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 _publ_section_title ;Synthesis, structure and magnetic properties of an amine-templated Mn2+ (S = 5/2) sulfate with the Kagome structure ; loop_ _publ_author_name C.N.R.Rao J.N.Behera _publ_contact_author_name 'Prof. C.N.R.Rao' _publ_contact_author_email CNRRAO@JNCASR.AC.IN # Attachment 'Compound I.cif' data_try _database_code_depnum_ccdc_archive 'CCDC 621801' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H20 F6 Mn3 N4 O8 S2' _chemical_formula_weight 595.20 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6128(2) _cell_length_b 7.60040(10) _cell_length_c 13.05010(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.8680(10) _cell_angle_gamma 90.00 _cell_volume 1688.45(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 25.68 _exptl_crystal_description Hexagonal _exptl_crystal_colour White _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 2.566 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.617010 _exptl_absorpt_correction_T_max 0.814000 _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 18444 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3197 _reflns_number_gt 2637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0367P)^2^+6.0435P] 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 3197 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _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 0.25325(3) 0.49993(7) 0.77793(4) 0.01134(15) Uani 1 1 d . . . Mn2 Mn 0.24534(3) 0.22457(7) 1.01912(4) 0.01086(14) Uani 1 1 d . . . Mn3 Mn 0.25086(3) -0.26879(7) 1.02816(4) 0.01098(15) Uani 1 1 d . . . S1 S 0.39847(5) -0.01566(11) 1.15702(7) 0.0119(2) Uani 1 1 d . . . S2 S 0.10182(5) 0.48749(11) 0.89402(6) 0.0122(2) Uani 1 1 d . . . F1 F 0.28296(12) 0.2840(3) 0.88160(15) 0.0193(5) Uani 1 1 d . . . F2 F 0.22180(12) 0.7128(3) 0.67166(15) 0.0175(4) Uani 1 1 d . . . F3 F 0.20547(12) 0.3191(3) 0.65567(15) 0.0204(5) Uani 1 1 d . . . F4 F 0.29730(12) 0.6886(3) 0.89749(15) 0.0192(5) Uani 1 1 d . . . O1 O 0.13683(16) 0.5231(4) 0.8063(2) 0.0285(7) Uani 1 1 d . . . O2 O 0.37413(15) 0.0300(4) 1.2546(2) 0.0232(6) Uani 1 1 d . . . F5 F 0.28247(12) 0.4738(3) 1.08665(16) 0.0174(5) Uani 1 1 d . . . F6 F 0.20659(13) -0.0280(3) 0.95732(16) 0.0192(5) Uani 1 1 d . . . O3 O 0.36140(15) 0.1055(4) 1.0716(2) 0.0254(6) Uani 1 1 d . . . O4 O 0.12523(15) 0.3101(4) 0.9371(2) 0.0244(6) Uani 1 1 d . . . O5 O 0.13027(15) 0.6182(4) 0.9790(2) 0.0250(6) Uani 1 1 d . . . O6 O 0.37166(14) -0.1967(3) 1.1249(2) 0.0212(6) Uani 1 1 d . . . O7 O 0.48401(14) -0.0068(3) 1.1786(2) 0.0198(6) Uani 1 1 d . . . O8 O 0.01585(14) 0.4978(3) 0.8596(2) 0.0189(6) Uani 1 1 d . . . N1 N 0.1543(2) 0.0086(5) 0.7355(3) 0.0207(7) Uani 1 1 d . . . N2 N 0.3459(2) -0.0054(5) 0.8038(3) 0.0217(7) Uani 1 1 d . . . C1 C -0.0405(2) 0.0970(5) 0.9056(3) 0.0232(9) Uani 1 1 d . . . H9 H -0.0384 0.1711 0.8459 0.028 Uiso 1 1 calc R . . H10 H -0.0952 0.0757 0.9032 0.028 Uiso 1 1 calc R . . N3 N 0.0006(2) -0.0752(6) 0.8990(3) 0.0400(10) Uani 1 1 d . . . H11 H -0.0242 -0.1327 0.8395 0.048 Uiso 1 1 calc R . . H12 H 0.0503 -0.0545 0.8962 0.048 Uiso 1 1 calc R . . C2 C 0.0009(2) -0.1863(5) 0.9935(2) 0.0111(7) Uani 1 1 d . . . H13 H -0.0528 -0.2136 0.9939 0.013 Uiso 1 1 calc R . . H14 H 0.0276 -0.2963 0.9883 0.013 Uiso 1 1 calc R . . C3 C 0.5035(2) -0.6877(5) 1.0128(3) 0.0215(8) Uani 1 1 d . . . H15 H 0.5553 -0.7044 1.0602 0.026 Uiso 1 1 calc R . . H16 H 0.4791 -0.8024 0.9969 0.026 Uiso 1 1 calc R . . N4 N 0.4544(2) -0.5748(5) 1.0666(3) 0.0378(9) Uani 1 1 d . . . H17 H 0.4051 -0.5668 1.0251 0.045 Uiso 1 1 calc R . . H18 H 0.4522 -0.6247 1.1284 0.045 Uiso 1 1 calc R . . C4 C 0.48922(19) -0.3971(4) 1.0867(2) 0.0080(6) Uani 1 1 d . . . H19 H 0.5408 -0.4057 1.1358 0.010 Uiso 1 1 calc R . . H20 H 0.4566 -0.3245 1.1193 0.010 Uiso 1 1 calc R . . H1 H 0.170(3) 0.001(6) 0.804(4) 0.037(14) Uiso 1 1 d . . . H2 H 0.174(2) -0.090(6) 0.712(3) 0.020(11) Uiso 1 1 d . . . H3 H 0.100(3) 0.012(6) 0.710(4) 0.045(15) Uiso 1 1 d . . . H4 H 0.172(2) 0.116(6) 0.714(3) 0.020(11) Uiso 1 1 d . . . H5 H 0.394(3) -0.007(6) 0.815(4) 0.039(15) Uiso 1 1 d . . . H6 H 0.329(3) 0.085(7) 0.833(4) 0.030(13) Uiso 1 1 d . . . H7 H 0.324(3) 0.007(6) 0.738(4) 0.027(13) Uiso 1 1 d . . . H8 H 0.328(3) -0.111(8) 0.832(4) 0.060(17) Uiso 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 0.0136(3) 0.0104(3) 0.0103(3) 0.00085(19) 0.0035(2) 0.0007(2) Mn2 0.0130(3) 0.0088(3) 0.0110(3) 0.0008(2) 0.0034(2) 0.0005(2) Mn3 0.0131(3) 0.0092(3) 0.0107(3) -0.0002(2) 0.0032(2) 0.0002(2) S1 0.0093(4) 0.0126(5) 0.0137(4) -0.0007(3) 0.0027(3) 0.0000(3) S2 0.0091(4) 0.0131(5) 0.0140(4) 0.0009(3) 0.0020(3) 0.0004(3) F1 0.0269(11) 0.0174(12) 0.0158(10) 0.0059(9) 0.0095(9) 0.0058(9) F2 0.0213(11) 0.0169(11) 0.0154(10) 0.0066(8) 0.0068(8) 0.0038(9) F3 0.0281(12) 0.0186(12) 0.0174(10) -0.0060(9) 0.0113(9) -0.0041(9) F4 0.0231(11) 0.0203(12) 0.0161(10) -0.0053(9) 0.0083(9) -0.0034(9) O1 0.0187(14) 0.048(2) 0.0216(14) 0.0106(13) 0.0098(11) 0.0057(13) O2 0.0156(13) 0.0360(17) 0.0193(13) -0.0107(12) 0.0070(11) -0.0046(12) F5 0.0199(11) 0.0096(11) 0.0210(10) -0.0008(8) 0.0021(9) 0.0009(8) F6 0.0245(11) 0.0096(11) 0.0201(10) 0.0005(8) -0.0008(9) 0.0019(9) O3 0.0172(14) 0.0286(17) 0.0301(15) 0.0139(13) 0.0057(11) 0.0043(12) O4 0.0164(13) 0.0150(15) 0.0394(16) 0.0073(12) 0.0028(12) 0.0023(11) O5 0.0161(13) 0.0246(16) 0.0314(15) -0.0128(13) 0.0009(11) -0.0021(12) O6 0.0147(13) 0.0159(15) 0.0323(14) -0.0078(12) 0.0048(11) -0.0015(11) O7 0.0100(12) 0.0258(16) 0.0232(13) 0.0007(11) 0.0037(10) -0.0008(11) O8 0.0090(12) 0.0191(15) 0.0267(14) 0.0006(11) 0.0012(10) 0.0012(10) N1 0.0162(18) 0.023(2) 0.0220(18) -0.0002(15) 0.0040(14) 0.0001(15) N2 0.0171(18) 0.023(2) 0.0240(19) -0.0029(16) 0.0041(15) 0.0009(16) C1 0.024(2) 0.022(2) 0.0215(18) 0.0026(16) 0.0019(16) 0.0029(17) N3 0.051(3) 0.037(2) 0.034(2) -0.0005(18) 0.0136(19) 0.004(2) C2 0.0178(17) 0.0021(16) 0.0157(16) -0.0010(13) 0.0087(13) 0.0018(13) C3 0.026(2) 0.019(2) 0.0214(18) 0.0013(16) 0.0080(16) 0.0015(17) N4 0.036(2) 0.041(2) 0.038(2) 0.0036(18) 0.0115(17) -0.0027(19) C4 0.0092(15) 0.0047(16) 0.0100(14) -0.0010(12) 0.0021(12) 0.0023(13) _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 F1 2.106(2) . ? Mn1 F2 2.111(2) . ? Mn1 F3 2.111(2) . ? Mn1 F4 2.115(2) . ? Mn1 O1 2.182(3) . ? Mn1 O2 2.238(3) 4_565 ? Mn2 F3 2.103(2) 4_566 ? Mn2 F1 2.115(2) . ? Mn2 F5 2.120(2) . ? Mn2 F6 2.126(2) . ? Mn2 O3 2.179(3) . ? Mn2 O4 2.210(3) . ? Mn3 F4 2.097(2) 1_545 ? Mn3 F6 2.108(2) . ? Mn3 F2 2.108(2) 4_566 ? Mn3 F5 2.122(2) 1_545 ? Mn3 O5 2.227(3) 1_545 ? Mn3 O6 2.246(2) . ? S1 O7 1.461(3) . ? S1 O3 1.464(3) . ? S1 O6 1.480(3) . ? S1 O2 1.485(3) . ? S2 O1 1.458(3) . ? S2 O8 1.467(3) . ? S2 O5 1.477(3) . ? S2 O4 1.478(3) . ? F2 Mn3 2.108(2) 4_565 ? F3 Mn2 2.103(2) 4_565 ? F4 Mn3 2.097(2) 1_565 ? O2 Mn1 2.238(3) 4_566 ? F5 Mn3 2.122(2) 1_565 ? O5 Mn3 2.227(3) 1_565 ? N1 H1 0.86(6) . ? N1 H2 0.91(5) . ? N1 H3 0.93(6) . ? N1 H4 0.94(5) . ? N2 H5 0.83(6) . ? N2 H6 0.88(5) . ? N2 H7 0.85(5) . ? N2 H8 0.97(6) . ? C1 C2 1.487(5) 3_557 ? C1 N3 1.509(6) . ? C1 H9 0.9700 . ? C1 H10 0.9700 . ? N3 C2 1.493(5) . ? N3 H11 0.9000 . ? N3 H12 0.9000 . ? C2 C1 1.487(5) 3_557 ? C2 H13 0.9700 . ? C2 H14 0.9700 . ? C3 C4 1.485(5) 3_647 ? C3 N4 1.513(5) . ? C3 H15 0.9700 . ? C3 H16 0.9700 . ? N4 C4 1.479(5) . ? N4 H17 0.9000 . ? N4 H18 0.9000 . ? C4 C3 1.485(5) 3_647 ? C4 H19 0.9700 . ? C4 H20 0.9700 . ? 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 F1 Mn1 F2 178.76(9) . . ? F1 Mn1 F3 87.89(9) . . ? F2 Mn1 F3 90.93(8) . . ? F1 Mn1 F4 94.06(8) . . ? F2 Mn1 F4 87.12(8) . . ? F3 Mn1 F4 177.59(9) . . ? F1 Mn1 O1 92.49(10) . . ? F2 Mn1 O1 87.12(9) . . ? F3 Mn1 O1 88.34(10) . . ? F4 Mn1 O1 90.17(10) . . ? F1 Mn1 O2 85.41(9) . 4_565 ? F2 Mn1 O2 94.99(9) . 4_565 ? F3 Mn1 O2 92.26(9) . 4_565 ? F4 Mn1 O2 89.30(9) . 4_565 ? O1 Mn1 O2 177.79(10) . 4_565 ? F3 Mn2 F1 176.59(8) 4_566 . ? F3 Mn2 F5 85.59(8) 4_566 . ? F1 Mn2 F5 91.80(9) . . ? F3 Mn2 F6 91.99(9) 4_566 . ? F1 Mn2 F6 90.62(9) . . ? F5 Mn2 F6 177.57(8) . . ? F3 Mn2 O3 99.11(9) 4_566 . ? F1 Mn2 O3 83.27(9) . . ? F5 Mn2 O3 94.36(10) . . ? F6 Mn2 O3 85.88(10) . . ? F3 Mn2 O4 88.32(10) 4_566 . ? F1 Mn2 O4 89.73(9) . . ? F5 Mn2 O4 95.35(9) . . ? F6 Mn2 O4 84.71(9) . . ? O3 Mn2 O4 168.20(11) . . ? F4 Mn3 F6 87.42(9) 1_545 . ? F4 Mn3 F2 171.13(8) 1_545 4_566 ? F6 Mn3 F2 93.88(9) . 4_566 ? F4 Mn3 F5 91.66(9) 1_545 1_545 ? F6 Mn3 F5 172.67(8) . 1_545 ? F2 Mn3 F5 88.14(8) 4_566 1_545 ? F4 Mn3 O5 104.36(9) 1_545 1_545 ? F6 Mn3 O5 89.45(10) . 1_545 ? F2 Mn3 O5 84.43(9) 4_566 1_545 ? F5 Mn3 O5 83.73(9) 1_545 1_545 ? F4 Mn3 O6 89.08(9) 1_545 . ? F6 Mn3 O6 103.02(9) . . ? F2 Mn3 O6 82.08(9) 4_566 . ? F5 Mn3 O6 84.23(9) 1_545 . ? O5 Mn3 O6 162.17(11) 1_545 . ? O7 S1 O3 110.76(16) . . ? O7 S1 O6 109.61(15) . . ? O3 S1 O6 108.77(16) . . ? O7 S1 O2 109.51(15) . . ? O3 S1 O2 109.57(16) . . ? O6 S1 O2 108.59(16) . . ? O1 S2 O8 111.17(16) . . ? O1 S2 O5 109.51(17) . . ? O8 S2 O5 108.58(15) . . ? O1 S2 O4 109.57(17) . . ? O8 S2 O4 109.28(15) . . ? O5 S2 O4 108.69(16) . . ? Mn1 F1 Mn2 129.15(10) . . ? Mn3 F2 Mn1 130.99(10) 4_565 . ? Mn2 F3 Mn1 126.04(10) 4_565 . ? Mn3 F4 Mn1 123.99(10) 1_565 . ? S2 O1 Mn1 136.31(17) . . ? S1 O2 Mn1 125.93(15) . 4_566 ? Mn2 F5 Mn3 130.52(10) . 1_565 ? Mn3 F6 Mn2 124.83(10) . . ? S1 O3 Mn2 134.42(16) . . ? S2 O4 Mn2 126.28(15) . . ? S2 O5 Mn3 126.19(16) . 1_565 ? S1 O6 Mn3 124.99(15) . . ? H1 N1 H2 104(4) . . ? H1 N1 H3 114(5) . . ? H2 N1 H3 110(4) . . ? H1 N1 H4 109(4) . . ? H2 N1 H4 116(4) . . ? H3 N1 H4 105(4) . . ? H5 N2 H6 113(5) . . ? H5 N2 H7 111(5) . . ? H6 N2 H7 104(4) . . ? H5 N2 H8 110(5) . . ? H6 N2 H8 107(5) . . ? H7 N2 H8 112(4) . . ? C2 C1 N3 108.9(3) 3_557 . ? C2 C1 H9 109.9 3_557 . ? N3 C1 H9 109.9 . . ? C2 C1 H10 109.9 3_557 . ? N3 C1 H10 109.9 . . ? H9 C1 H10 108.3 . . ? C2 N3 C1 110.1(3) . . ? C2 N3 H11 109.6 . . ? C1 N3 H11 109.6 . . ? C2 N3 H12 109.6 . . ? C1 N3 H12 109.6 . . ? H11 N3 H12 108.1 . . ? C1 C2 N3 112.0(3) 3_557 . ? C1 C2 H13 109.2 3_557 . ? N3 C2 H13 109.2 . . ? C1 C2 H14 109.2 3_557 . ? N3 C2 H14 109.2 . . ? H13 C2 H14 107.9 . . ? C4 C3 N4 110.4(3) 3_647 . ? C4 C3 H15 109.6 3_647 . ? N4 C3 H15 109.6 . . ? C4 C3 H16 109.6 3_647 . ? N4 C3 H16 109.6 . . ? H15 C3 H16 108.1 . . ? C4 N4 C3 109.8(3) . . ? C4 N4 H17 109.7 . . ? C3 N4 H17 109.7 . . ? C4 N4 H18 109.7 . . ? C3 N4 H18 109.7 . . ? H17 N4 H18 108.2 . . ? N4 C4 C3 111.5(3) . 3_647 ? N4 C4 H19 109.3 . . ? C3 C4 H19 109.3 3_647 . ? N4 C4 H20 109.3 . . ? C3 C4 H20 109.3 3_647 . ? H19 C4 H20 108.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.739 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.102