# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Erhard Kemnitz' 'Anton Dimitrov' 'Michael Feist' 'Anja Lehmann' 'Gudrun Scholz' 'Sergey Troyanov' 'Stefan Wuttke' _publ_contact_author_name 'Erhard Kemnitz' _publ_contact_author_email ERHARD.KEMNITZ@CHEMIE.HU-BERLIN.DE _publ_section_title ; Investigation of the fluorolysis of magnesium methoxide ; # Attachment 'comp1.CIF' data_mgome4n _database_code_depnum_ccdc_archive 'CCDC 717456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22.20 H80.80 Mg4 O22.20' _chemical_formula_weight 800.60 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 Orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 24.0550(10) _cell_length_b 31.7790(10) _cell_length_c 23.4540(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17929.3(12) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7034 _exptl_absorpt_coefficient_mu 0.151 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9484 _exptl_absorpt_correction_T_max 0.9712 _exptl_absorpt_process_details X-RED(Stoe) _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDS(Stoe) _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84144 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.70 _reflns_number_total 11576 _reflns_number_gt 8709 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Most but not all OH hydrogens could be found in the Fourier difference map. Therefore, there is a discrepancy between the numbers of H atoms in the formula calculated from atomic sites and that given in the CIF. ; _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^)+(0.0700P)^2^+46.0000P] 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 11576 _refine_ls_number_parameters 631 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2105 _refine_ls_wR_factor_gt 0.1982 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.19805(4) 0.03187(3) 0.58776(4) 0.0297(2) Uani 1 1 d . . . Mg2 Mg 0.20844(3) -0.03913(3) 0.49746(3) 0.0290(2) Uani 1 1 d . . . Mg3 Mg 0.04563(3) 0.21365(3) 0.79565(4) 0.0337(2) Uani 1 1 d . . . Mg4 Mg 0.04803(3) 0.21519(2) 1.20497(3) 0.02007(17) Uani 1 1 d . . . O1 O 0.21470(7) -0.03191(5) 0.58621(7) 0.0273(4) Uani 1 1 d . . . O2 O 0.20766(7) 0.02689(6) 0.49929(7) 0.0308(4) Uani 1 1 d . . . O3 O 0.11406(9) 0.02232(7) 0.58393(11) 0.0525(6) Uani 1 1 d . . . O4 O 0.20115(9) 0.09710(6) 0.57422(11) 0.0449(5) Uani 1 1 d . . . H4 H 0.2265(15) 0.1003(12) 0.5496(16) 0.054 Uiso 1 1 d . . . O5 O 0.19574(14) 0.03989(8) 0.67595(10) 0.0632(8) Uani 1 1 d D . . H5 H 0.2079(19) 0.0239(12) 0.6978(16) 0.076 Uiso 1 1 d D . . O6 O 0.22268(7) -0.10280(6) 0.49975(8) 0.0377(5) Uani 1 1 d . . . O7 O 0.12235(8) -0.03677(7) 0.51071(10) 0.0428(5) Uani 1 1 d . . . H7 H 0.1188(15) -0.0161(12) 0.5353(15) 0.051 Uiso 1 1 d . . . O8 O 0.19822(13) -0.04048(10) 0.40953(9) 0.0737(10) Uani 1 1 d . . . H8 H 0.219(2) -0.0327(16) 0.394(2) 0.088 Uiso 1 1 d . . . O9 O 0.04145(7) 0.22175(6) 0.70705(7) 0.0325(4) Uani 1 1 d . . . O10 O 0.03519(10) 0.15120(8) 0.78626(13) 0.0587(7) Uani 1 1 d . . . H10 H 0.012(4) 0.149(2) 0.761(4) 0.070 Uiso 0.50 1 d P . . O11 O 0.13334(8) 0.20809(8) 0.80077(10) 0.0484(6) Uani 1 1 d . . . H11 H 0.1509(16) 0.2166(12) 0.8382(16) 0.058 Uiso 1 1 d . . . O12 O 0.05064(13) 0.20940(12) 0.88457(11) 0.0699(10) Uani 1 1 d . . . H12 H 0.0339(19) 0.2194(15) 0.900(2) 0.065(16) Uiso 1 1 d . . . O13 O 0.03749(6) 0.28088(5) 1.20697(6) 0.0195(3) Uani 1 1 d . . . O14 O 0.13123(7) 0.22195(6) 1.21477(8) 0.0327(4) Uani 1 1 d . . . H14 H 0.1368(18) 0.2500 1.2500 0.039 Uiso 1 2 d S . . O15 O 0.05079(9) 0.21039(7) 1.11617(8) 0.0387(5) Uani 1 1 d . . . H15 H 0.0362(18) 0.2244(14) 1.0892(19) 0.078(14) Uiso 1 1 d . . . O16 O 0.05283(8) 0.14896(6) 1.20422(9) 0.0372(4) Uani 1 1 d . . . H16 H 0.0355(19) 0.1340(15) 1.177(2) 0.087(15) Uiso 1 1 d . . . O17 O 0.25878(11) 0.14644(11) 0.91405(15) 0.0886(12) Uani 1 1 d . . . H17 H 0.251(2) 0.1342(17) 0.941(2) 0.106 Uiso 1 1 d . . . O18 O 0.19547(15) 0.21267(11) 0.89183(16) 0.0989(12) Uani 1 1 d . . . O19 O 0.02604(17) 0.26411(14) 1.03800(15) 0.0394(9) Uani 0.50 1 d P . . H19 H -0.005(4) 0.242(2) 1.003(2) 0.047 Uiso 0.50 1 d P . . O20 O -0.0225(2) 0.22838(15) 0.96080(16) 0.0462(10) Uani 0.50 1 d P . . O21 O 0.22151(16) 0.02008(13) 0.33315(14) 0.0342(8) Uani 0.50 1 d P . . O22 O 0.2645(2) -0.01563(18) 0.25294(17) 0.0619(15) Uani 0.50 1 d P . . H22 H 0.243(5) 0.008(3) 0.290(3) 0.074 Uiso 0.50 1 d P . . O23 O 0.0655(3) -0.02061(19) 0.6700(3) 0.0599(16) Uani 0.50 1 d P . . O23A O 0.0422(3) -0.0238(2) 0.6343(6) 0.095(3) Uani 0.50 1 d P . . H23A H 0.065(3) -0.0101(19) 0.634(3) 0.115 Uiso 1 1 d . . . O24 O 0.0174(5) -0.1024(3) 0.6122(6) 0.158(6) Uani 0.50 1 d PD . . H24 H 0.022(8) -0.080(3) 0.628(7) 0.190 Uiso 0.50 1 d PD . . O24A O -0.0035(2) -0.0842(2) 0.6604(4) 0.075(2) Uani 0.50 1 d P . . H24A H 0.015(5) -0.071(3) 0.662(5) 0.090 Uiso 0.50 1 d P . . C1 C 0.18532(13) -0.05886(9) 0.62375(11) 0.0392(6) Uani 1 1 d . . . H1A H 0.1794 -0.0445 0.6602 0.059 Uiso 1 1 calc R . . H1B H 0.2069 -0.0846 0.6301 0.059 Uiso 1 1 calc R . . H1C H 0.1493 -0.0662 0.6069 0.059 Uiso 1 1 calc R . . C2 C 0.17220(14) 0.04899(12) 0.46136(15) 0.0585(11) Uani 1 1 d . . . H2A H 0.1617 0.0760 0.4784 0.088 Uiso 1 1 calc R . . H2B H 0.1387 0.0323 0.4542 0.088 Uiso 1 1 calc R . . H2C H 0.1917 0.0539 0.4253 0.088 Uiso 1 1 calc R . . C3 C 0.07596(15) 0.05441(13) 0.5687(3) 0.0917(18) Uani 1 1 d . . . H3A H 0.0492 0.0585 0.5996 0.138 Uiso 1 1 calc R . . H3B H 0.0562 0.0462 0.5339 0.138 Uiso 1 1 calc R . . H3C H 0.0962 0.0807 0.5619 0.138 Uiso 1 1 calc R . . C4 C 0.1833(2) 0.13511(11) 0.5965(2) 0.0816(14) Uani 1 1 d . . . H4A H 0.1478 0.1310 0.6163 0.122 Uiso 1 1 calc R . . H4B H 0.1783 0.1555 0.5656 0.122 Uiso 1 1 calc R . . H4C H 0.2110 0.1457 0.6235 0.122 Uiso 1 1 calc R . . C5 C 0.1887(5) 0.0736(3) 0.7097(4) 0.085(3) Uani 0.50 1 d P . . H5A H 0.1516 0.0855 0.7034 0.128 Uiso 0.50 1 calc PR . . H5B H 0.2170 0.0948 0.7007 0.128 Uiso 0.50 1 calc PR . . H5C H 0.1924 0.0650 0.7497 0.128 Uiso 0.50 1 calc PR . . C5A C 0.1398(4) 0.0557(3) 0.7027(3) 0.075(3) Uani 0.50 1 d P . . H5A1 H 0.1477 0.0723 0.7369 0.112 Uiso 0.50 1 calc PR . . H5A2 H 0.1166 0.0315 0.7130 0.112 Uiso 0.50 1 calc PR . . H5A3 H 0.1200 0.0732 0.6749 0.112 Uiso 0.50 1 calc PR . . C6 C 0.18254(13) -0.13224(10) 0.51899(14) 0.0461(7) Uani 1 1 d . . . H6A H 0.1473 -0.1177 0.5261 0.069 Uiso 1 1 calc R . . H6B H 0.1955 -0.1454 0.5544 0.069 Uiso 1 1 calc R . . H6C H 0.1771 -0.1539 0.4898 0.069 Uiso 1 1 calc R . . C7 C 0.07126(15) -0.04819(19) 0.4871(3) 0.110(2) Uani 1 1 d . . . H7A H 0.0647 -0.0318 0.4524 0.166 Uiso 1 1 calc R . . H7B H 0.0416 -0.0425 0.5147 0.166 Uiso 1 1 calc R . . H7C H 0.0717 -0.0783 0.4778 0.166 Uiso 1 1 calc R . . C8 C 0.16660(19) -0.06915(16) 0.37855(15) 0.0815(16) Uani 1 1 d . . . H8A H 0.1514 -0.0905 0.4044 0.122 Uiso 1 1 calc R . . H8B H 0.1901 -0.0828 0.3499 0.122 Uiso 1 1 calc R . . H8C H 0.1360 -0.0544 0.3596 0.122 Uiso 1 1 calc R . . C9 C 0.07378(13) 0.19624(13) 0.67011(15) 0.0577(10) Uani 1 1 d . . . H9A H 0.0583 0.1975 0.6315 0.086 Uiso 1 1 calc R . . H9B H 0.0732 0.1671 0.6837 0.086 Uiso 1 1 calc R . . H9C H 0.1122 0.2066 0.6696 0.086 Uiso 1 1 calc R . . C10 C 0.0558(4) 0.11531(17) 0.8010(4) 0.208(6) Uani 1 1 d . . . H10A H 0.0909 0.1198 0.8213 0.311 Uiso 1 1 calc R . . H10B H 0.0625 0.0982 0.7669 0.311 Uiso 1 1 calc R . . H10C H 0.0295 0.1007 0.8261 0.311 Uiso 1 1 calc R . . C11 C 0.1795(3) 0.2063(4) 0.7615(4) 0.069(2) Uani 0.50 1 d P . . H11A H 0.1992 0.1796 0.7663 0.103 Uiso 0.50 1 calc PR . . H11B H 0.2050 0.2297 0.7693 0.103 Uiso 0.50 1 calc PR . . H11C H 0.1656 0.2085 0.7223 0.103 Uiso 0.50 1 calc PR . . C11A C 0.1654(4) 0.1703(4) 0.7778(5) 0.096(4) Uani 0.50 1 d P . . H11D H 0.1393 0.1476 0.7689 0.144 Uiso 0.50 1 calc PR . . H11E H 0.1920 0.1607 0.8067 0.144 Uiso 0.50 1 calc PR . . H11F H 0.1854 0.1785 0.7432 0.144 Uiso 0.50 1 calc PR . . C12 C 0.0677(3) 0.17504(17) 0.91656(19) 0.112(2) Uani 1 1 d . . . H12A H 0.0768 0.1516 0.8910 0.169 Uiso 1 1 calc R . . H12B H 0.0377 0.1666 0.9424 0.169 Uiso 1 1 calc R . . H12C H 0.1007 0.1827 0.9388 0.169 Uiso 1 1 calc R . . C13 C 0.07098(10) 0.30576(8) 1.17053(10) 0.0297(5) Uani 1 1 d . . . H13A H 0.0705 0.2938 1.1320 0.045 Uiso 1 1 calc R . . H13B H 0.1092 0.3062 1.1849 0.045 Uiso 1 1 calc R . . H13C H 0.0564 0.3345 1.1694 0.045 Uiso 1 1 calc R . . C14 C 0.17551(17) 0.22422(19) 1.1772(2) 0.0477(16) Uani 0.726(13) 1 d P . . H14A H 0.2015 0.2460 1.1899 0.072 Uiso 0.726(13) 1 calc PR . . H14B H 0.1617 0.2312 1.1390 0.072 Uiso 0.726(13) 1 calc PR . . H14C H 0.1947 0.1970 1.1760 0.072 Uiso 0.726(13) 1 calc PR . . C14A C 0.1757(5) 0.1974(7) 1.2037(8) 0.066(6) Uani 0.274(13) 1 d P . . H14D H 0.1771 0.1912 1.1628 0.100 Uiso 0.274(13) 1 calc PR . . H14E H 0.1725 0.1711 1.2252 0.100 Uiso 0.274(13) 1 calc PR . . H14F H 0.2097 0.2121 1.2151 0.100 Uiso 0.274(13) 1 calc PR . . C15 C 0.0818(2) 0.1813(2) 1.08457(17) 0.122(3) Uani 1 1 d . . . H15A H 0.1092 0.1677 1.1095 0.182 Uiso 1 1 calc R . . H15B H 0.1011 0.1959 1.0535 0.182 Uiso 1 1 calc R . . H15C H 0.0569 0.1600 1.0686 0.182 Uiso 1 1 calc R . . C16 C 0.09584(18) 0.12214(11) 1.22432(16) 0.0619(10) Uani 1 1 d . . . H16A H 0.1265 0.1392 1.2392 0.093 Uiso 1 1 calc R . . H16B H 0.1094 0.1046 1.1929 0.093 Uiso 1 1 calc R . . H16C H 0.0813 0.1041 1.2547 0.093 Uiso 1 1 calc R . . C17 C 0.3105(2) 0.1579(2) 0.9152(4) 0.167(4) Uani 1 1 d . . . H17A H 0.3339 0.1346 0.9021 0.250 Uiso 1 1 calc R . . H17B H 0.3208 0.1655 0.9543 0.250 Uiso 1 1 calc R . . H17C H 0.3158 0.1822 0.8902 0.250 Uiso 1 1 calc R . . C18 C 0.2034(3) 0.24513(18) 0.9315(3) 0.117(2) Uani 1 1 d . . . H18A H 0.2011 0.2337 0.9702 0.176 Uiso 1 1 calc R . . H18B H 0.1746 0.2666 0.9263 0.176 Uiso 1 1 calc R . . H18C H 0.2401 0.2578 0.9256 0.176 Uiso 1 1 calc R . . C19 C 0.0717(4) 0.2852(4) 1.0139(3) 0.084(3) Uani 0.50 1 d P . . H19A H 0.0787 0.2741 0.9756 0.125 Uiso 0.50 1 calc PR . . H19B H 0.1046 0.2808 1.0378 0.125 Uiso 0.50 1 calc PR . . H19C H 0.0635 0.3154 1.0115 0.125 Uiso 0.50 1 calc PR . . C20 C -0.0573(4) 0.1965(3) 0.9837(3) 0.064(2) Uani 0.50 1 d P . . H20A H -0.0632 0.2017 1.0244 0.096 Uiso 0.50 1 calc PR . . H20B H -0.0394 0.1690 0.9786 0.096 Uiso 0.50 1 calc PR . . H20C H -0.0931 0.1967 0.9638 0.096 Uiso 0.50 1 calc PR . . C21 C 0.1815(4) 0.0487(3) 0.3123(3) 0.068(3) Uani 0.50 1 d P . . H21A H 0.1459 0.0436 0.3314 0.102 Uiso 0.50 1 calc PR . . H21B H 0.1771 0.0448 0.2711 0.102 Uiso 0.50 1 calc PR . . H21C H 0.1938 0.0775 0.3201 0.102 Uiso 0.50 1 calc PR . . C22 C 0.3006(5) -0.0459(4) 0.2774(3) 0.113(5) Uani 0.50 1 d P . . H22A H 0.3112 -0.0368 0.3159 0.169 Uiso 0.50 1 calc PR . . H22B H 0.3340 -0.0486 0.2538 0.169 Uiso 0.50 1 calc PR . . H22C H 0.2816 -0.0731 0.2795 0.169 Uiso 0.50 1 calc PR . . C23 C 0.0694(4) -0.0001(3) 0.7230(4) 0.082(3) Uani 0.50 1 d P . . H23B H 0.0530 0.0281 0.7200 0.123 Uiso 0.50 1 calc PR . . H23C H 0.1086 0.0023 0.7340 0.123 Uiso 0.50 1 calc PR . . H23D H 0.0493 -0.0164 0.7519 0.123 Uiso 0.50 1 calc PR . . C23A C 0.0035(5) -0.0007(4) 0.6661(7) 0.151(7) Uani 0.50 1 d P . . H23E H -0.0035 -0.0151 0.7024 0.227 Uiso 0.50 1 calc PR . . H23F H -0.0313 0.0016 0.6447 0.227 Uiso 0.50 1 calc PR . . H23G H 0.0183 0.0275 0.6736 0.227 Uiso 0.50 1 calc PR . . C24 C -0.0334(7) -0.1026(6) 0.5790(9) 0.241(16) Uani 0.50 1 d P . . H24B H -0.0250 -0.0948 0.5395 0.362 Uiso 0.50 1 calc PR . . H24C H -0.0597 -0.0824 0.5952 0.362 Uiso 0.50 1 calc PR . . H24D H -0.0498 -0.1308 0.5798 0.362 Uiso 0.50 1 calc PR . . C24A C 0.0457(3) -0.0756(3) -0.1210(4) 0.074(3) Uani 0.50 1 d P . . H24E H 0.0741 -0.0976 -0.1232 0.111 Uiso 0.50 1 calc PR . . H24F H 0.0299 -0.0749 -0.0825 0.111 Uiso 0.50 1 calc PR . . H24G H 0.0625 -0.0483 -0.1299 0.111 Uiso 0.50 1 calc PR . . O27 O 0.2018(4) 0.1442(4) 0.8001(5) 0.049(4) Uani 0.203(7) 1 d P A 1 C27 C 0.2439(9) 0.1505(10) 0.7566(8) 0.106(12) Uani 0.203(7) 1 d P A 1 H27A H 0.2266 0.1625 0.7224 0.158 Uiso 0.203(7) 1 calc PR A 1 H27B H 0.2611 0.1235 0.7470 0.158 Uiso 0.203(7) 1 calc PR A 1 H27C H 0.2723 0.1699 0.7709 0.158 Uiso 0.203(7) 1 calc PR A 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 Mg1 0.0367(4) 0.0252(4) 0.0272(4) 0.0022(3) 0.0072(3) -0.0015(3) Mg2 0.0285(4) 0.0397(5) 0.0186(4) -0.0021(3) 0.0029(3) -0.0184(3) Mg3 0.0264(4) 0.0493(6) 0.0253(4) -0.0011(4) -0.0043(3) 0.0110(4) Mg4 0.0185(3) 0.0241(4) 0.0176(4) -0.0003(3) 0.0007(3) 0.0058(3) O1 0.0380(9) 0.0251(8) 0.0188(8) 0.0024(6) 0.0098(6) -0.0048(7) O2 0.0285(8) 0.0392(10) 0.0247(8) 0.0116(7) -0.0092(7) -0.0153(7) O3 0.0353(11) 0.0353(11) 0.0868(18) -0.0001(11) 0.0218(11) -0.0035(8) O4 0.0434(11) 0.0256(9) 0.0656(15) 0.0051(9) 0.0103(10) -0.0007(8) O5 0.110(2) 0.0484(14) 0.0309(12) -0.0108(10) 0.0288(13) -0.0040(14) O6 0.0321(9) 0.0408(10) 0.0402(10) -0.0169(8) 0.0147(8) -0.0191(8) O7 0.0273(9) 0.0408(11) 0.0604(14) 0.0035(10) -0.0020(9) -0.0146(8) O8 0.101(2) 0.099(2) 0.0208(10) -0.0027(11) -0.0067(11) -0.0775(18) O9 0.0245(8) 0.0494(11) 0.0235(9) -0.0131(8) 0.0051(6) -0.0038(7) O10 0.0467(13) 0.0490(13) 0.0806(19) 0.0158(13) -0.0167(12) 0.0054(11) O11 0.0267(9) 0.0664(15) 0.0523(13) -0.0087(11) -0.0113(9) 0.0157(9) O12 0.0724(18) 0.109(3) 0.0279(12) 0.0087(13) -0.0090(12) 0.0490(18) O13 0.0185(7) 0.0242(8) 0.0156(7) 0.0039(6) 0.0049(5) 0.0020(5) O14 0.0176(7) 0.0385(10) 0.0419(10) 0.0000(8) 0.0062(7) 0.0051(7) O15 0.0492(11) 0.0469(12) 0.0199(9) -0.0048(8) 0.0079(8) 0.0187(9) O16 0.0288(9) 0.0266(9) 0.0561(13) -0.0059(9) -0.0062(8) 0.0096(7) O17 0.0518(15) 0.103(2) 0.111(3) 0.082(2) 0.0364(15) 0.0271(15) O18 0.102(3) 0.094(2) 0.100(3) -0.029(2) -0.058(2) 0.040(2) O19 0.046(2) 0.055(3) 0.0174(16) 0.0012(16) 0.0010(15) 0.0051(19) O20 0.061(3) 0.057(3) 0.0202(18) 0.0059(17) -0.0031(17) -0.004(2) O21 0.0402(19) 0.044(2) 0.0182(16) -0.0017(15) -0.0021(14) 0.0089(16) O22 0.086(4) 0.082(4) 0.0170(17) -0.005(2) -0.005(2) 0.051(3) O23 0.051(4) 0.041(3) 0.088(5) 0.002(3) 0.040(3) -0.008(3) O23A 0.049(4) 0.046(4) 0.192(10) 0.043(5) 0.062(5) 0.013(3) O24 0.142(8) 0.074(5) 0.258(13) 0.109(7) -0.156(9) -0.070(5) O24A 0.041(3) 0.050(4) 0.135(6) 0.048(4) -0.038(4) -0.016(2) C1 0.0579(17) 0.0334(14) 0.0262(13) 0.0067(10) 0.0177(12) -0.0069(12) C2 0.0495(18) 0.064(2) 0.062(2) 0.0356(17) -0.0369(16) -0.0341(16) C3 0.0326(17) 0.057(2) 0.185(6) -0.003(3) 0.009(2) 0.0021(16) C4 0.085(3) 0.0322(17) 0.127(4) -0.001(2) 0.026(3) 0.0123(18) C5 0.136(9) 0.062(5) 0.057(5) -0.020(4) 0.041(6) 0.007(6) C5A 0.096(7) 0.077(6) 0.052(4) -0.018(4) 0.030(4) 0.031(5) C6 0.0440(16) 0.0427(16) 0.0517(17) -0.0095(14) 0.0142(13) -0.0233(13) C7 0.0262(17) 0.133(5) 0.172(6) -0.061(4) -0.001(2) -0.029(2) C8 0.088(3) 0.122(4) 0.0352(18) -0.014(2) -0.0125(18) -0.067(3) C9 0.0400(16) 0.082(2) 0.0508(19) -0.0399(18) 0.0172(14) -0.0080(16) C10 0.289(11) 0.057(3) 0.277(11) -0.045(5) -0.194(9) 0.086(5) C11 0.029(3) 0.115(7) 0.063(5) -0.016(5) -0.002(3) 0.016(4) C11A 0.055(5) 0.118(9) 0.115(9) -0.047(8) -0.001(5) 0.032(6) C12 0.208(7) 0.081(3) 0.049(2) 0.031(2) -0.012(3) 0.006(4) C13 0.0322(12) 0.0310(12) 0.0261(11) 0.0079(10) 0.0139(9) 0.0018(9) C14 0.0278(19) 0.056(3) 0.059(3) 0.000(3) 0.0172(19) 0.0061(18) C14A 0.029(6) 0.097(15) 0.073(11) -0.019(10) -0.007(6) 0.031(7) C15 0.119(4) 0.208(7) 0.038(2) -0.030(3) -0.001(2) 0.114(5) C16 0.091(3) 0.0412(17) 0.054(2) -0.0051(15) -0.0141(19) 0.0368(18) C17 0.065(3) 0.142(5) 0.294(10) 0.169(7) 0.071(4) 0.030(3) C18 0.158(6) 0.083(4) 0.111(5) -0.022(3) -0.056(4) 0.040(4) C19 0.085(6) 0.132(9) 0.034(4) 0.017(5) -0.004(4) -0.048(6) C20 0.082(5) 0.080(6) 0.031(3) 0.006(4) 0.000(3) -0.027(4) C21 0.081(5) 0.098(6) 0.026(3) -0.006(3) -0.014(3) 0.053(5) C22 0.157(11) 0.155(11) 0.027(4) -0.002(5) -0.008(5) 0.118(10) C23 0.079(6) 0.091(6) 0.075(6) -0.002(5) 0.039(5) -0.022(5) C23A 0.110(9) 0.106(8) 0.238(17) 0.054(10) 0.135(11) 0.034(7) C24 0.190(17) 0.25(2) 0.28(2) 0.24(2) -0.193(19) -0.167(17) C24A 0.043(4) 0.085(7) 0.093(7) -0.057(5) -0.023(4) 0.010(4) O27 0.036(6) 0.067(8) 0.045(6) 0.006(5) 0.000(4) 0.019(5) C27 0.074(14) 0.21(3) 0.037(10) -0.001(14) 0.011(9) 0.078(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. Several methyl groups are disordered between two positions with occupation factors fixed to 0.5 or refined (in one case). Several methyl alkohol molecule are disordered around two-fold axes. They were refined with egual occupation factors of 0.5. ; 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 2.045(2) . ? Mg1 O1 2.0665(18) . ? Mg1 O5 2.085(2) . ? Mg1 O2 2.0937(19) . ? Mg1 O4 2.099(2) . ? Mg1 O1 2.0990(19) 2 ? Mg1 Mg2 3.0981(12) 2 ? Mg1 Mg2 3.1046(12) . ? Mg1 Mg1 3.2170(17) 2 ? Mg2 O6 2.053(2) . ? Mg2 O2 2.0559(17) 2 ? Mg2 O8 2.077(2) . ? Mg2 O7 2.095(2) . ? Mg2 O2 2.098(2) . ? Mg2 O1 2.0994(18) . ? Mg2 Mg1 3.0981(12) 2 ? Mg2 Mg2 3.1913(15) 2 ? Mg3 O10 2.012(3) . ? Mg3 O9 2.056(2) 8_456 ? Mg3 O12 2.093(3) . ? Mg3 O9 2.0963(19) . ? Mg3 O9 2.1114(18) 3_556 ? Mg3 O11 2.121(2) . ? Mg3 Mg3 3.0666(16) 3_556 ? Mg3 Mg3 3.1502(19) 8_456 ? Mg3 Mg3 3.1870(17) 6_455 ? Mg4 O14 2.0261(18) . ? Mg4 O13 2.0615(16) 6_455 ? Mg4 O13 2.0844(16) 8_457 ? Mg4 O15 2.089(2) . ? Mg4 O13 2.1036(17) . ? Mg4 O16 2.108(2) . ? Mg4 Mg4 3.0588(15) 8_457 ? Mg4 Mg4 3.1306(14) 3_557 ? Mg4 Mg4 3.1992(14) 6_455 ? O1 C1 1.417(3) . ? O1 Mg1 2.0990(19) 2 ? O2 C2 1.419(3) . ? O2 Mg2 2.0559(17) 2 ? O3 C3 1.417(5) . ? O4 C4 1.385(4) . ? O5 C5 1.342(8) . ? O5 C5A 1.568(8) . ? O6 C6 1.418(3) . ? O7 C7 1.396(4) . ? O8 C8 1.392(4) . ? O9 C9 1.419(3) . ? O9 Mg3 2.056(2) 8_456 ? O9 Mg3 2.1114(18) 3_556 ? O10 C10 1.291(5) . ? O11 C11 1.444(8) . ? O11 C11A 1.524(9) . ? O12 C12 1.387(5) . ? O13 C13 1.416(3) . ? O13 Mg4 2.0615(16) 6_455 ? O13 Mg4 2.0844(16) 8_457 ? O14 C14A 1.349(12) . ? O14 C14 1.384(4) . ? O15 C15 1.400(4) . ? O16 C16 1.421(4) . ? O17 C17 1.296(6) . ? O18 C18 1.402(6) . ? O19 C19 1.405(9) . ? O19 O19 1.541(9) 6_455 ? O20 C20 1.419(9) . ? O20 O20 1.750(9) 6_455 ? O20 C19 1.770(10) 6_455 ? O21 C21 1.410(7) . ? O21 C22 1.632(9) 2 ? O22 O22 1.213(9) 2 ? O22 C22 1.417(9) . ? O23 O23A 1.015(12) . ? O23 C23 1.406(11) . ? O23A C23A 1.400(12) . ? O24 O24A 1.368(17) . ? O24 C24 1.451(13) . ? O24 C24A 1.753(17) 3 ? O24A C24A 1.399(10) 3 ? C24A O24A 1.399(10) 3 ? O27 C27 1.45(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 O1 92.58(8) . . ? O3 Mg1 O5 92.03(12) . . ? O1 Mg1 O5 98.20(9) . . ? O3 Mg1 O2 93.11(9) . . ? O1 Mg1 O2 83.51(8) . . ? O5 Mg1 O2 174.51(11) . . ? O3 Mg1 O4 100.08(9) . . ? O1 Mg1 O4 163.62(9) . . ? O5 Mg1 O4 91.73(10) . . ? O2 Mg1 O4 85.46(9) . . ? O3 Mg1 O1 170.80(9) . 2 ? O1 Mg1 O1 78.85(8) . 2 ? O5 Mg1 O1 92.51(11) . 2 ? O2 Mg1 O1 82.67(7) . 2 ? O4 Mg1 O1 87.78(8) . 2 ? O3 Mg1 Mg2 134.29(8) . 2 ? O1 Mg1 Mg2 85.43(5) . 2 ? O5 Mg1 Mg2 133.51(10) . 2 ? O2 Mg1 Mg2 41.24(5) . 2 ? O4 Mg1 Mg2 78.30(7) . 2 ? O1 Mg1 Mg2 42.45(5) 2 2 ? O3 Mg1 Mg2 86.65(7) . . ? O1 Mg1 Mg2 42.23(5) . . ? O5 Mg1 Mg2 140.16(8) . . ? O2 Mg1 Mg2 42.28(6) . . ? O4 Mg1 Mg2 127.73(8) . . ? O1 Mg1 Mg2 84.73(5) 2 . ? Mg2 Mg1 Mg2 61.93(3) 2 . ? O3 Mg1 Mg1 132.38(8) . 2 ? O1 Mg1 Mg1 39.81(5) . 2 ? O5 Mg1 Mg1 95.61(9) . 2 ? O2 Mg1 Mg1 82.33(6) . 2 ? O4 Mg1 Mg1 126.47(8) . 2 ? O1 Mg1 Mg1 39.07(5) 2 2 ? Mg2 Mg1 Mg1 58.86(3) 2 2 ? Mg2 Mg1 Mg1 58.66(3) . 2 ? O6 Mg2 O2 91.27(8) . 2 ? O6 Mg2 O8 91.45(12) . . ? O2 Mg2 O8 98.09(10) 2 . ? O6 Mg2 O7 101.33(8) . . ? O2 Mg2 O7 163.80(9) 2 . ? O8 Mg2 O7 91.78(11) . . ? O6 Mg2 O2 170.52(8) . . ? O2 Mg2 O2 79.57(9) 2 . ? O8 Mg2 O2 92.29(11) . . ? O7 Mg2 O2 87.27(8) . . ? O6 Mg2 O1 94.00(8) . . ? O2 Mg2 O1 83.58(7) 2 . ? O8 Mg2 O1 174.27(13) . . ? O7 Mg2 O1 85.41(9) . . ? O2 Mg2 O1 82.60(7) . . ? O6 Mg2 Mg1 86.24(6) . 2 ? O2 Mg2 Mg1 42.17(5) 2 2 ? O8 Mg2 Mg1 140.00(9) . 2 ? O7 Mg2 Mg1 127.84(7) . 2 ? O2 Mg2 Mg1 85.30(5) . 2 ? O1 Mg2 Mg1 42.44(5) . 2 ? O6 Mg2 Mg1 135.39(7) . . ? O2 Mg2 Mg1 85.82(6) 2 . ? O8 Mg2 Mg1 133.06(11) . . ? O7 Mg2 Mg1 78.07(7) . . ? O2 Mg2 Mg1 42.16(5) . . ? O1 Mg2 Mg1 41.42(5) . . ? Mg1 Mg2 Mg1 62.48(3) 2 . ? O6 Mg2 Mg2 131.57(7) . 2 ? O2 Mg2 Mg2 40.30(6) 2 2 ? O8 Mg2 Mg2 95.18(6) . 2 ? O7 Mg2 Mg2 126.25(8) . 2 ? O2 Mg2 Mg2 39.32(5) . 2 ? O1 Mg2 Mg2 82.52(5) . 2 ? Mg1 Mg2 Mg2 59.14(2) 2 2 ? Mg1 Mg2 Mg2 58.94(3) . 2 ? O10 Mg3 O9 167.16(9) . 8_456 ? O10 Mg3 O12 93.02(14) . . ? O9 Mg3 O12 95.62(12) 8_456 . ? O10 Mg3 O9 90.38(11) . . ? O9 Mg3 O9 81.05(8) 8_456 . ? O12 Mg3 O9 176.60(13) . . ? O10 Mg3 O9 89.61(10) . 3_556 ? O9 Mg3 O9 80.15(9) 8_456 3_556 ? O12 Mg3 O9 95.45(10) . 3_556 ? O9 Mg3 O9 84.71(7) . 3_556 ? O10 Mg3 O11 92.76(10) . . ? O9 Mg3 O11 97.67(9) 8_456 . ? O12 Mg3 O11 83.16(11) . . ? O9 Mg3 O11 96.55(9) . . ? O9 Mg3 O11 177.30(10) 3_556 . ? O10 Mg3 Mg3 80.46(7) . 3_556 ? O9 Mg3 Mg3 86.76(5) 8_456 3_556 ? O12 Mg3 Mg3 137.47(10) . 3_556 ? O9 Mg3 Mg3 43.41(5) . 3_556 ? O9 Mg3 Mg3 43.02(5) 3_556 3_556 ? O11 Mg3 Mg3 138.74(8) . 3_556 ? O10 Mg3 Mg3 130.46(10) . 8_456 ? O9 Mg3 Mg3 41.13(5) 8_456 8_456 ? O12 Mg3 Mg3 136.43(12) . 8_456 ? O9 Mg3 Mg3 40.19(6) . 8_456 ? O9 Mg3 Mg3 83.69(5) 3_556 8_456 ? O11 Mg3 Mg3 95.72(7) . 8_456 ? Mg3 Mg3 Mg3 61.66(3) 3_556 8_456 ? O10 Mg3 Mg3 128.97(9) . 6_455 ? O9 Mg3 Mg3 40.76(5) 8_456 6_455 ? O12 Mg3 Mg3 94.96(8) . 6_455 ? O9 Mg3 Mg3 82.99(6) . 6_455 ? O9 Mg3 Mg3 39.49(6) 3_556 6_455 ? O11 Mg3 Mg3 138.21(9) . 6_455 ? Mg3 Mg3 Mg3 60.46(3) 3_556 6_455 ? Mg3 Mg3 Mg3 57.88(4) 8_456 6_455 ? O14 Mg4 O13 167.63(8) . 6_455 ? O14 Mg4 O13 90.08(7) . 8_457 ? O13 Mg4 O13 81.51(6) 6_455 8_457 ? O14 Mg4 O15 95.13(8) . . ? O13 Mg4 O15 93.37(8) 6_455 . ? O13 Mg4 O15 174.78(8) 8_457 . ? O14 Mg4 O13 90.64(7) . . ? O13 Mg4 O13 79.58(7) 6_455 . ? O13 Mg4 O13 84.48(7) 8_457 . ? O15 Mg4 O13 95.66(8) . . ? O14 Mg4 O16 93.03(8) . . ? O13 Mg4 O16 96.62(7) 6_455 . ? O13 Mg4 O16 94.28(8) 8_457 . ? O15 Mg4 O16 85.24(9) . . ? O13 Mg4 O16 176.13(8) . . ? O14 Mg4 Mg4 81.08(6) . 8_457 ? O13 Mg4 Mg4 86.59(5) 6_455 8_457 ? O13 Mg4 Mg4 43.33(5) 8_457 8_457 ? O15 Mg4 Mg4 137.83(8) . 8_457 ? O13 Mg4 Mg4 42.84(4) . 8_457 ? O16 Mg4 Mg4 136.72(7) . 8_457 ? O14 Mg4 Mg4 130.74(7) . 3_557 ? O13 Mg4 Mg4 41.24(4) 6_455 3_557 ? O13 Mg4 Mg4 40.69(4) 8_457 3_557 ? O15 Mg4 Mg4 134.10(7) . 3_557 ? O13 Mg4 Mg4 84.03(4) . 3_557 ? O16 Mg4 Mg4 92.64(6) . 3_557 ? Mg4 Mg4 Mg4 62.23(3) 8_457 3_557 ? O14 Mg4 Mg4 129.80(7) . 6_455 ? O13 Mg4 Mg4 40.30(5) 6_455 6_455 ? O13 Mg4 Mg4 82.57(5) 8_457 6_455 ? O15 Mg4 Mg4 94.21(6) . 6_455 ? O13 Mg4 Mg4 39.34(4) . 6_455 ? O16 Mg4 Mg4 136.89(7) . 6_455 ? Mg4 Mg4 Mg4 59.98(3) 8_457 6_455 ? Mg4 Mg4 Mg4 57.78(3) 3_557 6_455 ? C1 O1 Mg1 119.02(16) . . ? C1 O1 Mg1 119.23(17) . 2 ? Mg1 O1 Mg1 101.12(8) . 2 ? C1 O1 Mg2 120.94(16) . . ? Mg1 O1 Mg2 96.36(8) . . ? Mg1 O1 Mg2 95.11(7) 2 . ? C2 O2 Mg2 118.92(16) . 2 ? C2 O2 Mg1 121.2(2) . . ? Mg2 O2 Mg1 96.59(7) 2 . ? C2 O2 Mg2 119.18(18) . . ? Mg2 O2 Mg2 100.38(9) 2 . ? Mg1 O2 Mg2 95.56(7) . . ? C3 O3 Mg1 122.9(2) . . ? C4 O4 Mg1 142.5(3) . . ? C5 O5 C5A 53.1(6) . . ? C5 O5 Mg1 133.4(5) . . ? C5A O5 Mg1 117.3(4) . . ? C6 O6 Mg2 123.01(18) . . ? C7 O7 Mg2 143.3(3) . . ? C8 O8 Mg2 126.6(2) . . ? C9 O9 Mg3 121.7(2) . 8_456 ? C9 O9 Mg3 120.6(2) . . ? Mg3 O9 Mg3 98.67(8) 8_456 . ? C9 O9 Mg3 117.12(17) . 3_556 ? Mg3 O9 Mg3 99.75(9) 8_456 3_556 ? Mg3 O9 Mg3 93.57(7) . 3_556 ? C10 O10 Mg3 142.6(4) . . ? C11 O11 C11A 49.9(6) . . ? C11 O11 Mg3 137.1(3) . . ? C11A O11 Mg3 123.3(4) . . ? C12 O12 Mg3 127.4(3) . . ? C13 O13 Mg4 121.35(14) . 6_455 ? C13 O13 Mg4 119.70(14) . 8_457 ? Mg4 O13 Mg4 98.07(6) 6_455 8_457 ? C13 O13 Mg4 118.17(13) . . ? Mg4 O13 Mg4 100.36(7) 6_455 . ? Mg4 O13 Mg4 93.83(6) 8_457 . ? C14A O14 C14 45.4(9) . . ? C14A O14 Mg4 134.4(8) . . ? C14 O14 Mg4 133.9(3) . . ? C15 O15 Mg4 126.4(2) . . ? C16 O16 Mg4 129.5(2) . . ? C19 O19 O19 155.9(4) . 6_455 ? C20 O20 O20 157.8(4) . 6_455 ? C20 O20 C19 33.6(5) . 6_455 ? O20 O20 C19 127.2(4) 6_455 6_455 ? C21 O21 C22 34.6(4) . 2 ? O22 O22 C22 155.1(5) 2 . ? O23A O23 C23 144.4(10) . . ? O23 O23A C23A 82.8(12) . . ? O24A O24 C24 97.8(15) . . ? O24A O24 C24A 51.5(7) . 3 ? C24 O24 C24A 48.4(12) . 3 ? O24 O24A C24A 78.7(8) . 3 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.625 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.058 # Attachment 'comp2.CIF' data_sw139-3 _database_code_depnum_ccdc_archive 'CCDC 717457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H86 F2 Mg6 O24' _chemical_formula_weight 942.79 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' F F 0.0171 0.0103 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.7500(10) _cell_length_b 11.8766(5) _cell_length_c 19.9787(9) _cell_angle_alpha 90.00 _cell_angle_beta 127.910(3) _cell_angle_gamma 90.00 _cell_volume 5007.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 32000 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31031 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5969 _reflns_number_gt 4997 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+3.0000P] 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 5969 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.169 _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 0.18285(3) 0.24964(5) -0.10361(4) 0.02281(16) Uani 1 1 d . . . Mg2 Mg 0.19935(3) 0.40557(5) 0.03682(4) 0.02371(16) Uani 1 1 d . . . Mg3 Mg 0.18894(3) 0.14205(6) 0.04597(4) 0.02399(16) Uani 1 1 d . . . F F 0.24570(5) 0.14424(9) 0.00360(6) 0.0234(2) Uani 1 1 d . . . O1 O 0.14409(6) 0.38753(12) -0.17666(8) 0.0259(3) Uani 1 1 d . . . O2 O 0.13292(6) 0.11013(12) -0.16701(8) 0.0262(3) Uani 1 1 d . . . O3 O 0.24946(6) 0.27294(11) 0.11986(8) 0.0237(3) Uani 1 1 d . . . O4 O 0.14496(6) 0.27165(11) -0.04084(8) 0.0239(3) Uani 1 1 d . . . O5 O 0.27228(7) 0.51328(12) 0.12070(9) 0.0285(3) Uani 1 1 d . . . O6 O 0.15691(7) 0.51402(12) -0.06403(10) 0.0283(3) Uani 1 1 d . . . O7 O 0.14594(7) 0.45229(13) 0.07169(9) 0.0301(3) Uani 1 1 d . . . O8 O 0.13688(7) 0.02305(12) -0.04782(9) 0.0286(3) Uani 1 1 d . . . O9 O 0.25283(7) 0.02987(12) 0.13814(9) 0.0268(3) Uani 1 1 d . . . O10 O 0.13132(7) 0.14052(13) 0.07936(9) 0.0306(3) Uani 1 1 d . . . O11 O 0.07904(7) 0.31454(14) 0.07632(10) 0.0341(3) Uani 1 1 d . . . O12 O 0.09925(8) 0.29932(15) 0.22438(11) 0.0395(4) Uani 1 1 d . . . C1 C 0.08663(10) 0.40213(19) -0.25959(13) 0.0326(5) Uani 1 1 d . . . H1A H 0.0855 0.3499 -0.2985 0.049 Uiso 1 1 calc R . . H1B H 0.0840 0.4797 -0.2783 0.049 Uiso 1 1 calc R . . H1C H 0.0507 0.3869 -0.2593 0.049 Uiso 1 1 calc R . . C2 C 0.07881(10) 0.09841(19) -0.25207(13) 0.0348(5) Uani 1 1 d . . . H2A H 0.0423 0.1326 -0.2596 0.052 Uiso 1 1 calc R . . H2B H 0.0705 0.0183 -0.2667 0.052 Uiso 1 1 calc R . . H2C H 0.0860 0.1362 -0.2891 0.052 Uiso 1 1 calc R . . C3 C 0.26999(10) 0.28318(18) 0.20439(12) 0.0289(4) Uani 1 1 d . . . H3A H 0.3004 0.2232 0.2395 0.043 Uiso 1 1 calc R . . H3B H 0.2334 0.2769 0.2043 0.043 Uiso 1 1 calc R . . H3C H 0.2903 0.3566 0.2275 0.043 Uiso 1 1 calc R . . C4 C 0.07759(9) 0.28034(18) -0.09662(13) 0.0277(4) Uani 1 1 d . . . H4A H 0.0652 0.3581 -0.0970 0.042 Uiso 1 1 calc R . . H4B H 0.0599 0.2300 -0.0772 0.042 Uiso 1 1 calc R . . H4C H 0.0614 0.2589 -0.1541 0.042 Uiso 1 1 calc R . . C5 C 0.27996(11) 0.62715(18) 0.10553(15) 0.0367(5) Uani 1 1 d . . . H5A H 0.2924 0.6283 0.0685 0.055 Uiso 1 1 calc R . . H5B H 0.3129 0.6636 0.1596 0.055 Uiso 1 1 calc R . . H5C H 0.2399 0.6677 0.0781 0.055 Uiso 1 1 calc R . . C6 C 0.10892(11) 0.5968(2) -0.09452(15) 0.0399(5) Uani 1 1 d . . . H6A H 0.0674 0.5601 -0.1271 0.060 Uiso 1 1 calc R . . H6B H 0.1100 0.6501 -0.1310 0.060 Uiso 1 1 calc R . . H6C H 0.1163 0.6372 -0.0464 0.060 Uiso 1 1 calc R . . C7 C 0.15918(12) 0.5405(2) 0.12865(15) 0.0405(5) Uani 1 1 d . . . H7A H 0.2049 0.5544 0.1675 0.061 Uiso 1 1 calc R . . H7B H 0.1446 0.5187 0.1613 0.061 Uiso 1 1 calc R . . H7C H 0.1372 0.6092 0.0964 0.061 Uiso 1 1 calc R . . C8 C 0.08425(11) -0.0434(2) -0.07059(15) 0.0391(5) Uani 1 1 d . . . H8A H 0.0967 -0.0909 -0.0225 0.059 Uiso 1 1 calc R . . H8B H 0.0704 -0.0910 -0.1192 0.059 Uiso 1 1 calc R . . H8C H 0.0494 0.0061 -0.0857 0.059 Uiso 1 1 calc R . . C9 C 0.25245(10) -0.08983(17) 0.13040(14) 0.0327(5) Uani 1 1 d . . . H9A H 0.2145 -0.1209 0.1207 0.049 Uiso 1 1 calc R . . H9B H 0.2904 -0.1216 0.1827 0.049 Uiso 1 1 calc R . . H9C H 0.2522 -0.1091 0.0825 0.049 Uiso 1 1 calc R . . C10 C 0.13477(13) 0.0656(2) 0.13774(17) 0.0444(6) Uani 1 1 d . . . H10A H 0.1684 0.0102 0.1577 0.067 Uiso 1 1 calc R . . H10B H 0.0941 0.0266 0.1095 0.067 Uiso 1 1 calc R . . H10C H 0.1441 0.1084 0.1862 0.067 Uiso 1 1 calc R . . C11 C 0.01331(11) 0.3299(3) 0.01285(16) 0.0456(6) Uani 1 1 d . . . H11A H -0.0060 0.3547 0.0391 0.068 Uiso 1 1 calc R . . H11B H -0.0059 0.2587 -0.0170 0.068 Uiso 1 1 calc R . . H11C H 0.0062 0.3871 -0.0275 0.068 Uiso 1 1 calc R . . C12 C 0.04791(11) 0.2349(2) 0.20507(16) 0.0391(5) Uani 1 1 d . . . H12A H 0.0604 0.1938 0.2558 0.059 Uiso 1 1 calc R . . H12B H 0.0353 0.1813 0.1599 0.059 Uiso 1 1 calc R . . H12C H 0.0122 0.2848 0.1861 0.059 Uiso 1 1 calc R . . H5 H 0.3043(16) 0.479(3) 0.142(2) 0.061(10) Uiso 1 1 d . . . H6 H 0.1498(13) 0.483(3) -0.1023(18) 0.045(8) Uiso 1 1 d . . . H7 H 0.1238(17) 0.401(3) 0.070(2) 0.078(12) Uiso 1 1 d . . . H8 H 0.1295(12) 0.054(2) -0.0950(17) 0.043(7) Uiso 1 1 d . . . H9 H 0.2892(15) 0.050(3) 0.158(2) 0.062(9) Uiso 1 1 d . . . H10 H 0.1078(16) 0.215(3) 0.073(2) 0.072(10) Uiso 1 1 d . . . H12 H 0.0947(16) 0.306(3) 0.173(2) 0.069(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0276(3) 0.0194(3) 0.0253(3) -0.0006(2) 0.0183(3) 0.0003(2) Mg2 0.0302(3) 0.0190(3) 0.0264(3) -0.0004(3) 0.0196(3) 0.0010(2) Mg3 0.0291(3) 0.0203(3) 0.0271(3) 0.0006(3) 0.0196(3) 0.0000(2) F 0.0290(5) 0.0191(5) 0.0263(5) -0.0006(4) 0.0192(5) 0.0000(4) O1 0.0294(6) 0.0233(7) 0.0263(6) 0.0019(6) 0.0178(6) 0.0013(5) O2 0.0290(6) 0.0231(7) 0.0257(6) -0.0031(6) 0.0164(6) -0.0017(5) O3 0.0315(6) 0.0214(6) 0.0236(6) -0.0008(5) 0.0197(6) 0.0006(5) O4 0.0256(6) 0.0221(7) 0.0264(6) 0.0004(5) 0.0172(5) 0.0008(5) O5 0.0340(7) 0.0198(7) 0.0333(7) -0.0017(6) 0.0215(6) 0.0018(6) O6 0.0376(7) 0.0221(7) 0.0305(7) 0.0010(6) 0.0236(6) 0.0061(6) O7 0.0388(7) 0.0266(8) 0.0355(8) -0.0034(6) 0.0281(7) 0.0005(6) O8 0.0329(7) 0.0242(7) 0.0318(7) -0.0006(6) 0.0215(6) -0.0047(6) O9 0.0328(7) 0.0192(7) 0.0327(7) 0.0014(6) 0.0222(6) 0.0001(5) O10 0.0380(7) 0.0279(8) 0.0381(8) 0.0062(6) 0.0295(7) 0.0031(6) O11 0.0364(7) 0.0351(8) 0.0404(8) 0.0067(7) 0.0285(7) 0.0052(6) O12 0.0455(9) 0.0373(9) 0.0389(8) -0.0039(7) 0.0275(8) -0.0096(7) C1 0.0329(10) 0.0316(11) 0.0294(10) 0.0050(9) 0.0172(9) 0.0000(8) C2 0.0362(10) 0.0304(11) 0.0312(10) -0.0056(9) 0.0174(9) -0.0024(8) C3 0.0366(10) 0.0283(10) 0.0254(9) -0.0019(8) 0.0209(8) 0.0010(8) C4 0.0281(9) 0.0280(10) 0.0304(9) 0.0010(8) 0.0197(8) 0.0006(7) C5 0.0432(11) 0.0199(10) 0.0445(12) -0.0031(9) 0.0257(10) -0.0019(8) C6 0.0512(13) 0.0307(11) 0.0425(12) 0.0085(10) 0.0311(11) 0.0185(10) C7 0.0495(13) 0.0378(12) 0.0471(13) -0.0103(11) 0.0363(11) -0.0001(10) C8 0.0394(11) 0.0361(12) 0.0436(12) -0.0039(10) 0.0264(10) -0.0135(9) C9 0.0417(11) 0.0197(9) 0.0426(11) 0.0039(9) 0.0289(10) 0.0014(8) C10 0.0642(15) 0.0365(13) 0.0607(15) 0.0158(12) 0.0526(14) 0.0120(11) C11 0.0428(12) 0.0565(16) 0.0468(13) 0.0083(12) 0.0323(11) 0.0105(11) C12 0.0450(12) 0.0380(12) 0.0470(13) 0.0017(11) 0.0346(11) -0.0011(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 2.0069(15) . ? Mg1 O2 2.0135(15) . ? Mg1 O3 2.0440(14) 7 ? Mg1 O4 2.0567(15) . ? Mg1 F 2.1309(12) 7 ? Mg1 F 2.1345(12) . ? Mg1 Mg3 3.1448(9) 7 ? Mg1 Mg2 3.1530(9) 7 ? Mg1 Mg2 3.1583(9) . ? Mg1 Mg3 3.1610(9) . ? Mg1 Mg1 3.4306(13) 7 ? Mg2 O7 2.0140(16) . ? Mg2 O6 2.0486(16) . ? Mg2 O5 2.0575(16) . ? Mg2 O4 2.0688(15) . ? Mg2 O3 2.0730(15) . ? Mg2 F 2.1498(12) 7 ? Mg2 Mg1 3.1530(9) 7 ? Mg2 Mg3 3.1573(9) . ? Mg3 O10 2.0208(15) . ? Mg3 O9 2.0542(15) . ? Mg3 O8 2.0595(15) . ? Mg3 O4 2.0625(15) . ? Mg3 O3 2.0688(15) . ? Mg3 F 2.1454(12) . ? Mg3 Mg1 3.1448(9) 7 ? F Mg1 2.1308(12) 7 ? F Mg2 2.1498(12) 7 ? O1 C1 1.417(2) . ? O2 C2 1.407(2) . ? O3 C3 1.424(2) . ? O3 Mg1 2.0440(14) 7 ? O4 C4 1.426(2) . ? O5 C5 1.428(3) . ? O6 C6 1.423(2) . ? O7 C7 1.422(3) . ? O8 C8 1.423(2) . ? O9 C9 1.429(2) . ? O10 C10 1.425(3) . ? O11 C11 1.412(3) . ? O12 C12 1.403(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O2 111.56(6) . . ? O1 Mg1 O3 95.97(6) . 7 ? O2 Mg1 O3 95.86(6) . 7 ? O1 Mg1 O4 96.41(6) . . ? O2 Mg1 O4 95.92(6) . . ? O3 Mg1 O4 158.43(6) 7 . ? O1 Mg1 F 87.95(5) . 7 ? O2 Mg1 F 160.49(6) . 7 ? O3 Mg1 F 81.66(5) 7 7 ? O4 Mg1 F 81.21(5) . 7 ? O1 Mg1 F 160.87(6) . . ? O2 Mg1 F 87.58(5) . . ? O3 Mg1 F 81.60(5) 7 . ? O4 Mg1 F 80.91(5) . . ? F Mg1 F 72.92(5) 7 . ? O1 Mg1 Mg3 83.83(4) . 7 ? O2 Mg1 Mg3 136.02(5) . 7 ? O3 Mg1 Mg3 40.42(4) 7 7 ? O4 Mg1 Mg3 124.05(5) . 7 ? F Mg1 Mg3 42.84(3) 7 7 ? F Mg1 Mg3 82.13(4) . 7 ? O1 Mg1 Mg2 136.08(5) . 7 ? O2 Mg1 Mg2 83.64(4) . 7 ? O3 Mg1 Mg2 40.36(4) 7 7 ? O4 Mg1 Mg2 123.71(5) . 7 ? F Mg1 Mg2 82.05(4) 7 7 ? F Mg1 Mg2 42.80(3) . 7 ? Mg3 Mg1 Mg2 60.18(2) 7 7 ? O1 Mg1 Mg2 83.99(5) . . ? O2 Mg1 Mg2 135.88(5) . . ? O3 Mg1 Mg2 124.34(5) 7 . ? O4 Mg1 Mg2 40.18(4) . . ? F Mg1 Mg2 42.69(3) 7 . ? F Mg1 Mg2 81.86(4) . . ? Mg3 Mg1 Mg2 84.79(2) 7 . ? Mg2 Mg1 Mg2 114.15(2) 7 . ? O1 Mg1 Mg3 136.12(5) . . ? O2 Mg1 Mg3 83.74(5) . . ? O3 Mg1 Mg3 124.12(5) 7 . ? O4 Mg1 Mg3 39.95(4) . . ? F Mg1 Mg3 81.78(4) 7 . ? F Mg1 Mg3 42.52(3) . . ? Mg3 Mg1 Mg3 114.08(2) 7 . ? Mg2 Mg1 Mg3 84.61(2) 7 . ? Mg2 Mg1 Mg3 59.95(2) . . ? O1 Mg1 Mg1 124.44(5) . 7 ? O2 Mg1 Mg1 124.00(5) . 7 ? O3 Mg1 Mg1 79.57(4) 7 7 ? O4 Mg1 Mg1 78.86(4) . 7 ? F Mg1 Mg1 36.50(3) 7 7 ? F Mg1 Mg1 36.42(3) . 7 ? Mg3 Mg1 Mg1 57.27(2) 7 7 ? Mg2 Mg1 Mg1 57.15(2) 7 7 ? Mg2 Mg1 Mg1 57.00(2) . 7 ? Mg3 Mg1 Mg1 56.81(2) . 7 ? O7 Mg2 O6 94.86(7) . . ? O7 Mg2 O5 93.79(7) . . ? O6 Mg2 O5 94.89(7) . . ? O7 Mg2 O4 98.62(6) . . ? O6 Mg2 O4 92.08(6) . . ? O5 Mg2 O4 165.19(7) . . ? O7 Mg2 O3 100.37(6) . . ? O6 Mg2 O3 163.72(7) . . ? O5 Mg2 O3 89.84(6) . . ? O4 Mg2 O3 80.04(6) . . ? O7 Mg2 F 178.59(6) . 7 ? O6 Mg2 F 84.10(6) . 7 ? O5 Mg2 F 87.25(5) . 7 ? O4 Mg2 F 80.48(5) . 7 ? O3 Mg2 F 80.58(5) . 7 ? O7 Mg2 Mg1 138.72(5) . 7 ? O6 Mg2 Mg1 126.13(5) . 7 ? O5 Mg2 Mg1 79.50(5) . 7 ? O4 Mg2 Mg1 85.83(4) . 7 ? O3 Mg2 Mg1 39.68(4) . 7 ? F Mg2 Mg1 42.43(3) 7 7 ? O7 Mg2 Mg3 98.43(5) . . ? O6 Mg2 Mg3 131.67(5) . . ? O5 Mg2 Mg3 129.97(5) . . ? O4 Mg2 Mg3 40.09(4) . . ? O3 Mg2 Mg3 40.28(4) . . ? F Mg2 Mg3 81.60(4) 7 . ? Mg1 Mg2 Mg3 59.78(2) 7 . ? O7 Mg2 Mg1 136.65(5) . . ? O6 Mg2 Mg1 78.72(5) . . ? O5 Mg2 Mg1 129.28(5) . . ? O4 Mg2 Mg1 39.90(4) . . ? O3 Mg2 Mg1 86.22(4) . . ? F Mg2 Mg1 42.22(3) 7 . ? Mg1 Mg2 Mg1 65.85(2) 7 . ? Mg3 Mg2 Mg1 60.07(2) . . ? O10 Mg3 O9 94.67(6) . . ? O10 Mg3 O8 93.88(6) . . ? O9 Mg3 O8 95.48(6) . . ? O10 Mg3 O4 97.34(6) . . ? O9 Mg3 O4 165.56(6) . . ? O8 Mg3 O4 91.69(6) . . ? O10 Mg3 O3 101.10(6) . . ? O9 Mg3 O3 89.57(6) . . ? O8 Mg3 O3 163.76(7) . . ? O4 Mg3 O3 80.28(6) . . ? O10 Mg3 F 176.95(6) . . ? O9 Mg3 F 87.76(5) . . ? O8 Mg3 F 84.04(5) . . ? O4 Mg3 F 80.52(5) . . ? O3 Mg3 F 80.74(5) . . ? O10 Mg3 Mg1 139.83(5) . 7 ? O9 Mg3 Mg1 79.49(5) . 7 ? O8 Mg3 Mg1 126.12(5) . 7 ? O4 Mg3 Mg1 86.15(4) . 7 ? O3 Mg3 Mg1 39.84(4) . 7 ? F Mg3 Mg1 42.48(3) . 7 ? O10 Mg3 Mg2 98.07(5) . . ? O9 Mg3 Mg2 129.83(5) . . ? O8 Mg3 Mg2 131.45(5) . . ? O4 Mg3 Mg2 40.23(4) . . ? O3 Mg3 Mg2 40.38(4) . . ? F Mg3 Mg2 81.73(4) . . ? Mg1 Mg3 Mg2 60.04(2) 7 . ? O10 Mg3 Mg1 135.15(5) . . ? O9 Mg3 Mg1 129.86(5) . . ? O8 Mg3 Mg1 78.69(5) . . ? O4 Mg3 Mg1 39.81(4) . . ? O3 Mg3 Mg1 86.21(4) . . ? F Mg3 Mg1 42.26(3) . . ? Mg1 Mg3 Mg1 65.92(2) 7 . ? Mg2 Mg3 Mg1 59.98(2) . . ? Mg1 F Mg1 107.08(5) 7 . ? Mg1 F Mg3 94.68(5) 7 . ? Mg1 F Mg3 95.22(5) . . ? Mg1 F Mg2 95.09(5) 7 7 ? Mg1 F Mg2 94.77(5) . 7 ? Mg3 F Mg2 163.33(6) . 7 ? C1 O1 Mg1 130.90(13) . . ? C2 O2 Mg1 129.32(13) . . ? C3 O3 Mg1 117.75(12) . 7 ? C3 O3 Mg3 118.21(12) . . ? Mg1 O3 Mg3 99.75(6) 7 . ? C3 O3 Mg2 118.20(12) . . ? Mg1 O3 Mg2 99.96(6) 7 . ? Mg3 O3 Mg2 99.33(6) . . ? C4 O4 Mg1 113.10(11) . . ? C4 O4 Mg3 120.35(12) . . ? Mg1 O4 Mg3 100.24(6) . . ? C4 O4 Mg2 119.95(12) . . ? Mg1 O4 Mg2 99.91(6) . . ? Mg3 O4 Mg2 99.68(6) . . ? C5 O5 Mg2 127.15(13) . . ? C6 O6 Mg2 131.64(14) . . ? C7 O7 Mg2 126.79(14) . . ? C8 O8 Mg3 130.88(14) . . ? C9 O9 Mg3 126.97(13) . . ? C10 O10 Mg3 126.66(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.356 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.062 # Attachment 'comp3.CIF' data_comp2 _database_code_depnum_ccdc_archive 'CCDC 717458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H78 F2 Mg6 O22' _chemical_formula_weight 878.70 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' F F 0.0171 0.0103 '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 I222 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-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+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' _cell_length_a 11.6887(8) _cell_length_b 11.7792(8) _cell_length_c 17.1875(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2366.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDS(Stoe) _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14122 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.87 _reflns_number_total 2829 _reflns_number_gt 1905 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0500P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(7) _refine_ls_number_reflns 2829 _refine_ls_number_parameters 160 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.5000 0.64248(6) 0.5000 0.0283(2) Uani 1 2 d S . 1 Mg2 Mg 0.36561(4) 0.4998(2) 0.37243(3) 0.03473(19) Uani 1 1 d . . 1 F F 0.38969(10) 0.5000 0.5000 0.0316(3) Uani 1 2 d S . 1 O1 O 0.5015(4) 0.61410(10) 0.37990(6) 0.0326(3) Uani 1 1 d . . 1 O2 O 0.64269(10) 0.73995(10) 0.5005(3) 0.0438(3) Uani 1 1 d . A 1 O3 O 0.2496(3) 0.3714(4) 0.39630(19) 0.0499(10) Uani 1 1 d . B 1 H3 H 0.281(4) 0.327(3) 0.449(2) 0.060 Uiso 1 1 d . C 1 O4 O 0.2501(3) 0.6293(3) 0.3948(2) 0.0469(10) Uani 0.594(4) 1 d PD D 1 H4 H 0.285(3) 0.678(3) 0.4262(17) 0.056 Uiso 1 1 d D E 1 O5 O 0.33743(14) 0.4984(6) 0.25745(9) 0.0670(6) Uani 0.594(4) 1 d P D 1 H5 H 0.405(3) 0.524(4) 0.2351(18) 0.080 Uiso 1 1 d . F 1 O6 O 0.4960(10) 0.4427(3) 0.17307(15) 0.0641(10) Uani 0.50 1 d P . 1 C1 C 0.5033(6) 0.7129(2) 0.33144(13) 0.0538(6) Uani 1 1 d . G 1 H1A H 0.4810 0.6919 0.2784 0.081 Uiso 1 1 calc R G 1 H1B H 0.5807 0.7450 0.3309 0.081 Uiso 1 1 calc R G 1 H1C H 0.4495 0.7693 0.3519 0.081 Uiso 1 1 calc R G 1 C2 C 0.6560(2) 0.85846(19) 0.5000(6) 0.0695(8) Uani 1 1 d . A 1 H2A H 0.6076 0.8921 0.5405 0.104 Uiso 1 1 calc R A 1 H2B H 0.6334 0.8884 0.4491 0.104 Uiso 1 1 calc R A 1 H2C H 0.7362 0.8776 0.5101 0.104 Uiso 1 1 calc R A 1 C3 C 0.1431(7) 0.3430(11) 0.3845(8) 0.275(9) Uani 1 1 d . B 1 H3A H 0.0990 0.4106 0.3700 0.412 Uiso 1 1 calc R B 1 H3B H 0.1112 0.3102 0.4322 0.412 Uiso 1 1 calc R B 1 H3C H 0.1390 0.2870 0.3425 0.412 Uiso 1 1 calc R B 1 C4 C 0.1775(4) 0.6912(6) 0.3464(4) 0.0535(16) Uani 0.594(4) 1 d P D 1 H4A H 0.1341 0.6390 0.3132 0.080 Uiso 0.594(4) 1 calc PR D 1 H4B H 0.2230 0.7423 0.3137 0.080 Uiso 0.594(4) 1 calc PR D 1 H4C H 0.1244 0.7359 0.3781 0.080 Uiso 0.594(4) 1 calc PR D 1 C5 C 0.2459(6) 0.4488(14) 0.2164(5) 0.100(5) Uani 0.594(4) 1 d P D 1 H5A H 0.1880 0.5067 0.2054 0.150 Uiso 0.594(4) 1 calc PR D 1 H5B H 0.2119 0.3883 0.2480 0.150 Uiso 0.594(4) 1 calc PR D 1 H5C H 0.2742 0.4169 0.1674 0.150 Uiso 0.594(4) 1 calc PR D 1 C6 C 0.5000 0.5000 0.1019(2) 0.110(2) Uani 1 2 d S H 1 H6A H 0.5124 0.5812 0.1112 0.165 Uiso 0.50 1 calc PR H 1 H6B H 0.4275 0.4892 0.0742 0.165 Uiso 0.50 1 calc PR H 1 H6C H 0.5629 0.4698 0.0704 0.165 Uiso 0.50 1 calc PR H 1 O4A O 0.2501(3) 0.6293(3) 0.3948(2) 0.0469(10) Uani 0.41 1 d P D 2 O5A O 0.33743(14) 0.4984(6) 0.25745(9) 0.0670(6) Uani 0.41 1 d P D 2 C4A C 0.1323(5) 0.6297(8) 0.4099(5) 0.0427(18) Uani 0.406(4) 1 d PU D 2 H4A1 H 0.0996 0.5562 0.3953 0.064 Uiso 0.406(4) 1 calc PR D 2 H4A2 H 0.0957 0.6900 0.3795 0.064 Uiso 0.406(4) 1 calc PR D 2 H4A3 H 0.1193 0.6433 0.4655 0.064 Uiso 0.406(4) 1 calc PR D 2 C5A C 0.2380(16) 0.5510(18) 0.2213(9) 0.129(7) Uani 0.406(4) 1 d P D 2 H5A1 H 0.2241 0.5159 0.1705 0.194 Uiso 0.406(4) 1 calc PR D 2 H5A2 H 0.2520 0.6324 0.2145 0.194 Uiso 0.406(4) 1 calc PR D 2 H5A3 H 0.1709 0.5400 0.2546 0.194 Uiso 0.406(4) 1 calc PR D 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 0.0311(4) 0.0206(4) 0.0331(4) 0.000 -0.0027(12) 0.000 Mg2 0.0277(3) 0.0431(4) 0.0335(3) 0.0000(11) -0.0065(2) 0.0074(9) F 0.0313(6) 0.0304(7) 0.0329(7) 0.008(2) 0.000 0.000 O1 0.0307(5) 0.0364(6) 0.0308(6) 0.0111(5) -0.0007(18) 0.0007(18) O2 0.0464(6) 0.0234(6) 0.0616(8) 0.002(2) -0.004(2) -0.0113(5) O3 0.0364(17) 0.071(3) 0.0423(19) -0.0077(17) -0.0111(16) -0.011(2) O4 0.0329(16) 0.040(2) 0.068(2) 0.0046(17) -0.0113(17) 0.0124(17) O5 0.0560(9) 0.1109(16) 0.0342(8) -0.007(3) -0.0141(6) 0.004(3) O6 0.073(2) 0.088(2) 0.0318(14) 0.0018(13) 0.001(5) -0.007(6) C1 0.0541(12) 0.0562(14) 0.0510(12) 0.0298(10) -0.013(3) 0.010(3) C2 0.0852(16) 0.0286(12) 0.095(2) -0.014(4) -0.007(5) -0.0220(11) C3 0.122(7) 0.284(16) 0.42(2) 0.219(14) -0.154(10) -0.125(8) C4 0.0276(19) 0.068(3) 0.065(3) 0.050(3) -0.0063(19) 0.012(2) C5 0.049(3) 0.200(16) 0.050(5) -0.022(6) -0.012(3) 0.003(5) C6 0.114(4) 0.180(6) 0.0352(18) 0.000 0.000 -0.058(9) O4A 0.0329(16) 0.040(2) 0.068(2) 0.0046(17) -0.0113(17) 0.0124(17) O5A 0.0560(9) 0.1109(16) 0.0342(8) -0.007(3) -0.0141(6) 0.004(3) C4A 0.006(2) 0.055(4) 0.067(4) -0.017(3) 0.000(2) 0.007(2) C5A 0.198(15) 0.124(13) 0.067(8) -0.021(8) -0.102(9) 0.069(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 O2 2.0249(12) . ? Mg1 O2 2.0249(12) 3_656 ? Mg1 O1 2.0911(11) . ? Mg1 O1 2.0911(11) 3_656 ? Mg1 F 2.1164(9) 2_665 ? Mg1 F 2.1164(9) . ? Mg1 Mg2 3.1754(15) 2_665 ? Mg1 Mg2 3.1754(15) 4_566 ? Mg1 Mg2 3.1781(15) . ? Mg1 Mg2 3.1781(15) 3_656 ? Mg1 Mg1 3.3566(15) 2_665 ? Mg2 O5 2.0035(15) . ? Mg2 O1 2.056(4) 2_665 ? Mg2 O3 2.072(4) . ? Mg2 O1 2.086(4) . ? Mg2 O4 2.073(4) . ? Mg2 F 2.2106(6) . ? Mg2 Mg2 3.1417(10) 2_665 ? Mg2 Mg1 3.1754(15) 2_665 ? F Mg1 2.1164(9) 2_665 ? F Mg2 2.2106(6) 4_566 ? O1 C1 1.431(2) . ? O1 Mg2 2.056(4) 2_665 ? O2 C2 1.405(3) . ? O3 C3 1.305(8) . ? O4 C4 1.395(6) . ? O5 C5 1.408(10) . ? O6 O6 1.353(7) 2_665 ? O6 C6 1.397(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mg1 O2 110.91(8) . 3_656 ? O2 Mg1 O1 95.04(19) . . ? O2 Mg1 O1 95.36(19) 3_656 . ? O2 Mg1 O1 95.36(19) . 3_656 ? O2 Mg1 O1 95.04(19) 3_656 3_656 ? O1 Mg1 O1 161.60(7) . 3_656 ? O2 Mg1 F 87.01(4) . 2_665 ? O2 Mg1 F 162.08(5) 3_656 2_665 ? O1 Mg1 F 82.42(8) . 2_665 ? O1 Mg1 F 83.01(8) 3_656 2_665 ? O2 Mg1 F 162.08(5) . . ? O2 Mg1 F 87.01(4) 3_656 . ? O1 Mg1 F 83.01(8) . . ? O1 Mg1 F 82.42(8) 3_656 . ? F Mg1 F 75.07(5) 2_665 . ? O2 Mg1 Mg2 83.96(13) . 2_665 ? O2 Mg1 Mg2 134.73(16) 3_656 2_665 ? O1 Mg1 Mg2 39.63(9) . 2_665 ? O1 Mg1 Mg2 126.97(8) 3_656 2_665 ? F Mg1 Mg2 43.96(3) 2_665 2_665 ? F Mg1 Mg2 83.28(5) . 2_665 ? O2 Mg1 Mg2 134.73(16) . 4_566 ? O2 Mg1 Mg2 83.96(13) 3_656 4_566 ? O1 Mg1 Mg2 126.97(8) . 4_566 ? O1 Mg1 Mg2 39.63(9) 3_656 4_566 ? F Mg1 Mg2 83.28(5) 2_665 4_566 ? F Mg1 Mg2 43.96(3) . 4_566 ? Mg2 Mg1 Mg2 116.30(9) 2_665 4_566 ? O2 Mg1 Mg2 135.23(16) . . ? O2 Mg1 Mg2 83.67(12) 3_656 . ? O1 Mg1 Mg2 40.41(9) . . ? O1 Mg1 Mg2 126.32(8) 3_656 . ? F Mg1 Mg2 83.21(4) 2_665 . ? F Mg1 Mg2 43.90(3) . . ? Mg2 Mg1 Mg2 59.27(2) 2_665 . ? Mg2 Mg1 Mg2 87.29(2) 4_566 . ? O2 Mg1 Mg2 83.67(12) . 3_656 ? O2 Mg1 Mg2 135.23(16) 3_656 3_656 ? O1 Mg1 Mg2 126.32(8) . 3_656 ? O1 Mg1 Mg2 40.41(9) 3_656 3_656 ? F Mg1 Mg2 43.90(3) 2_665 3_656 ? F Mg1 Mg2 83.21(4) . 3_656 ? Mg2 Mg1 Mg2 87.29(2) 2_665 3_656 ? Mg2 Mg1 Mg2 59.27(2) 4_566 3_656 ? Mg2 Mg1 Mg2 116.14(8) . 3_656 ? O2 Mg1 Mg1 124.54(4) . 2_665 ? O2 Mg1 Mg1 124.54(4) 3_656 2_665 ? O1 Mg1 Mg1 80.80(4) . 2_665 ? O1 Mg1 Mg1 80.80(4) 3_656 2_665 ? F Mg1 Mg1 37.53(3) 2_665 2_665 ? F Mg1 Mg1 37.53(3) . 2_665 ? Mg2 Mg1 Mg1 58.15(4) 2_665 2_665 ? Mg2 Mg1 Mg1 58.15(4) 4_566 2_665 ? Mg2 Mg1 Mg1 58.07(4) . 2_665 ? Mg2 Mg1 Mg1 58.07(4) 3_656 2_665 ? O5 Mg2 O1 100.41(15) . 2_665 ? O5 Mg2 O3 94.70(19) . . ? O1 Mg2 O3 90.34(17) 2_665 . ? O5 Mg2 O1 101.01(16) . . ? O1 Mg2 O1 80.91(5) 2_665 . ? O3 Mg2 O1 163.15(11) . . ? O5 Mg2 O4 94.70(18) . . ? O1 Mg2 O4 163.79(12) 2_665 . ? O3 Mg2 O4 94.26(6) . . ? O1 Mg2 O4 90.53(16) . . ? O5 Mg2 F 177.81(8) . . ? O1 Mg2 F 80.95(5) 2_665 . ? O3 Mg2 F 83.56(11) . . ? O1 Mg2 F 80.87(6) . . ? O4 Mg2 F 84.14(11) . . ? O5 Mg2 Mg2 99.47(5) . 2_665 ? O1 Mg2 Mg2 41.04(9) 2_665 2_665 ? O3 Mg2 Mg2 130.97(16) . 2_665 ? O1 Mg2 Mg2 40.32(9) . 2_665 ? O4 Mg2 Mg2 130.52(16) . 2_665 ? F Mg2 Mg2 82.69(3) . 2_665 ? O5 Mg2 Mg1 139.31(19) . 2_665 ? O1 Mg2 Mg1 40.44(4) 2_665 2_665 ? O3 Mg2 Mg1 78.58(12) . 2_665 ? O1 Mg2 Mg1 85.49(6) . 2_665 ? O4 Mg2 Mg1 125.61(10) . 2_665 ? F Mg2 Mg1 41.65(3) . 2_665 ? Mg2 Mg2 Mg1 60.41(4) 2_665 2_665 ? O5 Mg2 Mg1 139.99(19) . . ? O1 Mg2 Mg1 85.90(6) 2_665 . ? O3 Mg2 Mg1 124.95(10) . . ? O1 Mg2 Mg1 40.52(4) . . ? O4 Mg2 Mg1 78.72(11) . . ? F Mg2 Mg1 41.60(3) . . ? Mg2 Mg2 Mg1 60.32(5) 2_665 . ? Mg1 Mg2 Mg1 63.78(2) 2_665 . ? Mg1 F Mg1 104.93(5) 2_665 . ? Mg1 F Mg2 94.39(5) 2_665 . ? Mg1 F Mg2 94.50(6) . . ? Mg1 F Mg2 94.50(6) 2_665 4_566 ? Mg1 F Mg2 94.39(6) . 4_566 ? Mg2 F Mg2 165.37(6) . 4_566 ? C1 O1 Mg2 118.9(3) . 2_665 ? C1 O1 Mg2 120.0(3) . . ? Mg2 O1 Mg2 98.64(5) 2_665 . ? C1 O1 Mg1 116.41(12) . . ? Mg2 O1 Mg1 99.92(11) 2_665 . ? Mg2 O1 Mg1 99.06(11) . . ? C2 O2 Mg1 130.89(13) . . ? C3 O3 Mg2 141.3(6) . . ? C4 O4 Mg2 132.1(4) . . ? C5 O5 Mg2 128.5(5) . . ? O6 O6 C6 61.05(15) 2_665 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.382 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.046