Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Partha Mukherjee' 'Rajesh Chakraborty' 'Kartik Chandra Mondal' 'Oindrila Sengupta' _publ_contact_author_name 'Partha Mukherjee' _publ_contact_author_address ; Inorganic and Physical Chem Dept Indian Institute of Science Bangalore Karnataka 560012 INDIA ; _publ_contact_author_email PSM@IPC.IISC.ERNET.IN _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Assembling metals (CoII & MnII) with pyridylcarboxylates in presence of azide: synthesis, structural aspects and properties of three coordination polymers ; data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 663080' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co1.50 N6 O6' _chemical_formula_sum 'C18 H12 Co1.50 N6 O6' _chemical_formula_weight 496.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6797(9) _cell_length_b 11.4092(12) _cell_length_c 12.0602(19) _cell_angle_alpha 112.634(2) _cell_angle_beta 100.312(2) _cell_angle_gamma 108.048(2) _cell_volume 985.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombus _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 501 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7679 _exptl_absorpt_correction_T_max 0.8360 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10094 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3735 _reflns_number_gt 3294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0653P)^2^+1.1064P] 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 3735 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.06964(5) 0.33474(4) 0.21080(4) 0.01967(14) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.0000 0.01865(16) Uani 1 2 d S . . O1 O -0.0704(3) 0.1879(2) 0.0200(2) 0.0261(5) Uani 1 1 d . . . O2 O -0.0054(3) 0.3002(2) -0.0947(2) 0.0257(5) Uani 1 1 d . . . O3 O 0.1988(3) 0.4703(2) 0.40630(19) 0.0254(5) Uani 1 1 d . . . C1 C -0.0474(4) 0.1947(3) -0.0784(3) 0.0212(6) Uani 1 1 d . . . N2 N 0.0685(4) 0.6019(3) 0.2777(3) 0.0325(7) Uani 1 1 d . . . N5 N 0.0892(3) 0.1737(3) 0.2574(2) 0.0240(5) Uani 1 1 d . . . N4 N -0.1758(3) 0.2870(3) 0.2466(2) 0.0244(6) Uani 1 1 d . . . O4 O 0.2842(3) 0.3382(3) 0.1493(2) 0.0375(6) Uani 1 1 d . . . N6 N 0.2698(3) 0.5970(3) 0.0281(2) 0.0259(6) Uani 1 1 d . . . O6 O 0.5339(3) 0.5265(3) 0.2614(3) 0.0483(7) Uani 1 1 d . . . C2 C 0.0863(4) 0.0565(3) 0.1699(3) 0.0205(6) Uani 1 1 d . . . H2 H 0.0955 0.0524 0.0930 0.025 Uiso 1 1 calc R . . C3 C 0.4317(4) 0.4126(4) 0.1631(3) 0.0292(7) Uani 1 1 d . . . C4 C 0.3333(4) 0.5591(3) -0.0672(3) 0.0251(7) Uani 1 1 d . . . H4 H 0.2618 0.4800 -0.1443 0.030 Uiso 1 1 calc R . . C5 C -0.0703(4) 0.0598(3) -0.1874(3) 0.0229(6) Uani 1 1 d . . . C6 C -0.3099(5) 0.1630(4) 0.1692(3) 0.0370(8) Uani 1 1 d . . . H6 H -0.3025 0.1048 0.0931 0.044 Uiso 1 1 calc R . . C7 C -0.1909(4) 0.3680(3) 0.3548(3) 0.0229(6) Uani 1 1 d . . . H7 H -0.1017 0.4561 0.4078 0.027 Uiso 1 1 calc R . . C8 C -0.3310(4) 0.3290(3) 0.3929(3) 0.0243(6) Uani 1 1 d . . . C9 C 0.4995(4) 0.3670(3) 0.0553(3) 0.0279(7) Uani 1 1 d . . . C10 C 0.3295(4) 0.5806(3) 0.4774(3) 0.0269(7) Uani 1 1 d . . . N3 N 0.0723(6) 0.6905(4) 0.3672(3) 0.0633(12) Uani 1 1 d . . . C11 C -0.4665(4) 0.2015(4) 0.3119(3) 0.0385(9) Uani 1 1 d . . . H11 H -0.5630 0.1721 0.3343 0.046 Uiso 1 1 calc R . . C12 C 0.3929(5) 0.2497(4) -0.0602(4) 0.0419(9) Uani 1 1 d . . . H12 H 0.2805 0.1968 -0.0703 0.050 Uiso 1 1 calc R . . C13 C 0.3756(4) 0.7082(4) 0.1399(3) 0.0363(8) Uani 1 1 d . . . H13 H 0.3341 0.7333 0.2074 0.044 Uiso 1 1 calc R . . C14 C -0.0685(6) 0.0491(4) -0.3051(3) 0.0452(10) Uani 1 1 d . . . H14 H -0.0585 0.1242 -0.3211 0.054 Uiso 1 1 calc R . . C15 C 0.4552(5) 0.2126(4) -0.1592(4) 0.0480(10) Uani 1 1 d . . . H15 H 0.3851 0.1355 -0.2380 0.058 Uiso 1 1 calc R . . C16 C -0.4577(5) 0.1173(4) 0.1966(3) 0.0447(10) Uani 1 1 d . . . H16 H -0.5495 0.0321 0.1390 0.054 Uiso 1 1 calc R . . N1 N 0.0637(3) 0.5076(3) 0.1849(2) 0.0237(5) Uani 1 1 d . . . O7 O 0.4612(4) 0.6276(3) 0.4504(3) 0.0565(9) Uani 1 1 d . . . C17 C 0.0819(7) 0.0746(4) 0.3987(4) 0.0563(13) Uani 1 1 d . . . H17 H 0.0868 0.0855 0.4799 0.068 Uiso 1 1 calc R . . C18 C 0.0879(6) 0.1822(4) 0.3708(3) 0.0391(9) Uani 1 1 d . . . H18 H 0.0911 0.2635 0.4332 0.047 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 0.0258(2) 0.0158(2) 0.0194(2) 0.00758(17) 0.01254(17) 0.00939(17) Co2 0.0240(3) 0.0148(3) 0.0191(3) 0.0070(2) 0.0126(2) 0.0088(2) O1 0.0372(12) 0.0200(11) 0.0202(11) 0.0077(9) 0.0150(9) 0.0102(9) O2 0.0394(13) 0.0165(10) 0.0253(11) 0.0093(9) 0.0170(10) 0.0139(9) O3 0.0305(12) 0.0197(11) 0.0210(11) 0.0060(9) 0.0105(9) 0.0081(10) C1 0.0234(15) 0.0205(15) 0.0200(15) 0.0080(12) 0.0090(12) 0.0105(12) N2 0.0551(19) 0.0267(15) 0.0257(15) 0.0156(13) 0.0167(13) 0.0233(14) N5 0.0341(14) 0.0176(12) 0.0207(13) 0.0078(11) 0.0126(11) 0.0112(11) N4 0.0259(13) 0.0236(13) 0.0210(13) 0.0084(11) 0.0109(11) 0.0082(11) O4 0.0342(13) 0.0419(14) 0.0455(15) 0.0210(12) 0.0277(12) 0.0185(12) N6 0.0264(13) 0.0245(13) 0.0270(14) 0.0102(12) 0.0151(11) 0.0100(11) O6 0.0422(15) 0.0478(16) 0.0403(15) 0.0078(13) 0.0286(13) 0.0096(13) C2 0.0255(15) 0.0185(14) 0.0173(14) 0.0072(12) 0.0095(12) 0.0091(12) C3 0.0309(18) 0.0343(18) 0.0343(18) 0.0195(16) 0.0203(15) 0.0185(15) C4 0.0275(16) 0.0255(16) 0.0240(16) 0.0105(13) 0.0132(13) 0.0119(13) C5 0.0295(16) 0.0180(15) 0.0207(15) 0.0071(12) 0.0110(12) 0.0104(13) C6 0.039(2) 0.0301(18) 0.0225(17) -0.0002(15) 0.0132(15) 0.0059(16) C7 0.0246(15) 0.0202(15) 0.0208(15) 0.0076(12) 0.0089(12) 0.0076(12) C8 0.0263(15) 0.0247(16) 0.0192(15) 0.0076(13) 0.0080(12) 0.0105(13) C9 0.0290(16) 0.0305(17) 0.0321(17) 0.0159(15) 0.0178(14) 0.0165(14) C10 0.0289(17) 0.0268(17) 0.0235(16) 0.0085(14) 0.0128(13) 0.0122(14) N3 0.136(4) 0.044(2) 0.0338(18) 0.0191(17) 0.037(2) 0.061(2) C11 0.0250(17) 0.042(2) 0.0291(18) 0.0052(16) 0.0136(14) 0.0027(15) C12 0.0270(18) 0.039(2) 0.044(2) 0.0087(18) 0.0182(16) 0.0061(16) C13 0.0317(18) 0.039(2) 0.0301(18) 0.0079(16) 0.0172(15) 0.0122(16) C14 0.092(3) 0.0243(18) 0.0308(19) 0.0163(16) 0.032(2) 0.028(2) C15 0.032(2) 0.044(2) 0.037(2) -0.0016(18) 0.0138(16) 0.0036(17) C16 0.0341(19) 0.035(2) 0.0297(19) -0.0042(16) 0.0126(16) -0.0045(16) N1 0.0350(14) 0.0181(12) 0.0193(13) 0.0081(11) 0.0123(11) 0.0118(11) O7 0.0414(16) 0.0497(17) 0.0401(16) -0.0035(13) 0.0272(13) -0.0035(13) C17 0.126(4) 0.035(2) 0.0266(19) 0.0191(17) 0.041(2) 0.041(3) C18 0.075(3) 0.0230(17) 0.0287(18) 0.0110(15) 0.0314(18) 0.0249(18) _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 O1 2.086(2) . ? Co1 O3 2.093(2) . ? Co1 O4 2.119(2) . ? Co1 N1 2.127(3) . ? Co1 N5 2.162(2) . ? Co1 N4 2.194(3) . ? Co2 O2 2.101(2) . ? Co2 O2 2.101(2) 2_565 ? Co2 N6 2.155(3) . ? Co2 N6 2.155(3) 2_565 ? Co2 N1 2.160(3) . ? Co2 N1 2.160(3) 2_565 ? O1 C1 1.265(4) . ? O2 C1 1.247(4) . ? O3 C10 1.242(4) . ? C1 C5 1.516(4) . ? N2 N3 1.147(4) . ? N2 N1 1.200(4) . ? N5 C2 1.336(4) . ? N5 C18 1.336(4) . ? N4 C7 1.335(4) . ? N4 C6 1.343(4) . ? O4 C3 1.237(4) . ? N6 C13 1.338(4) . ? N6 C4 1.343(4) . ? O6 C3 1.267(4) . ? C2 C5 1.391(4) 2 ? C3 C9 1.500(4) . ? C4 C9 1.383(4) 2_665 ? C5 C14 1.381(4) . ? C5 C2 1.391(4) 2 ? C6 C16 1.378(5) . ? C7 C8 1.382(4) . ? C8 C11 1.374(5) . ? C8 C10 1.501(4) 2_566 ? C9 C4 1.383(4) 2_665 ? C9 C12 1.387(5) . ? C10 O7 1.261(4) . ? C10 C8 1.501(4) 2_566 ? C11 C16 1.385(5) . ? C12 C15 1.373(5) . ? C13 C15 1.386(5) 2_665 ? C14 C17 1.381(5) 2 ? C15 C13 1.386(5) 2_665 ? C17 C14 1.381(5) 2 ? C17 C18 1.381(5) . ? 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 Co1 O3 175.36(8) . . ? O1 Co1 O4 83.24(9) . . ? O3 Co1 O4 99.56(9) . . ? O1 Co1 N1 94.55(9) . . ? O3 Co1 N1 89.00(9) . . ? O4 Co1 N1 93.30(10) . . ? O1 Co1 N5 91.23(9) . . ? O3 Co1 N5 85.21(9) . . ? O4 Co1 N5 87.64(10) . . ? N1 Co1 N5 174.22(9) . . ? O1 Co1 N4 87.37(9) . . ? O3 Co1 N4 89.41(9) . . ? O4 Co1 N4 168.62(10) . . ? N1 Co1 N4 93.85(10) . . ? N5 Co1 N4 86.14(10) . . ? O2 Co2 O2 180.00(12) . 2_565 ? O2 Co2 N6 91.08(9) . . ? O2 Co2 N6 88.92(9) 2_565 . ? O2 Co2 N6 88.92(9) . 2_565 ? O2 Co2 N6 91.08(9) 2_565 2_565 ? N6 Co2 N6 180.00(14) . 2_565 ? O2 Co2 N1 93.21(9) . . ? O2 Co2 N1 86.79(9) 2_565 . ? N6 Co2 N1 90.43(10) . . ? N6 Co2 N1 89.57(10) 2_565 . ? O2 Co2 N1 86.79(9) . 2_565 ? O2 Co2 N1 93.21(9) 2_565 2_565 ? N6 Co2 N1 89.57(10) . 2_565 ? N6 Co2 N1 90.43(10) 2_565 2_565 ? N1 Co2 N1 180.0 . 2_565 ? C1 O1 Co1 127.83(19) . . ? C1 O2 Co2 134.31(19) . . ? C10 O3 Co1 138.8(2) . . ? O2 C1 O1 127.4(3) . . ? O2 C1 C5 116.6(3) . . ? O1 C1 C5 116.0(3) . . ? N3 N2 N1 178.9(4) . . ? C2 N5 C18 117.7(3) . . ? C2 N5 Co1 121.1(2) . . ? C18 N5 Co1 120.8(2) . . ? C7 N4 C6 116.7(3) . . ? C7 N4 Co1 122.1(2) . . ? C6 N4 Co1 120.4(2) . . ? C3 O4 Co1 144.9(2) . . ? C13 N6 C4 118.1(3) . . ? C13 N6 Co2 119.4(2) . . ? C4 N6 Co2 122.2(2) . . ? N5 C2 C5 123.7(3) . 2 ? O4 C3 O6 125.9(3) . . ? O4 C3 C9 118.5(3) . . ? O6 C3 C9 115.6(3) . . ? N6 C4 C9 122.7(3) . 2_665 ? C14 C5 C2 117.6(3) . 2 ? C14 C5 C1 121.7(3) . . ? C2 C5 C1 120.6(3) 2 . ? N4 C6 C16 123.4(3) . . ? N4 C7 C8 124.0(3) . . ? C11 C8 C7 118.1(3) . . ? C11 C8 C10 121.1(3) . 2_566 ? C7 C8 C10 120.7(3) . 2_566 ? C4 C9 C12 118.6(3) 2_665 . ? C4 C9 C3 121.5(3) 2_665 . ? C12 C9 C3 120.0(3) . . ? O3 C10 O7 126.4(3) . . ? O3 C10 C8 117.8(3) . 2_566 ? O7 C10 C8 115.8(3) . 2_566 ? C8 C11 C16 119.3(3) . . ? C15 C12 C9 119.1(3) . . ? N6 C13 C15 122.6(3) . 2_665 ? C17 C14 C5 119.0(3) 2 . ? C12 C15 C13 118.9(3) . 2_665 ? C6 C16 C11 118.4(3) . . ? N2 N1 Co1 114.4(2) . . ? N2 N1 Co2 121.1(2) . . ? Co1 N1 Co2 123.28(11) . . ? C14 C17 C18 119.5(3) 2 . ? N5 C18 C17 122.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.621 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.096 # Attachment 'Complex2.cif' data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 663081' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H13 Co1.50 N5 O5' _chemical_formula_sum 'C16 H13 Co1.50 N5 O5' _chemical_formula_weight 443.71 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.716(4) _cell_length_b 11.927(6) _cell_length_c 13.137(7) _cell_angle_alpha 82.911(10) _cell_angle_beta 83.696(9) _cell_angle_gamma 87.902(10) _cell_volume 1037.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Pink _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 449 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5217 _exptl_absorpt_correction_T_max 0.6355 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10950 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.1418 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4212 _reflns_number_gt 2561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.2000P)^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_number_reflns 4212 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.1100 _refine_ls_wR_factor_ref 0.3502 _refine_ls_wR_factor_gt 0.3304 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _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 0.5000 0.5000 0.5000 0.0164(6) Uani 1 2 d S . . Co2 Co 0.7781(2) 0.65369(12) 0.66872(11) 0.0134(5) Uani 1 1 d . . . O5 O 1.0456(11) 0.7311(7) 0.6016(6) 0.0188(17) Uani 1 1 d . . . O4 O 0.7691(12) 0.4054(7) 0.4630(7) 0.027(2) Uani 1 1 d . . . N1 N 0.8718(14) 0.6632(8) 0.8213(7) 0.021(2) Uani 1 1 d . . . O3 O 0.4921(12) 0.4381(7) 0.6515(6) 0.0234(19) Uani 1 1 d . . . N2 N 0.6428(14) 0.8202(8) 0.6685(7) 0.018(2) Uani 1 1 d . . . O2 O 0.5173(11) 0.5801(6) 0.7449(6) 0.0181(17) Uani 1 1 d . . . O1 O 0.9240(13) 0.4915(7) 0.6650(6) 0.0251(19) Uani 1 1 d . . . H1 H 0.9740 0.4734 0.7190 0.038 Uiso 1 1 calc R . . C7 C 0.7897(17) 0.5991(9) 0.9037(9) 0.020(3) Uani 1 1 d . . . H7 H 0.7030 0.5432 0.8942 0.024 Uiso 1 1 calc R . . C1 C 0.4512(17) 0.4887(10) 0.7311(9) 0.021(3) Uani 1 1 d . . . N3 N 0.6930(13) 0.6346(8) 0.5198(7) 0.018(2) Uani 1 1 d . . . C8 C 1.2673(15) 0.8871(9) 0.4706(8) 0.016(2) Uani 1 1 d . . . H8 H 1.1714 0.9074 0.5221 0.019 Uiso 1 1 calc R . . C12 C 0.4874(19) 0.8392(11) 0.7357(11) 0.030(3) Uani 1 1 d . . . H12 H 0.4417 0.7794 0.7839 0.037 Uiso 1 1 calc R . . C16 C 1.0001(18) 0.7422(11) 0.8339(10) 0.026(3) Uiso 1 1 d . . . H16 H 1.0519 0.7896 0.7762 0.031 Uiso 1 1 calc R . . C6 C 0.8266(16) 0.6113(9) 1.0024(8) 0.016(2) Uani 1 1 d . . . C10 C 1.060(2) 0.7569(13) 0.9299(9) 0.041(4) Uani 1 1 d . . . H10 H 1.1563 0.8088 0.9362 0.049 Uiso 1 1 calc R . . C4 C 1.1851(16) 0.6982(9) 0.5400(9) 0.017(2) Uani 1 1 d . . . C13 C 0.3900(18) 0.9418(9) 0.7386(10) 0.028(3) Uani 1 1 d . . . H13 H 0.2765 0.9496 0.7848 0.034 Uiso 1 1 calc R . . C9 C 0.967(2) 0.6900(11) 1.0162(9) 0.031(3) Uani 1 1 d . . . H9 H 0.9993 0.6980 1.0820 0.037 Uiso 1 1 calc R . . C11 C 0.7120(16) 0.9080(9) 0.6020(8) 0.017(2) Uiso 1 1 d . . . H11 H 0.8194 0.8950 0.5535 0.020 Uiso 1 1 calc R . . C14 C 0.4620(19) 1.0333(11) 0.6723(10) 0.028(3) Uiso 1 1 d . . . H14 H 0.4007 1.1044 0.6738 0.034 Uiso 1 1 calc R . . C5 C 1.2992(16) 0.7836(9) 0.4688(9) 0.020(3) Uani 1 1 d . . . H5 H 1.3986 0.7596 0.4207 0.024 Uiso 1 1 calc R . . C15 C 0.6337(16) 1.0156(9) 0.6013(10) 0.020(3) Uani 1 1 d . . . N4 N 0.7743(14) 0.6905(9) 0.4455(7) 0.021(2) Uani 1 1 d . . . N5 N 0.8540(16) 0.7415(10) 0.3735(8) 0.032(3) Uani 1 1 d . . . C2 C 0.3139(19) 0.4276(11) 0.8159(11) 0.032(3) Uani 1 1 d . . . H2 H 0.2463 0.3659 0.8009 0.038 Uiso 1 1 calc R . . C3 C 0.2848(16) 0.4539(9) 0.9044(9) 0.016(2) Uani 1 1 d . . . H3 H 0.3379 0.5220 0.9147 0.020 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 0.0140(11) 0.0161(12) 0.0184(12) -0.0012(9) 0.0006(9) -0.0008(8) Co2 0.0127(8) 0.0121(8) 0.0137(8) 0.0023(6) 0.0012(6) -0.0005(6) O5 0.015(4) 0.024(4) 0.017(4) -0.004(3) 0.003(3) -0.001(3) O4 0.012(4) 0.017(4) 0.046(6) 0.001(4) 0.011(4) 0.001(3) N1 0.014(5) 0.027(6) 0.021(5) 0.001(4) -0.005(4) -0.009(4) O3 0.024(4) 0.025(5) 0.020(4) -0.001(4) 0.005(3) -0.003(4) N2 0.017(5) 0.018(5) 0.019(5) 0.001(4) 0.005(4) -0.006(4) O2 0.022(4) 0.013(4) 0.018(4) 0.000(3) 0.002(3) -0.005(3) O1 0.028(5) 0.018(4) 0.027(5) 0.003(4) -0.001(4) 0.004(4) C7 0.022(6) 0.013(6) 0.025(6) -0.001(5) 0.001(5) 0.000(5) C1 0.019(6) 0.019(6) 0.022(6) 0.008(5) -0.003(5) 0.000(5) N3 0.016(5) 0.020(5) 0.018(5) 0.003(4) -0.005(4) -0.003(4) C8 0.009(5) 0.027(6) 0.005(5) 0.010(4) 0.005(4) 0.015(4) C12 0.027(7) 0.022(7) 0.039(8) -0.005(6) 0.015(6) -0.002(5) C6 0.012(5) 0.019(6) 0.013(5) 0.006(4) 0.002(4) 0.000(4) C10 0.050(9) 0.057(10) 0.014(6) -0.002(6) 0.015(6) -0.043(8) C4 0.018(6) 0.008(5) 0.022(6) -0.001(4) 0.008(5) -0.008(4) C13 0.023(6) 0.011(6) 0.042(8) 0.002(5) 0.024(6) 0.002(5) C9 0.042(8) 0.041(8) 0.009(6) -0.005(5) -0.001(5) -0.007(6) C5 0.012(5) 0.016(6) 0.028(7) 0.004(5) 0.008(5) -0.007(5) C15 0.011(5) 0.012(6) 0.038(7) 0.000(5) -0.001(5) -0.003(4) N4 0.017(5) 0.031(6) 0.014(5) -0.004(4) -0.002(4) 0.007(4) N5 0.024(6) 0.043(7) 0.025(6) 0.005(5) 0.005(5) -0.009(5) C2 0.024(7) 0.026(7) 0.044(9) 0.000(6) 0.001(6) -0.014(6) C3 0.010(5) 0.013(5) 0.026(6) 0.001(5) -0.004(4) -0.007(4) _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 O3 2.032(8) . ? Co1 O3 2.032(8) 2_666 ? Co1 O4 2.137(8) 2_666 ? Co1 O4 2.137(8) . ? Co1 N3 2.157(9) . ? Co1 N3 2.157(9) 2_666 ? Co2 O2 2.086(7) . ? Co2 O5 2.104(8) . ? Co2 N3 2.138(9) . ? Co2 O1 2.140(8) . ? Co2 N2 2.153(10) . ? Co2 N1 2.183(10) . ? O5 C4 1.254(13) . ? O4 C4 1.268(13) 2_766 ? N1 C7 1.325(14) . ? N1 C16 1.337(15) . ? O3 C1 1.271(15) . ? N2 C12 1.323(15) . ? N2 C11 1.340(13) . ? O2 C1 1.233(14) . ? C7 C6 1.373(16) . ? C1 C2 1.499(16) . ? N3 N4 1.202(13) . ? C8 C5 1.248(16) . ? C8 C15 1.526(15) 2_776 ? C12 C13 1.369(17) . ? C16 C10 1.397(17) . ? C6 C9 1.397(17) . ? C6 C3 1.507(14) 2_667 ? C10 C9 1.402(16) . ? C4 O4 1.268(13) 2_766 ? C4 C5 1.471(13) . ? C13 C14 1.376(16) . ? C11 C15 1.369(15) . ? C14 C15 1.428(17) . ? C15 C8 1.526(15) 2_776 ? N4 N5 1.150(13) . ? C2 C3 1.234(17) . ? C3 C6 1.507(14) 2_667 ? 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 O3 Co1 O3 180.000(1) . 2_666 ? O3 Co1 O4 88.5(3) . 2_666 ? O3 Co1 O4 91.5(3) 2_666 2_666 ? O3 Co1 O4 91.5(3) . . ? O3 Co1 O4 88.5(3) 2_666 . ? O4 Co1 O4 180.0(5) 2_666 . ? O3 Co1 N3 91.6(3) . . ? O3 Co1 N3 88.4(3) 2_666 . ? O4 Co1 N3 93.8(3) 2_666 . ? O4 Co1 N3 86.2(3) . . ? O3 Co1 N3 88.4(3) . 2_666 ? O3 Co1 N3 91.6(3) 2_666 2_666 ? O4 Co1 N3 86.2(3) 2_666 2_666 ? O4 Co1 N3 93.8(3) . 2_666 ? N3 Co1 N3 180.000(1) . 2_666 ? O2 Co2 O5 176.1(3) . . ? O2 Co2 N3 92.9(3) . . ? O5 Co2 N3 91.0(3) . . ? O2 Co2 O1 91.2(3) . . ? O5 Co2 O1 89.7(3) . . ? N3 Co2 O1 86.6(3) . . ? O2 Co2 N2 91.3(3) . . ? O5 Co2 N2 87.8(3) . . ? N3 Co2 N2 93.1(4) . . ? O1 Co2 N2 177.5(3) . . ? O2 Co2 N1 86.8(3) . . ? O5 Co2 N1 89.4(3) . . ? N3 Co2 N1 176.7(4) . . ? O1 Co2 N1 90.1(4) . . ? N2 Co2 N1 90.2(4) . . ? C4 O5 Co2 131.3(7) . . ? C4 O4 Co1 135.4(7) 2_766 . ? C7 N1 C16 118.9(10) . . ? C7 N1 Co2 121.2(8) . . ? C16 N1 Co2 119.6(8) . . ? C1 O3 Co1 129.5(8) . . ? C12 N2 C11 117.6(10) . . ? C12 N2 Co2 120.4(8) . . ? C11 N2 Co2 122.0(7) . . ? C1 O2 Co2 125.9(8) . . ? N1 C7 C6 123.1(10) . . ? O2 C1 O3 126.2(11) . . ? O2 C1 C2 118.5(11) . . ? O3 C1 C2 115.3(11) . . ? N4 N3 Co2 118.8(8) . . ? N4 N3 Co1 119.9(8) . . ? Co2 N3 Co1 120.6(4) . . ? C5 C8 C15 128.0(10) . 2_776 ? N2 C12 C13 123.8(12) . . ? N1 C16 C10 122.9(11) . . ? C7 C6 C9 118.4(10) . . ? C7 C6 C3 122.2(10) . 2_667 ? C9 C6 C3 119.3(10) . 2_667 ? C16 C10 C9 117.1(12) . . ? O5 C4 O4 122.4(10) . 2_766 ? O5 C4 C5 118.5(10) . . ? O4 C4 C5 119.1(10) 2_766 . ? C12 C13 C14 119.2(11) . . ? C6 C9 C10 119.3(11) . . ? N2 C11 C15 123.8(10) . . ? C13 C14 C15 117.9(11) . . ? C8 C5 C4 122.3(10) . . ? C11 C15 C14 117.6(11) . . ? C11 C15 C8 120.5(10) . 2_776 ? C14 C15 C8 121.9(10) . 2_776 ? N5 N4 N3 178.3(12) . . ? C3 C2 C1 124.1(12) . . ? C2 C3 C6 127.7(11) . 2_667 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.046 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.269 # Attachment 'Complex3.cif' data_Complex3_m _database_code_depnum_ccdc_archive 'CCDC 663082' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H6 Mn0.50 N O2' _chemical_formula_sum 'C8 H6 Mn0.50 N O2' _chemical_formula_weight 175.61 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.9350(3) _cell_length_b 8.1072(5) _cell_length_c 9.5198(5) _cell_angle_alpha 70.4350(10) _cell_angle_beta 79.5600(10) _cell_angle_gamma 76.1370(10) _cell_volume 346.30(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 179 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8066 _exptl_absorpt_correction_T_max 0.8918 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4046 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.01 _reflns_number_total 1626 _reflns_number_gt 1579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0300P)^2^+0.1249P] 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 1626 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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 1.0000 0.0000 1.0000 0.01974(10) Uani 1 2 d S . . O1 O 0.6281(2) 0.16651(13) 0.90776(10) 0.0245(2) Uani 1 1 d . . . O2 O 0.2580(2) 0.15519(14) 0.80895(11) 0.0247(2) Uani 1 1 d . . . N1 N 0.9674(2) 0.18419(16) 0.15129(13) 0.0249(2) Uani 1 1 d . . . C1 C 0.5045(3) 0.17932(17) 0.79846(14) 0.0194(2) Uani 1 1 d . . . C2 C 0.6687(3) 0.2285(2) 0.64735(15) 0.0256(3) Uani 1 1 d . . . H2 H 0.8359 0.2657 0.6411 0.031 Uiso 1 1 calc R . . C3 C 0.5968(3) 0.22376(19) 0.52144(15) 0.0248(3) Uani 1 1 d . . . H3 H 0.4250 0.1937 0.5243 0.030 Uiso 1 1 calc R . . C4 C 0.7755(3) 0.26376(18) 0.37709(15) 0.0233(3) Uani 1 1 d . . . C5 C 0.9414(3) 0.3928(2) 0.33547(16) 0.0280(3) Uani 1 1 d . . . H5 H 0.9321 0.4638 0.3959 0.034 Uiso 1 1 calc R . . C6 C 1.1200(3) 0.4144(2) 0.20384(17) 0.0315(3) Uani 1 1 d . . . H6 H 1.2314 0.5005 0.1741 0.038 Uiso 1 1 calc R . . C7 C 1.1308(3) 0.3057(2) 0.11675(16) 0.0284(3) Uani 1 1 d . . . H7 H 1.2571 0.3176 0.0303 0.034 Uiso 1 1 calc R . . C8 C 0.7918(3) 0.16719(19) 0.27820(15) 0.0260(3) Uani 1 1 d . . . H8 H 0.6733 0.0859 0.3017 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01854(15) 0.02797(16) 0.01543(14) -0.00955(11) 0.00063(10) -0.00723(11) O1 0.0220(5) 0.0353(5) 0.0188(4) -0.0115(4) -0.0019(4) -0.0057(4) O2 0.0213(5) 0.0350(5) 0.0199(4) -0.0085(4) 0.0007(4) -0.0114(4) N1 0.0281(6) 0.0297(6) 0.0190(5) -0.0111(5) 0.0007(4) -0.0068(5) C1 0.0207(6) 0.0210(6) 0.0175(6) -0.0078(5) 0.0006(5) -0.0049(5) C2 0.0233(6) 0.0364(7) 0.0201(6) -0.0104(5) 0.0030(5) -0.0128(6) C3 0.0259(6) 0.0308(7) 0.0200(6) -0.0101(5) 0.0030(5) -0.0102(5) C4 0.0263(6) 0.0285(7) 0.0165(6) -0.0090(5) -0.0002(5) -0.0062(5) C5 0.0363(8) 0.0308(7) 0.0220(6) -0.0133(6) 0.0015(6) -0.0119(6) C6 0.0368(8) 0.0352(8) 0.0275(7) -0.0124(6) 0.0057(6) -0.0188(6) C7 0.0298(7) 0.0348(7) 0.0209(6) -0.0111(6) 0.0054(5) -0.0092(6) C8 0.0311(7) 0.0309(7) 0.0201(6) -0.0112(5) 0.0017(5) -0.0123(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.1363(10) 2_757 ? Mn1 O1 2.1363(10) . ? Mn1 O2 2.2153(9) 1_655 ? Mn1 O2 2.2153(9) 2_657 ? Mn1 N1 2.3604(11) 1_556 ? Mn1 N1 2.3604(11) 2_756 ? O1 C1 1.2622(15) . ? O2 C1 1.2591(16) . ? O2 Mn1 2.2153(9) 1_455 ? N1 C8 1.3402(17) . ? N1 C7 1.3404(19) . ? N1 Mn1 2.3604(11) 1_554 ? C1 C2 1.4944(17) . ? C2 C3 1.325(2) . ? C2 H2 0.9300 . ? C3 C4 1.4735(18) . ? C3 H3 0.9300 . ? C4 C5 1.392(2) . ? C4 C8 1.3935(19) . ? C5 C6 1.380(2) . ? C5 H5 0.9300 . ? C6 C7 1.384(2) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8 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 Mn1 O1 180.000(1) 2_757 . ? O1 Mn1 O2 90.34(4) 2_757 1_655 ? O1 Mn1 O2 89.66(4) . 1_655 ? O1 Mn1 O2 89.66(4) 2_757 2_657 ? O1 Mn1 O2 90.34(4) . 2_657 ? O2 Mn1 O2 180.0 1_655 2_657 ? O1 Mn1 N1 91.10(4) 2_757 1_556 ? O1 Mn1 N1 88.90(4) . 1_556 ? O2 Mn1 N1 95.00(4) 1_655 1_556 ? O2 Mn1 N1 85.00(4) 2_657 1_556 ? O1 Mn1 N1 88.90(4) 2_757 2_756 ? O1 Mn1 N1 91.10(4) . 2_756 ? O2 Mn1 N1 85.00(4) 1_655 2_756 ? O2 Mn1 N1 95.00(4) 2_657 2_756 ? N1 Mn1 N1 180.0 1_556 2_756 ? C1 O1 Mn1 133.99(9) . . ? C1 O2 Mn1 130.67(9) . 1_455 ? C8 N1 C7 117.20(12) . . ? C8 N1 Mn1 121.33(9) . 1_554 ? C7 N1 Mn1 121.42(9) . 1_554 ? O2 C1 O1 124.78(12) . . ? O2 C1 C2 119.36(11) . . ? O1 C1 C2 115.87(11) . . ? C3 C2 C1 125.67(12) . . ? C3 C2 H2 117.2 . . ? C1 C2 H2 117.2 . . ? C2 C3 C4 123.24(13) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C8 117.15(12) . . ? C5 C4 C3 122.41(12) . . ? C8 C4 C3 120.40(12) . . ? C6 C5 C4 119.48(13) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 118.93(13) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? N1 C7 C6 123.01(13) . . ? N1 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? N1 C8 C4 124.10(13) . . ? N1 C8 H8 118.0 . . ? C4 C8 H8 118.0 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.301 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.068