Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Robert Davies' _publ_contact_author_address ; Dept of Chemistry Imperial College London Exhibition Road South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email R.DAVIES@IMPERIAL.AC.UK _publ_section_title ; Framework Materials Assembled from Magnesium Carboxylate Building Units ; loop_ _publ_author_name 'Robert Davies' 'Robert J. Less' 'P. Lickiss' 'Andrew J. P. White' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 629623' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Mg1.50 N2 O8' _chemical_formula_sum 'C20 H24 Mg1.50 N2 O8' _chemical_formula_weight 456.88 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 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 15.076(3) _cell_length_b 9.821(2) _cell_length_c 16.555(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.21(3) _cell_angle_gamma 90.00 _cell_volume 2285.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9228 _cell_measurement_theta_min 3.7260 _cell_measurement_theta_max 32.1432 _exptl_crystal_description tablets _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72803 _exptl_absorpt_correction_T_max 1.26761 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24647 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 31.63 _reflns_number_total 6763 _reflns_number_gt 3869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 O(30) and O(40) coordinated dma solvent molecules were found to be extensively disordered. This disorder was handled by the refinement of multiple overlapping idealised orientations for which the bond lengths and angles were restrained either to set values or to be the same as their chemcial equivalents in the other orientations. The molecules were also restrained to be flat, and the isotropic thermal parameters of atoms of different orientations that were close to each other in space were restrained to be the same. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6763 _refine_ls_number_parameters 352 _refine_ls_number_restraints 271 _refine_ls_R_factor_all 0.1735 _refine_ls_R_factor_gt 0.1157 _refine_ls_wR_factor_ref 0.2895 _refine_ls_wR_factor_gt 0.2769 _refine_ls_goodness_of_fit_ref 1.642 _refine_ls_restrained_S_all 1.670 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.65487(9) -0.08092(12) 0.88722(7) 0.0296(3) Uani 1 1 d . . . Mg2 Mg 0.5000 0.0000 1.0000 0.0225(4) Uani 1 2 d S . . C1 C 0.6941(3) 0.1339(4) 1.0193(2) 0.0310(8) Uani 1 1 d . . . O2 O 0.7251(2) 0.0732(3) 0.96684(18) 0.0440(7) Uani 1 1 d . . . O3 O 0.61167(17) 0.1300(3) 1.01802(16) 0.0341(6) Uani 1 1 d . . . C4 C 0.7662(3) 0.2167(4) 1.0918(2) 0.0326(8) Uani 1 1 d . . . C5 C 0.7380(3) 0.2732(6) 1.1542(3) 0.0549(13) Uani 1 1 d . . . H5A H 0.6736 0.2651 1.1498 0.066 Uiso 1 1 calc R . . C6 C 0.8031(3) 0.3428(6) 1.2246(3) 0.0547(13) Uani 1 1 d . . . H6A H 0.7830 0.3788 1.2684 0.066 Uiso 1 1 calc R . . C7 C 0.8962(3) 0.3593(4) 1.2308(2) 0.0330(8) Uani 1 1 d . . . C8 C 0.9237(3) 0.3024(6) 1.1670(3) 0.0617(15) Uani 1 1 d . . . H8A H 0.9877 0.3120 1.1703 0.074 Uiso 1 1 calc R . . C9 C 0.8586(3) 0.2307(6) 1.0977(3) 0.0619(15) Uani 1 1 d . . . H9A H 0.8787 0.1916 1.0547 0.074 Uiso 1 1 calc R . . C10 C 0.9666(2) 0.4330(4) 1.3091(2) 0.0285(7) Uani 1 1 d . . . O11 O 0.93929(19) 0.4513(3) 1.37180(16) 0.0380(6) Uani 1 1 d . . . O12 O 1.04534(18) 0.4673(3) 1.30539(16) 0.0361(6) Uani 1 1 d . . . C21 C 0.5607(3) -0.2640(4) 0.9262(3) 0.0376(9) Uani 1 1 d . . . O22 O 0.5762(2) -0.2755(3) 0.85617(18) 0.0470(8) Uani 1 1 d . . . O23 O 0.58002(17) -0.1539(2) 0.96834(16) 0.0310(6) Uani 1 1 d . . . C24 C 0.5277(3) -0.3860(4) 0.9635(3) 0.0366(9) Uani 1 1 d . . . C25 C 0.4932(3) -0.5025(4) 0.9142(3) 0.0395(9) Uani 1 1 d . . . H25A H 0.4894 -0.5048 0.8557 0.047 Uiso 1 1 calc R . . C26 C 0.5359(3) -0.3842(4) 1.0512(3) 0.0403(9) Uani 1 1 d . . . H26A H 0.5609 -0.3065 1.0862 0.048 Uiso 1 1 calc R . . O30 O 0.7160(2) -0.0804(3) 0.7968(2) 0.0544(9) Uani 1 1 d D . . C30 C 0.7638(10) -0.0520(16) 0.7540(8) 0.088(8) Uiso 0.293(4) 1 d PD A 1 C31 C 0.8409(15) 0.058(2) 0.7858(16) 0.135(11) Uiso 0.293(4) 1 d PDU A 1 H31A H 0.9015 0.0137 0.8192 0.203 Uiso 0.293(4) 1 d PR A 1 H31B H 0.8253 0.1254 0.8221 0.203 Uiso 0.293(4) 1 d PR A 1 H31C H 0.8464 0.1029 0.7350 0.203 Uiso 0.293(4) 1 d PR A 1 N32 N 0.7515(8) -0.1140(10) 0.6791(6) 0.031(3) Uiso 0.293(4) 1 d PD A 1 C33 C 0.6733(15) -0.228(2) 0.6509(15) 0.128(10) Uiso 0.293(4) 1 d PDU A 1 H33A H 0.6992 -0.3141 0.6792 0.192 Uiso 0.293(4) 1 d PR A 1 H33B H 0.6508 -0.2394 0.5878 0.192 Uiso 0.293(4) 1 d PR A 1 H33C H 0.6201 -0.1995 0.6678 0.192 Uiso 0.293(4) 1 d PR A 1 C34 C 0.8050(12) -0.0915(17) 0.6220(9) 0.048(4) Uiso 0.293(4) 1 d PDU A 1 H34A H 0.7905 -0.0007 0.5959 0.072 Uiso 0.293(4) 1 d PR A 1 H34B H 0.7866 -0.1606 0.5762 0.072 Uiso 0.293(4) 1 d PR A 1 H34C H 0.8733 -0.0985 0.6555 0.072 Uiso 0.293(4) 1 d PR A 1 C30' C 0.7067(9) -0.0805(13) 0.7208(7) 0.040(4) Uiso 0.281(10) 1 d PD A 2 C31' C 0.6103(13) -0.128(3) 0.6538(13) 0.162(13) Uiso 0.281(10) 1 d PDU A 2 H31D H 0.6097 -0.2252 0.6412 0.243 Uiso 0.281(10) 1 d PR A 2 H31E H 0.6013 -0.0755 0.6009 0.243 Uiso 0.281(10) 1 d PR A 2 H31F H 0.5587 -0.1066 0.6746 0.243 Uiso 0.281(10) 1 d PR A 2 N32' N 0.7768(10) -0.0496(14) 0.6945(8) 0.062(6) Uiso 0.281(10) 1 d PD A 2 C33' C 0.8743(11) -0.005(2) 0.7615(12) 0.082(7) Uiso 0.281(10) 1 d PDU A 2 H33D H 0.8660 0.0621 0.8021 0.123 Uiso 0.281(10) 1 d PR A 2 H33E H 0.9137 0.0341 0.7316 0.123 Uiso 0.281(10) 1 d PR A 2 H33F H 0.9054 -0.0864 0.7935 0.123 Uiso 0.281(10) 1 d PR A 2 C34' C 0.7690(12) -0.0507(16) 0.6016(8) 0.032(4) Uiso 0.281(10) 1 d PDU A 2 H34D H 0.7648 -0.1444 0.5802 0.048 Uiso 0.281(10) 1 d PR A 2 H34E H 0.8249 -0.0061 0.5964 0.048 Uiso 0.281(10) 1 d PR A 2 H34F H 0.7115 -0.0007 0.5673 0.048 Uiso 0.281(10) 1 d PR A 2 C30" C 0.7290(9) -0.0331(12) 0.7334(7) 0.030(4) Uiso 0.276(11) 1 d PD A 3 C31" C 0.6815(16) 0.1008(17) 0.6950(14) 0.086(7) Uiso 0.276(11) 1 d PDU A 3 H31G H 0.6160 0.0997 0.6936 0.129 Uiso 0.276(11) 1 d PR A 3 H31H H 0.6809 0.1060 0.6357 0.129 Uiso 0.276(11) 1 d PR A 3 H31I H 0.7150 0.1801 0.7280 0.129 Uiso 0.276(11) 1 d PR A 3 N32" N 0.7903(9) -0.0915(15) 0.7026(8) 0.041(4) Uiso 0.276(11) 1 d PD A 3 C33" C 0.8394(17) -0.222(2) 0.7389(17) 0.126(11) Uiso 0.276(11) 1 d PDU A 3 H33G H 0.8673 -0.2140 0.8022 0.189 Uiso 0.276(11) 1 d PR A 3 H33H H 0.8902 -0.2364 0.7159 0.189 Uiso 0.276(11) 1 d PR A 3 H33I H 0.7954 -0.2994 0.7232 0.189 Uiso 0.276(11) 1 d PR A 3 C34" C 0.8086(19) -0.034(3) 0.6250(13) 0.139(14) Uiso 0.276(11) 1 d PDU A 3 H34G H 0.7495 0.0076 0.5859 0.208 Uiso 0.276(11) 1 d PR A 3 H34H H 0.8277 -0.1075 0.5949 0.208 Uiso 0.276(11) 1 d PR A 3 H34I H 0.8588 0.0356 0.6432 0.208 Uiso 0.276(11) 1 d PR A 3 C30* C 0.7439(12) -0.1184(16) 0.7397(9) 0.023(6) Uiso 0.150(10) 1 d PD A 4 C31* C 0.809(3) -0.241(3) 0.754(2) 0.156(19) Uiso 0.150(10) 1 d PDU A 4 H31J H 0.7987 -0.3088 0.7933 0.234 Uiso 0.150(10) 1 d PR A 4 H31K H 0.8745 -0.2058 0.7799 0.234 Uiso 0.150(10) 1 d PR A 4 H31L H 0.8006 -0.2838 0.6984 0.234 Uiso 0.150(10) 1 d PR A 4 N32* N 0.7194(15) -0.050(2) 0.6658(9) 0.055(8) Uiso 0.150(10) 1 d PD A 4 C33* C 0.652(2) 0.075(3) 0.654(2) 0.083(12) Uiso 0.150(10) 1 d PDU A 4 H33J H 0.6479 0.1045 0.7084 0.125 Uiso 0.150(10) 1 d PR A 4 H33K H 0.5895 0.0442 0.6143 0.125 Uiso 0.150(10) 1 d PR A 4 H33L H 0.6740 0.1504 0.6269 0.125 Uiso 0.150(10) 1 d PR A 4 C34* C 0.747(2) -0.082(3) 0.5901(13) 0.057(10) Uiso 0.150(10) 1 d PDU A 4 H34J H 0.8161 -0.0724 0.6082 0.085 Uiso 0.150(10) 1 d PR A 4 H34K H 0.7157 -0.0198 0.5418 0.085 Uiso 0.150(10) 1 d PR A 4 H34L H 0.7287 -0.1759 0.5716 0.085 Uiso 0.150(10) 1 d PR A 4 O40 O 0.7680(2) -0.2095(4) 0.9618(2) 0.0647(10) Uani 1 1 d D . . C40 C 0.8407(6) -0.1943(10) 1.0236(6) 0.077(3) Uani 0.604(8) 1 d PDU A 1 C41 C 0.9211(8) -0.1091(14) 1.0132(10) 0.135(5) Uani 0.604(8) 1 d PDU A 1 H41A H 0.9708 -0.1697 1.0087 0.203 Uiso 0.604(8) 1 calc PR A 1 H41B H 0.9481 -0.0494 1.0636 0.203 Uiso 0.604(8) 1 calc PR A 1 H41C H 0.8957 -0.0537 0.9606 0.203 Uiso 0.604(8) 1 calc PR A 1 N42 N 0.8496(7) -0.2507(11) 1.0983(5) 0.116(4) Uani 0.604(8) 1 d PDU A 1 C43 C 0.7708(9) -0.3330(13) 1.1070(8) 0.115(5) Uani 0.604(8) 1 d PDU A 1 H43A H 0.7248 -0.2725 1.1180 0.173 Uiso 0.604(8) 1 calc PR A 1 H43B H 0.7966 -0.3968 1.1554 0.173 Uiso 0.604(8) 1 calc PR A 1 H43C H 0.7392 -0.3840 1.0533 0.173 Uiso 0.604(8) 1 calc PR A 1 C44 C 0.9376(9) -0.2380(16) 1.1794(8) 0.147(6) Uani 0.604(8) 1 d PDU A 1 H44A H 0.9916 -0.2815 1.1700 0.220 Uiso 0.604(8) 1 calc PR A 1 H44B H 0.9264 -0.2828 1.2278 0.220 Uiso 0.604(8) 1 calc PR A 1 H44C H 0.9519 -0.1415 1.1931 0.220 Uiso 0.604(8) 1 calc PR A 1 C40' C 0.8228(8) -0.2316(12) 1.0356(7) 0.052(4) Uiso 0.396(8) 1 d PDU A 5 C41' C 0.7959(13) -0.1955(19) 1.1136(9) 0.098(6) Uiso 0.396(8) 1 d PDU A 5 H41D H 0.8364 -0.1210 1.1461 0.147 Uiso 0.396(8) 1 calc PR A 5 H41E H 0.8048 -0.2753 1.1512 0.147 Uiso 0.396(8) 1 calc PR A 5 H41F H 0.7291 -0.1669 1.0934 0.147 Uiso 0.396(8) 1 calc PR A 5 N42' N 0.9071(7) -0.2899(11) 1.0516(7) 0.077(4) Uiso 0.396(8) 1 d PDU A 5 C43' C 0.9394(14) -0.3331(19) 0.9783(11) 0.128(8) Uiso 0.396(8) 1 d PDU A 5 H43D H 0.8867 -0.3782 0.9329 0.192 Uiso 0.396(8) 1 calc PR A 5 H43E H 0.9931 -0.3963 1.0007 0.192 Uiso 0.396(8) 1 calc PR A 5 H43F H 0.9592 -0.2526 0.9541 0.192 Uiso 0.396(8) 1 calc PR A 5 C44' C 0.9772(9) -0.3221(15) 1.1406(8) 0.078(5) Uiso 0.396(8) 1 d PDU A 5 H44D H 1.0328 -0.2625 1.1537 0.118 Uiso 0.396(8) 1 calc PR A 5 H44E H 0.9973 -0.4173 1.1426 0.118 Uiso 0.396(8) 1 calc PR A 5 H44F H 0.9472 -0.3074 1.1834 0.118 Uiso 0.396(8) 1 calc PR A 5 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 0.0345(6) 0.0292(7) 0.0238(6) -0.0018(5) 0.0092(5) 0.0006(5) Mg2 0.0267(8) 0.0214(8) 0.0170(7) 0.0001(6) 0.0052(6) -0.0009(6) C1 0.0325(18) 0.0310(19) 0.0237(17) -0.0027(14) 0.0034(15) -0.0084(15) O2 0.0371(14) 0.0591(19) 0.0334(14) -0.0156(13) 0.0098(12) -0.0132(13) O3 0.0320(13) 0.0295(13) 0.0362(14) -0.0059(10) 0.0068(11) -0.0069(11) C4 0.0321(18) 0.039(2) 0.0248(17) -0.0045(15) 0.0083(15) -0.0090(16) C5 0.036(2) 0.087(4) 0.043(2) -0.029(2) 0.0167(19) -0.021(2) C6 0.044(2) 0.081(4) 0.043(2) -0.035(2) 0.020(2) -0.019(2) C7 0.0359(19) 0.041(2) 0.0193(16) -0.0055(14) 0.0060(14) -0.0068(16) C8 0.029(2) 0.111(4) 0.047(3) -0.042(3) 0.0160(19) -0.021(2) C9 0.039(2) 0.106(4) 0.045(3) -0.045(3) 0.021(2) -0.025(3) C10 0.0298(17) 0.0332(19) 0.0193(15) -0.0010(13) 0.0048(13) 0.0027(15) O11 0.0415(14) 0.0476(16) 0.0205(12) -0.0048(11) 0.0062(11) -0.0062(12) O12 0.0352(14) 0.0452(15) 0.0239(13) -0.0053(10) 0.0060(11) -0.0080(12) C21 0.050(2) 0.0239(18) 0.040(2) 0.0029(15) 0.0175(19) -0.0003(17) O22 0.076(2) 0.0340(15) 0.0386(16) -0.0084(12) 0.0294(15) -0.0107(14) O23 0.0388(14) 0.0226(12) 0.0326(13) 0.0038(10) 0.0141(11) 0.0006(10) C24 0.047(2) 0.0275(19) 0.039(2) 0.0014(15) 0.0208(18) -0.0021(16) C25 0.062(2) 0.0247(19) 0.035(2) 0.0004(15) 0.0213(19) -0.0042(18) C26 0.059(3) 0.0264(19) 0.039(2) -0.0037(15) 0.022(2) -0.0051(17) O30 0.072(2) 0.057(2) 0.0491(18) 0.0089(15) 0.0395(17) 0.0159(17) O40 0.067(2) 0.083(3) 0.0444(19) 0.0208(17) 0.0201(17) 0.0351(19) C40 0.044(5) 0.077(7) 0.096(7) 0.027(6) 0.010(5) 0.015(5) C41 0.084(7) 0.146(9) 0.160(10) 0.009(8) 0.025(7) 0.019(7) N42 0.111(8) 0.127(8) 0.069(6) 0.022(6) -0.018(6) -0.008(7) C43 0.129(10) 0.134(11) 0.081(8) 0.026(7) 0.034(7) -0.006(9) C44 0.146(9) 0.147(10) 0.118(9) 0.008(7) 0.012(7) 0.005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O30 2.022(3) . ? Mg1 O2 2.034(3) . ? Mg1 O12 2.046(3) 4_565 ? Mg1 O40 2.122(3) . ? Mg1 O23 2.165(3) . ? Mg1 O22 2.209(3) . ? Mg1 C21 2.515(4) . ? Mg1 Mg2 3.5670(14) . ? Mg2 O11 2.041(3) 2_647 ? Mg2 O11 2.041(3) 4_565 ? Mg2 O3 2.047(2) . ? Mg2 O3 2.047(2) 3_657 ? Mg2 O23 2.115(2) . ? Mg2 O23 2.115(2) 3_657 ? Mg2 Mg1 3.5670(15) 3_657 ? C1 O3 1.236(4) . ? C1 O2 1.273(5) . ? C1 C4 1.529(5) . ? C4 C9 1.368(6) . ? C4 C5 1.370(6) . ? C5 C6 1.400(6) . ? C6 C7 1.380(6) . ? C7 C8 1.384(6) . ? C7 C10 1.528(5) . ? C8 C9 1.400(6) . ? C10 O12 1.257(4) . ? C10 O11 1.260(4) . ? O11 Mg2 2.041(3) 2_657 ? O12 Mg1 2.046(3) 4_666 ? C21 O23 1.262(4) . ? C21 O22 1.269(5) . ? C21 C24 1.513(5) . ? C24 C25 1.392(6) . ? C24 C26 1.411(5) . ? C25 C26 1.393(6) 3_647 ? C26 C25 1.393(6) 3_647 ? O30 C30 1.212(12) . ? O30 C30' 1.213(10) . ? O30 C30* 1.224(12) . ? O30 C30" 1.227(10) . ? C30 N32 1.333(12) . ? C30 C31 1.532(15) . ? N32 C34 1.465(12) . ? N32 C33 1.567(14) . ? C30' N32' 1.317(12) . ? C30' C31' 1.547(14) . ? N32' C34' 1.499(13) . ? N32' C33' 1.550(15) . ? C30" N32" 1.335(11) . ? C30" C31" 1.522(14) . ? N32" C33" 1.493(15) . ? N32" C34" 1.518(15) . ? C30* N32* 1.328(13) . ? C30* C31* 1.521(15) . ? N32* C34* 1.490(15) . ? N32* C33* 1.550(16) . ? O40 C40 1.209(8) . ? O40 C40' 1.222(10) . ? C40 N42 1.316(10) . ? C40 C41 1.533(12) . ? N42 C43 1.486(12) . ? N42 C44 1.514(12) . ? C40' N42' 1.329(12) . ? C40' C41' 1.529(14) . ? N42' C44' 1.503(12) . ? N42' C43' 1.523(13) . ? 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 O30 Mg1 O2 102.02(14) . . ? O30 Mg1 O12 89.02(13) . 4_565 ? O2 Mg1 O12 97.44(13) . 4_565 ? O30 Mg1 O40 86.94(13) . . ? O2 Mg1 O40 86.89(15) . . ? O12 Mg1 O40 174.62(14) 4_565 . ? O30 Mg1 O23 159.97(13) . . ? O2 Mg1 O23 96.32(11) . . ? O12 Mg1 O23 96.56(11) 4_565 . ? O40 Mg1 O23 86.09(12) . . ? O30 Mg1 O22 100.36(13) . . ? O2 Mg1 O22 154.67(13) . . ? O12 Mg1 O22 94.64(13) 4_565 . ? O40 Mg1 O22 82.60(15) . . ? O23 Mg1 O22 60.11(10) . . ? O30 Mg1 C21 129.99(15) . . ? O2 Mg1 C21 125.09(13) . . ? O12 Mg1 C21 99.46(13) 4_565 . ? O40 Mg1 C21 80.48(15) . . ? O23 Mg1 C21 30.11(11) . . ? O22 Mg1 C21 30.28(11) . . ? O30 Mg1 Mg2 161.24(10) . . ? O2 Mg1 Mg2 77.34(9) . . ? O12 Mg1 Mg2 72.59(8) 4_565 . ? O40 Mg1 Mg2 111.64(10) . . ? O23 Mg1 Mg2 33.10(7) . . ? O22 Mg1 Mg2 85.22(8) . . ? C21 Mg1 Mg2 59.18(9) . . ? O11 Mg2 O11 180.000(1) 2_647 4_565 ? O11 Mg2 O3 87.64(11) 2_647 . ? O11 Mg2 O3 92.36(11) 4_565 . ? O11 Mg2 O3 92.36(11) 2_647 3_657 ? O11 Mg2 O3 87.64(11) 4_565 3_657 ? O3 Mg2 O3 180.0 . 3_657 ? O11 Mg2 O23 90.52(10) 2_647 . ? O11 Mg2 O23 89.48(10) 4_565 . ? O3 Mg2 O23 88.23(10) . . ? O3 Mg2 O23 91.77(10) 3_657 . ? O11 Mg2 O23 89.48(10) 2_647 3_657 ? O11 Mg2 O23 90.52(10) 4_565 3_657 ? O3 Mg2 O23 91.77(10) . 3_657 ? O3 Mg2 O23 88.23(10) 3_657 3_657 ? O23 Mg2 O23 180.00(12) . 3_657 ? O11 Mg2 Mg1 111.10(8) 2_647 . ? O11 Mg2 Mg1 68.90(8) 4_565 . ? O3 Mg2 Mg1 63.62(8) . . ? O3 Mg2 Mg1 116.38(8) 3_657 . ? O23 Mg2 Mg1 33.99(7) . . ? O23 Mg2 Mg1 146.01(7) 3_657 . ? O11 Mg2 Mg1 68.90(8) 2_647 3_657 ? O11 Mg2 Mg1 111.10(8) 4_565 3_657 ? O3 Mg2 Mg1 116.38(8) . 3_657 ? O3 Mg2 Mg1 63.62(8) 3_657 3_657 ? O23 Mg2 Mg1 146.01(7) . 3_657 ? O23 Mg2 Mg1 33.99(7) 3_657 3_657 ? Mg1 Mg2 Mg1 180.0 . 3_657 ? O3 C1 O2 126.1(3) . . ? O3 C1 C4 117.0(3) . . ? O2 C1 C4 116.9(3) . . ? C1 O2 Mg1 123.9(2) . . ? C1 O3 Mg2 142.2(2) . . ? C9 C4 C5 119.4(3) . . ? C9 C4 C1 121.7(3) . . ? C5 C4 C1 118.8(3) . . ? C4 C5 C6 120.7(4) . . ? C7 C6 C5 120.5(4) . . ? C6 C7 C8 118.3(3) . . ? C6 C7 C10 119.6(3) . . ? C8 C7 C10 122.1(3) . . ? C7 C8 C9 120.8(4) . . ? C4 C9 C8 120.3(4) . . ? O12 C10 O11 126.7(3) . . ? O12 C10 C7 117.6(3) . . ? O11 C10 C7 115.7(3) . . ? C10 O11 Mg2 137.1(2) . 2_657 ? C10 O12 Mg1 131.6(2) . 4_666 ? O23 C21 O22 120.0(3) . . ? O23 C21 C24 119.8(3) . . ? O22 C21 C24 119.9(3) . . ? O23 C21 Mg1 59.40(19) . . ? O22 C21 Mg1 61.4(2) . . ? C24 C21 Mg1 166.1(3) . . ? C21 O22 Mg1 88.3(2) . . ? C21 O23 Mg2 135.3(3) . . ? C21 O23 Mg1 90.5(2) . . ? Mg2 O23 Mg1 112.91(11) . . ? C25 C24 C26 119.2(3) . . ? C25 C24 C21 121.4(4) . . ? C26 C24 C21 119.3(3) . . ? C24 C25 C26 121.4(4) . 3_647 ? C25 C26 C24 119.3(4) 3_647 . ? C30 O30 C30' 42.7(9) . . ? C30 O30 C30* 34.4(10) . . ? C30' O30 C30* 31.0(8) . . ? C30 O30 C30" 25.8(8) . . ? C30' O30 C30" 26.9(7) . . ? C30* O30 C30" 41.3(9) . . ? C30 O30 Mg1 163.8(7) . . ? C30' O30 Mg1 148.7(6) . . ? C30* O30 Mg1 161.3(8) . . ? C30" O30 Mg1 153.1(6) . . ? O30 C30 N32 121.8(12) . . ? O30 C30 C31 120.0(13) . . ? N32 C30 C31 118.2(12) . . ? C30 N32 C34 127.4(10) . . ? C30 N32 C33 116.1(10) . . ? C34 N32 C33 116.5(11) . . ? O30 C30' N32' 122.6(10) . . ? O30 C30' C31' 118.0(12) . . ? N32' C30' C31' 119.3(12) . . ? C30' N32' C34' 124.3(11) . . ? C30' N32' C33' 119.6(11) . . ? C34' N32' C33' 116.0(11) . . ? O30 C30" N32" 120.7(10) . . ? O30 C30" C31" 119.2(11) . . ? N32" C30" C31" 119.9(11) . . ? C30" N32" C33" 121.7(12) . . ? C30" N32" C34" 121.6(13) . . ? C33" N32" C34" 116.5(13) . . ? O30 C30* N32* 119.8(12) . . ? O30 C30* C31* 120.3(14) . . ? N32* C30* C31* 119.9(14) . . ? C30* N32* C34* 126.6(14) . . ? C30* N32* C33* 118.2(13) . . ? C34* N32* C33* 115.2(13) . . ? C40 O40 C40' 25.4(7) . . ? C40 O40 Mg1 135.3(5) . . ? C40' O40 Mg1 142.9(6) . . ? O40 C40 N42 119.7(9) . . ? O40 C40 C41 118.9(9) . . ? N42 C40 C41 121.3(9) . . ? C40 N42 C43 120.5(8) . . ? C40 N42 C44 123.9(10) . . ? C43 N42 C44 115.7(9) . . ? O40 C40' N42' 121.9(10) . . ? O40 C40' C41' 120.9(11) . . ? N42' C40' C41' 117.3(11) . . ? C40' N42' C44' 124.7(10) . . ? C40' N42' C43' 121.3(10) . . ? C44' N42' C43' 114.1(10) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 31.63 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 1.288 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.119 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 629624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H12 Mg1.50 O7' _chemical_formula_sum 'C14 H12 Mg1.50 O7' _chemical_formula_weight 328.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 8.9778(18) _cell_length_b 17.2530(19) _cell_length_c 9.873(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.618(18) _cell_angle_gamma 90.00 _cell_volume 1527.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7923 _cell_measurement_theta_min 3.8073 _cell_measurement_theta_max 31.9108 _exptl_crystal_description 'tabular diamonds' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.168 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.983 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23806 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 31.91 _reflns_number_total 4942 _reflns_number_gt 3158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 O(30) coordinated ethanol solvent molecule was found to be disordered. This disorder was handled by the refinement of two overlapping idealised orientations for which the bond lengths and angles were restrained to be the same as their chemcial equivalents in the other orientation. ; _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^)+(0.0652P)^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 4942 _refine_ls_number_parameters 218 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.956 _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 Mg1 Mg 0.37771(6) 0.02010(3) 0.60268(5) 0.01247(13) Uani 1 1 d D . . Mg2 Mg 0.0000 0.0000 0.5000 0.00936(15) Uani 1 2 d S . . C1 C 0.19320(17) 0.14196(9) 0.44695(16) 0.0144(3) Uani 1 1 d . . . O2 O 0.31781(12) 0.11564(6) 0.49256(12) 0.0168(2) Uani 1 1 d . . . O3 O 0.06994(12) 0.11001(6) 0.45740(12) 0.0168(2) Uani 1 1 d . . . C4 C 0.19650(18) 0.21758(9) 0.37119(16) 0.0163(3) Uani 1 1 d . . . C5 C 0.07214(19) 0.24179(10) 0.29360(19) 0.0228(4) Uani 1 1 d . . . H5A H -0.0165 0.2117 0.2925 0.027 Uiso 1 1 calc R . . C6 C 0.07589(19) 0.30961(10) 0.21749(19) 0.0219(4) Uani 1 1 d . . . H6A H -0.0097 0.3254 0.1644 0.026 Uiso 1 1 calc R . . C7 C 0.20448(18) 0.35407(9) 0.21910(16) 0.0152(3) Uani 1 1 d . . . C8 C 0.3291(2) 0.33047(11) 0.2977(2) 0.0278(4) Uani 1 1 d . . . H8A H 0.4174 0.3609 0.2994 0.033 Uiso 1 1 calc R . . C9 C 0.3251(2) 0.26285(11) 0.3737(2) 0.0289(4) Uani 1 1 d . . . H9A H 0.4103 0.2474 0.4276 0.035 Uiso 1 1 calc R . . C10 C 0.21672(17) 0.42486(8) 0.13199(15) 0.0120(3) Uani 1 1 d . . . O11 O 0.09835(12) 0.45221(6) 0.07149(11) 0.0144(2) Uani 1 1 d . . . O12 O 0.34267(12) 0.45245(6) 0.11815(11) 0.0148(2) Uani 1 1 d . . . C21 C 0.19172(17) 0.02228(9) 0.77658(16) 0.0151(3) Uani 1 1 d . . . O22 O 0.31255(13) 0.05820(7) 0.79462(12) 0.0226(3) Uani 1 1 d . . . O23 O 0.15794(12) -0.00840(6) 0.66147(11) 0.0137(2) Uani 1 1 d . . . C24 C 0.09050(18) 0.01129(9) 0.89146(16) 0.0165(3) Uani 1 1 d . . . C25 C 0.1140(2) 0.05469(10) 1.00959(18) 0.0216(4) Uani 1 1 d . . . H25A H 0.1920 0.0919 1.0161 0.026 Uiso 1 1 calc R . . C26 C -0.02290(19) -0.04341(10) 0.88240(17) 0.0202(4) Uani 1 1 d . . . H26A H -0.0382 -0.0732 0.8020 0.024 Uiso 1 1 calc R . . O30 O 0.46455(17) -0.07949(8) 0.69927(14) 0.0328(3) Uani 1 1 d D . . H30 H 0.527(3) -0.1031(17) 0.644(3) 0.084(11) Uiso 1 1 d D . . C31 C 0.5300(6) -0.0859(3) 0.8290(4) 0.0545(15) Uani 0.582(6) 1 d PD A 1 H31A H 0.6365 -0.0988 0.8198 0.065 Uiso 0.582(6) 1 calc PR A 1 H31B H 0.5264 -0.0341 0.8720 0.065 Uiso 0.582(6) 1 calc PR A 1 C32 C 0.4727(10) -0.1380(5) 0.9163(6) 0.118(3) Uani 0.582(6) 1 d PDU A 1 H32A H 0.5287 -0.1353 1.0037 0.177 Uiso 0.582(6) 1 calc PR A 1 H32B H 0.4806 -0.1903 0.8788 0.177 Uiso 0.582(6) 1 calc PR A 1 H32C H 0.3677 -0.1257 0.9291 0.177 Uiso 0.582(6) 1 calc PR A 1 C31' C 0.4317(8) -0.1286(4) 0.8078(7) 0.055(2) Uiso 0.418(6) 1 d PD A 2 H31C H 0.5247 -0.1532 0.8442 0.066 Uiso 0.418(6) 1 calc PR A 2 H31D H 0.3897 -0.0975 0.8812 0.066 Uiso 0.418(6) 1 calc PR A 2 C32' C 0.3335(11) -0.1840(6) 0.7679(10) 0.101(4) Uiso 0.418(6) 1 d PD A 2 H32D H 0.3113 -0.2167 0.8457 0.152 Uiso 0.418(6) 1 calc PR A 2 H32E H 0.3764 -0.2159 0.6974 0.152 Uiso 0.418(6) 1 calc PR A 2 H32F H 0.2414 -0.1598 0.7317 0.152 Uiso 0.418(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0118(2) 0.0138(3) 0.0121(3) 0.00018(19) 0.00319(19) 0.0000(2) Mg2 0.0082(3) 0.0085(3) 0.0117(4) 0.0000(3) 0.0032(3) -0.0004(3) C1 0.0164(8) 0.0103(7) 0.0164(8) 0.0005(6) 0.0006(6) -0.0005(6) O2 0.0144(5) 0.0141(5) 0.0220(6) 0.0052(4) 0.0003(5) 0.0005(4) O3 0.0130(5) 0.0108(5) 0.0269(6) 0.0049(4) 0.0041(5) -0.0016(4) C4 0.0165(7) 0.0126(7) 0.0197(8) 0.0046(6) 0.0014(6) -0.0021(6) C5 0.0139(8) 0.0179(8) 0.0364(11) 0.0093(7) -0.0015(7) -0.0042(6) C6 0.0153(8) 0.0183(8) 0.0316(10) 0.0100(7) -0.0046(7) -0.0015(6) C7 0.0151(7) 0.0125(7) 0.0180(8) 0.0043(6) 0.0010(6) -0.0008(6) C8 0.0189(8) 0.0226(9) 0.0408(12) 0.0158(8) -0.0101(8) -0.0097(7) C9 0.0190(9) 0.0251(9) 0.0411(12) 0.0185(8) -0.0139(8) -0.0078(7) C10 0.0123(7) 0.0113(7) 0.0125(7) 0.0022(5) 0.0022(6) 0.0003(5) O11 0.0130(5) 0.0139(5) 0.0163(6) 0.0053(4) 0.0014(4) 0.0002(4) O12 0.0119(5) 0.0155(5) 0.0172(6) 0.0045(4) 0.0031(4) -0.0020(4) C21 0.0148(7) 0.0175(7) 0.0133(7) 0.0005(6) 0.0041(6) 0.0007(6) O22 0.0198(6) 0.0315(7) 0.0168(6) -0.0054(5) 0.0051(5) -0.0074(5) O23 0.0136(5) 0.0181(6) 0.0095(5) 0.0001(4) 0.0029(4) 0.0002(4) C24 0.0159(7) 0.0207(8) 0.0133(8) 0.0007(6) 0.0038(6) 0.0014(6) C25 0.0211(8) 0.0271(9) 0.0172(8) -0.0023(7) 0.0065(7) -0.0076(7) C26 0.0228(8) 0.0254(9) 0.0130(8) -0.0043(6) 0.0060(6) -0.0046(7) O30 0.0386(8) 0.0323(8) 0.0286(8) 0.0147(6) 0.0124(6) 0.0127(6) C31 0.063(3) 0.067(3) 0.032(2) 0.002(2) -0.016(2) 0.025(3) C32 0.160(6) 0.141(6) 0.052(4) 0.057(4) -0.011(4) -0.024(5) _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 O2 2.0335(12) . ? Mg1 O11 2.0742(12) 4_666 ? Mg1 O30 2.0979(14) . ? Mg1 O11 2.0996(12) 2_545 ? Mg1 O22 2.1133(13) . ? Mg1 O23 2.1392(12) . ? Mg1 C21 2.4493(17) . ? Mg1 Mg1 3.1336(12) 3_656 ? Mg1 Mg2 3.5118(9) . ? Mg2 O12 2.0443(11) 2_545 ? Mg2 O12 2.0443(11) 4_566 ? Mg2 O3 2.0488(11) 3_556 ? Mg2 O3 2.0488(11) . ? Mg2 O23 2.0896(12) . ? Mg2 O23 2.0896(12) 3_556 ? Mg2 Mg1 3.5118(9) 3_556 ? C1 O3 1.2448(19) . ? C1 O2 1.2706(19) . ? C1 C4 1.505(2) . ? C4 C5 1.389(2) . ? C4 C9 1.393(2) . ? C5 C6 1.392(2) . ? C6 C7 1.386(2) . ? C7 C8 1.393(2) . ? C7 C10 1.501(2) . ? C8 C9 1.388(2) . ? C10 O12 1.2402(18) . ? C10 O11 1.2848(18) . ? O11 Mg1 2.0742(12) 4_565 ? O11 Mg1 2.0996(12) 2 ? O12 Mg2 2.0443(11) 2 ? C21 O22 1.255(2) . ? C21 O23 1.2776(19) . ? C21 C24 1.497(2) . ? C24 C26 1.388(2) . ? C24 C25 1.394(2) . ? C25 C26 1.387(2) 3_557 ? C26 C25 1.387(2) 3_557 ? O30 C31 1.389(4) . ? O30 C31' 1.407(7) . ? C31 C32 1.362(8) . ? C31' C32' 1.347(10) . ? 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 Mg1 O11 87.99(5) . 4_666 ? O2 Mg1 O30 172.15(6) . . ? O11 Mg1 O30 85.33(6) 4_666 . ? O2 Mg1 O11 92.79(5) . 2_545 ? O11 Mg1 O11 82.69(5) 4_666 2_545 ? O30 Mg1 O11 82.28(6) . 2_545 ? O2 Mg1 O22 98.63(6) . . ? O11 Mg1 O22 111.52(5) 4_666 . ? O30 Mg1 O22 87.68(6) . . ? O11 Mg1 O22 161.93(5) 2_545 . ? O2 Mg1 O23 96.12(5) . . ? O11 Mg1 O23 172.79(5) 4_666 . ? O30 Mg1 O23 90.95(5) . . ? O11 Mg1 O23 102.95(5) 2_545 . ? O22 Mg1 O23 62.07(5) . . ? O2 Mg1 C21 100.96(5) . . ? O11 Mg1 C21 141.88(6) 4_666 . ? O30 Mg1 C21 86.85(6) . . ? O11 Mg1 C21 132.94(5) 2_545 . ? O22 Mg1 C21 30.82(5) . . ? O23 Mg1 C21 31.42(5) . . ? O2 Mg1 Mg1 90.54(4) . 3_656 ? O11 Mg1 Mg1 41.65(3) 4_666 3_656 ? O30 Mg1 Mg1 81.72(4) . 3_656 ? O11 Mg1 Mg1 41.04(3) 2_545 3_656 ? O22 Mg1 Mg1 151.62(5) . 3_656 ? O23 Mg1 Mg1 143.80(4) . 3_656 ? C21 Mg1 Mg1 167.75(5) . 3_656 ? O2 Mg1 Mg2 72.39(4) . . ? O11 Mg1 Mg2 153.63(4) 4_666 . ? O30 Mg1 Mg2 112.60(5) . . ? O11 Mg1 Mg2 80.92(4) 2_545 . ? O22 Mg1 Mg2 89.22(4) . . ? O23 Mg1 Mg2 33.41(3) . . ? C21 Mg1 Mg2 61.55(4) . . ? Mg1 Mg1 Mg2 119.16(3) 3_656 . ? O12 Mg2 O12 180.0 2_545 4_566 ? O12 Mg2 O3 88.37(5) 2_545 3_556 ? O12 Mg2 O3 91.63(5) 4_566 3_556 ? O12 Mg2 O3 91.63(5) 2_545 . ? O12 Mg2 O3 88.37(5) 4_566 . ? O3 Mg2 O3 180.00(2) 3_556 . ? O12 Mg2 O23 86.85(5) 2_545 . ? O12 Mg2 O23 93.15(5) 4_566 . ? O3 Mg2 O23 89.02(4) 3_556 . ? O3 Mg2 O23 90.98(4) . . ? O12 Mg2 O23 93.15(5) 2_545 3_556 ? O12 Mg2 O23 86.85(5) 4_566 3_556 ? O3 Mg2 O23 90.98(4) 3_556 3_556 ? O3 Mg2 O23 89.02(4) . 3_556 ? O23 Mg2 O23 180.0 . 3_556 ? O12 Mg2 Mg1 61.39(3) 2_545 . ? O12 Mg2 Mg1 118.61(3) 4_566 . ? O3 Mg2 Mg1 109.46(3) 3_556 . ? O3 Mg2 Mg1 70.54(3) . . ? O23 Mg2 Mg1 34.31(3) . . ? O23 Mg2 Mg1 145.69(3) 3_556 . ? O12 Mg2 Mg1 118.61(3) 2_545 3_556 ? O12 Mg2 Mg1 61.39(3) 4_566 3_556 ? O3 Mg2 Mg1 70.54(3) 3_556 3_556 ? O3 Mg2 Mg1 109.46(3) . 3_556 ? O23 Mg2 Mg1 145.69(3) . 3_556 ? O23 Mg2 Mg1 34.31(3) 3_556 3_556 ? Mg1 Mg2 Mg1 180.0 . 3_556 ? O3 C1 O2 125.74(14) . . ? O3 C1 C4 117.57(14) . . ? O2 C1 C4 116.68(14) . . ? C1 O2 Mg1 133.33(10) . . ? C1 O3 Mg2 135.17(10) . . ? C5 C4 C9 119.05(15) . . ? C5 C4 C1 120.09(14) . . ? C9 C4 C1 120.82(15) . . ? C4 C5 C6 120.79(15) . . ? C7 C6 C5 119.99(15) . . ? C6 C7 C8 119.48(15) . . ? C6 C7 C10 121.79(14) . . ? C8 C7 C10 118.64(14) . . ? C9 C8 C7 120.44(16) . . ? C8 C9 C4 120.24(16) . . ? O12 C10 O11 123.15(13) . . ? O12 C10 C7 117.81(14) . . ? O11 C10 C7 118.99(13) . . ? C10 O11 Mg1 142.26(10) . 4_565 ? C10 O11 Mg1 118.18(9) . 2 ? Mg1 O11 Mg1 97.31(5) 4_565 2 ? C10 O12 Mg2 150.94(11) . 2 ? O22 C21 O23 119.95(14) . . ? O22 C21 C24 120.38(14) . . ? O23 C21 C24 119.58(14) . . ? O22 C21 Mg1 59.63(8) . . ? O23 C21 Mg1 60.78(8) . . ? C24 C21 Mg1 170.30(12) . . ? C21 O22 Mg1 89.55(10) . . ? C21 O23 Mg2 140.82(10) . . ? C21 O23 Mg1 87.81(9) . . ? Mg2 O23 Mg1 112.29(5) . . ? C26 C24 C25 120.10(15) . . ? C26 C24 C21 120.40(14) . . ? C25 C24 C21 119.47(15) . . ? C26 C25 C24 119.74(16) 3_557 . ? C25 C26 C24 120.16(15) 3_557 . ? C31 O30 C31' 49.1(3) . . ? C31 O30 Mg1 128.1(2) . . ? C31' O30 Mg1 138.8(3) . . ? C32 C31 O30 118.7(5) . . ? C32' C31' O30 111.2(7) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 31.91 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.532 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.066 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 641077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H30 Mg1.50 N2 O8' _chemical_formula_sum 'C29 H30 Mg1.50 N2 O8' _chemical_formula_weight 571.02 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.7835(12) _cell_length_b 18.384(2) _cell_length_c 12.1948(15) _cell_angle_alpha 90.00 _cell_angle_beta 113.960(10) _cell_angle_gamma 90.00 _cell_volume 2823.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25932 _cell_measurement_theta_min 3.6959 _cell_measurement_theta_max 31.8695 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93321 _exptl_absorpt_correction_T_max 1.08008 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) (compiled May 11 2006,17:41:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45916 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 31.94 _reflns_number_total 9104 _reflns_number_gt 7243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0736P)^2^+0.4320P] 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 9104 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.08417(3) 0.47928(2) 0.31993(3) 0.01624(9) Uani 1 1 d . . . Mg2 Mg 0.0000 0.5000 0.0000 0.01279(10) Uani 1 2 d S . . C1 C 0.18146(8) 0.39851(6) 0.17301(10) 0.01724(19) Uani 1 1 d . . . O2 O 0.12306(6) 0.42316(4) 0.07155(7) 0.02048(16) Uani 1 1 d . . . O3 O 0.17378(7) 0.41155(6) 0.27040(8) 0.0301(2) Uani 1 1 d . . . C4 C 0.27246(8) 0.34881(6) 0.18299(10) 0.01738(19) Uani 1 1 d . . . C5 C 0.31847(9) 0.30319(6) 0.28203(11) 0.0221(2) Uani 1 1 d . . . H5A H 0.2902 0.3015 0.3412 0.027 Uiso 1 1 calc R . . C6 C 0.40563(9) 0.25995(6) 0.29503(10) 0.0224(2) Uani 1 1 d . . . H6A H 0.4348 0.2281 0.3619 0.027 Uiso 1 1 calc R . . C7 C 0.45070(8) 0.26286(6) 0.21105(10) 0.0183(2) Uani 1 1 d . . . C8 C 0.40288(9) 0.30759(6) 0.11070(10) 0.0208(2) Uani 1 1 d . . . H8A H 0.4312 0.3095 0.0515 0.025 Uiso 1 1 calc R . . C9 C 0.31396(8) 0.34948(6) 0.09634(10) 0.0201(2) Uani 1 1 d . . . H9A H 0.2815 0.3787 0.0267 0.024 Uiso 1 1 calc R . . C10 C 0.55003(8) 0.22229(6) 0.23149(10) 0.0186(2) Uani 1 1 d . . . C11 C 0.63186(9) 0.21829(6) 0.34708(10) 0.0221(2) Uani 1 1 d . . . H11A H 0.6239 0.2422 0.4120 0.026 Uiso 1 1 calc R . . C12 C 0.72466(9) 0.17965(6) 0.36765(10) 0.0209(2) Uani 1 1 d . . . H12A H 0.7795 0.1780 0.4462 0.025 Uiso 1 1 calc R . . C13 C 0.73787(8) 0.14352(6) 0.27437(10) 0.01787(19) Uani 1 1 d . . . C14 C 0.65820(9) 0.14899(7) 0.15888(10) 0.0235(2) Uani 1 1 d . . . H14A H 0.6670 0.1257 0.0940 0.028 Uiso 1 1 calc R . . C15 C 0.56574(9) 0.18823(7) 0.13758(10) 0.0238(2) Uani 1 1 d . . . H15A H 0.5127 0.1919 0.0581 0.029 Uiso 1 1 calc R . . C16 C 0.83335(8) 0.09505(6) 0.29804(10) 0.01747(19) Uani 1 1 d . . . O17 O 0.89379(6) 0.08269(4) 0.40582(7) 0.01899(16) Uani 1 1 d . . . O18 O 0.84249(7) 0.07000(5) 0.20689(8) 0.02670(19) Uani 1 1 d . . . C21 C -0.09949(8) 0.51341(5) 0.19665(10) 0.01568(18) Uani 1 1 d . . . O22 O -0.05575(6) 0.53586(4) 0.30246(7) 0.01997(16) Uani 1 1 d . . . O23 O -0.04500(6) 0.48553(4) 0.14371(7) 0.01575(14) Uani 1 1 d . . . C24 C -0.21764(8) 0.51334(6) 0.13513(10) 0.01656(19) Uani 1 1 d . . . C25 C -0.26779(9) 0.47128(7) 0.03332(12) 0.0248(2) Uani 1 1 d . . . H25A H -0.2267 0.4458 -0.0006 0.030 Uiso 1 1 calc R . . C26 C -0.37797(9) 0.46616(7) -0.01951(12) 0.0283(3) Uani 1 1 d . . . H26A H -0.4111 0.4368 -0.0889 0.034 Uiso 1 1 calc R . . C27 C -0.44105(8) 0.50348(6) 0.02752(10) 0.0192(2) Uani 1 1 d . . . C28 C -0.38910(8) 0.54783(7) 0.12751(11) 0.0220(2) Uani 1 1 d . . . H28A H -0.4300 0.5758 0.1588 0.026 Uiso 1 1 calc R . . C29 C -0.27893(8) 0.55198(6) 0.18212(10) 0.0209(2) Uani 1 1 d . . . H29A H -0.2454 0.5812 0.2516 0.025 Uiso 1 1 calc R . . O30 O 0.01168(7) 0.38751(5) 0.35080(8) 0.02678(19) Uani 1 1 d . . . C30 C 0.04756(11) 0.32462(7) 0.37958(13) 0.0293(3) Uani 1 1 d . . . C31 C 0.12562(16) 0.30910(10) 0.50642(15) 0.0522(5) Uani 1 1 d . . . H31A H 0.1964 0.3015 0.5076 0.078 Uiso 1 1 calc R . . H31B H 0.1035 0.2653 0.5360 0.078 Uiso 1 1 calc R . . H31C H 0.1276 0.3505 0.5580 0.078 Uiso 1 1 calc R . . N32 N 0.01780(11) 0.27060(6) 0.30099(12) 0.0366(3) Uani 1 1 d . . . C33 C -0.05680(17) 0.28678(10) 0.17838(16) 0.0564(5) Uani 1 1 d . . . H33A H -0.1002 0.3289 0.1788 0.085 Uiso 1 1 calc R . . H33B H -0.1029 0.2446 0.1449 0.085 Uiso 1 1 calc R . . H33C H -0.0174 0.2977 0.1292 0.085 Uiso 1 1 calc R . . C34 C 0.06259(15) 0.19702(8) 0.32697(18) 0.0472(4) Uani 1 1 d . . . H34A H 0.1342 0.1972 0.3284 0.071 Uiso 1 1 calc R . . H34B H 0.0175 0.1635 0.2646 0.071 Uiso 1 1 calc R . . H34C H 0.0660 0.1812 0.4052 0.071 Uiso 1 1 calc R . . O40 O 0.18527(7) 0.48449(5) 0.49386(8) 0.02790(19) Uani 1 1 d . . . C40 C 0.24530(11) 0.53297(7) 0.55658(12) 0.0293(3) Uani 1 1 d . . . C41 C 0.20041(17) 0.60027(9) 0.5888(2) 0.0530(5) Uani 1 1 d . . . H41A H 0.1230 0.5958 0.5586 0.080 Uiso 1 1 calc R . . H41B H 0.2184 0.6429 0.5526 0.080 Uiso 1 1 calc R . . H41C H 0.2305 0.6059 0.6762 0.080 Uiso 1 1 calc R . . N42 N 0.34968(10) 0.52526(7) 0.59631(12) 0.0375(3) Uani 1 1 d . . . C43 C 0.38919(15) 0.45983(11) 0.5604(2) 0.0569(5) Uani 1 1 d . . . H43A H 0.3726 0.4172 0.5979 0.085 Uiso 1 1 calc R . . H43B H 0.4663 0.4636 0.5863 0.085 Uiso 1 1 calc R . . H43C H 0.3553 0.4548 0.4729 0.085 Uiso 1 1 calc R . . C44 C 0.42666(15) 0.57675(11) 0.67589(17) 0.0569(5) Uani 1 1 d . . . H44A H 0.4623 0.6020 0.6318 0.085 Uiso 1 1 calc R . . H44B H 0.4794 0.5505 0.7440 0.085 Uiso 1 1 calc R . . H44C H 0.3900 0.6124 0.7053 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.01017(16) 0.01983(18) 0.01820(18) 0.00124(13) 0.00524(13) 0.00111(12) Mg2 0.00700(19) 0.0141(2) 0.0161(2) -0.00030(16) 0.00342(17) -0.00005(15) C1 0.0108(4) 0.0178(4) 0.0226(5) -0.0002(4) 0.0063(4) 0.0031(3) O2 0.0145(3) 0.0222(4) 0.0224(4) 0.0019(3) 0.0050(3) 0.0071(3) O3 0.0237(4) 0.0435(5) 0.0235(4) 0.0023(4) 0.0102(3) 0.0173(4) C4 0.0122(4) 0.0186(5) 0.0200(5) 0.0001(4) 0.0052(4) 0.0041(3) C5 0.0196(5) 0.0259(5) 0.0241(5) 0.0046(4) 0.0122(4) 0.0076(4) C6 0.0210(5) 0.0251(5) 0.0216(5) 0.0074(4) 0.0092(4) 0.0103(4) C7 0.0145(4) 0.0191(5) 0.0197(5) 0.0000(4) 0.0054(4) 0.0058(4) C8 0.0183(5) 0.0265(5) 0.0186(5) 0.0032(4) 0.0086(4) 0.0088(4) C9 0.0179(5) 0.0228(5) 0.0187(5) 0.0039(4) 0.0064(4) 0.0085(4) C10 0.0146(4) 0.0197(5) 0.0199(5) 0.0015(4) 0.0054(4) 0.0066(4) C11 0.0195(5) 0.0255(5) 0.0190(5) -0.0015(4) 0.0056(4) 0.0091(4) C12 0.0169(5) 0.0233(5) 0.0178(5) -0.0005(4) 0.0022(4) 0.0068(4) C13 0.0136(4) 0.0186(5) 0.0201(5) 0.0014(4) 0.0055(4) 0.0054(4) C14 0.0193(5) 0.0313(6) 0.0183(5) -0.0010(4) 0.0058(4) 0.0118(4) C15 0.0179(5) 0.0311(6) 0.0184(5) 0.0000(4) 0.0033(4) 0.0114(4) C16 0.0122(4) 0.0179(4) 0.0216(5) 0.0013(4) 0.0061(4) 0.0043(3) O17 0.0137(3) 0.0206(4) 0.0205(4) 0.0029(3) 0.0048(3) 0.0061(3) O18 0.0202(4) 0.0363(5) 0.0219(4) -0.0010(3) 0.0068(3) 0.0137(3) C21 0.0104(4) 0.0145(4) 0.0214(5) 0.0022(3) 0.0057(4) 0.0009(3) O22 0.0133(3) 0.0228(4) 0.0218(4) -0.0025(3) 0.0051(3) 0.0016(3) O23 0.0088(3) 0.0196(3) 0.0191(4) 0.0009(3) 0.0059(3) 0.0006(2) C24 0.0092(4) 0.0193(5) 0.0210(5) 0.0020(4) 0.0060(4) 0.0003(3) C25 0.0108(4) 0.0310(6) 0.0325(6) -0.0106(5) 0.0089(4) -0.0004(4) C26 0.0112(4) 0.0386(7) 0.0333(6) -0.0156(5) 0.0073(4) -0.0020(4) C27 0.0096(4) 0.0233(5) 0.0245(5) -0.0014(4) 0.0067(4) 0.0003(4) C28 0.0115(4) 0.0296(6) 0.0252(5) -0.0045(4) 0.0079(4) 0.0020(4) C29 0.0123(4) 0.0283(5) 0.0211(5) -0.0033(4) 0.0058(4) 0.0003(4) O30 0.0256(4) 0.0196(4) 0.0346(5) 0.0042(3) 0.0117(4) 0.0006(3) C30 0.0282(6) 0.0245(6) 0.0352(7) 0.0055(5) 0.0130(5) -0.0011(5) C31 0.0604(11) 0.0422(9) 0.0353(8) 0.0087(7) 0.0000(8) 0.0059(8) N32 0.0389(6) 0.0225(5) 0.0411(7) 0.0024(5) 0.0088(5) 0.0011(5) C33 0.0653(12) 0.0446(9) 0.0366(8) -0.0039(7) -0.0027(8) 0.0026(8) C34 0.0487(9) 0.0189(6) 0.0696(11) 0.0024(6) 0.0196(8) 0.0022(6) O40 0.0244(4) 0.0350(5) 0.0198(4) 0.0024(3) 0.0043(3) -0.0061(3) C40 0.0304(6) 0.0339(6) 0.0232(6) 0.0044(5) 0.0106(5) -0.0040(5) C41 0.0623(11) 0.0370(8) 0.0763(13) -0.0043(8) 0.0451(11) 0.0029(8) N42 0.0286(6) 0.0403(7) 0.0353(6) 0.0011(5) 0.0043(5) -0.0069(5) C43 0.0390(9) 0.0543(11) 0.0811(14) 0.0001(10) 0.0281(10) 0.0099(8) C44 0.0440(9) 0.0554(11) 0.0481(10) 0.0042(8) -0.0051(8) -0.0265(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O3 2.0117(9) . ? Mg1 O40 2.0122(10) . ? Mg1 O18 2.0442(9) 2_655 ? Mg1 O30 2.0717(9) . ? Mg1 O22 2.1243(8) . ? Mg1 O23 2.1664(9) . ? Mg1 C21 2.4435(11) . ? Mg1 Mg2 3.6106(6) . ? Mg2 O17 2.0994(7) 4_465 ? Mg2 O17 2.0994(8) 2_655 ? Mg2 O23 2.0999(8) . ? Mg2 O23 2.0999(8) 3_565 ? Mg2 O2 2.1052(8) 3_565 ? Mg2 O2 2.1053(8) . ? Mg2 Mg1 3.6106(6) 3_565 ? C1 O2 1.2551(13) . ? C1 O3 1.2575(14) . ? C1 C4 1.5162(14) . ? C4 C9 1.3910(15) . ? C4 C5 1.3936(15) . ? C5 C6 1.3948(15) . ? C6 C7 1.3980(16) . ? C7 C8 1.3976(15) . ? C7 C10 1.4885(14) . ? C8 C9 1.3970(14) . ? C10 C15 1.3971(16) . ? C10 C11 1.4047(15) . ? C11 C12 1.3939(15) . ? C12 C13 1.3916(15) . ? C13 C14 1.3941(15) . ? C13 C16 1.5169(14) . ? C14 C15 1.3940(15) . ? C16 O18 1.2559(13) . ? C16 O17 1.2585(13) . ? O17 Mg2 2.0994(7) 2_645 ? O18 Mg1 2.0442(9) 2_645 ? C21 O22 1.2517(14) . ? C21 O23 1.2796(13) . ? C21 C24 1.4909(14) . ? C24 C25 1.3857(16) . ? C24 C29 1.3927(15) . ? C25 C26 1.3913(15) . ? C26 C27 1.4002(15) . ? C27 C28 1.3982(16) . ? C27 C27 1.491(2) 3_465 ? C28 C29 1.3906(14) . ? O30 C30 1.2504(15) . ? C30 N32 1.3243(18) . ? C30 C31 1.510(2) . ? N32 C33 1.460(2) . ? N32 C34 1.4670(18) . ? O40 C40 1.2450(16) . ? C40 N42 1.3262(18) . ? C40 C41 1.505(2) . ? N42 C44 1.459(2) . ? N42 C43 1.459(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 O3 Mg1 O40 95.69(4) . . ? O3 Mg1 O18 93.05(4) . 2_655 ? O40 Mg1 O18 87.36(4) . 2_655 ? O3 Mg1 O30 87.17(4) . . ? O40 Mg1 O30 91.48(4) . . ? O18 Mg1 O30 178.84(4) 2_655 . ? O3 Mg1 O22 156.35(4) . . ? O40 Mg1 O22 107.12(4) . . ? O18 Mg1 O22 94.15(4) 2_655 . ? O30 Mg1 O22 86.09(4) . . ? O3 Mg1 O23 95.30(4) . . ? O40 Mg1 O23 168.93(4) . . ? O18 Mg1 O23 93.36(3) 2_655 . ? O30 Mg1 O23 87.75(3) . . ? O22 Mg1 O23 61.81(3) . . ? O3 Mg1 C21 125.67(4) . . ? O40 Mg1 C21 137.50(4) . . ? O18 Mg1 C21 98.52(4) 2_655 . ? O30 Mg1 C21 82.26(4) . . ? O22 Mg1 C21 30.81(3) . . ? O23 Mg1 C21 31.50(3) . . ? O3 Mg1 Mg2 73.02(3) . . ? O40 Mg1 Mg2 156.21(3) . . ? O18 Mg1 Mg2 72.77(3) 2_655 . ? O30 Mg1 Mg2 108.37(3) . . ? O22 Mg1 Mg2 87.69(3) . . ? O23 Mg1 Mg2 31.63(2) . . ? C21 Mg1 Mg2 60.67(3) . . ? O17 Mg2 O17 180.0 4_465 2_655 ? O17 Mg2 O23 89.32(3) 4_465 . ? O17 Mg2 O23 90.68(3) 2_655 . ? O17 Mg2 O23 90.68(3) 4_465 3_565 ? O17 Mg2 O23 89.32(3) 2_655 3_565 ? O23 Mg2 O23 180.00(4) . 3_565 ? O17 Mg2 O2 89.64(3) 4_465 3_565 ? O17 Mg2 O2 90.36(3) 2_655 3_565 ? O23 Mg2 O2 88.26(3) . 3_565 ? O23 Mg2 O2 91.74(3) 3_565 3_565 ? O17 Mg2 O2 90.36(3) 4_465 . ? O17 Mg2 O2 89.64(3) 2_655 . ? O23 Mg2 O2 91.74(3) . . ? O23 Mg2 O2 88.26(3) 3_565 . ? O2 Mg2 O2 180.00(3) 3_565 . ? O17 Mg2 Mg1 68.81(2) 4_465 3_565 ? O17 Mg2 Mg1 111.19(2) 2_655 3_565 ? O23 Mg2 Mg1 147.24(2) . 3_565 ? O23 Mg2 Mg1 32.76(2) 3_565 3_565 ? O2 Mg2 Mg1 68.29(2) 3_565 3_565 ? O2 Mg2 Mg1 111.71(2) . 3_565 ? O17 Mg2 Mg1 111.19(2) 4_465 . ? O17 Mg2 Mg1 68.81(2) 2_655 . ? O23 Mg2 Mg1 32.76(2) . . ? O23 Mg2 Mg1 147.24(2) 3_565 . ? O2 Mg2 Mg1 111.71(2) 3_565 . ? O2 Mg2 Mg1 68.29(2) . . ? Mg1 Mg2 Mg1 180.0 3_565 . ? O2 C1 O3 126.59(10) . . ? O2 C1 C4 118.37(9) . . ? O3 C1 C4 115.04(9) . . ? C1 O2 Mg2 137.48(7) . . ? C1 O3 Mg1 134.35(8) . . ? C9 C4 C5 118.75(9) . . ? C9 C4 C1 121.04(9) . . ? C5 C4 C1 120.18(10) . . ? C4 C5 C6 120.61(10) . . ? C5 C6 C7 120.89(10) . . ? C8 C7 C6 118.17(9) . . ? C8 C7 C10 121.07(10) . . ? C6 C7 C10 120.68(10) . . ? C9 C8 C7 120.79(10) . . ? C4 C9 C8 120.69(10) . . ? C15 C10 C11 118.07(9) . . ? C15 C10 C7 121.70(10) . . ? C11 C10 C7 120.23(10) . . ? C12 C11 C10 120.76(10) . . ? C13 C12 C11 120.75(10) . . ? C12 C13 C14 118.72(9) . . ? C12 C13 C16 121.08(9) . . ? C14 C13 C16 120.08(10) . . ? C15 C14 C13 120.73(10) . . ? C14 C15 C10 120.90(10) . . ? O18 C16 O17 126.61(9) . . ? O18 C16 C13 115.98(9) . . ? O17 C16 C13 117.39(9) . . ? C16 O17 Mg2 136.12(7) . 2_645 ? C16 O18 Mg1 132.42(8) . 2_645 ? O22 C21 O23 121.10(9) . . ? O22 C21 C24 119.30(9) . . ? O23 C21 C24 119.39(9) . . ? O22 C21 Mg1 60.36(5) . . ? O23 C21 Mg1 62.22(5) . . ? C24 C21 Mg1 163.02(7) . . ? C21 O22 Mg1 88.83(6) . . ? C21 O23 Mg2 143.43(7) . . ? C21 O23 Mg1 86.28(6) . . ? Mg2 O23 Mg1 115.61(3) . . ? C25 C24 C29 119.21(10) . . ? C25 C24 C21 119.79(9) . . ? C29 C24 C21 120.91(10) . . ? C24 C25 C26 120.41(10) . . ? C25 C26 C27 121.32(11) . . ? C28 C27 C26 117.36(10) . . ? C28 C27 C27 121.43(12) . 3_465 ? C26 C27 C27 121.21(13) . 3_465 ? C29 C28 C27 121.50(10) . . ? C28 C29 C24 120.12(10) . . ? C30 O30 Mg1 129.72(9) . . ? O30 C30 N32 121.29(13) . . ? O30 C30 C31 119.89(13) . . ? N32 C30 C31 118.82(13) . . ? C30 N32 C33 118.07(12) . . ? C30 N32 C34 123.76(13) . . ? C33 N32 C34 117.94(14) . . ? C40 O40 Mg1 133.21(9) . . ? O40 C40 N42 119.98(13) . . ? O40 C40 C41 120.51(14) . . ? N42 C40 C41 119.51(14) . . ? C40 N42 C44 124.19(15) . . ? C40 N42 C43 117.41(13) . . ? C44 N42 C43 118.38(15) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 31.94 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.863 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.059 #===END data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 641078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H22 Mg N2 O8, (C4 H9 N O)0.33' _chemical_formula_sum 'C18.33 H25 Mg N2.33 O8.33' _chemical_formula_weight 435.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 16.5986(19) _cell_length_b 16.5986(19) _cell_length_c 43.035(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10268(2) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 73632 _cell_measurement_theta_min 3.0722 _cell_measurement_theta_max 70.7665 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4140 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95712 _exptl_absorpt_correction_T_max 1.03004 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) (compiled May 11 2006,17:41:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81984 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0044 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 70.83 _reflns_number_total 2178 _reflns_number_gt 2074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 O(10) and O(20) dma solvent molecules were found to be disordered. For O(10) this disorder was handled by the refinement of two overlapping idealised orientations for which the bond lengths and angles were restrained either to set values or to be the same as their chemcial equivalents in the other orientation. The molecules were also restrained to be flat, and the isotropic thermal parameters of the equivalent atoms of the different orientations were restrained to be the same. For the O(20) molecule, which is adjacent to a bar 3 position, this disorder was handled by the refinement of a single, idealised, 1/6 occupancy, orientation for which the bond lengths and angles were restrained to set values. (The other overlapping orientations would automatically be generated from this one orientation by the action of the bar 3 symmetry operation. The unique molecule was restrained to be flat, and, due to the extensive overlap, all of the non-hydrogen atoms were lightly restrained to have the same isotropic thermal parameter. ; _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^)+(0.0745P)^2^+21.3460P] 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 2178 _refine_ls_number_parameters 185 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.094 _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 Mg Mg 0.6667 0.01073(5) 0.0833 0.0266(3) Uani 1 2 d SD . . O1 O 0.74170(9) 0.15905(9) 0.07851(4) 0.0383(4) Uani 1 1 d . . . O2 O 0.77600(9) -0.00943(9) 0.07570(4) 0.0412(4) Uani 1 1 d . . . O3 O 0.75009(10) -0.15164(10) 0.08544(6) 0.0704(7) Uani 1 1 d D . . H3 H 0.6890(10) -0.176(4) 0.0894(14) 0.08(2) Uiso 0.50 1 d PD . . C1 C 0.6667 0.15870(14) 0.0833 0.0310(6) Uani 1 2 d S . . C2 C 0.6667 0.24935(14) 0.0833 0.0291(5) Uani 1 2 d S . . C3 C 0.75045(14) 0.3333 0.0833 0.0299(5) Uani 1 2 d S . . H3A H 0.8077 0.3333 0.0833 0.036 Uiso 1 2 calc SR . . C4 C 0.80268(12) -0.06523(12) 0.08085(5) 0.0354(5) Uani 1 1 d . . . C5 C 0.90512(12) -0.03182(13) 0.08161(5) 0.0323(4) Uani 1 1 d . . . C6 C 0.93696(12) -0.09497(11) 0.08175(5) 0.0326(4) Uani 1 1 d . . . H6A H 0.8938 -0.1599 0.0820 0.039 Uiso 1 1 calc R . . O10 O 0.70266(13) 0.02358(12) 0.12906(4) 0.0564(5) Uani 1 1 d D . . C10 C 0.6869(4) 0.0296(5) 0.15610(9) 0.0586(15) Uani 0.695(14) 1 d PDU A 1 C11 C 0.5979(5) 0.0302(8) 0.16476(13) 0.099(2) Uani 0.695(14) 1 d PDU A 1 H11A H 0.5630 0.0257 0.1458 0.148 Uiso 0.695(14) 1 calc PR A 1 H11B H 0.6139 0.0881 0.1757 0.148 Uiso 0.695(14) 1 calc PR A 1 H11C H 0.5596 -0.0229 0.1783 0.148 Uiso 0.695(14) 1 calc PR A 1 N12 N 0.7441(4) 0.0384(6) 0.17868(8) 0.0682(14) Uani 0.695(14) 1 d PDU A 1 C13 C 0.8303(5) 0.0430(7) 0.17122(14) 0.080(2) Uani 0.695(14) 1 d PDU A 1 H13A H 0.8213 -0.0200 0.1706 0.120 Uiso 0.695(14) 1 calc PR A 1 H13B H 0.8768 0.0796 0.1871 0.120 Uiso 0.695(14) 1 calc PR A 1 H13C H 0.8520 0.0726 0.1509 0.120 Uiso 0.695(14) 1 calc PR A 1 C14 C 0.7280(5) 0.0417(8) 0.21193(11) 0.103(3) Uani 0.695(14) 1 d PDU A 1 H14A H 0.6724 0.0471 0.2150 0.155 Uiso 0.695(14) 1 calc PR A 1 H14B H 0.7819 0.0956 0.2212 0.155 Uiso 0.695(14) 1 calc PR A 1 H14C H 0.7190 -0.0153 0.2219 0.155 Uiso 0.695(14) 1 calc PR A 1 C10' C 0.6693(8) 0.0046(9) 0.15529(19) 0.043(3) Uiso 0.305(14) 1 d PDU A 2 C11' C 0.5699(8) -0.0198(10) 0.1607(3) 0.073(4) Uiso 0.305(14) 1 d PDU A 2 H11D H 0.5482 0.0017 0.1431 0.109 Uiso 0.305(14) 1 calc PR A 2 H11E H 0.5663 0.0105 0.1798 0.109 Uiso 0.305(14) 1 calc PR A 2 H11F H 0.5307 -0.0874 0.1629 0.109 Uiso 0.305(14) 1 calc PR A 2 N12' N 0.7177(9) 0.0026(8) 0.1788(2) 0.069(4) Uiso 0.305(14) 1 d PDU A 2 C13' C 0.8137(12) 0.0258(16) 0.1734(5) 0.138(11) Uiso 0.305(14) 1 d PDU A 2 H13D H 0.8250 -0.0195 0.1843 0.207 Uiso 0.305(14) 1 d PR A 2 H13E H 0.8560 0.0883 0.1815 0.207 Uiso 0.305(14) 1 d PR A 2 H13F H 0.8247 0.0239 0.1511 0.207 Uiso 0.305(14) 1 d PR A 2 C14' C 0.6892(12) -0.0157(11) 0.2112(2) 0.078(4) Uiso 0.305(14) 1 d PDU A 2 H14D H 0.6841 0.0364 0.2197 0.117 Uiso 0.305(14) 1 calc PR A 2 H14E H 0.7357 -0.0228 0.2231 0.117 Uiso 0.305(14) 1 calc PR A 2 H14F H 0.6289 -0.0730 0.2127 0.117 Uiso 0.305(14) 1 calc PR A 2 O20 O 0.984(4) -0.1119(16) -0.0008(4) 0.117(6) Uiso 0.17 1 d PDU B -1 C20 C 0.9822(15) -0.0367(8) -0.0003(5) 0.068(5) Uiso 0.17 1 d PDU B -1 C21 C 0.8905(15) -0.039(3) -0.0010(4) 0.076(5) Uiso 0.17 1 d PDU B -1 H21A H 0.8877 -0.0057 -0.0195 0.114 Uiso 0.17 1 calc PR B -1 H21B H 0.8846 -0.0080 0.0176 0.114 Uiso 0.17 1 calc PR B -1 H21C H 0.8395 -0.1032 -0.0016 0.114 Uiso 0.17 1 calc PR B -1 N22 N 1.0601(12) 0.0441(13) 0.0003(5) 0.098(6) Uiso 0.17 1 d PDU B -1 C23 C 1.1467(18) 0.041(4) 0.0007(7) 0.133(11) Uiso 0.17 1 d PDU B -1 H23A H 1.1864 0.0790 0.0178 0.200 Uiso 0.17 1 d PR B -1 H23B H 1.1796 0.0648 -0.0191 0.200 Uiso 0.17 1 d PR B -1 H23C H 1.1318 -0.0236 0.0035 0.200 Uiso 0.17 1 d PR B -1 C24 C 1.066(3) 0.1351(13) 0.0007(6) 0.115(11) Uiso 0.17 1 d PDU B -1 H24A H 1.0031 0.1265 -0.0004 0.172 Uiso 0.17 1 calc PR B -1 H24B H 1.1024 0.1718 -0.0172 0.172 Uiso 0.17 1 calc PR B -1 H24C H 1.0960 0.1678 0.0200 0.172 Uiso 0.17 1 calc PR B -1 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 Mg 0.0191(4) 0.0185(3) 0.0425(5) -0.00105(15) -0.0021(3) 0.0096(2) O1 0.0229(7) 0.0223(7) 0.0710(10) 0.0004(6) 0.0015(6) 0.0123(5) O2 0.0217(7) 0.0267(7) 0.0786(10) 0.0043(6) 0.0037(6) 0.0146(6) O3 0.0173(7) 0.0228(7) 0.169(2) 0.0134(9) 0.0032(9) 0.0084(6) C1 0.0245(12) 0.0222(9) 0.0472(14) -0.0012(5) -0.0024(10) 0.0123(6) C2 0.0247(12) 0.0226(9) 0.0408(13) 0.0008(5) 0.0017(10) 0.0124(6) C3 0.0218(9) 0.0269(12) 0.0426(14) 0.0014(10) 0.0007(5) 0.0134(6) C4 0.0202(9) 0.0226(9) 0.0631(12) -0.0014(8) -0.0004(8) 0.0103(7) C5 0.0191(9) 0.0260(9) 0.0520(11) 0.0004(7) 0.0002(7) 0.0114(7) C6 0.0223(8) 0.0170(8) 0.0551(11) 0.0010(7) 0.0000(7) 0.0072(7) O10 0.0622(11) 0.0592(11) 0.0450(10) -0.0013(7) -0.0109(8) 0.0282(9) C10 0.058(3) 0.048(3) 0.056(3) 0.0023(19) -0.0069(18) 0.016(2) C11 0.060(3) 0.151(7) 0.080(3) 0.006(4) -0.008(2) 0.049(4) N12 0.055(2) 0.099(4) 0.0486(19) -0.006(2) -0.0086(16) 0.037(3) C13 0.068(3) 0.126(5) 0.066(3) -0.008(3) -0.016(2) 0.063(3) C14 0.084(4) 0.172(7) 0.059(3) -0.013(3) -0.012(2) 0.068(5) _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 Mg O2 2.0298(14) . ? Mg O2 2.0298(14) 18_654 ? Mg O10 2.0364(16) . ? Mg O10 2.0365(16) 18_654 ? Mg O1 2.1422(14) 18_654 ? Mg O1 2.1423(14) . ? O1 C1 1.2597(17) . ? O2 C4 1.230(2) . ? O3 C4 1.267(2) . ? C1 O1 1.2597(17) 18_654 ? C1 C2 1.505(3) . ? C2 C3 1.3924(16) . ? C2 C3 1.3924(16) 3_665 ? C3 C2 1.3924(16) 2_655 ? C4 C5 1.502(2) . ? C5 C6 1.388(2) 3_765 ? C5 C6 1.390(2) . ? C6 C5 1.388(2) 2_645 ? O10 C10 1.208(5) . ? O10 C10' 1.227(9) . ? C10 N12 1.314(5) . ? C10 C11 1.529(7) . ? N12 C13 1.432(6) . ? N12 C14 1.462(6) . ? C10' N12' 1.301(11) . ? C10' C11' 1.506(12) . ? N12' C14' 1.457(12) . ? N12' C13' 1.460(14) . ? O20 C20 1.266(9) . ? C20 N22 1.318(9) . ? C20 C21 1.508(10) . ? N22 C23 1.464(10) . ? N22 C24 1.465(10) . ? 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 Mg O2 104.56(8) . 18_654 ? O2 Mg O10 86.22(7) . . ? O2 Mg O10 90.84(7) 18_654 . ? O2 Mg O10 90.84(7) . 18_654 ? O2 Mg O10 86.21(7) 18_654 18_654 ? O10 Mg O10 175.19(11) . 18_654 ? O2 Mg O1 158.55(6) . 18_654 ? O2 Mg O1 96.88(5) 18_654 18_654 ? O10 Mg O1 94.03(7) . 18_654 ? O10 Mg O1 90.09(7) 18_654 18_654 ? O2 Mg O1 96.88(5) . . ? O2 Mg O1 158.56(6) 18_654 . ? O10 Mg O1 90.10(7) . . ? O10 Mg O1 94.03(7) 18_654 . ? O1 Mg O1 61.69(7) 18_654 . ? C1 O1 Mg 88.48(11) . . ? C4 O2 Mg 141.54(13) . . ? O1 C1 O1 121.4(2) 18_654 . ? O1 C1 C2 119.32(11) 18_654 . ? O1 C1 C2 119.32(11) . . ? O1 C1 Mg 60.68(11) 18_654 . ? O1 C1 Mg 60.68(11) . . ? C2 C1 Mg 180.0 . . ? C3 C2 C3 119.8(2) . 3_665 ? C3 C2 C1 120.12(12) . . ? C3 C2 C1 120.12(12) 3_665 . ? C2 C3 C2 120.2(2) . 2_655 ? O2 C4 O3 125.21(17) . . ? O2 C4 C5 119.55(16) . . ? O3 C4 C5 115.24(16) . . ? C6 C5 C6 120.08(16) 3_765 . ? C6 C5 C4 119.34(15) 3_765 . ? C6 C5 C4 120.58(16) . . ? C5 C6 C5 119.92(16) 2_645 . ? C10 O10 C10' 17.5(6) . . ? C10 O10 Mg 151.1(3) . . ? C10' O10 Mg 142.2(5) . . ? O10 C10 N12 123.2(5) . . ? O10 C10 C11 119.0(4) . . ? N12 C10 C11 117.7(4) . . ? C10 N12 C13 119.2(4) . . ? C10 N12 C14 126.4(4) . . ? C13 N12 C14 114.4(4) . . ? O10 C10' N12' 121.0(9) . . ? O10 C10' C11' 120.4(8) . . ? N12' C10' C11' 118.6(9) . . ? C10' N12' C14' 127.6(10) . . ? C10' N12' C13' 118.6(11) . . ? C14' N12' C13' 113.7(11) . . ? O20 C20 N22 120.5(14) . . ? O20 C20 C21 120.2(12) . . ? N22 C20 C21 119.3(12) . . ? C20 N22 C23 116.5(13) . . ? C20 N22 C24 125.0(14) . . ? C23 N22 C24 118.5(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 70.83 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.348 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.054 #===END