# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ning Tang' _publ_contact_author_email TANGN@LZU.EDU.CN _publ_section_title ; Selective Colorimetric and Fluorescent Detection of HSO4- with Sodium (?), Magnesium (?), Aluminum (?) Xanthone-Crown Ether Complexes ; loop_ _publ_author_name 'Ning Tang.' 'Xiaobo Pan.' 'Rui Shen.' 'Huifang Wang.' 'Jincai Wu.' 'Lihui Yao.' # Attachment 'AlL.cif' data_pnna _database_code_depnum_ccdc_archive 'CCDC 670883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H28 Al0.50 Cl1.50 O16' _chemical_formula_weight 603.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 12.1838(11) _cell_length_b 28.772(3) _cell_length_c 14.5984(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5117.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3298 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 21.75 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.299 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9157 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26451 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5031 _reflns_number_gt 2727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5031 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1460 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2716 _refine_ls_wR_factor_gt 0.2387 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.25358(14) 0.2500 0.2500 0.0356(5) Uani 1 2 d S . . Cl1 Cl 0.61807(13) 0.29747(7) 0.10184(12) 0.0810(6) Uani 1 1 d . . . Cl2 Cl 0.2500 0.5000 0.89872(16) 0.0830(8) Uani 1 2 d S . . C1 C 0.1496(4) 0.36469(16) 0.5250(3) 0.0451(11) Uani 1 1 d . . . C2 C 0.1130(5) 0.37004(19) 0.6142(4) 0.0573(14) Uani 1 1 d . . . H2 H 0.0594 0.3502 0.6370 0.069 Uiso 1 1 calc R . . C3 C 0.1556(5) 0.4047(2) 0.6697(4) 0.0591(15) Uani 1 1 d . . . H3 H 0.1320 0.4070 0.7301 0.071 Uiso 1 1 calc R . . C4 C 0.2301(5) 0.43505(19) 0.6382(4) 0.0592(15) Uani 1 1 d . . . H4 H 0.2577 0.4583 0.6760 0.071 Uiso 1 1 calc R . . C5 C 0.2654(4) 0.43121(17) 0.5481(3) 0.0478(12) Uani 1 1 d . . . C6 C 0.3679(4) 0.46674(17) 0.4289(4) 0.0489(12) Uani 1 1 d . . . C7 C 0.4217(4) 0.50630(18) 0.4029(4) 0.0571(14) Uani 1 1 d . . . H7 H 0.4350 0.5300 0.4448 0.069 Uiso 1 1 calc R . . C8 C 0.4555(5) 0.51023(19) 0.3142(5) 0.0646(16) Uani 1 1 d . . . H8A H 0.4915 0.5372 0.2959 0.078 Uiso 1 1 calc R . . C9 C 0.4381(4) 0.47563(18) 0.2511(4) 0.0569(13) Uani 1 1 d . . . H9A H 0.4626 0.4792 0.1911 0.068 Uiso 1 1 calc R . . C10 C 0.3836(4) 0.43534(16) 0.2772(3) 0.0460(11) Uani 1 1 d . . . C11 C 0.3458(3) 0.43019(15) 0.3681(3) 0.0408(11) Uani 1 1 d . . . C12 C 0.2862(4) 0.38942(16) 0.4022(3) 0.0399(11) Uani 1 1 d . . . C13 C 0.0035(4) 0.31386(19) 0.4870(4) 0.0571(14) Uani 1 1 d . . . H13A H -0.0489 0.3392 0.4901 0.069 Uiso 1 1 calc R . . H13B H 0.0043 0.2983 0.5459 0.069 Uiso 1 1 calc R . . C14 C -0.0299(4) 0.28027(18) 0.4134(4) 0.0571(14) Uani 1 1 d . . . H14A H 0.0203 0.2541 0.4139 0.069 Uiso 1 1 calc R . . H14B H -0.1026 0.2685 0.4272 0.069 Uiso 1 1 calc R . . C15 C -0.1182(5) 0.3322(2) 0.3066(5) 0.0784(19) Uani 1 1 d . . . H15A H -0.1140 0.3581 0.3490 0.094 Uiso 1 1 calc R . . H15B H -0.1885 0.3169 0.3149 0.094 Uiso 1 1 calc R . . C16 C -0.1075(4) 0.3491(2) 0.2109(4) 0.0729(17) Uani 1 1 d . . . H16A H -0.1085 0.3231 0.1687 0.087 Uiso 1 1 calc R . . H16B H -0.1682 0.3695 0.1959 0.087 Uiso 1 1 calc R . . C17 C 0.0069(5) 0.3910(3) 0.1123(4) 0.080(2) Uani 1 1 d . . . H17A H -0.0420 0.4171 0.1019 0.096 Uiso 1 1 calc R . . H17B H -0.0096 0.3671 0.0675 0.096 Uiso 1 1 calc R . . C18 C 0.1216(5) 0.4060(2) 0.1028(4) 0.0729(17) Uani 1 1 d . . . H18A H 0.1326 0.4199 0.0429 0.088 Uiso 1 1 calc R . . H18B H 0.1385 0.4292 0.1488 0.088 Uiso 1 1 calc R . . C19 C 0.2982(4) 0.3737(2) 0.0742(4) 0.0562(13) Uani 1 1 d . . . H19A H 0.2895 0.3824 0.0104 0.067 Uiso 1 1 calc R . . H19B H 0.3382 0.3446 0.0762 0.067 Uiso 1 1 calc R . . C20 C 0.3640(5) 0.4102(2) 0.1215(3) 0.0612(15) Uani 1 1 d . . . H20A H 0.4388 0.4102 0.0986 0.073 Uiso 1 1 calc R . . H20B H 0.3324 0.4407 0.1106 0.073 Uiso 1 1 calc R . . C30 C 0.2322(4) 0.39519(15) 0.4906(3) 0.0398(11) Uani 1 1 d . . . O1 O 0.3375(3) 0.46419(12) 0.5188(2) 0.0565(9) Uani 1 1 d . . . O2 O 0.2860(3) 0.35232(11) 0.3608(2) 0.0474(8) Uani 1 1 d . . . O3 O 0.1105(3) 0.33176(11) 0.4669(2) 0.0487(8) Uani 1 1 d . . . O4 O -0.0307(3) 0.30018(12) 0.3238(3) 0.0583(10) Uani 1 1 d . . . O5 O -0.0086(3) 0.37308(14) 0.2033(3) 0.0635(10) Uani 1 1 d . . . O6 O 0.1928(3) 0.36695(12) 0.1134(2) 0.0533(9) Uani 1 1 d . . . O7 O 0.3631(3) 0.39971(12) 0.2183(2) 0.0539(9) Uani 1 1 d . . . O8 O 0.1481(2) 0.29540(10) 0.2267(2) 0.0414(8) Uani 1 1 d . . . H81 H 0.0976 0.2992 0.2700 0.050 Uiso 1 1 d R . . H82 H 0.1646 0.3228 0.2021 0.050 Uiso 1 1 d R . . O9 O 0.2563(2) 0.23621(11) 0.1225(2) 0.0423(8) Uani 1 1 d . . . H91 H 0.2501 0.2070 0.1034 0.051 Uiso 1 1 d R . . H92 H 0.2354 0.2528 0.0741 0.051 Uiso 1 1 d R . . O10 O 0.3630(2) 0.29528(10) 0.2341(2) 0.0444(8) Uani 1 1 d . . . H101 H 0.3539 0.3247 0.2510 0.053 Uiso 1 1 d R . . H102 H 0.4329 0.2946 0.2165 0.053 Uiso 1 1 d R . . O15 O 0.3112(16) 0.4941(5) 0.9660(10) 0.398(15) Uani 1 1 d . . . O16 O 0.2621(18) 0.4643(5) 0.8602(9) 0.455(15) Uani 1 1 d . . . O17 O 0.5186(6) 0.2834(4) 0.1036(10) 0.313(9) Uani 1 1 d . . . O18 O 0.6298(5) 0.3453(2) 0.1160(5) 0.155(3) Uani 1 1 d . . . O19 O 0.661(2) 0.2789(6) 0.1742(10) 0.459(15) Uani 1 1 d . . . O20 O 0.6768(6) 0.2812(2) 0.0326(5) 0.161(3) Uani 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 Al1 0.0317(9) 0.0354(10) 0.0395(10) -0.0040(8) 0.000 0.000 Cl1 0.0646(10) 0.1117(15) 0.0666(10) -0.0088(9) 0.0195(8) -0.0195(9) Cl2 0.123(2) 0.0754(16) 0.0506(12) 0.000 0.000 0.0285(14) C1 0.051(3) 0.041(3) 0.043(3) -0.001(2) 0.006(2) 0.007(2) C2 0.060(3) 0.059(3) 0.053(3) -0.005(3) 0.011(3) 0.011(3) C3 0.068(4) 0.069(4) 0.040(3) -0.005(3) 0.004(3) 0.022(3) C4 0.083(4) 0.051(3) 0.044(3) -0.018(2) -0.009(3) 0.020(3) C5 0.050(3) 0.043(3) 0.051(3) -0.008(2) -0.003(2) 0.011(2) C6 0.045(3) 0.044(3) 0.058(3) -0.005(2) -0.010(2) 0.004(2) C7 0.050(3) 0.043(3) 0.079(4) -0.004(3) -0.007(3) -0.004(2) C8 0.058(3) 0.045(3) 0.091(5) 0.010(3) -0.009(3) -0.011(3) C9 0.052(3) 0.055(3) 0.063(3) 0.013(3) 0.002(3) -0.006(3) C10 0.042(3) 0.040(3) 0.056(3) 0.001(2) -0.001(2) 0.002(2) C11 0.035(2) 0.039(3) 0.048(3) 0.002(2) -0.002(2) 0.0016(19) C12 0.037(2) 0.038(3) 0.045(3) -0.003(2) -0.004(2) 0.0079(19) C13 0.043(3) 0.068(3) 0.060(3) 0.000(3) 0.015(3) -0.001(3) C14 0.041(3) 0.060(3) 0.070(4) 0.001(3) 0.013(3) -0.005(2) C15 0.044(3) 0.098(5) 0.094(5) 0.014(4) 0.016(3) 0.018(3) C16 0.043(3) 0.100(5) 0.076(4) 0.002(4) -0.006(3) 0.017(3) C17 0.069(4) 0.102(5) 0.069(4) 0.024(4) -0.006(3) 0.033(4) C18 0.075(4) 0.065(4) 0.078(4) 0.018(3) -0.001(3) 0.013(3) C19 0.061(3) 0.070(4) 0.038(3) 0.002(3) 0.010(2) 0.002(3) C20 0.067(4) 0.074(4) 0.042(3) 0.005(3) 0.007(3) -0.011(3) C30 0.045(3) 0.036(2) 0.039(3) -0.0038(19) -0.002(2) 0.014(2) O1 0.062(2) 0.049(2) 0.058(2) -0.0170(17) -0.0033(18) -0.0042(18) O2 0.059(2) 0.0374(18) 0.0463(19) -0.0069(15) 0.0112(16) -0.0063(15) O3 0.0455(19) 0.0503(19) 0.0504(19) -0.0093(15) 0.0115(15) -0.0045(15) O4 0.0349(18) 0.074(3) 0.066(2) 0.0012(19) 0.0062(16) 0.0072(17) O5 0.049(2) 0.081(3) 0.061(2) 0.006(2) -0.0025(18) 0.0111(19) O6 0.054(2) 0.056(2) 0.050(2) 0.0061(16) 0.0008(16) 0.0048(17) O7 0.069(2) 0.051(2) 0.0423(19) 0.0041(15) 0.0006(17) -0.0052(17) O8 0.0308(15) 0.0454(18) 0.0481(19) 0.0040(14) 0.0061(13) 0.0081(13) O9 0.0484(18) 0.0402(18) 0.0384(17) -0.0044(13) -0.0020(14) 0.0013(14) O10 0.0379(16) 0.0399(18) 0.055(2) -0.0061(14) 0.0097(15) -0.0047(13) O15 0.67(4) 0.188(10) 0.340(16) -0.049(13) -0.37(2) 0.036(18) O16 0.78(3) 0.336(16) 0.250(14) -0.232(13) -0.228(18) 0.33(2) O17 0.092(5) 0.326(13) 0.52(2) -0.329(14) 0.142(8) -0.094(6) O18 0.137(5) 0.139(6) 0.189(7) -0.099(5) 0.026(5) -0.023(4) O19 0.81(5) 0.362(19) 0.208(13) 0.190(14) -0.06(2) -0.08(3) O20 0.163(6) 0.136(5) 0.184(7) -0.069(5) 0.125(6) -0.036(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O8 1.863(3) 4 ? Al1 O8 1.863(3) . ? Al1 O10 1.878(3) 4 ? Al1 O10 1.878(3) . ? Al1 O9 1.904(3) 4 ? Al1 O9 1.904(3) . ? Cl1 O17 1.279(6) . ? Cl1 O19 1.295(15) . ? Cl1 O20 1.325(5) . ? Cl1 O18 1.399(7) . ? Cl2 O16 1.179(8) . ? Cl2 O16 1.179(8) 2_565 ? Cl2 O15 1.245(10) . ? Cl2 O15 1.245(10) 2_565 ? C1 O3 1.358(6) . ? C1 C2 1.385(7) . ? C1 C30 1.426(7) . ? C2 C3 1.387(8) . ? C2 H2 0.9300 . ? C3 C4 1.340(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C4 H4 0.9300 . ? C5 O1 1.362(6) . ? C5 C30 1.395(6) . ? C6 O1 1.365(6) . ? C6 C7 1.368(7) . ? C6 C11 1.402(7) . ? C7 C8 1.363(8) . ? C7 H7 0.9300 . ? C8 C9 1.373(8) . ? C8 H8A 0.9300 . ? C9 C10 1.389(7) . ? C9 H9A 0.9300 . ? C10 O7 1.361(6) . ? C10 C11 1.413(7) . ? C11 C12 1.466(6) . ? C12 O2 1.227(5) . ? C12 C30 1.458(7) . ? C13 O3 1.432(6) . ? C13 C14 1.501(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O4 1.429(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.431(6) . ? C15 C16 1.486(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O5 1.392(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O5 1.437(7) . ? C17 C18 1.469(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O6 1.428(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O6 1.419(6) . ? C19 C20 1.491(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O7 1.445(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? O8 H81 0.8900 . ? O8 H82 0.8899 . ? O9 H91 0.8900 . ? O9 H92 0.8899 . ? O10 H101 0.8900 . ? O10 H102 0.8899 . ? O15 O15 1.53(4) 2_565 ? 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 O8 Al1 O8 92.82(19) 4 . ? O8 Al1 O10 88.89(13) 4 4 ? O8 Al1 O10 176.41(14) . 4 ? O8 Al1 O10 176.41(14) 4 . ? O8 Al1 O10 88.89(13) . . ? O10 Al1 O10 89.6(2) 4 . ? O8 Al1 O9 88.83(13) 4 4 ? O8 Al1 O9 92.55(13) . 4 ? O10 Al1 O9 90.64(13) 4 4 ? O10 Al1 O9 87.94(13) . 4 ? O8 Al1 O9 92.55(13) 4 . ? O8 Al1 O9 88.83(13) . . ? O10 Al1 O9 87.94(13) 4 . ? O10 Al1 O9 90.64(14) . . ? O9 Al1 O9 178.0(2) 4 . ? O17 Cl1 O19 103.8(12) . . ? O17 Cl1 O20 114.5(5) . . ? O19 Cl1 O20 104.9(11) . . ? O17 Cl1 O18 114.0(5) . . ? O19 Cl1 O18 104.1(9) . . ? O20 Cl1 O18 113.9(4) . . ? O16 Cl2 O16 123.0(16) . 2_565 ? O16 Cl2 O15 100.6(9) . . ? O16 Cl2 O15 124.7(14) 2_565 . ? O16 Cl2 O15 124.7(14) . 2_565 ? O16 Cl2 O15 100.6(9) 2_565 2_565 ? O15 Cl2 O15 75.9(19) . 2_565 ? O3 C1 C2 123.5(5) . . ? O3 C1 C30 117.2(4) . . ? C2 C1 C30 119.4(5) . . ? C1 C2 C3 120.6(5) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 121.4(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.9(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? O1 C5 C4 116.3(4) . . ? O1 C5 C30 121.0(4) . . ? C4 C5 C30 122.7(5) . . ? O1 C6 C7 116.2(5) . . ? O1 C6 C11 121.1(4) . . ? C7 C6 C11 122.7(5) . . ? C8 C7 C6 118.5(5) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 122.1(5) . . ? C7 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C8 C9 C10 119.6(5) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? O7 C10 C9 122.9(5) . . ? O7 C10 C11 117.0(4) . . ? C9 C10 C11 120.1(5) . . ? C6 C11 C10 117.0(4) . . ? C6 C11 C12 118.7(4) . . ? C10 C11 C12 124.3(4) . . ? O2 C12 C30 122.3(4) . . ? O2 C12 C11 122.0(4) . . ? C30 C12 C11 115.6(4) . . ? O3 C13 C14 109.4(4) . . ? O3 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? O3 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? O4 C14 C13 113.5(4) . . ? O4 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? O4 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? O4 C15 C16 108.0(5) . . ? O4 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? O4 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? O5 C16 C15 108.2(5) . . ? O5 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? O5 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O5 C17 C18 108.5(5) . . ? O5 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O5 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? O6 C18 C17 109.6(5) . . ? O6 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O6 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O6 C19 C20 113.4(4) . . ? O6 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? O6 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? O7 C20 C19 107.5(4) . . ? O7 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? O7 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C5 C30 C1 116.7(4) . . ? C5 C30 C12 119.1(4) . . ? C1 C30 C12 124.1(4) . . ? C5 O1 C6 121.0(4) . . ? C1 O3 C13 116.3(4) . . ? C14 O4 C15 115.1(4) . . ? C16 O5 C17 111.4(5) . . ? C19 O6 C18 113.4(4) . . ? C10 O7 C20 117.3(4) . . ? Al1 O8 H81 115.7 . . ? Al1 O8 H82 122.7 . . ? H81 O8 H82 109.4 . . ? Al1 O9 H91 120.1 . . ? Al1 O9 H92 131.2 . . ? H91 O9 H92 103.6 . . ? Al1 O10 H101 122.5 . . ? Al1 O10 H102 134.4 . . ? H101 O10 H102 102.8 . . ? Cl2 O15 O15 52.1(10) . 2_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H81 O4 0.89 1.75 2.603(4) 160.0 . O8 H82 O6 0.89 1.85 2.696(4) 159.2 . O9 H91 O2 0.89 1.84 2.584(4) 140.3 4 O9 H91 O3 0.89 2.28 2.947(4) 131.8 4 O9 H92 O20 0.89 1.90 2.781(6) 171.9 6 O10 H102 O17 0.89 1.98 2.709(8) 138.6 . O10 H101 O2 0.89 1.97 2.645(4) 131.5 . O10 H101 O7 0.89 2.21 3.013(4) 149.6 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.895 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.084 # Attachment 'NaL.cif' data_tn2 _database_code_depnum_ccdc_archive 'CCDC 670884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Cl2 Na2 O15' _chemical_formula_weight 631.27 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' Na Na 0.0362 0.0249 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5217(17) _cell_length_b 10.016(2) _cell_length_c 16.074(3) _cell_angle_alpha 75.61(3) _cell_angle_beta 74.83(3) _cell_angle_gamma 79.04(3) _cell_volume 1271.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1673 _cell_measurement_theta_min 2.541 _cell_measurement_theta_max 22.950 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.299 _exptl_crystal_size_mid 0.201 _exptl_crystal_size_min 0.178 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.367 _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 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7755 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5388 _reflns_number_gt 2745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; problem: Alert level A PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O12 PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for Cl2 Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O9 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Cl1 Author response: Due to the disorder of oxygen of perchlorate anion, O9 and O12 show high Ueqs. As a consequence of this, the chloride Cl1 and Cl2 Ueqs will be smaller than those of the oxygen atoms . 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^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5388 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1364 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1988 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 1.0123(2) 0.17894(17) 0.31604(11) 0.0503(5) Uani 1 1 d . . . Na2 Na 0.6023(2) 0.30360(18) 0.29416(12) 0.0595(5) Uani 1 1 d . . . Cl1 Cl 0.21595(14) 0.40435(12) 0.37239(8) 0.0535(3) Uani 1 1 d . . . Cl2 Cl 0.45616(13) 0.06807(12) 0.24416(8) 0.0532(3) Uani 1 1 d . . . O1 O 1.0351(4) 0.2663(3) -0.05924(18) 0.0534(8) Uani 1 1 d . . . O2 O 0.8708(3) 0.2640(3) 0.20280(17) 0.0439(7) Uani 1 1 d . . . O3 O 1.0022(3) 0.0006(3) 0.23316(17) 0.0451(7) Uani 1 1 d . . . O4 O 0.8947(4) -0.0195(3) 0.40612(19) 0.0539(8) Uani 1 1 d . . . O5 O 0.7389(3) 0.2486(3) 0.42458(18) 0.0469(7) Uani 1 1 d . . . O6 O 0.6385(3) 0.5089(3) 0.3267(2) 0.0539(8) Uani 1 1 d . . . O7 O 0.6576(4) 0.4848(3) 0.1597(2) 0.0710(10) Uani 1 1 d . . . O8 O 0.3300(5) 0.3496(4) 0.4269(3) 0.0941(13) Uani 1 1 d . . . O9 O 0.3127(6) 0.4069(5) 0.2856(2) 0.1039(14) Uani 1 1 d . . . O10 O 0.1438(6) 0.5352(4) 0.3834(4) 0.1260(19) Uani 1 1 d . . . O11 O 0.0974(4) 0.3109(4) 0.3941(3) 0.0900(13) Uani 1 1 d . . . O12 O 0.5127(6) 0.0835(5) 0.3158(3) 0.1108(15) Uani 1 1 d . . . O13 O 0.5285(6) 0.1660(4) 0.1719(3) 0.1116(16) Uani 1 1 d . . . O14 O 0.5024(6) -0.0659(4) 0.2295(3) 0.1158(16) Uani 1 1 d . . . O15 O 0.2861(4) 0.0981(5) 0.2626(4) 0.1234(19) Uani 1 1 d . . . C1 C 1.0796(5) 0.0209(4) 0.1462(3) 0.0393(9) Uani 1 1 d . . . C2 C 1.2015(6) -0.0759(5) 0.1122(3) 0.0535(11) Uani 1 1 d . . . H2 H 1.2394 -0.1558 0.1492 0.064 Uiso 1 1 calc R . . C3 C 1.2673(6) -0.0524(5) 0.0213(3) 0.0612(13) Uani 1 1 d . . . H3 H 1.3519 -0.1162 -0.0014 0.073 Uiso 1 1 calc R . . C4 C 1.2112(5) 0.0607(5) -0.0343(3) 0.0545(12) Uani 1 1 d . . . H4 H 1.2537 0.0735 -0.0948 0.065 Uiso 1 1 calc R . . C5 C 1.0893(5) 0.1569(4) 0.0008(3) 0.0440(10) Uani 1 1 d . . . C6 C 0.9101(5) 0.3628(4) -0.0332(3) 0.0454(10) Uani 1 1 d . . . C7 C 0.8537(6) 0.4601(5) -0.0998(3) 0.0609(13) Uani 1 1 d . . . H7 H 0.8985 0.4543 -0.1583 0.073 Uiso 1 1 calc R . . C8 C 0.7334(6) 0.5635(5) -0.0799(4) 0.0649(14) Uani 1 1 d . . . H8 H 0.6949 0.6282 -0.1251 0.078 Uiso 1 1 calc R . . C9 C 0.6667(6) 0.5752(5) 0.0057(4) 0.0609(13) Uani 1 1 d . . . H9 H 0.5848 0.6481 0.0179 0.073 Uiso 1 1 calc R . . C10 C 0.7208(5) 0.4788(4) 0.0741(3) 0.0487(11) Uani 1 1 d . . . C11 C 0.8432(5) 0.3670(4) 0.0562(3) 0.0397(9) Uani 1 1 d . . . C12 C 0.9088(4) 0.2589(4) 0.1238(3) 0.0365(9) Uani 1 1 d . . . C13 C 1.0243(4) 0.1451(4) 0.0917(2) 0.0355(9) Uani 1 1 d . . . C14 C 1.0337(6) -0.1326(4) 0.2895(3) 0.0517(11) Uani 1 1 d . . . H14A H 1.1386 -0.1428 0.3051 0.062 Uiso 1 1 calc R . . H14B H 1.0344 -0.2072 0.2608 0.062 Uiso 1 1 calc R . . C15 C 0.8966(6) -0.1346(5) 0.3693(3) 0.0599(13) Uani 1 1 d . . . H15A H 0.7931 -0.1291 0.3533 0.072 Uiso 1 1 calc R . . H15B H 0.9119 -0.2205 0.4121 0.072 Uiso 1 1 calc R . . C16 C 0.7426(7) 0.0034(6) 0.4693(3) 0.0705(15) Uani 1 1 d . . . H16A H 0.7360 -0.0735 0.5200 0.085 Uiso 1 1 calc R . . H16B H 0.6509 0.0083 0.4429 0.085 Uiso 1 1 calc R . . C17 C 0.7340(7) 0.1319(5) 0.4970(3) 0.0690(14) Uani 1 1 d . . . H17A H 0.6333 0.1451 0.5410 0.083 Uiso 1 1 calc R . . H17B H 0.8253 0.1259 0.5239 0.083 Uiso 1 1 calc R . . C18 C 0.7067(6) 0.3750(5) 0.4579(3) 0.0631(13) Uani 1 1 d . . . H18A H 0.5930 0.3881 0.4895 0.076 Uiso 1 1 calc R . . H18B H 0.7754 0.3671 0.4989 0.076 Uiso 1 1 calc R . . C19 C 0.7396(6) 0.4937(5) 0.3866(4) 0.0638(14) Uani 1 1 d . . . H19A H 0.7193 0.5772 0.4102 0.077 Uiso 1 1 calc R . . H19B H 0.8539 0.4817 0.3559 0.077 Uiso 1 1 calc R . . C20 C 0.6672(7) 0.6242(5) 0.2563(4) 0.0770(17) Uani 1 1 d . . . H20A H 0.7843 0.6250 0.2331 0.092 Uiso 1 1 calc R . . H20B H 0.6218 0.7098 0.2768 0.092 Uiso 1 1 calc R . . C21 C 0.5881(6) 0.6141(5) 0.1859(4) 0.0663(15) Uani 1 1 d . . . H21A H 0.4704 0.6168 0.2082 0.080 Uiso 1 1 calc R . . H21B H 0.6087 0.6913 0.1360 0.080 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 Na1 0.0565(10) 0.0489(10) 0.0478(10) -0.0126(8) -0.0143(8) -0.0058(8) Na2 0.0584(11) 0.0535(11) 0.0653(12) -0.0108(9) -0.0103(9) -0.0116(9) Cl1 0.0520(6) 0.0545(7) 0.0586(7) -0.0234(6) -0.0124(5) -0.0030(5) Cl2 0.0535(7) 0.0478(7) 0.0556(7) -0.0179(5) -0.0070(5) 0.0014(5) O1 0.065(2) 0.0555(19) 0.0356(16) -0.0062(14) -0.0048(14) -0.0110(16) O2 0.0509(17) 0.0430(16) 0.0346(16) -0.0075(13) -0.0105(13) 0.0018(13) O3 0.0617(18) 0.0331(15) 0.0386(16) -0.0077(12) -0.0117(14) -0.0011(13) O4 0.065(2) 0.0460(18) 0.0448(17) -0.0075(14) -0.0039(15) -0.0087(15) O5 0.0476(16) 0.0452(17) 0.0438(17) -0.0091(14) -0.0066(13) -0.0019(13) O6 0.0503(17) 0.0404(17) 0.070(2) -0.0112(15) -0.0143(16) -0.0029(13) O7 0.094(3) 0.0353(17) 0.056(2) 0.0013(15) 0.0059(18) 0.0108(16) O8 0.081(3) 0.107(3) 0.101(3) 0.005(2) -0.042(2) -0.033(2) O9 0.147(4) 0.107(3) 0.054(2) -0.013(2) -0.007(3) -0.035(3) O10 0.116(4) 0.078(3) 0.215(6) -0.089(3) -0.059(4) 0.019(3) O11 0.054(2) 0.086(3) 0.144(4) -0.046(3) -0.018(2) -0.0188(19) O12 0.128(4) 0.114(4) 0.111(3) -0.028(3) -0.065(3) -0.008(3) O13 0.130(4) 0.083(3) 0.083(3) 0.005(2) 0.017(3) -0.007(3) O14 0.120(4) 0.063(3) 0.156(4) -0.045(3) -0.009(3) 0.009(2) O15 0.040(2) 0.126(4) 0.228(6) -0.113(4) -0.004(3) -0.006(2) C1 0.047(2) 0.035(2) 0.040(2) -0.0139(18) -0.0112(19) -0.0066(18) C2 0.061(3) 0.044(3) 0.057(3) -0.017(2) -0.017(2) 0.004(2) C3 0.056(3) 0.057(3) 0.072(3) -0.031(3) -0.008(3) 0.007(2) C4 0.055(3) 0.065(3) 0.044(3) -0.024(2) 0.002(2) -0.012(2) C5 0.051(2) 0.044(2) 0.039(2) -0.0100(19) -0.0065(19) -0.0148(19) C6 0.051(2) 0.047(2) 0.041(2) 0.001(2) -0.016(2) -0.019(2) C7 0.077(3) 0.065(3) 0.041(3) 0.004(2) -0.020(2) -0.022(3) C8 0.071(3) 0.066(3) 0.061(3) 0.012(3) -0.037(3) -0.018(3) C9 0.055(3) 0.044(3) 0.078(4) 0.004(3) -0.025(3) -0.002(2) C10 0.048(2) 0.044(2) 0.049(3) 0.003(2) -0.012(2) -0.011(2) C11 0.042(2) 0.036(2) 0.040(2) -0.0020(18) -0.0101(18) -0.0087(17) C12 0.036(2) 0.038(2) 0.036(2) -0.0043(17) -0.0087(17) -0.0118(17) C13 0.037(2) 0.037(2) 0.038(2) -0.0113(17) -0.0112(17) -0.0068(16) C14 0.076(3) 0.029(2) 0.048(3) -0.0075(19) -0.016(2) -0.002(2) C15 0.080(3) 0.037(2) 0.058(3) 0.001(2) -0.017(3) -0.010(2) C16 0.076(3) 0.067(3) 0.050(3) -0.001(3) 0.008(3) -0.011(3) C17 0.075(3) 0.072(4) 0.044(3) -0.011(3) 0.006(2) -0.001(3) C18 0.065(3) 0.068(3) 0.064(3) -0.034(3) -0.022(3) 0.010(2) C19 0.058(3) 0.051(3) 0.093(4) -0.029(3) -0.029(3) 0.003(2) C20 0.085(4) 0.034(3) 0.111(5) -0.007(3) -0.027(4) -0.010(2) C21 0.063(3) 0.036(2) 0.078(4) 0.000(2) 0.000(3) 0.007(2) _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 Na1 O15 2.327(4) 1_655 ? Na1 O2 2.341(3) . ? Na1 O11 2.347(4) 1_655 ? Na1 O4 2.371(3) . ? Na1 O3 2.505(3) . ? Na1 O5 2.611(3) . ? Na1 Na2 3.558(3) . ? Na2 O6 2.336(3) . ? Na2 O12 2.384(5) . ? Na2 O2 2.394(3) . ? Na2 O7 2.455(4) . ? Na2 O9 2.513(5) . ? Na2 O5 2.552(3) . ? Na2 O8 2.764(5) . ? Na2 O13 2.912(6) . ? Na2 Cl2 3.217(2) . ? Na2 Cl1 3.262(2) . ? Cl1 O10 1.371(4) . ? Cl1 O9 1.419(4) . ? Cl1 O8 1.421(4) . ? Cl1 O11 1.425(4) . ? Cl2 O14 1.385(4) . ? Cl2 O15 1.390(4) . ? Cl2 O13 1.407(4) . ? Cl2 O12 1.410(4) . ? O1 C6 1.350(5) . ? O1 C5 1.364(5) . ? O2 C12 1.237(4) . ? O3 C1 1.362(5) . ? O3 C14 1.437(4) . ? O4 C15 1.416(5) . ? O4 C16 1.441(6) . ? O5 C17 1.429(5) . ? O5 C18 1.447(5) . ? O6 C20 1.409(5) . ? O6 C19 1.415(5) . ? O7 C10 1.352(5) . ? O7 C21 1.434(5) . ? O11 Na1 2.347(4) 1_455 ? O15 Na1 2.327(4) 1_455 ? C1 C2 1.379(6) . ? C1 C13 1.411(5) . ? C2 C3 1.397(6) . ? C2 H2 0.9300 . ? C3 C4 1.351(6) . ? C3 H3 0.9300 . ? C4 C5 1.381(6) . ? C4 H4 0.9300 . ? C5 C13 1.404(5) . ? C6 C7 1.378(6) . ? C6 C11 1.409(6) . ? C7 C8 1.348(7) . ? C7 H7 0.9300 . ? C8 C9 1.368(7) . ? C8 H8 0.9300 . ? C9 C10 1.387(6) . ? C9 H9 0.9300 . ? C10 C11 1.408(6) . ? C11 C12 1.472(5) . ? C12 C13 1.461(5) . ? C14 C15 1.491(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.447(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.446(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.492(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O15 Na1 O2 111.92(17) 1_655 . ? O15 Na1 O11 89.09(15) 1_655 1_655 ? O2 Na1 O11 126.77(14) . 1_655 ? O15 Na1 O4 105.34(16) 1_655 . ? O2 Na1 O4 106.74(12) . . ? O11 Na1 O4 114.00(15) 1_655 . ? O15 Na1 O3 75.44(13) 1_655 . ? O2 Na1 O3 65.95(10) . . ? O11 Na1 O3 163.51(14) 1_655 . ? O4 Na1 O3 66.01(10) . . ? O15 Na1 O5 160.90(17) 1_655 . ? O2 Na1 O5 87.14(10) . . ? O11 Na1 O5 77.85(12) 1_655 . ? O4 Na1 O5 68.47(11) . . ? O3 Na1 O5 115.56(11) . . ? O15 Na1 Na2 153.28(16) 1_655 . ? O2 Na1 Na2 41.87(8) . . ? O11 Na1 Na2 110.81(11) 1_655 . ? O4 Na1 Na2 83.28(10) . . ? O3 Na1 Na2 85.66(9) . . ? O5 Na1 Na2 45.76(7) . . ? O6 Na2 O12 159.02(16) . . ? O6 Na2 O2 96.31(12) . . ? O12 Na2 O2 100.21(16) . . ? O6 Na2 O7 68.95(12) . . ? O12 Na2 O7 129.93(16) . . ? O2 Na2 O7 66.32(11) . . ? O6 Na2 O9 88.96(14) . . ? O12 Na2 O9 86.10(16) . . ? O2 Na2 O9 141.60(13) . . ? O7 Na2 O9 80.55(14) . . ? O6 Na2 O5 69.65(11) . . ? O12 Na2 O5 98.15(14) . . ? O2 Na2 O5 87.40(11) . . ? O7 Na2 O5 127.19(13) . . ? O9 Na2 O5 129.52(13) . . ? O6 Na2 O8 76.82(13) . . ? O12 Na2 O8 84.46(16) . . ? O2 Na2 O8 167.37(13) . . ? O7 Na2 O8 119.47(14) . . ? O9 Na2 O8 49.89(12) . . ? O5 Na2 O8 80.29(11) . . ? O6 Na2 O13 148.65(13) . . ? O12 Na2 O13 48.59(13) . . ? O2 Na2 O13 80.06(13) . . ? O7 Na2 O13 81.34(13) . . ? O9 Na2 O13 76.14(15) . . ? O5 Na2 O13 140.39(13) . . ? O8 Na2 O13 111.34(13) . . ? O6 Na2 Cl2 164.29(11) . . ? O12 Na2 Cl2 23.72(11) . . ? O2 Na2 Cl2 95.42(9) . . ? O7 Na2 Cl2 106.65(11) . . ? O9 Na2 Cl2 75.36(11) . . ? O5 Na2 Cl2 121.38(9) . . ? O8 Na2 Cl2 93.42(10) . . ? O13 Na2 Cl2 25.94(8) . . ? O6 Na2 Cl1 83.11(10) . . ? O12 Na2 Cl1 84.04(13) . . ? O2 Na2 Cl1 165.62(10) . . ? O7 Na2 Cl1 100.37(11) . . ? O9 Na2 Cl1 24.31(9) . . ? O5 Na2 Cl1 105.71(9) . . ? O8 Na2 Cl1 25.61(8) . . ? O13 Na2 Cl1 92.93(11) . . ? Cl2 Na2 Cl1 82.93(5) . . ? O6 Na2 Na1 86.48(9) . . ? O12 Na2 Na1 97.65(13) . . ? O2 Na2 Na1 40.74(7) . . ? O7 Na2 Na1 99.15(11) . . ? O9 Na2 Na1 175.21(12) . . ? O5 Na2 Na1 47.15(8) . . ? O8 Na2 Na1 127.30(10) . . ? O13 Na2 Na1 108.58(11) . . ? Cl2 Na2 Na1 109.22(7) . . ? Cl1 Na2 Na1 152.84(7) . . ? O10 Cl1 O9 111.4(3) . . ? O10 Cl1 O8 110.7(3) . . ? O9 Cl1 O8 103.9(3) . . ? O10 Cl1 O11 111.5(3) . . ? O9 Cl1 O11 111.0(3) . . ? O8 Cl1 O11 108.0(2) . . ? O10 Cl1 Na2 127.6(2) . . ? O9 Cl1 Na2 46.8(2) . . ? O8 Cl1 Na2 57.22(19) . . ? O11 Cl1 Na2 120.72(17) . . ? O14 Cl2 O15 109.7(3) . . ? O14 Cl2 O13 111.4(3) . . ? O15 Cl2 O13 111.1(3) . . ? O14 Cl2 O12 111.1(3) . . ? O15 Cl2 O12 108.7(3) . . ? O13 Cl2 O12 104.7(3) . . ? O14 Cl2 Na2 139.8(2) . . ? O15 Cl2 Na2 108.37(19) . . ? O13 Cl2 Na2 64.8(2) . . ? O12 Cl2 Na2 42.8(2) . . ? C6 O1 C5 120.7(3) . . ? C12 O2 Na1 132.1(3) . . ? C12 O2 Na2 128.4(2) . . ? Na1 O2 Na2 97.39(11) . . ? C1 O3 C14 119.1(3) . . ? C1 O3 Na1 117.3(2) . . ? C14 O3 Na1 106.3(2) . . ? C15 O4 C16 110.7(4) . . ? C15 O4 Na1 119.8(3) . . ? C16 O4 Na1 117.6(3) . . ? C17 O5 C18 109.0(3) . . ? C17 O5 Na2 130.0(3) . . ? C18 O5 Na2 105.9(2) . . ? C17 O5 Na1 102.3(3) . . ? C18 O5 Na1 122.9(3) . . ? Na2 O5 Na1 87.10(10) . . ? C20 O6 C19 112.0(4) . . ? C20 O6 Na2 117.8(3) . . ? C19 O6 Na2 116.0(3) . . ? C10 O7 C21 121.5(3) . . ? C10 O7 Na2 132.3(3) . . ? C21 O7 Na2 105.7(3) . . ? Cl1 O8 Na2 97.2(2) . . ? Cl1 O9 Na2 108.9(2) . . ? Cl1 O11 Na1 134.8(3) . 1_455 ? Cl2 O12 Na2 113.4(3) . . ? Cl2 O13 Na2 89.2(2) . . ? Cl2 O15 Na1 166.1(3) . 1_455 ? O3 C1 C2 122.4(4) . . ? O3 C1 C13 116.3(3) . . ? C2 C1 C13 121.3(4) . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 121.7(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? O1 C5 C4 115.4(4) . . ? O1 C5 C13 121.4(4) . . ? C4 C5 C13 123.2(4) . . ? O1 C6 C7 115.8(4) . . ? O1 C6 C11 122.6(4) . . ? C7 C6 C11 121.6(4) . . ? C8 C7 C6 119.8(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 121.2(4) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? O7 C10 C9 122.6(4) . . ? O7 C10 C11 117.1(4) . . ? C9 C10 C11 120.3(4) . . ? C10 C11 C6 116.7(4) . . ? C10 C11 C12 124.7(4) . . ? C6 C11 C12 118.6(4) . . ? O2 C12 C13 121.7(3) . . ? O2 C12 C11 122.6(4) . . ? C13 C12 C11 115.8(3) . . ? C5 C13 C1 115.8(4) . . ? C5 C13 C12 119.7(4) . . ? C1 C13 C12 124.5(3) . . ? O3 C14 C15 105.0(3) . . ? O3 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? O3 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.8 . . ? O4 C15 C14 108.7(4) . . ? O4 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? O4 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O4 C16 C17 109.7(4) . . ? O4 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? O4 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? O5 C17 C16 111.6(4) . . ? O5 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? O5 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C19 C18 O5 110.7(4) . . ? C19 C18 H18A 109.5 . . ? O5 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? O5 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? O6 C19 C18 110.5(4) . . ? O6 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? O6 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O6 C20 C21 108.8(4) . . ? O6 C20 H20A 109.9 . . ? C21 C20 H20A 109.9 . . ? O6 C20 H20B 109.9 . . ? C21 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? O7 C21 C20 107.3(4) . . ? O7 C21 H21A 110.3 . . ? C20 C21 H21A 110.3 . . ? O7 C21 H21B 110.3 . . ? C20 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.785 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.082 # Attachment 'MgL.cif' data_tn3 _database_code_depnum_ccdc_archive 'CCDC 670885' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H52 Cl4 Mg2 O34' _chemical_formula_weight 1291.26 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.402(3) _cell_length_b 14.290(3) _cell_length_c 15.951(3) _cell_angle_alpha 100.64(3) _cell_angle_beta 97.21(3) _cell_angle_gamma 112.76(3) _cell_volume 2702.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.238 _cell_measurement_theta_max 24.456 _exptl_crystal_description block _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.345 _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 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33008 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.00 _reflns_number_total 11424 _reflns_number_gt 4998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11424 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1771 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.1940 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 0.30480(14) 0.60013(12) 0.30981(11) 0.0506(4) Uani 1 1 d . . . Mg2 Mg 0.84679(14) 0.12209(12) 0.26168(11) 0.0486(4) Uani 1 1 d . . . Cl1 Cl 0.51284(12) 0.78737(11) 0.07221(10) 0.0639(4) Uani 1 1 d . . . Cl2 Cl 0.32003(13) 0.97526(11) 0.33531(10) 0.0652(4) Uani 1 1 d . . . Cl3 Cl 0.83555(13) 0.78040(11) 0.33090(10) 0.0652(4) Uani 1 1 d . . . Cl4 Cl 0.68909(13) 0.41001(12) 0.37278(9) 0.0639(4) Uani 1 1 d . . . O1 O 0.0329(4) 0.3602(3) -0.0410(2) 0.0666(10) Uani 1 1 d . . . O2 O 0.1810(3) 0.4929(3) 0.2159(2) 0.0549(9) Uani 1 1 d . . . O3 O -0.0170(3) 0.4567(3) 0.2509(3) 0.0685(11) Uani 1 1 d . . . O4 O 0.1853(4) 0.6610(3) 0.3411(2) 0.0654(10) Uani 1 1 d . . . O5 O 0.3765(4) 0.7065(3) 0.4347(2) 0.0785(12) Uani 1 1 d . . . O6 O 0.4775(3) 0.6246(3) 0.3358(3) 0.0694(11) Uani 1 1 d . . . O7 O 0.3613(3) 0.4875(3) 0.1808(2) 0.0558(9) Uani 1 1 d . . . O8 O 0.3458(3) 0.7090(3) 0.2390(2) 0.0725(11) Uani 1 1 d . . . H8A H 0.3225 0.7441 0.2348 0.087 Uiso 1 1 d R . . H8B H 0.4197 0.7498 0.2583 0.087 Uiso 1 1 d R . . O9 O 0.2681(3) 0.4913(2) 0.3814(2) 0.0643(10) Uani 1 1 d . . . H9A H 0.2295 0.4308 0.3659 0.077 Uiso 1 1 d R . . H9B H 0.3009 0.5150 0.4466 0.077 Uiso 1 1 d R . . O10 O 1.1471(3) 0.1478(3) 0.0212(2) 0.0593(9) Uani 1 1 d . . . O11 O 0.9787(3) 0.1796(3) 0.2118(2) 0.0524(8) Uani 1 1 d . . . O12 O 0.8053(3) 0.1308(3) 0.0902(2) 0.0580(9) Uani 1 1 d . . . O13 O 0.6762(3) 0.0854(3) 0.2048(3) 0.0634(10) Uani 1 1 d . . . O14 O 0.7562(3) 0.0869(3) 0.3632(2) 0.0583(9) Uani 1 1 d . . . O15 O 0.9607(3) 0.1112(3) 0.3641(2) 0.0542(9) Uani 1 1 d . . . O16 O 1.1704(3) 0.2726(2) 0.3286(2) 0.0496(8) Uani 1 1 d . . . O17 O 0.8771(3) 0.2745(2) 0.3110(2) 0.0657(11) Uani 1 1 d . . . H17C H 0.8517 0.3138 0.3464 0.079 Uiso 1 1 d R . . H17D H 0.9376 0.3274 0.3036 0.079 Uiso 1 1 d R . . O18 O 0.8103(3) -0.0303(3) 0.2071(2) 0.0612(9) Uani 1 1 d . . . H18C H 0.7444 -0.0759 0.1675 0.073 Uiso 1 1 d R . . H18D H 0.8290 -0.0614 0.2319 0.073 Uiso 1 1 d R . . O19 O 0.4892(7) 0.7160(7) 0.1171(7) 0.244(6) Uani 1 1 d . . . O20 O 0.4683(4) 0.7377(6) -0.0163(4) 0.175(3) Uani 1 1 d . . . O21 O 0.4633(5) 0.8552(4) 0.0956(4) 0.132(2) Uani 1 1 d . . . O22 O 0.6285(3) 0.8390(4) 0.0787(3) 0.1092(17) Uani 1 1 d . . . O23 O 0.3130(8) 0.8917(5) 0.2746(4) 0.176(3) Uani 1 1 d . . . O24 O 0.2205(5) 0.9448(8) 0.3557(5) 0.192(4) Uani 1 1 d . . . O25 O 0.3425(7) 1.0570(5) 0.2977(5) 0.186(3) Uani 1 1 d . . . O26 O 0.4018(5) 0.9985(4) 0.4090(5) 0.151(3) Uani 1 1 d . . . O27 O 0.7346(6) 0.7405(9) 0.2763(5) 0.234(5) Uani 1 1 d . . . O28 O 0.8200(7) 0.8162(6) 0.4119(4) 0.158(3) Uani 1 1 d . . . O29 O 0.9018(5) 0.8602(5) 0.2994(5) 0.145(2) Uani 1 1 d . . . O30 O 0.8711(10) 0.7067(6) 0.3316(7) 0.245(6) Uani 1 1 d . . . O31 O 0.6836(5) 0.4344(4) 0.2918(3) 0.1082(17) Uani 1 1 d . . . O32 O 0.6871(9) 0.4831(6) 0.4369(4) 0.191(4) Uani 1 1 d . . . O33 O 0.5904(6) 0.3287(8) 0.3738(5) 0.220(5) Uani 1 1 d . . . O34 O 0.7666(7) 0.3769(8) 0.3934(5) 0.200(4) Uani 1 1 d . . . C1 C -0.0545(5) 0.4292(4) 0.1616(4) 0.0573(14) Uani 1 1 d . . . C2 C -0.1626(5) 0.4093(5) 0.1259(6) 0.085(2) Uani 1 1 d . . . H2 H -0.2082 0.4202 0.1623 0.102 Uiso 1 1 calc R . . C3 C -0.2026(6) 0.3736(5) 0.0372(7) 0.095(3) Uani 1 1 d . . . H3 H -0.2754 0.3607 0.0145 0.114 Uiso 1 1 calc R . . C4 C -0.1383(6) 0.3563(4) -0.0189(5) 0.082(2) Uani 1 1 d . . . H4 H -0.1662 0.3312 -0.0789 0.098 Uiso 1 1 calc R . . C5 C -0.0288(4) 0.3781(4) 0.0181(4) 0.0583(14) Uani 1 1 d . . . C6 C 0.1399(5) 0.3798(4) -0.0139(3) 0.0542(13) Uani 1 1 d . . . C7 C 0.1922(6) 0.3564(4) -0.0780(4) 0.0715(17) Uani 1 1 d . . . H7 H 0.1541 0.3270 -0.1360 0.086 Uiso 1 1 calc R . . C8 C 0.3007(7) 0.3772(5) -0.0547(5) 0.079(2) Uani 1 1 d . . . H8 H 0.3360 0.3604 -0.0978 0.095 Uiso 1 1 calc R . . C9 C 0.3612(5) 0.4222(4) 0.0300(5) 0.0688(16) Uani 1 1 d . . . H9 H 0.4361 0.4367 0.0431 0.083 Uiso 1 1 calc R . . C10 C 0.3092(4) 0.4456(4) 0.0953(3) 0.0466(12) Uani 1 1 d . . . C11 C 0.1950(4) 0.4245(3) 0.0738(3) 0.0415(11) Uani 1 1 d . . . C12 C 0.1359(4) 0.4482(3) 0.1391(3) 0.0407(11) Uani 1 1 d . . . C13 C 0.0172(4) 0.4162(3) 0.1075(3) 0.0464(12) Uani 1 1 d . . . C14 C -0.0171(6) 0.5532(4) 0.2967(5) 0.092(2) Uani 1 1 d . . . H14A H -0.0160 0.5539 0.3578 0.110 Uiso 1 1 calc R . . H14B H -0.0843 0.5583 0.2722 0.110 Uiso 1 1 calc R . . C15 C 0.0841(5) 0.6472(4) 0.2896(4) 0.0721(18) Uani 1 1 d . . . H15A H 0.0901 0.6384 0.2289 0.086 Uiso 1 1 calc R . . H15B H 0.0726 0.7104 0.3071 0.086 Uiso 1 1 calc R . . C16 C 0.2025(8) 0.7065(6) 0.4326(4) 0.095(2) Uani 1 1 d . . . H16A H 0.1761 0.6518 0.4630 0.114 Uiso 1 1 calc R . . H16B H 0.1622 0.7499 0.4416 0.114 Uiso 1 1 calc R . . C17 C 0.3222(9) 0.7708(5) 0.4662(4) 0.107(3) Uani 1 1 d . . . H17A H 0.3460 0.8336 0.4450 0.129 Uiso 1 1 calc R . . H17B H 0.3395 0.7913 0.5296 0.129 Uiso 1 1 calc R . . C18 C 0.4952(7) 0.7569(6) 0.4551(5) 0.110(3) Uani 1 1 d . . . H18A H 0.5231 0.7877 0.5175 0.133 Uiso 1 1 calc R . . H18B H 0.5215 0.8119 0.4250 0.133 Uiso 1 1 calc R . . C19 C 0.5320(6) 0.6748(6) 0.4257(5) 0.100(2) Uani 1 1 d . . . H19A H 0.6118 0.7052 0.4316 0.120 Uiso 1 1 calc R . . H19B H 0.5128 0.6242 0.4606 0.120 Uiso 1 1 calc R . . C20 C 0.5114(5) 0.5450(5) 0.3007(5) 0.0797(19) Uani 1 1 d . . . H20A H 0.4764 0.4837 0.3224 0.096 Uiso 1 1 calc R . . H20B H 0.5911 0.5706 0.3195 0.096 Uiso 1 1 calc R . . C21 C 0.4800(4) 0.5161(5) 0.2046(4) 0.0686(17) Uani 1 1 d . . . H21A H 0.5210 0.5748 0.1820 0.082 Uiso 1 1 calc R . . H21B H 0.4961 0.4573 0.1805 0.082 Uiso 1 1 calc R . . C22 C 0.8645(5) 0.1165(4) 0.0286(3) 0.0536(13) Uani 1 1 d . . . C23 C 0.8200(5) 0.0843(4) -0.0597(4) 0.0682(16) Uani 1 1 d . . . H23 H 0.7462 0.0698 -0.0804 0.082 Uiso 1 1 calc R . . C24 C 0.8860(7) 0.0738(5) -0.1172(4) 0.0764(18) Uani 1 1 d . . . H24 H 0.8546 0.0514 -0.1768 0.092 Uiso 1 1 calc R . . C25 C 0.9939(6) 0.0943(4) -0.0914(4) 0.0705(17) Uani 1 1 d . . . H25 H 1.0363 0.0866 -0.1318 0.085 Uiso 1 1 calc R . . C26 C 1.0396(5) 0.1278(4) -0.0014(3) 0.0523(13) Uani 1 1 d . . . C27 C 1.2025(4) 0.1857(4) 0.1070(3) 0.0485(12) Uani 1 1 d . . . C28 C 1.3127(5) 0.2027(4) 0.1219(4) 0.0623(15) Uani 1 1 d . . . H28 H 1.3452 0.1892 0.0756 0.075 Uiso 1 1 calc R . . C29 C 1.3729(5) 0.2394(4) 0.2057(4) 0.0650(15) Uani 1 1 d . . . H29 H 1.4468 0.2502 0.2167 0.078 Uiso 1 1 calc R . . C30 C 1.3237(5) 0.2613(4) 0.2761(4) 0.0604(14) Uani 1 1 d . . . H30 H 1.3652 0.2872 0.3332 0.073 Uiso 1 1 calc R . . C31 C 1.2152(4) 0.2439(3) 0.2591(3) 0.0459(12) Uani 1 1 d . . . C32 C 1.1492(4) 0.2039(3) 0.1743(3) 0.0401(11) Uani 1 1 d . . . C33 C 1.0312(4) 0.1750(3) 0.1528(3) 0.0432(11) Uani 1 1 d . . . C34 C 0.9772(4) 0.1406(3) 0.0608(3) 0.0427(11) Uani 1 1 d . . . C35 C 0.6892(5) 0.1027(5) 0.0599(4) 0.0708(17) Uani 1 1 d . . . H35A H 0.6498 0.0280 0.0330 0.085 Uiso 1 1 calc R . . H35B H 0.6787 0.1405 0.0174 0.085 Uiso 1 1 calc R . . C36 C 0.6480(5) 0.1322(5) 0.1387(5) 0.0778(18) Uani 1 1 d . . . H36A H 0.6811 0.2079 0.1608 0.093 Uiso 1 1 calc R . . H36B H 0.5682 0.1082 0.1233 0.093 Uiso 1 1 calc R . . C37 C 0.6024(5) 0.0717(5) 0.2647(4) 0.0769(18) Uani 1 1 d . . . H37A H 0.5266 0.0268 0.2337 0.092 Uiso 1 1 calc R . . H37B H 0.6058 0.1389 0.2943 0.092 Uiso 1 1 calc R . . C38 C 0.6406(5) 0.0227(4) 0.3283(4) 0.0698(17) Uani 1 1 d . . . H38A H 0.5999 0.0190 0.3746 0.084 Uiso 1 1 calc R . . H38B H 0.6289 -0.0479 0.2996 0.084 Uiso 1 1 calc R . . C39 C 0.8052(6) 0.0483(5) 0.4258(4) 0.0724(18) Uani 1 1 d . . . H39A H 0.7890 -0.0248 0.4018 0.087 Uiso 1 1 calc R . . H39B H 0.7763 0.0541 0.4783 0.087 Uiso 1 1 calc R . . C40 C 0.9269(5) 0.1138(5) 0.4460(3) 0.0706(17) Uani 1 1 d . . . H40A H 0.9438 0.1853 0.4763 0.085 Uiso 1 1 calc R . . H40B H 0.9653 0.0858 0.4828 0.085 Uiso 1 1 calc R . . C41 C 1.0657(4) 0.1067(4) 0.3640(3) 0.0519(13) Uani 1 1 d . . . H41A H 1.0655 0.0723 0.3055 0.062 Uiso 1 1 calc R . . H41B H 1.0753 0.0642 0.4026 0.062 Uiso 1 1 calc R . . C42 C 1.1629(5) 0.2131(4) 0.3928(3) 0.0626(15) Uani 1 1 d . . . H42A H 1.1562 0.2524 0.4466 0.075 Uiso 1 1 calc R . . H42B H 1.2308 0.2039 0.4049 0.075 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 0.0622(11) 0.0410(8) 0.0459(10) 0.0120(7) 0.0109(8) 0.0186(8) Mg2 0.0486(10) 0.0426(8) 0.0578(11) 0.0156(8) 0.0175(8) 0.0194(8) Cl1 0.0514(9) 0.0617(8) 0.0776(11) 0.0198(7) 0.0180(7) 0.0208(7) Cl2 0.0650(9) 0.0583(8) 0.0816(11) 0.0285(8) 0.0188(8) 0.0299(7) Cl3 0.0777(11) 0.0554(8) 0.0630(10) 0.0120(7) 0.0187(8) 0.0289(8) Cl4 0.0753(10) 0.0784(9) 0.0586(9) 0.0247(7) 0.0228(7) 0.0479(8) O1 0.076(3) 0.055(2) 0.052(2) 0.0150(18) -0.004(2) 0.015(2) O2 0.050(2) 0.065(2) 0.048(2) 0.0052(18) 0.0130(18) 0.0266(18) O3 0.077(3) 0.055(2) 0.094(3) 0.032(2) 0.051(2) 0.033(2) O4 0.096(3) 0.058(2) 0.059(3) 0.0148(18) 0.031(2) 0.045(2) O5 0.113(4) 0.045(2) 0.057(3) 0.0056(18) 0.005(2) 0.019(2) O6 0.052(2) 0.068(2) 0.071(3) 0.022(2) -0.003(2) 0.011(2) O7 0.0386(19) 0.068(2) 0.069(3) 0.0261(19) 0.0178(18) 0.0260(17) O8 0.086(3) 0.063(2) 0.081(3) 0.038(2) 0.027(2) 0.034(2) O9 0.097(3) 0.0349(17) 0.050(2) 0.0110(15) 0.010(2) 0.0179(18) O10 0.072(3) 0.062(2) 0.053(2) 0.0169(18) 0.027(2) 0.033(2) O11 0.044(2) 0.072(2) 0.043(2) 0.0188(17) 0.0116(16) 0.0240(18) O12 0.042(2) 0.066(2) 0.067(3) 0.0207(19) 0.0025(18) 0.0247(18) O13 0.052(2) 0.061(2) 0.086(3) 0.030(2) 0.023(2) 0.0252(19) O14 0.061(2) 0.051(2) 0.068(3) 0.0202(18) 0.031(2) 0.0214(18) O15 0.064(2) 0.067(2) 0.042(2) 0.0213(16) 0.0180(17) 0.0328(19) O16 0.058(2) 0.0429(17) 0.042(2) 0.0101(15) 0.0053(16) 0.0171(16) O17 0.079(3) 0.0426(19) 0.086(3) 0.0208(18) 0.041(2) 0.0277(19) O18 0.062(2) 0.0486(19) 0.069(3) 0.0101(17) 0.0047(19) 0.0242(18) O19 0.229(8) 0.287(10) 0.440(15) 0.311(11) 0.232(10) 0.194(8) O20 0.069(4) 0.255(8) 0.114(5) -0.057(5) 0.003(3) 0.029(4) O21 0.120(4) 0.125(4) 0.171(6) 0.022(4) 0.024(4) 0.084(4) O22 0.052(3) 0.119(4) 0.103(4) -0.017(3) 0.005(2) 0.004(3) O23 0.306(10) 0.124(5) 0.137(6) 0.017(4) 0.049(6) 0.136(6) O24 0.106(5) 0.360(12) 0.159(6) 0.099(7) 0.064(5) 0.123(6) O25 0.222(8) 0.116(5) 0.222(8) 0.113(5) 0.016(6) 0.053(5) O26 0.113(4) 0.101(4) 0.172(6) 0.047(4) -0.060(4) -0.001(3) O27 0.112(5) 0.344(12) 0.119(6) 0.059(7) -0.015(5) -0.023(7) O28 0.256(8) 0.206(7) 0.074(4) 0.026(4) 0.050(5) 0.160(7) O29 0.120(5) 0.113(4) 0.220(7) 0.091(5) 0.069(5) 0.036(4) O30 0.394(14) 0.177(7) 0.368(13) 0.177(8) 0.255(12) 0.232(9) O31 0.142(4) 0.156(5) 0.067(3) 0.055(3) 0.042(3) 0.087(4) O32 0.382(12) 0.191(7) 0.069(4) 0.020(4) 0.036(6) 0.203(8) O33 0.132(6) 0.310(12) 0.169(7) 0.155(8) 0.011(5) 0.006(7) O34 0.255(9) 0.397(12) 0.157(6) 0.164(7) 0.132(6) 0.286(10) C1 0.055(4) 0.039(3) 0.093(5) 0.035(3) 0.031(3) 0.022(2) C2 0.040(4) 0.068(4) 0.167(8) 0.057(5) 0.045(4) 0.024(3) C3 0.043(4) 0.074(5) 0.163(9) 0.056(5) 0.005(5) 0.013(3) C4 0.060(4) 0.057(4) 0.105(6) 0.031(4) -0.020(4) 0.007(3) C5 0.050(3) 0.042(3) 0.075(4) 0.025(3) 0.004(3) 0.011(3) C6 0.072(4) 0.048(3) 0.047(3) 0.017(2) 0.019(3) 0.026(3) C7 0.106(6) 0.060(3) 0.047(4) 0.012(3) 0.025(4) 0.032(4) C8 0.117(6) 0.070(4) 0.075(5) 0.031(4) 0.062(5) 0.048(4) C9 0.070(4) 0.068(4) 0.088(5) 0.032(3) 0.044(4) 0.036(3) C10 0.056(3) 0.045(3) 0.052(3) 0.022(2) 0.023(3) 0.027(2) C11 0.048(3) 0.038(2) 0.048(3) 0.018(2) 0.017(2) 0.023(2) C12 0.042(3) 0.040(2) 0.050(3) 0.020(2) 0.014(2) 0.022(2) C13 0.043(3) 0.036(2) 0.062(3) 0.019(2) 0.009(3) 0.017(2) C14 0.098(5) 0.055(3) 0.139(6) 0.020(4) 0.076(5) 0.036(4) C15 0.085(5) 0.050(3) 0.100(5) 0.026(3) 0.045(4) 0.038(3) C16 0.162(8) 0.090(5) 0.067(5) 0.018(4) 0.043(5) 0.085(6) C17 0.217(10) 0.052(4) 0.058(4) 0.009(3) 0.025(5) 0.066(5) C18 0.123(7) 0.078(5) 0.066(5) 0.004(4) -0.006(5) -0.010(5) C19 0.064(4) 0.117(6) 0.079(5) 0.024(5) -0.016(4) 0.007(4) C20 0.043(3) 0.073(4) 0.120(6) 0.045(4) -0.001(3) 0.017(3) C21 0.040(3) 0.076(4) 0.105(5) 0.041(4) 0.023(3) 0.029(3) C22 0.067(4) 0.041(3) 0.050(3) 0.019(2) 0.005(3) 0.019(3) C23 0.070(4) 0.062(3) 0.063(4) 0.021(3) -0.009(3) 0.022(3) C24 0.111(6) 0.074(4) 0.042(4) 0.013(3) 0.006(4) 0.039(4) C25 0.108(5) 0.058(3) 0.047(4) 0.015(3) 0.019(4) 0.036(4) C26 0.071(4) 0.043(3) 0.045(3) 0.015(2) 0.011(3) 0.026(3) C27 0.057(3) 0.043(3) 0.051(3) 0.020(2) 0.018(3) 0.021(2) C28 0.055(4) 0.057(3) 0.089(5) 0.031(3) 0.035(3) 0.028(3) C29 0.048(3) 0.058(3) 0.095(5) 0.027(3) 0.018(3) 0.024(3) C30 0.057(4) 0.050(3) 0.068(4) 0.017(3) 0.001(3) 0.019(3) C31 0.046(3) 0.031(2) 0.053(3) 0.011(2) 0.007(2) 0.010(2) C32 0.046(3) 0.032(2) 0.047(3) 0.014(2) 0.015(2) 0.018(2) C33 0.048(3) 0.031(2) 0.050(3) 0.017(2) 0.015(2) 0.012(2) C34 0.046(3) 0.035(2) 0.042(3) 0.009(2) 0.007(2) 0.014(2) C35 0.052(4) 0.072(4) 0.083(5) 0.034(3) -0.006(3) 0.021(3) C36 0.047(4) 0.076(4) 0.113(6) 0.037(4) 0.011(4) 0.025(3) C37 0.054(4) 0.079(4) 0.096(5) 0.011(4) 0.033(4) 0.026(3) C38 0.068(4) 0.056(3) 0.083(4) 0.016(3) 0.047(4) 0.014(3) C39 0.103(5) 0.075(4) 0.075(4) 0.040(3) 0.059(4) 0.054(4) C40 0.098(5) 0.091(4) 0.045(3) 0.029(3) 0.025(3) 0.055(4) C41 0.058(3) 0.052(3) 0.052(3) 0.023(2) 0.013(3) 0.024(3) C42 0.072(4) 0.066(3) 0.046(3) 0.024(3) 0.005(3) 0.023(3) _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 1.976(4) . ? Mg1 O8 2.035(4) . ? Mg1 O9 2.042(4) . ? Mg1 O5 2.115(4) . ? Mg1 O4 2.166(4) . ? Mg1 O6 2.176(4) . ? Mg1 O7 2.741(4) . ? Mg2 O11 1.976(4) . ? Mg2 O18 2.026(4) . ? Mg2 O17 2.033(4) . ? Mg2 O14 2.161(4) . ? Mg2 O15 2.163(4) . ? Mg2 O13 2.168(4) . ? Mg2 O12 2.758(4) . ? Cl1 O19 1.315(6) . ? Cl1 O21 1.394(5) . ? Cl1 O20 1.395(6) . ? Cl1 O22 1.416(4) . ? Cl2 O24 1.336(6) . ? Cl2 O23 1.354(6) . ? Cl2 O25 1.360(5) . ? Cl2 O26 1.395(5) . ? Cl3 O30 1.314(6) . ? Cl3 O27 1.356(7) . ? Cl3 O28 1.372(5) . ? Cl3 O29 1.372(5) . ? Cl4 O34 1.327(5) . ? Cl4 O32 1.332(6) . ? Cl4 O33 1.386(7) . ? Cl4 O31 1.399(4) . ? O1 C6 1.345(6) . ? O1 C5 1.382(7) . ? O2 C12 1.226(5) . ? O3 C1 1.377(7) . ? O3 C14 1.438(6) . ? O4 C15 1.416(7) . ? O4 C16 1.433(7) . ? O5 C18 1.433(9) . ? O5 C17 1.436(8) . ? O6 C20 1.429(7) . ? O6 C19 1.434(8) . ? O7 C10 1.357(6) . ? O7 C21 1.459(6) . ? O8 H8A 0.6954 . ? O8 H8B 0.9085 . ? O9 H9A 0.7864 . ? O9 H9B 1.0143 . ? O10 C26 1.343(6) . ? O10 C27 1.370(6) . ? O11 C33 1.250(5) . ? O12 C22 1.372(6) . ? O12 C35 1.440(6) . ? O13 C36 1.435(7) . ? O13 C37 1.443(6) . ? O14 C38 1.431(7) . ? O14 C39 1.433(7) . ? O15 C40 1.433(6) . ? O15 C41 1.434(6) . ? O16 C31 1.395(6) . ? O16 C42 1.436(6) . ? O17 H17C 0.9111 . ? O17 H17D 0.9082 . ? O18 H18C 0.9300 . ? O18 H18D 0.7374 . ? C1 C2 1.385(8) . ? C1 C13 1.409(7) . ? C2 C3 1.371(10) . ? C2 H2 0.9300 . ? C3 C4 1.371(10) . ? C3 H3 0.9300 . ? C4 C5 1.400(8) . ? C4 H4 0.9300 . ? C5 C13 1.394(7) . ? C6 C7 1.373(7) . ? C6 C11 1.399(7) . ? C7 C8 1.352(9) . ? C7 H7 0.9300 . ? C8 C9 1.376(9) . ? C8 H8 0.9300 . ? C9 C10 1.385(7) . ? C9 H9 0.9300 . ? C10 C11 1.422(7) . ? C11 C12 1.453(6) . ? C12 C13 1.465(7) . ? C14 C15 1.531(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.472(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.464(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.474(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.374(7) . ? C22 C34 1.414(7) . ? C23 C24 1.380(8) . ? C23 H23 0.9300 . ? C24 C25 1.350(9) . ? C24 H24 0.9300 . ? C25 C26 1.402(7) . ? C25 H25 0.9300 . ? C26 C34 1.406(7) . ? C27 C28 1.382(7) . ? C27 C32 1.402(6) . ? C28 C29 1.362(8) . ? C28 H28 0.9300 . ? C29 C30 1.418(8) . ? C29 H29 0.9300 . ? C30 C31 1.359(7) . ? C30 H30 0.9300 . ? C31 C32 1.401(7) . ? C32 C33 1.447(6) . ? C33 C34 1.453(6) . ? C35 C36 1.490(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.479(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.488(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.510(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mg1 O8 94.30(17) . . ? O2 Mg1 O9 86.62(16) . . ? O8 Mg1 O9 178.37(18) . . ? O2 Mg1 O5 154.77(18) . . ? O8 Mg1 O5 96.90(17) . . ? O9 Mg1 O5 82.77(15) . . ? O2 Mg1 O4 85.03(16) . . ? O8 Mg1 O4 83.97(15) . . ? O9 Mg1 O4 97.46(16) . . ? O5 Mg1 O4 73.80(18) . . ? O2 Mg1 O6 128.33(17) . . ? O8 Mg1 O6 88.27(16) . . ? O9 Mg1 O6 90.10(16) . . ? O5 Mg1 O6 74.68(19) . . ? O4 Mg1 O6 146.30(17) . . ? O2 Mg1 O7 63.78(12) . . ? O8 Mg1 O7 83.52(14) . . ? O9 Mg1 O7 95.70(13) . . ? O5 Mg1 O7 139.96(17) . . ? O4 Mg1 O7 145.24(15) . . ? O6 Mg1 O7 65.30(14) . . ? O11 Mg2 O18 95.19(16) . . ? O11 Mg2 O17 85.27(15) . . ? O18 Mg2 O17 176.86(19) . . ? O11 Mg2 O14 156.56(17) . . ? O18 Mg2 O14 93.94(15) . . ? O17 Mg2 O14 86.79(14) . . ? O11 Mg2 O15 84.48(14) . . ? O18 Mg2 O15 85.74(15) . . ? O17 Mg2 O15 97.40(16) . . ? O14 Mg2 O15 74.72(14) . . ? O11 Mg2 O13 127.92(16) . . ? O18 Mg2 O13 86.48(15) . . ? O17 Mg2 O13 90.80(16) . . ? O14 Mg2 O13 74.15(15) . . ? O15 Mg2 O13 147.24(15) . . ? O11 Mg2 O12 64.21(13) . . ? O18 Mg2 O12 83.54(14) . . ? O17 Mg2 O12 93.89(14) . . ? O14 Mg2 O12 138.46(15) . . ? O15 Mg2 O12 145.65(13) . . ? O13 Mg2 O12 64.32(13) . . ? O19 Cl1 O21 110.4(4) . . ? O19 Cl1 O20 108.9(7) . . ? O21 Cl1 O20 106.8(4) . . ? O19 Cl1 O22 111.4(5) . . ? O21 Cl1 O22 113.9(3) . . ? O20 Cl1 O22 105.0(3) . . ? O24 Cl2 O23 104.9(6) . . ? O24 Cl2 O25 112.1(5) . . ? O23 Cl2 O25 107.5(5) . . ? O24 Cl2 O26 110.1(4) . . ? O23 Cl2 O26 110.3(5) . . ? O25 Cl2 O26 111.7(4) . . ? O30 Cl3 O27 110.2(7) . . ? O30 Cl3 O28 110.5(5) . . ? O27 Cl3 O28 105.6(5) . . ? O30 Cl3 O29 112.9(5) . . ? O27 Cl3 O29 104.9(5) . . ? O28 Cl3 O29 112.4(5) . . ? O34 Cl4 O32 113.9(5) . . ? O34 Cl4 O33 104.8(6) . . ? O32 Cl4 O33 97.9(6) . . ? O34 Cl4 O31 114.9(3) . . ? O32 Cl4 O31 113.2(4) . . ? O33 Cl4 O31 110.3(4) . . ? C6 O1 C5 120.9(4) . . ? C12 O2 Mg1 152.9(3) . . ? C1 O3 C14 115.6(5) . . ? C15 O4 C16 115.0(5) . . ? C15 O4 Mg1 130.5(3) . . ? C16 O4 Mg1 113.5(4) . . ? C18 O5 C17 115.5(6) . . ? C18 O5 Mg1 114.9(4) . . ? C17 O5 Mg1 118.0(4) . . ? C20 O6 C19 111.4(5) . . ? C20 O6 Mg1 121.9(3) . . ? C19 O6 Mg1 112.5(4) . . ? C10 O7 C21 118.5(4) . . ? C10 O7 Mg1 128.1(3) . . ? C21 O7 Mg1 108.7(3) . . ? Mg1 O8 H8A 126.9 . . ? Mg1 O8 H8B 106.9 . . ? H8A O8 H8B 104.6 . . ? Mg1 O9 H9A 129.0 . . ? Mg1 O9 H9B 118.9 . . ? H9A O9 H9B 112.1 . . ? C26 O10 C27 120.9(4) . . ? C33 O11 Mg2 151.5(3) . . ? C22 O12 C35 117.6(4) . . ? C22 O12 Mg2 126.7(3) . . ? C35 O12 Mg2 110.1(3) . . ? C36 O13 C37 112.1(4) . . ? C36 O13 Mg2 122.0(3) . . ? C37 O13 Mg2 115.4(4) . . ? C38 O14 C39 113.4(4) . . ? C38 O14 Mg2 112.1(3) . . ? C39 O14 Mg2 113.6(3) . . ? C40 O15 C41 115.6(4) . . ? C40 O15 Mg2 113.9(3) . . ? C41 O15 Mg2 130.4(3) . . ? C31 O16 C42 115.2(4) . . ? Mg2 O17 H17C 140.3 . . ? Mg2 O17 H17D 120.8 . . ? H17C O17 H17D 98.6 . . ? Mg2 O18 H18C 123.5 . . ? Mg2 O18 H18D 120.9 . . ? H18C O18 H18D 107.9 . . ? O3 C1 C2 120.4(6) . . ? O3 C1 C13 118.8(5) . . ? C2 C1 C13 120.8(6) . . ? C3 C2 C1 120.3(7) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 121.8(7) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 117.2(7) . . ? C3 C4 H4 121.4 . . ? C5 C4 H4 121.4 . . ? O1 C5 C13 121.3(5) . . ? O1 C5 C4 115.0(6) . . ? C13 C5 C4 123.7(6) . . ? O1 C6 C7 115.8(6) . . ? O1 C6 C11 121.8(4) . . ? C7 C6 C11 122.3(6) . . ? C8 C7 C6 118.2(6) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C7 C8 C9 123.1(6) . . ? C7 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C8 C9 C10 119.2(6) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? O7 C10 C9 123.4(5) . . ? O7 C10 C11 117.0(4) . . ? C9 C10 C11 119.6(5) . . ? C6 C11 C10 117.5(4) . . ? C6 C11 C12 120.1(5) . . ? C10 C11 C12 122.4(5) . . ? O2 C12 C11 123.2(4) . . ? O2 C12 C13 121.0(4) . . ? C11 C12 C13 115.9(5) . . ? C5 C13 C1 116.2(5) . . ? C5 C13 C12 119.6(5) . . ? C1 C13 C12 124.1(5) . . ? O3 C14 C15 110.4(4) . . ? O3 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? O3 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? O4 C15 C14 114.0(5) . . ? O4 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? O4 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? O4 C16 C17 107.7(6) . . ? O4 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? O4 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O5 C17 C16 106.3(5) . . ? O5 C17 H17A 110.5 . . ? C16 C17 H17A 110.5 . . ? O5 C17 H17B 110.5 . . ? C16 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? O5 C18 C19 106.0(6) . . ? O5 C18 H18A 110.5 . . ? C19 C18 H18A 110.5 . . ? O5 C18 H18B 110.5 . . ? C19 C18 H18B 110.5 . . ? H18A C18 H18B 108.7 . . ? O6 C19 C18 107.6(6) . . ? O6 C19 H19A 110.2 . . ? C18 C19 H19A 110.2 . . ? O6 C19 H19B 110.2 . . ? C18 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? O6 C20 C21 109.9(5) . . ? O6 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? O6 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O7 C21 C20 107.0(4) . . ? O7 C21 H21A 110.3 . . ? C20 C21 H21A 110.3 . . ? O7 C21 H21B 110.3 . . ? C20 C21 H21B 110.3 . . ? H21A C21 H21B 108.6 . . ? C23 C22 O12 123.0(5) . . ? C23 C22 C34 120.8(5) . . ? O12 C22 C34 116.1(5) . . ? C22 C23 C24 119.3(6) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 123.3(6) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 C26 117.5(6) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? O10 C26 C25 115.4(5) . . ? O10 C26 C34 122.4(5) . . ? C25 C26 C34 122.2(6) . . ? O10 C27 C28 115.4(5) . . ? O10 C27 C32 121.6(5) . . ? C28 C27 C32 123.0(5) . . ? C29 C28 C27 118.8(5) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 120.5(5) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.1(5) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 O16 118.2(5) . . ? C30 C31 C32 122.5(5) . . ? O16 C31 C32 119.2(4) . . ? C27 C32 C31 116.0(5) . . ? C27 C32 C33 118.9(5) . . ? C31 C32 C33 124.9(4) . . ? O11 C33 C32 120.7(4) . . ? O11 C33 C34 121.9(4) . . ? C32 C33 C34 117.4(4) . . ? C26 C34 C22 116.9(5) . . ? C26 C34 C33 118.4(5) . . ? C22 C34 C33 124.7(4) . . ? O12 C35 C36 106.1(5) . . ? O12 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? O12 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? O13 C36 C35 109.6(5) . . ? O13 C36 H36A 109.7 . . ? C35 C36 H36A 109.7 . . ? O13 C36 H36B 109.7 . . ? C35 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? O13 C37 C38 106.2(5) . . ? O13 C37 H37A 110.5 . . ? C38 C37 H37A 110.5 . . ? O13 C37 H37B 110.5 . . ? C38 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? O14 C38 C37 107.0(4) . . ? O14 C38 H38A 110.3 . . ? C37 C38 H38A 110.3 . . ? O14 C38 H38B 110.3 . . ? C37 C38 H38B 110.3 . . ? H38A C38 H38B 108.6 . . ? O14 C39 C40 106.8(4) . . ? O14 C39 H39A 110.4 . . ? C40 C39 H39A 110.4 . . ? O14 C39 H39B 110.4 . . ? C40 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? O15 C40 C39 106.9(5) . . ? O15 C40 H40A 110.4 . . ? C39 C40 H40A 110.4 . . ? O15 C40 H40B 110.4 . . ? C39 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? O15 C41 C42 113.5(4) . . ? O15 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? O15 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? O16 C42 C41 112.9(4) . . ? O16 C42 H42A 109.0 . . ? C41 C42 H42A 109.0 . . ? O16 C42 H42B 109.0 . . ? C41 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.894 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.071