# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xiao-Ming Chen' _publ_contact_author_email CXM@MAIL.SYSU.EDU.CN _publ_section_title ; Spin Canting and/or Metamagnetic Behaviours of Four Isostructural Grid-Type Coordination Networks ; loop_ _publ_author_name 'Xiao-Ming Chen.' 'Xiao-Ning Cheng.' 'Jun-Hou Huang.' 'Wei Xue.' # Attachment 'B901524H.cif' data_1.Co _database_code_depnum_ccdc_archive 'CCDC 707684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 Co N O5' _chemical_formula_weight 306.13 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.5177(19) _cell_length_b 7.1669(8) _cell_length_c 18.958(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2244.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle-like _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7474 _exptl_absorpt_correction_T_max 0.9267 _exptl_absorpt_process_details SADABS _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 _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 6639 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2180 _reflns_number_gt 1908 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0559P)^2^+0.2627P] 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 2180 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Co1 Co 0.631415(19) 0.13362(4) 0.708095(15) 0.02750(15) Uani 1 1 d . . . N1 N 0.65136(12) 0.1865(3) 0.59801(10) 0.0291(4) Uani 1 1 d . . . O1 O 0.59136(11) -0.1145(2) 0.65461(8) 0.0349(4) Uani 1 1 d . . . O2 O 0.48393(11) -0.2420(3) 0.80805(9) 0.0381(4) Uani 1 1 d . . . O3 O 0.58270(11) -0.0408(3) 0.78654(8) 0.0356(4) Uani 1 1 d . . . O4 O 0.74362(11) -0.0009(3) 0.71392(8) 0.0417(5) Uani 1 1 d . . . O5 O 0.83720(12) -0.1556(3) 0.77423(10) 0.0411(5) Uani 1 1 d . . . C1 C 0.68041(16) 0.3408(3) 0.57015(13) 0.0354(6) Uani 1 1 d . . . H1A H 0.6994 0.4337 0.6001 0.043 Uiso 1 1 calc R . . C2 C 0.68395(16) 0.3711(4) 0.49690(13) 0.0391(6) Uani 1 1 d . . . H2A H 0.7043 0.4829 0.4794 0.047 Uiso 1 1 calc R . . C3 C 0.65774(17) 0.2373(3) 0.45194(12) 0.0381(6) Uani 1 1 d . . . H3A H 0.6599 0.2571 0.4035 0.046 Uiso 1 1 calc R . . C4 C 0.62731(14) 0.0683(4) 0.47869(12) 0.0316(5) Uani 1 1 d . . . C5 C 0.59855(17) -0.0789(4) 0.43650(13) 0.0405(6) Uani 1 1 d . . . H5A H 0.6006 -0.0689 0.3876 0.049 Uiso 1 1 calc R . . C6 C 0.56779(17) -0.2358(4) 0.46678(13) 0.0405(6) Uani 1 1 d . . . H6A H 0.5487 -0.3317 0.4382 0.049 Uiso 1 1 calc R . . C7 C 0.56440(16) -0.2556(3) 0.54078(12) 0.0362(6) Uani 1 1 d . . . H7A H 0.5435 -0.3638 0.5608 0.043 Uiso 1 1 calc R . . C8 C 0.59206(14) -0.1149(3) 0.58261(12) 0.0295(5) Uani 1 1 d . . . C9 C 0.62472(13) 0.0495(3) 0.55310(12) 0.0270(5) Uani 1 1 d . . . C10 C 0.53848(17) -0.2358(3) 0.69224(13) 0.0354(6) Uani 1 1 d . . . H10A H 0.5588 -0.3627 0.6907 0.042 Uiso 1 1 calc R . . H10B H 0.4849 -0.2338 0.6713 0.042 Uiso 1 1 calc R . . C11 C 0.53471(14) -0.1668(3) 0.76836(12) 0.0291(5) Uani 1 1 d . . . C12 C 0.78068(16) -0.0412(4) 0.76781(14) 0.0415(6) Uani 1 1 d . . . H12A H 0.7649 0.0207 0.8087 0.050 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 Co1 0.0296(2) 0.0314(2) 0.0214(2) -0.00209(12) 0.00146(12) -0.00083(13) N1 0.0270(10) 0.0335(10) 0.0268(10) -0.0007(8) 0.0005(8) -0.0006(8) O1 0.0456(10) 0.0357(9) 0.0234(8) -0.0006(7) 0.0050(7) -0.0113(8) O2 0.0363(10) 0.0513(11) 0.0266(8) 0.0060(8) 0.0021(7) -0.0090(8) O3 0.0395(10) 0.0404(10) 0.0268(8) 0.0001(7) 0.0020(7) -0.0063(8) O4 0.0376(10) 0.0564(12) 0.0311(9) -0.0013(8) -0.0016(7) 0.0130(9) O5 0.0413(10) 0.0457(11) 0.0363(10) -0.0129(8) -0.0075(9) 0.0170(9) C1 0.0354(14) 0.0364(13) 0.0345(13) 0.0010(11) 0.0001(11) -0.0054(11) C2 0.0381(15) 0.0420(15) 0.0373(14) 0.0094(11) 0.0046(11) -0.0062(12) C3 0.0378(15) 0.0507(17) 0.0260(12) 0.0093(12) 0.0031(10) 0.0007(12) C4 0.0287(13) 0.0416(14) 0.0244(12) 0.0004(10) 0.0000(9) 0.0038(10) C5 0.0453(15) 0.0534(16) 0.0228(12) -0.0034(11) -0.0027(11) 0.0014(13) C6 0.0485(17) 0.0418(15) 0.0311(13) -0.0119(12) -0.0062(11) -0.0010(12) C7 0.0408(15) 0.0332(13) 0.0345(13) -0.0034(11) 0.0003(11) -0.0024(11) C8 0.0275(12) 0.0335(13) 0.0275(12) 0.0002(10) 0.0027(9) 0.0035(9) C9 0.0244(12) 0.0320(12) 0.0247(11) -0.0027(9) 0.0028(9) 0.0044(9) C10 0.0432(15) 0.0334(13) 0.0296(12) 0.0031(11) 0.0067(11) -0.0081(11) C11 0.0321(13) 0.0299(12) 0.0254(11) 0.0058(10) -0.0018(10) 0.0030(10) C12 0.0440(15) 0.0458(15) 0.0346(13) -0.0124(12) -0.0011(12) 0.0133(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 Co1 O5 2.0303(17) 8_765 ? Co1 O4 2.0920(18) . ? Co1 O3 2.1028(16) . ? Co1 O2 2.1255(18) 3_656 ? Co1 N1 2.1464(19) . ? Co1 O1 2.1515(16) . ? N1 C1 1.316(3) . ? N1 C9 1.372(3) . ? O1 C8 1.365(3) . ? O1 C10 1.424(3) . ? O2 C11 1.249(3) . ? O2 Co1 2.1255(18) 3_646 ? O3 C11 1.250(3) . ? O4 C12 1.226(3) . ? O5 C12 1.249(3) . ? O5 Co1 2.0303(17) 8_755 ? C1 C2 1.407(3) . ? C1 H1A 0.9300 . ? C2 C3 1.354(4) . ? C2 H2A 0.9300 . ? C3 C4 1.406(3) . ? C3 H3A 0.9300 . ? C4 C5 1.406(4) . ? C4 C9 1.418(3) . ? C5 C6 1.361(4) . ? C5 H5A 0.9300 . ? C6 C7 1.411(3) . ? C6 H6A 0.9300 . ? C7 C8 1.362(3) . ? C7 H7A 0.9300 . ? C8 C9 1.412(3) . ? C10 C11 1.527(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 H12A 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 O5 Co1 O4 94.82(8) 8_765 . ? O5 Co1 O3 95.92(7) 8_765 . ? O4 Co1 O3 91.59(7) . . ? O5 Co1 O2 90.34(7) 8_765 3_656 ? O4 Co1 O2 174.22(6) . 3_656 ? O3 Co1 O2 90.47(7) . 3_656 ? O5 Co1 N1 115.47(8) 8_765 . ? O4 Co1 N1 89.81(7) . . ? O3 Co1 N1 148.35(7) . . ? O2 Co1 N1 85.61(7) 3_656 . ? O5 Co1 O1 169.90(7) 8_765 . ? O4 Co1 O1 85.21(7) . . ? O3 Co1 O1 73.99(6) . . ? O2 Co1 O1 90.17(7) 3_656 . ? N1 Co1 O1 74.62(7) . . ? C1 N1 C9 118.0(2) . . ? C1 N1 Co1 126.46(17) . . ? C9 N1 Co1 115.34(15) . . ? C8 O1 C10 120.33(18) . . ? C8 O1 Co1 118.06(13) . . ? C10 O1 Co1 117.20(14) . . ? C11 O2 Co1 134.11(16) . 3_646 ? C11 O3 Co1 118.49(14) . . ? C12 O4 Co1 126.52(16) . . ? C12 O5 Co1 128.27(17) . 8_755 ? N1 C1 C2 122.7(2) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.9(2) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 124.2(2) . . ? C3 C4 C9 116.8(2) . . ? C5 C4 C9 119.0(2) . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 121.1(2) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C8 C7 C6 119.4(2) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C7 C8 O1 125.5(2) . . ? C7 C8 C9 121.0(2) . . ? O1 C8 C9 113.4(2) . . ? N1 C9 C8 118.3(2) . . ? N1 C9 C4 122.7(2) . . ? C8 C9 C4 119.0(2) . . ? O1 C10 C11 107.53(19) . . ? O1 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? O1 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O2 C11 O3 124.8(2) . . ? O2 C11 C10 117.2(2) . . ? O3 C11 C10 117.9(2) . . ? O4 C12 O5 127.6(2) . . ? O4 C12 H12A 116.2 . . ? O5 C12 H12A 116.2 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.391 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.072 #========================================================END data_2.Co _database_code_depnum_ccdc_archive 'CCDC 707685' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H11 Co N O5' _chemical_formula_weight 320.16 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 15.9022(15) _cell_length_b 9.9651(9) _cell_length_c 7.5081(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1189.79(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 1.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7586 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details SADABS _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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5845 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2291 _reflns_number_gt 2172 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0298P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(16) _refine_ls_number_reflns 2291 _refine_ls_number_parameters 182 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Co1 Co -0.36672(2) -0.07379(3) 0.21790(6) 0.02293(11) Uani 1 1 d . . . O1 O -0.40261(13) -0.17813(17) -0.0259(3) 0.0279(5) Uani 1 1 d . . . O2 O -0.50803(12) 0.11473(18) -0.1701(3) 0.0330(5) Uani 1 1 d . . . O3 O -0.41929(14) 0.07033(17) 0.0515(3) 0.0287(5) Uani 1 1 d . . . O4 O -0.15117(14) 0.0436(2) -0.0694(3) 0.0340(5) Uani 1 1 d . . . O5 O -0.24846(14) -0.05532(17) 0.0964(3) 0.0338(5) Uani 1 1 d . . . N1 N -0.34750(14) -0.2819(2) 0.2718(3) 0.0243(6) Uani 1 1 d . . . C1 C -0.32019(19) -0.3321(3) 0.4221(4) 0.0310(7) Uani 1 1 d . . . H1A H -0.3006 -0.2736 0.5092 0.037 Uiso 1 1 calc R . . C2 C -0.3191(2) -0.4712(3) 0.4580(5) 0.0350(7) Uani 1 1 d . . . H2A H -0.2999 -0.5027 0.5673 0.042 Uiso 1 1 calc R . . C3 C -0.3463(2) -0.5585(3) 0.3320(5) 0.0330(7) Uani 1 1 d . . . H3A H -0.3464 -0.6502 0.3551 0.040 Uiso 1 1 calc R . . C4 C -0.37441(15) -0.5101(3) 0.1664(4) 0.0267(8) Uani 1 1 d . . . C5 C -0.4039(2) -0.5920(3) 0.0251(5) 0.0339(8) Uani 1 1 d . . . H5A H -0.4039 -0.6849 0.0378 0.041 Uiso 1 1 calc R . . C6 C -0.4320(2) -0.5364(3) -0.1275(5) 0.0363(8) Uani 1 1 d . . . H6A H -0.4511 -0.5918 -0.2186 0.044 Uiso 1 1 calc R . . C7 C -0.43311(19) -0.3954(3) -0.1519(5) 0.0319(7) Uani 1 1 d . . . H7A H -0.4530 -0.3585 -0.2576 0.038 Uiso 1 1 calc R . . C8 C -0.40471(18) -0.3148(3) -0.0189(4) 0.0248(6) Uani 1 1 d . . . C9 C -0.37440(16) -0.3682(3) 0.1422(4) 0.0235(6) Uani 1 1 d . . . C10 C -0.45693(18) -0.1078(3) -0.1449(4) 0.0286(7) Uani 1 1 d . . . H10A H -0.5124 -0.1483 -0.1445 0.034 Uiso 1 1 calc R . . H10B H -0.4348 -0.1117 -0.2652 0.034 Uiso 1 1 calc R . . C11 C -0.46218(17) 0.0379(3) -0.0822(4) 0.0237(6) Uani 1 1 d . . . C12 C -0.20313(17) 0.0417(3) 0.0584(4) 0.0248(6) Uani 1 1 d . . . C13 C -0.2071(2) 0.1687(3) 0.1672(4) 0.0409(8) Uani 1 1 d . . . H13A H -0.2134 0.1463 0.2909 0.061 Uiso 1 1 calc R . . H13B H -0.2542 0.2217 0.1293 0.061 Uiso 1 1 calc R . . H13C H -0.1562 0.2190 0.1508 0.061 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 Co1 0.02800(19) 0.01773(18) 0.02305(19) -0.0022(2) -0.0011(2) 0.00178(13) O1 0.0375(12) 0.0144(9) 0.0320(11) -0.0012(8) -0.0093(10) 0.0002(8) O2 0.0341(11) 0.0195(9) 0.0453(14) 0.0031(10) -0.0100(11) 0.0025(9) O3 0.0371(12) 0.0212(10) 0.0279(13) -0.0010(8) -0.0061(10) 0.0020(8) O4 0.0347(12) 0.0389(12) 0.0283(12) -0.0108(10) 0.0065(10) -0.0028(10) O5 0.0305(11) 0.0266(10) 0.0443(13) -0.0070(11) 0.0086(10) -0.0024(9) N1 0.0221(11) 0.0222(13) 0.0285(15) -0.0002(10) -0.0002(9) 0.0027(9) C1 0.0329(17) 0.0295(15) 0.0304(16) 0.0002(14) -0.0041(14) 0.0013(13) C2 0.0369(18) 0.0360(16) 0.0320(19) 0.0065(15) -0.0046(15) 0.0061(14) C3 0.0340(16) 0.0207(15) 0.044(2) 0.0084(14) 0.0020(16) 0.0060(13) C4 0.0242(14) 0.0189(16) 0.037(2) 0.0018(12) 0.0051(12) 0.0032(11) C5 0.0354(18) 0.0196(14) 0.047(2) -0.0037(14) 0.0003(16) 0.0012(13) C6 0.0376(17) 0.0265(16) 0.045(2) -0.0143(15) -0.0045(16) -0.0008(13) C7 0.0366(16) 0.0267(15) 0.0325(17) -0.0055(14) -0.0058(15) 0.0017(13) C8 0.0243(15) 0.0207(14) 0.0293(15) -0.0002(12) 0.0014(12) 0.0022(11) C9 0.0207(14) 0.0195(15) 0.0302(16) -0.0028(12) 0.0026(12) 0.0010(11) C10 0.0324(16) 0.0239(14) 0.0294(17) 0.0020(13) -0.0078(14) 0.0024(12) C11 0.0227(14) 0.0202(13) 0.0281(16) 0.0035(12) 0.0070(13) -0.0002(11) C12 0.0243(15) 0.0292(15) 0.0208(16) -0.0006(12) -0.0027(12) 0.0049(12) C13 0.057(2) 0.0308(16) 0.0349(19) -0.0037(13) 0.0124(15) -0.0061(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 Co1 O4 2.000(2) 3_455 ? Co1 O3 2.0789(19) . ? Co1 O5 2.098(2) . ? Co1 N1 2.135(2) . ? Co1 O1 2.181(2) . ? Co1 O2 2.200(2) 2_455 ? O1 C8 1.363(3) . ? O1 C10 1.427(3) . ? O2 C11 1.246(3) . ? O2 Co1 2.200(2) 2_454 ? O3 C11 1.256(4) . ? O4 C12 1.266(4) . ? O4 Co1 2.000(2) 3_454 ? O5 C12 1.239(3) . ? N1 C1 1.309(4) . ? N1 C9 1.367(4) . ? C1 C2 1.412(4) . ? C1 H1A 0.9300 . ? C2 C3 1.356(5) . ? C2 H2A 0.9300 . ? C3 C4 1.407(5) . ? C3 H3A 0.9300 . ? C4 C5 1.419(5) . ? C4 C9 1.425(4) . ? C5 C6 1.348(5) . ? C5 H5A 0.9300 . ? C6 C7 1.418(4) . ? C6 H6A 0.9300 . ? C7 C8 1.359(4) . ? C7 H7A 0.9300 . ? C8 C9 1.407(4) . ? C10 C11 1.529(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C13 1.508(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 Co1 O3 97.63(9) 3_455 . ? O4 Co1 O5 99.69(9) 3_455 . ? O3 Co1 O5 92.21(9) . . ? O4 Co1 N1 113.37(10) 3_455 . ? O3 Co1 N1 147.40(8) . . ? O5 Co1 N1 92.25(8) . . ? O4 Co1 O1 170.46(8) 3_455 . ? O3 Co1 O1 73.73(7) . . ? O5 Co1 O1 84.93(9) . . ? N1 Co1 O1 74.53(8) . . ? O4 Co1 O2 86.10(9) 3_455 2_455 ? O3 Co1 O2 89.64(9) . 2_455 ? O5 Co1 O2 173.62(8) . 2_455 ? N1 Co1 O2 82.94(8) . 2_455 ? O1 Co1 O2 89.74(8) . 2_455 ? C8 O1 C10 120.0(2) . . ? C8 O1 Co1 116.78(18) . . ? C10 O1 Co1 116.75(15) . . ? C11 O2 Co1 128.18(18) . 2_454 ? C11 O3 Co1 121.40(16) . . ? C12 O4 Co1 133.5(2) . 3_454 ? C12 O5 Co1 133.62(18) . . ? C1 N1 C9 118.5(2) . . ? C1 N1 Co1 125.6(2) . . ? C9 N1 Co1 115.58(19) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 124.6(3) . . ? C3 C4 C9 116.9(3) . . ? C5 C4 C9 118.4(3) . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C7 121.4(3) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C8 C7 C6 119.1(3) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C7 C8 O1 124.8(3) . . ? C7 C8 C9 121.5(3) . . ? O1 C8 C9 113.7(3) . . ? N1 C9 C8 118.7(3) . . ? N1 C9 C4 122.2(3) . . ? C8 C9 C4 119.0(3) . . ? O1 C10 C11 107.8(2) . . ? O1 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? O1 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? O2 C11 O3 125.7(2) . . ? O2 C11 C10 116.9(3) . . ? O3 C11 C10 117.5(2) . . ? O5 C12 O4 124.5(3) . . ? O5 C12 C13 120.4(3) . . ? O4 C12 C13 115.2(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.271 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.058 #========================================================END data_1 _database_code_depnum_ccdc_archive 'CCDC 707686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H11 Mn N O5' _chemical_formula_weight 316.17 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 15.9740(16) _cell_length_b 10.0241(10) _cell_length_c 7.6552(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1225.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8106 _exptl_absorpt_correction_T_max 0.8983 _exptl_absorpt_process_details SADABS _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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4676 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2242 _reflns_number_gt 2122 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0386P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(18) _refine_ls_number_reflns 2242 _refine_ls_number_parameters 182 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 -0.363323(18) -0.43625(3) 0.65716(5) 0.02817(11) Uani 1 1 d . . . O1 O -0.40077(10) -0.32138(15) 0.4099(2) 0.0320(4) Uani 1 1 d . . . O2 O -0.41741(11) -0.57298(15) 0.4730(2) 0.0361(4) Uani 1 1 d . . . O3 O -0.50908(10) -0.60753(16) 0.2590(3) 0.0422(4) Uani 1 1 d . . . O4 O -0.24086(12) -0.45849(16) 0.5406(3) 0.0420(4) Uani 1 1 d . . . N1 N -0.34465(12) -0.21664(19) 0.7025(2) 0.0302(4) Uani 1 1 d . . . C1 C -0.31856(15) -0.1655(2) 0.8522(3) 0.0369(5) Uani 1 1 d . . . H1A H -0.2989 -0.2229 0.9384 0.044 Uiso 1 1 calc R . . C2 C -0.31947(17) -0.0280(3) 0.8861(3) 0.0423(6) Uani 1 1 d . . . H2A H -0.3009 0.0041 0.9932 0.051 Uiso 1 1 calc R . . C3 C -0.34718(17) 0.0575(2) 0.7639(4) 0.0387(6) Uani 1 1 d . . . H3A H -0.3479 0.1486 0.7867 0.046 Uiso 1 1 calc R . . C4 C -0.37512(13) 0.0092(2) 0.6013(4) 0.0309(5) Uani 1 1 d . . . C5 C -0.40514(16) 0.0915(2) 0.4638(4) 0.0398(6) Uani 1 1 d . . . H5A H -0.4060 0.1837 0.4771 0.048 Uiso 1 1 calc R . . C6 C -0.43255(16) 0.0354(2) 0.3131(4) 0.0410(6) Uani 1 1 d . . . H6A H -0.4517 0.0904 0.2238 0.049 Uiso 1 1 calc R . . C7 C -0.43284(15) -0.1038(2) 0.2879(4) 0.0374(5) Uani 1 1 d . . . H7A H -0.4525 -0.1400 0.1838 0.045 Uiso 1 1 calc R . . C8 C -0.40402(13) -0.1850(2) 0.4180(3) 0.0291(5) Uani 1 1 d . . . C9 C -0.37322(12) -0.1316(2) 0.5766(3) 0.0271(5) Uani 1 1 d . . . C10 C -0.45416(14) -0.3897(2) 0.2891(3) 0.0336(5) Uani 1 1 d . . . H10A H -0.4310 -0.3844 0.1721 0.040 Uiso 1 1 calc R . . H10B H -0.5092 -0.3488 0.2881 0.040 Uiso 1 1 calc R . . C11 C -0.46070(14) -0.5347(2) 0.3462(3) 0.0298(5) Uani 1 1 d . . . C12 C -0.19809(14) -0.5578(2) 0.5007(3) 0.0312(5) Uani 1 1 d . . . C13 C -0.20237(19) -0.6825(2) 0.6090(4) 0.0468(7) Uani 1 1 d . . . H13A H -0.2068 -0.6591 0.7302 0.070 Uiso 1 1 calc R . . H13B H -0.1526 -0.7344 0.5908 0.070 Uiso 1 1 calc R . . H13C H -0.2505 -0.7338 0.5751 0.070 Uiso 1 1 calc R . . O5 O -0.15055(12) -0.56312(19) 0.3697(3) 0.0437(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.03332(17) 0.02081(17) 0.03038(18) 0.00218(18) -0.00114(16) -0.00090(11) O1 0.0407(9) 0.0200(8) 0.0354(8) 0.0017(7) -0.0093(7) -0.0019(7) O2 0.0473(10) 0.0219(8) 0.0391(9) 0.0003(7) -0.0072(8) -0.0014(7) O3 0.0410(9) 0.0269(9) 0.0585(11) -0.0055(9) -0.0149(9) -0.0017(7) O4 0.0400(9) 0.0326(9) 0.0533(11) 0.0077(9) 0.0070(8) 0.0024(8) N1 0.0298(8) 0.0257(10) 0.0351(12) 0.0032(9) -0.0008(7) -0.0026(7) C1 0.0399(13) 0.0328(13) 0.0379(13) -0.0008(11) -0.0068(11) -0.0013(10) C2 0.0464(15) 0.0372(14) 0.0432(15) -0.0083(12) -0.0081(12) -0.0051(11) C3 0.0387(12) 0.0246(13) 0.0528(18) -0.0082(12) 0.0024(13) -0.0047(10) C4 0.0305(11) 0.0201(12) 0.0422(14) -0.0005(10) 0.0038(9) -0.0018(9) C5 0.0410(13) 0.0195(11) 0.0589(17) 0.0071(12) -0.0006(12) -0.0001(10) C6 0.0445(13) 0.0298(12) 0.0489(16) 0.0143(12) -0.0055(12) -0.0004(11) C7 0.0402(12) 0.0326(12) 0.0394(14) 0.0051(12) -0.0068(11) -0.0026(10) C8 0.0282(11) 0.0219(12) 0.0371(12) 0.0013(10) 0.0000(9) -0.0020(9) C9 0.0253(10) 0.0195(12) 0.0363(13) 0.0039(10) 0.0033(9) -0.0017(8) C10 0.0372(12) 0.0264(12) 0.0372(13) -0.0038(11) -0.0082(11) -0.0039(9) C11 0.0304(11) 0.0239(11) 0.0353(12) -0.0037(10) 0.0028(10) 0.0009(9) C12 0.0296(11) 0.0328(13) 0.0312(13) 0.0028(10) -0.0036(10) -0.0050(9) C13 0.0627(16) 0.0356(15) 0.0420(14) 0.0076(12) 0.0113(12) 0.0055(12) O5 0.0447(10) 0.0511(13) 0.0352(11) 0.0121(8) 0.0089(8) 0.0067(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 Mn1 O5 2.0767(19) 3_455 ? Mn1 O2 2.1477(17) . ? Mn1 O4 2.1615(19) . ? Mn1 O3 2.2258(16) 2_445 ? Mn1 N1 2.2485(19) . ? Mn1 O1 2.2951(16) . ? O1 C8 1.369(3) . ? O1 C10 1.432(3) . ? O2 C11 1.252(3) . ? O3 C11 1.256(3) . ? O3 Mn1 2.2258(16) 2_444 ? O4 C12 1.245(3) . ? N1 C1 1.323(3) . ? N1 C9 1.365(3) . ? C1 C2 1.403(3) . ? C1 H1A 0.9300 . ? C2 C3 1.343(4) . ? C2 H2A 0.9300 . ? C3 C4 1.409(4) . ? C3 H3A 0.9300 . ? C4 C5 1.421(4) . ? C4 C9 1.424(3) . ? C5 C6 1.356(4) . ? C5 H5A 0.9300 . ? C6 C7 1.409(3) . ? C6 H6A 0.9300 . ? C7 C8 1.366(3) . ? C7 H7A 0.9300 . ? C8 C9 1.415(3) . ? C10 C11 1.521(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 O5 1.259(3) . ? C12 C13 1.501(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O5 Mn1 2.0767(19) 3_454 ? 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 O5 Mn1 O2 99.58(7) 3_455 . ? O5 Mn1 O4 99.41(7) 3_455 . ? O2 Mn1 O4 91.56(7) . . ? O5 Mn1 O3 86.80(7) 3_455 2_445 ? O2 Mn1 O3 89.27(7) . 2_445 ? O4 Mn1 O3 173.49(7) . 2_445 ? O5 Mn1 N1 117.68(8) 3_455 . ? O2 Mn1 N1 141.21(7) . . ? O4 Mn1 N1 92.56(6) . . ? O3 Mn1 N1 82.78(6) 2_445 . ? O5 Mn1 O1 168.86(7) 3_455 . ? O2 Mn1 O1 70.97(6) . . ? O4 Mn1 O1 86.97(7) . . ? O3 Mn1 O1 87.20(7) 2_445 . ? N1 Mn1 O1 70.77(6) . . ? C8 O1 C10 118.95(17) . . ? C8 O1 Mn1 118.24(13) . . ? C10 O1 Mn1 116.61(12) . . ? C11 O2 Mn1 122.37(14) . . ? C11 O3 Mn1 129.43(16) . 2_444 ? C12 O4 Mn1 132.87(15) . . ? C1 N1 C9 118.3(2) . . ? C1 N1 Mn1 123.71(16) . . ? C9 N1 Mn1 117.27(15) . . ? N1 C1 C2 122.5(2) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 120.1(2) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 120.0(2) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 124.2(2) . . ? C3 C4 C9 116.8(2) . . ? C5 C4 C9 119.0(2) . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 C7 121.9(2) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C8 C7 C6 119.3(2) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C7 C8 O1 125.1(2) . . ? C7 C8 C9 121.1(2) . . ? O1 C8 C9 113.8(2) . . ? N1 C9 C8 119.0(2) . . ? N1 C9 C4 122.2(2) . . ? C8 C9 C4 118.8(2) . . ? O1 C10 C11 108.18(18) . . ? O1 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? O1 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O2 C11 O3 125.0(2) . . ? O2 C11 C10 118.5(2) . . ? O3 C11 C10 116.4(2) . . ? O4 C12 O5 124.1(2) . . ? O4 C12 C13 120.3(2) . . ? O5 C12 C13 115.6(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 O5 Mn1 131.47(16) . 3_454 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.270 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.081 #========================================================END