data_gdp3o9 _publ_requested_journal 'Chemistry of Materials' _publ_contact_author_name 'Dr. Henning A. H\"oppe' _publ_contact_author_address ; Albert-Ludwigs-Universit\"at Freiburg Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 D-79104 Freiburg Germany ; _publ_contact_author_email henning.hoeppe@ac.uni-freiburg.de _publ_contact_author_phone +49-(0)761-203-6106 _publ_contact_author_fax +49-(0)761-203-6012 loop_ _publ_author_name _publ_author_address 'H\"oppe, Henning A.' ; Albert-Ludwigs-Universit\"at Freiburg Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 D-79104 Freiburg Germany ; 'Sedlmaier, Stefan J.' ; Albert-Ludwigs-Universit\"at Freiburg Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 D-79104 Freiburg Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'gadolinium metaphosphate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Gd O9 P3' _chemical_formula_weight 394.16 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, 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 26.0171(17) _cell_length_b 13.5114(8) _cell_length_c 10.0840(7) _cell_angle_alpha 90.00 _cell_angle_beta 119.311(6) _cell_angle_gamma 90.00 _cell_volume 3091.0(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 9.226 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7223 _exptl_absorpt_correction_T_max 0.8441 _exptl_absorpt_process_details ; X-Red and X-SHAPE (Stoe & Cie, 1999), ; _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_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_monochromator graphite _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type 'STOE' _diffrn_detector_area_resol_mean 6.67 _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 360 frames, detector distance = 78 mm ; _diffrn_standards_decay_% ? _diffrn_reflns_number 25450 _diffrn_reflns_av_R_equivalents 0.1147 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3556 _reflns_number_gt 2474 _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^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00022(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3556 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _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 Gd1 Gd 0.133580(18) 0.61434(3) 0.86417(5) 0.02040(13) Uani 1 1 d . . . Gd2 Gd -0.116228(18) 0.87122(3) 0.11769(5) 0.02110(13) Uani 1 1 d . . . P1 P 0.05682(9) 0.71383(17) 0.4926(3) 0.0218(4) Uani 1 1 d . . . P2 P -0.03448(10) 0.68049(17) 0.0327(3) 0.0239(5) Uani 1 1 d . . . P3 P -0.00514(9) 0.54549(16) 0.2856(3) 0.0212(4) Uani 1 1 d . . . P4 P 0.2500 0.2803(2) 1.0000 0.0208(6) Uani 1 2 d S . . P5 P 0.21084(10) 0.43111(17) 0.7629(3) 0.0219(5) Uani 1 1 d . . . P6 P -0.19903(10) 1.03981(17) 0.2267(3) 0.0215(4) Uani 1 1 d . . . P7 P -0.2500 1.2007(2) 0.0000 0.0221(6) Uani 1 2 d S . . O101 O 0.0692(3) 0.7185(6) 0.8968(8) 0.0337(15) Uani 1 1 d . . . O102 O 0.1063(3) 0.6599(5) 0.6176(7) 0.0294(14) Uani 1 1 d . . . O201 O -0.0667(3) 0.6506(6) -0.1287(8) 0.0350(15) Uani 1 1 d . . . O202 O -0.0653(3) 0.7428(5) 0.0925(8) 0.0349(16) Uani 1 1 d . . . O301 O 0.0466(3) 0.4802(5) 0.3588(8) 0.0357(16) Uani 1 1 d . . . O302 O -0.0632(3) 0.5034(5) 0.2485(9) 0.0355(16) Uani 1 1 d . . . O400 O 0.3059(3) 0.2253(5) 1.0750(9) 0.0329(16) Uani 1 1 d . . . O501 O 0.1589(3) 0.3809(5) 0.6398(8) 0.0309(14) Uani 1 1 d . . . O502 O -1.2994(3) 1.0161(5) -0.6595(8) 0.0284(14) Uani 1 1 d . . . O601 O -0.1651(3) 1.0034(5) 0.1536(7) 0.0269(13) Uani 1 1 d . . . O602 O -0.1666(3) 1.0629(5) 0.3919(7) 0.0318(14) Uani 1 1 d . . . O700 O -0.1957(3) 1.2568(5) 0.0399(8) 0.0365(17) Uani 1 1 d . . . O12 O 0.0257(3) 0.7689(6) 0.5709(8) 0.0414(17) Uani 1 1 d . . . O23 O -0.0094(3) 0.5837(5) 0.1330(8) 0.0333(16) Uani 1 1 d . . . O31 O 0.0054(3) 0.6411(5) 0.3865(8) 0.0253(13) Uani 1 1 d . . . O45 O 0.2542(3) 0.3538(5) 0.8827(8) 0.0260(14) Uani 1 1 d . . . O56 O 0.2512(3) 0.4612(5) 0.6915(7) 0.0280(13) Uani 1 1 d . . . O67 O -0.2394(3) 1.1313(5) 0.1360(9) 0.0292(15) 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 Gd1 0.0206(2) 0.0201(2) 0.0197(2) -0.00127(15) 0.00924(17) -0.00134(15) Gd2 0.0209(2) 0.0215(2) 0.0201(2) -0.00086(15) 0.00940(17) -0.00096(15) P1 0.0227(10) 0.0221(11) 0.0183(11) -0.0015(8) 0.0083(9) -0.0028(8) P2 0.0264(11) 0.0234(11) 0.0208(12) 0.0012(8) 0.0107(10) 0.0004(9) P3 0.0215(10) 0.0196(10) 0.0217(12) 0.0007(8) 0.0100(10) -0.0002(8) P4 0.0205(14) 0.0196(14) 0.0226(17) 0.000 0.0107(13) 0.000 P5 0.0216(10) 0.0252(11) 0.0170(11) 0.0011(9) 0.0079(9) 0.0004(8) P6 0.0248(10) 0.0198(10) 0.0197(11) -0.0002(8) 0.0107(9) 0.0015(8) P7 0.0234(15) 0.0196(14) 0.0232(17) 0.000 0.0112(13) 0.000 O101 0.031(3) 0.040(4) 0.026(4) -0.006(3) 0.011(3) 0.007(3) O102 0.027(3) 0.036(4) 0.017(3) 0.007(3) 0.005(3) 0.004(3) O201 0.039(4) 0.042(4) 0.016(3) -0.002(3) 0.008(3) -0.001(3) O202 0.037(4) 0.037(4) 0.029(4) 0.003(3) 0.015(3) 0.017(3) O301 0.034(3) 0.034(4) 0.036(4) 0.005(3) 0.015(3) 0.020(3) O302 0.027(3) 0.035(4) 0.046(5) -0.013(3) 0.019(3) -0.015(3) O400 0.026(3) 0.028(3) 0.047(5) 0.007(3) 0.019(3) 0.014(3) O501 0.027(3) 0.039(4) 0.018(3) -0.005(3) 0.005(3) -0.006(3) O502 0.028(3) 0.029(3) 0.025(4) -0.005(3) 0.010(3) 0.005(3) O601 0.027(3) 0.031(3) 0.025(4) -0.003(3) 0.015(3) 0.001(2) O602 0.037(3) 0.038(4) 0.015(3) 0.000(3) 0.009(3) 0.003(3) O700 0.041(4) 0.037(4) 0.033(4) -0.015(3) 0.019(3) -0.027(3) O12 0.042(4) 0.054(5) 0.029(4) -0.009(3) 0.017(3) 0.007(3) O23 0.052(4) 0.021(3) 0.036(4) 0.005(3) 0.029(4) 0.005(3) O31 0.022(3) 0.024(3) 0.026(4) -0.006(3) 0.009(3) -0.004(2) O45 0.022(3) 0.028(3) 0.030(4) 0.005(3) 0.015(3) 0.003(2) O56 0.035(3) 0.027(3) 0.027(4) -0.004(3) 0.019(3) -0.005(3) O67 0.037(4) 0.022(3) 0.035(4) 0.010(3) 0.023(3) 0.010(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 Gd1 O700 2.247(6) 5_576 ? Gd1 O302 2.266(6) 5_566 ? Gd1 O602 2.281(6) 4_446 ? Gd1 O502 2.295(6) 3_646 ? Gd1 O102 2.310(6) . ? Gd1 O101 2.331(6) . ? Gd2 O201 2.250(7) 8_565 ? Gd2 O301 2.255(6) 4_455 ? Gd2 O400 2.266(6) 6_564 ? Gd2 O202 2.272(6) . ? Gd2 O501 2.274(7) 4_455 ? Gd2 O601 2.322(6) . ? P1 O101 1.476(7) 8_564 ? P1 O102 1.479(7) . ? P1 O12 1.568(7) . ? P1 O31 1.580(7) . ? P2 O201 1.476(7) . ? P2 O202 1.479(7) . ? P2 O12 1.574(7) 8_564 ? P2 O23 1.585(7) . ? P3 O301 1.471(6) . ? P3 O302 1.481(6) . ? P3 O23 1.575(7) . ? P3 O31 1.583(7) . ? P4 O400 1.471(6) 2_557 ? P4 O400 1.471(6) . ? P4 O45 1.588(7) 2_557 ? P4 O45 1.588(7) . ? P5 O501 1.477(7) . ? P5 O502 1.485(6) 3_646 ? P5 O45 1.578(7) . ? P5 O56 1.588(6) . ? P6 O601 1.483(6) . ? P6 O602 1.486(7) . ? P6 O56 1.576(6) 3_454 ? P6 O67 1.589(7) . ? P7 O700 1.475(6) . ? P7 O700 1.475(6) 2_455 ? P7 O67 1.571(7) 2_455 ? P7 O67 1.571(7) . ? O101 P1 1.476(7) 8_565 ? O201 Gd2 2.250(7) 8_564 ? O301 Gd2 2.255(6) 4_445 ? O302 Gd1 2.266(6) 5_566 ? O400 Gd2 2.266(6) 6_666 ? O501 Gd2 2.274(7) 4_445 ? O502 P5 1.485(6) 3_353 ? O502 Gd1 2.295(6) 3_353 ? O602 Gd1 2.281(6) 4_456 ? O700 Gd1 2.247(6) 5_576 ? O12 P2 1.574(7) 8_565 ? O56 P6 1.576(6) 3_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 O700 Gd1 O302 173.7(3) 5_576 5_566 ? O700 Gd1 O602 87.7(3) 5_576 4_446 ? O302 Gd1 O602 96.5(3) 5_566 4_446 ? O700 Gd1 O502 94.0(3) 5_576 3_646 ? O302 Gd1 O502 90.6(2) 5_566 3_646 ? O602 Gd1 O502 91.8(2) 4_446 3_646 ? O700 Gd1 O102 92.0(3) 5_576 . ? O302 Gd1 O102 84.2(3) 5_566 . ? O602 Gd1 O102 175.5(2) 4_446 . ? O502 Gd1 O102 83.7(2) 3_646 . ? O700 Gd1 O101 83.5(3) 5_576 . ? O302 Gd1 O101 92.0(3) 5_566 . ? O602 Gd1 O101 87.1(2) 4_446 . ? O502 Gd1 O101 177.3(2) 3_646 . ? O102 Gd1 O101 97.3(2) . . ? O201 Gd2 O301 89.0(3) 8_565 4_455 ? O201 Gd2 O400 95.8(3) 8_565 6_564 ? O301 Gd2 O400 173.2(3) 4_455 6_564 ? O201 Gd2 O202 89.2(3) 8_565 . ? O301 Gd2 O202 91.6(3) 4_455 . ? O400 Gd2 O202 93.2(3) 6_564 . ? O201 Gd2 O501 173.5(2) 8_565 4_455 ? O301 Gd2 O501 90.0(3) 4_455 4_455 ? O400 Gd2 O501 85.7(3) 6_564 4_455 ? O202 Gd2 O501 84.4(2) . 4_455 ? O201 Gd2 O601 88.6(3) 8_565 . ? O301 Gd2 O601 87.4(2) 4_455 . ? O400 Gd2 O601 88.0(2) 6_564 . ? O202 Gd2 O601 177.7(3) . . ? O501 Gd2 O601 97.8(2) 4_455 . ? O101 P1 O102 119.1(4) 8_564 . ? O101 P1 O12 111.6(5) 8_564 . ? O102 P1 O12 104.7(4) . . ? O101 P1 O31 109.0(4) 8_564 . ? O102 P1 O31 111.4(4) . . ? O12 P1 O31 99.3(4) . . ? O201 P2 O202 118.4(4) . . ? O201 P2 O12 110.4(4) . 8_564 ? O202 P2 O12 109.1(5) . 8_564 ? O201 P2 O23 108.2(4) . . ? O202 P2 O23 110.2(4) . . ? O12 P2 O23 98.8(4) 8_564 . ? O301 P3 O302 117.8(4) . . ? O301 P3 O23 107.2(4) . . ? O302 P3 O23 107.7(4) . . ? O301 P3 O31 109.8(4) . . ? O302 P3 O31 108.1(4) . . ? O23 P3 O31 105.5(4) . . ? O400 P4 O400 119.3(6) 2_557 . ? O400 P4 O45 106.7(3) 2_557 2_557 ? O400 P4 O45 110.1(4) . 2_557 ? O400 P4 O45 110.1(4) 2_557 . ? O400 P4 O45 106.7(3) . . ? O45 P4 O45 102.7(5) 2_557 . ? O501 P5 O502 118.2(4) . 3_646 ? O501 P5 O45 110.8(4) . . ? O502 P5 O45 110.7(4) 3_646 . ? O501 P5 O56 105.8(4) . . ? O502 P5 O56 111.7(4) 3_646 . ? O45 P5 O56 97.6(3) . . ? O601 P6 O602 118.5(4) . . ? O601 P6 O56 106.7(4) . 3_454 ? O602 P6 O56 110.3(4) . 3_454 ? O601 P6 O67 111.0(4) . . ? O602 P6 O67 109.5(4) . . ? O56 P6 O67 99.0(4) 3_454 . ? O700 P7 O700 118.2(7) . 2_455 ? O700 P7 O67 106.3(4) . 2_455 ? O700 P7 O67 109.5(4) 2_455 2_455 ? O700 P7 O67 109.5(4) . . ? O700 P7 O67 106.3(4) 2_455 . ? O67 P7 O67 106.6(5) 2_455 . ? P1 O101 Gd1 150.3(4) 8_565 . ? P1 O102 Gd1 136.8(4) . . ? P2 O201 Gd2 171.7(5) . 8_564 ? P2 O202 Gd2 160.5(5) . . ? P3 O301 Gd2 159.3(5) . 4_445 ? P3 O302 Gd1 150.5(4) . 5_566 ? P4 O400 Gd2 162.8(5) . 6_666 ? P5 O501 Gd2 136.1(4) . 4_445 ? P5 O502 Gd1 147.4(4) 3_353 3_353 ? P6 O601 Gd2 146.9(4) . . ? P6 O602 Gd1 168.6(4) . 4_456 ? P7 O700 Gd1 155.0(5) . 5_576 ? P1 O12 P2 141.3(5) . 8_565 ? P3 O23 P2 134.7(5) . . ? P1 O31 P3 140.0(4) . . ? P5 O45 P4 134.4(4) . . ? P6 O56 P5 136.3(4) 3_545 . ? P7 O67 P6 138.7(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.694 _refine_diff_density_min -1.270 _refine_diff_density_rms 0.239