******************************************************************************** General Structure Analysis System-II Crystal Structure Refinement by Robert B. Von Dreele & Brian H. Toby Argonne National Laboratory(C), 2010 This product includes software developed by the UChicago Argonne, LLC, as Operator of Argonne National Laboratory. Please cite: B.H. Toby & R.B. Von Dreele, J. Appl. Cryst. 46, 544-549 (2013) ******************************************************************************** Least squares controls: Refinement type: analytic Hessian Maximum number of cycles: 3 Regularize hydrogens (if any): False Initial shift factor: 1.000 Phases: Phase name: La0.8Ca0.2MnO3 at 50 mag ======================================================================================================================================= X-ray scattering factors: Symbol fa fb fc --------------------------------------------------------------------------------------------------- Mn+3 9.84521 7.87194 3.56531 0.32361 4.91797 0.29439 10.81710 24.12810 0.39397 Neutron scattering factors: Symbol isotope mass b resonant terms --------------------------------------------------------------------------------------------------- Mn+3 Nat. Abund. 54.938 -0.375 Magnetic scattering factors: Symbol mfa mfb mfc --------------------------------------------------------------------------------------------------- Mn+3 0.41980 0.60540 0.92410 0.00000 14.28300 5.46900 -0.00900 0.00000 -0.94980 Magnetic scattering factors: Symbol nfa nfb nfc --------------------------------------------------------------------------------------------------- Mn+3 1.24270 1.95670 0.57320 0.00000 14.99700 6.11800 2.25800 0.00000 0.00310 Space Group: P b n m The lattice is centrosymmetric primitive orthorhombic The Laue symmetry is mmm The lattice point group is mmm Multiplicity of a general site is 8 The inversion center is located at 0,0,0 The equivalent positions are: ( 1) X, Y, Z ( 2) 1/2-X, 1/2+Y, Z ( 3) 1/2+X, 1/2-Y, 1/2+Z ( 4) -X, -Y, 1/2+Z Atoms: name type refine? x y z frac site sym mult I/A Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3 UM 0.50000 0.00000 0.00000 1.000 -1 4 I 0.00276 Magnetic moments: name type refine? Mx My Mz --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3 UM 0.44122 0.00000 3.27206 Unit cell: a = 5.48260 b = 5.46675 c = 7.72463 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 231.523 Refine? True Spherical harmonics texture: Order:0 Phase name: La0.8Ca0.2MnO3 at 50 ======================================================================================================================================= X-ray scattering factors: Symbol fa fb fc --------------------------------------------------------------------------------------------------- Ca 8.62660 7.38730 1.58990 1.02110 10.44210 0.65990 85.74840 178.43700 1.37510 Mn+3 9.84521 7.87194 3.56531 0.32361 4.91797 0.29439 10.81710 24.12810 0.39397 O 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890 0.25080 La 20.57800 19.59900 11.37270 3.28719 2.94817 0.24447 18.77260 133.12400 2.14678 Neutron scattering factors: Symbol isotope mass b resonant terms --------------------------------------------------------------------------------------------------- Ca Nat. Abund. 40.080 0.470 Mn+3 Nat. Abund. 54.938 -0.375 O Nat. Abund. 15.999 0.581 La Nat. Abund. 138.906 0.824 Space Group: P b n m The lattice is centrosymmetric primitive orthorhombic The Laue symmetry is mmm The lattice point group is mmm Multiplicity of a general site is 8 The inversion center is located at 0,0,0 The equivalent positions are: ( 1) X, Y, Z ( 2) 1/2-X, 1/2+Y, Z ( 3) 1/2+X, 1/2-Y, 1/2+Z ( 4) -X, -Y, 1/2+Z Atoms: name type refine? x y z frac site sym mult I/A Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- La La XU -0.00657 0.02325 0.25000 0.785 m(z) 4 I 0.00476 Mn Mn+3 XU 0.50000 0.00000 0.00000 1.000 -1 4 I 0.00276 O1 O XU 0.06266 0.49105 0.25000 1.000 m(z) 4 I 0.00571 O2 O XU 0.72423 0.27649 0.03374 1.000 1 8 I 0.00716 Ca Ca XU -0.00079 0.01502 0.25000 0.215 m(z) 4 I 0.00881 Unit cell: a = 5.48260 b = 5.46675 c = 7.72463 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 231.523 Refine? True Spherical harmonics texture: Order:0 Phase: La0.8Ca0.2MnO3 at 50 mag in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Phase fraction : 1.0000 Refine? 0.0 Extinction coeff: 0.0000 Refine? False March-Dollase PO: 1.0000 Refine? False Axis: 0 0 1 Size model : isotropic equatorial: 1.000 Refine? False LG mixing coeff.: 1.0000 Refine? False Mustrain model: isotropic equatorial: 1000.0 Refine? False LG mixing coeff.: 1.0000 Refine? False Hydrostatic/elastic strain: names : D11 D22 D33 values: 0 0 0 refine: False False False Phase: La0.8Ca0.2MnO3 at 50 in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Phase fraction : 1.0000 Refine? False Extinction coeff: 0.0000 Refine? False March-Dollase PO: 1.0000 Refine? False Axis: 0 0 1 Size model : isotropic equatorial: 1.000 Refine? False LG mixing coeff.: 1.0000 Refine? False Mustrain model: isotropic equatorial: 1000.0 Refine? False LG mixing coeff.: 1.0000 Refine? False Hydrostatic/elastic strain: names : D11 D22 D33 values: 0 0 0 refine: False False False Histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 histogram Id: 0 ======================================================================================================================================= Instrument type: Debye-Scherrer Histogram limits: 9.35 deg to 157.50 deg Sample Parameters: Goniometer omega = 0.00, chi = 0.00, phi = 0.00 name : Scale Absorption DisplaceX DisplaceY value : 5490.8395 0.0000 626.9276 39.4396 refine: True False True True Instrument Parameters: name : Azimuth Bank Lam Polariz. SH/L U V value : 0.000000 1.000000 1.540300 0.000000 0.002000 239.700000 -298.200000 refine: False False False False False False name : W X Y Z Zero value : 180.800000 0.000000 0.000000 0.000000 0.000400 refine: False False False False False Background function: chebyschev Refine? True Coefficients: 135.385 21.958 5.355 -60.913 48.958 37.691 Refinement results: --------------------------------------------------------------------------------------------------------------------------------------- Number of function calls: 5 No. of observations: 2963 No. of parameters: 28 User rejected: 0 Sp. gp. extinct: 0 Refinement time = 6.782s, 6.782s/cycle, for 1 cycles wR = 7.62%, chi**2 = 5735.68, GOF = 1.40 ---------------------------------------------------------------------------------------------------------------------------------- Variables generated by constraints name : 1::AUiso:0 1::A0 1::A1 1::A2 value : 0.0028 0.0333 0.0335 0.0168 sig : 0.0003 0.0000 0.0000 0.0000 Phases: Result for phase: La0.8Ca0.2MnO3 at 50 mag ======================================================================================================================================= Reciprocal metric tensor: names : A11 A22 A33 A12 A13 A23 values: 0.033268144 0.033461197 0.016758900 0.000000000 0.000000000 0.000000000 esds : 0.000001550 0.000001619 0.000000797 New unit cell: names : a b c alpha beta gamma Volume values: 5.482589 5.466751 7.724622 90.0000 90.0000 90.0000 231.522 esds : 0.000128 0.000132 0.000184 0.013 Atoms: name x y z frac Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3: values: 0.50000 0.00000 0.00000 1.000 0.00279 sig : 0.00034 Magnetic Moments: name Mx My Mz |Mag| --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3: values: 0.522 0.000 3.269 3.311 sig : 0.095 0.024 Result for phase: La0.8Ca0.2MnO3 at 50 ======================================================================================================================================= Reciprocal metric tensor: names : A11 A22 A33 A12 A13 A23 values: 0.033268144 0.033461197 0.016758900 0.000000000 0.000000000 0.000000000 esds : 0.000001550 0.000001619 0.000000797 New unit cell: names : a b c alpha beta gamma Volume values: 5.482589 5.466751 7.724622 90.0000 90.0000 90.0000 231.522 esds : Atoms: name x y z frac Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- La La: values: -0.00571 0.02384 0.25000 0.785 0.00469 sig : 0.00136 0.00185 0.00235 Mn Mn+3: values: 0.50000 0.00000 0.00000 1.000 0.00279 sig : 0.000 0.00034 O1 O: values: 0.06265 0.49104 0.25000 1.000 0.00572 sig : 0.00034 0.00037 0.00034 O2 O: values: 0.72423 0.27649 0.03373 1.000 0.00717 sig : 0.00024 0.00025 0.00015 0.00027 Ca Ca: values: -0.00809 0.01099 0.25000 0.215 0.00870 sig : 0.01042 0.01140 0.01711 Phase: La0.8Ca0.2MnO3 at 50 mag in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Final refinement RF, RF^2 = 2.19%, 7.36% on 166 reflections Durbin-Watson statistic = 0.681 Bragg intensity sum = 3.22e+04 Phase fraction : 1.00000, sig 0.00000 Weight fraction : 0.00000, sig 0.00000 Phase: La0.8Ca0.2MnO3 at 50 in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Final refinement RF, RF^2 = 2.46%, 2.84% on 262 reflections Durbin-Watson statistic = 0.681 Bragg intensity sum = 4.81e+05 Histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 histogram Id: 0 ======================================================================================================================================= PWDR histogram weight factor = 1.000 Final refinement wR = 7.62% on 2963 observations in this histogram Other residuals: R = 5.59%, R-bkg = 4.82%, wR-bkg = 7.62% wRmin = 5.47% Instrument type: Debye-Scherrer Sample Parameters: names : Scale Absorption DisplaceX DisplaceY values: 5491.4047 0.0000 627.0876 40.3088 sig : 29.3748 30.7161 51.6157 Background function: chebyschev value : 135.4 22.01 5.226 -61.46 49.5 37.85 sig : 0.6782 2.647 4.558 11 5.227 10.08 Background sums: empirical 4.36e+05, Debye 0, peaks 0, Total 4.36e+05