******************************************************************************** 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 0.50000 0.00000 0.00000 1.000 -1 4 I 0.00348 Magnetic moments: name type refine? Mx My Mz --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3 1.00000 1.00000 1.00000 Unit cell: a = 5.48070 b = 5.46656 c = 7.72684 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 231.501 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 -0.00530 0.02294 0.25000 0.785 m(z) 4 I 0.00415 Mn Mn+3 0.50000 0.00000 0.00000 1.000 -1 4 I 0.00348 O1 O 0.06520 0.49190 0.25000 1.000 m(z) 4 I 0.00590 O2 O 0.72364 0.27509 0.03332 1.000 1 8 I 0.00579 Ca Ca -0.00530 0.02294 0.25000 0.215 m(z) 4 I 0.00415 Unit cell: a = 5.48070 b = 5.46656 c = 7.72684 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 231.501 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 : 5279.8604 0.0000 0.0000 0.0000 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: 136.045 5.316 30.992 Refinement results: --------------------------------------------------------------------------------------------------------------------------------------- Number of function calls: 7 No. of observations: 2963 No. of parameters: 9 User rejected: 0 Sp. gp. extinct: 0 Refinement time = 10.093s, 3.364s/cycle, for 3 cycles wR = 13.63%, chi**2 = 18377.7, GOF = 2.49 ---------------------------------------------------------------------------------------------------------------------------------- Variables generated by constraints name : 1::A0 1::A1 1::A2 value : 0.0333 0.0335 0.0168 sig : 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: 0.033265868 0.033460940 0.016757313 0.000000000 0.000000000 0.000000000 esds : 0.000002626 0.000002770 0.000001327 New unit cell: names : a b c alpha beta gamma Volume values: 5.482777 5.466772 7.724988 90.0000 90.0000 90.0000 231.542 esds : 0.000216 0.000226 0.000306 0.021 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 0.00348 sig : Magnetic Moments: name Mx My Mz |Mag| --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3: values: 1.000 1.000 1.000 1.732 sig : Result for phase: La0.8Ca0.2MnO3 at 50 ======================================================================================================================================= Reciprocal metric tensor: names : A11 A22 A33 A12 A13 A23 values: 0.033265868 0.033460940 0.016757313 0.000000000 0.000000000 0.000000000 esds : 0.000002626 0.000002770 0.000001327 New unit cell: names : a b c alpha beta gamma Volume values: 5.482777 5.466772 7.724988 90.0000 90.0000 90.0000 231.542 esds : Atoms: name x y z frac Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- La La: values: -0.00530 0.02294 0.25000 0.785 0.00415 sig : Mn Mn+3: values: 0.50000 0.00000 0.00000 1.000 0.00348 sig : 0.000 0.00000 O1 O: values: 0.06520 0.49190 0.25000 1.000 0.00590 sig : O2 O: values: 0.72364 0.27509 0.03332 1.000 0.00579 sig : Ca Ca: values: -0.00530 0.02294 0.25000 0.215 0.00415 sig : Phase: La0.8Ca0.2MnO3 at 50 mag in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Final refinement RF, RF^2 = 10.82%, 39.97% on 168 reflections Durbin-Watson statistic = 0.256 Bragg intensity sum = 1.3e+04 Phase fraction : 1.00000, sig 0.00000 Weight fraction : 0.05861, sig 0.00000 Phase: La0.8Ca0.2MnO3 at 50 in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Final refinement RF, RF^2 = 4.83%, 7.40% on 262 reflections Durbin-Watson statistic = 0.256 Bragg intensity sum = 4.88e+05 Histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 histogram Id: 0 ======================================================================================================================================= PWDR histogram weight factor = 1.000 Final refinement wR = 13.63% on 2963 observations in this histogram Other residuals: R = 9.45%, R-bkg = 9.69%, wR-bkg = 13.63% wRmin = 5.47% Instrument type: Debye-Scherrer Sample Parameters: names : Scale Absorption DisplaceX DisplaceY values: 5419.1442 0.0000 697.1858 -20.4013 sig : 24.0742 57.6653 90.4168 Background function: chebyschev value : 133 3.482 33.21 sig : 0.9705 1.239 2.264 Background sums: empirical 4.27e+05, Debye 0, peaks 0, Total 4.27e+05