# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email WZM@CHEM.PKU.EDU.CN _publ_contact_author_name 'Prof Zheming Wang' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_method SHELXL-97 _publ_contact_author_address ; College of Chemistry Peking University Beijing 100871 CHINA ; _publ_section_title ; Mn3(HCOO)6: a 3D porous magnet of diamond framework with nodes of Mn-centered MnMn4 tetrahedron and guest-modulated ordering temperature ; loop_ _publ_author_name 'Zheming Wang' 'Hideki Fujiwara' 'Hayao Kobayashi' 'Mohamedally Kurmoo' 'Bin Zhang' data_1 _database_code_depnum_ccdc_archive 'CCDC 210639' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)6][CH3OH][H2O] _chemical_formula_sum 'C7 H12 Mn3 O14' _chemical_formula_weight 484.99 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 2(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 11.6495(11) _cell_length_b 10.1279(11) _cell_length_c 18.6135(15) _cell_angle_alpha 90.00 _cell_angle_beta 127.056(3) _cell_angle_gamma 90.00 _cell_volume 1752.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 11774 _cell_measurement_theta_min 3.0222 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 2.192 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8621 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28835 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3950 _reflns_number_gt 3251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0507P)^2^+0.0320P] 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 3950 _refine_ls_number_parameters 245 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _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 0.37432(3) 0.08441(3) 0.131153(19) 0.01478(10) Uani 1 1 d . . . Mn2 Mn 0.57553(3) -0.10029(3) 0.31508(2) 0.01689(10) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.01871(12) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.02111(13) Uani 1 2 d S . . O1 O 0.43917(16) 0.20728(14) 0.24728(9) 0.0196(3) Uani 1 1 d . . . O2 O 0.55274(19) 0.07452(16) 0.36767(10) 0.0273(4) Uani 1 1 d . . . O3 O 0.59193(16) 0.00050(14) 0.21930(10) 0.0190(3) Uani 1 1 d . . . O4 O 0.68006(18) 0.00373(18) 0.14175(11) 0.0321(4) Uani 1 1 d . . . O5 O 0.45245(16) 0.26268(15) 0.10609(9) 0.0194(3) Uani 1 1 d . . . O6 O 0.48175(19) 0.21092(17) 0.00144(10) 0.0296(4) Uani 1 1 d . . . O7 O 0.34591(16) -0.07601(15) 0.19747(9) 0.0202(3) Uani 1 1 d . . . O8 O 0.11091(19) -0.10724(19) 0.12488(11) 0.0367(5) Uani 1 1 d . . . O9 O 0.33469(16) -0.02882(15) 0.02115(9) 0.0209(3) Uani 1 1 d . . . O10 O 0.11621(19) -0.10695(17) -0.03739(12) 0.0330(4) Uani 1 1 d . . . O11 O 0.15904(16) 0.16232(15) 0.05982(10) 0.0212(3) Uani 1 1 d . . . O12 O 0.19788(17) 0.37827(16) 0.09046(10) 0.0267(4) Uani 1 1 d . . . C1 C 0.4980(3) 0.1814(2) 0.32915(14) 0.0245(5) Uani 1 1 d . . . H1 H 0.5007 0.2506 0.3646 0.029 Uiso 1 1 calc R . . C2 C 0.6925(3) -0.0073(2) 0.21150(15) 0.0243(5) Uani 1 1 d . . . H2 H 0.7865 -0.0234 0.2650 0.029 Uiso 1 1 calc R . . C3 C 0.4753(3) 0.2907(2) 0.04908(15) 0.0251(5) Uani 1 1 d . . . H3 H 0.4886 0.3812 0.0426 0.030 Uiso 1 1 calc R . . C4 C 0.2377(3) -0.1274(3) 0.18717(15) 0.0297(6) Uani 1 1 d . . . H4 H 0.2568 -0.1877 0.2323 0.036 Uiso 1 1 calc R . . C5 C 0.2254(3) -0.1017(2) -0.03191(15) 0.0261(5) Uani 1 1 d . . . H5 H 0.2299 -0.1576 -0.0712 0.031 Uiso 1 1 calc R . . C6 C 0.1194(3) 0.2816(2) 0.05222(15) 0.0257(5) Uani 1 1 d . . . H6 H 0.0188 0.2979 0.0130 0.031 Uiso 1 1 calc R . . O22 O 0.1865(18) -0.4472(11) -0.0864(7) 0.209(8) Uani 0.50 1 d PD . . C22 C 0.2116(17) -0.430(2) -0.1491(9) 0.198(10) Uani 0.50 1 d PD . . O23 O -0.1124(13) -0.1765(17) -0.2449(8) 0.225(6) Uani 0.50 1 d PD . . C23 C -0.020(3) -0.224(4) -0.2652(16) 0.39(4) Uani 0.50 1 d PD . . O101 O 0.101(3) -0.409(3) -0.1763(17) 0.175(9) Uiso 0.25 1 d P . . O102 O -0.073(5) -0.181(5) -0.342(3) 0.293(19) Uiso 0.25 1 d P . . O103 O -0.062(5) -0.256(5) -0.289(4) 0.24(2) Uiso 0.25 1 d P . . O104 O 0.152(4) -0.530(5) -0.110(2) 0.244(17) Uiso 0.25 1 d P . . 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 0.01472(18) 0.01445(18) 0.01490(16) -0.00099(11) 0.00879(14) -0.00067(12) Mn2 0.0185(2) 0.01449(19) 0.01723(17) 0.00203(11) 0.01056(14) 0.00154(12) Mn3 0.0189(3) 0.0228(3) 0.0198(2) -0.00304(17) 0.0145(2) -0.00234(19) Mn4 0.0138(3) 0.0230(3) 0.0237(2) -0.00398(18) 0.0098(2) -0.00456(19) O1 0.0267(9) 0.0156(8) 0.0172(7) -0.0001(6) 0.0136(6) -0.0004(6) O2 0.0382(11) 0.0207(9) 0.0216(8) 0.0025(6) 0.0173(8) 0.0064(7) O3 0.0184(8) 0.0205(9) 0.0216(7) 0.0043(6) 0.0140(6) 0.0017(6) O4 0.0221(9) 0.0561(13) 0.0211(8) -0.0006(7) 0.0146(7) -0.0008(8) O5 0.0258(9) 0.0164(8) 0.0227(7) -0.0017(6) 0.0181(7) -0.0023(6) O6 0.0462(11) 0.0243(9) 0.0347(9) -0.0008(7) 0.0331(9) 0.0000(8) O7 0.0170(8) 0.0199(9) 0.0226(7) 0.0027(6) 0.0113(7) -0.0010(6) O8 0.0176(10) 0.0504(13) 0.0326(9) 0.0100(8) 0.0100(8) -0.0062(8) O9 0.0190(8) 0.0262(9) 0.0214(7) -0.0081(6) 0.0142(7) -0.0059(7) O10 0.0223(10) 0.0369(11) 0.0452(10) -0.0132(8) 0.0231(8) -0.0091(8) O11 0.0152(8) 0.0184(9) 0.0260(8) -0.0038(6) 0.0103(6) -0.0016(6) O12 0.0202(9) 0.0196(9) 0.0300(8) -0.0035(6) 0.0097(7) -0.0014(7) C1 0.0332(14) 0.0189(12) 0.0221(11) -0.0024(9) 0.0171(10) 0.0004(10) C2 0.0169(12) 0.0310(14) 0.0221(11) 0.0012(9) 0.0103(9) 0.0013(9) C3 0.0373(14) 0.0152(12) 0.0318(12) 0.0001(9) 0.0256(11) -0.0022(10) C4 0.0225(14) 0.0339(15) 0.0271(12) 0.0071(10) 0.0121(11) -0.0060(11) C5 0.0280(14) 0.0286(14) 0.0269(12) -0.0117(9) 0.0193(11) -0.0082(10) C6 0.0153(12) 0.0261(14) 0.0284(11) -0.0022(9) 0.0093(9) 0.0000(10) O22 0.36(2) 0.087(7) 0.118(7) 0.019(6) 0.113(10) 0.030(10) C22 0.109(11) 0.40(3) 0.092(9) -0.098(13) 0.065(8) -0.149(15) O23 0.160(11) 0.338(19) 0.141(9) -0.071(10) 0.071(8) -0.091(12) C23 0.69(8) 0.43(5) 0.26(3) -0.22(3) 0.40(5) -0.30(5) _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. The solvents were treated as two positions (occupacy 0.50) for one methanol and four positions (occupancy 0.25) for one water per unique unit. Hydrogen atoms of solvents were not added in structure refinement. ; 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 O9 2.1404(14) . ? Mn1 O11 2.1592(15) . ? Mn1 O7 2.1830(14) . ? Mn1 O5 2.1948(15) . ? Mn1 O1 2.1962(14) . ? Mn1 O3 2.1972(15) . ? Mn2 O2 2.1158(16) . ? Mn2 O12 2.1244(16) 2_645 ? Mn2 O3 2.1605(14) . ? Mn2 O5 2.1820(14) 2_645 ? Mn2 O1 2.2216(15) 2_645 ? Mn2 O7 2.2251(16) . ? Mn3 O6 2.1485(18) . ? Mn3 O6 2.1485(18) 3_655 ? Mn3 O4 2.1663(16) 3_655 ? Mn3 O4 2.1663(16) . ? Mn3 O9 2.2052(14) . ? Mn3 O9 2.2052(14) 3_655 ? Mn4 O10 2.1507(16) . ? Mn4 O10 2.1507(16) 3 ? Mn4 O8 2.1524(17) 3 ? Mn4 O8 2.1524(17) . ? Mn4 O11 2.2111(15) . ? Mn4 O11 2.2111(15) 3 ? O1 C1 1.265(2) . ? O1 Mn2 2.2216(15) 2_655 ? O2 C1 1.242(3) . ? O3 C2 1.267(3) . ? O4 C2 1.221(3) . ? O5 C3 1.272(3) . ? O5 Mn2 2.1820(14) 2_655 ? O6 C3 1.235(3) . ? O7 C4 1.267(3) . ? O8 C4 1.226(3) . ? O9 C5 1.275(3) . ? O10 C5 1.215(3) . ? O11 C6 1.270(3) . ? O12 C6 1.231(3) . ? O12 Mn2 2.1244(16) 2_655 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O22 C22 1.375(14) . ? O23 C23 1.424(19) . ? 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 O9 Mn1 O11 96.11(6) . . ? O9 Mn1 O7 97.08(6) . . ? O11 Mn1 O7 95.97(6) . . ? O9 Mn1 O5 96.63(5) . . ? O11 Mn1 O5 92.60(6) . . ? O7 Mn1 O5 162.94(5) . . ? O9 Mn1 O1 173.24(6) . . ? O11 Mn1 O1 88.93(6) . . ? O7 Mn1 O1 86.83(5) . . ? O5 Mn1 O1 78.60(5) . . ? O9 Mn1 O3 89.65(6) . . ? O11 Mn1 O3 172.07(5) . . ? O7 Mn1 O3 77.86(6) . . ? O5 Mn1 O3 92.14(6) . . ? O1 Mn1 O3 85.78(6) . . ? O2 Mn2 O12 98.18(7) . 2_645 ? O2 Mn2 O3 94.85(6) . . ? O12 Mn2 O3 92.73(6) 2_645 . ? O2 Mn2 O5 96.31(6) . 2_645 ? O12 Mn2 O5 89.60(6) 2_645 2_645 ? O3 Mn2 O5 168.16(6) . 2_645 ? O2 Mn2 O1 169.80(7) . 2_645 ? O12 Mn2 O1 90.51(6) 2_645 2_645 ? O3 Mn2 O1 90.04(5) . 2_645 ? O5 Mn2 O1 78.33(5) 2_645 2_645 ? O2 Mn2 O7 87.20(6) . . ? O12 Mn2 O7 169.47(6) 2_645 . ? O3 Mn2 O7 77.73(6) . . ? O5 Mn2 O7 98.84(6) 2_645 . ? O1 Mn2 O7 85.09(6) 2_645 . ? O6 Mn3 O6 180.00(10) . 3_655 ? O6 Mn3 O4 90.12(6) . 3_655 ? O6 Mn3 O4 89.88(6) 3_655 3_655 ? O6 Mn3 O4 89.88(6) . . ? O6 Mn3 O4 90.12(6) 3_655 . ? O4 Mn3 O4 180.00(8) 3_655 . ? O6 Mn3 O9 91.48(6) . . ? O6 Mn3 O9 88.52(6) 3_655 . ? O4 Mn3 O9 84.63(6) 3_655 . ? O4 Mn3 O9 95.37(6) . . ? O6 Mn3 O9 88.52(6) . 3_655 ? O6 Mn3 O9 91.48(6) 3_655 3_655 ? O4 Mn3 O9 95.37(6) 3_655 3_655 ? O4 Mn3 O9 84.63(6) . 3_655 ? O9 Mn3 O9 180.00(11) . 3_655 ? O10 Mn4 O10 180.00(6) . 3 ? O10 Mn4 O8 89.42(7) . 3 ? O10 Mn4 O8 90.58(7) 3 3 ? O10 Mn4 O8 90.58(7) . . ? O10 Mn4 O8 89.42(7) 3 . ? O8 Mn4 O8 180.00(12) 3 . ? O10 Mn4 O11 92.15(6) . . ? O10 Mn4 O11 87.85(6) 3 . ? O8 Mn4 O11 86.80(6) 3 . ? O8 Mn4 O11 93.20(6) . . ? O10 Mn4 O11 87.85(6) . 3 ? O10 Mn4 O11 92.15(6) 3 3 ? O8 Mn4 O11 93.20(6) 3 3 ? O8 Mn4 O11 86.80(6) . 3 ? O11 Mn4 O11 180.0 . 3 ? C1 O1 Mn1 133.11(14) . . ? C1 O1 Mn2 128.74(14) . 2_655 ? Mn1 O1 Mn2 96.33(5) . 2_655 ? C1 O2 Mn2 128.78(14) . . ? C2 O3 Mn2 127.78(14) . . ? C2 O3 Mn1 132.00(14) . . ? Mn2 O3 Mn1 99.38(6) . . ? C2 O4 Mn3 134.48(16) . . ? C3 O5 Mn2 127.63(14) . 2_655 ? C3 O5 Mn1 133.05(14) . . ? Mn2 O5 Mn1 97.54(5) 2_655 . ? C3 O6 Mn3 135.11(15) . . ? C4 O7 Mn1 134.13(15) . . ? C4 O7 Mn2 126.87(14) . . ? Mn1 O7 Mn2 97.85(6) . . ? C4 O8 Mn4 134.60(16) . . ? C5 O9 Mn1 126.20(14) . . ? C5 O9 Mn3 120.65(13) . . ? Mn1 O9 Mn3 113.06(7) . . ? C5 O10 Mn4 141.48(16) . . ? C6 O11 Mn1 128.71(14) . . ? C6 O11 Mn4 120.87(14) . . ? Mn1 O11 Mn4 110.38(7) . . ? C6 O12 Mn2 132.76(15) . 2_655 ? O2 C1 O1 126.4(2) . . ? O2 C1 H1 116.8 . . ? O1 C1 H1 116.8 . . ? O4 C2 O3 126.2(2) . . ? O4 C2 H2 116.9 . . ? O3 C2 H2 116.9 . . ? O6 C3 O5 126.0(2) . . ? O6 C3 H3 117.0 . . ? O5 C3 H3 117.0 . . ? O8 C4 O7 126.6(2) . . ? O8 C4 H4 116.7 . . ? O7 C4 H4 116.7 . . ? O10 C5 O9 126.6(2) . . ? O10 C5 H5 116.7 . . ? O9 C5 H5 116.7 . . ? O12 C6 O11 126.8(2) . . ? O12 C6 H6 116.6 . . ? O11 C6 H6 116.6 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.657 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.080 ## END of data_1 data_2 _database_code_depnum_ccdc_archive 'CCDC 210640' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)6] _chemical_formula_sum 'C6 H6 Mn3 O12' _chemical_formula_weight 434.93 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 2(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 11.7293(13) _cell_length_b 10.1923(11) _cell_length_c 18.7417(18) _cell_angle_alpha 90.00 _cell_angle_beta 127.178(3) _cell_angle_gamma 90.00 _cell_volume 1785.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 8995 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 2.134 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8678 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 29323 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4068 _reflns_number_gt 3043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4068 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0622 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _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 0.37402(3) 0.07946(3) 0.13103(2) 0.01420(10) Uani 1 1 d . . . Mn2 Mn 0.57349(3) -0.10669(3) 0.31325(2) 0.01633(10) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.01874(12) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.01954(13) Uani 1 2 d S . . O1 O 0.44272(14) 0.20093(14) 0.24796(10) 0.0187(3) Uani 1 1 d . . . O2 O 0.54968(16) 0.06624(15) 0.36606(11) 0.0258(4) Uani 1 1 d . . . O3 O 0.59009(14) -0.00669(14) 0.21803(10) 0.0183(3) Uani 1 1 d . . . O4 O 0.67779(16) 0.00309(17) 0.14110(11) 0.0307(4) Uani 1 1 d . . . O5 O 0.45256(15) 0.25796(14) 0.10686(10) 0.0189(3) Uani 1 1 d . . . O6 O 0.48107(18) 0.21084(16) 0.00195(12) 0.0294(4) Uani 1 1 d . . . O7 O 0.34538(14) -0.08110(14) 0.19631(10) 0.0189(3) Uani 1 1 d . . . O8 O 0.11038(15) -0.10977(17) 0.12284(12) 0.0324(4) Uani 1 1 d . . . O9 O 0.33525(14) -0.02887(15) 0.02050(10) 0.0200(3) Uani 1 1 d . . . O10 O 0.11822(16) -0.10612(16) -0.03521(12) 0.0287(4) Uani 1 1 d . . . O11 O 0.16067(14) 0.15884(14) 0.06136(10) 0.0205(3) Uani 1 1 d . . . O12 O 0.20088(15) 0.37288(15) 0.09375(11) 0.0259(4) Uani 1 1 d . . . C1 C 0.5001(2) 0.1737(2) 0.32922(16) 0.0226(5) Uani 1 1 d . . . C2 C 0.6893(2) -0.0128(2) 0.20992(17) 0.0238(5) Uani 1 1 d . . . C3 C 0.4704(3) 0.2874(2) 0.04858(17) 0.0255(6) Uani 1 1 d . . . C4 C 0.2365(2) -0.1329(3) 0.18452(18) 0.0280(6) Uani 1 1 d . . . C5 C 0.2252(2) -0.1005(2) -0.03206(17) 0.0234(5) Uani 1 1 d . . . C6 C 0.1213(2) 0.2772(2) 0.05467(17) 0.0242(5) Uani 1 1 d . . . H1 H 0.501(2) 0.245(2) 0.3648(18) 0.031(7) Uiso 1 1 d . . . H2 H 0.779(2) -0.034(2) 0.2637(17) 0.028(7) Uiso 1 1 d . . . H3 H 0.477(2) 0.376(2) 0.0413(16) 0.028(7) Uiso 1 1 d . . . H4 H 0.259(2) -0.200(3) 0.2280(18) 0.034(7) Uiso 1 1 d . . . H5 H 0.226(2) -0.156(2) -0.0739(17) 0.029(6) Uiso 1 1 d . . . H6 H 0.014(2) 0.297(2) 0.0106(17) 0.028(6) 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 0.01386(16) 0.01429(18) 0.01431(19) -0.00071(14) 0.00844(14) -0.00049(12) Mn2 0.01764(17) 0.01412(18) 0.0166(2) 0.00210(14) 0.01004(15) 0.00160(13) Mn3 0.0191(2) 0.0229(3) 0.0201(3) -0.0033(2) 0.0149(2) -0.00242(19) Mn4 0.0131(2) 0.0213(3) 0.0219(3) -0.0034(2) 0.0094(2) -0.00407(19) O1 0.0248(8) 0.0152(8) 0.0152(9) -0.0021(7) 0.0116(7) -0.0008(6) O2 0.0355(9) 0.0190(9) 0.0192(9) 0.0027(7) 0.0146(8) 0.0072(7) O3 0.0168(7) 0.0198(8) 0.0203(9) 0.0040(7) 0.0122(7) 0.0022(6) O4 0.0234(8) 0.0516(12) 0.0212(10) 0.0006(9) 0.0157(8) -0.0003(8) O5 0.0261(8) 0.0153(8) 0.0217(9) -0.0018(7) 0.0179(8) -0.0026(6) O6 0.0462(10) 0.0243(9) 0.0348(11) -0.0017(8) 0.0335(9) -0.0008(8) O7 0.0155(7) 0.0175(8) 0.0208(9) 0.0022(7) 0.0094(7) -0.0020(6) O8 0.0148(8) 0.0464(11) 0.0271(10) 0.0077(8) 0.0080(8) -0.0060(7) O9 0.0196(8) 0.0251(9) 0.0199(9) -0.0071(7) 0.0144(7) -0.0054(7) O10 0.0213(8) 0.0325(10) 0.0390(11) -0.0112(8) 0.0218(8) -0.0081(7) O11 0.0143(7) 0.0182(8) 0.0247(9) -0.0009(7) 0.0095(7) -0.0006(6) O12 0.0186(8) 0.0187(9) 0.0296(10) -0.0044(7) 0.0090(7) -0.0010(7) C1 0.0281(12) 0.0174(13) 0.0222(15) -0.0046(11) 0.0152(11) -0.0001(10) C2 0.0170(11) 0.0322(15) 0.0214(14) 0.0026(11) 0.0112(11) 0.0028(10) C3 0.0382(14) 0.0172(13) 0.0312(15) 0.0016(11) 0.0263(13) -0.0018(11) C4 0.0250(13) 0.0290(14) 0.0271(15) 0.0063(12) 0.0142(12) -0.0047(11) C5 0.0279(13) 0.0252(13) 0.0230(14) -0.0108(11) 0.0184(11) -0.0070(10) C6 0.0151(11) 0.0239(14) 0.0258(14) -0.0017(11) 0.0083(11) -0.0004(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 O9 2.1398(15) . ? Mn1 O11 2.1616(14) . ? Mn1 O7 2.1873(15) . ? Mn1 O1 2.2023(15) . ? Mn1 O3 2.2042(14) . ? Mn1 O5 2.2064(14) . ? Mn2 O2 2.1210(16) . ? Mn2 O12 2.1238(14) 2_645 ? Mn2 O3 2.1637(15) . ? Mn2 O5 2.1888(15) 2_645 ? Mn2 O1 2.2210(15) 2_645 ? Mn2 O7 2.2233(14) . ? Mn3 O4 2.1629(17) 3_655 ? Mn3 O4 2.1629(17) . ? Mn3 O6 2.1629(16) 3_655 ? Mn3 O6 2.1629(16) . ? Mn3 O9 2.2058(13) . ? Mn3 O9 2.2058(13) 3_655 ? Mn4 O8 2.1508(17) . ? Mn4 O8 2.1508(17) 3 ? Mn4 O10 2.1527(15) 3 ? Mn4 O10 2.1527(15) . ? Mn4 O11 2.2081(14) 3 ? Mn4 O11 2.2081(14) . ? O1 C1 1.269(3) . ? O1 Mn2 2.2210(15) 2_655 ? O2 C1 1.236(3) . ? O3 C2 1.263(3) . ? O4 C2 1.223(3) . ? O5 C3 1.267(3) . ? O5 Mn2 2.1888(15) 2_655 ? O6 C3 1.233(3) . ? O7 C4 1.272(3) . ? O8 C4 1.230(3) . ? O9 C5 1.277(3) . ? O10 C5 1.222(3) . ? O11 C6 1.271(3) . ? O12 C6 1.237(3) . ? O12 Mn2 2.1238(14) 2_655 ? C1 H1 0.98(3) . ? C2 H2 0.94(2) . ? C3 H3 0.93(2) . ? C4 H4 0.97(3) . ? C5 H5 0.97(3) . ? C6 H6 1.03(2) . ? 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 O9 Mn1 O11 96.73(6) . . ? O9 Mn1 O7 98.10(6) . . ? O11 Mn1 O7 96.02(5) . . ? O9 Mn1 O1 171.61(5) . . ? O11 Mn1 O1 89.11(6) . . ? O7 Mn1 O1 87.22(6) . . ? O9 Mn1 O3 89.27(5) . . ? O11 Mn1 O3 171.82(6) . . ? O7 Mn1 O3 77.57(5) . . ? O1 Mn1 O3 85.53(5) . . ? O9 Mn1 O5 95.60(6) . . ? O11 Mn1 O5 92.40(5) . . ? O7 Mn1 O5 162.95(6) . . ? O1 Mn1 O5 78.09(6) . . ? O3 Mn1 O5 92.54(5) . . ? O2 Mn2 O12 98.55(6) . 2_645 ? O2 Mn2 O3 95.52(6) . . ? O12 Mn2 O3 91.98(6) 2_645 . ? O2 Mn2 O5 95.30(6) . 2_645 ? O12 Mn2 O5 89.81(6) 2_645 2_645 ? O3 Mn2 O5 168.64(6) . 2_645 ? O2 Mn2 O1 168.63(6) . 2_645 ? O12 Mn2 O1 90.72(6) 2_645 2_645 ? O3 Mn2 O1 90.70(6) . 2_645 ? O5 Mn2 O1 78.06(5) 2_645 2_645 ? O2 Mn2 O7 86.74(6) . . ? O12 Mn2 O7 168.82(6) 2_645 . ? O3 Mn2 O7 77.65(5) . . ? O5 Mn2 O7 99.55(5) 2_645 . ? O1 Mn2 O7 85.30(5) 2_645 . ? O4 Mn3 O4 180.00(13) 3_655 . ? O4 Mn3 O6 89.88(7) 3_655 3_655 ? O4 Mn3 O6 90.12(7) . 3_655 ? O4 Mn3 O6 90.12(7) 3_655 . ? O4 Mn3 O6 89.88(7) . . ? O6 Mn3 O6 180.00(11) 3_655 . ? O4 Mn3 O9 84.96(6) 3_655 . ? O4 Mn3 O9 95.04(6) . . ? O6 Mn3 O9 88.86(5) 3_655 . ? O6 Mn3 O9 91.14(5) . . ? O4 Mn3 O9 95.04(6) 3_655 3_655 ? O4 Mn3 O9 84.96(6) . 3_655 ? O6 Mn3 O9 91.14(5) 3_655 3_655 ? O6 Mn3 O9 88.86(5) . 3_655 ? O9 Mn3 O9 180.00(7) . 3_655 ? O8 Mn4 O8 180.00(11) . 3 ? O8 Mn4 O10 90.90(7) . 3 ? O8 Mn4 O10 89.10(7) 3 3 ? O8 Mn4 O10 89.10(7) . . ? O8 Mn4 O10 90.90(7) 3 . ? O10 Mn4 O10 180.00(6) 3 . ? O8 Mn4 O11 87.04(6) . 3 ? O8 Mn4 O11 92.96(6) 3 3 ? O10 Mn4 O11 91.31(5) 3 3 ? O10 Mn4 O11 88.69(5) . 3 ? O8 Mn4 O11 92.96(6) . . ? O8 Mn4 O11 87.04(6) 3 . ? O10 Mn4 O11 88.69(5) 3 . ? O10 Mn4 O11 91.31(5) . . ? O11 Mn4 O11 180.00(9) 3 . ? C1 O1 Mn1 132.91(14) . . ? C1 O1 Mn2 129.11(14) . 2_655 ? Mn1 O1 Mn2 96.70(6) . 2_655 ? C1 O2 Mn2 128.72(16) . . ? C2 O3 Mn2 128.66(15) . . ? C2 O3 Mn1 131.44(15) . . ? Mn2 O3 Mn1 99.29(5) . . ? C2 O4 Mn3 134.24(15) . . ? C3 O5 Mn2 127.24(15) . 2_655 ? C3 O5 Mn1 132.80(15) . . ? Mn2 O5 Mn1 97.53(6) 2_655 . ? C3 O6 Mn3 134.11(16) . . ? C4 O7 Mn1 133.70(15) . . ? C4 O7 Mn2 127.34(15) . . ? Mn1 O7 Mn2 97.99(5) . . ? C4 O8 Mn4 135.20(16) . . ? C5 O9 Mn1 124.47(13) . . ? C5 O9 Mn3 121.66(14) . . ? Mn1 O9 Mn3 113.81(6) . . ? C5 O10 Mn4 142.64(15) . . ? C6 O11 Mn1 129.34(13) . . ? C6 O11 Mn4 120.00(12) . . ? Mn1 O11 Mn4 110.63(6) . . ? C6 O12 Mn2 133.08(14) . 2_655 ? O2 C1 O1 126.4(2) . . ? O2 C1 H1 118.0(15) . . ? O1 C1 H1 115.5(15) . . ? O4 C2 O3 126.7(2) . . ? O4 C2 H2 119.8(14) . . ? O3 C2 H2 113.6(14) . . ? O6 C3 O5 127.0(2) . . ? O6 C3 H3 117.5(15) . . ? O5 C3 H3 115.5(15) . . ? O8 C4 O7 126.5(2) . . ? O8 C4 H4 119.0(14) . . ? O7 C4 H4 114.4(14) . . ? O10 C5 O9 126.4(2) . . ? O10 C5 H5 116.4(13) . . ? O9 C5 H5 117.2(13) . . ? O12 C6 O11 126.2(2) . . ? O12 C6 H6 116.2(13) . . ? O11 C6 H6 117.6(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.376 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.077 ## END of data_2 data_3 _database_code_depnum_ccdc_archive 'CCDC 218686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)5(CH3COO)](CH3COOH) _chemical_formula_sum 'C9 H12 Mn3 O14' _chemical_formula_weight 509.01 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 2(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 11.688(2) _cell_length_b 10.2438(17) _cell_length_c 18.753(4) _cell_angle_alpha 90.00 _cell_angle_beta 127.408(3) _cell_angle_gamma 90.00 _cell_volume 1783.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8650 _cell_measurement_theta_min 3.2130 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'slightly pink' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 2.159 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8065 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29575 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4062 _reflns_number_gt 2952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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. H atoms were not included in refinement. ; _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^)+(0.0800P)^2^+1.8807P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'not included' _refine_ls_hydrogen_treatment 'not included' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4062 _refine_ls_number_parameters 260 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.37545(7) 0.08643(6) 0.12980(4) 0.0149(2) Uani 1 1 d . . . Mn2 Mn 0.57461(7) -0.10038(6) 0.31488(4) 0.0152(2) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.0282(3) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.0177(3) Uani 1 2 d S . . O1 O 0.4432(3) 0.2082(3) 0.24617(19) 0.0163(7) Uani 1 1 d . . . O2 O 0.5590(4) 0.0774(3) 0.3662(2) 0.0233(7) Uani 1 1 d . . . O3 O 0.5900(3) -0.0017(3) 0.2187(2) 0.0166(7) Uani 1 1 d . . . O4 O 0.6772(4) 0.0015(4) 0.1416(2) 0.0384(10) Uani 1 1 d . . . O5 O 0.4568(4) 0.2628(3) 0.1082(2) 0.0206(7) Uani 1 1 d . . . O6 O 0.4785(5) 0.2064(4) 0.0023(3) 0.0428(11) Uani 1 1 d . . . O7 O 0.3452(3) -0.0713(3) 0.1980(2) 0.0177(7) Uani 1 1 d . . . O8 O 0.1101(4) -0.0988(4) 0.1274(2) 0.0328(9) Uani 1 1 d . . . O9 O 0.3365(4) -0.0280(3) 0.0217(2) 0.0245(8) Uani 1 1 d . . . O10 O 0.1188(4) -0.1032(4) -0.0334(2) 0.0306(9) Uani 1 1 d . . . O11 O 0.1577(3) 0.1614(3) 0.0578(2) 0.0207(7) Uani 1 1 d . . . O12 O 0.2019(4) 0.3739(3) 0.0908(2) 0.0307(8) Uani 1 1 d . . . C1 C 0.5075(5) 0.1851(4) 0.3289(3) 0.0214(10) Uani 1 1 d . . . C2 C 0.6924(6) -0.0092(5) 0.2121(3) 0.0262(11) Uani 1 1 d . . . C21 C 0.831(4) -0.015(4) 0.284(2) 0.100(16) Uani 0.30(2) 1 d P . . C3 C 0.4818(8) 0.2856(6) 0.0522(4) 0.0487(18) Uani 1 1 d . . . C31 C 0.569(2) 0.4005(14) 0.0624(12) 0.052(6) Uani 0.42(2) 1 d P . . C4 C 0.2387(5) -0.1190(5) 0.1904(3) 0.0282(11) Uani 1 1 d . . . C5 C 0.2252(6) -0.0997(5) -0.0322(4) 0.0303(12) Uani 1 1 d . . . C6 C 0.1197(6) 0.2801(5) 0.0504(3) 0.0282(11) Uani 1 1 d . . . C61 C -0.024(3) 0.330(3) -0.009(2) 0.080(13) Uani 0.29(2) 1 d P . . O13 O 0.0815(10) -0.2137(11) 0.2818(5) 0.167(5) Uani 1 1 d . . . O14 O -0.0861(8) -0.2385(8) 0.1343(4) 0.102(2) Uani 1 1 d . . . C7 C -0.0416(13) -0.2569(11) 0.2142(8) 0.091(3) Uani 1 1 d . . . C8 C -0.1418(10) -0.3386(11) 0.2207(7) 0.104(4) 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 0.0166(4) 0.0149(4) 0.0121(3) -0.0009(3) 0.0082(3) -0.0018(3) Mn2 0.0179(4) 0.0134(4) 0.0140(3) 0.0007(3) 0.0095(3) 0.0010(3) Mn3 0.0226(6) 0.0506(8) 0.0184(5) -0.0092(5) 0.0161(5) -0.0094(5) Mn4 0.0138(5) 0.0191(5) 0.0173(5) -0.0022(4) 0.0079(4) -0.0048(4) O1 0.0223(17) 0.0145(15) 0.0122(15) 0.0011(12) 0.0105(14) -0.0009(13) O2 0.033(2) 0.0175(17) 0.0155(16) 0.0011(13) 0.0128(16) 0.0054(15) O3 0.0177(16) 0.0166(16) 0.0197(16) 0.0036(13) 0.0135(15) 0.0045(13) O4 0.027(2) 0.073(3) 0.0195(19) -0.0090(19) 0.0161(18) -0.009(2) O5 0.032(2) 0.0179(16) 0.0198(16) -0.0035(13) 0.0199(16) -0.0051(14) O6 0.056(3) 0.055(3) 0.035(2) -0.012(2) 0.037(2) -0.011(2) O7 0.0177(17) 0.0182(17) 0.0178(16) 0.0001(13) 0.0112(15) -0.0019(13) O8 0.0183(18) 0.051(2) 0.0265(19) 0.0122(17) 0.0124(17) -0.0045(17) O9 0.0196(18) 0.040(2) 0.0178(17) -0.0098(15) 0.0133(15) -0.0086(15) O10 0.0222(19) 0.039(2) 0.032(2) -0.0150(17) 0.0175(18) -0.0095(16) O11 0.0185(17) 0.0177(17) 0.0238(17) -0.0023(14) 0.0117(15) -0.0051(13) O12 0.0216(19) 0.0194(18) 0.034(2) -0.0002(15) 0.0078(17) -0.0022(15) C1 0.027(3) 0.014(2) 0.020(2) 0.0002(19) 0.013(2) 0.003(2) C2 0.025(3) 0.032(3) 0.025(3) -0.002(2) 0.017(2) -0.002(2) C21 0.10(3) 0.14(4) 0.09(3) 0.04(2) 0.08(3) 0.04(2) C3 0.095(6) 0.036(3) 0.048(4) -0.009(3) 0.061(4) -0.021(3) C31 0.095(15) 0.029(8) 0.068(12) -0.014(7) 0.068(12) -0.022(8) C4 0.022(3) 0.034(3) 0.025(3) 0.004(2) 0.012(2) -0.003(2) C5 0.026(3) 0.040(3) 0.029(3) -0.013(2) 0.019(3) -0.007(2) C6 0.023(3) 0.022(3) 0.032(3) 0.000(2) 0.013(2) -0.004(2) C61 0.033(15) 0.059(18) 0.11(3) -0.041(17) 0.028(17) -0.032(13) O13 0.110(7) 0.249(12) 0.066(5) 0.062(6) 0.014(5) -0.068(7) O14 0.083(5) 0.147(7) 0.080(4) 0.012(4) 0.052(4) -0.013(4) C7 0.100(8) 0.106(8) 0.085(7) 0.044(6) 0.066(7) 0.023(6) C8 0.070(6) 0.141(10) 0.122(9) 0.075(7) 0.069(7) 0.018(6) _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 O9 2.138(3) . ? Mn1 O11 2.171(3) . ? Mn1 O5 2.190(3) . ? Mn1 O3 2.192(3) . ? Mn1 O1 2.201(3) . ? Mn1 O7 2.218(3) . ? Mn2 O12 2.099(3) 2_645 ? Mn2 O2 2.120(3) . ? Mn2 O3 2.168(3) . ? Mn2 O5 2.196(3) 2_645 ? Mn2 O1 2.216(3) 2_645 ? Mn2 O7 2.223(3) . ? Mn3 O6 2.133(5) 3_655 ? Mn3 O6 2.133(5) . ? Mn3 O4 2.159(4) 3_655 ? Mn3 O4 2.159(4) . ? Mn3 O9 2.201(3) 3_655 ? Mn3 O9 2.201(3) . ? Mn4 O10 2.120(3) . ? Mn4 O10 2.120(3) 3 ? Mn4 O8 2.157(3) 3 ? Mn4 O8 2.157(3) . ? Mn4 O11 2.209(3) 3 ? Mn4 O11 2.209(3) . ? O1 C1 1.270(5) . ? O1 Mn2 2.216(3) 2_655 ? O2 C1 1.248(5) . ? O3 C2 1.278(6) . ? O4 C2 1.227(6) . ? O5 C3 1.272(6) . ? O5 Mn2 2.196(3) 2_655 ? O6 C3 1.221(7) . ? O7 C4 1.263(6) . ? O8 C4 1.241(6) . ? O9 C5 1.287(6) . ? O10 C5 1.231(6) . ? O11 C6 1.273(6) . ? O12 C6 1.239(6) . ? O12 Mn2 2.099(3) 2_655 ? C2 C21 1.34(4) . ? C3 C31 1.489(15) . ? C6 C61 1.43(3) . ? O13 C7 1.287(13) . ? O14 C7 1.267(11) . ? C7 C8 1.503(13) . ? 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 O9 Mn1 O11 96.32(12) . . ? O9 Mn1 O5 98.24(12) . . ? O11 Mn1 O5 93.98(12) . . ? O9 Mn1 O3 88.93(12) . . ? O11 Mn1 O3 170.39(11) . . ? O5 Mn1 O3 93.22(12) . . ? O9 Mn1 O1 172.74(12) . . ? O11 Mn1 O1 89.78(12) . . ? O5 Mn1 O1 77.35(11) . . ? O3 Mn1 O1 85.59(11) . . ? O9 Mn1 O7 97.47(12) . . ? O11 Mn1 O7 94.57(11) . . ? O5 Mn1 O7 161.15(11) . . ? O3 Mn1 O7 76.72(11) . . ? O1 Mn1 O7 85.92(11) . . ? O12 Mn2 O2 97.57(14) 2_645 . ? O12 Mn2 O3 94.02(13) 2_645 . ? O2 Mn2 O3 92.93(12) . . ? O12 Mn2 O5 89.15(14) 2_645 2_645 ? O2 Mn2 O5 98.92(12) . 2_645 ? O3 Mn2 O5 167.22(12) . 2_645 ? O12 Mn2 O1 90.13(13) 2_645 2_645 ? O2 Mn2 O1 171.24(13) . 2_645 ? O3 Mn2 O1 90.68(11) . 2_645 ? O5 Mn2 O1 76.93(11) 2_645 2_645 ? O12 Mn2 O7 170.24(13) 2_645 . ? O2 Mn2 O7 87.02(12) . . ? O3 Mn2 O7 77.09(11) . . ? O5 Mn2 O7 98.68(12) 2_645 . ? O1 Mn2 O7 86.01(12) 2_645 . ? O6 Mn3 O6 180.0(3) 3_655 . ? O6 Mn3 O4 90.26(16) 3_655 3_655 ? O6 Mn3 O4 89.74(16) . 3_655 ? O6 Mn3 O4 89.74(16) 3_655 . ? O6 Mn3 O4 90.26(16) . . ? O4 Mn3 O4 180.0(3) 3_655 . ? O6 Mn3 O9 89.96(14) 3_655 3_655 ? O6 Mn3 O9 90.04(14) . 3_655 ? O4 Mn3 O9 93.72(12) 3_655 3_655 ? O4 Mn3 O9 86.28(12) . 3_655 ? O6 Mn3 O9 90.04(14) 3_655 . ? O6 Mn3 O9 89.96(14) . . ? O4 Mn3 O9 86.28(12) 3_655 . ? O4 Mn3 O9 93.72(12) . . ? O9 Mn3 O9 180.00(14) 3_655 . ? O10 Mn4 O10 180.0(2) . 3 ? O10 Mn4 O8 87.93(14) . 3 ? O10 Mn4 O8 92.07(14) 3 3 ? O10 Mn4 O8 92.07(14) . . ? O10 Mn4 O8 87.93(14) 3 . ? O8 Mn4 O8 180.0(2) 3 . ? O10 Mn4 O11 89.02(12) . 3 ? O10 Mn4 O11 90.98(12) 3 3 ? O8 Mn4 O11 92.85(13) 3 3 ? O8 Mn4 O11 87.15(13) . 3 ? O10 Mn4 O11 90.98(12) . . ? O10 Mn4 O11 89.02(12) 3 . ? O8 Mn4 O11 87.15(13) 3 . ? O8 Mn4 O11 92.85(13) . . ? O11 Mn4 O11 180.00(11) 3 . ? C1 O1 Mn1 134.1(3) . . ? C1 O1 Mn2 126.6(3) . 2_655 ? Mn1 O1 Mn2 97.17(11) . 2_655 ? C1 O2 Mn2 130.5(3) . . ? C2 O3 Mn2 127.4(3) . . ? C2 O3 Mn1 131.1(3) . . ? Mn2 O3 Mn1 100.97(12) . . ? C2 O4 Mn3 136.7(4) . . ? C3 O5 Mn1 130.4(3) . . ? C3 O5 Mn2 129.7(3) . 2_655 ? Mn1 O5 Mn2 98.09(11) . 2_655 ? C3 O6 Mn3 136.5(4) . . ? C4 O7 Mn1 135.1(3) . . ? C4 O7 Mn2 125.1(3) . . ? Mn1 O7 Mn2 98.47(12) . . ? C4 O8 Mn4 134.0(3) . . ? C5 O9 Mn1 126.1(3) . . ? C5 O9 Mn3 120.4(3) . . ? Mn1 O9 Mn3 113.28(14) . . ? C5 O10 Mn4 144.7(3) . . ? C6 O11 Mn1 127.2(3) . . ? C6 O11 Mn4 122.0(3) . . ? Mn1 O11 Mn4 110.72(14) . . ? C6 O12 Mn2 135.9(3) . 2_655 ? O2 C1 O1 125.1(4) . . ? O4 C2 O3 124.6(5) . . ? O4 C2 C21 112.7(12) . . ? O3 C2 C21 122.4(12) . . ? O6 C3 O5 126.5(5) . . ? O6 C3 C31 109.0(7) . . ? O5 C3 C31 121.3(7) . . ? O8 C4 O7 125.7(5) . . ? O10 C5 O9 124.0(4) . . ? O12 C6 O11 125.8(5) . . ? O12 C6 C61 108.0(11) . . ? O11 C6 C61 126.1(11) . . ? O14 C7 O13 121.6(9) . . ? O14 C7 C8 113.4(11) . . ? O13 C7 C8 124.9(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.869 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.131 ## END of data_3 data_4 _database_code_depnum_ccdc_archive 'CCDC 218687' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)6]DMF _chemical_formula_sum 'C9 H13 Mn3 N O13' _chemical_formula_weight 508.02 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' O O 0.0106 0.0060 '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' 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 'P 2(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 11.7047(18) _cell_length_b 10.0946(13) _cell_length_c 18.556(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.585(2) _cell_angle_gamma 90.00 _cell_volume 1737.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 94(2) _cell_measurement_reflns_used 10041 _cell_measurement_theta_min 3.0267 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'slightly pink' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 2.213 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 94(2) _diffrn_radiation_type MoK\a _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28817 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3936 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3936 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _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 0.37408(4) 0.08529(3) 0.13052(2) 0.00899(9) Uani 1 1 d . . . Mn2 Mn 0.57784(4) -0.09805(3) 0.31711(2) 0.00998(9) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.01070(12) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.01091(12) Uani 1 2 d S . . O1 O 0.44342(16) 0.20932(15) 0.24833(9) 0.0111(3) Uani 1 1 d . . . O2 O 0.56645(17) 0.08003(15) 0.37196(9) 0.0149(4) Uani 1 1 d . . . O3 O 0.59248(17) 0.00295(15) 0.21952(9) 0.0116(3) Uani 1 1 d . . . O4 O 0.68230(18) 0.00583(16) 0.14271(10) 0.0170(4) Uani 1 1 d . . . O5 O 0.44488(17) 0.26508(15) 0.10202(9) 0.0120(3) Uani 1 1 d . . . O6 O 0.47115(18) 0.21121(16) -0.00393(9) 0.0153(4) Uani 1 1 d . . . O7 O 0.34862(16) -0.07350(15) 0.19945(9) 0.0115(3) Uani 1 1 d . . . O8 O 0.11428(17) -0.11989(16) 0.12075(10) 0.0169(4) Uani 1 1 d . . . O9 O 0.33502(17) -0.02925(15) 0.02072(9) 0.0121(3) Uani 1 1 d . . . O10 O 0.11249(17) -0.10265(16) -0.04207(10) 0.0161(4) Uani 1 1 d . . . O11 O 0.15893(17) 0.16216(15) 0.06360(9) 0.0124(3) Uani 1 1 d . . . O12 O 0.19321(17) 0.38001(15) 0.09305(10) 0.0147(4) Uani 1 1 d . . . C1 C 0.5115(3) 0.1868(2) 0.33272(14) 0.0127(5) Uani 1 1 d . . . C2 C 0.6940(3) -0.0051(2) 0.21304(16) 0.0138(5) Uani 1 1 d . . . C3 C 0.4645(3) 0.2921(2) 0.04268(14) 0.0136(5) Uani 1 1 d . . . C4 C 0.2419(3) -0.1351(2) 0.18581(15) 0.0144(5) Uani 1 1 d . . . C5 C 0.2242(3) -0.1028(2) -0.03422(15) 0.0127(5) Uani 1 1 d . . . C6 C 0.1161(3) 0.2803(2) 0.05771(14) 0.0138(5) Uani 1 1 d . . . C7 C 0.1608(3) -0.4582(3) -0.13593(18) 0.0298(7) Uani 1 1 d . . . C8 C 0.0575(4) -0.6769(3) -0.1494(2) 0.0345(7) Uani 1 1 d . . . C9 C 0.1866(4) -0.6339(3) -0.2140(2) 0.0296(7) Uani 1 1 d . . . N1 N 0.1372(2) -0.5846(2) -0.16381(13) 0.0233(5) Uani 1 1 d . . . O13 O 0.2214(2) -0.3747(2) -0.14899(13) 0.0361(5) Uani 1 1 d . . . H1 H 0.516(3) 0.260(2) 0.3676(15) 0.014(6) Uiso 1 1 d . . . H2 H 0.787(3) -0.026(3) 0.2692(17) 0.024(7) Uiso 1 1 d . . . H3 H 0.478(2) 0.389(2) 0.0376(14) 0.011(6) Uiso 1 1 d . . . H4 H 0.269(3) -0.201(3) 0.2344(15) 0.018(6) Uiso 1 1 d . . . H5 H 0.232(3) -0.161(2) -0.0712(15) 0.016(6) Uiso 1 1 d . . . H6 H 0.011(3) 0.294(3) 0.0219(16) 0.024(7) Uiso 1 1 d . . . H7 H 0.114(3) -0.439(3) -0.1041(16) 0.027(7) Uiso 1 1 d . . . H81 H -0.024(4) -0.717(3) -0.211(2) 0.052(10) Uiso 1 1 d . . . H82 H 0.120(4) -0.753(3) -0.114(2) 0.049(10) Uiso 1 1 d . . . H83 H 0.027(3) -0.627(3) -0.117(2) 0.049(9) Uiso 1 1 d . . . H91 H 0.106(4) -0.648(3) -0.277(2) 0.043(9) Uiso 1 1 d . . . H92 H 0.237(3) -0.727(3) -0.1888(16) 0.027(7) Uiso 1 1 d . . . H93 H 0.254(4) -0.568(4) -0.207(2) 0.061(11) 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 0.00928(18) 0.00852(18) 0.00902(17) -0.00025(12) 0.00550(14) -0.00025(14) Mn2 0.01102(19) 0.00878(18) 0.00998(17) 0.00103(13) 0.00631(14) 0.00080(15) Mn3 0.0108(3) 0.0123(3) 0.0110(2) -0.00132(18) 0.0076(2) -0.0010(2) Mn4 0.0093(3) 0.0109(3) 0.0118(2) -0.00065(18) 0.0061(2) -0.0018(2) O1 0.0130(9) 0.0101(8) 0.0089(7) -0.0006(6) 0.0060(7) -0.0003(7) O2 0.0184(9) 0.0116(9) 0.0121(8) 0.0026(6) 0.0080(7) 0.0040(7) O3 0.0122(8) 0.0120(8) 0.0124(7) 0.0027(6) 0.0084(7) 0.0008(7) O4 0.0144(9) 0.0249(10) 0.0139(8) 0.0001(7) 0.0098(7) -0.0008(7) O5 0.0152(9) 0.0114(8) 0.0135(8) -0.0002(6) 0.0108(7) -0.0011(7) O6 0.0204(10) 0.0143(9) 0.0160(8) -0.0020(7) 0.0136(7) -0.0007(7) O7 0.0097(8) 0.0123(9) 0.0136(8) 0.0014(6) 0.0076(7) -0.0007(7) O8 0.0109(9) 0.0207(10) 0.0149(8) 0.0023(7) 0.0057(7) -0.0022(7) O9 0.0111(9) 0.0143(9) 0.0111(7) -0.0022(6) 0.0069(7) -0.0030(7) O10 0.0125(9) 0.0189(9) 0.0191(8) -0.0037(7) 0.0107(7) -0.0019(8) O11 0.0109(8) 0.0117(9) 0.0137(8) -0.0012(6) 0.0071(7) 0.0002(7) O12 0.0120(9) 0.0114(9) 0.0162(8) -0.0031(6) 0.0062(7) -0.0017(7) C1 0.0136(13) 0.0121(13) 0.0140(12) -0.0036(9) 0.0092(10) -0.0019(10) C2 0.0112(12) 0.0123(13) 0.0167(12) 0.0005(9) 0.0079(10) -0.0002(10) C3 0.0157(13) 0.0103(13) 0.0161(11) 0.0008(9) 0.0103(10) 0.0002(10) C4 0.0157(13) 0.0138(13) 0.0151(12) 0.0004(9) 0.0101(10) -0.0009(10) C5 0.0171(13) 0.0123(12) 0.0134(11) -0.0018(9) 0.0117(10) -0.0027(11) C6 0.0131(13) 0.0145(13) 0.0130(11) 0.0017(10) 0.0075(10) 0.0012(11) C7 0.0301(17) 0.0313(17) 0.0307(15) -0.0023(13) 0.0199(14) -0.0029(14) C8 0.039(2) 0.0347(19) 0.0370(17) 0.0035(15) 0.0268(16) -0.0077(16) C9 0.0373(19) 0.0248(17) 0.0315(17) 0.0028(13) 0.0234(15) 0.0019(15) N1 0.0259(13) 0.0230(12) 0.0252(11) 0.0022(9) 0.0178(10) -0.0019(10) O13 0.0402(13) 0.0297(12) 0.0401(11) -0.0044(9) 0.0254(10) -0.0105(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 O9 2.1357(15) . ? Mn1 O11 2.1613(16) . ? Mn1 O7 2.1815(15) . ? Mn1 O5 2.1898(16) . ? Mn1 O3 2.1916(16) . ? Mn1 O1 2.2002(14) . ? Mn2 O2 2.1097(16) . ? Mn2 O12 2.1354(16) 2_645 ? Mn2 O5 2.1723(15) 2_645 ? Mn2 O3 2.1741(15) . ? Mn2 O7 2.2093(15) . ? Mn2 O1 2.2247(15) 2_645 ? Mn3 O6 2.1529(17) 3_655 ? Mn3 O6 2.1529(17) . ? Mn3 O4 2.1624(15) . ? Mn3 O4 2.1624(15) 3_655 ? Mn3 O9 2.2067(16) 3_655 ? Mn3 O9 2.2067(16) . ? Mn4 O8 2.1490(15) 3 ? Mn4 O8 2.1490(15) . ? Mn4 O10 2.1611(16) 3 ? Mn4 O10 2.1611(16) . ? Mn4 O11 2.2033(16) . ? Mn4 O11 2.2033(16) 3 ? O1 C1 1.272(2) . ? O1 Mn2 2.2247(15) 2_655 ? O2 C1 1.239(3) . ? O3 C2 1.268(3) . ? O4 C2 1.231(3) . ? O5 C3 1.283(3) . ? O5 Mn2 2.1723(15) 2_655 ? O6 C3 1.226(3) . ? O7 C4 1.275(3) . ? O8 C4 1.230(3) . ? O9 C5 1.288(3) . ? O10 C5 1.225(3) . ? O11 C6 1.272(3) . ? O12 C6 1.239(3) . ? O12 Mn2 2.1354(16) 2_655 ? C1 H1 0.96(2) . ? C2 H2 0.97(3) . ? C3 H3 1.00(2) . ? C4 H4 1.01(2) . ? C5 H5 0.95(2) . ? C6 H6 0.99(3) . ? C7 O13 1.217(3) . ? C7 N1 1.341(4) . ? C7 H7 1.04(3) . ? C8 N1 1.453(4) . ? C8 H81 1.02(3) . ? C8 H82 0.99(3) . ? C8 H83 1.01(3) . ? C9 N1 1.450(4) . ? C9 H91 0.97(3) . ? C9 H92 1.06(3) . ? C9 H93 0.98(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 O9 Mn1 O11 98.62(6) . . ? O9 Mn1 O7 97.78(6) . . ? O11 Mn1 O7 94.17(6) . . ? O9 Mn1 O5 96.35(6) . . ? O11 Mn1 O5 92.50(6) . . ? O7 Mn1 O5 163.29(5) . . ? O9 Mn1 O3 89.21(6) . . ? O11 Mn1 O3 169.71(5) . . ? O7 Mn1 O3 78.07(6) . . ? O5 Mn1 O3 93.27(6) . . ? O9 Mn1 O1 172.13(6) . . ? O11 Mn1 O1 87.76(6) . . ? O7 Mn1 O1 86.28(6) . . ? O5 Mn1 O1 78.68(5) . . ? O3 Mn1 O1 85.02(6) . . ? O2 Mn2 O12 97.48(6) . 2_645 ? O2 Mn2 O5 97.95(6) . 2_645 ? O12 Mn2 O5 91.08(6) 2_645 2_645 ? O2 Mn2 O3 93.59(6) . . ? O12 Mn2 O3 90.00(6) 2_645 . ? O5 Mn2 O3 168.17(6) 2_645 . ? O2 Mn2 O7 89.15(6) . . ? O12 Mn2 O7 166.52(6) 2_645 . ? O5 Mn2 O7 99.64(6) 2_645 . ? O3 Mn2 O7 77.84(6) . . ? O2 Mn2 O1 171.57(6) . 2_645 ? O12 Mn2 O1 90.27(6) 2_645 2_645 ? O5 Mn2 O1 78.52(5) 2_645 2_645 ? O3 Mn2 O1 89.69(5) . 2_645 ? O7 Mn2 O1 83.95(6) . 2_645 ? O6 Mn3 O6 180.00(9) 3_655 . ? O6 Mn3 O4 88.18(6) 3_655 . ? O6 Mn3 O4 91.82(6) . . ? O6 Mn3 O4 91.82(6) 3_655 3_655 ? O6 Mn3 O4 88.18(6) . 3_655 ? O4 Mn3 O4 180.00(8) . 3_655 ? O6 Mn3 O9 90.14(6) 3_655 3_655 ? O6 Mn3 O9 89.86(6) . 3_655 ? O4 Mn3 O9 83.97(6) . 3_655 ? O4 Mn3 O9 96.03(6) 3_655 3_655 ? O6 Mn3 O9 89.86(6) 3_655 . ? O6 Mn3 O9 90.14(6) . . ? O4 Mn3 O9 96.03(6) . . ? O4 Mn3 O9 83.97(6) 3_655 . ? O9 Mn3 O9 180.00(6) 3_655 . ? O8 Mn4 O8 180.00(11) 3 . ? O8 Mn4 O10 88.72(6) 3 3 ? O8 Mn4 O10 91.28(6) . 3 ? O8 Mn4 O10 91.28(6) 3 . ? O8 Mn4 O10 88.72(6) . . ? O10 Mn4 O10 180.00(6) 3 . ? O8 Mn4 O11 85.72(6) 3 . ? O8 Mn4 O11 94.28(6) . . ? O10 Mn4 O11 87.23(6) 3 . ? O10 Mn4 O11 92.77(6) . . ? O8 Mn4 O11 94.28(6) 3 3 ? O8 Mn4 O11 85.72(6) . 3 ? O10 Mn4 O11 92.77(6) 3 3 ? O10 Mn4 O11 87.23(6) . 3 ? O11 Mn4 O11 180.00(10) . 3 ? C1 O1 Mn1 134.13(14) . . ? C1 O1 Mn2 127.30(14) . 2_655 ? Mn1 O1 Mn2 95.99(5) . 2_655 ? C1 O2 Mn2 128.39(14) . . ? C2 O3 Mn2 127.13(14) . . ? C2 O3 Mn1 133.06(14) . . ? Mn2 O3 Mn1 99.04(6) . . ? C2 O4 Mn3 133.19(16) . . ? C3 O5 Mn2 128.22(15) . 2_655 ? C3 O5 Mn1 132.48(14) . . ? Mn2 O5 Mn1 97.84(6) 2_655 . ? C3 O6 Mn3 135.39(15) . . ? C4 O7 Mn1 135.22(15) . . ? C4 O7 Mn2 126.41(14) . . ? Mn1 O7 Mn2 98.28(6) . . ? C4 O8 Mn4 134.81(16) . . ? C5 O9 Mn1 126.40(14) . . ? C5 O9 Mn3 120.31(14) . . ? Mn1 O9 Mn3 113.14(7) . . ? C5 O10 Mn4 143.10(15) . . ? C6 O11 Mn1 130.23(15) . . ? C6 O11 Mn4 119.38(15) . . ? Mn1 O11 Mn4 110.38(7) . . ? C6 O12 Mn2 131.27(16) . 2_655 ? O2 C1 O1 126.2(2) . . ? O2 C1 H1 118.4(13) . . ? O1 C1 H1 115.4(13) . . ? O4 C2 O3 126.2(2) . . ? O4 C2 H2 118.9(15) . . ? O3 C2 H2 114.8(15) . . ? O6 C3 O5 125.8(2) . . ? O6 C3 H3 120.2(13) . . ? O5 C3 H3 114.0(13) . . ? O8 C4 O7 126.2(2) . . ? O8 C4 H4 119.3(14) . . ? O7 C4 H4 114.5(14) . . ? O10 C5 O9 125.4(2) . . ? O10 C5 H5 118.8(15) . . ? O9 C5 H5 115.8(15) . . ? O12 C6 O11 126.5(2) . . ? O12 C6 H6 116.4(16) . . ? O11 C6 H6 117.1(16) . . ? O13 C7 N1 126.2(3) . . ? O13 C7 H7 123.7(15) . . ? N1 C7 H7 110.1(15) . . ? N1 C8 H81 108.5(18) . . ? N1 C8 H82 109(2) . . ? H81 C8 H82 104(3) . . ? N1 C8 H83 107.1(19) . . ? H81 C8 H83 116(3) . . ? H82 C8 H83 112(3) . . ? N1 C9 H91 111.0(19) . . ? N1 C9 H92 111.0(14) . . ? H91 C9 H92 106(2) . . ? N1 C9 H93 106(2) . . ? H91 C9 H93 111(3) . . ? H92 C9 H93 111(3) . . ? C7 N1 C9 120.4(2) . . ? C7 N1 C8 122.9(2) . . ? C9 N1 C8 116.7(2) . . ? 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 C1 H1 O3 0.96(2) 2.78(2) 3.342(3) 117.8(15) 2_655 C1 H1 O6 0.96(2) 2.75(2) 3.495(3) 134.9(18) 4_566 C1 H1 O9 0.96(2) 2.73(2) 3.589(3) 148.7(19) 2_655 C2 H2 O12 0.97(3) 2.60(2) 3.200(3) 120(2) 2_645 C3 H3 O2 1.00(2) 2.80(2) 3.433(3) 121.3(16) 2_655 C4 H4 O5 1.01(2) 2.86(2) 3.514(3) 123.5(18) 2_645 C5 H5 O4 0.95(2) 2.62(2) 2.983(3) 103.2(17) 3_655 C5 H5 O6 0.95(2) 2.89(2) 3.366(3) 112.1(17) 3_655 C6 H6 O8 0.99(3) 2.74(3) 3.157(3) 105.5(17) 3 C6 H6 O10 0.99(3) 2.57(3) 3.084(3) 111.9(19) 3 C5 H5 O13 0.95(2) 2.55(3) 3.462(3) 160(2) . C3 H3 O13 1.00(2) 2.80(2) 3.043(3) 94.5(14) 3_655 C4 H4 O13 1.01(2) 2.65(2) 3.219(3) 115.7(17) 4_556 C8 H82 O8 0.99(3) 2.95(3) 3.137(3) 91(2) 3_545 C8 H82 O11 0.99(3) 3.15(3) 3.736(3) 119(2) 1_545 C8 H83 O12 1.01(3) 3.12(3) 3.792(3) 126(2) 1_545 C8 H81 O13 1.02(3) 2.70(3) 3.707(4) 167(2) 2_544 C8 H82 O11 0.99(3) 3.15(3) 3.736(3) 119(2) 1_545 C8 H83 O12 1.01(3) 3.12(3) 3.792(3) 126(2) 1_545 C9 H91 O10 0.97(3) 2.74(3) 3.677(3) 162(2) 2_544 C9 H92 O4 1.06(3) 2.92(3) 3.965(4) 168(2) 3_645 C9 H92 O6 1.06(3) 2.86(3) 3.590(3) 126.3(17) 1_545 C9 H93 O2 0.98(4) 3.00(4) 3.737(4) 133(3) 4 C9 H93 O7 0.98(4) 2.94(4) 3.779(3) 145(2) 4 C9 H93 O8 0.98(4) 3.18(3) 3.678(3) 113(2) 4 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.474 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.088 ## End of data_4 data_5 _database_code_depnum_ccdc_archive 'CCDC 218688' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)6]FURAN _chemical_formula_sum 'C10 H10 Mn3 O13' _chemical_formula_weight 503.00 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 2(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 11.519(2) _cell_length_b 10.0050(15) _cell_length_c 18.685(4) _cell_angle_alpha 90.00 _cell_angle_beta 126.821(3) _cell_angle_gamma 90.00 _cell_volume 1723.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 11035 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'slightly pink' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 2.229 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7829 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28562 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3899 _reflns_number_gt 3173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0455P)^2^+0.2855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3899 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _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 0.37537(4) 0.08589(4) 0.13161(2) 0.00868(11) Uani 1 1 d . . . Mn2 Mn 0.57903(4) -0.09713(4) 0.31485(3) 0.00974(11) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.01051(14) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.01112(14) Uani 1 2 d S . . O1 O 0.43287(19) 0.20852(17) 0.24635(11) 0.0127(4) Uani 1 1 d . . . O2 O 0.5519(2) 0.07714(17) 0.36771(12) 0.0146(4) Uani 1 1 d . . . O3 O 0.59702(19) 0.00500(16) 0.21985(12) 0.0118(4) Uani 1 1 d . . . O4 O 0.6837(2) -0.00206(18) 0.14044(12) 0.0162(4) Uani 1 1 d . . . O5 O 0.45699(19) 0.26608(16) 0.10953(11) 0.0112(4) Uani 1 1 d . . . O6 O 0.4880(2) 0.21473(18) 0.00554(12) 0.0151(4) Uani 1 1 d . . . O7 O 0.34807(19) -0.07764(17) 0.19695(12) 0.0122(4) Uani 1 1 d . . . O8 O 0.11000(19) -0.10551(18) 0.12572(13) 0.0171(4) Uani 1 1 d . . . O9 O 0.33602(19) -0.03015(17) 0.02251(12) 0.0123(4) Uani 1 1 d . . . O10 O 0.1173(2) -0.11568(18) -0.03452(13) 0.0163(4) Uani 1 1 d . . . O11 O 0.15817(19) 0.16495(16) 0.05777(12) 0.0125(4) Uani 1 1 d . . . O12 O 0.19351(19) 0.38365(16) 0.09015(12) 0.0140(4) Uani 1 1 d . . . C1 C 0.4920(3) 0.1831(3) 0.32820(18) 0.0132(5) Uani 1 1 d . . . C2 C 0.6983(3) -0.0079(3) 0.21116(18) 0.0141(6) Uani 1 1 d . . . C3 C 0.4790(3) 0.2945(3) 0.05232(18) 0.0142(6) Uani 1 1 d . . . C4 C 0.2373(3) -0.1284(3) 0.18659(19) 0.0161(6) Uani 1 1 d . . . C5 C 0.2289(3) -0.1081(3) -0.02888(19) 0.0141(6) Uani 1 1 d . . . C6 C 0.1163(3) 0.2856(3) 0.04842(18) 0.0143(6) Uani 1 1 d . . . O13 O 0.1674(3) 0.3677(3) -0.08509(18) 0.0475(7) Uani 1 1 d . . . C7 C 0.1517(5) 0.5019(4) -0.0993(3) 0.0442(10) Uani 1 1 d . . . C8 C 0.1132(4) 0.5305(4) -0.1813(3) 0.0463(10) Uani 1 1 d . . . C9 C 0.1032(5) 0.4055(4) -0.2212(3) 0.0472(11) Uani 1 1 d . . . C10 C 0.1374(5) 0.3110(4) -0.1611(3) 0.0461(10) Uani 1 1 d . . . H1 H 0.496(3) 0.254(3) 0.364(2) 0.021(8) Uiso 1 1 d . . . H2 H 0.793(3) -0.026(3) 0.2645(19) 0.011(7) Uiso 1 1 d . . . H3 H 0.494(3) 0.389(3) 0.0457(19) 0.015(8) Uiso 1 1 d . . . H4 H 0.258(3) -0.195(3) 0.231(2) 0.026(8) Uiso 1 1 d . . . H5 H 0.238(3) -0.163(3) -0.065(2) 0.011(7) Uiso 1 1 d . . . H6 H 0.014(3) 0.299(3) 0.0045(17) 0.005(6) Uiso 1 1 d . . . H7 H 0.162(5) 0.562(5) -0.046(3) 0.070(14) Uiso 1 1 d . . . H8 H 0.102(5) 0.625(4) -0.206(3) 0.057(12) Uiso 1 1 d . . . H9 H 0.072(5) 0.388(4) -0.280(3) 0.072(15) Uiso 1 1 d . . . H10 H 0.144(4) 0.201(4) -0.161(3) 0.058(12) 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 0.0099(2) 0.00809(19) 0.0079(2) -0.00013(14) 0.00521(17) -0.00013(15) Mn2 0.0117(2) 0.00806(19) 0.0090(2) 0.00084(15) 0.00595(17) 0.00081(15) Mn3 0.0116(3) 0.0116(3) 0.0108(3) -0.0015(2) 0.0080(2) -0.0015(2) Mn4 0.0097(3) 0.0116(3) 0.0106(3) -0.0020(2) 0.0053(2) -0.0026(2) O1 0.0182(9) 0.0100(8) 0.0102(9) -0.0005(7) 0.0087(8) -0.0020(7) O2 0.0201(10) 0.0105(9) 0.0121(9) 0.0026(7) 0.0090(8) 0.0047(8) O3 0.0129(9) 0.0116(9) 0.0127(9) 0.0034(7) 0.0086(8) 0.0022(7) O4 0.0139(9) 0.0248(10) 0.0114(10) 0.0012(8) 0.0084(8) 0.0005(8) O5 0.0152(9) 0.0085(8) 0.0123(9) 0.0001(7) 0.0095(8) -0.0010(7) O6 0.0226(10) 0.0139(9) 0.0169(10) -0.0015(8) 0.0162(9) -0.0014(8) O7 0.0129(9) 0.0115(9) 0.0129(9) -0.0003(7) 0.0081(8) -0.0022(7) O8 0.0117(9) 0.0221(10) 0.0142(10) 0.0018(8) 0.0060(8) -0.0031(8) O9 0.0122(9) 0.0153(9) 0.0101(9) -0.0039(7) 0.0070(8) -0.0035(8) O10 0.0139(9) 0.0180(9) 0.0204(10) -0.0046(8) 0.0122(8) -0.0036(8) O11 0.0130(9) 0.0095(9) 0.0144(9) -0.0015(7) 0.0078(8) -0.0010(7) O12 0.0134(9) 0.0104(9) 0.0157(10) -0.0022(8) 0.0074(8) -0.0011(8) C1 0.0152(13) 0.0096(12) 0.0125(13) -0.0038(11) 0.0071(11) -0.0034(11) C2 0.0121(13) 0.0142(13) 0.0128(13) -0.0009(11) 0.0057(11) 0.0000(11) C3 0.0191(14) 0.0104(13) 0.0158(13) -0.0004(11) 0.0120(12) -0.0015(11) C4 0.0194(14) 0.0150(13) 0.0155(14) -0.0003(11) 0.0112(12) -0.0039(12) C5 0.0188(14) 0.0133(13) 0.0135(13) -0.0055(11) 0.0115(12) -0.0034(11) C6 0.0143(14) 0.0148(13) 0.0152(13) 0.0016(11) 0.0095(12) 0.0006(12) O13 0.0664(19) 0.0413(15) 0.0323(14) 0.0069(12) 0.0283(14) 0.0111(14) C7 0.050(2) 0.041(2) 0.043(2) 0.0018(18) 0.028(2) 0.0029(18) C8 0.043(2) 0.052(2) 0.040(2) 0.0165(19) 0.0227(19) 0.004(2) C9 0.040(2) 0.071(3) 0.0209(19) -0.0019(19) 0.0133(18) -0.004(2) C10 0.052(2) 0.048(2) 0.033(2) -0.0011(18) 0.0233(19) 0.005(2) _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 O9 2.1452(18) . ? Mn1 O11 2.1566(18) . ? Mn1 O7 2.1740(18) . ? Mn1 O5 2.1839(17) . ? Mn1 O1 2.1995(18) . ? Mn1 O3 2.2014(18) . ? Mn2 O12 2.1162(18) 2_645 ? Mn2 O2 2.1175(18) . ? Mn2 O3 2.1631(18) . ? Mn2 O5 2.1780(18) 2_645 ? Mn2 O1 2.2181(18) 2_645 ? Mn2 O7 2.2234(18) . ? Mn3 O6 2.1593(18) 3_655 ? Mn3 O6 2.1593(18) . ? Mn3 O4 2.1699(19) . ? Mn3 O4 2.1699(19) 3_655 ? Mn3 O9 2.1881(19) 3_655 ? Mn3 O9 2.1881(19) . ? Mn4 O10 2.1506(19) 3 ? Mn4 O10 2.1506(19) . ? Mn4 O8 2.1611(19) . ? Mn4 O8 2.1611(19) 3 ? Mn4 O11 2.2025(17) 3 ? Mn4 O11 2.2025(17) . ? O1 C1 1.272(3) . ? O1 Mn2 2.2181(18) 2_655 ? O2 C1 1.238(3) . ? O3 C2 1.277(3) . ? O4 C2 1.229(3) . ? O5 C3 1.270(3) . ? O5 Mn2 2.1780(18) 2_655 ? O6 C3 1.233(3) . ? O7 C4 1.276(3) . ? O8 C4 1.223(3) . ? O9 C5 1.278(3) . ? O10 C5 1.227(3) . ? O11 C6 1.272(3) . ? O12 C6 1.237(3) . ? O12 Mn2 2.1162(18) 2_655 ? C1 H1 0.96(3) . ? C2 H2 0.96(3) . ? C3 H3 0.98(3) . ? C4 H4 0.98(3) . ? C5 H5 0.93(3) . ? C6 H6 0.96(3) . ? O13 C7 1.360(4) . ? O13 C10 1.368(5) . ? C7 C8 1.346(6) . ? C7 H7 1.10(5) . ? C8 C9 1.424(6) . ? C8 H8 1.03(4) . ? C9 C10 1.334(6) . ? C9 H9 0.94(5) . ? C10 H10 1.10(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 O9 Mn1 O11 95.00(7) . . ? O9 Mn1 O7 96.14(7) . . ? O11 Mn1 O7 97.62(7) . . ? O9 Mn1 O5 97.87(7) . . ? O11 Mn1 O5 92.41(7) . . ? O7 Mn1 O5 161.97(7) . . ? O9 Mn1 O1 175.45(7) . . ? O11 Mn1 O1 88.58(7) . . ? O7 Mn1 O1 86.15(7) . . ? O5 Mn1 O1 79.13(7) . . ? O9 Mn1 O3 90.14(7) . . ? O11 Mn1 O3 173.74(7) . . ? O7 Mn1 O3 78.22(7) . . ? O5 Mn1 O3 90.43(6) . . ? O1 Mn1 O3 86.47(7) . . ? O12 Mn2 O2 97.95(7) 2_645 . ? O12 Mn2 O3 92.97(7) 2_645 . ? O2 Mn2 O3 96.16(7) . . ? O12 Mn2 O5 91.16(7) 2_645 2_645 ? O2 Mn2 O5 94.36(7) . 2_645 ? O3 Mn2 O5 168.05(7) . 2_645 ? O12 Mn2 O1 90.90(7) 2_645 2_645 ? O2 Mn2 O1 168.99(7) . 2_645 ? O3 Mn2 O1 89.87(7) . 2_645 ? O5 Mn2 O1 78.85(7) 2_645 2_645 ? O12 Mn2 O7 169.67(7) 2_645 . ? O2 Mn2 O7 88.07(7) . . ? O3 Mn2 O7 77.98(7) . . ? O5 Mn2 O7 96.77(7) 2_645 . ? O1 Mn2 O7 84.18(7) 2_645 . ? O6 Mn3 O6 180.00(11) 3_655 . ? O6 Mn3 O4 90.25(7) 3_655 . ? O6 Mn3 O4 89.75(7) . . ? O6 Mn3 O4 89.75(7) 3_655 3_655 ? O6 Mn3 O4 90.25(7) . 3_655 ? O4 Mn3 O4 180.00(10) . 3_655 ? O6 Mn3 O9 92.31(7) 3_655 3_655 ? O6 Mn3 O9 87.69(7) . 3_655 ? O4 Mn3 O9 84.56(7) . 3_655 ? O4 Mn3 O9 95.44(7) 3_655 3_655 ? O6 Mn3 O9 87.69(7) 3_655 . ? O6 Mn3 O9 92.31(7) . . ? O4 Mn3 O9 95.44(7) . . ? O4 Mn3 O9 84.56(7) 3_655 . ? O9 Mn3 O9 180.00(8) 3_655 . ? O10 Mn4 O10 180.00(8) 3 . ? O10 Mn4 O8 90.08(8) 3 . ? O10 Mn4 O8 89.92(8) . . ? O10 Mn4 O8 89.92(8) 3 3 ? O10 Mn4 O8 90.08(8) . 3 ? O8 Mn4 O8 180.00(13) . 3 ? O10 Mn4 O11 93.81(7) 3 3 ? O10 Mn4 O11 86.19(7) . 3 ? O8 Mn4 O11 86.59(7) . 3 ? O8 Mn4 O11 93.41(7) 3 3 ? O10 Mn4 O11 86.19(7) 3 . ? O10 Mn4 O11 93.81(7) . . ? O8 Mn4 O11 93.41(7) . . ? O8 Mn4 O11 86.59(7) 3 . ? O11 Mn4 O11 180.00(19) 3 . ? C1 O1 Mn1 133.75(16) . . ? C1 O1 Mn2 128.19(16) . 2_655 ? Mn1 O1 Mn2 95.57(7) . 2_655 ? C1 O2 Mn2 127.72(18) . . ? C2 O3 Mn2 126.92(17) . . ? C2 O3 Mn1 132.82(17) . . ? Mn2 O3 Mn1 98.61(7) . . ? C2 O4 Mn3 134.94(18) . . ? C3 O5 Mn2 128.09(16) . 2_655 ? C3 O5 Mn1 132.05(16) . . ? Mn2 O5 Mn1 97.19(7) 2_655 . ? C3 O6 Mn3 135.51(18) . . ? C4 O7 Mn1 133.04(17) . . ? C4 O7 Mn2 127.55(17) . . ? Mn1 O7 Mn2 97.62(7) . . ? C4 O8 Mn4 134.22(19) . . ? C5 O9 Mn1 127.09(18) . . ? C5 O9 Mn3 119.74(17) . . ? Mn1 O9 Mn3 113.14(8) . . ? C5 O10 Mn4 138.99(17) . . ? C6 O11 Mn1 129.40(16) . . ? C6 O11 Mn4 120.62(16) . . ? Mn1 O11 Mn4 109.90(7) . . ? C6 O12 Mn2 131.42(17) . 2_655 ? O2 C1 O1 126.4(2) . . ? O2 C1 H1 116.2(18) . . ? O1 C1 H1 117.3(18) . . ? O4 C2 O3 125.8(3) . . ? O4 C2 H2 117.7(18) . . ? O3 C2 H2 116.5(18) . . ? O6 C3 O5 126.5(2) . . ? O6 C3 H3 116.1(18) . . ? O5 C3 H3 117.3(18) . . ? O8 C4 O7 126.8(3) . . ? O8 C4 H4 117.7(19) . . ? O7 C4 H4 115.5(19) . . ? O10 C5 O9 126.3(3) . . ? O10 C5 H5 118.1(18) . . ? O9 C5 H5 115.5(18) . . ? O12 C6 O11 126.6(2) . . ? O12 C6 H6 118.4(16) . . ? O11 C6 H6 115.1(16) . . ? C7 O13 C10 106.6(3) . . ? C8 C7 O13 110.3(4) . . ? C8 C7 H7 134(2) . . ? O13 C7 H7 116(2) . . ? C7 C8 C9 106.1(4) . . ? C7 C8 H8 125(2) . . ? C9 C8 H8 128(2) . . ? C10 C9 C8 107.0(4) . . ? C10 C9 H9 124(3) . . ? C8 C9 H9 129(3) . . ? C9 C10 O13 110.1(4) . . ? C9 C10 H10 134(2) . . ? O13 C10 H10 116(2) . . ? 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 C1 H1 O3 0.96(3) 2.81(3) 3.336(3) 116(2) 2_655 C1 H1 O6 0.96(3) 2.72(3) 3.495(3) 138(2) 4_566 C1 H1 O9 0.96(3) 2.83(3) 3.649(3) 145(2) 2_655 C2 H2 O12 0.96(3) 2.78(3) 3.312(3) 116(2) 2_645 C3 H3 O2 0.98(3) 2.73(3) 3.315(3) 119(2) 2_655 C4 H4 O5 0.98(3) 2.84(3) 3.457(3) 122(2) 2_645 C5 H5 O4 0.93(3) 2.65(3) 3.015(3) 104.0(19) 3_655 C5 H5 O6 0.93(3) 2.69(3) 3.204(3) 115(2) 3_655 C6 H6 O8 0.96(3) 2.75(3) 3.234(3) 112.1(19) 3 C6 H6 O10 0.96(3) 2.65(3) 3.059(3) 106.4(19) 3 C7 H7 O12 1.10(5) 2.95(5) 3.482(5) 110(3) . C7 H7 O2 1.10(5) 2.98(5) 3.639(5) 119(3) 2_655 C8 H8 O8 1.03(4) 3.20(4) 3.661(5) 109(3) 4_565 C9 H9 O10 0.94(5) 2.78(5) 3.666(4) 157(4) 2_554 C10 H10 O4 1.10(4) 2.67(4) 3.605(5) 143(3) 3_655 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.427 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.105 ## END of data_5 data_6 _database_code_depnum_ccdc_archive 'CCDC 218689' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)6]BENZENE _chemical_formula_sum 'C12 H12 Mn3 O12' _chemical_formula_weight 513.04 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 2(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 11.6548(16) _cell_length_b 10.1617(11) _cell_length_c 19.042(3) _cell_angle_alpha 90.00 _cell_angle_beta 126.580(2) _cell_angle_gamma 90.00 _cell_volume 1811.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 82(2) _cell_measurement_reflns_used 11109 _cell_measurement_theta_min 3.3341 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 2.119 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8775 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 82(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30158 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4087 _reflns_number_gt 3111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4087 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.37661(3) 0.07793(3) 0.131843(19) 0.00873(9) Uani 1 1 d . . . Mn2 Mn 0.57012(3) -0.11043(3) 0.308554(19) 0.00966(10) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.01001(12) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.01006(12) Uani 1 2 d S . . O1 O 0.43763(15) 0.19632(14) 0.24736(8) 0.0111(3) Uani 1 1 d . . . O2 O 0.54695(16) 0.05971(16) 0.36237(9) 0.0148(4) Uani 1 1 d . . . O3 O 0.59047(15) -0.00774(14) 0.21628(9) 0.0113(3) Uani 1 1 d . . . O4 O 0.67399(16) -0.01977(16) 0.13721(9) 0.0158(4) Uani 1 1 d . . . O5 O 0.46238(15) 0.25679(15) 0.11468(8) 0.0119(3) Uani 1 1 d . . . O6 O 0.50735(16) 0.21043(16) 0.01824(9) 0.0153(4) Uani 1 1 d . . . O7 O 0.34494(15) -0.08754(15) 0.19152(9) 0.0118(3) Uani 1 1 d . . . O8 O 0.11030(15) -0.12904(16) 0.11176(9) 0.0153(4) Uani 1 1 d . . . O9 O 0.33247(15) -0.02258(15) 0.01907(9) 0.0121(3) Uani 1 1 d . . . O10 O 0.11013(16) -0.09620(16) -0.04377(9) 0.0143(4) Uani 1 1 d . . . O11 O 0.16324(14) 0.15603(15) 0.06634(9) 0.0109(3) Uani 1 1 d . . . O12 O 0.20337(15) 0.37013(15) 0.10165(9) 0.0128(3) Uani 1 1 d . . . C1 C 0.4958(2) 0.1681(2) 0.32724(13) 0.0128(5) Uani 1 1 d . . . C2 C 0.6887(2) -0.0252(2) 0.20696(14) 0.0132(5) Uani 1 1 d . . . C3 C 0.4996(2) 0.2867(2) 0.06556(14) 0.0146(5) Uani 1 1 d . . . C4 C 0.2362(2) -0.1511(2) 0.17336(14) 0.0131(5) Uani 1 1 d . . . C5 C 0.2214(2) -0.0898(2) -0.03756(14) 0.0144(5) Uani 1 1 d . . . C6 C 0.1243(2) 0.2740(2) 0.06362(13) 0.0121(5) Uani 1 1 d . . . C7 C 0.0773(3) -0.0673(3) 0.27286(17) 0.0259(6) Uani 1 1 d . . . C8 C 0.1265(3) 0.0547(3) 0.26943(16) 0.0268(6) Uani 1 1 d . . . C9 C 0.1713(3) 0.1463(3) 0.33444(17) 0.0277(6) Uani 1 1 d . . . C10 C 0.1661(3) 0.1157(3) 0.40308(18) 0.0368(8) Uani 1 1 d . . . C11 C 0.1194(3) -0.0064(3) 0.40775(17) 0.0339(7) Uani 1 1 d . . . C12 C 0.0751(3) -0.0977(3) 0.34222(17) 0.0256(6) Uani 1 1 d . . . H1 H 0.496(2) 0.245(2) 0.3632(13) 0.009(6) Uiso 1 1 d . . . H2 H 0.789(3) -0.047(3) 0.2620(17) 0.034(8) Uiso 1 1 d . . . H3 H 0.532(3) 0.379(3) 0.0709(16) 0.034(8) Uiso 1 1 d . . . H4 H 0.257(3) -0.224(3) 0.2123(14) 0.020(7) Uiso 1 1 d . . . H5 H 0.228(2) -0.142(2) -0.0796(14) 0.017(6) Uiso 1 1 d . . . H6 H 0.022(3) 0.288(3) 0.0289(15) 0.019(6) Uiso 1 1 d . . . H7 H 0.050(3) -0.132(3) 0.2291(16) 0.028(7) Uiso 1 1 d . . . H8 H 0.131(3) 0.077(3) 0.2229(19) 0.040(8) Uiso 1 1 d . . . H9 H 0.206(3) 0.235(3) 0.3322(15) 0.029(7) Uiso 1 1 d . . . H10 H 0.197(4) 0.186(4) 0.449(2) 0.069(11) Uiso 1 1 d . . . H11 H 0.120(3) -0.028(3) 0.4552(19) 0.041(8) Uiso 1 1 d . . . H12 H 0.039(2) -0.178(3) 0.3406(14) 0.015(6) 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 0.00876(16) 0.00899(19) 0.00855(17) 0.00005(12) 0.00522(14) 0.00037(13) Mn2 0.00994(17) 0.00927(19) 0.00908(17) 0.00080(12) 0.00530(14) 0.00048(13) Mn3 0.0092(2) 0.0122(3) 0.0103(2) -0.00176(17) 0.0068(2) -0.00104(18) Mn4 0.0080(2) 0.0113(3) 0.0102(2) -0.00168(17) 0.0051(2) -0.00123(18) O1 0.0146(8) 0.0091(8) 0.0103(8) 0.0007(6) 0.0078(7) 0.0003(6) O2 0.0193(8) 0.0116(9) 0.0119(8) 0.0005(6) 0.0085(7) 0.0030(7) O3 0.0106(7) 0.0120(9) 0.0137(8) 0.0037(6) 0.0085(7) 0.0017(6) O4 0.0133(8) 0.0237(10) 0.0112(8) -0.0008(6) 0.0077(7) 0.0011(7) O5 0.0142(8) 0.0116(9) 0.0121(7) -0.0007(6) 0.0091(7) -0.0010(6) O6 0.0204(8) 0.0142(9) 0.0181(8) -0.0010(6) 0.0151(7) 0.0007(7) O7 0.0100(7) 0.0116(9) 0.0115(8) 0.0006(6) 0.0051(7) -0.0016(6) O8 0.0102(8) 0.0190(10) 0.0131(8) 0.0018(6) 0.0051(7) -0.0027(7) O9 0.0106(7) 0.0149(9) 0.0121(8) -0.0042(6) 0.0074(7) -0.0032(6) O10 0.0118(7) 0.0179(10) 0.0170(8) -0.0049(6) 0.0107(7) -0.0032(7) O11 0.0097(7) 0.0104(9) 0.0120(7) -0.0001(6) 0.0061(6) 0.0002(6) O12 0.0115(7) 0.0111(9) 0.0128(8) -0.0019(6) 0.0056(7) 0.0005(6) C1 0.0142(11) 0.0117(13) 0.0134(12) -0.0010(9) 0.0088(10) -0.0021(9) C2 0.0094(11) 0.0144(13) 0.0155(12) 0.0001(9) 0.0072(10) 0.0000(9) C3 0.0198(12) 0.0114(13) 0.0171(12) 0.0012(9) 0.0134(11) -0.0002(10) C4 0.0133(11) 0.0123(13) 0.0127(11) 0.0019(9) 0.0072(10) -0.0014(9) C5 0.0154(11) 0.0177(14) 0.0133(11) -0.0039(9) 0.0104(10) -0.0012(10) C6 0.0093(11) 0.0131(13) 0.0116(11) -0.0009(9) 0.0050(10) 0.0003(9) C7 0.0279(14) 0.0268(16) 0.0270(14) -0.0077(11) 0.0186(13) -0.0027(12) C8 0.0315(15) 0.0309(17) 0.0192(14) -0.0004(11) 0.0158(13) -0.0026(12) C9 0.0295(14) 0.0259(17) 0.0295(15) -0.0031(11) 0.0185(13) -0.0100(12) C10 0.0373(16) 0.049(2) 0.0275(15) -0.0164(14) 0.0210(14) -0.0214(15) C11 0.0303(16) 0.053(2) 0.0171(14) -0.0020(12) 0.0134(13) -0.0129(14) C12 0.0192(13) 0.0212(17) 0.0341(16) 0.0056(11) 0.0145(13) -0.0002(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 O9 2.1455(15) . ? Mn1 O11 2.1617(15) . ? Mn1 O7 2.1806(15) . ? Mn1 O3 2.1861(14) . ? Mn1 O5 2.1906(16) . ? Mn1 O1 2.2197(14) . ? Mn2 O2 2.1076(16) . ? Mn2 O12 2.1335(14) 2_645 ? Mn2 O3 2.1748(15) . ? Mn2 O5 2.1820(15) 2_645 ? Mn2 O1 2.2098(15) 2_645 ? Mn2 O7 2.2220(14) . ? Mn3 O4 2.1597(14) 3_655 ? Mn3 O4 2.1597(14) . ? Mn3 O6 2.1599(16) 3_655 ? Mn3 O6 2.1599(16) . ? Mn3 O9 2.2004(15) 3_655 ? Mn3 O9 2.2004(15) . ? Mn4 O10 2.1385(16) 3 ? Mn4 O10 2.1385(16) . ? Mn4 O8 2.1541(15) . ? Mn4 O8 2.1541(15) 3 ? Mn4 O11 2.2056(14) 3 ? Mn4 O11 2.2056(14) . ? O1 C1 1.275(3) . ? O1 Mn2 2.2098(15) 2_655 ? O2 C1 1.242(3) . ? O3 C2 1.271(3) . ? O4 C2 1.235(3) . ? O5 C3 1.280(3) . ? O5 Mn2 2.1820(15) 2_655 ? O6 C3 1.232(3) . ? O7 C4 1.273(3) . ? O8 C4 1.236(3) . ? O9 C5 1.281(3) . ? O10 C5 1.232(3) . ? O11 C6 1.272(3) . ? O12 C6 1.238(3) . ? O12 Mn2 2.1335(14) 2_655 ? C1 H1 1.04(2) . ? C2 H2 1.02(3) . ? C3 H3 0.99(3) . ? C4 H4 0.97(3) . ? C5 H5 1.00(2) . ? C6 H6 0.97(2) . ? C7 C12 1.372(4) . ? C7 C8 1.384(4) . ? C7 H7 0.96(3) . ? C8 C9 1.379(4) . ? C8 H8 0.94(3) . ? C9 C10 1.379(4) . ? C9 H9 0.99(3) . ? C10 C11 1.380(4) . ? C10 H10 1.02(4) . ? C11 C12 1.384(4) . ? C11 H11 0.92(3) . ? C12 H12 0.91(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 O9 Mn1 O11 95.17(5) . . ? O9 Mn1 O7 98.07(6) . . ? O11 Mn1 O7 95.16(6) . . ? O9 Mn1 O3 91.99(6) . . ? O11 Mn1 O3 170.38(6) . . ? O7 Mn1 O3 77.44(5) . . ? O9 Mn1 O5 95.98(6) . . ? O11 Mn1 O5 94.57(6) . . ? O7 Mn1 O5 162.09(5) . . ? O3 Mn1 O5 91.06(6) . . ? O9 Mn1 O1 173.75(6) . . ? O11 Mn1 O1 87.24(5) . . ? O7 Mn1 O1 87.44(6) . . ? O3 Mn1 O1 86.30(5) . . ? O5 Mn1 O1 78.05(5) . . ? O2 Mn2 O12 98.17(6) . 2_645 ? O2 Mn2 O3 96.12(6) . . ? O12 Mn2 O3 90.76(6) 2_645 . ? O2 Mn2 O5 93.31(6) . 2_645 ? O12 Mn2 O5 91.82(6) 2_645 2_645 ? O3 Mn2 O5 169.77(6) . 2_645 ? O2 Mn2 O1 169.40(6) . 2_645 ? O12 Mn2 O1 88.83(6) 2_645 2_645 ? O3 Mn2 O1 91.72(6) . 2_645 ? O5 Mn2 O1 78.44(6) 2_645 2_645 ? O2 Mn2 O7 89.13(6) . . ? O12 Mn2 O7 166.23(6) 2_645 . ? O3 Mn2 O7 76.81(5) . . ? O5 Mn2 O7 99.43(6) 2_645 . ? O1 Mn2 O7 85.70(5) 2_645 . ? O4 Mn3 O4 180.00(11) 3_655 . ? O4 Mn3 O6 88.79(6) 3_655 3_655 ? O4 Mn3 O6 91.21(6) . 3_655 ? O4 Mn3 O6 91.21(6) 3_655 . ? O4 Mn3 O6 88.79(6) . . ? O6 Mn3 O6 180.00(9) 3_655 . ? O4 Mn3 O9 94.38(6) 3_655 3_655 ? O4 Mn3 O9 85.62(6) . 3_655 ? O6 Mn3 O9 91.76(6) 3_655 3_655 ? O6 Mn3 O9 88.24(6) . 3_655 ? O4 Mn3 O9 85.62(6) 3_655 . ? O4 Mn3 O9 94.38(6) . . ? O6 Mn3 O9 88.24(6) 3_655 . ? O6 Mn3 O9 91.76(6) . . ? O9 Mn3 O9 180.00(11) 3_655 . ? O10 Mn4 O10 180.00(6) 3 . ? O10 Mn4 O8 92.10(6) 3 . ? O10 Mn4 O8 87.90(6) . . ? O10 Mn4 O8 87.90(6) 3 3 ? O10 Mn4 O8 92.10(6) . 3 ? O8 Mn4 O8 180.00(10) . 3 ? O10 Mn4 O11 92.21(6) 3 3 ? O10 Mn4 O11 87.79(6) . 3 ? O8 Mn4 O11 86.07(5) . 3 ? O8 Mn4 O11 93.93(5) 3 3 ? O10 Mn4 O11 87.79(6) 3 . ? O10 Mn4 O11 92.21(6) . . ? O8 Mn4 O11 93.93(5) . . ? O8 Mn4 O11 86.07(5) 3 . ? O11 Mn4 O11 180.00(15) 3 . ? C1 O1 Mn2 127.91(14) . 2_655 ? C1 O1 Mn1 133.54(14) . . ? Mn2 O1 Mn1 96.16(5) 2_655 . ? C1 O2 Mn2 128.72(14) . . ? C2 O3 Mn2 125.93(14) . . ? C2 O3 Mn1 132.84(14) . . ? Mn2 O3 Mn1 99.19(6) . . ? C2 O4 Mn3 137.21(15) . . ? C3 O5 Mn2 127.78(15) . 2_655 ? C3 O5 Mn1 133.57(15) . . ? Mn2 O5 Mn1 97.83(6) 2_655 . ? C3 O6 Mn3 136.63(16) . . ? C4 O7 Mn1 134.43(14) . . ? C4 O7 Mn2 127.51(14) . . ? Mn1 O7 Mn2 97.92(6) . . ? C4 O8 Mn4 136.07(15) . . ? C5 O9 Mn1 128.00(14) . . ? C5 O9 Mn3 117.88(14) . . ? Mn1 O9 Mn3 114.11(6) . . ? C5 O10 Mn4 141.31(15) . . ? C6 O11 Mn1 129.00(13) . . ? C6 O11 Mn4 119.29(13) . . ? Mn1 O11 Mn4 111.69(7) . . ? C6 O12 Mn2 132.54(15) . 2_655 ? O2 C1 O1 125.8(2) . . ? O2 C1 H1 120.0(12) . . ? O1 C1 H1 114.2(12) . . ? O4 C2 O3 125.8(2) . . ? O4 C2 H2 117.1(16) . . ? O3 C2 H2 117.2(16) . . ? O6 C3 O5 126.2(2) . . ? O6 C3 H3 118.8(16) . . ? O5 C3 H3 114.9(16) . . ? O8 C4 O7 126.3(2) . . ? O8 C4 H4 118.7(15) . . ? O7 C4 H4 115.0(15) . . ? O10 C5 O9 125.9(2) . . ? O10 C5 H5 118.3(14) . . ? O9 C5 H5 115.8(14) . . ? O12 C6 O11 126.6(2) . . ? O12 C6 H6 117.9(15) . . ? O11 C6 H6 115.5(15) . . ? C12 C7 C8 119.6(3) . . ? C12 C7 H7 119.8(17) . . ? C8 C7 H7 120.5(17) . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 118.3(19) . . ? C7 C8 H8 121.2(18) . . ? C8 C9 C10 119.5(3) . . ? C8 C9 H9 121.2(15) . . ? C10 C9 H9 119.4(15) . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 118(2) . . ? C11 C10 H10 122(2) . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 120(2) . . ? C12 C11 H11 120(2) . . ? C7 C12 C11 120.4(3) . . ? C7 C12 H12 116.3(15) . . ? C11 C12 H12 123.2(15) . . ? 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 C1 H1 O3 1.04(2) 2.79(2) 3.399(3) 117.5(14) 2_655 C1 H1 O6 1.04(2) 2.91(2) 3.766(3) 140.1(16) 4_566 C1 H1 O9 1.04(2) 3.04(2) 3.933(3) 144.7(16) 2_655 C2 H2 O12 1.02(3) 2.68(3) 3.245(3) 115.0(19) 2_645 C3 H3 O2 0.99(3) 2.69(3) 3.281(3) 119(2) 2_655 C4 H4 O5 0.97(3) 2.96(2) 3.551(2) 120.5(18) 2_645 C5 H5 O4 1.00(2) 2.59(2) 3.014(3) 105.2(16) 3_655 C5 H5 O6 1.00(2) 2.66(2) 3.201(3) 114.2(15) 3_655 C6 H6 O8 0.97(2) 2.69(2) 3.149(3) 109.5(18) 3 C6 H6 O10 0.97(2) 2.60(3) 3.105(3) 112.5(18) 3 C7 H7 O8 0.96(3) 2.71(3) 3.371(3) 127(2) . C8 H8 O8 0.94(3) 2.89(3) 3.444(3) 119(2) . C8 H8 O10 0.94(3) 2.85(3) 3.482(3) 125(2) 3 C9 H9 O4 0.99(3) 2.75(3) 3.728(3) 168.0(19) 2_655 C10 H10 O6 1.02(4) 3.20(3) 3.654(3) 108(2) 4_566 C10 H10 O11 1.02(4) 2.96(4) 3.895(3) 154(3) 4_566 C10 H10 O12 1.02(4) 2.92(3) 3.543(3) 120(2) 4_566 C11 H11 O12 0.92(3) 2.84(3) 3.493(3) 129(2) 4_566 C12 H12 O10 0.91(3) 2.94(3) 3.674(3) 139.1(17) 4_556 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.566 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.091 ## END of data_6 data_7 _database_code_depnum_ccdc_archive 'CCDC 218690' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mn3(HCOO)6](I2)0.87 _chemical_formula_sum 'C6 H6 I1.74 Mn3 O12' _chemical_formula_weight 655.73 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 11.8341(16) _cell_length_b 10.1956(11) _cell_length_c 18.848(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.905(2) _cell_angle_gamma 90.00 _cell_volume 1794.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 82(2) _cell_measurement_reflns_used 12464 _cell_measurement_theta_min 3.2080 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1221 _exptl_absorpt_coefficient_mu 5.121 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8069 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 82(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29902 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4083 _reflns_number_gt 3326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0394P)^2^+6.4897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00088(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4083 _refine_ls_number_parameters 247 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _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 0.37622(7) 0.08303(6) 0.13012(4) 0.01145(16) Uani 1 1 d . . . Mn2 Mn 0.57699(7) -0.10455(6) 0.31418(5) 0.01259(16) Uani 1 1 d . . . Mn3 Mn 0.5000 0.0000 0.0000 0.0136(2) Uani 1 2 d S . . Mn4 Mn 0.0000 0.0000 0.0000 0.0131(2) Uani 1 2 d S . . O1 O 0.4508(3) 0.2032(3) 0.2491(2) 0.0142(7) Uani 1 1 d . . . O2 O 0.5610(4) 0.0690(3) 0.3684(2) 0.0178(7) Uani 1 1 d . . . O3 O 0.5891(3) -0.0069(3) 0.2171(2) 0.0150(7) Uani 1 1 d . . . O4 O 0.6763(4) -0.0033(3) 0.1409(2) 0.0212(7) Uani 1 1 d . . . O5 O 0.4504(4) 0.2619(3) 0.1066(2) 0.0151(7) Uani 1 1 d . . . O6 O 0.4893(4) 0.2107(3) 0.0078(2) 0.0190(7) Uani 1 1 d . . . O7 O 0.3454(3) -0.0767(3) 0.1956(2) 0.0148(7) Uani 1 1 d . . . O8 O 0.1138(4) -0.1233(3) 0.1199(2) 0.0184(7) Uani 1 1 d . . . O9 O 0.3348(3) -0.0247(3) 0.0195(2) 0.0152(7) Uani 1 1 d . . . O10 O 0.1155(4) -0.0966(3) -0.0378(2) 0.0190(7) Uani 1 1 d . . . O11 O 0.1612(3) 0.1564(3) 0.0654(2) 0.0138(6) Uani 1 1 d . . . O12 O 0.1982(3) 0.3708(3) 0.0984(2) 0.0171(7) Uani 1 1 d . . . C1 C 0.5123(5) 0.1779(5) 0.3316(3) 0.0169(10) Uani 1 1 d . . . C2 C 0.6894(5) -0.0172(4) 0.2101(3) 0.0158(9) Uani 1 1 d . . . C3 C 0.4747(5) 0.2901(5) 0.0509(3) 0.0170(10) Uani 1 1 d . . . C4 C 0.2431(5) -0.1418(5) 0.1818(3) 0.0159(9) Uani 1 1 d . . . C5 C 0.2203(5) -0.0910(4) -0.0368(3) 0.0166(10) Uani 1 1 d . . . C6 C 0.1200(5) 0.2738(5) 0.0617(3) 0.0167(10) Uani 1 1 d . . . H1 H 0.540(7) 0.257(6) 0.378(4) 0.030(16) Uiso 1 1 d . . . H2 H 0.793(7) -0.041(6) 0.271(4) 0.040(17) Uiso 1 1 d . . . H3 H 0.489(6) 0.386(5) 0.048(3) 0.016(13) Uiso 1 1 d . . . H4 H 0.277(7) -0.221(6) 0.229(4) 0.037(18) Uiso 1 1 d . . . H5 H 0.216(6) -0.149(5) -0.087(4) 0.019(14) Uiso 1 1 d . . . H6 H 0.008(7) 0.283(6) 0.028(4) 0.028(16) Uiso 1 1 d . . . I1 I -0.04941(4) -0.25854(3) 0.15997(2) 0.01728(12) Uani 0.87 1 d P . . I2 I -0.1828(6) -0.3847(7) 0.2148(4) 0.0274(6) Uani 0.57(3) 1 d P . . I3 I -0.1841(12) -0.4031(16) 0.2034(10) 0.036(2) Uani 0.31(3) 1 d P . . 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 0.0111(3) 0.0115(3) 0.0115(3) -0.0001(3) 0.0069(3) -0.0001(2) Mn2 0.0130(3) 0.0112(3) 0.0129(3) 0.0011(3) 0.0076(3) 0.0006(3) Mn3 0.0131(5) 0.0149(5) 0.0141(5) -0.0007(4) 0.0091(4) -0.0009(4) Mn4 0.0106(5) 0.0135(5) 0.0136(5) -0.0008(4) 0.0066(4) -0.0016(4) O1 0.0173(16) 0.0115(15) 0.0108(15) 0.0017(12) 0.0070(13) -0.0005(13) O2 0.0243(18) 0.0147(16) 0.0166(16) 0.0027(13) 0.0137(15) 0.0039(13) O3 0.0161(16) 0.0150(16) 0.0142(15) 0.0012(13) 0.0094(14) 0.0020(13) O4 0.0186(18) 0.0291(19) 0.0172(17) 0.0009(15) 0.0117(15) 0.0006(15) O5 0.0190(17) 0.0139(15) 0.0173(16) -0.0010(13) 0.0136(14) -0.0019(13) O6 0.0246(18) 0.0176(16) 0.0216(17) -0.0014(14) 0.0177(16) -0.0019(14) O7 0.0130(16) 0.0138(15) 0.0165(16) -0.0002(13) 0.0085(14) -0.0017(12) O8 0.0141(17) 0.0215(17) 0.0163(16) 0.0009(14) 0.0077(14) -0.0021(13) O9 0.0152(16) 0.0165(16) 0.0148(16) -0.0018(13) 0.0096(14) -0.0032(13) O10 0.0158(17) 0.0219(17) 0.0219(17) -0.0045(14) 0.0129(15) -0.0033(13) O11 0.0111(15) 0.0154(15) 0.0153(16) -0.0004(13) 0.0084(13) -0.0005(12) O12 0.0142(16) 0.0155(16) 0.0191(17) -0.0036(13) 0.0090(14) -0.0017(13) C1 0.019(2) 0.017(2) 0.017(2) 0.000(2) 0.012(2) 0.0008(19) C2 0.016(2) 0.015(2) 0.019(2) 0.0002(19) 0.012(2) -0.0001(18) C3 0.022(3) 0.013(2) 0.017(2) 0.0004(19) 0.013(2) -0.0002(19) C4 0.013(2) 0.016(2) 0.016(2) 0.0008(19) 0.0078(19) -0.0023(18) C5 0.019(2) 0.014(2) 0.016(2) -0.0022(19) 0.010(2) -0.0020(19) C6 0.013(2) 0.018(2) 0.015(2) -0.0010(19) 0.0065(19) 0.0011(19) I1 0.01285(18) 0.02226(19) 0.01764(19) 0.00603(14) 0.00983(15) -0.00007(14) I2 0.0244(7) 0.0356(13) 0.0315(10) 0.0155(9) 0.0220(7) 0.0056(6) I3 0.0342(16) 0.042(4) 0.048(4) 0.021(3) 0.033(2) 0.0023(17) _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 O9 2.130(3) . ? Mn1 O11 2.170(3) . ? Mn1 O5 2.184(3) . ? Mn1 O3 2.190(3) . ? Mn1 O7 2.204(3) . ? Mn1 O1 2.208(3) . ? Mn2 O2 2.110(3) . ? Mn2 O12 2.114(3) 2_645 ? Mn2 O3 2.164(3) . ? Mn2 O5 2.187(3) 2_645 ? Mn2 O1 2.211(3) 2_645 ? Mn2 O7 2.249(3) . ? Mn3 O4 2.144(3) 3_655 ? Mn3 O4 2.144(3) . ? Mn3 O6 2.162(3) 3_655 ? Mn3 O6 2.162(3) . ? Mn3 O9 2.215(3) 3_655 ? Mn3 O9 2.215(3) . ? Mn4 O10 2.130(3) 3 ? Mn4 O10 2.130(3) . ? Mn4 O8 2.182(3) . ? Mn4 O8 2.182(3) 3 ? Mn4 O11 2.194(3) . ? Mn4 O11 2.194(3) 3 ? O1 C1 1.274(6) . ? O1 Mn2 2.211(3) 2_655 ? O2 C1 1.247(6) . ? O3 C2 1.278(6) . ? O4 C2 1.224(6) . ? O5 C3 1.280(6) . ? O5 Mn2 2.187(3) 2_655 ? O6 C3 1.233(6) . ? O7 C4 1.260(6) . ? O8 C4 1.243(6) . ? O9 C5 1.285(6) . ? O10 C5 1.231(6) . ? O11 C6 1.279(6) . ? O12 C6 1.236(6) . ? O12 Mn2 2.114(3) 2_655 ? C1 H1 1.09(6) . ? C2 H2 1.07(7) . ? C3 H3 1.00(5) . ? C4 H4 1.08(6) . ? C5 H5 1.09(5) . ? C6 H6 1.06(6) . ? I1 I3 2.644(12) . ? I1 I2 2.687(7) . ? 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 O9 Mn1 O11 98.15(12) . . ? O9 Mn1 O5 96.39(12) . . ? O11 Mn1 O5 94.39(12) . . ? O9 Mn1 O3 89.11(12) . . ? O11 Mn1 O3 167.73(12) . . ? O5 Mn1 O3 94.63(12) . . ? O9 Mn1 O7 98.57(12) . . ? O11 Mn1 O7 91.70(12) . . ? O5 Mn1 O7 162.88(12) . . ? O3 Mn1 O7 77.37(12) . . ? O9 Mn1 O1 171.12(12) . . ? O11 Mn1 O1 88.80(12) . . ? O5 Mn1 O1 77.47(12) . . ? O3 Mn1 O1 85.04(12) . . ? O7 Mn1 O1 86.68(12) . . ? O2 Mn2 O12 99.60(13) . 2_645 ? O2 Mn2 O3 95.52(12) . . ? O12 Mn2 O3 90.47(12) 2_645 . ? O2 Mn2 O5 95.51(12) . 2_645 ? O12 Mn2 O5 92.14(12) 2_645 2_645 ? O3 Mn2 O5 168.08(12) . 2_645 ? O2 Mn2 O1 167.66(13) . 2_645 ? O12 Mn2 O1 90.80(12) 2_645 2_645 ? O3 Mn2 O1 91.00(12) . 2_645 ? O5 Mn2 O1 77.34(12) 2_645 2_645 ? O2 Mn2 O7 87.63(12) . . ? O12 Mn2 O7 166.12(13) 2_645 . ? O3 Mn2 O7 76.97(12) . . ? O5 Mn2 O7 98.98(12) 2_645 . ? O1 Mn2 O7 83.63(12) 2_645 . ? O4 Mn3 O4 180.0(3) 3_655 . ? O4 Mn3 O6 89.11(13) 3_655 3_655 ? O4 Mn3 O6 90.89(13) . 3_655 ? O4 Mn3 O6 90.89(13) 3_655 . ? O4 Mn3 O6 89.11(13) . . ? O6 Mn3 O6 180.00(19) 3_655 . ? O4 Mn3 O9 94.55(12) 3_655 3_655 ? O4 Mn3 O9 85.45(12) . 3_655 ? O6 Mn3 O9 90.41(12) 3_655 3_655 ? O6 Mn3 O9 89.59(12) . 3_655 ? O4 Mn3 O9 85.45(12) 3_655 . ? O4 Mn3 O9 94.55(12) . . ? O6 Mn3 O9 89.59(12) 3_655 . ? O6 Mn3 O9 90.41(12) . . ? O9 Mn3 O9 180.00(14) 3_655 . ? O10 Mn4 O10 180.00(13) 3 . ? O10 Mn4 O8 92.02(13) 3 . ? O10 Mn4 O8 87.98(13) . . ? O10 Mn4 O8 87.98(13) 3 3 ? O10 Mn4 O8 92.02(13) . 3 ? O8 Mn4 O8 180.0(2) . 3 ? O10 Mn4 O11 89.51(12) 3 . ? O10 Mn4 O11 90.49(12) . . ? O8 Mn4 O11 93.82(12) . . ? O8 Mn4 O11 86.18(12) 3 . ? O10 Mn4 O11 90.49(12) 3 3 ? O10 Mn4 O11 89.51(12) . 3 ? O8 Mn4 O11 86.18(12) . 3 ? O8 Mn4 O11 93.82(12) 3 3 ? O11 Mn4 O11 180.0(4) . 3 ? C1 O1 Mn1 134.4(3) . . ? C1 O1 Mn2 128.4(3) . 2_655 ? Mn1 O1 Mn2 96.32(12) . 2_655 ? C1 O2 Mn2 128.7(3) . . ? C2 O3 Mn2 126.7(3) . . ? C2 O3 Mn1 132.2(3) . . ? Mn2 O3 Mn1 100.52(13) . . ? C2 O4 Mn3 135.4(3) . . ? C3 O5 Mn1 132.5(3) . . ? C3 O5 Mn2 128.5(3) . 2_655 ? Mn1 O5 Mn2 97.74(13) . 2_655 ? C3 O6 Mn3 137.3(3) . . ? C4 O7 Mn1 137.9(3) . . ? C4 O7 Mn2 124.6(3) . . ? Mn1 O7 Mn2 97.47(12) . . ? C4 O8 Mn4 132.9(3) . . ? C5 O9 Mn1 124.8(3) . . ? C5 O9 Mn3 120.9(3) . . ? Mn1 O9 Mn3 114.08(14) . . ? C5 O10 Mn4 145.2(3) . . ? C6 O11 Mn1 129.0(3) . . ? C6 O11 Mn4 118.6(3) . . ? Mn1 O11 Mn4 112.35(13) . . ? C6 O12 Mn2 133.0(3) . 2_655 ? O2 C1 O1 125.6(4) . . ? O2 C1 H1 114(3) . . ? O1 C1 H1 120(3) . . ? O4 C2 O3 125.7(4) . . ? O4 C2 H2 119(4) . . ? O3 C2 H2 116(4) . . ? O6 C3 O5 125.9(4) . . ? O6 C3 H3 121(3) . . ? O5 C3 H3 113(3) . . ? O8 C4 O7 125.9(4) . . ? O8 C4 H4 120(3) . . ? O7 C4 H4 114(3) . . ? O10 C5 O9 125.4(4) . . ? O10 C5 H5 117(3) . . ? O9 C5 H5 118(3) . . ? O12 C6 O11 126.1(4) . . ? O12 C6 H6 120(3) . . ? O11 C6 H6 114(3) . . ? I3 I1 I2 5.9(5) . . ? 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 C1 H1 O3 1.09(6) 2.82(6) 3.355(6) 110(4) 2_655 C1 H1 O6 1.09(6) 2.87(6) 3.675(6) 131(4) 4_566 C1 H1 O9 1.09(6) 2.71(6) 3.756(6) 161(5) 2_655 C2 H2 O12 1.07(7) 2.56(6) 3.193(6) 117(4) 2_645 C3 H3 O2 1.00(5) 2.73(5) 3.371(6) 122(4) 2_655 C4 H4 O5 1.08(6) 2.79(6) 3.501(6) 123(4) 2_645 C5 H5 O4 1.09(5) 2.58(5) 3.037(6) 104(3) 3_655 C5 H5 O6 1.09(5) 2.90(5) 3.360(6) 106(3) 3_655 C6 H6 O8 1.06(6) 2.75(6) 3.176(6) 104(4) 3 C6 H6 O10 1.06(6) 2.47(6) 3.112(6) 118(4) 3 C4 H4 I1 1.08(6) 3.25(6) 3.438(5) 91(4) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.034 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.152 ## END of data_7