# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email liudongsheng@jgsu.edu.cn _publ_contact_author_name 'Dong-Sheng Liu' loop_ _publ_author_name 'Dong-Sheng Liu' 'Yan Sui' 'Tiangwei Wang' 'Chang-Cang Huang' 'Zhong Jian' 'Xiaozeng You' data_compound1Mn _database_code_depnum_ccdc_archive 'CCDC 722568' #TrackingRef '- complex1Mn.cif' _audit_update_record ; 2012-01-31 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H13 Mn2 N7 O6), (H2 O)' _chemical_formula_sum 'C26 H28 Mn4 N14 O13' _chemical_formula_weight 964.38 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 P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.092(2) _cell_length_b 6.8365(14) _cell_length_c 26.072(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.17(3) _cell_angle_gamma 90.00 _cell_volume 1798.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.742 _exptl_absorpt_process_details 'RAPID AUTO (Rigaku Corporation, 1998)' _exptl_special_details ? _diffrn_ambient_temperature 298(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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number None _diffrn_standards_interval_count ? _diffrn_standards_interval_time None _diffrn_standards_decay_% 0 _diffrn_reflns_number 12707 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3675 _reflns_number_gt 3373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2002)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. The hydrogen atoms bonded to carbon in this compound have been placed in calculated positions using a riding model for refinement. The hydroxyl H atoms and H atoms of water molecules were refined with O-H distance restraint 0.83(1) \%A. ; _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^)+(0.0696P)^2^+4.9313P] 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 3675 _refine_ls_number_parameters 285 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 0.37679(5) 0.42566(8) 0.13235(2) 0.01864(18) Uani 1 1 d . . . Mn2 Mn 0.25040(5) 0.67394(8) 0.24974(2) 0.01840(18) Uani 1 1 d . . . O1 O 1.0528(3) 0.2604(4) 0.22550(12) 0.0313(7) Uani 1 1 d . . . O2 O 1.0553(3) 0.5880(4) 0.22438(13) 0.0314(7) Uani 1 1 d . . . O3 O -0.3022(3) 0.3190(5) 0.04116(14) 0.0383(8) Uani 1 1 d . . . O4 O -0.2759(3) 0.6343(6) 0.02430(14) 0.0441(9) Uani 1 1 d . . . O5 O 0.3413(3) 0.4235(4) 0.21538(11) 0.0198(6) Uani 1 1 d D . . OW1 O 0.4468(3) 0.4173(6) 0.05567(11) 0.0383(8) Uani 1 1 d D . . OW2 O -0.2036(7) 1.0023(8) -0.0192(2) 0.0338(15) Uani 0.50 1 d PD . . N1 N 0.6014(3) 0.4266(5) 0.16006(14) 0.0260(8) Uani 1 1 d . . . N2 N 0.1631(3) 0.4427(5) 0.10144(14) 0.0266(8) Uani 1 1 d . . . N3 N 0.5085(5) 0.9277(7) 0.07441(18) 0.0406(11) Uani 1 1 d . . . N4 N 0.3742(3) 1.0873(5) 0.13628(13) 0.0219(7) Uani 1 1 d . . . N5 N 0.2975(3) 1.0193(5) 0.17481(13) 0.0219(7) Uani 1 1 d . . . N6 N 0.2994(3) 0.8294(5) 0.17493(13) 0.0217(7) Uani 1 1 d . . . N7 N 0.3779(3) 0.7638(5) 0.13661(12) 0.0211(7) Uani 1 1 d . . . C1 C 0.6615(4) 0.2614(7) 0.17457(19) 0.0363(11) Uani 1 1 d . . . H3 H 0.6148 0.1446 0.1717 0.044 Uiso 1 1 calc R . . C2 C 0.7894(4) 0.2550(7) 0.19354(19) 0.0347(11) Uani 1 1 d . . . H6 H 0.8270 0.1363 0.2032 0.042 Uiso 1 1 calc R . . C3 C 0.8605(4) 0.4256(6) 0.19806(15) 0.0216(8) Uani 1 1 d . . . C4 C 0.8006(4) 0.5977(6) 0.18306(19) 0.0315(10) Uani 1 1 d . . . H12 H 0.8456 0.7161 0.1854 0.038 Uiso 1 1 calc R . . C5 C 0.6718(4) 0.5905(7) 0.1644(2) 0.0346(11) Uani 1 1 d . . . H11 H 0.6322 0.7072 0.1543 0.042 Uiso 1 1 calc R . . C6 C 1.0023(4) 0.4237(6) 0.21751(16) 0.0224(8) Uani 1 1 d . . . C7 C 0.1113(4) 0.6116(7) 0.08363(19) 0.0339(10) Uani 1 1 d . . . H10 H 0.1633 0.7239 0.0851 0.041 Uiso 1 1 calc R . . C8 C -0.0150(4) 0.6264(7) 0.06327(18) 0.0331(10) Uani 1 1 d . . . H9 H -0.0464 0.7462 0.0515 0.040 Uiso 1 1 calc R . . C9 C -0.0941(4) 0.4620(7) 0.06050(16) 0.0270(9) Uani 1 1 d . . . C10 C -0.0414(4) 0.2877(7) 0.07751(18) 0.0336(10) Uani 1 1 d . . . H5 H -0.0913 0.1734 0.0758 0.040 Uiso 1 1 calc R . . C11 C 0.0862(4) 0.2836(7) 0.09708(18) 0.0318(10) Uani 1 1 d . . . H7 H 0.1205 0.1641 0.1078 0.038 Uiso 1 1 calc R . . C12 C -0.2352(4) 0.4732(7) 0.04006(16) 0.0275(9) Uani 1 1 d . . . C13 C 0.4212(4) 0.9270(6) 0.11340(16) 0.0221(8) Uani 1 1 d . . . HW1A H 0.5224(16) 0.387(7) 0.0464(14) 0.027 Uiso 1 1 d D . . HW1B H 0.397(3) 0.406(7) 0.0303(10) 0.027 Uiso 1 1 d D . . HW2A H -0.218(8) 0.896(5) -0.006(3) 0.027 Uiso 0.50 1 d PD . . HW2B H -0.242(8) 1.087(7) -0.003(3) 0.027 Uiso 0.50 1 d PD . . H4 H 0.416(2) 0.417(7) 0.2294(16) 0.027 Uiso 1 1 d D . . H1 H 0.529(5) 0.818(9) 0.058(2) 0.044(16) Uiso 1 1 d . . . H2 H 0.537(6) 1.029(9) 0.062(2) 0.055(19) Uiso 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 0.0167(3) 0.0155(3) 0.0237(3) 0.0004(2) -0.0030(2) 0.0007(2) Mn2 0.0159(3) 0.0133(3) 0.0260(3) -0.0006(2) -0.0015(2) -0.0012(2) O1 0.0181(14) 0.0265(17) 0.0493(19) 0.0020(14) -0.0101(13) 0.0028(12) O2 0.0186(14) 0.0272(17) 0.0484(19) -0.0023(14) -0.0097(13) -0.0024(12) O3 0.0223(15) 0.0360(19) 0.057(2) -0.0032(16) -0.0082(14) 0.0011(14) O4 0.0287(17) 0.044(2) 0.059(2) 0.0091(18) -0.0182(16) 0.0040(15) O5 0.0157(12) 0.0162(13) 0.0274(14) -0.0003(11) -0.0024(11) 0.0006(11) OW1 0.0178(15) 0.072(3) 0.0247(16) 0.0033(16) -0.0020(12) 0.0012(16) OW2 0.063(4) 0.006(3) 0.032(3) -0.001(2) 0.015(3) 0.002(3) N1 0.0159(16) 0.031(2) 0.0309(19) 0.0007(15) -0.0055(14) -0.0009(14) N2 0.0193(16) 0.032(2) 0.0291(18) -0.0025(15) -0.0048(14) 0.0012(14) N3 0.053(3) 0.023(2) 0.046(3) 0.0005(19) 0.022(2) 0.0032(19) N4 0.0221(17) 0.0170(17) 0.0265(18) 0.0027(13) 0.0002(13) -0.0011(13) N5 0.0218(16) 0.0159(16) 0.0280(18) 0.0006(14) -0.0014(13) 0.0016(13) N6 0.0205(16) 0.0157(16) 0.0289(18) -0.0012(13) -0.0027(13) 0.0010(13) N7 0.0223(17) 0.0184(17) 0.0227(17) -0.0031(13) -0.0001(13) 0.0005(13) C1 0.024(2) 0.026(2) 0.058(3) 0.006(2) -0.013(2) -0.0052(18) C2 0.022(2) 0.026(2) 0.056(3) 0.008(2) -0.012(2) 0.0014(18) C3 0.0156(18) 0.026(2) 0.0233(19) -0.0031(16) -0.0028(15) -0.0002(15) C4 0.021(2) 0.021(2) 0.053(3) -0.001(2) -0.0078(19) -0.0018(17) C5 0.022(2) 0.027(2) 0.055(3) 0.003(2) -0.013(2) 0.0062(18) C6 0.0136(17) 0.027(2) 0.026(2) -0.0003(16) -0.0033(15) 0.0020(15) C7 0.027(2) 0.030(2) 0.045(3) 0.006(2) -0.014(2) -0.0005(18) C8 0.029(2) 0.031(2) 0.039(3) 0.006(2) -0.0113(19) 0.0027(19) C9 0.0198(19) 0.038(2) 0.023(2) -0.0046(18) -0.0031(15) 0.0059(17) C10 0.023(2) 0.034(2) 0.043(3) -0.004(2) -0.0047(19) 0.0010(19) C11 0.025(2) 0.029(2) 0.041(3) -0.001(2) -0.0084(19) 0.0062(18) C12 0.022(2) 0.040(3) 0.021(2) -0.0030(18) -0.0025(15) 0.0064(19) C13 0.0208(19) 0.019(2) 0.026(2) -0.0006(16) -0.0035(15) 0.0020(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 OW1 2.123(3) . ? Mn1 O5 2.195(3) . ? Mn1 N2 2.303(3) . ? Mn1 N7 2.314(3) . ? Mn1 N4 2.315(3) 1_545 ? Mn1 N1 2.377(3) . ? Mn2 O5 2.140(3) . ? Mn2 O5 2.145(3) 2 ? Mn2 O2 2.157(3) 1_455 ? Mn2 O1 2.168(3) 2_655 ? Mn2 N6 2.277(3) . ? Mn2 N5 2.286(3) 2_545 ? O1 C6 1.245(5) . ? O1 Mn2 2.168(3) 2_645 ? O2 C6 1.257(5) . ? O2 Mn2 2.157(3) 1_655 ? O3 C12 1.253(6) . ? O4 C12 1.245(6) . ? O5 Mn2 2.145(3) 2_545 ? O5 H4 0.835(10) . ? OW1 HW1A 0.828(10) . ? OW1 HW1B 0.832(10) . ? OW2 HW2A 0.822(10) . ? OW2 HW2B 0.821(10) . ? N1 C5 1.331(6) . ? N1 C1 1.336(6) . ? N2 C11 1.340(6) . ? N2 C7 1.349(6) . ? N3 C13 1.347(6) . ? N3 H1 0.89(6) . ? N3 H2 0.82(6) . ? N4 C13 1.336(5) . ? N4 N5 1.352(5) . ? N4 Mn1 2.315(3) 1_565 ? N5 N6 1.299(5) . ? N5 Mn2 2.286(3) 2 ? N6 N7 1.354(5) . ? N7 C13 1.343(5) . ? C1 C2 1.381(6) . ? C1 H3 0.9300 . ? C2 C3 1.374(6) . ? C2 H6 0.9300 . ? C3 C4 1.379(6) . ? C3 C6 1.516(5) . ? C4 C5 1.388(6) . ? C4 H12 0.9300 . ? C5 H11 0.9300 . ? C7 C8 1.383(6) . ? C7 H10 0.9300 . ? C8 C9 1.380(7) . ? C8 H9 0.9300 . ? C9 C10 1.378(6) . ? C9 C12 1.521(6) . ? C10 C11 1.384(6) . ? C10 H5 0.9300 . ? C11 H7 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 OW1 Mn1 O5 169.78(11) . . ? OW1 Mn1 N2 89.19(12) . . ? O5 Mn1 N2 100.94(12) . . ? OW1 Mn1 N7 94.05(13) . . ? O5 Mn1 N7 87.71(10) . . ? N2 Mn1 N7 88.32(12) . . ? OW1 Mn1 N4 91.06(13) . 1_545 ? O5 Mn1 N4 87.01(11) . 1_545 ? N2 Mn1 N4 93.17(12) . 1_545 ? N7 Mn1 N4 174.69(12) . 1_545 ? OW1 Mn1 N1 88.09(12) . . ? O5 Mn1 N1 81.88(12) . . ? N2 Mn1 N1 175.84(13) . . ? N7 Mn1 N1 88.74(12) . . ? N4 Mn1 N1 90.02(12) 1_545 . ? O5 Mn2 O5 179.56(9) . 2 ? O5 Mn2 O2 92.61(11) . 1_455 ? O5 Mn2 O2 87.27(11) 2 1_455 ? O5 Mn2 O1 87.10(11) . 2_655 ? O5 Mn2 O1 93.03(11) 2 2_655 ? O2 Mn2 O1 179.47(13) 1_455 2_655 ? O5 Mn2 N6 85.43(11) . . ? O5 Mn2 N6 94.99(11) 2 . ? O2 Mn2 N6 93.73(12) 1_455 . ? O1 Mn2 N6 85.80(12) 2_655 . ? O5 Mn2 N5 94.73(11) . 2_545 ? O5 Mn2 N5 84.85(11) 2 2_545 ? O2 Mn2 N5 86.70(12) 1_455 2_545 ? O1 Mn2 N5 93.77(12) 2_655 2_545 ? N6 Mn2 N5 179.54(12) . 2_545 ? C6 O1 Mn2 132.0(3) . 2_645 ? C6 O2 Mn2 132.5(3) . 1_655 ? Mn2 O5 Mn2 105.84(12) . 2_545 ? Mn2 O5 Mn1 118.62(12) . . ? Mn2 O5 Mn1 119.70(12) 2_545 . ? Mn2 O5 H4 104(3) . . ? Mn2 O5 H4 99(3) 2_545 . ? Mn1 O5 H4 106(3) . . ? Mn1 OW1 HW1A 126(3) . . ? Mn1 OW1 HW1B 123(3) . . ? HW1A OW1 HW1B 107.2(17) . . ? HW2A OW2 HW2B 108.6(19) . . ? C5 N1 C1 116.4(4) . . ? C5 N1 Mn1 122.4(3) . . ? C1 N1 Mn1 121.0(3) . . ? C11 N2 C7 116.3(4) . . ? C11 N2 Mn1 122.0(3) . . ? C7 N2 Mn1 121.7(3) . . ? C13 N3 H1 121(4) . . ? C13 N3 H2 123(4) . . ? H1 N3 H2 116(6) . . ? C13 N4 N5 104.7(3) . . ? C13 N4 Mn1 142.7(3) . 1_565 ? N5 N4 Mn1 112.5(2) . 1_565 ? N6 N5 N4 109.7(3) . . ? N6 N5 Mn2 117.6(3) . 2 ? N4 N5 Mn2 127.1(2) . 2 ? N5 N6 N7 109.8(3) . . ? N5 N6 Mn2 117.7(3) . . ? N7 N6 Mn2 127.4(2) . . ? C13 N7 N6 104.4(3) . . ? C13 N7 Mn1 144.1(3) . . ? N6 N7 Mn1 111.3(2) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H3 118.3 . . ? C2 C1 H3 118.3 . . ? C3 C2 C1 119.4(4) . . ? C3 C2 H6 120.3 . . ? C1 C2 H6 120.3 . . ? C2 C3 C4 118.1(4) . . ? C2 C3 C6 120.9(4) . . ? C4 C3 C6 121.0(4) . . ? C3 C4 C5 118.6(4) . . ? C3 C4 H12 120.7 . . ? C5 C4 H12 120.7 . . ? N1 C5 C4 124.0(4) . . ? N1 C5 H11 118.0 . . ? C4 C5 H11 118.0 . . ? O1 C6 O2 127.1(4) . . ? O1 C6 C3 116.7(3) . . ? O2 C6 C3 116.2(3) . . ? N2 C7 C8 123.3(4) . . ? N2 C7 H10 118.3 . . ? C8 C7 H10 118.3 . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H9 120.2 . . ? C7 C8 H9 120.2 . . ? C10 C9 C8 117.7(4) . . ? C10 C9 C12 121.1(4) . . ? C8 C9 C12 121.2(4) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H5 120.2 . . ? C11 C10 H5 120.2 . . ? N2 C11 C10 123.5(4) . . ? N2 C11 H7 118.2 . . ? C10 C11 H7 118.2 . . ? O4 C12 O3 125.1(4) . . ? O4 C12 C9 117.9(4) . . ? O3 C12 C9 117.0(4) . . ? N4 C13 N7 111.3(3) . . ? N4 C13 N3 124.6(4) . . ? N7 C13 N3 123.9(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.970 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.114 # Attachment '- complex2Co.cif' data_complex2Co _database_code_depnum_ccdc_archive 'CCDC 748323' #TrackingRef '- complex2Co.cif' _audit_update_record ; 2012-01-31 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H13 Co2 N7 O6), (H2 O)' _chemical_formula_sum 'C26 H28 Co4 N14 O13' _chemical_formula_weight 980.34 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 monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.913(2) _cell_length_b 6.6138(13) _cell_length_c 25.912(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.35(3) _cell_angle_gamma 90.00 _cell_volume 1698.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Lamellar _exptl_crystal_colour 'Orange red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 2.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_T_max 0.688 _exptl_absorpt_process_details 'RAPID AUTO (Rigaku Corporation, 1998)' _exptl_special_details ? _diffrn_ambient_temperature 298(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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number None _diffrn_standards_interval_count ? _diffrn_standards_interval_time None _diffrn_standards_decay_% 0 _diffrn_reflns_number 12630 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3470 _reflns_number_gt 3248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2002)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. The hydrogen atoms bonded to carbon in this compound have been placed in calculated positions using a riding model for refinement. The hydroxyl H atoms and H atoms of water molecules were refined with O-H distance restraint 0.83(1) \%A. ; _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^)+(0.0928P)^2^+3.7056P] 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 3470 _refine_ls_number_parameters 288 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.006 _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 0.37731(5) 0.43094(8) 0.13563(2) 0.0176(2) Uani 1 1 d . . . Co2 Co 0.25031(5) 0.18089(8) 0.25035(2) 0.0171(2) Uani 1 1 d . . . OW1 O 0.4425(3) 0.4401(5) 0.06101(12) 0.0302(8) Uani 1 1 d D . . OW2 O -0.1974(8) 0.9997(11) -0.0187(3) 0.0394(17) Uani 0.50 1 d PD . . O1 O 0.3375(3) 0.4300(4) 0.21570(11) 0.0172(6) Uani 1 1 d D . . O2 O 1.0587(3) 0.6011(5) 0.22277(13) 0.0258(7) Uani 1 1 d . . . O3 O 1.0571(3) 0.2612(5) 0.22529(13) 0.0268(7) Uani 1 1 d . . . O4 O -0.2727(4) 0.6233(6) 0.01939(15) 0.0438(10) Uani 1 1 d . . . O5 O -0.3076(3) 0.3088(6) 0.04521(14) 0.0379(9) Uani 1 1 d . . . N1 N 0.5944(4) 0.4296(5) 0.16118(15) 0.0235(8) Uani 1 1 d . . . N2 N 0.1676(4) 0.4397(6) 0.10495(15) 0.0240(8) Uani 1 1 d . . . N3 N 0.3716(3) 0.0988(5) 0.13993(13) 0.0187(8) Uani 1 1 d . . . N4 N 0.2979(3) 0.0292(5) 0.18031(14) 0.0203(7) Uani 1 1 d . . . N5 N 0.2986(3) -0.1664(5) 0.18012(14) 0.0209(7) Uani 1 1 d . . . N6 N 0.3723(3) -0.2369(5) 0.14032(13) 0.0197(8) Uani 1 1 d . . . N7 N 0.5002(5) -0.0717(7) 0.07539(19) 0.0370(11) Uani 1 1 d . . . C1 C 1.0045(4) 0.4303(6) 0.21696(16) 0.0197(9) Uani 1 1 d . . . C2 C 0.8610(4) 0.4315(6) 0.19768(17) 0.0205(9) Uani 1 1 d . . . C3 C 0.8009(5) 0.6059(7) 0.1797(2) 0.0289(10) Uani 1 1 d . . . H3 H 0.8483 0.7273 0.1796 0.035 Uiso 1 1 calc R . . C4 C 0.6694(4) 0.5983(7) 0.1619(2) 0.0299(11) Uani 1 1 d . . . H4 H 0.6306 0.7172 0.1497 0.036 Uiso 1 1 calc R . . C5 C 0.6550(4) 0.2609(7) 0.1786(2) 0.0306(11) Uani 1 1 d . . . H5 H 0.6061 0.1409 0.1782 0.037 Uiso 1 1 calc R . . C6 C 0.7858(4) 0.2562(7) 0.1969(2) 0.0305(11) Uani 1 1 d . . . H6 H 0.8231 0.1355 0.2087 0.037 Uiso 1 1 calc R . . C7 C 0.1154(5) 0.6097(8) 0.08499(19) 0.0315(11) Uani 1 1 d . . . H7 H 0.1680 0.7262 0.0860 0.038 Uiso 1 1 calc R . . C8 C -0.0121(5) 0.6227(8) 0.06295(19) 0.0315(11) Uani 1 1 d . . . H8 H -0.0427 0.7444 0.0492 0.038 Uiso 1 1 calc R . . C9 C -0.0929(5) 0.4533(7) 0.06158(17) 0.0260(10) Uani 1 1 d . . . C10 C -0.2352(5) 0.4632(8) 0.03990(18) 0.0290(10) Uani 1 1 d . . . C11 C -0.0402(5) 0.2752(8) 0.08083(19) 0.0317(11) Uani 1 1 d . . . H11 H -0.0906 0.1567 0.0795 0.038 Uiso 1 1 calc R . . C12 C 0.0884(5) 0.2739(8) 0.10222(19) 0.0298(10) Uani 1 1 d . . . H12 H 0.1218 0.1528 0.1153 0.036 Uiso 1 1 calc R . . C13 C 0.4157(4) -0.0691(6) 0.11625(17) 0.0196(9) Uani 1 1 d . . . H1 H 0.412(3) 0.439(8) 0.2299(19) 0.035(16) Uiso 1 1 d D . . H13 H 0.389(3) 0.415(7) 0.0373(12) 0.027(14) Uiso 1 1 d D . . H14 H 0.5199(16) 0.412(7) 0.0517(15) 0.022(13) Uiso 1 1 d D . . H15 H -0.274(3) 0.984(16) -0.030(3) 0.026 Uiso 0.50 1 d PD . . H16 H -0.202(8) 1.054(13) 0.0099(17) 0.026 Uiso 0.50 1 d PD . . H10 H 0.515(7) -0.214(13) 0.059(3) 0.09(3) Uiso 1 1 d . . . H9 H 0.535(6) 0.025(10) 0.066(2) 0.048(19) Uiso 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 Co1 0.0154(3) 0.0162(3) 0.0213(3) 0.0006(2) -0.0022(2) 0.0008(2) Co2 0.0144(3) 0.0137(3) 0.0232(3) 0.0006(2) -0.0018(2) 0.0009(2) OW1 0.0163(16) 0.051(2) 0.0236(17) 0.0001(14) -0.0036(13) 0.0039(15) OW2 0.062(5) 0.023(3) 0.033(4) -0.008(3) 0.015(3) -0.002(4) O1 0.0121(13) 0.0177(15) 0.0218(14) -0.0034(11) -0.0024(11) -0.0001(11) O2 0.0146(14) 0.0245(17) 0.0382(18) -0.0011(14) -0.0086(13) -0.0018(12) O3 0.0178(15) 0.0237(16) 0.0387(19) 0.0012(14) -0.0060(13) 0.0030(13) O4 0.0313(19) 0.048(2) 0.052(2) 0.014(2) -0.0198(17) -0.0023(17) O5 0.0207(16) 0.041(2) 0.052(2) 0.0000(17) -0.0048(15) 0.0017(15) N1 0.0175(18) 0.027(2) 0.0262(19) -0.0007(15) -0.0043(14) -0.0009(15) N2 0.0137(17) 0.031(2) 0.028(2) -0.0007(15) -0.0025(14) 0.0013(15) N3 0.0162(17) 0.0202(19) 0.0197(17) 0.0005(14) -0.0008(13) -0.0013(13) N4 0.0193(17) 0.0167(17) 0.0249(18) 0.0022(14) -0.0034(14) 0.0004(14) N5 0.0211(17) 0.0162(18) 0.0255(18) 0.0006(14) -0.0001(14) 0.0007(14) N6 0.0203(17) 0.0180(18) 0.0207(18) -0.0027(14) 0.0026(14) -0.0011(14) N7 0.047(3) 0.024(2) 0.040(3) 0.0004(19) 0.020(2) 0.000(2) C1 0.0142(19) 0.026(2) 0.019(2) -0.0011(16) -0.0032(15) 0.0041(17) C2 0.0134(19) 0.026(2) 0.022(2) -0.0015(16) -0.0025(16) 0.0014(16) C3 0.019(2) 0.023(2) 0.045(3) 0.003(2) -0.0066(19) -0.0001(18) C4 0.017(2) 0.028(3) 0.045(3) 0.004(2) -0.0077(19) 0.0047(18) C5 0.021(2) 0.022(2) 0.049(3) 0.003(2) -0.010(2) -0.0038(18) C6 0.020(2) 0.026(2) 0.045(3) 0.006(2) -0.012(2) -0.0020(19) C7 0.028(2) 0.028(3) 0.038(3) 0.004(2) -0.009(2) -0.003(2) C8 0.025(2) 0.036(3) 0.034(3) 0.008(2) -0.0090(19) 0.003(2) C9 0.024(2) 0.033(3) 0.021(2) -0.0020(18) -0.0043(17) 0.0072(19) C10 0.022(2) 0.039(3) 0.027(2) -0.002(2) -0.0043(18) 0.003(2) C11 0.024(2) 0.035(3) 0.036(3) -0.002(2) -0.0081(19) -0.003(2) C12 0.026(2) 0.028(2) 0.035(3) 0.001(2) -0.0109(19) 0.0008(19) C13 0.020(2) 0.017(2) 0.022(2) -0.0026(16) -0.0028(16) 0.0008(16) _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 OW1 2.043(3) . ? Co1 O1 2.114(3) . ? Co1 N3 2.200(4) . ? Co1 N6 2.201(4) 1_565 ? Co1 N2 2.222(4) . ? Co1 N1 2.247(4) . ? Co2 O1 2.068(3) . ? Co2 O1 2.073(3) 2_545 ? Co2 O2 2.081(3) 2_645 ? Co2 O3 2.088(3) 1_455 ? Co2 N5 2.124(4) 2 ? Co2 N4 2.129(4) . ? OW1 H13 0.827(10) . ? OW1 H14 0.827(10) . ? OW2 H15 0.825(10) . ? OW2 H16 0.826(10) . ? O1 Co2 2.073(3) 2 ? O1 H1 0.825(10) . ? O2 C1 1.260(5) . ? O2 Co2 2.081(3) 2_655 ? O3 C1 1.252(5) . ? O3 Co2 2.088(3) 1_655 ? O4 C10 1.241(6) . ? O5 C10 1.256(6) . ? N1 C4 1.341(6) . ? N1 C5 1.344(6) . ? N2 C7 1.340(6) . ? N2 C12 1.350(6) . ? N3 C13 1.343(5) . ? N3 N4 1.360(5) . ? N4 N5 1.294(5) . ? N5 N6 1.351(5) . ? N5 Co2 2.124(4) 2_545 ? N6 C13 1.345(5) . ? N6 Co1 2.201(4) 1_545 ? N7 C13 1.354(6) . ? N7 H10 1.05(8) . ? N7 H9 0.77(7) . ? C1 C2 1.505(5) . ? C2 C3 1.378(6) . ? C2 C6 1.379(6) . ? C3 C4 1.380(6) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.378(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.386(6) . ? C7 H7 0.9300 . ? C8 C9 1.377(7) . ? C8 H8 0.9300 . ? C9 C11 1.381(7) . ? C9 C10 1.517(6) . ? C11 C12 1.387(6) . ? C11 H11 0.9300 . ? C12 H12 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 OW1 Co1 O1 172.17(12) . . ? OW1 Co1 N3 94.92(14) . . ? O1 Co1 N3 86.69(12) . . ? OW1 Co1 N6 91.73(14) . 1_565 ? O1 Co1 N6 86.81(11) . 1_565 ? N3 Co1 N6 173.31(13) . 1_565 ? OW1 Co1 N2 87.78(13) . . ? O1 Co1 N2 99.87(13) . . ? N3 Co1 N2 91.13(13) . . ? N6 Co1 N2 88.42(13) 1_565 . ? OW1 Co1 N1 88.35(13) . . ? O1 Co1 N1 83.97(13) . . ? N3 Co1 N1 90.35(13) . . ? N6 Co1 N1 90.54(13) 1_565 . ? N2 Co1 N1 175.96(14) . . ? O1 Co2 O1 179.38(7) . 2_545 ? O1 Co2 O2 88.03(12) . 2_645 ? O1 Co2 O2 92.20(12) 2_545 2_645 ? O1 Co2 O3 92.72(12) . 1_455 ? O1 Co2 O3 87.07(12) 2_545 1_455 ? O2 Co2 O3 178.57(13) 2_645 1_455 ? O1 Co2 N5 95.03(13) . 2 ? O1 Co2 N5 85.53(13) 2_545 2 ? O2 Co2 N5 92.78(13) 2_645 2 ? O3 Co2 N5 85.93(13) 1_455 2 ? O1 Co2 N4 84.82(12) . . ? O1 Co2 N4 94.61(13) 2_545 . ? O2 Co2 N4 87.70(13) 2_645 . ? O3 Co2 N4 93.59(13) 1_455 . ? N5 Co2 N4 179.49(13) 2 . ? Co1 OW1 H13 119(3) . . ? Co1 OW1 H14 125(3) . . ? H13 OW1 H14 109.4(18) . . ? H15 OW2 H16 109.3(19) . . ? Co2 O1 Co2 106.01(13) . 2 ? Co2 O1 Co1 120.63(13) . . ? Co2 O1 Co1 119.70(13) 2 . ? Co2 O1 H1 104(4) . . ? Co2 O1 H1 97(4) 2 . ? Co1 O1 H1 105(4) . . ? C1 O2 Co2 130.9(3) . 2_655 ? C1 O3 Co2 131.4(3) . 1_655 ? C4 N1 C5 116.0(4) . . ? C4 N1 Co1 122.1(3) . . ? C5 N1 Co1 121.8(3) . . ? C7 N2 C12 116.0(4) . . ? C7 N2 Co1 121.2(3) . . ? C12 N2 Co1 122.7(3) . . ? C13 N3 N4 104.4(3) . . ? C13 N3 Co1 142.5(3) . . ? N4 N3 Co1 113.0(3) . . ? N5 N4 N3 109.5(3) . . ? N5 N4 Co2 118.4(3) . . ? N3 N4 Co2 128.3(3) . . ? N4 N5 N6 110.5(3) . . ? N4 N5 Co2 118.1(3) . 2_545 ? N6 N5 Co2 127.7(3) . 2_545 ? C13 N6 N5 104.2(3) . . ? C13 N6 Co1 142.3(3) . 1_545 ? N5 N6 Co1 113.5(3) . 1_545 ? C13 N7 H10 115(4) . . ? C13 N7 H9 121(5) . . ? H10 N7 H9 123(6) . . ? O3 C1 O2 127.1(4) . . ? O3 C1 C2 117.0(4) . . ? O2 C1 C2 115.9(4) . . ? C3 C2 C6 117.8(4) . . ? C3 C2 C1 121.5(4) . . ? C6 C2 C1 120.7(4) . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? N1 C4 C3 123.9(4) . . ? N1 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? N1 C5 C6 123.5(4) . . ? N1 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C2 119.5(4) . . ? C5 C6 H6 120.2 . . ? C2 C6 H6 120.2 . . ? N2 C7 C8 124.0(5) . . ? N2 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C9 C8 C7 119.3(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C11 117.8(4) . . ? C8 C9 C10 120.9(4) . . ? C11 C9 C10 121.3(4) . . ? O4 C10 O5 124.8(4) . . ? O4 C10 C9 118.1(4) . . ? O5 C10 C9 117.1(4) . . ? C9 C11 C12 119.6(5) . . ? C9 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N2 C12 C11 123.3(4) . . ? N2 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? N3 C13 N6 111.4(4) . . ? N3 C13 N7 124.9(4) . . ? N6 C13 N7 123.6(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.537 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.089