data_ziggy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Mg O12 P2 Zr' _chemical_formula_weight 377.53 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' '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.3049(2) _cell_length_b 9.3372(4) _cell_length_c 9.6282(4) _cell_angle_alpha 97.3480(10) _cell_angle_beta 91.5340(10) _cell_angle_gamma 90.5120(10) _cell_volume 472.79(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 1.629 _exptl_absorpt_correction_type ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5497 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2766 _reflns_number_gt 2691 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.3745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2766 _refine_ls_number_parameters 173 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.199 _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 Zr Zr 0.25362(4) 0.74773(3) 0.49040(2) 0.00794(9) Uani 1 1 d . . . P1 P 0.26500(14) 0.45008(8) 0.68108(8) 0.01287(15) Uani 1 1 d . . . P2 P 0.23232(14) 0.06111(8) 0.32252(8) 0.01227(15) Uani 1 1 d . . . Mg1 Mg 0.0000 0.0000 0.0000 0.0185(3) Uani 1 2 d S . . Mg2 Mg 0.5000 0.5000 0.0000 0.0199(3) Uani 1 2 d S . . O1 O 0.3139(5) 0.5903(3) 0.6181(3) 0.0234(5) Uani 1 1 d . . . O2 O 0.2402(4) 0.4846(3) 0.8389(2) 0.0197(4) Uani 1 1 d . . . O3 O 0.4845(4) 0.3458(3) 0.6475(2) 0.0195(4) Uani 1 1 d . . . O4 O 0.0220(4) 0.3765(3) 0.6176(3) 0.0228(5) Uani 1 1 d . . . O5 O 0.0048(4) 0.1545(3) 0.3686(3) 0.0219(5) Uani 1 1 d . . . O6 O 0.2539(4) 0.0557(3) 0.1641(2) 0.0188(4) Uani 1 1 d . . . O7 O 0.4720(4) 0.1273(3) 0.3959(2) 0.0201(5) Uani 1 1 d . . . O8 O 0.1909(5) -0.0929(2) 0.3600(3) 0.0200(5) Uani 1 1 d . . . O9 O 0.2710(5) 0.8701(3) 0.8935(3) 0.0247(5) Uani 1 1 d D . . O10 O 0.1377(5) 0.1631(3) 0.8947(3) 0.0311(6) Uani 1 1 d D . . O11 O 0.2305(5) 0.3942(3) 0.1149(3) 0.0275(5) Uani 1 1 d D . . O12 O 0.3467(6) 0.6878(3) 0.0819(3) 0.0313(6) Uani 1 1 d D . . H1 H 0.436(6) 0.912(7) 0.877(7) 0.083(8) Uiso 1 1 d D . . H2 H 0.203(12) 0.819(7) 0.805(4) 0.083(8) Uiso 1 1 d D . . H3 H 0.135(13) 0.260(3) 0.947(6) 0.083(8) Uiso 1 1 d D . . H4 H 0.112(13) 0.156(7) 0.7928(10) 0.083(8) Uiso 1 1 d D . . H5 H 0.075(7) 0.449(6) 0.133(7) 0.083(8) Uiso 1 1 d D . . H6 H 0.273(13) 0.360(7) 0.205(4) 0.083(8) Uiso 1 1 d D . . H7 H 0.320(13) 0.764(5) 0.022(6) 0.083(8) Uiso 1 1 d D . . H8 H 0.420(12) 0.717(7) 0.176(3) 0.083(8) Uiso 1 1 d 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 Zr 0.00537(13) 0.00889(13) 0.00943(13) 0.00079(8) -0.00038(8) -0.00084(8) P1 0.0104(3) 0.0144(3) 0.0137(3) 0.0016(3) -0.0005(2) -0.0010(3) P2 0.0102(3) 0.0132(3) 0.0133(3) 0.0014(2) -0.0003(2) -0.0013(2) Mg1 0.0126(7) 0.0290(8) 0.0139(7) 0.0029(6) -0.0010(5) -0.0030(6) Mg2 0.0179(7) 0.0242(8) 0.0168(7) 0.0004(6) -0.0017(6) -0.0002(6) O1 0.0225(12) 0.0209(11) 0.0279(12) 0.0073(9) 0.0006(9) -0.0004(9) O2 0.0173(10) 0.0272(12) 0.0140(10) 0.0010(8) -0.0005(8) 0.0020(9) O3 0.0165(10) 0.0217(11) 0.0205(11) 0.0025(8) 0.0025(8) 0.0055(8) O4 0.0159(11) 0.0254(12) 0.0254(11) -0.0014(9) -0.0035(9) -0.0062(9) O5 0.0169(11) 0.0233(12) 0.0248(11) -0.0003(9) 0.0040(9) 0.0035(9) O6 0.0136(10) 0.0286(12) 0.0145(10) 0.0043(8) -0.0009(8) -0.0032(9) O7 0.0162(11) 0.0222(11) 0.0213(11) 0.0021(9) -0.0032(8) -0.0056(8) O8 0.0214(11) 0.0144(10) 0.0247(11) 0.0054(8) -0.0042(9) -0.0035(8) O9 0.0160(11) 0.0356(14) 0.0218(11) 0.0014(10) 0.0006(9) -0.0026(10) O10 0.0298(14) 0.0305(14) 0.0333(14) 0.0064(11) -0.0013(11) -0.0092(11) O11 0.0221(12) 0.0312(14) 0.0300(13) 0.0056(11) 0.0039(10) 0.0012(10) O12 0.0353(15) 0.0309(14) 0.0270(13) 0.0018(11) -0.0031(11) 0.0094(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 Zr O4 2.036(2) 2_566 ? Zr O1 2.056(2) . ? Zr O7 2.059(2) 2_666 ? Zr O3 2.069(2) 2_666 ? Zr O5 2.088(2) 2_566 ? Zr O8 2.089(2) 1_565 ? P1 O2 1.522(2) . ? P1 O4 1.530(2) . ? P1 O1 1.534(3) . ? P1 O3 1.539(2) . ? P2 O7 1.524(2) . ? P2 O6 1.527(2) . ? P2 O5 1.537(2) . ? P2 O8 1.542(2) . ? Mg1 O6 2.060(2) 2 ? Mg1 O6 2.060(2) . ? Mg1 O10 2.073(3) 1_554 ? Mg1 O10 2.073(3) 2_556 ? Mg1 O9 2.093(3) 2_566 ? Mg1 O9 2.093(3) 1_544 ? Mg2 O12 2.016(3) . ? Mg2 O12 2.016(3) 2_665 ? Mg2 O2 2.038(2) 2_666 ? Mg2 O2 2.038(2) 1_554 ? Mg2 O11 2.141(3) . ? Mg2 O11 2.141(3) 2_665 ? O2 Mg2 2.038(2) 1_556 ? O3 Zr 2.069(2) 2_666 ? O4 Zr 2.036(2) 2_566 ? O5 Zr 2.088(2) 2_566 ? O7 Zr 2.059(2) 2_666 ? O8 Zr 2.089(2) 1_545 ? O9 Mg1 2.093(3) 1_566 ? O9 H1 0.9800(11) . ? O9 H2 0.9800(11) . ? O10 Mg1 2.073(3) 1_556 ? O10 H3 0.9800(11) . ? O10 H4 0.9800(10) . ? O11 H5 0.9800(10) . ? O11 H6 0.9800(10) . ? O12 H7 0.9800(10) . ? O12 H8 0.9800(10) . ? 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 Zr O1 90.17(10) 2_566 . ? O4 Zr O7 178.58(9) 2_566 2_666 ? O1 Zr O7 88.96(10) . 2_666 ? O4 Zr O3 89.47(10) 2_566 2_666 ? O1 Zr O3 90.42(10) . 2_666 ? O7 Zr O3 91.66(9) 2_666 2_666 ? O4 Zr O5 91.75(10) 2_566 2_566 ? O1 Zr O5 89.81(10) . 2_566 ? O7 Zr O5 87.13(9) 2_666 2_566 ? O3 Zr O5 178.76(9) 2_666 2_566 ? O4 Zr O8 89.55(10) 2_566 1_565 ? O1 Zr O8 179.71(9) . 1_565 ? O7 Zr O8 91.33(9) 2_666 1_565 ? O3 Zr O8 89.58(9) 2_666 1_565 ? O5 Zr O8 90.20(10) 2_566 1_565 ? O2 P1 O4 109.27(14) . . ? O2 P1 O1 109.37(14) . . ? O4 P1 O1 110.27(14) . . ? O2 P1 O3 110.20(13) . . ? O4 P1 O3 108.20(14) . . ? O1 P1 O3 109.51(14) . . ? O7 P2 O6 109.78(13) . . ? O7 P2 O5 109.75(13) . . ? O6 P2 O5 108.33(14) . . ? O7 P2 O8 109.94(13) . . ? O6 P2 O8 109.61(14) . . ? O5 P2 O8 109.40(14) . . ? O6 Mg1 O6 180.00(8) 2 . ? O6 Mg1 O10 88.89(10) 2 1_554 ? O6 Mg1 O10 91.11(10) . 1_554 ? O6 Mg1 O10 91.11(10) 2 2_556 ? O6 Mg1 O10 88.89(10) . 2_556 ? O10 Mg1 O10 180.0 1_554 2_556 ? O6 Mg1 O9 90.23(9) 2 2_566 ? O6 Mg1 O9 89.77(9) . 2_566 ? O10 Mg1 O9 94.42(11) 1_554 2_566 ? O10 Mg1 O9 85.58(11) 2_556 2_566 ? O6 Mg1 O9 89.77(9) 2 1_544 ? O6 Mg1 O9 90.23(9) . 1_544 ? O10 Mg1 O9 85.58(11) 1_554 1_544 ? O10 Mg1 O9 94.42(11) 2_556 1_544 ? O9 Mg1 O9 180.00(9) 2_566 1_544 ? O12 Mg2 O12 180.00(15) . 2_665 ? O12 Mg2 O2 90.33(10) . 2_666 ? O12 Mg2 O2 89.67(10) 2_665 2_666 ? O12 Mg2 O2 89.67(10) . 1_554 ? O12 Mg2 O2 90.33(10) 2_665 1_554 ? O2 Mg2 O2 180.00(14) 2_666 1_554 ? O12 Mg2 O11 87.03(11) . . ? O12 Mg2 O11 92.97(11) 2_665 . ? O2 Mg2 O11 92.47(10) 2_666 . ? O2 Mg2 O11 87.53(10) 1_554 . ? O12 Mg2 O11 92.97(11) . 2_665 ? O12 Mg2 O11 87.03(11) 2_665 2_665 ? O2 Mg2 O11 87.53(10) 2_666 2_665 ? O2 Mg2 O11 92.47(10) 1_554 2_665 ? O11 Mg2 O11 180.00(13) . 2_665 ? P1 O1 Zr 157.37(17) . . ? P1 O2 Mg2 132.01(14) . 1_556 ? P1 O3 Zr 150.47(15) . 2_666 ? P1 O4 Zr 168.53(16) . 2_566 ? P2 O5 Zr 155.91(16) . 2_566 ? P2 O6 Mg1 132.36(13) . . ? P2 O7 Zr 167.82(16) . 2_666 ? P2 O8 Zr 151.29(15) . 1_545 ? Mg1 O9 H1 120(4) 1_566 . ? Mg1 O9 H2 112(4) 1_566 . ? H1 O9 H2 109(5) . . ? Mg1 O10 H3 115(4) 1_556 . ? Mg1 O10 H4 119(4) 1_556 . ? H3 O10 H4 117(6) . . ? Mg2 O11 H5 114(4) . . ? Mg2 O11 H6 122(4) . . ? H5 O11 H6 104(5) . . ? Mg2 O12 H7 119(4) . . ? Mg2 O12 H8 109(4) . . ? H7 O12 H8 117(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.557 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.128