data_publication_text _publ_requested_journal 'Inorg. Chem.' _publ_contact_author_name 'Kenneth W. Henderson' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 USA ; _publ_contact_author_email khenders@nd.edu _publ_contact_author_phone 011(574)6318025 _publ_contact_author_fax 011(574)6316652 loop_ _publ_author_name _publ_author_address 'Rood, Jeffrey A.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 USA ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 USA ; 'Henderson, Kenneth W.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 USA ; data_jr33 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H6 Mg3 O12, O.5(C4 H10 O)' _chemical_formula_sum 'C8 H11 Mg3 O12.50' _chemical_formula_weight 380.10 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3805(4) _cell_length_b 9.8406(3) _cell_length_c 14.5057(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.429(2) _cell_angle_gamma 90.00 _cell_volume 1624.00(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8677 _cell_measurement_theta_min 2.3027 _cell_measurement_theta_max 34.3137 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ; Blessing, R.H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany ; _exptl_special_details ; CheckCIF prefers Z=2 however we have kept Z=4 to keep consistent with the others in this series. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-ApexII CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49843 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 34.40 _reflns_number_total 6798 _reflns_number_gt 5461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)' _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^)+(0.0479P)^2^+0.7929P] 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 6798 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.433 _refine_ls_restrained_S_all 1.433 _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 0.25647(4) 0.41905(5) 0.63437(4) 0.00875(10) Uani 1 1 d . . . Mg2 Mg 0.0000 0.5000 0.5000 0.00987(14) Uani 1 2 d S . . Mg3 Mg 0.26071(5) 0.10922(5) 0.68940(4) 0.00920(10) Uani 1 1 d . . . Mg4 Mg 0.5000 0.5000 0.5000 0.01028(14) Uani 1 2 d S . . O1 O 0.13109(9) 0.50375(10) 0.71982(8) 0.01056(19) Uani 1 1 d . . . O2 O -0.03690(10) 0.50172(12) 0.63788(8) 0.0152(2) Uani 1 1 d . . . O3 O 0.15722(9) 0.24187(10) 0.61046(8) 0.01070(19) Uani 1 1 d . . . O4 O 0.01837(10) 0.29229(11) 0.50396(8) 0.0144(2) Uani 1 1 d . . . O5 O 0.39986(9) 0.34726(10) 0.56333(8) 0.01102(19) Uani 1 1 d . . . O6 O 0.39008(10) 0.12511(11) 0.59708(8) 0.0131(2) Uani 1 1 d . . . O7 O 0.30748(9) 0.29732(10) 0.74687(7) 0.01045(19) Uani 1 1 d . . . O8 O 0.18714(10) -0.05988(11) 0.63259(8) 0.0132(2) Uani 1 1 d . . . O9 O 0.18277(9) 0.52389(11) 0.52466(8) 0.01094(19) Uani 1 1 d . . . O10 O 0.34981(10) 0.60195(11) 0.46589(9) 0.0147(2) Uani 1 1 d . . . O11 O 0.34829(9) 0.57942(10) 0.69661(8) 0.01091(19) Uani 1 1 d . . . O12 O 0.51428(10) 0.61049(12) 0.61969(9) 0.0157(2) Uani 1 1 d . . . C1 C 0.02053(13) 0.51646(15) 0.71069(11) 0.0129(3) Uani 1 1 d . . . H1 H -0.0208 0.5387 0.7631 0.015 Uiso 1 1 calc R . . C2 C 0.07663(14) 0.21114(14) 0.55138(11) 0.0139(3) Uani 1 1 d . . . H2 H 0.0602 0.1193 0.5432 0.017 Uiso 1 1 calc R . . C3 C 0.43339(13) 0.22355(14) 0.55705(11) 0.0130(3) Uani 1 1 d . . . H3 H 0.4961 0.2060 0.5189 0.016 Uiso 1 1 calc R . . C4 C 0.17124(13) -0.17257(14) 0.66875(11) 0.0123(3) Uani 1 1 d . . . H4 H 0.1411 -0.2412 0.6310 0.015 Uiso 1 1 calc R . . C5 C 0.24174(13) 0.59788(15) 0.46970(11) 0.0129(3) Uani 1 1 d . . . H5 H 0.1993 0.6534 0.4291 0.015 Uiso 1 1 calc R . . C6 C 0.44822(14) 0.63435(15) 0.68384(11) 0.0141(3) Uani 1 1 d . . . H6 H 0.4736 0.6985 0.7270 0.017 Uiso 1 1 calc R . . O1S O 0.7188(4) 0.1645(4) 0.7007(3) 0.0510(10) Uani 0.50 1 d P . . C4S C 0.6485(4) 0.3675(5) 0.7860(4) 0.0364(10) Uani 0.50 1 d P . . H4S1 H 0.6528 0.4205 0.7306 0.055 Uiso 0.50 1 calc PR A . H4S2 H 0.6654 0.4244 0.8385 0.055 Uiso 0.50 1 calc PR . . H4S3 H 0.5710 0.3301 0.7907 0.055 Uiso 0.50 1 calc PR . . C3S C 0.7364(4) 0.2545(5) 0.7833(5) 0.0441(13) Uani 0.50 1 d P A . H3S1 H 0.7305 0.2002 0.8388 0.053 Uiso 0.50 1 calc PR . . H3S2 H 0.8149 0.2929 0.7826 0.053 Uiso 0.50 1 calc PR . . C2S C 0.7802(7) 0.0494(8) 0.6928(5) 0.0274(17) Uani 0.278(6) 1 d P A 1 H2S1 H 0.7747 -0.0024 0.7494 0.033 Uiso 0.278(6) 1 calc PR A 1 H2S2 H 0.8623 0.0716 0.6845 0.033 Uiso 0.278(6) 1 calc PR A 1 C1S C 0.7373(9) -0.0363(12) 0.6134(6) 0.043(2) Uani 0.278(6) 1 d P A 1 H1S1 H 0.6542 -0.0503 0.6177 0.064 Uiso 0.278(6) 1 calc PR A 1 H1S2 H 0.7768 -0.1225 0.6151 0.064 Uiso 0.278(6) 1 calc PR A 1 H1S3 H 0.7536 0.0090 0.5565 0.064 Uiso 0.278(6) 1 calc PR A 1 C1X C 0.8623(8) -0.0292(9) 0.6359(8) 0.028(2) Uani 0.222(6) 1 d P A 2 H1X1 H 0.9226 0.0169 0.6713 0.042 Uiso 0.222(6) 1 calc PR A 2 H1X2 H 0.8912 -0.0511 0.5761 0.042 Uiso 0.222(6) 1 calc PR A 2 H1X3 H 0.8408 -0.1112 0.6670 0.042 Uiso 0.222(6) 1 calc PR A 2 C2X C 0.7630(10) 0.0559(11) 0.6260(8) 0.033(2) Uani 0.222(6) 1 d P A 2 H2X1 H 0.6969 -0.0042 0.6139 0.039 Uiso 0.222(6) 1 calc PR A 2 H2X2 H 0.7740 0.1070 0.5697 0.039 Uiso 0.222(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 0.0094(2) 0.00689(19) 0.0099(2) -0.00006(16) -0.00119(17) 0.00028(16) Mg2 0.0090(3) 0.0097(3) 0.0108(3) 0.0007(2) -0.0019(2) -0.0001(2) Mg3 0.0105(2) 0.00688(19) 0.0102(2) 0.00085(16) -0.00131(17) 0.00002(16) Mg4 0.0096(3) 0.0095(3) 0.0118(3) 0.0012(2) 0.0007(2) -0.0007(2) O1 0.0095(4) 0.0099(4) 0.0122(5) -0.0018(3) -0.0020(4) 0.0003(3) O2 0.0117(5) 0.0216(5) 0.0120(5) 0.0000(4) -0.0024(4) -0.0008(4) O3 0.0109(4) 0.0093(4) 0.0117(5) 0.0007(3) -0.0035(4) -0.0004(3) O4 0.0151(5) 0.0108(4) 0.0171(5) 0.0005(4) -0.0065(4) 0.0009(4) O5 0.0116(4) 0.0086(4) 0.0129(5) 0.0010(4) 0.0011(4) 0.0003(3) O6 0.0155(5) 0.0091(4) 0.0150(5) 0.0015(4) 0.0024(4) -0.0001(3) O7 0.0130(4) 0.0080(4) 0.0102(5) -0.0003(3) -0.0023(4) -0.0003(3) O8 0.0184(5) 0.0090(4) 0.0122(5) 0.0013(4) -0.0026(4) -0.0020(4) O9 0.0102(4) 0.0114(4) 0.0112(5) 0.0022(4) -0.0009(4) -0.0004(3) O10 0.0109(5) 0.0150(5) 0.0183(5) 0.0044(4) 0.0000(4) -0.0007(4) O11 0.0106(4) 0.0093(4) 0.0129(5) -0.0007(3) 0.0006(4) -0.0010(3) O12 0.0147(5) 0.0178(5) 0.0146(5) -0.0019(4) 0.0023(4) -0.0041(4) C1 0.0114(6) 0.0150(6) 0.0122(6) -0.0007(5) 0.0001(5) 0.0002(5) C2 0.0150(6) 0.0088(5) 0.0176(7) -0.0011(5) -0.0057(5) -0.0007(5) C3 0.0132(6) 0.0110(5) 0.0148(7) 0.0006(5) 0.0029(5) 0.0011(5) C4 0.0157(6) 0.0092(5) 0.0118(6) -0.0010(4) -0.0024(5) -0.0006(4) C5 0.0123(6) 0.0131(5) 0.0132(6) 0.0025(5) -0.0015(5) 0.0011(5) C6 0.0143(6) 0.0132(6) 0.0149(7) -0.0023(5) 0.0009(5) -0.0043(5) O1S 0.081(3) 0.045(2) 0.0267(18) 0.0032(15) 0.0034(19) -0.018(2) C4S 0.035(2) 0.035(2) 0.039(3) -0.0012(19) -0.0017(19) 0.0018(18) C3S 0.025(2) 0.037(2) 0.070(4) 0.023(2) -0.007(2) -0.0002(17) C2S 0.028(3) 0.032(3) 0.022(4) 0.000(3) -0.003(3) -0.001(3) C1S 0.045(5) 0.057(6) 0.027(4) -0.016(4) 0.012(4) -0.011(4) C1X 0.023(4) 0.024(4) 0.039(5) 0.009(4) 0.016(4) 0.000(3) C2X 0.040(5) 0.029(5) 0.029(5) 0.008(4) 0.008(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O9 2.0576(12) . ? Mg1 O5 2.0756(12) . ? Mg1 O11 2.0858(11) . ? Mg1 O1 2.0869(12) . ? Mg1 O7 2.0947(12) . ? Mg1 O3 2.1016(11) . ? Mg1 Mg3 3.1518(7) . ? Mg1 Mg3 3.1780(7) 2_556 ? Mg1 Mg4 3.5191(5) . ? Mg1 Mg2 3.5593(5) . ? Mg2 O2 2.0540(12) . ? Mg2 O2 2.0540(12) 3_566 ? Mg2 O4 2.0552(11) 3_566 ? Mg2 O4 2.0553(11) . ? Mg2 O9 2.1149(11) . ? Mg2 O9 2.1149(11) 3_566 ? Mg2 Mg1 3.5593(5) 3_566 ? Mg3 O6 2.0208(13) . ? Mg3 O8 2.0285(12) . ? Mg3 O1 2.0607(11) 2_546 ? Mg3 O3 2.0821(11) . ? Mg3 O7 2.0934(11) . ? Mg3 O11 2.1122(13) 2_546 ? Mg3 Mg1 3.1781(7) 2_546 ? Mg4 O10 2.0324(11) 3_666 ? Mg4 O10 2.0324(11) . ? Mg4 O12 2.0516(12) . ? Mg4 O12 2.0516(12) 3_666 ? Mg4 O5 2.1104(11) 3_666 ? Mg4 O5 2.1105(11) . ? Mg4 Mg1 3.5191(5) 3_666 ? O1 C1 1.2681(18) . ? O1 Mg3 2.0607(11) 2_556 ? O2 C1 1.2367(18) . ? O3 C2 1.2759(17) . ? O4 C2 1.2360(18) . ? O5 C3 1.2797(17) . ? O6 C3 1.2381(18) . ? O7 C4 1.2767(18) 2_556 ? O8 C4 1.2419(17) . ? O9 C5 1.2817(19) . ? O10 C5 1.2332(19) . ? O11 C6 1.2768(18) . ? O11 Mg3 2.1121(13) 2_556 ? O12 C6 1.233(2) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 O7 1.2766(18) 2_546 ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? O1S C2S 1.338(9) . ? O1S C3S 1.498(8) . ? O1S C2X 1.612(12) . ? C4S C3S 1.497(7) . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C2S C1S 1.500(12) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C1X C2X 1.411(14) . ? C1X H1X1 0.9600 . ? C1X H1X2 0.9600 . ? C1X H1X3 0.9600 . ? C2X H2X1 0.9700 . ? C2X H2X2 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Mg1 O5 95.57(5) . . ? O9 Mg1 O11 98.37(5) . . ? O5 Mg1 O11 94.64(5) . . ? O9 Mg1 O1 89.29(5) . . ? O5 Mg1 O1 171.30(5) . . ? O11 Mg1 O1 77.49(4) . . ? O9 Mg1 O7 171.48(5) . . ? O5 Mg1 O7 89.20(5) . . ? O11 Mg1 O7 88.25(5) . . ? O1 Mg1 O7 86.90(5) . . ? O9 Mg1 O3 94.66(5) . . ? O5 Mg1 O3 93.54(5) . . ? O11 Mg1 O3 163.85(5) . . ? O1 Mg1 O3 93.25(5) . . ? O7 Mg1 O3 77.96(4) . . ? O9 Mg1 Mg3 133.18(4) . . ? O5 Mg1 Mg3 77.83(3) . . ? O11 Mg1 Mg3 128.17(4) . . ? O1 Mg1 Mg3 104.02(4) . . ? O7 Mg1 Mg3 41.17(3) . . ? O3 Mg1 Mg3 40.89(3) . . ? O9 Mg1 Mg3 107.15(4) . 2_556 ? O5 Mg1 Mg3 131.66(4) . 2_556 ? O11 Mg1 Mg3 41.11(3) . 2_556 ? O1 Mg1 Mg3 39.68(3) . 2_556 ? O7 Mg1 Mg3 74.42(3) . 2_556 ? O3 Mg1 Mg3 125.28(4) . 2_556 ? Mg3 Mg1 Mg3 111.515(17) . 2_556 ? O9 Mg1 Mg4 76.68(3) . . ? O5 Mg1 Mg4 33.10(3) . . ? O11 Mg1 Mg4 71.06(3) . . ? O1 Mg1 Mg4 142.95(3) . . ? O7 Mg1 Mg4 110.74(4) . . ? O3 Mg1 Mg4 121.59(4) . . ? Mg3 Mg1 Mg4 110.606(17) . . ? Mg3 Mg1 Mg4 112.169(17) 2_556 . ? O9 Mg1 Mg2 31.94(3) . . ? O5 Mg1 Mg2 116.64(4) . . ? O11 Mg1 Mg2 117.57(3) . . ? O1 Mg1 Mg2 70.88(3) . . ? O7 Mg1 Mg2 139.65(4) . . ? O3 Mg1 Mg2 70.45(3) . . ? Mg3 Mg1 Mg2 111.246(17) . . ? Mg3 Mg1 Mg2 104.042(16) 2_556 . ? Mg4 Mg1 Mg2 107.004(14) . . ? O2 Mg2 O2 179.999(13) . 3_566 ? O2 Mg2 O4 89.77(5) . 3_566 ? O2 Mg2 O4 90.24(5) . . ? O2 Mg2 O4 89.76(5) 3_566 . ? O4 Mg2 O4 179.999(5) 3_566 . ? O2 Mg2 O9 93.35(4) . . ? O2 Mg2 O9 86.65(4) 3_566 . ? O4 Mg2 O9 89.61(4) 3_566 . ? O4 Mg2 O9 90.39(4) . . ? O2 Mg2 O9 86.65(4) . 3_566 ? O4 Mg2 O9 89.61(4) . 3_566 ? O9 Mg2 O9 180.00(6) . 3_566 ? O2 Mg2 Mg1 110.28(3) . 3_566 ? O4 Mg2 Mg1 108.62(3) . 3_566 ? O9 Mg2 Mg1 149.03(3) . 3_566 ? O2 Mg2 Mg1 69.72(3) . . ? O2 Mg2 Mg1 110.28(3) 3_566 . ? O4 Mg2 Mg1 108.62(3) 3_566 . ? O4 Mg2 Mg1 71.38(3) . . ? O9 Mg2 Mg1 30.98(3) . . ? O9 Mg2 Mg1 149.02(3) 3_566 . ? Mg1 Mg2 Mg1 180.0 3_566 . ? O6 Mg3 O8 95.42(5) . . ? O6 Mg3 O1 91.65(5) . 2_546 ? O8 Mg3 O1 94.61(5) . 2_546 ? O6 Mg3 O3 89.92(5) . . ? O8 Mg3 O3 93.95(5) . . ? O1 Mg3 O3 171.11(5) 2_546 . ? O6 Mg3 O7 90.76(5) . . ? O8 Mg3 O7 170.19(5) . . ? O1 Mg3 O7 92.81(5) 2_546 . ? O3 Mg3 O7 78.42(4) . . ? O6 Mg3 O11 168.92(5) . 2_546 ? O8 Mg3 O11 87.69(5) . 2_546 ?? O3 Mg3 O11 100.51(5) . 2_546 ? O7 Mg3 O11 87.68(5) . 2_546 ? O6 Mg3 Mg1 76.36(3) . . ? O8 Mg3 Mg1 133.40(4) . . ? O1 Mg3 Mg1 130.86(4) 2_546 . ? O3 Mg3 Mg1 41.35(3) . . ? O7 Mg3 Mg1 41.20(3) . . ? O11 Mg3 Mg1 109.09(3) 2_546 . ? O6 Mg3 Mg1 129.72(4) . 2_546 ? O8 Mg3 Mg1 79.09(4) . 2_546 ? O3 Mg3 Mg1 140.01(4) . 2_546 ? O7 Mg3 Mg1 102.74(4) . 2_546 ? Mg1 Mg3 Mg1 140.58(2) . 2_546 ? O10 Mg4 O10 180.00(7) 3_666 . ? O10 Mg4 O12 90.41(5) 3_666 . ? O10 Mg4 O12 89.59(5) . . ? O10 Mg4 O12 90.41(5) . 3_666 ? O12 Mg4 O12 180.00(5) . 3_666 ? O10 Mg4 O5 90.14(4) . 3_666 ? O12 Mg4 O5 87.63(4) . 3_666 ? O10 Mg4 O5 90.14(4) 3_666 . ? O10 Mg4 O5 89.86(4) . . ? O12 Mg4 O5 92.37(4) . . ? O12 Mg4 O5 87.63(4) 3_666 . ? O5 Mg4 O5 180.0 3_666 . ? O10 Mg4 Mg1 115.00(3) . 3_666 ? O12 Mg4 Mg1 107.57(3) . 3_666 ? O5 Mg4 Mg1 147.52(3) . 3_666 ? O10 Mg4 Mg1 115.00(3) 3_666 . ? O10 Mg4 Mg1 65.00(3) . . ? O12 Mg4 Mg1 72.43(3) . . ? O12 Mg4 Mg1 107.57(3) 3_666 . ? O5 Mg4 Mg1 147.52(3) 3_666 . ? O5 Mg4 Mg1 32.48(3) . . ? Mg1 Mg4 Mg1 180.0 3_666 . ? C1 O1 Mg3 126.34(10) . 2_556 ? C1 O1 Mg1 131.97(10) . . ? Mg3 O1 Mg1 100.03(5) 2_556 . ? C1 O2 Mg2 135.73(11) . . ? C2 O3 Mg3 127.45(9) . . ? C2 O3 Mg1 132.99(10) . . ? Mg3 O3 Mg1 97.76(5) . . ? C2 O4 Mg2 135.31(10) . . ? C3 O5 Mg1 126.78(10) . . ? C3 O5 Mg4 118.77(10) . . ? Mg1 O5 Mg4 114.42(5) . . ? C3 O6 Mg3 132.57(10) . . ? C4 O7 Mg3 128.85(9) 2_556 . ? C4 O7 Mg1 131.03(9) 2_556 . ? Mg3 O7 Mg1 97.63(5) . . ? C4 O8 Mg3 128.61(10) . . ? C5 O9 Mg1 123.80(9) . . ? C5 O9 Mg2 119.07(9) . . ? Mg1 O9 Mg2 117.09(5) . . ? C5 O10 Mg4 143.78(10) . . ? C6 O11 Mg1 134.10(10) . . ? C6 O11 Mg3 126.69(10) . 2_556 ? Mg1 O11 Mg3 98.41(5) . 2_556 ? C6 O12 Mg4 134.62(11) . . ? O2 C1 O1 125.42(15) . . ? O2 C1 H1 117.3 . . ? O1 C1 H1 117.3 . . ? O4 C2 O3 125.96(13) . . ? O4 C2 H2 117.0 . . ? O3 C2 H2 117.0 . . ? O6 C3 O5 126.02(15) . . ? O6 C3 H3 117.0 . . ? O5 C3 H3 117.0 . . ? O8 C4 O7 125.87(13) . 2_546 ? O8 C4 H4 117.1 . . ? O7 C4 H4 117.1 2_546 . ? O10 C5 O9 125.77(14) . . ? O10 C5 H5 117.1 . . ? O9 C5 H5 117.1 . . ? O12 C6 O11 126.22(14) . . ? O12 C6 H6 116.9 . . ? O11 C6 H6 116.9 . . ? C2S O1S C3S 120.6(5) . . ? C2S O1S C2X 37.6(5) . . ? C3S O1S C2X 153.0(6) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C4S C3S O1S 112.6(4) . . ? C4S C3S H3S1 109.1 . . ? O1S C3S H3S1 109.1 . . ? C4S C3S H3S2 109.1 . . ? O1S C3S H3S2 109.1 . . ? H3S1 C3S H3S2 107.8 . . ? O1S C2S C1S 112.4(7) . . ? O1S C2S H2S1 109.1 . . ? C1S C2S H2S1 109.1 . . ? O1S C2S H2S2 109.1 . . ? C1S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 107.8 . . ? C2X C1X H1X1 109.5 . . ? C2X C1X H1X2 109.5 . . ? H1X1 C1X H1X2 109.5 . . ? C2X C1X H1X3 109.5 . . ? H1X1 C1X H1X3 109.5 . . ? H1X2 C1X H1X3 109.5 . . ? C1X C2X O1S 126.0(9) . . ? C1X C2X H2X1 105.8 . . ? O1S C2X H2X1 105.8 . . ? C1X C2X H2X2 105.8 . . ? O1S C2X H2X2 105.8 . . ? H2X1 C2X H2X2 106.2 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 34.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.629 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.103 _chemical_compound_source Synthesized _exptl_crystal_recrystallization_method 'From DMF at 110 C'