# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email yyw_9@163.com _publ_contact_author_name 'Yanyan Wang' loop_ _publ_author_name 'Yanyan Wang' 'Lang Shao' 'Yi Li' 'Xu Li' 'Jiyang Li' 'Jihong Yu' 'Ruren Xu' data_MgAPO-CJ67(a) _database_code_depnum_ccdc_archive 'CCDC 839155' #TrackingRef 'web_deposit_cif_file_0_YanyanWang_1313313008.MgAPO-CJ67(a).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H4.67 Al1.17 Mg0.33 N0.33 O6 P1.50' _chemical_formula_weight 215.43 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.2385(5) _cell_length_b 13.2385(5) _cell_length_c 46.3808(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7039.6(5) _cell_formula_units_Z 36 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1884 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3912 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9189 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_reflns_number 14411 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.88 _reflns_number_total 1884 _reflns_number_gt 1474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART Apex 2' _computing_cell_refinement 'Bruker SMART Apex 2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.1133P)^2^+17.4881P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1884 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1674 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.004 _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 P1 P 0.90809(7) 0.3333 0.0833 0.0221(3) Uani 1 2 d S . . P2 P 0.75777(6) -0.00559(5) 0.033628(14) 0.0237(3) Uani 1 1 d . . . Al1 Al 0.99443(6) 0.23291(7) 0.033478(16) 0.0222(3) Uani 0.78 1 d P . . Mg1 Mg 0.99443(6) 0.23291(7) 0.033478(16) 0.0222(3) Uani 0.22 1 d P . . Al2 Al 0.6667 0.08948(7) 0.0833 0.0175(3) Uani 0.78 2 d SP . . Mg2 Mg 0.6667 0.08948(7) 0.0833 0.0175(3) Uani 0.22 2 d SP . . O1 O 0.9677(2) 0.3218(2) 0.05647(5) 0.0464(6) Uani 1 1 d . . . O2 O 0.8958(2) 0.4393(2) 0.07955(6) 0.0497(7) Uani 1 1 d . . . O3 O 0.7435(3) -0.12285(18) 0.04178(6) 0.0473(7) Uani 1 1 d . . . O4 O 0.88459(19) 0.08592(19) 0.03766(5) 0.0422(6) Uani 1 1 d . . . O5 O 0.7193(2) -0.00748(18) 0.00269(4) 0.0414(6) Uani 1 1 d . . . O6 O 0.6797(2) 0.0188(2) 0.05240(5) 0.0481(6) Uani 1 1 d . . . N1 N 0.3333 -0.3333 0.0355(5) 0.184(7) Uiso 1 3 d S . . C2 C 0.3860(11) -0.2195(15) 0.0254(4) 0.139(5) Uiso 0.67 1 d P . . C3 C 0.3876(17) -0.224(2) -0.0040(6) 0.212(9) Uiso 0.67 1 d P . . C4 C 0.293(3) -0.289(3) -0.0201(9) 0.175(14) Uiso 0.33 1 d P . . C5 C 0.386(3) -0.306(4) 0.0659(7) 0.173(16) Uiso 0.33 1 d P . . 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 P1 0.0212(4) 0.0193(5) 0.0252(5) -0.0057(3) -0.00283(15) 0.0096(2) P2 0.0310(4) 0.0175(4) 0.0204(4) -0.0011(2) 0.0056(2) 0.0105(3) Al1 0.0211(4) 0.0289(5) 0.0184(5) -0.0018(3) 0.0019(3) 0.0139(3) Mg1 0.0211(4) 0.0289(5) 0.0184(5) -0.0018(3) 0.0019(3) 0.0139(3) Al2 0.0162(5) 0.0161(4) 0.0203(6) 0.00209(17) 0.0042(3) 0.0081(3) Mg2 0.0162(5) 0.0161(4) 0.0203(6) 0.00209(17) 0.0042(3) 0.0081(3) O1 0.0484(14) 0.0525(14) 0.0411(13) -0.0075(10) 0.0081(10) 0.0273(12) O2 0.0662(19) 0.0364(12) 0.0588(17) -0.0094(10) -0.0158(14) 0.0349(12) O3 0.0772(19) 0.0255(10) 0.0422(13) 0.0064(9) 0.0143(13) 0.0280(11) O4 0.0350(11) 0.0304(11) 0.0485(13) -0.0004(9) -0.0019(9) 0.0069(9) O5 0.0479(13) 0.0501(14) 0.0256(11) -0.0030(9) -0.0021(9) 0.0240(10) O6 0.0495(14) 0.0508(14) 0.0458(13) -0.0135(10) 0.0122(10) 0.0264(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2 1.502(2) 17_554 ? P1 O2 1.502(2) . ? P1 O1 1.522(2) 17_554 ? P1 O1 1.522(2) . ? P1 Mg1 3.1528(9) 17_554 ? P2 O6 1.505(2) . ? P2 O4 1.512(2) . ? P2 O3 1.5148(19) . ? P2 O5 1.519(2) . ? P2 Mg1 3.1128(11) 21_545 ? P2 Mg1 3.1466(10) 2_645 ? Al1 O1 1.751(2) . ? Al1 O3 1.751(2) 3_765 ? Al1 O4 1.763(2) . ? Al1 O5 1.764(2) 20_665 ? Al2 O2 1.744(2) 17_554 ? Al2 O2 1.744(2) 3_665 ? Al2 O6 1.767(2) 18_654 ? Al2 O6 1.768(2) . ? O2 Mg2 1.744(2) 2_655 ? O2 Al2 1.744(2) 2_655 ? O3 Mg1 1.751(2) 2_645 ? O3 Al1 1.751(2) 2_645 ? O5 Mg1 1.764(2) 21_545 ? O5 Al1 1.764(2) 21_545 ? N1 C2 1.388(17) . ? N1 C2 1.389(17) 2_545 ? N1 C2 1.389(17) 3_655 ? N1 C5 1.53(3) . ? N1 C5 1.53(3) 2_545 ? N1 C5 1.53(3) 3_655 ? C2 C3 1.36(2) . ? C3 C4 1.34(3) . ? C3 C4 1.39(3) 3_655 ? C4 C3 1.39(3) 2_545 ? C4 C4 1.67(7) 3_655 ? C4 C4 1.67(7) 2_545 ? C5 C5 1.05(6) 3_655 ? C5 C5 1.05(6) 2_545 ? 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 P1 O2 109.7(2) 17_554 . ? O2 P1 O1 107.58(14) 17_554 17_554 ? O2 P1 O1 110.65(14) . 17_554 ? O2 P1 O1 110.63(14) 17_554 . ? O2 P1 O1 107.57(14) . . ? O1 P1 O1 110.7(2) 17_554 . ? O2 P1 Mg1 122.69(11) 17_554 17_554 ? O2 P1 Mg1 96.92(10) . 17_554 ? O1 P1 Mg1 16.73(10) 17_554 17_554 ? O1 P1 Mg1 107.82(10) . 17_554 ? O6 P2 O4 111.28(14) . . ? O6 P2 O3 109.19(15) . . ? O4 P2 O3 108.05(15) . . ? O6 P2 O5 106.84(15) . . ? O4 P2 O5 111.02(13) . . ? O3 P2 O5 110.47(14) . . ? O6 P2 Mg1 126.22(11) . 21_545 ? O4 P2 Mg1 96.45(10) . 21_545 ? O3 P2 Mg1 104.09(10) . 21_545 ? O5 P2 Mg1 20.00(10) . 21_545 ? O6 P2 Mg1 125.41(10) . 2_645 ? O4 P2 Mg1 102.33(10) . 2_645 ? O3 P2 Mg1 16.76(10) . 2_645 ? O5 P2 Mg1 99.13(9) . 2_645 ? Mg1 P2 Mg1 89.40(2) 21_545 2_645 ? O1 Al1 O3 107.15(12) . 3_765 ? O1 Al1 O4 110.02(12) . . ? O3 Al1 O4 112.73(13) 3_765 . ? O1 Al1 O5 109.75(13) . 20_665 ? O3 Al1 O5 109.14(12) 3_765 20_665 ? O4 Al1 O5 108.03(12) . 20_665 ? O2 Al2 O2 109.2(2) 17_554 3_665 ? O2 Al2 O6 108.75(12) 17_554 18_654 ? O2 Al2 O6 110.38(12) 3_665 18_654 ? O2 Al2 O6 110.36(12) 17_554 . ? O2 Al2 O6 108.73(12) 3_665 . ? O6 Al2 O6 109.39(18) 18_654 . ? P1 O1 Al1 148.77(17) . . ? P1 O2 Mg2 163.34(19) . 2_655 ? P1 O2 Al2 163.34(19) . 2_655 ? Mg2 O2 Al2 0.00(5) 2_655 2_655 ? P2 O3 Mg1 148.81(18) . 2_645 ? P2 O3 Al1 148.81(18) . 2_645 ? Mg1 O3 Al1 0.00(6) 2_645 2_645 ? P2 O4 Al1 147.46(18) . . ? P2 O5 Mg1 142.87(18) . 21_545 ? P2 O5 Al1 142.87(18) . 21_545 ? Mg1 O5 Al1 0.00(5) 21_545 21_545 ? P2 O6 Al2 147.38(17) . . ? C2 N1 C2 109.2(13) . 2_545 ? C2 N1 C2 109.2(13) . 3_655 ? C2 N1 C2 109.2(13) 2_545 3_655 ? C2 N1 C5 97.5(19) . . ? C2 N1 C5 133(2) 2_545 . ? C2 N1 C5 96.9(19) 3_655 . ? C2 N1 C5 96.9(19) . 2_545 ? C2 N1 C5 97.6(19) 2_545 2_545 ? C2 N1 C5 133(2) 3_655 2_545 ? C5 N1 C5 40(2) . 2_545 ? C2 N1 C5 133(2) . 3_655 ? C2 N1 C5 96.9(19) 2_545 3_655 ? C2 N1 C5 97.6(19) 3_655 3_655 ? C5 N1 C5 40(2) . 3_655 ? C5 N1 C5 40(2) 2_545 3_655 ? C3 C2 N1 107.6(18) . . ? C4 C3 C2 124(2) . . ? C4 C3 C4 76(4) . 3_655 ? C2 C3 C4 126(2) . 3_655 ? C3 C4 C3 106(4) . 2_545 ? C3 C4 C4 53(2) . 3_655 ? C3 C4 C4 100(2) 2_545 3_655 ? C3 C4 C4 102(2) . 2_545 ? C3 C4 C4 51(2) 2_545 2_545 ? C4 C4 C4 59.998(2) 3_655 2_545 ? C5 C5 C5 59.999(7) 3_655 2_545 ? C5 C5 N1 70.0(11) 3_655 . ? C5 C5 N1 70.0(11) 2_545 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.010 _refine_diff_density_min -1.486 _refine_diff_density_rms 0.123 # Attachment 'web_deposit_cif_file_1_YanyanWang_1313313008.MgAPO-CJ67(b).cif' data_MgAPO-CJ67(b) _database_code_depnum_ccdc_archive 'CCDC 839156' #TrackingRef 'web_deposit_cif_file_1_YanyanWang_1313313008.MgAPO-CJ67(b).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al1.07 Mg0.43 O6 P1.50' _chemical_formula_weight 181.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.2577(4) _cell_length_b 13.2577(4) _cell_length_c 45.677(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6952.9(6) _cell_formula_units_Z 36 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3225 _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6724 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16193 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1933 _reflns_number_gt 1537 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+24.9082P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1933 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 P1 P 0.75902(6) -0.00576(5) 0.034338(15) 0.0375(2) Uani 1 1 d . . . P2 P 0.90599(6) 0.3333 0.0833 0.0297(3) Uani 1 2 d S . . Al1 Al 0.99438(7) 0.23139(7) 0.034128(18) 0.0358(3) Uani 0.71 1 d P . . Mg1 Mg 0.99438(7) 0.23139(7) 0.034128(18) 0.0358(3) Uani 0.29 1 d P . . Al2 Al 0.6667 0.09146(7) 0.0833 0.0251(3) Uani 0.71 2 d SP . . Mg2 Mg 0.6667 0.09146(7) 0.0833 0.0251(3) Uani 0.29 2 d SP . . O1 O 0.9643(2) 0.3211(2) 0.05628(5) 0.0638(7) Uani 1 1 d . . . O2 O 0.8932(2) 0.43845(19) 0.07909(6) 0.0656(8) Uani 1 1 d . . . O3 O 0.7429(3) -0.12296(18) 0.04315(6) 0.0631(7) Uani 1 1 d . . . O4 O 0.8851(2) 0.0849(2) 0.03913(6) 0.0626(7) Uani 1 1 d . . . O5 O 0.7232(2) -0.00733(19) 0.00280(5) 0.0581(6) Uani 1 1 d . . . O6 O 0.6802(2) 0.0211(2) 0.05254(5) 0.0653(7) 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 P1 0.0490(4) 0.0258(3) 0.0336(4) -0.0029(2) 0.0088(3) 0.0156(3) P2 0.0256(3) 0.0236(4) 0.0392(5) -0.0070(3) -0.00350(16) 0.0118(2) Al1 0.0309(4) 0.0449(5) 0.0328(5) -0.0033(3) 0.0047(3) 0.0198(4) Mg1 0.0309(4) 0.0449(5) 0.0328(5) -0.0033(3) 0.0047(3) 0.0198(4) Al2 0.0216(5) 0.0206(4) 0.0336(6) 0.00265(18) 0.0053(4) 0.0108(2) Mg2 0.0216(5) 0.0206(4) 0.0336(6) 0.00265(18) 0.0053(4) 0.0108(2) O1 0.0651(15) 0.0629(15) 0.0634(15) -0.0047(11) 0.0228(12) 0.0320(13) O2 0.0731(18) 0.0370(11) 0.097(2) -0.0142(12) -0.0241(15) 0.0353(12) O3 0.099(2) 0.0351(11) 0.0574(14) 0.0074(10) 0.0211(14) 0.0346(12) O4 0.0517(13) 0.0427(12) 0.0814(18) -0.0027(11) -0.0012(12) 0.0146(11) O5 0.0689(16) 0.0582(15) 0.0414(12) -0.0014(10) 0.0022(10) 0.0274(12) O6 0.0693(16) 0.0663(15) 0.0620(15) -0.0204(12) 0.0144(12) 0.0353(13) _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 P1 O4 1.509(2) . ? P1 O6 1.511(2) . ? P1 O3 1.513(2) . ? P1 O5 1.514(2) . ? P1 Mg1 3.1277(12) 21_545 ? P1 Mg1 3.1314(10) 2_645 ? P2 O2 1.498(2) 17_554 ? P2 O2 1.498(2) . ? P2 O1 1.508(2) 17_554 ? P2 O1 1.508(2) . ? P2 Mg1 3.1361(9) 17_554 ? P2 Mg2 3.1899(7) 2_655 ? Al1 O1 1.753(2) . ? Al1 O3 1.757(2) 3_765 ? Al1 O5 1.764(2) 20_665 ? Al1 O4 1.764(2) . ? Al2 O2 1.731(2) 17_554 ? Al2 O2 1.731(2) 3_665 ? Al2 O6 1.746(2) 18_654 ? Al2 O6 1.746(2) . ? O2 Mg2 1.731(2) 2_655 ? O2 Al2 1.731(2) 2_655 ? O3 Mg1 1.757(2) 2_645 ? O3 Al1 1.757(2) 2_645 ? O5 Mg1 1.764(2) 21_545 ? O5 Al1 1.764(2) 21_545 ? 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 O4 P1 O6 110.75(15) . . ? O4 P1 O3 108.08(16) . . ? O6 P1 O3 109.65(15) . . ? O4 P1 O5 111.33(14) . . ? O6 P1 O5 106.14(16) . . ? O3 P1 O5 110.89(14) . . ? O4 P1 Mg1 97.64(11) . 21_545 ? O6 P1 Mg1 124.30(12) . 21_545 ? O3 P1 Mg1 105.08(10) . 21_545 ? O5 P1 Mg1 18.81(11) . 21_545 ? O4 P1 Mg1 102.04(11) . 2_645 ? O6 P1 Mg1 127.15(11) . 2_645 ? O3 P1 Mg1 18.11(10) . 2_645 ? O5 P1 Mg1 98.59(9) . 2_645 ? Mg1 P1 Mg1 89.35(3) 21_545 2_645 ? O2 P2 O2 109.3(2) 17_554 . ? O2 P2 O1 107.26(16) 17_554 17_554 ? O2 P2 O1 111.00(14) . 17_554 ? O2 P2 O1 110.99(14) 17_554 . ? O2 P2 O1 107.25(16) . . ? O1 P2 O1 111.0(2) 17_554 . ? O2 P2 Mg1 123.29(12) 17_554 17_554 ? O2 P2 Mg1 97.63(10) . 17_554 ? O1 P2 Mg1 17.20(10) 17_554 17_554 ? O1 P2 Mg1 106.75(11) . 17_554 ? O2 P2 Mg2 114.62(11) 17_554 2_655 ? O2 P2 Mg2 9.67(10) . 2_655 ? O1 P2 Mg2 101.39(10) 17_554 2_655 ? O1 P2 Mg2 111.08(10) . 2_655 ? Mg1 P2 Mg2 87.992(17) 17_554 2_655 ? O1 Al1 O3 107.97(13) . 3_765 ? O1 Al1 O5 108.56(14) . 20_665 ? O3 Al1 O5 109.38(12) 3_765 20_665 ? O1 Al1 O4 109.42(13) . . ? O3 Al1 O4 112.89(14) 3_765 . ? O5 Al1 O4 108.54(12) 20_665 . ? O2 Al2 O2 108.76(19) 17_554 3_665 ? O2 Al2 O6 108.82(14) 17_554 18_654 ? O2 Al2 O6 111.09(12) 3_665 18_654 ? O2 Al2 O6 111.08(12) 17_554 . ? O2 Al2 O6 108.81(14) 3_665 . ? O6 Al2 O6 108.29(19) 18_654 . ? P2 O1 Al1 148.05(18) . . ? P2 O2 Mg2 161.97(19) . 2_655 ? P2 O2 Al2 161.97(19) . 2_655 ? Mg2 O2 Al2 0.00(5) 2_655 2_655 ? P1 O3 Mg1 146.36(17) . 2_645 ? P1 O3 Al1 146.36(17) . 2_645 ? Mg1 O3 Al1 0.00(7) 2_645 2_645 ? P1 O4 Al1 146.18(19) . . ? P1 O5 Mg1 145.13(19) . 21_545 ? P1 O5 Al1 145.13(19) . 21_545 ? Mg1 O5 Al1 0.00(6) 21_545 21_545 ? P1 O6 Al2 146.83(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.569 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.081 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 9 1 ' ' 2 -0.004 0.496 0.000 477 126 ' ' 3 -0.033 -0.017 0.167 479 126 ' ' 4 -0.031 -0.018 0.333 479 126 ' ' 5 -0.004 0.497 0.500 477 126 ' ' 6 0.000 0.000 0.500 9 1 ' ' 7 -0.033 -0.027 0.667 479 126 ' ' 8 -0.031 -0.021 0.833 479 126 ' ' 9 0.333 0.667 0.167 9 1 ' ' 10 0.333 0.667 0.667 9 1 ' ' 11 0.666 0.333 0.333 9 1 ' ' 12 0.666 0.333 0.833 9 1 ' '