Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Giacomo D. Gatta' 'Silvia Masci' 'Riccardo Vivani' _publ_contact_author_name 'Riccardo Vivani' _publ_contact_author_address ; Prof. Riccardo Vivani Department of Chemistry University of Perugia via Elce di Sotto, 8 06123 Perugia - Italy ; _publ_contact_author_email ric@unipg.it _publ_section_title ; Dimensional reduction in zirconium phosphate; from layers to ribbons to chains ; # COMPOUND 1 data_Compound_1 _database_code_CSD 197154 _audit_creation_date 'Nov 4 2002' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H18 F2 N4 O9 P2 Zr' _chemical_formula_weight 409.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall -P_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.889(3) _cell_length_b 10.520(3) _cell_length_c 12.412(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.70(2) _cell_angle_gamma 90.00 _cell_volume 1281.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; XCALIBUR CCD Oxford Instruments diffractometer ; _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 3345 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.68 _diffrn_reflns_theta_max 32.84 _reflns_number_total 2142 _reflns_number_gt 1483 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^)+(0.0269P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2142 _refine_ls_number_parameters 236 _refine_ls_number_restraints 176 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 2.924 _refine_ls_shift/su_mean 0.015 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 Zr1 Zr 0.22731(6) 0.12641(7) 0.73979(4) 0.0120(2) Uani 1 1 d . . . P1 P 0.05423(17) -0.13478(18) 0.78581(11) 0.0120(5) Uani 1 1 d . . . P2 P 0.04518(17) 0.38850(16) 0.76714(11) 0.0119(5) Uani 1 1 d . . . O1 O 0.0934(6) -0.0058(4) 0.7509(4) 0.0271(19) Uani 1 1 d . . . O2 O 0.0808(5) 0.2614(4) 0.7242(4) 0.0240(17) Uani 1 1 d . . . O6 O 0.0795(5) 0.3791(7) 0.8991(3) 0.0342(16) Uani 1 1 d . . . O7 O -0.0919(5) -0.1680(4) 0.7079(3) 0.0251(17) Uani 1 1 d . . . O8 O 0.0857(5) -0.1303(6) 0.9180(3) 0.0240(14) Uani 1 1 d . . . O5 O -0.1026(5) 0.4219(4) 0.6925(4) 0.0238(16) Uani 1 1 d . . . O3 O 0.3537(6) 0.2646(5) 0.7290(5) 0.037(2) Uani 1 1 d . . . N3 N 0.1366(6) 0.6314(7) 0.0335(4) 0.0233(16) Uani 1 1 d DU . . F1 F 0.3199(4) 0.1410(4) 0.9191(3) 0.0306(12) Uani 1 1 d . . . O4 O 0.3639(6) -0.0102(4) 0.7517(5) 0.027(2) Uani 1 1 d . . . F2 F 0.1363(4) 0.1103(4) 0.5615(3) 0.0294(12) Uani 1 1 d . . . N1 N 0.8524(7) 0.1184(7) 0.5649(5) 0.0366(19) Uani 1 1 d DU . . N4 N 0.6074(6) 0.1348(6) 0.9589(5) 0.0277(17) Uani 1 1 d DU . . N2 N 0.8675(6) 0.8723(7) 0.9799(4) 0.0231(16) Uani 1 1 d DU . . Ow O 0.6990(9) 0.1203(8) 0.7110(6) 0.067(2) Uani 1 1 d DU . . H2c H 0.931(4) 0.890(5) 0.944(4) 0.025(4) Uiso 1 1 d DU . . H3b H 0.231(3) 0.651(4) 0.096(3) 0.023(4) Uiso 1 1 d DU . . H4a H 0.581(5) 0.201(3) 0.895(3) 0.028(4) Uiso 1 1 d DU . . H2b H 0.774(3) 0.851(4) 0.916(3) 0.026(4) Uiso 1 1 d DU . . H3a H 0.075(4) 0.614(5) 0.071(4) 0.022(4) Uiso 1 1 d DU . . H2a H 0.901(5) 0.801(3) 1.038(3) 0.025(4) Uiso 1 1 d DU . . Hwa H 0.749(10) 0.058(6) 0.776(5) 0.084(6) Uiso 1 1 d DU . . Hwb H 0.665(10) 0.193(7) 0.743(6) 0.084(6) Uiso 1 1 d DU . . H4c H 0.543(4) 0.129(5) 0.994(4) 0.028(4) Uiso 1 1 d DU . . H3c H 0.104(5) 0.709(3) -0.020(3) 0.024(4) Uiso 1 1 d DU . . H3d H 0.141(5) 0.558(4) -0.016(4) 0.025(4) Uiso 1 1 d DU . . H1a H 0.821(5) 0.076(5) 0.621(4) 0.033(4) Uiso 1 1 d DU . . H1b H 0.771(4) 0.157(5) 0.498(4) 0.034(4) Uiso 1 1 d DU . . H1c H 0.907(6) 0.195(3) 0.604(5) 0.035(4) Uiso 1 1 d DU . . H1d H 0.900(5) 0.061(5) 0.535(4) 0.033(4) Uiso 1 1 d DU . . H2d H 0.858(5) 0.951(3) 1.022(4) 0.023(4) Uiso 1 1 d DU . . H4d H 0.701(3) 0.159(4) 1.023(3) 0.028(4) Uiso 1 1 d DU . . H4b H 0.618(5) 0.052(3) 0.924(4) 0.028(4) Uiso 1 1 d DU . . 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 Zr1 0.0149(4) 0.0092(2) 0.0147(2) 0.0014(2) 0.0090(2) 0.0019(3) P1 0.0094(10) 0.0122(7) 0.0172(5) -0.0025(6) 0.0085(6) -0.0001(7) P2 0.0113(10) 0.0095(8) 0.0169(5) -0.0008(6) 0.0078(7) -0.0009(6) O1 0.033(4) 0.014(2) 0.034(2) 0.0067(18) 0.014(3) -0.0023(19) O2 0.010(3) 0.018(2) 0.045(3) -0.0055(19) 0.013(2) 0.0024(17) O6 0.029(3) 0.052(3) 0.0169(14) 0.007(2) 0.005(2) 0.004(3) O7 0.017(3) 0.027(2) 0.0236(17) -0.0030(16) 0.001(2) -0.0036(18) O8 0.028(3) 0.031(2) 0.0168(14) 0.000(2) 0.0127(18) 0.001(3) O5 0.011(3) 0.029(2) 0.0280(18) 0.0005(17) 0.005(2) 0.0059(18) O3 0.041(4) 0.020(2) 0.060(3) 0.000(2) 0.031(3) -0.009(2) N3 0.021(3) 0.024(2) 0.0256(18) 0.000(2) 0.011(2) 0.001(3) F1 0.026(3) 0.050(3) 0.0187(13) -0.0027(17) 0.0123(16) -0.006(2) O4 0.018(4) 0.019(2) 0.047(3) -0.004(2) 0.017(3) 0.010(2) F2 0.037(3) 0.033(2) 0.0187(12) -0.0002(16) 0.0129(16) -0.0021(19) N1 0.027(3) 0.033(3) 0.039(2) -0.005(3) 0.005(3) 0.003(3) N4 0.027(3) 0.024(2) 0.0302(19) -0.003(2) 0.011(2) 0.003(2) N2 0.019(3) 0.026(2) 0.0272(18) -0.003(3) 0.013(2) 0.000(3) Ow 0.092(5) 0.058(3) 0.083(3) 0.000(4) 0.068(4) 0.005(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 Zr1 F2 2.001(3) . ? Zr1 F1 2.012(3) . ? Zr1 O4 2.027(6) . ? Zr1 O3 2.046(7) . ? Zr1 O1 2.062(7) . ? Zr1 O2 2.082(5) . ? P1 O7 1.502(5) . ? P1 O3 1.523(7) 2_546 ? P1 O8 1.525(4) . ? P1 O1 1.540(6) . ? P2 O5 1.509(5) . ? P2 O6 1.517(4) . ? P2 O4 1.539(6) 2_556 ? P2 O2 1.549(5) . ? O3 P1 1.523(7) 2_556 ? O4 P2 1.539(6) 2_546 ? 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 F2 Zr1 F1 179.4(2) . . ? F2 Zr1 O4 90.9(2) . . ? F1 Zr1 O4 88.5(2) . . ? F2 Zr1 O3 90.7(2) . . ? F1 Zr1 O3 89.4(2) . . ? O4 Zr1 O3 90.9(2) . . ? F2 Zr1 O1 89.49(19) . . ? F1 Zr1 O1 90.4(2) . . ? O4 Zr1 O1 92.0(3) . . ? O3 Zr1 O1 177.1(3) . . ? F2 Zr1 O2 87.87(19) . . ? F1 Zr1 O2 92.70(19) . . ? O4 Zr1 O2 177.7(2) . . ? O3 Zr1 O2 91.1(2) . . ? O1 Zr1 O2 86.0(2) . . ? O7 P1 O3 109.3(3) . 2_546 ? O7 P1 O8 112.4(3) . . ? O3 P1 O8 107.4(3) 2_546 . ? O7 P1 O1 111.7(2) . . ? O3 P1 O1 107.6(4) 2_546 . ? O8 P1 O1 108.4(3) . . ? O5 P2 O6 112.1(3) . . ? O5 P2 O1 109.3(3) . 2_556 ? O6 P2 O1 109.6(3) . 2_556 ? O5 P2 O2 110.4(2) . . ? O6 P2 O2 109.5(3) . . ? O4 P2 O2 105.8(4) 2_556 . ? P1 O1 Zr1 154.5(4) . . ? P2 O2 Zr1 148.5(3) . . ? P1 O3 Zr1 177.0(4) 2_556 . ? P2 O4 Zr1 168.3(4) 2_546 . ? _diffrn_measured_fraction_theta_max 0.450 _diffrn_reflns_theta_full 32.84 _diffrn_measured_fraction_theta_full 0.450 _refine_diff_density_max 0.588 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.114 #===END # COMPOUND 2 data_compound_2 _database_code_CSD 197155 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 'Nov 4, 2002' _computing_structure_refinement GSAS _refine_ls_number_parameters 86 _refine_ls_goodness_of_fit_all 4.36 _refine_ls_number_restraints 27 _refine_ls_matrix_type full _chemical_formula_weight 363.22 _chemical_formula_sum 'F H13 N3 O8.5 P2 Zr' _computing_structure_solution 'EXPO (A. Altomare, et al., 1995)' _cell_length_a 5.3511(2) _cell_length_b 9.2466(3) _cell_length_c 22.6443(7) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 1120.43(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall P_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, +y+1/2, -z+1/2' '-x+1/2, -y, +z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_attached_hydrogens _atom_site_calc_flag _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv Zr1 Zr -0.751(2) 0.4530(3) -0.0542(1) 1.000 4 a ? d Uiso 0.024(1) O2 O -0.492(5) 0.443(4) -0.122(1) 1.000 4 a ? d Uiso 0.034(2) O7 O -0.253(10) 0.364(2) -0.2104(6) 1.000 4 a ? d Uiso 0.047(3) O5 O -0.274(5) 0.269(2) 0.0498(7) 1.000 4 a ? d Uiso 0.034(2) Ow O -0.722(11) 0.491(3) 0.1720(9) 0.500 4 a ? d Uiso 0.028(3) O1 O -0.514(4) 0.476(4) 0.020(1) 1.000 4 a ? d Uiso 0.034(2) N3 N -0.286(7) 0.289(2) 0.2050(7) 1.000 4 a ? d Uiso 0.028(3) P2 P -0.249(6) 0.4750(8) -0.1605(3) 1.000 4 a ? d Biso 0.036(3) F1 F -0.714(4) 0.686(1) -0.0567(7) 1.000 4 a ? d Uiso 0.034(2) N1 N -0.738(11) 0.774(2) -0.1851(7) 1.000 4 a ? d Uiso 0.028(3) P1 P -0.255(4) 0.4330(8) 0.0437(2) 1.000 4 a ? d Uiso 0.013(2) O3 O -0.047(5) 0.459(4) -0.109(1) 1.000 4 a ? d Uiso 0.034(2) N2 N -0.714(6) 0.734(2) 0.0687(7) 1.000 4 a ? d Uiso 0.028(3) O6 O -0.279(8) 0.633(2) -0.1845(6) 1.000 4 a ? d Uiso 0.047(3) O8 O -0.271(8) 0.501(2) 0.1056(6) 1.000 4 a ? d Uiso 0.047(3) O4 O -0.039(5) 0.491(3) 0.009(1) 1.000 4 a ? d Uiso 0.034(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 F1 2.16(1) . 1_555 N Zr1 O3 2.02(3) . 1_455 N Zr1 O5 2.06(2) . 2_455 N Zr1 O4 2.13(3) . 1_455 N Zr1 O1 2.12(3) . 1_555 N Zr1 O2 2.07(3) . 1_555 N P1 O5 1.53(2) . 1_555 N P1 O4 1.50(3) . 1_555 N P1 O1 1.54(3) . 1_555 N P1 O8 1.54(2) . 1_555 N P2 O3 1.59(3) . 1_555 N P2 O2 1.60(4) . 1_555 N P2 O6 1.57(2) . 1_555 N P2 O7 1.53(2) . 1_555 N N1 O6 2.78(6) . 1_555 N N1 O7 2.51(2) . 3_454 N N1 O8 2.76(2) . 2_465 N N2 F1 2.87(2) . 1_555 N N2 F1 2.79(4) . 2_465 N N2 F1 2.79(3) . 2_565 N N2 O6 2.92(3) . 2_465 N N3 O6 2.63(2) . 4_465 N N3 O7 2.87(4) . 2_455 N N3 O8 2.87(5) . 1_555 N Ow O8 2.84(4) . 1_555 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Zr1 O3 91.5(10) 1_555 . 1_455 N F1 Zr1 O5 177.9(10) 1_555 . 2_455 N F1 Zr1 O4 85.3(9) 1_555 . 1_455 N F1 Zr1 O1 82.4(10) 1_555 . 1_555 N F1 Zr1 O2 88.1(10) 1_555 . 1_555 N O3 Zr1 O5 90.6(11) 1_455 . 2_455 N O3 Zr1 O4 80.6(8) 1_455 . 1_455 N O3 Zr1 O1 163.4(9) 1_455 . 1_555 N O3 Zr1 O2 94.1(6) 1_455 . 1_555 N O5 Zr1 O4 95.1(10) 2_455 . 1_455 N O5 Zr1 O1 95.6(10) 2_455 . 1_555 N O5 Zr1 O2 91.7(10) 2_455 . 1_555 N O4 Zr1 O1 83.5(5) 1_455 . 1_555 N O4 Zr1 O2 171.4(12) 1_455 . 1_555 N O1 Zr1 O2 101.1(7) 1_555 . 1_555 N O5 P1 O4 117.1(17) 1_555 . 1_555 N O5 P1 O1 103.1(20) 1_555 . 1_555 N O5 P1 O8 108.5(9) 1_555 . 1_555 N O4 P1 O1 114.7(9) 1_555 . 1_555 N O4 P1 O8 112.4(20) 1_555 . 1_555 N O1 P1 O8 99.2(22) 1_555 . 1_555 N O3 P2 O2 97.7(9) 1_555 . 1_555 N O3 P2 O6 114.0(20) 1_555 . 1_555 N O3 P2 O7 119.2(24) 1_555 . 1_555 N O2 P2 O6 106.3(26) 1_555 . 1_555 N O2 P2 O7 105.4(25) 1_555 . 1_555 N O6 P2 O7 111.8(9) 1_555 . 1_555 N Zr1 O3 P2 170.3(17) 1_655 . 1_555 N Zr1 O5 P1 172.3(19) 2_555 . 1_555 N Zr1 O4 P1 148.5(18) 1_655 . 1_555 N Zr1 O1 P1 142.2(14) 1_555 . 1_555 N Zr1 O2 P2 160.7(17) 1_555 . 1_555 N _diffrn_ambient_temperature 298 _diffrn_source 'ceramic lff sealed tube' _pd_meas_scan_method step _diffrn_radiation_monochromator graphite _pd_spec_size_thick 0.200 _pd_spec_mounting ; Aluminium sample holder with an oriented quartz crystal underneath ; _pd_spec_mount_mode reflection _pd_spec_shape flat_sheet loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source ZR 4.0 -0.314 2.245 17.8765 1.27618 10.9480 11.9160 5.41732 0.11762 3.65721 87.6627 2.06929 International_Tables_Vol_C P 8.0 0.283 0.434 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C F 4.0 0.069 0.053 3.53920 10.2825 2.64120 4.29440 1.51700 0.26150 1.02430 26.1476 0.27760 International_Tables_Vol_C O 34.0 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C N 12.0 0.029 0.018 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.75 loop_ _diffrn_radiation_wavelength _diffrn_radiation_wavelength_wt _diffrn_radiation_type _diffrn_radiation_wavelength_id 1.540500 1.000 K\a~1~ 1 1.544300 0.500 K\a~2~ 2 _pd_proc_ls_prof_r_factor 0.077 _pd_proc_ls_prof_wr_factor 0.104 _pd_proc_ls_prof_wr_expected 0.024 _refine_ls_R_Fsqd_factor 0.069 _pd_proc_ls_background_function ; GSAS Background function number 1 with 20 terms. Shifted Chebyshev function of 1st kind 1: 592.049 2: -14.5746 3: 114.343 4: 70.1465 5: -25.9923 6: -13.9345 7: 8.52756 8: -20.7512 9: 3.71931 10: -15.3227 11: -6.56506 12: 30.4468 13: -46.6884 14: 18.0580 15: -26.6332 16: -18.3998 17: 9.70494 18: -12.8170 19: -8.86812 20: -1.94432 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_t_min 1.00000 _gsas_exptl_extinct_corr_t_max 1.00000 _pd_proc_ls_pref_orient_corr ; March-Dollase AXIS 1 Ratio= 0.98081 h= 0.000 k= 0.000 l= 1.000 Prefered orientation correction range: Min= 0.97135, Max= 1.05986 ; _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 259.523 #2(GV) = 10.031 #3(GW) = -8.314 #4(GP) = 0.000 #5(LX) = 8.273 #6(LY) = 0.000 #7(S/L) = 0.0329 #8(H/L) = 0.0258 #9(trns) = 0.00 #10(shft)= 0.0000 #11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000 #17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00100 _pd_proc_info_datetime 2002-11-04T00:15:35 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 3.0 _pd_meas_2theta_range_max 139.0 _pd_meas_2theta_range_inc 0.02 _pd_proc_2theta_range_min 2.99446 _pd_proc_2theta_range_max 138.99446 _pd_proc_2theta_range_inc 0.02 _pd_meas_number_of_points 6801 _pd_proc_number_of_points 6801 _reflns_number_observed 2529 _reflns_limit_h_min 0 _reflns_limit_h_max 6 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _reflns_d_resolution_high 0.823 _reflns_d_resolution_low 8.560 #===END