Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (c) The Royal Society of Chemistry 2004 data_global _pd_block_id 2003-09-18T17:00|La960GeGe_RT||Overall _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2003-09-18T17:00 _audit_author_name ? _audit_update_record ; 2003-09-18T17:00 Initial CIF as created by GSAS2CIF ; _journal_coden_Cambridge 1145 loop_ _publ_author_name _publ_author_address 'Miguel A.G. Aranda' ; ? ; 'Sebastian Bruque' '' 'Laura Leon-Reina' '' 'Enrique R. Losilla' '' 'Maria Martinez-Lara' '' _publ_contact_author_name 'Dr Miguel A.G. Aranda' _publ_contact_author_address ; Quimica Inorganica Universidad de Malaga Campus Teatinos S/N Malaga 29071 SPAIN ; _publ_contact_author_email G_ARANDA@UMA.ES _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Interstitial oxygen conduction in lanthanum oxy-apatite electrolytes ; data_La960GeGe_RT_overall _database_code_depnum_ccdc_archive 'CCDC 230199' _refine_ls_shift/su_max 0.99 _refine_ls_shift/su_mean 0.07 _computing_structure_refinement GSAS _refine_ls_number_parameters 115 _refine_ls_goodness_of_fit_all 66.75 _refine_ls_number_restraints 0 # Overall powder R-factors _pd_proc_ls_prof_R_factor 0.0615 _pd_proc_ls_prof_wR_factor 0.0332 _refine_ls_matrix_type full # pointers to the phase blocks loop_ _pd_phase_block_id 2003-09-18T17:00|La960GeGe_RT_phase1||| # pointers to the diffraction patterns loop_ _pd_block_diffractogram_id 2003-09-18T17:00|La960GeGe_RT_H_01|| 2003-09-18T17:00|La960GeGe_RT_H_02|| # Information for phase 1 #data_La960GeGe_RT_phase_1 _pd_block_id 2003-09-18T17:00|La960GeGe_RT_phase1||| # Histograms for phase 1 #loop_ #_pd_block_diffractogram_id #2003-09-18T17:00|La960GeGe_RT_H_01|| #2003-09-18T17:00|La960GeGe_RT_H_02|| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name La9.60Ge6O26.4 _cell_length_a 9.93931(13) _cell_length_b 9.93931 _cell_length_c 7.28485(10) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 623.25305 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z+1/2 3 -y,x-y,+z 4 -x,-y,+z+1/2 5 y-x,-x,+z 6 +y,y-x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z+1/2 -3 +y,y-x,-z -4 +x,+y,-z+1/2 -5 x-y,+x,-z -6 -y,x-y,-z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity LA La1 0.23322(11) -0.01011(13) 0.25 1.0 Uani 0.01294 6 LA La2 0.3333 0.6667 0.00094(21) 0.9 Uani 0.02132 4 GE Ge 0.40019(11) 0.37311(11) 0.25 1.0 Uani 0.00925 6 O O1 0.31535(20) 0.48930(18) 0.25 1.0 Uani 0.03383 6 O O2 0.60076(15) 0.47303(16) 0.25 1.0 Uani 0.01852 6 O O3 0.34521(20) 0.25003(15) 0.06170(13) 1.0 Uani 0.05481 12 O O4 0.0 0.0 0.25 0.879(6) Uani 0.05854 2 O O5 0.0159(21) 0.2277(20) 0.6062(15) 0.0771(19) Uiso 0.03 12 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 La1 0.0179(6) 0.0088(5) 0.0 0.0126(6) 0.0 0.0099(4) La2 0.0211(5) 0.01055(25) 0.0 0.0211(5) 0.0 0.0218(8) Ge 0.0150(5) 0.0118(5) 0.0 0.0095(6) 0.0 0.0108(5) O1 0.0666(14) 0.0585(13) 0.0 0.0560(13) 0.0 0.0160(9) O2 0.0061(8) 0.0028(7) 0.0 0.0062(8) 0.0 0.0429(10) O3 0.1012(13) 0.0435(9) -0.0318(8) 0.0429(9) -0.0157(6) 0.0302(7) O4 0.0047(11) 0.0023(5) 0.0 0.0047(11) 0.0 0.166(4) loop_ _atom_type_symbol _atom_type_number_in_cell LA 9.6 GE 6.0 O 26.684 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'Ge La1.60 O4.45' _chemical_formula_weight 366.00 _cell_formula_units_Z 6 # MOLECULAR GEOMETRY 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 La1 La1 4.1048(14) . 3_555 N La1 La1 4.1048(14) . 5_555 N La1 Ge 3.3077(16) . 1_555 N La1 Ge 3.4198(15) . 5_555 N La1 O1 2.7864(21) . 5_555 N La1 O2 2.5301(14) . 3_655 N La1 O3 2.6321(16) . 1_555 N La1 O3 2.4577(10) . 6_555 N La1 O3 2.4577(10) . -3_555 N La1 O3 2.6321(16) . -4_556 N La1 O4 2.3699(8) . 1_555 N La1 O5 2.560(18) . 4_554 N La1 O5 2.602(11) . 5_555 N La1 O5 2.467(16) . 6_554 N La1 O5 2.560(18) . -1_556 N La1 O5 2.602(11) . -2_556 N La1 O5 2.467(16) . -3_556 N La2 La2 3.6561(31) . -2_565 N La2 La2 3.6288(31) . -2_566 N La2 Ge 3.4000(10) . 2_554 N La2 Ge 3.4005(10) . 4_664 N La2 Ge 3.3997(10) . 6_564 N La2 O1 2.4735(15) . 1_555 N La2 O1 2.4732(15) . 3_665 N La2 O1 2.4728(15) . 5_565 N La2 O2 2.5704(15) . 2_554 N La2 O2 2.5710(15) . 4_664 N La2 O2 2.5705(15) . 6_564 N La2 O3 2.9084(18) . -1_665 N La2 O3 2.9075(18) . -3_565 N La2 O3 2.9082(18) . -5_555 N Ge La1 3.3077(16) . 1_555 N Ge La1 3.4198(15) . 3_555 N Ge La2 3.3997(10) . 2_655 N Ge La2 3.4005(10) . -1_665 N Ge O1 1.7374(14) . 1_555 N Ge O2 1.7265(14) . 1_555 N Ge O3 1.7344(12) . 1_555 N Ge O3 1.7344(12) . -4_556 N Ge O5 1.965(13) . 6_554 N Ge O5 1.965(13) . -3_556 N O1 La1 2.7864(21) . 3_555 N O1 La2 2.4735(15) . 1_555 N O1 La2 2.4732(15) . -2_566 N O1 Ge 1.7374(14) . 1_555 N O2 La1 2.5301(14) . 5_665 N O2 La2 2.5705(15) . 2_655 N O2 La2 2.5710(15) . -1_665 N O2 Ge 1.7265(14) . 1_555 N O3 La1 2.6321(16) . 1_555 N O3 La1 2.4577(10) . 2_554 N O3 La2 2.9084(18) . -1_665 N O3 Ge 1.7344(12) . 1_555 N O3 O5 1.082(17) . 6_554 N O4 La1 2.3699(8) . 1_555 N O4 La1 2.3699(8) . 3_555 N O4 La1 2.3699(8) . 5_555 N O5 La1 2.467(16) . 2_555 N O5 La1 2.602(11) . 3_555 N O5 La1 2.560(18) . 4_555 N O5 Ge 1.965(13) . 2_555 N O5 O3 1.082(17) . 2_555 N O5 O5 2.096(21) . -4_557 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 O2 La1 O3 70.21(5) 3_655 . 1_555 N O2 La1 O3 85.86(4) 3_655 . 6_555 N O2 La1 O3 85.86(4) 3_655 . -3_555 N O2 La1 O3 70.21(5) 3_655 . -4_556 N O2 La1 O4 149.93(6) 3_655 . 1_555 N O2 La1 O5 145.54(32) 3_655 . 4_554 N O2 La1 O5 94.11(31) 3_655 . 5_555 N O2 La1 O5 92.9(4) 3_655 . 6_554 N O2 La1 O5 145.54(32) 3_655 . -1_556 N O2 La1 O5 94.11(31) 3_655 . -2_556 N O2 La1 O5 92.9(4) 3_655 . -3_556 N O3 La1 O3 138.71(6) 1_555 . 6_555 N O3 La1 O3 77.782(27) 1_555 . -3_555 N O3 La1 O3 62.82(5) 1_555 . -4_556 N O3 La1 O4 84.29(5) 1_555 . 1_555 N O3 La1 O5 111.83(28) 1_555 . 4_554 N O3 La1 O5 122.1(4) 1_555 . 5_555 N O3 La1 O5 24.2(4) 1_555 . 6_554 N O3 La1 O5 143.00(33) 1_555 . -1_556 N O3 La1 O5 59.5(4) 1_555 . -2_556 N O3 La1 O5 62.01(25) 1_555 . -3_556 N O3 La1 O3 135.01(9) 6_555 . -3_555 N O3 La1 O3 77.782(27) 6_555 . -4_556 N O3 La1 O4 104.52(4) 6_555 . 1_555 N O3 La1 O5 106.92(28) 6_555 . 4_554 N O3 La1 O5 24.5(4) 6_555 . 5_555 N O3 La1 O5 137.37(27) 6_555 . 6_554 N O3 La1 O5 62.26(31) 6_555 . -1_556 N O3 La1 O5 158.9(4) 6_555 . -2_556 N O3 La1 O5 87.18(25) 6_555 . -3_556 N O3 La1 O3 138.71(6) -3_555 . -4_556 N O3 La1 O4 104.52(4) -3_555 . 1_555 N O3 La1 O5 62.26(31) -3_555 . 4_554 N O3 La1 O5 158.9(4) -3_555 . 5_555 N O3 La1 O5 87.18(25) -3_555 . 6_554 N O3 La1 O5 106.92(28) -3_555 . -1_556 N O3 La1 O5 24.5(4) -3_555 . -2_556 N O3 La1 O5 137.37(27) -3_555 . -3_556 N O3 La1 O4 84.29(5) -4_556 . 1_555 N O3 La1 O5 143.00(33) -4_556 . 4_554 N O3 La1 O5 59.5(4) -4_556 . 5_555 N O3 La1 O5 62.01(25) -4_556 . 6_554 N O3 La1 O5 111.83(28) -4_556 . -1_556 N O3 La1 O5 122.1(4) -4_556 . -2_556 N O3 La1 O5 24.2(4) -4_556 . -3_556 N O4 La1 O5 58.82(32) 1_555 . 4_554 N O4 La1 O5 85.98(33) 1_555 . 5_555 N O4 La1 O5 60.2(4) 1_555 . 6_554 N O4 La1 O5 58.82(32) 1_555 . -1_556 N O4 La1 O5 85.98(33) 1_555 . -2_556 N O4 La1 O5 60.2(4) 1_555 . -3_556 N O5 La1 O5 110.8(5) 4_554 . 5_555 N O5 La1 O5 97.9(6) 4_554 . 6_554 N O5 La1 O5 48.3(6) 4_554 . -1_556 N O5 La1 O5 62.55(33) 4_554 . -2_556 N O5 La1 O5 119.0(6) 4_554 . -3_556 N O5 La1 O5 113.9(6) 5_555 . 6_554 N O5 La1 O5 62.55(33) 5_555 . -1_556 N O5 La1 O5 171.6(6) 5_555 . -2_556 N O5 La1 O5 63.8(4) 5_555 . -3_556 N O5 La1 O5 119.0(6) 6_554 . -1_556 N O5 La1 O5 63.8(4) 6_554 . -2_556 N O5 La1 O5 50.3(5) 6_554 . -3_556 N O5 La1 O5 110.8(5) -1_556 . -2_556 N O5 La1 O5 97.9(6) -1_556 . -3_556 N O5 La1 O5 113.9(6) -2_556 . -3_556 N La2 La2 La2 179.9604 -2_565 . -2_566 N La2 La2 O1 137.177(32) -2_565 . 1_555 N La2 La2 O1 137.182(32) -2_565 . 3_665 N La2 La2 O1 137.216(32) -2_565 . 5_565 N La2 La2 O2 44.683(33) -2_565 . 2_554 N La2 La2 O2 44.671(33) -2_565 . 4_664 N La2 La2 O2 44.668(33) -2_565 . 6_564 N La2 La2 O1 42.810(32) -2_566 . 1_555 N La2 La2 O1 42.800(32) -2_566 . 3_665 N La2 La2 O1 42.815(32) -2_566 . 5_565 N La2 La2 O2 135.347(33) -2_566 . 2_554 N La2 La2 O2 135.305(33) -2_566 . 4_664 N La2 La2 O2 135.326(33) -2_566 . 6_564 N O1 La2 O1 72.10(5) 1_555 . 3_665 N O1 La2 O1 72.10(5) 1_555 . 5_565 N O1 La2 O2 125.11(4) 1_555 . 2_554 N O1 La2 O2 94.790(31) 1_555 . 4_664 N O1 La2 O2 154.96(5) 1_555 . 6_564 N O1 La2 O1 72.11(5) 3_665 . 5_565 N O1 La2 O2 155.00(5) 3_665 . 2_554 N O1 La2 O2 125.09(4) 3_665 . 4_664 N O1 La2 O2 94.810(31) 3_665 . 6_564 N O1 La2 O2 94.823(31) 5_565 . 2_554 N O1 La2 O2 154.97(5) 5_565 . 4_664 N O1 La2 O2 125.13(4) 5_565 . 6_564 N O2 La2 O2 75.01(5) 2_554 . 4_664 N O2 La2 O2 75.02(5) 2_554 . 6_564 N O2 La2 O2 75.01(5) 4_664 . 6_564 N O1 Ge O2 114.97(10) 1_555 . 1_555 N O1 Ge O3 112.48(6) 1_555 . 1_555 N O1 Ge O3 112.48(6) 1_555 . -4_556 N O1 Ge O5 91.6(5) 1_555 . 6_554 N O1 Ge O5 91.6(5) 1_555 . -3_556 N O2 Ge O3 105.76(7) 1_555 . 1_555 N O2 Ge O3 105.76(7) 1_555 . -4_556 N O2 Ge O5 139.0(5) 1_555 . 6_554 N O2 Ge O5 139.0(5) 1_555 . -3_556 N O3 Ge O3 104.53(10) 1_555 . -4_556 N O3 Ge O5 33.3(4) 1_555 . 6_554 N O3 Ge O5 90.4(4) 1_555 . -3_556 N O3 Ge O5 90.4(4) -4_556 . 6_554 N O3 Ge O5 33.3(4) -4_556 . -3_556 N O5 Ge O5 64.5(7) 6_554 . -3_556 N La2 O1 La2 94.37(6) 1_555 . -2_566 N La2 O1 Ge 126.00(5) 1_555 . 1_555 N La2 O1 Ge 125.99(5) -2_566 . 1_555 N La1 O2 La2 116.68(4) 5_665 . 2_655 N La1 O2 La2 116.67(4) 5_665 . -1_665 N La1 O2 Ge 121.91(9) 5_665 . 1_555 N La2 O2 La2 90.65(7) 2_655 . -1_665 N La2 O2 Ge 102.82(5) 2_655 . 1_555 N La2 O2 Ge 102.84(5) -1_665 . 1_555 N La1 O3 La1 117.21(6) 1_555 . 2_554 N La1 O3 Ge 96.32(5) 1_555 . 1_555 N La1 O3 O5 69.3(9) 1_555 . 6_554 N La1 O3 Ge 138.80(7) 2_554 . 1_555 N La1 O3 O5 85.2(6) 2_554 . 6_554 N Ge O3 O5 85.1(6) 1_555 . 6_554 N La1 O4 La1 120.0 1_555 . 3_555 N La1 O4 La1 120.0 1_555 . 5_555 N La1 O4 La1 120.0 3_555 . 5_555 N La1 O5 La1 118.0(5) 2_555 . 3_555 N La1 O5 La1 109.5(5) 2_555 . 4_555 N La1 O5 Ge 95.9(6) 2_555 . 2_555 N La1 O5 O3 86.5(10) 2_555 . 2_555 N La1 O5 La1 114.7(6) 3_555 . 4_555 N La1 O5 Ge 118.2(6) 3_555 . 2_555 N La1 O5 O3 70.3(6) 3_555 . 2_555 N La1 O5 Ge 97.3(5) 4_555 . 2_555 N La1 O5 O3 155.5(10) 4_555 . 2_555 N Ge O5 O3 61.6(7) 2_555 . 2_555 N # Powder diffraction data for histogram 1 #data_La960GeGe_RT_p_01 #_pd_block_id #2003-09-18T17:00|La960GeGe_RT_H_01|| #loop_ #_pd_phase_id #_pd_phase_block_id #_pd_phase_mass_% #_pd_proc_ls_profile_function #_pd_proc_ls_peak_cutoff #1 2003-09-18T17:00|La960GeGe_RT_phase1||| #? #; #CW Profile function number 4 with 15 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. #Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 0.024 #4(GP) = 0.000 #5(LX) = 0.000 #6(ptec) = 0.00 #7(trns) = 0.00 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0011 #11(H/L) = 0.0029 #12(eta) = 0.3606 #13(S400 ) = 8.2E-02 #14(S004 ) = 5.7E-02 #15(S202 ) = 1.0E-01 #Peak tails are ignored where the intensity is below 0.0050 times the peak #Aniso. broadening axis 0.0 0.0 1.0 #; #0.00500 #loop_ #_atom_type_symbol #_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 #LA -1.661 0.887 #20.5780 2.94817 19.5990 0.24448 11.3727 18.7726 3.28719 133.124 2.14678 #International_Tables_Vol_C #GE 0.194 0.648 #16.0816 2.85090 6.37470 0.25160 3.70680 11.4468 3.68300 54.7625 2.13130 #International_Tables_Vol_C #O -0.002 0.002 #3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 #International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 1.0 _diffrn_radiation_wavelength 0.400269 _diffrn_radiation_type ? #_pd_proc_ls_prof_R_factor 0.0780 #_pd_proc_ls_prof_wR_factor 0.0941 _pd_proc_ls_prof_wR_expected 0.0088 _refine_ls_R_Fsqd_factor 0.04954 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 116.045 2: 596.733 3: 815.881 4: 689.454 5: 695.405 6: 720.005 7: 892.195 8: 836.272 9: 1053.51 10: 688.365 11: 692.221 12: 935.266 13: 980.955 14: 1256.16 15: 1008.24 16: 963.418 17: 1189.13 18: 910.087 19: 912.848 20: 1115.36 21: 1037.85 22: 1220.93 23: 1004.59 24: 1091.92 25: 1081.03 26: 974.297 27: 1050.01 28: 1003.82 29: 999.187 30: 950.235 31: 962.265 32: 979.760 33: 974.849 34: 928.935 35: 919.452 36: 882.655 ; _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_info_datetime 2003-09-18T17:00:15 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.003 _pd_meas_2theta_range_max 0.648 _pd_meas_2theta_range_inc 0.003 _pd_proc_2theta_range_min 0.000798 _pd_proc_2theta_range_max 0.645798 _pd_proc_2theta_range_inc 0.003 _reflns_number_observed 609 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _reflns_d_resolution_high 0.727 _reflns_d_resolution_low 8.608 # Powder diffraction data for histogram 2 #data_La960GeGe_RT_p_02 #_pd_block_id 2003-09-18T17:00|La960GeGe_RT_H_02|| #============================================================================== #loop_ #_pd_phase_id #_pd_phase_block_id #_pd_phase_mass_% #_pd_proc_ls_profile_function #_pd_proc_ls_peak_cutoff #1 2003-09-18T17:00|La960GeGe_RT_phase1||| ? #; #CW Profile function number 2 with 18 terms #Profile coefficients for Simpson's rule integration of pseudovoigt function #C.J. Howard (1982). J. Appl. Cryst.,15,615-620. #P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 302.532 #2(GV) = -437.876 #3(GW) = 398.945 #4(LX) = 0.000 #5(LY) = 13.200 #6(trns) = 0.000 #7(asym) = 5.7583 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 #Peak tails are ignored where the intensity is below 0.0050 times the peak #Aniso. broadening axis 0.0 0.0 1.0 #; #0.00500 #loop_ #_atom_type_symbol #_atom_type_scat_length_neutron #_atom_type_scat_source #LA 0.8240 International_Tables_Vol_C #GE 0.8185 International_Tables_Vol_C #O 0.5803 International_Tables_Vol_C #_diffrn_radiation_probe neutron #_diffrn_radiation_wavelength 1.886 #_pd_proc_ls_prof_R_factor 0.0255 #_pd_proc_ls_prof_wR_factor 0.0329 #_pd_proc_ls_prof_wR_expected 0.0170 #_refine_ls_R_Fsqd_factor 0.03584 #_pd_proc_ls_background_function #; #GSAS Background function number 7 with 20 terms. #Linear interpolation #1: 2509.14 2: 2274.52 3: 2143.53 4: 2146.94 #5: 2184.22 6: 2524.91 7: 2605.55 8: 2487.94 #9: 2556.15 10: 2557.62 11: 2648.85 12: 2669.11 #13: 2760.42 14: 2681.50 15: 2773.81 16: 2475.79 #17: 2448.31 18: 2451.90 19: 2577.20 20: 2800.12 #; #_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_info_datetime 2003-09-18T17:00:15 #_pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- #_pd_meas_2theta_range_min 4.45 #_pd_meas_2theta_range_max 0.0 #_pd_meas_2theta_range_inc 4.45 #_pd_proc_2theta_range_min 4.55 #_pd_proc_2theta_range_max 0.1 #_pd_proc_2theta_range_inc 4.45 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_LA955_773K_publ _database_code_depnum_ccdc_archive 'CCDC 230200' _pd_block_id 2003-09-18T15:38|LA955_773K|| _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2003-09-18T15:38 _audit_update_record ; 2003-09-18T15:38 Initial CIF as created by GSAS2CIF ; # 8. Phase information from GSAS _pd_phase_name 'from C:/users/leon/La955Si_sinQ/La955Si6_RT/La955si.exp' _cell_length_a 9.76655(18) _cell_length_b 9.76655 _cell_length_c 7.20962(14) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 595.55951 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z+1/2 3 -y,x-y,+z 4 -x,-y,+z+1/2 5 y-x,-x,+z 6 +y,y-x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z+1/2 -3 +y,y-x,-z -4 +x,+y,-z+1/2 -5 x-y,+x,-z -6 -y,x-y,-z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity LA La1 0.22741(23) -0.01331(29) 0.25 1.0 Uani 0.02285 6 LA La2 0.3333 0.6667 0.0001(5) 0.887 Uani 0.02986 4 SI SI 0.4004(4) 0.3706(4) 0.25 1.0 Uani 0.02015 6 O O1 0.3248(4) 0.4852(4) 0.25 1.0 Uani 0.0418 6 O O2 0.59313(35) 0.4717(4) 0.25 1.0 Uani 0.03418 6 O O3 0.34590(32) 0.25826(27) 0.06990(25) 1.0 Uani 0.04395 12 O O4 0.0 0.0 0.25 0.986(19) Uani 0.09156 2 O O5 -0.007(14) 0.229(13) 0.596(9) 0.024(4) Uiso 0.03 12 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 La1 0.0253(12) 0.0094(10) 0.0 0.0203(12) 0.0 0.0203(8) La2 0.0243(11) 0.0121(6) 0.0 0.0243(11) 0.0 0.0410(17) SI 0.0250(22) 0.0097(18) 0.0 0.0092(20) 0.0 0.0279(22) O1 0.0621(26) 0.0394(21) 0.0 0.0446(28) 0.0 0.0356(22) O2 0.0236(19) 0.0070(19) 0.0 0.0284(19) 0.0 0.0425(23) O3 0.0684(21) 0.0268(13) -0.0202(12) 0.0346(16) -0.0074(9) 0.0303(12) O4 0.0241(27) 0.0121(14) 0.0 0.0241(27) 0.0 0.226(10) # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'La1.59 O4.38 Si' _chemical_formula_weight 319.15 _cell_formula_units_Z 6 # MOLECULAR GEOMETRY 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 La1 La1 3.9644(30) . 3_555 N La1 La1 3.9644(30) . 5_555 N La1 SI 3.253(5) . 1_555 N La1 SI 3.332(4) . 5_555 N La1 O1 2.773(5) . 5_555 N La1 O2 2.550(4) . 3_655 N La1 O3 2.6440(31) . 1_555 N La1 O3 2.4810(19) . 6_555 N La1 O3 2.4810(19) . -3_555 N La1 O3 2.6440(31) . -4_556 N La1 O4 2.2889(18) . 1_555 N La1 O5 2.40(11) . 4_554 N La1 O5 2.50(7) . 5_555 N La1 O5 2.67(10) . 6_554 N La1 O5 2.40(11) . -1_556 N La1 O5 2.50(7) . -2_556 N La1 O5 2.67(10) . -3_556 N La2 La2 3.606(7) . -2_565 N La2 La2 3.604(7) . -2_566 N La2 SI 3.331(4) . 2_554 N La2 SI 3.331(4) . 4_664 N La2 SI 3.331(4) . 6_564 N La2 O1 2.5000(33) . 1_555 N La2 O1 2.4997(33) . 3_665 N La2 O1 2.4993(33) . 5_565 N La2 O2 2.5614(34) . 2_554 N La2 O2 2.5620(34) . 4_664 N La2 O2 2.5615(34) . 6_564 N La2 O3 2.8831(29) . -1_665 N La2 O3 2.8821(29) . -3_565 N La2 O3 2.8828(29) . -5_555 N SI La1 3.253(5) . 1_555 N SI La1 3.332(4) . 3_555 N SI La2 3.331(4) . 2_655 N SI La2 3.331(4) . -1_665 N SI O1 1.619(5) . 1_555 N SI O2 1.631(4) . 1_555 N SI O3 1.6091(30) . 1_555 N SI O3 1.6091(30) . -4_556 N SI O5 1.89(9) . 6_554 N SI O5 1.89(9) . -3_556 N O1 La1 2.773(5) . 3_555 N O1 La2 2.5000(33) . 1_555 N O1 La2 2.4997(33) . -2_566 N O1 SI 1.619(5) . 1_555 N O2 La1 2.550(4) . 5_665 N O2 La2 2.5615(34) . 2_655 N O2 La2 2.5620(34) . -1_665 N O2 SI 1.631(4) . 1_555 N O3 La1 2.6440(31) . 1_555 N O3 La1 2.4810(19) . 2_554 N O3 La2 2.8831(29) . -1_665 N O3 SI 1.6091(30) . 1_555 N O3 O5 1.07(11) . 6_554 N O4 La1 2.2889(18) . 1_555 N O4 La1 2.2889(18) . 3_555 N O4 La1 2.2889(18) . 5_555 N O5 La1 2.67(10) . 2_555 N O5 La1 2.50(7) . 3_555 N O5 La1 2.40(11) . 4_555 N O5 SI 1.89(9) . 2_555 N O5 O3 1.07(11) . 2_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 O2 La1 O3 70.66(11) 3_655 . 1_555 N O2 La1 O3 82.75(7) 3_655 . 6_555 N O2 La1 O3 82.75(7) 3_655 . -3_555 N O2 La1 O3 70.66(11) 3_655 . -4_556 N O2 La1 O4 150.62(14) 3_655 . 1_555 N O2 La1 O5 138.5(23) 3_655 . 4_554 N O2 La1 O5 88.6(22) 3_655 . 5_555 N O2 La1 O5 92.9(24) 3_655 . 6_554 N O2 La1 O5 138.5(23) 3_655 . -1_556 N O2 La1 O5 88.6(22) 3_655 . -2_556 N O2 La1 O5 92.9(24) 3_655 . -3_556 N O3 La1 O3 133.93(12) 1_555 . 6_555 N O3 La1 O3 77.33(5) 1_555 . -3_555 N O3 La1 O3 58.82(10) 1_555 . -4_556 N O3 La1 O4 83.88(8) 1_555 . 1_555 N O3 La1 O5 113.8(21) 1_555 . 4_554 N O3 La1 O5 115.4(28) 1_555 . 5_555 N O3 La1 O5 23.2(23) 1_555 . 6_554 N O3 La1 O5 149.0(23) 1_555 . -1_556 N O3 La1 O5 56.6(27) 1_555 . -2_556 N O3 La1 O5 59.2(17) 1_555 . -3_556 N O3 La1 O3 136.74(15) 6_555 . -3_555 N O3 La1 O3 77.33(5) 6_555 . -4_556 N O3 La1 O4 106.25(7) 6_555 . 1_555 N O3 La1 O5 111.0(21) 6_555 . 4_554 N O3 La1 O5 24.8(27) 6_555 . 5_555 N O3 La1 O5 135.0(16) 6_555 . 6_554 N O3 La1 O5 60.1(21) 6_555 . -1_556 N O3 La1 O5 161.2(26) 6_555 . -2_556 N O3 La1 O5 86.3(16) 6_555 . -3_556 N O3 La1 O3 133.93(12) -3_555 . -4_556 N O3 La1 O4 106.25(7) -3_555 . 1_555 N O3 La1 O5 60.1(21) -3_555 . 4_554 N O3 La1 O5 161.2(26) -3_555 . 5_555 N O3 La1 O5 86.3(16) -3_555 . 6_554 N O3 La1 O5 111.0(21) -3_555 . -1_556 N O3 La1 O5 24.8(27) -3_555 . -2_556 N O3 La1 O5 135.0(16) -3_555 . -3_556 N O3 La1 O4 83.88(8) -4_556 . 1_555 N O3 La1 O5 149.0(23) -4_556 . 4_554 N O3 La1 O5 56.6(27) -4_556 . 5_555 N O3 La1 O5 59.2(17) -4_556 . 6_554 N O3 La1 O5 113.8(21) -4_556 . -1_556 N O3 La1 O5 115.4(28) -4_556 . -2_556 N O3 La1 O5 23.2(23) -4_556 . -3_556 N O4 La1 O5 65.2(23) 1_555 . 4_554 N O4 La1 O5 89.4(23) 1_555 . 5_555 N O4 La1 O5 60.7(24) 1_555 . 6_554 N O4 La1 O5 65.2(23) 1_555 . -1_556 N O4 La1 O5 89.4(23) 1_555 . -2_556 N O4 La1 O5 60.7(24) 1_555 . -3_556 N O5 La1 O5 121(4) 4_554 . 5_555 N O5 La1 O5 102(4) 4_554 . 6_554 N O5 La1 O5 55(4) 4_554 . -1_556 N O5 La1 O5 65.8(24) 4_554 . -2_556 N O5 La1 O5 126(4) 4_554 . -3_556 N O5 La1 O5 110.9(35) 5_555 . 6_554 N O5 La1 O5 65.8(24) 5_555 . -1_556 N O5 La1 O5 172(6) 5_555 . -2_556 N O5 La1 O5 61.9(27) 5_555 . -3_556 N O5 La1 O5 126(4) 6_554 . -1_556 N O5 La1 O5 61.9(27) 6_554 . -2_556 N O5 La1 O5 49.0(32) 6_554 . -3_556 N O5 La1 O5 121(4) -1_556 . -2_556 N O5 La1 O5 102(4) -1_556 . -3_556 N O5 La1 O5 110.9(35) -2_556 . -3_556 N La2 La2 La2 179.9604 -2_565 . -2_566 N La2 La2 O1 136.11(8) -2_565 . 1_555 N La2 La2 O1 136.11(8) -2_565 . 3_665 N La2 La2 O1 136.15(8) -2_565 . 5_565 N La2 La2 O2 45.27(9) -2_565 . 2_554 N La2 La2 O2 45.26(9) -2_565 . 4_664 N La2 La2 O2 45.26(9) -2_565 . 6_564 N La2 La2 O1 43.88(8) -2_566 . 1_555 N La2 La2 O1 43.87(8) -2_566 . 3_665 N La2 La2 O1 43.88(8) -2_566 . 5_565 N La2 La2 O2 134.76(9) -2_566 . 2_554 N La2 La2 O2 134.71(9) -2_566 . 4_664 N La2 La2 O2 134.74(9) -2_566 . 6_564 N O1 La2 O1 73.77(12) 1_555 . 3_665 N O1 La2 O1 73.78(12) 1_555 . 5_565 N O1 La2 O2 124.93(9) 1_555 . 2_554 N O1 La2 O2 92.97(6) 1_555 . 4_664 N O1 La2 O2 153.79(10) 1_555 . 6_564 N O1 La2 O1 73.78(12) 3_665 . 5_565 N O1 La2 O2 153.83(10) 3_665 . 2_554 N O1 La2 O2 124.92(9) 3_665 . 4_664 N O1 La2 O2 92.99(6) 3_665 . 6_564 N O1 La2 O2 93.00(7) 5_565 . 2_554 N O1 La2 O2 153.80(10) 5_565 . 4_664 N O1 La2 O2 124.96(9) 5_565 . 6_564 N O2 La2 O2 75.93(13) 2_554 . 4_664 N O2 La2 O2 75.94(13) 2_554 . 6_564 N O2 La2 O2 75.93(13) 4_664 . 6_564 N O1 SI O2 111.65(31) 1_555 . 1_555 N O1 SI O3 111.20(18) 1_555 . 1_555 N O1 SI O3 111.20(18) 1_555 . -4_556 N O1 SI O5 86(4) 1_555 . 6_554 N O1 SI O5 86(4) 1_555 . -3_556 N O2 SI O3 107.49(19) 1_555 . 1_555 N O2 SI O3 107.49(19) 1_555 . -4_556 N O2 SI O5 140.9(28) 1_555 . 6_554 N O2 SI O5 140.9(28) 1_555 . -3_556 N O3 SI O3 107.60(25) 1_555 . -4_556 N O3 SI O5 34.5(31) 1_555 . 6_554 N O3 SI O5 97.0(25) 1_555 . -3_556 N O3 SI O5 97.0(25) -4_556 . 6_554 N O3 SI O5 34.5(31) -4_556 . -3_556 N O5 SI O5 72(5) 6_554 . -3_556 N La2 O1 La2 92.24(16) 1_555 . -2_566 N La2 O1 SI 128.68(10) 1_555 . 1_555 N La2 O1 SI 128.66(10) -2_566 . 1_555 N La1 O2 La2 115.05(9) 5_665 . 2_655 N La1 O2 La2 115.04(9) 5_665 . -1_665 N La1 O2 SI 125.04(25) 5_665 . 1_555 N La2 O2 La2 89.47(17) 2_655 . -1_665 N La2 O2 SI 102.93(16) 2_655 . 1_555 N La2 O2 SI 102.95(16) -1_665 . 1_555 N La1 O3 La1 112.81(11) 1_555 . 2_554 N La1 O3 SI 96.74(13) 1_555 . 1_555 N La1 O3 O5 80(5) 1_555 . 6_554 N La1 O3 SI 143.96(17) 2_554 . 1_555 N La1 O3 O5 79(4) 2_554 . 6_554 N SI O3 O5 87(4) 1_555 . 6_554 N La1 O4 La1 120.0 1_555 . 3_555 N La1 O4 La1 120.0 1_555 . 5_555 N La1 O4 La1 120.0 3_555 . 5_555 N La1 O5 La1 111(4) 2_555 . 3_555 N La1 O5 La1 102.8(29) 2_555 . 4_555 N La1 O5 SI 89(4) 2_555 . 2_555 N La1 O5 O3 77(6) 2_555 . 2_555 N La1 O5 La1 121(5) 3_555 . 4_555 N La1 O5 SI 125(4) 3_555 . 2_555 N La1 O5 O3 76(4) 3_555 . 2_555 N La1 O5 SI 101.4(34) 4_555 . 2_555 N La1 O5 O3 160(6) 4_555 . 2_555 N SI O5 O3 58(4) 2_555 . 2_555 N # Powder diffraction data for histogram 1 #============================================================================== loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_length_neutron _atom_type_scat_source LA 9.548 0.8240 International_Tables_Vol_C SI 6.0 0.4149 International_Tables_Vol_C O 26.255 0.5803 International_Tables_Vol_C _diffrn_radiation_probe neutron _diffrn_radiation_wavelength 1.88604 _pd_proc_ls_prof_R_factor 0.0353 _pd_proc_ls_prof_wR_factor 0.0467 _pd_proc_ls_prof_wR_expected 0.0206 _refine_ls_R_Fsqd_factor 0.05287 _pd_proc_ls_background_function ; GSAS Background function number 8 with 20 terms. Reciprocal interpolation 1: 1195.33 2: 1194.11 3: 1196.78 4: 1160.09 5: 1107.96 6: 1171.43 7: 1174.96 8: 1192.40 9: 1180.78 10: 1203.91 11: 1217.85 12: 1220.87 13: 1224.47 14: 1264.77 15: 1251.84 16: 1313.19 17: 1603.93 18: 1634.01 19: 1649.61 20: 1819.89 ; _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_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 97.724 #2(GV) = -296.312 #3(GW) = 371.706 #4(LX) = 0.000 #5(LY) = 4.366 #6(trns) = 0.000 #7(asym) = 23.2453 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00500 _pd_proc_info_datetime 2003-09-18T15:38:34 _pd_calc_method 'Rietveld Refinement' #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_LA955SI_RT_publ _database_code_depnum_ccdc_archive 'CCDC 230201' _pd_block_id 2003-09-18T13:17|LA955SI_RT||Overall _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2003-09-18T13:17 _audit_update_record ; 2003-09-18T13:17 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= #data_LA955SI_RT_overall _refine_ls_shift/su_max 0.08 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement GSAS _refine_ls_number_parameters 116 _refine_ls_goodness_of_fit_all 91.35 _refine_ls_number_restraints 0 # Overall powder R-factors _pd_proc_ls_prof_R_factor 0.0282 _pd_proc_ls_prof_wR_factor 0.0318 _refine_ls_matrix_type full # pointers to the phase blocks loop_ _pd_phase_block_id 2003-09-18T13:17|LA955SI_RT_phase1||| # pointers to the diffraction patterns loop_ _pd_block_diffractogram_id 2003-09-18T13:17|LA955SI_RT_H_01|| 2003-09-18T13:17|LA955SI_RT_H_02|| # Information for phase 1 #data_LA955SI_RT_phase_1 #_pd_block_id #2003-09-18T13:17|LA955SI_RT_phase1||| # Histograms for phase 1 #loop_ #_pd_block_diffractogram_id #2003-09-18T13:17|LA955SI_RT_H_01|| #2003-09-18T13:17|LA955SI_RT_H_02|| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name La9.55Si6O26.325 _cell_length_a 9.72566(4) _cell_length_b 9.72566 _cell_length_c 7.18636(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 588.67871 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z+1/2 3 -y,x-y,+z 4 -x,-y,+z+1/2 5 y-x,-x,+z 6 +y,y-x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z+1/2 -3 +y,y-x,-z -4 +x,+y,-z+1/2 -5 x-y,+x,-z -6 -y,x-y,-z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity LA La1 0.22824(10) -0.01255(12) 0.25 1.0 Uani 0.0075 6 LA La2 0.3333 0.6667 -0.00152(20) 0.887 Uani 0.01363 4 SI SI 0.40142(19) 0.37118(18) 0.25 1.0 Uani 0.00519 6 O O1 0.32274(17) 0.48395(19) 0.25 1.0 Uani 0.01969 6 O O2 0.59498(15) 0.47319(17) 0.25 1.0 Uani 0.01241 6 O O3 0.34667(14) 0.25656(12) 0.06956(11) 1.0 Uani 0.02453 12 O O4 0.0 0.0 0.25 0.973(8) Uani 0.0736 2 O O5 -0.001(9) 0.224(8) 0.580(6) 0.0185(19) Uiso 0.03 12 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 La1 0.0100(5) 0.0022(4) 0.0 0.0049(5) 0.0 0.0055(4) La2 0.0077(4) 0.00384(22) 0.0 0.0077(4) 0.0 0.0255(7) SI 0.0079(9) 0.0059(8) 0.0 0.0041(8) 0.0 0.0075(9) O1 0.0268(9) 0.0234(8) 0.0 0.0276(11) 0.0 0.0177(9) O2 0.0094(7) 0.0038(7) 0.0 0.0072(8) 0.0 0.0203(8) O3 0.0479(9) 0.0174(6) -0.0168(4) 0.0149(6) -0.0077(4) 0.0131(5) O4 0.0051(11) 0.0025(5) 0.0 0.0051(11) 0.0 0.211(4) loop_ _atom_type_symbol _atom_type_number_in_cell LA 9.548 SI 6.0 O 26.169 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'La1.59 O4.36 Si' _chemical_formula_weight 318.92 _cell_formula_units_Z 6 # MOLECULAR GEOMETRY 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 ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? # Powder diffraction data for histogram 1 #data_LA955SI_RT_p_01 #_pd_block_id 2003-09-18T13:17|LA955SI_RT_H_01|| #loop_ #_pd_phase_id #_pd_phase_block_id #_pd_phase_mass_% #_pd_proc_ls_profile_function #_pd_proc_ls_peak_cutoff #1 2003-09-18T13:17|LA955SI_RT_phase1||| ? #; #CW Profile function number 4 with 15 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. #Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 7.507 #4(GP) = 0.000 #5(LX) = 2.825 #6(ptec) = 0.00 #7(trns) = 0.00 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0557 #11(H/L) = 0.0253 #12(eta) = 0.6578 #13(S400 ) = 9.8E-03 #14(S004 ) = 2.2E-02 #15(S202 ) = 9.4E-03 #Peak tails are ignored where the intensity is below 0.0050 times the peak #Aniso. broadening axis 0.0 0.0 1.0 #;0.00500 #loop_ #_atom_type_symbol #_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 #LA -1.720 9.040 20.5780 2.94817 19.5990 0.24448 11.3727 18.7726 3.28719 133.124 #2.14678 International_Tables_Vol_C #SI 0.244 0.330 6.29150 2.43860 3.03530 32.3337 1.98910 0.67850 1.54100 81.6937 #1.14070 International_Tables_Vol_C #O 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 #_diffrn_radiation_probe x-ray #_diffrn_radiation_polarisn_ratio 0.58 loop_ _diffrn_radiation_wavelength _diffrn_radiation_wavelength_wt _diffrn_radiation_type _diffrn_radiation_wavelength_id 1.540598 1.000 K\a~1~ 1 1.544398 0.470 K\a~2~ 2 #_pd_proc_ls_prof_R_factor 0.0566 #_pd_proc_ls_prof_wR_factor 0.0770 _pd_proc_ls_prof_wR_expected 0.0461 _refine_ls_R_Fsqd_factor 0.03241 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 262.822 2: 179.214 3: 212.804 4: 185.495 5: 136.456 6: 169.595 7: 115.501 8: 109.212 9: 113.082 10: 124.517 11: 119.154 12: 144.085 13: 143.151 14: 168.197 15: 113.914 16: 106.643 17: 96.9342 18: 107.919 19: 103.212 20: 90.2960 21: 87.0013 22: 82.6587 23: 87.3404 24: 104.939 25: 101.409 26: 90.2478 27: 95.1814 28: 95.5179 29: 96.0519 30: 85.8099 31: 80.6924 32: 92.1068 33: 88.9361 34: 93.6357 35: 93.0526 36: 94.8351 ; _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_info_datetime 2003-09-18T13:17:02 _pd_calc_method 'Rietveld Refinement' # Powder diffraction data for histogram 2 #data_LA955SI_RT_p_02 #_pd_block_id #2003-09-18T13:17|LA955SI_RT_H_02|| #loop_ #_pd_phase_id #_pd_phase_block_id #_pd_phase_mass_% #_pd_proc_ls_profile_function #_pd_proc_ls_peak_cutoff #1 2003-09-18T13:17|LA955SI_RT_phase1||| #? #; #CW Profile function number 2 with 18 terms #Profile coefficients for Simpson's rule integration of pseudovoigt function #C.J. Howard (1982). J. Appl. Cryst.,15,615-620. #P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 159.454 #2(GV) = -426.755 #3(GW) = 449.623 #4(LX) = 0.000 #5(LY) = 3.767 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 1.05 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 #Peak tails are ignored where the intensity is below 0.0050 times the peak #Aniso. broadening axis 0.0 0.0 1.0 #; #0.00500 #loop_ #_atom_type_symbol #_atom_type_scat_length_neutron #_atom_type_scat_source #LA 0.8240 #International_Tables_Vol_C #SI 0.4149 #International_Tables_Vol_C #O 0.5803 #International_Tables_Vol_C #_diffrn_radiation_probe neutron #_diffrn_radiation_wavelength 1.886034 #_pd_proc_ls_prof_R_factor 0.0243 #_pd_proc_ls_prof_wR_factor 0.0318 #_pd_proc_ls_prof_wR_expected 0.0182 #_refine_ls_R_Fsqd_factor 0.02164 #_pd_proc_ls_background_function #; GSAS Background function number 1 with 20 terms. #Shifted Chebyshev function of 1st kind #1: 1965.85 2: 130.057 3: -53.6013 4: -50.0350 #5: 70.0462 6: -24.2087 7: 59.5588 8: -18.5318 #9: -57.2662 10: -13.7982 11: -11.0552 12: -47.3278 #13: 5.51479 14: -8.01329 15: -16.7049 16: -10.4535 #17: 0.629400 18: -0.311340 19: 19.7079 20: 15.6816 #; #_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_info_datetime 2003-09-18T13:17:02 #_pd_calc_method "Rietveld Refinement" #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_La960Ge_1173K_publ _database_code_depnum_ccdc_archive 'CCDC 230202' _pd_block_id 2003-09-18T17:10|La960Ge_1173K|La960Ge_1173K|HRPT _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2003-09-18T17:10 _audit_author_name La960Ge_1173K _audit_update_record ; 2003-09-18T17:10 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 1.42 _refine_ls_shift/su_mean 0.11 _computing_structure_refinement GSAS _refine_ls_number_parameters 71 _refine_ls_goodness_of_fit_all 2.42 _refine_ls_number_restraints 0 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from C:/users/leon/La960GeGe_sinQ/La960Ge(O4).EXP' _cell_length_a 10.00745(28) _cell_length_b 10.00745 _cell_length_c 7.33341(22) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 636.03766 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z+1/2 3 -y,x-y,+z 4 -x,-y,+z+1/2 5 y-x,-x,+z 6 +y,y-x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z+1/2 -3 +y,y-x,-z -4 +x,+y,-z+1/2 -5 x-y,+x,-z -6 -y,x-y,-z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity LA La1 0.22891(27) -0.0104(4) 0.25 1.0 Uani 0.03636 6 LA La2 0.3333 0.6667 0.0018(6) 0.9 Uani 0.04393 4 GE Ge 0.40024(32) 0.37335(29) 0.25 1.0 Uani 0.0322 6 O O1 0.3175(5) 0.4902(5) 0.25 1.0 Uani 0.06511 6 O O2 0.6017(4) 0.4730(4) 0.25 1.0 Uani 0.0569 6 O O3 0.3417(5) 0.2525(4) 0.0632(4) 1.0 Uani 0.0803 12 O O4 0.0 0.0 0.25 0.981(15) Uani 0.08524 2 O O5 0.003(9) 0.224(8) 0.589(6) 0.041(5) Uiso 0.03 12 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 La1 0.0376(17) 0.0120(15) 0.0 0.0276(16) 0.0 0.0381(13) La2 0.0489(17) 0.0245(8) 0.0 0.0489(17) 0.0 0.0340(23) Ge 0.0282(16) 0.0136(13) 0.0 0.0308(16) 0.0 0.0359(14) O1 0.099(4) 0.0620(34) 0.0 0.0714(35) 0.0 0.0513(31) O2 0.0424(24) 0.0160(23) 0.0 0.0355(26) 0.0 0.088(4) O3 0.130(4) 0.0548(23) -0.0447(24) 0.0578(24) -0.0204(19) 0.0630(23) O4 0.0382(30) 0.0191(15) 0.0 0.0382(30) 0.0 0.179(10) # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'Ge La1.60 O4.41' _chemical_formula_weight 365.40 _cell_formula_units_Z 6 # MOLECULAR GEOMETRY 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 La1 La1 4.0607(35) . 3_555 N La1 La1 4.0607(35) . 5_555 N La1 Ge 3.332(4) . 1_555 N La1 Ge 3.433(4) . 5_555 N La1 O1 2.834(6) . 5_555 N La1 O2 2.585(4) . 3_655 N La1 O3 2.665(4) . 1_555 N La1 O3 2.4781(28) . 6_555 N La1 O3 2.4781(28) . -3_555 N La1 O3 2.665(4) . -4_556 N La1 O4 2.3444(20) . 1_555 N La1 O5 2.52(7) . 4_554 N La1 O5 2.49(4) . 5_555 N La1 O5 2.62(6) . 6_554 N La1 O5 2.52(7) . -1_556 N La1 O5 2.49(4) . -2_556 N La1 O5 2.62(6) . -3_556 N La2 La2 3.693(9) . -2_565 N La2 La2 3.641(9) . -2_566 N La2 Ge 3.4272(30) . 2_554 N La2 Ge 3.4277(30) . 4_664 N La2 Ge 3.4268(30) . 6_564 N La2 O1 2.486(4) . 1_555 N La2 O1 2.486(4) . 3_665 N La2 O1 2.485(4) . 5_565 N La2 O2 2.587(4) . 2_554 N La2 O2 2.587(4) . 4_664 N La2 O2 2.587(4) . 6_564 N La2 O3 2.971(5) . -1_665 N La2 O3 2.970(5) . -3_565 N La2 O3 2.971(5) . -5_555 N Ge La1 3.332(4) . 1_555 N Ge La1 3.433(4) . 3_555 N Ge La2 3.4268(30) . 2_655 N Ge La2 3.4277(30) . -1_665 N Ge O1 1.738(4) . 1_555 N Ge O2 1.746(4) . 1_555 N Ge O3 1.7242(30) . 1_555 N Ge O3 1.7242(30) . -4_556 N Ge O5 2.03(6) . 6_554 N Ge O5 2.03(6) . -3_556 N O1 La1 2.834(6) . 3_555 N O1 La2 2.486(4) . 1_555 N O1 La2 2.486(4) . -2_566 N O1 Ge 1.738(4) . 1_555 N O2 La1 2.585(4) . 5_665 N O2 La2 2.587(4) . 2_655 N O2 La2 2.587(4) . -1_665 N O2 Ge 1.746(4) . 1_555 N O3 La1 2.665(4) . 1_555 N O3 La1 2.4781(28) . 2_554 N O3 La2 2.971(5) . -1_665 N O3 Ge 1.7242(30) . 1_555 N O3 O5 1.07(7) . 6_554 N O4 La1 2.3444(20) . 1_555 N O4 La1 2.3444(20) . 3_555 N O4 La1 2.3444(20) . 5_555 N O5 La1 2.62(6) . 2_555 N O5 La1 2.49(4) . 3_555 N O5 La1 2.52(7) . 4_555 N O5 Ge 2.03(6) . 2_555 N O5 O3 1.07(7) . 2_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 O2 La1 O3 70.32(15) 3_655 . 1_555 N O2 La1 O3 84.45(10) 3_655 . 6_555 N O2 La1 O3 84.45(10) 3_655 . -3_555 N O2 La1 O3 70.32(15) 3_655 . -4_556 N O2 La1 O4 150.00(19) 3_655 . 1_555 N O2 La1 O5 141.2(13) 3_655 . 4_554 N O2 La1 O5 91.7(12) 3_655 . 5_555 N O2 La1 O5 92.9(16) 3_655 . 6_554 N O2 La1 O5 141.2(13) 3_655 . -1_556 N O2 La1 O5 91.7(12) 3_655 . -2_556 N O2 La1 O5 92.9(16) 3_655 . -3_556 N O3 La1 O3 136.87(16) 1_555 . 6_555 N O3 La1 O3 77.12(7) 1_555 . -3_555 N O3 La1 O3 61.85(14) 1_555 . -4_556 N O3 La1 O4 84.10(12) 1_555 . 1_555 N O3 La1 O5 110.6(12) 1_555 . 4_554 N O3 La1 O5 119.2(18) 1_555 . 5_555 N O3 La1 O5 23.4(15) 1_555 . 6_554 N O3 La1 O5 146.3(12) 1_555 . -1_556 N O3 La1 O5 57.4(18) 1_555 . -2_556 N O3 La1 O5 62.9(10) 1_555 . -3_556 N O3 La1 O3 135.93(24) 6_555 . -3_555 N O3 La1 O3 77.12(7) 6_555 . -4_556 N O3 La1 O4 105.36(11) 6_555 . 1_555 N O3 La1 O5 110.9(13) 6_555 . 4_554 N O3 La1 O5 25.0(17) 6_555 . 5_555 N O3 La1 O5 138.1(10) 6_555 . 6_554 N O3 La1 O5 59.4(13) 6_555 . -1_556 N O3 La1 O5 160.9(19) 6_555 . -2_556 N O3 La1 O5 84.9(10) 6_555 . -3_556 N O3 La1 O3 136.87(16) -3_555 . -4_556 N O3 La1 O4 105.36(11) -3_555 . 1_555 N O3 La1 O5 59.4(13) -3_555 . 4_554 N O3 La1 O5 160.9(19) -3_555 . 5_555 N O3 La1 O5 84.9(10) -3_555 . 6_554 N O3 La1 O5 110.9(13) -3_555 . -1_556 N O3 La1 O5 25.0(17) -3_555 . -2_556 N O3 La1 O5 138.1(10) -3_555 . -3_556 N O3 La1 O4 84.10(12) -4_556 . 1_555 N O3 La1 O5 146.3(12) -4_556 . 4_554 N O3 La1 O5 57.4(18) -4_556 . 5_555 N O3 La1 O5 62.9(10) -4_556 . 6_554 N O3 La1 O5 110.6(12) -4_556 . -1_556 N O3 La1 O5 119.2(18) -4_556 . -2_556 N O3 La1 O5 23.4(15) -4_556 . -3_556 N O4 La1 O5 62.2(12) 1_555 . 4_554 N O4 La1 O5 87.3(13) 1_555 . 5_555 N O4 La1 O5 60.7(16) 1_555 . 6_554 N O4 La1 O5 62.2(12) 1_555 . -1_556 N O4 La1 O5 87.3(13) 1_555 . -2_556 N O4 La1 O5 60.7(16) 1_555 . -3_556 N O5 La1 O5 117.5(24) 4_554 . 5_555 N O5 La1 O5 97.1(24) 4_554 . 6_554 N O5 La1 O5 55.6(27) 4_554 . -1_556 N O5 La1 O5 62.0(13) 4_554 . -2_556 N O5 La1 O5 122.8(21) 4_554 . -3_556 N O5 La1 O5 114.0(24) 5_555 . 6_554 N O5 La1 O5 62.0(13) 5_555 . -1_556 N O5 La1 O5 173.9(33) 5_555 . -2_556 N O5 La1 O5 60.6(19) 5_555 . -3_556 N O5 La1 O5 122.8(21) 6_554 . -1_556 N O5 La1 O5 60.6(19) 6_554 . -2_556 N O5 La1 O5 53.4(20) 6_554 . -3_556 N O5 La1 O5 117.5(24) -1_556 . -2_556 N O5 La1 O5 97.1(24) -1_556 . -3_556 N O5 La1 O5 114.0(24) -2_556 . -3_556 N La2 La2 La2 179.9604 -2_565 . -2_566 N La2 La2 O1 137.07(10) -2_565 . 1_555 N La2 La2 O1 137.08(10) -2_565 . 3_665 N La2 La2 O1 137.11(10) -2_565 . 5_565 N La2 La2 O2 44.48(10) -2_565 . 2_554 N La2 La2 O2 44.47(10) -2_565 . 4_664 N La2 La2 O2 44.46(10) -2_565 . 6_564 N La2 La2 O1 42.91(10) -2_566 . 1_555 N La2 La2 O1 42.90(10) -2_566 . 3_665 N La2 La2 O1 42.92(10) -2_566 . 5_565 N La2 La2 O2 135.55(10) -2_566 . 2_554 N La2 La2 O2 135.51(10) -2_566 . 4_664 N La2 La2 O2 135.53(10) -2_566 . 6_564 N O1 La2 O1 72.26(15) 1_555 . 3_665 N O1 La2 O1 72.27(15) 1_555 . 5_565 N O1 La2 O2 125.66(12) 1_555 . 2_554 N O1 La2 O2 94.73(8) 1_555 . 4_664 N O1 La2 O2 154.44(13) 1_555 . 6_564 N O1 La2 O1 72.27(15) 3_665 . 5_565 N O1 La2 O2 154.48(13) 3_665 . 2_554 N O1 La2 O2 125.64(12) 3_665 . 4_664 N O1 La2 O2 94.75(8) 3_665 . 6_564 N O1 La2 O2 94.76(8) 5_565 . 2_554 N O1 La2 O2 154.46(13) 5_565 . 4_664 N O1 La2 O2 125.68(12) 5_565 . 6_564 N O2 La2 O2 74.70(15) 2_554 . 4_664 N O2 La2 O2 74.70(15) 2_554 . 6_564 N O2 La2 O2 74.69(15) 4_664 . 6_564 N O1 Ge O2 114.73(28) 1_555 . 1_555 N O1 Ge O3 111.27(16) 1_555 . 1_555 N O1 Ge O3 111.27(16) 1_555 . -4_556 N O1 Ge O5 88.7(21) 1_555 . 6_554 N O1 Ge O5 88.7(21) 1_555 . -3_556 N O2 Ge O3 106.90(18) 1_555 . 1_555 N O2 Ge O3 106.90(18) 1_555 . -4_556 N O2 Ge O5 138.6(18) 1_555 . 6_554 N O2 Ge O5 138.6(18) 1_555 . -3_556 N O3 Ge O3 105.20(26) 1_555 . -4_556 N O3 Ge O5 31.9(18) 1_555 . 6_554 N O3 Ge O5 94.1(14) 1_555 . -3_556 N O3 Ge O5 94.1(14) -4_556 . 6_554 N O3 Ge O5 31.9(18) -4_556 . -3_556 N O5 Ge O5 70.8(28) 6_554 . -3_556 N La2 O1 La2 94.17(19) 1_555 . -2_566 N La2 O1 Ge 126.55(12) 1_555 . 1_555 N La2 O1 Ge 126.53(12) -2_566 . 1_555 N La1 O2 La2 116.60(12) 5_665 . 2_655 N La1 O2 La2 116.59(12) 5_665 . -1_665 N La1 O2 Ge 121.85(26) 5_665 . 1_555 N La2 O2 La2 91.06(20) 2_655 . -1_665 N La2 O2 Ge 102.79(14) 2_655 . 1_555 N La2 O2 Ge 102.81(14) -1_665 . 1_555 N La1 O3 La1 115.55(16) 1_555 . 2_554 N La1 O3 Ge 96.41(15) 1_555 . 1_555 N La1 O3 O5 76.0(32) 1_555 . 6_554 N La1 O3 Ge 141.49(20) 2_554 . 1_555 N La1 O3 O5 78.2(26) 2_554 . 6_554 N Ge O3 O5 90.1(24) 1_555 . 6_554 N La1 O4 La1 120.0 1_555 . 3_555 N La1 O4 La1 120.0 1_555 . 5_555 N La1 O4 La1 120.0 3_555 . 5_555 N La1 O5 La1 116.6(22) 2_555 . 3_555 N La1 O5 La1 104.2(18) 2_555 . 4_555 N La1 O5 Ge 90.5(25) 2_555 . 2_555 N La1 O5 O3 81(4) 2_555 . 2_555 N La1 O5 La1 120.3(30) 3_555 . 4_555 N La1 O5 Ge 122.6(26) 3_555 . 2_555 N La1 O5 O3 76.8(25) 3_555 . 2_555 N La1 O5 Ge 97.1(19) 4_555 . 2_555 N La1 O5 O3 155.0(35) 4_555 . 2_555 N Ge O5 O3 58.0(26) 2_555 . 2_555 N # Powder diffraction data for histogram 1 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_length_neutron _atom_type_scat_source LA 9.6 0.8240 International_Tables_Vol_C GE 6.0 0.8185 International_Tables_Vol_C O 26.458 0.5803 International_Tables_Vol_C _diffrn_radiation_probe neutron _diffrn_radiation_wavelength 1.88604 _pd_proc_ls_prof_R_factor 0.0242 _pd_proc_ls_prof_wR_factor 0.0319 _pd_proc_ls_prof_wR_expected 0.0134 _refine_ls_R_Fsqd_factor 0.41286 _pd_proc_ls_background_function ; GSAS Background function number 1 with 20 terms. Shifted Chebyshev function of 1st kind 1: 4480.34 2: 1486.73 3: -252.024 4: -41.6234 5: 196.354 6: -90.1996 7: 131.306 8: 54.5032 9: -86.9946 10: -2.25287 11: 67.1059 12: -63.7134 13: -23.8562 14: 99.2931 15: 11.6076 16: -61.3141 17: -10.3926 18: 14.1177 19: -20.2926 20: 1.73966 ; _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_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 316.000 #2(GV) = -680.575 #3(GW) = 557.587 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 14.7768 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00500 _pd_proc_info_datetime 2003-09-18T17:10:41 _pd_calc_method 'Rietveld Refinement' #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_La960Ge_773k_publ _database_code_depnum_ccdc_archive 'CCDC 230203' _pd_block_id 2003-09-18T17:07|La960Ge_773k|La960Ge_773K|Overall _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2003-09-18T17:07 _audit_author_name La960Ge_773K _audit_update_record ; 2003-09-18T17:07 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= #data_La960Ge_773k_overall _refine_ls_shift/su_max 0.38 _refine_ls_shift/su_mean 0.08 _computing_structure_refinement GSAS _refine_ls_number_parameters 72 _refine_ls_goodness_of_fit_all 2.09 _refine_ls_number_restraints 0 _refine_ls_matrix_type full # pointers to the phase blocks loop_ _pd_phase_block_id 2003-09-18T17:07|La960Ge_773k_phase1|La960Ge_773K|| 2003-09-18T17:07|La960Ge_773k_phase2|La960Ge_773K|| 2003-09-18T17:07|La960Ge_773k_phase3|La960Ge_773K|| # pointers to the diffraction patterns #loop_ #_pd_block_diffractogram_id #2003-09-18T17:07|La960Ge_773k_H_01|La960Ge_773K|HRPT # Information for phase 1 #data_La960Ge_773k_phase_1 #_pd_block_id #2003-09-18T17:07|La960Ge_773k_phase1|La960Ge_773K|| # Histograms for phase 1 #loop_ #_pd_block_diffractogram_id #2003-09-18T17:07|La960Ge_773k_H_01|La960Ge_773K|HRPT #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from C:/users/leon/La960GeGe_sinQ/La960Ge(O4).EXP' _cell_length_a 9.96580(19) _cell_length_b 9.9658 _cell_length_c 7.31160(16) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 628.87958 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z+1/2 3 -y,x-y,+z 4 -x,-y,+z+1/2 5 y-x,-x,+z 6 +y,y-x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z+1/2 -3 +y,y-x,-z -4 +x,+y,-z+1/2 -5 x-y,+x,-z -6 -y,x-y,-z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity LA La1 0.22897(22) -0.01249(27) 0.25 1.0 Uani 0.02777 6 LA La2 0.3333 0.6667 0.0034(4) 0.9 Uani 0.03354 4 GE Ge 0.40015(24) 0.37321(22) 0.25 1.0 Uani 0.02234 6 O O1 0.3132(4) 0.4869(4) 0.25 1.0 Uani 0.05092 6 O O2 0.60202(34) 0.47181(34) 0.25 1.0 Uani 0.03934 6 O O3 0.3428(4) 0.24979(29) 0.06095(29) 1.0 Uani 0.06446 12 O O4 0.0 0.0 0.25 0.937(13) Uani 0.06959 2 O O5 0.010(5) 0.234(5) 0.605(4) 0.058(4) Uiso 0.03 12 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 La1 0.0274(13) 0.0060(11) 0.0 0.0176(12) 0.0 0.0313(10) La2 0.0365(12) 0.0182(6) 0.0 0.0365(12) 0.0 0.0277(17) Ge 0.0229(11) 0.0114(11) 0.0 0.0183(11) 0.0 0.0273(11) O1 0.0859(32) 0.0520(26) 0.0 0.0580(27) 0.0 0.0303(22) O2 0.0292(19) 0.0132(17) 0.0 0.0280(18) 0.0 0.0594(25) O3 0.1095(26) 0.0468(17) -0.0373(18) 0.0462(17) -0.0226(14) 0.0483(17) O4 0.0231(24) 0.0116(12) 0.0 0.0231(24) 0.0 0.162(8) loop_ _atom_type_symbol _atom_type_number_in_cell LA 9.6 GE 6.0 O 26.57 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'Ge La1.60 O4.43' _chemical_formula_weight 365.70 _cell_formula_units_Z 6 # MOLECULAR GEOMETRY 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 La1 La1 4.0645(29) . 3_555 N La1 La1 4.0645(29) . 5_555 N La1 Ge 3.3359(33) . 1_555 N La1 Ge 3.4025(31) . 5_555 N La1 O1 2.763(5) . 5_555 N La1 O2 2.5834(31) . 3_655 N La1 O3 2.6580(32) . 1_555 N La1 O3 2.4540(22) . 6_555 N La1 O3 2.4540(22) . -3_555 N La1 O3 2.6580(32) . -4_556 N La1 O4 2.3466(17) . 1_555 N La1 O5 2.53(4) . 4_554 N La1 O5 2.599(29) . 5_555 N La1 O5 2.56(4) . 6_554 N La1 O5 2.53(4) . -1_556 N La1 O5 2.599(29) . -2_556 N La1 O5 2.56(4) . -3_556 N La2 La2 3.705(6) . -2_565 N La2 La2 3.607(6) . -2_566 N La2 Ge 3.4204(22) . 2_554 N La2 Ge 3.4209(22) . 4_664 N La2 Ge 3.4200(22) . 6_564 N La2 O1 2.4789(32) . 1_555 N La2 O1 2.4786(32) . 3_665 N La2 O1 2.4782(32) . 5_565 N La2 O2 2.5766(32) . 2_554 N La2 O2 2.5772(32) . 4_664 N La2 O2 2.5767(32) . 6_564 N La2 O3 2.941(4) . -1_665 N La2 O3 2.940(4) . -3_565 N La2 O3 2.940(4) . -5_555 N Ge La1 3.3359(33) . 1_555 N Ge La1 3.4025(31) . 3_555 N Ge La2 3.4200(22) . 2_655 N Ge La2 3.4209(22) . -1_665 N Ge O1 1.7365(32) . 1_555 N Ge O2 1.7424(30) . 1_555 N Ge O3 1.7456(24) . 1_555 N Ge O3 1.7456(24) . -4_556 N Ge O5 1.900(34) . 6_554 N Ge O5 1.900(34) . -3_556 N O1 La1 2.763(5) . 3_555 N O1 La2 2.4789(32) . 1_555 N O1 La2 2.4786(32) . -2_566 N O1 Ge 1.7365(32) . 1_555 N O2 La1 2.5834(31) . 5_665 N O2 La2 2.5767(32) . 2_655 N O2 La2 2.5772(32) . -1_665 N O2 Ge 1.7424(30) . 1_555 N O3 La1 2.6580(32) . 1_555 N O3 La1 2.4540(22) . 2_554 N O3 La2 2.941(4) . -1_665 N O3 Ge 1.7456(24) . 1_555 N O3 O5 1.04(4) . 6_554 N O4 La1 2.3466(17) . 1_555 N O4 La1 2.3466(17) . 3_555 N O4 La1 2.3466(17) . 5_555 N O5 La1 2.56(4) . 2_555 N O5 La1 2.599(29) . 3_555 N O5 La1 2.53(4) . 4_555 N O5 Ge 1.900(34) . 2_555 N O5 O3 1.04(4) . 2_555 N O5 O5 2.12(6) . -4_557 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 O1 La1 O2 98.42(12) 5_555 . 3_655 N O1 La1 O3 145.32(7) 5_555 . 1_555 N O1 La1 O3 69.45(9) 5_555 . 6_555 N O1 La1 O3 69.45(9) 5_555 . -3_555 N O1 La1 O3 145.32(7) 5_555 . -4_556 N O1 La1 O4 112.68(11) 5_555 . 1_555 N O1 La1 O5 57.5(8) 5_555 . 4_554 N O1 La1 O5 91.0(10) 5_555 . 5_555 N O1 La1 O5 154.1(6) 5_555 . 6_554 N O1 La1 O5 57.5(8) 5_555 . -1_556 N O1 La1 O5 91.0(10) 5_555 . -2_556 N O1 La1 O5 154.1(6) 5_555 . -3_556 N O2 La1 O3 69.58(11) 3_655 . 1_555 N O2 La1 O3 85.24(8) 3_655 . 6_555 N O2 La1 O3 85.24(8) 3_655 . -3_555 N O2 La1 O3 69.58(11) 3_655 . -4_556 N O2 La1 O4 148.89(14) 3_655 . 1_555 N O2 La1 O5 143.5(8) 3_655 . 4_554 N O2 La1 O5 90.9(8) 3_655 . 5_555 N O2 La1 O5 90.5(9) 3_655 . 6_554 N O2 La1 O5 143.5(8) 3_655 . -1_556 N O2 La1 O5 90.9(8) 3_655 . -2_556 N O2 La1 O5 90.5(9) 3_655 . -3_556 N O3 La1 O3 137.65(12) 1_555 . 6_555 N O3 La1 O3 77.02(6) 1_555 . -3_555 N O3 La1 O3 62.67(11) 1_555 . -4_556 N O3 La1 O4 84.03(10) 1_555 . 1_555 N O3 La1 O5 113.1(7) 1_555 . 4_554 N O3 La1 O5 120.7(10) 1_555 . 5_555 N O3 La1 O5 22.8(9) 1_555 . 6_554 N O3 La1 O5 145.9(8) 1_555 . -1_556 N O3 La1 O5 58.0(10) 1_555 . -2_556 N O3 La1 O5 60.5(6) 1_555 . -3_556 N O3 La1 O3 135.78(20) 6_555 . -3_555 N O3 La1 O3 77.02(6) 6_555 . -4_556 N O3 La1 O4 105.12(9) 6_555 . 1_555 N O3 La1 O5 107.4(8) 6_555 . 4_554 N O3 La1 O5 23.5(10) 6_555 . 5_555 N O3 La1 O5 135.8(7) 6_555 . 6_554 N O3 La1 O5 61.5(8) 6_555 . -1_556 N O3 La1 O5 159.2(11) 6_555 . -2_556 N O3 La1 O5 87.3(6) 6_555 . -3_556 N O3 La1 O3 137.65(12) -3_555 . -4_556 N O3 La1 O4 105.12(9) -3_555 . 1_555 N O3 La1 O5 61.5(8) -3_555 . 4_554 N O3 La1 O5 159.2(11) -3_555 . 5_555 N O3 La1 O5 87.3(6) -3_555 . 6_554 N O3 La1 O5 107.4(8) -3_555 . -1_556 N O3 La1 O5 23.5(10) -3_555 . -2_556 N O3 La1 O5 135.8(7) -3_555 . -3_556 N O3 La1 O4 84.03(10) -4_556 . 1_555 N O3 La1 O5 145.9(8) -4_556 . 4_554 N O3 La1 O5 58.0(10) -4_556 . 5_555 N O3 La1 O5 60.5(6) -4_556 . 6_554 N O3 La1 O5 113.1(7) -4_556 . -1_556 N O3 La1 O5 120.7(10) -4_556 . -2_556 N O3 La1 O5 22.8(9) -4_556 . -3_556 N O4 La1 O5 62.0(8) 1_555 . 4_554 N O4 La1 O5 88.6(8) 1_555 . 5_555 N O4 La1 O5 61.5(10) 1_555 . 6_554 N O4 La1 O5 62.0(8) 1_555 . -1_556 N O4 La1 O5 88.6(8) 1_555 . -2_556 N O4 La1 O5 61.5(10) 1_555 . -3_556 N O5 La1 O5 114.4(14) 4_554 . 5_555 N O5 La1 O5 101.9(15) 4_554 . 6_554 N O5 La1 O5 49.5(15) 4_554 . -1_556 N O5 La1 O5 65.0(9) 4_554 . -2_556 N O5 La1 O5 123.5(14) 4_554 . -3_556 N O5 La1 O5 113.2(14) 5_555 . 6_554 N O5 La1 O5 65.0(9) 5_555 . -1_556 N O5 La1 O5 177.0(18) 5_555 . -2_556 N O5 La1 O5 64.5(10) 5_555 . -3_556 N O5 La1 O5 123.5(14) 6_554 . -1_556 N O5 La1 O5 64.5(10) 6_554 . -2_556 N O5 La1 O5 48.7(13) 6_554 . -3_556 N O5 La1 O5 114.4(14) -1_556 . -2_556 N O5 La1 O5 101.9(15) -1_556 . -3_556 N O5 La1 O5 113.2(14) -2_556 . -3_556 N La2 La2 La2 179.9604 -2_565 . -2_566 N La2 La2 O1 136.67(7) -2_565 . 1_555 N La2 La2 O1 136.67(7) -2_565 . 3_665 N La2 La2 O1 136.71(7) -2_565 . 5_565 N La2 La2 O2 44.05(7) -2_565 . 2_554 N La2 La2 O2 44.04(7) -2_565 . 4_664 N La2 La2 O2 44.03(7) -2_565 . 6_564 N La2 La2 O1 43.32(7) -2_566 . 1_555 N La2 La2 O1 43.31(7) -2_566 . 3_665 N La2 La2 O1 43.32(7) -2_566 . 5_565 N La2 La2 O2 135.98(7) -2_566 . 2_554 N La2 La2 O2 135.94(7) -2_566 . 4_664 N La2 La2 O2 135.96(7) -2_566 . 6_564 N O1 La2 O1 72.89(11) 1_555 . 3_665 N O1 La2 O1 72.90(11) 1_555 . 5_565 N O1 La2 O2 124.95(9) 1_555 . 2_554 N O1 La2 O2 95.00(7) 1_555 . 4_664 N O1 La2 O2 155.33(10) 1_555 . 6_564 N O1 La2 O1 72.90(11) 3_665 . 5_565 N O1 La2 O2 155.37(10) 3_665 . 2_554 N O1 La2 O2 124.93(9) 3_665 . 4_664 N O1 La2 O2 95.02(7) 3_665 . 6_564 N O1 La2 O2 95.03(7) 5_565 . 2_554 N O1 La2 O2 155.35(10) 5_565 . 4_664 N O1 La2 O2 124.97(9) 5_565 . 6_564 N O2 La2 O2 74.03(11) 2_554 . 4_664 N O2 La2 O2 74.03(11) 2_554 . 6_564 N O2 La2 O2 74.02(11) 4_664 . 6_564 N O1 Ge O2 116.36(21) 1_555 . 1_555 N O1 Ge O3 111.42(13) 1_555 . 1_555 N O1 Ge O3 111.42(13) 1_555 . -4_556 N O1 Ge O5 89.1(13) 1_555 . 6_554 N O1 Ge O5 89.1(13) 1_555 . -3_556 N O2 Ge O3 106.04(15) 1_555 . 1_555 N O2 Ge O3 106.04(15) 1_555 . -4_556 N O2 Ge O5 138.7(12) 1_555 . 6_554 N O2 Ge O5 138.7(12) 1_555 . -3_556 N O3 Ge O3 104.72(19) 1_555 . -4_556 N O3 Ge O5 32.7(12) 1_555 . 6_554 N O3 Ge O5 92.3(10) 1_555 . -3_556 N O3 Ge O5 92.3(10) -4_556 . 6_554 N O3 Ge O5 32.7(12) -4_556 . -3_556 N O5 Ge O5 67.6(20) 6_554 . -3_556 N La1 O1 La2 107.44(10) 3_555 . 1_555 N La1 O1 La2 107.46(10) 3_555 . -2_566 N La1 O1 Ge 95.55(16) 3_555 . 1_555 N La2 O1 La2 93.36(14) 1_555 . -2_566 N La2 O1 Ge 125.83(10) 1_555 . 1_555 N La2 O1 Ge 125.81(10) -2_566 . 1_555 N La1 O2 La2 116.74(9) 5_665 . 2_655 N La1 O2 La2 116.74(9) 5_665 . -1_665 N La1 O2 Ge 120.76(19) 5_665 . 1_555 N La2 O2 La2 91.92(14) 2_655 . -1_665 N La2 O2 Ge 103.01(11) 2_655 . 1_555 N La2 O2 Ge 103.03(11) -1_665 . 1_555 N La1 O3 La1 116.32(13) 1_555 . 2_554 N La1 O3 Ge 96.29(11) 1_555 . 1_555 N La1 O3 O5 73.5(21) 1_555 . 6_554 N La1 O3 Ge 140.28(15) 2_554 . 1_555 N La1 O3 O5 86.1(18) 2_554 . 6_554 N Ge O3 O5 81.9(17) 1_555 . 6_554 N La1 O4 La1 120.0 1_555 . 3_555 N La1 O4 La1 120.0 1_555 . 5_555 N La1 O4 La1 120.0 3_555 . 5_555 N La1 O5 La1 114.6(13) 2_555 . 3_555 N La1 O5 La1 105.9(13) 2_555 . 4_555 N La1 O5 Ge 95.6(15) 2_555 . 2_555 N La1 O5 O3 83.7(25) 2_555 . 2_555 N La1 O5 La1 115.9(16) 3_555 . 4_555 N La1 O5 Ge 122.4(17) 3_555 . 2_555 N La1 O5 O3 70.4(16) 3_555 . 2_555 N La1 O5 Ge 99.5(14) 4_555 . 2_555 N La1 O5 O3 163.2(26) 4_555 . 2_555 N Ge O5 O3 65.4(19) 2_555 . 2_555 N # Information for phase 2 data_La960Ge_773k_phase_2 _database_code_depnum_ccdc_archive 'CCDC 230204' _pd_block_id 2003-09-18T17:07|La960Ge_773k_phase2|La960Ge_773K|| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from C:/users/leon/fases/fe-gamma.cif' _cell_length_a 3.62266 _cell_length_b 3.62266 _cell_length_c 3.62266 _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 47.54258 _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F m 3 m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 +z,+x,+y 3 +y,+z,+x 4 +x,+y,-z 5 -z,+x,+y 6 +y,-z,+x 7 -z,+x,-y 8 -y,-z,+x 9 +y,-z,-x 10 -x,+y,-z 11 -z,-x,+y 12 +x,-y,-z 13 +y,+x,+z 14 +z,+y,+x 15 +x,+z,+y 16 +y,+x,-z 17 -z,+y,+x 18 +x,-z,+y 19 -z,+y,-x 20 -x,-z,+y 21 +x,-z,-y 22 -y,+x,-z 23 -z,-y,+x 24 +y,-x,-z -1 -x,-y,-z -2 -z,-x,-y -3 -y,-z,-x -4 -x,-y,+z -5 +z,-x,-y -6 -y,+z,-x -7 +z,-x,+y -8 +y,+z,-x -9 -y,+z,+x -10 +x,-y,+z -11 +z,+x,-y -12 -x,+y,+z -13 -y,-x,-z -14 -z,-y,-x -15 -x,-z,-y -16 -y,-x,+z -17 +z,-y,-x -18 -x,+z,-y -19 +z,-y,+x -20 +x,+z,-y -21 -x,+z,+y -22 +y,-x,+z -23 +z,+y,-x -24 -y,+x,+z 101 +x,+y+1/2,+z+1/2 102 +z,+x+1/2,+y+1/2 103 +y,+z+1/2,+x+1/2 104 +x,+y+1/2,-z+1/2 105 -z,+x+1/2,+y+1/2 106 +y,-z+1/2,+x+1/2 107 -z,+x+1/2,-y+1/2 108 -y,-z+1/2,+x+1/2 109 +y,-z+1/2,-x+1/2 110 -x,+y+1/2,-z+1/2 111 -z,-x+1/2,+y+1/2 112 +x,-y+1/2,-z+1/2 113 +y,+x+1/2,+z+1/2 114 +z,+y+1/2,+x+1/2 115 +x,+z+1/2,+y+1/2 116 +y,+x+1/2,-z+1/2 117 -z,+y+1/2,+x+1/2 118 +x,-z+1/2,+y+1/2 119 -z,+y+1/2,-x+1/2 120 -x,-z+1/2,+y+1/2 121 +x,-z+1/2,-y+1/2 122 -y,+x+1/2,-z+1/2 123 -z,-y+1/2,+x+1/2 124 +y,-x+1/2,-z+1/2 -101 -x,-y+1/2,-z+1/2 -102 -z,-x+1/2,-y+1/2 -103 -y,-z+1/2,-x+1/2 -104 -x,-y+1/2,+z+1/2 -105 +z,-x+1/2,-y+1/2 -106 -y,+z+1/2,-x+1/2 -107 +z,-x+1/2,+y+1/2 -108 +y,+z+1/2,-x+1/2 -109 -y,+z+1/2,+x+1/2 -110 +x,-y+1/2,+z+1/2 -111 +z,+x+1/2,-y+1/2 -112 -x,+y+1/2,+z+1/2 -113 -y,-x+1/2,-z+1/2 -114 -z,-y+1/2,-x+1/2 -115 -x,-z+1/2,-y+1/2 -116 -y,-x+1/2,+z+1/2 -117 +z,-y+1/2,-x+1/2 -118 -x,+z+1/2,-y+1/2 -119 +z,-y+1/2,+x+1/2 -120 +x,+z+1/2,-y+1/2 -121 -x,+z+1/2,+y+1/2 -122 +y,-x+1/2,+z+1/2 -123 +z,+y+1/2,-x+1/2 -124 -y,+x+1/2,+z+1/2 201 +x+1/2,+y,+z+1/2 202 +z+1/2,+x,+y+1/2 203 +y+1/2,+z,+x+1/2 204 +x+1/2,+y,-z+1/2 205 -z+1/2,+x,+y+1/2 206 +y+1/2,-z,+x+1/2 207 -z+1/2,+x,-y+1/2 208 -y+1/2,-z,+x+1/2 209 +y+1/2,-z,-x+1/2 210 -x+1/2,+y,-z+1/2 211 -z+1/2,-x,+y+1/2 212 +x+1/2,-y,-z+1/2 213 +y+1/2,+x,+z+1/2 214 +z+1/2,+y,+x+1/2 215 +x+1/2,+z,+y+1/2 216 +y+1/2,+x,-z+1/2 217 -z+1/2,+y,+x+1/2 218 +x+1/2,-z,+y+1/2 219 -z+1/2,+y,-x+1/2 220 -x+1/2,-z,+y+1/2 221 +x+1/2,-z,-y+1/2 222 -y+1/2,+x,-z+1/2 223 -z+1/2,-y,+x+1/2 224 +y+1/2,-x,-z+1/2 -201 -x+1/2,-y,-z+1/2 -202 -z+1/2,-x,-y+1/2 -203 -y+1/2,-z,-x+1/2 -204 -x+1/2,-y,+z+1/2 -205 +z+1/2,-x,-y+1/2 -206 -y+1/2,+z,-x+1/2 -207 +z+1/2,-x,+y+1/2 -208 +y+1/2,+z,-x+1/2 -209 -y+1/2,+z,+x+1/2 -210 +x+1/2,-y,+z+1/2 -211 +z+1/2,+x,-y+1/2 -212 -x+1/2,+y,+z+1/2 -213 -y+1/2,-x,-z+1/2 -214 -z+1/2,-y,-x+1/2 -215 -x+1/2,-z,-y+1/2 -216 -y+1/2,-x,+z+1/2 -217 +z+1/2,-y,-x+1/2 -218 -x+1/2,+z,-y+1/2 -219 +z+1/2,-y,+x+1/2 -220 +x+1/2,+z,-y+1/2 -221 -x+1/2,+z,+y+1/2 -222 +y+1/2,-x,+z+1/2 -223 +z+1/2,+y,-x+1/2 -224 -y+1/2,+x,+z+1/2 301 +x+1/2,+y+1/2,+z 302 +z+1/2,+x+1/2,+y 303 +y+1/2,+z+1/2,+x 304 +x+1/2,+y+1/2,-z 305 -z+1/2,+x+1/2,+y 306 +y+1/2,-z+1/2,+x 307 -z+1/2,+x+1/2,-y 308 -y+1/2,-z+1/2,+x 309 +y+1/2,-z+1/2,-x 310 -x+1/2,+y+1/2,-z 311 -z+1/2,-x+1/2,+y 312 +x+1/2,-y+1/2,-z 313 +y+1/2,+x+1/2,+z 314 +z+1/2,+y+1/2,+x 315 +x+1/2,+z+1/2,+y 316 +y+1/2,+x+1/2,-z 317 -z+1/2,+y+1/2,+x 318 +x+1/2,-z+1/2,+y 319 -z+1/2,+y+1/2,-x 320 -x+1/2,-z+1/2,+y 321 +x+1/2,-z+1/2,-y 322 -y+1/2,+x+1/2,-z 323 -z+1/2,-y+1/2,+x 324 +y+1/2,-x+1/2,-z -301 -x+1/2,-y+1/2,-z -302 -z+1/2,-x+1/2,-y -303 -y+1/2,-z+1/2,-x -304 -x+1/2,-y+1/2,+z -305 +z+1/2,-x+1/2,-y -306 -y+1/2,+z+1/2,-x -307 +z+1/2,-x+1/2,+y -308 +y+1/2,+z+1/2,-x -309 -y+1/2,+z+1/2,+x -310 +x+1/2,-y+1/2,+z -311 +z+1/2,+x+1/2,-y -312 -x+1/2,+y+1/2,+z -313 -y+1/2,-x+1/2,-z -314 -z+1/2,-y+1/2,-x -315 -x+1/2,-z+1/2,-y -316 -y+1/2,-x+1/2,+z -317 +z+1/2,-y+1/2,-x -318 -x+1/2,+z+1/2,-y -319 +z+1/2,-y+1/2,+x -320 +x+1/2,+z+1/2,-y -321 -x+1/2,+z+1/2,+y -322 +y+1/2,-x+1/2,+z -323 +z+1/2,+y+1/2,-x -324 -y+1/2,+x+1/2,+z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity FE Fe1 0.0 0.0 0.0 1.0 Uiso 0.00777 4 loop_ _atom_type_symbol _atom_type_number_in_cell FE 4.0 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum Fe _chemical_formula_weight 55.85 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY 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 Fe1 Fe1 2.56161 . 101_544 N Fe1 Fe1 2.56161 . 101_545 N Fe1 Fe1 2.56161 . 101_554 N Fe1 Fe1 2.56161 . 101_555 N Fe1 Fe1 2.56161 . 201_454 N Fe1 Fe1 2.56161 . 201_455 N Fe1 Fe1 2.56161 . 201_554 N Fe1 Fe1 2.56161 . 201_555 N Fe1 Fe1 2.56161 . 301_445 N Fe1 Fe1 2.56161 . 301_455 N Fe1 Fe1 2.56161 . 301_545 N Fe1 Fe1 2.56161 . 301_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 ? ? ? ? ? ? ? ? # Information for phase 3 data_La960Ge_773k_phase_3 _database_code_depnum_ccdc_archive 'CCDC 230205' _pd_block_id 2003-09-18T17:07|La960Ge_773k_phase3|La960Ge_773K|| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from C:/users/leon/fases/fe-alfa.cif' _cell_length_a 2.886 _cell_length_b 2.886 _cell_length_c 2.886 _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 24.03748 _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I m 3 m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 +z,+x,+y 3 +y,+z,+x 4 +x,+y,-z 5 -z,+x,+y 6 +y,-z,+x 7 -z,+x,-y 8 -y,-z,+x 9 +y,-z,-x 10 -x,+y,-z 11 -z,-x,+y 12 +x,-y,-z 13 +y,+x,+z 14 +z,+y,+x 15 +x,+z,+y 16 +y,+x,-z 17 -z,+y,+x 18 +x,-z,+y 19 -z,+y,-x 20 -x,-z,+y 21 +x,-z,-y 22 -y,+x,-z 23 -z,-y,+x 24 +y,-x,-z -1 -x,-y,-z -2 -z,-x,-y -3 -y,-z,-x -4 -x,-y,+z -5 +z,-x,-y -6 -y,+z,-x -7 +z,-x,+y -8 +y,+z,-x -9 -y,+z,+x -10 +x,-y,+z -11 +z,+x,-y -12 -x,+y,+z -13 -y,-x,-z -14 -z,-y,-x -15 -x,-z,-y -16 -y,-x,+z -17 +z,-y,-x -18 -x,+z,-y -19 +z,-y,+x -20 +x,+z,-y -21 -x,+z,+y -22 +y,-x,+z -23 +z,+y,-x -24 -y,+x,+z 101 +x+1/2,+y+1/2,+z+1/2 102 +z+1/2,+x+1/2,+y+1/2 103 +y+1/2,+z+1/2,+x+1/2 104 +x+1/2,+y+1/2,-z+1/2 105 -z+1/2,+x+1/2,+y+1/2 106 +y+1/2,-z+1/2,+x+1/2 107 -z+1/2,+x+1/2,-y+1/2 108 -y+1/2,-z+1/2,+x+1/2 109 +y+1/2,-z+1/2,-x+1/2 110 -x+1/2,+y+1/2,-z+1/2 111 -z+1/2,-x+1/2,+y+1/2 112 +x+1/2,-y+1/2,-z+1/2 113 +y+1/2,+x+1/2,+z+1/2 114 +z+1/2,+y+1/2,+x+1/2 115 +x+1/2,+z+1/2,+y+1/2 116 +y+1/2,+x+1/2,-z+1/2 117 -z+1/2,+y+1/2,+x+1/2 118 +x+1/2,-z+1/2,+y+1/2 119 -z+1/2,+y+1/2,-x+1/2 120 -x+1/2,-z+1/2,+y+1/2 121 +x+1/2,-z+1/2,-y+1/2 122 -y+1/2,+x+1/2,-z+1/2 123 -z+1/2,-y+1/2,+x+1/2 124 +y+1/2,-x+1/2,-z+1/2 -101 -x+1/2,-y+1/2,-z+1/2 -102 -z+1/2,-x+1/2,-y+1/2 -103 -y+1/2,-z+1/2,-x+1/2 -104 -x+1/2,-y+1/2,+z+1/2 -105 +z+1/2,-x+1/2,-y+1/2 -106 -y+1/2,+z+1/2,-x+1/2 -107 +z+1/2,-x+1/2,+y+1/2 -108 +y+1/2,+z+1/2,-x+1/2 -109 -y+1/2,+z+1/2,+x+1/2 -110 +x+1/2,-y+1/2,+z+1/2 -111 +z+1/2,+x+1/2,-y+1/2 -112 -x+1/2,+y+1/2,+z+1/2 -113 -y+1/2,-x+1/2,-z+1/2 -114 -z+1/2,-y+1/2,-x+1/2 -115 -x+1/2,-z+1/2,-y+1/2 -116 -y+1/2,-x+1/2,+z+1/2 -117 +z+1/2,-y+1/2,-x+1/2 -118 -x+1/2,+z+1/2,-y+1/2 -119 +z+1/2,-y+1/2,+x+1/2 -120 +x+1/2,+z+1/2,-y+1/2 -121 -x+1/2,+z+1/2,+y+1/2 -122 +y+1/2,-x+1/2,+z+1/2 -123 +z+1/2,+y+1/2,-x+1/2 -124 -y+1/2,+x+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity FE Fe1 0.0 0.0 0.0 1.0 Uiso 0.0025 2 loop_ _atom_type_symbol _atom_type_number_in_cell FE 2.0 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum Fe _chemical_formula_weight 55.85 _cell_formula_units_Z 2 # MOLECULAR GEOMETRY 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 Fe1 Fe1 2.886 . 1_455 N Fe1 Fe1 2.886 . 1_545 N Fe1 Fe1 2.886 . 1_554 N Fe1 Fe1 2.886 . 1_556 N Fe1 Fe1 2.886 . 1_565 N Fe1 Fe1 2.886 . 1_655 N Fe1 Fe1 2.49935 . 101_444 N Fe1 Fe1 2.49935 . 101_445 N Fe1 Fe1 2.49935 . 101_454 N Fe1 Fe1 2.49935 . 101_455 N Fe1 Fe1 2.49935 . 101_544 N Fe1 Fe1 2.49935 . 101_545 N Fe1 Fe1 2.49935 . 101_554 N Fe1 Fe1 2.49935 . 101_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 Fe1 Fe1 Fe1 70.5288 101_444 . 101_445 N Fe1 Fe1 Fe1 70.5288 101_444 . 101_454 N Fe1 Fe1 Fe1 109.4712 101_444 . 101_455 N Fe1 Fe1 Fe1 70.5288 101_444 . 101_544 N Fe1 Fe1 Fe1 109.4712 101_444 . 101_545 N Fe1 Fe1 Fe1 109.4712 101_444 . 101_554 N Fe1 Fe1 Fe1 179.972 101_444 . 101_555 N Fe1 Fe1 Fe1 109.4712 101_445 . 101_454 N Fe1 Fe1 Fe1 70.5288 101_445 . 101_455 N Fe1 Fe1 Fe1 109.4712 101_445 . 101_544 N Fe1 Fe1 Fe1 70.5288 101_445 . 101_545 N Fe1 Fe1 Fe1 180.0 101_445 . 101_554 N Fe1 Fe1 Fe1 109.4712 101_445 . 101_555 N Fe1 Fe1 Fe1 70.5288 101_454 . 101_455 N Fe1 Fe1 Fe1 109.4712 101_454 . 101_544 N Fe1 Fe1 Fe1 180.0 101_454 . 101_545 N Fe1 Fe1 Fe1 70.5288 101_454 . 101_554 N Fe1 Fe1 Fe1 109.4712 101_454 . 101_555 N Fe1 Fe1 Fe1 180.0 101_455 . 101_544 N Fe1 Fe1 Fe1 109.4712 101_455 . 101_545 N Fe1 Fe1 Fe1 109.4712 101_455 . 101_554 N Fe1 Fe1 Fe1 70.5288 101_455 . 101_555 N Fe1 Fe1 Fe1 70.5288 101_544 . 101_545 N Fe1 Fe1 Fe1 70.5288 101_544 . 101_554 N Fe1 Fe1 Fe1 109.4712 101_544 . 101_555 N Fe1 Fe1 Fe1 109.4712 101_545 . 101_554 N Fe1 Fe1 Fe1 70.5288 101_545 . 101_555 N Fe1 Fe1 Fe1 70.5288 101_554 . 101_555 N # Powder diffraction data for histogram 1 #data_La960Ge_773k_p_01 #_pd_block_id #2003-09-18T17:07|La960Ge_773k_H_01|La960Ge_773K|HRPT #============================================================================== #loop_ #_pd_phase_id #_pd_phase_block_id #_pd_phase_mass_% #_pd_proc_ls_profile_function #_pd_proc_ls_peak_cutoff #1 2003-09-18T17:07|La960Ge_773k_phase1|La960Ge_773K|| 100.0 #; #CW Profile function number 2 with 18 terms #Profile coefficients for Simpson's rule integration of pseudovoigt function #C.J. Howard (1982). J. Appl. Cryst.,15,615-620. #P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 101.843 #2(GV) = -291.110 #3(GW) = 376.839 #4(LX) = 0.000 #5(LY) = 7.566 #6(trns) = 0.000 #7(asym) = 20.3280 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 #Peak tails are ignored where the intensity is below 0.0050 times the peak #Aniso. broadening axis 0.0 0.0 1.0 #; #0.00500 #loop_ #_atom_type_symbol #_atom_type_scat_length_neutron #_atom_type_scat_source #LA 0.8240 International_Tables_Vol_C #GE 0.8185 International_Tables_Vol_C #O 0.5803 International_Tables_Vol_C #FE 0.9450 International_Tables_Vol_C #_diffrn_radiation_probe neutron #_diffrn_radiation_wavelength 1.88604 #_pd_proc_ls_prof_R_factor 0.0236 #_pd_proc_ls_prof_wR_factor 0.0297 #_pd_proc_ls_prof_wR_expected 0.0144 #_refine_ls_R_Fsqd_factor 0.05907 #_pd_proc_ls_background_function #; GSAS Background function number 1 with 20 terms. #Shifted Chebyshev function of 1st kind #1: 3657.85 2: 874.658 3: -156.880 4: -44.0621 #5: 109.995 6: -81.9636 7: 96.9632 8: 34.6446 #9: -75.8949 10: -10.3253 11: 35.3694 12: -50.4744 #13: -15.1058 14: 96.2921 15: 35.1857 16: -34.1330 #17: -5.30571 18: 2.57277 19: -15.6879 20: 12.5054 #; #_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_info_datetime 2003-09-18T17:07:11 _pd_calc_method 'Rietveld Refinement' #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_LA955_1173K_publ _database_code_depnum_ccdc_archive 'CCDC 230206' _pd_block_id 2003-09-18T15:57|LA955_1173K|| _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2003-09-18T15:57 _audit_update_record ; 2003-09-18T15:57 Initial CIF as created by GSAS2CIF ; _publ_section_title_footnote ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 1.17 _refine_ls_shift/su_mean 0.05 _computing_structure_refinement GSAS _refine_ls_number_parameters 72 _refine_ls_goodness_of_fit_all 1.99 _refine_ls_number_restraints 0 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from C:/users/leon/La955Si_sinQ/La955Si6_500C/LA955SI6_500C.EXP' _cell_length_a 9.80882(20) _cell_length_b 9.80882 _cell_length_c 7.23353(16) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 602.71912 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z+1/2 3 -y,x-y,+z 4 -x,-y,+z+1/2 5 y-x,-x,+z 6 +y,y-x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z+1/2 -3 +y,y-x,-z -4 +x,+y,-z+1/2 -5 x-y,+x,-z -6 -y,x-y,-z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity LA La1 0.22681(23) -0.01380(28) 0.25 1.0 Uani 0.03184 6 LA La2 0.3333 0.6667 0.0001(5) 0.887 Uani 0.04046 4 SI SI 0.4012(5) 0.3713(4) 0.25 1.0 Uani 0.02831 6 O O1 0.3245(4) 0.4849(4) 0.25 1.0 Uani 0.05749 6 O O2 0.5922(4) 0.4709(4) 0.25 1.0 Uani 0.04452 6 O O3 0.3455(4) 0.25975(27) 0.07049(26) 1.0 Uani 0.05969 12 O O4 0.0 0.0 0.25 0.983(18) Uani 0.10971 2 O O5 0.005(15) 0.237(13) 0.576(10) 0.023(4) Uiso 0.03 12 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 La1 0.0361(12) 0.0114(10) 0.0 0.0228(12) 0.0 0.0322(9) La2 0.0356(12) 0.0178(6) 0.0 0.0356(12) 0.0 0.0503(17) SI 0.0402(23) 0.0169(20) 0.0 0.0177(21) 0.0 0.0302(21) O1 0.0869(29) 0.0568(24) 0.0 0.0597(29) 0.0 0.0527(25) O2 0.0322(20) 0.0076(20) 0.0 0.0328(19) 0.0 0.0570(25) O3 0.0912(24) 0.0369(15) -0.0265(13) 0.0483(17) -0.0120(10) 0.0422(12) O4 0.0209(28) -0.0085(14) 0.0 0.0209(28) 0.0 0.262(11) # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'La1.59 O4.37 Si' _chemical_formula_weight 319.11 _cell_formula_units_Z 6 # MOLECULAR GEOMETRY 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 La1 La1 3.9758(32) . 3_555 N La1 La1 3.9758(32) . 5_555 N La1 SI 3.276(5) . 1_555 N La1 SI 3.349(5) . 5_555 N La1 O1 2.780(5) . 5_555 N La1 O2 2.573(4) . 3_655 N La1 O3 2.6677(32) . 1_555 N La1 O3 2.4911(21) . 6_555 N La1 O3 2.4911(21) . -3_555 N La1 O3 2.6677(32) . -4_556 N La1 O4 2.2954(19) . 1_555 N La1 O5 2.56(11) . 4_554 N La1 O5 2.36(7) . 5_555 N La1 O5 2.68(11) . 6_554 N La1 O5 2.56(11) . -1_556 N La1 O5 2.36(7) . -2_556 N La1 O5 2.68(11) . -3_556 N La2 La2 3.618(7) . -2_565 N La2 La2 3.615(7) . -2_566 N La2 SI 3.341(4) . 2_554 N La2 SI 3.341(4) . 4_664 N La2 SI 3.340(4) . 6_564 N La2 O1 2.5104(34) . 1_555 N La2 O1 2.5101(34) . 3_665 N La2 O1 2.5097(34) . 5_565 N La2 O2 2.5712(34) . 2_554 N La2 O2 2.5719(34) . 4_664 N La2 O2 2.5714(34) . 6_564 N La2 O3 2.904(4) . -1_665 N La2 O3 2.903(4) . -3_565 N La2 O3 2.903(4) . -5_555 N SI La1 3.276(5) . 1_555 N SI La1 3.349(5) . 3_555 N SI La2 3.340(4) . 2_655 N SI La2 3.341(4) . -1_665 N SI O1 1.627(5) . 1_555 N SI O2 1.623(4) . 1_555 N SI O3 1.6076(28) . 1_555 N SI O3 1.6076(28) . -4_556 N SI O5 1.96(10) . 6_554 N SI O5 1.96(10) . -3_556 N O1 La1 2.780(5) . 3_555 N O1 La2 2.5104(34) . 1_555 N O1 La2 2.5101(34) . -2_566 N O1 SI 1.627(5) . 1_555 N O2 La1 2.573(4) . 5_665 N O2 La2 2.5714(34) . 2_655 N O2 La2 2.5719(34) . -1_665 N O2 SI 1.623(4) . 1_555 N O3 La1 2.6677(32) . 1_555 N O3 La1 2.4911(21) . 2_554 N O3 La2 2.904(4) . -1_665 N O3 SI 1.6076(28) . 1_555 N O3 O5 0.96(12) . 6_554 N O4 La1 2.2954(19) . 1_555 N O4 La1 2.2954(19) . 3_555 N O4 La1 2.2954(19) . 5_555 N O5 La1 2.68(11) . 2_555 N O5 La1 2.36(7) . 3_555 N O5 La1 2.56(11) . 4_555 N O5 SI 1.96(10) . 2_555 N O5 O3 0.96(12) . 2_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 O2 La1 O3 70.78(10) 3_655 . 1_555 N O2 La1 O3 82.33(8) 3_655 . 6_555 N O2 La1 O3 82.33(8) 3_655 . -3_555 N O2 La1 O3 70.78(10) 3_655 . -4_556 N O2 La1 O4 150.58(14) 3_655 . 1_555 N O2 La1 O5 137.9(22) 3_655 . 4_554 N O2 La1 O5 89.0(23) 3_655 . 5_555 N O2 La1 O5 91.3(24) 3_655 . 6_554 N O2 La1 O5 137.9(22) 3_655 . -1_556 N O2 La1 O5 89.0(23) 3_655 . -2_556 N O2 La1 O5 91.3(24) 3_655 . -3_556 N O3 La1 O3 133.22(12) 1_555 . 6_555 N O3 La1 O3 77.23(6) 1_555 . -3_555 N O3 La1 O3 58.25(10) 1_555 . -4_556 N O3 La1 O4 83.64(10) 1_555 . 1_555 N O3 La1 O5 112.0(21) 1_555 . 4_554 N O3 La1 O5 117.3(31) 1_555 . 5_555 N O3 La1 O5 20.7(24) 1_555 . 6_554 N O3 La1 O5 148.5(21) 1_555 . -1_556 N O3 La1 O5 59.0(31) 1_555 . -2_556 N O3 La1 O5 61.4(17) 1_555 . -3_556 N O3 La1 O3 137.06(19) 6_555 . -3_555 N O3 La1 O3 77.23(6) 6_555 . -4_556 N O3 La1 O4 106.48(8) 6_555 . 1_555 N O3 La1 O5 113.6(22) 6_555 . 4_554 N O3 La1 O5 22.7(29) 6_555 . 5_555 N O3 La1 O5 137.8(16) 6_555 . 6_554 N O3 La1 O5 59.1(23) 6_555 . -1_556 N O3 La1 O5 159.6(29) 6_555 . -2_556 N O3 La1 O5 82.4(15) 6_555 . -3_556 N O3 La1 O3 133.22(12) -3_555 . -4_556 N O3 La1 O4 106.48(8) -3_555 . 1_555 N O3 La1 O5 59.1(23) -3_555 . 4_554 N O3 La1 O5 159.6(29) -3_555 . 5_555 N O3 La1 O5 82.4(15) -3_555 . 6_554 N O3 La1 O5 113.6(22) -3_555 . -1_556 N O3 La1 O5 22.7(29) -3_555 . -2_556 N O3 La1 O5 137.8(16) -3_555 . -3_556 N O3 La1 O4 83.64(10) -4_556 . 1_555 N O3 La1 O5 148.5(21) -4_556 . 4_554 N O3 La1 O5 59.0(31) -4_556 . 5_555 N O3 La1 O5 61.4(17) -4_556 . 6_554 N O3 La1 O5 112.0(21) -4_556 . -1_556 N O3 La1 O5 117.3(31) -4_556 . -2_556 N O3 La1 O5 20.7(24) -4_556 . -3_556 N O4 La1 O5 65.0(21) 1_555 . 4_554 N O4 La1 O5 90.0(24) 1_555 . 5_555 N O4 La1 O5 63.0(24) 1_555 . 6_554 N O4 La1 O5 65.0(21) 1_555 . -1_556 N O4 La1 O5 90.0(24) 1_555 . -2_556 N O4 La1 O5 63.0(24) 1_555 . -3_556 N O5 La1 O5 121(4) 4_554 . 5_555 N O5 La1 O5 99(4) 4_554 . 6_554 N O5 La1 O5 59(4) 4_554 . -1_556 N O5 La1 O5 62.3(24) 4_554 . -2_556 N O5 La1 O5 128.1(32) 4_554 . -3_556 N O5 La1 O5 116(4) 5_555 . 6_554 N O5 La1 O5 62.3(24) 5_555 . -1_556 N O5 La1 O5 176(6) 5_555 . -2_556 N O5 La1 O5 60.4(31) 5_555 . -3_556 N O5 La1 O5 128.1(32) 6_554 . -1_556 N O5 La1 O5 60.4(31) 6_554 . -2_556 N O5 La1 O5 56.0(31) 6_554 . -3_556 N O5 La1 O5 121(4) -1_556 . -2_556 N O5 La1 O5 99(4) -1_556 . -3_556 N O5 La1 O5 116(4) -2_556 . -3_556 N La2 La2 La2 179.9604 -2_565 . -2_566 N La2 La2 O1 136.06(7) -2_565 . 1_555 N La2 La2 O1 136.06(7) -2_565 . 3_665 N La2 La2 O1 136.09(7) -2_565 . 5_565 N La2 La2 O2 45.30(8) -2_565 . 2_554 N La2 La2 O2 45.29(8) -2_565 . 4_664 N La2 La2 O2 45.29(8) -2_565 . 6_564 N La2 La2 O1 43.93(7) -2_566 . 1_555 N La2 La2 O1 43.92(7) -2_566 . 3_665 N La2 La2 O1 43.94(7) -2_566 . 5_565 N La2 La2 O2 134.73(8) -2_566 . 2_554 N La2 La2 O2 134.69(8) -2_566 . 4_664 N La2 La2 O2 134.71(8) -2_566 . 6_564 N O1 La2 O1 73.85(11) 1_555 . 3_665 N O1 La2 O1 73.86(11) 1_555 . 5_565 N O1 La2 O2 124.69(9) 1_555 . 2_554 N O1 La2 O2 92.96(6) 1_555 . 4_664 N O1 La2 O2 154.01(10) 1_555 . 6_564 N O1 La2 O1 73.86(11) 3_665 . 5_565 N O1 La2 O2 154.05(10) 3_665 . 2_554 N O1 La2 O2 124.67(9) 3_665 . 4_664 N O1 La2 O2 92.98(6) 3_665 . 6_564 N O1 La2 O2 92.99(6) 5_565 . 2_554 N O1 La2 O2 154.02(10) 5_565 . 4_664 N O1 La2 O2 124.71(9) 5_565 . 6_564 N O2 La2 O2 75.97(12) 2_554 . 4_664 N O2 La2 O2 75.98(12) 2_554 . 6_564 N O2 La2 O2 75.97(12) 4_664 . 6_564 N O1 SI O2 112.21(30) 1_555 . 1_555 N O1 SI O3 110.49(19) 1_555 . 1_555 N O1 SI O3 110.49(19) 1_555 . -4_556 N O1 SI O5 89(4) 1_555 . 6_554 N O1 SI O5 89(4) 1_555 . -3_556 N O2 SI O3 107.87(20) 1_555 . 1_555 N O2 SI O3 107.87(20) 1_555 . -4_556 N O2 SI O5 136.1(26) 1_555 . 6_554 N O2 SI O5 136.1(26) 1_555 . -3_556 N O3 SI O3 107.75(26) 1_555 . -4_556 N O3 SI O5 29.2(30) 1_555 . 6_554 N O3 SI O5 99.3(23) 1_555 . -3_556 N O3 SI O5 99.3(23) -4_556 . 6_554 N O3 SI O5 29.2(30) -4_556 . -3_556 N O5 SI O5 80(4) 6_554 . -3_556 N La2 O1 La2 92.13(14) 1_555 . -2_566 N La2 O1 SI 128.54(11) 1_555 . 1_555 N La2 O1 SI 128.53(11) -2_566 . 1_555 N La1 O2 La2 114.86(9) 5_665 . 2_655 N La1 O2 La2 114.85(9) 5_665 . -1_665 N La1 O2 SI 124.93(25) 5_665 . 1_555 N La2 O2 La2 89.41(15) 2_655 . -1_665 N La2 O2 SI 103.24(15) 2_655 . 1_555 N La2 O2 SI 103.26(15) -1_665 . 1_555 N La1 O3 La1 112.22(12) 1_555 . 2_554 N La1 O3 SI 96.92(14) 1_555 . 1_555 N La1 O3 O5 80(6) 1_555 . 6_554 N La1 O3 SI 144.86(18) 2_554 . 1_555 N La1 O3 O5 71(4) 2_554 . 6_554 N SI O3 O5 96(5) 1_555 . 6_554 N La1 O4 La1 120.0 1_555 . 3_555 N La1 O4 La1 120.0 1_555 . 5_555 N La1 O4 La1 120.0 3_555 . 5_555 N La1 O5 La1 116(4) 2_555 . 3_555 N La1 O5 La1 98.8(25) 2_555 . 4_555 N La1 O5 SI 88(4) 2_555 . 2_555 N La1 O5 O3 79(7) 2_555 . 2_555 N La1 O5 La1 121(5) 3_555 . 4_555 N La1 O5 SI 130(4) 3_555 . 2_555 N La1 O5 O3 86(4) 3_555 . 2_555 N La1 O5 SI 94.7(29) 4_555 . 2_555 N La1 O5 O3 149(6) 4_555 . 2_555 N SI O5 O3 55(5) 2_555 . 2_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_length_neutron _atom_type_scat_source LA 9.548 0.8240 International_Tables_Vol_C SI 6.0 0.4149 International_Tables_Vol_C O 26.241 0.5803 International_Tables_Vol_C _diffrn_radiation_probe neutron _diffrn_radiation_wavelength 1.88604 _pd_proc_ls_prof_R_factor 0.0302 _pd_proc_ls_prof_wR_factor 0.0392 _pd_proc_ls_prof_wR_expected 0.0199 _refine_ls_R_Fsqd_factor 0.04755 _pd_proc_ls_background_function ; GSAS Background function number 8 with 20 terms. Reciprocal interpolation 1: 1268.83 2: 1304.70 3: 1326.78 4: 1271.42 5: 1216.75 6: 1286.27 7: 1268.67 8: 1313.66 9: 1299.31 10: 1352.36 11: 1323.32 12: 1366.86 13: 1370.49 14: 1428.10 15: 1421.57 16: 1521.17 17: 1856.66 18: 1931.08 19: 1943.93 20: 2132.49 ; _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_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 102.978 #2(GV) = -319.807 #3(GW) = 388.625 #4(LX) = 0.000 #5(LY) = 4.308 #6(trns) = 0.000 #7(asym) = 21.1969 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00500 _pd_proc_info_datetime 2003-09-18T15:57:42 _pd_calc_method 'Rietveld Refinement' #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#