# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Srinivasan Natarajan' _publ_contact_author_address ; Solid State and Structural Chemistry Unit Indian Institute of Science C.V. Raman Avenue Bangalore 560 012 INDIA ; _publ_contact_author_email SNATARAJAN@SSCU.IISC.ERNET.IN _publ_section_title ; Long-range magnetic ordering in a three-dimensional metal-organic framework possessing -Mn-O-Mn- Kagome layers ; loop_ _publ_author_name 'Srinivasan Natarajan' 'Partha Mahata' 'Diptiman Sen' # Attachment 'pm2390_m.cif.txt' data_Compound(I) _database_code_depnum_ccdc_archive 'CCDC 637648' #=============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common 'Manganese Carboxylate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 Mn3 O12' _chemical_formula_weight 579.04 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' K K 0.2009 0.2494 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.314(3) _cell_length_b 6.5962(16) _cell_length_c 11.391(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.029(4) _cell_angle_gamma 90.00 _cell_volume 793.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1853 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.97 _exptl_crystal_description Rectangular _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7588 _exptl_absorpt_correction_T_max 0.8290 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART CCD area detector' _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 6663 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.97 _reflns_number_total 1853 _reflns_number_gt 1600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0263P)^2^+0.9220P] 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 1853 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Mn1 Mn 0.32208(4) 0.21367(7) 0.22612(4) 0.01751(12) Uani 1 1 d . . . Mn2 Mn 0.5000 0.0000 0.5000 0.01318(14) Uani 1 2 d S . . O1 O 0.00119(18) 0.3227(3) 0.71336(19) 0.0243(5) Uani 1 1 d . . . O2 O 0.23396(18) 0.4976(3) 0.42370(17) 0.0228(4) Uani 1 1 d . . . O3 O 0.38228(18) 0.2689(3) 0.43618(17) 0.0180(4) Uani 1 1 d . . . O4 O 0.61155(17) 0.1855(3) 0.66001(17) 0.0193(4) Uani 1 1 d . . . O5 O 0.66184(17) 0.4540(3) 0.77886(17) 0.0191(4) Uani 1 1 d . . . O6 O 0.11929(19) 0.3837(3) 0.91321(18) 0.0248(5) Uani 1 1 d . . . C1 C 0.2249(2) 0.3475(4) 0.7717(2) 0.0150(5) Uani 1 1 d . . . C2 C 0.3405(3) 0.3414(4) 0.8701(2) 0.0190(6) Uani 1 1 d . . . H2 H 0.3435 0.3381 0.9528 0.023 Uiso 1 1 calc R . . C3 C 0.4506(3) 0.3401(4) 0.8454(2) 0.0190(6) Uani 1 1 d . . . H3 H 0.5278 0.3395 0.9122 0.023 Uiso 1 1 calc R . . C4 C 0.4498(2) 0.3398(4) 0.7223(2) 0.0135(5) Uani 1 1 d . . . C5 C 0.3332(2) 0.3518(4) 0.6216(2) 0.0128(5) Uani 1 1 d . . . C6 C 0.2224(2) 0.3578(4) 0.6488(2) 0.0154(5) Uani 1 1 d . . . H6 H 0.1448 0.3690 0.5831 0.018 Uiso 1 1 calc R . . C7 C 0.1056(3) 0.3515(4) 0.8010(3) 0.0181(6) Uani 1 1 d . . . C8 C 0.5792(2) 0.3287(4) 0.7165(2) 0.0145(5) Uani 1 1 d . . . C9 C 0.3167(2) 0.3749(4) 0.4842(2) 0.0141(5) 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 Mn1 0.0117(2) 0.0221(2) 0.0193(2) -0.00477(16) 0.00629(16) -0.00163(16) Mn2 0.0133(3) 0.0153(3) 0.0132(3) 0.0008(2) 0.0074(2) 0.0004(2) O1 0.0145(10) 0.0290(11) 0.0317(11) 0.0021(9) 0.0110(9) 0.0013(8) O2 0.0194(10) 0.0307(11) 0.0193(10) 0.0089(8) 0.0081(8) 0.0111(8) O3 0.0181(10) 0.0227(10) 0.0158(9) -0.0002(7) 0.0093(8) 0.0049(8) O4 0.0130(9) 0.0265(10) 0.0194(10) -0.0060(8) 0.0073(8) 0.0012(8) O5 0.0152(9) 0.0200(9) 0.0211(10) -0.0008(8) 0.0052(8) -0.0029(8) O6 0.0260(11) 0.0308(11) 0.0266(11) 0.0014(9) 0.0204(9) 0.0055(9) C1 0.0162(13) 0.0113(11) 0.0222(13) -0.0005(10) 0.0126(11) 0.0011(10) C2 0.0202(14) 0.0243(14) 0.0146(13) -0.0003(11) 0.0090(11) 0.0003(11) C3 0.0168(14) 0.0254(14) 0.0143(13) 0.0006(11) 0.0050(11) 0.0000(11) C4 0.0132(12) 0.0141(12) 0.0154(12) -0.0014(10) 0.0078(10) 0.0003(10) C5 0.0118(12) 0.0132(11) 0.0146(12) -0.0008(9) 0.0064(10) -0.0009(10) C6 0.0113(12) 0.0154(12) 0.0179(13) -0.0003(10) 0.0033(10) 0.0000(10) C7 0.0202(14) 0.0129(12) 0.0263(14) 0.0031(11) 0.0146(12) 0.0020(10) C8 0.0132(12) 0.0186(13) 0.0117(12) 0.0041(10) 0.0045(10) 0.0002(10) C9 0.0120(12) 0.0141(12) 0.0156(13) -0.0001(10) 0.0044(10) -0.0021(10) _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 O1 2.097(2) 4_665 ? Mn1 O2 2.1376(19) 2_545 ? Mn1 O5 2.202(2) 3_666 ? Mn1 O3 2.2700(19) . ? Mn1 O4 2.3229(19) 4_565 ? Mn1 O5 2.3776(19) 4_565 ? Mn2 O6 2.0845(19) 2_546 ? Mn2 O6 2.0845(19) 4_665 ? Mn2 O3 2.1804(19) . ? Mn2 O3 2.1804(19) 3_656 ? Mn2 O4 2.1819(19) . ? Mn2 O4 2.1819(19) 3_656 ? O1 C7 1.257(3) . ? O1 Mn1 2.097(2) 4_566 ? O2 C9 1.243(3) . ? O2 Mn1 2.1376(19) 2 ? O3 C9 1.276(3) . ? O4 C8 1.269(3) . ? O4 Mn1 2.3229(19) 4_666 ? O5 C8 1.259(3) . ? O5 Mn1 2.202(2) 3_666 ? O5 Mn1 2.3776(19) 4_666 ? O6 C7 1.249(3) . ? O6 Mn2 2.0845(19) 2_556 ? C1 C2 1.385(4) . ? C1 C6 1.391(4) . ? C1 C7 1.503(4) . ? C2 C3 1.373(4) . ? C3 C4 1.398(3) . ? C4 C5 1.406(3) . ? C4 C8 1.491(4) . ? C5 C6 1.396(4) . ? C5 C9 1.516(3) . ? 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 Mn1 O2 83.42(8) 4_665 2_545 ? O1 Mn1 O5 91.23(8) 4_665 3_666 ? O2 Mn1 O5 130.30(8) 2_545 3_666 ? O1 Mn1 O3 99.18(7) 4_665 . ? O2 Mn1 O3 147.08(8) 2_545 . ? O5 Mn1 O3 82.59(7) 3_666 . ? O1 Mn1 O4 156.12(8) 4_665 4_565 ? O2 Mn1 O4 87.50(7) 2_545 4_565 ? O5 Mn1 O4 77.94(7) 3_666 4_565 ? O3 Mn1 O4 100.41(7) . 4_565 ? O1 Mn1 O5 143.87(7) 4_665 4_565 ? O2 Mn1 O5 81.77(7) 2_545 4_565 ? O5 Mn1 O5 123.18(6) 3_666 4_565 ? O3 Mn1 O5 77.05(7) . 4_565 ? O4 Mn1 O5 55.19(6) 4_565 4_565 ? O6 Mn2 O6 180.0 2_546 4_665 ? O6 Mn2 O3 92.04(8) 2_546 . ? O6 Mn2 O3 87.96(8) 4_665 . ? O6 Mn2 O3 87.96(8) 2_546 3_656 ? O6 Mn2 O3 92.04(8) 4_665 3_656 ? O3 Mn2 O3 180.0 . 3_656 ? O6 Mn2 O4 95.11(8) 2_546 . ? O6 Mn2 O4 84.89(8) 4_665 . ? O3 Mn2 O4 85.61(7) . . ? O3 Mn2 O4 94.39(7) 3_656 . ? O6 Mn2 O4 84.89(8) 2_546 3_656 ? O6 Mn2 O4 95.11(8) 4_665 3_656 ? O3 Mn2 O4 94.39(7) . 3_656 ? O3 Mn2 O4 85.61(7) 3_656 3_656 ? O4 Mn2 O4 180.0 . 3_656 ? C7 O1 Mn1 128.15(19) . 4_566 ? C9 O2 Mn1 145.66(18) . 2 ? C9 O3 Mn2 133.00(16) . . ? C9 O3 Mn1 122.62(16) . . ? Mn2 O3 Mn1 97.88(7) . . ? C8 O4 Mn2 130.95(16) . . ? C8 O4 Mn1 94.09(15) . 4_666 ? Mn2 O4 Mn1 130.53(8) . 4_666 ? C8 O5 Mn1 133.66(17) . 3_666 ? C8 O5 Mn1 91.79(16) . 4_666 ? Mn1 O5 Mn1 112.28(8) 3_666 4_666 ? C7 O6 Mn2 133.14(19) . 2_556 ? C2 C1 C6 119.3(2) . . ? C2 C1 C7 118.9(2) . . ? C6 C1 C7 121.8(2) . . ? C3 C2 C1 119.8(2) . . ? C2 C3 C4 121.7(2) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 C8 113.0(2) . . ? C5 C4 C8 128.0(2) . . ? C6 C5 C4 118.4(2) . . ? C6 C5 C9 116.1(2) . . ? C4 C5 C9 125.4(2) . . ? C1 C6 C5 121.7(2) . . ? O6 C7 O1 125.1(3) . . ? O6 C7 C1 116.0(2) . . ? O1 C7 C1 118.9(2) . . ? O5 C8 O4 118.9(2) . . ? O5 C8 C4 119.0(2) . . ? O4 C8 C4 121.7(2) . . ? O2 C9 O3 123.9(2) . . ? O2 C9 C5 115.3(2) . . ? O3 C9 C5 120.8(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.593 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.089