# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chia-Her Lin' _publ_contact_author_email CHIAHER@CYCU.EDU.TW _publ_section_title ; Direct-Mixing Assembly of a Magnesium Coordination Molecule as Recyclable Water Adsorbent ; loop_ _publ_author_name 'Chia-Her Lin.' 'Hsin-Kuan Liu.' 'Tai-Hsing Tsao' 'Vitezslav Zima' data_1 _database_code_depnum_ccdc_archive 'CCDC 734422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H17 Mg O12' _chemical_formula_weight 293.50 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' Mg Mg 0.0486 0.0363 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7240(9) _cell_length_b 11.8927(19) _cell_length_c 16.302(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.894(10) _cell_angle_gamma 90.00 _cell_volume 1298.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1458 _cell_measurement_theta_min 2.508 _cell_measurement_theta_max 20.083 _exptl_crystal_description lamellar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9811 _exptl_absorpt_correction_T_max 0.9905 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21748 _diffrn_reflns_av_R_equivalents 0.1520 _diffrn_reflns_av_sigmaI/netI 0.1141 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.80 _reflns_number_total 3334 _reflns_number_gt 1602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2008)' _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^)+(0.0664P)^2^+1.0058P] 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 3334 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1568 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 0.74991(17) 0.35774(10) 0.22353(8) 0.0245(3) Uani 1 1 d . . . O1 O 0.6579(4) 0.22881(19) 0.14038(15) 0.0264(6) Uani 1 1 d . . . O2 O 1.0279(4) 0.3536(2) 0.18148(17) 0.0345(7) Uani 1 1 d . . . H10 H 1.0825 0.2909 0.1631 0.052 Uiso 1 1 d R . . H14 H 1.0929 0.4240 0.1717 0.052 Uiso 1 1 d R . . O3 O 0.4855(4) 0.3672(2) 0.27296(17) 0.0378(7) Uani 1 1 d . . . H17 H 0.4175 0.3160 0.2911 0.057 Uiso 1 1 d R . . H29 H 0.4170 0.4266 0.2818 0.057 Uiso 1 1 d R . . O4 O 0.8373(4) 0.2314(2) 0.31024(16) 0.0319(6) Uani 1 1 d . . . H16 H 0.8375 0.2126 0.3674 0.048 Uiso 1 1 d R . . H28 H 0.8139 0.1579 0.2918 0.048 Uiso 1 1 d R . . O5 O 0.6486(4) 0.4771(2) 0.13841(17) 0.0393(7) Uani 1 1 d . . . H3 H 0.5178 0.4711 0.1073 0.059 Uiso 1 1 d R . . H22 H 0.6702 0.5532 0.1519 0.059 Uiso 1 1 d R . . O6 O 0.8785(4) 0.4809(2) 0.30088(17) 0.0383(7) Uani 1 1 d . . . H6 H 0.8316 0.5425 0.3298 0.057 Uiso 1 1 d R . . H23 H 1.0239 0.4784 0.2798 0.057 Uiso 1 1 d R . . O7 O 0.7222(4) 0.0669(2) 0.20671(15) 0.0293(6) Uani 1 1 d . . . O8 O 0.2108(4) 0.1742(2) 0.12713(17) 0.0339(7) Uani 1 1 d . . . O9 O 0.2135(4) 0.2624(2) 0.00715(16) 0.0374(7) Uani 1 1 d . . . C1 C 0.6552(5) 0.1241(3) 0.1452(2) 0.0215(8) Uani 1 1 d . . . C2 C 0.5707(5) 0.0597(3) 0.0707(2) 0.0221(8) Uani 1 1 d . . . C3 C 0.3921(5) 0.0918(3) 0.0267(2) 0.0219(8) Uani 1 1 d . . . C4 C 0.2649(5) 0.1835(3) 0.0558(2) 0.0241(8) Uani 1 1 d . . . C5 C 0.6749(5) -0.0321(3) 0.0440(2) 0.0235(8) Uani 1 1 d . . . H2 H 0.7921 -0.0544 0.0740 0.028 Uiso 1 1 calc R . . O1W O 0.2664(4) 0.2058(2) 0.34670(17) 0.0368(7) Uani 1 1 d . . . H12 H 0.1283 0.2148 0.3232 0.055 Uiso 1 1 d R . . H21 H 0.2421 0.1997 0.4062 0.055 Uiso 1 1 d R . . O2W O 0.8008(4) 0.3001(3) -0.01904(17) 0.0443(8) Uani 1 1 d . . . H1 H 0.9368 0.2796 -0.0031 0.066 Uiso 1 1 d R . . H15 H 0.7300 0.2809 0.0308 0.066 Uiso 1 1 d R . . O3W O 0.2533(4) 0.4798(2) 0.07557(18) 0.0452(8) Uani 1 1 d . . . H18 H 0.2310 0.5491 0.0460 0.068 Uiso 1 1 d R . . H24 H 0.2699 0.4358 0.0336 0.068 Uiso 1 1 d 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 0.0255(6) 0.0199(6) 0.0277(7) -0.0032(5) 0.0002(5) 0.0006(5) O1 0.0334(14) 0.0161(12) 0.0287(14) -0.0021(11) -0.0025(11) -0.0021(11) O2 0.0293(15) 0.0260(14) 0.0492(18) -0.0065(13) 0.0100(12) 0.0008(11) O3 0.0315(15) 0.0261(15) 0.0576(19) -0.0007(14) 0.0152(13) 0.0043(11) O4 0.0383(15) 0.0281(15) 0.0276(14) -0.0016(12) -0.0062(12) -0.0012(12) O5 0.0434(16) 0.0269(15) 0.0458(18) 0.0056(14) -0.0068(13) -0.0006(13) O6 0.0332(15) 0.0332(15) 0.0490(18) -0.0203(14) 0.0067(13) -0.0030(12) O7 0.0362(15) 0.0238(13) 0.0262(15) 0.0000(11) -0.0066(11) -0.0002(11) O8 0.0461(16) 0.0253(14) 0.0324(15) 0.0006(12) 0.0152(13) 0.0053(12) O9 0.0529(18) 0.0288(15) 0.0304(15) 0.0038(13) 0.0036(13) 0.0164(13) C1 0.0177(17) 0.0223(19) 0.0241(19) -0.0042(15) -0.0008(14) -0.0004(14) C2 0.0225(18) 0.0148(16) 0.028(2) -0.0046(15) -0.0008(15) -0.0029(14) C3 0.0217(18) 0.0187(17) 0.0251(19) -0.0036(15) 0.0007(14) -0.0007(14) C4 0.0254(19) 0.0204(17) 0.026(2) -0.0012(16) -0.0025(16) 0.0022(15) C5 0.0238(18) 0.0197(18) 0.0258(19) -0.0036(15) -0.0039(14) 0.0039(14) O1W 0.0410(16) 0.0348(16) 0.0349(16) 0.0001(13) 0.0051(12) -0.0004(13) O2W 0.0478(18) 0.0507(19) 0.0347(17) 0.0079(15) 0.0048(13) 0.0053(15) O3W 0.0530(18) 0.0330(16) 0.0492(19) 0.0001(15) 0.0024(14) -0.0013(14) _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 2.017(3) . ? Mg1 O2 2.046(3) . ? Mg1 O5 2.060(3) . ? Mg1 O6 2.073(3) . ? Mg1 O1 2.104(3) . ? Mg1 O4 2.111(3) . ? O1 C1 1.249(4) . ? O2 H10 0.8934 . ? O2 H14 0.9640 . ? O3 H17 0.8311 . ? O3 H29 0.8616 . ? O4 H16 0.9581 . ? O4 H28 0.9335 . ? O5 H3 0.9802 . ? O5 H22 0.9400 . ? O6 H6 0.9399 . ? O6 H23 1.0641 . ? O7 C1 1.262(4) . ? O8 C4 1.253(4) . ? O9 C4 1.258(4) . ? C1 C2 1.505(5) . ? C2 C5 1.387(5) . ? C2 C3 1.398(4) . ? C3 C5 1.395(5) 3_655 ? C3 C4 1.488(5) . ? C5 C3 1.395(5) 3_655 ? C5 H2 0.9300 . ? O1W H12 0.9800 . ? O1W H21 1.0002 . ? O2W H1 0.9607 . ? O2W H15 1.0019 . ? O3W H18 0.9602 . ? O3W H24 0.8753 . ? 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 O2 175.63(13) . . ? O3 Mg1 O5 88.77(12) . . ? O2 Mg1 O5 92.87(12) . . ? O3 Mg1 O6 93.08(12) . . ? O2 Mg1 O6 82.84(11) . . ? O5 Mg1 O6 91.11(12) . . ? O3 Mg1 O1 94.43(11) . . ? O2 Mg1 O1 89.62(11) . . ? O5 Mg1 O1 90.35(11) . . ? O6 Mg1 O1 172.38(12) . . ? O3 Mg1 O4 88.67(11) . . ? O2 Mg1 O4 89.83(11) . . ? O5 Mg1 O4 176.75(12) . . ? O6 Mg1 O4 91.02(11) . . ? O1 Mg1 O4 87.86(10) . . ? C1 O1 Mg1 133.8(2) . . ? Mg1 O2 H10 123.1 . . ? Mg1 O2 H14 118.3 . . ? H10 O2 H14 117.6 . . ? Mg1 O3 H17 129.2 . . ? Mg1 O3 H29 127.9 . . ? H17 O3 H29 102.9 . . ? Mg1 O4 H16 142.6 . . ? Mg1 O4 H28 114.9 . . ? H16 O4 H28 94.6 . . ? Mg1 O5 H3 121.9 . . ? Mg1 O5 H22 118.1 . . ? H3 O5 H22 107.8 . . ? Mg1 O6 H6 135.6 . . ? Mg1 O6 H23 97.5 . . ? H6 O6 H23 122.8 . . ? O1 C1 O7 125.5(3) . . ? O1 C1 C2 117.6(3) . . ? O7 C1 C2 116.9(3) . . ? C5 C2 C3 119.2(3) . . ? C5 C2 C1 119.1(3) . . ? C3 C2 C1 121.6(3) . . ? C5 C3 C2 119.2(3) 3_655 . ? C5 C3 C4 118.8(3) 3_655 . ? C2 C3 C4 121.9(3) . . ? O8 C4 O9 124.4(3) . . ? O8 C4 C3 116.9(3) . . ? O9 C4 C3 118.7(3) . . ? C2 C5 C3 121.5(3) . 3_655 ? C2 C5 H2 119.2 . . ? C3 C5 H2 119.2 3_655 . ? H12 O1W H21 99.1 . . ? H1 O2W H15 103.3 . . ? H18 O3W H24 98.5 . . ? 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 O1 C1 -86.8(3) . . . . ? O2 Mg1 O1 C1 91.6(3) . . . . ? O5 Mg1 O1 C1 -175.6(3) . . . . ? O6 Mg1 O1 C1 83.4(10) . . . . ? O4 Mg1 O1 C1 1.7(3) . . . . ? Mg1 O1 C1 O7 -3.4(5) . . . . ? Mg1 O1 C1 C2 178.4(2) . . . . ? O1 C1 C2 C5 133.2(3) . . . . ? O7 C1 C2 C5 -45.1(5) . . . . ? O1 C1 C2 C3 -45.4(5) . . . . ? O7 C1 C2 C3 136.3(3) . . . . ? C5 C2 C3 C5 -1.4(6) . . . 3_655 ? C1 C2 C3 C5 177.2(3) . . . 3_655 ? C5 C2 C3 C4 175.0(3) . . . . ? C1 C2 C3 C4 -6.5(5) . . . . ? C5 C3 C4 O8 121.3(4) 3_655 . . . ? C2 C3 C4 O8 -55.1(5) . . . . ? C5 C3 C4 O9 -56.4(5) 3_655 . . . ? C2 C3 C4 O9 127.2(4) . . . . ? C3 C2 C5 C3 1.5(6) . . . 3_655 ? C1 C2 C5 C3 -177.2(3) . . . 3_655 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.368 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.084 data_2 _database_code_depnum_ccdc_archive 'CCDC 734431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 Mg2 O19' _chemical_formula_weight 496.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3927(7) _cell_length_b 10.1933(6) _cell_length_c 11.1398(7) _cell_angle_alpha 87.557(4) _cell_angle_beta 77.136(3) _cell_angle_gamma 69.927(4) _cell_volume 975.96(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3005 _cell_measurement_theta_min 2.389 _cell_measurement_theta_max 25.330 _exptl_crystal_description acicular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9448 _exptl_absorpt_correction_T_max 0.9847 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17211 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.39 _reflns_number_total 4760 _reflns_number_gt 2893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2008)' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2008)' _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^)+(0.0505P)^2^+0.4273P] 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 4760 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.30764(9) 0.76121(8) 0.75311(7) 0.0178(2) Uani 1 1 d . . . Mg2 Mg 0.37516(10) 0.79134(9) 1.26185(8) 0.0209(2) Uani 1 1 d . . . O1 O 0.53222(19) 0.65120(17) 0.66323(16) 0.0214(4) Uani 1 1 d . . . O2 O 0.0852(2) 0.87114(18) 0.84899(17) 0.0261(4) Uani 1 1 d . . . O3 O 0.21501(19) 0.66380(18) 0.64578(16) 0.0233(4) Uani 1 1 d . . . O4 O 0.3864(2) 0.87707(18) 0.86645(17) 0.0256(4) Uani 1 1 d . . . O5 O 0.3408(2) 0.60863(18) 0.88281(16) 0.0303(5) Uani 1 1 d . . . O6 O 0.3177(2) 0.90846(19) 0.62484(17) 0.0310(5) Uani 1 1 d . . . O7 O 0.60056(19) 0.67480(17) 1.16845(16) 0.0213(4) Uani 1 1 d . . . O8 O 0.4577(2) 0.90674(18) 1.35870(18) 0.0298(4) Uani 1 1 d . . . O9 O 0.1592(2) 0.8993(2) 1.36419(19) 0.0365(5) Uani 1 1 d . . . O10 O 0.2845(2) 0.69208(18) 1.15425(18) 0.0293(4) Uani 1 1 d . . . O11 O 0.3980(2) 0.63757(19) 1.39455(17) 0.0345(5) Uani 1 1 d . . . O12 O 0.3412(3) 0.9463(2) 1.12963(18) 0.0428(6) Uani 1 1 d . . . O13 O -0.0371(2) 0.7923(2) 0.69274(19) 0.0385(5) Uani 1 1 d . . . O14 O 0.1165(2) 0.12684(19) 0.5470(2) 0.0390(5) Uani 1 1 d . . . O15 O 0.3281(2) 0.17069(18) 0.45296(18) 0.0280(4) Uani 1 1 d . . . O16 O 0.7368(2) 0.8091(2) 1.19216(19) 0.0368(5) Uani 1 1 d . . . O17 O 0.7151(2) 0.56679(19) 0.8122(2) 0.0377(5) Uani 1 1 d . . . O18 O 0.6727(2) 0.76991(18) 0.90511(17) 0.0276(4) Uani 1 1 d . . . C1 C 0.0753(3) 0.6930(2) 0.6374(2) 0.0200(5) Uani 1 1 d . . . C2 C 0.0399(3) 0.5958(2) 0.5595(2) 0.0157(5) Uani 1 1 d . . . C3 C 0.1290(3) 0.4548(2) 0.5508(2) 0.0162(5) Uani 1 1 d . . . C4 C 0.0890(3) 0.3588(2) 0.4931(2) 0.0165(5) Uani 1 1 d . . . C5 C 0.1851(3) 0.2071(2) 0.4968(2) 0.0198(5) Uani 1 1 d . . . C6 C 0.7236(3) 0.7045(3) 1.1475(2) 0.0203(5) Uani 1 1 d . . . C7 C 0.8676(3) 0.6016(2) 1.0680(2) 0.0169(5) Uani 1 1 d . . . C8 C 0.9933(3) 0.5333(3) 1.1198(2) 0.0186(5) Uani 1 1 d . . . C9 C 0.8747(3) 0.5691(2) 0.9461(2) 0.0159(5) Uani 1 1 d . . . C10 C 0.7433(3) 0.6427(3) 0.8838(2) 0.0207(5) Uani 1 1 d . . . O1W O -0.0090(2) 1.14955(19) 0.89768(17) 0.0286(4) Uani 1 1 d . . . H1 H 0.2197 0.4231 0.5918 0.050 Uiso 1 1 d . . . H2 H 0.0878 1.1649 0.8658 0.050 Uiso 1 1 d . . . H3 H 0.9960 0.5438 1.2049 0.050 Uiso 1 1 d . . . H4 H 0.2392 0.9736 0.6104 0.050 Uiso 1 1 d . . . H5 H 0.2794 0.6124 1.1664 0.050 Uiso 1 1 d . . . H6 H 0.0745 0.8863 1.4030 0.050 Uiso 1 1 d . . . H7 H 0.4267 0.5455 1.3778 0.050 Uiso 1 1 d . . . H8 H 0.3664 0.9665 0.8409 0.050 Uiso 1 1 d . . . H9 H 0.6030 0.6197 0.7008 0.050 Uiso 1 1 d . . . H10 H 0.5861 0.6984 0.6151 0.050 Uiso 1 1 d . . . H11 H 0.4096 0.9926 1.3900 0.050 Uiso 1 1 d . . . H12 H 0.0337 0.8526 0.7988 0.050 Uiso 1 1 d . . . H13 H 0.4938 0.8215 0.8622 0.050 Uiso 1 1 d . . . H14 H 0.1877 0.7526 1.1525 0.050 Uiso 1 1 d . . . H15 H 0.3630 0.5159 0.8669 0.050 Uiso 1 1 d . . . H16 H 0.3115 1.0435 1.1378 0.050 Uiso 1 1 d . . . H17 H 0.3493 0.6517 1.4837 0.050 Uiso 1 1 d . . . H18 H 0.3495 0.6237 0.9609 0.050 Uiso 1 1 d . . . H19 H 0.1336 0.9941 1.3736 0.050 Uiso 1 1 d . . . H20 H 0.5609 0.8825 1.3296 0.050 Uiso 1 1 d . . . H21 H 0.3761 0.8876 0.5601 0.050 Uiso 1 1 d . . . H22 H 0.3369 0.9436 1.0567 0.050 Uiso 1 1 d . . . H23 H 0.0426 0.9706 0.8549 0.050 Uiso 1 1 d . . . H24 H -0.0362 1.1848 0.9895 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0161(4) 0.0177(4) 0.0200(4) -0.0006(3) -0.0060(3) -0.0050(4) Mg2 0.0161(4) 0.0187(4) 0.0260(5) -0.0042(4) -0.0019(4) -0.0048(4) O1 0.0157(9) 0.0220(9) 0.0270(10) 0.0033(8) -0.0073(7) -0.0058(8) O2 0.0199(10) 0.0245(10) 0.0327(10) -0.0116(8) -0.0070(8) -0.0039(8) O3 0.0162(9) 0.0247(9) 0.0307(10) -0.0069(8) -0.0075(8) -0.0068(8) O4 0.0237(10) 0.0201(9) 0.0349(11) 0.0008(8) -0.0131(8) -0.0055(8) O5 0.0421(12) 0.0223(10) 0.0254(10) 0.0052(8) -0.0067(9) -0.0105(9) O6 0.0259(11) 0.0285(10) 0.0323(11) 0.0105(9) -0.0057(9) -0.0031(9) O7 0.0134(9) 0.0195(9) 0.0283(10) -0.0041(8) -0.0003(7) -0.0046(7) O8 0.0182(10) 0.0256(10) 0.0423(11) -0.0140(9) -0.0006(8) -0.0054(8) O9 0.0192(10) 0.0289(10) 0.0548(13) -0.0127(10) 0.0073(9) -0.0081(9) O10 0.0266(11) 0.0191(9) 0.0443(12) 0.0000(8) -0.0149(9) -0.0060(8) O11 0.0453(13) 0.0235(10) 0.0277(11) -0.0015(8) 0.0002(9) -0.0080(9) O12 0.0697(17) 0.0235(10) 0.0349(12) 0.0041(9) -0.0122(11) -0.0155(11) O13 0.0218(11) 0.0351(11) 0.0541(13) -0.0268(10) -0.0116(10) 0.0011(9) O14 0.0194(10) 0.0200(10) 0.0743(15) 0.0170(10) -0.0054(10) -0.0073(8) O15 0.0142(9) 0.0170(9) 0.0473(12) 0.0011(8) -0.0002(8) -0.0028(7) O16 0.0220(10) 0.0334(11) 0.0523(13) -0.0237(10) 0.0039(9) -0.0106(9) O17 0.0420(13) 0.0235(10) 0.0570(14) 0.0023(10) -0.0378(11) -0.0061(9) O18 0.0219(10) 0.0185(9) 0.0403(11) -0.0001(8) -0.0134(8) -0.0001(8) C1 0.0206(13) 0.0173(12) 0.0234(13) -0.0029(11) -0.0083(11) -0.0057(11) C2 0.0142(12) 0.0150(11) 0.0183(12) -0.0008(10) -0.0035(10) -0.0054(10) C3 0.0135(12) 0.0165(12) 0.0188(12) -0.0003(10) -0.0053(10) -0.0041(10) C4 0.0130(12) 0.0157(12) 0.0189(12) -0.0008(10) -0.0019(10) -0.0035(10) C5 0.0179(13) 0.0146(12) 0.0273(14) 0.0001(10) -0.0055(11) -0.0057(10) C6 0.0167(13) 0.0181(12) 0.0226(13) -0.0020(11) -0.0041(10) -0.0015(10) C7 0.0115(12) 0.0165(12) 0.0212(13) 0.0001(10) -0.0021(9) -0.0040(10) C8 0.0186(13) 0.0202(12) 0.0171(12) -0.0004(10) -0.0043(10) -0.0064(10) C9 0.0132(12) 0.0153(12) 0.0203(13) 0.0030(10) -0.0069(10) -0.0045(10) C10 0.0166(13) 0.0207(13) 0.0257(14) 0.0020(11) -0.0085(11) -0.0050(11) O1W 0.0220(10) 0.0289(10) 0.0347(11) -0.0029(9) -0.0053(8) -0.0088(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O6 2.0392(19) . ? Mg1 O1 2.0595(19) . ? Mg1 O5 2.0687(19) . ? Mg1 O2 2.0650(19) . ? Mg1 O3 2.0808(18) . ? Mg1 O4 2.1631(19) . ? Mg1 H12 2.3578 . ? Mg2 O9 2.042(2) . ? Mg2 O8 2.0628(19) . ? Mg2 O10 2.0818(19) . ? Mg2 O7 2.0914(18) . ? Mg2 O11 2.098(2) . ? Mg2 O12 2.105(2) . ? O1 H9 0.8283 . ? O1 H10 0.8941 . ? O2 H12 0.8797 . ? O2 H23 0.9528 . ? O3 C1 1.266(3) . ? O4 H8 0.9118 . ? O4 H13 0.9640 . ? O5 H15 0.9116 . ? O5 H18 0.9157 . ? O6 H4 0.8475 . ? O6 H21 0.7893 . ? O7 C6 1.263(3) . ? O8 H11 0.8809 . ? O8 H20 0.8992 . ? O9 H6 0.8671 . ? O9 H19 0.9168 . ? O10 H5 0.8336 . ? O10 H14 0.9110 . ? O11 H7 0.8984 . ? O11 H17 0.9904 . ? O12 H16 0.9354 . ? O12 H22 0.8246 . ? O13 C1 1.245(3) . ? O14 C5 1.248(3) . ? O15 C5 1.250(3) . ? O16 C6 1.250(3) . ? O17 C10 1.263(3) . ? O18 C10 1.242(3) . ? C1 C2 1.508(3) . ? C2 C3 1.388(3) . ? C2 C4 1.390(3) 2_566 ? C3 C4 1.388(3) . ? C3 H1 1.0051 . ? C4 C2 1.390(3) 2_566 ? C4 C5 1.504(3) . ? C6 C7 1.512(3) . ? C7 C8 1.384(3) . ? C7 C9 1.393(3) . ? C8 C9 1.392(3) 2_767 ? C8 H3 0.9655 . ? C9 C8 1.392(3) 2_767 ? C9 C10 1.506(3) . ? O1W H2 0.9622 . ? O1W H24 1.0452 . ? 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 O6 Mg1 O1 85.77(8) . . ? O6 Mg1 O5 169.00(9) . . ? O1 Mg1 O5 85.76(8) . . ? O6 Mg1 O2 95.38(8) . . ? O1 Mg1 O2 177.96(8) . . ? O5 Mg1 O2 92.89(8) . . ? O6 Mg1 O3 91.47(8) . . ? O1 Mg1 O3 92.36(7) . . ? O5 Mg1 O3 95.88(8) . . ? O2 Mg1 O3 89.29(7) . . ? O6 Mg1 O4 86.64(8) . . ? O1 Mg1 O4 91.80(7) . . ? O5 Mg1 O4 86.62(8) . . ? O2 Mg1 O4 86.59(7) . . ? O3 Mg1 O4 175.29(8) . . ? O6 Mg1 H12 90.7 . . ? O1 Mg1 H12 160.2 . . ? O5 Mg1 H12 99.6 . . ? O2 Mg1 H12 21.7 . . ? O3 Mg1 H12 68.2 . . ? O4 Mg1 H12 107.5 . . ? O9 Mg2 O8 86.69(8) . . ? O9 Mg2 O10 92.03(8) . . ? O8 Mg2 O10 174.43(9) . . ? O9 Mg2 O7 175.99(9) . . ? O8 Mg2 O7 91.57(7) . . ? O10 Mg2 O7 90.05(8) . . ? O9 Mg2 O11 88.96(9) . . ? O8 Mg2 O11 91.38(8) . . ? O10 Mg2 O11 94.02(8) . . ? O7 Mg2 O11 87.48(8) . . ? O9 Mg2 O12 88.97(9) . . ? O8 Mg2 O12 90.25(9) . . ? O10 Mg2 O12 84.30(8) . . ? O7 Mg2 O12 94.65(8) . . ? O11 Mg2 O12 177.28(10) . . ? Mg1 O1 H9 121.7 . . ? Mg1 O1 H10 117.8 . . ? H9 O1 H10 90.4 . . ? Mg1 O2 H12 98.2 . . ? Mg1 O2 H23 123.4 . . ? H12 O2 H23 101.0 . . ? C1 O3 Mg1 129.37(16) . . ? Mg1 O4 H8 109.8 . . ? Mg1 O4 H13 104.6 . . ? H8 O4 H13 116.9 . . ? Mg1 O5 H15 124.8 . . ? Mg1 O5 H18 123.8 . . ? H15 O5 H18 110.8 . . ? Mg1 O6 H4 124.5 . . ? Mg1 O6 H21 120.5 . . ? H4 O6 H21 104.8 . . ? C6 O7 Mg2 130.02(16) . . ? Mg2 O8 H11 127.9 . . ? Mg2 O8 H20 108.4 . . ? H11 O8 H20 115.9 . . ? Mg2 O9 H6 140.7 . . ? Mg2 O9 H19 117.0 . . ? H6 O9 H19 102.3 . . ? Mg2 O10 H5 124.3 . . ? Mg2 O10 H14 106.1 . . ? H5 O10 H14 108.4 . . ? Mg2 O11 H7 124.7 . . ? Mg2 O11 H17 126.7 . . ? H7 O11 H17 106.0 . . ? Mg2 O12 H16 130.9 . . ? Mg2 O12 H22 132.2 . . ? H16 O12 H22 96.4 . . ? O13 C1 O3 125.4(2) . . ? O13 C1 C2 116.8(2) . . ? O3 C1 C2 117.7(2) . . ? C3 C2 C4 119.2(2) . 2_566 ? C3 C2 C1 118.9(2) . . ? C4 C2 C1 121.6(2) 2_566 . ? C2 C3 C4 120.9(2) . . ? C2 C3 H1 118.2 . . ? C4 C3 H1 120.7 . . ? C3 C4 C2 119.9(2) . 2_566 ? C3 C4 C5 117.1(2) . . ? C2 C4 C5 122.9(2) 2_566 . ? O14 C5 O15 124.5(2) . . ? O14 C5 C4 117.4(2) . . ? O15 C5 C4 118.0(2) . . ? O16 C6 O7 124.9(2) . . ? O16 C6 C7 117.7(2) . . ? O7 C6 C7 117.3(2) . . ? C8 C7 C9 119.2(2) . . ? C8 C7 C6 118.8(2) . . ? C9 C7 C6 121.9(2) . . ? C7 C8 C9 121.6(2) . 2_767 ? C7 C8 H3 125.0 . . ? C9 C8 H3 113.1 2_767 . ? C8 C9 C7 119.2(2) 2_767 . ? C8 C9 C10 119.3(2) 2_767 . ? C7 C9 C10 121.6(2) . . ? O18 C10 O17 125.3(2) . . ? O18 C10 C9 119.2(2) . . ? O17 C10 C9 115.5(2) . . ? H2 O1W H24 102.2 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.307 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.069