Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Cheng-Bing Ma' 'Chang-Neng Chen' 'Qiu-Tian Liu' _publ_contact_author_name 'Prof. Qiu-Tian Liu' _publ_contact_author_address ; Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences 155# West Yangqiao Road Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email lqt@ms.fjirsm.ac.cn _publ_section_title ; Framework variations in Mn(II)-organic coordination polymers: solvent templated formation and characterisation of 1D zigzag and straight chain network isomers ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; data_1a _database_code_depnum_ccdc_archive 'CCDC 281959' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H25 Mn N3 O6' _chemical_formula_weight 590.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7627(3) _cell_length_b 11.4014(2) _cell_length_c 14.1535(3) _cell_angle_alpha 67.0620(10) _cell_angle_beta 75.6750(10) _cell_angle_gamma 62.1140(10) _cell_volume 1409.18(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4716 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.06 _exptl_crystal_description rhombohedral _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max .35 _exptl_crystal_size_mid .33 _exptl_crystal_size_min .29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .834 _exptl_absorpt_correction_T_max .861 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7340 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4905 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+1.3875P] 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 4905 _refine_ls_number_parameters 384 _refine_ls_number_restraints 4 _refine_ls_R_factor_ref 0.0677 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Mn Mn 0.27058(5) -0.18786(5) 1.45287(3) 0.03554(18) Uani 1 1 d . . . N1 N 0.5003(3) -0.2434(3) 1.4576(2) 0.0418(6) Uani 1 1 d . . . N2 N 0.2937(3) 0.0163(3) 1.3917(2) 0.0416(6) Uani 1 1 d . . . N3 N -0.3554(10) 0.0003(13) 1.1095(7) 0.163(3) Uani 1 1 d . . . O1 O 0.3181(2) -0.2907(3) 1.34373(18) 0.0474(6) Uani 1 1 d . . . O2 O 0.1118(3) -0.2370(5) 1.2944(3) 0.1021(14) Uani 1 1 d . . . O3 O 0.2703(3) -0.3716(2) 1.58966(18) 0.0533(6) Uani 1 1 d . . . O4 O 0.1705(2) -0.1653(2) 1.61102(17) 0.0429(5) Uani 1 1 d . . . O5 O 0.0541(3) -0.0901(3) 1.4139(2) 0.0619(7) Uani 1 1 d D . . H5A H -0.015(4) -0.012(3) 1.408(4) 0.076(15) Uiso 1 1 d D . . H5B H 0.049(6) -0.125(5) 1.374(3) 0.095(18) Uiso 1 1 d D . . O6 O -0.050(2) -0.016(2) 1.1087(16) 0.512(17) Uani 1 1 d D . . H6B H -0.060(5) -0.087(4) 1.102(3) 0.050 Uiso 1 1 d D . . H6C H 0.008(5) 0.021(5) 1.094(4) 0.050 Uiso 1 1 d D . . C1 C 0.2433(4) -0.2908(4) 1.2877(3) 0.0521(9) Uani 1 1 d . . . C2 C 0.3198(4) -0.3605(4) 1.2066(3) 0.0482(8) Uani 1 1 d . . . C3 C 0.2464(4) -0.3560(6) 1.1369(4) 0.0824(16) Uani 1 1 d . . . H3A H 0.1483 -0.3165 1.1441 0.099 Uiso 1 1 calc R . . C4 C 0.3158(5) -0.4092(6) 1.0568(4) 0.0872(18) Uani 1 1 d . . . H4A H 0.2634 -0.4019 1.0098 0.105 Uiso 1 1 calc R . . C5 C 0.4620(4) -0.4734(4) 1.0445(3) 0.0465(8) Uani 1 1 d . . . C6 C 0.5346(4) -0.4850(4) 1.1185(3) 0.0494(8) Uani 1 1 d . . . H6A H 0.6324 -0.5312 1.1149 0.059 Uiso 1 1 calc R . . C7 C 0.4644(4) -0.4293(4) 1.1974(3) 0.0489(8) Uani 1 1 d . . . H7A H 0.5163 -0.4385 1.2456 0.059 Uiso 1 1 calc R . . C8 C 0.1980(3) -0.2948(3) 1.6450(2) 0.0391(7) Uani 1 1 d . . . C9 C 0.1426(3) -0.3559(3) 1.7508(2) 0.0397(7) Uani 1 1 d . . . C10 C 0.1528(4) -0.4916(4) 1.7828(3) 0.0543(9) Uani 1 1 d . . . H10A H 0.1966 -0.5451 1.7387 0.065 Uiso 1 1 calc R . . C11 C 0.0977(5) -0.5475(4) 1.8801(3) 0.0610(11) Uani 1 1 d . . . H11A H 0.1064 -0.6389 1.9010 0.073 Uiso 1 1 calc R . . C12 C 0.0297(3) -0.4696(4) 1.9474(2) 0.0438(8) Uani 1 1 d . . . C13 C 0.0227(4) -0.3350(4) 1.9142(3) 0.0495(8) Uani 1 1 d . . . H13A H -0.0197 -0.2816 1.9583 0.059 Uiso 1 1 calc R . . C14 C 0.0770(4) -0.2785(4) 1.8173(3) 0.0468(8) Uani 1 1 d . . . H14A H 0.0693 -0.1875 1.7967 0.056 Uiso 1 1 calc R . . C15 C 0.6015(4) -0.3718(4) 1.4890(3) 0.0557(9) Uani 1 1 d . . . H15A H 0.5765 -0.4471 1.5190 0.067 Uiso 1 1 calc R . . C16 C 0.7439(4) -0.3982(5) 1.4788(4) 0.0733(13) Uani 1 1 d . . . H16A H 0.8121 -0.4894 1.5010 0.088 Uiso 1 1 calc R . . C17 C 0.7812(4) -0.2885(5) 1.4360(4) 0.0731(12) Uani 1 1 d . . . H17A H 0.8756 -0.3047 1.4287 0.088 Uiso 1 1 calc R . . C18 C 0.6782(4) -0.1518(4) 1.4030(3) 0.0558(9) Uani 1 1 d . . . C19 C 0.7066(5) -0.0284(5) 1.3583(4) 0.0690(12) Uani 1 1 d . . . H19A H 0.7992 -0.0390 1.3508 0.083 Uiso 1 1 calc R . . C20 C 0.6044(5) 0.1002(5) 1.3275(4) 0.0671(11) Uani 1 1 d . . . H20A H 0.6269 0.1770 1.2990 0.081 Uiso 1 1 calc R . . C21 C 0.4611(4) 0.1211(4) 1.3379(3) 0.0533(9) Uani 1 1 d . . . C22 C 0.3497(5) 0.2533(4) 1.3055(4) 0.0689(12) Uani 1 1 d . . . H22A H 0.3674 0.3331 1.2761 0.083 Uiso 1 1 calc R . . C23 C 0.2167(5) 0.2646(4) 1.3171(4) 0.0723(12) Uani 1 1 d . . . H23A H 0.1422 0.3521 1.2962 0.087 Uiso 1 1 calc R . . C24 C 0.1919(4) 0.1437(4) 1.3609(3) 0.0578(10) Uani 1 1 d . . . H24A H 0.0996 0.1532 1.3688 0.069 Uiso 1 1 calc R . . C25 C 0.5375(3) -0.1336(4) 1.4147(2) 0.0422(7) Uani 1 1 d . . . C26 C 0.4273(4) 0.0036(4) 1.3812(2) 0.0413(7) Uani 1 1 d . . . C30 C -0.3823(17) -0.1049(11) 1.1564(7) 0.163(5) Uani 1 1 d . . . H30A H -0.3096 -0.1918 1.1830 0.196 Uiso 1 1 calc R . . C31 C -0.511(3) -0.0938(19) 1.1682(11) 0.221(12) Uani 1 1 d . . . H31A H -0.5297 -0.1728 1.2031 0.265 Uiso 1 1 calc R . . C32 C -0.618(2) 0.032(3) 1.1300(14) 0.244(13) Uani 1 1 d . . . H32A H -0.7100 0.0396 1.1373 0.293 Uiso 1 1 calc R . . C33 C -0.5897(19) 0.145(2) 1.0813(12) 0.218(9) Uani 1 1 d . . . H33A H -0.6597 0.2343 1.0546 0.262 Uiso 1 1 calc R . . C34 C -0.4535(18) 0.1220(11) 1.0738(7) 0.159(4) Uani 1 1 d . . . H34A H -0.4295 0.1977 1.0410 0.191 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 Mn 0.0351(3) 0.0388(3) 0.0340(3) -0.0145(2) 0.00371(18) -0.0172(2) N1 0.0387(14) 0.0439(15) 0.0464(15) -0.0204(12) -0.0008(12) -0.0165(12) N2 0.0406(15) 0.0404(15) 0.0426(15) -0.0115(12) -0.0019(11) -0.0180(12) N3 0.198(9) 0.165(8) 0.124(6) -0.052(6) -0.002(6) -0.076(8) O1 0.0456(13) 0.0534(14) 0.0451(13) -0.0274(11) -0.0007(10) -0.0142(11) O2 0.0405(16) 0.167(4) 0.140(3) -0.126(3) 0.0046(17) -0.0201(19) O3 0.0654(16) 0.0437(13) 0.0400(13) -0.0154(11) 0.0137(11) -0.0211(12) O4 0.0465(13) 0.0387(12) 0.0390(12) -0.0119(10) 0.0063(10) -0.0192(10) O5 0.0387(14) 0.0717(19) 0.083(2) -0.0516(17) -0.0093(13) -0.0057(13) O6 0.46(3) 0.47(3) 0.39(2) -0.23(2) -0.10(2) 0.09(2) C1 0.045(2) 0.061(2) 0.058(2) -0.0357(19) -0.0020(16) -0.0151(17) C2 0.0423(18) 0.056(2) 0.053(2) -0.0314(17) -0.0029(15) -0.0146(16) C3 0.039(2) 0.127(4) 0.100(4) -0.086(3) -0.003(2) -0.011(2) C4 0.050(2) 0.141(5) 0.095(4) -0.089(4) -0.013(2) -0.014(3) C5 0.0433(18) 0.0474(19) 0.049(2) -0.0244(16) -0.0073(15) -0.0104(15) C6 0.0413(18) 0.057(2) 0.0470(19) -0.0259(17) -0.0077(15) -0.0085(16) C7 0.048(2) 0.057(2) 0.0432(19) -0.0261(16) -0.0060(15) -0.0143(16) C8 0.0332(15) 0.0461(18) 0.0346(16) -0.0138(14) 0.0014(12) -0.0151(13) C9 0.0370(16) 0.0446(18) 0.0319(16) -0.0105(14) -0.0024(13) -0.0141(14) C10 0.066(2) 0.048(2) 0.0402(19) -0.0177(16) 0.0130(16) -0.0220(18) C11 0.081(3) 0.042(2) 0.046(2) -0.0122(16) 0.0137(19) -0.0244(19) C12 0.0417(17) 0.0461(18) 0.0342(17) -0.0094(14) 0.0000(13) -0.0151(14) C13 0.056(2) 0.052(2) 0.0341(17) -0.0162(15) 0.0054(15) -0.0191(17) C14 0.055(2) 0.0424(18) 0.0372(17) -0.0110(14) 0.0032(15) -0.0209(16) C15 0.049(2) 0.046(2) 0.070(3) -0.0240(18) -0.0063(18) -0.0141(17) C16 0.047(2) 0.056(2) 0.110(4) -0.034(2) -0.016(2) -0.0060(19) C17 0.039(2) 0.084(3) 0.103(4) -0.042(3) -0.008(2) -0.021(2) C18 0.043(2) 0.068(2) 0.067(2) -0.029(2) -0.0053(17) -0.0259(18) C19 0.054(2) 0.092(3) 0.081(3) -0.024(3) -0.006(2) -0.049(2) C20 0.070(3) 0.070(3) 0.076(3) -0.011(2) -0.011(2) -0.048(2) C21 0.065(2) 0.057(2) 0.049(2) -0.0121(17) -0.0044(17) -0.0388(19) C22 0.084(3) 0.047(2) 0.081(3) -0.008(2) -0.017(2) -0.037(2) C23 0.072(3) 0.043(2) 0.091(3) -0.007(2) -0.022(2) -0.020(2) C24 0.050(2) 0.045(2) 0.070(3) -0.0088(18) -0.0084(18) -0.0184(17) C25 0.0407(17) 0.0515(19) 0.0402(17) -0.0193(15) -0.0012(13) -0.0210(15) C26 0.0474(19) 0.0479(18) 0.0351(16) -0.0129(14) -0.0022(14) -0.0259(15) C30 0.282(17) 0.097(6) 0.086(6) -0.033(5) 0.006(7) -0.066(8) C31 0.43(3) 0.254(18) 0.111(9) -0.097(11) 0.097(15) -0.28(2) C32 0.24(2) 0.46(4) 0.139(16) -0.17(2) 0.042(13) -0.20(3) C33 0.179(14) 0.242(19) 0.144(12) -0.080(11) -0.059(11) 0.018(12) C34 0.263(14) 0.090(6) 0.115(7) -0.012(5) -0.027(8) -0.078(8) _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 Mn O1 2.117(2) . ? Mn O5 2.169(3) . ? Mn O3 2.231(2) . ? Mn N2 2.257(3) . ? Mn N1 2.258(3) . ? Mn O4 2.288(2) . ? Mn C8 2.597(3) . ? N1 C15 1.329(5) . ? N1 C25 1.361(4) . ? N2 C24 1.324(5) . ? N2 C26 1.351(4) . ? N3 C30 1.254(13) . ? N3 C34 1.282(13) . ? O1 C1 1.262(4) . ? O2 C1 1.247(5) . ? O3 C8 1.258(4) . ? O4 C8 1.267(4) . ? O5 H5A 0.844(19) . ? O5 H5B 0.84(2) . ? C1 C2 1.503(5) . ? C2 C7 1.375(5) . ? C2 C3 1.382(5) . ? C3 C4 1.380(6) . ? C3 H3A 0.9300 . ? C4 C5 1.389(6) . ? C4 H4A 0.9300 . ? C5 C6 1.387(5) . ? C5 C5 1.498(7) 2_647 ? C6 C7 1.382(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.490(4) . ? C9 C14 1.377(5) . ? C9 C10 1.390(5) . ? C10 C11 1.386(5) . ? C10 H10A 0.9300 . ? C11 C12 1.392(5) . ? C11 H11A 0.9300 . ? C12 C13 1.388(5) . ? C12 C12 1.498(6) 2_549 ? C13 C14 1.380(5) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.397(6) . ? C15 H15A 0.9300 . ? C16 C17 1.360(7) . ? C16 H16A 0.9300 . ? C17 C18 1.396(6) . ? C17 H17A 0.9300 . ? C18 C25 1.405(5) . ? C18 C19 1.444(6) . ? C19 C20 1.334(6) . ? C19 H19A 0.9300 . ? C20 C21 1.424(6) . ? C20 H20A 0.9300 . ? C21 C22 1.401(6) . ? C21 C26 1.417(5) . ? C22 C23 1.349(6) . ? C22 H22A 0.9300 . ? C23 C24 1.396(6) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.429(5) . ? C30 C31 1.31(2) . ? C30 H30A 0.9300 . ? C31 C32 1.35(2) . ? C31 H31A 0.9300 . ? C32 C33 1.35(2) . ? C32 H32A 0.9300 . ? C33 C34 1.345(18) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn O5 86.26(10) . . ? O1 Mn O3 95.01(9) . . ? O5 Mn O3 101.19(12) . . ? O1 Mn N2 115.46(10) . . ? O5 Mn N2 93.82(11) . . ? O3 Mn N2 146.87(10) . . ? O1 Mn N1 92.26(9) . . ? O5 Mn N1 165.16(12) . . ? O3 Mn N1 93.65(10) . . ? N2 Mn N1 73.48(10) . . ? O1 Mn O4 148.75(9) . . ? O5 Mn O4 84.30(10) . . ? O3 Mn O4 58.03(8) . . ? N2 Mn O4 94.87(9) . . ? N1 Mn O4 104.05(9) . . ? O1 Mn C8 121.82(10) . . ? O5 Mn C8 91.36(11) . . ? O3 Mn C8 28.94(9) . . ? N2 Mn C8 122.70(10) . . ? N1 Mn C8 101.90(10) . . ? O4 Mn C8 29.20(9) . . ? C15 N1 C25 118.3(3) . . ? C15 N1 Mn 126.3(2) . . ? C25 N1 Mn 115.1(2) . . ? C24 N2 C26 118.1(3) . . ? C24 N2 Mn 126.7(2) . . ? C26 N2 Mn 115.1(2) . . ? C30 N3 C34 121.1(12) . . ? C1 O1 Mn 133.1(2) . . ? C8 O3 Mn 91.90(19) . . ? C8 O4 Mn 89.08(18) . . ? Mn O5 H5A 137(3) . . ? Mn O5 H5B 109(4) . . ? H5A O5 H5B 109(5) . . ? O2 C1 O1 125.0(3) . . ? O2 C1 C2 118.0(3) . . ? O1 C1 C2 117.0(3) . . ? C7 C2 C3 117.3(3) . . ? C7 C2 C1 122.0(3) . . ? C3 C2 C1 120.7(3) . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 121.6(4) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C6 C5 C4 116.6(3) . . ? C6 C5 C5 121.5(4) . 2_647 ? C4 C5 C5 121.8(4) . 2_647 ? C7 C6 C5 121.4(3) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C2 121.7(3) . . ? C6 C7 H7A 119.2 . . ? C2 C7 H7A 119.2 . . ? O3 C8 O4 120.5(3) . . ? O3 C8 C9 119.8(3) . . ? O4 C8 C9 119.7(3) . . ? O3 C8 Mn 59.16(16) . . ? O4 C8 Mn 61.72(16) . . ? C9 C8 Mn 173.4(2) . . ? C14 C9 C10 119.0(3) . . ? C14 C9 C8 121.0(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 121.3(4) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C13 C12 C11 117.3(3) . . ? C13 C12 C12 121.5(4) . 2_549 ? C11 C12 C12 121.1(4) . 2_549 ? C14 C13 C12 121.7(3) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C9 C14 C13 120.5(3) . . ? C9 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? N1 C15 C16 122.7(4) . . ? N1 C15 H15A 118.7 . . ? C16 C15 H15A 118.7 . . ? C17 C16 C15 119.1(4) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C25 117.5(4) . . ? C17 C18 C19 124.4(4) . . ? C25 C18 C19 118.0(4) . . ? C20 C19 C18 122.2(4) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C22 C21 C26 117.3(3) . . ? C22 C21 C20 123.3(4) . . ? C26 C21 C20 119.4(4) . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? N2 C24 C23 123.1(4) . . ? N2 C24 H24A 118.5 . . ? C23 C24 H24A 118.5 . . ? N1 C25 C18 122.2(3) . . ? N1 C25 C26 117.5(3) . . ? C18 C25 C26 120.2(3) . . ? N2 C26 C21 122.2(3) . . ? N2 C26 C25 118.4(3) . . ? C21 C26 C25 119.4(3) . . ? N3 C30 C31 120.7(14) . . ? N3 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C30 C31 C32 120.5(16) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C33 C32 C31 119(2) . . ? C33 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? C32 C33 C34 115.8(17) . . ? C32 C33 H33A 122.1 . . ? C34 C33 H33A 122.1 . . ? N3 C34 C33 123.2(12) . . ? N3 C34 H34A 118.4 . . ? C33 C34 H34A 118.4 . . ? 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 O1 Mn N1 C15 -63.2(3) . . . . ? O5 Mn N1 C15 -147.1(4) . . . . ? O3 Mn N1 C15 32.0(3) . . . . ? N2 Mn N1 C15 -179.1(3) . . . . ? O4 Mn N1 C15 89.9(3) . . . . ? C8 Mn N1 C15 60.0(3) . . . . ? O1 Mn N1 C25 110.3(2) . . . . ? O5 Mn N1 C25 26.4(5) . . . . ? O3 Mn N1 C25 -154.5(2) . . . . ? N2 Mn N1 C25 -5.6(2) . . . . ? O4 Mn N1 C25 -96.6(2) . . . . ? C8 Mn N1 C25 -126.5(2) . . . . ? O1 Mn N2 C24 96.6(3) . . . . ? O5 Mn N2 C24 9.0(3) . . . . ? O3 Mn N2 C24 -108.3(3) . . . . ? N1 Mn N2 C24 -178.8(3) . . . . ? O4 Mn N2 C24 -75.6(3) . . . . ? C8 Mn N2 C24 -85.1(3) . . . . ? O1 Mn N2 C26 -79.7(2) . . . . ? O5 Mn N2 C26 -167.3(2) . . . . ? O3 Mn N2 C26 75.4(3) . . . . ? N1 Mn N2 C26 4.9(2) . . . . ? O4 Mn N2 C26 108.1(2) . . . . ? C8 Mn N2 C26 98.6(2) . . . . ? O5 Mn O1 C1 -2.2(4) . . . . ? O3 Mn O1 C1 98.8(4) . . . . ? N2 Mn O1 C1 -94.6(4) . . . . ? N1 Mn O1 C1 -167.4(3) . . . . ? O4 Mn O1 C1 70.4(4) . . . . ? C8 Mn O1 C1 87.1(4) . . . . ? O1 Mn O3 C8 -159.3(2) . . . . ? O5 Mn O3 C8 -72.1(2) . . . . ? N2 Mn O3 C8 43.2(3) . . . . ? N1 Mn O3 C8 108.2(2) . . . . ? O4 Mn O3 C8 3.86(18) . . . . ? O1 Mn O4 C8 30.1(3) . . . . ? O5 Mn O4 C8 103.2(2) . . . . ? O3 Mn O4 C8 -3.82(18) . . . . ? N2 Mn O4 C8 -163.47(19) . . . . ? N1 Mn O4 C8 -89.31(19) . . . . ? Mn O1 C1 O2 -9.2(7) . . . . ? Mn O1 C1 C2 170.4(2) . . . . ? O2 C1 C2 C7 -176.3(4) . . . . ? O1 C1 C2 C7 4.1(6) . . . . ? O2 C1 C2 C3 4.6(7) . . . . ? O1 C1 C2 C3 -175.0(4) . . . . ? C7 C2 C3 C4 -4.7(8) . . . . ? C1 C2 C3 C4 174.4(5) . . . . ? C2 C3 C4 C5 2.1(10) . . . . ? C3 C4 C5 C6 1.8(8) . . . . ? C3 C4 C5 C5 -177.7(6) . . . 2_647 ? C4 C5 C6 C7 -3.0(6) . . . . ? C5 C5 C6 C7 176.5(4) 2_647 . . . ? C5 C6 C7 C2 0.3(6) . . . . ? C3 C2 C7 C6 3.6(6) . . . . ? C1 C2 C7 C6 -175.6(4) . . . . ? Mn O3 C8 O4 -6.9(3) . . . . ? Mn O3 C8 C9 172.4(3) . . . . ? Mn O4 C8 O3 6.7(3) . . . . ? Mn O4 C8 C9 -172.6(3) . . . . ? O1 Mn C8 O3 24.5(2) . . . . ? O5 Mn C8 O3 111.0(2) . . . . ? N2 Mn C8 O3 -153.6(2) . . . . ? N1 Mn C8 O3 -75.7(2) . . . . ? O4 Mn C8 O3 -173.3(3) . . . . ? O1 Mn C8 O4 -162.18(17) . . . . ? O5 Mn C8 O4 -75.74(19) . . . . ? O3 Mn C8 O4 173.3(3) . . . . ? N2 Mn C8 O4 19.7(2) . . . . ? N1 Mn C8 O4 97.56(18) . . . . ? O1 Mn C8 C9 -58(2) . . . . ? O5 Mn C8 C9 28(2) . . . . ? O3 Mn C8 C9 -83(2) . . . . ? N2 Mn C8 C9 123(2) . . . . ? N1 Mn C8 C9 -159(2) . . . . ? O4 Mn C8 C9 104(2) . . . . ? O3 C8 C9 C14 172.5(3) . . . . ? O4 C8 C9 C14 -8.2(5) . . . . ? Mn C8 C9 C14 -108(2) . . . . ? O3 C8 C9 C10 -9.5(5) . . . . ? O4 C8 C9 C10 169.8(3) . . . . ? Mn C8 C9 C10 70(2) . . . . ? C14 C9 C10 C11 -0.1(6) . . . . ? C8 C9 C10 C11 -178.1(4) . . . . ? C9 C10 C11 C12 0.9(7) . . . . ? C10 C11 C12 C13 -1.8(6) . . . . ? C10 C11 C12 C12 180.0(4) . . . 2_549 ? C11 C12 C13 C14 1.9(6) . . . . ? C12 C12 C13 C14 -179.9(4) 2_549 . . . ? C10 C9 C14 C13 0.2(5) . . . . ? C8 C9 C14 C13 178.2(3) . . . . ? C12 C13 C14 C9 -1.1(6) . . . . ? C25 N1 C15 C16 -0.7(6) . . . . ? Mn N1 C15 C16 172.6(3) . . . . ? N1 C15 C16 C17 0.7(7) . . . . ? C15 C16 C17 C18 0.1(8) . . . . ? C16 C17 C18 C25 -0.8(7) . . . . ? C16 C17 C18 C19 178.9(5) . . . . ? C17 C18 C19 C20 179.7(5) . . . . ? C25 C18 C19 C20 -0.6(7) . . . . ? C18 C19 C20 C21 0.1(7) . . . . ? C19 C20 C21 C22 -179.0(4) . . . . ? C19 C20 C21 C26 -0.1(6) . . . . ? C26 C21 C22 C23 0.6(7) . . . . ? C20 C21 C22 C23 179.5(4) . . . . ? C21 C22 C23 C24 -0.4(7) . . . . ? C26 N2 C24 C23 0.9(6) . . . . ? Mn N2 C24 C23 -175.3(3) . . . . ? C22 C23 C24 N2 -0.4(7) . . . . ? C15 N1 C25 C18 -0.1(5) . . . . ? Mn N1 C25 C18 -174.1(3) . . . . ? C15 N1 C25 C26 179.9(3) . . . . ? Mn N1 C25 C26 5.8(4) . . . . ? C17 C18 C25 N1 0.8(6) . . . . ? C19 C18 C25 N1 -178.9(3) . . . . ? C17 C18 C25 C26 -179.2(4) . . . . ? C19 C18 C25 C26 1.1(5) . . . . ? C24 N2 C26 C21 -0.6(5) . . . . ? Mn N2 C26 C21 176.0(3) . . . . ? C24 N2 C26 C25 179.7(3) . . . . ? Mn N2 C26 C25 -3.7(4) . . . . ? C22 C21 C26 N2 -0.1(5) . . . . ? C20 C21 C26 N2 -179.0(3) . . . . ? C22 C21 C26 C25 179.6(3) . . . . ? C20 C21 C26 C25 0.6(5) . . . . ? N1 C25 C26 N2 -1.5(4) . . . . ? C18 C25 C26 N2 178.5(3) . . . . ? N1 C25 C26 C21 178.9(3) . . . . ? C18 C25 C26 C21 -1.2(5) . . . . ? C34 N3 C30 C31 1.4(16) . . . . ? N3 C30 C31 C32 0(2) . . . . ? C30 C31 C32 C33 -1(3) . . . . ? C31 C32 C33 C34 1(2) . . . . ? C30 N3 C34 C33 -1.6(17) . . . . ? C32 C33 C34 N3 0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.632 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.066 #===========END data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 Mn N6 O5' _chemical_formula_weight 665.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7030(11) _cell_length_b 19.5247(13) _cell_length_c 10.4621(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.899(3) _cell_angle_gamma 90.00 _cell_volume 2949.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4938 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max .40 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .824 _exptl_absorpt_correction_T_max .860 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16159 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4497 _reflns_number_gt 4105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+2.4232P] 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 0.0050(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4497 _refine_ls_number_parameters 316 _refine_ls_number_restraints 2 _refine_ls_R_factor_ref 0.0623 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Mn Mn 0.12498(3) 0.31978(2) 0.34498(4) 0.0373(2) Uani 1 1 d . . . N1 N 0.1190(2) 0.38553(13) 0.5248(2) 0.0481(7) Uani 1 1 d . . . N2 N 0.1073(2) 0.43103(13) 0.2775(3) 0.0478(7) Uani 1 1 d . . . O1 O 0.27675(18) 0.31902(14) 0.3964(2) 0.0603(7) Uani 1 1 d . . . O2 O 0.21848(18) 0.30377(15) 0.1917(3) 0.0613(7) Uani 1 1 d . . . O3 O 0.96216(17) 0.31877(13) 0.0200(2) 0.0545(7) Uani 1 1 d . . . O4 O 1.00468(16) 0.28680(13) 0.2270(2) 0.0530(6) Uani 1 1 d . . . O5 O 0.12013(18) 0.22658(12) 0.4534(2) 0.0455(6) Uani 1 1 d D . . H5B H 0.1620(19) 0.2167(17) 0.516(3) 0.047(10) Uiso 1 1 d D . . H5C H 0.069(2) 0.214(2) 0.472(4) 0.081(16) Uiso 1 1 d D . . C1 C 0.1256(3) 0.3630(2) 0.6452(3) 0.0637(11) Uani 1 1 d . . . H1A H 0.1240 0.3161 0.6592 0.076 Uiso 1 1 calc R . . C2 C 0.1350(4) 0.4070(2) 0.7526(4) 0.0821(14) Uani 1 1 d . . . H2A H 0.1399 0.3893 0.8362 0.099 Uiso 1 1 calc R . . C3 C 0.1370(4) 0.4753(2) 0.7333(4) 0.0838(15) Uani 1 1 d . . . H3A H 0.1436 0.5050 0.8040 0.101 Uiso 1 1 calc R . . C4 C 0.1292(3) 0.50138(19) 0.6074(4) 0.0661(11) Uani 1 1 d . . . C5 C 0.1287(4) 0.5725(2) 0.5777(5) 0.0898(16) Uani 1 1 d . . . H5A H 0.1350 0.6041 0.6454 0.108 Uiso 1 1 calc R . . C6 C 0.1195(4) 0.5955(2) 0.4550(5) 0.0871(15) Uani 1 1 d . . . H6A H 0.1181 0.6424 0.4393 0.105 Uiso 1 1 calc R . . C7 C 0.1116(3) 0.54910(18) 0.3487(4) 0.0621(10) Uani 1 1 d . . . C8 C 0.1022(3) 0.5699(2) 0.2188(4) 0.0747(13) Uani 1 1 d . . . H8A H 0.0999 0.6163 0.1981 0.090 Uiso 1 1 calc R . . C9 C 0.0965(3) 0.5223(2) 0.1234(4) 0.0713(12) Uani 1 1 d . . . H9A H 0.0906 0.5356 0.0369 0.086 Uiso 1 1 calc R . . C10 C 0.0994(3) 0.4530(2) 0.1563(3) 0.0627(10) Uani 1 1 d . . . H10A H 0.0956 0.4208 0.0900 0.075 Uiso 1 1 calc R . . C11 C 0.1129(3) 0.47838(16) 0.3732(3) 0.0485(8) Uani 1 1 d . . . C12 C 0.1207(3) 0.45388(16) 0.5051(3) 0.0485(8) Uani 1 1 d . . . C13 C 0.2885(3) 0.31085(16) 0.2818(4) 0.0465(9) Uani 1 1 d . . . C14 C 0.3829(3) 0.31086(17) 0.2529(3) 0.0456(9) Uani 1 1 d . . . C15 C 0.4005(3) 0.3060(2) 0.1282(4) 0.0605(11) Uani 1 1 d . . . H15A H 0.3511 0.3021 0.0585 0.073 Uiso 1 1 calc R . . C16 C 0.4901(3) 0.3068(2) 0.1047(4) 0.0585(11) Uani 1 1 d . . . H16A H 0.4998 0.3054 0.0194 0.070 Uiso 1 1 calc R . . C17 C 0.5658(3) 0.30969(17) 0.2068(3) 0.0477(9) Uani 1 1 d . . . C18 C 0.5473(3) 0.3147(2) 0.3324(4) 0.0576(11) Uani 1 1 d . . . H18A H 0.5965 0.3170 0.4026 0.069 Uiso 1 1 calc R . . C19 C 0.4583(3) 0.3162(2) 0.3553(4) 0.0560(10) Uani 1 1 d . . . H19A H 0.4484 0.3208 0.4400 0.067 Uiso 1 1 calc R . . C20 C 0.9441(2) 0.30331(15) 0.1276(3) 0.0402(8) Uani 1 1 d . . . C21 C 0.8456(2) 0.30302(15) 0.1451(3) 0.0370(8) Uani 1 1 d . . . C22 C 0.7772(3) 0.33555(18) 0.0566(3) 0.0461(9) Uani 1 1 d . . . H22A H 0.7923 0.3558 -0.0171 0.055 Uiso 1 1 calc R . . C23 C 0.6876(3) 0.3383(2) 0.0763(3) 0.0529(9) Uani 1 1 d . . . H23A H 0.6433 0.3612 0.0163 0.063 Uiso 1 1 calc R . . C24 C 0.6613(2) 0.30757(17) 0.1837(3) 0.0448(9) Uani 1 1 d . . . C25 C 0.7303(3) 0.27418(17) 0.2719(3) 0.0485(9) Uani 1 1 d . . . H25A H 0.7149 0.2531 0.3446 0.058 Uiso 1 1 calc R . . C26 C 0.8207(3) 0.27180(16) 0.2535(3) 0.0434(8) Uani 1 1 d . . . H26A H 0.8653 0.2493 0.3137 0.052 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 Mn 0.0325(4) 0.0453(3) 0.0354(3) -0.00087(17) 0.0099(2) -0.00186(18) N1 0.060(2) 0.0453(14) 0.0417(14) 0.0034(11) 0.0169(13) 0.0046(13) N2 0.053(2) 0.0479(15) 0.0433(14) 0.0053(11) 0.0104(12) -0.0025(12) O1 0.0375(19) 0.096(2) 0.0508(14) 0.0002(12) 0.0172(12) -0.0025(12) O2 0.0310(17) 0.0947(19) 0.0595(15) -0.0236(13) 0.0118(12) -0.0083(12) O3 0.0352(17) 0.0846(18) 0.0478(13) 0.0067(11) 0.0184(11) 0.0072(11) O4 0.0317(15) 0.0733(16) 0.0519(13) 0.0056(11) 0.0025(10) -0.0020(11) O5 0.0362(18) 0.0580(14) 0.0423(12) 0.0082(10) 0.0072(11) -0.0047(11) C1 0.092(3) 0.057(2) 0.0476(19) 0.0053(16) 0.0263(19) 0.006(2) C2 0.126(4) 0.082(3) 0.046(2) 0.0015(19) 0.035(2) 0.004(3) C3 0.133(5) 0.073(3) 0.053(2) -0.016(2) 0.037(3) -0.005(3) C4 0.092(3) 0.056(2) 0.058(2) -0.0080(17) 0.031(2) -0.003(2) C5 0.144(5) 0.052(2) 0.084(3) -0.019(2) 0.047(3) -0.010(3) C6 0.136(5) 0.041(2) 0.092(3) 0.000(2) 0.041(3) -0.004(2) C7 0.074(3) 0.0454(19) 0.069(2) 0.0086(16) 0.021(2) -0.0036(17) C8 0.091(4) 0.052(2) 0.081(3) 0.023(2) 0.018(2) -0.004(2) C9 0.088(3) 0.068(3) 0.056(2) 0.0189(19) 0.009(2) -0.015(2) C10 0.075(3) 0.069(2) 0.0439(19) 0.0074(16) 0.0085(17) -0.0102(19) C11 0.052(2) 0.0466(18) 0.0501(18) 0.0016(14) 0.0165(15) -0.0031(15) C12 0.058(3) 0.0458(17) 0.0461(17) -0.0001(14) 0.0206(16) 0.0006(15) C13 0.032(3) 0.0517(19) 0.057(2) -0.0060(14) 0.0121(17) -0.0034(14) C14 0.030(3) 0.0555(19) 0.0547(19) -0.0073(14) 0.0162(16) -0.0053(14) C15 0.037(3) 0.094(3) 0.051(2) -0.0194(18) 0.0093(17) -0.0068(19) C16 0.035(3) 0.095(3) 0.048(2) -0.0138(18) 0.0148(17) -0.0049(18) C17 0.029(3) 0.064(2) 0.0518(19) -0.0057(15) 0.0126(16) -0.0007(15) C18 0.033(3) 0.093(3) 0.0469(19) -0.0032(17) 0.0086(16) -0.0050(17) C19 0.032(3) 0.093(3) 0.0451(19) -0.0031(16) 0.0128(16) -0.0048(17) C20 0.031(2) 0.0455(16) 0.0445(17) -0.0061(13) 0.0088(14) 0.0018(13) C21 0.030(2) 0.0441(16) 0.0370(15) -0.0085(12) 0.0079(13) -0.0012(13) C22 0.031(3) 0.070(2) 0.0380(16) -0.0012(14) 0.0101(14) 0.0014(15) C23 0.030(3) 0.081(2) 0.0469(18) 0.0063(16) 0.0056(15) 0.0066(17) C24 0.030(3) 0.0576(19) 0.0486(18) -0.0080(14) 0.0132(15) -0.0029(14) C25 0.038(3) 0.059(2) 0.0516(18) 0.0087(15) 0.0155(16) 0.0006(15) C26 0.038(3) 0.0453(17) 0.0477(17) 0.0030(13) 0.0086(14) 0.0023(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O4 2.060(2) 1_455 ? Mn O5 2.153(2) . ? Mn O1 2.194(3) . ? Mn N2 2.283(3) . ? Mn N1 2.293(3) . ? Mn O2 2.322(3) . ? Mn C13 2.617(4) . ? N1 C1 1.320(4) . ? N1 C12 1.351(4) . ? N2 C10 1.323(4) . ? N2 C11 1.354(4) . ? O1 C13 1.254(4) . ? O2 C13 1.265(4) . ? O3 C20 1.241(4) . ? O4 C20 1.276(4) . ? O4 Mn 2.060(2) 1_655 ? O5 H5B 0.833(18) . ? O5 H5C 0.843(19) . ? C1 C2 1.400(6) . ? C1 H1A 0.9300 . ? C2 C3 1.350(6) . ? C2 H2A 0.9300 . ? C3 C4 1.397(6) . ? C3 H3A 0.9300 . ? C4 C12 1.404(5) . ? C4 C5 1.423(6) . ? C5 C6 1.342(7) . ? C5 H5A 0.9300 . ? C6 C7 1.422(6) . ? C6 H6A 0.9300 . ? C7 C8 1.400(6) . ? C7 C11 1.404(5) . ? C8 C9 1.356(6) . ? C8 H8A 0.9300 . ? C9 C10 1.393(5) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.444(5) . ? C13 C14 1.475(6) . ? C14 C15 1.380(5) . ? C14 C19 1.393(5) . ? C15 C16 1.385(6) . ? C15 H15A 0.9300 . ? C16 C17 1.390(5) . ? C16 H16A 0.9300 . ? C17 C18 1.395(5) . ? C17 C24 1.470(5) . ? C18 C19 1.373(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.494(5) . ? C21 C22 1.385(5) . ? C21 C26 1.396(4) . ? C22 C23 1.373(5) . ? C22 H22A 0.9300 . ? C23 C24 1.391(5) . ? C23 H23A 0.9300 . ? C24 C25 1.396(5) . ? C25 C26 1.380(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? 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 O4 Mn O5 86.64(10) 1_455 . ? O4 Mn O1 149.67(10) 1_455 . ? O5 Mn O1 89.91(10) . . ? O4 Mn N2 94.45(10) 1_455 . ? O5 Mn N2 162.51(10) . . ? O1 Mn N2 97.66(10) . . ? O4 Mn N1 120.35(11) 1_455 . ? O5 Mn N1 91.76(9) . . ? O1 Mn N1 89.85(10) . . ? N2 Mn N1 72.61(9) . . ? O4 Mn O2 95.59(9) 1_455 . ? O5 Mn O2 109.46(10) . . ? O1 Mn O2 57.39(9) . . ? N2 Mn O2 87.84(10) . . ? N1 Mn O2 139.59(10) . . ? O4 Mn C13 123.62(10) 1_455 . ? O5 Mn C13 101.55(10) . . ? O1 Mn C13 28.51(10) . . ? N2 Mn C13 92.39(10) . . ? N1 Mn C13 115.09(11) . . ? O2 Mn C13 28.90(10) . . ? C1 N1 C12 118.3(3) . . ? C1 N1 Mn 126.1(2) . . ? C12 N1 Mn 115.0(2) . . ? C10 N2 C11 118.0(3) . . ? C10 N2 Mn 126.1(2) . . ? C11 N2 Mn 115.7(2) . . ? C13 O1 Mn 94.8(2) . . ? C13 O2 Mn 88.6(2) . . ? C20 O4 Mn 142.9(2) . 1_655 ? Mn O5 H5B 121(2) . . ? Mn O5 H5C 119(3) . . ? H5B O5 H5C 108(4) . . ? N1 C1 C2 122.7(4) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C12 117.2(4) . . ? C3 C4 C5 123.9(4) . . ? C12 C4 C5 118.9(4) . . ? C6 C5 C4 122.0(4) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C7 120.9(4) . . ? C5 C6 H6A 119.6 . . ? C7 C6 H6A 119.6 . . ? C8 C7 C11 117.3(4) . . ? C8 C7 C6 123.5(4) . . ? C11 C7 C6 119.2(3) . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C8 C9 C10 119.3(4) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? N2 C10 C9 123.0(4) . . ? N2 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? N2 C11 C7 122.7(3) . . ? N2 C11 C12 117.6(3) . . ? C7 C11 C12 119.7(3) . . ? N1 C12 C4 122.5(3) . . ? N1 C12 C11 118.2(3) . . ? C4 C12 C11 119.3(3) . . ? O1 C13 O2 119.1(3) . . ? O1 C13 C14 120.1(3) . . ? O2 C13 C14 120.8(3) . . ? O1 C13 Mn 56.67(19) . . ? O2 C13 Mn 62.52(19) . . ? C14 C13 Mn 175.3(2) . . ? C15 C14 C19 117.9(4) . . ? C15 C14 C13 123.1(3) . . ? C19 C14 C13 119.0(3) . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C15 C16 C17 120.9(3) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C16 C17 C18 117.2(4) . . ? C16 C17 C24 121.5(3) . . ? C18 C17 C24 121.3(3) . . ? C19 C18 C17 121.8(4) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C14 120.7(3) . . ? C18 C19 H19A 119.7 . . ? C14 C19 H19A 119.7 . . ? O3 C20 O4 124.4(3) . . ? O3 C20 C21 119.4(3) . . ? O4 C20 C21 116.2(3) . . ? C22 C21 C26 118.3(3) . . ? C22 C21 C20 120.9(3) . . ? C26 C21 C20 120.7(3) . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 121.7(3) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C23 C24 C25 117.2(3) . . ? C23 C24 C17 122.7(3) . . ? C25 C24 C17 120.1(3) . . ? C26 C25 C24 121.5(3) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C25 C26 C21 120.4(3) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 0.325 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.078 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA #============END data_2 _database_code_depnum_ccdc_archive 'CCDC 281961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 Mn N2 O4' _chemical_formula_weight 475.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.467(3) _cell_length_b 11.7435(10) _cell_length_c 7.3557(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.913(2) _cell_angle_gamma 90.00 _cell_volume 2219.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1041 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25.07 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max .52 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .813 _exptl_absorpt_correction_T_max .881 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3161 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.07 _reflns_number_total 1807 _reflns_number_gt 1171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+15.7889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1807 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1293 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Mn Mn 0.0000 0.38350(11) 1.2500 0.0412(4) Uani 1 2 d S . . O1 O -0.06359(15) 0.4817(4) 1.1144(7) 0.0570(13) Uani 1 1 d . . . O2 O -0.04001(14) 0.6352(3) 0.9771(6) 0.0514(12) Uani 1 1 d . . . N N -0.04666(17) 0.2231(4) 1.1237(7) 0.0420(12) Uani 1 1 d . . . C1 C -0.0928(2) 0.2245(6) 1.0066(10) 0.0563(18) Uani 1 1 d . . . H1A H -0.1079 0.2946 0.9672 0.068 Uiso 1 1 calc R . . C2 C -0.1200(3) 0.1263(7) 0.9392(11) 0.066(2) Uani 1 1 d . . . H2A H -0.1522 0.1303 0.8541 0.079 Uiso 1 1 calc R . . C3 C -0.0985(3) 0.0240(7) 1.0004(11) 0.063(2) Uani 1 1 d . . . H3A H -0.1169 -0.0424 0.9603 0.076 Uiso 1 1 calc R . . C4 C -0.0488(3) 0.0169(5) 1.1231(10) 0.0491(17) Uani 1 1 d . . . C5 C -0.0254(2) 0.1204(5) 1.1833(8) 0.0376(13) Uani 1 1 d . . . C6 C -0.0236(3) -0.0871(5) 1.1887(9) 0.060(2) Uani 1 1 d . . . H6A H -0.0397 -0.1559 1.1470 0.072 Uiso 1 1 calc R . . C7 C -0.07154(19) 0.5774(5) 1.0401(9) 0.0412(15) Uani 1 1 d . . . C8 C -0.12563(19) 0.6263(5) 1.0254(8) 0.0349(13) Uani 1 1 d . . . C9 C -0.1581(2) 0.5835(6) 1.1238(11) 0.069(2) Uani 1 1 d . . . H9A H -0.1476 0.5210 1.2013 0.082 Uiso 1 1 calc R . . C10 C -0.2066(2) 0.6299(6) 1.1128(12) 0.075(2) Uani 1 1 d . . . H10A H -0.2283 0.5969 1.1805 0.090 Uiso 1 1 calc R . . C11 C -0.22355(18) 0.7236(5) 1.0040(8) 0.0380(14) Uani 1 1 d . . . C12 C -0.1907(2) 0.7658(5) 0.9032(10) 0.0533(18) Uani 1 1 d . . . H12A H -0.2011 0.8284 0.8260 0.064 Uiso 1 1 calc R . . C13 C -0.1420(2) 0.7180(6) 0.9123(10) 0.0543(18) Uani 1 1 d . . . H13A H -0.1205 0.7486 0.8414 0.065 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 Mn 0.0255(6) 0.0334(7) 0.0689(10) 0.000 0.0195(6) 0.000 O1 0.039(2) 0.040(3) 0.095(4) 0.017(2) 0.022(2) 0.0119(19) O2 0.031(2) 0.046(3) 0.082(3) 0.001(2) 0.023(2) -0.0001(18) N 0.038(3) 0.041(3) 0.050(3) -0.004(3) 0.017(2) -0.003(2) C1 0.047(4) 0.050(4) 0.072(5) -0.002(4) 0.013(4) 0.003(3) C2 0.046(4) 0.082(6) 0.071(5) -0.011(5) 0.017(3) -0.012(4) C3 0.072(5) 0.056(5) 0.068(5) -0.012(4) 0.030(4) -0.025(4) C4 0.062(4) 0.041(4) 0.058(4) -0.004(3) 0.040(4) -0.013(3) C5 0.048(3) 0.033(3) 0.042(3) -0.002(3) 0.031(3) -0.004(3) C6 0.096(6) 0.038(4) 0.063(5) -0.004(3) 0.051(4) -0.015(3) C7 0.017(3) 0.047(4) 0.062(4) -0.005(3) 0.014(3) 0.002(2) C8 0.028(3) 0.031(3) 0.046(3) -0.005(3) 0.011(2) 0.004(2) C9 0.036(3) 0.086(6) 0.091(6) 0.044(5) 0.031(4) 0.025(3) C10 0.047(4) 0.089(6) 0.106(6) 0.050(5) 0.049(4) 0.030(4) C11 0.026(3) 0.040(3) 0.051(4) 0.012(3) 0.015(3) 0.011(2) C12 0.033(3) 0.057(4) 0.081(5) 0.030(4) 0.035(3) 0.018(3) C13 0.032(3) 0.059(4) 0.079(5) 0.013(4) 0.029(3) 0.005(3) _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 Mn O1 2.086(4) 2_557 ? Mn O1 2.086(4) . ? Mn O2 2.193(4) 5_567 ? Mn O2 2.193(4) 6_566 ? Mn N 2.320(5) . ? Mn N 2.320(5) 2_557 ? O1 C7 1.245(7) . ? O2 C7 1.248(7) . ? O2 Mn 2.193(4) 5_567 ? N C1 1.315(7) . ? N C5 1.358(7) . ? C1 C2 1.387(9) . ? C1 H1A 0.9300 . ? C2 C3 1.358(10) . ? C2 H2A 0.9300 . ? C3 C4 1.407(10) . ? C3 H3A 0.9300 . ? C4 C5 1.387(8) . ? C4 C6 1.419(9) . ? C5 C5 1.463(11) 2_557 ? C6 C6 1.355(14) 2_557 ? C6 H6A 0.9300 . ? C7 C8 1.522(7) . ? C8 C9 1.347(8) . ? C8 C13 1.367(8) . ? C9 C10 1.378(8) . ? C9 H9A 0.9300 . ? C10 C11 1.371(8) . ? C10 H10A 0.9300 . ? C11 C12 1.365(8) . ? C11 C11 1.520(10) 7_467 ? C12 C13 1.392(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn O1 112.9(2) 2_557 . ? O1 Mn O2 86.43(17) 2_557 5_567 ? O1 Mn O2 99.96(17) . 5_567 ? O1 Mn O2 99.96(17) 2_557 6_566 ? O1 Mn O2 86.43(17) . 6_566 ? O2 Mn O2 168.5(2) 5_567 6_566 ? O1 Mn N 158.57(17) 2_557 . ? O1 Mn N 88.09(17) . . ? O2 Mn N 85.52(16) 5_567 . ? O2 Mn N 85.16(16) 6_566 . ? O1 Mn N 88.09(17) 2_557 2_557 ? O1 Mn N 158.57(17) . 2_557 ? O2 Mn N 85.16(16) 5_567 2_557 ? O2 Mn N 85.52(16) 6_566 2_557 ? N Mn N 71.5(2) . 2_557 ? C7 O1 Mn 137.8(4) . . ? C7 O2 Mn 135.8(4) . 5_567 ? C1 N C5 118.0(5) . . ? C1 N Mn 125.0(4) . . ? C5 N Mn 116.9(4) . . ? N C1 C2 123.0(7) . . ? N C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 118.5(6) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 121.2(6) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 115.4(6) . . ? C5 C4 C6 120.5(6) . . ? C3 C4 C6 124.0(6) . . ? N C5 C4 123.9(5) . . ? N C5 C5 117.3(3) . 2_557 ? C4 C5 C5 118.8(4) . 2_557 ? C6 C6 C4 120.6(4) 2_557 . ? C6 C6 H6A 119.7 2_557 . ? C4 C6 H6A 119.7 . . ? O2 C7 O1 126.6(5) . . ? O2 C7 C8 118.0(5) . . ? O1 C7 C8 115.4(5) . . ? C9 C8 C13 118.1(5) . . ? C9 C8 C7 122.2(5) . . ? C13 C8 C7 119.7(5) . . ? C8 C9 C10 121.8(6) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C9 C10 C11 121.4(6) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C12 C11 C10 116.5(5) . . ? C12 C11 C11 122.2(6) . 7_467 ? C10 C11 C11 121.3(6) . 7_467 ? C11 C12 C13 122.1(6) . . ? C11 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? C8 C13 C12 120.0(6) . . ? C8 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? 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 O1 Mn O1 C7 28.3(6) 2_557 . . . ? O2 Mn O1 C7 -62.0(7) 5_567 . . . ? O2 Mn O1 C7 127.6(7) 6_566 . . . ? N Mn O1 C7 -147.1(7) . . . . ? N Mn O1 C7 -164.3(6) 2_557 . . . ? O1 Mn N C1 -164.5(5) 2_557 . . . ? O1 Mn N C1 3.8(5) . . . . ? O2 Mn N C1 -96.3(5) 5_567 . . . ? O2 Mn N C1 90.4(5) 6_566 . . . ? N Mn N C1 177.3(6) 2_557 . . . ? O1 Mn N C5 18.8(8) 2_557 . . . ? O1 Mn N C5 -172.8(4) . . . . ? O2 Mn N C5 87.0(4) 5_567 . . . ? O2 Mn N C5 -86.2(4) 6_566 . . . ? N Mn N C5 0.6(3) 2_557 . . . ? C5 N C1 C2 -1.3(10) . . . . ? Mn N C1 C2 -177.9(5) . . . . ? N C1 C2 C3 1.6(11) . . . . ? C1 C2 C3 C4 -2.6(11) . . . . ? C2 C3 C4 C5 3.3(10) . . . . ? C2 C3 C4 C6 -178.4(6) . . . . ? C1 N C5 C4 2.2(8) . . . . ? Mn N C5 C4 179.1(4) . . . . ? C1 N C5 C5 -178.7(6) . . . 2_557 ? Mn N C5 C5 -1.8(8) . . . 2_557 ? C3 C4 C5 N -3.1(9) . . . . ? C6 C4 C5 N 178.5(6) . . . . ? C3 C4 C5 C5 177.8(6) . . . 2_557 ? C6 C4 C5 C5 -0.6(10) . . . 2_557 ? C5 C4 C6 C6 0.2(12) . . . 2_557 ? C3 C4 C6 C6 -178.0(8) . . . 2_557 ? Mn O2 C7 O1 64.1(9) 5_567 . . . ? Mn O2 C7 C8 -115.5(5) 5_567 . . . ? Mn O1 C7 O2 22.6(11) . . . . ? Mn O1 C7 C8 -157.9(4) . . . . ? O2 C7 C8 C9 -165.1(6) . . . . ? O1 C7 C8 C9 15.3(9) . . . . ? O2 C7 C8 C13 13.5(9) . . . . ? O1 C7 C8 C13 -166.1(6) . . . . ? C13 C8 C9 C10 0.0(11) . . . . ? C7 C8 C9 C10 178.6(7) . . . . ? C8 C9 C10 C11 -1.5(13) . . . . ? C9 C10 C11 C12 2.1(12) . . . . ? C9 C10 C11 C11 -178.4(8) . . . 7_467 ? C10 C11 C12 C13 -1.2(11) . . . . ? C11 C11 C12 C13 179.3(7) 7_467 . . . ? C9 C8 C13 C12 0.9(10) . . . . ? C7 C8 C13 C12 -177.7(6) . . . . ? C11 C12 C13 C8 -0.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.650 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.082 #===========END