# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Zhong-Min Su' 'Xinlong Wang' 'Haining Wang' _publ_contact_author_name 'Hai-Ning Wang' _publ_contact_author_email wanghn913@nenu.edu.cn data_1 _database_code_depnum_ccdc_archive 'CCDC 846618' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Mg3 N8 O24' _chemical_formula_sum 'C48 H66 Mg3 N8 O24' _chemical_formula_weight 1212.02 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 'Pnnm ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8470(17) _cell_length_b 14.8440(19) _cell_length_c 15.148(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2888.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 28.39 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9725 _exptl_absorpt_correction_T_max 0.9834 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16915 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.39 _reflns_number_total 3608 _reflns_number_gt 2395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.1154P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3608 _refine_ls_number_parameters 144 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1983 _refine_ls_wR_factor_gt 0.1873 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Mg2 Mg 0.44329(7) 0.76236(7) 1.0000 0.0162(3) Uani 1 2 d S . . O4 O 0.52884(14) 0.69490(12) 0.90546(12) 0.0353(5) Uani 1 1 d . . . O3 O 0.66320(16) 0.78325(13) 0.87087(15) 0.0490(6) Uani 1 1 d . . . C2 C 0.6594(2) 0.63433(16) 0.81359(17) 0.0295(6) Uani 1 1 d . . . C6 C 0.6738(2) 0.47519(17) 0.7842(2) 0.0406(7) Uani 1 1 d . . . C7 C 0.6310(2) 0.54653(17) 0.83202(19) 0.0376(7) Uani 1 1 d . . . H7 H 0.5830 0.5349 0.8766 0.045 Uiso 1 1 calc R . . C1 C 0.6138(2) 0.71019(17) 0.86717(17) 0.0317(6) Uani 1 1 d . . . C5 C 0.7446(2) 0.49359(17) 0.71776(18) 0.0344(6) Uani 1 1 d . . . H5 H 0.7742 0.4464 0.6861 0.041 Uiso 1 1 calc R . . C4 C 0.77207(18) 0.58153(16) 0.69787(16) 0.0270(5) Uani 1 1 d . . . C3 C 0.72936(19) 0.65206(16) 0.74594(16) 0.0286(6) Uani 1 1 d . . . H3A H 0.7476 0.7112 0.7328 0.034 Uiso 1 1 calc R . . C8 C 0.84867(18) 0.59860(16) 0.62463(15) 0.0245(5) Uani 1 1 d . . . O2 O 0.85858(15) 0.67731(12) 0.59850(13) 0.0407(5) Uani 1 1 d . . . O1 O 0.89596(17) 0.53228(13) 0.59514(15) 0.0494(6) Uani 1 1 d . . . O1W O 0.3353(2) 0.6574(2) 1.0000 0.0404(7) Uani 1 2 d SD . . N1 N 0.6476(2) 0.3861(2) 0.8052(2) 0.0667(9) Uiso 1 1 d . . . H1A H 0.6756 0.3422 0.7767 0.080 Uiso 1 1 calc R . . H1B H 0.6035 0.3753 0.8466 0.080 Uiso 1 1 calc R . . Mg1 Mg 1.0000 0.5000 0.5000 0.0153(3) Uani 1 4 d S . . O2W O 0.94004(17) 0.36731(15) 0.5000 0.0212(5) Uani 1 2 d SD . . H5A H 0.912(3) 0.346(2) 0.4542(15) 0.080(13) Uiso 1 1 d D . . H1A' H 0.305(4) 0.642(3) 0.9530(19) 0.14(2) 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 Mg2 0.0171(5) 0.0145(5) 0.0170(5) 0.000 0.000 0.0005(4) O4 0.0332(10) 0.0335(10) 0.0393(10) -0.0147(8) 0.0162(8) -0.0055(8) O3 0.0517(12) 0.0298(11) 0.0656(15) -0.0169(10) 0.0323(11) -0.0105(9) C2 0.0346(13) 0.0220(13) 0.0321(13) -0.0041(10) 0.0161(11) 0.0024(10) C6 0.0567(18) 0.0180(13) 0.0471(17) 0.0030(11) 0.0248(15) 0.0012(12) C7 0.0474(16) 0.0259(14) 0.0394(15) 0.0020(11) 0.0309(13) -0.0011(12) C1 0.0361(14) 0.0262(13) 0.0327(14) -0.0048(10) 0.0149(11) 0.0020(11) C5 0.0420(15) 0.0217(13) 0.0396(15) -0.0020(11) 0.0191(12) 0.0053(11) C4 0.0300(12) 0.0224(12) 0.0287(13) -0.0011(9) 0.0166(10) 0.0018(10) C3 0.0370(14) 0.0171(11) 0.0316(13) 0.0007(9) 0.0140(11) -0.0010(10) C8 0.0255(11) 0.0266(13) 0.0213(11) -0.0010(9) 0.0102(9) 0.0003(10) O2 0.0481(12) 0.0303(10) 0.0436(11) 0.0110(8) 0.0267(9) 0.0040(9) O1 0.0643(14) 0.0269(10) 0.0569(13) -0.0030(9) 0.0451(11) 0.0029(9) O1W 0.0406(16) 0.0400(17) 0.0406(17) 0.000 0.000 -0.0185(13) Mg1 0.0159(7) 0.0152(7) 0.0147(7) 0.000 0.000 0.0026(6) O2W 0.0229(12) 0.0157(11) 0.0251(12) 0.000 0.000 -0.0026(9) _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 Mg2 O2 2.0525(18) 3_466 ? Mg2 O2 2.0525(18) 8_576 ? Mg2 O4 2.0644(18) 6_557 ? Mg2 O4 2.0644(18) . ? Mg2 O1W 2.087(3) . ? Mg2 O2W 2.162(2) 7_766 ? Mg2 Mg1 3.6020(11) 3_466 ? O4 C1 1.257(3) . ? O3 C1 1.258(3) . ? C2 C7 1.382(3) . ? C2 C3 1.388(3) . ? C2 C1 1.507(3) . ? C6 C5 1.384(4) . ? C6 C7 1.396(4) . ? C6 N1 1.401(4) . ? C5 C4 1.385(3) . ? C4 C3 1.388(3) . ? C4 C8 1.504(3) . ? C8 O2 1.240(3) . ? C8 O1 1.240(3) . ? O2 Mg2 2.0525(18) 3_566 ? O1 Mg1 2.0231(18) . ? Mg1 O1 2.0231(18) 2_765 ? Mg1 O1 2.0231(18) 6_556 ? Mg1 O1 2.0231(18) 5_766 ? Mg1 O2W 2.115(2) . ? Mg1 O2W 2.115(2) 5_766 ? Mg1 Mg2 3.6020(11) 3_566 ? Mg1 Mg2 3.6020(11) 7_755 ? O2W Mg2 2.162(2) 7_755 ? 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 Mg2 O2 93.26(13) 3_466 8_576 ? O2 Mg2 O4 176.62(9) 3_466 6_557 ? O2 Mg2 O4 89.41(9) 8_576 6_557 ? O2 Mg2 O4 89.41(9) 3_466 . ? O2 Mg2 O4 176.62(9) 8_576 . ? O4 Mg2 O4 87.85(12) 6_557 . ? O2 Mg2 O1W 88.47(8) 3_466 . ? O2 Mg2 O1W 88.47(8) 8_576 . ? O4 Mg2 O1W 89.52(9) 6_557 . ? O4 Mg2 O1W 89.52(9) . . ? O2 Mg2 O2W 93.05(7) 3_466 7_766 ? O2 Mg2 O2W 93.05(7) 8_576 7_766 ? O4 Mg2 O2W 88.88(7) 6_557 7_766 ? O4 Mg2 O2W 88.88(7) . 7_766 ? O1W Mg2 O2W 177.78(12) . 7_766 ? O2 Mg2 Mg1 71.33(6) 3_466 3_466 ? O2 Mg2 Mg1 71.33(6) 8_576 3_466 ? O4 Mg2 Mg1 111.56(6) 6_557 3_466 ? O4 Mg2 Mg1 111.56(6) . 3_466 ? O1W Mg2 Mg1 149.99(10) . 3_466 ? O2W Mg2 Mg1 32.23(6) 7_766 3_466 ? C1 O4 Mg2 134.03(17) . . ? C7 C2 C3 119.9(2) . . ? C7 C2 C1 119.5(2) . . ? C3 C2 C1 120.5(2) . . ? C5 C6 C7 119.1(2) . . ? C5 C6 N1 120.6(3) . . ? C7 C6 N1 120.2(3) . . ? C2 C7 C6 120.4(2) . . ? O4 C1 O3 125.0(2) . . ? O4 C1 C2 116.9(2) . . ? O3 C1 C2 118.2(2) . . ? C6 C5 C4 120.8(2) . . ? C5 C4 C3 119.7(2) . . ? C5 C4 C8 119.1(2) . . ? C3 C4 C8 121.2(2) . . ? C2 C3 C4 120.0(2) . . ? O2 C8 O1 125.6(2) . . ? O2 C8 C4 117.5(2) . . ? O1 C8 C4 116.9(2) . . ? C8 O2 Mg2 134.23(16) . 3_566 ? C8 O1 Mg1 140.20(17) . . ? O1 Mg1 O1 180.0 2_765 6_556 ? O1 Mg1 O1 89.15(15) 2_765 . ? O1 Mg1 O1 90.85(15) 6_556 . ? O1 Mg1 O1 90.85(15) 2_765 5_766 ? O1 Mg1 O1 89.15(14) 6_556 5_766 ? O1 Mg1 O1 180.0 . 5_766 ? O1 Mg1 O2W 91.15(7) 2_765 . ? O1 Mg1 O2W 88.85(7) 6_556 . ? O1 Mg1 O2W 88.85(7) . . ? O1 Mg1 O2W 91.15(7) 5_766 . ? O1 Mg1 O2W 88.85(7) 2_765 5_766 ? O1 Mg1 O2W 91.15(7) 6_556 5_766 ? O1 Mg1 O2W 91.15(7) . 5_766 ? O1 Mg1 O2W 88.85(7) 5_766 5_766 ? O2W Mg1 O2W 180.0 . 5_766 ? O1 Mg1 Mg2 111.44(6) 2_765 3_566 ? O1 Mg1 Mg2 68.56(6) 6_556 3_566 ? O1 Mg1 Mg2 68.56(6) . 3_566 ? O1 Mg1 Mg2 111.44(6) 5_766 3_566 ? O2W Mg1 Mg2 146.97(6) . 3_566 ? O2W Mg1 Mg2 33.03(6) 5_766 3_566 ? O1 Mg1 Mg2 68.56(6) 2_765 7_755 ? O1 Mg1 Mg2 111.44(6) 6_556 7_755 ? O1 Mg1 Mg2 111.44(6) . 7_755 ? O1 Mg1 Mg2 68.56(6) 5_766 7_755 ? O2W Mg1 Mg2 33.03(6) . 7_755 ? O2W Mg1 Mg2 146.97(6) 5_766 7_755 ? Mg2 Mg1 Mg2 180.0 3_566 7_755 ? Mg1 O2W Mg2 114.75(10) . 7_755 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.404 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.068 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.008 0.000 666.6 178.9 2 0.500 0.917 0.500 666.6 178.9 _platon_squeeze_details ; ; # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 846619' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Mg3 N8 O24' _chemical_formula_sum 'C48 H66 Mg3 N8 O24' _chemical_formula_weight 1211.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Mg Mg 0.0490 0.0360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 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 P21/c 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 14.4840(14) _cell_length_b 13.3890(13) _cell_length_c 20.3730(14) _cell_angle_alpha 90.00 _cell_angle_beta 133.800(14) _cell_angle_gamma 90.00 _cell_volume 2851.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14184 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.07 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9694 _exptl_absorpt_correction_T_max 0.9776 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14184 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.07 _reflns_number_total 5047 _reflns_number_gt 3854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0634P)^2^+3.3424P] 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 5047 _refine_ls_number_parameters 390 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.065 _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 Mg1 Mg 0.0000 -1.0000 0.0000 0.01270(12) Uani 1 2 d S . . Mg2 Mg 0.24819(2) -0.94059(2) 0.006088(16) 0.01380(9) Uani 1 1 d . . . O1 O 0.26868(5) -0.85797(6) 0.09905(4) 0.0270(2) Uani 1 1 d . . . O1W O 0.35891(5) -0.83688(6) 0.00934(4) 0.0286(2) Uani 1 1 d . . . H1W H 0.4184 -0.8264 0.0637 0.043 Uiso 1 1 d R . . H2W H 0.3403 -0.7880 -0.0197 0.043 Uiso 1 1 d R . . O2 O 0.11794(5) -0.89435(6) 0.09880(4) 0.0290(2) Uani 1 1 d . . . O11 O 0.14759(5) -1.05313(5) 0.01120(3) 0.01663(19) Uani 1 1 d D . . O3 O 0.63149(5) -0.64418(7) 0.34963(5) 0.0395(3) Uani 1 1 d . . . O4 O 0.58090(5) -0.51608(6) 0.39006(4) 0.0237(2) Uani 1 1 d . . . O5 O 0.08830(5) -0.86323(6) -0.10596(4) 0.0232(2) Uani 1 1 d . . . O6 O -0.05039(5) -0.90334(6) -0.09577(4) 0.0299(2) Uani 1 1 d . . . O7 O -0.09209(5) -0.64568(6) -0.37504(4) 0.0382(2) Uani 1 1 d . . . H7 H -0.0895 -0.6111 -0.4070 0.057 Uiso 1 1 calc R . . O8 O -0.23087(5) -0.52858(5) -0.41258(4) 0.0210(2) Uani 1 1 d . . . N1 N 0.16412(6) -0.62383(7) 0.29402(5) 0.0264(3) Uani 1 1 d . . . H1A H 0.1954 -0.5738 0.3327 0.032 Uiso 1 1 d R . . H1B H 0.0895 -0.6052 0.2440 0.032 Uiso 1 1 d R . . N2 N -0.42347(6) -0.67638(8) -0.29969(5) 0.0347(3) Uani 1 1 d . . . H2A H -0.4194 -0.7101 -0.2605 0.042 Uiso 1 1 d R . . H2B H -0.4491 -0.6115 -0.3096 0.042 Uiso 1 1 d R . . C1 C 0.21216(7) -0.84613(8) 0.12465(5) 0.0198(3) Uani 1 1 d . . . C2 C 0.26340(7) -0.76470(8) 0.19423(5) 0.0200(3) Uani 1 1 d . . . C3 C 0.19352(7) -0.73382(8) 0.21435(5) 0.0218(3) Uani 1 1 d . . . H3 H 0.1157 -0.7637 0.1863 0.026 Uiso 1 1 calc R . . C4 C 0.24173(7) -0.65817(8) 0.27665(5) 0.0206(3) Uani 1 1 d . . . C5 C 0.35831(7) -0.61410(8) 0.32167(5) 0.0219(3) Uani 1 1 d . . . H5 H 0.3894 -0.5643 0.3645 0.026 Uiso 1 1 calc R . . C6 C 0.42916(7) -0.64512(8) 0.30228(5) 0.0214(3) Uani 1 1 d . . . C7 C 0.55759(7) -0.59826(8) 0.35086(5) 0.0216(3) Uani 1 1 d . . . C8 C 0.38004(7) -0.71990(8) 0.23804(5) 0.0225(3) Uani 1 1 d . . . H8 H 0.4263 -0.7403 0.2242 0.027 Uiso 1 1 calc R . . C9 C -0.01758(7) -0.85493(8) -0.12881(5) 0.0186(3) Uani 1 1 d . . . C10 C -0.11350(7) -0.78077(8) -0.20163(5) 0.0191(3) Uani 1 1 d . . . C11 C -0.09565(7) -0.73005(8) -0.25148(5) 0.0210(3) Uani 1 1 d . . . H11 H -0.0230 -0.7422 -0.2409 0.025 Uiso 1 1 calc R . . C12 C -0.18587(7) -0.66120(8) -0.31716(5) 0.0199(3) Uani 1 1 d . . . C13 C -0.16754(7) -0.60859(8) -0.37247(5) 0.0205(3) Uani 1 1 d . . . C14 C -0.29393(7) -0.64283(8) -0.33255(6) 0.0224(3) Uani 1 1 d . . . H14 H -0.3546 -0.5970 -0.3768 0.027 Uiso 1 1 calc R . . C15 C -0.31205(7) -0.69227(9) -0.28237(6) 0.0228(3) Uani 1 1 d . . . C16 C -0.22209(7) -0.76210(8) -0.21766(6) 0.0235(3) Uani 1 1 d . . . H16 H -0.2347 -0.7967 -0.1848 0.028 Uiso 1 1 calc R . . O9 O -0.29233(11) -0.17199(9) -0.40944(7) 0.0925(5) Uani 1 1 d . . . N3 N -0.39021(19) -0.07634(17) -0.38584(11) 0.1885(9) Uani 1 1 d . . . C17 C -0.5199(2) -0.1591(2) -0.46914(15) 0.1263(14) Uani 1 1 d . . . H17A H -0.5976 -0.1214 -0.5113 0.190 Uiso 1 1 calc R . . H17B H -0.5290 -0.2078 -0.4394 0.190 Uiso 1 1 calc R . . H17C H -0.5023 -0.1924 -0.5013 0.190 Uiso 1 1 calc R . . C18 C -0.4221(2) -0.00912(19) -0.35039(14) 0.1486(11) Uani 1 1 d . . . H18A H -0.4610 0.0495 -0.3879 0.223 Uiso 1 1 calc R . . H18B H -0.3460 0.0093 -0.2895 0.223 Uiso 1 1 calc R . . H18C H -0.4810 -0.0407 -0.3498 0.223 Uiso 1 1 calc R . . C19 C -0.3272(2) -0.11198(18) -0.38663(12) 0.1597(9) Uani 1 1 d . . . C20 C -0.19636(18) -0.02934(15) -0.30426(11) 0.0925(9) Uani 1 1 d . . . H20A H -0.1285 -0.0405 -0.3017 0.139 Uiso 1 1 calc R . . H20B H -0.1658 -0.0420 -0.2456 0.139 Uiso 1 1 calc R . . H20C H -0.2249 0.0386 -0.3215 0.139 Uiso 1 1 calc R . . O10 O 0.03911(10) -0.05021(11) -0.62833(6) 0.0851(5) Uani 1 1 d . . . N4 N 0.14855(18) 0.0023(2) -0.49129(11) 0.1389(11) Uani 1 1 d . . . C21 C 0.2231(3) -0.0045(2) -0.39397(12) 0.1510(16) Uani 1 1 d . . . H21A H 0.3122 0.0040 -0.3599 0.227 Uiso 1 1 calc R . . H21B H 0.2099 -0.0688 -0.3807 0.227 Uiso 1 1 calc R . . H21C H 0.1960 0.0467 -0.3774 0.227 Uiso 1 1 calc R . . C22 C 0.1169(2) 0.11102(16) -0.53084(15) 0.1332(14) Uani 1 1 d . . . H22A H 0.1934 0.1507 -0.4926 0.200 Uiso 1 1 calc R . . H22B H 0.0544 0.1403 -0.5330 0.200 Uiso 1 1 calc R . . H22C H 0.0836 0.1085 -0.5911 0.200 Uiso 1 1 calc R . . C23 C 0.10522(16) -0.0555(2) -0.54847(11) 0.1055(10) Uani 1 1 d . . . C24 C 0.1473(2) -0.16943(15) -0.50185(15) 0.1325(15) Uani 1 1 d . . . H24A H 0.1380 -0.2163 -0.5418 0.199 Uiso 1 1 calc R . . H24B H 0.0934 -0.1889 -0.4925 0.199 Uiso 1 1 calc R . . H24C H 0.2349 -0.1684 -0.4445 0.199 Uiso 1 1 calc R . . H11B H 0.2113(8) -1.0807(6) 0.0607(2) 0.071(5) Uiso 1 1 d D . . H11A H 0.1243(7) -1.0916(5) -0.0300(2) 0.055(4) 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 Mg1 0.01352(11) 0.0121(2) 0.01269(11) -0.00011(13) 0.00916(8) -0.00124(14) Mg2 0.01377(8) 0.01457(16) 0.01377(8) -0.00016(9) 0.00980(5) 0.00022(10) O1 0.02892(19) 0.0305(4) 0.0313(2) -0.0152(2) 0.02451(13) -0.0100(2) O1W 0.0266(2) 0.0290(4) 0.0264(2) 0.0024(3) 0.01696(15) -0.0061(3) O2 0.02663(19) 0.0332(4) 0.0336(2) -0.0196(2) 0.02323(14) -0.0168(3) O11 0.01755(17) 0.0171(3) 0.01692(17) -0.0001(2) 0.01256(12) 0.0009(2) O3 0.0239(2) 0.0437(5) 0.0537(3) -0.0267(3) 0.02785(16) -0.0121(3) O4 0.01681(19) 0.0224(4) 0.0244(2) -0.0073(2) 0.01140(14) -0.0051(2) O5 0.01850(18) 0.0272(4) 0.0234(2) 0.0102(2) 0.01434(13) 0.0081(2) O6 0.0286(2) 0.0341(4) 0.0327(2) 0.0204(2) 0.02337(14) 0.0115(3) O7 0.0504(2) 0.0420(5) 0.0502(2) 0.0276(3) 0.04530(14) 0.0238(3) O8 0.02784(19) 0.0173(3) 0.02256(19) 0.0071(2) 0.01922(13) 0.0060(2) N1 0.0211(2) 0.0360(5) 0.0255(2) -0.0113(3) 0.01743(16) -0.0033(3) N2 0.0240(2) 0.0461(6) 0.0405(3) 0.0167(3) 0.02478(18) 0.0126(3) C1 0.0195(3) 0.0204(5) 0.0191(3) -0.0034(3) 0.01317(18) -0.0006(3) C2 0.0191(3) 0.0222(5) 0.0207(3) -0.0065(3) 0.01453(17) -0.0036(3) C3 0.0203(3) 0.0233(5) 0.0254(3) -0.0070(3) 0.01715(18) -0.0058(3) C4 0.0215(3) 0.0229(5) 0.0229(3) -0.0056(3) 0.01749(17) -0.0015(3) C5 0.0228(3) 0.0209(5) 0.0217(3) -0.0089(3) 0.01525(19) -0.0048(3) C6 0.0174(3) 0.0239(5) 0.0208(3) -0.0052(3) 0.01248(18) -0.0035(3) C7 0.0172(3) 0.0271(6) 0.0191(3) -0.0047(3) 0.01208(18) -0.0045(3) C8 0.0203(3) 0.0262(6) 0.0249(3) -0.0078(3) 0.01707(18) -0.0037(3) C9 0.0202(3) 0.0201(5) 0.0173(3) 0.0030(3) 0.01360(17) 0.0032(3) C10 0.0177(3) 0.0204(5) 0.0186(3) 0.0040(3) 0.01242(18) 0.0030(3) C11 0.0197(2) 0.0234(5) 0.0252(3) 0.0070(3) 0.01756(17) 0.0066(3) C12 0.0224(3) 0.0193(5) 0.0205(3) 0.0041(3) 0.01574(18) 0.0024(3) C13 0.0222(3) 0.0225(5) 0.0202(3) 0.0034(3) 0.01601(18) 0.0020(3) C14 0.0213(3) 0.0213(5) 0.0234(3) 0.0090(3) 0.01506(19) 0.0081(3) C15 0.0182(3) 0.0269(6) 0.0255(3) 0.0045(3) 0.01593(18) 0.0037(3) C16 0.0222(3) 0.0281(6) 0.0245(3) 0.0079(3) 0.01782(18) 0.0027(3) O9 0.1630(6) 0.0506(7) 0.0919(4) -0.0251(4) 0.0987(3) -0.0152(6) N3 0.3582(11) 0.1277(13) 0.1983(7) 0.1065(8) 0.2372(6) 0.1494(10) C17 0.1190(13) 0.1106(19) 0.1001(12) 0.0155(13) 0.0573(9) -0.0066(14) C18 0.2308(11) 0.1096(17) 0.1779(11) 0.0509(11) 0.1687(7) 0.0862(12) C19 0.3374(11) 0.0848(13) 0.1775(7) 0.0795(8) 0.2236(6) 0.1090(11) C20 0.1339(10) 0.0564(11) 0.0693(7) -0.0150(7) 0.0636(6) -0.0080(10) O10 0.0768(5) 0.1124(10) 0.0328(4) -0.0152(5) 0.0253(3) -0.0257(6) N4 0.1245(11) 0.190(2) 0.0605(7) -0.0357(11) 0.0485(6) -0.0167(14) C21 0.212(2) 0.1007(19) 0.0453(8) -0.0149(10) 0.0530(10) -0.0063(17) C22 0.1967(17) 0.0497(12) 0.1141(12) 0.0310(10) 0.0928(10) 0.0285(13) C23 0.0616(7) 0.176(2) 0.0562(7) -0.0386(11) 0.0320(5) -0.0178(12) C24 0.1752(17) 0.0434(11) 0.1098(13) 0.0007(10) 0.0726(11) 0.0221(12) _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 O6 2.0107(8) . ? Mg1 O6 2.0107(8) 3_535 ? Mg1 O2 2.0520(7) 3_535 ? Mg1 O2 2.0520(7) . ? Mg1 O11 2.1102(8) . ? Mg1 O11 2.1102(8) 3_535 ? Mg2 O1 2.0298(9) . ? Mg2 O5 2.0805(7) . ? Mg2 O1W 2.0875(9) . ? Mg2 O4 2.0919(7) 2_645 ? Mg2 O8 2.1021(9) 2_544 ? Mg2 O11 2.1480(8) . ? O1 C1 1.2485(16) . ? O1W H1W 0.8170 . ? O1W H2W 0.7934 . ? O2 C1 1.2497(13) . ? O11 H11B 0.847(5) . ? O11 H11A 0.831(5) . ? O3 C7 1.2496(15) . ? O4 C7 1.2606(13) . ? O4 Mg2 2.0919(7) 2_655 ? O5 C9 1.2620(13) . ? O6 C9 1.2418(15) . ? O7 C13 1.2340(15) . ? O7 H7 0.8200 . ? O8 C13 1.2724(12) . ? O8 Mg2 2.1021(9) 2_554 ? N1 C4 1.4666(16) . ? N1 H1A 0.8835 . ? N1 H1B 0.8630 . ? N2 C15 1.4091(15) . ? N2 H2A 0.8833 . ? N2 H2B 0.9102 . ? C1 C2 1.5141(14) . ? C2 C8 1.3869(13) . ? C2 C3 1.3921(18) . ? C3 C4 1.3774(14) . ? C3 H3 0.9300 . ? C4 C5 1.3772(13) . ? C5 C6 1.3940(18) . ? C5 H5 0.9300 . ? C6 C8 1.3901(15) . ? C6 C7 1.5115(13) . ? C8 H8 0.9300 . ? C9 C10 1.5046(12) . ? C10 C11 1.3866(17) . ? C10 C16 1.3900(16) . ? C11 C12 1.3883(12) . ? C11 H11 0.9300 . ? C12 C14 1.3889(16) . ? C12 C13 1.5003(17) . ? C14 C15 1.3870(18) . ? C14 H14 0.9300 . ? C15 C16 1.3900(13) . ? C16 H16 0.9300 . ? O9 C19 1.201(3) . ? N3 C19 1.039(4) . ? N3 C18 1.417(4) . ? N3 C17 1.796(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.797(3) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O10 C23 1.189(2) . ? N4 C23 1.156(3) . ? N4 C21 1.463(3) . ? N4 C22 1.571(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.673(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mg1 O6 180.0 . 3_535 ? O6 Mg1 O2 89.73(3) . 3_535 ? O6 Mg1 O2 90.27(3) 3_535 3_535 ? O6 Mg1 O2 90.27(3) . . ? O6 Mg1 O2 89.73(3) 3_535 . ? O2 Mg1 O2 180.0 3_535 . ? O6 Mg1 O11 88.97(3) . . ? O6 Mg1 O11 91.03(3) 3_535 . ? O2 Mg1 O11 88.11(3) 3_535 . ? O2 Mg1 O11 91.89(3) . . ? O6 Mg1 O11 91.03(3) . 3_535 ? O6 Mg1 O11 88.97(3) 3_535 3_535 ? O2 Mg1 O11 91.89(3) 3_535 3_535 ? O2 Mg1 O11 88.11(3) . 3_535 ? O11 Mg1 O11 180.00(3) . 3_535 ? O1 Mg2 O5 94.90(3) . . ? O1 Mg2 O1W 89.71(4) . . ? O5 Mg2 O1W 87.19(3) . . ? O1 Mg2 O4 90.75(3) . 2_645 ? O5 Mg2 O4 171.72(4) . 2_645 ? O1W Mg2 O4 86.79(3) . 2_645 ? O1 Mg2 O8 178.50(3) . 2_544 ? O5 Mg2 O8 86.60(3) . 2_544 ? O1W Mg2 O8 90.50(4) . 2_544 ? O4 Mg2 O8 87.78(3) 2_645 2_544 ? O1 Mg2 O11 90.18(3) . . ? O5 Mg2 O11 97.19(3) . . ? O1W Mg2 O11 175.61(2) . . ? O4 Mg2 O11 88.83(3) 2_645 . ? O8 Mg2 O11 89.50(3) 2_544 . ? C1 O1 Mg2 138.10(6) . . ? Mg2 O1W H1W 102.9 . . ? Mg2 O1W H2W 131.9 . . ? H1W O1W H2W 111.3 . . ? C1 O2 Mg1 133.98(8) . . ? Mg1 O11 Mg2 115.38(3) . . ? Mg1 O11 H11B 117.6(8) . . ? Mg2 O11 H11B 98.5(7) . . ? Mg1 O11 H11A 115.2(6) . . ? Mg2 O11 H11A 101.6(7) . . ? H11B O11 H11A 106.2(7) . . ? C7 O4 Mg2 132.30(6) . 2_655 ? C9 O5 Mg2 126.45(7) . . ? C9 O6 Mg1 147.55(6) . . ? C13 O7 H7 109.5 . . ? C13 O8 Mg2 129.39(8) . 2_554 ? C4 N1 H1A 116.6 . . ? C4 N1 H1B 110.4 . . ? H1A N1 H1B 106.5 . . ? C15 N2 H2A 110.4 . . ? C15 N2 H2B 114.8 . . ? H2A N2 H2B 116.8 . . ? O1 C1 O2 126.79(10) . . ? O1 C1 C2 116.39(9) . . ? O2 C1 C2 116.82(11) . . ? C8 C2 C3 119.48(10) . . ? C8 C2 C1 120.22(11) . . ? C3 C2 C1 120.30(8) . . ? C4 C3 C2 118.78(9) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 122.32(11) . . ? C5 C4 N1 119.74(9) . . ? C3 C4 N1 117.93(9) . . ? C4 C5 C6 119.16(10) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C8 C6 C5 118.94(9) . . ? C8 C6 C7 120.76(11) . . ? C5 C6 C7 120.30(9) . . ? O3 C7 O4 125.77(9) . . ? O3 C7 C6 117.75(10) . . ? O4 C7 C6 116.47(10) . . ? C2 C8 C6 121.27(12) . . ? C2 C8 H8 119.4 . . ? C6 C8 H8 119.4 . . ? O6 C9 O5 125.27(8) . . ? O6 C9 C10 116.12(9) . . ? O5 C9 C10 118.61(10) . . ? C11 C10 C16 119.61(8) . . ? C11 C10 C9 122.17(10) . . ? C16 C10 C9 118.22(11) . . ? C10 C11 C12 120.19(10) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C14 119.80(11) . . ? C11 C12 C13 119.86(10) . . ? C14 C12 C13 120.32(8) . . ? O7 C13 O8 125.29(11) . . ? O7 C13 C12 117.72(9) . . ? O8 C13 C12 116.99(10) . . ? C15 C14 C12 120.51(8) . . ? C15 C14 H14 119.7 . . ? C12 C14 H14 119.7 . . ? C14 C15 C16 119.25(11) . . ? C14 C15 N2 120.76(8) . . ? C16 C15 N2 119.89(11) . . ? C10 C16 C15 120.62(11) . . ? C10 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C19 N3 C18 154.0(2) . . ? C19 N3 C17 93.3(2) . . ? C18 N3 C17 112.1(2) . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 O9 157.2(2) . . ? N3 C19 C20 94.2(2) . . ? O9 C19 C20 108.6(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 N4 C21 134.5(3) . . ? C23 N4 C22 109.9(2) . . ? C21 N4 C22 115.6(2) . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 O10 134.5(3) . . ? N4 C23 C24 107.9(2) . . ? O10 C23 C24 117.6(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.865 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.087 data_3 _database_code_depnum_ccdc_archive 'CCDC 846620' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Mg3 N8 O24' _chemical_formula_sum 'C48 H66 Mg3 N8 O24' _chemical_formula_weight 1211.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Mg Mg 0.0490 0.0360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.706(4) _cell_length_b 14.974(3) _cell_length_c 19.760(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5830.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27641 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2551 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9714 _exptl_absorpt_correction_T_max 0.9795 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; The crystal was small and weakly scattering, which led to the high Rint, and many kinds of restrict commands we used lead to the high R1 and wR2. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27641 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5125 _reflns_number_gt 3265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; The 'DFIX' command was used to bind o1w, o2w and hydeogen atoms respectively. The 'OMIT' order was used to confirm the data completeless. Due to high levels of disorder about the solvent, we removed the electronic contribution of the unidentified solvent with SQUEEZE. About 4 DMA molecules were removed by this process. 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^)+(0.0812P)^2^+47.6865P] 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 SHELXL _refine_ls_extinction_coef 0.00069(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5125 _refine_ls_number_parameters 280 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.1199 _refine_ls_wR_factor_ref 0.2962 _refine_ls_wR_factor_gt 0.2767 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.005 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 0.5000 0.5000 0.0000 0.0204(6) Uani 1 2 d S . . Mg2 Mg 0.47417(10) 0.26455(12) 0.02532(10) 0.0229(5) Uani 1 1 d . . . O1 O 0.4024(2) 0.4683(3) -0.0140(3) 0.0615(17) Uani 1 1 d . . . O2W O 0.4232(3) 0.1620(4) 0.0747(4) 0.0573(16) Uani 1 1 d D . . O2 O 0.3833(2) 0.3258(3) 0.0092(3) 0.0497(14) Uani 1 1 d . . . O3 O 0.4930(4) 0.4689(3) 0.0995(2) 0.0674(19) Uani 1 1 d . . . O4 O 0.4870(3) 0.3232(3) 0.1174(2) 0.0490(14) Uani 1 1 d . . . O5 O 0.0647(2) 0.3041(3) -0.0378(3) 0.0430(12) Uani 1 1 d . . . O6 O 0.1450(3) 0.2132(3) 0.0015(4) 0.085(2) Uani 1 1 d . . . O7 O 0.5096(4) 0.2157(3) 0.3560(3) 0.074(2) Uani 1 1 d . . . H7 H 0.5089 0.1792 0.3868 0.111 Uiso 1 1 calc R . . O8 O 0.4633(3) 0.3037(3) 0.4352(2) 0.0408(12) Uani 1 1 d . . . N1 N 0.1733(5) 0.6095(6) -0.0387(5) 0.090(3) Uiso 1 1 d . . . H1A H 0.2016 0.6532 -0.0399 0.107 Uiso 1 1 calc R . . H1B H 0.1306 0.6195 -0.0433 0.107 Uiso 1 1 calc R . . N2 N 0.4686(7) 0.6100(4) 0.3281(4) 0.127(5) Uani 1 1 d . . . H2A H 0.4676 0.6541 0.3002 0.153 Uiso 1 1 calc R . . H2B H 0.4659 0.6197 0.3709 0.153 Uiso 1 1 calc R . . C10 C 0.4850(5) 0.4190(4) 0.2119(3) 0.054(2) Uani 1 1 d . . . C2 C 0.2888(3) 0.4177(4) -0.0125(5) 0.060(3) Uani 1 1 d . . . C7 C 0.1969(4) 0.5217(5) -0.0292(6) 0.076(3) Uani 1 1 d . . . C8 C 0.2645(4) 0.5058(5) -0.0220(6) 0.079(3) Uani 1 1 d . . . H8 H 0.2950 0.5532 -0.0232 0.095 Uiso 1 1 calc R . . C12 C 0.4821(5) 0.3646(4) 0.3265(3) 0.048(2) Uani 1 1 d . . . C13 C 0.4848(4) 0.2891(4) 0.3765(4) 0.0451(19) Uani 1 1 d . . . C4 C 0.1738(4) 0.3637(5) -0.0176(5) 0.054(2) Uani 1 1 d . . . C15 C 0.4746(6) 0.5223(5) 0.3037(4) 0.075(3) Uani 1 1 d . . . C1 C 0.3630(3) 0.4031(4) -0.0061(4) 0.0459(19) Uani 1 1 d . . . C3 C 0.2430(4) 0.3476(4) -0.0129(5) 0.064(3) Uani 1 1 d . . . H3 H 0.2587 0.2892 -0.0098 0.077 Uiso 1 1 calc R . . C6 C 0.1514(4) 0.4513(5) -0.0278(6) 0.080(3) Uani 1 1 d . . . H6 H 0.1053 0.4624 -0.0337 0.096 Uiso 1 1 calc R . . C14 C 0.4756(5) 0.4507(5) 0.3503(4) 0.063(3) Uani 1 1 d . . . H14 H 0.4719 0.4616 0.3965 0.075 Uiso 1 1 calc R . . C11 C 0.4868(5) 0.3484(4) 0.2574(4) 0.055(2) Uani 1 1 d . . . H11 H 0.4912 0.2902 0.2416 0.066 Uiso 1 1 calc R . . C16 C 0.4790(6) 0.5051(5) 0.2356(4) 0.076(3) Uani 1 1 d . . . H16 H 0.4779 0.5523 0.2051 0.091 Uiso 1 1 calc R . . C9 C 0.4890(4) 0.4023(4) 0.1365(3) 0.0439(19) Uani 1 1 d . . . C5 C 0.1243(4) 0.2881(4) -0.0188(5) 0.052(2) Uani 1 1 d . . . O1W O 0.5296(2) 0.3686(3) -0.0259(2) 0.0269(10) Uani 1 1 d D . . H1W1 H 0.515(4) 0.342(5) -0.060(3) 0.07(3) Uiso 1 1 d D . . H1W2 H 0.556(10) 0.337(9) -0.003(8) 0.36(14) Uiso 1 1 d D . . H2W1 H 0.436(4) 0.139(5) 0.111(2) 0.07(3) Uiso 1 1 d D . . H2W2 H 0.431(11) 0.132(9) 0.042(3) 0.29(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 Mg1 0.0213(13) 0.0176(12) 0.0223(14) 0.0023(11) 0.0030(12) -0.0012(11) Mg2 0.0290(10) 0.0165(9) 0.0231(10) -0.0009(8) 0.0032(9) -0.0011(8) O1 0.031(3) 0.029(3) 0.124(5) -0.001(3) -0.007(3) -0.008(2) O2W 0.067(4) 0.041(3) 0.064(4) 0.012(3) 0.020(4) -0.015(3) O2 0.031(3) 0.035(3) 0.083(4) -0.001(3) -0.003(3) 0.004(2) O3 0.152(6) 0.026(2) 0.024(3) 0.004(2) 0.002(3) -0.009(3) O4 0.095(4) 0.026(2) 0.026(3) -0.0026(19) -0.002(3) 0.003(3) O5 0.030(3) 0.036(3) 0.063(3) 0.007(2) -0.005(2) -0.007(2) O6 0.038(3) 0.033(3) 0.184(8) 0.026(4) -0.001(4) -0.005(2) O7 0.149(6) 0.033(3) 0.041(3) 0.014(2) 0.023(4) 0.025(3) O8 0.052(3) 0.040(3) 0.030(3) 0.009(2) 0.004(2) 0.017(2) N2 0.323(16) 0.022(3) 0.037(4) -0.005(3) -0.017(7) -0.011(6) C10 0.116(8) 0.022(3) 0.024(4) 0.003(3) -0.002(4) -0.001(4) C2 0.021(3) 0.021(3) 0.137(9) -0.008(4) 0.000(4) 0.004(3) C7 0.032(4) 0.019(4) 0.176(11) -0.011(5) 0.004(5) 0.009(3) C8 0.035(5) 0.021(4) 0.180(11) 0.001(5) -0.004(5) 0.004(3) C12 0.094(6) 0.029(3) 0.021(4) 0.001(3) 0.002(4) -0.001(4) C13 0.073(6) 0.030(4) 0.032(4) 0.003(3) 0.005(4) 0.001(4) C4 0.022(3) 0.031(4) 0.108(7) 0.008(4) -0.003(4) -0.003(3) C15 0.159(10) 0.031(4) 0.034(4) 0.001(3) -0.009(5) 0.004(5) C1 0.033(4) 0.023(3) 0.081(6) 0.000(4) 0.002(4) 0.000(3) C3 0.043(4) 0.015(3) 0.135(9) -0.007(4) 0.002(5) -0.002(3) C6 0.038(5) 0.024(4) 0.178(11) -0.002(5) 0.011(6) 0.003(3) C14 0.128(8) 0.036(4) 0.025(4) 0.001(3) -0.012(5) 0.001(5) C11 0.118(8) 0.022(3) 0.025(4) -0.004(3) 0.003(4) 0.006(4) C16 0.176(11) 0.024(4) 0.028(4) 0.002(3) -0.001(5) 0.006(5) C9 0.078(6) 0.030(4) 0.024(4) 0.000(3) 0.004(4) -0.005(4) C5 0.038(4) 0.021(3) 0.097(7) 0.000(4) 0.014(4) 0.000(3) O1W 0.028(2) 0.020(2) 0.033(3) -0.0029(19) 0.006(2) -0.0004(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 2.000(5) . ? Mg1 O1 2.000(5) 5_665 ? Mg1 O3 2.025(5) 5_665 ? Mg1 O3 2.025(5) . ? Mg1 O1W 2.116(4) . ? Mg1 O1W 2.116(4) 5_665 ? Mg2 O2 2.037(5) . ? Mg2 O4 2.037(5) . ? Mg2 O8 2.064(5) 8_565 ? Mg2 O2W 2.079(6) . ? Mg2 O5 2.073(5) 3 ? Mg2 O1W 2.156(4) . ? O1 C1 1.256(8) . ? O2W H2W1 0.84(2) . ? O2W H2W2 0.80(2) . ? O2 C1 1.261(8) . ? O3 C9 1.240(8) . ? O4 C9 1.243(8) . ? O5 C5 1.256(9) . ? O5 Mg2 2.073(5) 3_455 ? O6 C5 1.260(8) . ? O7 C13 1.270(8) . ? O7 H7 0.8200 . ? O8 C13 1.253(8) . ? O8 Mg2 2.064(5) 8_566 ? N1 C7 1.408(11) . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N2 C15 1.404(10) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? C10 C16 1.377(10) . ? C10 C11 1.388(9) . ? C10 C9 1.512(10) . ? C2 C3 1.385(10) . ? C2 C8 1.416(10) . ? C2 C1 1.484(9) . ? C7 C8 1.361(11) . ? C7 C6 1.384(11) . ? C8 H8 0.9300 . ? C12 C14 1.379(10) . ? C12 C11 1.390(10) . ? C12 C13 1.501(9) . ? C4 C3 1.388(10) . ? C4 C6 1.398(10) . ? C4 C5 1.495(9) . ? C15 C16 1.373(11) . ? C15 C14 1.413(10) . ? C3 H3 0.9300 . ? C6 H6 0.9300 . ? C14 H14 0.9300 . ? C11 H11 0.9300 . ? C16 H16 0.9300 . ? O1W H1W1 0.83(2) . ? O1W H1W2 0.84(2) . ? 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 Mg1 O1 180.0(3) . 5_665 ? O1 Mg1 O3 89.2(3) . 5_665 ? O1 Mg1 O3 90.8(3) 5_665 5_665 ? O1 Mg1 O3 90.8(3) . . ? O1 Mg1 O3 89.2(3) 5_665 . ? O3 Mg1 O3 180.0(3) 5_665 . ? O1 Mg1 O1W 90.63(19) . . ? O1 Mg1 O1W 89.37(19) 5_665 . ? O3 Mg1 O1W 87.73(19) 5_665 . ? O3 Mg1 O1W 92.27(19) . . ? O1 Mg1 O1W 89.37(19) . 5_665 ? O1 Mg1 O1W 90.63(19) 5_665 5_665 ? O3 Mg1 O1W 92.27(19) 5_665 5_665 ? O3 Mg1 O1W 87.73(19) . 5_665 ? O1W Mg1 O1W 180.0(2) . 5_665 ? O2 Mg2 O4 93.1(2) . . ? O2 Mg2 O8 89.8(2) . 8_565 ? O4 Mg2 O8 175.8(2) . 8_565 ? O2 Mg2 O2W 88.9(2) . . ? O4 Mg2 O2W 87.7(3) . . ? O8 Mg2 O2W 89.4(2) 8_565 . ? O2 Mg2 O5 176.4(2) . 3 ? O4 Mg2 O5 90.1(2) . 3 ? O8 Mg2 O5 86.9(2) 8_565 3 ? O2W Mg2 O5 89.7(2) . 3 ? O2 Mg2 O1W 92.69(19) . . ? O4 Mg2 O1W 92.59(19) . . ? O8 Mg2 O1W 90.28(18) 8_565 . ? O2W Mg2 O1W 178.4(2) . . ? O5 Mg2 O1W 88.72(19) 3 . ? C1 O1 Mg1 139.6(5) . . ? Mg2 O2W H2W1 125(6) . . ? Mg2 O2W H2W2 87(10) . . ? H2W1 O2W H2W2 113(6) . . ? C1 O2 Mg2 136.8(5) . . ? C9 O3 Mg1 139.7(5) . . ? C9 O4 Mg2 133.3(4) . . ? C5 O5 Mg2 132.4(5) . 3_455 ? C13 O7 H7 109.5 . . ? C13 O8 Mg2 132.6(4) . 8_566 ? C7 N1 H1A 120.0 . . ? C7 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C15 N2 H2A 120.0 . . ? C15 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C16 C10 C11 119.6(7) . . ? C16 C10 C9 119.7(6) . . ? C11 C10 C9 120.7(6) . . ? C3 C2 C8 118.9(7) . . ? C3 C2 C1 122.1(6) . . ? C8 C2 C1 118.8(6) . . ? C8 C7 C6 119.9(7) . . ? C8 C7 N1 120.0(8) . . ? C6 C7 N1 120.0(8) . . ? C7 C8 C2 120.6(7) . . ? C7 C8 H8 119.7 . . ? C2 C8 H8 119.7 . . ? C14 C12 C11 120.2(6) . . ? C14 C12 C13 118.9(6) . . ? C11 C12 C13 120.9(6) . . ? O8 C13 O7 125.2(6) . . ? O8 C13 C12 117.8(6) . . ? O7 C13 C12 117.0(6) . . ? C3 C4 C6 118.9(7) . . ? C3 C4 C5 120.7(6) . . ? C6 C4 C5 120.2(7) . . ? C16 C15 N2 121.1(7) . . ? C16 C15 C14 119.7(7) . . ? N2 C15 C14 119.2(7) . . ? O1 C1 O2 123.1(6) . . ? O1 C1 C2 119.0(6) . . ? O2 C1 C2 117.9(6) . . ? C2 C3 C4 120.6(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C7 C6 C4 120.8(7) . . ? C7 C6 H6 119.6 . . ? C4 C6 H6 119.6 . . ? C12 C14 C15 119.3(7) . . ? C12 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C10 C11 C12 120.2(6) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C10 C16 C15 121.0(7) . . ? C10 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? O3 C9 O4 126.1(6) . . ? O3 C9 C10 116.8(6) . . ? O4 C9 C10 117.1(6) . . ? O5 C5 O6 124.7(6) . . ? O5 C5 C4 118.0(6) . . ? O6 C5 C4 117.2(7) . . ? Mg1 O1W Mg2 114.73(19) . . ? Mg1 O1W H1W1 123(6) . . ? Mg2 O1W H1W1 82(6) . . ? Mg1 O1W H1W2 124(8) . . ? Mg2 O1W H1W2 70(10) . . ? H1W1 O1W H1W2 113(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.018 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.097 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.483 -0.009 665.5 106.3 2 0.250 -0.015 -0.005 678.5 111.2 3 0.750 0.517 -0.007 665.5 103.4 4 0.750 0.015 -0.005 678.4 114.6 5 -0.004 0.248 0.147 15.0 1.3 6 0.496 0.752 0.147 15.0 1.3 7 0.003 0.752 0.647 14.9 1.3 8 0.503 0.248 0.647 15.0 1.3 _platon_squeeze_details ; ;