******************************************************************************** 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 0.00284 Magnetic moments: name type refine? Mx My Mz --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3 UM -0.31370 3.23945 -0.00909 Unit cell: a = 5.48268 b = 5.46683 c = 7.72491 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 231.538 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 -0.00566 0.01801 0.25000 0.785 m(z) 4 I 0.00469 Mn Mn+3 XU 0.50000 0.00000 0.00000 1.000 -1 4 I 0.00284 O1 O XU 0.06267 0.49112 0.25000 1.000 m(z) 4 I 0.00605 O2 O XU 0.72430 0.27621 0.03380 1.000 1 8 I 0.00702 Ca Ca XU -0.00404 0.05276 0.25000 0.215 m(z) 4 I-0.00338 Unit cell: a = 5.48268 b = 5.46683 c = 7.72491 alpha = 90.000 beta = 90.000 gamma = 90.000 volume = 231.538 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 : 5502.0666 0.0000 719.6736 -47.6361 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: 135.445 24.565 4.662 -72.041 50.893 46.836 Refinement results: --------------------------------------------------------------------------------------------------------------------------------------- Number of function calls: 6 No. of observations: 2963 No. of parameters: 29 User rejected: 0 Sp. gp. extinct: 0 Refinement time = 8.860s, 4.430s/cycle, for 2 cycles wR = 7.72%, chi**2 = 5886.81, GOF = 1.42 ---------------------------------------------------------------------------------------------------------------------------------- Variables generated by constraints name : 1::AUiso:0 1::A0 1::A1 1::A2 value : 0.0029 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: 0.033267407 0.033460321 0.016757813 0.000000000 0.000000000 0.000000000 esds : 0.000001562 0.000001671 0.000000796 New unit cell: names : a b c alpha beta gamma Volume values: 5.482650 5.466822 7.724873 90.0000 90.0000 90.0000 231.535 esds : 0.000129 0.000136 0.000183 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 0.00291 sig : 0.00034 Magnetic Moments: name Mx My Mz |Mag| --------------------------------------------------------------------------------------------------------------------------------------- Mn Mn+3: values: -0.373 3.222 -0.308 3.258 sig : 0.132 0.026 0.223 Result for phase: La0.8Ca0.2MnO3 at 50 ======================================================================================================================================= Reciprocal metric tensor: names : A11 A22 A33 A12 A13 A23 values: 0.033267407 0.033460321 0.016757813 0.000000000 0.000000000 0.000000000 esds : 0.000001562 0.000001671 0.000000796 New unit cell: names : a b c alpha beta gamma Volume values: 5.482650 5.466822 7.724873 90.0000 90.0000 90.0000 231.535 esds : Atoms: name x y z frac Uiso U11 U22 U33 U12 U13 U23 --------------------------------------------------------------------------------------------------------------------------------------- La La: values: -0.00556 0.01748 0.25000 0.785 0.00596 sig : 0.00093 0.00060 0.00109 Mn Mn+3: values: 0.50000 0.00000 0.00000 1.000 0.00291 sig : 0.000 0.00034 O1 O: values: 0.06264 0.49106 0.25000 1.000 0.00594 sig : 0.00034 0.00038 0.00035 O2 O: values: 0.72427 0.27625 0.03376 1.000 0.00714 sig : 0.00024 0.00025 0.00015 0.00027 Ca Ca: values: -0.00821 0.04894 0.25000 0.215-0.00678 sig : 0.00358 0.00395 0.00485 Phase: La0.8Ca0.2MnO3 at 50 mag in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Final refinement RF, RF^2 = 3.72%, 7.54% on 166 reflections Durbin-Watson statistic = 0.668 Bragg intensity sum = 3.11e+04 Phase fraction : 1.00000, sig 0.00000 Weight fraction : 0.16707, sig 0.00000 Phase: La0.8Ca0.2MnO3 at 50 in histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 ======================================================================================================================================= Final refinement RF, RF^2 = 2.49%, 2.81% on 262 reflections Durbin-Watson statistic = 0.668 Bragg intensity sum = 4.82e+05 Histogram: PWDR La7Ca3MnO3_50k.gsas Bank 1 histogram Id: 0 ======================================================================================================================================= PWDR histogram weight factor = 1.000 Final refinement wR = 7.72% on 2963 observations in this histogram Other residuals: R = 5.74%, R-bkg = 5.02%, wR-bkg = 7.72% wRmin = 5.47% Instrument type: Debye-Scherrer Sample Parameters: names : Scale Absorption DisplaceX DisplaceY values: 5508.2546 0.0000 712.4781 -32.4450 sig : 29.3620 31.1840 52.4537 Background function: chebyschev value : 135.7 24.72 2.929 -74.44 52.48 49.44 sig : 0.6906 2.688 4.681 11.21 5.359 10.29 Background sums: empirical 4.36e+05, Debye 0, peaks 0, Total 4.36e+05