# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email hongjie@ciac.jl.cn _publ_contact_author_name 'Hongjie Zhang' loop_ _publ_author_name 'Shengqun Su' 'Chao Qin' 'Shuyan Song' 'Zhiyong Guo' 'Ruiping Deng' 'Wan Chen' 'Xuezhi Song' 'Song Wang' 'Guanghua Li' 'Hongjie Zhang' data_m _database_code_depnum_ccdc_archive 'CCDC 810535' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C22 H30 Co2 N2 O13' _chemical_formula_sum 'C22 H30 Co2 N2 O13' _chemical_formula_weight 648.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.0660(5) _cell_length_b 13.8214(6) _cell_length_c 16.8387(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.3100(10) _cell_angle_gamma 90.00 _cell_volume 2506.26(19) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 4940 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 26.07 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.397 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7215 _exptl_absorpt_correction_T_max 0.7871 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13636 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.07 _reflns_number_total 4940 _reflns_number_gt 3976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The C22 were refined with isotropic temperature parameters ; _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^)+(0.0472P)^2^+3.2794P] 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 4940 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.05672(4) 0.08925(3) 0.17407(2) 0.01067(11) Uani 1 1 d . . . Co2 Co 0.14177(4) -0.00273(3) -0.00506(2) 0.01151(12) Uani 1 1 d . . . C1 C -0.3264(3) 0.0580(2) 0.20162(18) 0.0130(6) Uani 1 1 d . . . C2 C -0.4487(3) 0.0502(2) 0.15661(17) 0.0125(6) Uani 1 1 d . . . H2 H -0.4652 0.0384 0.0995 0.050 Uiso 1 1 calc R . . C3 C -0.5461(3) 0.0596(2) 0.19516(17) 0.0129(6) Uani 1 1 d . . . C4 C -0.5218(3) 0.0744(2) 0.27912(17) 0.0130(6) Uani 1 1 d . . . H4 H -0.5889 0.0812 0.3052 0.050 Uiso 1 1 calc R . . C5 C -0.3998(3) 0.0791(2) 0.32538(17) 0.0121(6) Uani 1 1 d . . . C6 C -0.3033(3) 0.0718(2) 0.28600(18) 0.0132(6) Uani 1 1 d . . . H6 H -0.2200 0.0763 0.3168 0.050 Uiso 1 1 calc R . . C7 C -0.3761(3) 0.0907(2) 0.41671(18) 0.0152(6) Uani 1 1 d . . . C8 C -0.3464(3) -0.0028(2) 0.46507(17) 0.0140(6) Uani 1 1 d . . . C9 C -0.3965(3) -0.0917(2) 0.43588(17) 0.0141(6) Uani 1 1 d . . . H9 H -0.4513 -0.0954 0.3835 0.050 Uiso 1 1 calc R . . C10 C -0.3675(3) -0.1759(2) 0.48260(17) 0.0130(6) Uani 1 1 d . . . C11 C -0.2900(3) -0.1695(2) 0.56021(17) 0.0143(6) Uani 1 1 d . . . H11 H -0.2703 -0.2262 0.5926 0.050 Uiso 1 1 calc R . . C12 C -0.2412(3) -0.0809(2) 0.59054(17) 0.0138(6) Uani 1 1 d . . . C13 C -0.2687(3) 0.0017(2) 0.54308(18) 0.0156(6) Uani 1 1 d . . . H13 H -0.2344 0.0621 0.5639 0.050 Uiso 1 1 calc R . . C14 C -0.2207(3) 0.0468(2) 0.15981(17) 0.0133(6) Uani 1 1 d . . . C15 C -0.6788(3) 0.0527(2) 0.14716(17) 0.0130(6) Uani 1 1 d . . . C16 C -0.4161(3) -0.2747(2) 0.45330(17) 0.0137(6) Uani 1 1 d . . . C17 C -0.1613(3) -0.0751(2) 0.67564(17) 0.0140(6) Uani 1 1 d . . . C18 C -0.0861(4) 0.3117(3) 0.2916(3) 0.0363(9) Uani 1 1 d . . . H18A H -0.0728 0.3173 0.2362 0.050 Uiso 1 1 calc R . . H18B H -0.1402 0.3643 0.3015 0.050 Uiso 1 1 calc R . . H18C H -0.1252 0.2493 0.2975 0.050 Uiso 1 1 calc R . . C19 C 0.0242(4) 0.3103(3) 0.4366(2) 0.0422(10) Uani 1 1 d . . . H19A H 0.1069 0.3152 0.4730 0.050 Uiso 1 1 calc R . . H19B H -0.0130 0.2479 0.4450 0.050 Uiso 1 1 calc R . . H19C H -0.0285 0.3628 0.4486 0.050 Uiso 1 1 calc R . . C20 C 0.4080(4) 0.2767(3) 0.1304(3) 0.0338(9) Uani 1 1 d . . . C21 C 0.5461(4) 0.3249(3) 0.2594(3) 0.0494(12) Uani 1 1 d . . . H21A H 0.6283 0.3545 0.2770 0.050 Uiso 1 1 calc R . . H21B H 0.5465 0.2609 0.2845 0.050 Uiso 1 1 calc R . . H21C H 0.4841 0.3660 0.2761 0.050 Uiso 1 1 calc R . . C22 C 0.6070(6) 0.3429(5) 0.1288(4) 0.090(2) Uiso 1 1 d . . . H22A H 0.6790 0.3695 0.1678 0.050 Uiso 1 1 calc R . . H22B H 0.5727 0.3921 0.0880 0.050 Uiso 1 1 calc R . . H22C H 0.6327 0.2864 0.1017 0.050 Uiso 1 1 calc R . . N1 N 0.0347(3) 0.3179(2) 0.35140(17) 0.0244(6) Uani 1 1 d . . . H1A H 0.0855 0.2691 0.3410 0.050 Uiso 1 1 calc R . . H1B H 0.0718 0.3759 0.3445 0.050 Uiso 1 1 calc R . . N2 N 0.5151(3) 0.3149(3) 0.1709(2) 0.0476(10) Uani 1 1 d . . . O1 O -0.11675(19) 0.07870(16) 0.19762(12) 0.0176(5) Uani 1 1 d . . . O2 O -0.2449(2) 0.00517(16) 0.09159(13) 0.0195(5) Uani 1 1 d . . . O3 O -0.69945(19) -0.00572(15) 0.08752(12) 0.0160(5) Uani 1 1 d . . . O4 O -0.75649(19) 0.10505(15) 0.17039(12) 0.0154(4) Uani 1 1 d . . . O5 O -0.50855(19) -0.28061(15) 0.39259(12) 0.0158(5) Uani 1 1 d . . . O6 O -0.3616(2) -0.34440(15) 0.49286(12) 0.0193(5) Uani 1 1 d . . . O7 O -0.11548(19) -0.15402(14) 0.70965(12) 0.0144(4) Uani 1 1 d . . . O8 O -0.1438(2) 0.00384(15) 0.71296(12) 0.0162(5) Uani 1 1 d . . . O9 O 0.03072(19) -0.00722(17) 0.08246(12) 0.0123(4) Uani 1 1 d . . . O10 O 0.1540(2) 0.15584(17) -0.00773(14) 0.0193(5) Uani 1 1 d . . . O11 O 0.3733(3) 0.2645(2) 0.05654(19) 0.0427(7) Uani 1 1 d . . . O1W O 0.3265(3) -0.1398(2) 0.26734(18) 0.0445(7) Uani 1 1 d . . . H7A H -0.443(3) 0.123(3) 0.435(2) 0.022(9) Uiso 1 1 d . . . H7B H -0.308(3) 0.135(2) 0.4365(18) 0.011(8) Uiso 1 1 d . . . H10A H 0.225(4) 0.183(3) 0.005(2) 0.037(12) Uiso 1 1 d . . . H10B H 0.120(4) 0.176(3) 0.024(3) 0.034(13) Uiso 1 1 d . . . H20 H 0.354(4) 0.256(3) 0.169(3) 0.046(12) Uiso 1 1 d . . . H9OH H 0.038(3) -0.059(3) 0.098(2) 0.015(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0102(2) 0.0131(2) 0.00790(19) -0.00116(16) 0.00041(15) -0.00009(15) Co2 0.0099(2) 0.0149(2) 0.0089(2) -0.00218(15) 0.00049(15) 0.00001(15) C1 0.0159(15) 0.0086(14) 0.0144(14) 0.0007(11) 0.0032(12) -0.0001(11) C2 0.0147(15) 0.0130(15) 0.0093(13) -0.0008(11) 0.0014(12) -0.0006(11) C3 0.0137(15) 0.0112(15) 0.0131(14) -0.0002(11) 0.0017(12) -0.0003(11) C4 0.0132(15) 0.0138(15) 0.0128(14) 0.0009(12) 0.0046(12) -0.0004(11) C5 0.0167(15) 0.0087(14) 0.0098(13) 0.0016(11) 0.0007(11) 0.0005(11) C6 0.0119(14) 0.0121(15) 0.0136(14) -0.0005(12) -0.0014(11) -0.0008(11) C7 0.0187(16) 0.0154(16) 0.0108(14) -0.0013(12) 0.0022(12) 0.0000(13) C8 0.0151(15) 0.0177(16) 0.0097(13) 0.0000(12) 0.0035(11) 0.0020(12) C9 0.0120(14) 0.0186(16) 0.0110(14) 0.0010(12) 0.0012(11) 0.0031(12) C10 0.0131(15) 0.0151(15) 0.0108(13) -0.0005(12) 0.0025(11) -0.0008(11) C11 0.0152(15) 0.0153(16) 0.0113(14) 0.0010(12) 0.0012(12) 0.0009(12) C12 0.0145(15) 0.0160(16) 0.0103(14) -0.0001(12) 0.0018(11) 0.0006(12) C13 0.0155(16) 0.0167(16) 0.0137(14) -0.0036(12) 0.0018(12) 0.0001(12) C14 0.0140(15) 0.0129(15) 0.0125(14) 0.0026(12) 0.0018(12) 0.0011(11) C15 0.0125(15) 0.0143(15) 0.0118(14) 0.0032(12) 0.0023(12) -0.0017(11) C16 0.0148(15) 0.0163(16) 0.0110(14) -0.0027(12) 0.0047(12) -0.0029(12) C17 0.0128(15) 0.0190(17) 0.0094(14) 0.0003(12) 0.0010(11) -0.0005(12) C18 0.032(2) 0.027(2) 0.047(2) 0.0017(18) 0.0036(18) 0.0063(16) C19 0.048(3) 0.048(3) 0.036(2) -0.005(2) 0.0221(19) -0.004(2) C20 0.027(2) 0.0163(19) 0.057(3) -0.0094(18) 0.0090(19) 0.0022(15) C21 0.046(3) 0.027(2) 0.065(3) -0.012(2) -0.007(2) 0.0073(19) N1 0.0277(16) 0.0174(15) 0.0312(16) 0.0020(12) 0.0133(13) 0.0006(12) N2 0.035(2) 0.038(2) 0.073(3) -0.0224(19) 0.0188(18) -0.0118(16) O1 0.0106(11) 0.0263(13) 0.0157(11) -0.0038(9) 0.0025(9) -0.0025(9) O2 0.0141(11) 0.0306(13) 0.0148(11) -0.0077(10) 0.0053(9) -0.0026(9) O3 0.0119(11) 0.0212(12) 0.0135(10) -0.0063(9) 0.0002(8) 0.0002(8) O4 0.0126(11) 0.0189(11) 0.0145(10) -0.0026(9) 0.0026(8) 0.0003(8) O5 0.0165(11) 0.0148(11) 0.0136(10) -0.0017(8) -0.0015(8) -0.0020(8) O6 0.0224(12) 0.0144(11) 0.0176(11) 0.0020(9) -0.0026(9) -0.0022(9) O7 0.0163(11) 0.0143(11) 0.0108(10) -0.0005(8) -0.0005(8) 0.0015(8) O8 0.0208(12) 0.0136(11) 0.0117(10) -0.0035(8) -0.0012(9) -0.0010(8) O9 0.0139(11) 0.0123(12) 0.0099(10) 0.0000(9) 0.0012(8) -0.0001(8) O10 0.0225(13) 0.0181(12) 0.0186(12) -0.0014(10) 0.0071(11) -0.0012(10) O11 0.0423(18) 0.0334(16) 0.0569(19) -0.0113(14) 0.0205(15) -0.0115(13) O1W 0.0551(19) 0.0346(16) 0.0533(18) 0.0082(14) 0.0320(15) 0.0127(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O9 2.009(2) . ? Co1 O1 2.053(2) . ? Co1 O4 2.094(2) 1_655 ? Co1 O7 2.1147(19) 3_556 ? Co1 O5 2.122(2) 2_455 ? Co1 O8 2.315(2) 3_556 ? Co2 O2 2.048(2) 3 ? Co2 O9 2.053(2) 3 ? Co2 O3 2.064(2) 1_655 ? Co2 O6 2.113(2) 4_655 ? Co2 O9 2.126(2) . ? Co2 O10 2.197(2) . ? C1 C2 1.395(4) . ? C1 C6 1.398(4) . ? C1 C14 1.506(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.392(4) . ? C3 C15 1.507(4) . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 C7 1.508(4) . ? C6 H6 0.9500 . ? C7 C8 1.522(4) . ? C7 H7A 0.97(4) . ? C7 H7B 0.97(3) . ? C8 C9 1.392(4) . ? C8 C13 1.395(4) . ? C9 C10 1.400(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(4) . ? C10 C16 1.507(4) . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.387(4) . ? C12 C17 1.503(4) . ? C13 H13 0.9500 . ? C14 O2 1.257(3) . ? C14 O1 1.259(4) . ? C15 O4 1.253(4) . ? C15 O3 1.267(3) . ? C16 O6 1.245(4) . ? C16 O5 1.272(3) . ? C17 O8 1.251(3) . ? C17 O7 1.281(4) . ? C18 N1 1.479(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.470(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O11 1.226(5) . ? C20 N2 1.332(5) . ? C20 H20 1.02(4) . ? C21 N2 1.456(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N2 1.420(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? O2 Co2 2.048(2) 3 ? O3 Co2 2.063(2) 1_455 ? O4 Co1 2.094(2) 1_455 ? O5 Co1 2.122(2) 2_445 ? O6 Co2 2.113(2) 4_556 ? O7 Co1 2.1147(19) 3_556 ? O8 Co1 2.315(2) 3_556 ? O9 Co2 2.053(2) 3 ? O9 H9OH 0.76(4) . ? O10 H10A 0.85(4) . ? O10 H10B 0.77(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 O9 Co1 O1 97.25(8) . . ? O9 Co1 O4 90.83(8) . 1_655 ? O1 Co1 O4 170.63(8) . 1_655 ? O9 Co1 O7 162.01(9) . 3_556 ? O1 Co1 O7 87.31(8) . 3_556 ? O4 Co1 O7 83.57(8) 1_655 3_556 ? O9 Co1 O5 100.50(9) . 2_455 ? O1 Co1 O5 91.73(8) . 2_455 ? O4 Co1 O5 91.45(8) 1_655 2_455 ? O7 Co1 O5 96.73(8) 3_556 2_455 ? O9 Co1 O8 102.77(8) . 3_556 ? O1 Co1 O8 91.86(8) . 3_556 ? O4 Co1 O8 81.69(8) 1_655 3_556 ? O7 Co1 O8 59.56(7) 3_556 3_556 ? O5 Co1 O8 155.79(8) 2_455 3_556 ? O2 Co2 O9 97.96(8) 3 3 ? O2 Co2 O3 91.15(8) 3 1_655 ? O9 Co2 O3 170.54(8) 3 1_655 ? O2 Co2 O6 88.99(9) 3 4_655 ? O9 Co2 O6 92.64(9) 3 4_655 ? O3 Co2 O6 90.07(8) 1_655 4_655 ? O2 Co2 O9 177.04(9) 3 . ? O9 Co2 O9 80.83(9) 3 . ? O3 Co2 O9 90.19(8) 1_655 . ? O6 Co2 O9 88.36(9) 4_655 . ? O2 Co2 O10 87.41(9) 3 . ? O9 Co2 O10 88.45(9) 3 . ? O3 Co2 O10 89.40(9) 1_655 . ? O6 Co2 O10 176.35(9) 4_655 . ? O9 Co2 O10 95.26(9) . . ? C2 C1 C6 119.4(3) . . ? C2 C1 C14 119.9(3) . . ? C6 C1 C14 120.6(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 C15 120.6(3) . . ? C4 C3 C15 119.4(3) . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 118.9(3) . . ? C6 C5 C7 121.6(3) . . ? C4 C5 C7 119.5(3) . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C5 C7 C8 114.9(2) . . ? C5 C7 H7A 114(2) . . ? C8 C7 H7A 108(2) . . ? C5 C7 H7B 110.9(18) . . ? C8 C7 H7B 107.6(18) . . ? H7A C7 H7B 101(3) . . ? C9 C8 C13 118.7(3) . . ? C9 C8 C7 122.8(3) . . ? C13 C8 C7 118.4(3) . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 119.2(3) . . ? C11 C10 C16 117.5(3) . . ? C9 C10 C16 123.4(3) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 C17 120.6(3) . . ? C11 C12 C17 119.4(3) . . ? C12 C13 C8 120.8(3) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O2 C14 O1 126.9(3) . . ? O2 C14 C1 116.7(3) . . ? O1 C14 C1 116.4(3) . . ? O4 C15 O3 127.1(3) . . ? O4 C15 C3 116.7(3) . . ? O3 C15 C3 116.2(3) . . ? O6 C16 O5 125.5(3) . . ? O6 C16 C10 115.7(2) . . ? O5 C16 C10 118.8(3) . . ? O8 C17 O7 121.2(3) . . ? O8 C17 C12 121.0(3) . . ? O7 C17 C12 117.8(3) . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O11 C20 N2 127.5(4) . . ? O11 C20 H20 121(2) . . ? N2 C20 H20 111(2) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 N1 C18 113.4(3) . . ? C19 N1 H1A 108.9 . . ? C18 N1 H1A 108.9 . . ? C19 N1 H1B 108.9 . . ? C18 N1 H1B 108.9 . . ? H1A N1 H1B 107.7 . . ? C20 N2 C22 120.5(5) . . ? C20 N2 C21 122.2(4) . . ? C22 N2 C21 117.2(4) . . ? C14 O1 Co1 135.49(19) . . ? C14 O2 Co2 128.39(19) . 3 ? C15 O3 Co2 123.54(19) . 1_455 ? C15 O4 Co1 134.56(19) . 1_455 ? C16 O5 Co1 122.52(19) . 2_445 ? C16 O6 Co2 141.93(19) . 4_556 ? C17 O7 Co1 93.38(17) . 3_556 ? C17 O8 Co1 85.13(16) . 3_556 ? Co1 O9 Co2 113.01(10) . 3 ? Co1 O9 Co2 120.62(10) . . ? Co2 O9 Co2 99.17(9) 3 . ? Co1 O9 H9OH 112(3) . . ? Co2 O9 H9OH 107(3) 3 . ? Co2 O9 H9OH 104(3) . . ? Co2 O10 H10A 119(3) . . ? Co2 O10 H10B 107(3) . . ? H10A O10 H10B 104(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10B O5 0.77(4) 2.16(5) 2.926(3) 174(4) 2_455 O10 H10A O11 0.85(4) 2.01(4) 2.847(4) 165(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.838 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.087 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 810536' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C44 H46 Mn3 N4 O18' _chemical_formula_sum 'C44 H46 Mn3 N4 O18' _chemical_formula_weight 1083.67 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.2417(11) _cell_length_b 10.7616(7) _cell_length_c 25.6486(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4483.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 4445 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 26.09 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8102 _exptl_absorpt_correction_T_max 0.8674 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 23535 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.09 _reflns_number_total 4445 _reflns_number_gt 3500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1099P)^2^+24.4574P] 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 4445 _refine_ls_number_parameters 319 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1890 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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 0.06817(4) 0.34777(6) 0.38048(3) 0.0146(2) Uani 1 1 d . . . Mn2 Mn 0.0000 0.5000 0.5000 0.0128(3) Uani 1 2 d S . . C1 C 0.2341(3) 0.3950(4) 0.49978(17) 0.0159(9) Uani 1 1 d . . . C2 C 0.3035(3) 0.3205(4) 0.50461(18) 0.0166(9) Uani 1 1 d . . . H2A H 0.3142 0.2570 0.4798 0.020 Uiso 1 1 calc R . . C3 C 0.3575(3) 0.3396(4) 0.54635(18) 0.0176(10) Uani 1 1 d . . . C4 C 0.3390(3) 0.4279(4) 0.58400(18) 0.0174(9) Uani 1 1 d . . . H4A H 0.3750 0.4388 0.6128 0.021 Uiso 1 1 calc R . . C5 C 0.2687(3) 0.5005(4) 0.58020(17) 0.0158(9) Uani 1 1 d . . . C6 C 0.2183(3) 0.4868(4) 0.53659(17) 0.0163(9) Uani 1 1 d . . . H6A H 0.1726 0.5408 0.5319 0.020 Uiso 1 1 calc R . . C7 C 0.2395(3) 0.5849(4) 0.62357(17) 0.0181(10) Uani 1 1 d . . . H7A H 0.2124 0.5328 0.6504 0.022 Uiso 1 1 calc R . . H7B H 0.1972 0.6413 0.6091 0.022 Uiso 1 1 calc R . . C8 C 0.3046(3) 0.6636(4) 0.65044(18) 0.0161(9) Uani 1 1 d . . . C9 C 0.3503(3) 0.7507(4) 0.62256(17) 0.0167(9) Uani 1 1 d . . . H9A H 0.3439 0.7565 0.5858 0.020 Uiso 1 1 calc R . . C10 C 0.4051(3) 0.8293(4) 0.64796(17) 0.0159(9) Uani 1 1 d . . . C11 C 0.4164(3) 0.8184(5) 0.70217(18) 0.0186(10) Uani 1 1 d . . . H11A H 0.4531 0.8725 0.7200 0.022 Uiso 1 1 calc R . . C12 C 0.3735(3) 0.7282(4) 0.72909(17) 0.0178(9) Uani 1 1 d . . . C13 C 0.3173(3) 0.6537(4) 0.70357(18) 0.0170(9) Uani 1 1 d . . . H13A H 0.2866 0.5943 0.7229 0.020 Uiso 1 1 calc R . . C14 C 0.1741(3) 0.3753(4) 0.45610(17) 0.0169(9) Uani 1 1 d . . . C15 C 0.4326(3) 0.2577(4) 0.55123(17) 0.0157(9) Uani 1 1 d . . . C16 C 0.4529(3) 0.9246(4) 0.61705(18) 0.0181(10) Uani 1 1 d . . . C17 C 0.3891(3) 0.7066(5) 0.78657(18) 0.0186(10) Uani 1 1 d . . . O1 O 0.11018(19) 0.4438(3) 0.45348(12) 0.0183(7) Uani 1 1 d . . . O2 O 0.1862(2) 0.2929(3) 0.42255(13) 0.0256(8) Uani 1 1 d . . . O3 O 0.4406(2) 0.1724(3) 0.51900(14) 0.0218(8) Uani 1 1 d . . . O4 O 0.4822(2) 0.2808(3) 0.58811(14) 0.0245(8) Uani 1 1 d . . . O5 O 0.4561(2) 0.9091(3) 0.56875(13) 0.0228(8) Uani 1 1 d . . . O6 O 0.4863(2) 1.0120(3) 0.64209(14) 0.0268(8) Uani 1 1 d . . . O7 O 0.4349(2) 0.7795(3) 0.81156(13) 0.0256(8) Uani 1 1 d . . . O8 O 0.3574(3) 0.6146(4) 0.80836(14) 0.0334(10) Uani 1 1 d . . . C18 C 0.6647(8) 0.4881(11) 0.6164(6) 0.111(4) Uani 1 1 d U . . H18A H 0.6811 0.4356 0.6458 0.167 Uiso 1 1 calc R . . H18B H 0.6937 0.5678 0.6184 0.167 Uiso 1 1 calc R . . H18C H 0.6787 0.4464 0.5836 0.167 Uiso 1 1 calc R . . C19 C 0.5355(8) 0.5914(10) 0.5774(5) 0.103(4) Uani 1 1 d . . . H19A H 0.4762 0.6030 0.5824 0.154 Uiso 1 1 calc R . . H19B H 0.5455 0.5525 0.5435 0.154 Uiso 1 1 calc R . . H19C H 0.5631 0.6723 0.5787 0.154 Uiso 1 1 calc R . . C20 C 0.608(2) 0.618(3) 0.7714(14) 0.041(2) Uani 0.25 1 d PU . . C20' C 0.5869(7) 0.6435(9) 0.7552(4) 0.041(2) Uani 0.75 1 d PU . . C21 C 0.6292(8) 0.8437(11) 0.7858(5) 0.062(3) Uani 0.75 1 d P . . C21' C 0.588(3) 0.898(4) 0.7809(15) 0.062(3) Uani 0.25 1 d P . . C22 C 0.6469(9) 0.7933(14) 0.6878(6) 0.135(6) Uani 1 1 d . . . N1 N 0.5677(5) 0.5118(9) 0.6186(4) 0.095(3) Uani 1 1 d . . . H1A H 0.5413 0.4363 0.6170 0.114 Uiso 1 1 calc R . . H1B H 0.5551 0.5471 0.6503 0.114 Uiso 1 1 calc R . . N2 N 0.6199(5) 0.7554(8) 0.7435(3) 0.085(2) Uani 1 1 d . . . O9 O 0.5640(7) 0.5758(8) 0.7151(4) 0.129(4) 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 0.0148(4) 0.0180(4) 0.0108(4) -0.0025(3) -0.0001(3) -0.0005(3) Mn2 0.0139(5) 0.0142(5) 0.0103(5) -0.0012(4) -0.0010(3) 0.0002(4) C1 0.015(2) 0.019(2) 0.013(2) 0.0000(18) 0.0005(17) -0.0032(18) C2 0.018(2) 0.017(2) 0.015(2) -0.0004(17) -0.0006(18) -0.0007(18) C3 0.017(2) 0.017(2) 0.018(2) 0.0005(18) 0.0007(18) 0.0020(18) C4 0.018(2) 0.019(2) 0.016(2) 0.0002(18) -0.0021(18) -0.0011(19) C5 0.017(2) 0.015(2) 0.015(2) -0.0010(17) -0.0005(17) -0.0014(18) C6 0.015(2) 0.018(2) 0.016(2) 0.0007(18) -0.0013(17) 0.0008(18) C7 0.017(2) 0.022(2) 0.015(2) -0.0030(19) -0.0031(18) 0.0031(19) C8 0.015(2) 0.014(2) 0.019(2) -0.0024(18) -0.0007(18) 0.0023(18) C9 0.023(2) 0.016(2) 0.011(2) 0.0011(17) -0.0008(17) 0.0045(19) C10 0.016(2) 0.019(2) 0.013(2) 0.0018(17) 0.0025(17) 0.0030(18) C11 0.019(2) 0.022(2) 0.015(2) -0.0003(19) -0.0032(18) -0.0005(19) C12 0.021(2) 0.018(2) 0.014(2) 0.0010(18) 0.0009(18) 0.0020(19) C13 0.021(2) 0.017(2) 0.013(2) 0.0025(17) 0.0012(18) -0.0010(19) C14 0.016(2) 0.020(2) 0.015(2) 0.0002(18) 0.0020(18) -0.0007(18) C15 0.017(2) 0.016(2) 0.014(2) 0.0023(18) 0.0003(17) 0.0009(18) C16 0.019(2) 0.018(2) 0.018(2) 0.0033(18) 0.0018(18) 0.0008(19) C17 0.019(2) 0.019(2) 0.018(2) 0.0018(19) -0.0005(19) 0.0005(19) O1 0.0152(16) 0.0268(19) 0.0131(15) -0.0029(13) -0.0031(12) 0.0030(14) O2 0.0235(18) 0.031(2) 0.0224(18) -0.0114(15) -0.0057(14) 0.0076(15) O3 0.0215(17) 0.0210(18) 0.0230(18) -0.0064(14) -0.0024(14) 0.0055(14) O4 0.0254(18) 0.0233(19) 0.0247(18) -0.0061(15) -0.0098(15) 0.0080(15) O5 0.0281(18) 0.0256(19) 0.0146(16) 0.0030(14) 0.0028(14) -0.0055(15) O6 0.038(2) 0.0234(19) 0.0189(18) -0.0009(15) 0.0053(15) -0.0110(16) O7 0.036(2) 0.0259(19) 0.0147(17) 0.0028(14) -0.0080(14) -0.0091(16) O8 0.044(2) 0.039(2) 0.0176(18) 0.0102(16) -0.0074(16) -0.0204(19) C18 0.091(7) 0.090(7) 0.153(9) 0.020(6) 0.044(6) 0.009(6) C19 0.108(9) 0.070(7) 0.129(10) 0.021(7) 0.029(8) 0.002(7) C20 0.046(5) 0.032(4) 0.045(5) -0.009(4) 0.013(4) -0.005(4) C20' 0.046(5) 0.032(4) 0.045(5) -0.009(4) 0.013(4) -0.005(4) C21 0.076(9) 0.053(7) 0.055(6) -0.023(6) 0.012(6) -0.025(5) C21' 0.076(9) 0.053(7) 0.055(6) -0.023(6) 0.012(6) -0.025(5) C22 0.127(11) 0.124(11) 0.155(13) 0.084(10) 0.046(10) 0.000(9) N1 0.084(6) 0.095(7) 0.105(7) 0.031(6) 0.007(5) -0.035(5) N2 0.079(5) 0.090(6) 0.087(6) -0.009(5) 0.005(5) 0.008(5) O9 0.211(11) 0.073(5) 0.103(6) -0.006(5) 0.007(6) -0.017(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O6 2.094(4) 4_466 ? Mn1 O4 2.125(3) 4_456 ? Mn1 O7 2.237(4) 2_564 ? Mn1 O1 2.245(3) . ? Mn1 O8 2.247(4) 2_564 ? Mn1 O2 2.277(3) . ? Mn1 C17 2.574(5) 2_564 ? Mn1 C14 2.610(5) . ? Mn2 O5 2.139(3) 8_655 ? Mn2 O5 2.139(3) 4_466 ? Mn2 O3 2.147(3) 8_665 ? Mn2 O3 2.147(3) 4_456 ? Mn2 O1 2.234(3) 5_566 ? Mn2 O1 2.234(3) . ? C1 C6 1.391(6) . ? C1 C2 1.388(7) . ? C1 C14 1.500(6) . ? C2 C3 1.399(7) . ? C3 C4 1.388(7) . ? C3 C15 1.511(6) . ? C4 C5 1.388(6) . ? C5 C6 1.393(6) . ? C5 C7 1.512(6) . ? C7 C8 1.520(6) . ? C8 C13 1.382(6) . ? C8 C9 1.393(7) . ? C9 C10 1.390(7) . ? C10 C11 1.407(7) . ? C10 C16 1.511(6) . ? C11 C12 1.380(7) . ? C12 C13 1.381(7) . ? C12 C17 1.514(6) . ? C14 O2 1.251(6) . ? C14 O1 1.275(6) . ? C15 O3 1.242(6) . ? C15 O4 1.266(6) . ? C16 O5 1.251(6) . ? C16 O6 1.261(6) . ? C17 O7 1.257(6) . ? C17 O8 1.249(6) . ? C17 Mn1 2.574(5) 2_565 ? O3 Mn2 2.147(3) 4_556 ? O4 Mn1 2.125(3) 4_556 ? O5 Mn2 2.139(3) 4_566 ? O6 Mn1 2.094(4) 4_566 ? O7 Mn1 2.237(4) 2_565 ? O8 Mn1 2.247(4) 2_565 ? C18 N1 1.596(15) . ? C19 N1 1.457(14) . ? C20 C20' 0.61(3) . ? C20 N2 1.65(4) . ? C20 O9 1.68(4) . ? C20' O9 1.314(14) . ? C20' N2 1.352(13) . ? C21 C21' 0.91(4) . ? C21 N2 1.450(13) . ? C21' N2 1.89(4) . ? C22 N2 1.549(15) . ? 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 O6 Mn1 O4 98.99(15) 4_466 4_456 ? O6 Mn1 O7 102.06(14) 4_466 2_564 ? O4 Mn1 O7 83.47(13) 4_456 2_564 ? O6 Mn1 O1 95.28(13) 4_466 . ? O4 Mn1 O1 100.56(13) 4_456 . ? O7 Mn1 O1 161.39(13) 2_564 . ? O6 Mn1 O8 89.11(16) 4_466 2_564 ? O4 Mn1 O8 141.58(14) 4_456 2_564 ? O7 Mn1 O8 58.12(13) 2_564 2_564 ? O1 Mn1 O8 116.11(13) . 2_564 ? O6 Mn1 O2 148.52(14) 4_466 . ? O4 Mn1 O2 101.83(15) 4_456 . ? O7 Mn1 O2 103.54(13) 2_564 . ? O1 Mn1 O2 57.88(12) . . ? O8 Mn1 O2 89.07(15) 2_564 . ? O6 Mn1 C17 94.38(15) 4_466 2_564 ? O4 Mn1 C17 112.58(14) 4_456 2_564 ? O7 Mn1 C17 29.22(14) 2_564 2_564 ? O1 Mn1 C17 143.45(14) . 2_564 ? O8 Mn1 C17 29.02(14) 2_564 2_564 ? O2 Mn1 C17 99.07(14) . 2_564 ? O6 Mn1 C14 122.88(15) 4_466 . ? O4 Mn1 C14 103.04(15) 4_456 . ? O7 Mn1 C14 132.17(15) 2_564 . ? O1 Mn1 C14 29.24(13) . . ? O8 Mn1 C14 103.68(14) 2_564 . ? O2 Mn1 C14 28.64(13) . . ? C17 Mn1 C14 122.93(15) 2_564 . ? O5 Mn2 O5 180.00 8_655 4_466 ? O5 Mn2 O3 93.37(14) 8_655 8_665 ? O5 Mn2 O3 86.63(14) 4_466 8_665 ? O5 Mn2 O3 86.63(14) 8_655 4_456 ? O5 Mn2 O3 93.37(14) 4_466 4_456 ? O3 Mn2 O3 180.000 8_665 4_456 ? O5 Mn2 O1 87.16(12) 8_655 5_566 ? O5 Mn2 O1 92.84(12) 4_466 5_566 ? O3 Mn2 O1 90.25(13) 8_665 5_566 ? O3 Mn2 O1 89.75(13) 4_456 5_566 ? O5 Mn2 O1 92.84(12) 8_655 . ? O5 Mn2 O1 87.16(12) 4_466 . ? O3 Mn2 O1 89.75(13) 8_665 . ? O3 Mn2 O1 90.25(13) 4_456 . ? O1 Mn2 O1 180.00 5_566 . ? C6 C1 C2 120.0(4) . . ? C6 C1 C14 119.2(4) . . ? C2 C1 C14 120.8(4) . . ? C1 C2 C3 119.4(4) . . ? C4 C3 C2 119.9(4) . . ? C4 C3 C15 121.1(4) . . ? C2 C3 C15 118.9(4) . . ? C5 C4 C3 121.0(4) . . ? C4 C5 C6 118.7(4) . . ? C4 C5 C7 123.0(4) . . ? C6 C5 C7 118.1(4) . . ? C1 C6 C5 120.8(4) . . ? C5 C7 C8 116.8(4) . . ? C13 C8 C9 118.6(4) . . ? C13 C8 C7 120.5(4) . . ? C9 C8 C7 120.9(4) . . ? C10 C9 C8 120.7(4) . . ? C9 C10 C11 119.7(4) . . ? C9 C10 C16 119.7(4) . . ? C11 C10 C16 120.5(4) . . ? C12 C11 C10 119.1(4) . . ? C13 C12 C11 120.4(4) . . ? C13 C12 C17 118.9(4) . . ? C11 C12 C17 120.7(4) . . ? C12 C13 C8 121.4(4) . . ? O2 C14 O1 120.1(4) . . ? O2 C14 C1 120.8(4) . . ? O1 C14 C1 119.1(4) . . ? O2 C14 Mn1 60.8(2) . . ? O1 C14 Mn1 59.3(2) . . ? C1 C14 Mn1 178.3(3) . . ? O3 C15 O4 125.1(4) . . ? O3 C15 C3 117.4(4) . . ? O4 C15 C3 117.5(4) . . ? O5 C16 O6 125.9(5) . . ? O5 C16 C10 116.8(4) . . ? O6 C16 C10 117.4(4) . . ? O7 C17 O8 120.8(4) . . ? O7 C17 C12 120.0(4) . . ? O8 C17 C12 119.2(4) . . ? O7 C17 Mn1 60.4(2) . 2_565 ? O8 C17 Mn1 60.8(2) . 2_565 ? C12 C17 Mn1 172.5(3) . 2_565 ? C14 O1 Mn2 141.3(3) . . ? C14 O1 Mn1 91.5(3) . . ? Mn2 O1 Mn1 109.07(13) . . ? C14 O2 Mn1 90.6(3) . . ? C15 O3 Mn2 146.8(3) . 4_556 ? C15 O4 Mn1 125.0(3) . 4_556 ? C16 O5 Mn2 140.3(3) . 4_566 ? C16 O6 Mn1 132.0(3) . 4_566 ? C17 O7 Mn1 90.4(3) . 2_565 ? C17 O8 Mn1 90.2(3) . 2_565 ? C20' C20 N2 51(3) . . ? C20' C20 O9 44(3) . . ? N2 C20 O9 85.3(17) . . ? C20 C20' O9 117(4) . . ? C20 C20' N2 109(4) . . ? O9 C20' N2 115.6(9) . . ? C21' C21 N2 104(3) . . ? C21 C21' N2 48(2) . . ? C19 N1 C18 115.0(9) . . ? C20' N2 C21 117.4(9) . . ? C20' N2 C22 123.4(10) . . ? C21 N2 C22 119.2(10) . . ? C20' N2 C20 20.4(13) . . ? C21 N2 C20 105.9(14) . . ? C22 N2 C20 131.8(15) . . ? C20' N2 C21' 120.2(13) . . ? C21 N2 C21' 27.7(13) . . ? C22 N2 C21' 109.4(15) . . ? C20 N2 C21' 118.6(18) . . ? C20' O9 C20 18.9(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.399 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.133 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 810537' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H40 Mg3 N3 O21' _chemical_formula_sum 'C39 H40 Mg3 N3 O21' _chemical_formula_weight 959.67 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 10.7810(5) _cell_length_b 15.8837(7) _cell_length_c 25.1737(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4310.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 8471 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 26.05 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9674 _exptl_absorpt_correction_T_max 0.9766 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 22780 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.05 _reflns_number_total 8471 _reflns_number_gt 6364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1365P)^2^+1.7301P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(4) _refine_ls_number_reflns 8471 _refine_ls_number_parameters 567 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2232 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.004 _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 Mg1 Mg 0.29454(17) 0.17574(11) -0.28175(7) 0.0165(4) Uani 1 1 d . . . Mg2 Mg 0.43367(17) 0.24978(12) -0.39740(7) 0.0134(3) Uani 1 1 d . . . Mg3 Mg 0.57241(16) 0.32989(12) -0.51669(7) 0.0166(4) Uani 1 1 d . . . C1 C 0.3260(5) 0.0132(4) -0.4007(2) 0.0178(11) Uani 1 1 d . . . C2 C 0.2484(5) -0.0571(4) -0.4048(2) 0.0203(12) Uani 1 1 d . . . H2A H 0.1884 -0.0678 -0.3780 0.024 Uiso 1 1 calc R . . C3 C 0.2588(5) -0.1116(3) -0.4481(2) 0.0173(11) Uani 1 1 d . . . C4 C 0.3452(5) -0.0937(3) -0.4879(2) 0.0161(11) Uani 1 1 d . . . H4A H 0.3507 -0.1296 -0.5179 0.019 Uiso 1 1 calc R . . C5 C 0.4245(5) -0.0234(3) -0.4843(2) 0.0177(11) Uani 1 1 d . . . C6 C 0.4153(5) 0.0274(3) -0.4393(2) 0.0179(11) Uani 1 1 d . . . H6A H 0.4715 0.0729 -0.4350 0.021 Uiso 1 1 calc R . . C7 C 0.5045(5) 0.0037(4) -0.5294(2) 0.0210(12) Uani 1 1 d . . . H7A H 0.5512 0.0540 -0.5176 0.025 Uiso 1 1 calc R . . H7B H 0.4490 0.0221 -0.5585 0.025 Uiso 1 1 calc R . . C8 C 0.5967(5) -0.0571(4) -0.5527(2) 0.0206(12) Uani 1 1 d . . . C9 C 0.6021(5) -0.0667(4) -0.6079(2) 0.0217(12) Uani 1 1 d . . . H9A H 0.5428 -0.0393 -0.6298 0.026 Uiso 1 1 calc R . . C10 C 0.6945(5) -0.1167(4) -0.6309(2) 0.0221(12) Uani 1 1 d . . . C11 C 0.7769(5) -0.1605(4) -0.5988(2) 0.0220(12) Uani 1 1 d . . . H11A H 0.8391 -0.1947 -0.6146 0.026 Uiso 1 1 calc R . . C12 C 0.7691(5) -0.1546(4) -0.5443(2) 0.0182(11) Uani 1 1 d . . . C13 C 0.6786(5) -0.1035(4) -0.5217(2) 0.0186(11) Uani 1 1 d . . . H13A H 0.6727 -0.1001 -0.4841 0.022 Uiso 1 1 calc R . . C14 C 0.3123(5) 0.0732(3) -0.3565(2) 0.0162(11) Uani 1 1 d . . . C15 C 0.1735(5) -0.1859(3) -0.4524(2) 0.0155(11) Uani 1 1 d . . . C16 C 0.7010(5) -0.1263(4) -0.6898(2) 0.0221(13) Uani 1 1 d . . . C17 C 0.8581(5) -0.2043(3) -0.5106(2) 0.0184(12) Uani 1 1 d . . . C18 C 0.5460(5) 0.4832(4) -0.3895(2) 0.0164(11) Uani 1 1 d . . . C19 C 0.6219(5) 0.5526(4) -0.3854(2) 0.0203(12) Uani 1 1 d . . . H19A H 0.6845 0.5618 -0.4113 0.024 Uiso 1 1 calc R . . C20 C 0.6078(5) 0.6087(3) -0.3442(2) 0.0150(11) Uani 1 1 d . . . C21 C 0.5217(5) 0.5937(4) -0.3042(2) 0.0168(11) Uani 1 1 d . . . H21A H 0.5143 0.6314 -0.2751 0.020 Uiso 1 1 calc R . . C22 C 0.4466(5) 0.5229(3) -0.3074(2) 0.0149(11) Uani 1 1 d . . . C23 C 0.4558(5) 0.4699(3) -0.3508(2) 0.0168(11) Uani 1 1 d . . . H23A H 0.4001 0.4239 -0.3543 0.020 Uiso 1 1 calc R . . C24 C 0.3615(5) 0.4987(4) -0.2607(2) 0.0176(11) Uani 1 1 d . . . H24A H 0.3052 0.4533 -0.2726 0.021 Uiso 1 1 calc R . . H24B H 0.4137 0.4754 -0.2318 0.021 Uiso 1 1 calc R . . C25 C 0.2840(5) 0.5687(4) -0.2380(2) 0.0165(11) Uani 1 1 d . . . C26 C 0.2941(5) 0.5935(4) -0.1856(2) 0.0178(12) Uani 1 1 d . . . H26A H 0.3559 0.5687 -0.1636 0.021 Uiso 1 1 calc R . . C27 C 0.2146(5) 0.6545(4) -0.1642(2) 0.0201(12) Uani 1 1 d . . . C28 C 0.1230(5) 0.6898(4) -0.1952(2) 0.0212(12) Uani 1 1 d . . . H28A H 0.0665 0.7289 -0.1801 0.025 Uiso 1 1 calc R . . C29 C 0.1129(5) 0.6679(4) -0.2493(2) 0.0177(12) Uani 1 1 d . . . C30 C 0.1931(5) 0.6068(3) -0.2699(2) 0.0173(11) Uani 1 1 d . . . H30A H 0.1858 0.5907 -0.3061 0.021 Uiso 1 1 calc R . . C31 C 0.5599(5) 0.4226(4) -0.4355(2) 0.0149(11) Uani 1 1 d . . . C32 C 0.6908(5) 0.6862(3) -0.3409(2) 0.0160(11) Uani 1 1 d . . . C33 C 0.2305(5) 0.6812(4) -0.1072(2) 0.0233(12) Uani 1 1 d . . . C34 C 0.0189(5) 0.7091(3) -0.2836(2) 0.0174(11) Uani 1 1 d . . . C35 C 0.3264(8) 0.4048(6) -0.5636(3) 0.0521(8) Uani 1 1 d . . . H35A H 0.2675 0.4162 -0.5364 0.063 Uiso 1 1 calc R . . C36 C 0.3725(7) 0.3707(6) -0.6569(3) 0.0521(8) Uani 1 1 d . . . H36A H 0.4579 0.3787 -0.6445 0.078 Uiso 1 1 calc R . . H36B H 0.3547 0.4107 -0.6855 0.078 Uiso 1 1 calc R . . H36C H 0.3623 0.3131 -0.6701 0.078 Uiso 1 1 calc R . . C37 C 0.1559(7) 0.3747(6) -0.6224(3) 0.0521(8) Uani 1 1 d . . . H37A H 0.1086 0.3878 -0.5902 0.078 Uiso 1 1 calc R . . H37B H 0.1398 0.3164 -0.6330 0.078 Uiso 1 1 calc R . . H37C H 0.1305 0.4128 -0.6511 0.078 Uiso 1 1 calc R . . C38 C -0.4249(7) 0.4089(5) -0.0029(3) 0.049(2) Uani 1 1 d . . . H38A H -0.3415 0.4330 -0.0057 0.074 Uiso 1 1 calc R . . H38B H -0.4743 0.4423 0.0221 0.074 Uiso 1 1 calc R . . H38C H -0.4647 0.4096 -0.0379 0.074 Uiso 1 1 calc R . . C39 C -0.5306(7) 0.2782(5) 0.0242(4) 0.056(2) Uani 1 1 d . . . H39A H -0.5134 0.2212 0.0374 0.083 Uiso 1 1 calc R . . H39B H -0.5757 0.2746 -0.0095 0.083 Uiso 1 1 calc R . . H39C H -0.5810 0.3086 0.0503 0.083 Uiso 1 1 calc R . . O1 O 0.3770(3) 0.1398(2) -0.35436(14) 0.0173(8) Uani 1 1 d . . . O2 O 0.2335(4) 0.0606(3) -0.31924(15) 0.0259(9) Uani 1 1 d . . . O3 O 0.0870(3) -0.1879(2) -0.41941(15) 0.0196(8) Uani 1 1 d . . . O4 O 0.1938(4) -0.2398(2) -0.48741(15) 0.0210(9) Uani 1 1 d . . . O5 O 0.6194(4) -0.0949(3) -0.71923(16) 0.0339(11) Uani 1 1 d . . . O6 O 0.7897(4) -0.1678(3) -0.70888(15) 0.0294(10) Uani 1 1 d . . . O7 O 0.9513(4) -0.2355(3) -0.53358(15) 0.0247(9) Uani 1 1 d . . . O8 O 0.8344(4) -0.2114(3) -0.46214(14) 0.0202(8) Uani 1 1 d . . . O9 O 0.4910(3) 0.3578(2) -0.43803(13) 0.0179(8) Uani 1 1 d . . . O10 O 0.6369(3) 0.4372(2) -0.47140(14) 0.0202(8) Uani 1 1 d . . . O11 O 0.7779(3) 0.6900(3) -0.37276(16) 0.0218(9) Uani 1 1 d . . . O12 O 0.6650(4) 0.7416(3) -0.30610(15) 0.0219(9) Uani 1 1 d . . . O13 O 0.3222(4) 0.6544(3) -0.08214(16) 0.0259(9) Uani 1 1 d . . . O14 O 0.1487(4) 0.7297(3) -0.08849(17) 0.0389(12) Uani 1 1 d . . . H14 H 0.1657 0.7411 -0.0567 0.058 Uiso 1 1 calc . . . O15 O -0.0763(4) 0.7380(3) -0.26160(15) 0.0257(10) Uani 1 1 d . . . O16 O 0.0397(4) 0.7113(3) -0.33275(14) 0.0209(8) Uani 1 1 d . . . O17 O 0.4396(5) 0.4085(4) -0.5525(2) 0.0521(8) Uani 1 1 d . . . N1 N 0.2854(6) 0.3853(4) -0.6121(3) 0.0521(8) Uani 1 1 d . . . N2 N -0.4163(5) 0.3218(4) 0.0162(3) 0.0424(15) Uani 1 1 d . . . O1W O -0.3044(6) 0.3046(5) 0.1203(3) 0.0702(19) Uani 1 1 d . . . O2W O 0.6317(13) 0.1476(9) -0.6024(5) 0.073(4) Uiso 0.50 1 d P . . O3W O 0.3648(15) -0.0548(11) -0.7352(6) 0.083(4) Uiso 0.50 1 d P . . O7W O 0.571(2) 0.1578(15) -0.6368(9) 0.100(7) Uiso 0.40 1 d P . . O6W O 0.8008(18) 0.1021(14) -0.6273(8) 0.094(6) Uiso 0.40 1 d P . . O5W O 0.567(3) 0.097(2) -0.7195(14) 0.071(9) Uiso 0.20 1 d P . . O4W O 1.062(4) -0.103(3) -0.7782(19) 0.072(12) Uiso 0.15 1 d P . . O8W O 1.038(3) -0.1587(19) -0.7425(11) 0.074(8) Uiso 0.25 1 d P . . O9W O 0.297(3) -0.095(2) -0.7311(13) 0.090(10) Uiso 0.25 1 d P . . 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 Mg1 0.0209(9) 0.0168(9) 0.0118(8) -0.0006(7) 0.0014(7) -0.0001(7) Mg2 0.0155(8) 0.0149(8) 0.0097(7) -0.0010(6) 0.0013(6) -0.0007(6) Mg3 0.0195(9) 0.0166(9) 0.0138(8) 0.0002(7) 0.0025(7) 0.0009(8) C1 0.019(3) 0.019(3) 0.016(3) -0.004(2) 0.000(2) -0.001(2) C2 0.023(3) 0.024(3) 0.015(3) -0.001(2) 0.000(2) -0.002(2) C3 0.017(3) 0.013(3) 0.022(3) -0.001(2) 0.000(2) -0.001(2) C4 0.016(3) 0.020(3) 0.012(2) 0.000(2) 0.000(2) 0.002(2) C5 0.019(3) 0.013(3) 0.021(3) -0.002(2) -0.001(2) 0.003(2) C6 0.019(3) 0.014(3) 0.021(3) 0.004(2) -0.003(2) 0.004(2) C7 0.019(3) 0.024(3) 0.020(3) -0.003(2) 0.006(2) -0.001(2) C8 0.023(3) 0.019(3) 0.019(3) -0.002(2) -0.001(2) -0.004(2) C9 0.021(3) 0.026(3) 0.018(3) 0.003(2) 0.001(2) 0.004(2) C10 0.030(3) 0.027(3) 0.009(2) 0.000(2) 0.003(2) 0.003(3) C11 0.021(3) 0.023(3) 0.023(3) -0.002(2) 0.003(2) 0.004(2) C12 0.017(3) 0.020(3) 0.018(3) 0.003(2) -0.002(2) -0.002(2) C13 0.015(3) 0.025(3) 0.015(2) -0.001(2) -0.006(2) -0.001(2) C14 0.017(3) 0.015(3) 0.016(3) 0.001(2) -0.004(2) 0.004(2) C15 0.014(2) 0.018(3) 0.015(2) 0.002(2) 0.002(2) 0.001(2) C16 0.027(3) 0.030(3) 0.010(2) -0.002(2) -0.002(2) 0.001(3) C17 0.019(3) 0.014(3) 0.022(3) 0.000(2) -0.004(2) -0.004(2) C18 0.017(3) 0.015(3) 0.017(3) -0.002(2) 0.004(2) 0.006(2) C19 0.020(3) 0.021(3) 0.020(3) 0.000(2) 0.004(2) -0.002(2) C20 0.016(3) 0.015(3) 0.014(3) 0.001(2) 0.000(2) -0.004(2) C21 0.016(3) 0.019(3) 0.015(2) -0.006(2) 0.003(2) 0.000(2) C22 0.012(2) 0.020(3) 0.013(2) 0.001(2) 0.000(2) 0.001(2) C23 0.017(3) 0.016(3) 0.018(3) -0.003(2) 0.002(2) -0.002(2) C24 0.022(3) 0.016(3) 0.015(3) -0.001(2) 0.005(2) -0.001(2) C25 0.011(2) 0.023(3) 0.016(3) -0.002(2) 0.0035(19) -0.001(2) C26 0.016(3) 0.024(3) 0.014(2) 0.006(2) -0.004(2) 0.002(2) C27 0.022(3) 0.020(3) 0.018(3) 0.001(2) 0.005(2) 0.001(2) C28 0.020(3) 0.029(3) 0.015(3) -0.001(2) -0.001(2) -0.002(3) C29 0.017(3) 0.022(3) 0.013(2) 0.003(2) 0.002(2) -0.004(2) C30 0.023(3) 0.021(3) 0.008(2) -0.001(2) 0.002(2) -0.002(2) C31 0.011(2) 0.021(3) 0.012(2) 0.000(2) 0.000(2) -0.001(2) C32 0.013(3) 0.014(3) 0.021(3) 0.005(2) -0.001(2) 0.001(2) C33 0.028(3) 0.024(3) 0.018(3) -0.002(2) -0.003(2) -0.002(3) C34 0.022(3) 0.019(3) 0.011(2) -0.001(2) -0.002(2) 0.000(2) C35 0.0467(17) 0.054(2) 0.0560(18) 0.0102(16) -0.0110(14) -0.0001(16) C36 0.0467(17) 0.054(2) 0.0560(18) 0.0102(16) -0.0110(14) -0.0001(16) C37 0.0467(17) 0.054(2) 0.0560(18) 0.0102(16) -0.0110(14) -0.0001(16) C38 0.038(4) 0.048(5) 0.062(5) -0.012(4) -0.006(4) 0.002(4) C39 0.034(4) 0.032(4) 0.100(7) -0.008(4) 0.016(4) -0.001(3) O1 0.021(2) 0.016(2) 0.0152(17) -0.0008(15) 0.0014(15) -0.0004(16) O2 0.034(2) 0.023(2) 0.020(2) -0.0033(17) 0.0115(18) -0.0068(19) O3 0.025(2) 0.016(2) 0.0184(18) -0.0012(16) 0.0044(16) -0.0026(17) O4 0.024(2) 0.018(2) 0.021(2) -0.0083(17) 0.0048(16) -0.0044(17) O5 0.036(2) 0.047(3) 0.019(2) -0.0037(19) -0.0006(18) 0.016(2) O6 0.031(2) 0.044(3) 0.0133(19) -0.0088(18) -0.0006(17) 0.017(2) O7 0.026(2) 0.031(2) 0.018(2) 0.0005(18) 0.0015(16) 0.0084(19) O8 0.0236(19) 0.028(2) 0.0095(18) 0.0059(16) 0.0017(15) 0.0007(17) O9 0.027(2) 0.0148(19) 0.0120(18) -0.0025(15) 0.0035(15) -0.0033(17) O10 0.026(2) 0.020(2) 0.0149(18) -0.0017(16) 0.0058(16) 0.0009(17) O11 0.018(2) 0.024(2) 0.023(2) 0.0019(17) 0.0055(16) -0.0018(17) O12 0.0198(19) 0.022(2) 0.0235(19) -0.0082(17) -0.0001(16) -0.0039(17) O13 0.033(2) 0.027(2) 0.0184(19) -0.0033(17) -0.0074(17) 0.0095(19) O14 0.041(3) 0.052(3) 0.023(2) -0.016(2) -0.005(2) 0.014(2) O15 0.022(2) 0.036(3) 0.019(2) 0.0038(18) -0.0020(16) 0.0123(19) O16 0.028(2) 0.021(2) 0.0138(19) 0.0003(17) -0.0019(17) 0.0033(17) O17 0.0467(17) 0.054(2) 0.0560(18) 0.0102(16) -0.0110(14) -0.0001(16) N1 0.0467(17) 0.054(2) 0.0560(18) 0.0102(16) -0.0110(14) -0.0001(16) N2 0.033(3) 0.042(4) 0.052(4) 0.005(3) 0.005(3) 0.009(3) O1W 0.053(4) 0.091(5) 0.066(4) -0.030(4) 0.005(3) 0.008(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 Mg1 O12 2.013(4) 3_465 ? Mg1 O15 2.018(4) 3_565 ? Mg1 O6 2.051(4) 2_655 ? Mg1 O1 2.111(4) . ? Mg1 O2 2.161(4) . ? Mg1 O5 2.233(5) 2_655 ? Mg1 C16 2.446(5) 2_655 ? Mg1 C14 2.496(6) . ? Mg1 Mg2 3.480(3) . ? Mg2 O3 2.001(4) 3 ? Mg2 O11 2.030(4) 3_465 ? Mg2 O8 2.043(4) 3_455 ? Mg2 O16 2.083(4) 3_565 ? Mg2 O9 2.091(4) . ? Mg2 O1 2.144(4) . ? Mg2 Mg3 3.588(2) . ? Mg3 O13 2.017(4) 2_664 ? Mg3 O7 2.033(4) 3_455 ? Mg3 O4 2.074(4) 3 ? Mg3 O17 2.104(6) . ? Mg3 O10 2.166(4) . ? Mg3 O9 2.211(4) . ? Mg3 C31 2.523(5) . ? C1 C6 1.387(8) . ? C1 C2 1.399(8) . ? C1 C14 1.473(7) . ? C2 C3 1.397(8) . ? C3 C4 1.396(7) . ? C3 C15 1.500(7) . ? C4 C5 1.408(8) . ? C5 C6 1.394(8) . ? C5 C7 1.490(8) . ? C7 C8 1.505(8) . ? C8 C13 1.390(8) . ? C8 C9 1.399(8) . ? C9 C10 1.400(8) . ? C10 C11 1.387(8) . ? C10 C16 1.491(7) . ? C11 C12 1.380(8) . ? C12 C13 1.391(8) . ? C12 C17 1.504(7) . ? C14 O1 1.270(7) . ? C14 O2 1.281(7) . ? C15 O4 1.249(7) . ? C15 O3 1.249(6) . ? C16 O5 1.254(7) . ? C16 O6 1.257(7) . ? C16 Mg1 2.446(5) 2_654 ? C17 O8 1.251(6) . ? C17 O7 1.261(7) . ? C18 C19 1.376(8) . ? C18 C23 1.391(7) . ? C18 C31 1.514(7) . ? C19 C20 1.377(8) . ? C20 C21 1.390(7) . ? C20 C32 1.524(7) . ? C21 C22 1.388(8) . ? C22 C23 1.384(7) . ? C22 C24 1.540(7) . ? C24 C25 1.504(8) . ? C25 C26 1.381(7) . ? C25 C30 1.404(7) . ? C26 C27 1.401(8) . ? C27 C28 1.378(8) . ? C27 C33 1.507(8) . ? C28 C29 1.408(8) . ? C29 C30 1.400(8) . ? C29 C34 1.484(8) . ? C31 O10 1.249(6) . ? C31 O9 1.272(6) . ? C32 O11 1.236(6) . ? C32 O12 1.272(7) . ? C33 O13 1.248(7) . ? C33 O14 1.262(7) . ? C34 O15 1.253(7) . ? C34 O16 1.258(6) . ? C35 O17 1.253(9) . ? C35 N1 1.337(11) . ? C36 N1 1.484(11) . ? C37 N1 1.430(10) . ? C38 N2 1.468(11) . ? C39 N2 1.428(9) . ? O3 Mg2 2.001(4) 3_455 ? O4 Mg3 2.074(4) 3_455 ? O5 Mg1 2.233(5) 2_654 ? O6 Mg1 2.051(4) 2_654 ? O7 Mg3 2.033(4) 3 ? O8 Mg2 2.043(4) 3 ? O11 Mg2 2.030(4) 3_565 ? O12 Mg1 2.013(4) 3_565 ? O13 Mg3 2.017(4) 2_665 ? O15 Mg1 2.018(4) 3_465 ? O16 Mg2 2.083(4) 3_465 ? O2W O7W 1.10(2) . ? O3W O9W 0.97(3) . ? O5W O8W 1.18(4) 3_455 ? O5W O4W 1.48(6) 3_455 ? O4W O8W 1.29(5) . ? O4W O5W 1.48(6) 3 ? O8W O5W 1.18(4) 3 ? 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 O12 Mg1 O15 96.45(19) 3_465 3_565 ? O12 Mg1 O6 90.31(17) 3_465 2_655 ? O15 Mg1 O6 97.04(19) 3_565 2_655 ? O12 Mg1 O1 101.82(17) 3_465 . ? O15 Mg1 O1 96.34(16) 3_565 . ? O6 Mg1 O1 160.79(19) 2_655 . ? O12 Mg1 O2 101.99(18) 3_465 . ? O15 Mg1 O2 153.45(18) 3_565 . ? O6 Mg1 O2 101.75(19) 2_655 . ? O1 Mg1 O2 61.42(15) . . ? O12 Mg1 O5 151.41(18) 3_465 2_655 ? O15 Mg1 O5 85.80(19) 3_565 2_655 ? O6 Mg1 O5 61.18(16) 2_655 2_655 ? O1 Mg1 O5 106.26(17) . 2_655 ? O2 Mg1 O5 86.99(19) . 2_655 ? O12 Mg1 C16 120.76(19) 3_465 2_655 ? O15 Mg1 C16 88.06(19) 3_565 2_655 ? O6 Mg1 C16 30.90(17) 2_655 2_655 ? O1 Mg1 C16 136.46(19) . 2_655 ? O2 Mg1 C16 98.51(19) . 2_655 ? O5 Mg1 C16 30.67(17) 2_655 2_655 ? O12 Mg1 C14 104.45(18) 3_465 . ? O15 Mg1 C14 125.43(19) 3_565 . ? O6 Mg1 C14 131.9(2) 2_655 . ? O1 Mg1 C14 30.56(16) . . ? O2 Mg1 C14 30.87(16) . . ? O5 Mg1 C14 97.12(18) 2_655 . ? C16 Mg1 C14 120.2(2) 2_655 . ? O12 Mg1 Mg2 79.86(13) 3_465 . ? O15 Mg1 Mg2 71.55(12) 3_565 . ? O6 Mg1 Mg2 163.76(16) 2_655 . ? O1 Mg1 Mg2 35.44(11) . . ? O2 Mg1 Mg2 92.98(12) . . ? O5 Mg1 Mg2 127.23(13) 2_655 . ? C16 Mg1 Mg2 153.14(16) 2_655 . ? C14 Mg1 Mg2 63.71(13) . . ? O3 Mg2 O11 178.0(2) 3 3_465 ? O3 Mg2 O8 93.74(17) 3 3_455 ? O11 Mg2 O8 87.18(17) 3_465 3_455 ? O3 Mg2 O16 84.77(17) 3 3_565 ? O11 Mg2 O16 94.34(17) 3_465 3_565 ? O8 Mg2 O16 178.29(19) 3_455 3_565 ? O3 Mg2 O9 91.36(16) 3 . ? O11 Mg2 O9 90.42(17) 3_465 . ? O8 Mg2 O9 90.55(16) 3_455 . ? O16 Mg2 O9 88.65(16) 3_565 . ? O3 Mg2 O1 88.58(17) 3 . ? O11 Mg2 O1 89.63(17) 3_465 . ? O8 Mg2 O1 90.61(16) 3_455 . ? O16 Mg2 O1 90.20(16) 3_565 . ? O9 Mg2 O1 178.84(18) . . ? O3 Mg2 Mg1 114.94(14) 3 . ? O11 Mg2 Mg1 63.06(13) 3_465 . ? O8 Mg2 Mg1 109.91(13) 3_455 . ? O16 Mg2 Mg1 71.54(12) 3_565 . ? O9 Mg2 Mg1 144.48(13) . . ? O1 Mg2 Mg1 34.83(10) . . ? O3 Mg2 Mg3 66.31(13) 3 . ? O11 Mg2 Mg3 115.70(14) 3_465 . ? O8 Mg2 Mg3 69.92(12) 3_455 . ? O16 Mg2 Mg3 108.65(13) 3_565 . ? O9 Mg2 Mg3 34.56(10) . . ? O1 Mg2 Mg3 146.16(13) . . ? Mg1 Mg2 Mg3 178.74(7) . . ? O13 Mg3 O7 106.40(18) 2_664 3_455 ? O13 Mg3 O4 91.18(17) 2_664 3 ? O7 Mg3 O4 88.36(18) 3_455 3 ? O13 Mg3 O17 87.7(2) 2_664 . ? O7 Mg3 O17 84.9(2) 3_455 . ? O4 Mg3 O17 172.5(2) 3 . ? O13 Mg3 O10 98.73(17) 2_664 . ? O7 Mg3 O10 153.74(17) 3_455 . ? O4 Mg3 O10 98.81(17) 3 . ? O17 Mg3 O10 88.7(2) . . ? O13 Mg3 O9 158.51(18) 2_664 . ? O7 Mg3 O9 94.59(16) 3_455 . ? O4 Mg3 O9 94.04(16) 3 . ? O17 Mg3 O9 89.7(2) . . ? O10 Mg3 O9 59.88(14) . . ? O13 Mg3 C31 128.29(19) 2_664 . ? O7 Mg3 C31 124.44(18) 3_455 . ? O4 Mg3 C31 98.52(17) 3 . ? O17 Mg3 C31 88.0(2) . . ? O10 Mg3 C31 29.66(15) . . ? O9 Mg3 C31 30.25(15) . . ? O13 Mg3 Mg2 164.25(14) 2_664 . ? O7 Mg3 Mg2 69.25(12) 3_455 . ? O4 Mg3 Mg2 73.79(12) 3 . ? O17 Mg3 Mg2 106.58(17) . . ? O10 Mg3 Mg2 88.42(11) . . ? O9 Mg3 Mg2 32.44(11) . . ? C31 Mg3 Mg2 60.45(13) . . ? C6 C1 C2 119.5(5) . . ? C6 C1 C14 119.7(5) . . ? C2 C1 C14 120.8(5) . . ? C3 C2 C1 120.3(5) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 C15 121.3(5) . . ? C2 C3 C15 119.6(5) . . ? C3 C4 C5 121.4(5) . . ? C6 C5 C4 117.9(5) . . ? C6 C5 C7 119.5(5) . . ? C4 C5 C7 122.2(5) . . ? C1 C6 C5 121.7(5) . . ? C5 C7 C8 119.6(5) . . ? C13 C8 C9 118.3(5) . . ? C13 C8 C7 122.7(5) . . ? C9 C8 C7 119.0(5) . . ? C8 C9 C10 120.2(5) . . ? C11 C10 C9 119.9(5) . . ? C11 C10 C16 119.8(5) . . ? C9 C10 C16 120.2(5) . . ? C12 C11 C10 120.5(5) . . ? C11 C12 C13 119.3(5) . . ? C11 C12 C17 119.2(5) . . ? C13 C12 C17 121.5(5) . . ? C8 C13 C12 121.7(5) . . ? O1 C14 O2 117.6(5) . . ? O1 C14 C1 121.1(5) . . ? O2 C14 C1 121.3(5) . . ? O1 C14 Mg1 57.7(3) . . ? O2 C14 Mg1 59.9(3) . . ? C1 C14 Mg1 178.6(4) . . ? O4 C15 O3 125.6(5) . . ? O4 C15 C3 118.9(5) . . ? O3 C15 C3 115.5(5) . . ? O5 C16 O6 121.0(5) . . ? O5 C16 C10 121.0(5) . . ? O6 C16 C10 118.0(5) . . ? O5 C16 Mg1 65.3(3) . 2_654 ? O6 C16 Mg1 56.9(3) . 2_654 ? C10 C16 Mg1 167.1(5) . 2_654 ? O8 C17 O7 125.1(5) . . ? O8 C17 C12 117.8(5) . . ? O7 C17 C12 117.1(5) . . ? C19 C18 C23 119.1(5) . . ? C19 C18 C31 120.4(5) . . ? C23 C18 C31 120.5(5) . . ? C18 C19 C20 120.6(5) . . ? C19 C20 C21 120.6(5) . . ? C19 C20 C32 120.0(5) . . ? C21 C20 C32 119.4(5) . . ? C22 C21 C20 119.1(5) . . ? C23 C22 C21 119.8(5) . . ? C23 C22 C24 119.7(5) . . ? C21 C22 C24 120.3(5) . . ? C22 C23 C18 120.7(5) . . ? C25 C24 C22 115.9(4) . . ? C26 C25 C30 118.7(5) . . ? C26 C25 C24 121.9(5) . . ? C30 C25 C24 119.3(5) . . ? C25 C26 C27 121.0(5) . . ? C28 C27 C26 120.1(5) . . ? C28 C27 C33 120.5(5) . . ? C26 C27 C33 119.4(5) . . ? C27 C28 C29 120.2(5) . . ? C30 C29 C28 118.8(5) . . ? C30 C29 C34 120.8(5) . . ? C28 C29 C34 120.5(5) . . ? C29 C30 C25 121.1(5) . . ? O10 C31 O9 120.2(5) . . ? O10 C31 C18 120.1(5) . . ? O9 C31 C18 119.7(5) . . ? O10 C31 Mg3 59.1(3) . . ? O9 C31 Mg3 61.2(3) . . ? C18 C31 Mg3 175.3(4) . . ? O11 C32 O12 125.4(5) . . ? O11 C32 C20 116.7(5) . . ? O12 C32 C20 117.9(5) . . ? O13 C33 O14 125.1(5) . . ? O13 C33 C27 118.4(5) . . ? O14 C33 C27 116.6(5) . . ? O15 C34 O16 124.8(5) . . ? O15 C34 C29 117.6(4) . . ? O16 C34 C29 117.6(5) . . ? O17 C35 N1 122.4(8) . . ? C14 O1 Mg1 91.7(3) . . ? C14 O1 Mg2 144.6(3) . . ? Mg1 O1 Mg2 109.73(18) . . ? C14 O2 Mg1 89.2(3) . . ? C15 O3 Mg2 144.4(4) . 3_455 ? C15 O4 Mg3 127.9(4) . 3_455 ? C16 O5 Mg1 84.1(3) . 2_654 ? C16 O6 Mg1 92.2(3) . 2_654 ? C17 O7 Mg3 134.9(4) . 3 ? C17 O8 Mg2 134.2(4) . 3 ? C31 O9 Mg2 144.3(3) . . ? C31 O9 Mg3 88.6(3) . . ? Mg2 O9 Mg3 113.00(18) . . ? C31 O10 Mg3 91.2(3) . . ? C32 O11 Mg2 148.1(4) . 3_565 ? C32 O12 Mg1 120.6(4) . 3_565 ? C33 O13 Mg3 144.8(4) . 2_665 ? C34 O15 Mg1 134.6(4) . 3_465 ? C34 O16 Mg2 132.7(4) . 3_465 ? C35 O17 Mg3 136.9(6) . . ? C35 N1 C37 121.0(7) . . ? C35 N1 C36 121.4(7) . . ? C37 N1 C36 117.5(7) . . ? C39 N2 C38 116.7(6) . . ? O8W O5W O4W 56(3) 3_455 3_455 ? O8W O4W O5W 50(2) . 3 ? O5W O8W O4W 74(3) 3 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.174 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.120