . . . C5 C -0.5087(5) -0.4877(3) 0.3274(3) 0.0397(6) Uani 1 d . . . H5A H -0.5913 -0.4831 0.4071 0.080 Uiso 1 d R . . C6 C -0.4237(4) -0.3681(3) 0.2346(3) 0.0365(6) Uani 1 d . . . H6A H -0.4472 -0.2797 0.2490 0.080 Uiso 1 d R . . O3 O 0.5155(3) -0.0657(2) -0.30060(16) 0.0349(4) Uani 1 d . . . O4 O 0.6547(3) 0.04628(19) -0.19842(15) 0.0342(4) Uani 1 d . . . C7 C 0.6373(4) 0.0220(2) -0.2956(2) 0.0238(4) Uani 1 d . . . C8 C 0.7702(4) 0.1099(2) -0.4187(2) 0.0238(4) Uani 1 d . . . C9 C 0.7686(4) 0.0852(2) -0.5303(2) 0.0258(5) Uani 1 d . . . H9A H 0.6897 0.0066 -0.5262 0.080 Uiso 1 d R . . C10 C 0.9858(4) 0.2741(3) -0.6475(2) 0.0370(6) Uani 1 d . . . H10A H 1.0639 0.3305 -0.7271 0.080 Uiso 1 d R . . N2 N 0.8712(3) 0.1654(2) -0.64352(19) 0.0295(4) Uani 1 d . . . C11 C 0.9962(5) 0.3059(3) -0.5409(3) 0.0424(7) Uani 1 d . . . H11A H 1.0763 0.3850 -0.5474 0.080 Uiso 1 d R . . C12 C 0.8877(4) 0.2233(3) -0.4248(2) 0.0347(6) Uani 1 d . . . H12A H 0.8936 0.2437 -0.3501 0.080 Uiso 1 d 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 Mn1 0.0263(3) 0.0209(2) 0.0174(2) -0.00535(17) -0.00339(18) -0.00252(18) Mn2 0.0299(2) 0.02152(19) 0.01864(19) -0.00473(13) -0.00347(14) -0.00539(14) O1W 0.0373(10) 0.0295(9) 0.0430(11) -0.0141(8) -0.0144(8) 0.0025(8) N3 0.0372(11) 0.0264(10) 0.0237(10) -0.0063(8) -0.0084(8) -0.0088(8) N4 0.0342(11) 0.0289(10) 0.0264(10) -0.0069(8) -0.0113(9) -0.0042(9) N5 0.0601(17) 0.0483(15) 0.0332(13) 0.0038(11) -0.0135(12) -0.0226(13) O1 0.0332(9) 0.0270(9) 0.0267(8) -0.0072(7) -0.0002(7) -0.0067(7) O2 0.0343(9) 0.0222(8) 0.0372(9) -0.0094(7) -0.0113(8) 0.0035(7) C1 0.0225(10) 0.0253(11) 0.0270(11) -0.0098(9) -0.0078(9) -0.0017(8) C2 0.0272(11) 0.0249(11) 0.0281(12) -0.0066(9) -0.0046(9) -0.0005(9) C3 0.0331(13) 0.0248(11) 0.0290(12) -0.0084(9) -0.0016(10) -0.0036(9) C4 0.0376(14) 0.0301(13) 0.0334(13) -0.0034(10) 0.0032(11) -0.0005(11) N1 0.0372(12) 0.0226(10) 0.0335(11) -0.0065(8) -0.0012(9) -0.0025(8) C5 0.0405(15) 0.0371(14) 0.0311(13) -0.0079(11) 0.0056(11) 0.0010(12) C6 0.0377(14) 0.0314(13) 0.0342(13) -0.0117(11) 0.0035(11) -0.0009(11) O3 0.0339(10) 0.0428(10) 0.0236(8) -0.0061(7) -0.0021(7) -0.0148(8) O4 0.0437(11) 0.0386(10) 0.0182(8) -0.0090(7) -0.0023(7) -0.0090(8) C7 0.0247(11) 0.0254(11) 0.0187(10) -0.0064(8) -0.0013(8) -0.0002(8) C8 0.0238(10) 0.0278(11) 0.0179(10) -0.0049(8) -0.0037(8) -0.0009(9) C9 0.0289(11) 0.0265(11) 0.0211(10) -0.0068(9) -0.0046(9) -0.0047(9) C10 0.0403(14) 0.0421(15) 0.0232(12) -0.0068(10) 0.0004(10) -0.0169(12) N2 0.0331(11) 0.0342(11) 0.0197(9) -0.0079(8) -0.0031(8) -0.0073(9) C11 0.0478(17) 0.0449(16) 0.0315(14) -0.0096(12) -0.0031(12) -0.0256(13) C12 0.0376(14) 0.0428(15) 0.0244(12) -0.0114(10) -0.0057(10) -0.0134(11) _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 Mn1 O4 2.1844(18) . ? Mn1 O4 2.1844(18) 2_655 ? Mn1 O2 2.2118(19) 2 ? Mn1 O2 2.2118(19) 1_655 ? Mn1 N3 2.257(2) 2_655 ? Mn1 N3 2.257(2) . ? Mn2 O3 2.1504(18) . ? Mn2 O1 2.1941(18) . ? Mn2 O1W 2.206(2) . ? Mn2 N3 2.233(2) 2_655 ? Mn2 N1 2.292(2) 2_545 ? Mn2 N2 2.321(2) 2_654 ? N3 N4 1.212(3) . ? N3 Mn2 2.233(2) 2_655 ? N4 N5 1.153(3) . ? O1 C1 1.253(3) . ? O2 C1 1.263(3) . ? O2 Mn1 2.2118(19) 1_455 ? C1 C2 1.522(3) . ? C2 C6 1.391(4) . ? C2 C3 1.399(3) . ? C3 N1 1.345(3) . ? C4 N1 1.358(3) . ? C4 C5 1.381(4) . ? N1 Mn2 2.292(2) 2_545 ? C5 C6 1.392(4) . ? O3 C7 1.260(3) . ? O4 C7 1.260(3) . ? C7 C8 1.515(3) . ? C8 C9 1.395(3) . ? C8 C12 1.399(3) . ? C9 N2 1.348(3) . ? C10 N2 1.357(3) . ? C10 C11 1.387(4) . ? N2 Mn2 2.321(2) 2_654 ? C11 C12 1.391(4) . ? 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 O4 Mn1 O4 180.0 . 2_655 ? O4 Mn1 O2 93.01(7) . 2 ? O4 Mn1 O2 86.99(7) 2_655 2 ? O4 Mn1 O2 86.99(7) . 1_655 ? O4 Mn1 O2 93.01(7) 2_655 1_655 ? O2 Mn1 O2 180.0 2 1_655 ? O4 Mn1 N3 92.51(7) . 2_655 ? O4 Mn1 N3 87.49(7) 2_655 2_655 ? O2 Mn1 N3 87.78(8) 2 2_655 ? O2 Mn1 N3 92.22(8) 1_655 2_655 ? O4 Mn1 N3 87.49(7) . . ? O4 Mn1 N3 92.51(7) 2_655 . ? O2 Mn1 N3 92.22(8) 2 . ? O2 Mn1 N3 87.78(8) 1_655 . ? N3 Mn1 N3 180.0 2_655 . ? O3 Mn2 O1 174.59(7) . . ? O3 Mn2 O1W 89.11(8) . . ? O1 Mn2 O1W 93.17(8) . . ? O3 Mn2 N3 94.88(8) . 2_655 ? O1 Mn2 N3 89.88(7) . 2_655 ? O1W Mn2 N3 93.45(8) . 2_655 ? O3 Mn2 N1 89.84(8) . 2_545 ? O1 Mn2 N1 87.16(8) . 2_545 ? O1W Mn2 N1 171.22(8) . 2_545 ? N3 Mn2 N1 95.33(8) 2_655 2_545 ? O3 Mn2 N2 88.74(7) . 2_654 ? O1 Mn2 N2 86.45(7) . 2_654 ? O1W Mn2 N2 87.90(8) . 2_654 ? N3 Mn2 N2 176.15(7) 2_655 2_654 ? N1 Mn2 N2 83.36(8) 2_545 2_654 ? N4 N3 Mn2 116.69(16) . 2_655 ? N4 N3 Mn1 123.92(16) . . ? Mn2 N3 Mn1 118.63(9) 2_655 . ? N5 N4 N3 179.0(3) . . ? C1 O1 Mn2 130.26(15) . . ? C1 O2 Mn1 132.87(16) . 1_455 ? O1 C1 O2 126.0(2) . . ? O1 C1 C2 116.7(2) . . ? O2 C1 C2 117.2(2) . . ? C6 C2 C3 118.2(2) . . ? C6 C2 C1 121.4(2) . . ? C3 C2 C1 120.3(2) . . ? N1 C3 C2 123.4(2) . . ? N1 C4 C5 123.0(2) . . ? C3 N1 C4 117.3(2) . . ? C3 N1 Mn2 121.12(17) . 2_545 ? C4 N1 Mn2 119.61(17) . 2_545 ? C4 C5 C6 119.0(2) . . ? C2 C6 C5 119.1(2) . . ? C7 O3 Mn2 134.36(16) . . ? C7 O4 Mn1 140.63(17) . . ? O4 C7 O3 126.2(2) . . ? O4 C7 C8 116.9(2) . . ? O3 C7 C8 116.8(2) . . ? C9 C8 C12 118.0(2) . . ? C9 C8 C7 120.7(2) . . ? C12 C8 C7 121.2(2) . . ? N2 C9 C8 123.8(2) . . ? N2 C10 C11 122.6(2) . . ? C9 N2 C10 117.4(2) . . ? C9 N2 Mn2 120.25(16) . 2_654 ? C10 N2 Mn2 119.20(17) . 2_654 ? C10 C11 C12 119.5(2) . . ? C11 C12 C8 118.8(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.365 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.087