# Electronic Supplementary Material (ESI) for Energy & Environmental Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Energy Environ.Sci.' _journal_coden_cambridge 1148 #TrackingRef '- jm-EES-composite.cif' _publ_contact_author_name 'Muldoon, John' _publ_contact_author_address ; Toyota Research Institute of North America 1555 Woodridge Avenue Ann Arbor, MI 48105 USA ; _publ_contact_author_email john.muldoon@tema.toyota.com _publ_contact_author_phone '734 262 4102' _publ_requested_category FI loop_ _publ_author_name _publ_author_address J.Muldoon ; Toyota Research Institute of North America 1555 Woodridge Avenue Ann Arbor, MI 48105 USA ; C.B.Bucur ; Toyota Research Institute of North America 1555 Woodridge Avenue Ann Arbor, MI 48105 USA ; A.G.Oliver ; Department of Chemistry and Biochemistry, University of Notre Dame Notre Dame, IN 46556 USA ; M.Matsui ; Toyota Research Institute of North America, 1555 Woodridge Avenue, Ann Arbor, MI 48105, USA ; H.S.Kim ; Toyota Research Institute of North America, 1555 Woodridge Avenue, Ann Arbor, MI 48105, USA ; G.D.Allred ; Sunthonix Inc. 2713 Connector Drive Wake Forest, NC 2758 USA ; ; J.Zajicek ; ; Department of Chemistry and Biochemistry, University of Notre Dame Notre Dame, IN 46556 USA ; Yu.Kotani ; Toyota Motor Corporation 1200 Mishuku Susono, Shizuku 410-1193 Japan ; #TrackingRef '- jm001.cif' _publ_section_title jm001 #================END data_cmpd2 _database_code_depnum_ccdc_archive 'CCDC 852856' #TrackingRef '- jm-EES-composite.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Cl3 Mg2 O6, C12 H10 Al Cl2' _chemical_formula_sum 'C36 H58 Al Cl5 Mg2 O6' _chemical_formula_weight 839.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9569(3) _cell_length_b 13.0714(3) _cell_length_c 13.4709(3) _cell_angle_alpha 77.7570(10) _cell_angle_beta 85.9360(10) _cell_angle_gamma 72.0740(10) _cell_volume 2121.33(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9651 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8890 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS, Sheldrick, 2008' _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 'Bruker APEX-II' _diffrn_measurement_method 'combination of \w and \f-scans ' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 29686 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.40 _reflns_number_total 8601 _reflns_number_gt 6821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-II v2009-7' _computing_cell_refinement 'Bruker SAINT v7.60A' _computing_data_reduction 'Bruker SAINT v7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0314P)^2^+0.9662P] 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 8601 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _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 0.19145(5) 0.62555(5) 0.56277(4) 0.01910(14) Uani 1 1 d . . . Mg2 Mg 0.18602(5) 0.79534(5) 0.35742(4) 0.01890(14) Uani 1 1 d . . . Cl1 Cl 0.11988(4) 0.62939(4) 0.39280(3) 0.02255(11) Uani 1 1 d . . . Cl2 Cl 0.09738(4) 0.82869(3) 0.52320(3) 0.02075(10) Uani 1 1 d . . . Cl3 Cl 0.34644(4) 0.67258(4) 0.46309(3) 0.02218(11) Uani 1 1 d . . . O1 O 0.26463(10) 0.62737(10) 0.69396(9) 0.0218(3) Uani 1 1 d . . . O2 O 0.25938(10) 0.45632(10) 0.58292(10) 0.0228(3) Uani 1 1 d . . . O3 O 0.05716(10) 0.60349(10) 0.64590(9) 0.0215(3) Uani 1 1 d . . . O4 O 0.23335(10) 0.93804(10) 0.33754(9) 0.0203(3) Uani 1 1 d . . . O5 O 0.27176(11) 0.76338(10) 0.22665(9) 0.0237(3) Uani 1 1 d . . . O6 O 0.04738(10) 0.88029(10) 0.26813(9) 0.0210(3) Uani 1 1 d . . . C1 C 0.26038(17) 0.72891(16) 0.72470(14) 0.0264(4) Uani 1 1 d . . . H1A H 0.1849 0.7694 0.7403 0.032 Uiso 1 1 calc R . . H1B H 0.2896 0.7767 0.6704 0.032 Uiso 1 1 calc R . . C2 C 0.33007(17) 0.69284(17) 0.81847(15) 0.0283(5) Uani 1 1 d . . . H2A H 0.2892 0.6705 0.8798 0.034 Uiso 1 1 calc R . . H2B H 0.3588 0.7517 0.8288 0.034 Uiso 1 1 calc R . . C3 C 0.42036(18) 0.59570(17) 0.79334(17) 0.0335(5) Uani 1 1 d . . . H3A H 0.4772 0.6203 0.7509 0.040 Uiso 1 1 calc R . . H3B H 0.4540 0.5447 0.8559 0.040 Uiso 1 1 calc R . . C4 C 0.36289(17) 0.54182(16) 0.73534(16) 0.0295(5) Uani 1 1 d . . . H4A H 0.4098 0.5133 0.6799 0.035 Uiso 1 1 calc R . . H4B H 0.3441 0.4801 0.7812 0.035 Uiso 1 1 calc R . . C5 C 0.35232(18) 0.40173(16) 0.52554(17) 0.0328(5) Uani 1 1 d . . . H5A H 0.4134 0.4319 0.5273 0.039 Uiso 1 1 calc R . . H5B H 0.3327 0.4104 0.4539 0.039 Uiso 1 1 calc R . . C6 C 0.38175(19) 0.28305(17) 0.57855(18) 0.0390(5) Uani 1 1 d . . . H6A H 0.4200 0.2342 0.5319 0.047 Uiso 1 1 calc R . . H6B H 0.4281 0.2691 0.6383 0.047 Uiso 1 1 calc R . . C7 C 0.27331(18) 0.26699(17) 0.61018(17) 0.0351(5) Uani 1 1 d . . . H7A H 0.2804 0.2055 0.6692 0.042 Uiso 1 1 calc R . . H7B H 0.2388 0.2523 0.5536 0.042 Uiso 1 1 calc R . . C8 C 0.20890(17) 0.37502(15) 0.63800(15) 0.0263(4) Uani 1 1 d . . . H8A H 0.1322 0.3949 0.6177 0.032 Uiso 1 1 calc R . . H8B H 0.2116 0.3703 0.7122 0.032 Uiso 1 1 calc R . . C9 C 0.04521(17) 0.58462(17) 0.75606(14) 0.0267(4) Uani 1 1 d . . . H9A H 0.0360 0.6528 0.7812 0.032 Uiso 1 1 calc R . . H9B H 0.1092 0.5269 0.7892 0.032 Uiso 1 1 calc R . . C10 C -0.05540(17) 0.54822(17) 0.77607(15) 0.0273(4) Uani 1 1 d . . . H10A H -0.0878 0.5597 0.8431 0.033 Uiso 1 1 calc R . . H10B H -0.0400 0.4701 0.7723 0.033 Uiso 1 1 calc R . . C11 C -0.12829(16) 0.62397(16) 0.68948(15) 0.0279(4) Uani 1 1 d . . . H11A H -0.1849 0.5928 0.6750 0.033 Uiso 1 1 calc R . . H11B H -0.1635 0.6975 0.7054 0.033 Uiso 1 1 calc R . . C12 C -0.04980(16) 0.62969(17) 0.60115(15) 0.0259(4) Uani 1 1 d . . . H12A H -0.0500 0.5761 0.5592 0.031 Uiso 1 1 calc R . . H12B H -0.0700 0.7041 0.5578 0.031 Uiso 1 1 calc R . . C13 C 0.17367(16) 1.03597(15) 0.37679(15) 0.0239(4) Uani 1 1 d . . . H13A H 0.1041 1.0286 0.4080 0.029 Uiso 1 1 calc R . . H13B H 0.1582 1.1019 0.3216 0.029 Uiso 1 1 calc R . . C14 C 0.24720(18) 1.04460(19) 0.45622(17) 0.0376(5) Uani 1 1 d . . . H14A H 0.2160 1.0308 0.5252 0.045 Uiso 1 1 calc R . . H14B H 0.2574 1.1183 0.4424 0.045 Uiso 1 1 calc R . . C15 C 0.35488(16) 0.95631(16) 0.44661(14) 0.0258(4) Uani 1 1 d . . . H15A H 0.4172 0.9843 0.4494 0.031 Uiso 1 1 calc R . . H15B H 0.3624 0.8904 0.5010 0.031 Uiso 1 1 calc R . . C16 C 0.34679(15) 0.93128(16) 0.34356(14) 0.0223(4) Uani 1 1 d . . . H16A H 0.3664 0.9859 0.2888 0.027 Uiso 1 1 calc R . . H16B H 0.3946 0.8570 0.3389 0.027 Uiso 1 1 calc R . . C17 C 0.3217(2) 0.65340(18) 0.20449(17) 0.0407(6) Uani 1 1 d . . . H17A H 0.2659 0.6162 0.2034 0.049 Uiso 1 1 calc R . . H17B H 0.3762 0.6081 0.2567 0.049 Uiso 1 1 calc R . . C18 C 0.37490(19) 0.66958(18) 0.10221(16) 0.0339(5) Uani 1 1 d . . . H18A H 0.3667 0.6171 0.0622 0.041 Uiso 1 1 calc R . . H18B H 0.4531 0.6601 0.1089 0.041 Uiso 1 1 calc R . . C19 C 0.31453(18) 0.78705(17) 0.05277(15) 0.0312(5) Uani 1 1 d . . . H19A H 0.3598 0.8188 0.0005 0.037 Uiso 1 1 calc R . . H19B H 0.2461 0.7913 0.0215 0.037 Uiso 1 1 calc R . . C20 C 0.29286(17) 0.84413(16) 0.14166(14) 0.0259(4) Uani 1 1 d . . . H20A H 0.3566 0.8656 0.1553 0.031 Uiso 1 1 calc R . . H20B H 0.2293 0.9106 0.1286 0.031 Uiso 1 1 calc R . . C21 C 0.02641(16) 0.84014(17) 0.18015(14) 0.0271(4) Uani 1 1 d . . . H21A H 0.0639 0.7605 0.1877 0.033 Uiso 1 1 calc R . . H21B H 0.0523 0.8792 0.1169 0.033 Uiso 1 1 calc R . . C22 C -0.09493(18) 0.8626(2) 0.17723(17) 0.0373(5) Uani 1 1 d . . . H22A H -0.1168 0.7989 0.2152 0.045 Uiso 1 1 calc R . . H22B H -0.1211 0.8807 0.1065 0.045 Uiso 1 1 calc R . . C23 C -0.13774(16) 0.96108(18) 0.22866(16) 0.0311(5) Uani 1 1 d . . . H23A H -0.1383 1.0304 0.1812 0.037 Uiso 1 1 calc R . . H23B H -0.2117 0.9672 0.2565 0.037 Uiso 1 1 calc R . . C24 C -0.05626(16) 0.93305(18) 0.31190(15) 0.0299(5) Uani 1 1 d . . . H24A H -0.0541 1.0002 0.3335 0.036 Uiso 1 1 calc R . . H24B H -0.0746 0.8826 0.3715 0.036 Uiso 1 1 calc R . . Al1 Al 0.31255(5) 0.27824(5) 0.02108(4) 0.02245(13) Uani 1 1 d . . . Cl4 Cl 0.37992(4) 0.24056(4) -0.12521(4) 0.03246(12) Uani 1 1 d . . . Cl5 Cl 0.29198(5) 0.45145(4) 0.01385(4) 0.03436(13) Uani 1 1 d . . . C25 C 0.41580(15) 0.18821(15) 0.13038(14) 0.0222(4) Uani 1 1 d . . . C26 C 0.41380(16) 0.22154(16) 0.22301(15) 0.0257(4) Uani 1 1 d . . . H26A H 0.3634 0.2893 0.2318 0.031 Uiso 1 1 calc R . . C27 C 0.48321(16) 0.15863(17) 0.30246(15) 0.0279(5) Uani 1 1 d . . . H27A H 0.4791 0.1835 0.3644 0.033 Uiso 1 1 calc R . . C28 C 0.55823(16) 0.05988(17) 0.29151(15) 0.0266(4) Uani 1 1 d . . . H28A H 0.6063 0.0172 0.3453 0.032 Uiso 1 1 calc R . . C29 C 0.56230(16) 0.02405(17) 0.20114(15) 0.0276(4) Uani 1 1 d . . . H29A H 0.6130 -0.0438 0.1929 0.033 Uiso 1 1 calc R . . C30 C 0.49229(16) 0.08728(16) 0.12279(14) 0.0250(4) Uani 1 1 d . . . H30A H 0.4963 0.0612 0.0615 0.030 Uiso 1 1 calc R . . C31 C 0.16804(16) 0.25446(15) 0.04014(14) 0.0223(4) Uani 1 1 d . . . C32 C 0.07300(17) 0.32978(16) -0.00468(15) 0.0267(4) Uani 1 1 d . . . H32A H 0.0770 0.3970 -0.0461 0.032 Uiso 1 1 calc R . . C33 C -0.02687(17) 0.31000(16) 0.00907(15) 0.0274(4) Uani 1 1 d . . . H34A H -0.0898 0.3630 -0.0225 0.033 Uiso 1 1 calc R . . C35 C -0.03384(17) 0.21228(17) 0.06930(15) 0.0275(4) Uani 1 1 d . . . H35A H -0.1017 0.1978 0.0788 0.033 Uiso 1 1 calc R . . C36 C 0.05793(17) 0.13599(17) 0.11548(15) 0.0282(5) Uani 1 1 d . . . H36A H 0.0534 0.0691 0.1573 0.034 Uiso 1 1 calc R . . C37 C 0.15716(17) 0.15765(16) 0.10045(15) 0.0264(4) Uani 1 1 d . . . H37A H 0.2197 0.1045 0.1325 0.032 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 0.0214(3) 0.0156(3) 0.0210(3) -0.0039(2) 0.0016(3) -0.0067(3) Mg2 0.0218(3) 0.0164(3) 0.0198(3) -0.0049(2) 0.0014(3) -0.0071(3) Cl1 0.0283(3) 0.0196(2) 0.0234(2) -0.00630(18) 0.00057(19) -0.0114(2) Cl2 0.0249(3) 0.0158(2) 0.0208(2) -0.00481(17) 0.00163(18) -0.00463(19) Cl3 0.0208(2) 0.0196(2) 0.0253(2) -0.00199(18) 0.00103(18) -0.00667(19) O1 0.0251(7) 0.0168(6) 0.0241(7) -0.0046(5) -0.0017(6) -0.0062(6) O2 0.0238(7) 0.0152(6) 0.0284(7) -0.0039(5) 0.0042(6) -0.0060(6) O3 0.0210(7) 0.0235(7) 0.0201(7) -0.0037(5) 0.0014(5) -0.0075(6) O4 0.0199(7) 0.0178(6) 0.0249(7) -0.0066(5) 0.0014(5) -0.0071(6) O5 0.0302(8) 0.0179(7) 0.0217(7) -0.0054(5) 0.0061(6) -0.0056(6) O6 0.0213(7) 0.0213(7) 0.0216(7) -0.0074(5) 0.0003(5) -0.0062(6) C1 0.0346(12) 0.0203(10) 0.0263(10) -0.0074(8) -0.0014(9) -0.0094(9) C2 0.0333(12) 0.0279(11) 0.0270(10) -0.0054(8) -0.0043(9) -0.0132(10) C3 0.0316(12) 0.0283(11) 0.0420(13) -0.0083(9) -0.0091(10) -0.0083(10) C4 0.0306(12) 0.0215(10) 0.0352(11) -0.0042(9) -0.0082(9) -0.0054(9) C5 0.0315(12) 0.0232(11) 0.0407(12) -0.0107(9) 0.0095(10) -0.0032(10) C6 0.0374(14) 0.0249(11) 0.0504(14) -0.0102(10) 0.0063(11) -0.0029(10) C7 0.0421(14) 0.0194(10) 0.0437(13) -0.0083(9) 0.0008(11) -0.0083(10) C8 0.0308(12) 0.0170(10) 0.0321(11) -0.0024(8) 0.0011(9) -0.0106(9) C9 0.0325(12) 0.0300(11) 0.0219(10) -0.0087(8) 0.0045(8) -0.0143(10) C10 0.0322(12) 0.0277(11) 0.0265(10) -0.0093(8) 0.0086(9) -0.0151(10) C11 0.0247(11) 0.0244(10) 0.0366(12) -0.0095(9) 0.0062(9) -0.0095(9) C12 0.0233(11) 0.0263(10) 0.0292(10) -0.0036(8) -0.0019(8) -0.0097(9) C13 0.0253(11) 0.0150(9) 0.0302(10) -0.0054(8) 0.0007(8) -0.0039(8) C14 0.0363(13) 0.0427(13) 0.0399(13) -0.0248(11) -0.0014(10) -0.0094(11) C15 0.0288(11) 0.0276(11) 0.0245(10) -0.0048(8) -0.0015(8) -0.0136(9) C16 0.0204(10) 0.0223(10) 0.0266(10) -0.0046(8) 0.0006(8) -0.0104(8) C17 0.0545(16) 0.0238(11) 0.0350(12) -0.0112(9) 0.0081(11) 0.0026(11) C18 0.0383(13) 0.0345(12) 0.0362(12) -0.0188(10) 0.0078(10) -0.0153(11) C19 0.0339(12) 0.0391(12) 0.0241(10) -0.0098(9) 0.0044(9) -0.0149(10) C20 0.0308(12) 0.0259(10) 0.0218(10) -0.0033(8) 0.0042(8) -0.0117(9) C21 0.0298(12) 0.0310(11) 0.0232(10) -0.0088(8) -0.0038(8) -0.0099(9) C22 0.0298(12) 0.0520(15) 0.0390(13) -0.0216(11) 0.0026(10) -0.0174(11) C23 0.0201(11) 0.0375(12) 0.0356(12) -0.0067(9) -0.0018(9) -0.0088(10) C24 0.0231(11) 0.0346(12) 0.0322(11) -0.0142(9) 0.0020(9) -0.0048(9) Al1 0.0244(3) 0.0187(3) 0.0249(3) -0.0028(2) -0.0013(2) -0.0082(3) Cl4 0.0391(3) 0.0323(3) 0.0270(3) -0.0077(2) 0.0020(2) -0.0116(2) Cl5 0.0394(3) 0.0200(2) 0.0453(3) -0.0056(2) 0.0024(2) -0.0124(2) C25 0.0211(10) 0.0224(10) 0.0264(10) -0.0039(8) -0.0004(8) -0.0119(8) C26 0.0229(11) 0.0253(10) 0.0307(11) -0.0087(8) 0.0038(8) -0.0086(9) C27 0.0277(11) 0.0356(12) 0.0244(10) -0.0097(9) 0.0007(8) -0.0132(10) C28 0.0235(11) 0.0303(11) 0.0265(10) -0.0016(8) -0.0026(8) -0.0111(9) C29 0.0229(11) 0.0239(10) 0.0358(11) -0.0058(9) 0.0001(9) -0.0067(9) C30 0.0278(11) 0.0268(11) 0.0242(10) -0.0081(8) 0.0011(8) -0.0118(9) C31 0.0256(11) 0.0198(9) 0.0221(10) -0.0071(8) -0.0017(8) -0.0053(8) C32 0.0316(12) 0.0223(10) 0.0255(10) -0.0020(8) -0.0029(9) -0.0084(9) C33 0.0253(11) 0.0276(11) 0.0265(10) -0.0068(8) -0.0059(8) -0.0019(9) C35 0.0256(11) 0.0341(11) 0.0278(11) -0.0118(9) 0.0015(9) -0.0126(10) C36 0.0329(12) 0.0247(10) 0.0292(11) -0.0021(8) -0.0007(9) -0.0141(10) C37 0.0265(11) 0.0247(10) 0.0282(10) -0.0033(8) -0.0054(8) -0.0080(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O3 2.0640(14) . ? Mg1 O1 2.0717(13) . ? Mg1 O2 2.0791(14) . ? Mg1 Cl3 2.4983(7) . ? Mg1 Cl2 2.5140(7) . ? Mg1 Cl1 2.5156(7) . ? Mg1 Mg2 3.1480(8) . ? Mg2 O5 2.0643(14) . ? Mg2 O4 2.0968(13) . ? Mg2 O6 2.1020(14) . ? Mg2 Cl2 2.4974(7) . ? Mg2 Cl1 2.5128(7) . ? Mg2 Cl3 2.5138(8) . ? O1 C1 1.456(2) . ? O1 C4 1.464(2) . ? O2 C5 1.459(2) . ? O2 C8 1.460(2) . ? O3 C9 1.457(2) . ? O3 C12 1.463(2) . ? O4 C16 1.452(2) . ? O4 C13 1.461(2) . ? O5 C20 1.456(2) . ? O5 C17 1.469(2) . ? O6 C24 1.455(2) . ? O6 C21 1.467(2) . ? C1 C2 1.510(3) . ? C2 C3 1.519(3) . ? C3 C4 1.516(3) . ? C5 C6 1.505(3) . ? C6 C7 1.503(3) . ? C7 C8 1.512(3) . ? C9 C10 1.509(3) . ? C10 C11 1.524(3) . ? C11 C12 1.514(3) . ? C13 C14 1.526(3) . ? C14 C15 1.530(3) . ? C15 C16 1.510(3) . ? C17 C18 1.500(3) . ? C18 C19 1.521(3) . ? C19 C20 1.507(3) . ? C21 C22 1.510(3) . ? C22 C23 1.526(3) . ? C23 C24 1.504(3) . ? Al1 C25 1.979(2) . ? Al1 C31 1.981(2) . ? Al1 Cl5 2.1783(7) . ? Al1 Cl4 2.1889(8) . ? C25 C26 1.402(3) . ? C25 C30 1.404(3) . ? C26 C27 1.392(3) . ? C27 C28 1.386(3) . ? C28 C29 1.386(3) . ? C29 C30 1.387(3) . ? C31 C37 1.392(3) . ? C31 C32 1.399(3) . ? C32 C33 1.388(3) . ? C33 C35 1.385(3) . ? C35 C36 1.381(3) . ? C36 C37 1.392(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C32 H32A 0.9500 . ? C33 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? 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 90.26(5) . . ? O3 Mg1 O2 89.85(5) . . ? O1 Mg1 O2 91.02(5) . . ? O3 Mg1 Cl3 174.12(5) . . ? O1 Mg1 Cl3 88.62(4) . . ? O2 Mg1 Cl3 95.94(4) . . ? O3 Mg1 Cl2 89.16(4) . . ? O1 Mg1 Cl2 95.12(4) . . ? O2 Mg1 Cl2 173.79(5) . . ? Cl3 Mg1 Cl2 85.20(2) . . ? O3 Mg1 Cl1 96.07(4) . . ? O1 Mg1 Cl1 173.61(5) . . ? O2 Mg1 Cl1 89.86(4) . . ? Cl3 Mg1 Cl1 84.99(2) . . ? Cl2 Mg1 Cl1 84.15(2) . . ? O3 Mg1 Mg2 125.42(4) . . ? O1 Mg1 Mg2 123.84(4) . . ? O2 Mg1 Mg2 125.72(4) . . ? Cl3 Mg1 Mg2 51.311(19) . . ? Cl2 Mg1 Mg2 50.850(18) . . ? Cl1 Mg1 Mg2 51.202(18) . . ? O5 Mg2 O4 87.85(5) . . ? O5 Mg2 O6 88.79(5) . . ? O4 Mg2 O6 91.13(5) . . ? O5 Mg2 Cl2 175.13(5) . . ? O4 Mg2 Cl2 90.97(4) . . ? O6 Mg2 Cl2 95.95(4) . . ? O5 Mg2 Cl1 96.69(4) . . ? O4 Mg2 Cl1 175.43(5) . . ? O6 Mg2 Cl1 88.47(4) . . ? Cl2 Mg2 Cl1 84.55(2) . . ? O5 Mg2 Cl3 90.20(4) . . ? O4 Mg2 Cl3 95.80(4) . . ? O6 Mg2 Cl3 172.96(4) . . ? Cl2 Mg2 Cl3 85.22(2) . . ? Cl1 Mg2 Cl3 84.73(2) . . ? O5 Mg2 Mg1 126.25(4) . . ? O4 Mg2 Mg1 125.97(4) . . ? O6 Mg2 Mg1 125.13(4) . . ? Cl2 Mg2 Mg1 51.320(18) . . ? Cl1 Mg2 Mg1 51.282(18) . . ? Cl3 Mg2 Mg1 50.872(18) . . ? Mg2 Cl1 Mg1 77.52(2) . . ? Mg2 Cl2 Mg1 77.83(2) . . ? Mg1 Cl3 Mg2 77.82(2) . . ? C1 O1 C4 108.91(14) . . ? C1 O1 Mg1 122.44(11) . . ? C4 O1 Mg1 122.51(11) . . ? C5 O2 C8 108.95(14) . . ? C5 O2 Mg1 124.34(11) . . ? C8 O2 Mg1 125.39(11) . . ? C9 O3 C12 108.47(14) . . ? C9 O3 Mg1 126.86(11) . . ? C12 O3 Mg1 123.34(11) . . ? C16 O4 C13 104.85(13) . . ? C16 O4 Mg2 120.71(11) . . ? C13 O4 Mg2 124.68(11) . . ? C20 O5 C17 108.69(14) . . ? C20 O5 Mg2 126.51(11) . . ? C17 O5 Mg2 124.80(11) . . ? C24 O6 C21 108.42(14) . . ? C24 O6 Mg2 122.23(11) . . ? C21 O6 Mg2 120.33(11) . . ? O1 C1 C2 104.76(15) . . ? C1 C2 C3 102.11(16) . . ? C4 C3 C2 103.54(17) . . ? O1 C4 C3 106.05(15) . . ? O2 C5 C6 104.27(16) . . ? C7 C6 C5 103.00(18) . . ? C6 C7 C8 103.42(16) . . ? O2 C8 C7 106.08(16) . . ? O3 C9 C10 104.15(15) . . ? C9 C10 C11 101.30(15) . . ? C12 C11 C10 102.94(16) . . ? O3 C12 C11 106.09(15) . . ? O4 C13 C14 105.67(15) . . ? C13 C14 C15 104.96(16) . . ? C16 C15 C14 103.01(16) . . ? O4 C16 C15 103.39(15) . . ? O5 C17 C18 106.34(17) . . ? C17 C18 C19 103.79(17) . . ? C20 C19 C18 102.26(16) . . ? O5 C20 C19 104.67(15) . . ? O6 C21 C22 106.06(16) . . ? C21 C22 C23 102.69(16) . . ? C24 C23 C22 101.57(17) . . ? O6 C24 C23 105.32(16) . . ? C25 Al1 C31 113.17(8) . . ? C25 Al1 Cl5 109.53(6) . . ? C31 Al1 Cl5 108.53(6) . . ? C25 Al1 Cl4 109.28(6) . . ? C31 Al1 Cl4 108.93(6) . . ? Cl5 Al1 Cl4 107.23(3) . . ? C26 C25 C30 115.75(18) . . ? C26 C25 Al1 120.74(15) . . ? C30 C25 Al1 123.48(14) . . ? C27 C26 C25 122.18(19) . . ? C28 C27 C26 120.23(18) . . ? C27 C28 C29 119.21(19) . . ? C28 C29 C30 119.94(19) . . ? C29 C30 C25 122.67(18) . . ? C37 C31 C32 116.17(18) . . ? C37 C31 Al1 119.92(15) . . ? C32 C31 Al1 123.91(14) . . ? C33 C32 C31 122.52(18) . . ? C35 C33 C32 119.36(19) . . ? C36 C35 C33 119.97(19) . . ? C35 C36 C37 119.60(18) . . ? C36 C37 C31 122.38(19) . . ? O1 C1 H1A 110.8 . . ? C2 C1 H1A 110.8 . . ? O1 C1 H1B 110.8 . . ? C2 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? C1 C2 H2A 111.3 . . ? C3 C2 H2A 111.3 . . ? C1 C2 H2B 111.3 . . ? C3 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? C4 C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? C4 C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.0 . . ? O1 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O1 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? O2 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? O2 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? C7 C6 H6A 111.2 . . ? C5 C6 H6A 111.2 . . ? C7 C6 H6B 111.2 . . ? C5 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C6 C7 H7A 111.1 . . ? C8 C7 H7A 111.1 . . ? C6 C7 H7B 111.1 . . ? C8 C7 H7B 111.1 . . ? H7A C7 H7B 109.0 . . ? O2 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O2 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? O3 C9 H9A 110.9 . . ? C10 C9 H9A 110.9 . . ? O3 C9 H9B 110.9 . . ? C10 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? C9 C10 H10A 111.5 . . ? C11 C10 H10A 111.5 . . ? C9 C10 H10B 111.5 . . ? C11 C10 H10B 111.5 . . ? H10A C10 H10B 109.3 . . ? C12 C11 H11A 111.2 . . ? C10 C11 H11A 111.2 . . ? C12 C11 H11B 111.2 . . ? C10 C11 H11B 111.2 . . ? H11A C11 H11B 109.1 . . ? O3 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? O3 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? O4 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? O4 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C13 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? C13 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.8 . . ? C16 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? C16 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? O4 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? O4 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.0 . . ? O5 C17 H17A 110.5 . . ? C18 C17 H17A 110.5 . . ? O5 C17 H17B 110.5 . . ? C18 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? C17 C18 H18A 111.0 . . ? C19 C18 H18A 111.0 . . ? C17 C18 H18B 111.0 . . ? C19 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C20 C19 H19A 111.3 . . ? C18 C19 H19A 111.3 . . ? C20 C19 H19B 111.3 . . ? C18 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? O5 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? O5 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.9 . . ? O6 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O6 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? C24 C23 H23A 111.5 . . ? C22 C23 H23A 111.5 . . ? C24 C23 H23B 111.5 . . ? C22 C23 H23B 111.5 . . ? H23A C23 H23B 109.3 . . ? O6 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? O6 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? C27 C26 H26A 118.9 . . ? C25 C26 H26A 118.9 . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 H30A 118.7 . . ? C25 C30 H30A 118.7 . . ? C33 C32 H32A 118.7 . . ? C31 C32 H32A 118.7 . . ? C35 C33 H34A 120.3 . . ? C32 C33 H34A 120.3 . . ? C36 C35 H35A 120.0 . . ? C33 C35 H35A 120.0 . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? C36 C37 H37A 118.8 . . ? C31 C37 H37A 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mg1 Mg2 O5 -132.35(7) . . . . ? O1 Mg1 Mg2 O5 108.73(7) . . . . ? O2 Mg1 Mg2 O5 -11.85(8) . . . . ? Cl3 Mg1 Mg2 O5 53.77(5) . . . . ? Cl2 Mg1 Mg2 O5 174.68(6) . . . . ? Cl1 Mg1 Mg2 O5 -66.25(6) . . . . ? O3 Mg1 Mg2 O4 109.31(7) . . . . ? O1 Mg1 Mg2 O4 -9.61(8) . . . . ? O2 Mg1 Mg2 O4 -130.19(7) . . . . ? Cl3 Mg1 Mg2 O4 -64.57(5) . . . . ? Cl2 Mg1 Mg2 O4 56.34(5) . . . . ? Cl1 Mg1 Mg2 O4 175.41(6) . . . . ? O3 Mg1 Mg2 O6 -13.40(8) . . . . ? O1 Mg1 Mg2 O6 -132.32(7) . . . . ? O2 Mg1 Mg2 O6 107.10(7) . . . . ? Cl3 Mg1 Mg2 O6 172.72(5) . . . . ? Cl2 Mg1 Mg2 O6 -66.37(5) . . . . ? Cl1 Mg1 Mg2 O6 52.70(5) . . . . ? O3 Mg1 Mg2 Cl2 52.97(5) . . . . ? O1 Mg1 Mg2 Cl2 -65.96(5) . . . . ? O2 Mg1 Mg2 Cl2 173.47(6) . . . . ? Cl3 Mg1 Mg2 Cl2 -120.91(3) . . . . ? Cl1 Mg1 Mg2 Cl2 119.06(3) . . . . ? O3 Mg1 Mg2 Cl1 -66.09(5) . . . . ? O1 Mg1 Mg2 Cl1 174.98(6) . . . . ? O2 Mg1 Mg2 Cl1 54.40(5) . . . . ? Cl3 Mg1 Mg2 Cl1 120.03(3) . . . . ? Cl2 Mg1 Mg2 Cl1 -119.06(3) . . . . ? O3 Mg1 Mg2 Cl3 173.88(6) . . . . ? O1 Mg1 Mg2 Cl3 54.95(5) . . . . ? O2 Mg1 Mg2 Cl3 -65.62(5) . . . . ? Cl2 Mg1 Mg2 Cl3 120.91(3) . . . . ? Cl1 Mg1 Mg2 Cl3 -120.03(3) . . . . ? O5 Mg2 Cl1 Mg1 132.00(5) . . . . ? O6 Mg2 Cl1 Mg1 -139.40(4) . . . . ? Cl2 Mg2 Cl1 Mg1 -43.27(2) . . . . ? Cl3 Mg2 Cl1 Mg1 42.41(2) . . . . ? O3 Mg1 Cl1 Mg2 131.48(4) . . . . ? O2 Mg1 Cl1 Mg2 -138.69(4) . . . . ? Cl3 Mg1 Cl1 Mg2 -42.72(2) . . . . ? Cl2 Mg1 Cl1 Mg2 42.95(2) . . . . ? O4 Mg2 Cl2 Mg1 -137.64(4) . . . . ? O6 Mg2 Cl2 Mg1 131.12(4) . . . . ? Cl1 Mg2 Cl2 Mg1 43.24(2) . . . . ? Cl3 Mg2 Cl2 Mg1 -41.90(2) . . . . ? O3 Mg1 Cl2 Mg2 -139.41(4) . . . . ? O1 Mg1 Cl2 Mg2 130.40(4) . . . . ? Cl3 Mg1 Cl2 Mg2 42.22(2) . . . . ? Cl1 Mg1 Cl2 Mg2 -43.22(2) . . . . ? O1 Mg1 Cl3 Mg2 -137.14(4) . . . . ? O2 Mg1 Cl3 Mg2 131.97(4) . . . . ? Cl2 Mg1 Cl3 Mg2 -41.89(2) . . . . ? Cl1 Mg1 Cl3 Mg2 42.64(2) . . . . ? O5 Mg2 Cl3 Mg1 -139.42(4) . . . . ? O4 Mg2 Cl3 Mg1 132.72(4) . . . . ? Cl2 Mg2 Cl3 Mg1 42.23(2) . . . . ? Cl1 Mg2 Cl3 Mg1 -42.72(2) . . . . ? O3 Mg1 O1 C1 -96.50(14) . . . . ? O2 Mg1 O1 C1 173.65(13) . . . . ? Cl3 Mg1 O1 C1 77.73(13) . . . . ? Cl2 Mg1 O1 C1 -7.32(13) . . . . ? Mg2 Mg1 O1 C1 38.00(15) . . . . ? O3 Mg1 O1 C4 114.15(13) . . . . ? O2 Mg1 O1 C4 24.30(13) . . . . ? Cl3 Mg1 O1 C4 -71.61(13) . . . . ? Cl2 Mg1 O1 C4 -156.67(12) . . . . ? Mg2 Mg1 O1 C4 -111.35(13) . . . . ? O3 Mg1 O2 C5 166.24(15) . . . . ? O1 Mg1 O2 C5 -103.50(15) . . . . ? Cl3 Mg1 O2 C5 -14.78(15) . . . . ? Cl1 Mg1 O2 C5 70.17(14) . . . . ? Mg2 Mg1 O2 C5 30.84(16) . . . . ? O3 Mg1 O2 C8 0.77(14) . . . . ? O1 Mg1 O2 C8 91.03(14) . . . . ? Cl3 Mg1 O2 C8 179.75(13) . . . . ? Cl1 Mg1 O2 C8 -95.30(13) . . . . ? Mg2 Mg1 O2 C8 -134.63(12) . . . . ? O1 Mg1 O3 C9 -6.36(14) . . . . ? O2 Mg1 O3 C9 84.66(14) . . . . ? Cl2 Mg1 O3 C9 -101.47(13) . . . . ? Cl1 Mg1 O3 C9 174.51(13) . . . . ? Mg2 Mg1 O3 C9 -139.72(13) . . . . ? O1 Mg1 O3 C12 158.94(13) . . . . ? O2 Mg1 O3 C12 -110.04(13) . . . . ? Cl2 Mg1 O3 C12 63.82(13) . . . . ? Cl1 Mg1 O3 C12 -20.20(13) . . . . ? Mg2 Mg1 O3 C12 25.57(15) . . . . ? O5 Mg2 O4 C16 -64.74(12) . . . . ? O6 Mg2 O4 C16 -153.49(12) . . . . ? Cl2 Mg2 O4 C16 110.54(11) . . . . ? Cl3 Mg2 O4 C16 25.24(12) . . . . ? Mg1 Mg2 O4 C16 70.00(13) . . . . ? O5 Mg2 O4 C13 154.59(13) . . . . ? O6 Mg2 O4 C13 65.84(13) . . . . ? Cl2 Mg2 O4 C13 -30.13(13) . . . . ? Cl3 Mg2 O4 C13 -115.42(12) . . . . ? Mg1 Mg2 O4 C13 -70.66(14) . . . . ? O4 Mg2 O5 C20 -28.09(14) . . . . ? O6 Mg2 O5 C20 63.09(14) . . . . ? Cl1 Mg2 O5 C20 151.40(13) . . . . ? Cl3 Mg2 O5 C20 -123.88(14) . . . . ? Mg1 Mg2 O5 C20 -162.62(12) . . . . ? O4 Mg2 O5 C17 152.04(16) . . . . ? O6 Mg2 O5 C17 -116.79(16) . . . . ? Cl1 Mg2 O5 C17 -28.48(16) . . . . ? Cl3 Mg2 O5 C17 56.24(16) . . . . ? Mg1 Mg2 O5 C17 17.50(18) . . . . ? O5 Mg2 O6 C24 -179.13(13) . . . . ? O4 Mg2 O6 C24 -91.31(13) . . . . ? Cl2 Mg2 O6 C24 -0.21(13) . . . . ? Cl1 Mg2 O6 C24 84.14(13) . . . . ? Mg1 Mg2 O6 C24 45.76(14) . . . . ? O5 Mg2 O6 C21 37.59(13) . . . . ? O4 Mg2 O6 C21 125.42(12) . . . . ? Cl2 Mg2 O6 C21 -143.49(12) . . . . ? Cl1 Mg2 O6 C21 -59.13(12) . . . . ? Mg1 Mg2 O6 C21 -97.51(12) . . . . ? C4 O1 C1 C2 -22.9(2) . . . . ? Mg1 O1 C1 C2 -175.89(12) . . . . ? O1 C1 C2 C3 36.57(19) . . . . ? C1 C2 C3 C4 -36.3(2) . . . . ? C1 O1 C4 C3 -0.3(2) . . . . ? Mg1 O1 C4 C3 152.65(13) . . . . ? C2 C3 C4 O1 23.1(2) . . . . ? C8 O2 C5 C6 -21.5(2) . . . . ? Mg1 O2 C5 C6 170.96(13) . . . . ? O2 C5 C6 C7 35.8(2) . . . . ? C5 C6 C7 C8 -36.4(2) . . . . ? C5 O2 C8 C7 -1.4(2) . . . . ? Mg1 O2 C8 C7 165.98(13) . . . . ? C6 C7 C8 O2 23.7(2) . . . . ? C12 O3 C9 C10 25.81(19) . . . . ? Mg1 O3 C9 C10 -167.11(12) . . . . ? O3 C9 C10 C11 -39.71(19) . . . . ? C9 C10 C11 C12 38.55(18) . . . . ? C9 O3 C12 C11 -1.01(19) . . . . ? Mg1 O3 C12 C11 -168.65(11) . . . . ? C10 C11 C12 O3 -23.77(19) . . . . ? C16 O4 C13 C14 -31.68(19) . . . . ? Mg2 O4 C13 C14 114.00(15) . . . . ? O4 C13 C14 C15 7.8(2) . . . . ? C13 C14 C15 C16 17.8(2) . . . . ? C13 O4 C16 C15 43.40(17) . . . . ? Mg2 O4 C16 C15 -103.97(14) . . . . ? C14 C15 C16 O4 -37.32(18) . . . . ? C20 O5 C17 C18 0.1(2) . . . . ? Mg2 O5 C17 C18 -179.97(13) . . . . ? O5 C17 C18 C19 -22.7(2) . . . . ? C17 C18 C19 C20 35.9(2) . . . . ? C17 O5 C20 C19 22.8(2) . . . . ? Mg2 O5 C20 C19 -157.10(13) . . . . ? C18 C19 C20 O5 -36.1(2) . . . . ? C24 O6 C21 C22 -4.5(2) . . . . ? Mg2 O6 C21 C22 143.25(14) . . . . ? O6 C21 C22 C23 27.1(2) . . . . ? C21 C22 C23 C24 -38.7(2) . . . . ? C21 O6 C24 C23 -20.5(2) . . . . ? Mg2 O6 C24 C23 -167.55(12) . . . . ? C22 C23 C24 O6 36.7(2) . . . . ? C31 Al1 C25 C26 -81.63(16) . . . . ? Cl5 Al1 C25 C26 39.60(16) . . . . ? Cl4 Al1 C25 C26 156.79(13) . . . . ? C31 Al1 C25 C30 96.35(16) . . . . ? Cl5 Al1 C25 C30 -142.41(14) . . . . ? Cl4 Al1 C25 C30 -25.22(17) . . . . ? C30 C25 C26 C27 0.0(3) . . . . ? Al1 C25 C26 C27 178.15(14) . . . . ? C25 C26 C27 C28 0.6(3) . . . . ? C26 C27 C28 C29 -0.8(3) . . . . ? C27 C28 C29 C30 0.5(3) . . . . ? C28 C29 C30 C25 0.1(3) . . . . ? C26 C25 C30 C29 -0.3(3) . . . . ? Al1 C25 C30 C29 -178.43(15) . . . . ? C25 Al1 C31 C37 -22.27(18) . . . . ? Cl5 Al1 C31 C37 -144.07(14) . . . . ? Cl4 Al1 C31 C37 99.50(15) . . . . ? C25 Al1 C31 C32 158.33(15) . . . . ? Cl5 Al1 C31 C32 36.53(17) . . . . ? Cl4 Al1 C31 C32 -79.90(16) . . . . ? C37 C31 C32 C33 -0.3(3) . . . . ? Al1 C31 C32 C33 179.09(15) . . . . ? C31 C32 C33 C35 0.0(3) . . . . ? C32 C33 C35 C36 0.4(3) . . . . ? C33 C35 C36 C37 -0.5(3) . . . . ? C35 C36 C37 C31 0.1(3) . . . . ? C32 C31 C37 C36 0.3(3) . . . . ? Al1 C31 C37 C36 -179.19(15) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.730 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.052 #==============END data_cmpd3 _database_code_depnum_ccdc_archive 'CCDC 852857' #TrackingRef '- jm-EES-composite.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Cl3 Mg2 O6, C24 H20 B' _chemical_formula_sum 'C48 H68 B Cl3 Mg2 O6' _chemical_formula_weight 906.80 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 16.4151(16) _cell_length_b 16.5787(16) _cell_length_c 18.5617(19) _cell_angle_alpha 90.00 _cell_angle_beta 109.3640(10) _cell_angle_gamma 90.00 _cell_volume 4765.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9895 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.20 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9396 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS, Sheldrick, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker APEX-II' _diffrn_measurement_method 'combination of \w and \f-scans ' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 76313 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.35 _reflns_number_total 11872 _reflns_number_gt 9917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-II v2011-4.1' _computing_cell_refinement 'Bruker SAINT v7.66A' _computing_data_reduction 'Bruker SAINT v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0433P)^2^+2.1779P] 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 11872 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.21996(3) 0.66751(3) 0.32592(3) 0.01823(10) Uani 1 1 d . . . Mg2 Mg 0.34630(3) 0.80839(3) 0.32451(3) 0.01750(10) Uani 1 1 d . . . Cl1 Cl 0.33264(2) 0.672045(19) 0.263824(18) 0.01933(7) Uani 1 1 d . . . Cl2 Cl 0.32916(2) 0.735291(19) 0.438336(18) 0.02009(7) Uani 1 1 d . . . Cl3 Cl 0.18627(2) 0.80968(2) 0.275034(19) 0.02195(7) Uani 1 1 d . . . O1 O 0.13106(6) 0.66444(6) 0.38459(6) 0.0246(2) Uani 1 1 d . . . O2 O 0.12439(6) 0.62304(6) 0.23001(6) 0.0229(2) Uani 1 1 d . . . O3 O 0.26444(6) 0.55469(6) 0.37253(6) 0.0220(2) Uani 1 1 d . . . O4 O 0.36454(6) 0.86283(6) 0.23040(6) 0.0224(2) Uani 1 1 d . . . O5 O 0.35062(6) 0.92119(6) 0.37713(5) 0.02038(19) Uani 1 1 d . . . O6 O 0.47939(6) 0.79999(6) 0.37280(6) 0.0209(2) Uani 1 1 d . . . C1 C 0.06309(10) 0.72395(11) 0.37536(10) 0.0345(4) Uani 1 1 d . . . H1A H 0.0064 0.6975 0.3660 0.041 Uiso 1 1 calc R . . H1B H 0.0591 0.7611 0.3325 0.041 Uiso 1 1 calc R . . C2 C 0.09104(13) 0.76825(12) 0.45049(12) 0.0472(5) Uani 1 1 d . . . H2A H 0.0407 0.7913 0.4613 0.057 Uiso 1 1 calc R . . H2B H 0.1318 0.8123 0.4505 0.057 Uiso 1 1 calc R . . C3 C 0.13472(15) 0.70409(14) 0.50837(11) 0.0518(5) Uani 1 1 d . . . H3A H 0.1894 0.7247 0.5451 0.062 Uiso 1 1 calc R . . H3B H 0.0966 0.6865 0.5370 0.062 Uiso 1 1 calc R . . C4 C 0.15203(12) 0.63522(10) 0.46210(9) 0.0337(4) Uani 1 1 d . . . H4A H 0.2134 0.6189 0.4825 0.040 Uiso 1 1 calc R . . H4B H 0.1157 0.5881 0.4638 0.040 Uiso 1 1 calc R . . C5 C 0.03848(10) 0.59599(11) 0.22574(10) 0.0363(4) Uani 1 1 d . . . H5A H 0.0001 0.6424 0.2245 0.044 Uiso 1 1 calc R . . H5B H 0.0411 0.5611 0.2697 0.044 Uiso 1 1 calc R . . C6 C 0.00789(11) 0.54949(12) 0.15238(10) 0.0404(4) Uani 1 1 d . . . H6A H -0.0559 0.5465 0.1324 0.048 Uiso 1 1 calc R . . H6B H 0.0318 0.4941 0.1593 0.048 Uiso 1 1 calc R . . C7 C 0.04266(10) 0.59845(10) 0.09895(9) 0.0298(3) Uani 1 1 d . . . H7A H -0.0028 0.6338 0.0653 0.036 Uiso 1 1 calc R . . H7B H 0.0644 0.5624 0.0668 0.036 Uiso 1 1 calc R . . C8 C 0.11619(10) 0.64858(10) 0.15272(8) 0.0276(3) Uani 1 1 d . . . H8A H 0.1707 0.6387 0.1423 0.033 Uiso 1 1 calc R . . H8B H 0.1025 0.7068 0.1460 0.033 Uiso 1 1 calc R . . C9 C 0.21434(9) 0.48079(8) 0.36261(8) 0.0236(3) Uani 1 1 d . . . H9A H 0.2064 0.4563 0.3121 0.028 Uiso 1 1 calc R . . H9B H 0.1569 0.4913 0.3672 0.028 Uiso 1 1 calc R . . C10 C 0.26749(10) 0.42641(9) 0.42626(9) 0.0278(3) Uani 1 1 d . . . H10A H 0.2545 0.3688 0.4133 0.033 Uiso 1 1 calc R . . H10B H 0.2573 0.4385 0.4748 0.033 Uiso 1 1 calc R . . C11 C 0.35998(10) 0.44744(9) 0.43117(10) 0.0297(3) Uani 1 1 d . . . H11A H 0.4005 0.4393 0.4836 0.036 Uiso 1 1 calc R . . H11B H 0.3789 0.4140 0.3954 0.036 Uiso 1 1 calc R . . C12 C 0.35534(10) 0.53518(9) 0.40904(10) 0.0320(3) Uani 1 1 d . . . H12A H 0.3807 0.5692 0.4549 0.038 Uiso 1 1 calc R . . H12B H 0.3877 0.5447 0.3733 0.038 Uiso 1 1 calc R . . C13 C 0.40899(11) 0.82375(9) 0.18403(9) 0.0276(3) Uani 1 1 d . . . H13A H 0.3698 0.7868 0.1463 0.033 Uiso 1 1 calc R . . H13B H 0.4596 0.7929 0.2162 0.033 Uiso 1 1 calc R . . C14 C 0.43660(11) 0.89331(10) 0.14468(9) 0.0312(3) Uani 1 1 d . . . H14A H 0.4467 0.8754 0.0975 0.037 Uiso 1 1 calc R . . H14B H 0.4895 0.9194 0.1789 0.037 Uiso 1 1 calc R . . C15 C 0.35867(11) 0.94995(10) 0.12665(9) 0.0308(3) Uani 1 1 d . . . H15A H 0.3769 1.0070 0.1279 0.037 Uiso 1 1 calc R . . H15B H 0.3164 0.9380 0.0757 0.037 Uiso 1 1 calc R . . C16 C 0.32022(12) 0.93299(10) 0.18961(10) 0.0364(4) Uani 1 1 d . . . H16A H 0.3290 0.9798 0.2245 0.044 Uiso 1 1 calc R . . H16B H 0.2575 0.9223 0.1673 0.044 Uiso 1 1 calc R . . C17 C 0.28207(9) 0.98124(8) 0.35798(8) 0.0234(3) Uani 1 1 d . . . H17A H 0.2366 0.9676 0.3092 0.028 Uiso 1 1 calc R . . H17B H 0.3052 1.0355 0.3535 0.028 Uiso 1 1 calc R . . C18 C 0.24660(10) 0.97840(9) 0.42408(9) 0.0270(3) Uani 1 1 d . . . H18A H 0.1955 0.9426 0.4119 0.032 Uiso 1 1 calc R . . H18B H 0.2300 1.0330 0.4359 0.032 Uiso 1 1 calc R . . C19 C 0.32170(10) 0.94468(9) 0.49161(9) 0.0279(3) Uani 1 1 d . . . H19A H 0.3390 0.9834 0.5347 0.033 Uiso 1 1 calc R . . H19B H 0.3056 0.8928 0.5097 0.033 Uiso 1 1 calc R . . C20 C 0.39396(9) 0.93290(9) 0.45820(8) 0.0255(3) Uani 1 1 d . . . H20A H 0.4318 0.9810 0.4676 0.031 Uiso 1 1 calc R . . H20B H 0.4294 0.8852 0.4810 0.031 Uiso 1 1 calc R . . C21 C 0.52684(9) 0.72653(9) 0.40516(9) 0.0251(3) Uani 1 1 d . . . H21A H 0.5150 0.6835 0.3661 0.030 Uiso 1 1 calc R . . H21B H 0.5099 0.7070 0.4486 0.030 Uiso 1 1 calc R . . C22 C 0.62207(9) 0.74956(9) 0.43194(9) 0.0265(3) Uani 1 1 d . . . H22A H 0.6539 0.7229 0.4809 0.032 Uiso 1 1 calc R . . H22B H 0.6491 0.7347 0.3934 0.032 Uiso 1 1 calc R . . C23 C 0.62065(9) 0.84074(9) 0.44160(8) 0.0247(3) Uani 1 1 d . . . H23A H 0.6146 0.8556 0.4912 0.030 Uiso 1 1 calc R . . H23B H 0.6733 0.8662 0.4372 0.030 Uiso 1 1 calc R . . C24 C 0.54129(9) 0.86382(9) 0.37553(9) 0.0254(3) Uani 1 1 d . . . H24A H 0.5188 0.9169 0.3846 0.030 Uiso 1 1 calc R . . H24B H 0.5544 0.8662 0.3272 0.030 Uiso 1 1 calc R . . B1 B 0.77143(9) 0.72624(9) 0.26252(8) 0.0155(3) Uani 1 1 d . . . C25 C 0.76945(8) 0.81080(8) 0.30874(7) 0.0168(2) Uani 1 1 d . . . C26 C 0.83663(9) 0.83528(8) 0.37447(8) 0.0217(3) Uani 1 1 d . . . H26A H 0.8823 0.7985 0.3974 0.026 Uiso 1 1 calc R . . C27 C 0.83912(10) 0.91124(9) 0.40743(8) 0.0261(3) Uani 1 1 d . . . H27A H 0.8856 0.9250 0.4521 0.031 Uiso 1 1 calc R . . C28 C 0.77393(10) 0.96668(9) 0.37523(9) 0.0263(3) Uani 1 1 d . . . H28A H 0.7757 1.0187 0.3971 0.032 Uiso 1 1 calc R . . C29 C 0.70607(10) 0.94498(9) 0.31064(9) 0.0246(3) Uani 1 1 d . . . H29A H 0.6610 0.9824 0.2878 0.029 Uiso 1 1 calc R . . C30 C 0.70388(9) 0.86832(8) 0.27911(8) 0.0198(3) Uani 1 1 d . . . H30A H 0.6560 0.8543 0.2357 0.024 Uiso 1 1 calc R . . C31 C 0.67135(8) 0.69515(8) 0.22044(7) 0.0169(2) Uani 1 1 d . . . C32 C 0.63206(9) 0.64039(8) 0.25637(8) 0.0208(3) Uani 1 1 d . . . H32A H 0.6652 0.6194 0.3049 0.025 Uiso 1 1 calc R . . C33 C 0.54647(9) 0.61542(9) 0.22397(9) 0.0269(3) Uani 1 1 d . . . H33A H 0.5226 0.5784 0.2506 0.032 Uiso 1 1 calc R . . C34 C 0.49609(9) 0.64445(10) 0.15313(9) 0.0283(3) Uani 1 1 d . . . H34A H 0.4379 0.6274 0.1307 0.034 Uiso 1 1 calc R . . C35 C 0.53230(9) 0.69895(9) 0.11567(8) 0.0249(3) Uani 1 1 d . . . H35A H 0.4986 0.7195 0.0672 0.030 Uiso 1 1 calc R . . C36 C 0.61774(9) 0.72367(8) 0.14886(8) 0.0201(3) Uani 1 1 d . . . H36A H 0.6408 0.7613 0.1222 0.024 Uiso 1 1 calc R . . C37 C 0.82517(8) 0.65266(8) 0.31805(7) 0.0165(2) Uani 1 1 d . . . C38 C 0.83311(9) 0.64288(8) 0.39543(8) 0.0203(3) Uani 1 1 d . . . H38A H 0.8085 0.6825 0.4189 0.024 Uiso 1 1 calc R . . C39 C 0.87564(9) 0.57726(9) 0.43909(8) 0.0237(3) Uani 1 1 d . . . H39A H 0.8805 0.5737 0.4914 0.028 Uiso 1 1 calc R . . C40 C 0.91094(9) 0.51720(9) 0.40621(8) 0.0239(3) Uani 1 1 d . . . H40A H 0.9400 0.4725 0.4356 0.029 Uiso 1 1 calc R . . C41 C 0.90303(9) 0.52378(8) 0.32970(8) 0.0218(3) Uani 1 1 d . . . H41A H 0.9259 0.4828 0.3061 0.026 Uiso 1 1 calc R . . C42 C 0.86163(8) 0.59033(8) 0.28735(7) 0.0181(3) Uani 1 1 d . . . H42A H 0.8579 0.5937 0.2353 0.022 Uiso 1 1 calc R . . C43 C 0.82087(8) 0.74700(8) 0.20018(7) 0.0166(2) Uani 1 1 d . . . C44 C 0.80071(9) 0.70802(8) 0.12896(8) 0.0197(3) Uani 1 1 d . . . H44A H 0.7550 0.6698 0.1151 0.024 Uiso 1 1 calc R . . C45 C 0.84494(9) 0.72309(9) 0.07784(8) 0.0233(3) Uani 1 1 d . . . H45A H 0.8286 0.6959 0.0301 0.028 Uiso 1 1 calc R . . C46 C 0.91279(9) 0.77781(9) 0.09675(8) 0.0248(3) Uani 1 1 d . . . H46A H 0.9431 0.7885 0.0622 0.030 Uiso 1 1 calc R . . C47 C 0.93569(9) 0.81674(9) 0.16686(8) 0.0237(3) Uani 1 1 d . . . H47A H 0.9825 0.8538 0.1808 0.028 Uiso 1 1 calc R . . C48 C 0.89011(8) 0.80158(8) 0.21685(8) 0.0198(3) Uani 1 1 d . . . H48A H 0.9066 0.8294 0.2643 0.024 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 0.0151(2) 0.0181(2) 0.0211(2) 0.00097(17) 0.00548(17) -0.00198(17) Mg2 0.0150(2) 0.0159(2) 0.0213(2) 0.00057(17) 0.00572(17) -0.00060(16) Cl1 0.01831(15) 0.01784(15) 0.02319(15) -0.00130(11) 0.00870(12) -0.00154(11) Cl2 0.01962(15) 0.01993(15) 0.02028(15) -0.00119(12) 0.00601(12) -0.00310(12) Cl3 0.01573(15) 0.01863(15) 0.02902(17) 0.00087(12) 0.00412(12) 0.00018(11) O1 0.0202(5) 0.0292(5) 0.0261(5) 0.0039(4) 0.0099(4) 0.0019(4) O2 0.0176(5) 0.0255(5) 0.0237(5) 0.0000(4) 0.0043(4) -0.0046(4) O3 0.0177(5) 0.0172(5) 0.0297(5) 0.0021(4) 0.0058(4) -0.0027(4) O4 0.0246(5) 0.0200(5) 0.0252(5) 0.0038(4) 0.0116(4) 0.0042(4) O5 0.0183(5) 0.0173(5) 0.0232(5) -0.0009(4) 0.0037(4) 0.0022(4) O6 0.0142(4) 0.0177(5) 0.0297(5) 0.0034(4) 0.0059(4) -0.0002(4) C1 0.0198(7) 0.0439(10) 0.0413(9) 0.0072(7) 0.0123(7) 0.0074(7) C2 0.0359(10) 0.0395(10) 0.0643(13) -0.0114(9) 0.0139(9) 0.0070(8) C3 0.0649(14) 0.0566(13) 0.0362(10) -0.0083(9) 0.0199(10) 0.0115(11) C4 0.0425(9) 0.0360(9) 0.0292(8) 0.0077(7) 0.0205(7) 0.0066(7) C5 0.0245(8) 0.0436(10) 0.0398(9) -0.0030(7) 0.0092(7) -0.0098(7) C6 0.0288(9) 0.0445(10) 0.0449(10) -0.0127(8) 0.0083(7) -0.0151(7) C7 0.0222(7) 0.0344(8) 0.0277(7) -0.0088(6) 0.0013(6) 0.0039(6) C8 0.0274(8) 0.0338(8) 0.0204(7) -0.0031(6) 0.0065(6) -0.0041(6) C9 0.0235(7) 0.0173(6) 0.0303(7) -0.0036(5) 0.0092(6) -0.0061(5) C10 0.0311(8) 0.0180(7) 0.0345(8) 0.0003(6) 0.0110(6) -0.0045(6) C11 0.0280(8) 0.0207(7) 0.0386(8) 0.0015(6) 0.0088(7) 0.0025(6) C12 0.0190(7) 0.0256(8) 0.0471(9) 0.0112(7) 0.0053(7) 0.0003(6) C13 0.0338(8) 0.0249(7) 0.0289(7) 0.0019(6) 0.0169(6) 0.0044(6) C14 0.0357(9) 0.0326(8) 0.0306(8) 0.0052(6) 0.0183(7) 0.0008(7) C15 0.0390(9) 0.0288(8) 0.0242(7) 0.0053(6) 0.0100(6) 0.0026(7) C16 0.0417(10) 0.0300(8) 0.0441(10) 0.0176(7) 0.0230(8) 0.0142(7) C17 0.0239(7) 0.0155(6) 0.0286(7) 0.0022(5) 0.0060(6) 0.0054(5) C18 0.0237(7) 0.0235(7) 0.0339(8) 0.0011(6) 0.0099(6) 0.0048(6) C19 0.0335(8) 0.0235(7) 0.0260(7) -0.0019(6) 0.0089(6) 0.0053(6) C20 0.0222(7) 0.0232(7) 0.0250(7) -0.0048(5) -0.0002(6) 0.0014(5) C21 0.0200(7) 0.0196(7) 0.0338(8) 0.0023(6) 0.0065(6) 0.0030(5) C22 0.0182(7) 0.0277(8) 0.0308(7) 0.0015(6) 0.0041(6) 0.0039(6) C23 0.0196(7) 0.0263(7) 0.0272(7) 0.0020(6) 0.0064(6) -0.0041(5) C24 0.0172(6) 0.0239(7) 0.0353(8) 0.0066(6) 0.0090(6) -0.0035(5) B1 0.0158(6) 0.0156(6) 0.0156(6) 0.0006(5) 0.0057(5) 0.0003(5) C25 0.0186(6) 0.0168(6) 0.0171(6) 0.0006(5) 0.0087(5) -0.0018(5) C26 0.0222(7) 0.0207(7) 0.0214(6) -0.0003(5) 0.0063(5) -0.0020(5) C27 0.0303(8) 0.0246(7) 0.0237(7) -0.0048(6) 0.0095(6) -0.0089(6) C28 0.0339(8) 0.0180(7) 0.0331(8) -0.0064(6) 0.0191(7) -0.0059(6) C29 0.0263(7) 0.0188(7) 0.0328(7) 0.0014(6) 0.0156(6) 0.0024(5) C30 0.0202(6) 0.0201(6) 0.0203(6) 0.0001(5) 0.0083(5) 0.0003(5) C31 0.0180(6) 0.0150(6) 0.0178(6) -0.0027(5) 0.0063(5) 0.0013(5) C32 0.0205(7) 0.0207(6) 0.0214(6) -0.0013(5) 0.0070(5) -0.0014(5) C33 0.0235(7) 0.0279(8) 0.0309(8) -0.0025(6) 0.0113(6) -0.0072(6) C34 0.0183(7) 0.0335(8) 0.0299(7) -0.0090(6) 0.0037(6) -0.0038(6) C35 0.0219(7) 0.0281(7) 0.0211(7) -0.0035(5) 0.0023(5) 0.0046(6) C36 0.0201(6) 0.0197(6) 0.0201(6) -0.0011(5) 0.0059(5) 0.0021(5) C37 0.0134(6) 0.0168(6) 0.0185(6) 0.0006(5) 0.0042(5) -0.0022(5) C38 0.0206(6) 0.0211(6) 0.0198(6) 0.0008(5) 0.0074(5) 0.0012(5) C39 0.0256(7) 0.0253(7) 0.0188(6) 0.0050(5) 0.0056(5) -0.0007(6) C40 0.0222(7) 0.0196(7) 0.0266(7) 0.0065(5) 0.0037(6) 0.0018(5) C41 0.0209(7) 0.0165(6) 0.0280(7) -0.0001(5) 0.0078(6) 0.0008(5) C42 0.0178(6) 0.0180(6) 0.0184(6) 0.0005(5) 0.0060(5) -0.0015(5) C43 0.0167(6) 0.0148(6) 0.0180(6) 0.0036(5) 0.0053(5) 0.0040(5) C44 0.0215(6) 0.0175(6) 0.0209(6) 0.0015(5) 0.0079(5) 0.0014(5) C45 0.0265(7) 0.0249(7) 0.0197(6) 0.0019(5) 0.0094(6) 0.0062(6) C46 0.0247(7) 0.0269(7) 0.0277(7) 0.0091(6) 0.0152(6) 0.0064(6) C47 0.0188(7) 0.0224(7) 0.0306(7) 0.0071(6) 0.0093(6) 0.0007(5) C48 0.0182(6) 0.0192(6) 0.0207(6) 0.0029(5) 0.0045(5) 0.0026(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 2.0789(11) . ? Mg1 O3 2.0883(11) . ? Mg1 O1 2.0908(11) . ? Mg1 Cl1 2.4838(6) . ? Mg1 Cl2 2.5199(6) . ? Mg1 Cl3 2.5312(6) . ? Mg1 Mg2 3.1294(7) . ? Mg2 O6 2.0729(10) . ? Mg2 O4 2.0743(11) . ? Mg2 O5 2.0999(10) . ? Mg2 Cl3 2.4788(6) . ? Mg2 Cl1 2.5023(6) . ? Mg2 Cl2 2.5309(6) . ? O1 C4 1.4474(18) . ? O1 C1 1.4564(18) . ? O2 C5 1.4566(18) . ? O2 C8 1.4587(17) . ? O3 C9 1.4529(16) . ? O3 C12 1.4560(17) . ? O4 C16 1.4458(18) . ? O4 C13 1.4524(17) . ? O5 C20 1.4487(17) . ? O5 C17 1.4555(16) . ? O6 C24 1.4563(16) . ? O6 C21 1.4630(16) . ? C1 C2 1.507(3) . ? C2 C3 1.513(3) . ? C3 C4 1.511(3) . ? C5 C6 1.499(2) . ? C6 C7 1.531(3) . ? C7 C8 1.531(2) . ? C9 C10 1.512(2) . ? C10 C11 1.531(2) . ? C11 C12 1.507(2) . ? C13 C14 1.513(2) . ? C14 C15 1.532(2) . ? C15 C16 1.527(2) . ? C17 C18 1.523(2) . ? C18 C19 1.542(2) . ? C19 C20 1.522(2) . ? C21 C22 1.523(2) . ? C22 C23 1.523(2) . ? C23 C24 1.513(2) . ? B1 C25 1.6495(19) . ? B1 C31 1.6503(19) . ? B1 C37 1.6511(19) . ? B1 C43 1.6551(19) . ? C25 C26 1.4061(18) . ? C25 C30 1.4063(18) . ? C26 C27 1.395(2) . ? C27 C28 1.387(2) . ? C28 C29 1.386(2) . ? C29 C30 1.3947(19) . ? C31 C32 1.4036(19) . ? C31 C36 1.4100(18) . ? C32 C33 1.3953(19) . ? C33 C34 1.387(2) . ? C34 C35 1.388(2) . ? C35 C36 1.393(2) . ? C37 C42 1.4060(18) . ? C37 C38 1.4078(18) . ? C38 C39 1.3974(19) . ? C39 C40 1.391(2) . ? C40 C41 1.387(2) . ? C41 C42 1.3938(19) . ? C43 C48 1.4046(18) . ? C43 C44 1.4087(18) . ? C44 C45 1.3952(19) . ? C45 C46 1.388(2) . ? C46 C47 1.388(2) . ? C47 C48 1.3944(19) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? 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 O3 95.63(4) . . ? O2 Mg1 O1 88.77(4) . . ? O3 Mg1 O1 88.34(4) . . ? O2 Mg1 Cl1 94.59(3) . . ? O3 Mg1 Cl1 90.43(3) . . ? O1 Mg1 Cl1 176.52(4) . . ? O2 Mg1 Cl2 174.21(4) . . ? O3 Mg1 Cl2 90.08(3) . . ? O1 Mg1 Cl2 90.42(3) . . ? Cl1 Mg1 Cl2 86.330(19) . . ? O2 Mg1 Cl3 90.07(3) . . ? O3 Mg1 Cl3 172.62(3) . . ? O1 Mg1 Cl3 96.50(3) . . ? Cl1 Mg1 Cl3 84.422(17) . . ? Cl2 Mg1 Cl3 84.326(18) . . ? O2 Mg1 Mg2 124.86(3) . . ? O3 Mg1 Mg2 122.02(3) . . ? O1 Mg1 Mg2 126.97(4) . . ? Cl1 Mg1 Mg2 51.388(14) . . ? Cl2 Mg1 Mg2 51.873(14) . . ? Cl3 Mg1 Mg2 50.600(14) . . ? O6 Mg2 O4 88.15(4) . . ? O6 Mg2 O5 89.46(4) . . ? O4 Mg2 O5 90.70(4) . . ? O6 Mg2 Cl3 175.03(4) . . ? O4 Mg2 Cl3 96.62(3) . . ? O5 Mg2 Cl3 91.88(3) . . ? O6 Mg2 Cl1 93.34(3) . . ? O4 Mg2 Cl1 91.74(3) . . ? O5 Mg2 Cl1 176.35(3) . . ? Cl3 Mg2 Cl1 85.136(17) . . ? O6 Mg2 Cl2 89.99(3) . . ? O4 Mg2 Cl2 176.74(4) . . ? O5 Mg2 Cl2 91.96(3) . . ? Cl3 Mg2 Cl2 85.179(18) . . ? Cl1 Mg2 Cl2 85.703(18) . . ? O6 Mg2 Mg1 123.55(3) . . ? O4 Mg2 Mg1 127.80(3) . . ? O5 Mg2 Mg1 125.52(3) . . ? Cl3 Mg2 Mg1 52.098(14) . . ? Cl1 Mg2 Mg1 50.862(14) . . ? Cl2 Mg2 Mg1 51.556(14) . . ? Mg1 Cl1 Mg2 77.750(17) . . ? Mg1 Cl2 Mg2 76.571(18) . . ? Mg2 Cl3 Mg1 77.301(17) . . ? C4 O1 C1 105.30(11) . . ? C4 O1 Mg1 123.29(9) . . ? C1 O1 Mg1 124.20(9) . . ? C5 O2 C8 105.30(11) . . ? C5 O2 Mg1 126.72(9) . . ? C8 O2 Mg1 122.46(8) . . ? C9 O3 C12 108.74(10) . . ? C9 O3 Mg1 126.68(8) . . ? C12 O3 Mg1 123.74(8) . . ? C16 O4 C13 108.24(11) . . ? C16 O4 Mg2 127.09(9) . . ? C13 O4 Mg2 123.10(8) . . ? C20 O5 C17 103.62(10) . . ? C20 O5 Mg2 122.13(8) . . ? C17 O5 Mg2 126.26(8) . . ? C24 O6 C21 108.67(10) . . ? C24 O6 Mg2 126.11(8) . . ? C21 O6 Mg2 125.09(8) . . ? O1 C1 C2 103.59(13) . . ? C1 C2 C3 103.99(15) . . ? C4 C3 C2 105.17(15) . . ? O1 C4 C3 106.53(14) . . ? O2 C5 C6 103.57(13) . . ? C5 C6 C7 103.36(13) . . ? C6 C7 C8 104.37(12) . . ? O2 C8 C7 106.21(12) . . ? O3 C9 C10 104.36(11) . . ? C9 C10 C11 102.40(12) . . ? C12 C11 C10 104.14(12) . . ? O3 C12 C11 107.02(12) . . ? O4 C13 C14 103.64(12) . . ? C13 C14 C15 102.16(12) . . ? C16 C15 C14 104.30(12) . . ? O4 C16 C15 106.56(12) . . ? O5 C17 C18 104.67(11) . . ? C17 C18 C19 104.46(12) . . ? C20 C19 C18 103.67(12) . . ? O5 C20 C19 105.06(11) . . ? O6 C21 C22 105.92(11) . . ? C23 C22 C21 103.48(11) . . ? C24 C23 C22 101.43(12) . . ? O6 C24 C23 104.35(11) . . ? C25 B1 C31 108.87(10) . . ? C25 B1 C37 113.70(10) . . ? C31 B1 C37 107.85(10) . . ? C25 B1 C43 106.60(10) . . ? C31 B1 C43 112.09(10) . . ? C37 B1 C43 107.80(10) . . ? C26 C25 C30 114.97(12) . . ? C26 C25 B1 123.47(12) . . ? C30 C25 B1 121.15(11) . . ? C27 C26 C25 122.79(13) . . ? C28 C27 C26 120.22(14) . . ? C29 C28 C27 118.99(13) . . ? C28 C29 C30 120.05(14) . . ? C29 C30 C25 122.95(13) . . ? C32 C31 C36 115.03(12) . . ? C32 C31 B1 121.29(11) . . ? C36 C31 B1 123.61(11) . . ? C33 C32 C31 122.88(13) . . ? C34 C33 C32 120.29(14) . . ? C33 C34 C35 118.75(13) . . ? C34 C35 C36 120.35(13) . . ? C35 C36 C31 122.70(13) . . ? C42 C37 C38 114.89(12) . . ? C42 C37 B1 120.08(11) . . ? C38 C37 B1 124.86(12) . . ? C39 C38 C37 122.74(13) . . ? C40 C39 C38 120.23(13) . . ? C41 C40 C39 118.81(13) . . ? C40 C41 C42 120.16(13) . . ? C41 C42 C37 123.14(12) . . ? C48 C43 C44 115.06(12) . . ? C48 C43 B1 121.90(11) . . ? C44 C43 B1 122.93(11) . . ? C45 C44 C43 122.86(13) . . ? C46 C45 C44 119.99(13) . . ? C47 C46 C45 119.07(13) . . ? C46 C47 C48 120.12(13) . . ? C47 C48 C43 122.88(13) . . ? O1 C1 H1A 111.0 . . ? C2 C1 H1A 111.0 . . ? O1 C1 H1B 111.0 . . ? C2 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? C1 C2 H2A 111.0 . . ? C3 C2 H2A 111.0 . . ? C1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? C4 C3 H3A 110.7 . . ? C2 C3 H3A 110.7 . . ? C4 C3 H3B 110.7 . . ? C2 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? O1 C4 H4A 110.4 . . ? C3 C4 H4A 110.4 . . ? O1 C4 H4B 110.4 . . ? C3 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? O2 C5 H5A 111.0 . . ? C6 C5 H5A 111.0 . . ? O2 C5 H5B 111.0 . . ? C6 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C5 C6 H6A 111.1 . . ? C7 C6 H6A 111.1 . . ? C5 C6 H6B 111.1 . . ? C7 C6 H6B 111.1 . . ? H6A C6 H6B 109.1 . . ? C6 C7 H7A 110.9 . . ? C8 C7 H7A 110.9 . . ? C6 C7 H7B 110.9 . . ? C8 C7 H7B 110.9 . . ? H7A C7 H7B 108.9 . . ? O2 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O2 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? O3 C9 H9A 110.9 . . ? C10 C9 H9A 110.9 . . ? O3 C9 H9B 110.9 . . ? C10 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? C9 C10 H10A 111.3 . . ? C11 C10 H10A 111.3 . . ? C9 C10 H10B 111.3 . . ? C11 C10 H10B 111.3 . . ? H10A C10 H10B 109.2 . . ? C12 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? C12 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? O3 C12 H12A 110.3 . . ? C11 C12 H12A 110.3 . . ? O3 C12 H12B 110.3 . . ? C11 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? O4 C13 H13A 111.0 . . ? C14 C13 H13A 111.0 . . ? O4 C13 H13B 111.0 . . ? C14 C13 H13B 111.0 . . ? H13A C13 H13B 109.0 . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14B 111.3 . . ? C15 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C16 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? C16 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? O4 C16 H16A 110.4 . . ? C15 C16 H16A 110.4 . . ? O4 C16 H16B 110.4 . . ? C15 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? O5 C17 H17A 110.8 . . ? C18 C17 H17A 110.8 . . ? O5 C17 H17B 110.8 . . ? C18 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? C17 C18 H18A 110.9 . . ? C19 C18 H18A 110.9 . . ? C17 C18 H18B 110.9 . . ? C19 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? C20 C19 H19A 111.0 . . ? C18 C19 H19A 111.0 . . ? C20 C19 H19B 111.0 . . ? C18 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? O5 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? O5 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? O6 C21 H21A 110.6 . . ? C22 C21 H21A 110.6 . . ? O6 C21 H21B 110.6 . . ? C22 C21 H21B 110.6 . . ? H21A C21 H21B 108.7 . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22B 111.1 . . ? C21 C22 H22B 111.1 . . ? H22A C22 H22B 109.0 . . ? C24 C23 H23A 111.5 . . ? C22 C23 H23A 111.5 . . ? C24 C23 H23B 111.5 . . ? C22 C23 H23B 111.5 . . ? H23A C23 H23B 109.3 . . ? O6 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? O6 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C27 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 H30A 118.5 . . ? C25 C30 H30A 118.5 . . ? C33 C32 H32A 118.6 . . ? C31 C32 H32A 118.6 . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 H36A 118.6 . . ? C31 C36 H36A 118.6 . . ? C39 C38 H38A 118.6 . . ? C37 C38 H38A 118.6 . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C41 C40 H40A 120.6 . . ? C39 C40 H40A 120.6 . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C41 C42 H42A 118.4 . . ? C37 C42 H42A 118.4 . . ? C45 C44 H44A 118.6 . . ? C43 C44 H44A 118.6 . . ? C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C47 C46 H46A 120.5 . . ? C45 C46 H46A 120.5 . . ? C46 C47 H47A 119.9 . . ? C48 C47 H47A 119.9 . . ? C47 C48 H48A 118.6 . . ? C43 C48 H48A 118.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mg1 Mg2 O6 -127.72(5) . . . . ? O3 Mg1 Mg2 O6 -2.51(6) . . . . ? O1 Mg1 Mg2 O6 112.83(6) . . . . ? Cl1 Mg1 Mg2 O6 -63.29(4) . . . . ? Cl2 Mg1 Mg2 O6 58.22(4) . . . . ? Cl3 Mg1 Mg2 O6 177.04(4) . . . . ? O2 Mg1 Mg2 O4 -10.01(6) . . . . ? O3 Mg1 Mg2 O4 115.21(5) . . . . ? O1 Mg1 Mg2 O4 -129.45(5) . . . . ? Cl1 Mg1 Mg2 O4 54.43(4) . . . . ? Cl2 Mg1 Mg2 O4 175.94(4) . . . . ? Cl3 Mg1 Mg2 O4 -65.24(4) . . . . ? O2 Mg1 Mg2 O5 114.93(5) . . . . ? O3 Mg1 Mg2 O5 -119.86(5) . . . . ? O1 Mg1 Mg2 O5 -4.52(6) . . . . ? Cl1 Mg1 Mg2 O5 179.36(4) . . . . ? Cl2 Mg1 Mg2 O5 -59.13(4) . . . . ? Cl3 Mg1 Mg2 O5 59.69(4) . . . . ? O2 Mg1 Mg2 Cl3 55.23(4) . . . . ? O3 Mg1 Mg2 Cl3 -179.55(4) . . . . ? O1 Mg1 Mg2 Cl3 -64.21(4) . . . . ? Cl1 Mg1 Mg2 Cl3 119.67(2) . . . . ? Cl2 Mg1 Mg2 Cl3 -118.82(2) . . . . ? O2 Mg1 Mg2 Cl1 -64.44(4) . . . . ? O3 Mg1 Mg2 Cl1 60.78(4) . . . . ? O1 Mg1 Mg2 Cl1 176.12(4) . . . . ? Cl2 Mg1 Mg2 Cl1 121.51(2) . . . . ? Cl3 Mg1 Mg2 Cl1 -119.67(2) . . . . ? O2 Mg1 Mg2 Cl2 174.05(4) . . . . ? O3 Mg1 Mg2 Cl2 -60.73(4) . . . . ? O1 Mg1 Mg2 Cl2 54.60(4) . . . . ? Cl1 Mg1 Mg2 Cl2 -121.51(2) . . . . ? Cl3 Mg1 Mg2 Cl2 118.82(2) . . . . ? O2 Mg1 Cl1 Mg2 132.05(3) . . . . ? O3 Mg1 Cl1 Mg2 -132.27(3) . . . . ? Cl2 Mg1 Cl1 Mg2 -42.223(16) . . . . ? Cl3 Mg1 Cl1 Mg2 42.424(16) . . . . ? O6 Mg2 Cl1 Mg1 131.78(3) . . . . ? O4 Mg2 Cl1 Mg1 -139.98(3) . . . . ? Cl3 Mg2 Cl1 Mg1 -43.479(17) . . . . ? Cl2 Mg2 Cl1 Mg1 42.036(16) . . . . ? O3 Mg1 Cl2 Mg2 132.30(3) . . . . ? O1 Mg1 Cl2 Mg2 -139.36(3) . . . . ? Cl1 Mg1 Cl2 Mg2 41.877(16) . . . . ? Cl3 Mg1 Cl2 Mg2 -42.873(16) . . . . ? O6 Mg2 Cl2 Mg1 -134.88(3) . . . . ? O5 Mg2 Cl2 Mg1 135.66(3) . . . . ? Cl3 Mg2 Cl2 Mg1 43.932(17) . . . . ? Cl1 Mg2 Cl2 Mg1 -41.537(16) . . . . ? O4 Mg2 Cl3 Mg1 133.75(3) . . . . ? O5 Mg2 Cl3 Mg1 -135.33(3) . . . . ? Cl1 Mg2 Cl3 Mg1 42.560(17) . . . . ? Cl2 Mg2 Cl3 Mg1 -43.524(16) . . . . ? O2 Mg1 Cl3 Mg2 -137.62(3) . . . . ? O1 Mg1 Cl3 Mg2 133.61(3) . . . . ? Cl1 Mg1 Cl3 Mg2 -43.014(17) . . . . ? Cl2 Mg1 Cl3 Mg2 43.838(16) . . . . ? O2 Mg1 O1 C4 136.64(11) . . . . ? O3 Mg1 O1 C4 40.97(11) . . . . ? Cl2 Mg1 O1 C4 -49.10(11) . . . . ? Cl3 Mg1 O1 C4 -133.43(11) . . . . ? Mg2 Mg1 O1 C4 -88.98(11) . . . . ? O2 Mg1 O1 C1 -77.46(12) . . . . ? O3 Mg1 O1 C1 -173.12(11) . . . . ? Cl2 Mg1 O1 C1 96.81(11) . . . . ? Cl3 Mg1 O1 C1 12.47(11) . . . . ? Mg2 Mg1 O1 C1 56.92(12) . . . . ? O3 Mg1 O2 C5 81.88(12) . . . . ? O1 Mg1 O2 C5 -6.33(12) . . . . ? Cl1 Mg1 O2 C5 172.77(12) . . . . ? Cl3 Mg1 O2 C5 -102.82(12) . . . . ? Mg2 Mg1 O2 C5 -142.23(11) . . . . ? O3 Mg1 O2 C8 -128.30(10) . . . . ? O1 Mg1 O2 C8 143.49(11) . . . . ? Cl1 Mg1 O2 C8 -37.41(10) . . . . ? Cl3 Mg1 O2 C8 47.00(10) . . . . ? Mg2 Mg1 O2 C8 7.59(12) . . . . ? O2 Mg1 O3 C9 -28.58(11) . . . . ? O1 Mg1 O3 C9 60.02(11) . . . . ? Cl1 Mg1 O3 C9 -123.24(10) . . . . ? Cl2 Mg1 O3 C9 150.43(10) . . . . ? Mg2 Mg1 O3 C9 -166.23(9) . . . . ? O2 Mg1 O3 C12 139.72(11) . . . . ? O1 Mg1 O3 C12 -131.68(11) . . . . ? Cl1 Mg1 O3 C12 45.06(11) . . . . ? Cl2 Mg1 O3 C12 -41.27(11) . . . . ? Mg2 Mg1 O3 C12 2.07(12) . . . . ? O6 Mg2 O4 C16 -136.17(13) . . . . ? O5 Mg2 O4 C16 -46.74(13) . . . . ? Cl3 Mg2 O4 C16 45.24(13) . . . . ? Cl1 Mg2 O4 C16 130.54(12) . . . . ? Mg1 Mg2 O4 C16 91.41(13) . . . . ? O6 Mg2 O4 C13 59.84(11) . . . . ? O5 Mg2 O4 C13 149.27(11) . . . . ? Cl3 Mg2 O4 C13 -118.75(10) . . . . ? Cl1 Mg2 O4 C13 -33.45(11) . . . . ? Mg1 Mg2 O4 C13 -72.58(11) . . . . ? O6 Mg2 O5 C20 -52.18(10) . . . . ? O4 Mg2 O5 C20 -140.32(10) . . . . ? Cl3 Mg2 O5 C20 123.03(10) . . . . ? Cl2 Mg2 O5 C20 37.79(10) . . . . ? Mg1 Mg2 O5 C20 80.06(10) . . . . ? O6 Mg2 O5 C17 164.16(10) . . . . ? O4 Mg2 O5 C17 76.02(10) . . . . ? Cl3 Mg2 O5 C17 -20.63(10) . . . . ? Cl2 Mg2 O5 C17 -105.87(10) . . . . ? Mg1 Mg2 O5 C17 -63.60(11) . . . . ? O4 Mg2 O6 C24 45.93(11) . . . . ? O5 Mg2 O6 C24 -44.79(11) . . . . ? Cl1 Mg2 O6 C24 137.56(10) . . . . ? Cl2 Mg2 O6 C24 -136.74(11) . . . . ? Mg1 Mg2 O6 C24 -178.49(9) . . . . ? O4 Mg2 O6 C21 -129.54(11) . . . . ? O5 Mg2 O6 C21 139.74(11) . . . . ? Cl1 Mg2 O6 C21 -37.91(10) . . . . ? Cl2 Mg2 O6 C21 47.78(10) . . . . ? Mg1 Mg2 O6 C21 6.04(12) . . . . ? C4 O1 C1 C2 40.01(17) . . . . ? Mg1 O1 C1 C2 -110.93(14) . . . . ? O1 C1 C2 C3 -34.12(19) . . . . ? C1 C2 C3 C4 15.9(2) . . . . ? C1 O1 C4 C3 -29.94(18) . . . . ? Mg1 O1 C4 C3 121.33(14) . . . . ? C2 C3 C4 O1 8.0(2) . . . . ? C8 O2 C5 C6 41.72(17) . . . . ? Mg1 O2 C5 C6 -164.37(11) . . . . ? O2 C5 C6 C7 -38.09(17) . . . . ? C5 C6 C7 C8 20.50(17) . . . . ? C5 O2 C8 C7 -28.25(15) . . . . ? Mg1 O2 C8 C7 176.45(9) . . . . ? C6 C7 C8 O2 4.14(16) . . . . ? C12 O3 C9 C10 27.64(15) . . . . ? Mg1 O3 C9 C10 -162.62(9) . . . . ? O3 C9 C10 C11 -36.41(14) . . . . ? C9 C10 C11 C12 31.79(16) . . . . ? C9 O3 C12 C11 -7.16(17) . . . . ? Mg1 O3 C12 C11 -177.27(10) . . . . ? C10 C11 C12 O3 -15.89(17) . . . . ? C16 O4 C13 C14 34.49(16) . . . . ? Mg2 O4 C13 C14 -158.91(10) . . . . ? O4 C13 C14 C15 -38.74(15) . . . . ? C13 C14 C15 C16 29.07(17) . . . . ? C13 O4 C16 C15 -15.59(17) . . . . ? Mg2 O4 C16 C15 178.48(10) . . . . ? C14 C15 C16 O4 -9.22(18) . . . . ? C20 O5 C17 C18 -41.43(13) . . . . ? Mg2 O5 C17 C18 107.48(11) . . . . ? O5 C17 C18 C19 24.19(14) . . . . ? C17 C18 C19 C20 1.09(15) . . . . ? C17 O5 C20 C19 42.40(13) . . . . ? Mg2 O5 C20 C19 -108.15(11) . . . . ? C18 C19 C20 O5 -26.20(14) . . . . ? C24 O6 C21 C22 2.79(15) . . . . ? Mg2 O6 C21 C22 178.93(9) . . . . ? O6 C21 C22 C23 21.77(15) . . . . ? C21 C22 C23 C24 -36.93(15) . . . . ? C21 O6 C24 C23 -26.55(15) . . . . ? Mg2 O6 C24 C23 157.36(9) . . . . ? C22 C23 C24 O6 39.13(14) . . . . ? C31 B1 C25 C26 151.50(12) . . . . ? C37 B1 C25 C26 31.24(17) . . . . ? C43 B1 C25 C26 -87.39(14) . . . . ? C31 B1 C25 C30 -36.22(15) . . . . ? C37 B1 C25 C30 -156.48(12) . . . . ? C43 B1 C25 C30 84.88(14) . . . . ? C30 C25 C26 C27 -0.92(19) . . . . ? B1 C25 C26 C27 171.79(13) . . . . ? C25 C26 C27 C28 -0.4(2) . . . . ? C26 C27 C28 C29 0.8(2) . . . . ? C27 C28 C29 C30 0.2(2) . . . . ? C28 C29 C30 C25 -1.7(2) . . . . ? C26 C25 C30 C29 1.97(19) . . . . ? B1 C25 C30 C29 -170.93(12) . . . . ? C25 B1 C31 C32 -93.06(14) . . . . ? C37 B1 C31 C32 30.74(16) . . . . ? C43 B1 C31 C32 149.25(12) . . . . ? C25 B1 C31 C36 83.60(14) . . . . ? C37 B1 C31 C36 -152.59(12) . . . . ? C43 B1 C31 C36 -34.08(17) . . . . ? C36 C31 C32 C33 0.3(2) . . . . ? B1 C31 C32 C33 177.19(13) . . . . ? C31 C32 C33 C34 0.2(2) . . . . ? C32 C33 C34 C35 -0.4(2) . . . . ? C33 C34 C35 C36 0.1(2) . . . . ? C34 C35 C36 C31 0.4(2) . . . . ? C32 C31 C36 C35 -0.58(19) . . . . ? B1 C31 C36 C35 -177.44(12) . . . . ? C25 B1 C37 C42 -155.04(11) . . . . ? C31 B1 C37 C42 84.12(14) . . . . ? C43 B1 C37 C42 -37.09(15) . . . . ? C25 B1 C37 C38 29.91(17) . . . . ? C31 B1 C37 C38 -90.93(14) . . . . ? C43 B1 C37 C38 147.86(12) . . . . ? C42 C37 C38 C39 1.38(19) . . . . ? B1 C37 C38 C39 176.66(13) . . . . ? C37 C38 C39 C40 -1.3(2) . . . . ? C38 C39 C40 C41 0.0(2) . . . . ? C39 C40 C41 C42 1.1(2) . . . . ? C40 C41 C42 C37 -1.0(2) . . . . ? C38 C37 C42 C41 -0.28(19) . . . . ? B1 C37 C42 C41 -175.80(12) . . . . ? C25 B1 C43 C48 35.89(15) . . . . ? C31 B1 C43 C48 154.93(11) . . . . ? C37 B1 C43 C48 -86.53(14) . . . . ? C25 B1 C43 C44 -148.20(12) . . . . ? C31 B1 C43 C44 -29.16(16) . . . . ? C37 B1 C43 C44 89.38(14) . . . . ? C48 C43 C44 C45 -1.00(19) . . . . ? B1 C43 C44 C45 -177.17(12) . . . . ? C43 C44 C45 C46 0.8(2) . . . . ? C44 C45 C46 C47 0.1(2) . . . . ? C45 C46 C47 C48 -0.9(2) . . . . ? C46 C47 C48 C43 0.7(2) . . . . ? C44 C43 C48 C47 0.26(19) . . . . ? B1 C43 C48 C47 176.47(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.148 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.049 _vrf_PLAT094_cmpd3 ; RESPONSE: The slightly large positive electron density, which leads to this alert is located near a carbon of on thf ligand. Presumably this is due to thermal motion or disorder at this carbon. Attempts to model this did not significantly iomprove the model and it was retained as a single carbon. ;