# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kimoon Kim.' 'Jong-San Chang.' 'Young Kyu Hwang.' 'Hyunuk Kim.' 'Denis G Samsonenko' 'Minyoung Yoon.' 'Ji Woong Yoon.' _publ_contact_author_name 'Kimoon Kim' _publ_contact_author_email KKIM@POSTECH.AC.KR _publ_section_title ; Temperature-Triggered Gate Opening for Gas Adsorption in Microporous Manganese Formate ; # Attachment 'KimoonKim(CIF-Mg(HCOO)2-196K).cif' data_p21_n _database_code_depnum_ccdc_archive 'CCDC 693548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Mg(II) Formate' _chemical_melting_point ? _chemical_formula_moiety 'C2 H2 Mg O4' _chemical_formula_sum 'C2 H2 Mg O4' _chemical_formula_weight 114.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0017 '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 -0.0041 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0468 0.0388 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3590(10) _cell_length_b 9.8850(10) _cell_length_c 14.5840(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.3700(10) _cell_angle_gamma 90.00 _cell_volume 1637.1(2) _cell_formula_units_Z 12 _cell_measurement_temperature 196(2) _cell_measurement_reflns_used 2878 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 26.00 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9294 _exptl_absorpt_correction_T_max 0.9756 _exptl_absorpt_process_details HKL2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 196(2) _diffrn_radiation_wavelength 0.73000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PAL 4A MXW Beamline' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'ADSC Quantum 210' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5357 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2878 _reflns_number_gt 2694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ADSC Quantum software' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Materials Studio 4.1' _computing_publication_material 'Materials Studio 4.1' _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^)+(0.0572P)^2^+0.3970P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2878 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Mg1 Mg 0.25624(4) 0.07763(4) 0.13469(3) 0.01131(15) Uani 1 1 d . . . Mg2 Mg 0.0000 0.0000 0.0000 0.01431(18) Uani 1 2 d S . . Mg3 Mg 0.26033(4) 0.38684(4) 0.19071(3) 0.01247(15) Uani 1 1 d . . . Mg4 Mg 0.5000 0.0000 0.0000 0.01481(18) Uani 1 2 d S . . O1 O 0.13080(8) -0.00857(9) 0.21943(7) 0.0142(2) Uani 1 1 d . . . O2 O 0.15673(8) 0.25443(9) 0.11163(6) 0.0148(2) Uani 1 1 d . . . O3 O 0.30704(8) 0.19857(9) 0.24709(6) 0.0144(2) Uani 1 1 d . . . O4 O 0.39855(8) 0.15113(9) 0.06296(6) 0.0152(2) Uani 1 1 d . . . O5 O 0.34937(8) -0.08267(9) 0.19604(7) 0.0148(2) Uani 1 1 d . . . O6 O 0.18312(8) -0.02597(10) 0.02483(7) 0.0149(2) Uani 1 1 d . . . O7 O -0.03668(9) -0.00178(11) 0.13763(7) 0.0226(3) Uani 1 1 d . . . O8 O 0.01984(9) 0.20660(11) 0.00391(7) 0.0220(3) Uani 1 1 d . . . O9 O 0.38848(9) 0.37161(10) 0.09732(7) 0.0188(2) Uani 1 1 d . . . O10 O 0.51676(9) -0.10730(11) 0.12039(7) 0.0236(3) Uani 1 1 d . . . O11 O 0.35009(9) -0.10484(11) -0.03291(7) 0.0217(3) Uani 1 1 d . . . O12 O 0.31438(9) 0.05526(10) 0.36560(7) 0.0191(2) Uani 1 1 d . . . C1 C 0.02008(12) -0.01842(15) 0.20926(10) 0.0185(3) Uani 1 1 d . . . H1 H -0.0230 -0.0408 0.2622 0.022 Uiso 1 1 calc R . . C2 C 0.07862(13) 0.28579(15) 0.05137(10) 0.0198(3) Uani 1 1 d . . . H2 H 0.0642 0.3795 0.0421 0.024 Uiso 1 1 calc R . . C3 C 0.32948(12) 0.16759(14) 0.33031(10) 0.0174(3) Uani 1 1 d . . . H3 H 0.3607 0.2370 0.3689 0.021 Uiso 1 1 calc R . . C4 C 0.43044(12) 0.27471(14) 0.05628(10) 0.0187(3) Uani 1 1 d . . . H4 H 0.4925 0.2936 0.0157 0.022 Uiso 1 1 calc R . . C5 C 0.45097(13) -0.13227(15) 0.18382(10) 0.0207(3) Uani 1 1 d . . . H5 H 0.4790 -0.1953 0.2284 0.025 Uiso 1 1 calc R . . C6 C 0.24262(12) -0.09956(15) -0.02966(10) 0.0180(3) Uani 1 1 d . . . H6 H 0.1992 -0.1552 -0.0714 0.022 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0090(2) 0.0134(2) 0.0115(3) -0.00034(16) 0.00038(17) -0.00012(16) Mg2 0.0084(3) 0.0192(4) 0.0153(4) -0.0020(2) -0.0020(2) 0.0005(2) Mg3 0.0115(3) 0.0129(3) 0.0130(3) -0.00129(16) 0.00026(18) 0.00022(16) Mg4 0.0096(3) 0.0187(4) 0.0163(4) -0.0023(2) 0.0036(3) 0.0013(2) O1 0.0104(5) 0.0169(5) 0.0154(5) 0.0027(4) 0.0001(4) -0.0007(4) O2 0.0121(5) 0.0159(5) 0.0162(5) -0.0011(4) -0.0025(4) 0.0012(4) O3 0.0164(5) 0.0142(5) 0.0125(5) 0.0001(3) -0.0013(4) 0.0002(4) O4 0.0126(5) 0.0156(5) 0.0176(5) -0.0016(4) 0.0043(4) -0.0005(4) O5 0.0120(5) 0.0163(5) 0.0161(5) 0.0015(4) 0.0024(4) 0.0017(4) O6 0.0094(5) 0.0203(5) 0.0148(5) -0.0040(4) -0.0005(4) 0.0012(4) O7 0.0128(5) 0.0384(7) 0.0164(6) 0.0005(4) -0.0019(4) 0.0004(4) O8 0.0189(5) 0.0204(6) 0.0262(6) -0.0015(4) -0.0103(4) -0.0010(4) O9 0.0193(5) 0.0172(5) 0.0203(6) -0.0021(4) 0.0068(4) -0.0009(4) O10 0.0167(5) 0.0340(6) 0.0205(6) 0.0042(4) 0.0062(4) 0.0078(4) O11 0.0108(5) 0.0259(6) 0.0286(6) -0.0081(4) 0.0032(4) 0.0006(4) O12 0.0256(6) 0.0164(5) 0.0152(5) 0.0014(4) -0.0036(4) -0.0031(4) C1 0.0124(7) 0.0271(8) 0.0159(8) 0.0016(6) 0.0023(6) -0.0008(6) C2 0.0189(7) 0.0163(7) 0.0239(8) 0.0007(6) -0.0070(6) 0.0020(6) C3 0.0208(7) 0.0157(7) 0.0155(8) -0.0017(5) -0.0036(6) -0.0012(5) C4 0.0153(7) 0.0207(7) 0.0203(8) -0.0004(6) 0.0072(6) -0.0019(6) C5 0.0179(7) 0.0249(8) 0.0193(8) 0.0048(6) 0.0023(6) 0.0084(6) C6 0.0132(7) 0.0227(7) 0.0181(8) -0.0065(6) -0.0019(5) 0.0004(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. ; 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 Mg1 O6 2.0596(10) . ? Mg1 O4 2.0775(10) . ? Mg1 O1 2.0899(10) . ? Mg1 O5 2.0941(10) . ? Mg1 O3 2.0986(10) . ? Mg1 O2 2.1040(11) . ? Mg1 Mg3 3.1639(7) . ? Mg1 Mg3 3.1780(6) 2_545 ? Mg1 Mg4 3.5177(5) . ? Mg1 Mg2 3.5560(5) . ? Mg2 O8 2.0553(11) . ? Mg2 O8 2.0553(11) 3 ? Mg2 O7 2.0598(11) . ? Mg2 O7 2.0598(11) 3 ? Mg2 O6 2.1184(9) 3 ? Mg2 O6 2.1184(9) . ? Mg2 Mg1 3.5560(5) 3 ? Mg3 O9 2.0227(11) . ? Mg3 O12 2.0330(11) 2 ? Mg3 O1 2.0587(11) 2 ? Mg3 O2 2.0887(10) . ? Mg3 O3 2.0977(10) . ? Mg3 O5 2.1143(10) 2 ? Mg3 Mg1 3.1780(6) 2 ? Mg4 O11 2.0408(10) 3_655 ? Mg4 O11 2.0408(10) . ? Mg4 O10 2.0562(11) 3_655 ? Mg4 O10 2.0562(11) . ? Mg4 O4 2.1103(9) . ? Mg4 O4 2.1103(9) 3_655 ? Mg4 Mg1 3.5177(5) 3_655 ? O1 C1 1.2666(18) . ? O1 Mg3 2.0587(11) 2_545 ? O2 C2 1.2722(18) . ? O3 C3 1.2716(17) . ? O4 C4 1.2786(17) . ? O5 C5 1.2705(18) . ? O5 Mg3 2.1143(10) 2_545 ? O6 C6 1.2818(17) . ? O7 C1 1.2255(18) . ? O8 C2 1.2311(18) . ? O9 C4 1.2315(18) . ? O10 C5 1.2280(19) . ? O11 C6 1.2239(18) . ? O12 C3 1.2375(18) . ? O12 Mg3 2.0330(11) 2_545 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 O6 Mg1 O4 94.95(4) . . ? O6 Mg1 O1 89.39(4) . . ? O4 Mg1 O1 171.90(4) . . ? O6 Mg1 O5 98.41(4) . . ? O4 Mg1 O5 95.08(4) . . ? O1 Mg1 O5 77.49(4) . . ? O6 Mg1 O3 171.55(4) . . ? O4 Mg1 O3 89.51(4) . . ? O1 Mg1 O3 87.07(4) . . ? O5 Mg1 O3 88.32(4) . . ? O6 Mg1 O2 94.80(4) . . ? O4 Mg1 O2 92.90(4) . . ? O1 Mg1 O2 93.55(4) . . ? O5 Mg1 O2 163.90(4) . . ? O3 Mg1 O2 77.78(4) . . ? O6 Mg1 Mg3 133.19(3) . . ? O4 Mg1 Mg3 77.61(3) . . ? O1 Mg1 Mg3 104.31(3) . . ? O5 Mg1 Mg3 128.06(3) . . ? O3 Mg1 Mg3 41.05(3) . . ? O2 Mg1 Mg3 40.83(3) . . ? O6 Mg1 Mg3 107.32(3) . 2_545 ? O4 Mg1 Mg3 132.28(3) . 2_545 ? O1 Mg1 Mg3 39.64(3) . 2_545 ? O5 Mg1 Mg3 41.20(3) . 2_545 ? O3 Mg1 Mg3 74.49(3) . 2_545 ? O2 Mg1 Mg3 125.39(3) . 2_545 ? Mg3 Mg1 Mg3 111.542(15) . 2_545 ? O6 Mg1 Mg4 76.43(3) . . ? O4 Mg1 Mg4 33.15(3) . . ? O1 Mg1 Mg4 142.95(3) . . ? O5 Mg1 Mg4 71.17(3) . . ? O3 Mg1 Mg4 110.80(3) . . ? O2 Mg1 Mg4 121.26(3) . . ? Mg3 Mg1 Mg4 110.366(14) . . ? Mg3 Mg1 Mg4 112.363(15) 2_545 . ? O6 Mg1 Mg2 32.17(3) . . ? O4 Mg1 Mg2 115.71(3) . . ? O1 Mg1 Mg2 71.22(3) . . ? O5 Mg1 Mg2 118.11(3) . . ? O3 Mg1 Mg2 139.51(3) . . ? O2 Mg1 Mg2 70.22(3) . . ? Mg3 Mg1 Mg2 110.970(14) . . ? Mg3 Mg1 Mg2 104.548(14) 2_545 . ? Mg4 Mg1 Mg2 106.815(13) . . ? O8 Mg2 O8 180.00(6) . 3 ? O8 Mg2 O7 90.35(4) . . ? O8 Mg2 O7 89.65(4) 3 . ? O8 Mg2 O7 89.65(4) . 3 ? O8 Mg2 O7 90.35(4) 3 3 ? O7 Mg2 O7 180.00(8) . 3 ? O8 Mg2 O6 89.48(4) . 3 ? O8 Mg2 O6 90.52(4) 3 3 ? O7 Mg2 O6 86.96(4) . 3 ? O7 Mg2 O6 93.04(4) 3 3 ? O8 Mg2 O6 90.52(4) . . ? O8 Mg2 O6 89.48(4) 3 . ? O7 Mg2 O6 93.04(4) . . ? O7 Mg2 O6 86.96(4) 3 . ? O6 Mg2 O6 180.00(5) 3 . ? O8 Mg2 Mg1 108.51(3) . 3 ? O8 Mg2 Mg1 71.49(3) 3 3 ? O7 Mg2 Mg1 110.76(3) . 3 ? O7 Mg2 Mg1 69.24(3) 3 3 ? O6 Mg2 Mg1 31.17(3) 3 3 ? O6 Mg2 Mg1 148.83(3) . 3 ? O8 Mg2 Mg1 71.49(3) . . ? O8 Mg2 Mg1 108.51(3) 3 . ? O7 Mg2 Mg1 69.24(3) . . ? O7 Mg2 Mg1 110.76(3) 3 . ? O6 Mg2 Mg1 148.83(3) 3 . ? O6 Mg2 Mg1 31.17(3) . . ? Mg1 Mg2 Mg1 180.000(12) 3 . ? O9 Mg3 O12 95.11(4) . 2 ? O9 Mg3 O1 92.01(4) . 2 ? O12 Mg3 O1 94.84(4) 2 2 ? O9 Mg3 O2 89.23(4) . . ? O12 Mg3 O2 93.78(4) 2 . ? O1 Mg3 O2 171.14(4) 2 . ? O9 Mg3 O3 91.07(4) . . ? O12 Mg3 O3 169.78(5) 2 . ? O1 Mg3 O3 93.07(4) 2 . ? O2 Mg3 O3 78.13(4) . . ? O9 Mg3 O5 169.64(5) . 2 ? O12 Mg3 O5 87.17(4) 2 2 ? O1 Mg3 O5 77.72(4) 2 2 ? O2 Mg3 O5 100.71(4) . 2 ? O3 Mg3 O5 88.19(4) . 2 ? O9 Mg3 Mg1 76.15(3) . . ? O12 Mg3 Mg1 133.11(3) 2 . ? O1 Mg3 Mg1 130.88(3) 2 . ? O2 Mg3 Mg1 41.19(3) . . ? O3 Mg3 Mg1 41.08(3) . . ? O5 Mg3 Mg1 109.52(3) 2 . ? O9 Mg3 Mg1 129.87(3) . 2 ? O12 Mg3 Mg1 78.79(3) 2 2 ? O1 Mg3 Mg1 40.36(3) 2 2 ? O2 Mg3 Mg1 140.43(3) . 2 ? O3 Mg3 Mg1 103.39(3) . 2 ? O5 Mg3 Mg1 40.72(3) 2 2 ? Mg1 Mg3 Mg1 141.208(17) . 2 ? O11 Mg4 O11 180.00(8) 3_655 . ? O11 Mg4 O10 89.92(5) 3_655 3_655 ? O11 Mg4 O10 90.08(5) . 3_655 ? O11 Mg4 O10 90.08(5) 3_655 . ? O11 Mg4 O10 89.92(5) . . ? O10 Mg4 O10 180.00(6) 3_655 . ? O11 Mg4 O4 89.97(4) 3_655 . ? O11 Mg4 O4 90.03(4) . . ? O10 Mg4 O4 88.05(4) 3_655 . ? O10 Mg4 O4 91.95(4) . . ? O11 Mg4 O4 90.03(4) 3_655 3_655 ? O11 Mg4 O4 89.97(4) . 3_655 ? O10 Mg4 O4 91.95(4) 3_655 3_655 ? O10 Mg4 O4 88.05(4) . 3_655 ? O4 Mg4 O4 180.00(5) . 3_655 ? O11 Mg4 Mg1 114.92(3) 3_655 . ? O11 Mg4 Mg1 65.08(3) . . ? O10 Mg4 Mg1 107.83(3) 3_655 . ? O10 Mg4 Mg1 72.17(3) . . ? O4 Mg4 Mg1 32.57(3) . . ? O4 Mg4 Mg1 147.43(3) 3_655 . ? O11 Mg4 Mg1 65.08(3) 3_655 3_655 ? O11 Mg4 Mg1 114.92(3) . 3_655 ? O10 Mg4 Mg1 72.17(3) 3_655 3_655 ? O10 Mg4 Mg1 107.83(3) . 3_655 ? O4 Mg4 Mg1 147.43(3) . 3_655 ? O4 Mg4 Mg1 32.57(3) 3_655 3_655 ? Mg1 Mg4 Mg1 180.000(13) . 3_655 ? C1 O1 Mg3 127.99(9) . 2_545 ? C1 O1 Mg1 130.63(9) . . ? Mg3 O1 Mg1 100.00(4) 2_545 . ? C2 O2 Mg3 127.10(9) . . ? C2 O2 Mg1 132.53(9) . . ? Mg3 O2 Mg1 97.98(4) . . ? C3 O3 Mg3 129.11(9) . . ? C3 O3 Mg1 130.81(9) . . ? Mg3 O3 Mg1 97.87(4) . . ? C4 O4 Mg1 126.71(9) . . ? C4 O4 Mg4 118.98(8) . . ? Mg1 O4 Mg4 114.27(4) . . ? C5 O5 Mg1 133.11(9) . . ? C5 O5 Mg3 127.51(9) . 2_545 ? Mg1 O5 Mg3 98.08(4) . 2_545 ? C6 O6 Mg1 123.75(9) . . ? C6 O6 Mg2 119.54(9) . . ? Mg1 O6 Mg2 116.66(4) . . ? C1 O7 Mg2 135.83(10) . . ? C2 O8 Mg2 134.83(10) . . ? C4 O9 Mg3 132.71(9) . . ? C5 O10 Mg4 134.54(10) . . ? C6 O11 Mg4 142.80(10) . . ? C3 O12 Mg3 128.87(9) . 2_545 ? O7 C1 O1 126.17(13) . . ? O7 C1 H1 116.9 . . ? O1 C1 H1 116.9 . . ? O8 C2 O2 126.40(13) . . ? O8 C2 H2 116.8 . . ? O2 C2 H2 116.8 . . ? O12 C3 O3 125.90(13) . . ? O12 C3 H3 117.1 . . ? O3 C3 H3 117.1 . . ? O9 C4 O4 126.33(13) . . ? O9 C4 H4 116.8 . . ? O4 C4 H4 116.8 . . ? O10 C5 O5 126.81(14) . . ? O10 C5 H5 116.6 . . ? O5 C5 H5 116.6 . . ? O11 C6 O6 126.13(13) . . ? O11 C6 H6 116.9 . . ? O6 C6 H6 116.9 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.220 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.055 # Attachment 'KimoonKim(CIF-Mg(HCOO)2-90K).cif' data_p21_n2 _database_code_depnum_ccdc_archive 'CCDC 693549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Mg(II) Formate' _chemical_melting_point ? _chemical_formula_moiety 'C2 H2 Mg O4' _chemical_formula_sum 'C2 H2 Mg O4' _chemical_formula_weight 114.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0017 '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 -0.0041 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0468 0.0388 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3410(10) _cell_length_b 9.8490(10) _cell_length_c 14.5470(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.3880(10) _cell_angle_gamma 90.00 _cell_volume 1624.4(2) _cell_formula_units_Z 12 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2568 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 25.00 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9288 _exptl_absorpt_correction_T_max 0.9755 _exptl_absorpt_process_details HKL2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.73000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PAL 4A MXW Beamline' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'ADSC Quantum 210' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4820 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2568 _reflns_number_gt 2470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ADSC Quantum software' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Materials Studio 4.1' _computing_publication_material 'Materials Studio 4.1' _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^)+(0.0610P)^2^+0.4989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2568 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Mg1 Mg 0.25630(4) 0.07865(5) 0.13466(3) 0.01014(17) Uani 1 1 d . . . Mg2 Mg 0.0000 0.0000 0.0000 0.0118(2) Uani 1 2 d S . . Mg3 Mg 0.26041(4) 0.38846(5) 0.19005(3) 0.01062(18) Uani 1 1 d . . . Mg4 Mg 0.5000 0.0000 0.0000 0.0118(2) Uani 1 2 d S . . O1 O 0.13085(9) -0.00628(10) 0.22016(7) 0.0118(3) Uani 1 1 d . . . O2 O 0.15667(9) 0.25581(10) 0.11107(7) 0.0119(3) Uani 1 1 d . . . O3 O 0.30791(9) 0.20033(10) 0.24662(7) 0.0119(3) Uani 1 1 d . . . O4 O 0.39844(9) 0.15190(10) 0.06251(7) 0.0122(3) Uani 1 1 d . . . O5 O 0.34948(9) -0.08188(10) 0.19644(7) 0.0120(3) Uani 1 1 d . . . O6 O 0.18300(9) -0.02614(10) 0.02513(7) 0.0122(3) Uani 1 1 d . . . O7 O -0.03733(10) 0.00024(11) 0.13788(8) 0.0159(3) Uani 1 1 d . . . O8 O 0.01995(9) 0.20736(11) 0.00254(7) 0.0152(3) Uani 1 1 d . . . O9 O 0.38861(9) 0.37372(10) 0.09632(7) 0.0136(3) Uani 1 1 d . . . O10 O 0.51753(10) -0.10690(11) 0.12100(7) 0.0161(3) Uani 1 1 d . . . O11 O 0.35024(9) -0.10617(11) -0.03262(7) 0.0154(3) Uani 1 1 d . . . O12 O 0.31514(9) 0.05728(10) 0.36636(7) 0.0139(3) Uani 1 1 d . . . C1 C 0.01951(13) -0.01602(15) 0.21012(11) 0.0137(3) Uani 1 1 d . . . H1 H -0.0237 -0.0378 0.2633 0.016 Uiso 1 1 calc R . . C2 C 0.07874(13) 0.28741(15) 0.05008(10) 0.0142(3) Uani 1 1 d . . . H2 H 0.0646 0.3815 0.0403 0.017 Uiso 1 1 calc R . . C3 C 0.33073(13) 0.16996(15) 0.33051(10) 0.0131(3) Uani 1 1 d . . . H3 H 0.3624 0.2398 0.3688 0.016 Uiso 1 1 calc R . . C4 C 0.43056(13) 0.27603(15) 0.05515(10) 0.0138(3) Uani 1 1 d . . . H4 H 0.4925 0.2947 0.0142 0.017 Uiso 1 1 calc R . . C5 C 0.45151(13) -0.13176(16) 0.18478(11) 0.0148(4) Uani 1 1 d . . . H5 H 0.4796 -0.1945 0.2298 0.018 Uiso 1 1 calc R . . C6 C 0.24239(13) -0.10101(15) -0.02910(11) 0.0136(3) Uani 1 1 d . . . H6 H 0.1988 -0.1577 -0.0704 0.016 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0081(3) 0.0120(3) 0.0103(3) -0.00011(18) 0.0005(2) -0.00021(19) Mg2 0.0079(4) 0.0149(4) 0.0124(4) -0.0006(3) -0.0006(3) 0.0001(3) Mg3 0.0089(3) 0.0120(3) 0.0109(3) -0.00069(18) 0.0002(2) 0.00009(18) Mg4 0.0079(4) 0.0147(4) 0.0128(4) -0.0011(3) 0.0019(3) 0.0007(3) O1 0.0088(6) 0.0134(5) 0.0132(6) 0.0010(4) 0.0001(4) -0.0005(4) O2 0.0089(5) 0.0139(5) 0.0129(6) -0.0010(4) -0.0007(4) 0.0003(4) O3 0.0112(5) 0.0132(5) 0.0112(6) 0.0002(4) -0.0002(4) 0.0002(4) O4 0.0097(5) 0.0131(5) 0.0138(6) -0.0006(4) 0.0016(4) -0.0006(4) O5 0.0096(6) 0.0134(5) 0.0130(6) 0.0003(4) 0.0011(4) 0.0004(4) O6 0.0088(5) 0.0156(5) 0.0121(6) -0.0016(4) -0.0001(4) 0.0015(4) O7 0.0106(6) 0.0235(6) 0.0134(6) 0.0000(4) -0.0009(5) 0.0003(4) O8 0.0132(5) 0.0151(6) 0.0172(6) -0.0010(4) -0.0046(4) -0.0012(4) O9 0.0131(6) 0.0138(6) 0.0141(6) -0.0010(4) 0.0028(4) -0.0002(4) O10 0.0121(6) 0.0216(6) 0.0148(6) 0.0015(4) 0.0035(5) 0.0033(4) O11 0.0094(6) 0.0188(6) 0.0179(6) -0.0029(4) 0.0014(4) 0.0004(4) O12 0.0155(6) 0.0136(6) 0.0123(6) 0.0004(4) -0.0015(4) -0.0013(4) C1 0.0112(8) 0.0162(8) 0.0137(9) 0.0000(6) 0.0026(6) 0.0000(6) C2 0.0120(7) 0.0139(7) 0.0167(8) 0.0014(6) -0.0017(6) 0.0015(6) C3 0.0117(8) 0.0144(8) 0.0132(9) -0.0015(6) -0.0009(6) -0.0001(6) C4 0.0111(8) 0.0171(8) 0.0133(8) 0.0001(6) 0.0024(6) -0.0007(6) C5 0.0128(8) 0.0167(8) 0.0148(8) 0.0007(6) -0.0004(6) 0.0027(6) C6 0.0113(8) 0.0162(8) 0.0132(8) -0.0022(6) -0.0006(6) 0.0003(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 Mg1 O6 2.0569(11) . ? Mg1 O4 2.0743(11) . ? Mg1 O1 2.0873(11) . ? Mg1 O5 2.0924(11) . ? Mg1 O3 2.0941(11) . ? Mg1 O2 2.1024(11) . ? Mg1 Mg3 3.1560(7) . ? Mg1 Mg3 3.1734(7) 2_545 ? Mg1 Mg4 3.5125(5) . ? Mg1 Mg2 3.5511(5) . ? Mg2 O8 2.0550(11) 3 ? Mg2 O8 2.0550(11) . ? Mg2 O7 2.0599(11) 3 ? Mg2 O7 2.0599(11) . ? Mg2 O6 2.1144(10) . ? Mg2 O6 2.1144(10) 3 ? Mg2 Mg1 3.5511(5) 3 ? Mg3 O9 2.0224(11) . ? Mg3 O12 2.0342(11) 2 ? Mg3 O1 2.0551(12) 2 ? Mg3 O2 2.0846(11) . ? Mg3 O3 2.0926(11) . ? Mg3 O5 2.1130(11) 2 ? Mg3 Mg1 3.1734(7) 2 ? Mg4 O11 2.0406(11) 3_655 ? Mg4 O11 2.0406(11) . ? Mg4 O10 2.0565(11) . ? Mg4 O10 2.0565(11) 3_655 ? Mg4 O4 2.1077(10) 3_655 ? Mg4 O4 2.1077(10) . ? Mg4 Mg1 3.5125(5) 3_655 ? O1 C1 1.2713(19) . ? O1 Mg3 2.0551(12) 2_545 ? O2 C2 1.2757(19) . ? O3 C3 1.2770(19) . ? O4 C4 1.2808(18) . ? O5 C5 1.2722(19) . ? O5 Mg3 2.1130(11) 2_545 ? O6 C6 1.2827(19) . ? O7 C1 1.230(2) . ? O8 C2 1.2337(19) . ? O9 C4 1.2347(19) . ? O10 C5 1.2309(19) . ? O11 C6 1.2265(19) . ? O12 C3 1.2408(19) . ? O12 Mg3 2.0342(11) 2_545 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 O6 Mg1 O4 94.99(4) . . ? O6 Mg1 O1 89.54(4) . . ? O4 Mg1 O1 171.97(5) . . ? O6 Mg1 O5 98.28(4) . . ? O4 Mg1 O5 95.14(4) . . ? O1 Mg1 O5 77.62(4) . . ? O6 Mg1 O3 171.78(5) . . ? O4 Mg1 O3 89.34(4) . . ? O1 Mg1 O3 86.99(4) . . ? O5 Mg1 O3 88.26(4) . . ? O6 Mg1 O2 94.85(4) . . ? O4 Mg1 O2 92.86(4) . . ? O1 Mg1 O2 93.35(4) . . ? O5 Mg1 O2 163.95(5) . . ? O3 Mg1 O2 77.93(4) . . ? O6 Mg1 Mg3 133.32(4) . . ? O4 Mg1 Mg3 77.65(3) . . ? O1 Mg1 Mg3 103.97(3) . . ? O5 Mg1 Mg3 128.08(4) . . ? O3 Mg1 Mg3 41.06(3) . . ? O2 Mg1 Mg3 40.87(3) . . ? O6 Mg1 Mg3 107.18(4) . 2_545 ? O4 Mg1 Mg3 132.39(4) . 2_545 ? O1 Mg1 Mg3 39.62(3) . 2_545 ? O5 Mg1 Mg3 41.25(3) . 2_545 ? O3 Mg1 Mg3 74.57(3) . 2_545 ? O2 Mg1 Mg3 125.36(3) . 2_545 ? Mg3 Mg1 Mg3 111.489(16) . 2_545 ? O6 Mg1 Mg4 76.47(3) . . ? O4 Mg1 Mg4 33.17(3) . . ? O1 Mg1 Mg4 143.21(3) . . ? O5 Mg1 Mg4 71.15(3) . . ? O3 Mg1 Mg4 110.55(3) . . ? O2 Mg1 Mg4 121.27(3) . . ? Mg3 Mg1 Mg4 110.407(16) . . ? Mg3 Mg1 Mg4 112.399(16) 2_545 . ? O6 Mg1 Mg2 32.13(3) . . ? O4 Mg1 Mg2 115.63(3) . . ? O1 Mg1 Mg2 71.38(3) . . ? O5 Mg1 Mg2 118.05(3) . . ? O3 Mg1 Mg2 139.77(3) . . ? O2 Mg1 Mg2 70.22(3) . . ? Mg3 Mg1 Mg2 111.011(16) . . ? Mg3 Mg1 Mg2 104.505(16) 2_545 . ? Mg4 Mg1 Mg2 106.790(14) . . ? O8 Mg2 O8 180.0 3 . ? O8 Mg2 O7 90.37(4) 3 3 ? O8 Mg2 O7 89.63(4) . 3 ? O8 Mg2 O7 89.63(4) 3 . ? O8 Mg2 O7 90.37(4) . . ? O7 Mg2 O7 180.00(8) 3 . ? O8 Mg2 O6 89.38(4) 3 . ? O8 Mg2 O6 90.62(4) . . ? O7 Mg2 O6 86.80(4) 3 . ? O7 Mg2 O6 93.20(4) . . ? O8 Mg2 O6 90.62(4) 3 3 ? O8 Mg2 O6 89.38(4) . 3 ? O7 Mg2 O6 93.20(4) 3 3 ? O7 Mg2 O6 86.80(4) . 3 ? O6 Mg2 O6 180.00(6) . 3 ? O8 Mg2 Mg1 108.36(3) 3 . ? O8 Mg2 Mg1 71.64(3) . . ? O7 Mg2 Mg1 110.64(3) 3 . ? O7 Mg2 Mg1 69.36(3) . . ? O6 Mg2 Mg1 31.16(3) . . ? O6 Mg2 Mg1 148.84(3) 3 . ? O8 Mg2 Mg1 71.64(3) 3 3 ? O8 Mg2 Mg1 108.36(3) . 3 ? O7 Mg2 Mg1 69.36(3) 3 3 ? O7 Mg2 Mg1 110.64(3) . 3 ? O6 Mg2 Mg1 148.84(3) . 3 ? O6 Mg2 Mg1 31.16(3) 3 3 ? Mg1 Mg2 Mg1 180.000(16) . 3 ? O9 Mg3 O12 95.12(5) . 2 ? O9 Mg3 O1 91.98(5) . 2 ? O12 Mg3 O1 94.85(4) 2 2 ? O9 Mg3 O2 89.36(4) . . ? O12 Mg3 O2 93.63(5) 2 . ? O1 Mg3 O2 171.27(5) 2 . ? O9 Mg3 O3 91.10(4) . . ? O12 Mg3 O3 169.82(5) 2 . ? O1 Mg3 O3 92.98(4) 2 . ? O2 Mg3 O3 78.36(4) . . ? O9 Mg3 O5 169.75(5) . 2 ? O12 Mg3 O5 87.23(4) 2 2 ? O1 Mg3 O5 77.87(4) 2 2 ? O2 Mg3 O5 100.47(4) . 2 ? O3 Mg3 O5 88.06(4) . 2 ? O9 Mg3 Mg1 76.40(3) . . ? O12 Mg3 Mg1 133.14(4) 2 . ? O1 Mg3 Mg1 130.91(4) 2 . ? O2 Mg3 Mg1 41.30(3) . . ? O3 Mg3 Mg1 41.10(3) . . ? O5 Mg3 Mg1 109.14(3) 2 . ? O9 Mg3 Mg1 129.94(4) . 2 ? O12 Mg3 Mg1 78.99(3) 2 2 ? O1 Mg3 Mg1 40.37(3) 2 2 ? O2 Mg3 Mg1 140.26(3) . 2 ? O3 Mg3 Mg1 103.09(3) . 2 ? O5 Mg3 Mg1 40.77(3) 2 2 ? Mg1 Mg3 Mg1 140.812(19) . 2 ? O11 Mg4 O11 180.00(8) 3_655 . ? O11 Mg4 O10 90.04(4) 3_655 . ? O11 Mg4 O10 89.96(4) . . ? O11 Mg4 O10 89.96(4) 3_655 3_655 ? O11 Mg4 O10 90.04(4) . 3_655 ? O10 Mg4 O10 180.00(6) . 3_655 ? O11 Mg4 O4 90.21(4) 3_655 3_655 ? O11 Mg4 O4 89.79(4) . 3_655 ? O10 Mg4 O4 87.90(4) . 3_655 ? O10 Mg4 O4 92.10(4) 3_655 3_655 ? O11 Mg4 O4 89.79(4) 3_655 . ? O11 Mg4 O4 90.21(4) . . ? O10 Mg4 O4 92.10(4) . . ? O10 Mg4 O4 87.90(4) 3_655 . ? O4 Mg4 O4 180.00(6) 3_655 . ? O11 Mg4 Mg1 65.23(3) 3_655 3_655 ? O11 Mg4 Mg1 114.77(3) . 3_655 ? O10 Mg4 Mg1 107.66(3) . 3_655 ? O10 Mg4 Mg1 72.34(3) 3_655 3_655 ? O4 Mg4 Mg1 32.57(3) 3_655 3_655 ? O4 Mg4 Mg1 147.43(3) . 3_655 ? O11 Mg4 Mg1 114.77(3) 3_655 . ? O11 Mg4 Mg1 65.23(3) . . ? O10 Mg4 Mg1 72.34(3) . . ? O10 Mg4 Mg1 107.66(3) 3_655 . ? O4 Mg4 Mg1 147.43(3) 3_655 . ? O4 Mg4 Mg1 32.57(3) . . ? Mg1 Mg4 Mg1 180.00(2) 3_655 . ? C1 O1 Mg3 127.88(10) . 2_545 ? C1 O1 Mg1 130.63(10) . . ? Mg3 O1 Mg1 100.00(5) 2_545 . ? C2 O2 Mg3 127.06(10) . . ? C2 O2 Mg1 132.58(10) . . ? Mg3 O2 Mg1 97.83(5) . . ? C3 O3 Mg3 128.86(9) . . ? C3 O3 Mg1 130.97(9) . . ? Mg3 O3 Mg1 97.84(5) . . ? C4 O4 Mg1 126.89(9) . . ? C4 O4 Mg4 118.81(9) . . ? Mg1 O4 Mg4 114.26(5) . . ? C5 O5 Mg1 133.32(10) . . ? C5 O5 Mg3 127.33(10) . 2_545 ? Mg1 O5 Mg3 97.98(5) . 2_545 ? C6 O6 Mg1 123.81(10) . . ? C6 O6 Mg2 119.44(10) . . ? Mg1 O6 Mg2 116.71(5) . . ? C1 O7 Mg2 135.72(10) . . ? C2 O8 Mg2 134.66(10) . . ? C4 O9 Mg3 132.43(10) . . ? C5 O10 Mg4 134.35(10) . . ? C6 O11 Mg4 142.59(10) . . ? C3 O12 Mg3 128.64(10) . 2_545 ? O7 C1 O1 125.94(14) . . ? O7 C1 H1 117.0 . . ? O1 C1 H1 117.0 . . ? O8 C2 O2 126.15(14) . . ? O8 C2 H2 116.9 . . ? O2 C2 H2 116.9 . . ? O12 C3 O3 125.70(14) . . ? O12 C3 H3 117.1 . . ? O3 C3 H3 117.1 . . ? O9 C4 O4 126.13(13) . . ? O9 C4 H4 116.9 . . ? O4 C4 H4 116.9 . . ? O10 C5 O5 126.55(14) . . ? O10 C5 H5 116.7 . . ? O5 C5 H5 116.7 . . ? O11 C6 O6 126.05(14) . . ? O11 C6 H6 117.0 . . ? O6 C6 H6 117.0 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.275 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.066 # Attachment 'KimoonKim(CIF-Mn(HCOO)2-196K).cif' data_p21_n3 _database_code_depnum_ccdc_archive 'CCDC 693550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Mn(II) Formate' _chemical_melting_point ? _chemical_formula_moiety 'C2 H2 Mn O4' _chemical_formula_sum 'C2 H2 Mn O4' _chemical_formula_weight 144.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0017 '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 -0.0041 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2252 0.7704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7320(10) _cell_length_b 10.2000(10) _cell_length_c 14.9470(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.5380(10) _cell_angle_gamma 90.00 _cell_volume 1788.0(3) _cell_formula_units_Z 12 _cell_measurement_temperature 196(2) _cell_measurement_reflns_used 2724 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.99 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4406 _exptl_absorpt_correction_T_max 0.6585 _exptl_absorpt_process_details HKL2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 196(2) _diffrn_radiation_wavelength 0.73000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PAL 4A MXW Beamline' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'ADSC Quantum 210' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5103 _diffrn_reflns_av_R_equivalents 0.1309 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2724 _reflns_number_gt 2532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ADSC Quantum software' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Materials Studio 4.1' _computing_publication_material 'Materials Studio 4.1' _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^)+(0.1550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0096(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2724 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.25706(4) 0.07916(5) 0.13103(3) 0.0079(3) Uani 1 1 d . . . Mn2 Mn 0.0000 0.0000 0.0000 0.0134(4) Uani 1 2 d S . . Mn3 Mn 0.26015(5) 0.39283(5) 0.18681(4) 0.0100(3) Uani 1 1 d . . . Mn4 Mn 0.5000 0.0000 0.0000 0.0138(4) Uani 1 2 d S . . O1 O 0.1287(2) -0.0070(2) 0.21776(19) 0.0154(7) Uani 1 1 d . . . O2 O 0.1540(2) 0.2578(2) 0.10741(15) 0.0135(6) Uani 1 1 d . . . O3 O 0.3051(2) 0.2006(2) 0.24794(15) 0.0124(6) Uani 1 1 d . . . O4 O 0.4009(2) 0.1586(2) 0.06168(18) 0.0155(6) Uani 1 1 d . . . O5 O 0.3511(2) -0.0807(2) 0.19596(18) 0.0139(6) Uani 1 1 d . . . O6 O 0.1856(2) -0.0294(3) 0.02033(18) 0.0153(6) Uani 1 1 d . . . O7 O -0.0366(2) 0.0031(3) 0.1411(2) 0.0266(8) Uani 1 1 d . . . O8 O 0.0212(3) 0.2107(3) 0.00238(19) 0.0252(7) Uani 1 1 d . . . O9 O 0.3924(2) 0.3726(3) 0.09408(19) 0.0211(7) Uani 1 1 d . . . O10 O 0.5123(3) -0.1102(3) 0.1229(2) 0.0276(8) Uani 1 1 d . . . O11 O 0.3469(2) -0.1056(3) -0.0354(2) 0.0256(8) Uani 1 1 d . . . O12 O 0.3159(3) 0.0657(3) 0.36633(18) 0.0209(7) Uani 1 1 d . . . C1 C 0.0200(3) -0.0134(4) 0.2102(3) 0.0175(9) Uani 1 1 d . . . H1 H -0.0204 -0.0327 0.2628 0.021 Uiso 1 1 calc R . . C2 C 0.0773(4) 0.2869(4) 0.0487(3) 0.0227(9) Uani 1 1 d . . . H2 H 0.0622 0.3776 0.0401 0.027 Uiso 1 1 calc R . . C3 C 0.3286(3) 0.1736(3) 0.3293(2) 0.0176(9) Uani 1 1 d . . . H3 H 0.3587 0.2427 0.3654 0.021 Uiso 1 1 calc R . . C4 C 0.4332(3) 0.2770(4) 0.0552(3) 0.0207(9) Uani 1 1 d . . . H4 H 0.4947 0.2938 0.0168 0.025 Uiso 1 1 calc R . . C5 C 0.4477(4) -0.1328(4) 0.1846(3) 0.0233(10) Uani 1 1 d . . . H5 H 0.4727 -0.1954 0.2279 0.028 Uiso 1 1 calc R . . C6 C 0.2420(4) -0.0995(4) -0.0325(3) 0.0205(10) Uani 1 1 d . . . H6 H 0.1997 -0.1524 -0.0738 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0061(5) 0.0097(5) 0.0080(5) -0.0006(2) -0.0002(3) -0.00010(19) Mn2 0.0044(6) 0.0199(6) 0.0156(6) -0.0040(3) -0.0044(4) 0.0010(3) Mn3 0.0102(5) 0.0096(5) 0.0104(5) -0.0024(2) -0.0006(3) -0.00011(19) Mn4 0.0073(6) 0.0179(6) 0.0165(6) -0.0035(3) 0.0050(4) 0.0021(3) O1 0.0082(16) 0.0173(14) 0.0208(15) 0.0061(11) -0.0008(11) 0.0001(10) O2 0.0133(15) 0.0134(14) 0.0135(13) -0.0019(10) -0.0059(10) 0.0024(10) O3 0.0184(14) 0.0098(14) 0.0088(13) 0.0015(10) -0.0025(10) -0.0002(10) O4 0.0107(14) 0.0126(14) 0.0234(15) -0.0025(11) 0.0070(11) -0.0004(11) O5 0.0105(15) 0.0170(14) 0.0144(15) 0.0022(11) 0.0026(11) 0.0049(10) O6 0.0075(14) 0.0210(15) 0.0172(15) -0.0070(11) -0.0022(11) 0.0017(10) O7 0.0093(16) 0.051(2) 0.0189(16) -0.0010(13) -0.0050(12) 0.0014(12) O8 0.0216(17) 0.0184(15) 0.0347(18) -0.0024(13) -0.0183(13) -0.0019(12) O9 0.0215(17) 0.0171(15) 0.0252(16) -0.0052(12) 0.0119(13) -0.0016(11) O10 0.0170(17) 0.044(2) 0.0218(17) 0.0073(14) 0.0091(14) 0.0129(13) O11 0.0060(16) 0.0331(19) 0.0379(19) -0.0129(13) 0.0016(13) 0.0013(11) O12 0.0317(18) 0.0163(15) 0.0146(15) -0.0001(12) -0.0056(13) -0.0068(12) C1 0.011(2) 0.027(2) 0.015(2) 0.0032(16) 0.0030(16) 0.0011(15) C2 0.024(2) 0.0117(19) 0.031(2) 0.0028(17) -0.0085(18) 0.0043(16) C3 0.027(2) 0.0091(19) 0.016(2) -0.0025(15) -0.0066(17) -0.0030(15) C4 0.016(2) 0.021(2) 0.025(2) -0.0040(18) 0.0124(17) -0.0025(16) C5 0.025(2) 0.028(2) 0.017(2) 0.0086(18) 0.0038(18) 0.0145(19) C6 0.013(2) 0.028(2) 0.020(2) -0.0127(18) -0.0017(17) -0.0011(15) _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 O6 2.143(3) . ? Mn1 O4 2.161(3) . ? Mn1 O5 2.182(2) . ? Mn1 O1 2.197(3) . ? Mn1 O3 2.203(2) . ? Mn1 O2 2.209(2) . ? Mn2 O7 2.163(3) . ? Mn2 O7 2.163(3) 3 ? Mn2 O8 2.164(3) . ? Mn2 O8 2.164(3) 3 ? Mn2 O6 2.211(3) . ? Mn2 O6 2.211(3) 3 ? Mn3 O9 2.118(3) . ? Mn3 O12 2.121(3) 2 ? Mn3 O1 2.163(3) 2 ? Mn3 O2 2.186(2) . ? Mn3 O3 2.221(2) . ? Mn3 O5 2.229(3) 2 ? Mn4 O11 2.149(3) 3_655 ? Mn4 O11 2.149(3) . ? Mn4 O10 2.156(3) . ? Mn4 O10 2.156(3) 3_655 ? Mn4 O4 2.208(2) . ? Mn4 O4 2.208(2) 3_655 ? O1 C1 1.279(5) . ? O1 Mn3 2.163(3) 2_545 ? O2 C2 1.275(5) . ? O3 C3 1.270(4) . ? O4 C4 1.271(5) . ? O5 C5 1.268(5) . ? O5 Mn3 2.229(3) 2_545 ? O6 C6 1.266(5) . ? O7 C1 1.225(5) . ? O8 C2 1.222(5) . ? O9 C4 1.238(5) . ? O10 C5 1.230(5) . ? O11 C6 1.234(5) . ? O12 C3 1.243(5) . ? O12 Mn3 2.121(3) 2_545 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 O6 Mn1 O4 96.76(10) . . ? O6 Mn1 O5 98.06(10) . . ? O4 Mn1 O5 95.82(10) . . ? O6 Mn1 O1 89.35(10) . . ? O4 Mn1 O1 171.62(10) . . ? O5 Mn1 O1 77.58(10) . . ? O6 Mn1 O3 171.69(10) . . ? O4 Mn1 O3 89.04(9) . . ? O5 Mn1 O3 87.23(9) . . ? O1 Mn1 O3 85.52(10) . . ? O6 Mn1 O2 95.83(9) . . ? O4 Mn1 O2 92.58(10) . . ? O5 Mn1 O2 162.78(9) . . ? O1 Mn1 O2 92.50(9) . . ? O3 Mn1 O2 77.90(9) . . ? O7 Mn2 O7 180.0(2) . 3 ? O7 Mn2 O8 89.73(11) . . ? O7 Mn2 O8 90.27(11) 3 . ? O7 Mn2 O8 90.27(11) . 3 ? O7 Mn2 O8 89.73(11) 3 3 ? O8 Mn2 O8 180.00(16) . 3 ? O7 Mn2 O6 95.08(10) . . ? O7 Mn2 O6 84.92(10) 3 . ? O8 Mn2 O6 91.15(10) . . ? O8 Mn2 O6 88.85(10) 3 . ? O7 Mn2 O6 84.92(10) . 3 ? O7 Mn2 O6 95.08(10) 3 3 ? O8 Mn2 O6 88.85(10) . 3 ? O8 Mn2 O6 91.15(10) 3 3 ? O6 Mn2 O6 180.00(14) . 3 ? O9 Mn3 O12 98.29(12) . 2 ? O9 Mn3 O1 92.18(11) . 2 ? O12 Mn3 O1 95.43(10) 2 2 ? O9 Mn3 O2 90.00(10) . . ? O12 Mn3 O2 95.33(10) 2 . ? O1 Mn3 O2 168.60(10) 2 . ? O9 Mn3 O3 90.76(10) . . ? O12 Mn3 O3 168.82(11) 2 . ? O1 Mn3 O3 90.75(9) 2 . ? O2 Mn3 O3 78.02(9) . . ? O9 Mn3 O5 168.74(11) . 2 ? O12 Mn3 O5 86.79(11) 2 2 ? O1 Mn3 O5 77.28(10) 2 2 ? O2 Mn3 O5 99.57(9) . 2 ? O3 Mn3 O5 85.49(9) . 2 ? O11 Mn4 O11 180.0(2) 3_655 . ? O11 Mn4 O10 90.86(12) 3_655 . ? O11 Mn4 O10 89.14(12) . . ? O11 Mn4 O10 89.14(12) 3_655 3_655 ? O11 Mn4 O10 90.86(12) . 3_655 ? O10 Mn4 O10 180.00(15) . 3_655 ? O11 Mn4 O4 88.62(10) 3_655 . ? O11 Mn4 O4 91.38(10) . . ? O10 Mn4 O4 92.88(10) . . ? O10 Mn4 O4 87.12(10) 3_655 . ? O11 Mn4 O4 91.38(10) 3_655 3_655 ? O11 Mn4 O4 88.62(10) . 3_655 ? O10 Mn4 O4 87.12(10) . 3_655 ? O10 Mn4 O4 92.88(10) 3_655 3_655 ? O4 Mn4 O4 180.00(18) . 3_655 ? C1 O1 Mn3 128.1(3) . 2_545 ? C1 O1 Mn1 131.7(3) . . ? Mn3 O1 Mn1 99.64(11) 2_545 . ? C2 O2 Mn3 127.5(2) . . ? C2 O2 Mn1 132.5(2) . . ? Mn3 O2 Mn1 97.57(9) . . ? C3 O3 Mn1 133.0(2) . . ? C3 O3 Mn3 128.9(2) . . ? Mn1 O3 Mn3 96.73(9) . . ? C4 O4 Mn1 129.1(2) . . ? C4 O4 Mn4 120.2(2) . . ? Mn1 O4 Mn4 110.63(10) . . ? C5 O5 Mn1 134.2(3) . . ? C5 O5 Mn3 126.8(2) . 2_545 ? Mn1 O5 Mn3 98.08(10) . 2_545 ? C6 O6 Mn1 125.0(2) . . ? C6 O6 Mn2 121.4(2) . . ? Mn1 O6 Mn2 113.56(12) . . ? C1 O7 Mn2 134.6(3) . . ? C2 O8 Mn2 134.5(3) . . ? C4 O9 Mn3 133.1(3) . . ? C5 O10 Mn4 135.0(3) . . ? C6 O11 Mn4 142.5(3) . . ? C3 O12 Mn3 128.6(2) . 2_545 ? O7 C1 O1 125.8(4) . . ? O7 C1 H1 117.1 . . ? O1 C1 H1 117.1 . . ? O8 C2 O2 127.0(4) . . ? O8 C2 H2 116.5 . . ? O2 C2 H2 116.5 . . ? O12 C3 O3 126.4(3) . . ? O12 C3 H3 116.8 . . ? O3 C3 H3 116.8 . . ? O9 C4 O4 126.4(4) . . ? O9 C4 H4 116.8 . . ? O4 C4 H4 116.8 . . ? O10 C5 O5 126.4(4) . . ? O10 C5 H5 116.8 . . ? O5 C5 H5 116.8 . . ? O11 C6 O6 126.1(4) . . ? O11 C6 H6 116.9 . . ? O6 C6 H6 116.9 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 1.412 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.272 # Attachment 'KimoonKim(CIF-Mn(HCOO)2-90K).cif' data_p21_n4 _database_code_depnum_ccdc_archive 'CCDC 693551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Mn(II) Formate' _chemical_melting_point ? _chemical_formula_moiety 'C2 H2 Mn O4' _chemical_formula_sum 'C2 H2 Mn O4' _chemical_formula_weight 144.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0017 '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 -0.0041 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2252 0.7704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7190(10) _cell_length_b 10.1720(10) _cell_length_c 14.9200(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.5530(10) _cell_angle_gamma 90.00 _cell_volume 1777.9(3) _cell_formula_units_Z 12 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2720 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.00 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 2.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4389 _exptl_absorpt_correction_T_max 0.6571 _exptl_absorpt_process_details HKL2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.73000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PAL 4A MXW Beamline' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'ADSC Quantum 210' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5171 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2720 _reflns_number_gt 2578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ADSC Quantum software' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Materials Studio 4.1' _computing_publication_material 'Materials Studio 4.1' _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^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0051(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2720 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.25720(3) 0.07996(4) 0.13103(3) 0.0049(2) Uani 1 1 d . . . Mn2 Mn 0.0000 0.0000 0.0000 0.0073(2) Uani 1 2 d S . . Mn3 Mn 0.26022(3) 0.39428(4) 0.18633(3) 0.0059(2) Uani 1 1 d . . . Mn4 Mn 0.5000 0.0000 0.0000 0.0077(2) Uani 1 2 d S . . O1 O 0.12812(16) -0.00518(17) 0.21838(14) 0.0086(5) Uani 1 1 d . . . O2 O 0.15410(16) 0.25853(19) 0.10661(12) 0.0086(5) Uani 1 1 d . . . O3 O 0.30597(16) 0.20189(18) 0.24784(12) 0.0087(4) Uani 1 1 d . . . O4 O 0.40051(16) 0.15920(18) 0.06094(13) 0.0095(5) Uani 1 1 d . . . O5 O 0.35110(16) -0.08091(18) 0.19631(14) 0.0094(5) Uani 1 1 d . . . O6 O 0.18523(16) -0.02960(19) 0.02058(13) 0.0086(4) Uani 1 1 d . . . O7 O -0.03732(17) 0.0051(2) 0.14109(14) 0.0153(5) Uani 1 1 d . . . O8 O 0.02117(17) 0.2113(2) 0.00064(13) 0.0139(5) Uani 1 1 d . . . O9 O 0.39282(17) 0.37387(19) 0.09274(14) 0.0123(5) Uani 1 1 d . . . O10 O 0.51341(18) -0.1099(2) 0.12354(14) 0.0162(5) Uani 1 1 d . . . O11 O 0.34693(17) -0.1073(2) -0.03505(15) 0.0149(5) Uani 1 1 d . . . O12 O 0.31669(18) 0.0677(2) 0.36683(13) 0.0120(5) Uani 1 1 d . . . C1 C 0.0201(3) -0.0114(3) 0.2108(2) 0.0115(7) Uani 1 1 d . . . H1 H -0.0203 -0.0305 0.2636 0.014 Uiso 1 1 calc R . . C2 C 0.0777(2) 0.2885(3) 0.04717(19) 0.0129(6) Uani 1 1 d . . . H2 H 0.0631 0.3794 0.0381 0.015 Uiso 1 1 calc R . . C3 C 0.3298(2) 0.1752(3) 0.32951(18) 0.0107(6) Uani 1 1 d . . . H3 H 0.3607 0.2444 0.3654 0.013 Uiso 1 1 calc R . . C4 C 0.4338(2) 0.2785(3) 0.05456(19) 0.0120(6) Uani 1 1 d . . . H4 H 0.4961 0.2950 0.0167 0.014 Uiso 1 1 calc R . . C5 C 0.4483(2) -0.1329(3) 0.1854(2) 0.0138(7) Uani 1 1 d . . . H5 H 0.4734 -0.1953 0.2291 0.017 Uiso 1 1 calc R . . C6 C 0.2419(2) -0.1018(3) -0.0322(2) 0.0110(6) Uani 1 1 d . . . H6 H 0.1995 -0.1561 -0.0728 0.013 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0040(3) 0.0048(3) 0.0059(3) -0.00035(15) -0.0003(2) -0.00015(14) Mn2 0.0035(4) 0.0101(4) 0.0082(4) -0.0016(2) -0.0023(3) 0.0007(2) Mn3 0.0061(3) 0.0048(3) 0.0069(3) -0.00138(15) -0.0003(2) 0.00027(15) Mn4 0.0049(4) 0.0092(4) 0.0092(4) -0.0017(2) 0.0023(3) 0.0013(2) O1 0.0060(12) 0.0106(10) 0.0092(10) 0.0029(8) -0.0008(8) -0.0001(7) O2 0.0078(11) 0.0074(10) 0.0106(10) -0.0009(8) -0.0027(8) 0.0010(7) O3 0.0105(10) 0.0062(10) 0.0092(10) -0.0012(8) -0.0013(7) 0.0001(7) O4 0.0069(10) 0.0082(10) 0.0137(10) -0.0014(8) 0.0041(8) -0.0002(8) O5 0.0068(11) 0.0094(10) 0.0121(11) 0.0010(8) 0.0015(8) 0.0023(7) O6 0.0072(10) 0.0095(10) 0.0088(10) -0.0031(8) -0.0011(8) 0.0022(7) O7 0.0069(11) 0.0279(13) 0.0112(11) -0.0007(9) -0.0022(9) 0.0016(8) O8 0.0118(11) 0.0119(11) 0.0174(12) -0.0003(8) -0.0093(8) -0.0010(8) O9 0.0144(11) 0.0076(10) 0.0152(11) -0.0012(8) 0.0064(9) -0.0002(8) O10 0.0107(11) 0.0254(13) 0.0128(12) 0.0036(9) 0.0029(9) 0.0072(9) O11 0.0066(12) 0.0171(11) 0.0210(12) -0.0065(9) 0.0019(9) 0.0001(8) O12 0.0164(12) 0.0085(11) 0.0108(11) 0.0015(8) -0.0035(8) -0.0030(8) C1 0.0076(18) 0.0163(16) 0.0108(16) 0.0006(11) 0.0035(12) -0.0003(11) C2 0.0127(16) 0.0089(14) 0.0170(15) -0.0012(12) -0.0023(12) 0.0033(11) C3 0.0132(16) 0.0099(15) 0.0087(15) -0.0042(12) -0.0039(11) 0.0010(11) C4 0.0090(15) 0.0120(16) 0.0153(15) -0.0010(12) 0.0046(11) 0.0003(11) C5 0.0130(16) 0.0179(16) 0.0107(15) 0.0021(12) 0.0010(12) 0.0067(13) C6 0.0081(18) 0.0140(15) 0.0108(16) -0.0073(12) 0.0002(11) 0.0020(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 O6 2.1433(19) . ? Mn1 O4 2.1584(19) . ? Mn1 O5 2.1861(19) . ? Mn1 O1 2.201(2) . ? Mn1 O3 2.2019(19) . ? Mn1 O2 2.2064(19) . ? Mn2 O7 2.162(2) . ? Mn2 O7 2.162(2) 3 ? Mn2 O8 2.164(2) 3 ? Mn2 O8 2.164(2) . ? Mn2 O6 2.2048(19) . ? Mn2 O6 2.2048(19) 3 ? Mn3 O12 2.125(2) 2 ? Mn3 O9 2.127(2) . ? Mn3 O1 2.1630(19) 2 ? Mn3 O2 2.1881(19) . ? Mn3 O3 2.2209(19) . ? Mn3 O5 2.226(2) 2 ? Mn4 O11 2.152(2) 3_655 ? Mn4 O11 2.152(2) . ? Mn4 O10 2.158(2) . ? Mn4 O10 2.158(2) 3_655 ? Mn4 O4 2.2058(19) . ? Mn4 O4 2.2058(19) 3_655 ? O1 C1 1.270(4) . ? O1 Mn3 2.1630(19) 2_545 ? O2 C2 1.280(3) . ? O3 C3 1.272(3) . ? O4 C4 1.279(3) . ? O5 C5 1.270(4) . ? O5 Mn3 2.226(2) 2_545 ? O6 C6 1.276(4) . ? O7 C1 1.235(4) . ? O8 C2 1.229(4) . ? O9 C4 1.229(3) . ? O10 C5 1.236(4) . ? O11 C6 1.234(4) . ? O12 C3 1.239(3) . ? O12 Mn3 2.125(2) 2_545 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 O6 Mn1 O4 96.71(7) . . ? O6 Mn1 O5 97.83(7) . . ? O4 Mn1 O5 96.12(7) . . ? O6 Mn1 O1 89.33(7) . . ? O4 Mn1 O1 171.95(8) . . ? O5 Mn1 O1 77.72(7) . . ? O6 Mn1 O3 171.79(7) . . ? O4 Mn1 O3 89.11(7) . . ? O5 Mn1 O3 87.26(7) . . ? O1 Mn1 O3 85.46(7) . . ? O6 Mn1 O2 95.67(7) . . ? O4 Mn1 O2 92.43(7) . . ? O5 Mn1 O2 163.05(7) . . ? O1 Mn1 O2 92.27(7) . . ? O3 Mn1 O2 78.24(7) . . ? O7 Mn2 O7 180.00(10) . 3 ? O7 Mn2 O8 90.11(8) . 3 ? O7 Mn2 O8 89.89(8) 3 3 ? O7 Mn2 O8 89.89(8) . . ? O7 Mn2 O8 90.11(8) 3 . ? O8 Mn2 O8 180.00(11) 3 . ? O7 Mn2 O6 95.28(7) . . ? O7 Mn2 O6 84.72(7) 3 . ? O8 Mn2 O6 88.70(7) 3 . ? O8 Mn2 O6 91.30(7) . . ? O7 Mn2 O6 84.72(7) . 3 ? O7 Mn2 O6 95.28(7) 3 3 ? O8 Mn2 O6 91.30(7) 3 3 ? O8 Mn2 O6 88.70(7) . 3 ? O6 Mn2 O6 180.0 . 3 ? O12 Mn3 O9 98.40(8) 2 . ? O12 Mn3 O1 95.50(7) 2 2 ? O9 Mn3 O1 92.17(8) . 2 ? O12 Mn3 O2 95.27(7) 2 . ? O9 Mn3 O2 89.78(7) . . ? O1 Mn3 O2 168.65(7) 2 . ? O12 Mn3 O3 168.81(8) 2 . ? O9 Mn3 O3 90.73(7) . . ? O1 Mn3 O3 90.58(7) 2 . ? O2 Mn3 O3 78.22(7) . . ? O12 Mn3 O5 87.01(8) 2 2 ? O9 Mn3 O5 168.96(8) . 2 ? O1 Mn3 O5 77.67(8) 2 2 ? O2 Mn3 O5 99.36(7) . 2 ? O3 Mn3 O5 85.12(7) . 2 ? O11 Mn4 O11 180.00(11) 3_655 . ? O11 Mn4 O10 90.81(8) 3_655 . ? O11 Mn4 O10 89.19(8) . . ? O11 Mn4 O10 89.19(8) 3_655 3_655 ? O11 Mn4 O10 90.81(8) . 3_655 ? O10 Mn4 O10 180.00(11) . 3_655 ? O11 Mn4 O4 88.51(7) 3_655 . ? O11 Mn4 O4 91.49(7) . . ? O10 Mn4 O4 93.17(8) . . ? O10 Mn4 O4 86.83(8) 3_655 . ? O11 Mn4 O4 91.49(7) 3_655 3_655 ? O11 Mn4 O4 88.51(7) . 3_655 ? O10 Mn4 O4 86.83(8) . 3_655 ? O10 Mn4 O4 93.17(8) 3_655 3_655 ? O4 Mn4 O4 180.00(12) . 3_655 ? C1 O1 Mn3 128.24(18) . 2_545 ? C1 O1 Mn1 131.81(19) . . ? Mn3 O1 Mn1 99.32(8) 2_545 . ? C2 O2 Mn3 127.11(18) . . ? C2 O2 Mn1 132.84(18) . . ? Mn3 O2 Mn1 97.42(7) . . ? C3 O3 Mn1 133.12(18) . . ? C3 O3 Mn3 128.92(18) . . ? Mn1 O3 Mn3 96.59(7) . . ? C4 O4 Mn1 129.27(18) . . ? C4 O4 Mn4 120.03(17) . . ? Mn1 O4 Mn4 110.64(8) . . ? C5 O5 Mn1 134.18(19) . . ? C5 O5 Mn3 126.87(18) . 2_545 ? Mn1 O5 Mn3 97.86(8) . 2_545 ? C6 O6 Mn1 124.96(18) . . ? C6 O6 Mn2 121.31(18) . . ? Mn1 O6 Mn2 113.67(9) . . ? C1 O7 Mn2 134.19(19) . . ? C2 O8 Mn2 134.14(19) . . ? C4 O9 Mn3 133.06(19) . . ? C5 O10 Mn4 134.8(2) . . ? C6 O11 Mn4 142.60(19) . . ? C3 O12 Mn3 128.45(18) . 2_545 ? O7 C1 O1 126.0(3) . . ? O7 C1 H1 117.0 . . ? O1 C1 H1 117.0 . . ? O8 C2 O2 126.6(3) . . ? O8 C2 H2 116.7 . . ? O2 C2 H2 116.7 . . ? O12 C3 O3 126.3(3) . . ? O12 C3 H3 116.8 . . ? O3 C3 H3 116.8 . . ? O9 C4 O4 126.2(3) . . ? O9 C4 H4 116.9 . . ? O4 C4 H4 116.9 . . ? O10 C5 O5 126.2(3) . . ? O10 C5 H5 116.9 . . ? O5 C5 H5 116.9 . . ? O11 C6 O6 125.7(3) . . ? O11 C6 H6 117.1 . . ? O6 C6 H6 117.1 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.716 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.180