# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Susumu Kitagawa' 'Wakako Kaneko' 'Tapas Maji' 'Masaaki Ohba' _publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry Kyoto University Graduate School of Engineering Nishikyo-ku Katsura campus Kyoto 615-8510 JAPAN ; _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_requested_journal 'Chemical Communications' _publ_section_title ; Diversity in magnetic properties of 3D isomorphous networks of Co(II) and Mn(II) constructed by napthalene-1,4-dicarboxylate ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #--------------------------------------------------------------------------- data_Co_g _database_code_depnum_ccdc_archive 'CCDC 274483' _audit_creation_date 'Fri Jun 11 14:54:04 2004' _audit_creation_method 'by teXsan' _audit_update_record ? _chemical_formula_sum 'C12 H6 Co O4 ' _chemical_formula_moiety 'C12 H6 Co O4 ' _chemical_formula_weight 273.11 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 4.728(5) _cell_length_b 14.84(2) _cell_length_c 13.48(3) _cell_angle_alpha 90 _cell_angle_beta 90.46(6) _cell_angle_gamma 90 _cell_volume 946.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 78 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.2 #--------------------------------------------------------------------------- _exptl_crystal_description Prism _exptl_crystal_colour Violet _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.811 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details REQABA _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 0.696 #--------------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 9938 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.9856 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.9856 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #--------------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2128 _reflns_number_gt 1661 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0417 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1661 _refine_ls_number_parameters 154 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0015 _refine_diff_density_max 0.66 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co Co 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co(1) Co 0.24954(4) 0.44309(2) 0.50083(2) 0.01184(9) Uani 1.00 d . . . O(1) O 0.6272(3) 0.44585(8) 0.59006(10) 0.0130(3) Uani 1.00 d . . . O(2) O 1.0210(3) 0.36152(9) 0.59105(9) 0.0165(3) Uani 1.00 d . . . O(3) O 0.4847(3) 0.36613(9) 0.40866(10) 0.0172(3) Uani 1.00 d . . . O(4) O 0.8829(3) 0.44781(8) 0.40696(10) 0.0128(3) Uani 1.00 d . . . C(1) C 0.7745(4) 0.3790(1) 0.6202(1) 0.0129(4) Uani 1.00 d . . . C(2) C 0.6442(4) 0.3159(1) 0.6942(1) 0.0145(4) Uani 1.00 d . . . C(3) C 0.6846(4) 0.2252(1) 0.6825(1) 0.0181(4) Uani 1.00 d . . . C(4) C 0.5519(4) 0.1629(1) 0.7451(1) 0.0181(5) Uani 1.00 d . . . C(5) C 0.3768(4) 0.1915(1) 0.8200(1) 0.0139(4) Uani 1.00 d . . . C(6) C 0.3400(4) 0.2856(1) 0.8376(1) 0.0167(4) Uani 1.00 d . . . C(7) C 0.4769(4) 0.3491(1) 0.7747(1) 0.0164(4) Uani 1.00 d . . . C(8) C 0.1854(5) 0.3192(1) 0.9199(2) 0.0287(5) Uani 1.00 d . . . C(9) C 0.1778(6) 0.4090(2) 0.9404(2) 0.0383(7) Uani 1.00 d . . . C(10) C 0.3166(5) 0.4713(2) 0.8798(2) 0.0337(6) Uani 1.00 d . . . C(11) C 0.4592(5) 0.4423(1) 0.7979(2) 0.0245(5) Uani 1.00 d . . . C(12) C 0.7371(4) 0.3784(1) 0.3832(1) 0.0130(4) Uani 1.00 d . . . H(1) H 0.8043 0.2041 0.6312 0.0217 Uiso 1.00 calc . . . H(2) H 0.5831 0.1003 0.7357 0.0217 Uiso 1.00 calc . . . H(3) H 0.0860 0.2783 0.9612 0.0345 Uiso 1.00 calc . . . H(4) H 0.0770 0.4297 0.9967 0.0459 Uiso 1.00 calc . . . H(5) H 0.3117 0.5337 0.8955 0.0404 Uiso 1.00 calc . . . H(6) H 0.5476 0.4851 0.7558 0.0294 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0116(2) 0.0100(2) 0.0140(2) 0.00009(8) 0.0037(1) 0.00008(8) O(1) 0.0125(7) 0.0129(7) 0.0136(6) -0.0005(4) 0.0020(5) 0.0022(4) O(2) 0.0142(6) 0.0157(7) 0.0197(6) 0.0000(5) 0.0051(5) 0.0047(5) O(3) 0.0133(6) 0.0171(7) 0.0213(6) 0.0005(5) 0.0035(5) -0.0056(5) O(4) 0.0127(7) 0.0120(7) 0.0138(6) 0.0014(4) 0.0015(5) -0.0029(4) C(1) 0.0150(8) 0.0112(8) 0.0127(7) -0.0020(6) 0.0006(6) 0.0002(6) C(2) 0.0133(8) 0.0158(9) 0.0146(8) -0.0012(7) 0.0023(6) 0.0041(7) C(3) 0.0188(9) 0.0174(9) 0.0181(8) 0.0011(7) 0.0053(7) 0.0027(7) C(4) 0.0215(10) 0.0135(9) 0.0193(9) 0.0029(7) 0.0046(7) 0.0027(7) C(5) 0.0122(8) 0.0136(9) 0.0160(8) 0.0001(6) 0.0021(6) 0.0041(7) C(6) 0.0177(9) 0.0158(9) 0.0167(8) 0.0007(7) 0.0029(7) 0.0035(7) C(7) 0.0178(9) 0.0160(9) 0.0155(8) 0.0003(7) 0.0030(7) 0.0029(7) C(8) 0.040(1) 0.021(1) 0.0249(10) 0.0006(9) 0.0160(9) 0.0040(8) C(9) 0.060(2) 0.024(1) 0.031(1) 0.005(1) 0.025(1) -0.0015(9) C(10) 0.055(1) 0.0166(10) 0.030(1) 0.001(1) 0.015(1) -0.0012(9) C(11) 0.035(1) 0.016(1) 0.0220(9) -0.0028(8) 0.0057(9) 0.0027(7) C(12) 0.0145(8) 0.0128(9) 0.0117(7) 0.0014(6) 0.0007(6) -0.0017(6) #--------------------------------------------------------------------------- _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co(1) O(1) 2.145(2) . . yes Co(1) O(1) 2.138(1) . 3_666 yes Co(1) O(2) 2.033(1) . 1_455 yes Co(1) O(3) 2.026(1) . . yes Co(1) O(4) 2.139(2) . 1_455 yes Co(1) O(4) 2.138(1) . 3_666 yes O(1) C(1) 1.278(2) . . yes O(2) C(1) 1.260(2) . . yes O(3) C(12) 1.258(2) . . yes O(4) C(12) 1.278(2) . . yes C(1) C(2) 1.503(2) . . yes C(2) C(3) 1.370(3) . . yes C(2) C(7) 1.435(2) . . yes C(3) C(4) 1.403(3) . . yes C(4) C(5) 1.378(2) . . yes C(5) C(6) 1.427(2) . . yes C(5) C(12) 1.500(2) . 4_455 yes C(6) C(7) 1.426(2) . . yes C(6) C(8) 1.424(3) . . yes C(7) C(11) 1.421(3) . . yes C(8) C(9) 1.362(3) . . yes C(9) C(10) 1.401(3) . . yes C(10) C(11) 1.368(3) . . yes #--------------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Co(1) O(1) 94.42(6) . . 3_666 yes O(1) Co(1) O(2) 96.89(7) . . 1_455 yes O(1) Co(1) O(3) 84.04(7) . . . yes O(1) Co(1) O(4) 176.32(4) . . 1_455 yes O(1) Co(1) O(4) 84.60(6) . . 3_666 yes O(1) Co(1) O(2) 161.93(6) 3_666 . 1_455 yes O(1) Co(1) O(3) 85.98(5) 3_666 . . yes O(1) Co(1) O(4) 81.90(6) 3_666 . 1_455 yes O(1) Co(1) O(4) 80.30(6) 3_666 . 3_666 yes O(2) Co(1) O(3) 109.14(7) 1_455 . . yes O(2) Co(1) O(4) 86.63(7) 1_455 . 1_455 yes O(2) Co(1) O(4) 86.78(5) 1_455 . 3_666 yes O(3) Co(1) O(4) 95.85(7) . . 1_455 yes O(3) Co(1) O(4) 161.43(6) . . 3_666 yes O(4) Co(1) O(4) 94.55(6) 1_455 . 3_666 yes Co(1) O(1) Co(1) 85.58(6) . . 3_666 yes Co(1) O(1) C(1) 127.8(1) . . . yes Co(1) O(1) C(1) 129.2(1) 3_666 . . yes Co(1) O(2) C(1) 124.2(1) 1_655 . . yes Co(1) O(3) C(12) 127.7(1) . . . yes Co(1) O(4) Co(1) 85.45(6) 1_655 . 3_666 yes Co(1) O(4) C(12) 123.7(1) 1_655 . . yes Co(1) O(4) C(12) 126.6(1) 3_666 . . yes O(1) C(1) O(2) 124.3(2) . . . yes O(1) C(1) C(2) 118.0(2) . . . yes O(2) C(1) C(2) 117.7(2) . . . yes C(1) C(2) C(3) 118.5(2) . . . yes C(1) C(2) C(7) 121.3(2) . . . yes C(3) C(2) C(7) 120.2(2) . . . yes C(2) C(3) C(4) 121.0(2) . . . yes C(3) C(4) C(5) 120.8(2) . . . yes C(4) C(5) C(6) 119.9(2) . . . yes C(4) C(5) C(12) 118.2(2) . . 4_455 yes C(6) C(5) C(12) 121.9(1) . . 4_455 yes C(5) C(6) C(7) 119.4(2) . . . yes C(5) C(6) C(8) 122.4(2) . . . yes C(7) C(6) C(8) 118.0(2) . . . yes C(2) C(7) C(6) 118.6(2) . . . yes C(2) C(7) C(11) 122.3(2) . . . yes C(6) C(7) C(11) 119.0(2) . . . yes C(6) C(8) C(9) 121.0(2) . . . yes C(8) C(9) C(10) 121.0(2) . . . yes C(9) C(10) C(11) 119.9(2) . . . yes C(7) C(11) C(10) 121.0(2) . . . yes O(3) C(12) O(4) 124.0(2) . . . yes O(3) C(12) C(5) 118.5(2) . . 4_554 yes O(4) C(12) C(5) 117.4(2) . . 4_554 yes #--------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co(1) O(1) Co(1) O(1) 0.0000(1) . . 3_666 3_666 yes Co(1) O(1) Co(1) O(2) -128.7(2) . . 3_666 3_766 yes Co(1) O(1) Co(1) O(3) 83.70(7) . . 3_666 3_666 yes Co(1) O(1) Co(1) O(4) -83.74(6) . . 3_666 . yes Co(1) O(1) Co(1) O(4) -179.81(4) . . 3_666 3_766 yes Co(1) O(1) C(1) O(2) 111.9(2) . . . . yes Co(1) O(1) C(1) C(2) -67.1(2) . . . . yes Co(1) O(1) Co(1) O(1) 0.0 . 3_666 3_666 . yes Co(1) O(1) Co(1) O(2) 165.89(5) . 3_666 3_666 3_766 yes Co(1) O(1) Co(1) O(3) -85.48(5) . 3_666 3_666 3_666 yes Co(1) O(1) Co(1) O(4) 79.80(6) . 3_666 3_666 . yes Co(1) O(1) Co(1) O(4) 3.0(6) . 3_666 3_666 3_766 yes Co(1) O(1) C(1) O(2) 8.5(3) . 3_666 3_666 3_666 yes Co(1) O(1) C(1) C(2) -172.5(1) . 3_666 3_666 3_666 yes Co(1) O(3) C(12) O(4) -5.5(3) . . . . yes Co(1) O(3) C(12) C(5) 175.3(1) . . . 4_554 yes Co(1) O(4) Co(1) O(1) -176.40(4) . 1_455 3_566 3_566 yes Co(1) O(4) Co(1) O(3) -123.9(2) . 1_455 3_566 3_566 yes Co(1) O(4) Co(1) O(1) 76.5(6) . 3_666 3_566 3_566 yes Co(1) O(4) Co(1) O(3) 164.60(5) . 3_666 3_566 3_566 yes Co(1) O(4) C(12) O(3) -2.8(3) . 3_666 3_666 3_666 yes O(1) Co(1) O(1) Co(1) 0.0 . . 3_666 3_666 yes O(1) Co(1) O(1) C(1) -136.9(2) . . 3_666 3_666 yes O(1) Co(1) O(3) C(12) -43.2(2) . . . . yes O(1) Co(1) O(4) C(12) 47.1(1) . . 3_666 3_666 yes O(1) Co(1) O(1) Co(1) 0.0000(1) . 3_666 3_666 . yes O(1) Co(1) O(1) C(1) 137.9(2) . 3_666 3_666 3_666 yes O(1) Co(1) O(2) C(1) -1.0(3) . 3_666 3_766 3_766 yes O(1) Co(1) O(3) C(12) -51.7(2) . 3_666 3_666 3_666 yes O(1) Co(1) O(4) C(12) 48.4(1) . 3_666 . . yes O(1) Co(1) O(4) C(12) -148.8(1) . 3_666 3_766 3_766 yes O(1) C(1) C(2) C(3) 138.3(2) . . . . yes O(1) C(1) C(2) C(7) -40.7(2) . . . . yes O(2) Co(1) O(1) C(1) -8.2(3) . 1_655 3_766 3_766 yes O(2) Co(1) O(4) C(12) -45.2(1) . 1_655 . . yes O(2) Co(1) O(4) C(12) 144.3(1) . 1_655 3_766 3_766 yes O(2) C(1) C(2) C(3) -40.7(2) . . . . yes O(2) C(1) C(2) C(7) 140.3(2) . . . . yes O(3) Co(1) O(1) C(1) -52.4(1) . . . . yes O(3) Co(1) O(1) C(1) 139.4(2) . . 3_666 3_666 yes O(3) Co(1) O(4) C(12) -5.4(3) . . 3_666 3_666 yes O(4) Co(1) O(1) C(1) 42.9(2) . 1_655 3_766 3_766 yes O(4) Co(1) O(2) C(1) -49.5(1) . 1_655 . . yes O(4) Co(1) O(4) C(12) -129.3(2) . 1_655 3_766 3_766 yes O(4) Co(1) O(1) C(1) 53.1(1) . 3_666 . . yes O(4) Co(1) O(1) C(1) -142.3(1) . 3_666 3_666 3_666 yes O(4) Co(1) O(2) C(1) -45.3(1) . 3_666 3_766 3_766 yes O(4) Co(1) O(3) C(12) -9.4(3) . 3_666 3_666 3_666 yes O(4) Co(1) O(4) C(12) 131.7(1) . 3_666 3_766 3_766 yes C(1) C(2) C(3) C(4) -175.5(2) . . . . yes C(1) C(2) C(7) C(6) 175.0(2) . . . . yes C(1) C(2) C(7) C(11) -9.5(3) . . . . yes C(2) C(3) C(4) C(5) 0.1(3) . . . . yes C(2) C(7) C(6) C(5) 1.1(3) . . . . yes C(2) C(7) C(6) C(8) 177.1(2) . . . . yes C(2) C(7) C(11) C(10) -174.7(2) . . . . yes C(3) C(2) C(7) C(6) -4.0(3) . . . . yes C(3) C(2) C(7) C(11) 171.5(2) . . . . yes C(3) C(4) C(5) C(6) -3.1(3) . . . . yes C(3) C(4) C(5) C(12) 178.9(2) . . . 4_455 yes C(4) C(3) C(2) C(7) 3.5(3) . . . . yes C(4) C(5) C(6) C(7) 2.4(3) . . . . yes C(4) C(5) C(6) C(8) -173.5(2) . . . . yes C(5) C(6) C(7) C(11) -174.6(2) . . . . yes C(5) C(6) C(8) C(9) 173.3(2) . . . . yes C(6) C(7) C(11) C(10) 0.8(3) . . . . yes C(6) C(8) C(9) C(10) 1.5(4) . . . . yes C(7) C(6) C(5) C(12) -179.7(2) . . . 4_455 yes C(7) C(6) C(8) C(9) -2.6(3) . . . . yes C(7) C(11) C(10) C(9) -2.0(4) . . . . yes C(8) C(6) C(5) C(12) 4.5(3) . . . 4_455 yes C(8) C(6) C(7) C(11) 1.5(3) . . . . yes C(8) C(9) C(10) C(11) 0.9(4) . . . . yes C(8) C(9) C(10) C(11) 0.9(4) . . . . yes #--------------------------------------------------------------------------- data_Mn_f _database_code_depnum_ccdc_archive 'CCDC 274484' _audit_creation_date 'Wed May 25 14:00:14 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C12 H6 Mn O4 ' _chemical_formula_moiety 'C12 H6 Mn O4 ' _chemical_formula_weight 269.11 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 4.892(9) _cell_length_b 14.99(2) _cell_length_c 13.37(4) _cell_angle_alpha 90 _cell_angle_beta 91.82(6) _cell_angle_gamma 90 _cell_volume 980(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 60 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 233.2 #--------------------------------------------------------------------------- _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details REQABA _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.874 #--------------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 8752 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9836 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9836 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 #--------------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2221 _reflns_number_gt 1514 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0395 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1514 _refine_ls_number_parameters 154 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.44 _refine_diff_density_min -0.29 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #--------------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.24976(7) 0.43827(2) 0.49707(2) 0.01093(9) Uani 1.00 d . . . O(1) O 0.6201(3) 0.4452(1) 0.5946(1) 0.0113(4) Uani 1.00 d . . . O(2) O 1.0032(3) 0.3639(1) 0.5936(1) 0.0166(4) Uani 1.00 d . . . O(3) O 0.4917(3) 0.3593(1) 0.4038(1) 0.0160(4) Uani 1.00 d . . . O(4) O 0.8683(3) 0.4448(1) 0.4068(1) 0.0118(4) Uani 1.00 d . . . C(1) C 0.7610(4) 0.3760(2) 0.6180(2) 0.0120(6) Uani 1.00 d . . . C(2) C 0.6238(4) 0.3064(2) 0.6796(2) 0.0136(6) Uani 1.00 d . . . C(3) C 0.4525(5) 0.3353(2) 0.7527(2) 0.0165(6) Uani 1.00 d . . . C(4) C 0.3191(5) 0.2735(2) 0.8137(2) 0.0165(6) Uani 1.00 d . . . C(5) C 0.3563(4) 0.1835(2) 0.8017(2) 0.0129(5) Uani 1.00 d . . . C(6) C 0.5204(5) 0.1506(2) 0.7226(2) 0.0149(6) Uani 1.00 d . . . C(7) C 0.6587(5) 0.2135(2) 0.6621(2) 0.0148(6) Uani 1.00 d . . . C(8) C 0.5385(6) 0.0585(2) 0.6996(2) 0.0223(6) Uani 1.00 d . . . C(9) C 0.6833(7) 0.0295(2) 0.6202(2) 0.0326(8) Uani 1.00 d . . . C(10) C 0.8233(7) 0.0912(2) 0.5617(2) 0.0389(9) Uani 1.00 d . . . C(11) C 0.8142(6) 0.1800(2) 0.5816(2) 0.0275(7) Uani 1.00 d . . . C(12) C 0.7269(4) 0.3781(1) 0.3751(2) 0.0111(5) Uani 1.00 d . . . H(1) H 0.4240 0.3973 0.7620 0.0198 Uiso 1.00 calc . . . H(2) H 0.2015 0.2944 0.8638 0.0198 Uiso 1.00 calc . . . H(3) H 0.4484 0.0162 0.7401 0.0267 Uiso 1.00 calc . . . H(4) H 0.6894 -0.0323 0.6046 0.0392 Uiso 1.00 calc . . . H(5) H 0.9262 0.0705 0.5072 0.0466 Uiso 1.00 calc . . . H(6) H 0.9128 0.2204 0.5415 0.0330 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0089(2) 0.0089(2) 0.0153(2) -0.0001(2) 0.0047(1) -0.0001(2) O(1) 0.0113(7) 0.0114(8) 0.0114(7) -0.0004(7) 0.0030(6) 0.0020(6) O(2) 0.0113(8) 0.0159(9) 0.0228(9) -0.0003(7) 0.0047(7) 0.0076(7) O(3) 0.0128(8) 0.0154(9) 0.0202(8) -0.0002(7) 0.0063(7) -0.0054(7) O(4) 0.0116(8) 0.0112(8) 0.0128(7) 0.0008(7) 0.0031(6) -0.0032(6) C(1) 0.010(1) 0.014(1) 0.012(1) 0.0000(9) 0.0003(8) 0.0009(9) C(2) 0.010(1) 0.016(1) 0.015(1) -0.0006(9) 0.0030(8) 0.0051(9) C(3) 0.020(1) 0.011(1) 0.019(1) 0.0028(9) 0.0061(9) 0.0033(9) C(4) 0.015(1) 0.017(1) 0.018(1) 0.0020(10) 0.0082(9) 0.0033(9) C(5) 0.012(1) 0.012(1) 0.015(1) -0.0009(9) 0.0025(8) 0.0044(9) C(6) 0.016(1) 0.015(1) 0.014(1) 0.0011(10) 0.0030(9) 0.0040(9) C(7) 0.015(1) 0.013(1) 0.016(1) 0.0002(9) 0.0036(9) 0.0050(9) C(8) 0.032(1) 0.015(1) 0.020(1) -0.003(1) 0.007(1) 0.0007(10) C(9) 0.056(2) 0.013(1) 0.029(1) 0.001(1) 0.016(1) -0.002(1) C(10) 0.059(2) 0.025(2) 0.035(2) 0.006(1) 0.030(2) 0.000(1) C(11) 0.038(2) 0.020(1) 0.025(1) 0.000(1) 0.017(1) 0.004(1) C(12) 0.013(1) 0.009(1) 0.0120(10) 0.0030(9) 0.0022(8) -0.0018(8) #--------------------------------------------------------------------------- _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) O(1) 2.200(3) . . yes Mn(1) O(1) 2.238(2) . 3_666 yes Mn(1) O(2) 2.113(2) . 1_455 yes Mn(1) O(3) 2.110(2) . . yes Mn(1) O(4) 2.192(3) . 1_455 yes Mn(1) O(4) 2.260(2) . 3_666 yes O(1) C(1) 1.279(3) . . yes O(2) C(1) 1.252(3) . . yes O(3) C(12) 1.256(3) . . yes O(4) C(12) 1.281(3) . . yes C(1) C(2) 1.501(3) . . yes C(2) C(3) 1.376(3) . . yes C(2) C(7) 1.424(3) . . yes C(3) C(4) 1.409(3) . . yes C(4) C(5) 1.371(4) . . yes C(5) C(6) 1.436(3) . . yes C(5) C(12) 1.502(3) . 4_455 yes C(6) C(7) 1.427(3) . . yes C(6) C(8) 1.419(4) . . yes C(7) C(11) 1.428(3) . . yes C(8) C(9) 1.366(4) . . yes C(9) C(10) 1.404(4) . . yes C(10) C(11) 1.360(4) . . yes #--------------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(1) 92.54(8) . . 3_666 yes O(1) Mn(1) O(2) 97.9(1) . . 1_455 yes O(1) Mn(1) O(3) 84.8(1) . . . yes O(1) Mn(1) O(4) 173.97(6) . . 1_455 yes O(1) Mn(1) O(4) 81.19(8) . . 3_666 yes O(1) Mn(1) O(2) 157.59(6) 3_666 . 1_455 yes O(1) Mn(1) O(3) 86.57(7) 3_666 . . yes O(1) Mn(1) O(4) 85.17(8) 3_666 . 1_455 yes O(1) Mn(1) O(4) 77.75(6) 3_666 . 3_666 yes O(2) Mn(1) O(3) 113.98(8) 1_455 . . yes O(2) Mn(1) O(4) 82.4(1) 1_455 . 1_455 yes O(2) Mn(1) O(4) 84.33(7) 1_455 . 3_666 yes O(3) Mn(1) O(4) 100.57(10) . . 1_455 yes O(3) Mn(1) O(4) 158.42(6) . . 3_666 yes O(4) Mn(1) O(4) 92.87(7) 1_455 . 3_666 yes Mn(1) O(1) Mn(1) 87.46(8) . . 3_666 yes Mn(1) O(1) C(1) 122.3(1) . . . yes Mn(1) O(1) C(1) 127.3(2) 3_666 . . yes Mn(1) O(2) C(1) 130.2(2) 1_655 . . yes Mn(1) O(3) C(12) 126.2(2) . . . yes Mn(1) O(4) Mn(1) 87.13(7) 1_655 . 3_666 yes Mn(1) O(4) C(12) 126.1(1) 1_655 . . yes Mn(1) O(4) C(12) 130.5(2) 3_666 . . yes O(1) C(1) O(2) 124.2(2) . . . yes O(1) C(1) C(2) 116.8(2) . . . yes O(2) C(1) C(2) 119.0(2) . . . yes C(1) C(2) C(3) 117.7(2) . . . yes C(1) C(2) C(7) 122.1(2) . . . yes C(3) C(2) C(7) 120.2(2) . . . yes C(2) C(3) C(4) 120.5(2) . . . yes C(3) C(4) C(5) 120.9(2) . . . yes C(4) C(5) C(6) 120.2(2) . . . yes C(4) C(5) C(12) 117.9(2) . . 4_455 yes C(6) C(5) C(12) 121.8(2) . . 4_455 yes C(5) C(6) C(7) 118.5(2) . . . yes C(5) C(6) C(8) 122.3(2) . . . yes C(7) C(6) C(8) 119.1(2) . . . yes C(2) C(7) C(6) 119.5(2) . . . yes C(2) C(7) C(11) 122.5(2) . . . yes C(6) C(7) C(11) 117.9(2) . . . yes C(6) C(8) C(9) 121.1(2) . . . yes C(8) C(9) C(10) 119.8(3) . . . yes C(9) C(10) C(11) 121.1(3) . . . yes C(7) C(11) C(10) 120.9(2) . . . yes O(3) C(12) O(4) 124.4(2) . . . yes O(3) C(12) C(5) 118.1(2) . . 4_554 yes O(4) C(12) C(5) 117.5(2) . . 4_554 yes #--------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn(1) O(1) Mn(1) O(1) 0.0 . . 3_666 3_666 yes Mn(1) O(1) Mn(1) O(2) -118.1(2) . . 3_666 3_766 yes Mn(1) O(1) Mn(1) O(3) 84.7(1) . . 3_666 3_666 yes Mn(1) O(1) Mn(1) O(4) -80.41(9) . . 3_666 . yes Mn(1) O(1) Mn(1) O(4) -174.41(6) . . 3_666 3_766 yes Mn(1) O(1) C(1) O(2) 116.1(2) . . . . yes Mn(1) O(1) C(1) C(2) -64.7(2) . . . . yes Mn(1) O(1) Mn(1) O(1) 0.0 . 3_666 3_666 . yes Mn(1) O(1) Mn(1) O(2) 160.14(6) . 3_666 3_666 3_766 yes Mn(1) O(1) Mn(1) O(3) -86.32(7) . 3_666 3_666 3_666 yes Mn(1) O(1) Mn(1) O(4) 77.19(6) . 3_666 3_666 . yes Mn(1) O(1) Mn(1) O(4) 67.5(5) . 3_666 3_666 3_766 yes Mn(1) O(1) C(1) O(2) -1.5(3) . 3_666 3_666 3_666 yes Mn(1) O(1) C(1) C(2) 179.3(1) . 3_666 3_666 3_666 yes Mn(1) O(3) C(12) O(4) 7.5(3) . . . . yes Mn(1) O(3) C(12) C(5) -175.0(1) . . . 4_554 yes Mn(1) O(4) Mn(1) O(1) -178.99(6) . 1_455 3_566 3_566 yes Mn(1) O(4) Mn(1) O(3) -128.7(2) . 1_455 3_566 3_566 yes Mn(1) O(4) Mn(1) O(1) 9.6(5) . 3_666 3_566 3_566 yes Mn(1) O(4) Mn(1) O(3) 163.03(6) . 3_666 3_566 3_566 yes Mn(1) O(4) C(12) O(3) 9.6(3) . 3_666 3_666 3_666 yes O(1) Mn(1) O(1) Mn(1) 0.0 . . 3_666 3_666 yes O(1) Mn(1) O(1) C(1) -129.7(2) . . 3_666 3_666 yes O(1) Mn(1) O(3) C(12) -49.6(2) . . . . yes O(1) Mn(1) O(4) C(12) 41.9(2) . . 3_666 3_666 yes O(1) Mn(1) O(1) Mn(1) 0.0 . 3_666 3_666 . yes O(1) Mn(1) O(1) C(1) 133.6(2) . 3_666 3_666 3_666 yes O(1) Mn(1) O(4) C(12) 52.6(2) . 3_666 . . yes O(1) Mn(1) O(4) C(12) -142.4(2) . 3_666 3_766 3_766 yes O(1) C(1) C(2) C(3) -37.6(3) . . . . yes O(1) C(1) C(2) C(7) 140.1(2) . . . . yes O(2) Mn(1) O(1) C(1) -11.6(3) . 1_655 3_766 3_766 yes O(2) Mn(1) O(4) C(12) -56.3(2) . 1_655 . . yes O(2) Mn(1) O(4) C(12) 140.9(2) . 1_655 3_766 3_766 yes O(2) C(1) C(2) C(3) 141.6(2) . . . . yes O(2) C(1) C(2) C(7) -40.7(3) . . . . yes O(3) Mn(1) O(1) C(1) -47.3(2) . . . . yes O(3) Mn(1) O(1) C(1) 145.7(2) . . 3_666 3_666 yes O(3) Mn(1) O(4) C(12) -8.3(3) . . 3_666 3_666 yes O(4) Mn(1) O(1) C(1) 44.8(2) . 1_655 3_766 3_766 yes O(4) Mn(1) O(2) C(1) -40.7(2) . 1_655 . . yes O(4) Mn(1) O(4) C(12) -137.1(2) . 1_655 3_766 3_766 yes O(4) Mn(1) O(1) C(1) 49.2(2) . 3_666 . . yes O(4) Mn(1) O(1) C(1) -149.2(2) . 3_666 3_666 3_666 yes O(4) Mn(1) O(4) C(12) 140.1(2) . 3_666 3_766 3_766 yes C(1) C(2) C(3) C(4) -179.5(2) . . . . yes C(1) C(2) C(3) H(1) 0.5 . . . . no C(1) C(2) C(7) C(6) -179.3(2) . . . . yes C(1) C(2) C(7) C(11) -3.4(4) . . . . yes C(2) C(3) C(4) C(5) 0.0(4) . . . . yes C(2) C(3) C(4) H(2) 180.0 . . . . no C(2) C(7) C(6) C(5) -1.9(3) . . . . yes C(2) C(7) C(6) C(8) 175.0(2) . . . . yes C(2) C(7) C(11) C(10) -174.1(3) . . . . yes C(2) C(7) C(11) H(6) 5.9 . . . . no C(3) C(2) C(7) C(6) -1.7(3) . . . . yes C(3) C(2) C(7) C(11) 174.3(3) . . . . yes C(3) C(4) C(5) C(6) -3.6(4) . . . . yes C(3) C(4) C(5) C(12) 174.8(2) . . . 4_455 yes C(4) C(3) C(2) C(7) 2.7(4) . . . . yes C(4) C(5) C(6) C(7) 4.5(3) . . . . yes C(4) C(5) C(6) C(8) -172.2(2) . . . . yes C(5) C(4) C(3) H(1) 179.9 . . . . no C(5) C(6) C(7) C(11) -178.0(2) . . . . yes C(5) C(6) C(8) C(9) 176.1(3) . . . . yes C(5) C(6) C(8) H(3) -3.9 . . . . no C(6) C(5) C(4) H(2) 176.4 . . . . no C(6) C(7) C(11) C(10) 1.9(4) . . . . yes C(6) C(7) C(11) H(6) -178.1 . . . . no C(6) C(8) C(9) C(10) 1.8(5) . . . . yes C(6) C(8) C(9) H(4) -178.3 . . . . no C(7) C(2) C(3) H(1) -177.3 . . . . no C(7) C(6) C(5) C(12) -173.9(2) . . . 4_455 yes C(7) C(6) C(8) C(9) -0.6(4) . . . . yes C(7) C(6) C(8) H(3) 179.4 . . . . no C(7) C(11) C(10) C(9) -0.8(5) . . . . yes C(7) C(11) C(10) H(5) 179.2 . . . . no C(8) C(6) C(5) C(12) 9.4(4) . . . 4_455 yes C(8) C(6) C(7) C(11) -1.2(4) . . . . yes C(8) C(9) C(10) C(11) -1.0(5) . . . . yes C(8) C(9) C(10) H(5) 178.9 . . . . no C(9) C(10) C(11) H(6) 179.1 . . . . no C(10) C(9) C(8) H(3) -178.2 . . . . no C(11) C(10) C(9) H(4) 179.0 . . . . no H(1) C(3) C(4) H(2) -0.1 . . . . no H(3) C(8) C(9) H(4) 1.7 . . . . no H(4) C(9) C(10) H(5) -1.0 . . . . no H(5) C(10) C(11) H(6) -0.9 . . . . no H(5) C(10) C(11) H(6) -0.9 . . . . no #---------------------------------------------------------------------------