# 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_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wang Yaoyu' _publ_contact_author_email WYAOYU@NWU.EDU.CN loop_ _publ_author_name W.Yaoyu J.-C.Jin E.Kh.Lermontova J.-Q.Liu Q.-Z.Shi Y.-N.Zhang # Attachment '2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 710084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H12 N4 O6 S Zn' _chemical_formula_sum 'C13 H12 N4 O6 S Zn' _chemical_formula_weight 417.70 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.731(3) _cell_length_b 6.9651(18) _cell_length_c 19.709(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.721(4) _cell_angle_gamma 90.00 _cell_volume 1451.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2596 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6508 _exptl_absorpt_correction_T_max 0.7166 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 6876 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0554 _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 -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.20 _reflns_number_total 2596 _reflns_number_gt 2082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0600P)^2^+0.0100P] 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 2596 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _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 Zn1 Zn 0.84554(4) 0.82754(6) 0.175368(19) 0.02410(17) Uani 1 1 d . . . S1 S 1.06619(8) 0.50505(12) 0.16983(4) 0.0221(2) Uani 1 1 d . . . O6 O 0.7377(2) 1.0832(4) 0.18036(12) 0.0363(6) Uani 1 1 d . . . H6WB H 0.7718 1.1466 0.2134 0.054 Uiso 1 1 d R . . H6WA H 0.7085 1.1504 0.1471 0.054 Uiso 1 1 d R . . O4 O 0.9365(2) 0.5605(4) 0.17552(13) 0.0312(6) Uani 1 1 d . . . O5 O 1.0050(2) 0.9757(3) 0.15490(12) 0.0326(6) Uani 1 1 d . . . H5WA H 1.0650 0.9007 0.1640 0.049 Uiso 1 1 d R . . H5WB H 1.0243 1.0870 0.1663 0.049 Uiso 1 1 d R . . O3 O 1.1043(2) 0.3408(3) 0.21711(13) 0.0301(6) Uani 1 1 d . . . O2 O 1.0733(2) 0.4428(4) 0.09955(12) 0.0360(6) Uani 1 1 d . . . O1 O 1.1525(2) 0.6678(3) 0.18895(13) 0.0301(6) Uani 1 1 d . . . N1 N 0.6754(3) 0.6745(4) 0.18049(14) 0.0220(6) Uani 1 1 d . . . N2 N 0.7562(3) 0.8176(4) 0.06909(15) 0.0241(7) Uani 1 1 d . . . N3 N 0.2569(3) 0.6023(4) 0.03408(14) 0.0260(7) Uani 1 1 d . . . H3 H 0.2071 0.5548 0.0596 0.031 Uiso 1 1 calc R . . N4 N 0.3236(3) 0.7182(4) -0.05903(15) 0.0284(7) Uani 1 1 d . . . C1 C 0.6424(3) 0.5917(5) 0.23538(18) 0.0275(8) Uani 1 1 d . . . H1 H 0.7022 0.5824 0.2753 0.017(8) Uiso 1 1 d R . . C2 C 0.5222(3) 0.5186(5) 0.23606(17) 0.0290(8) Uani 1 1 d . . . H2 H 0.5028 0.4603 0.2754 0.042(11) Uiso 1 1 d R . . C3 C 0.4326(3) 0.5333(5) 0.17785(18) 0.0270(8) Uani 1 1 d . . . H3A H 0.3515 0.4857 0.1774 0.030(10) Uiso 1 1 d R . . C4 C 0.4644(3) 0.6204(5) 0.11887(17) 0.0218(7) Uani 1 1 d . . . C5 C 0.3828(3) 0.6444(5) 0.05370(17) 0.0226(7) Uani 1 1 d . . . C6 C 0.2271(3) 0.6492(5) -0.03198(18) 0.0283(8) Uani 1 1 d . . . H6 H 0.1461 0.6351 -0.0571 0.035(11) Uiso 1 1 d R . . C7 C 0.4237(3) 0.7163(5) -0.00364(17) 0.0232(8) Uani 1 1 d . . . C8 C 0.5511(3) 0.7756(5) -0.00253(17) 0.0230(7) Uani 1 1 d . . . C9 C 0.6013(3) 0.8448(5) -0.05949(18) 0.0272(8) Uani 1 1 d . . . H9 H 0.5500 0.8572 -0.1023 0.051(13) Uiso 1 1 d R . . C10 C 0.7267(4) 0.8923(5) -0.05090(18) 0.0316(9) Uani 1 1 d . . . H10 H 0.7616 0.9344 -0.0884 0.018(8) Uiso 1 1 d R . . C11 C 0.8009(3) 0.8788(5) 0.01339(18) 0.0294(8) Uani 1 1 d . . . H11 H 0.8855 0.9138 0.0182 0.029(10) Uiso 1 1 d R . . C12 C 0.6333(3) 0.7634(5) 0.06135(16) 0.0209(7) Uani 1 1 d . . . C13 C 0.5895(3) 0.6851(4) 0.12193(17) 0.0220(8) 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 Zn1 0.0202(3) 0.0303(3) 0.0204(3) 0.00078(16) -0.00060(17) -0.00058(16) S1 0.0197(4) 0.0293(5) 0.0161(4) -0.0001(3) -0.0001(3) 0.0016(3) O6 0.0474(17) 0.0372(15) 0.0205(13) 0.0013(11) -0.0049(12) 0.0097(13) O4 0.0220(13) 0.0312(14) 0.0396(15) -0.0004(11) 0.0024(11) 0.0030(11) O5 0.0306(15) 0.0302(14) 0.0356(15) 0.0007(11) 0.0015(12) -0.0034(11) O3 0.0348(14) 0.0265(13) 0.0259(14) 0.0008(10) -0.0039(12) 0.0033(10) O2 0.0404(16) 0.0486(17) 0.0196(13) -0.0069(11) 0.0070(11) -0.0065(13) O1 0.0251(13) 0.0335(14) 0.0297(14) -0.0008(11) -0.0012(11) -0.0037(10) N1 0.0190(15) 0.0305(17) 0.0159(15) 0.0011(11) 0.0017(12) 0.0009(12) N2 0.0218(16) 0.0278(16) 0.0228(16) -0.0016(11) 0.0038(13) -0.0005(12) N3 0.0193(15) 0.0336(17) 0.0241(16) 0.0024(12) 0.0009(12) -0.0035(12) N4 0.0276(16) 0.0332(17) 0.0216(16) -0.0009(12) -0.0036(13) 0.0011(13) C1 0.0276(19) 0.034(2) 0.0193(18) 0.0039(14) -0.0020(15) 0.0006(16) C2 0.033(2) 0.036(2) 0.0186(19) 0.0061(15) 0.0053(16) -0.0019(16) C3 0.0190(18) 0.034(2) 0.028(2) -0.0005(15) 0.0038(14) -0.0021(15) C4 0.0206(18) 0.0242(17) 0.0198(17) -0.0007(13) 0.0008(14) 0.0028(14) C5 0.0224(18) 0.0249(18) 0.0190(18) -0.0012(14) -0.0011(14) 0.0018(14) C6 0.0236(19) 0.032(2) 0.025(2) -0.0014(15) -0.0079(16) 0.0026(15) C7 0.0246(18) 0.0218(18) 0.0208(18) -0.0001(13) -0.0031(15) 0.0018(14) C8 0.0269(18) 0.0208(17) 0.0202(18) -0.0021(13) 0.0011(15) 0.0013(14) C9 0.033(2) 0.029(2) 0.0199(19) 0.0007(14) 0.0035(16) 0.0003(15) C10 0.040(2) 0.033(2) 0.025(2) 0.0015(15) 0.0144(18) -0.0033(17) C11 0.025(2) 0.039(2) 0.026(2) -0.0017(16) 0.0105(16) -0.0072(16) C12 0.0212(18) 0.0244(17) 0.0171(17) -0.0006(13) 0.0028(14) 0.0004(14) C13 0.0203(18) 0.0229(18) 0.0218(18) -0.0001(13) 0.0010(15) 0.0010(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 Zn1 O5 2.095(2) . ? Zn1 O3 2.099(2) 2_755 ? Zn1 O4 2.101(3) . ? Zn1 N1 2.131(3) . ? Zn1 O6 2.135(3) . ? Zn1 N2 2.152(3) . ? S1 O2 1.466(3) . ? S1 O4 1.466(2) . ? S1 O1 1.472(2) . ? S1 O3 1.489(2) . ? O6 H6WB 0.8207 . ? O6 H6WA 0.8224 . ? O5 H5WA 0.8248 . ? O5 H5WB 0.8242 . ? O3 Zn1 2.099(2) 2_745 ? N1 C1 1.326(4) . ? N1 C13 1.352(4) . ? N2 C11 1.339(5) . ? N2 C12 1.356(4) . ? N3 C6 1.328(4) . ? N3 C5 1.373(4) . ? N3 H3 0.8600 . ? N4 C6 1.332(5) . ? N4 C7 1.396(4) . ? C1 C2 1.389(5) . ? C1 H1 0.9301 . ? C2 C3 1.371(5) . ? C2 H2 0.9301 . ? C3 C4 1.404(5) . ? C3 H3A 0.9300 . ? C4 C13 1.407(5) . ? C4 C5 1.437(4) . ? C5 C7 1.374(5) . ? C6 H6 0.9300 . ? C7 C8 1.425(5) . ? C8 C9 1.410(5) . ? C8 C12 1.412(5) . ? C9 C10 1.367(5) . ? C9 H9 0.9301 . ? C10 C11 1.381(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.461(4) . ? 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 Zn1 O3 95.40(10) . 2_755 ? O5 Zn1 O4 92.39(10) . . ? O3 Zn1 O4 89.86(9) 2_755 . ? O5 Zn1 N1 171.74(10) . . ? O3 Zn1 N1 92.86(10) 2_755 . ? O4 Zn1 N1 87.64(10) . . ? O5 Zn1 O6 93.71(10) . . ? O3 Zn1 O6 88.02(9) 2_755 . ? O4 Zn1 O6 173.70(10) . . ? N1 Zn1 O6 86.54(10) . . ? O5 Zn1 N2 94.15(10) . . ? O3 Zn1 N2 168.61(10) 2_755 . ? O4 Zn1 N2 95.93(10) . . ? N1 Zn1 N2 77.63(10) . . ? O6 Zn1 N2 85.18(9) . . ? O2 S1 O4 110.57(15) . . ? O2 S1 O1 109.80(15) . . ? O4 S1 O1 109.99(15) . . ? O2 S1 O3 108.17(15) . . ? O4 S1 O3 108.55(15) . . ? O1 S1 O3 109.72(14) . . ? Zn1 O6 H6WB 108.2 . . ? Zn1 O6 H6WA 125.1 . . ? H6WB O6 H6WA 112.7 . . ? S1 O4 Zn1 132.83(16) . . ? Zn1 O5 H5WA 106.2 . . ? Zn1 O5 H5WB 125.9 . . ? H5WA O5 H5WB 112.7 . . ? S1 O3 Zn1 131.49(14) . 2_745 ? C1 N1 C13 118.8(3) . . ? C1 N1 Zn1 127.3(2) . . ? C13 N1 Zn1 113.5(2) . . ? C11 N2 C12 118.2(3) . . ? C11 N2 Zn1 128.7(2) . . ? C12 N2 Zn1 112.5(2) . . ? C6 N3 C5 106.7(3) . . ? C6 N3 H3 126.7 . . ? C5 N3 H3 126.7 . . ? C6 N4 C7 103.4(3) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.1(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C13 117.8(3) . . ? C3 C4 C5 126.4(3) . . ? C13 C4 C5 115.7(3) . . ? N3 C5 C7 106.4(3) . . ? N3 C5 C4 130.5(3) . . ? C7 C5 C4 123.1(3) . . ? N3 C6 N4 113.9(3) . . ? N3 C6 H6 123.1 . . ? N4 C6 H6 123.0 . . ? C5 C7 N4 109.6(3) . . ? C5 C7 C8 122.1(3) . . ? N4 C7 C8 128.2(3) . . ? C9 C8 C12 117.8(3) . . ? C9 C8 C7 125.6(3) . . ? C12 C8 C7 116.7(3) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 120.0(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 120.2 . . ? N2 C11 C10 122.9(3) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.5 . . ? N2 C12 C8 122.2(3) . . ? N2 C12 C13 117.0(3) . . ? C8 C12 C13 120.8(3) . . ? N1 C13 C4 121.8(3) . . ? N1 C13 C12 116.8(3) . . ? C4 C13 C12 121.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.682 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.148 #===END # Attachment '3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 710085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H12 Mn N4 O6 S' _chemical_formula_sum 'C13 H12 Mn N4 O6 S' _chemical_formula_weight 407.27 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.916(4) _cell_length_b 7.017(2) _cell_length_c 19.690(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.353(7) _cell_angle_gamma 90.00 _cell_volume 1488.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2672 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 25.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7494 _exptl_absorpt_correction_T_max 0.8977 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 7330 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.1612 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.19 _reflns_number_total 2672 _reflns_number_gt 1220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0100P)^2^+0.2200P] 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 2672 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _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 0.34885(7) 0.82387(12) 0.17471(4) 0.0340(2) Uani 1 1 d . . . S1 S 0.56891(12) 0.5001(2) 0.16741(6) 0.0322(4) Uani 1 1 d . . . O1 O 0.2407(3) 1.0837(4) 0.18054(15) 0.0515(11) Uani 1 1 d . . . H1B H 0.2101 1.1595 0.1497 0.077 Uiso 1 1 d R . . H1C H 0.2838 1.1444 0.2118 0.077 Uiso 1 1 d R . . O2 O 0.5124(3) 0.9758(5) 0.15092(14) 0.0472(10) Uani 1 1 d . . . H2B H 0.5468 1.0808 0.1597 0.071 Uiso 1 1 d R . . H2C H 0.5684 0.8912 0.1619 0.071 Uiso 1 1 d R . . O3 O 0.4399(3) 0.5544(5) 0.17257(15) 0.0423(10) Uani 1 1 d . . . O4 O 0.5754(3) 0.4377(5) 0.09748(14) 0.0450(11) Uani 1 1 d . . . O5 O 0.6527(3) 0.6637(5) 0.18649(14) 0.0379(9) Uani 1 1 d . . . O6 O 0.6063(3) 0.3385(5) 0.21489(14) 0.0366(9) Uani 1 1 d . . . N1 N 0.1702(3) 0.6663(6) 0.17652(19) 0.0307(10) Uani 1 1 d . . . N2 N 0.2490(4) 0.8133(6) 0.06481(18) 0.0313(11) Uani 1 1 d . . . N3 N -0.2430(3) 0.6036(5) 0.03263(18) 0.0316(12) Uani 1 1 d . . . H3A H -0.2923 0.5562 0.0581 0.038 Uiso 1 1 d R . . N4 N -0.1774(4) 0.7187(6) -0.05999(18) 0.0353(12) Uani 1 1 d . . . C1 C 0.1372(5) 0.5847(7) 0.2312(2) 0.0357(15) Uani 1 1 d . . . H1A H 0.1962 0.5730 0.2708 0.043 Uiso 1 1 calc R . . C2 C 0.0180(5) 0.5155(8) 0.2322(2) 0.0386(14) Uani 1 1 d . . . H2A H -0.0010 0.4579 0.2717 0.046 Uiso 1 1 calc R . . C3 C -0.0700(5) 0.5319(7) 0.1759(2) 0.0383(15) Uani 1 1 d . . . H3 H -0.1499 0.4865 0.1763 0.046 Uiso 1 1 calc R . . C4 C -0.0387(5) 0.6196(7) 0.1158(2) 0.0281(13) Uani 1 1 d . . . C5 C -0.1181(5) 0.6449(7) 0.0530(2) 0.0313(13) Uani 1 1 d . . . C6 C -0.2725(4) 0.6506(7) -0.0335(2) 0.0349(14) Uani 1 1 d . . . H6 H -0.3519 0.6371 -0.0585 0.042 Uiso 1 1 calc R . . C7 C -0.0812(5) 0.7161(7) -0.0066(2) 0.0296(13) Uani 1 1 d . . . C8 C 0.0451(4) 0.7758(6) -0.0044(2) 0.0271(13) Uani 1 1 d . . . C9 C 0.0917(5) 0.8453(7) -0.0625(2) 0.0333(13) Uani 1 1 d . . . H9 H 0.0403 0.8583 -0.1048 0.040 Uiso 1 1 calc R . . C10 C 0.2158(5) 0.8934(7) -0.0545(2) 0.0403(16) Uani 1 1 d . . . H10 H 0.2494 0.9376 -0.0921 0.048 Uiso 1 1 calc R . . C11 C 0.2905(5) 0.8758(7) 0.0093(2) 0.0379(15) Uani 1 1 d . . . H11 H 0.3737 0.9097 0.0133 0.046 Uiso 1 1 calc R . . C12 C 0.1273(4) 0.7593(7) 0.0572(2) 0.0276(13) Uani 1 1 d . . . C13 C 0.0853(5) 0.6821(7) 0.1187(2) 0.0282(12) 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 0.0302(5) 0.0366(6) 0.0345(4) -0.0009(4) 0.0033(4) -0.0002(5) S1 0.0287(8) 0.0351(10) 0.0321(7) -0.0020(7) 0.0032(6) 0.0017(8) O1 0.062(3) 0.047(3) 0.040(2) 0.0058(18) -0.007(2) 0.017(2) O2 0.038(2) 0.033(2) 0.071(2) 0.008(2) 0.013(2) -0.003(2) O3 0.027(2) 0.041(3) 0.058(2) 0.0010(18) 0.0054(19) 0.0064(19) O4 0.050(3) 0.062(3) 0.0245(19) -0.0062(18) 0.0106(19) -0.011(2) O5 0.031(2) 0.034(2) 0.046(2) 0.0013(19) -0.0029(17) -0.008(2) O6 0.042(2) 0.031(2) 0.0334(18) 0.0078(18) -0.0040(17) 0.006(2) N1 0.032(3) 0.030(3) 0.029(2) 0.001(2) 0.002(2) 0.003(2) N2 0.030(3) 0.032(3) 0.033(2) -0.003(2) 0.008(2) 0.001(2) N3 0.024(3) 0.041(3) 0.031(3) -0.001(2) 0.007(2) -0.006(2) N4 0.036(3) 0.034(3) 0.034(3) 0.003(2) -0.001(2) 0.004(2) C1 0.044(4) 0.035(4) 0.024(3) 0.004(3) -0.006(3) 0.001(3) C2 0.040(4) 0.041(4) 0.036(3) 0.009(3) 0.008(3) -0.008(3) C3 0.038(3) 0.046(4) 0.033(3) -0.002(3) 0.012(3) 0.002(3) C4 0.028(3) 0.021(3) 0.034(3) -0.004(2) 0.002(3) 0.003(3) C5 0.026(3) 0.032(4) 0.036(3) -0.005(3) 0.005(3) -0.002(3) C6 0.028(3) 0.036(4) 0.039(3) 0.000(3) 0.000(3) 0.005(3) C7 0.023(3) 0.029(4) 0.036(3) 0.003(3) 0.001(3) 0.005(3) C8 0.024(3) 0.022(4) 0.034(3) 0.000(2) 0.002(3) 0.002(3) C9 0.040(4) 0.024(3) 0.035(3) -0.002(3) 0.004(3) 0.001(3) C10 0.055(4) 0.042(4) 0.029(3) -0.003(3) 0.021(3) -0.002(3) C11 0.035(4) 0.042(4) 0.040(3) 0.005(3) 0.015(3) -0.003(3) C12 0.028(3) 0.026(4) 0.028(3) -0.001(2) 0.003(3) 0.002(3) C13 0.033(3) 0.022(3) 0.029(3) -0.002(3) 0.004(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.140(3) . ? Mn1 O6 2.152(3) 2_655 ? Mn1 O1 2.185(3) . ? Mn1 O2 2.194(3) . ? Mn1 N1 2.247(4) . ? Mn1 N2 2.261(4) . ? S1 O4 1.457(3) . ? S1 O5 1.478(3) . ? S1 O3 1.478(3) . ? S1 O6 1.484(3) . ? O1 H1B 0.8351 . ? O1 H1C 0.8289 . ? O2 H2B 0.8326 . ? O2 H2C 0.8546 . ? O6 Mn1 2.152(3) 2_645 ? N1 C1 1.320(5) . ? N1 C13 1.351(5) . ? N2 C11 1.325(5) . ? N2 C12 1.365(5) . ? N3 C6 1.330(5) . ? N3 C5 1.388(5) . ? N3 H3A 0.8600 . ? N4 C6 1.325(5) . ? N4 C7 1.359(5) . ? C1 C2 1.393(6) . ? C1 H1A 0.9300 . ? C2 C3 1.348(6) . ? C2 H2A 0.9300 . ? C3 C4 1.424(6) . ? C3 H3 0.9300 . ? C4 C5 1.401(6) . ? C4 C13 1.415(6) . ? C5 C7 1.394(6) . ? C6 H6 0.9300 . ? C7 C8 1.435(6) . ? C8 C12 1.391(6) . ? C8 C9 1.412(6) . ? C9 C10 1.380(6) . ? C9 H9 0.9300 . ? C10 C11 1.388(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.467(6) . ? 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 Mn1 O6 91.84(12) . 2_655 ? O3 Mn1 O1 174.25(13) . . ? O6 Mn1 O1 86.74(12) 2_655 . ? O3 Mn1 O2 91.63(13) . . ? O6 Mn1 O2 97.66(12) 2_655 . ? O1 Mn1 O2 94.08(13) . . ? O3 Mn1 N1 88.43(14) . . ? O6 Mn1 N1 93.61(13) 2_655 . ? O1 Mn1 N1 86.11(14) . . ? O2 Mn1 N1 168.73(13) . . ? O3 Mn1 N2 96.05(13) . . ? O6 Mn1 N2 164.53(13) 2_655 . ? O1 Mn1 N2 84.09(13) . . ? O2 Mn1 N2 95.41(13) . . ? N1 Mn1 N2 73.39(14) . . ? O4 S1 O5 110.51(18) . . ? O4 S1 O3 109.6(2) . . ? O5 S1 O3 109.83(19) . . ? O4 S1 O6 108.4(2) . . ? O5 S1 O6 109.7(2) . . ? O3 S1 O6 108.77(19) . . ? Mn1 O1 H1B 130.5 . . ? Mn1 O1 H1C 102.8 . . ? H1B O1 H1C 108.9 . . ? Mn1 O2 H2B 137.8 . . ? Mn1 O2 H2C 100.5 . . ? H2B O2 H2C 106.3 . . ? S1 O3 Mn1 132.9(2) . . ? S1 O6 Mn1 131.9(2) . 2_645 ? C1 N1 C13 118.8(4) . . ? C1 N1 Mn1 125.4(3) . . ? C13 N1 Mn1 115.1(3) . . ? C11 N2 C12 117.3(4) . . ? C11 N2 Mn1 127.1(3) . . ? C12 N2 Mn1 115.1(3) . . ? C6 N3 C5 107.6(4) . . ? C6 N3 H3A 126.2 . . ? C5 N3 H3A 126.2 . . ? C6 N4 C7 104.3(4) . . ? N1 C1 C2 122.8(5) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 120.1(5) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C13 116.5(4) . . ? C5 C4 C3 126.2(5) . . ? C13 C4 C3 117.2(5) . . ? N3 C5 C7 103.7(4) . . ? N3 C5 C4 131.8(4) . . ? C7 C5 C4 124.5(5) . . ? N4 C6 N3 113.2(4) . . ? N4 C6 H6 123.4 . . ? N3 C6 H6 123.4 . . ? N4 C7 C5 111.3(4) . . ? N4 C7 C8 129.6(4) . . ? C5 C7 C8 119.1(5) . . ? C12 C8 C9 117.9(4) . . ? C12 C8 C7 118.9(4) . . ? C9 C8 C7 123.1(5) . . ? C10 C9 C8 118.0(5) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? N2 C11 C10 123.2(5) . . ? N2 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? N2 C12 C8 123.5(4) . . ? N2 C12 C13 116.1(4) . . ? C8 C12 C13 120.4(4) . . ? N1 C13 C4 122.0(4) . . ? N1 C13 C12 117.6(4) . . ? C4 C13 C12 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.516 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.095 # Attachment '4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 710086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 N8 O12 S2 Zn2, 2(H2 O)' _chemical_formula_sum 'C26 H28 N8 O14 S2 Zn2' _chemical_formula_weight 871.42 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.310(5) _cell_length_b 9.031(4) _cell_length_c 17.003(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.960(9) _cell_angle_gamma 90.00 _cell_volume 1563.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2772 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.09 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5987 _exptl_absorpt_correction_T_max 0.8080 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 7402 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.09 _reflns_number_total 2772 _reflns_number_gt 2098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0484P)^2^+0.3488P] 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 2772 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 Zn1 Zn 0.68679(4) 0.31979(4) 0.04023(2) 0.02979(17) Uani 1 1 d . . . S1 S 0.46717(10) 0.39830(9) -0.11264(5) 0.0279(2) Uani 1 1 d . . . N1 N 0.7575(3) 0.0969(3) 0.03288(16) 0.0272(7) Uani 1 1 d . . . N2 N 1.1448(3) -0.2047(3) 0.13930(17) 0.0366(8) Uani 1 1 d . . . N3 N 1.2456(3) -0.0105(3) 0.20290(16) 0.0367(8) Uani 1 1 d . . . H3 H 1.3054 0.0406 0.2317 0.044 Uiso 1 1 calc R . . N4 N 0.8731(3) 0.3249(3) 0.11697(16) 0.0306(7) Uani 1 1 d . . . O1 O 0.6338(3) 0.5292(2) 0.07432(14) 0.0359(6) Uani 1 1 d . . . O2 O 0.7955(3) 0.4361(3) -0.04044(13) 0.0379(7) Uani 1 1 d . . . H2B H 0.8302 0.3732 -0.0688 0.057 Uiso 1 1 d R . . H2C H 0.7260 0.4678 -0.0693 0.057 Uiso 1 1 d R . . O3 O 0.5696(3) 0.2359(3) 0.11972(16) 0.0560(8) Uani 1 1 d . . . H3B H 0.5226 0.2973 0.1372 0.084 Uiso 1 1 d R . . H3C H 0.5668 0.1530 0.1439 0.084 Uiso 1 1 d R . . O4 O 0.5391(3) 0.2896(2) -0.05771(13) 0.0325(6) Uani 1 1 d . . . O5 O 0.4056(3) 0.3217(2) -0.18493(14) 0.0428(7) Uani 1 1 d . . . O6 O 0.5594(3) 0.5101(2) -0.13554(13) 0.0341(6) Uani 1 1 d . . . C1 C 0.6922(4) -0.0158(4) -0.0063(2) 0.0342(9) Uani 1 1 d . . . H1 H 0.6100 0.0019 -0.0360 0.041 Uiso 1 1 calc R . . C2 C 0.7432(4) -0.1578(4) -0.0041(2) 0.0357(9) Uani 1 1 d . . . H2A H 0.6951 -0.2343 -0.0312 0.043 Uiso 1 1 calc R . . C3 C 0.8658(4) -0.1851(4) 0.0386(2) 0.0345(9) Uani 1 1 d . . . H3A H 0.9017 -0.2796 0.0397 0.041 Uiso 1 1 calc R . . C4 C 0.9360(4) -0.0688(3) 0.08059(18) 0.0280(8) Uani 1 1 d . . . C5 C 1.0641(4) -0.0810(3) 0.12649(19) 0.0290(8) Uani 1 1 d . . . C6 C 1.2507(4) -0.1548(4) 0.1853(2) 0.0403(10) Uani 1 1 d . . . H6 H 1.3225 -0.2144 0.2039 0.048 Uiso 1 1 calc R . . C7 C 1.1258(4) 0.0397(4) 0.16579(19) 0.0306(9) Uani 1 1 d . . . C8 C 1.0675(4) 0.1830(3) 0.16536(19) 0.0272(8) Uani 1 1 d . . . C9 C 1.1246(4) 0.3081(4) 0.2049(2) 0.0352(9) Uani 1 1 d . . . H9 H 1.2077 0.3028 0.2353 0.042 Uiso 1 1 calc R . . C10 C 1.0566(4) 0.4383(4) 0.1981(2) 0.0389(10) Uani 1 1 d . . . H10 H 1.0939 0.5238 0.2224 0.047 Uiso 1 1 calc R . . C11 C 0.9306(4) 0.4415(4) 0.1543(2) 0.0329(9) Uani 1 1 d . . . H11 H 0.8845 0.5304 0.1511 0.040 Uiso 1 1 calc R . . C12 C 0.9407(4) 0.1953(3) 0.12122(18) 0.0277(8) Uani 1 1 d . . . C13 C 0.8759(4) 0.0704(3) 0.07704(18) 0.0250(8) Uani 1 1 d . . . O7 O 0.5897(4) 0.9871(3) 0.20153(16) 0.0710(11) Uani 1 1 d . . . H7C H 0.5863 0.9893 0.2513 0.106 Uiso 1 1 d R . . H7B H 0.5906 0.8976 0.1859 0.106 Uiso 1 1 d 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 Zn1 0.0292(3) 0.0299(2) 0.0301(2) 0.00170(16) 0.00435(19) 0.00615(19) S1 0.0306(6) 0.0263(4) 0.0255(4) -0.0013(3) 0.0009(4) 0.0061(4) N1 0.0214(19) 0.0317(15) 0.0285(14) 0.0024(12) 0.0046(13) 0.0021(14) N2 0.039(2) 0.0378(16) 0.0325(16) 0.0025(13) 0.0043(15) 0.0131(16) N3 0.030(2) 0.0408(16) 0.0359(16) -0.0003(14) -0.0043(14) 0.0009(16) N4 0.035(2) 0.0271(14) 0.0300(15) 0.0010(12) 0.0063(14) 0.0069(14) O1 0.0326(18) 0.0283(11) 0.0501(15) -0.0005(11) 0.0169(13) 0.0051(12) O2 0.0375(18) 0.0409(14) 0.0357(13) -0.0011(11) 0.0069(12) 0.0077(13) O3 0.075(2) 0.0333(13) 0.0711(19) 0.0164(14) 0.0460(17) 0.0177(15) O4 0.0321(17) 0.0296(11) 0.0340(13) 0.0024(10) -0.0001(11) 0.0029(11) O5 0.051(2) 0.0415(14) 0.0311(13) -0.0090(11) -0.0091(13) 0.0074(14) O6 0.0363(18) 0.0318(12) 0.0362(13) 0.0064(11) 0.0118(12) 0.0063(12) C1 0.027(2) 0.0393(19) 0.0363(19) -0.0056(17) 0.0038(16) -0.0017(18) C2 0.039(3) 0.0319(17) 0.036(2) -0.0059(16) 0.0042(18) -0.0056(19) C3 0.041(3) 0.0282(18) 0.0349(19) 0.0012(15) 0.0080(18) 0.0012(18) C4 0.033(2) 0.0295(17) 0.0231(16) 0.0023(14) 0.0092(16) 0.0031(17) C5 0.031(2) 0.0327(18) 0.0240(17) 0.0016(14) 0.0070(15) 0.0077(17) C6 0.039(3) 0.047(2) 0.033(2) 0.0028(17) 0.0021(19) 0.019(2) C7 0.029(2) 0.0386(18) 0.0247(17) 0.0028(15) 0.0065(16) 0.0078(18) C8 0.028(2) 0.0304(17) 0.0233(17) 0.0018(14) 0.0055(15) 0.0007(17) C9 0.029(3) 0.040(2) 0.035(2) -0.0024(16) 0.0009(17) -0.0024(19) C10 0.049(3) 0.0343(19) 0.034(2) -0.0066(16) 0.0089(19) -0.005(2) C11 0.036(3) 0.0298(17) 0.0335(19) -0.0006(15) 0.0073(17) 0.0036(18) C12 0.029(2) 0.0319(17) 0.0230(17) 0.0018(14) 0.0059(15) 0.0017(17) C13 0.023(2) 0.0280(16) 0.0246(16) 0.0025(14) 0.0065(15) 0.0024(16) O7 0.138(4) 0.0353(14) 0.0450(16) 0.0071(13) 0.0319(19) 0.0157(19) _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 Zn1 O1 2.076(2) . ? Zn1 O3 2.090(3) . ? Zn1 O4 2.092(2) . ? Zn1 N4 2.148(3) . ? Zn1 N1 2.151(3) . ? Zn1 O2 2.173(3) . ? S1 O1 1.465(3) 3_665 ? S1 O5 1.466(2) . ? S1 O4 1.473(2) . ? S1 O6 1.480(3) . ? N1 C1 1.339(4) . ? N1 C13 1.351(4) . ? N2 C6 1.320(5) . ? N2 C5 1.390(4) . ? N3 C6 1.340(4) . ? N3 C7 1.373(4) . ? N3 H3 0.8600 . ? N4 C11 1.321(4) . ? N4 C12 1.359(4) . ? O1 S1 1.465(3) 3_665 ? O2 H2B 0.8589 . ? O2 H2C 0.8518 . ? O3 H3B 0.8212 . ? O3 H3C 0.8576 . ? C1 C2 1.384(5) . ? C1 H1 0.9300 . ? C2 C3 1.378(5) . ? C2 H2A 0.9300 . ? C3 C4 1.406(5) . ? C3 H3A 0.9300 . ? C4 C13 1.399(4) . ? C4 C5 1.429(5) . ? C5 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.427(5) . ? C8 C9 1.397(4) . ? C8 C12 1.407(5) . ? C9 C10 1.365(5) . ? C9 H9 0.9300 . ? C10 C11 1.394(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.458(4) . ? O7 H7C 0.8518 . ? O7 H7B 0.8520 . ? 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 Zn1 O3 86.89(10) . . ? O1 Zn1 O4 98.65(9) . . ? O3 Zn1 O4 92.60(12) . . ? O1 Zn1 N4 93.45(10) . . ? O3 Zn1 N4 99.63(12) . . ? O4 Zn1 N4 163.24(11) . . ? O1 Zn1 N1 167.16(10) . . ? O3 Zn1 N1 86.21(11) . . ? O4 Zn1 N1 92.47(10) . . ? N4 Zn1 N1 77.08(10) . . ? O1 Zn1 O2 85.40(10) . . ? O3 Zn1 O2 172.07(10) . . ? O4 Zn1 O2 86.75(10) . . ? N4 Zn1 O2 82.69(11) . . ? N1 Zn1 O2 101.72(11) . . ? O1 S1 O5 109.81(17) 3_665 . ? O1 S1 O4 109.76(15) 3_665 . ? O5 S1 O4 109.07(14) . . ? O1 S1 O6 110.02(14) 3_665 . ? O5 S1 O6 108.26(16) . . ? O4 S1 O6 109.90(15) . . ? C1 N1 C13 118.9(3) . . ? C1 N1 Zn1 126.2(2) . . ? C13 N1 Zn1 114.7(2) . . ? C6 N2 C5 103.8(3) . . ? C6 N3 C7 106.4(3) . . ? C6 N3 H3 126.8 . . ? C7 N3 H3 126.8 . . ? C11 N4 C12 118.3(3) . . ? C11 N4 Zn1 126.9(2) . . ? C12 N4 Zn1 114.6(2) . . ? S1 O1 Zn1 140.09(16) 3_665 . ? Zn1 O2 H2B 109.7 . . ? Zn1 O2 H2C 93.2 . . ? H2B O2 H2C 106.6 . . ? Zn1 O3 H3B 115.0 . . ? Zn1 O3 H3C 133.9 . . ? H3B O3 H3C 110.5 . . ? S1 O4 Zn1 130.56(14) . . ? N1 C1 C2 122.0(3) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C13 C4 C3 117.4(3) . . ? C13 C4 C5 117.3(3) . . ? C3 C4 C5 125.3(3) . . ? C7 C5 N2 109.8(3) . . ? C7 C5 C4 121.4(3) . . ? N2 C5 C4 128.9(3) . . ? N2 C6 N3 114.0(3) . . ? N2 C6 H6 123.0 . . ? N3 C6 H6 123.0 . . ? N3 C7 C5 106.0(3) . . ? N3 C7 C8 130.5(3) . . ? C5 C7 C8 123.4(3) . . ? C9 C8 C12 118.7(3) . . ? C9 C8 C7 125.8(3) . . ? C12 C8 C7 115.5(3) . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N4 C11 C10 123.4(3) . . ? N4 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? N4 C12 C8 121.5(3) . . ? N4 C12 C13 116.7(3) . . ? C8 C12 C13 121.8(3) . . ? N1 C13 C4 122.6(3) . . ? N1 C13 C12 116.8(3) . . ? C4 C13 C12 120.6(3) . . ? H7C O7 H7B 109.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 N1 C1 132.4(5) . . . . ? O3 Zn1 N1 C1 74.8(3) . . . . ? O4 Zn1 N1 C1 -17.6(3) . . . . ? N4 Zn1 N1 C1 175.6(3) . . . . ? O2 Zn1 N1 C1 -104.8(3) . . . . ? O1 Zn1 N1 C13 -43.0(6) . . . . ? O3 Zn1 N1 C13 -100.7(2) . . . . ? O4 Zn1 N1 C13 166.9(2) . . . . ? N4 Zn1 N1 C13 0.1(2) . . . . ? O2 Zn1 N1 C13 79.7(2) . . . . ? O1 Zn1 N4 C11 -12.7(3) . . . . ? O3 Zn1 N4 C11 -100.2(3) . . . . ? O4 Zn1 N4 C11 123.5(4) . . . . ? N1 Zn1 N4 C11 176.0(3) . . . . ? O2 Zn1 N4 C11 72.2(3) . . . . ? O1 Zn1 N4 C12 172.8(3) . . . . ? O3 Zn1 N4 C12 85.3(3) . . . . ? O4 Zn1 N4 C12 -51.0(5) . . . . ? N1 Zn1 N4 C12 1.5(2) . . . . ? O2 Zn1 N4 C12 -102.3(3) . . . . ? O3 Zn1 O1 S1 -18.9(3) . . . 3_665 ? O4 Zn1 O1 S1 73.3(2) . . . 3_665 ? N4 Zn1 O1 S1 -118.3(2) . . . 3_665 ? N1 Zn1 O1 S1 -76.4(6) . . . 3_665 ? O2 Zn1 O1 S1 159.3(2) . . . 3_665 ? O1 S1 O4 Zn1 -77.7(2) 3_665 . . . ? O5 S1 O4 Zn1 162.0(2) . . . . ? O6 S1 O4 Zn1 43.5(2) . . . . ? O1 Zn1 O4 S1 29.1(2) . . . . ? O3 Zn1 O4 S1 116.4(2) . . . . ? N4 Zn1 O4 S1 -106.6(3) . . . . ? N1 Zn1 O4 S1 -157.3(2) . . . . ? O2 Zn1 O4 S1 -55.7(2) . . . . ? C13 N1 C1 C2 -1.1(5) . . . . ? Zn1 N1 C1 C2 -176.4(3) . . . . ? N1 C1 C2 C3 -1.0(6) . . . . ? C1 C2 C3 C4 1.3(6) . . . . ? C2 C3 C4 C13 0.5(5) . . . . ? C2 C3 C4 C5 -179.4(4) . . . . ? C6 N2 C5 C7 0.1(4) . . . . ? C6 N2 C5 C4 179.8(4) . . . . ? C13 C4 C5 C7 0.1(5) . . . . ? C3 C4 C5 C7 179.9(4) . . . . ? C13 C4 C5 N2 -179.6(3) . . . . ? C3 C4 C5 N2 0.2(6) . . . . ? C5 N2 C6 N3 -0.3(4) . . . . ? C7 N3 C6 N2 0.4(5) . . . . ? C6 N3 C7 C5 -0.3(4) . . . . ? C6 N3 C7 C8 178.7(4) . . . . ? N2 C5 C7 N3 0.1(4) . . . . ? C4 C5 C7 N3 -179.6(3) . . . . ? N2 C5 C7 C8 -179.0(3) . . . . ? C4 C5 C7 C8 1.3(5) . . . . ? N3 C7 C8 C9 0.3(6) . . . . ? C5 C7 C8 C9 179.1(4) . . . . ? N3 C7 C8 C12 -179.2(3) . . . . ? C5 C7 C8 C12 -0.4(5) . . . . ? C12 C8 C9 C10 -1.2(5) . . . . ? C7 C8 C9 C10 179.4(4) . . . . ? C8 C9 C10 C11 2.2(6) . . . . ? C12 N4 C11 C10 -0.3(6) . . . . ? Zn1 N4 C11 C10 -174.7(3) . . . . ? C9 C10 C11 N4 -1.5(6) . . . . ? C11 N4 C12 C8 1.4(5) . . . . ? Zn1 N4 C12 C8 176.4(3) . . . . ? C11 N4 C12 C13 -177.9(3) . . . . ? Zn1 N4 C12 C13 -2.9(4) . . . . ? C9 C8 C12 N4 -0.6(5) . . . . ? C7 C8 C12 N4 178.9(3) . . . . ? C9 C8 C12 C13 178.7(3) . . . . ? C7 C8 C12 C13 -1.9(5) . . . . ? C1 N1 C13 C4 3.0(5) . . . . ? Zn1 N1 C13 C4 178.9(3) . . . . ? C1 N1 C13 C12 -177.5(3) . . . . ? Zn1 N1 C13 C12 -1.7(4) . . . . ? C3 C4 C13 N1 -2.7(5) . . . . ? C5 C4 C13 N1 177.2(3) . . . . ? C3 C4 C13 C12 177.9(3) . . . . ? C5 C4 C13 C12 -2.3(5) . . . . ? N4 C12 C13 N1 3.1(5) . . . . ? C8 C12 C13 N1 -176.2(3) . . . . ? N4 C12 C13 C4 -177.4(3) . . . . ? C8 C12 C13 C4 3.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.567 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.095 # Attachment '5.cif' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 710087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Co2 N8 O12 S2, 2(H2 O)' _chemical_formula_sum 'C26 H28 Co2 N8 O14 S2' _chemical_formula_weight 858.54 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' S S 0.1246 0.1234 '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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.316(2) _cell_length_b 9.0660(18) _cell_length_c 16.860(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.088(2) _cell_angle_gamma 90.00 _cell_volume 1557.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3141 _cell_measurement_theta_min 2.447 _cell_measurement_theta_max 25.816 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6770 _exptl_absorpt_correction_T_max 0.7848 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11278 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2897 _reflns_number_gt 2306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0462P)^2^+0.6572P] 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 2897 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.68861(4) 0.18074(4) 0.04111(2) 0.02861(14) Uani 1 1 d . . . S1 S 0.53203(7) -0.10090(7) 0.11268(4) 0.0300(2) Uani 1 1 d . . . O1 O 0.6355(2) -0.0306(2) 0.07551(14) 0.0399(5) Uani 1 1 d . . . O6 O 0.5904(2) -0.1773(2) 0.18644(13) 0.0450(6) Uani 1 1 d . . . O4 O 0.4612(2) -0.2099(2) 0.05719(13) 0.0356(5) Uani 1 1 d . . . O5 O 0.43872(19) 0.0123(2) 0.13379(13) 0.0358(5) Uani 1 1 d . . . N2 N 0.7568(2) 0.4024(3) 0.03306(15) 0.0305(6) Uani 1 1 d . . . N1 N 0.8745(2) 0.1765(2) 0.11685(15) 0.0314(6) Uani 1 1 d . . . N4 N 1.2459(2) 0.5127(3) 0.20283(16) 0.0380(6) Uani 1 1 d . . . H4D H 1.3061 0.4617 0.2316 0.046 Uiso 1 1 calc R . . N3 N 1.1437(3) 0.7063(3) 0.13927(16) 0.0387(6) Uani 1 1 d . . . C1 C 0.6915(3) 0.5151(3) -0.00614(19) 0.0361(7) Uani 1 1 d . . . H1 H 0.6093 0.4973 -0.0361 0.043 Uiso 1 1 calc R . . C2 C 0.7417(3) 0.6576(3) -0.0039(2) 0.0388(8) Uani 1 1 d . . . H2 H 0.6926 0.7335 -0.0309 0.047 Uiso 1 1 calc R . . C3 C 0.8638(3) 0.6857(3) 0.03832(19) 0.0347(7) Uani 1 1 d . . . H3 H 0.8992 0.7801 0.0389 0.042 Uiso 1 1 calc R . . C4 C 0.9352(3) 0.5706(3) 0.08077(17) 0.0290(6) Uani 1 1 d . . . C5 C 1.0638(3) 0.5819(3) 0.12628(18) 0.0308(7) Uani 1 1 d . . . C7 C 1.1260(3) 0.4633(3) 0.16580(18) 0.0311(7) Uani 1 1 d . . . C8 C 1.0681(3) 0.3195(3) 0.16539(18) 0.0298(7) Uani 1 1 d . . . C9 C 1.1263(3) 0.1939(3) 0.2051(2) 0.0376(7) Uani 1 1 d . . . H9 H 1.2097 0.1992 0.2354 0.045 Uiso 1 1 calc R . . C10 C 1.0585(3) 0.0639(3) 0.1984(2) 0.0397(8) Uani 1 1 d . . . H10 H 1.0960 -0.0210 0.2232 0.048 Uiso 1 1 calc R . . C11 C 0.9329(3) 0.0598(3) 0.15409(19) 0.0358(7) Uani 1 1 d . . . H11 H 0.8875 -0.0292 0.1504 0.043 Uiso 1 1 calc R . . C12 C 0.9416(3) 0.3063(3) 0.12110(17) 0.0286(6) Uani 1 1 d . . . C13 C 0.8761(3) 0.4301(3) 0.07732(17) 0.0274(6) Uani 1 1 d . . . C6 C 1.2505(3) 0.6572(4) 0.1851(2) 0.0425(8) Uani 1 1 d . . . H6 H 1.3223 0.7169 0.2034 0.051 Uiso 1 1 calc R . . O3 O 0.7945(2) 0.0651(2) -0.03948(13) 0.0398(5) Uani 1 1 d . . . H3C H 0.7426 0.0209 -0.0731 0.060 Uiso 1 1 d R . . H3B H 0.8371 0.1274 -0.0617 0.060 Uiso 1 1 d R . . O2 O 0.5750(2) 0.2637(3) 0.12145(15) 0.0540(7) Uani 1 1 d . . . H2C H 0.5250 0.1993 0.1326 0.081 Uiso 1 1 d R . . H2B H 0.5768 0.3378 0.1491 0.081 Uiso 1 1 d R . . O7 O 0.5866(3) 0.5147(3) 0.20115(16) 0.0712(9) Uani 1 1 d . . . H7B H 0.5835 0.5074 0.2500 0.107 Uiso 1 1 d R . . H7C H 0.5899 0.6003 0.1866 0.107 Uiso 1 1 d 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 0.0284(2) 0.0230(2) 0.0326(2) -0.00178(17) -0.00088(17) -0.00489(16) S1 0.0313(4) 0.0228(4) 0.0329(4) 0.0013(3) -0.0037(3) -0.0050(3) O1 0.0353(12) 0.0271(10) 0.0584(15) 0.0012(10) 0.0108(11) -0.0038(9) O6 0.0571(15) 0.0333(12) 0.0384(13) 0.0063(10) -0.0120(11) -0.0045(10) O4 0.0360(12) 0.0253(10) 0.0414(13) -0.0053(9) -0.0064(10) -0.0037(9) O5 0.0352(12) 0.0285(11) 0.0430(13) -0.0061(9) 0.0039(10) -0.0027(9) N2 0.0289(14) 0.0277(13) 0.0330(14) 0.0004(11) -0.0005(11) -0.0023(10) N1 0.0357(14) 0.0231(12) 0.0340(14) 0.0007(11) 0.0014(11) -0.0030(10) N4 0.0337(15) 0.0363(14) 0.0398(16) 0.0025(12) -0.0073(12) -0.0048(12) N3 0.0420(16) 0.0311(14) 0.0409(16) -0.0015(12) -0.0002(13) -0.0126(12) C1 0.0323(17) 0.0323(16) 0.0415(19) 0.0044(14) -0.0013(14) 0.0017(13) C2 0.0395(19) 0.0296(16) 0.045(2) 0.0057(15) -0.0009(15) 0.0053(14) C3 0.0412(18) 0.0226(14) 0.0395(18) -0.0028(13) 0.0040(15) -0.0017(13) C4 0.0348(17) 0.0252(14) 0.0268(16) -0.0027(12) 0.0041(13) -0.0017(12) C5 0.0344(17) 0.0267(15) 0.0303(16) -0.0020(13) 0.0023(13) -0.0069(12) C7 0.0297(16) 0.0325(15) 0.0300(16) -0.0022(13) 0.0008(13) -0.0067(13) C8 0.0304(16) 0.0286(15) 0.0290(16) -0.0033(13) 0.0001(13) -0.0020(12) C9 0.0322(17) 0.0372(17) 0.0405(19) 0.0028(14) -0.0029(14) 0.0031(14) C10 0.0441(19) 0.0302(16) 0.043(2) 0.0036(14) 0.0020(16) 0.0041(14) C11 0.0435(19) 0.0242(15) 0.0387(18) 0.0008(13) 0.0034(15) -0.0038(13) C12 0.0328(16) 0.0258(14) 0.0263(15) -0.0027(12) 0.0022(13) -0.0027(12) C13 0.0288(15) 0.0246(14) 0.0275(16) -0.0007(12) 0.0010(12) -0.0029(12) C6 0.041(2) 0.0402(18) 0.043(2) -0.0035(15) -0.0047(16) -0.0178(15) O3 0.0408(13) 0.0357(12) 0.0418(13) -0.0004(10) 0.0036(10) -0.0052(10) O2 0.0692(17) 0.0327(12) 0.0667(17) -0.0162(12) 0.0314(14) -0.0159(12) O7 0.135(3) 0.0316(13) 0.0512(17) -0.0070(12) 0.0283(17) -0.0145(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 O2 2.067(2) . ? Co1 O4 2.097(2) 3_655 ? Co1 O1 2.100(2) . ? Co1 N1 2.130(2) . ? Co1 N2 2.140(2) . ? Co1 O3 2.147(2) . ? S1 O1 1.466(2) . ? S1 O6 1.467(2) . ? S1 O4 1.473(2) . ? S1 O5 1.488(2) . ? O4 Co1 2.097(2) 3_655 ? N2 C1 1.340(4) . ? N2 C13 1.358(4) . ? N1 C11 1.325(4) . ? N1 C12 1.361(3) . ? N4 C6 1.347(4) . ? N4 C7 1.370(4) . ? N4 H4D 0.8600 . ? N3 C6 1.319(4) . ? N3 C5 1.394(4) . ? C1 C2 1.390(4) . ? C1 H1 0.9300 . ? C2 C3 1.369(4) . ? C2 H2 0.9300 . ? C3 C4 1.406(4) . ? C3 H3 0.9300 . ? C4 C13 1.409(4) . ? C4 C5 1.428(4) . ? C5 C7 1.370(4) . ? C7 C8 1.434(4) . ? C8 C12 1.403(4) . ? C8 C9 1.406(4) . ? C9 C10 1.366(4) . ? C9 H9 0.9300 . ? C10 C11 1.390(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.451(4) . ? C6 H6 0.9300 . ? O3 H3C 0.8200 . ? O3 H3B 0.8387 . ? O2 H2C 0.8200 . ? O2 H2B 0.8165 . ? O7 H7B 0.8327 . ? O7 H7C 0.8159 . ? 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 O2 Co1 O4 92.80(10) . 3_655 ? O2 Co1 O1 87.22(9) . . ? O4 Co1 O1 98.13(8) 3_655 . ? O2 Co1 N1 99.42(10) . . ? O4 Co1 N1 163.27(9) 3_655 . ? O1 Co1 N1 93.87(9) . . ? O2 Co1 N2 85.75(9) . . ? O4 Co1 N2 92.31(8) 3_655 . ? O1 Co1 N2 167.69(9) . . ? N1 Co1 N2 77.35(9) . . ? O2 Co1 O3 171.96(8) . . ? O4 Co1 O3 86.93(8) 3_655 . ? O1 Co1 O3 84.86(8) . . ? N1 Co1 O3 82.55(9) . . ? N2 Co1 O3 102.29(9) . . ? O1 S1 O6 109.78(14) . . ? O1 S1 O4 109.98(13) . . ? O6 S1 O4 108.52(12) . . ? O1 S1 O5 110.16(12) . . ? O6 S1 O5 108.51(14) . . ? O4 S1 O5 109.87(12) . . ? S1 O1 Co1 138.94(13) . . ? S1 O4 Co1 130.35(12) . 3_655 ? C1 N2 C13 118.1(2) . . ? C1 N2 Co1 127.1(2) . . ? C13 N2 Co1 114.68(18) . . ? C11 N1 C12 118.4(3) . . ? C11 N1 Co1 126.7(2) . . ? C12 N1 Co1 114.70(19) . . ? C6 N4 C7 106.1(3) . . ? C6 N4 H4D 127.0 . . ? C7 N4 H4D 127.0 . . ? C6 N3 C5 103.7(3) . . ? N2 C1 C2 122.6(3) . . ? N2 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C13 117.5(3) . . ? C3 C4 C5 126.0(3) . . ? C13 C4 C5 116.5(3) . . ? C7 C5 N3 109.8(3) . . ? C7 C5 C4 122.0(3) . . ? N3 C5 C4 128.2(3) . . ? N4 C7 C5 106.6(3) . . ? N4 C7 C8 130.2(3) . . ? C5 C7 C8 123.3(3) . . ? C12 C8 C9 118.4(3) . . ? C12 C8 C7 115.6(3) . . ? C9 C8 C7 126.0(3) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N1 C11 C10 123.3(3) . . ? N1 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? N1 C12 C8 121.6(3) . . ? N1 C12 C13 116.8(2) . . ? C8 C12 C13 121.6(3) . . ? N2 C13 C4 122.6(3) . . ? N2 C13 C12 116.4(2) . . ? C4 C13 C12 121.0(3) . . ? N3 C6 N4 113.8(3) . . ? N3 C6 H6 123.1 . . ? N4 C6 H6 123.1 . . ? Co1 O3 H3C 109.5 . . ? Co1 O3 H3B 108.0 . . ? H3C O3 H3B 110.6 . . ? Co1 O2 H2C 109.4 . . ? Co1 O2 H2B 135.2 . . ? H2C O2 H2B 114.4 . . ? H7B O7 H7C 112.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 S1 O1 Co1 -121.2(2) . . . . ? O4 S1 O1 Co1 119.5(2) . . . . ? O5 S1 O1 Co1 -1.7(3) . . . . ? O2 Co1 O1 S1 21.2(2) . . . . ? O4 Co1 O1 S1 -71.2(2) 3_655 . . . ? N1 Co1 O1 S1 120.5(2) . . . . ? N2 Co1 O1 S1 76.5(5) . . . . ? O3 Co1 O1 S1 -157.4(2) . . . . ? O1 S1 O4 Co1 -80.49(19) . . . 3_655 ? O6 S1 O4 Co1 159.41(16) . . . 3_655 ? O5 S1 O4 Co1 40.9(2) . . . 3_655 ? O2 Co1 N2 C1 -75.2(3) . . . . ? O4 Co1 N2 C1 17.4(3) 3_655 . . . ? O1 Co1 N2 C1 -130.6(4) . . . . ? N1 Co1 N2 C1 -175.9(3) . . . . ? O3 Co1 N2 C1 104.8(3) . . . . ? O2 Co1 N2 C13 100.3(2) . . . . ? O4 Co1 N2 C13 -167.1(2) 3_655 . . . ? O1 Co1 N2 C13 44.9(5) . . . . ? N1 Co1 N2 C13 -0.4(2) . . . . ? O3 Co1 N2 C13 -79.7(2) . . . . ? O2 Co1 N1 C11 100.5(3) . . . . ? O4 Co1 N1 C11 -123.1(3) 3_655 . . . ? O1 Co1 N1 C11 12.7(3) . . . . ? N2 Co1 N1 C11 -176.1(3) . . . . ? O3 Co1 N1 C11 -71.6(3) . . . . ? O2 Co1 N1 C12 -84.8(2) . . . . ? O4 Co1 N1 C12 51.6(4) 3_655 . . . ? O1 Co1 N1 C12 -172.6(2) . . . . ? N2 Co1 N1 C12 -1.3(2) . . . . ? O3 Co1 N1 C12 103.1(2) . . . . ? C13 N2 C1 C2 0.8(5) . . . . ? Co1 N2 C1 C2 176.1(2) . . . . ? N2 C1 C2 C3 1.5(5) . . . . ? C1 C2 C3 C4 -1.9(5) . . . . ? C2 C3 C4 C13 0.1(4) . . . . ? C2 C3 C4 C5 178.9(3) . . . . ? C6 N3 C5 C7 0.6(4) . . . . ? C6 N3 C5 C4 179.7(3) . . . . ? C3 C4 C5 C7 -180.0(3) . . . . ? C13 C4 C5 C7 -1.1(4) . . . . ? C3 C4 C5 N3 1.1(5) . . . . ? C13 C4 C5 N3 179.9(3) . . . . ? C6 N4 C7 C5 0.6(3) . . . . ? C6 N4 C7 C8 -178.9(3) . . . . ? N3 C5 C7 N4 -0.8(3) . . . . ? C4 C5 C7 N4 -179.9(3) . . . . ? N3 C5 C7 C8 178.8(3) . . . . ? C4 C5 C7 C8 -0.4(5) . . . . ? N4 C7 C8 C12 179.7(3) . . . . ? C5 C7 C8 C12 0.2(4) . . . . ? N4 C7 C8 C9 -0.1(6) . . . . ? C5 C7 C8 C9 -179.5(3) . . . . ? C12 C8 C9 C10 0.7(5) . . . . ? C7 C8 C9 C10 -179.5(3) . . . . ? C8 C9 C10 C11 -1.4(5) . . . . ? C12 N1 C11 C10 1.0(5) . . . . ? Co1 N1 C11 C10 175.6(2) . . . . ? C9 C10 C11 N1 0.6(5) . . . . ? C11 N1 C12 C8 -1.7(4) . . . . ? Co1 N1 C12 C8 -176.9(2) . . . . ? C11 N1 C12 C13 178.0(3) . . . . ? Co1 N1 C12 C13 2.8(3) . . . . ? C9 C8 C12 N1 0.9(4) . . . . ? C7 C8 C12 N1 -178.9(3) . . . . ? C9 C8 C12 C13 -178.8(3) . . . . ? C7 C8 C12 C13 1.4(4) . . . . ? C1 N2 C13 C4 -2.6(4) . . . . ? Co1 N2 C13 C4 -178.5(2) . . . . ? C1 N2 C13 C12 177.9(3) . . . . ? Co1 N2 C13 C12 1.9(3) . . . . ? C3 C4 C13 N2 2.2(4) . . . . ? C5 C4 C13 N2 -176.8(3) . . . . ? C3 C4 C13 C12 -178.3(3) . . . . ? C5 C4 C13 C12 2.7(4) . . . . ? N1 C12 C13 N2 -3.2(4) . . . . ? C8 C12 C13 N2 176.5(3) . . . . ? N1 C12 C13 C4 177.3(3) . . . . ? C8 C12 C13 C4 -3.0(4) . . . . ? C5 N3 C6 N4 -0.3(4) . . . . ? C7 N4 C6 N3 -0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.500 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.068 # Attachment '6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 710088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H36 Mn2 N16 O6 S,C14 H8 O6 S, 6.5H2O' _chemical_formula_sum 'C66 H57 Mn2 N16 O18.50 S2' _chemical_formula_weight 1544.28 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 17.074(3) _cell_length_b 16.970(3) _cell_length_c 22.935(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.510(3) _cell_angle_gamma 90.00 _cell_volume 6554.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3735 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3180 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9000 _exptl_absorpt_correction_T_max 0.9482 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 32130 _diffrn_reflns_av_R_equivalents 0.1021 _diffrn_reflns_av_sigmaI/netI 0.1907 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11522 _reflns_number_gt 3730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0080P)^2^+4.0000P] 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 11522 _refine_ls_number_parameters 835 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.1866 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.026 _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 0.06071(6) 0.58108(6) 0.23139(4) 0.0501(3) Uani 1 1 d U . . Mn2 Mn 0.43044(5) 0.57154(5) 0.27437(4) 0.0485(3) Uani 1 1 d . . . S1 S 0.24813(13) 0.64897(10) 0.25126(10) 0.0569(4) Uani 1 1 d U . . O1 O 0.3104(2) 0.5921(2) 0.23954(17) 0.0592(12) Uani 1 1 d . . . O2 O 0.1814(2) 0.6031(2) 0.26821(17) 0.0618(12) Uani 1 1 d U . . O3 O 0.2204(2) 0.6934(3) 0.1972(2) 0.0779(15) Uani 1 1 d U . . O4 O 0.2804(3) 0.6999(3) 0.3004(2) 0.0839(15) Uani 1 1 d U . . O5 O 0.0613(2) 0.6962(2) 0.19151(16) 0.0565(12) Uani 1 1 d U . . H5A H 0.1082 0.7007 0.1839 0.068 Uiso 1 1 d R . . H5B H 0.0300 0.7080 0.1609 0.068 Uiso 1 1 d R . . O6 O 0.4387(2) 0.6955(2) 0.30243(16) 0.0575(13) Uani 1 1 d . . . H6A H 0.3897 0.6965 0.2930 0.086 Uiso 1 1 d R . . H6B H 0.4673 0.7113 0.3331 0.086 Uiso 1 1 d R . . N1 N -0.0548(3) 0.5588(3) 0.1689(2) 0.0459(14) Uani 1 1 d . . . N2 N 0.0890(3) 0.4959(3) 0.1625(2) 0.0535(16) Uani 1 1 d . . . N3 N -0.1587(3) 0.4258(3) -0.0193(2) 0.0590(16) Uani 1 1 d U . . N4 N -0.0406(3) 0.3667(3) -0.0214(2) 0.0528(15) Uani 1 1 d . . . H4C H -0.0057 0.3376 -0.0339 0.063 Uiso 1 1 calc R . . N5 N -0.0085(3) 0.6297(3) 0.2988(2) 0.0539(15) Uani 1 1 d U . . N6 N 0.0502(3) 0.4841(3) 0.2994(2) 0.0545(14) Uani 1 1 d U . . N7 N -0.0792(3) 0.4317(3) 0.4725(2) 0.0658(16) Uani 1 1 d U . . N8 N -0.1236(3) 0.5542(3) 0.4744(2) 0.0680(16) Uani 1 1 d U . . H8A H -0.1461 0.5950 0.4866 0.082 Uiso 1 1 calc R . . N9 N 0.3993(3) 0.4942(3) 0.3491(2) 0.0474(15) Uani 1 1 d U . . N10 N 0.5435(3) 0.5530(3) 0.3400(2) 0.0405(13) Uani 1 1 d U . . N11 N 0.5300(3) 0.3523(3) 0.5276(2) 0.0476(15) Uani 1 1 d DU . . H11B H 0.4956 0.3230 0.5407 0.057 Uiso 1 1 calc R . . N12 N 0.6502(3) 0.4083(3) 0.5243(2) 0.0525(15) Uani 1 1 d DU . . N13 N 0.4248(3) 0.4623(3) 0.2154(2) 0.0550(16) Uani 1 1 d . . . N14 N 0.4987(3) 0.5970(3) 0.1999(2) 0.0562(16) Uani 1 1 d U . . N15 N 0.5272(3) 0.3547(3) 0.0423(2) 0.0856(19) Uani 1 1 d DU . . H15B H 0.5105 0.3071 0.0362 0.103 Uiso 1 1 calc R . . N16 N 0.5958(3) 0.4704(4) 0.0301(2) 0.0778(19) Uani 1 1 d DU . . C1 C -0.1246(4) 0.5905(3) 0.1717(3) 0.054(2) Uani 1 1 d . . . H1A H -0.1291 0.6218 0.2042 0.065 Uiso 1 1 calc R . . C2 C -0.1915(4) 0.5802(4) 0.1294(3) 0.063(2) Uani 1 1 d . . . H2A H -0.2393 0.6040 0.1338 0.075 Uiso 1 1 calc R . . C3 C -0.1861(4) 0.5341(4) 0.0806(3) 0.0583(19) Uani 1 1 d U . . H3A H -0.2299 0.5267 0.0510 0.070 Uiso 1 1 calc R . . C4 C -0.1122(2) 0.4983(2) 0.07675(19) 0.0429(17) Uani 1 1 d GU . . C5 C -0.1029(2) 0.4481(2) 0.03049(17) 0.0439(17) Uani 1 1 d G . . C6 C -0.0300(2) 0.41227(19) 0.02918(13) 0.0485(18) Uani 1 1 d G . . C7 C 0.03362(19) 0.42664(16) 0.07413(13) 0.0505(18) Uani 1 1 d GDU . . C8 C 0.0243(2) 0.4768(2) 0.12040(13) 0.0472(18) Uani 1 1 d GU . . C9 C -0.0486(3) 0.5126(2) 0.12171(16) 0.0476(18) Uani 1 1 d GU . . C10 C 0.1103(2) 0.3887(2) 0.0720(2) 0.059(2) Uani 1 1 d GDU . . H10A H 0.1179 0.3544 0.0419 0.070 Uiso 1 1 calc R . . C11 C 0.1705(4) 0.4074(4) 0.1178(3) 0.070(2) Uani 1 1 d D . . H11A H 0.2198 0.3834 0.1201 0.084 Uiso 1 1 calc R . . C12 C 0.1579(4) 0.4617(4) 0.1605(3) 0.066(2) Uani 1 1 d D . . H12A H 0.2007 0.4749 0.1895 0.080 Uiso 1 1 calc R . . C13 C -0.1180(4) 0.3773(4) -0.0474(3) 0.062(2) Uani 1 1 d U . . H13A H -0.1400 0.3520 -0.0823 0.074 Uiso 1 1 calc R . . C14 C -0.0396(4) 0.7022(4) 0.2964(3) 0.060(2) Uani 1 1 d U . . H14A H -0.0289 0.7361 0.2668 0.072 Uiso 1 1 calc R . . C15 C -0.0876(4) 0.7298(4) 0.3363(3) 0.067(2) Uani 1 1 d D . . H15A H -0.1088 0.7804 0.3332 0.081 Uiso 1 1 calc R . . C16 C -0.1023(4) 0.6794(4) 0.3802(3) 0.065(2) Uani 1 1 d D . . H16A H -0.1342 0.6955 0.4071 0.077 Uiso 1 1 calc R . . C17 C -0.0691(2) 0.6039(2) 0.38429(19) 0.0489(19) Uani 1 1 d GD . . C18 C -0.0854(2) 0.5504(3) 0.42664(17) 0.0554(19) Uani 1 1 d G . . C19 C -0.0567(2) 0.4738(3) 0.42665(15) 0.0517(19) Uani 1 1 d GU . . C20 C -0.01183(18) 0.4505(2) 0.38432(14) 0.0544(19) Uani 1 1 d GD . . C21 C 0.0044(2) 0.5040(2) 0.34197(14) 0.0517(18) Uani 1 1 d GU . . C22 C -0.0242(2) 0.5807(2) 0.34196(17) 0.0485(17) Uani 1 1 d G . . C23 C 0.0267(3) 0.3711(2) 0.3822(2) 0.066(2) Uani 1 1 d GDU . . H23A H 0.0208 0.3333 0.4105 0.080 Uiso 1 1 calc R . . C24 C 0.0703(4) 0.3542(4) 0.3387(3) 0.090(3) Uani 1 1 d DU . . H24A H 0.0926 0.3045 0.3365 0.108 Uiso 1 1 calc R . . C25 C 0.0808(4) 0.4128(4) 0.2976(3) 0.071(2) Uani 1 1 d DU . . H25A H 0.1103 0.4011 0.2681 0.085 Uiso 1 1 calc R . . C26 C -0.1195(4) 0.4811(4) 0.4991(3) 0.068(2) Uani 1 1 d U . . H26A H -0.1430 0.4679 0.5316 0.081 Uiso 1 1 calc R . . C27 C 0.3274(4) 0.4648(4) 0.3514(3) 0.060(2) Uani 1 1 d DU . . H27A H 0.2848 0.4814 0.3235 0.071 Uiso 1 1 calc R . . C28 C 0.3137(4) 0.4098(4) 0.3941(3) 0.063(2) Uani 1 1 d D . . H28A H 0.2633 0.3892 0.3942 0.075 Uiso 1 1 calc R . . C29 C 0.3764(4) 0.3874(4) 0.4357(3) 0.0581(19) Uani 1 1 d DU . . H29A H 0.3691 0.3507 0.4645 0.070 Uiso 1 1 calc R . . C30 C 0.45334(19) 0.4203(2) 0.43505(17) 0.0420(16) Uani 1 1 d GDU . . C31 C 0.5171(2) 0.40047(19) 0.47845(15) 0.0509(17) Uani 1 1 d GU . . C32 C 0.5917(2) 0.4325(2) 0.47692(13) 0.0497(17) Uani 1 1 d GU . . C33 C 0.60246(17) 0.48434(16) 0.43200(13) 0.0456(16) Uani 1 1 d GU . . C34 C 0.5387(2) 0.50414(18) 0.38859(13) 0.0444(16) Uani 1 1 d GU . . C35 C 0.46410(18) 0.4721(2) 0.39012(15) 0.0412(15) Uani 1 1 d GU . . C36 C 0.6729(2) 0.5261(2) 0.4243(2) 0.0572(18) Uani 1 1 d GDU . . H36A H 0.7172 0.5195 0.4535 0.069 Uiso 1 1 calc R . . C37 C 0.6817(4) 0.5746(3) 0.3786(3) 0.054(2) Uani 1 1 d D . . H37A H 0.7296 0.5990 0.3753 0.065 Uiso 1 1 calc R . . C38 C 0.6135(4) 0.5848(4) 0.3372(3) 0.0514(19) Uani 1 1 d U . . H38A H 0.6173 0.6165 0.3047 0.062 Uiso 1 1 calc R . . C39 C 0.6072(4) 0.3602(4) 0.5509(3) 0.064(2) Uani 1 1 d DU . . H39A H 0.6294 0.3326 0.5847 0.077 Uiso 1 1 calc R . . C40 C 0.3848(4) 0.3962(4) 0.2219(3) 0.062(2) Uani 1 1 d D . . H40A H 0.3584 0.3936 0.2542 0.074 Uiso 1 1 calc R . . C41 C 0.3788(4) 0.3298(4) 0.1843(3) 0.075(2) Uani 1 1 d D . . H41A H 0.3480 0.2861 0.1897 0.090 Uiso 1 1 calc R . . C42 C 0.4220(4) 0.3351(4) 0.1394(3) 0.072(2) Uani 1 1 d D . . H42A H 0.4219 0.2925 0.1139 0.087 Uiso 1 1 calc R . . C43 C 0.4672(2) 0.4029(2) 0.1300(2) 0.060(2) Uani 1 1 d GDU . . C44 C 0.5121(3) 0.4101(2) 0.08494(18) 0.072(2) Uani 1 1 d GU . . C45 C 0.5536(2) 0.4794(3) 0.07898(15) 0.062(2) Uani 1 1 d GU . . C46 C 0.55007(17) 0.5414(2) 0.11805(14) 0.0649(19) Uani 1 1 d GU . . C47 C 0.5051(2) 0.5342(3) 0.16307(15) 0.0546(19) Uani 1 1 d GU . . C48 C 0.4637(2) 0.4649(3) 0.16902(17) 0.059(2) Uani 1 1 d G . . C49 C 0.5826(3) 0.6146(3) 0.1069(2) 0.067(2) Uani 1 1 d GDU . . H49A H 0.6069 0.6218 0.0738 0.081 Uiso 1 1 calc R . . C50 C 0.5780(4) 0.6766(4) 0.1465(3) 0.072(2) Uani 1 1 d D . . H50A H 0.6039 0.7242 0.1429 0.086 Uiso 1 1 calc R . . C51 C 0.5325(4) 0.6645(4) 0.1923(3) 0.069(2) Uani 1 1 d DU . . H51A H 0.5265 0.7060 0.2177 0.082 Uiso 1 1 calc R . . C52 C 0.5755(4) 0.3979(5) 0.0136(3) 0.077(2) Uani 1 1 d DU . . H52A H 0.5948 0.3760 -0.0184 0.092 Uiso 1 1 calc R . . S2 S 0.74691(13) 0.46349(9) 0.25649(9) 0.0503(4) Uani 1 1 d . . . O7 O 0.5339(3) 0.2288(3) 0.40894(19) 0.0641(14) Uani 1 1 d . . . O8 O 0.6510(3) 0.2223(3) 0.4670(2) 0.0684(16) Uani 1 1 d . . . O9 O 0.8466(3) 0.2344(2) 0.0411(2) 0.0643(14) Uani 1 1 d . . . O10 O 0.9634(3) 0.2394(2) 0.10110(19) 0.0624(14) Uani 1 1 d . . . O11 O 0.6821(3) 0.5075(2) 0.22334(18) 0.0607(13) Uani 1 1 d . . . O12 O 0.8120(3) 0.5051(2) 0.29226(18) 0.0588(13) Uani 1 1 d . . . C53 C 0.6066(5) 0.2451(4) 0.4216(3) 0.055(2) Uani 1 1 d . . . C54 C 0.6419(3) 0.2983(2) 0.37879(18) 0.0460(18) Uani 1 1 d G . . C55 C 0.7228(3) 0.3147(2) 0.38882(15) 0.059(2) Uani 1 1 d G . . H55A H 0.7556 0.2921 0.4209 0.071 Uiso 1 1 calc R . . C56 C 0.75466(18) 0.3649(2) 0.3510(2) 0.058(2) Uani 1 1 d G . . H56A H 0.8088 0.3759 0.3577 0.069 Uiso 1 1 calc R . . C57 C 0.7056(3) 0.3987(2) 0.30306(17) 0.0414(17) Uani 1 1 d G . . C58 C 0.6248(3) 0.3823(2) 0.29303(15) 0.0473(18) Uani 1 1 d G . . H58A H 0.5920 0.4049 0.2610 0.057 Uiso 1 1 calc R . . C59 C 0.59292(19) 0.3321(2) 0.3309(2) 0.0485(18) Uani 1 1 d G . . H59A H 0.5388 0.3211 0.3242 0.058 Uiso 1 1 calc R . . C60 C 0.7882(3) 0.4026(2) 0.20779(18) 0.0421(17) Uani 1 1 d GU . . C61 C 0.8668(2) 0.3783(2) 0.22170(15) 0.0551(19) Uani 1 1 d GU . . H61A H 0.8976 0.3942 0.2570 0.066 Uiso 1 1 calc R . . C62 C 0.89947(18) 0.3305(2) 0.1828(2) 0.0528(19) Uani 1 1 d G . . H62A H 0.9521 0.3142 0.1921 0.063 Uiso 1 1 calc R . . C63 C 0.8535(3) 0.3068(2) 0.12993(18) 0.0432(17) Uani 1 1 d G . . C64 C 0.7748(3) 0.3310(2) 0.11603(15) 0.0492(18) Uani 1 1 d G . . H64A H 0.7440 0.3152 0.0807 0.059 Uiso 1 1 calc R . . C65 C 0.74219(17) 0.3789(2) 0.1550(2) 0.0507(19) Uani 1 1 d G . . H65A H 0.6896 0.3951 0.1456 0.061 Uiso 1 1 calc R . . C66 C 0.8899(5) 0.2552(4) 0.0874(3) 0.050(2) Uani 1 1 d . . . O13 O 0.1957(3) 0.3001(3) 0.4886(2) 0.1036(17) Uiso 1 1 d . . . H13E H 0.2391 0.2982 0.4750 0.155 Uiso 1 1 d R . . H13C H 0.1661 0.2652 0.4707 0.155 Uiso 1 1 d R . . O14 O 0.1984(3) 0.6082(3) 0.4040(2) 0.124(2) Uiso 1 1 d . . . H14C H 0.1920 0.5713 0.3788 0.185 Uiso 1 1 d R . . H14D H 0.1878 0.6568 0.3958 0.185 Uiso 1 1 d R . . O15 O 0.0694(3) 0.7269(3) 0.5014(2) 0.1227(19) Uiso 1 1 d . . . H15C H 0.1070 0.7499 0.5240 0.184 Uiso 1 1 d R . . H15D H 0.0472 0.6915 0.5217 0.184 Uiso 1 1 d R . . O16 O 0.1685(3) 1.1905(3) 0.3889(2) 0.145(2) Uiso 1 1 d . . . H16C H 0.1897 1.1253 0.4008 0.218 Uiso 1 1 d R . . H16D H 0.2095 1.2048 0.3742 0.218 Uiso 1 1 d R . . O17A O 0.1926(7) 1.0537(7) 0.4119(5) 0.128(5) Uiso 0.50 1 d P A 1 H17A H 0.1764 1.0307 0.4406 0.192 Uiso 0.50 1 d PR A 1 H17B H 0.2386 1.0342 0.4126 0.192 Uiso 0.50 1 d PR A 1 O18A O 0.1732(7) 0.9097(7) 0.4795(5) 0.142(4) Uiso 0.50 1 d P B 1 H18A H 0.1370 0.9357 0.4579 0.213 Uiso 0.50 1 d PR B 1 H18B H 0.1540 0.8612 0.4846 0.213 Uiso 0.50 1 d PR B 1 O19A O 0.2101(4) 0.7458(5) 0.4617(3) 0.059(2) Uiso 0.50 1 d P C 1 H19A H 0.1905 0.7877 0.4449 0.089 Uiso 0.50 1 d PR C 1 H19B H 0.2412 0.7544 0.4901 0.089 Uiso 0.50 1 d PR C 1 O17B O 0.1882(7) 1.0127(7) 0.4400(5) 0.130(5) Uiso 0.50 1 d P D 2 H17C H 0.1703 1.0094 0.4724 0.196 Uiso 0.50 1 d PR D 2 H17D H 0.2372 1.0003 0.4458 0.196 Uiso 0.50 1 d PR D 2 O18B O 0.2026(9) 0.8097(9) 0.4882(6) 0.199(6) Uiso 0.50 1 d P E 2 H18C H 0.2001 0.8116 0.4509 0.298 Uiso 0.50 1 d PR E 2 H18D H 0.2501 0.7982 0.5034 0.298 Uiso 0.50 1 d PR E 2 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 0.0445(7) 0.0598(7) 0.0456(7) -0.0003(5) 0.0063(6) 0.0022(6) Mn2 0.0424(7) 0.0586(7) 0.0445(7) 0.0000(5) 0.0071(6) 0.0003(5) S1 0.0393(10) 0.0770(13) 0.0545(12) 0.0050(12) 0.0080(9) 0.0051(12) O1 0.040(3) 0.073(3) 0.063(3) -0.008(2) 0.004(3) 0.008(2) O2 0.039(2) 0.090(3) 0.056(3) 0.023(2) 0.006(2) -0.002(2) O3 0.049(3) 0.106(4) 0.079(3) 0.045(3) 0.011(3) 0.012(3) O4 0.054(3) 0.103(4) 0.093(3) -0.046(3) 0.006(3) 0.003(3) O5 0.035(3) 0.074(3) 0.059(3) 0.009(2) 0.003(2) 0.003(2) O6 0.044(3) 0.065(3) 0.060(3) -0.004(2) -0.002(3) -0.008(2) N1 0.038(4) 0.048(4) 0.053(4) 0.004(3) 0.013(3) 0.007(3) N2 0.038(4) 0.058(4) 0.064(4) -0.001(3) 0.006(3) 0.010(3) N3 0.062(4) 0.071(4) 0.040(4) 0.007(3) -0.002(3) -0.006(3) N4 0.057(4) 0.060(4) 0.041(4) 0.005(3) 0.007(3) 0.005(3) N5 0.054(4) 0.060(3) 0.048(4) 0.000(3) 0.010(3) -0.003(3) N6 0.042(4) 0.060(3) 0.056(4) 0.002(3) -0.007(3) -0.003(3) N7 0.048(4) 0.105(4) 0.043(4) 0.006(3) 0.004(3) -0.015(3) N8 0.054(4) 0.100(4) 0.049(4) -0.001(3) 0.004(3) -0.005(3) N9 0.039(3) 0.059(4) 0.046(4) -0.012(3) 0.010(3) -0.003(3) N10 0.035(3) 0.039(3) 0.050(3) -0.013(2) 0.013(3) -0.003(2) N11 0.063(4) 0.048(4) 0.032(3) 0.000(2) 0.007(3) -0.001(3) N12 0.060(4) 0.063(4) 0.033(4) -0.004(3) 0.004(3) 0.006(3) N13 0.056(4) 0.060(4) 0.050(4) 0.007(3) 0.012(3) 0.012(3) N14 0.043(4) 0.072(4) 0.053(4) 0.007(3) 0.007(3) 0.008(3) N15 0.090(5) 0.097(5) 0.072(5) -0.007(3) 0.019(4) 0.017(4) N16 0.053(4) 0.126(5) 0.050(4) -0.020(4) -0.004(3) 0.026(4) C1 0.049(5) 0.048(5) 0.068(6) -0.003(4) 0.017(5) 0.003(4) C2 0.042(5) 0.062(5) 0.081(6) 0.012(5) 0.000(5) -0.006(4) C3 0.042(4) 0.066(5) 0.064(5) 0.006(4) 0.000(4) -0.002(4) C4 0.047(4) 0.036(4) 0.048(5) 0.008(3) 0.015(4) 0.004(3) C5 0.048(5) 0.047(4) 0.036(5) 0.001(3) 0.007(4) -0.001(4) C6 0.068(6) 0.049(4) 0.033(4) -0.006(4) 0.021(4) -0.012(4) C7 0.056(4) 0.053(5) 0.043(4) 0.008(3) 0.008(4) 0.003(3) C8 0.056(5) 0.037(4) 0.048(5) 0.006(3) 0.006(4) 0.000(3) C9 0.049(5) 0.053(5) 0.041(5) 0.006(3) 0.008(4) 0.013(3) C10 0.070(5) 0.066(5) 0.040(5) -0.002(4) 0.010(4) 0.002(4) C11 0.071(6) 0.085(6) 0.051(5) -0.015(4) 0.002(5) 0.035(5) C12 0.049(5) 0.088(6) 0.057(5) -0.007(4) -0.003(4) 0.006(4) C13 0.068(6) 0.073(6) 0.037(5) 0.001(4) -0.012(4) -0.019(4) C14 0.063(5) 0.064(4) 0.055(5) -0.009(4) 0.011(4) -0.005(4) C15 0.068(5) 0.066(5) 0.072(6) -0.011(4) 0.025(5) 0.008(4) C16 0.056(5) 0.094(6) 0.045(5) -0.001(4) 0.014(4) -0.011(5) C17 0.041(5) 0.062(5) 0.045(5) -0.005(4) 0.011(4) -0.011(4) C18 0.040(4) 0.081(6) 0.044(5) 0.002(4) 0.006(4) -0.010(4) C19 0.036(5) 0.073(5) 0.044(5) 0.007(4) 0.002(4) -0.002(4) C20 0.042(5) 0.060(5) 0.053(5) 0.004(4) -0.018(4) -0.011(4) C21 0.041(5) 0.070(5) 0.043(5) 0.012(4) 0.001(3) -0.004(4) C22 0.038(4) 0.062(5) 0.044(5) 0.000(4) 0.004(4) -0.009(4) C23 0.062(6) 0.065(5) 0.062(6) 0.021(4) -0.020(4) -0.014(4) C24 0.089(7) 0.089(6) 0.089(7) 0.000(5) 0.007(5) -0.005(5) C25 0.073(6) 0.059(4) 0.076(6) 0.001(4) -0.001(5) -0.001(4) C26 0.062(5) 0.097(6) 0.046(5) 0.016(4) 0.012(4) -0.021(4) C27 0.041(4) 0.080(6) 0.054(5) -0.012(4) -0.004(4) -0.007(4) C28 0.052(5) 0.067(5) 0.069(6) 0.014(4) 0.010(5) -0.017(4) C29 0.063(4) 0.066(5) 0.044(5) 0.005(4) 0.007(4) -0.014(4) C30 0.042(3) 0.045(4) 0.041(4) -0.006(3) 0.012(3) 0.000(3) C31 0.056(4) 0.063(5) 0.037(4) 0.008(3) 0.015(3) 0.018(3) C32 0.056(4) 0.063(5) 0.030(4) 0.000(3) 0.008(3) 0.019(3) C33 0.042(3) 0.044(4) 0.050(4) -0.006(3) 0.004(3) 0.011(3) C34 0.041(3) 0.050(4) 0.046(4) 0.001(3) 0.018(3) 0.008(3) C35 0.045(4) 0.046(4) 0.033(4) -0.002(3) 0.006(3) -0.003(3) C36 0.059(4) 0.051(5) 0.061(5) -0.012(4) 0.010(4) 0.009(3) C37 0.044(5) 0.053(5) 0.068(5) -0.003(4) 0.015(4) -0.011(4) C38 0.040(4) 0.057(5) 0.058(5) 0.001(4) 0.011(4) -0.003(4) C39 0.081(6) 0.059(5) 0.052(6) -0.003(4) 0.010(5) 0.012(4) C40 0.054(5) 0.071(6) 0.057(5) -0.006(4) 0.001(4) 0.004(4) C41 0.089(6) 0.070(5) 0.067(6) -0.010(5) 0.016(5) 0.009(5) C42 0.074(6) 0.096(6) 0.046(5) -0.001(4) 0.009(4) 0.022(5) C43 0.069(6) 0.067(5) 0.042(5) -0.001(4) 0.005(4) 0.010(4) C44 0.060(5) 0.105(5) 0.051(5) -0.008(4) 0.003(4) 0.030(4) C45 0.038(5) 0.112(5) 0.032(4) 0.009(3) -0.007(4) 0.027(4) C46 0.043(5) 0.096(5) 0.055(5) 0.013(4) 0.005(4) 0.010(4) C47 0.037(5) 0.088(6) 0.039(4) 0.009(4) 0.008(3) 0.021(4) C48 0.046(5) 0.075(6) 0.052(5) -0.003(4) -0.003(4) 0.001(4) C49 0.053(5) 0.103(5) 0.043(5) 0.026(4) 0.001(4) 0.018(4) C50 0.054(5) 0.093(6) 0.064(6) 0.026(5) 0.001(5) -0.007(5) C51 0.051(5) 0.090(6) 0.064(5) 0.020(5) 0.008(4) 0.002(4) C52 0.051(5) 0.140(7) 0.040(5) 0.010(4) 0.008(4) 0.024(5) S2 0.0523(11) 0.0482(10) 0.0522(12) -0.0005(10) 0.0134(10) 0.0040(12) O7 0.053(3) 0.084(4) 0.054(3) -0.009(3) 0.008(3) -0.018(3) O8 0.076(4) 0.074(4) 0.055(4) 0.020(3) 0.010(3) -0.004(3) O9 0.070(4) 0.068(3) 0.055(3) -0.006(3) 0.008(3) 0.003(3) O10 0.051(3) 0.078(4) 0.059(3) 0.000(2) 0.010(3) 0.012(3) O11 0.057(3) 0.063(3) 0.062(3) 0.015(2) 0.009(3) 0.022(3) O12 0.061(3) 0.059(3) 0.057(3) -0.015(2) 0.007(3) -0.015(3) C53 0.069(7) 0.049(5) 0.048(6) -0.017(4) 0.015(5) -0.005(5) C54 0.049(5) 0.049(4) 0.041(5) -0.010(3) 0.010(4) 0.003(4) C55 0.046(5) 0.080(5) 0.049(5) 0.017(4) 0.000(4) 0.005(4) C56 0.043(5) 0.066(5) 0.064(5) 0.004(4) 0.012(5) -0.001(4) C57 0.046(5) 0.042(4) 0.035(4) -0.001(3) 0.004(4) 0.005(4) C58 0.039(5) 0.053(5) 0.046(5) -0.001(3) -0.003(4) 0.003(4) C59 0.033(4) 0.057(5) 0.053(5) -0.001(4) -0.001(4) -0.004(4) C60 0.033(4) 0.055(4) 0.037(4) -0.002(3) 0.002(4) -0.003(3) C61 0.049(4) 0.060(5) 0.054(5) -0.008(4) 0.001(4) 0.003(4) C62 0.030(4) 0.065(5) 0.060(5) -0.002(4) -0.003(4) 0.007(4) C63 0.044(5) 0.042(4) 0.045(5) 0.006(3) 0.012(4) -0.001(4) C64 0.032(5) 0.068(5) 0.044(5) 0.005(4) -0.004(4) -0.007(4) C65 0.026(4) 0.068(5) 0.058(5) 0.007(4) 0.007(4) 0.004(4) C66 0.055(6) 0.051(5) 0.042(5) 0.012(4) 0.008(5) -0.005(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 Mn1 O2 2.127(4) . ? Mn1 O5 2.157(4) . ? Mn1 N2 2.251(5) . ? Mn1 N5 2.251(5) . ? Mn1 N1 2.270(5) . ? Mn1 N6 2.294(5) . ? Mn2 O1 2.102(4) . ? Mn2 O6 2.198(4) . ? Mn2 N14 2.263(5) . ? Mn2 N10 2.265(5) . ? Mn2 N13 2.287(5) . ? Mn2 N9 2.289(5) . ? S1 O4 1.455(4) . ? S1 O3 1.461(4) . ? S1 O2 1.483(4) . ? S1 O1 1.492(4) . ? O5 H5A 0.8504 . ? O5 H5B 0.8334 . ? O6 H6A 0.8291 . ? O6 H6B 0.8308 . ? N1 C1 1.319(6) . ? N1 C9 1.354(5) . ? N2 C12 1.320(7) . ? N2 C8 1.380(6) . ? N3 C13 1.313(7) . ? N3 C5 1.413(6) . ? N4 C13 1.369(7) . ? N4 C6 1.380(5) . ? N4 H4C 0.8600 . ? N5 C14 1.337(7) . ? N5 C22 1.354(5) . ? N6 C25 1.321(7) . ? N6 C21 1.390(5) . ? N7 C26 1.300(7) . ? N7 C19 1.377(5) . ? N8 C26 1.360(7) . ? N8 C18 1.367(5) . ? N8 H8A 0.8600 . ? N9 C27 1.335(7) . ? N9 C35 1.381(6) . ? N10 C38 1.324(6) . ? N10 C34 1.401(5) . ? N11 C39 1.345(6) . ? N11 C31 1.381(5) . ? N11 H11B 0.8600 . ? N12 C39 1.314(6) . ? N12 C32 1.410(5) . ? N13 C40 1.335(7) . ? N13 C48 1.345(5) . ? N14 C51 1.307(7) . ? N14 C47 1.377(6) . ? N15 C52 1.353(6) . ? N15 C44 1.411(6) . ? N15 H15B 0.8600 . ? N16 C52 1.315(7) . ? N16 C45 1.438(6) . ? C1 C2 1.381(8) . ? C1 H1A 0.9300 . ? C2 C3 1.383(7) . ? C2 H2A 0.9300 . ? C3 C4 1.417(6) . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C7 C10 1.4669 . ? C8 C9 1.3900 . ? C10 C11 1.378(6) . ? C10 H10A 0.9300 . ? C11 C12 1.387(6) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.407(7) . ? C14 H14A 0.9300 . ? C15 C16 1.374(6) . ? C15 H15A 0.9300 . ? C16 C17 1.397(6) . ? C16 H16A 0.9300 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 C23 1.5037 . ? C21 C22 1.3900 . ? C23 C24 1.369(6) . ? C23 H23A 0.9300 . ? C24 C25 1.403(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.400(6) . ? C27 H27A 0.9300 . ? C28 C29 1.366(8) . ? C28 H28A 0.9300 . ? C29 C30 1.429(5) . ? C29 H29A 0.9300 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 C36 1.4324 . ? C34 C35 1.3900 . ? C36 C37 1.361(6) . ? C36 H36A 0.9300 . ? C37 C38 1.387(8) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.411(6) . ? C40 H40A 0.9300 . ? C41 C42 1.365(6) . ? C41 H41A 0.9300 . ? C42 C43 1.421(6) . ? C42 H42A 0.9300 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C46 C49 1.4014 . ? C47 C48 1.3900 . ? C49 C50 1.402(6) . ? C49 H49A 0.9300 . ? C50 C51 1.421(6) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? S2 O11 1.443(4) . ? S2 O12 1.451(4) . ? S2 C60 1.753(3) . ? S2 C57 1.759(3) . ? O7 C53 1.257(8) . ? O8 C53 1.245(8) . ? O9 C66 1.240(7) . ? O10 C66 1.271(7) . ? C53 C54 1.529(7) . ? C54 C55 1.3900 . ? C54 C59 1.3900 . ? C55 C56 1.3900 . ? C55 H55A 0.9300 . ? C56 C57 1.3900 . ? C56 H56A 0.9300 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C61 C62 1.3900 . ? C61 H61A 0.9300 . ? C62 C63 1.3900 . ? C62 H62A 0.9300 . ? C63 C64 1.3900 . ? C63 C66 1.519(7) . ? C64 C65 1.3900 . ? C64 H64A 0.9300 . ? C65 H65A 0.9300 . ? O13 H13E 0.8501 . ? O13 H13C 0.8406 . ? O14 H14C 0.8468 . ? O14 H14D 0.8603 . ? O15 H15C 0.8499 . ? O15 H15D 0.8834 . ? O16 H16C 1.1821 . ? O16 H16D 0.8609 . ? O17A H17A 0.8501 . ? O17A H17B 0.8500 . ? O18A H18A 0.8500 . ? O18A H18B 0.8993 . ? O19A H19A 0.8500 . ? O19A H19B 0.7837 . ? O17B H17C 0.8498 . ? O17B H17D 0.8504 . ? O18B H18C 0.8499 . ? O18B H18D 0.8504 . ? 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 O2 Mn1 O5 86.39(15) . . ? O2 Mn1 N2 94.91(18) . . ? O5 Mn1 N2 105.51(16) . . ? O2 Mn1 N5 104.27(17) . . ? O5 Mn1 N5 89.93(16) . . ? N2 Mn1 N5 156.15(19) . . ? O2 Mn1 N1 164.49(16) . . ? O5 Mn1 N1 86.98(16) . . ? N2 Mn1 N1 73.43(19) . . ? N5 Mn1 N1 89.72(18) . . ? O2 Mn1 N6 92.04(17) . . ? O5 Mn1 N6 160.71(16) . . ? N2 Mn1 N6 93.78(18) . . ? N5 Mn1 N6 71.80(19) . . ? N1 Mn1 N6 98.78(17) . . ? O1 Mn2 O6 87.92(15) . . ? O1 Mn2 N14 105.83(17) . . ? O6 Mn2 N14 91.23(17) . . ? O1 Mn2 N10 161.02(15) . . ? O6 Mn2 N10 86.09(15) . . ? N14 Mn2 N10 92.30(17) . . ? O1 Mn2 N13 88.12(17) . . ? O6 Mn2 N13 160.63(16) . . ? N14 Mn2 N13 71.67(19) . . ? N10 Mn2 N13 103.19(16) . . ? O1 Mn2 N9 92.72(17) . . ? O6 Mn2 N9 109.96(15) . . ? N14 Mn2 N9 152.46(18) . . ? N10 Mn2 N9 72.54(18) . . ? N13 Mn2 N9 89.16(18) . . ? O4 S1 O3 112.3(3) . . ? O4 S1 O2 108.5(3) . . ? O3 S1 O2 109.7(3) . . ? O4 S1 O1 109.5(3) . . ? O3 S1 O1 108.7(3) . . ? O2 S1 O1 108.0(2) . . ? S1 O1 Mn2 135.9(3) . . ? S1 O2 Mn1 136.4(3) . . ? Mn1 O5 H5A 103.8 . . ? Mn1 O5 H5B 121.8 . . ? H5A O5 H5B 107.5 . . ? Mn2 O6 H6A 86.0 . . ? Mn2 O6 H6B 123.8 . . ? H6A O6 H6B 129.8 . . ? C1 N1 C9 117.7(5) . . ? C1 N1 Mn1 126.9(5) . . ? C9 N1 Mn1 115.2(3) . . ? C12 N2 C8 119.1(5) . . ? C12 N2 Mn1 127.1(5) . . ? C8 N2 Mn1 113.7(3) . . ? C13 N3 C5 103.0(5) . . ? C13 N4 C6 106.1(5) . . ? C13 N4 H4C 127.0 . . ? C6 N4 H4C 127.0 . . ? C14 N5 C22 118.0(5) . . ? C14 N5 Mn1 124.0(4) . . ? C22 N5 Mn1 117.8(4) . . ? C25 N6 C21 121.0(5) . . ? C25 N6 Mn1 124.1(4) . . ? C21 N6 Mn1 114.8(3) . . ? C26 N7 C19 105.1(6) . . ? C26 N8 C18 107.1(5) . . ? C26 N8 H8A 126.5 . . ? C18 N8 H8A 126.5 . . ? C27 N9 C35 120.6(5) . . ? C27 N9 Mn2 125.0(5) . . ? C35 N9 Mn2 114.1(3) . . ? C38 N10 C34 116.9(5) . . ? C38 N10 Mn2 126.0(4) . . ? C34 N10 Mn2 117.1(3) . . ? C39 N11 C31 106.2(5) . . ? C39 N11 H11B 126.9 . . ? C31 N11 H11B 126.9 . . ? C39 N12 C32 99.3(5) . . ? C40 N13 C48 116.4(5) . . ? C40 N13 Mn2 126.0(4) . . ? C48 N13 Mn2 117.6(4) . . ? C51 N14 C47 121.0(5) . . ? C51 N14 Mn2 124.2(5) . . ? C47 N14 Mn2 114.7(3) . . ? C52 N15 C44 99.8(6) . . ? C52 N15 H15B 130.1 . . ? C44 N15 H15B 130.1 . . ? C52 N16 C45 100.4(6) . . ? N1 C1 C2 124.4(6) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 C3 118.8(7) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C2 C3 C4 118.2(6) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C5 C4 C9 120.0 . . ? C5 C4 C3 121.7(4) . . ? C9 C4 C3 118.3(4) . . ? C4 C5 C6 120.0 . . ? C4 C5 N3 129.4(3) . . ? C6 C5 N3 110.6(3) . . ? N4 C6 C7 134.4(3) . . ? N4 C6 C5 105.6(3) . . ? C7 C6 C5 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 C10 120.6 . . ? C6 C7 C10 119.4 . . ? N2 C8 C7 120.0(3) . . ? N2 C8 C9 119.9(3) . . ? C7 C8 C9 120.0 . . ? N1 C9 C8 117.3(4) . . ? N1 C9 C4 122.6(4) . . ? C8 C9 C4 120.0 . . ? C11 C10 C7 115.5(3) . . ? C11 C10 H10A 122.2 . . ? C7 C10 H10A 122.2 . . ? C10 C11 C12 120.5(6) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? N2 C12 C11 124.0(7) . . ? N2 C12 H12A 118.0 . . ? C11 C12 H12A 118.0 . . ? N3 C13 N4 114.7(6) . . ? N3 C13 H13A 122.6 . . ? N4 C13 H13A 122.6 . . ? N5 C14 C15 123.4(6) . . ? N5 C14 H14A 118.3 . . ? C15 C14 H14A 118.3 . . ? C16 C15 C14 117.7(6) . . ? C16 C15 H15A 121.1 . . ? C14 C15 H15A 121.1 . . ? C15 C16 C17 120.0(6) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 C16 121.3(4) . . ? C22 C17 C16 118.5(4) . . ? N8 C18 C17 135.0(4) . . ? N8 C18 C19 104.9(4) . . ? C17 C18 C19 120.0 . . ? N7 C19 C20 129.9(4) . . ? N7 C19 C18 110.1(4) . . ? C20 C19 C18 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 C23 115.0 . . ? C19 C20 C23 124.9 . . ? N6 C21 C20 122.2(3) . . ? N6 C21 C22 117.8(3) . . ? C20 C21 C22 120.0 . . ? N5 C22 C21 117.6(3) . . ? N5 C22 C17 122.4(3) . . ? C21 C22 C17 120.0 . . ? C24 C23 C20 120.3(4) . . ? C24 C23 H23A 119.8 . . ? C20 C23 H23A 119.8 . . ? C23 C24 C25 119.1(7) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N6 C25 C24 122.3(7) . . ? N6 C25 H25A 118.9 . . ? C24 C25 H25A 118.9 . . ? N7 C26 N8 112.8(6) . . ? N7 C26 H26A 123.6 . . ? N8 C26 H26A 123.6 . . ? N9 C27 C28 122.6(6) . . ? N9 C27 H27A 118.7 . . ? C28 C27 H27A 118.7 . . ? C29 C28 C27 118.2(6) . . ? C29 C28 H28A 120.9 . . ? C27 C28 H28A 120.9 . . ? C28 C29 C30 120.0(6) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 C29 120.7(4) . . ? C35 C30 C29 119.3(4) . . ? N11 C31 C30 136.7(4) . . ? N11 C31 C32 103.3(4) . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 N12 126.3(3) . . ? C31 C32 N12 113.7(3) . . ? C34 C33 C32 120.0 . . ? C34 C33 C36 111.5 . . ? C32 C33 C36 128.4 . . ? C33 C34 C35 120.0 . . ? C33 C34 N10 124.8(3) . . ? C35 C34 N10 115.2(3) . . ? N9 C35 C34 120.7(3) . . ? N9 C35 C30 119.3(3) . . ? C34 C35 C30 120.0 . . ? C37 C36 C33 126.6(4) . . ? C37 C36 H36A 116.7 . . ? C33 C36 H36A 116.7 . . ? C36 C37 C38 114.6(6) . . ? C36 C37 H37A 122.7 . . ? C38 C37 H37A 122.7 . . ? N10 C38 C37 125.3(6) . . ? N10 C38 H38A 117.3 . . ? C37 C38 H38A 117.3 . . ? N12 C39 N11 117.5(6) . . ? N12 C39 H39A 121.2 . . ? N11 C39 H39A 121.2 . . ? N13 C40 C41 126.1(6) . . ? N13 C40 H40A 117.0 . . ? C41 C40 H40A 117.0 . . ? C42 C41 C40 114.5(7) . . ? C42 C41 H41A 122.7 . . ? C40 C41 H41A 122.7 . . ? C41 C42 C43 122.9(6) . . ? C41 C42 H42A 118.6 . . ? C43 C42 H42A 118.6 . . ? C44 C43 C48 120.0 . . ? C44 C43 C42 124.4(4) . . ? C48 C43 C42 115.6(4) . . ? C43 C44 C45 120.0 . . ? C43 C44 N15 130.0(4) . . ? C45 C44 N15 110.0(4) . . ? C44 C45 C46 120.0 . . ? C44 C45 N16 108.4(4) . . ? C46 C45 N16 131.6(4) . . ? C47 C46 C45 120.0 . . ? C47 C46 C49 119.9 . . ? C45 C46 C49 119.5 . . ? N14 C47 C46 119.8(3) . . ? N14 C47 C48 120.1(3) . . ? C46 C47 C48 120.0 . . ? N13 C48 C47 115.6(4) . . ? N13 C48 C43 124.4(4) . . ? C47 C48 C43 120.0 . . ? C46 C49 C50 118.8(4) . . ? C46 C49 H49A 120.6 . . ? C50 C49 H49A 120.6 . . ? C49 C50 C51 117.8(6) . . ? C49 C50 H50A 121.1 . . ? C51 C50 H50A 121.1 . . ? N14 C51 C50 122.2(7) . . ? N14 C51 H51A 118.9 . . ? C50 C51 H51A 118.9 . . ? N16 C52 N15 121.4(7) . . ? N16 C52 H52A 119.3 . . ? N15 C52 H52A 119.3 . . ? O11 S2 O12 119.7(2) . . ? O11 S2 C60 108.9(3) . . ? O12 S2 C60 107.2(2) . . ? O11 S2 C57 107.1(2) . . ? O12 S2 C57 107.9(3) . . ? C60 S2 C57 105.18(17) . . ? O8 C53 O7 124.5(7) . . ? O8 C53 C54 118.0(7) . . ? O7 C53 C54 117.5(7) . . ? C55 C54 C59 120.0 . . ? C55 C54 C53 119.9(5) . . ? C59 C54 C53 120.0(5) . . ? C54 C55 C56 120.0 . . ? C54 C55 H55A 120.0 . . ? C56 C55 H55A 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 S2 119.2(3) . . ? C58 C57 S2 120.8(3) . . ? C59 C58 C57 120.0 . . ? C59 C58 H58A 120.0 . . ? C57 C58 H58A 120.0 . . ? C58 C59 C54 120.0 . . ? C58 C59 H59A 120.0 . . ? C54 C59 H59A 120.0 . . ? C61 C60 C65 120.0 . . ? C61 C60 S2 120.2(3) . . ? C65 C60 S2 119.8(3) . . ? C62 C61 C60 120.0 . . ? C62 C61 H61A 120.0 . . ? C60 C61 H61A 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 C66 120.4(4) . . ? C62 C63 C66 119.6(4) . . ? C63 C64 C65 120.0 . . ? C63 C64 H64A 120.0 . . ? C65 C64 H64A 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 H65A 120.0 . . ? C60 C65 H65A 120.0 . . ? O9 C66 O10 125.2(7) . . ? O9 C66 C63 117.6(6) . . ? O10 C66 C63 117.1(6) . . ? H13E O13 H13C 106.6 . . ? H14C O14 H14D 124.2 . . ? H15C O15 H15D 109.7 . . ? H16C O16 H16D 96.7 . . ? H17A O17A H17B 103.0 . . ? H18A O18A H18B 107.7 . . ? H19A O19A H19B 112.5 . . ? H17C O17B H17D 109.5 . . ? H18C O18B H18D 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Mn2 -2.3(4) . . . . ? O3 S1 O1 Mn2 120.7(4) . . . . ? O2 S1 O1 Mn2 -120.3(3) . . . . ? O6 Mn2 O1 S1 -24.7(3) . . . . ? N14 Mn2 O1 S1 -115.4(4) . . . . ? N10 Mn2 O1 S1 46.9(7) . . . . ? N13 Mn2 O1 S1 174.2(4) . . . . ? N9 Mn2 O1 S1 85.1(4) . . . . ? O4 S1 O2 Mn1 127.7(4) . . . . ? O3 S1 O2 Mn1 4.7(5) . . . . ? O1 S1 O2 Mn1 -113.7(4) . . . . ? O5 Mn1 O2 S1 -29.8(4) . . . . ? N2 Mn1 O2 S1 75.5(4) . . . . ? N5 Mn1 O2 S1 -118.8(4) . . . . ? N1 Mn1 O2 S1 35.1(9) . . . . ? N6 Mn1 O2 S1 169.5(4) . . . . ? O2 Mn1 N1 C1 -136.6(6) . . . . ? O5 Mn1 N1 C1 -71.8(5) . . . . ? N2 Mn1 N1 C1 -179.0(5) . . . . ? N5 Mn1 N1 C1 18.1(5) . . . . ? N6 Mn1 N1 C1 89.7(5) . . . . ? O2 Mn1 N1 C9 38.1(8) . . . . ? O5 Mn1 N1 C9 102.9(3) . . . . ? N2 Mn1 N1 C9 -4.3(3) . . . . ? N5 Mn1 N1 C9 -167.2(3) . . . . ? N6 Mn1 N1 C9 -95.7(3) . . . . ? O2 Mn1 N2 C12 14.0(5) . . . . ? O5 Mn1 N2 C12 101.6(5) . . . . ? N5 Mn1 N2 C12 -129.7(6) . . . . ? N1 Mn1 N2 C12 -176.4(5) . . . . ? N6 Mn1 N2 C12 -78.4(5) . . . . ? O2 Mn1 N2 C8 -168.9(3) . . . . ? O5 Mn1 N2 C8 -81.3(3) . . . . ? N5 Mn1 N2 C8 47.4(7) . . . . ? N1 Mn1 N2 C8 0.7(3) . . . . ? N6 Mn1 N2 C8 98.7(3) . . . . ? O2 Mn1 N5 C14 94.9(5) . . . . ? O5 Mn1 N5 C14 8.7(5) . . . . ? N2 Mn1 N5 C14 -122.6(6) . . . . ? N1 Mn1 N5 C14 -78.3(5) . . . . ? N6 Mn1 N5 C14 -177.7(6) . . . . ? O2 Mn1 N5 C22 -90.0(4) . . . . ? O5 Mn1 N5 C22 -176.2(4) . . . . ? N2 Mn1 N5 C22 52.6(7) . . . . ? N1 Mn1 N5 C22 96.8(4) . . . . ? N6 Mn1 N5 C22 -2.5(4) . . . . ? O2 Mn1 N6 C25 -75.4(5) . . . . ? O5 Mn1 N6 C25 -160.3(5) . . . . ? N2 Mn1 N6 C25 19.7(5) . . . . ? N5 Mn1 N6 C25 -179.8(6) . . . . ? N1 Mn1 N6 C25 93.5(5) . . . . ? O2 Mn1 N6 C21 108.2(3) . . . . ? O5 Mn1 N6 C21 23.3(7) . . . . ? N2 Mn1 N6 C21 -156.7(3) . . . . ? N5 Mn1 N6 C21 3.9(3) . . . . ? N1 Mn1 N6 C21 -82.9(4) . . . . ? O1 Mn2 N9 C27 13.7(5) . . . . ? O6 Mn2 N9 C27 102.5(5) . . . . ? N14 Mn2 N9 C27 -119.3(5) . . . . ? N10 Mn2 N9 C27 -178.5(5) . . . . ? N13 Mn2 N9 C27 -74.4(5) . . . . ? O1 Mn2 N9 C35 -173.1(3) . . . . ? O6 Mn2 N9 C35 -84.4(3) . . . . ? N14 Mn2 N9 C35 53.9(6) . . . . ? N10 Mn2 N9 C35 -5.3(3) . . . . ? N13 Mn2 N9 C35 98.8(3) . . . . ? O1 Mn2 N10 C38 -136.2(5) . . . . ? O6 Mn2 N10 C38 -64.3(4) . . . . ? N14 Mn2 N10 C38 26.8(5) . . . . ? N13 Mn2 N10 C38 98.5(5) . . . . ? N9 Mn2 N10 C38 -176.6(5) . . . . ? O1 Mn2 N10 C34 43.0(7) . . . . ? O6 Mn2 N10 C34 114.9(3) . . . . ? N14 Mn2 N10 C34 -154.0(3) . . . . ? N13 Mn2 N10 C34 -82.3(3) . . . . ? N9 Mn2 N10 C34 2.6(3) . . . . ? O1 Mn2 N13 C40 -69.5(5) . . . . ? O6 Mn2 N13 C40 -147.8(5) . . . . ? N14 Mn2 N13 C40 -176.8(6) . . . . ? N10 Mn2 N13 C40 95.1(5) . . . . ? N9 Mn2 N13 C40 23.3(5) . . . . ? O1 Mn2 N13 C48 108.9(4) . . . . ? O6 Mn2 N13 C48 30.6(8) . . . . ? N14 Mn2 N13 C48 1.5(4) . . . . ? N10 Mn2 N13 C48 -86.5(4) . . . . ? N9 Mn2 N13 C48 -158.4(4) . . . . ? O1 Mn2 N14 C51 95.3(5) . . . . ? O6 Mn2 N14 C51 7.2(5) . . . . ? N10 Mn2 N14 C51 -79.0(5) . . . . ? N13 Mn2 N14 C51 177.9(6) . . . . ? N9 Mn2 N14 C51 -134.1(5) . . . . ? O1 Mn2 N14 C47 -86.9(4) . . . . ? O6 Mn2 N14 C47 -175.1(4) . . . . ? N10 Mn2 N14 C47 98.8(4) . . . . ? N13 Mn2 N14 C47 -4.4(3) . . . . ? N9 Mn2 N14 C47 43.7(6) . . . . ? C9 N1 C1 C2 -0.6(9) . . . . ? Mn1 N1 C1 C2 173.9(4) . . . . ? N1 C1 C2 C3 -0.2(10) . . . . ? C1 C2 C3 C4 1.1(9) . . . . ? C2 C3 C4 C5 176.9(4) . . . . ? C2 C3 C4 C9 -1.2(7) . . . . ? C9 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C6 -178.1(4) . . . . ? C9 C4 C5 N3 -179.6(4) . . . . ? C3 C4 C5 N3 2.3(5) . . . . ? C13 N3 C5 C4 -179.3(4) . . . . ? C13 N3 C5 C6 1.0(5) . . . . ? C13 N4 C6 C7 179.6(4) . . . . ? C13 N4 C6 C5 0.0(4) . . . . ? C4 C5 C6 N4 179.7(3) . . . . ? N3 C5 C6 N4 -0.6(3) . . . . ? C4 C5 C6 C7 0.0 . . . . ? N3 C5 C6 C7 179.7(4) . . . . ? N4 C6 C7 C8 -179.6(4) . . . . ? C5 C6 C7 C8 0.0 . . . . ? N4 C6 C7 C10 0.7(4) . . . . ? C5 C6 C7 C10 -179.7 . . . . ? C12 N2 C8 C7 -4.6(7) . . . . ? Mn1 N2 C8 C7 178.06(18) . . . . ? C12 N2 C8 C9 -179.6(4) . . . . ? Mn1 N2 C8 C9 3.1(4) . . . . ? C6 C7 C8 N2 -175.0(4) . . . . ? C10 C7 C8 N2 4.7(4) . . . . ? C6 C7 C8 C9 0.0 . . . . ? C10 C7 C8 C9 179.7 . . . . ? C1 N1 C9 C8 -177.3(4) . . . . ? Mn1 N1 C9 C8 7.5(4) . . . . ? C1 N1 C9 C4 0.4(6) . . . . ? Mn1 N1 C9 C4 -174.76(19) . . . . ? N2 C8 C9 N1 -7.2(4) . . . . ? C7 C8 C9 N1 177.8(4) . . . . ? N2 C8 C9 C4 175.0(4) . . . . ? C7 C8 C9 C4 0.0 . . . . ? C5 C4 C9 N1 -177.7(4) . . . . ? C3 C4 C9 N1 0.5(4) . . . . ? C5 C4 C9 C8 0.0 . . . . ? C3 C4 C9 C8 178.2(4) . . . . ? C8 C7 C10 C11 -0.9(4) . . . . ? C6 C7 C10 C11 178.8(4) . . . . ? C7 C10 C11 C12 -3.1(8) . . . . ? C8 N2 C12 C11 0.6(9) . . . . ? Mn1 N2 C12 C11 177.6(5) . . . . ? C10 C11 C12 N2 3.4(10) . . . . ? C5 N3 C13 N4 -1.1(7) . . . . ? C6 N4 C13 N3 0.7(7) . . . . ? C22 N5 C14 C15 0.0(9) . . . . ? Mn1 N5 C14 C15 175.1(5) . . . . ? N5 C14 C15 C16 0.7(10) . . . . ? C14 C15 C16 C17 0.6(10) . . . . ? C15 C16 C17 C18 -177.4(5) . . . . ? C15 C16 C17 C22 -2.5(8) . . . . ? C26 N8 C18 C17 -179.6(4) . . . . ? C26 N8 C18 C19 -2.4(5) . . . . ? C22 C17 C18 N8 176.9(5) . . . . ? C16 C17 C18 N8 -8.2(6) . . . . ? C22 C17 C18 C19 0.0 . . . . ? C16 C17 C18 C19 174.8(4) . . . . ? C26 N7 C19 C20 179.1(4) . . . . ? C26 N7 C19 C18 -0.2(5) . . . . ? N8 C18 C19 N7 1.7(4) . . . . ? C17 C18 C19 N7 179.4(4) . . . . ? N8 C18 C19 C20 -177.8(4) . . . . ? C17 C18 C19 C20 0.0 . . . . ? N7 C19 C20 C21 -179.3(5) . . . . ? C18 C19 C20 C21 0.0 . . . . ? N7 C19 C20 C23 -3.4(5) . . . . ? C18 C19 C20 C23 175.9 . . . . ? C25 N6 C21 C20 -0.3(7) . . . . ? Mn1 N6 C21 C20 176.2(2) . . . . ? C25 N6 C21 C22 178.5(5) . . . . ? Mn1 N6 C21 C22 -5.0(4) . . . . ? C19 C20 C21 N6 178.8(4) . . . . ? C23 C20 C21 N6 2.5(4) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C23 C20 C21 C22 -176.3 . . . . ? C14 N5 C22 C21 176.3(4) . . . . ? Mn1 N5 C22 C21 0.9(5) . . . . ? C14 N5 C22 C17 -2.0(7) . . . . ? Mn1 N5 C22 C17 -177.4(2) . . . . ? N6 C21 C22 N5 2.8(4) . . . . ? C20 C21 C22 N5 -178.3(4) . . . . ? N6 C21 C22 C17 -178.9(4) . . . . ? C20 C21 C22 C17 0.0 . . . . ? C18 C17 C22 N5 178.2(4) . . . . ? C16 C17 C22 N5 3.2(5) . . . . ? C18 C17 C22 C21 0.0 . . . . ? C16 C17 C22 C21 -175.0(4) . . . . ? C21 C20 C23 C24 -3.5(5) . . . . ? C19 C20 C23 C24 -179.5(5) . . . . ? C20 C23 C24 C25 2.2(9) . . . . ? C21 N6 C25 C24 -1.2(10) . . . . ? Mn1 N6 C25 C24 -177.4(5) . . . . ? C23 C24 C25 N6 0.2(11) . . . . ? C19 N7 C26 N8 -1.4(8) . . . . ? C18 N8 C26 N7 2.5(8) . . . . ? C35 N9 C27 C28 -1.0(9) . . . . ? Mn2 N9 C27 C28 171.7(4) . . . . ? N9 C27 C28 C29 1.7(10) . . . . ? C27 C28 C29 C30 0.4(9) . . . . ? C28 C29 C30 C31 177.4(5) . . . . ? C28 C29 C30 C35 -3.0(7) . . . . ? C39 N11 C31 C30 180.0(4) . . . . ? C39 N11 C31 C32 1.0(5) . . . . ? C35 C30 C31 N11 -178.8(5) . . . . ? C29 C30 C31 N11 0.8(5) . . . . ? C35 C30 C31 C32 0.0 . . . . ? C29 C30 C31 C32 179.5(4) . . . . ? N11 C31 C32 C33 179.1(3) . . . . ? C30 C31 C32 C33 0.0 . . . . ? N11 C31 C32 N12 -2.0(3) . . . . ? C30 C31 C32 N12 178.8(4) . . . . ? C39 N12 C32 C33 -179.2(4) . . . . ? C39 N12 C32 C31 2.1(5) . . . . ? C31 C32 C33 C34 0.0 . . . . ? N12 C32 C33 C34 -178.7(4) . . . . ? C31 C32 C33 C36 176.7 . . . . ? N12 C32 C33 C36 -2.0(4) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C36 C33 C34 C35 -177.2 . . . . ? C32 C33 C34 N10 -177.1(4) . . . . ? C36 C33 C34 N10 5.6(4) . . . . ? C38 N10 C34 C33 -2.9(6) . . . . ? Mn2 N10 C34 C33 177.84(19) . . . . ? C38 N10 C34 C35 179.8(4) . . . . ? Mn2 N10 C34 C35 0.6(3) . . . . ? C27 N9 C35 C34 -178.5(4) . . . . ? Mn2 N9 C35 C34 8.0(4) . . . . ? C27 N9 C35 C30 -1.7(6) . . . . ? Mn2 N9 C35 C30 -175.20(17) . . . . ? C33 C34 C35 N9 176.7(4) . . . . ? N10 C34 C35 N9 -5.9(3) . . . . ? C33 C34 C35 C30 0.0 . . . . ? N10 C34 C35 C30 177.4(3) . . . . ? C31 C30 C35 N9 -176.8(4) . . . . ? C29 C30 C35 N9 3.7(4) . . . . ? C31 C30 C35 C34 0.0 . . . . ? C29 C30 C35 C34 -179.5(4) . . . . ? C34 C33 C36 C37 -5.3(4) . . . . ? C32 C33 C36 C37 177.8(4) . . . . ? C33 C36 C37 C38 2.1(7) . . . . ? C34 N10 C38 C37 -1.0(8) . . . . ? Mn2 N10 C38 C37 178.1(4) . . . . ? C36 C37 C38 N10 1.4(9) . . . . ? C32 N12 C39 N11 -1.4(7) . . . . ? C31 N11 C39 N12 0.3(7) . . . . ? C48 N13 C40 C41 -0.9(10) . . . . ? Mn2 N13 C40 C41 177.5(5) . . . . ? N13 C40 C41 C42 3.2(11) . . . . ? C40 C41 C42 C43 -2.1(10) . . . . ? C41 C42 C43 C44 179.6(5) . . . . ? C41 C42 C43 C48 -1.1(8) . . . . ? C48 C43 C44 C45 0.0 . . . . ? C42 C43 C44 C45 179.2(4) . . . . ? C48 C43 C44 N15 176.9(5) . . . . ? C42 C43 C44 N15 -3.8(6) . . . . ? C52 N15 C44 C43 -178.6(4) . . . . ? C52 N15 C44 C45 -1.5(5) . . . . ? C43 C44 C45 C46 0.0 . . . . ? N15 C44 C45 C46 -177.5(4) . . . . ? C43 C44 C45 N16 178.9(4) . . . . ? N15 C44 C45 N16 1.4(4) . . . . ? C52 N16 C45 C44 -0.7(6) . . . . ? C52 N16 C45 C46 178.0(5) . . . . ? C44 C45 C46 C47 0.0 . . . . ? N16 C45 C46 C47 -178.6(5) . . . . ? C44 C45 C46 C49 -171.1 . . . . ? N16 C45 C46 C49 10.3(5) . . . . ? C51 N14 C47 C46 1.9(7) . . . . ? Mn2 N14 C47 C46 -175.9(2) . . . . ? C51 N14 C47 C48 -174.9(5) . . . . ? Mn2 N14 C47 C48 7.2(4) . . . . ? C45 C46 C47 N14 -176.9(4) . . . . ? C49 C46 C47 N14 -5.8(4) . . . . ? C45 C46 C47 C48 0.0 . . . . ? C49 C46 C47 C48 171.0 . . . . ? C40 N13 C48 C47 -179.9(4) . . . . ? Mn2 N13 C48 C47 1.6(4) . . . . ? C40 N13 C48 C43 -2.9(7) . . . . ? Mn2 N13 C48 C43 178.6(2) . . . . ? N14 C47 C48 N13 -6.0(4) . . . . ? C46 C47 C48 N13 177.2(4) . . . . ? N14 C47 C48 C43 176.9(4) . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 N13 -176.9(5) . . . . ? C42 C43 C48 N13 3.8(5) . . . . ? C44 C43 C48 C47 0.0 . . . . ? C42 C43 C48 C47 -179.3(4) . . . . ? C47 C46 C49 C50 8.4(5) . . . . ? C45 C46 C49 C50 179.5(5) . . . . ? C46 C49 C50 C51 -7.0(8) . . . . ? C47 N14 C51 C50 -0.7(10) . . . . ? Mn2 N14 C51 C50 176.9(4) . . . . ? C49 C50 C51 N14 3.3(10) . . . . ? C45 N16 C52 N15 -0.3(9) . . . . ? C44 N15 C52 N16 1.1(9) . . . . ? O8 C53 C54 C55 5.1(7) . . . . ? O7 C53 C54 C55 -176.5(4) . . . . ? O8 C53 C54 C59 -173.0(5) . . . . ? O7 C53 C54 C59 5.4(7) . . . . ? C59 C54 C55 C56 0.0 . . . . ? C53 C54 C55 C56 -178.1(4) . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C58 0.0 . . . . ? C55 C56 C57 S2 178.8(3) . . . . ? O11 S2 C57 C56 -162.5(2) . . . . ? O12 S2 C57 C56 -32.4(3) . . . . ? C60 S2 C57 C56 81.8(3) . . . . ? O11 S2 C57 C58 16.3(3) . . . . ? O12 S2 C57 C58 146.4(2) . . . . ? C60 S2 C57 C58 -99.4(3) . . . . ? C56 C57 C58 C59 0.0 . . . . ? S2 C57 C58 C59 -178.8(3) . . . . ? C57 C58 C59 C54 0.0 . . . . ? C55 C54 C59 C58 0.0 . . . . ? C53 C54 C59 C58 178.1(4) . . . . ? O11 S2 C60 C61 154.6(2) . . . . ? O12 S2 C60 C61 23.8(3) . . . . ? C57 S2 C60 C61 -90.9(3) . . . . ? O11 S2 C60 C65 -25.0(3) . . . . ? O12 S2 C60 C65 -155.8(2) . . . . ? C57 S2 C60 C65 89.6(3) . . . . ? C65 C60 C61 C62 0.0 . . . . ? S2 C60 C61 C62 -179.6(3) . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C61 C62 C63 C66 179.4(4) . . . . ? C62 C63 C64 C65 0.0 . . . . ? C66 C63 C64 C65 -179.4(4) . . . . ? C63 C64 C65 C60 0.0 . . . . ? C61 C60 C65 C64 0.0 . . . . ? S2 C60 C65 C64 179.6(3) . . . . ? C64 C63 C66 O9 -1.6(7) . . . . ? C62 C63 C66 O9 179.0(4) . . . . ? C64 C63 C66 O10 175.5(4) . . . . ? C62 C63 C66 O10 -3.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.465 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.076 # Attachment '7.cif' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 710089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Mn N8 O2, C14 H6 Mn N2 O8, 4(H2 O)' _chemical_formula_sum 'C40 H34 Mn2 N10 O14' _chemical_formula_weight 988.65 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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.337(3) _cell_length_b 17.261(3) _cell_length_c 17.477(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.743(5) _cell_angle_gamma 90.00 _cell_volume 4014.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3728 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8196 _exptl_absorpt_correction_T_max 0.8882 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 10239 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3728 _reflns_number_gt 2109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0749P)^2^] 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 3728 _refine_ls_number_parameters 321 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.820 _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 C1 C -0.1745(3) 0.1934(2) 0.36587(19) 0.0503(9) Uani 1 1 d . . . H1 H -0.2118 0.2166 0.3252 0.060 Uiso 1 1 calc R . . C2 C -0.2186(2) 0.1848(2) 0.43494(19) 0.0509(9) Uani 1 1 d . . . H2 H -0.2847 0.2004 0.4396 0.061 Uiso 1 1 calc R . . C3 C -0.1646(2) 0.1532(2) 0.49611(19) 0.0474(9) Uani 1 1 d . . . H3 H -0.1933 0.1472 0.5428 0.057 Uiso 1 1 calc R . . C4 C -0.0654(2) 0.12985(19) 0.48775(18) 0.0408(8) Uani 1 1 d . . . C5 C -0.0276(2) 0.13802(18) 0.41504(17) 0.0392(8) Uani 1 1 d . . . C6 C 0.0727(2) 0.11073(18) 0.40031(18) 0.0397(7) Uani 1 1 d . . . C7 C 0.1362(2) 0.07864(18) 0.45982(17) 0.0386(8) Uani 1 1 d . . . C8 C 0.2303(2) 0.05151(19) 0.44171(19) 0.0457(9) Uani 1 1 d . . . H8 H 0.2743 0.0304 0.4796 0.055 Uiso 1 1 calc R . . C9 C 0.2567(3) 0.05623(19) 0.36848(19) 0.0479(9) Uani 1 1 d . . . H9 H 0.3188 0.0377 0.3556 0.058 Uiso 1 1 calc R . . C10 C 0.1914(2) 0.08846(19) 0.31292(19) 0.0445(8) Uani 1 1 d . . . H10 H 0.2113 0.0914 0.2630 0.053 Uiso 1 1 calc R . . C11 C 0.0009(2) 0.09789(19) 0.54788(17) 0.0412(8) Uani 1 1 d . . . C12 C 0.0966(2) 0.07531(18) 0.53343(18) 0.0418(8) Uani 1 1 d . . . C13 C 0.0702(3) 0.0567(2) 0.65269(19) 0.0522(9) Uani 1 1 d . . . H13 H 0.0813 0.0430 0.7040 0.063 Uiso 1 1 calc R . . C14 C 0.3870(3) 0.0559(2) 0.1335(2) 0.0484(9) Uani 1 1 d . . . C15 C 0.4544(2) 0.1042(2) 0.08546(18) 0.0433(8) Uani 1 1 d . . . C16 C 0.4586(3) 0.1003(2) 0.00745(19) 0.0556(10) Uani 1 1 d . . . H16 H 0.4168 0.0666 -0.0213 0.067 Uiso 1 1 calc R . . C17 C 0.5258(3) 0.1471(2) -0.0283(2) 0.0579(10) Uani 1 1 d . . . H17 H 0.5284 0.1461 -0.0813 0.069 Uiso 1 1 calc R . . C18 C 0.5888(3) 0.1953(2) 0.01579(19) 0.0517(9) Uani 1 1 d . . . H18 H 0.6357 0.2263 -0.0069 0.062 Uiso 1 1 calc R . . C19 C 0.5809(2) 0.19667(19) 0.09402(18) 0.0423(8) Uani 1 1 d . . . C20 C 0.6489(3) 0.2418(2) 0.1507(2) 0.0475(9) Uani 1 1 d . . . Mn1 Mn 0.0000 0.19323(4) 0.2500 0.0419(2) Uani 1 2 d S . . Mn2 Mn 0.5000 0.16000(4) 0.2500 0.0437(2) Uani 1 2 d S . . N1 N -0.08185(19) 0.17030(16) 0.35493(14) 0.0426(7) Uani 1 1 d . . . N2 N 0.10085(19) 0.11575(15) 0.32756(14) 0.0419(7) Uani 1 1 d . . . N3 N 0.51314(19) 0.15317(15) 0.12728(14) 0.0391(6) Uani 1 1 d . . . N4 N -0.0169(2) 0.08609(16) 0.62410(15) 0.0504(7) Uani 1 1 d . . . N5 N 0.1390(2) 0.04858(18) 0.60308(17) 0.0485(7) Uani 1 1 d D . . O1 O 0.39258(17) 0.06934(13) 0.20437(12) 0.0508(6) Uani 1 1 d . . . O2 O 0.3320(2) 0.00698(16) 0.09991(14) 0.0694(8) Uani 1 1 d . . . O3 O 0.62414(17) 0.23937(14) 0.22007(13) 0.0546(6) Uani 1 1 d . . . O4 O 0.72363(18) 0.27369(15) 0.12700(14) 0.0607(7) Uani 1 1 d . . . O1W O 0.09669(17) 0.28530(14) 0.29206(14) 0.0527(6) Uani 1 1 d D . . H1W H 0.098(3) 0.3288(14) 0.274(2) 0.079 Uiso 1 1 d D . . H2W H 0.1531(19) 0.2774(19) 0.3163(19) 0.079 Uiso 1 1 d D . . O2W O 0.1124(2) 0.41878(16) 0.21377(18) 0.0712(8) Uani 1 1 d D . . H3W H 0.1708(19) 0.413(3) 0.200(2) 0.107 Uiso 1 1 d D . . H4W H 0.113(3) 0.456(2) 0.245(2) 0.107 Uiso 1 1 d D . . O3W O 0.3048(2) 0.36727(17) 0.19092(16) 0.0676(8) Uani 1 1 d D . . H5W H 0.359(2) 0.377(2) 0.165(2) 0.101 Uiso 1 1 d D . . H6W H 0.324(3) 0.3264(18) 0.215(2) 0.101 Uiso 1 1 d D . . H5A H 0.1997(16) 0.035(2) 0.609(2) 0.065(12) Uiso 1 1 d 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 C1 0.041(2) 0.061(2) 0.048(2) -0.0025(18) -0.0006(17) 0.0068(18) C2 0.0305(19) 0.068(3) 0.055(2) -0.0080(19) 0.0066(17) 0.0050(17) C3 0.037(2) 0.060(2) 0.046(2) -0.0047(17) 0.0074(16) 0.0010(17) C4 0.0330(18) 0.046(2) 0.0433(19) -0.0040(15) 0.0022(15) -0.0027(15) C5 0.0357(19) 0.042(2) 0.0392(18) -0.0040(15) 0.0010(14) -0.0022(15) C6 0.0353(18) 0.0426(19) 0.0413(19) -0.0021(15) 0.0030(15) -0.0011(15) C7 0.0355(18) 0.0399(19) 0.0402(18) -0.0020(15) 0.0012(14) 0.0002(15) C8 0.0316(19) 0.051(2) 0.054(2) -0.0032(16) -0.0016(16) 0.0067(15) C9 0.0346(19) 0.055(2) 0.055(2) -0.0040(17) 0.0069(16) 0.0068(16) C10 0.040(2) 0.051(2) 0.0433(19) -0.0018(16) 0.0090(15) 0.0028(16) C11 0.0406(19) 0.047(2) 0.0358(18) -0.0027(15) 0.0029(15) -0.0041(15) C12 0.043(2) 0.043(2) 0.0390(18) -0.0004(15) -0.0018(15) -0.0015(16) C13 0.064(3) 0.058(2) 0.0337(19) 0.0047(16) -0.0015(18) 0.0002(19) C14 0.034(2) 0.061(2) 0.049(2) -0.0014(18) 0.0031(16) -0.0027(17) C15 0.0326(18) 0.056(2) 0.0412(19) -0.0037(16) 0.0007(15) -0.0014(16) C16 0.056(2) 0.067(3) 0.044(2) -0.0072(18) -0.0006(18) -0.0087(19) C17 0.063(3) 0.072(3) 0.0385(19) -0.0006(18) 0.0054(18) -0.003(2) C18 0.047(2) 0.061(2) 0.047(2) 0.0100(18) 0.0052(17) -0.0009(18) C19 0.0377(19) 0.045(2) 0.0440(19) 0.0051(16) 0.0021(15) 0.0024(16) C20 0.045(2) 0.044(2) 0.052(2) 0.0076(17) -0.0022(17) 0.0009(17) Mn1 0.0370(4) 0.0520(5) 0.0365(4) 0.000 0.0014(3) 0.000 Mn2 0.0413(4) 0.0540(5) 0.0356(4) 0.000 0.0011(3) 0.000 N1 0.0351(16) 0.0526(18) 0.0398(15) 0.0011(13) 0.0006(12) 0.0066(13) N2 0.0362(16) 0.0488(17) 0.0412(16) 0.0014(13) 0.0060(12) 0.0012(13) N3 0.0329(15) 0.0461(17) 0.0379(15) 0.0024(13) 0.0000(12) -0.0043(13) N4 0.0510(18) 0.060(2) 0.0403(16) 0.0033(14) 0.0058(14) 0.0008(15) N5 0.044(2) 0.0546(19) 0.0466(17) 0.0015(14) 0.0005(16) 0.0067(15) O1 0.0482(14) 0.0647(16) 0.0401(14) -0.0024(11) 0.0065(11) -0.0132(12) O2 0.0633(17) 0.086(2) 0.0579(16) -0.0095(14) 0.0001(13) -0.0335(16) O3 0.0517(15) 0.0617(16) 0.0496(15) -0.0019(12) -0.0039(12) -0.0120(12) O4 0.0443(15) 0.0722(18) 0.0651(16) 0.0122(14) 0.0011(12) -0.0183(13) O1W 0.0456(15) 0.0534(16) 0.0578(16) 0.0020(12) -0.0058(12) -0.0032(12) O2W 0.0693(19) 0.0624(19) 0.084(2) 0.0019(15) 0.0186(16) -0.0042(15) O3W 0.0574(17) 0.082(2) 0.0644(18) 0.0157(15) 0.0119(14) 0.0026(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 C1 N1 1.325(4) . ? C1 C2 1.385(4) . ? C1 H1 0.9300 . ? C2 C3 1.364(5) . ? C2 H2 0.9300 . ? C3 C4 1.399(4) . ? C3 H3 0.9300 . ? C4 C5 1.405(4) . ? C4 C11 1.438(4) . ? C5 N1 1.356(4) . ? C5 C6 1.457(4) . ? C6 N2 1.352(4) . ? C6 C7 1.411(4) . ? C7 C8 1.394(4) . ? C7 C12 1.424(4) . ? C8 C9 1.352(5) . ? C8 H8 0.9300 . ? C9 C10 1.378(5) . ? C9 H9 0.9300 . ? C10 N2 1.337(4) . ? C10 H10 0.9300 . ? C11 C12 1.374(4) . ? C11 N4 1.383(4) . ? C12 N5 1.387(4) . ? C13 N5 1.311(4) . ? C13 N4 1.334(4) . ? C13 H13 0.9300 . ? C14 O2 1.241(4) . ? C14 O1 1.257(4) . ? C14 C15 1.518(5) . ? C15 N3 1.338(4) . ? C15 C16 1.370(4) . ? C16 C17 1.385(5) . ? C16 H16 0.9300 . ? C17 C18 1.381(5) . ? C17 H17 0.9300 . ? C18 C19 1.378(4) . ? C18 H18 0.9300 . ? C19 N3 1.337(4) . ? C19 C20 1.514(5) . ? C20 O4 1.234(4) . ? C20 O3 1.278(4) . ? Mn1 O1W 2.146(2) . ? Mn1 O1W 2.146(2) 2 ? Mn1 N1 2.230(3) 2 ? Mn1 N1 2.230(3) . ? Mn1 N2 2.280(3) 2 ? Mn1 N2 2.280(3) . ? Mn2 N3 2.167(2) . ? Mn2 N3 2.167(2) 2_655 ? Mn2 O1 2.233(2) . ? Mn2 O1 2.233(2) 2_655 ? Mn2 O3 2.237(2) . ? Mn2 O3 2.237(2) 2_655 ? N5 H5A 0.844(18) . ? O1W H1W 0.817(18) . ? O1W H2W 0.850(17) . ? O2W H3W 0.836(18) . ? O2W H4W 0.840(18) . ? O3W H5W 0.887(18) . ? O3W H6W 0.855(18) . ? 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 N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 117.6(3) . . ? C3 C4 C11 125.0(3) . . ? C5 C4 C11 117.4(3) . . ? N1 C5 C4 122.5(3) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 121.0(3) . . ? N2 C6 C7 121.9(3) . . ? N2 C6 C5 117.4(3) . . ? C7 C6 C5 120.7(3) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 C12 125.8(3) . . ? C6 C7 C12 116.2(3) . . ? C9 C8 C7 119.2(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.0(3) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N2 C10 C9 123.0(3) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C12 C11 N4 110.8(3) . . ? C12 C11 C4 120.6(3) . . ? N4 C11 C4 128.6(3) . . ? C11 C12 N5 105.3(3) . . ? C11 C12 C7 124.0(3) . . ? N5 C12 C7 130.7(3) . . ? N5 C13 N4 115.0(3) . . ? N5 C13 H13 122.5 . . ? N4 C13 H13 122.5 . . ? O2 C14 O1 125.9(3) . . ? O2 C14 C15 117.7(3) . . ? O1 C14 C15 116.4(3) . . ? N3 C15 C16 120.9(3) . . ? N3 C15 C14 113.1(3) . . ? C16 C15 C14 126.0(3) . . ? C15 C16 C17 119.4(3) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 119.2(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 118.7(3) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? N3 C19 C18 121.3(3) . . ? N3 C19 C20 113.4(3) . . ? C18 C19 C20 125.2(3) . . ? O4 C20 O3 126.7(3) . . ? O4 C20 C19 118.2(3) . . ? O3 C20 C19 115.1(3) . . ? O1W Mn1 O1W 84.44(13) . 2 ? O1W Mn1 N1 95.60(10) . 2 ? O1W Mn1 N1 99.51(10) 2 2 ? O1W Mn1 N1 99.51(10) . . ? O1W Mn1 N1 95.60(10) 2 . ? N1 Mn1 N1 159.55(14) 2 . ? O1W Mn1 N2 162.97(9) . 2 ? O1W Mn1 N2 85.00(9) 2 2 ? N1 Mn1 N2 73.05(9) 2 2 ? N1 Mn1 N2 94.78(10) . 2 ? O1W Mn1 N2 85.00(9) . . ? O1W Mn1 N2 162.97(9) 2 . ? N1 Mn1 N2 94.78(9) 2 . ? N1 Mn1 N2 73.05(9) . . ? N2 Mn1 N2 108.16(13) 2 . ? N3 Mn2 N3 173.76(14) . 2_655 ? N3 Mn2 O1 72.54(9) . . ? N3 Mn2 O1 102.93(9) 2_655 . ? N3 Mn2 O1 102.93(9) . 2_655 ? N3 Mn2 O1 72.54(9) 2_655 2_655 ? O1 Mn2 O1 91.04(12) . 2_655 ? N3 Mn2 O3 72.12(9) . . ? N3 Mn2 O3 111.95(9) 2_655 . ? O1 Mn2 O3 144.38(8) . . ? O1 Mn2 O3 92.60(9) 2_655 . ? N3 Mn2 O3 111.95(9) . 2_655 ? N3 Mn2 O3 72.12(9) 2_655 2_655 ? O1 Mn2 O3 92.60(9) . 2_655 ? O1 Mn2 O3 144.38(8) 2_655 2_655 ? O3 Mn2 O3 104.47(13) . 2_655 ? C1 N1 C5 117.9(3) . . ? C1 N1 Mn1 125.2(2) . . ? C5 N1 Mn1 116.4(2) . . ? C10 N2 C6 117.9(3) . . ? C10 N2 Mn1 126.8(2) . . ? C6 N2 Mn1 114.0(2) . . ? C19 N3 C15 120.4(3) . . ? C19 N3 Mn2 120.0(2) . . ? C15 N3 Mn2 119.5(2) . . ? C13 N4 C11 102.5(3) . . ? C13 N5 C12 106.4(3) . . ? C13 N5 H5A 131(3) . . ? C12 N5 H5A 123(3) . . ? C14 O1 Mn2 118.4(2) . . ? C20 O3 Mn2 118.8(2) . . ? Mn1 O1W H1W 125(3) . . ? Mn1 O1W H2W 123(2) . . ? H1W O1W H2W 108(2) . . ? H3W O2W H4W 107(2) . . ? H5W O3W H6W 101(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.301 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.125 # Attachment '8.cif' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 710090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H12 Mn N4 O5, H2 O' _chemical_formula_sum 'C17 H14 Mn N4 O6' _chemical_formula_weight 425.26 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.407(2) _cell_length_b 9.540(3) _cell_length_c 11.475(3) _cell_angle_alpha 94.888(5) _cell_angle_beta 97.642(5) _cell_angle_gamma 106.120(5) _cell_volume 869.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3022 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 434 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8365 _exptl_absorpt_correction_T_max 0.9026 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 4387 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3022 _reflns_number_gt 1693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0600P)^2^+0.9475P] 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 3022 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _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 0.68976(9) 0.08723(8) 0.16494(7) 0.0392(3) Uani 1 1 d . . . N1 N 0.9286(5) 0.0692(4) 0.2854(3) 0.0384(10) Uani 1 1 d . . . N2 N 0.7180(5) 0.2187(4) 0.3473(4) 0.0392(10) Uani 1 1 d . . . N3 N 1.1173(6) 0.4017(5) 0.7218(4) 0.0541(12) Uani 1 1 d . . . H3B H 1.0752 0.4558 0.7649 0.065 Uiso 1 1 calc R . . N4 N 1.2968(5) 0.2842(5) 0.6681(4) 0.0491(12) Uani 1 1 d . . . O1 O 0.5258(4) -0.1046(4) 0.2299(3) 0.0572(10) Uani 1 1 d . . . H1B H 0.6059 -0.1280 0.2601 0.086 Uiso 1 1 d R . . H1C H 0.4569 -0.1740 0.1867 0.086 Uiso 1 1 d R . . O2 O 0.4866(4) 0.1669(4) 0.1048(3) 0.0532(10) Uani 1 1 d . . . O3 O 0.2620(4) 0.0473(4) -0.0269(3) 0.0601(11) Uani 1 1 d . . . O4 O -0.1514(4) 0.2879(3) 0.1163(3) 0.0419(8) Uani 1 1 d . . . O5 O 0.0847(4) 0.4692(4) 0.1547(3) 0.0553(10) Uani 1 1 d . . . C1 C 1.0267(6) -0.0089(5) 0.2539(5) 0.0411(13) Uani 1 1 d . . . H1A H 0.9932 -0.0696 0.1818 0.049 Uiso 1 1 calc R . . C2 C 1.1783(6) -0.0055(5) 0.3230(5) 0.0461(14) Uani 1 1 d . . . H2 H 1.2441 -0.0623 0.2978 0.055 Uiso 1 1 calc R . . C3 C 1.2267(6) 0.0846(5) 0.4295(5) 0.0439(13) Uani 1 1 d . . . H3 H 1.3280 0.0909 0.4766 0.053 Uiso 1 1 calc R . . C4 C 1.1256(6) 0.1659(5) 0.4668(4) 0.0371(12) Uani 1 1 d . . . C5 C 1.1606(6) 0.2582(5) 0.5777(5) 0.0376(12) Uani 1 1 d . . . C6 C 1.2633(7) 0.3700(6) 0.7507(5) 0.0530(15) Uani 1 1 d . . . H6 H 1.3339 0.4059 0.8230 0.064 Uiso 1 1 calc R . . C7 C 1.0494(6) 0.3296(5) 0.6093(4) 0.0414(13) Uani 1 1 d . . . C8 C 0.8935(6) 0.3210(5) 0.5363(4) 0.0375(12) Uani 1 1 d . . . C9 C 0.7717(7) 0.3844(6) 0.5680(5) 0.0501(14) Uani 1 1 d . . . H9 H 0.7884 0.4398 0.6416 0.060 Uiso 1 1 calc R . . C10 C 0.6280(7) 0.3638(6) 0.4894(5) 0.0547(15) Uani 1 1 d . . . H10 H 0.5447 0.4037 0.5094 0.066 Uiso 1 1 calc R . . C11 C 0.6077(6) 0.2829(6) 0.3797(5) 0.0499(14) Uani 1 1 d . . . H11 H 0.5111 0.2732 0.3259 0.060 Uiso 1 1 calc R . . C12 C 0.8611(6) 0.2360(5) 0.4257(4) 0.0352(12) Uani 1 1 d . . . C13 C 0.9756(6) 0.1561(5) 0.3911(4) 0.0339(11) Uani 1 1 d . . . C14 C 0.3409(6) 0.1503(5) 0.0524(5) 0.0370(12) Uani 1 1 d . . . C15 C 0.2569(6) 0.2608(5) 0.0903(4) 0.0401(13) Uani 1 1 d . . . H15 H 0.3237 0.3512 0.1302 0.048 Uiso 1 1 calc R . . C16 C 0.0933(6) 0.2376(5) 0.0706(4) 0.0361(12) Uani 1 1 d . . . H16 H 0.0284 0.1509 0.0239 0.043 Uiso 1 1 calc R . . C17 C 0.0041(6) 0.3393(5) 0.1171(4) 0.0371(12) Uani 1 1 d . . . O6 O 0.3611(5) 0.6421(5) 0.0756(4) 0.0941(16) Uani 1 1 d . . . H6WB H 0.3473 0.6681 0.0091 0.141 Uiso 1 1 d R . . H6WA H 0.2929 0.6670 0.1160 0.141 Uiso 1 1 d 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 0.0281(4) 0.0429(4) 0.0466(5) -0.0009(3) 0.0021(3) 0.0143(3) N1 0.031(2) 0.043(2) 0.043(3) 0.001(2) 0.0086(19) 0.0146(19) N2 0.031(2) 0.038(2) 0.056(3) 0.015(2) 0.009(2) 0.0166(18) N3 0.058(3) 0.053(3) 0.049(3) -0.010(2) 0.002(2) 0.021(2) N4 0.041(3) 0.057(3) 0.048(3) -0.002(2) 0.002(2) 0.018(2) O1 0.036(2) 0.053(2) 0.084(3) 0.013(2) 0.009(2) 0.0152(17) O2 0.029(2) 0.065(2) 0.066(3) -0.001(2) -0.0019(18) 0.0224(18) O3 0.032(2) 0.065(2) 0.076(3) -0.027(2) 0.0013(19) 0.0173(18) O4 0.0274(19) 0.052(2) 0.051(2) 0.0084(17) 0.0066(16) 0.0180(16) O5 0.041(2) 0.047(2) 0.073(3) -0.0165(19) 0.0070(19) 0.0121(18) C1 0.045(3) 0.039(3) 0.045(3) 0.003(2) 0.008(3) 0.021(2) C2 0.038(3) 0.053(3) 0.053(4) 0.000(3) 0.014(3) 0.021(3) C3 0.033(3) 0.052(3) 0.054(4) 0.018(3) 0.011(3) 0.018(2) C4 0.029(3) 0.042(3) 0.041(3) 0.004(2) 0.010(2) 0.010(2) C5 0.027(3) 0.039(3) 0.051(3) 0.007(2) 0.007(2) 0.016(2) C6 0.048(4) 0.055(3) 0.050(4) 0.001(3) -0.010(3) 0.016(3) C7 0.040(3) 0.041(3) 0.043(3) 0.003(2) 0.004(3) 0.012(2) C8 0.038(3) 0.033(3) 0.047(3) 0.009(2) 0.010(2) 0.016(2) C9 0.047(4) 0.057(3) 0.050(4) -0.004(3) 0.012(3) 0.023(3) C10 0.051(4) 0.060(3) 0.064(4) 0.000(3) 0.016(3) 0.033(3) C11 0.034(3) 0.066(4) 0.057(4) 0.004(3) 0.010(3) 0.026(3) C12 0.027(3) 0.039(3) 0.043(3) 0.005(2) 0.011(2) 0.011(2) C13 0.032(3) 0.032(2) 0.042(3) 0.008(2) 0.010(2) 0.013(2) C14 0.025(3) 0.039(3) 0.049(3) 0.005(2) 0.010(2) 0.010(2) C15 0.027(3) 0.043(3) 0.045(3) -0.004(2) 0.001(2) 0.006(2) C16 0.029(3) 0.035(3) 0.039(3) -0.006(2) 0.001(2) 0.007(2) C17 0.028(3) 0.052(3) 0.030(3) 0.000(2) -0.001(2) 0.015(2) O6 0.082(3) 0.090(3) 0.094(4) 0.036(3) -0.013(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.106(3) 2_655 ? Mn1 O2 2.113(4) . ? Mn1 O4 2.173(3) 1_655 ? Mn1 O1 2.216(3) . ? Mn1 N2 2.294(4) . ? Mn1 N1 2.338(4) . ? N1 C1 1.319(6) . ? N1 C13 1.355(6) . ? N2 C11 1.320(6) . ? N2 C12 1.364(6) . ? N3 C6 1.350(7) . ? N3 C7 1.379(6) . ? N3 H3B 0.8600 . ? N4 C6 1.309(6) . ? N4 C5 1.390(6) . ? O1 H1B 0.8115 . ? O1 H1C 0.8213 . ? O2 C14 1.252(6) . ? O3 C14 1.248(5) . ? O3 Mn1 2.106(3) 2_655 ? O4 C17 1.261(5) . ? O4 Mn1 2.173(3) 1_455 ? O5 C17 1.243(5) . ? C1 C2 1.400(7) . ? C1 H1A 0.9300 . ? C2 C3 1.376(7) . ? C2 H2 0.9300 . ? C3 C4 1.383(6) . ? C3 H3 0.9300 . ? C4 C13 1.408(7) . ? C4 C5 1.431(7) . ? C5 C7 1.367(6) . ? C6 H6 0.9300 . ? C7 C8 1.436(7) . ? C8 C9 1.396(6) . ? C8 C12 1.398(6) . ? C9 C10 1.363(7) . ? C9 H9 0.9300 . ? C10 C11 1.383(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.456(6) . ? C14 C15 1.489(6) . ? C15 C16 1.316(6) . ? C15 H15 0.9300 . ? C16 C17 1.487(6) . ? C16 H16 0.9300 . ? O6 H6WB 0.8264 . ? O6 H6WA 0.8529 . ? 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 Mn1 O2 110.59(15) 2_655 . ? O3 Mn1 O4 93.29(13) 2_655 1_655 ? O2 Mn1 O4 85.88(13) . 1_655 ? O3 Mn1 O1 92.12(14) 2_655 . ? O2 Mn1 O1 92.94(14) . . ? O4 Mn1 O1 174.53(13) 1_655 . ? O3 Mn1 N2 160.34(15) 2_655 . ? O2 Mn1 N2 89.00(14) . . ? O4 Mn1 N2 86.25(12) 1_655 . ? O1 Mn1 N2 88.39(13) . . ? O3 Mn1 N1 89.32(14) 2_655 . ? O2 Mn1 N1 159.25(14) . . ? O4 Mn1 N1 87.21(13) 1_655 . ? O1 Mn1 N1 92.09(13) . . ? N2 Mn1 N1 71.03(14) . . ? C1 N1 C13 118.4(4) . . ? C1 N1 Mn1 125.0(3) . . ? C13 N1 Mn1 116.3(3) . . ? C11 N2 C12 117.9(4) . . ? C11 N2 Mn1 124.3(4) . . ? C12 N2 Mn1 117.7(3) . . ? C6 N3 C7 105.9(4) . . ? C6 N3 H3B 127.0 . . ? C7 N3 H3B 127.0 . . ? C6 N4 C5 103.5(4) . . ? Mn1 O1 H1B 91.9 . . ? Mn1 O1 H1C 124.2 . . ? H1B O1 H1C 111.5 . . ? C14 O2 Mn1 152.7(3) . . ? C14 O3 Mn1 139.0(3) . 2_655 ? C17 O4 Mn1 134.5(3) . 1_455 ? N1 C1 C2 123.6(4) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 117.7(5) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C13 117.9(4) . . ? C3 C4 C5 124.9(5) . . ? C13 C4 C5 117.1(4) . . ? C7 C5 N4 110.7(4) . . ? C7 C5 C4 120.8(5) . . ? N4 C5 C4 128.4(5) . . ? N4 C6 N3 114.1(5) . . ? N4 C6 H6 122.9 . . ? N3 C6 H6 122.9 . . ? C5 C7 N3 105.7(5) . . ? C5 C7 C8 124.2(4) . . ? N3 C7 C8 130.1(5) . . ? C9 C8 C12 118.3(5) . . ? C9 C8 C7 126.1(5) . . ? C12 C8 C7 115.6(4) . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.2(5) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 C10 123.6(5) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C12 C8 121.8(4) . . ? N2 C12 C13 116.9(4) . . ? C8 C12 C13 121.3(5) . . ? N1 C13 C4 121.9(4) . . ? N1 C13 C12 117.1(4) . . ? C4 C13 C12 121.0(4) . . ? O3 C14 O2 124.6(5) . . ? O3 C14 C15 118.6(4) . . ? O2 C14 C15 116.7(4) . . ? C16 C15 C14 123.7(4) . . ? C16 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C15 C16 C17 125.1(4) . . ? C15 C16 H16 117.5 . . ? C17 C16 H16 117.5 . . ? O5 C17 O4 123.3(5) . . ? O5 C17 C16 119.2(4) . . ? O4 C17 C16 117.5(4) . . ? H6WB O6 H6WA 108.8 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.696 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.098 # Attachment '9.cif' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 710091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H31 Cd3 N12 O12, 8(H2 O)' _chemical_formula_sum 'C51 H47 Cd3 N12 O20' _chemical_formula_weight 1485.21 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' Cd Cd -0.8075 1.2024 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.890(4) _cell_length_b 25.221(12) _cell_length_c 19.959(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.217(7) _cell_angle_gamma 90.00 _cell_volume 5377(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4957 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7179 _exptl_absorpt_correction_T_max 0.8133 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13724 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.1278 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4957 _reflns_number_gt 2298 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0457P)^2^+0.7404P] 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 4957 _refine_ls_number_parameters 389 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.897 _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 C26 C 0.0000 -0.3445(4) 0.7500 0.079(3) Uani 1 2 d S . . Cd1 Cd 0.74037(4) 0.059658(18) 0.64086(3) 0.05241(19) Uani 1 1 d . . . Cd2 Cd 0.0000 -0.04650(3) 0.7500 0.0721(3) Uani 1 2 d S . . O1 O 0.5405(4) 0.05399(19) 0.6564(3) 0.0743(15) Uani 1 1 d . . . O2 O 0.5878(4) -0.0295(2) 0.6344(3) 0.0800(16) Uani 1 1 d . . . O3 O 0.8237(5) 0.0104(2) 0.5656(3) 0.098(2) Uani 1 1 d . . . O4 O 0.9622(5) 0.0670(2) 0.6141(3) 0.0934(18) Uani 1 1 d . . . O6 O 0.1408(4) -0.03915(18) 0.6757(3) 0.0662(14) Uani 1 1 d . . . O11 O 0.1617(4) 0.01604(16) 0.7616(2) 0.0588(12) Uani 1 1 d . . . N3 N 0.6125(5) 0.3228(2) 0.5515(3) 0.0658(17) Uani 1 1 d . . . N1 N 0.6690(5) 0.1281(2) 0.5620(3) 0.0538(15) Uani 1 1 d . . . N2 N 0.7893(4) 0.14126(19) 0.6944(3) 0.0511(14) Uani 1 1 d . . . N4 N 0.7239(5) 0.3345(2) 0.6568(3) 0.0548(15) Uani 1 1 d . . . H4 H 0.7606 0.3503 0.6934 0.066 Uiso 1 1 calc R . . N5 N -0.0842(5) -0.1194(2) 0.6899(4) 0.0634(17) Uani 1 1 d . . . N6 N -0.0582(5) -0.3151(2) 0.6972(3) 0.0638(16) Uani 1 1 d . . . H6 H -0.0996 -0.3262 0.6587 0.077 Uiso 1 1 calc R . . C9 C 0.6318(5) 0.2221(3) 0.5483(4) 0.0488(18) Uani 1 1 d . . . C23 C -0.0432(5) -0.1673(3) 0.7169(3) 0.0491(18) Uani 1 1 d . . . C5 C 0.7499(5) 0.1851(2) 0.6578(3) 0.0453(17) Uani 1 1 d . . . C25 C -0.0371(5) -0.2629(2) 0.7183(3) 0.0520(19) Uani 1 1 d . . . C24 C -0.0811(6) -0.2152(2) 0.6840(4) 0.0515(18) Uani 1 1 d . . . C18 C 0.9259(8) 0.0310(3) 0.5727(4) 0.069(2) Uani 1 1 d . . . C4 C 0.7719(6) 0.2362(2) 0.6850(4) 0.0511(18) Uani 1 1 d . . . C13 C 0.6088(6) 0.1207(3) 0.4981(4) 0.065(2) Uani 1 1 d . . . H13 H 0.6016 0.0864 0.4808 0.078 Uiso 1 1 calc R . . C8 C 0.6526(6) 0.2735(2) 0.5794(4) 0.0514(18) Uani 1 1 d . . . C10 C 0.6820(5) 0.1778(2) 0.5875(4) 0.0455(16) Uani 1 1 d . . . C1 C 0.8523(6) 0.1472(3) 0.7597(4) 0.0586(19) Uani 1 1 d . . . H1 H 0.8789 0.1172 0.7854 0.070 Uiso 1 1 calc R . . C14 C 0.5147(7) 0.0050(3) 0.6480(4) 0.065(2) Uani 1 1 d . . . C3 C 0.8382(6) 0.2409(3) 0.7535(4) 0.0577(19) Uani 1 1 d . . . H3 H 0.8542 0.2741 0.7736 0.069 Uiso 1 1 calc R . . C11 C 0.5678(6) 0.2124(3) 0.4813(4) 0.062(2) Uani 1 1 d . . . H11 H 0.5329 0.2405 0.4540 0.074 Uiso 1 1 calc R . . C20 C -0.1639(7) -0.1193(3) 0.6281(5) 0.070(2) Uani 1 1 d . . . H20 H -0.1925 -0.0868 0.6093 0.085 Uiso 1 1 calc R . . C7 C 0.6597(7) 0.3562(3) 0.6028(5) 0.066(2) Uani 1 1 d . . . H7 H 0.6466 0.3926 0.5994 0.079 Uiso 1 1 calc R . . C6 C 0.7219(5) 0.2800(2) 0.6439(4) 0.0481(17) Uani 1 1 d . . . C22 C -0.1638(6) -0.2127(3) 0.6189(4) 0.063(2) Uani 1 1 d . . . H22 H -0.1896 -0.2438 0.5951 0.076 Uiso 1 1 calc R . . C19 C 1.0170(8) 0.0147(3) 0.5249(4) 0.078(2) Uani 1 1 d . . . H19 H 1.0988 0.0273 0.5341 0.094 Uiso 1 1 calc R . . C12 C 0.5567(6) 0.1616(3) 0.4561(4) 0.062(2) Uani 1 1 d . . . H12 H 0.5148 0.1549 0.4117 0.075 Uiso 1 1 calc R . . C15 C 0.3895(6) -0.0114(3) 0.6601(3) 0.0556(19) Uani 1 1 d . . . H15 H 0.3598 -0.0444 0.6437 0.067 Uiso 1 1 calc R . . C21 C -0.2045(7) -0.1649(3) 0.5919(4) 0.072(2) Uani 1 1 d . . . H21 H -0.2587 -0.1628 0.5498 0.086 Uiso 1 1 calc R . . C16 C 0.3176(6) 0.0168(2) 0.6918(3) 0.0532(18) Uani 1 1 d . . . H16 H 0.3413 0.0514 0.7038 0.064 Uiso 1 1 calc R . . C2 C 0.8778(6) 0.1964(3) 0.7887(4) 0.060(2) Uani 1 1 d . . . H2 H 0.9229 0.1991 0.8332 0.072 Uiso 1 1 calc R . . H26 H 0.0000 -0.3817 0.7500 0.072 Uiso 1 2 d SR . . C17 C 0.2005(6) -0.0035(2) 0.7096(4) 0.0489(17) Uani 1 1 d . . . O3W O 0.3920(4) 0.12451(17) 0.2786(2) 0.0794(15) Uani 1 1 d D . . H6W H 0.3676 0.0936 0.2865 0.119 Uiso 1 1 d RD . . H5W H 0.4341 0.1208 0.2474 0.119 Uiso 1 1 d RD . . O1W O 0.8221(5) 0.6392(2) 0.5755(3) 0.1075(19) Uani 1 1 d D . . H1W H 0.7448 0.6438 0.5763 0.161 Uiso 1 1 d RD . . H2W H 0.8606 0.6455 0.6159 0.161 Uiso 1 1 d RD . . O4W O 0.5697(5) 0.3500(2) 0.0581(3) 0.1017(18) Uani 1 1 d D . . H7W H 0.5037 0.3355 0.0349 0.152 Uiso 1 1 d RD . . H8W H 0.5430 0.3786 0.0731 0.152 Uiso 1 1 d RD . . O2W O 0.6326(7) 0.9535(3) 0.4937(4) 0.178(3) Uani 1 1 d D . . H3W H 0.6110 0.9485 0.5322 0.267 Uiso 1 1 d RD . . H4W H 0.6991 0.9726 0.5033 0.267 Uiso 1 1 d RD . . 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 C26 0.071(7) 0.058(7) 0.112(12) 0.000 0.028(8) 0.000 Cd1 0.0573(3) 0.0470(3) 0.0562(4) 0.0036(3) 0.0192(3) 0.0039(2) Cd2 0.0603(5) 0.0545(5) 0.1097(8) 0.000 0.0371(5) 0.000 O1 0.063(3) 0.075(3) 0.089(4) 0.008(3) 0.026(3) -0.017(3) O2 0.070(3) 0.092(4) 0.087(4) -0.002(3) 0.036(3) 0.015(3) O3 0.101(4) 0.075(4) 0.139(6) -0.023(3) 0.077(4) -0.013(3) O4 0.098(4) 0.107(5) 0.081(5) -0.015(4) 0.030(4) 0.021(4) O6 0.066(3) 0.063(3) 0.075(4) -0.027(3) 0.027(3) -0.024(2) O11 0.054(3) 0.062(3) 0.063(4) -0.015(3) 0.016(3) -0.003(2) N3 0.068(4) 0.040(4) 0.090(5) -0.002(3) 0.017(4) 0.006(3) N1 0.049(3) 0.051(4) 0.060(5) -0.004(3) 0.005(3) -0.007(3) N2 0.046(3) 0.046(3) 0.060(4) 0.006(3) 0.006(3) 0.003(3) N4 0.059(4) 0.047(4) 0.058(5) -0.019(3) 0.012(3) -0.007(3) N5 0.053(3) 0.056(4) 0.087(5) 0.014(4) 0.027(4) 0.003(3) N6 0.059(4) 0.058(4) 0.071(5) 0.003(3) 0.002(3) -0.001(3) C9 0.043(4) 0.049(4) 0.054(5) -0.002(4) 0.007(4) -0.003(3) C23 0.037(4) 0.051(4) 0.060(5) 0.000(3) 0.012(3) -0.003(3) C5 0.048(4) 0.040(4) 0.049(5) 0.000(3) 0.012(4) 0.001(3) C25 0.053(4) 0.044(4) 0.057(6) 0.000(3) 0.005(4) -0.001(3) C24 0.045(4) 0.057(4) 0.051(5) -0.002(4) 0.004(4) -0.002(3) C18 0.087(6) 0.056(5) 0.065(6) 0.003(4) 0.019(6) 0.018(5) C4 0.051(4) 0.042(4) 0.059(5) -0.002(4) 0.004(4) 0.001(3) C13 0.061(5) 0.054(5) 0.079(7) -0.012(5) 0.010(5) -0.006(4) C8 0.051(4) 0.043(4) 0.062(5) -0.006(4) 0.013(4) 0.000(3) C10 0.047(4) 0.042(4) 0.049(5) 0.001(4) 0.014(4) -0.002(3) C1 0.051(4) 0.062(5) 0.058(6) 0.012(4) -0.002(4) 0.001(3) C14 0.062(5) 0.078(6) 0.056(5) 0.007(4) 0.009(4) -0.014(4) C3 0.060(4) 0.050(4) 0.059(6) -0.009(4) 0.003(4) -0.005(3) C11 0.067(5) 0.055(5) 0.063(6) 0.008(4) 0.011(4) 0.002(4) C20 0.066(5) 0.072(6) 0.074(7) 0.023(5) 0.012(5) 0.012(4) C7 0.065(5) 0.039(4) 0.098(7) -0.001(5) 0.023(5) 0.003(4) C6 0.045(4) 0.044(4) 0.056(5) -0.006(4) 0.011(4) -0.003(3) C22 0.062(5) 0.077(5) 0.052(6) 0.002(4) 0.013(4) -0.007(4) C19 0.090(6) 0.072(6) 0.080(8) -0.004(4) 0.033(6) 0.001(5) C12 0.069(5) 0.057(5) 0.056(5) -0.005(4) -0.001(4) -0.012(4) C15 0.055(4) 0.060(4) 0.057(5) -0.010(4) 0.021(4) -0.011(3) C21 0.075(5) 0.084(6) 0.055(6) 0.016(5) 0.008(4) 0.004(5) C16 0.053(4) 0.051(4) 0.062(5) 0.002(4) 0.027(4) -0.008(3) C2 0.069(5) 0.054(5) 0.051(5) 0.001(4) -0.003(4) -0.006(4) C17 0.049(4) 0.040(4) 0.058(5) 0.003(4) 0.010(4) 0.002(3) O3W 0.086(3) 0.074(3) 0.080(4) -0.003(3) 0.021(3) 0.003(3) O1W 0.105(4) 0.129(5) 0.078(4) -0.004(4) -0.009(4) 0.002(4) O4W 0.118(4) 0.095(4) 0.078(4) -0.008(3) -0.016(4) -0.004(3) O2W 0.152(7) 0.279(10) 0.095(6) -0.013(6) 0.007(5) -0.050(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 C26 N6 1.342(7) 2_556 ? C26 N6 1.342(7) . ? C26 H26 0.9382 . ? Cd1 O1 2.262(4) . ? Cd1 O3 2.271(5) . ? Cd1 O11 2.309(4) 2_656 ? Cd1 N2 2.332(5) . ? Cd1 N1 2.363(5) . ? Cd1 O4 2.580(6) . ? Cd2 N5 2.288(6) . ? Cd2 N5 2.288(6) 2_556 ? Cd2 O6 2.339(5) . ? Cd2 O6 2.339(5) 2_556 ? Cd2 O11 2.342(4) . ? Cd2 O11 2.342(4) 2_556 ? Cd2 C17 2.698(7) 2_556 ? O1 C14 1.272(8) . ? O2 C14 1.243(8) . ? O3 C18 1.211(8) . ? O4 C18 1.240(8) . ? O6 C17 1.233(7) . ? O11 C17 1.292(7) . ? O11 Cd1 2.309(4) 2_656 ? N3 C7 1.348(8) . ? N3 C8 1.398(8) . ? N1 C13 1.329(8) . ? N1 C10 1.350(7) . ? N2 C5 1.349(7) . ? N2 C1 1.357(7) . ? N4 C7 1.286(8) . ? N4 C6 1.398(7) . ? N4 H4 0.8600 . ? N5 C23 1.362(7) . ? N5 C20 1.363(8) . ? N6 C25 1.388(7) . ? N6 H6 0.8600 . ? C9 C11 1.403(8) . ? C9 C10 1.412(8) . ? C9 C8 1.437(9) . ? C23 C24 1.398(8) . ? C23 C23 1.465(12) 2_556 ? C5 C4 1.400(8) . ? C5 C10 1.465(8) . ? C25 C25 1.362(12) 2_556 ? C25 C24 1.421(8) . ? C24 C22 1.430(8) . ? C18 C19 1.559(10) . ? C4 C6 1.420(8) . ? C4 C3 1.421(8) . ? C13 C12 1.380(9) . ? C13 H13 0.9300 . ? C8 C6 1.369(8) . ? C1 C2 1.376(9) . ? C1 H1 0.9300 . ? C14 C15 1.488(9) . ? C3 C2 1.350(8) . ? C3 H3 0.9300 . ? C11 C12 1.374(8) . ? C11 H11 0.9300 . ? C20 C21 1.384(9) . ? C20 H20 0.9300 . ? C7 H7 0.9300 . ? C22 C21 1.361(9) . ? C22 H22 0.9300 . ? C19 C19 1.238(13) 5_756 ? C19 H19 0.9300 . ? C12 H12 0.9300 . ? C15 C16 1.307(8) . ? C15 H15 0.9300 . ? C21 H21 0.9300 . ? C16 C17 1.480(8) . ? C16 H16 0.9300 . ? C2 H2 0.9300 . ? O3W H6W 0.8488 . ? O3W H5W 0.8482 . ? O1W H1W 0.8517 . ? O1W H2W 0.8485 . ? O4W H7W 0.8573 . ? O4W H8W 0.8533 . ? O2W H3W 0.8547 . ? O2W H4W 0.8593 . ? 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 N6 C26 N6 112.9(9) 2_556 . ? N6 C26 H26 123.5 2_556 . ? N6 C26 H26 123.5 . . ? O1 Cd1 O3 125.1(2) . . ? O1 Cd1 O11 98.84(17) . 2_656 ? O3 Cd1 O11 96.80(19) . 2_656 ? O1 Cd1 N2 97.65(18) . . ? O3 Cd1 N2 134.51(18) . . ? O11 Cd1 N2 90.42(18) 2_656 . ? O1 Cd1 N1 86.36(17) . . ? O3 Cd1 N1 94.7(2) . . ? O11 Cd1 N1 161.40(17) 2_656 . ? N2 Cd1 N1 71.1(2) . . ? O1 Cd1 O4 175.95(19) . . ? O3 Cd1 O4 52.51(17) . . ? O11 Cd1 O4 84.91(17) 2_656 . ? N2 Cd1 O4 83.80(17) . . ? N1 Cd1 O4 90.55(17) . . ? N5 Cd2 N5 73.0(3) . 2_556 ? N5 Cd2 O6 88.64(18) . . ? N5 Cd2 O6 98.69(18) 2_556 . ? N5 Cd2 O6 98.69(18) . 2_556 ? N5 Cd2 O6 88.64(18) 2_556 2_556 ? O6 Cd2 O6 170.9(2) . 2_556 ? N5 Cd2 O11 144.12(18) . . ? N5 Cd2 O11 105.83(18) 2_556 . ? O6 Cd2 O11 55.69(15) . . ? O6 Cd2 O11 117.18(17) 2_556 . ? N5 Cd2 O11 105.83(18) . 2_556 ? N5 Cd2 O11 144.12(18) 2_556 2_556 ? O6 Cd2 O11 117.18(17) . 2_556 ? O6 Cd2 O11 55.69(15) 2_556 2_556 ? O11 Cd2 O11 95.3(2) . 2_556 ? N5 Cd2 C17 102.43(18) . 2_556 ? N5 Cd2 C17 115.6(2) 2_556 2_556 ? O6 Cd2 C17 145.7(2) . 2_556 ? O6 Cd2 C17 27.15(17) 2_556 2_556 ? O11 Cd2 C17 109.63(18) . 2_556 ? O11 Cd2 C17 28.61(16) 2_556 2_556 ? C14 O1 Cd1 103.7(5) . . ? C18 O3 Cd1 99.5(5) . . ? C18 O4 Cd1 84.0(5) . . ? C17 O6 Cd2 92.9(4) . . ? C17 O11 Cd1 133.6(4) . 2_656 ? C17 O11 Cd2 91.2(4) . . ? Cd1 O11 Cd2 128.3(2) 2_656 . ? C7 N3 C8 102.1(6) . . ? C13 N1 C10 119.2(6) . . ? C13 N1 Cd1 125.0(4) . . ? C10 N1 Cd1 115.5(4) . . ? C5 N2 C1 118.5(5) . . ? C5 N2 Cd1 117.1(4) . . ? C1 N2 Cd1 124.4(4) . . ? C7 N4 C6 106.1(6) . . ? C7 N4 H4 126.9 . . ? C6 N4 H4 126.9 . . ? C23 N5 C20 117.6(6) . . ? C23 N5 Cd2 116.0(5) . . ? C20 N5 Cd2 126.3(5) . . ? C26 N6 C25 105.1(7) . . ? C26 N6 H6 127.4 . . ? C25 N6 H6 127.4 . . ? C11 C9 C10 117.3(6) . . ? C11 C9 C8 125.2(6) . . ? C10 C9 C8 117.5(7) . . ? N5 C23 C24 122.4(6) . . ? N5 C23 C23 117.4(4) . 2_556 ? C24 C23 C23 120.2(4) . 2_556 ? N2 C5 C4 122.2(6) . . ? N2 C5 C10 117.5(5) . . ? C4 C5 C10 120.3(6) . . ? C25 C25 N6 108.4(4) 2_556 . ? C25 C25 C24 122.1(4) 2_556 . ? N6 C25 C24 129.5(6) . . ? C23 C24 C25 117.6(6) . . ? C23 C24 C22 117.7(6) . . ? C25 C24 C22 124.6(6) . . ? O3 C18 O4 123.9(8) . . ? O3 C18 C19 119.7(8) . . ? O4 C18 C19 116.3(8) . . ? C5 C4 C6 118.3(6) . . ? C5 C4 C3 117.8(6) . . ? C6 C4 C3 123.8(6) . . ? N1 C13 C12 123.1(6) . . ? N1 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C6 C8 N3 109.9(6) . . ? C6 C8 C9 121.8(6) . . ? N3 C8 C9 128.3(7) . . ? N1 C10 C9 121.6(6) . . ? N1 C10 C5 118.4(6) . . ? C9 C10 C5 120.0(6) . . ? N2 C1 C2 121.8(6) . . ? N2 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? O2 C14 O1 125.0(7) . . ? O2 C14 C15 119.2(7) . . ? O1 C14 C15 115.7(7) . . ? C2 C3 C4 118.8(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C12 C11 C9 120.2(6) . . ? C12 C11 H11 119.9 . . ? C9 C11 H11 119.9 . . ? N5 C20 C21 123.6(7) . . ? N5 C20 H20 118.2 . . ? C21 C20 H20 118.2 . . ? N4 C7 N3 115.8(6) . . ? N4 C7 H7 122.1 . . ? N3 C7 H7 122.1 . . ? C8 C6 N4 106.1(6) . . ? C8 C6 C4 121.9(6) . . ? N4 C6 C4 131.9(7) . . ? C21 C22 C24 119.8(7) . . ? C21 C22 H22 120.1 . . ? C24 C22 H22 120.1 . . ? C19 C19 C18 121.5(11) 5_756 . ? C19 C19 H19 119.2 5_756 . ? C18 C19 H19 119.2 . . ? C11 C12 C13 118.6(7) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C16 C15 C14 125.6(7) . . ? C16 C15 H15 117.2 . . ? C14 C15 H15 117.2 . . ? C22 C21 C20 118.9(7) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C15 C16 C17 123.7(6) . . ? C15 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C3 C2 C1 120.8(7) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? O6 C17 O11 120.0(6) . . ? O6 C17 C16 120.5(7) . . ? O11 C17 C16 119.6(6) . . ? H6W O3W H5W 105.6 . . ? H1W O1W H2W 105.4 . . ? H7W O4W H8W 104.1 . . ? H3W O2W H4W 104.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.830 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.112 data_compound10 _database_code_depnum_ccdc_archive 'CCDC 710092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H30 N12 O12 Zn3, 8(H2 O)' _chemical_formula_sum 'C51 H46 N12 O20 Zn3' _chemical_formula_weight 1343.11 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.868(3) _cell_length_b 25.099(8) _cell_length_c 19.916(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.955(5) _cell_angle_gamma 90.00 _cell_volume 5334(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4685 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 1.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7629 _exptl_absorpt_correction_T_max 0.8585 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13112 _diffrn_reflns_av_R_equivalents 0.1225 _diffrn_reflns_av_sigmaI/netI 0.1627 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4678 _reflns_number_gt 2117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.1486P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4678 _refine_ls_number_parameters 366 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.2602 _refine_ls_wR_factor_gt 0.2292 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _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 N5 N 1.0833(11) 0.6207(4) 0.3111(6) 0.106(3) Uani 1 1 d . . . C18 C 1.0431(10) 0.6686(4) 0.2828(6) 0.080(3) Uani 1 1 d . . . C19 C 1.0789(11) 0.7160(5) 0.3146(6) 0.082(3) Uani 1 1 d . . . C22 C 1.1621(12) 0.7146(5) 0.3791(7) 0.099(4) Uani 1 1 d . . . H22 H 1.1894 0.7463 0.4010 0.119 Uiso 1 1 calc R . . C21 C 1.2030(14) 0.6666(6) 0.4095(8) 0.111(4) Uani 1 1 d . . . H21 H 1.2572 0.6648 0.4516 0.133 Uiso 1 1 calc R . . C20 C 1.1572(15) 0.6207(6) 0.3726(8) 0.115(5) Uani 1 1 d . . . H20 H 1.1803 0.5878 0.3927 0.138 Uiso 1 1 calc R . . O3 O 0.4594(10) 0.4479(4) 0.3419(6) 0.135(4) Uani 1 1 d . . . C27 C 0.6108(12) 0.5116(5) 0.3413(7) 0.096(4) Uani 1 1 d . . . H59 H 0.6414 0.5443 0.3591 0.115 Uiso 1 1 calc R . . C1 C 0.8555(7) 0.3543(3) 0.2617(4) 0.099(4) Uani 1 1 d G . . H1 H 0.8824 0.3845 0.2873 0.119 Uiso 1 1 calc R . . C2 C 0.8812(8) 0.3040(4) 0.2901(3) 0.107(4) Uani 1 1 d G . . H2 H 0.9253 0.3005 0.3347 0.128 Uiso 1 1 calc R . . C3 C 0.8409(7) 0.2588(3) 0.2518(4) 0.095(4) Uani 1 1 d G . . H3 H 0.8581 0.2251 0.2707 0.113 Uiso 1 1 calc R . . C4 C 0.7750(7) 0.2639(2) 0.1851(4) 0.087(3) Uani 1 1 d G . . C5 C 0.7493(6) 0.3142(3) 0.1567(3) 0.075(3) Uani 1 1 d G . . N1 N 0.7895(7) 0.3594(2) 0.1950(4) 0.093(3) Uani 1 1 d G . . C11 C 0.6546(12) 0.2282(5) 0.0785(7) 0.085(3) Uani 1 1 d . . . N4 N 0.6153(10) 0.1774(4) 0.0522(6) 0.106(4) Uani 1 1 d . . . C13 C 0.6579(15) 0.1436(5) 0.1026(8) 0.111(5) Uani 1 1 d . . . H13 H 0.6401 0.1074 0.0995 0.133 Uiso 1 1 calc R . . N3 N 0.7264(10) 0.1649(4) 0.1567(6) 0.097(3) Uani 1 1 d . . . H3A H 0.7655 0.1489 0.1926 0.117 Uiso 1 1 calc R . . C12 C 0.7218(11) 0.2202(5) 0.1428(6) 0.084(3) Uani 1 1 d . . . C6 C 0.6837(7) 0.3217(3) 0.0903(3) 0.079(3) Uani 1 1 d G . . N2 N 0.6713(7) 0.3730(2) 0.0636(4) 0.098(3) Uani 1 1 d G . . C7 C 0.6077(8) 0.3815(3) -0.0029(4) 0.094(4) Uani 1 1 d G . . H7 H 0.5994 0.4158 -0.0208 0.113 Uiso 1 1 calc R . . C8 C 0.5564(7) 0.3386(4) -0.0428(3) 0.101(4) Uani 1 1 d G . . H8 H 0.5139 0.3443 -0.0874 0.122 Uiso 1 1 calc R . . C9 C 0.5688(7) 0.2873(3) -0.0162(4) 0.103(4) Uani 1 1 d G . . H9 H 0.5345 0.2586 -0.0429 0.124 Uiso 1 1 calc R . . C10 C 0.6324(7) 0.2788(2) 0.0504(4) 0.071(3) Uani 1 1 d G . . Zn1 Zn 0.74102(9) 0.44042(3) 0.14150(5) 0.0446(4) Uani 1 1 d . . . Zn2 Zn 1.0000 0.54679(5) 0.2500 0.0618(6) Uani 1 2 d S . . N6 N 1.0582(10) 0.8164(4) 0.3018(6) 0.099(3) Uani 1 1 d . . . H6 H 1.1006 0.8274 0.3402 0.119 Uiso 0.50 1 calc PR . . C23 C 1.0371(12) 0.7634(4) 0.2818(5) 0.085(3) Uani 1 1 d . . . O1 O 0.8420(8) 0.4848(3) 0.2403(4) 0.104(3) Uani 1 1 d . . . O2 O 0.8573(8) 0.5413(3) 0.3227(5) 0.102(3) Uani 1 1 d . . . C26 C 0.6833(12) 0.4828(5) 0.3079(6) 0.091(4) Uani 1 1 d . . . H53 H 0.6594 0.4483 0.2941 0.109 Uiso 1 1 calc R . . C25 C 0.7994(10) 0.5047(5) 0.2929(6) 0.075(3) Uani 1 1 d . . . O4 O 0.4119(9) 0.5301(4) 0.3673(5) 0.120(3) Uani 1 1 d . . . O4W O 0.8891(9) 0.1253(4) 0.2802(5) 0.139(4) Uani 1 1 d . . . H4B H 0.8987 0.1154 0.2434 0.167 Uiso 1 1 d R . . O2W O 0.1762(12) 0.8616(4) 0.4256(5) 0.161(4) Uani 1 1 d . . . H2B H 0.1536 0.8327 0.4314 0.194 Uiso 1 1 d R . . O3W O 0.4339(12) 0.1509(4) 0.9418(5) 0.152(4) Uani 1 1 d . . . O1W O 0.6377(13) 0.5431(6) 0.9924(7) 0.193(6) Uani 1 1 d . . . C24 C 1.0000 0.8468(7) 0.2500 0.099(6) Uani 1 2 d S . . H24A H 1.0000 0.8839 0.2500 0.119 Uiso 1 2 calc SR . . O5 O 0.9650(11) 0.4329(4) 0.1165(6) 0.132(4) Uani 1 1 d . . . O6 O 0.8285(12) 0.4897(4) 0.0686(6) 0.147(4) Uani 1 1 d . . . C30 C 0.9298(14) 0.4680(5) 0.0710(7) 0.094(4) Uani 1 1 d D . . C29 C 1.0123(17) 0.4843(6) 0.0238(7) 0.136(6) Uani 1 1 d D . . H29A H 1.0916 0.4690 0.0309 0.164 Uiso 1 1 calc R . . C28 C 0.4885(13) 0.4956(5) 0.3515(8) 0.106(4) Uani 1 1 d . . . H3C H 0.4623 0.1252 0.9232 0.159 Uiso 1 1 d R . . H3D H 0.4857 0.1582 0.9732 0.159 Uiso 1 1 d R . . H1A H 0.6925 0.5272 1.0143 0.159 Uiso 1 1 d R . . H1B H 0.6461 0.5713 0.9722 0.159 Uiso 1 1 d R . . H2A H 0.2424 0.8575 0.4291 0.159 Uiso 1 1 d R . . H4A H 0.8872 0.0974 0.3010 0.159 Uiso 1 1 d 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 N5 0.110(9) 0.070(7) 0.133(10) 0.014(6) 0.011(8) 0.002(6) C18 0.072(7) 0.063(7) 0.102(9) 0.004(6) 0.012(6) -0.004(6) C19 0.069(7) 0.090(9) 0.084(8) -0.003(7) 0.008(7) 0.008(6) C22 0.096(10) 0.099(10) 0.102(10) 0.014(8) 0.016(9) 0.008(8) C21 0.101(11) 0.125(12) 0.111(11) 0.025(10) 0.028(9) 0.006(10) C20 0.126(13) 0.092(11) 0.110(12) 0.031(9) -0.019(10) -0.003(9) O3 0.116(8) 0.102(7) 0.197(11) 0.014(7) 0.057(8) -0.021(6) C27 0.091(10) 0.099(9) 0.100(10) -0.011(8) 0.025(8) -0.018(8) C1 0.089(9) 0.103(10) 0.102(10) 0.003(8) 0.007(9) -0.005(7) C2 0.132(12) 0.087(9) 0.091(9) 0.011(8) -0.005(9) 0.008(8) C3 0.108(10) 0.084(9) 0.086(9) -0.002(7) 0.003(8) 0.010(7) C4 0.088(9) 0.084(9) 0.089(9) 0.009(7) 0.018(8) 0.003(7) C5 0.082(8) 0.063(7) 0.077(8) -0.003(6) 0.010(7) 0.002(5) N1 0.077(7) 0.090(7) 0.109(8) -0.008(6) 0.011(6) -0.003(5) C11 0.094(9) 0.066(8) 0.086(9) 0.002(6) -0.005(8) -0.005(6) N4 0.117(9) 0.061(7) 0.137(10) 0.015(6) 0.014(8) 0.002(6) C13 0.145(14) 0.057(8) 0.121(12) 0.008(8) 0.000(10) 0.000(8) N3 0.104(9) 0.079(7) 0.104(8) 0.018(6) 0.007(7) 0.013(6) C12 0.092(9) 0.063(8) 0.097(9) -0.011(7) 0.017(8) -0.010(6) C6 0.083(8) 0.078(8) 0.081(8) 0.009(7) 0.030(7) 0.007(6) N2 0.093(8) 0.062(6) 0.143(10) 0.013(6) 0.029(7) 0.001(5) C7 0.083(9) 0.079(9) 0.111(10) 0.001(8) -0.008(8) 0.009(7) C8 0.109(10) 0.083(9) 0.103(9) 0.004(8) -0.002(8) 0.030(8) C9 0.092(10) 0.098(10) 0.118(11) -0.006(8) 0.016(9) -0.003(7) C10 0.071(7) 0.068(8) 0.069(7) -0.003(6) -0.003(6) -0.009(5) Zn1 0.0522(6) 0.0322(6) 0.0503(6) -0.0038(4) 0.0117(5) -0.0029(4) Zn2 0.0562(10) 0.0364(9) 0.0983(13) 0.000 0.0286(9) 0.000 N6 0.096(8) 0.080(7) 0.123(9) 0.011(6) 0.026(7) 0.010(6) C23 0.113(11) 0.055(7) 0.082(8) -0.004(5) 0.008(7) -0.001(6) O1 0.123(7) 0.088(6) 0.100(6) -0.011(5) 0.021(6) -0.012(5) O2 0.091(6) 0.102(6) 0.112(7) -0.033(5) 0.014(5) -0.036(5) C26 0.094(9) 0.079(8) 0.104(9) 0.001(7) 0.030(8) -0.009(7) C25 0.065(7) 0.081(8) 0.079(8) -0.008(6) 0.016(7) -0.004(6) O4 0.094(7) 0.141(8) 0.125(8) -0.012(6) 0.019(6) 0.018(6) O4W 0.140(9) 0.134(8) 0.140(8) 0.031(6) 0.019(7) 0.021(6) O2W 0.184(12) 0.141(9) 0.139(9) 0.015(7) -0.020(8) -0.011(8) O3W 0.188(11) 0.147(9) 0.107(7) -0.003(6) -0.009(7) -0.008(8) O1W 0.139(11) 0.269(15) 0.159(11) 0.048(10) -0.002(9) 0.039(9) C24 0.110(15) 0.061(11) 0.127(16) 0.000 0.024(14) 0.000 O5 0.142(9) 0.130(8) 0.130(8) 0.028(7) 0.038(7) -0.035(7) O6 0.179(11) 0.087(7) 0.206(12) 0.015(7) 0.119(10) 0.010(7) C30 0.110(11) 0.075(9) 0.107(10) 0.000(8) 0.046(10) 0.002(8) C29 0.208(17) 0.118(13) 0.101(12) 0.020(8) 0.075(13) 0.018(12) C28 0.109(11) 0.065(9) 0.150(13) 0.004(8) 0.042(10) -0.011(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 N5 C20 1.332(15) . ? N5 C18 1.364(13) . ? N5 Zn2 2.306(11) . ? C18 C19 1.368(14) . ? C18 C18 1.46(2) 2_755 ? C19 C23 1.392(14) . ? C19 C22 1.423(16) . ? C22 C21 1.383(17) . ? C22 H22 0.9300 . ? C21 C20 1.406(18) . ? C21 H21 0.9300 . ? C20 H20 0.9300 . ? O3 C28 1.245(13) . ? O3 Zn1 2.272(9) 2_655 ? C27 C26 1.336(16) . ? C27 C28 1.440(16) . ? C27 H59 0.9300 . ? C1 C2 1.3900 . ? C1 N1 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 C12 1.436(12) . ? C5 N1 1.3900 . ? C5 C6 1.39075 . ? N1 Zn1 2.310(6) . ? C11 C12 1.363(15) . ? C11 C10 1.391(13) . ? C11 N4 1.415(14) . ? N4 C13 1.328(15) . ? C13 N3 1.301(15) . ? C13 H13 0.9300 . ? N3 C12 1.415(14) . ? N3 H3A 0.8600 . ? C6 N2 1.3900 . ? C6 C10 1.3900 . ? N2 C7 1.3900 . ? N2 Zn1 2.322(6) . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? Zn1 O6 2.251(9) . ? Zn1 O3 2.272(9) 2_655 ? Zn1 O1 2.345(8) . ? Zn2 O1 2.299(8) . ? Zn2 O1 2.299(8) 2_755 ? Zn2 N5 2.306(11) 2_755 ? Zn2 O2 2.317(8) . ? Zn2 O2 2.317(8) 2_755 ? N6 C24 1.342(12) . ? N6 C23 1.395(13) . ? N6 H6 0.8600 . ? C23 C23 1.37(2) 2_755 ? O1 C25 1.320(12) . ? O2 C25 1.203(12) . ? C26 C25 1.460(15) . ? C26 H53 0.9300 . ? O4 C28 1.281(14) . ? O4W H4B 0.7988 . ? O4W H4A 0.8143 . ? O2W H2B 0.7812 . ? O2W H2A 0.7168 . ? O3W H3C 0.8335 . ? O3W H3D 0.7788 . ? O1W H1A 0.7788 . ? O1W H1B 0.8271 . ? C24 N6 1.342(12) 2_755 ? C24 H24A 0.9300 . ? O5 C30 1.268(16) . ? O6 C30 1.221(15) . ? C30 C29 1.48(2) . ? C29 C29 1.22(2) 5_765 ? C29 H29A 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 C20 N5 C18 118.0(12) . . ? C20 N5 Zn2 126.4(9) . . ? C18 N5 Zn2 115.4(9) . . ? N5 C18 C19 122.3(11) . . ? N5 C18 C18 118.1(7) . 2_755 ? C19 C18 C18 119.6(7) . 2_755 ? C18 C19 C23 119.1(12) . . ? C18 C19 C22 118.2(11) . . ? C23 C19 C22 122.7(12) . . ? C21 C22 C19 120.8(13) . . ? C21 C22 H22 119.6 . . ? C19 C22 H22 119.6 . . ? C22 C21 C20 115.6(14) . . ? C22 C21 H21 122.2 . . ? C20 C21 H21 122.2 . . ? N5 C20 C21 124.9(13) . . ? N5 C20 H20 117.5 . . ? C21 C20 H20 117.5 . . ? C28 O3 Zn1 106.2(9) . 2_655 ? C26 C27 C28 124.5(13) . . ? C26 C27 H59 117.7 . . ? C28 C27 H59 117.7 . . ? C2 C1 N1 120.0 . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 C12 115.4(8) . . ? C3 C4 C12 124.5(8) . . ? C4 C5 N1 120.0 . . ? C4 C5 C6 122.48 . . ? N1 C5 C6 117.52 . . ? C5 N1 C1 120.0 . . ? C5 N1 Zn1 116.4(4) . . ? C1 N1 Zn1 123.6(4) . . ? C12 C11 C10 122.3(11) . . ? C12 C11 N4 106.6(10) . . ? C10 C11 N4 131.1(11) . . ? C13 N4 C11 104.9(11) . . ? N3 C13 N4 115.2(12) . . ? N3 C13 H13 122.4 . . ? N4 C13 H13 122.4 . . ? C13 N3 C12 104.4(10) . . ? C13 N3 H3A 127.8 . . ? C12 N3 H3A 127.8 . . ? C11 C12 N3 108.7(10) . . ? C11 C12 C4 121.5(11) . . ? N3 C12 C4 129.8(12) . . ? N2 C6 C10 120.0 . . ? N2 C6 C5 118.96 . . ? C10 C6 C5 121.07 . . ? C7 N2 C6 120.0 . . ? C7 N2 Zn1 124.5(4) . . ? C6 N2 Zn1 115.1(4) . . ? C8 C7 N2 120.0 . . ? C8 C7 H7 120.0 . . ? N2 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C6 120.0 . . ? C9 C10 C11 122.7(8) . . ? C6 C10 C11 117.1(8) . . ? O6 Zn1 O3 125.7(4) . 2_655 ? O6 Zn1 N1 133.9(3) . . ? O3 Zn1 N1 98.4(3) 2_655 . ? O6 Zn1 N2 95.3(4) . . ? O3 Zn1 N2 87.5(3) 2_655 . ? N1 Zn1 N2 71.6(3) . . ? O6 Zn1 O1 95.4(4) . . ? O3 Zn1 O1 98.5(4) 2_655 . ? N1 Zn1 O1 90.1(3) . . ? N2 Zn1 O1 161.4(3) . . ? O1 Zn2 O1 94.8(4) . 2_755 ? O1 Zn2 N5 143.2(4) . . ? O1 Zn2 N5 106.7(4) 2_755 . ? O1 Zn2 N5 106.7(4) . 2_755 ? O1 Zn2 N5 143.2(4) 2_755 2_755 ? N5 Zn2 N5 73.0(6) . 2_755 ? O1 Zn2 O2 55.5(3) . . ? O1 Zn2 O2 119.0(3) 2_755 . ? N5 Zn2 O2 87.8(3) . . ? N5 Zn2 O2 97.8(4) 2_755 . ? O1 Zn2 O2 119.0(3) . 2_755 ? O1 Zn2 O2 55.5(3) 2_755 2_755 ? N5 Zn2 O2 97.8(4) . 2_755 ? N5 Zn2 O2 87.8(3) 2_755 2_755 ? O2 Zn2 O2 173.2(4) . 2_755 ? C24 N6 C23 107.2(12) . . ? C24 N6 H6 126.4 . . ? C23 N6 H6 126.4 . . ? C23 C23 C19 121.2(7) 2_755 . ? C23 C23 N6 107.5(7) 2_755 . ? C19 C23 N6 131.2(11) . . ? C25 O1 Zn2 92.6(7) . . ? C25 O1 Zn1 131.8(8) . . ? Zn2 O1 Zn1 127.9(4) . . ? C25 O2 Zn2 95.0(7) . . ? C27 C26 C25 120.9(12) . . ? C27 C26 H53 119.6 . . ? C25 C26 H53 119.6 . . ? O2 C25 O1 116.8(10) . . ? O2 C25 C26 125.3(11) . . ? O1 C25 C26 117.8(11) . . ? H4B O4W H4A 102.7 . . ? H2B O2W H2A 101.0 . . ? H3C O3W H3D 105.6 . . ? H1A O1W H1B 124.6 . . ? N6 C24 N6 110.6(16) 2_755 . ? N6 C24 H24A 124.7 2_755 . ? N6 C24 H24A 124.7 . . ? C30 O6 Zn1 102.6(8) . . ? O6 C30 O5 119.0(11) . . ? O6 C30 C29 120.3(15) . . ? O5 C30 C29 120.7(13) . . ? C29 C29 C30 127(2) 5_765 . ? C29 C29 H29A 116.5 5_765 . ? C30 C29 H29A 116.5 . . ? O3 C28 O4 122.0(13) . . ? O3 C28 C27 117.5(13) . . ? O4 C28 C27 120.4(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.225 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.136 # Attachment '11.cif' data_compound11 _database_code_depnum_ccdc_archive 'CCDC 710093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H26 Cd2 N8 O11, 7.3(H2 O)' _chemical_formula_sum 'C43 H40.60 Cd2 N8 O18.30' _chemical_formula_weight 1187.03 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.533(3) _cell_length_b 18.506(3) _cell_length_c 26.518(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.683(5) _cell_angle_gamma 90.00 _cell_volume 9933(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4292 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 25.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4776 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8723 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 25027 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.1313 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.19 _reflns_number_total 8905 _reflns_number_gt 4292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0836P)^2^+0.9502P] 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 8905 _refine_ls_number_parameters 636 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1653 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.80311(3) 0.88115(3) 0.05681(2) 0.0419(2) Uani 1 1 d . . . Cd2 Cd 1.03599(3) 0.63594(3) -0.01124(2) 0.0468(2) Uani 1 1 d . . . N1 N 0.8786(3) 0.9750(3) 0.0710(3) 0.0486(17) Uani 1 1 d . . . N2 N 0.8343(3) 0.9096(3) -0.0202(2) 0.0456(17) Uani 1 1 d . . . N3 N 1.1070(3) 0.6895(3) 0.0583(2) 0.0444(16) Uani 1 1 d . . . N4 N 1.1109(3) 0.7128(3) -0.0422(3) 0.0518(18) Uani 1 1 d . . . N5 N 1.2579(3) 0.9209(3) 0.0147(3) 0.0572(19) Uani 1 1 d U . . H5 H 1.2680 0.9413 -0.0120 0.069 Uiso 1 1 calc R . . N6 N 1.2545(4) 0.9029(4) 0.0960(3) 0.061(2) Uani 1 1 d . . . N7 N 0.9554(4) 1.0968(4) -0.1006(3) 0.068(2) Uani 1 1 d . . . H7 H 0.9481 1.0889 -0.1330 0.082 Uiso 1 1 calc R . . N8 N 0.9947(4) 1.1478(4) -0.0244(3) 0.063(2) Uani 1 1 d U . . O1 O 0.7889(3) 0.5009(3) 0.4299(2) 0.0569(15) Uani 1 1 d . . . O2 O 0.7483(3) 0.4118(3) 0.37799(19) 0.0610(16) Uani 1 1 d . . . O3 O 0.9501(3) 0.7038(3) 0.0449(2) 0.0622(16) Uani 1 1 d . . . O4 O 0.9730(3) 0.5870(3) 0.04180(19) 0.0502(14) Uani 1 1 d . . . O5 O 0.8736(3) 0.8080(3) 0.12035(19) 0.0539(15) Uani 1 1 d . . . O6 O 0.8152(3) 0.7571(3) 0.05259(19) 0.0524(15) Uani 1 1 d . . . O7 O 0.7609(3) 0.6186(3) 0.2331(2) 0.082(2) Uani 1 1 d . . . O8 O 0.8950(3) 0.3852(3) 0.4308(2) 0.0743(19) Uani 1 1 d . . . O9 O 0.9934(3) 0.4105(3) 0.41257(19) 0.0567(15) Uani 1 1 d . . . C17 C 0.9407(4) 1.0647(4) 0.0313(3) 0.049(2) Uani 1 1 d . . . C40 C 0.9325(5) 0.4161(4) 0.4043(3) 0.042(2) Uani 1 1 d . . . C6 C 1.2182(4) 0.8589(4) 0.0160(3) 0.044(2) Uani 1 1 d . . . C32 C 0.8378(4) 0.6645(4) 0.1612(2) 0.0402(19) Uani 1 1 d . . . H32 H 0.8124 0.7002 0.1731 0.048 Uiso 1 1 calc R . . C27 C 0.9452(4) 0.6410(4) 0.0596(3) 0.042(2) Uani 1 1 d . . . C31 C 0.8440(4) 0.5990(4) 0.1855(3) 0.0401(19) Uani 1 1 d . . . C28 C 0.9039(4) 0.6260(4) 0.1012(2) 0.0359(18) Uani 1 1 d . . . C5 C 1.1465(4) 0.7576(4) -0.0080(3) 0.0408(19) Uani 1 1 d . . . C7 C 1.2165(4) 0.8487(4) 0.0667(3) 0.047(2) Uani 1 1 d . . . C33 C 0.8675(4) 0.6790(3) 0.1203(3) 0.0361(18) Uani 1 1 d . . . C39 C 0.8992(4) 0.4621(4) 0.3605(2) 0.041(2) Uani 1 1 d . . . C41 C 0.8342(4) 0.4822(4) 0.3543(2) 0.0355(18) Uani 1 1 d . . . C9 C 1.1431(4) 0.7451(4) 0.0461(3) 0.0405(19) Uani 1 1 d . . . C3 C 1.1867(4) 0.8201(5) -0.0760(3) 0.057(2) Uani 1 1 d . . . H3 H 1.2125 0.8556 -0.0878 0.069 Uiso 1 1 calc R . . C4 C 1.1850(4) 0.8147(4) -0.0234(3) 0.044(2) Uani 1 1 d . . . C18 C 0.8985(4) 1.0043(4) 0.0282(3) 0.0422(19) Uani 1 1 d . . . C14 C 0.9006(4) 1.0032(4) 0.1162(3) 0.059(2) Uani 1 1 d . . . H14 H 0.8869 0.9831 0.1449 0.071 Uiso 1 1 calc R . . C20 C 0.8915(4) 0.9948(4) -0.0659(3) 0.046(2) Uani 1 1 d . . . C22 C 0.9568(4) 1.0907(4) -0.0147(3) 0.046(2) Uani 1 1 d U . . C1 C 1.1142(4) 0.7210(5) -0.0916(3) 0.057(2) Uani 1 1 d . . . H1 H 1.0904 0.6891 -0.1148 0.069 Uiso 1 1 calc R . . C36 C 0.8448(4) 0.5439(4) 0.2756(3) 0.044(2) Uani 1 1 d . . . C29 C 0.9084(4) 0.5588(4) 0.1237(3) 0.045(2) Uani 1 1 d . . . H29 H 0.9318 0.5224 0.1104 0.054 Uiso 1 1 calc R . . C34 C 0.8526(4) 0.7527(4) 0.0954(3) 0.0407(19) Uani 1 1 d . . . C30 C 0.8786(4) 0.5444(4) 0.1660(3) 0.045(2) Uani 1 1 d . . . H30 H 0.8818 0.4989 0.1810 0.054 Uiso 1 1 calc R . . C12 C 1.1768(4) 0.7754(5) 0.1336(3) 0.061(2) Uani 1 1 d . . . H12 H 1.2004 0.8035 0.1594 0.073 Uiso 1 1 calc R . . C42 C 0.7885(4) 0.4633(4) 0.3907(3) 0.044(2) Uani 1 1 d . . . C43 C 0.8072(4) 0.5222(4) 0.3123(3) 0.044(2) Uani 1 1 d . . . H43 H 0.7628 0.5352 0.3082 0.052 Uiso 1 1 calc R . . C38 C 0.9386(4) 0.4845(4) 0.3246(3) 0.052(2) Uani 1 1 d . . . H38 H 0.9830 0.4719 0.3292 0.062 Uiso 1 1 calc R . . C15 C 0.9440(5) 1.0626(5) 0.1230(4) 0.068(3) Uani 1 1 d . . . H15 H 0.9587 1.0814 0.1554 0.082 Uiso 1 1 calc R . . C19 C 0.8738(4) 0.9683(4) -0.0203(3) 0.043(2) Uani 1 1 d . . . C37 C 0.9109(4) 0.5258(4) 0.2821(3) 0.053(2) Uani 1 1 d . . . H37 H 0.9368 0.5408 0.2585 0.063 Uiso 1 1 calc R . . C16 C 0.9639(4) 1.0921(4) 0.0807(4) 0.059(2) Uani 1 1 d . . . H16 H 0.9933 1.1308 0.0846 0.071 Uiso 1 1 calc R . . C10 C 1.1066(4) 0.6764(4) 0.1062(3) 0.060(2) Uani 1 1 d . . . H10 H 1.0831 0.6365 0.1147 0.072 Uiso 1 1 calc R . . C13 C 1.2760(4) 0.9409(4) 0.0618(4) 0.051(2) Uani 1 1 d U . . H13 H 1.3031 0.9808 0.0704 0.062 Uiso 1 1 calc R . . C11 C 1.1392(5) 0.7187(5) 0.1452(3) 0.069(3) Uani 1 1 d . . . H11 H 1.1357 0.7089 0.1790 0.083 Uiso 1 1 calc R . . C8 C 1.1792(4) 0.7900(4) 0.0840(3) 0.051(2) Uani 1 1 d . . . C23 C 0.8677(4) 0.9585(5) -0.1106(3) 0.060(2) Uani 1 1 d . . . H23 H 0.8781 0.9749 -0.1414 0.071 Uiso 1 1 calc R . . C24 C 0.8287(5) 0.8985(5) -0.1099(3) 0.065(3) Uani 1 1 d . . . H24 H 0.8129 0.8738 -0.1400 0.078 Uiso 1 1 calc R . . C26 C 0.9907(5) 1.1473(5) -0.0746(5) 0.074(3) Uani 1 1 d U . . H26 H 1.0123 1.1820 -0.0910 0.089 Uiso 1 1 calc R . . C21 C 0.9323(4) 1.0583(4) -0.0607(3) 0.055(2) Uani 1 1 d . . . C25 C 0.8136(4) 0.8756(4) -0.0643(3) 0.058(2) Uani 1 1 d . . . H25 H 0.7876 0.8345 -0.0640 0.069 Uiso 1 1 calc R . . C2 C 1.1506(5) 0.7735(5) -0.1104(3) 0.068(3) Uani 1 1 d . . . H2 H 1.1509 0.7775 -0.1453 0.082 Uiso 1 1 calc R . . C35 C 0.8145(5) 0.5882(5) 0.2309(3) 0.051(2) Uani 1 1 d . . . O11 O 0.7006(3) 0.8608(3) 0.0103(2) 0.0697(18) Uani 1 1 d . . . H11A H 0.6961 0.8263 -0.0081 0.105 Uiso 1 1 d R . . H11B H 0.6729 0.8679 0.0277 0.105 Uiso 1 1 d R . . O12 O 0.9027(3) 0.4682(3) 0.00405(18) 0.0573(15) Uani 1 1 d . . . H12A H 0.8707 0.4765 -0.0168 0.086 Uiso 1 1 d R . . H12B H 0.9235 0.5028 0.0152 0.086 Uiso 1 1 d R . . O14 O 0.9365(12) 0.8235(11) 0.2284(8) 0.334(18) Uiso 0.67 1 d PD . . H14A H 0.9174 0.8206 0.1995 0.501 Uiso 0.67 1 d PRD A . H14B H 0.9325 0.8528 0.2498 0.501 Uiso 0.67 1 d PR . . O14A O 0.8985(14) 0.8102(11) 0.2252(8) 0.125(10) Uiso 0.33 1 d PD A 2 H14C H 0.8936 0.8094 0.1947 0.187 Uiso 0.33 1 d PR A 2 H14D H 0.9086 0.8429 0.2447 0.187 Uiso 0.33 1 d PRD A 2 O15 O 0.7711(8) 0.8508(8) 0.2238(6) 0.290(8) Uiso 1 1 d . B 2 H15A H 0.7519 0.8188 0.2073 0.436 Uiso 1 1 d R B 2 H15B H 0.7684 0.8807 0.2018 0.436 Uiso 1 1 d R B 2 O17 O 0.0421(4) 0.2478(3) 0.0563(3) 0.113(3) Uani 1 1 d D C 2 H17A H 0.0291 0.2198 0.0339 0.169 Uiso 1 1 d R C 2 H17B H 0.0601 0.2863 0.0601 0.169 Uiso 1 1 d RD C 2 O19 O 0.3107(11) 0.8890(12) 0.2013(6) 0.239(15) Uiso 0.60 1 d PD D 1 H19A H 0.2931 0.8950 0.1723 0.358 Uiso 0.60 1 d PRD D 1 H19B H 0.2877 0.8796 0.2219 0.358 Uiso 0.60 1 d PRD D 1 O19A O 0.2899(13) 0.9139(13) 0.2003(7) 0.41(5) Uiso 0.40 1 d PD E 2 H19C H 0.2838 0.8885 0.2235 0.621 Uiso 0.40 1 d PRD E 2 H19D H 0.2897 0.9066 0.1706 0.621 Uiso 0.40 1 d PR E 2 O20 O 0.6912(11) 0.7786(11) 0.1540(7) 0.085(7) Uiso 0.30 1 d P . . H20A H 0.7192 0.8049 0.1468 0.127 Uiso 0.30 1 d PR . . H20B H 0.6602 0.7983 0.1373 0.127 Uiso 0.30 1 d PR . . O13 O 0.0440(8) 0.2433(6) 0.1608(4) 0.269(8) Uani 1 1 d . . . H13A H 0.0439 0.2449 0.1306 0.403 Uiso 1 1 d R . . H13B H 0.0740 0.2511 0.1835 0.403 Uiso 1 1 d R . . O16 O 0.9253(9) 0.0801(7) 0.7947(4) 0.272(8) Uani 1 1 d . . . O18A O 0.137(2) 0.848(2) 0.7738(14) 0.245(18) Uiso 0.34 1 d P F 1 H18C H 0.1725 0.8566 0.7671 0.368 Uiso 0.34 1 d PR F 1 H18D H 0.1173 0.8256 0.7500 0.368 Uiso 0.34 1 d PR F 1 O18 O 0.0537(10) 0.6576(11) 0.7838(7) 0.249(9) Uiso 0.66 1 d P G 2 H18B H 0.0293 0.6824 0.7968 0.373 Uiso 0.66 1 d PR G 2 H18A H 0.0916 0.6453 0.7877 0.373 Uiso 0.66 1 d PR G 2 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 Cd1 0.0505(4) 0.0357(3) 0.0408(3) 0.0004(2) 0.0119(3) 0.0004(3) Cd2 0.0472(4) 0.0498(4) 0.0449(4) -0.0080(3) 0.0122(3) -0.0134(3) N1 0.044(5) 0.046(4) 0.054(4) -0.007(3) 0.004(4) -0.006(3) N2 0.054(5) 0.036(4) 0.046(4) -0.004(3) 0.007(3) -0.015(3) N3 0.041(4) 0.045(4) 0.047(4) 0.004(3) 0.007(3) -0.006(3) N4 0.047(5) 0.051(4) 0.057(5) -0.002(3) 0.009(4) -0.009(4) N5 0.064(5) 0.042(4) 0.072(5) 0.016(3) 0.031(4) -0.004(4) N6 0.065(6) 0.061(5) 0.058(5) -0.007(4) 0.013(4) -0.008(4) N7 0.070(6) 0.057(5) 0.086(6) -0.001(4) 0.034(5) -0.007(4) N8 0.052(5) 0.047(4) 0.092(5) -0.003(4) 0.024(5) -0.009(4) O1 0.056(4) 0.068(4) 0.052(3) -0.001(3) 0.022(3) 0.004(3) O2 0.067(5) 0.076(4) 0.041(3) 0.004(3) 0.012(3) -0.024(4) O3 0.078(5) 0.047(3) 0.070(4) 0.012(3) 0.033(3) -0.006(3) O4 0.051(4) 0.049(3) 0.056(3) -0.014(3) 0.023(3) -0.009(3) O5 0.073(4) 0.041(3) 0.050(3) -0.001(3) 0.016(3) 0.004(3) O6 0.067(4) 0.046(3) 0.041(3) 0.008(2) -0.001(3) 0.000(3) O7 0.081(5) 0.110(5) 0.060(4) 0.046(4) 0.029(4) 0.031(4) O8 0.066(5) 0.079(4) 0.084(5) 0.041(4) 0.030(4) 0.028(4) O9 0.050(4) 0.061(4) 0.055(4) 0.013(3) -0.004(3) 0.001(3) C17 0.041(6) 0.030(4) 0.077(6) -0.007(4) 0.015(5) 0.002(4) C40 0.055(6) 0.032(4) 0.040(5) 0.003(3) 0.008(5) 0.008(4) C6 0.040(5) 0.037(4) 0.052(5) 0.004(4) 0.003(4) 0.001(4) C32 0.046(5) 0.040(4) 0.033(4) 0.005(3) 0.005(4) 0.004(4) C27 0.038(5) 0.051(5) 0.036(4) 0.004(4) 0.005(4) -0.014(4) C31 0.037(5) 0.055(5) 0.030(4) 0.004(4) 0.008(4) 0.002(4) C28 0.039(5) 0.040(4) 0.028(4) 0.002(3) 0.004(3) -0.005(4) C5 0.037(5) 0.037(4) 0.049(5) 0.002(4) 0.009(4) -0.003(4) C7 0.035(5) 0.045(5) 0.061(6) -0.007(4) 0.005(4) -0.002(4) C33 0.043(5) 0.029(4) 0.035(4) 0.002(3) 0.005(4) 0.004(4) C39 0.050(6) 0.046(5) 0.028(4) 0.001(3) 0.006(4) -0.003(4) C41 0.035(5) 0.046(4) 0.026(4) 0.001(3) 0.005(4) -0.001(4) C9 0.028(5) 0.032(4) 0.058(5) -0.004(4) -0.002(4) 0.000(4) C3 0.054(6) 0.054(6) 0.070(6) 0.019(5) 0.030(5) 0.010(5) C4 0.038(5) 0.037(4) 0.059(5) 0.004(4) 0.015(4) 0.006(4) C18 0.035(5) 0.032(4) 0.059(5) -0.001(4) 0.007(4) 0.006(4) C14 0.076(7) 0.051(5) 0.050(5) -0.008(4) 0.008(5) 0.003(5) C20 0.046(6) 0.045(5) 0.049(5) 0.009(4) 0.017(4) -0.003(4) C22 0.040(6) 0.036(4) 0.064(6) -0.003(4) 0.011(4) -0.008(4) C1 0.057(7) 0.064(6) 0.051(6) -0.002(4) 0.006(5) -0.011(5) C36 0.042(6) 0.053(5) 0.036(4) 0.005(4) 0.008(4) 0.005(4) C29 0.047(6) 0.043(5) 0.044(5) 0.001(4) 0.002(4) 0.009(4) C34 0.048(6) 0.036(4) 0.044(5) -0.001(4) 0.026(4) -0.004(4) C30 0.049(6) 0.042(5) 0.046(5) 0.014(4) 0.012(4) 0.005(4) C12 0.063(7) 0.062(6) 0.050(6) -0.003(4) -0.007(5) -0.017(5) C42 0.045(6) 0.049(5) 0.036(5) 0.010(4) 0.005(4) 0.009(4) C43 0.038(5) 0.047(5) 0.045(5) 0.003(4) 0.003(4) 0.004(4) C38 0.049(6) 0.063(5) 0.042(5) 0.010(4) 0.005(4) 0.007(5) C15 0.070(8) 0.064(6) 0.069(6) -0.021(5) 0.003(6) -0.010(6) C19 0.043(5) 0.040(5) 0.047(5) 0.002(4) 0.012(4) 0.006(4) C37 0.042(6) 0.079(6) 0.039(5) 0.010(4) 0.013(4) -0.004(5) C16 0.049(6) 0.041(5) 0.083(7) -0.023(5) 0.000(5) -0.012(4) C10 0.071(7) 0.057(6) 0.052(6) 0.004(4) 0.009(5) -0.019(5) C13 0.036(5) 0.040(5) 0.077(6) -0.005(4) 0.006(5) -0.016(4) C11 0.081(8) 0.077(7) 0.047(5) 0.003(5) 0.003(5) -0.024(6) C8 0.059(6) 0.040(5) 0.054(5) 0.005(4) 0.010(5) -0.002(4) C23 0.065(7) 0.077(6) 0.039(5) 0.007(4) 0.015(5) -0.011(5) C24 0.060(7) 0.078(7) 0.057(6) -0.021(5) 0.011(5) -0.015(5) C26 0.060(7) 0.039(5) 0.134(8) 0.006(6) 0.049(7) -0.008(5) C21 0.047(6) 0.045(5) 0.076(6) 0.018(5) 0.022(5) 0.011(5) C25 0.057(6) 0.065(6) 0.050(5) -0.001(4) 0.007(5) -0.019(5) C2 0.084(8) 0.077(7) 0.048(5) -0.006(5) 0.024(5) -0.003(6) C35 0.049(6) 0.061(6) 0.044(5) 0.005(4) 0.008(5) 0.009(5) O11 0.057(4) 0.091(5) 0.062(4) -0.030(3) 0.015(3) -0.002(4) O12 0.051(4) 0.061(4) 0.059(3) -0.011(3) 0.005(3) -0.010(3) O17 0.167(8) 0.066(4) 0.108(6) -0.021(4) 0.033(5) -0.056(5) O13 0.40(2) 0.243(14) 0.140(10) -0.001(9) -0.027(11) -0.046(15) O16 0.46(3) 0.197(12) 0.169(11) 0.045(9) 0.094(13) -0.019(14) _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 Cd1 O2 2.245(5) 4_655 ? Cd1 O11 2.284(6) . ? Cd1 N2 2.301(6) . ? Cd1 O6 2.313(5) . ? Cd1 N1 2.315(6) . ? Cd1 O5 2.438(5) . ? Cd1 C34 2.717(8) . ? Cd2 O9 2.234(5) 6_565 ? Cd2 O4 2.256(5) . ? Cd2 O12 2.291(5) 5_765 ? Cd2 N4 2.342(6) . ? Cd2 N3 2.367(6) . ? N1 C14 1.316(9) . ? N1 C18 1.381(9) . ? N2 C25 1.333(9) . ? N2 C19 1.355(9) . ? N3 C10 1.296(9) . ? N3 C9 1.338(9) . ? N4 C1 1.332(9) . ? N4 C5 1.350(9) . ? N5 C13 1.296(9) . ? N5 C6 1.410(9) . ? N5 H5 0.8600 . ? N6 C13 1.282(9) . ? N6 C7 1.419(10) . ? N7 C26 1.307(11) . ? N7 C21 1.421(10) . ? N7 H7 0.8600 . ? N8 C26 1.320(11) . ? N8 C22 1.362(9) . ? O1 C42 1.249(8) . ? O2 C42 1.268(9) . ? O2 Cd1 2.245(5) 4_645 ? O3 C27 1.234(8) . ? O4 C27 1.280(9) . ? O5 C34 1.255(8) . ? O6 C34 1.262(8) . ? O7 C35 1.247(9) . ? O8 C40 1.262(9) . ? O9 C40 1.237(9) . ? O9 Cd2 2.234(5) 6_566 ? C17 C22 1.401(11) . ? C17 C18 1.409(10) . ? C17 C16 1.411(11) . ? C40 C39 1.509(10) . ? C6 C7 1.365(10) . ? C6 C4 1.408(10) . ? C32 C33 1.357(9) . ? C32 C31 1.369(9) . ? C32 H32 0.9300 . ? C27 C28 1.525(10) . ? C31 C30 1.383(10) . ? C31 C35 1.450(10) . ? C28 C29 1.376(9) . ? C28 C33 1.381(9) . ? C5 C4 1.420(10) . ? C5 C9 1.468(10) . ? C7 C8 1.448(11) . ? C33 C34 1.523(9) . ? C39 C41 1.369(10) . ? C39 C38 1.410(10) . ? C41 C43 1.375(9) . ? C41 C42 1.497(10) . ? C9 C8 1.413(10) . ? C3 C2 1.378(11) . ? C3 C4 1.405(10) . ? C3 H3 0.9300 . ? C18 C19 1.461(10) . ? C14 C15 1.407(11) . ? C14 H14 0.9300 . ? C20 C23 1.379(10) . ? C20 C19 1.408(9) . ? C20 C21 1.435(11) . ? C22 C21 1.377(11) . ? C1 C2 1.368(11) . ? C1 H1 0.9300 . ? C36 C37 1.379(10) . ? C36 C43 1.400(10) . ? C36 C35 1.488(10) . ? C29 C30 1.392(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C12 C8 1.351(10) . ? C12 C11 1.368(11) . ? C12 H12 0.9300 . ? C43 H43 0.9300 . ? C38 C37 1.400(10) . ? C38 H38 0.9300 . ? C15 C16 1.370(11) . ? C15 H15 0.9300 . ? C37 H37 0.9300 . ? C16 H16 0.9300 . ? C10 C11 1.376(11) . ? C10 H10 0.9300 . ? C13 H13 0.9300 . ? C11 H11 0.9300 . ? C23 C24 1.371(11) . ? C23 H23 0.9300 . ? C24 C25 1.366(11) . ? C24 H24 0.9300 . ? C26 H26 0.9300 . ? C25 H25 0.9300 . ? C2 H2 0.9300 . ? O11 H11A 0.8000 . ? O11 H11B 0.8001 . ? O12 Cd2 2.291(5) 5_765 ? O12 H12A 0.8003 . ? O12 H12B 0.7998 . ? O14 O14A 0.81(4) . ? O14 H14A 0.8001 . ? O14 H14B 0.8000 . ? O14 H14C 1.1737 . ? O14 H14D 0.8536 . ? O14A H14A 0.8610 . ? O14A H14B 1.1754 . ? O14A H14C 0.7998 . ? O14A H14D 0.8001 . ? O15 H15A 0.8000 . ? O15 H15B 0.7999 . ? O17 H17A 0.7998 . ? O17 H17B 0.8000 . ? O19 H19A 0.8001 . ? O19 H19B 0.8000 . ? O19 H19C 0.8712 . ? O19 H19D 0.9159 . ? O19A H19A 0.8331 . ? O19A H19B 0.8625 . ? O19A H19C 0.8000 . ? O19A H19D 0.7998 . ? O20 H20A 0.7999 . ? O20 H20B 0.8000 . ? O13 H13A 0.8000 . ? O13 H13B 0.8000 . ? O18A H18C 0.8000 . ? O18A H18D 0.8001 . ? O18 H18B 0.8000 . ? O18 H18A 0.8000 . ? 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 O2 Cd1 O11 87.0(2) 4_655 . ? O2 Cd1 N2 149.6(2) 4_655 . ? O11 Cd1 N2 85.9(2) . . ? O2 Cd1 O6 110.8(2) 4_655 . ? O11 Cd1 O6 84.7(2) . . ? N2 Cd1 O6 97.81(19) . . ? O2 Cd1 N1 94.2(2) 4_655 . ? O11 Cd1 N1 137.9(2) . . ? N2 Cd1 N1 72.2(2) . . ? O6 Cd1 N1 132.6(2) . . ? O2 Cd1 O5 84.80(19) 4_655 . ? O11 Cd1 O5 131.85(19) . . ? N2 Cd1 O5 121.2(2) . . ? O6 Cd1 O5 55.01(17) . . ? N1 Cd1 O5 90.0(2) . . ? O2 Cd1 C34 97.2(2) 4_655 . ? O11 Cd1 C34 108.1(2) . . ? N2 Cd1 C34 113.1(2) . . ? O6 Cd1 C34 27.59(19) . . ? N1 Cd1 C34 113.4(2) . . ? O5 Cd1 C34 27.50(19) . . ? O9 Cd2 O4 103.4(2) 6_565 . ? O9 Cd2 O12 82.98(19) 6_565 5_765 ? O4 Cd2 O12 88.56(19) . 5_765 ? O9 Cd2 N4 95.5(2) 6_565 . ? O4 Cd2 N4 160.4(2) . . ? O12 Cd2 N4 99.0(2) 5_765 . ? O9 Cd2 N3 164.0(2) 6_565 . ? O4 Cd2 N3 91.5(2) . . ? O12 Cd2 N3 91.71(19) 5_765 . ? N4 Cd2 N3 70.3(2) . . ? C14 N1 C18 119.3(7) . . ? C14 N1 Cd1 124.3(6) . . ? C18 N1 Cd1 116.3(5) . . ? C25 N2 C19 118.6(7) . . ? C25 N2 Cd1 125.1(5) . . ? C19 N2 Cd1 116.2(5) . . ? C10 N3 C9 118.4(7) . . ? C10 N3 Cd2 125.5(5) . . ? C9 N3 Cd2 115.4(5) . . ? C1 N4 C5 118.6(7) . . ? C1 N4 Cd2 124.0(5) . . ? C5 N4 Cd2 116.8(5) . . ? C13 N5 C6 106.5(6) . . ? C13 N5 H5 126.8 . . ? C6 N5 H5 126.8 . . ? C13 N6 C7 103.0(7) . . ? C26 N7 C21 101.0(8) . . ? C26 N7 H7 129.5 . . ? C21 N7 H7 129.5 . . ? C26 N8 C22 104.1(7) . . ? C42 O2 Cd1 110.8(5) . 4_645 ? C27 O4 Cd2 104.7(4) . . ? C34 O5 Cd1 88.7(5) . . ? C34 O6 Cd1 94.3(4) . . ? C40 O9 Cd2 115.0(5) . 6_566 ? C22 C17 C18 117.0(7) . . ? C22 C17 C16 126.3(8) . . ? C18 C17 C16 116.6(8) . . ? O9 C40 O8 123.8(7) . . ? O9 C40 C39 119.8(7) . . ? O8 C40 C39 116.4(8) . . ? C7 C6 C4 124.1(7) . . ? C7 C6 N5 104.3(7) . . ? C4 C6 N5 131.6(7) . . ? C33 C32 C31 122.2(7) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? O3 C27 O4 123.6(7) . . ? O3 C27 C28 119.0(7) . . ? O4 C27 C28 117.4(6) . . ? C32 C31 C30 118.9(7) . . ? C32 C31 C35 119.6(7) . . ? C30 C31 C35 121.5(7) . . ? C29 C28 C33 119.0(7) . . ? C29 C28 C27 118.2(7) . . ? C33 C28 C27 122.5(6) . . ? N4 C5 C4 121.9(7) . . ? N4 C5 C9 116.8(7) . . ? C4 C5 C9 121.3(7) . . ? C6 C7 N6 109.8(7) . . ? C6 C7 C8 121.3(7) . . ? N6 C7 C8 129.0(8) . . ? C32 C33 C28 119.8(6) . . ? C32 C33 C34 116.1(6) . . ? C28 C33 C34 123.9(6) . . ? C41 C39 C38 119.7(7) . . ? C41 C39 C40 123.5(7) . . ? C38 C39 C40 116.7(7) . . ? C39 C41 C43 119.8(7) . . ? C39 C41 C42 124.3(6) . . ? C43 C41 C42 115.8(7) . . ? N3 C9 C8 121.8(7) . . ? N3 C9 C5 118.4(6) . . ? C8 C9 C5 119.8(7) . . ? C2 C3 C4 120.8(8) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C6 127.2(8) . . ? C3 C4 C5 116.5(7) . . ? C6 C4 C5 116.2(7) . . ? N1 C18 C17 121.8(7) . . ? N1 C18 C19 116.0(7) . . ? C17 C18 C19 122.2(7) . . ? N1 C14 C15 122.6(8) . . ? N1 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C23 C20 C19 117.6(7) . . ? C23 C20 C21 126.7(7) . . ? C19 C20 C21 115.7(7) . . ? N8 C22 C21 107.9(7) . . ? N8 C22 C17 131.0(8) . . ? C21 C22 C17 121.1(7) . . ? N4 C1 C2 124.1(8) . . ? N4 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C37 C36 C43 119.3(7) . . ? C37 C36 C35 120.3(7) . . ? C43 C36 C35 120.3(8) . . ? C28 C29 C30 121.0(7) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? O5 C34 O6 121.6(7) . . ? O5 C34 C33 118.4(7) . . ? O6 C34 C33 119.7(6) . . ? O5 C34 Cd1 63.8(4) . . ? O6 C34 Cd1 58.1(4) . . ? C33 C34 Cd1 169.0(5) . . ? C31 C30 C29 119.0(7) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C8 C12 C11 119.1(8) . . ? C8 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? O1 C42 O2 123.5(8) . . ? O1 C42 C41 119.3(8) . . ? O2 C42 C41 117.1(7) . . ? C41 C43 C36 121.5(7) . . ? C41 C43 H43 119.3 . . ? C36 C43 H43 119.3 . . ? C37 C38 C39 120.2(8) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C16 C15 C14 118.6(8) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? N2 C19 C20 121.5(7) . . ? N2 C19 C18 118.8(7) . . ? C20 C19 C18 119.7(7) . . ? C36 C37 C38 119.4(7) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C15 C16 C17 121.0(8) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? N3 C10 C11 123.1(8) . . ? N3 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? N6 C13 N5 116.5(7) . . ? N6 C13 H13 121.8 . . ? N5 C13 H13 121.8 . . ? C12 C11 C10 119.3(8) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C12 C8 C9 118.2(8) . . ? C12 C8 C7 124.5(8) . . ? C9 C8 C7 117.3(7) . . ? C24 C23 C20 120.4(8) . . ? C24 C23 H23 119.8 . . ? C20 C23 H23 119.8 . . ? C25 C24 C23 119.0(8) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? N7 C26 N8 118.2(8) . . ? N7 C26 H26 120.9 . . ? N8 C26 H26 120.9 . . ? C22 C21 N7 108.8(8) . . ? C22 C21 C20 124.2(8) . . ? N7 C21 C20 126.9(8) . . ? N2 C25 C24 122.9(8) . . ? N2 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C1 C2 C3 118.0(8) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? O7 C35 C31 118.0(7) . . ? O7 C35 C36 117.9(7) . . ? C31 C35 C36 124.0(8) . . ? Cd1 O11 H11A 117.6 . . ? Cd1 O11 H11B 110.0 . . ? H11A O11 H11B 117.6 . . ? Cd2 O12 H12A 126.6 5_765 . ? Cd2 O12 H12B 113.1 5_765 . ? H12A O12 H12B 115.3 . . ? O14A O14 H14A 64.7 . . ? O14A O14 H14B 93.8 . . ? H14A O14 H14B 129.2 . . ? O14A O14 H14C 42.8 . . ? H14A O14 H14C 22.1 . . ? H14B O14 H14C 122.6 . . ? O14A O14 H14D 57.4 . . ? H14A O14 H14D 104.4 . . ? H14B O14 H14D 36.5 . . ? H14C O14 H14D 89.9 . . ? O14 O14A H14A 57.1 . . ? O14 O14A H14B 42.8 . . ? H14A O14A H14B 89.0 . . ? O14 O14A H14C 93.7 . . ? H14A O14A H14C 36.7 . . ? H14B O14A H14C 122.4 . . ? O14 O14A H14D 64.1 . . ? H14A O14A H14D 103.8 . . ? H14B O14A H14D 21.4 . . ? H14C O14A H14D 130.0 . . ? H15A O15 H15B 98.4 . . ? H17A O17 H17B 139.5 . . ? H19A O19 H19B 117.7 . . ? H19A O19 H19C 114.5 . . ? H19B O19 H19C 12.1 . . ? H19A O19 H19D 13.1 . . ? H19B O19 H19D 116.2 . . ? H19C O19 H19D 110.3 . . ? H19A O19A H19B 107.7 . . ? H19A O19A H19C 118.9 . . ? H19B O19A H19C 12.4 . . ? H19A O19A H19D 15.8 . . ? H19B O19A H19D 122.6 . . ? H19C O19A H19D 133.0 . . ? H20A O20 H20B 97.4 . . ? H13A O13 H13B 128.1 . . ? H18C O18A H18D 106.7 . . ? H18B O18 H18A 140.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cd1 N1 C14 30.5(7) 4_655 . . . ? O11 Cd1 N1 C14 120.7(6) . . . . ? N2 Cd1 N1 C14 -177.3(7) . . . . ? O6 Cd1 N1 C14 -93.1(7) . . . . ? O5 Cd1 N1 C14 -54.3(6) . . . . ? C34 Cd1 N1 C14 -69.2(7) . . . . ? O2 Cd1 N1 C18 -146.3(5) 4_655 . . . ? O11 Cd1 N1 C18 -56.2(6) . . . . ? N2 Cd1 N1 C18 5.9(5) . . . . ? O6 Cd1 N1 C18 90.1(5) . . . . ? O5 Cd1 N1 C18 128.9(5) . . . . ? C34 Cd1 N1 C18 114.0(5) . . . . ? O2 Cd1 N2 C25 -115.2(7) 4_655 . . . ? O11 Cd1 N2 C25 -38.4(7) . . . . ? O6 Cd1 N2 C25 45.6(7) . . . . ? N1 Cd1 N2 C25 178.0(7) . . . . ? O5 Cd1 N2 C25 99.2(7) . . . . ? C34 Cd1 N2 C25 69.5(7) . . . . ? O2 Cd1 N2 C19 60.7(7) 4_655 . . . ? O11 Cd1 N2 C19 137.5(6) . . . . ? O6 Cd1 N2 C19 -138.5(5) . . . . ? N1 Cd1 N2 C19 -6.1(5) . . . . ? O5 Cd1 N2 C19 -84.9(6) . . . . ? C34 Cd1 N2 C19 -114.6(5) . . . . ? O9 Cd2 N3 C10 -148.6(8) 6_565 . . . ? O4 Cd2 N3 C10 10.1(7) . . . . ? O12 Cd2 N3 C10 -78.5(7) 5_765 . . . ? N4 Cd2 N3 C10 -177.4(7) . . . . ? O9 Cd2 N3 C9 41.7(10) 6_565 . . . ? O4 Cd2 N3 C9 -159.6(5) . . . . ? O12 Cd2 N3 C9 111.8(5) 5_765 . . . ? N4 Cd2 N3 C9 12.9(5) . . . . ? O9 Cd2 N4 C1 4.3(7) 6_565 . . . ? O4 Cd2 N4 C1 -160.4(6) . . . . ? O12 Cd2 N4 C1 88.1(7) 5_765 . . . ? N3 Cd2 N4 C1 176.7(7) . . . . ? O9 Cd2 N4 C5 175.6(5) 6_565 . . . ? O4 Cd2 N4 C5 10.9(10) . . . . ? O12 Cd2 N4 C5 -100.7(5) 5_765 . . . ? N3 Cd2 N4 C5 -12.1(5) . . . . ? O9 Cd2 O4 C27 -118.2(5) 6_565 . . . ? O12 Cd2 O4 C27 159.3(5) 5_765 . . . ? N4 Cd2 O4 C27 46.1(9) . . . . ? N3 Cd2 O4 C27 67.7(5) . . . . ? O2 Cd1 O5 C34 116.5(5) 4_655 . . . ? O11 Cd1 O5 C34 35.3(5) . . . . ? N2 Cd1 O5 C34 -80.1(5) . . . . ? O6 Cd1 O5 C34 -3.5(4) . . . . ? N1 Cd1 O5 C34 -149.2(5) . . . . ? O2 Cd1 O6 C34 -63.9(5) 4_655 . . . ? O11 Cd1 O6 C34 -148.6(5) . . . . ? N2 Cd1 O6 C34 126.3(5) . . . . ? N1 Cd1 O6 C34 53.4(5) . . . . ? O5 Cd1 O6 C34 3.5(4) . . . . ? Cd2 O9 C40 O8 -14.4(10) 6_566 . . . ? Cd2 O9 C40 C39 165.5(5) 6_566 . . . ? C13 N5 C6 C7 0.6(9) . . . . ? C13 N5 C6 C4 179.6(8) . . . . ? Cd2 O4 C27 O3 6.0(9) . . . . ? Cd2 O4 C27 C28 -174.3(5) . . . . ? C33 C32 C31 C30 -3.7(11) . . . . ? C33 C32 C31 C35 176.1(7) . . . . ? O3 C27 C28 C29 -168.5(7) . . . . ? O4 C27 C28 C29 11.8(10) . . . . ? O3 C27 C28 C33 5.0(11) . . . . ? O4 C27 C28 C33 -174.7(7) . . . . ? C1 N4 C5 C4 2.5(11) . . . . ? Cd2 N4 C5 C4 -169.2(5) . . . . ? C1 N4 C5 C9 -178.0(7) . . . . ? Cd2 N4 C5 C9 10.2(9) . . . . ? C4 C6 C7 N6 -179.4(7) . . . . ? N5 C6 C7 N6 -0.4(9) . . . . ? C4 C6 C7 C8 0.0(13) . . . . ? N5 C6 C7 C8 179.1(7) . . . . ? C13 N6 C7 C6 0.0(9) . . . . ? C13 N6 C7 C8 -179.4(8) . . . . ? C31 C32 C33 C28 1.8(11) . . . . ? C31 C32 C33 C34 176.4(7) . . . . ? C29 C28 C33 C32 1.0(11) . . . . ? C27 C28 C33 C32 -172.5(7) . . . . ? C29 C28 C33 C34 -173.2(7) . . . . ? C27 C28 C33 C34 13.3(11) . . . . ? O9 C40 C39 C41 -167.4(7) . . . . ? O8 C40 C39 C41 12.5(11) . . . . ? O9 C40 C39 C38 12.8(10) . . . . ? O8 C40 C39 C38 -167.3(7) . . . . ? C38 C39 C41 C43 2.1(11) . . . . ? C40 C39 C41 C43 -177.8(6) . . . . ? C38 C39 C41 C42 -178.2(7) . . . . ? C40 C39 C41 C42 1.9(11) . . . . ? C10 N3 C9 C8 -1.2(11) . . . . ? Cd2 N3 C9 C8 169.3(6) . . . . ? C10 N3 C9 C5 176.7(7) . . . . ? Cd2 N3 C9 C5 -12.8(8) . . . . ? N4 C5 C9 N3 1.9(10) . . . . ? C4 C5 C9 N3 -178.6(7) . . . . ? N4 C5 C9 C8 179.9(7) . . . . ? C4 C5 C9 C8 -0.7(11) . . . . ? C2 C3 C4 C6 -179.0(8) . . . . ? C2 C3 C4 C5 2.2(12) . . . . ? C7 C6 C4 C3 -177.2(8) . . . . ? N5 C6 C4 C3 4.0(14) . . . . ? C7 C6 C4 C5 1.6(12) . . . . ? N5 C6 C4 C5 -177.2(8) . . . . ? N4 C5 C4 C3 -2.9(11) . . . . ? C9 C5 C4 C3 177.7(7) . . . . ? N4 C5 C4 C6 178.2(7) . . . . ? C9 C5 C4 C6 -1.2(11) . . . . ? C14 N1 C18 C17 -1.3(11) . . . . ? Cd1 N1 C18 C17 175.7(5) . . . . ? C14 N1 C18 C19 177.9(7) . . . . ? Cd1 N1 C18 C19 -5.1(8) . . . . ? C22 C17 C18 N1 -178.9(7) . . . . ? C16 C17 C18 N1 2.5(11) . . . . ? C22 C17 C18 C19 1.9(11) . . . . ? C16 C17 C18 C19 -176.7(7) . . . . ? C18 N1 C14 C15 0.0(12) . . . . ? Cd1 N1 C14 C15 -176.7(6) . . . . ? C26 N8 C22 C21 0.5(10) . . . . ? C26 N8 C22 C17 -178.3(9) . . . . ? C18 C17 C22 N8 178.6(8) . . . . ? C16 C17 C22 N8 -3.0(15) . . . . ? C18 C17 C22 C21 0.0(12) . . . . ? C16 C17 C22 C21 178.4(8) . . . . ? C5 N4 C1 C2 -1.5(13) . . . . ? Cd2 N4 C1 C2 169.6(7) . . . . ? C33 C28 C29 C30 -1.8(11) . . . . ? C27 C28 C29 C30 171.9(7) . . . . ? Cd1 O5 C34 O6 6.1(7) . . . . ? Cd1 O5 C34 C33 -167.9(6) . . . . ? Cd1 O6 C34 O5 -6.5(8) . . . . ? Cd1 O6 C34 C33 167.4(6) . . . . ? C32 C33 C34 O5 67.1(10) . . . . ? C28 C33 C34 O5 -118.5(8) . . . . ? C32 C33 C34 O6 -107.0(8) . . . . ? C28 C33 C34 O6 67.4(11) . . . . ? C32 C33 C34 Cd1 -32(3) . . . . ? C28 C33 C34 Cd1 143(2) . . . . ? O2 Cd1 C34 O5 -63.9(5) 4_655 . . . ? O11 Cd1 C34 O5 -153.0(4) . . . . ? N2 Cd1 C34 O5 113.7(4) . . . . ? O6 Cd1 C34 O5 173.8(7) . . . . ? N1 Cd1 C34 O5 33.9(5) . . . . ? O2 Cd1 C34 O6 122.2(5) 4_655 . . . ? O11 Cd1 C34 O6 33.1(5) . . . . ? N2 Cd1 C34 O6 -60.2(5) . . . . ? N1 Cd1 C34 O6 -140.0(4) . . . . ? O5 Cd1 C34 O6 -173.8(7) . . . . ? O2 Cd1 C34 C33 40(3) 4_655 . . . ? O11 Cd1 C34 C33 -49(3) . . . . ? N2 Cd1 C34 C33 -142(3) . . . . ? O6 Cd1 C34 C33 -82(3) . . . . ? N1 Cd1 C34 C33 138(3) . . . . ? O5 Cd1 C34 C33 104(3) . . . . ? C32 C31 C30 C29 2.7(11) . . . . ? C35 C31 C30 C29 -177.0(7) . . . . ? C28 C29 C30 C31 0.0(11) . . . . ? Cd1 O2 C42 O1 -13.5(9) 4_645 . . . ? Cd1 O2 C42 C41 170.7(5) 4_645 . . . ? C39 C41 C42 O1 82.5(10) . . . . ? C43 C41 C42 O1 -97.8(8) . . . . ? C39 C41 C42 O2 -101.5(9) . . . . ? C43 C41 C42 O2 78.2(9) . . . . ? C39 C41 C43 C36 -0.7(11) . . . . ? C42 C41 C43 C36 179.5(7) . . . . ? C37 C36 C43 C41 -1.1(11) . . . . ? C35 C36 C43 C41 -179.0(7) . . . . ? C41 C39 C38 C37 -1.6(11) . . . . ? C40 C39 C38 C37 178.3(7) . . . . ? N1 C14 C15 C16 0.0(14) . . . . ? C25 N2 C19 C20 1.7(11) . . . . ? Cd1 N2 C19 C20 -174.4(6) . . . . ? C25 N2 C19 C18 -178.0(7) . . . . ? Cd1 N2 C19 C18 5.9(9) . . . . ? C23 C20 C19 N2 -0.5(12) . . . . ? C21 C20 C19 N2 178.6(7) . . . . ? C23 C20 C19 C18 179.2(7) . . . . ? C21 C20 C19 C18 -1.7(11) . . . . ? N1 C18 C19 N2 -0.5(10) . . . . ? C17 C18 C19 N2 178.7(7) . . . . ? N1 C18 C19 C20 179.8(7) . . . . ? C17 C18 C19 C20 -1.0(11) . . . . ? C43 C36 C37 C38 1.6(12) . . . . ? C35 C36 C37 C38 179.5(7) . . . . ? C39 C38 C37 C36 -0.3(12) . . . . ? C14 C15 C16 C17 1.2(13) . . . . ? C22 C17 C16 C15 179.1(8) . . . . ? C18 C17 C16 C15 -2.4(12) . . . . ? C9 N3 C10 C11 2.8(13) . . . . ? Cd2 N3 C10 C11 -166.6(7) . . . . ? C7 N6 C13 N5 0.4(10) . . . . ? C6 N5 C13 N6 -0.7(10) . . . . ? C8 C12 C11 C10 2.3(14) . . . . ? N3 C10 C11 C12 -3.4(15) . . . . ? C11 C12 C8 C9 -0.8(13) . . . . ? C11 C12 C8 C7 179.3(8) . . . . ? N3 C9 C8 C12 0.2(12) . . . . ? C5 C9 C8 C12 -177.7(7) . . . . ? N3 C9 C8 C7 -179.9(7) . . . . ? C5 C9 C8 C7 2.2(11) . . . . ? C6 C7 C8 C12 177.9(8) . . . . ? N6 C7 C8 C12 -2.7(14) . . . . ? C6 C7 C8 C9 -2.0(12) . . . . ? N6 C7 C8 C9 177.4(8) . . . . ? C19 C20 C23 C24 -0.6(13) . . . . ? C21 C20 C23 C24 -179.6(8) . . . . ? C20 C23 C24 C25 0.5(14) . . . . ? C21 N7 C26 N8 0.4(11) . . . . ? C22 N8 C26 N7 -0.6(12) . . . . ? N8 C22 C21 N7 -0.2(9) . . . . ? C17 C22 C21 N7 178.6(7) . . . . ? N8 C22 C21 C20 178.2(7) . . . . ? C17 C22 C21 C20 -2.9(13) . . . . ? C26 N7 C21 C22 -0.1(9) . . . . ? C26 N7 C21 C20 -178.5(8) . . . . ? C23 C20 C21 C22 -177.3(8) . . . . ? C19 C20 C21 C22 3.7(12) . . . . ? C23 C20 C21 N7 0.9(14) . . . . ? C19 C20 C21 N7 -178.1(7) . . . . ? C19 N2 C25 C24 -1.9(13) . . . . ? Cd1 N2 C25 C24 173.9(7) . . . . ? C23 C24 C25 N2 0.8(14) . . . . ? N4 C1 C2 C3 0.9(14) . . . . ? C4 C3 C2 C1 -1.3(13) . . . . ? C32 C31 C35 O7 35.6(12) . . . . ? C30 C31 C35 O7 -144.6(8) . . . . ? C32 C31 C35 C36 -143.5(8) . . . . ? C30 C31 C35 C36 36.2(12) . . . . ? C37 C36 C35 O7 -162.0(8) . . . . ? C43 C36 C35 O7 15.8(12) . . . . ? C37 C36 C35 C31 17.1(12) . . . . ? C43 C36 C35 C31 -165.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.510 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.123 # Attachment '12.cif' data_compound12 _database_code_depnum_ccdc_archive 'CCDC 710094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H26 N8 O11 Zn2, 3(H2 O)' _chemical_formula_sum 'C43 H32 N8 O14 Zn2' _chemical_formula_weight 1015.51 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.500(3) _cell_length_b 18.480(3) _cell_length_c 26.562(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.660(5) _cell_angle_gamma 90.00 _cell_volume 9920(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2712 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7602 _exptl_absorpt_correction_T_max 0.8355 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 24723 _diffrn_reflns_av_R_equivalents 0.1562 _diffrn_reflns_av_sigmaI/netI 0.3195 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.20 _reflns_number_total 8904 _reflns_number_gt 2711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.1945P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8904 _refine_ls_number_parameters 595 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.2408 _refine_ls_R_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.3698 _refine_ls_wR_factor_gt 0.3190 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.905 _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 Zn1 Zn 0.19706(6) 0.88111(7) 0.94279(5) 0.0449(5) Uani 1 1 d . . . Zn2 Zn 0.53556(7) 0.86383(8) 0.98855(5) 0.0501(6) Uani 1 1 d . . . O1 O 0.4954(6) 0.9117(7) 0.9122(5) 0.113(4) Uani 1 1 d . . . O2 O 0.3969(7) 0.8846(8) 0.9319(5) 0.137(5) Uani 1 1 d . . . O3 O 0.2908(6) 1.0003(8) 0.9315(5) 0.126(5) Uani 1 1 d . . . O5 O 0.4492(6) 1.2032(7) 0.5447(5) 0.116(4) Uani 1 1 d . . . O6 O 0.4722(6) 1.0889(7) 0.5417(4) 0.106(4) Uani 1 1 d . . . O7 O 0.2603(7) 1.1214(9) 0.7321(6) 0.163(7) Uani 1 1 d . . . O8 O 0.3165(6) 1.2549(7) 0.5521(5) 0.121(5) Uani 1 1 d . . . O9 O 0.3722(6) 1.3073(7) 0.6193(4) 0.116(4) Uani 1 1 d . . . C27 C 0.2892(10) 0.9626(13) 0.8932(8) 0.121(5) Uani 1 1 d DU . . C28 C 0.3354(8) 0.9810(10) 0.8544(5) 0.086(5) Uani 1 1 d D . . C29 C 0.4000(8) 0.9609(9) 0.8586(6) 0.083(5) Uani 1 1 d . . . C30 C 0.4351(10) 0.9188(9) 0.9048(8) 0.097(6) Uani 1 1 d . . . C31 C 0.4380(10) 0.9788(10) 0.8235(7) 0.117(7) Uani 1 1 d . . . H31A H 0.4812 0.9621 0.8263 0.140 Uiso 1 1 calc R . . C32 C 0.4093(9) 1.0250(10) 0.7811(6) 0.099(6) Uani 1 1 d . . . H32A H 0.4356 1.0416 0.7583 0.118 Uiso 1 1 calc R . . C33 C 0.3448(9) 1.0439(11) 0.7747(8) 0.124(8) Uani 1 1 d . . . C34 C 0.3068(9) 1.0280(10) 0.8118(7) 0.109(6) Uani 1 1 d . . . H34A H 0.2643 1.0466 0.8097 0.131 Uiso 1 1 calc R . . C35 C 0.3139(10) 1.0893(13) 0.7296(8) 0.121(7) Uani 1 1 d . . . C36 C 0.3425(6) 1.0985(7) 0.6846(4) 0.097(6) Uani 1 1 d G . . C37 C 0.3788(6) 1.0447(5) 0.6655(5) 0.132(8) Uani 1 1 d G . . H37A H 0.3829 0.9993 0.6808 0.159 Uiso 1 1 calc R . . C38 C 0.4091(5) 1.0587(6) 0.6234(4) 0.099(6) Uani 1 1 d G . . H38A H 0.4334 1.0227 0.6106 0.119 Uiso 1 1 calc R . . C39 C 0.4030(5) 1.1266(7) 0.6005(3) 0.085(5) Uani 1 1 d G . . C40 C 0.3666(6) 1.1804(5) 0.6197(4) 0.074(4) Uani 1 1 d G . . C41 C 0.3363(5) 1.1664(6) 0.6617(4) 0.098(6) Uani 1 1 d G . . H41A H 0.3120 1.2024 0.6746 0.118 Uiso 1 1 calc R . . C42 C 0.4399(10) 1.1413(10) 0.5593(9) 0.113(7) Uani 1 1 d . . . C43 C 0.3529(10) 1.2458(10) 0.5952(6) 0.090(5) Uani 1 1 d . . . C18 C 0.0680(9) 1.0584(11) 1.0590(8) 0.096(6) Uani 1 1 d . . . N7 N 0.0454(9) 1.0971(13) 1.0989(10) 0.173(8) Uani 1 1 d . . . C19 C 0.0156(14) 1.1514(14) 1.0721(14) 0.182(16) Uani 1 1 d . . . H19A H 0.0026 1.1920 1.0886 0.218 Uiso 1 1 calc R . . N8 N 0.0046(9) 1.1481(12) 1.0224(10) 0.154(9) Uani 1 1 d . . . H8A H -0.0197 1.1755 1.0007 0.185 Uiso 1 1 calc R . . C20 C 0.0442(8) 1.0860(10) 1.0134(9) 0.089(5) Uani 1 1 d . . . C21 C 0.0576(8) 1.0619(10) 0.9671(6) 0.091(5) Uani 1 1 d D . . C25 C 0.0987(8) 1.0078(8) 0.9729(7) 0.084(5) Uani 1 1 d D . . N5 N 0.1662(8) 0.9104(9) 1.0219(6) 0.117(5) Uani 1 1 d . . . C14 C 0.1873(10) 0.8753(10) 1.0651(8) 0.121(7) Uani 1 1 d D . . H14A H 0.2132 0.8340 1.0651 0.145 Uiso 1 1 calc R . . C15 C 0.1703(11) 0.9010(13) 1.1101(7) 0.171(12) Uani 1 1 d D . . H15A H 0.1872 0.8784 1.1408 0.205 Uiso 1 1 calc R . . C16 C 0.1279(13) 0.9606(12) 1.1098(7) 0.140(9) Uani 1 1 d D . . H16A H 0.1133 0.9751 1.1396 0.168 Uiso 1 1 calc R . . C17 C 0.1082(8) 0.9973(9) 1.0645(7) 0.083(5) Uani 1 1 d D . . C26 C 0.1248(9) 0.9687(11) 1.0211(9) 0.118(7) Uani 1 1 d . . . C5 C 0.7171(8) 0.6512(10) 1.0662(7) 0.086(5) Uani 1 1 d . . . N3 N 0.7539(8) 0.5971(10) 1.0946(6) 0.112(5) Uani 1 1 d . . . C6 C 0.7788(10) 0.5598(12) 1.0633(9) 0.112(7) Uani 1 1 d . . . H6A H 0.8090 0.5226 1.0726 0.134 Uiso 1 1 calc R . . N4 N 0.7570(7) 0.5796(8) 1.0153(8) 0.116(5) Uani 1 1 d . . . H4A H 0.7659 0.5579 0.9886 0.140 Uiso 1 1 calc R . . C7 C 0.7171(8) 0.6417(9) 1.0151(7) 0.081(5) Uani 1 1 d . . . N2 N 0.6124(8) 0.7882(10) 0.9574(7) 0.135(6) Uani 1 1 d . . . C12 C 0.6497(9) 0.7406(11) 0.9942(7) 0.096(6) Uani 1 1 d . . . C8 C 0.6850(8) 0.6867(10) 0.9768(9) 0.107(6) Uani 1 1 d . . . C9 C 0.6885(9) 0.6800(11) 0.9236(7) 0.109(5) Uani 1 1 d U . . H9A H 0.7149 0.6440 0.9129 0.131 Uiso 1 1 calc R . . C10 C 0.6545(9) 0.7244(11) 0.8889(8) 0.116(5) Uani 1 1 d U . . H10A H 0.6588 0.7215 0.8546 0.139 Uiso 1 1 calc R . . C11 C 0.6120(10) 0.7757(11) 0.9058(8) 0.125(5) Uani 1 1 d U . . H11A H 0.5831 0.8019 0.8817 0.150 Uiso 1 1 calc R . . C1 C 0.6125(10) 0.8226(13) 1.1080(7) 0.123(7) Uani 1 1 d . . . H1A H 0.5930 0.8645 1.1180 0.148 Uiso 1 1 calc R . . C2 C 0.6406(11) 0.7791(13) 1.1427(8) 0.146(9) Uani 1 1 d . . . H2A H 0.6348 0.7882 1.1761 0.175 Uiso 1 1 calc R . . C3 C 0.6768(9) 0.7230(11) 1.1352(7) 0.108(6) Uani 1 1 d . . . H3A H 0.6983 0.6940 1.1615 0.129 Uiso 1 1 calc R . . C4 C 0.6801(9) 0.7104(9) 1.0811(8) 0.101(6) Uani 1 1 d . . . C13 C 0.6466(7) 0.7515(9) 1.0463(7) 0.077(4) Uani 1 1 d . . . N1 N 0.6099(6) 0.8098(8) 1.0572(6) 0.100(4) Uani 1 1 d . . . O10 O 0.5965(6) 0.9701(6) 0.9943(5) 0.137(5) Uani 1 1 d . . . H10C H 0.6286 0.9785 1.0151 0.205 Uiso 1 1 d R . . H10D H 0.5764 1.0054 0.9834 0.205 Uiso 1 1 d R . . O12 O 0.9521(9) 0.2488(8) 0.9440(7) 0.210(8) Uani 1 1 d . . . H12C H 0.9351 0.2878 0.9401 0.316 Uiso 1 1 d R . . H12D H 0.9820 0.2589 0.9663 0.316 Uiso 1 1 d R . . O13 O 0.0494(17) 0.321(2) 0.7779(12) 0.49(2) Uani 1 1 d . . . H13C H 0.0281 0.2986 0.7951 0.733 Uiso 1 1 d R . . H13D H 0.0216 0.3490 0.7634 0.733 Uiso 1 1 d R . . O11 O 0.2993(6) 0.8618(8) 0.9912(5) 0.151(6) Uani 1 1 d . . . H11C H 0.3272 0.8688 0.9741 0.227 Uiso 1 1 d R . . H11D H 0.3043 0.8272 1.0096 0.227 Uiso 1 1 d R . . O14 O 0.965(2) 0.2406(17) 0.8425(11) 0.55(3) Uani 1 1 d . . . H14C H 0.9620 0.2430 0.8722 0.825 Uiso 1 1 d R . . H14D H 0.9426 0.2097 0.8271 0.825 Uiso 1 1 d R . . O4 O 0.2483(6) 0.9110(8) 0.8795(5) 0.131(4) Uani 1 1 d U . . N6 N 0.1206(7) 0.9757(8) 0.9280(7) 0.114(5) Uani 1 1 d . . . C24 C 0.0976(10) 1.0037(10) 0.8858(7) 0.140(6) Uani 1 1 d DU . . H24A H 0.1097 0.9830 0.8568 0.168 Uiso 1 1 calc R . . C22 C 0.0342(9) 1.0951(10) 0.9204(6) 0.134(6) Uani 1 1 d DU . . H22A H 0.0066 1.1354 0.9177 0.160 Uiso 1 1 calc R . . C23 C 0.0551(10) 1.0636(11) 0.8784(6) 0.137(6) Uani 1 1 d DU . . H23A H 0.0411 1.0820 0.8457 0.164 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 Zn1 0.0521(9) 0.0468(9) 0.0381(9) -0.0004(7) 0.0147(6) -0.0005(6) Zn2 0.0471(9) 0.0615(10) 0.0440(9) 0.0094(7) 0.0144(7) 0.0117(7) O1 0.102(10) 0.121(11) 0.111(10) 0.042(8) 0.006(8) 0.014(8) O2 0.131(11) 0.186(15) 0.103(10) 0.057(9) 0.042(9) 0.035(10) O3 0.136(11) 0.149(12) 0.098(10) -0.025(8) 0.032(8) -0.009(9) O5 0.147(11) 0.096(9) 0.114(10) 0.003(8) 0.041(8) -0.030(8) O6 0.099(9) 0.138(11) 0.091(8) -0.008(8) 0.041(7) -0.014(8) O7 0.088(9) 0.254(19) 0.159(13) 0.074(12) 0.058(9) 0.030(11) O8 0.136(11) 0.147(12) 0.074(9) 0.016(8) 0.004(8) 0.018(9) O9 0.125(10) 0.124(11) 0.102(9) -0.006(8) 0.027(8) 0.007(9) C27 0.093(12) 0.162(15) 0.108(11) -0.007(11) 0.017(10) -0.013(9) C28 0.092(13) 0.122(15) 0.045(9) 0.007(9) 0.012(9) -0.013(11) C29 0.074(11) 0.100(13) 0.083(12) 0.038(10) 0.039(10) 0.032(9) C30 0.074(13) 0.078(12) 0.139(18) 0.030(12) 0.025(13) 0.013(10) C31 0.136(17) 0.127(17) 0.091(14) 0.034(12) 0.034(13) 0.021(13) C32 0.081(13) 0.140(17) 0.078(12) 0.016(11) 0.021(10) -0.002(11) C33 0.057(11) 0.18(2) 0.131(17) 0.095(15) 0.018(11) 0.005(12) C34 0.091(13) 0.130(16) 0.111(16) 0.009(13) 0.029(12) -0.020(11) C35 0.076(14) 0.16(2) 0.128(19) 0.006(15) 0.035(13) 0.003(13) C36 0.106(14) 0.139(17) 0.053(10) 0.000(11) 0.037(10) 0.013(12) C37 0.144(18) 0.109(16) 0.17(2) 0.028(14) 0.097(16) 0.019(13) C38 0.129(15) 0.115(16) 0.062(11) 0.000(10) 0.038(11) 0.005(12) C39 0.089(12) 0.081(12) 0.089(12) 0.036(10) 0.030(9) 0.019(9) C40 0.106(13) 0.051(10) 0.061(10) 0.017(8) 0.001(9) 0.007(8) C41 0.132(15) 0.075(12) 0.088(13) 0.033(10) 0.020(11) 0.024(10) C42 0.143(18) 0.053(12) 0.17(2) 0.015(12) 0.090(16) 0.020(11) C43 0.128(16) 0.086(14) 0.059(11) -0.016(10) 0.026(11) -0.019(11) C18 0.110(15) 0.107(15) 0.083(14) -0.013(12) 0.045(12) 0.025(12) N7 0.093(13) 0.17(2) 0.27(3) -0.03(2) 0.071(16) -0.040(13) C19 0.16(2) 0.083(18) 0.28(4) 0.04(2) -0.06(3) 0.032(15) N8 0.091(13) 0.128(17) 0.23(3) 0.041(18) -0.011(16) -0.005(12) C20 0.062(11) 0.090(14) 0.111(17) 0.009(12) 0.010(11) 0.011(9) C21 0.071(12) 0.110(15) 0.096(14) 0.012(12) 0.026(11) 0.009(10) C25 0.086(13) 0.060(11) 0.101(14) 0.004(10) 0.003(11) -0.001(9) N5 0.146(14) 0.120(14) 0.087(12) 0.002(10) 0.023(10) 0.027(11) C14 0.153(19) 0.126(18) 0.083(14) 0.024(13) 0.017(14) -0.003(13) C15 0.18(3) 0.27(4) 0.058(15) 0.020(18) 0.016(15) -0.08(2) C16 0.20(3) 0.12(2) 0.097(18) -0.005(14) 0.025(17) 0.048(16) C17 0.078(12) 0.081(12) 0.086(13) -0.010(11) 0.006(10) 0.009(9) C26 0.089(14) 0.125(17) 0.131(19) -0.048(15) -0.009(13) 0.046(12) C5 0.101(13) 0.085(13) 0.070(12) 0.026(10) 0.008(10) 0.024(10) N3 0.127(14) 0.116(14) 0.101(13) 0.010(11) 0.041(11) 0.007(11) C6 0.115(17) 0.133(19) 0.079(15) 0.016(14) -0.009(13) 0.003(14) N4 0.107(12) 0.092(12) 0.158(17) -0.051(11) 0.045(12) -0.004(10) C7 0.076(11) 0.073(12) 0.097(15) 0.000(10) 0.024(10) 0.005(9) N2 0.114(13) 0.169(17) 0.125(15) 0.009(13) 0.028(12) -0.014(12) C12 0.102(14) 0.118(16) 0.074(13) 0.021(11) 0.033(11) 0.025(12) C8 0.069(12) 0.086(14) 0.17(2) 0.004(15) 0.037(13) 0.011(10) C9 0.114(12) 0.129(14) 0.094(12) 0.004(9) 0.043(10) 0.001(9) C10 0.121(12) 0.128(13) 0.110(11) 0.009(8) 0.052(9) 0.007(8) C11 0.129(13) 0.135(14) 0.121(12) 0.014(10) 0.053(10) 0.012(9) C1 0.146(18) 0.16(2) 0.062(13) -0.005(13) 0.008(13) 0.002(15) C2 0.17(2) 0.17(2) 0.094(16) 0.052(15) -0.006(14) 0.081(18) C3 0.100(14) 0.119(17) 0.091(15) 0.003(12) -0.020(12) 0.028(12) C4 0.116(15) 0.061(12) 0.118(17) 0.015(11) 0.001(13) 0.018(10) C13 0.070(11) 0.071(11) 0.095(13) 0.005(10) 0.024(10) 0.015(8) N1 0.089(10) 0.121(12) 0.085(11) -0.017(9) -0.001(8) 0.027(9) O10 0.139(11) 0.113(11) 0.149(12) 0.035(9) -0.003(9) -0.002(8) O12 0.29(2) 0.129(13) 0.237(19) 0.020(13) 0.107(17) 0.027(14) O13 0.45(5) 0.68(6) 0.34(5) -0.10(4) 0.07(3) -0.08(5) O11 0.126(11) 0.212(16) 0.128(12) 0.037(10) 0.059(9) -0.006(10) O14 0.81(8) 0.42(5) 0.32(4) 0.00(3) -0.22(5) 0.17(5) O4 0.104(10) 0.172(14) 0.114(9) -0.004(9) 0.013(8) -0.014(8) N6 0.105(12) 0.114(13) 0.118(13) 0.032(11) 0.006(10) -0.003(9) C24 0.153(14) 0.160(15) 0.099(11) 0.052(11) 0.001(11) 0.022(11) C22 0.140(13) 0.157(15) 0.098(12) 0.057(11) 0.003(11) 0.017(11) C23 0.145(13) 0.157(14) 0.101(11) 0.056(11) -0.001(10) 0.023(10) _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 Zn1 O4 2.196(13) . ? Zn1 O11 2.295(14) . ? Zn1 N6 2.337(15) . ? Zn1 O8 2.355(13) 4_546 ? Zn1 N5 2.358(15) . ? Zn1 O9 2.410(12) 4_546 ? Zn2 O1 2.239(11) . ? Zn2 O6 2.249(11) 6_576 ? Zn2 O10 2.320(12) . ? Zn2 N2 2.358(19) . ? Zn2 N1 2.390(13) . ? O1 C30 1.225(18) . ? O2 C30 1.313(19) . ? O3 C27 1.23(2) . ? O5 C42 1.232(18) . ? O6 C42 1.304(18) . ? O6 Zn2 2.249(11) 6_575 ? O7 C35 1.26(2) . ? O8 C43 1.267(18) . ? O8 Zn1 2.355(13) 4_556 ? O9 C43 1.332(18) . ? O9 Zn1 2.410(12) 4_556 ? C27 O4 1.28(2) . ? C27 C28 1.549(16) . ? C28 C29 1.362(19) . ? C28 C34 1.47(2) . ? C29 C31 1.35(2) . ? C29 C30 1.53(2) . ? C31 C32 1.46(2) . ? C31 H31A 0.9300 . ? C32 C33 1.35(2) . ? C32 H32A 0.9300 . ? C33 C34 1.39(2) . ? C33 C35 1.51(2) . ? C34 H34A 0.9300 . ? C35 C36 1.43(2) . ? C36 C37 1.3900 . ? C36 C41 1.3900 . ? C37 C38 1.3900 . ? C37 H37A 0.9300 . ? C38 C39 1.3900 . ? C38 H38A 0.9300 . ? C39 C40 1.3900 . ? C39 C42 1.46(2) . ? C40 C43 1.379(19) . ? C40 C41 1.3900 . ? C41 H41A 0.9300 . ? C18 C20 1.33(2) . ? C18 C17 1.39(2) . ? C18 N7 1.42(2) . ? N7 C19 1.32(3) . ? C19 N8 1.30(3) . ? C19 H19A 0.9300 . ? N8 C20 1.45(2) . ? N8 H8A 0.8600 . ? C20 C21 1.38(2) . ? C21 C25 1.300(18) . ? C21 C22 1.40(2) . ? C25 N6 1.47(2) . ? C25 C26 1.49(2) . ? N5 C14 1.33(2) . ? N5 C26 1.37(2) . ? C14 C15 1.38(3) . ? C14 H14A 0.9300 . ? C15 C16 1.40(3) . ? C15 H15A 0.9300 . ? C16 C17 1.38(3) . ? C16 H16A 0.9300 . ? C17 C26 1.36(2) . ? C5 C7 1.37(2) . ? C5 N3 1.40(2) . ? C5 C4 1.43(2) . ? N3 C6 1.25(2) . ? C6 N4 1.33(2) . ? C6 H6A 0.9300 . ? N4 C7 1.41(2) . ? N4 H4A 0.8600 . ? C7 C8 1.39(2) . ? N2 C11 1.39(2) . ? N2 C12 1.44(2) . ? C12 C8 1.36(2) . ? C12 C13 1.41(2) . ? C8 C9 1.43(2) . ? C9 C10 1.34(2) . ? C9 H9A 0.9300 . ? C10 C11 1.41(2) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C1 C2 1.28(2) . ? C1 N1 1.362(19) . ? C1 H1A 0.9300 . ? C2 C3 1.31(2) . ? C2 H2A 0.9300 . ? C3 C4 1.47(2) . ? C3 H3A 0.9300 . ? C4 C13 1.30(2) . ? C13 N1 1.373(18) . ? O10 H10C 0.7999 . ? O10 H10D 0.8000 . ? O12 H12C 0.7999 . ? O12 H12D 0.7997 . ? O13 H13C 0.8001 . ? O13 H13D 0.8164 . ? O11 H11C 0.7999 . ? O11 H11D 0.8001 . ? O14 H14C 0.8004 . ? O14 H14D 0.7998 . ? N6 C24 1.253(19) . ? C24 C23 1.40(3) . ? C24 H24A 0.9300 . ? C22 C23 1.39(2) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O11 87.6(5) . . ? O4 Zn1 N6 94.4(6) . . ? O11 Zn1 N6 137.3(5) . . ? O4 Zn1 O8 111.7(5) . 4_546 ? O11 Zn1 O8 85.4(5) . 4_546 ? N6 Zn1 O8 131.9(5) . 4_546 ? O4 Zn1 N5 149.2(6) . . ? O11 Zn1 N5 83.8(5) . . ? N6 Zn1 N5 72.9(6) . . ? O8 Zn1 N5 97.1(5) 4_546 . ? O4 Zn1 O9 85.5(5) . 4_546 ? O11 Zn1 O9 132.3(5) . 4_546 ? N6 Zn1 O9 90.4(5) . 4_546 ? O8 Zn1 O9 54.3(4) 4_546 4_546 ? N5 Zn1 O9 121.6(5) . 4_546 ? O1 Zn2 O6 104.6(5) . 6_576 ? O1 Zn2 O10 80.6(4) . . ? O6 Zn2 O10 89.5(5) 6_576 . ? O1 Zn2 N2 94.7(6) . . ? O6 Zn2 N2 160.2(6) 6_576 . ? O10 Zn2 N2 98.1(5) . . ? O1 Zn2 N1 161.2(5) . . ? O6 Zn2 N1 92.5(5) 6_576 . ? O10 Zn2 N1 92.1(5) . . ? N2 Zn2 N1 69.1(6) . . ? C30 O1 Zn2 113.3(13) . . ? C42 O6 Zn2 108.5(12) . 6_575 ? C43 O8 Zn1 97.9(11) . 4_556 ? C43 O9 Zn1 93.5(11) . 4_556 ? O3 C27 O4 125.5(19) . . ? O3 C27 C28 119(2) . . ? O4 C27 C28 114.8(19) . . ? C29 C28 C34 118.7(15) . . ? C29 C28 C27 125.5(16) . . ? C34 C28 C27 115.6(17) . . ? C31 C29 C28 122.7(15) . . ? C31 C29 C30 115.5(16) . . ? C28 C29 C30 121.7(15) . . ? O1 C30 O2 122.6(17) . . ? O1 C30 C29 120.7(18) . . ? O2 C30 C29 116.2(16) . . ? C29 C31 C32 118.2(18) . . ? C29 C31 H31A 120.9 . . ? C32 C31 H31A 120.9 . . ? C33 C32 C31 120.6(17) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 120.6(17) . . ? C32 C33 C35 121.0(17) . . ? C34 C33 C35 118.1(17) . . ? C33 C34 C28 118.3(17) . . ? C33 C34 H34A 120.8 . . ? C28 C34 H34A 120.8 . . ? O7 C35 C36 118.1(19) . . ? O7 C35 C33 118.2(19) . . ? C36 C35 C33 123.6(18) . . ? C37 C36 C41 120.0 . . ? C37 C36 C35 122.8(13) . . ? C41 C36 C35 117.0(13) . . ? C38 C37 C36 120.0 . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 C42 118.5(11) . . ? C40 C39 C42 121.3(11) . . ? C43 C40 C39 122.3(11) . . ? C43 C40 C41 117.3(11) . . ? C39 C40 C41 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 H41A 120.0 . . ? C36 C41 H41A 120.0 . . ? O5 C42 O6 117.6(18) . . ? O5 C42 C39 122.5(16) . . ? O6 C42 C39 119.3(15) . . ? O8 C43 O9 113.7(17) . . ? O8 C43 C40 125.8(16) . . ? O9 C43 C40 120.1(16) . . ? C20 C18 C17 121.7(18) . . ? C20 C18 N7 112(2) . . ? C17 C18 N7 126(2) . . ? C19 N7 C18 99(3) . . ? N8 C19 N7 120(3) . . ? N8 C19 H19A 120.1 . . ? N7 C19 H19A 120.1 . . ? C19 N8 C20 101(2) . . ? C19 N8 H8A 129.3 . . ? C20 N8 H8A 129.3 . . ? C18 C20 C21 126.4(18) . . ? C18 C20 N8 106.4(19) . . ? C21 C20 N8 127(2) . . ? C25 C21 C20 111.3(15) . . ? C25 C21 C22 124.4(15) . . ? C20 C21 C22 124.1(17) . . ? C21 C25 N6 119.6(14) . . ? C21 C25 C26 127.4(18) . . ? N6 C25 C26 112.8(15) . . ? C14 N5 C26 120.8(18) . . ? C14 N5 Zn1 124.1(13) . . ? C26 N5 Zn1 115.1(14) . . ? N5 C14 C15 119.1(19) . . ? N5 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C14 C15 C16 121(2) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C17 C16 C15 119(2) . . ? C17 C16 H16A 120.7 . . ? C15 C16 H16A 120.7 . . ? C26 C17 C16 118.0(18) . . ? C26 C17 C18 117.0(17) . . ? C16 C17 C18 124.8(19) . . ? C17 C26 N5 122.2(19) . . ? C17 C26 C25 115.8(18) . . ? N5 C26 C25 121.9(19) . . ? C7 C5 N3 110.8(17) . . ? C7 C5 C4 117.6(16) . . ? N3 C5 C4 131.6(19) . . ? C6 N3 C5 106.2(18) . . ? N3 C6 N4 112(2) . . ? N3 C6 H6A 123.9 . . ? N4 C6 H6A 123.9 . . ? C6 N4 C7 109.1(17) . . ? C6 N4 H4A 125.4 . . ? C7 N4 H4A 125.4 . . ? C5 C7 C8 124.8(18) . . ? C5 C7 N4 101.4(16) . . ? C8 C7 N4 133.8(19) . . ? C11 N2 C12 119.0(19) . . ? C11 N2 Zn2 123.5(14) . . ? C12 N2 Zn2 115.7(13) . . ? C8 C12 C13 123.6(19) . . ? C8 C12 N2 118.0(19) . . ? C13 C12 N2 118.3(18) . . ? C12 C8 C7 114(2) . . ? C12 C8 C9 121(2) . . ? C7 C8 C9 125.0(19) . . ? C10 C9 C8 121(2) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 118(2) . . ? C9 C10 H10A 120.9 . . ? C11 C10 H10A 120.9 . . ? N2 C11 C10 122(2) . . ? N2 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C2 C1 N1 123(2) . . ? C2 C1 H1A 118.7 . . ? N1 C1 H1A 118.7 . . ? C1 C2 C3 126(2) . . ? C1 C2 H2A 117.1 . . ? C3 C2 H2A 117.1 . . ? C2 C3 C4 113.2(17) . . ? C2 C3 H3A 123.4 . . ? C4 C3 H3A 123.4 . . ? C13 C4 C5 119(2) . . ? C13 C4 C3 119.9(18) . . ? C5 C4 C3 120.5(17) . . ? C4 C13 N1 123.4(18) . . ? C4 C13 C12 120.6(18) . . ? N1 C13 C12 115.9(16) . . ? C1 N1 C13 114.5(16) . . ? C1 N1 Zn2 126.7(13) . . ? C13 N1 Zn2 117.9(11) . . ? Zn2 O10 H10C 125.5 . . ? Zn2 O10 H10D 115.2 . . ? H10C O10 H10D 114.1 . . ? H12C O12 H12D 98.4 . . ? H13C O13 H13D 101.2 . . ? Zn1 O11 H11C 109.3 . . ? Zn1 O11 H11D 118.6 . . ? H11C O11 H11D 116.4 . . ? H14C O14 H14D 114.5 . . ? C27 O4 Zn1 110.2(12) . . ? C24 N6 C25 116.0(16) . . ? C24 N6 Zn1 127.0(15) . . ? C25 N6 Zn1 117.0(11) . . ? N6 C24 C23 125.7(17) . . ? N6 C24 H24A 117.1 . . ? C23 C24 H24A 117.1 . . ? C23 C22 C21 115.0(11) . . ? C23 C22 H22A 122.5 . . ? C21 C22 H22A 122.5 . . ? C22 C23 C24 119.1(12) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.931 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.181 # Attachment '13.cif' data_compound13 _database_code_depnum_ccdc_archive 'CCDC 710095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21H14CdN4O5, 0.5(H2O)' _chemical_formula_sum 'C21 H15 Cd N4 O5.50' _chemical_formula_weight 523.77 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 25.355(4) _cell_length_b 6.7343(10) _cell_length_c 11.0811(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1892.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3512 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7218 _exptl_absorpt_correction_T_max 0.8126 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 9425 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1931 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.1920P)^2^+2.4017P] 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), 1484 Friedel pairs ' _refine_ls_abs_structure_Flack 0.001(7) _refine_ls_number_reflns 1931 _refine_ls_number_parameters 290 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2342 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.006 _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 Cd1 Cd 0.29812(5) 0.4061(2) 0.09270(11) 0.0423(5) Uani 1 1 d . . . O1 O 0.2611(3) 0.2964(15) 0.2403(7) 0.020(2) Uani 1 1 d . . . O2 O 0.1808(4) 0.4233(17) 0.2044(8) 0.027(2) Uani 1 1 d . . . O3 O 0.1913(4) 0.2001(14) 0.8457(7) 0.023(2) Uani 1 1 d . . . O4 O 0.1119(4) 0.3101(17) 0.8058(8) 0.030(2) Uani 1 1 d U . . N1 N 0.3751(4) 0.3145(17) 0.1586(9) 0.017(2) Uani 1 1 d . . . N2 N 0.3411(4) 0.3730(15) -0.0678(9) 0.015(2) Uani 1 1 d U . . N3 N 0.5242(4) 0.2343(17) -0.1989(9) 0.018(2) Uani 1 1 d . . . N4 N 0.5513(4) 0.2211(17) -0.0069(10) 0.020(2) Uani 1 1 d . . . H4A H 0.5727 0.2122 0.0531 0.024 Uiso 1 1 calc R . . C1 C 0.3236(5) 0.400(2) -0.1825(12) 0.018(3) Uani 1 1 d U . . H1A H 0.2883 0.4336 -0.1934 0.022 Uiso 1 1 calc R . . C2 C 0.3538(6) 0.382(2) -0.2808(13) 0.027(3) Uani 1 1 d . . . H2A H 0.3398 0.4030 -0.3573 0.032 Uiso 1 1 calc R . . C3 C 0.4083(5) 0.330(2) -0.2660(12) 0.020(3) Uani 1 1 d . . . H3A H 0.4304 0.3183 -0.3326 0.024 Uiso 1 1 calc R . . C4 C 0.4276(5) 0.2960(18) -0.1496(11) 0.015(3) Uani 1 1 d . . . C5 C 0.3929(5) 0.3191(17) -0.0550(11) 0.013(2) Uani 1 1 d U . . C6 C 0.4812(5) 0.2574(17) -0.1265(12) 0.017(3) Uani 1 1 d . . . C7 C 0.5645(5) 0.2103(17) -0.1300(12) 0.019(3) Uani 1 1 d . . . H7A H 0.5985 0.1884 -0.1583 0.023 Uiso 1 1 calc R . . C8 C 0.4990(6) 0.2477(17) -0.0009(10) 0.018(3) Uani 1 1 d . . . C9 C 0.4649(4) 0.2615(16) 0.0958(12) 0.013(2) Uani 1 1 d . . . C10 C 0.4780(5) 0.248(2) 0.2200(11) 0.020(3) Uani 1 1 d U . . H10A H 0.5128 0.2264 0.2428 0.024 Uiso 1 1 calc R . . C11 C 0.4406(6) 0.266(2) 0.3047(12) 0.030(3) Uani 1 1 d U . . H11A H 0.4490 0.2570 0.3862 0.036 Uiso 1 1 calc R . . C12 C 0.3909(6) 0.298(2) 0.2694(14) 0.032(3) Uani 1 1 d . . . H12A H 0.3654 0.3098 0.3294 0.038 Uiso 1 1 calc R . . C13 C 0.4105(5) 0.2956(17) 0.0712(10) 0.013(2) Uani 1 1 d . . . C14 C 0.2143(5) 0.3438(18) 0.2724(11) 0.013(3) Uani 1 1 d U . . C15 C 0.1997(5) 0.3153(17) 0.3995(10) 0.014(2) Uani 1 1 d . . . C16 C 0.2363(5) 0.253(2) 0.4850(12) 0.020(3) Uani 1 1 d . . . H16A H 0.2705 0.2233 0.4609 0.024 Uiso 1 1 calc R . . C17 C 0.2227(5) 0.2366(18) 0.6033(11) 0.016(2) Uani 1 1 d . . . H17A H 0.2478 0.1953 0.6591 0.019 Uiso 1 1 calc R . . C18 C 0.1722(5) 0.2799(19) 0.6416(10) 0.014(2) Uani 1 1 d . . . C19 C 0.1346(5) 0.340(2) 0.5605(10) 0.020(3) Uani 1 1 d . . . H19A H 0.1005 0.3672 0.5864 0.024 Uiso 1 1 calc R . . C20 C 0.1479(5) 0.362(2) 0.4376(11) 0.020(3) Uani 1 1 d U . . H20A H 0.1230 0.4068 0.3824 0.024 Uiso 1 1 calc R . . C21 C 0.1577(5) 0.2613(18) 0.7749(10) 0.014(2) Uani 1 1 d U . . O1W O 0.0006(15) 0.378(5) 0.447(2) 0.071(8) Uani 0.50 1 d PU . . H1C H 0.0097 0.3447 0.3776 0.107 Uiso 0.50 1 d PR . . H1D H 0.0303 0.3724 0.4835 0.107 Uiso 0.50 1 d PR . . O2W O 0.2296(3) 0.4858(15) 0.0008(7) 0.0183(19) Uani 1 1 d U . . H2C H 0.2050 0.4723 0.0453 0.027 Uiso 1 1 d R . . H2D H 0.2187 0.4024 -0.0441 0.027 Uiso 1 1 d 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 Cd1 0.0347(8) 0.0586(8) 0.0336(7) 0.0050(6) 0.0039(6) 0.0058(6) O1 0.021(5) 0.030(5) 0.010(4) 0.003(4) 0.002(4) 0.004(4) O2 0.017(5) 0.050(6) 0.015(4) 0.002(5) 0.005(4) 0.004(5) O3 0.029(5) 0.030(5) 0.009(4) 0.006(4) -0.008(4) -0.004(4) O4 0.016(4) 0.060(6) 0.013(4) 0.010(4) 0.010(4) 0.009(4) N1 0.009(5) 0.028(6) 0.014(5) 0.007(5) -0.004(4) -0.001(4) N2 0.005(4) 0.021(5) 0.019(5) 0.001(4) -0.006(4) -0.002(4) N3 0.015(5) 0.028(6) 0.011(5) -0.002(5) -0.005(4) -0.004(5) N4 0.018(6) 0.021(6) 0.021(5) 0.006(5) -0.010(5) -0.010(5) C1 0.006(5) 0.028(6) 0.020(5) 0.001(5) 0.000(4) 0.005(5) C2 0.038(8) 0.028(7) 0.014(6) 0.006(6) -0.008(6) -0.007(6) C3 0.013(6) 0.031(7) 0.016(6) -0.004(5) 0.003(5) 0.000(5) C4 0.021(7) 0.008(6) 0.016(6) 0.000(5) -0.001(5) -0.004(5) C5 0.006(5) 0.011(5) 0.023(6) 0.006(4) 0.003(5) -0.003(4) C6 0.019(7) 0.007(5) 0.027(7) 0.006(5) 0.003(5) -0.004(4) C7 0.022(7) 0.007(5) 0.029(7) 0.000(5) 0.019(6) -0.001(5) C8 0.033(7) 0.009(5) 0.011(5) 0.000(4) -0.011(6) -0.003(6) C9 0.005(5) 0.012(5) 0.023(6) 0.004(5) -0.005(5) 0.000(4) C10 0.021(6) 0.022(6) 0.016(5) -0.003(5) -0.014(5) 0.002(5) C11 0.035(7) 0.040(7) 0.015(6) -0.002(6) -0.007(5) -0.006(6) C12 0.038(9) 0.028(8) 0.030(7) 0.000(7) 0.003(7) -0.002(7) C13 0.017(6) 0.011(5) 0.011(6) 0.002(5) -0.001(5) -0.003(5) C14 0.011(5) 0.022(5) 0.005(5) -0.003(4) 0.004(4) -0.004(4) C15 0.014(6) 0.019(5) 0.010(5) -0.005(5) 0.006(5) -0.008(5) C16 0.011(6) 0.020(6) 0.029(7) 0.007(6) 0.007(6) 0.002(5) C17 0.015(6) 0.020(6) 0.012(5) 0.004(5) -0.001(5) -0.001(5) C18 0.012(6) 0.022(6) 0.008(5) 0.002(5) 0.000(5) 0.004(5) C19 0.011(6) 0.045(8) 0.004(5) -0.002(5) 0.000(5) 0.005(5) C20 0.013(5) 0.038(6) 0.009(5) 0.006(5) -0.004(4) 0.005(5) C21 0.017(4) 0.016(4) 0.008(4) -0.001(4) -0.004(4) 0.000(4) O1W 0.077(11) 0.098(12) 0.039(9) -0.001(9) 0.002(9) 0.002(10) O2W 0.014(4) 0.035(4) 0.005(3) -0.003(4) -0.001(4) -0.003(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 Cd1 O1 2.025(9) . ? Cd1 O2W 2.084(8) . ? Cd1 N2 2.098(10) . ? Cd1 O3 2.112(9) 3_556 ? Cd1 N1 2.173(10) . ? O1 C14 1.280(14) . ? O2 C14 1.254(16) . ? O3 C21 1.228(15) . ? O3 Cd1 2.112(9) 3_546 ? O4 C21 1.256(16) . ? N1 C12 1.296(18) . ? N1 C13 1.326(17) . ? N2 C1 1.359(16) . ? N2 C5 1.371(15) . ? N3 C7 1.284(18) . ? N3 C6 1.363(16) . ? N4 C8 1.339(19) . ? N4 C7 1.407(18) . ? N4 H4A 0.8600 . ? C1 C2 1.337(19) . ? C1 H1A 0.9300 . ? C2 C3 1.44(2) . ? C2 H2A 0.9300 . ? C3 C4 1.398(18) . ? C3 H3A 0.9300 . ? C4 C5 1.377(17) . ? C4 C6 1.407(18) . ? C5 C13 1.476(16) . ? C6 C8 1.465(17) . ? C7 H7A 0.9300 . ? C8 C9 1.379(19) . ? C9 C10 1.418(17) . ? C9 C13 1.426(16) . ? C10 C11 1.34(2) . ? C10 H10A 0.9300 . ? C11 C12 1.34(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 C15 1.469(15) . ? C15 C16 1.390(18) . ? C15 C20 1.413(17) . ? C16 C17 1.360(18) . ? C16 H16A 0.9300 . ? C17 C18 1.381(17) . ? C17 H17A 0.9300 . ? C18 C19 1.372(17) . ? C18 C21 1.527(16) . ? C19 C20 1.410(16) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? O1W O1W 1.65(7) 2_565 ? O1W H1C 0.8318 . ? O1W H1D 0.8560 . ? O2W H2C 0.7999 . ? O2W H2D 0.8000 . ? 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 Cd1 O2W 95.8(3) . . ? O1 Cd1 N2 152.5(4) . . ? O2W Cd1 N2 92.7(3) . . ? O1 Cd1 O3 98.0(4) . 3_556 ? O2W Cd1 O3 91.3(4) . 3_556 ? N2 Cd1 O3 107.9(4) . 3_556 ? O1 Cd1 N1 92.4(4) . . ? O2W Cd1 N1 170.4(4) . . ? N2 Cd1 N1 77.8(4) . . ? O3 Cd1 N1 92.5(4) 3_556 . ? C14 O1 Cd1 124.3(8) . . ? C21 O3 Cd1 127.5(8) . 3_546 ? C12 N1 C13 118.3(12) . . ? C12 N1 Cd1 128.3(10) . . ? C13 N1 Cd1 112.9(8) . . ? C1 N2 C5 116.5(10) . . ? C1 N2 Cd1 127.5(8) . . ? C5 N2 Cd1 116.0(8) . . ? C7 N3 C6 107.5(11) . . ? C8 N4 C7 106.9(10) . . ? C8 N4 H4A 126.6 . . ? C7 N4 H4A 126.6 . . ? C2 C1 N2 124.3(11) . . ? C2 C1 H1A 117.9 . . ? N2 C1 H1A 117.9 . . ? C1 C2 C3 118.7(13) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 118.9(12) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C5 C4 C3 117.4(11) . . ? C5 C4 C6 120.0(12) . . ? C3 C4 C6 122.4(12) . . ? N2 C5 C4 124.3(12) . . ? N2 C5 C13 114.5(10) . . ? C4 C5 C13 121.1(11) . . ? N3 C6 C4 133.5(12) . . ? N3 C6 C8 107.9(11) . . ? C4 C6 C8 118.6(12) . . ? N3 C7 N4 112.4(11) . . ? N3 C7 H7A 123.8 . . ? N4 C7 H7A 123.8 . . ? N4 C8 C9 131.9(11) . . ? N4 C8 C6 105.3(11) . . ? C9 C8 C6 122.8(12) . . ? C10 C9 C8 127.1(11) . . ? C10 C9 C13 114.9(11) . . ? C8 C9 C13 118.0(11) . . ? C11 C10 C9 120.6(12) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 118.5(13) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N1 C12 C11 125.6(14) . . ? N1 C12 H12A 117.2 . . ? C11 C12 H12A 117.2 . . ? N1 C13 C9 122.1(11) . . ? N1 C13 C5 118.5(11) . . ? C9 C13 C5 119.3(11) . . ? O2 C14 O1 124.6(11) . . ? O2 C14 C15 117.4(11) . . ? O1 C14 C15 117.9(11) . . ? C16 C15 C20 118.9(11) . . ? C16 C15 C14 121.6(11) . . ? C20 C15 C14 119.4(11) . . ? C17 C16 C15 120.8(12) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 120.9(11) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.4(11) . . ? C19 C18 C21 119.4(11) . . ? C17 C18 C21 120.2(11) . . ? C18 C19 C20 119.8(12) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C19 C20 C15 119.2(11) . . ? C19 C20 H20A 120.4 . . ? C15 C20 H20A 120.4 . . ? O3 C21 O4 123.7(11) . . ? O3 C21 C18 118.6(11) . . ? O4 C21 C18 117.7(10) . . ? O1W O1W H1C 105.8 2_565 . ? O1W O1W H1D 93.3 2_565 . ? H1C O1W H1D 100.5 . . ? Cd1 O2W H2C 108.7 . . ? Cd1 O2W H2D 114.3 . . ? H2C O2W H2D 91.9 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.558 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.260 # Attachment '14.cif' data_compound14 _database_code_depnum_ccdc_archive 'CCDC 710096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H14 Mn N4 O5, H2 O' _chemical_formula_sum 'C21 H16 Mn N4 O6' _chemical_formula_weight 475.32 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.048(3) _cell_length_b 24.077(5) _cell_length_c 16.737(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.561(3) _cell_angle_gamma 90.00 _cell_volume 5643(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5249 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8763 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 14600 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.1126 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5249 _reflns_number_gt 2122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.2106P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5249 _refine_ls_number_parameters 290 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2004 _refine_ls_R_factor_gt 0.1324 _refine_ls_wR_factor_ref 0.3987 _refine_ls_wR_factor_gt 0.3694 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.004 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 -0.14840(8) 0.16797(5) -0.03560(6) 0.0609(6) Uani 1 1 d . . . O1 O -0.0698(7) 0.2414(4) 0.0340(6) 0.154(3) Uani 1 1 d . . . O2 O -0.0342(8) 0.1556(4) 0.0828(5) 0.150(3) Uani 1 1 d . . . O3 O 0.2297(8) 0.3476(5) 0.3523(6) 0.159(4) Uani 1 1 d . . . O4 O 0.2868(7) 0.2645(4) 0.3812(5) 0.160(4) Uani 1 1 d . . . N1 N -0.0256(9) 0.1517(5) -0.1114(6) 0.130(4) Uani 1 1 d . . . N2 N -0.1341(9) 0.0725(5) -0.0507(7) 0.134(4) Uani 1 1 d . . . N3 N 0.1705(9) 0.0023(7) -0.2111(7) 0.151(4) Uani 1 1 d . . . N4 N 0.0811(14) -0.0665(5) -0.1629(8) 0.191(7) Uani 1 1 d . . . H4A H 0.0598 -0.0982 -0.1487 0.229 Uiso 1 1 calc R . . C1 C 0.0243(15) 0.1935(7) -0.1369(9) 0.164(6) Uani 1 1 d . . . H1 H 0.0082 0.2299 -0.1249 0.197 Uiso 1 1 calc R . . C2 C 0.1079(14) 0.1819(10) -0.1856(10) 0.187(8) Uani 1 1 d . . . H2 H 0.1438 0.2105 -0.2054 0.225 Uiso 1 1 calc R . . C3 C 0.1299(12) 0.1234(9) -0.2004(9) 0.153(6) Uani 1 1 d . . . H3 H 0.1791 0.1144 -0.2321 0.184 Uiso 1 1 calc R . . C4 C 0.0776(13) 0.0814(7) -0.1674(8) 0.136(5) Uani 1 1 d . . . C5 C -0.0034(10) 0.0983(6) -0.1213(7) 0.109(4) Uani 1 1 d . . . C6 C 0.0953(12) 0.0270(7) -0.1737(8) 0.118(4) Uani 1 1 d . . . C7 C 0.0379(12) -0.0125(8) -0.1471(8) 0.136(5) Uani 1 1 d . . . C8 C 0.1696(15) -0.0576(11) -0.2083(12) 0.197(9) Uani 1 1 d . . . H8 H 0.2110 -0.0833 -0.2285 0.237 Uiso 1 1 calc R . . C9 C -0.0451(11) -0.0015(7) -0.1018(8) 0.126(4) Uani 1 1 d . . . C10 C -0.1077(13) -0.0368(6) -0.0673(9) 0.137(5) Uani 1 1 d . . . H10 H -0.0958 -0.0746 -0.0720 0.164 Uiso 1 1 calc R . . C11 C -0.1832(12) -0.0229(9) -0.0282(9) 0.146(6) Uani 1 1 d . . . H11 H -0.2255 -0.0482 -0.0085 0.175 Uiso 1 1 calc R . . C12 C -0.1904(12) 0.0342(8) -0.0207(8) 0.151(6) Uani 1 1 d . . . H12 H -0.2396 0.0473 0.0083 0.181 Uiso 1 1 calc R . . C13 C -0.0598(11) 0.0571(6) -0.0917(7) 0.116(4) Uani 1 1 d . . . C14 C -0.0189(11) 0.2074(7) 0.0855(7) 0.130(5) Uani 1 1 d . . . C15 C 0.0501(9) 0.2312(5) 0.1457(7) 0.110(4) Uani 1 1 d . . . C16 C 0.0591(10) 0.2852(6) 0.1571(8) 0.138(5) Uani 1 1 d . . . H16 H 0.0268 0.3090 0.1206 0.165 Uiso 1 1 calc R . . C17 C 0.1140(10) 0.3077(6) 0.2202(8) 0.134(4) Uani 1 1 d . . . H17 H 0.1134 0.3458 0.2295 0.160 Uiso 1 1 calc R . . C18 C 0.1698(9) 0.2734(6) 0.2695(7) 0.116(4) Uani 1 1 d . . . C19 C 0.1610(10) 0.2183(7) 0.2565(8) 0.138(5) Uani 1 1 d . . . H19 H 0.1959 0.1943 0.2910 0.166 Uiso 1 1 calc R . . C20 C 0.1042(11) 0.1966(6) 0.1963(8) 0.146(5) Uani 1 1 d . . . H20 H 0.1014 0.1583 0.1888 0.176 Uiso 1 1 calc R . . C21 C 0.2292(10) 0.2987(7) 0.3384(7) 0.122(4) Uani 1 1 d . . . O1W O -0.2671(7) 0.1650(4) 0.0433(7) 0.205(6) Uani 1 1 d D . . O2W O 0.1634(8) 0.4577(5) 0.2840(8) 0.278(7) Uani 1 1 d D . . H2B H 0.1799 0.4280 0.3014 0.417 Uiso 1 1 d RD . . H2C H 0.2074 0.4698 0.2619 0.417 Uiso 1 1 d RD . . H1B H -0.3070 0.1910 0.0461 0.417 Uiso 1 1 d RD . . H1C H -0.3105 0.1481 0.0133 0.417 Uiso 1 1 d RD . . 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 0.0712(10) 0.0593(9) 0.0498(8) -0.0058(6) -0.0093(5) 0.0065(6) O1 0.168(8) 0.157(8) 0.131(7) 0.009(6) -0.020(6) -0.020(7) O2 0.182(9) 0.151(9) 0.113(7) -0.012(6) -0.009(6) -0.036(7) O3 0.208(10) 0.138(8) 0.124(7) -0.022(6) -0.028(6) -0.038(8) O4 0.163(8) 0.198(10) 0.112(6) 0.010(6) -0.035(6) -0.024(7) N1 0.163(10) 0.106(8) 0.120(8) 0.009(7) 0.007(7) -0.004(8) N2 0.137(10) 0.157(11) 0.105(7) -0.025(7) -0.013(7) -0.005(8) N3 0.153(11) 0.166(13) 0.134(9) 0.000(9) 0.005(8) 0.007(10) N4 0.29(2) 0.131(11) 0.134(10) -0.030(8) -0.073(12) 0.057(13) C1 0.25(2) 0.102(11) 0.144(13) 0.016(9) 0.039(13) -0.005(12) C2 0.168(16) 0.25(3) 0.152(15) 0.056(15) 0.038(13) 0.008(16) C3 0.179(15) 0.145(14) 0.136(12) 0.005(11) 0.013(10) 0.006(13) C4 0.186(16) 0.127(13) 0.091(8) 0.010(9) -0.014(9) -0.022(12) C5 0.122(10) 0.103(10) 0.099(8) 0.008(7) -0.004(7) -0.023(8) C6 0.152(13) 0.108(10) 0.095(8) 0.006(8) 0.015(8) 0.002(10) C7 0.146(13) 0.161(15) 0.099(9) 0.022(9) 0.004(9) 0.011(12) C8 0.175(17) 0.22(3) 0.200(19) 0.049(16) 0.043(14) -0.043(17) C9 0.139(12) 0.136(12) 0.096(8) 0.000(8) -0.033(8) -0.002(10) C10 0.161(13) 0.114(10) 0.128(11) 0.024(9) -0.027(10) -0.056(11) C11 0.135(12) 0.192(19) 0.110(10) 0.018(11) 0.006(9) -0.020(12) C12 0.185(15) 0.143(14) 0.121(11) 0.029(10) -0.010(9) -0.070(13) C13 0.155(13) 0.100(10) 0.090(8) -0.001(7) -0.014(8) 0.008(9) C14 0.188(14) 0.119(10) 0.081(8) 0.008(8) -0.001(8) -0.028(10) C15 0.146(10) 0.089(8) 0.089(7) 0.006(6) -0.022(7) -0.022(7) C16 0.168(13) 0.123(11) 0.118(10) -0.001(8) -0.019(9) -0.024(9) C17 0.156(12) 0.120(10) 0.118(10) 0.022(8) -0.030(9) -0.030(9) C18 0.125(10) 0.118(10) 0.102(8) 0.022(8) -0.008(7) -0.025(8) C19 0.150(11) 0.141(13) 0.120(10) 0.003(9) -0.022(8) -0.038(10) C20 0.184(14) 0.123(10) 0.123(10) 0.018(9) -0.044(10) -0.031(10) C21 0.140(11) 0.130(11) 0.092(8) 0.000(8) -0.020(8) -0.013(10) O1W 0.227(13) 0.204(13) 0.194(11) -0.040(8) 0.083(10) -0.040(8) O2W 0.228(14) 0.33(2) 0.282(17) 0.021(13) 0.050(13) -0.004(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 Mn1 O1W 2.209(11) . ? Mn1 N1 2.256(12) . ? Mn1 O4 2.283(9) 8_455 ? Mn1 N2 2.322(13) . ? Mn1 O1 2.345(9) . ? Mn1 O2 2.467(9) . ? Mn1 O3 2.466(10) 8_455 ? O1 C14 1.351(15) . ? O2 C14 1.264(15) . ? O3 C21 1.202(16) . ? O3 Mn1 2.466(10) 8_556 ? O4 C21 1.324(15) . ? O4 Mn1 2.283(9) 8_556 ? N1 C1 1.316(18) . ? N1 C5 1.336(15) . ? N2 C12 1.339(16) . ? N2 C13 1.347(15) . ? N3 C6 1.403(16) . ? N3 C8 1.44(2) . ? N4 C7 1.466(17) . ? N4 C8 1.52(2) . ? N4 H4A 0.8600 . ? C1 C2 1.51(2) . ? C1 H1 0.9300 . ? C2 C3 1.47(2) . ? C2 H2 0.9300 . ? C3 C4 1.390(19) . ? C3 H3 0.9300 . ? C4 C6 1.338(18) . ? C4 C5 1.482(18) . ? C5 C13 1.387(16) . ? C6 C7 1.346(17) . ? C7 C9 1.465(19) . ? C8 H8 0.9300 . ? C9 C10 1.382(17) . ? C9 C13 1.438(17) . ? C10 C11 1.332(19) . ? C10 H10 0.9300 . ? C11 C12 1.38(2) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C15 1.460(16) . ? C15 C16 1.317(15) . ? C15 C20 1.373(15) . ? C16 C17 1.369(16) . ? C16 H16 0.9300 . ? C17 C18 1.368(16) . ? C17 H17 0.9300 . ? C18 C19 1.348(18) . ? C18 C21 1.498(17) . ? C19 C20 1.341(15) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? O1W H1B 0.8445 . ? O1W H1C 0.8600 . ? O2W H2B 0.7998 . ? O2W H2C 0.8001 . ? 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 O1W Mn1 N1 168.0(4) . . ? O1W Mn1 O4 96.0(4) . 8_455 ? N1 Mn1 O4 93.8(4) . 8_455 ? O1W Mn1 N2 96.3(4) . . ? N1 Mn1 N2 72.0(5) . . ? O4 Mn1 N2 132.2(3) 8_455 . ? O1W Mn1 O1 94.3(3) . . ? N1 Mn1 O1 93.4(4) . . ? O4 Mn1 O1 85.1(4) 8_455 . ? N2 Mn1 O1 139.4(3) . . ? O1W Mn1 O2 89.4(4) . . ? N1 Mn1 O2 87.3(4) . . ? O4 Mn1 O2 141.1(4) 8_455 . ? N2 Mn1 O2 85.0(3) . . ? O1 Mn1 O2 56.0(3) . . ? O1W Mn1 O3 86.4(4) . 8_455 ? N1 Mn1 O3 93.5(4) . 8_455 ? O4 Mn1 O3 54.9(3) 8_455 8_455 ? N2 Mn1 O3 80.1(3) . 8_455 ? O1 Mn1 O3 139.8(4) . 8_455 ? O2 Mn1 O3 163.9(4) . 8_455 ? C14 O1 Mn1 93.7(8) . . ? C14 O2 Mn1 90.4(8) . . ? C21 O3 Mn1 89.5(9) . 8_556 ? C21 O4 Mn1 94.8(8) . 8_556 ? C1 N1 C5 124.1(14) . . ? C1 N1 Mn1 120.0(12) . . ? C5 N1 Mn1 115.6(10) . . ? C12 N2 C13 120.4(15) . . ? C12 N2 Mn1 125.7(13) . . ? C13 N2 Mn1 113.9(10) . . ? C6 N3 C8 113.6(15) . . ? C7 N4 C8 109.4(16) . . ? C7 N4 H4A 125.3 . . ? C8 N4 H4A 125.3 . . ? N1 C1 C2 119.4(16) . . ? N1 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C3 C2 C1 116.9(17) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.6 . . ? C4 C3 C2 120.4(17) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C6 C4 C3 125.0(19) . . ? C6 C4 C5 117.8(15) . . ? C3 C4 C5 117.3(15) . . ? N1 C5 C13 120.0(14) . . ? N1 C5 C4 121.7(12) . . ? C13 C5 C4 118.2(14) . . ? C4 C6 C7 123.1(17) . . ? C4 C6 N3 127.0(17) . . ? C7 C6 N3 109.9(14) . . ? C6 C7 C9 124.4(17) . . ? C6 C7 N4 107.4(15) . . ? C9 C7 N4 127.7(18) . . ? N3 C8 N4 99.5(18) . . ? N3 C8 H8 130.2 . . ? N4 C8 H8 130.2 . . ? C10 C9 C13 116.9(15) . . ? C10 C9 C7 131.6(17) . . ? C13 C9 C7 111.5(15) . . ? C11 C10 C9 127.5(16) . . ? C11 C10 H10 116.3 . . ? C9 C10 H10 116.3 . . ? C10 C11 C12 111.2(17) . . ? C10 C11 H11 124.4 . . ? C12 C11 H11 124.4 . . ? N2 C12 C11 126.9(19) . . ? N2 C12 H12 116.5 . . ? C11 C12 H12 116.5 . . ? N2 C13 C5 118.2(14) . . ? N2 C13 C9 117.1(14) . . ? C5 C13 C9 124.7(16) . . ? O2 C14 O1 119.7(12) . . ? O2 C14 C15 120.9(13) . . ? O1 C14 C15 119.4(12) . . ? C16 C15 C20 117.9(12) . . ? C16 C15 C14 122.6(13) . . ? C20 C15 C14 119.5(12) . . ? C15 C16 C17 122.9(14) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 119.1(14) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 117.1(13) . . ? C19 C18 C21 124.2(13) . . ? C17 C18 C21 118.5(13) . . ? C20 C19 C18 123.1(15) . . ? C20 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C19 C20 C15 119.6(14) . . ? C19 C20 H20 120.2 . . ? C15 C20 H20 120.2 . . ? O3 C21 O4 120.7(12) . . ? O3 C21 C18 122.8(13) . . ? O4 C21 C18 116.3(13) . . ? Mn1 O1W H1B 123.1 . . ? Mn1 O1W H1C 101.5 . . ? H1B O1W H1C 86.6 . . ? H2B O2W H2C 106.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.812 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.193 # Attachment '15.cif' data_compound15 _database_code_depnum_ccdc_archive 'CCDC 710097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29H16N4O8Zn2, 2.5(H2O)' _chemical_formula_sum 'C29 H21 N4 O10.50 Zn2' _chemical_formula_weight 724.24 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' Zn Zn 0.2839 1.4301 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.079(2) _cell_length_b 12.415(3) _cell_length_c 13.982(3) _cell_angle_alpha 102.897(5) _cell_angle_beta 99.497(4) _cell_angle_gamma 105.805(4) _cell_volume 1434.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5060 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 1.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6232 _exptl_absorpt_correction_T_max 0.7563 _exptl_absorpt_process_details SADABS _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 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7322 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.1557 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5060 _reflns_number_gt 2325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0600P)^2^+0.0059P] 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 5060 _refine_ls_number_parameters 416 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.893 _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 C28 C 1.6188(7) 0.9553(7) 1.0271(5) 0.0421(19) Uani 1 1 d . . . H28 H 1.6989 0.9251 1.0452 0.050 Uiso 1 1 calc R . . O3W O 0.8944(18) 0.6202(11) 0.3209(9) 0.152(6) Uani 0.50 1 d PD . . H5W H 0.8858 0.6521 0.3709 0.227 Uiso 0.50 1 d PRD . . H6W H 0.9717 0.6450 0.2931 0.227 Uiso 0.50 1 d PRD . . O2 O 0.9282(5) 1.1007(4) 0.5421(3) 0.0442(12) Uani 1 1 d . . . C29 C 1.4680(7) 0.8801(6) 0.9800(5) 0.0412(18) Uani 1 1 d . . . H29 H 1.4472 0.7999 0.9668 0.049 Uiso 1 1 calc R . . C25 C 0.3478(8) 0.4569(7) 0.9420(5) 0.060(2) Uani 1 1 d . . . H25 H 0.2453 0.4278 0.9020 0.072 Uiso 1 1 calc R . . C21 C 0.4128(7) 0.4884(6) 0.4041(5) 0.0457(19) Uani 1 1 d . . . H21 H 0.3557 0.4806 0.3399 0.055 Uiso 1 1 calc R . . C17 C 0.3867(7) 0.8917(6) 0.4751(4) 0.0375(17) Uani 1 1 d . . . H17 H 0.3108 0.8186 0.4580 0.045 Uiso 1 1 calc R . . C24 C 0.4626(9) 0.5392(7) 0.9171(5) 0.059(2) Uani 1 1 d . . . H24 H 0.4359 0.5654 0.8614 0.070 Uiso 1 1 calc R . . C16 C 0.5455(7) 0.9039(7) 0.5090(5) 0.0437(19) Uani 1 1 d . . . H16 H 0.5752 0.8393 0.5153 0.052 Uiso 1 1 calc R . . N1 N 0.2062(6) 0.8098(5) 0.6496(4) 0.0406(14) Uani 1 1 d . . . N2 N 0.2342(6) 1.0343(6) 0.6857(4) 0.0423(15) Uani 1 1 d . . . C13 C 0.3674(7) 1.0083(7) 0.7175(4) 0.0411(19) Uani 1 1 d . . . C5 C 0.3500(7) 0.8839(6) 0.6989(4) 0.0351(17) Uani 1 1 d . . . C1 C 0.1860(8) 0.6972(7) 0.6327(5) 0.052(2) Uani 1 1 d . . . H1 H 0.0866 0.6449 0.5984 0.062 Uiso 1 1 calc R . . C2 C 0.3040(8) 0.6522(7) 0.6628(5) 0.055(2) Uani 1 1 d . . . H2 H 0.2835 0.5720 0.6500 0.066 Uiso 1 1 calc R . . Zn1 Zn 1.04044(8) 0.88710(7) 0.59580(6) 0.0377(3) Uani 1 1 d . . . Zn2 Zn 0.86185(8) 0.79632(8) 0.82479(6) 0.0449(3) Uani 1 1 d . . . O7 O 1.0792(5) 0.8906(5) 0.8815(3) 0.0622(15) Uani 1 1 d . . . C6 C 0.6256(7) 0.9375(7) 0.7794(4) 0.0346(17) Uani 1 1 d . . . O1 O 0.8630(5) 0.9557(4) 0.6127(3) 0.0496(13) Uani 1 1 d . . . N3 N 0.7732(6) 0.9274(5) 0.8192(4) 0.0361(14) Uani 1 1 d . . . O3 O 0.8644(5) 0.7305(4) 0.5271(3) 0.0549(14) Uani 1 1 d . . . N4 N 0.7980(6) 1.1167(6) 0.8429(4) 0.0483(16) Uani 1 1 d . . . H4 H 0.8423 1.1912 0.8609 0.058 Uiso 1 1 calc R . . O4 O 0.8488(5) 0.7223(4) 0.6818(3) 0.0546(14) Uani 1 1 d . . . C18 C 0.7960(7) 0.6884(6) 0.5871(6) 0.0426(18) Uani 1 1 d . . . O5 O 0.7166(5) 0.6734(5) 0.8579(4) 0.0655(16) Uani 1 1 d . . . O8 O 1.1568(6) 0.7365(6) 0.8822(4) 0.0739(17) Uani 1 1 d . . . C7 C 0.6393(7) 1.0544(7) 0.7944(5) 0.0381(17) Uani 1 1 d . . . C8 C 0.8653(8) 1.0368(7) 0.8552(5) 0.0470(19) Uani 1 1 d . . . H8 H 0.9712 1.0568 0.8872 0.056 Uiso 1 1 calc R . . C3 C 0.4501(8) 0.7276(7) 0.7116(5) 0.052(2) Uani 1 1 d . . . H3 H 0.5313 0.6993 0.7322 0.062 Uiso 1 1 calc R . . C27 C 1.3477(7) 0.9246(7) 0.9522(4) 0.0381(18) Uani 1 1 d . . . C9 C 0.5108(8) 1.0944(7) 0.7655(5) 0.0384(17) Uani 1 1 d . . . C4 C 0.4786(7) 0.8483(7) 0.7309(5) 0.0387(18) Uani 1 1 d . . . C20 C 0.5540(7) 0.5779(6) 0.4469(5) 0.0454(19) Uani 1 1 d . . . H20 H 0.5903 0.6309 0.4117 0.054 Uiso 1 1 calc R . . C26 C 1.1819(8) 0.8426(8) 0.9017(5) 0.049(2) Uani 1 1 d . . . C19 C 0.6436(7) 0.5898(6) 0.5432(5) 0.0383(17) Uani 1 1 d . . . C12 C 0.2464(8) 1.1463(8) 0.7036(5) 0.056(2) Uani 1 1 d . . . H12 H 0.1562 1.1653 0.6831 0.067 Uiso 1 1 calc R . . C14 C 0.8292(7) 1.0238(7) 0.5652(5) 0.043(2) Uani 1 1 d . . . C23 C 0.6159(8) 0.5816(6) 0.9750(5) 0.0449(19) Uani 1 1 d . . . C11 C 0.3849(9) 1.2357(7) 0.7506(5) 0.059(2) Uani 1 1 d . . . H11 H 0.3869 1.3128 0.7606 0.070 Uiso 1 1 calc R . . O6 O 0.8531(7) 0.7371(6) 1.0150(5) 0.116(3) Uani 1 1 d . . . C22 C 0.7382(9) 0.6721(8) 0.9480(7) 0.057(2) Uani 1 1 d . . . C10 C 0.5192(9) 1.2116(7) 0.7825(5) 0.056(2) Uani 1 1 d . . . H10 H 0.6137 1.2713 0.8147 0.068 Uiso 1 1 calc R . . C15 C 0.6582(7) 1.0126(6) 0.5333(5) 0.0352(17) Uani 1 1 d . . . O1W O 0.8936(8) 0.3629(7) 0.9284(7) 0.192(4) Uani 1 1 d . . . H1W H 0.9645 0.3324 0.9412 0.289 Uiso 1 1 d RD . . H2W H 0.8382 0.4023 0.9557 0.289 Uiso 1 1 d RD . . O2W O 0.9510(11) 0.4985(9) 0.7851(9) 0.254(6) Uani 1 1 d . . . H3W H 1.0113 0.5669 0.8100 0.382 Uiso 1 1 d RD . . H4W H 0.9328 0.4567 0.8238 0.382 Uiso 1 1 d RD . . 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 C28 0.022(4) 0.058(6) 0.043(4) 0.014(4) 0.001(3) 0.012(4) O3W 0.217(17) 0.062(10) 0.119(11) -0.003(9) 0.067(12) -0.039(11) O2 0.020(2) 0.051(4) 0.054(3) 0.021(3) 0.004(2) -0.003(2) C29 0.033(4) 0.032(5) 0.052(4) 0.007(4) 0.008(3) 0.006(4) C25 0.034(4) 0.074(7) 0.058(5) 0.024(5) 0.001(4) -0.004(4) C21 0.032(4) 0.045(5) 0.052(4) 0.015(4) 0.003(4) 0.002(4) C17 0.019(3) 0.036(5) 0.052(4) 0.014(4) 0.006(3) 0.001(3) C24 0.053(5) 0.063(6) 0.063(5) 0.041(5) 0.013(4) 0.005(5) C16 0.032(4) 0.059(6) 0.054(5) 0.030(5) 0.016(4) 0.021(4) N1 0.025(3) 0.038(4) 0.052(4) 0.012(3) 0.002(3) 0.004(3) N2 0.030(3) 0.048(5) 0.047(4) 0.013(3) 0.001(3) 0.015(3) C13 0.029(4) 0.061(6) 0.031(4) 0.016(4) 0.005(3) 0.010(4) C5 0.023(4) 0.041(5) 0.034(4) 0.012(4) 0.002(3) 0.001(4) C1 0.029(4) 0.041(6) 0.074(5) 0.014(5) 0.001(4) 0.001(4) C2 0.034(4) 0.036(5) 0.082(6) 0.009(5) -0.001(4) 0.005(4) Zn1 0.0157(4) 0.0433(6) 0.0511(5) 0.0221(5) 0.0020(4) 0.0008(4) Zn2 0.0226(4) 0.0533(7) 0.0536(5) 0.0224(5) 0.0033(4) 0.0014(4) O7 0.020(3) 0.078(4) 0.078(4) 0.029(3) -0.004(2) 0.002(3) C6 0.022(4) 0.045(5) 0.036(4) 0.017(4) 0.005(3) 0.006(4) O1 0.029(3) 0.064(4) 0.067(3) 0.039(3) 0.012(2) 0.014(3) N3 0.025(3) 0.037(4) 0.040(3) 0.012(3) 0.004(3) 0.001(3) O3 0.028(3) 0.057(4) 0.068(3) 0.024(3) 0.008(3) -0.009(3) N4 0.032(3) 0.051(5) 0.052(4) 0.018(4) -0.003(3) 0.002(3) O4 0.035(3) 0.058(4) 0.049(3) 0.003(3) -0.005(2) 0.000(3) C18 0.020(4) 0.034(5) 0.068(5) 0.018(5) 0.002(4) 0.001(3) O5 0.043(3) 0.079(5) 0.073(4) 0.048(4) 0.014(3) -0.004(3) O8 0.043(3) 0.057(5) 0.095(4) 0.009(4) -0.009(3) 0.001(3) C7 0.022(4) 0.043(5) 0.043(4) 0.016(4) 0.005(3) 0.000(4) C8 0.028(4) 0.054(6) 0.045(4) 0.014(4) -0.005(3) -0.001(4) C3 0.032(4) 0.056(6) 0.064(5) 0.027(5) -0.002(4) 0.008(4) C27 0.024(4) 0.050(6) 0.033(4) 0.003(4) 0.004(3) 0.010(4) C9 0.032(4) 0.036(5) 0.041(4) 0.017(4) 0.002(3) 0.001(4) C4 0.023(4) 0.049(6) 0.042(4) 0.021(4) 0.008(3) 0.002(4) C20 0.032(4) 0.046(5) 0.048(4) 0.021(4) 0.005(3) -0.008(4) C26 0.032(4) 0.066(7) 0.043(5) 0.013(5) 0.007(4) 0.007(5) C19 0.023(3) 0.039(5) 0.047(4) 0.014(4) 0.004(3) 0.001(3) C12 0.035(5) 0.059(7) 0.064(5) 0.012(5) -0.004(4) 0.014(5) C14 0.017(4) 0.065(6) 0.041(4) 0.019(4) 0.003(3) 0.004(4) C23 0.036(4) 0.038(5) 0.054(5) 0.016(4) 0.011(4) -0.001(4) C11 0.050(5) 0.053(6) 0.065(5) 0.019(5) 0.000(4) 0.011(5) O6 0.075(5) 0.121(6) 0.093(5) 0.034(5) 0.007(4) -0.057(4) C22 0.036(5) 0.060(7) 0.075(6) 0.034(6) 0.015(5) 0.004(5) C10 0.045(5) 0.058(7) 0.049(5) 0.016(5) -0.005(4) -0.002(5) C15 0.023(4) 0.044(5) 0.042(4) 0.020(4) 0.014(3) 0.007(4) O1W 0.094(6) 0.124(8) 0.314(12) 0.073(8) -0.040(7) 0.006(6) O2W 0.136(8) 0.198(12) 0.399(16) 0.125(12) 0.007(9) 0.007(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 C28 C29 1.382(9) . ? C28 C27 1.390(9) 2_877 ? C28 H28 0.9300 . ? O3W H5W 0.7499 . ? O3W H6W 0.8738 . ? O2 C14 1.261(8) . ? O2 Zn1 2.028(4) 2_776 ? C29 C27 1.391(8) . ? C29 H29 0.9300 . ? C25 C23 1.375(8) 2_667 ? C25 C24 1.397(9) . ? C25 H25 0.9300 . ? C21 C20 1.382(9) . ? C21 C19 1.386(8) 2_666 ? C21 H21 0.9300 . ? C17 C15 1.379(8) 2_676 ? C17 C16 1.396(7) . ? C17 H17 0.9300 . ? C24 C23 1.381(9) . ? C24 H24 0.9300 . ? C16 C15 1.383(9) . ? C16 H16 0.9300 . ? N1 C1 1.320(8) . ? N1 C5 1.339(8) . ? N1 Zn1 2.119(5) 1_455 ? N2 C12 1.327(9) . ? N2 C13 1.365(7) . ? N2 Zn1 2.123(6) 1_455 ? C13 C9 1.386(9) . ? C13 C5 1.467(9) . ? C5 C4 1.398(8) . ? C1 C2 1.386(8) . ? C1 H1 0.9300 . ? C2 C3 1.357(9) . ? C2 H2 0.9300 . ? Zn1 O2 2.028(4) 2_776 ? Zn1 O1 2.040(4) . ? Zn1 O3 2.055(5) . ? Zn1 N1 2.119(5) 1_655 ? Zn1 N2 2.123(6) 1_655 ? Zn2 O5 1.924(5) . ? Zn2 O7 1.925(5) . ? Zn2 O4 1.974(5) . ? Zn2 N3 2.013(5) . ? O7 C26 1.264(8) . ? C6 C7 1.387(9) . ? C6 N3 1.413(7) . ? C6 C4 1.424(9) . ? O1 C14 1.256(7) . ? N3 C8 1.317(8) . ? O3 C18 1.247(7) . ? N4 C8 1.326(8) . ? N4 C7 1.404(8) . ? N4 H4 0.8600 . ? O4 C18 1.261(7) . ? C18 C19 1.501(9) . ? O5 C22 1.247(8) . ? O8 C26 1.231(9) . ? C7 C9 1.421(8) . ? C8 H8 0.9300 . ? C3 C4 1.404(9) . ? C3 H3 0.9300 . ? C27 C28 1.390(9) 2_877 ? C27 C26 1.514(9) . ? C9 C10 1.400(9) . ? C20 C19 1.407(8) . ? C20 H20 0.9300 . ? C19 C21 1.386(8) 2_666 ? C12 C11 1.374(10) . ? C12 H12 0.9300 . ? C14 C15 1.502(8) . ? C23 C25 1.375(8) 2_667 ? C23 C22 1.511(9) . ? C11 C10 1.362(9) . ? C11 H11 0.9300 . ? O6 C22 1.224(9) . ? C10 H10 0.9300 . ? C15 C17 1.379(8) 2_676 ? O1W H1W 0.8449 . ? O1W H2W 0.8668 . ? O2W H3W 0.8331 . ? O2W H4W 0.8351 . ? 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 C29 C28 C27 121.0(6) . 2_877 ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 2_877 . ? H5W O3W H6W 124.7 . . ? C14 O2 Zn1 129.7(4) . 2_776 ? C28 C29 C27 119.9(6) . . ? C28 C29 H29 120.1 . . ? C27 C29 H29 120.1 . . ? C23 C25 C24 120.9(7) 2_667 . ? C23 C25 H25 119.5 2_667 . ? C24 C25 H25 119.5 . . ? C20 C21 C19 120.0(6) . 2_666 ? C20 C21 H21 120.0 . . ? C19 C21 H21 120.0 2_666 . ? C15 C17 C16 120.4(6) 2_676 . ? C15 C17 H17 119.8 2_676 . ? C16 C17 H17 119.8 . . ? C23 C24 C25 120.1(6) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C1 N1 C5 117.3(6) . . ? C1 N1 Zn1 126.9(5) . 1_455 ? C5 N1 Zn1 115.5(5) . 1_455 ? C12 N2 C13 117.3(7) . . ? C12 N2 Zn1 128.1(5) . 1_455 ? C13 N2 Zn1 114.0(5) . 1_455 ? N2 C13 C9 122.1(7) . . ? N2 C13 C5 116.2(6) . . ? C9 C13 C5 121.8(6) . . ? N1 C5 C4 123.6(7) . . ? N1 C5 C13 115.8(6) . . ? C4 C5 C13 120.6(6) . . ? N1 C1 C2 124.0(7) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.5(7) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? O2 Zn1 O1 103.30(17) 2_776 . ? O2 Zn1 O3 89.28(19) 2_776 . ? O1 Zn1 O3 85.88(19) . . ? O2 Zn1 N1 105.54(18) 2_776 1_655 ? O1 Zn1 N1 151.16(19) . 1_655 ? O3 Zn1 N1 94.3(2) . 1_655 ? O2 Zn1 N2 98.24(19) 2_776 1_655 ? O1 Zn1 N2 98.7(2) . 1_655 ? O3 Zn1 N2 170.0(2) . 1_655 ? N1 Zn1 N2 77.4(2) 1_655 1_655 ? O5 Zn2 O7 134.8(2) . . ? O5 Zn2 O4 101.5(2) . . ? O7 Zn2 O4 105.44(19) . . ? O5 Zn2 N3 110.5(2) . . ? O7 Zn2 N3 97.4(2) . . ? O4 Zn2 N3 103.84(19) . . ? C26 O7 Zn2 119.7(5) . . ? C7 C6 N3 109.6(6) . . ? C7 C6 C4 121.0(6) . . ? N3 C6 C4 129.4(7) . . ? C14 O1 Zn1 123.6(4) . . ? C8 N3 C6 103.0(5) . . ? C8 N3 Zn2 120.5(5) . . ? C6 N3 Zn2 136.4(5) . . ? C18 O3 Zn1 113.5(5) . . ? C8 N4 C7 105.6(6) . . ? C8 N4 H4 127.2 . . ? C7 N4 H4 127.2 . . ? C18 O4 Zn2 158.2(4) . . ? O3 C18 O4 124.0(7) . . ? O3 C18 C19 117.6(7) . . ? O4 C18 C19 118.5(6) . . ? C22 O5 Zn2 117.7(5) . . ? C6 C7 N4 105.8(6) . . ? C6 C7 C9 123.6(6) . . ? N4 C7 C9 130.6(7) . . ? N3 C8 N4 116.0(6) . . ? N3 C8 H8 122.0 . . ? N4 C8 H8 122.0 . . ? C2 C3 C4 119.9(7) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C28 C27 C29 119.2(6) 2_877 . ? C28 C27 C26 120.8(6) 2_877 . ? C29 C27 C26 120.1(7) . . ? C13 C9 C10 119.0(7) . . ? C13 C9 C7 115.8(7) . . ? C10 C9 C7 125.1(7) . . ? C5 C4 C3 116.6(7) . . ? C5 C4 C6 117.1(7) . . ? C3 C4 C6 126.2(6) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? O8 C26 O7 125.0(8) . . ? O8 C26 C27 119.2(7) . . ? O7 C26 C27 115.8(8) . . ? C21 C19 C20 119.2(6) 2_666 . ? C21 C19 C18 121.7(6) 2_666 . ? C20 C19 C18 119.1(6) . . ? N2 C12 C11 123.6(7) . . ? N2 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? O1 C14 O2 124.8(6) . . ? O1 C14 C15 117.6(6) . . ? O2 C14 C15 117.6(6) . . ? C25 C23 C24 119.0(6) 2_667 . ? C25 C23 C22 121.5(7) 2_667 . ? C24 C23 C22 119.5(7) . . ? C10 C11 C12 120.0(8) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? O6 C22 O5 124.4(7) . . ? O6 C22 C23 118.2(7) . . ? O5 C22 C23 117.4(8) . . ? C11 C10 C9 118.0(7) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C17 C15 C16 120.0(6) 2_676 . ? C17 C15 C14 120.8(6) 2_676 . ? C16 C15 C14 119.1(6) . . ? H1W O1W H2W 143.8 . . ? H3W O2W H4W 118.3 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.694 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.113