******************************************************* *** PROGRAM FULLPROF (Version 3.5 - Dec97-LLB JRC) *** ******************************************************* Rietveld, Profile Matching & Integrated Intensity Refinement of X-ray and/or Neutron Data Date: 05/16/98 Time: 19:39:21.11 => PCR file code: zhu3 => DAT file code: zhu3 => Title: Co etc Siemens 2 Zhu P21 ==> CONDITIONS OF THIS RUN: => Global Refinement of X-ray powder diffraction data Bragg-Brentano or Debye-Scherrer geometry => The 5th default profile function was selected => Data supplied in free format => Wavelengths: 1.54056 1.54439 => Cos(Monochromator angle)= 0.7998 => Absorption correction (muR-eff): 0.0000 => Base of peaks: 2.0*HW* 12.00 ==> Angular range, step and number of points: 2Thmin: 10.0000 2Thmax: 119.6000 Step: 0.0200 No. of points: 5481 => Crystal Structure Refinement for phase: 1 => Constraints on distances for phase 1 Distance between C and O1 is 1.25000 with standard error: 0.02000 Distance between C and O2 is 1.25000 with standard error: 0.02000 Distance between C and O3 is 1.25000 with standard error: 0.02000 Distance between O1 and O2 is 2.25000 with standard error: 0.02000 Distance between O1 and O3 is 2.25000 with standard error: 0.02000 Distance between O2 and O3 is 2.25000 with standard error: 0.02000 Distance between N6 and O4 is 1.27000 with standard error: 0.02000 Distance between N6 and O5 is 1.27000 with standard error: 0.02000 Distance between N6 and O6 is 1.27000 with standard error: 0.02000 Distance between O4 and O5 is 2.27000 with standard error: 0.02000 Distance between O4 and O6 is 2.27000 with standard error: 0.02000 Distance between O5 and O6 is 2.27000 with standard error: 0.02000 (See output file *.OUT for symmetry details) => Crystal Structure Refinement for phase: 2 => Scor: 4.1832 ==> RESULTS OF REFINEMENT: => No. of fitted parameters: 68 ------------------------------------------------------------------------------ => Phase No. 1 Co ..; Number 2, Zhu P 21 ------------------------------------------------------------------------------ => No. of reflections: 1566 ==> ATOM PARAMETERS: Name x sx y sy z sz B sB occ. socc. CO 0.81898( 42) 0.25000( 0) 0.44028( 36) 2.392( 68) 1.000( 0) N1 0.25886( 172) 0.88330( 155) 0.80177( 193) 1.368(128) 1.000( 0) N2 0.26125( 169) 0.89297( 126) 0.37363( 186) 1.368(128) 1.000( 0) N3 0.89213( 154) 0.11141( 117) 0.27124( 237) 1.368(128) 1.000( 0) N4 0.43185( 161) 0.66161( 130) 0.63531( 177) 1.368(128) 1.000( 0) N5 0.89916( 155) 0.11561( 138) 0.67023( 200) 1.368(128) 1.000( 0) O1 0.07304( 127) 0.35080( 109) 0.53251( 167) 3.085(166) 1.000( 0) C 0.21818( 176) 0.28341( 126) 0.55656( 257) 3.085(166) 1.000( 0) O2 0.25269( 151) 0.15803( 99) 0.61609( 177) 3.085(166) 1.000( 0) O3 0.34839( 132) 0.36868( 106) 0.54500( 147) 3.085(166) 1.000( 0) N6 0.19699( 171) 0.30241( 119) 0.03481( 227) 4.411(184) 1.000( 0) O4 0.34704( 128) 0.37436( 124) 0.03452( 145) 4.411(184) 1.000( 0) O5 0.20239( 154) 0.17807( 96) 0.10358( 165) 4.411(184) 1.000( 0) O6 0.05397( 139) 0.37650( 111) 0.02331( 153) 4.411(184) 1.000( 0) OW 0.58879( 123) 0.14714( 110) 0.88460( 131) 1.430(304) 1.000( 0) => Slack Constraints(dist): Sum{W(Dobs-Dcal)**2}/12 = 80.3 SM/S2 = 0.17808 SM=Chi2*Sum{W(Dobs-Dcal)**2} = 0.853E+04 S2= Sum{w(yobs-ycal)**2} = 0.479E+05 Rms=Sqrt{Sum[Dobs-Dcal]**2/12}= 0.0602 ==> PROFILE PARAMETERS: => Cell parameters : 7.67341 0.00036 9.63964 0.00052 7.08511 0.00033 90.00000 0.00000 106.19501 0.00285 90.00000 0.00000 => Overall scale factor : 0.010182448 0.000058541 => ETA(p-V) or M(P-VII) : 0.51635 0.00877 => Overall Tem. factor : 0.00000 0.00000 => Halfwidth parameters : 0.25000 0.00000 -0.26833 0.00487 0.12774 0.00169 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : 0.14360 0.00179 0.03521 0.00069 0.00000 0.00000 0.00000 0.00000 => X and Y parameters : 0.00000 0.00000 0.00000 0.00000 => Strain parameters : 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 => Size parameters : 0.00000 0.00000 0.00000 0.00000 ------------------------------------------------------------------------------ => Phase No. 2 Co ..; Number 2, Zhu P 21 ------------------------------------------------------------------------------ => No. of reflections: 10 ==> ATOM PARAMETERS: Name x sx y sy z sz B sB occ. socc. CO 0.81898( 42) 0.25000( 0) 0.44028( 36) 2.392( 68) 1.000( 0) N1 0.25886( 172) 0.88330( 155) 0.80177( 193) 1.368(128) 1.000( 0) N2 0.26125( 169) 0.89297( 126) 0.37363( 186) 1.368(128) 1.000( 0) N3 0.89213( 154) 0.11141( 117) 0.27124( 237) 1.368(128) 1.000( 0) N4 0.43185( 161) 0.66161( 130) 0.63531( 177) 1.368(128) 1.000( 0) N5 0.89916( 155) 0.11561( 138) 0.67023( 200) 1.368(128) 1.000( 0) O1 0.07304( 127) 0.35080( 109) 0.53251( 167) 3.085(166) 1.000( 0) C 0.21818( 176) 0.28341( 126) 0.55656( 257) 3.085(166) 1.000( 0) O2 0.25269( 151) 0.15803( 99) 0.61609( 177) 3.085(166) 1.000( 0) O3 0.34839( 132) 0.36868( 106) 0.54500( 147) 3.085(166) 1.000( 0) N6 0.19699( 171) 0.30241( 119) 0.03481( 227) 4.411(184) 1.000( 0) O4 0.34704( 128) 0.37436( 124) 0.03452( 145) 4.411(184) 1.000( 0) O5 0.20239( 154) 0.17807( 96) 0.10358( 165) 4.411(184) 1.000( 0) O6 0.05397( 139) 0.37650( 111) 0.02331( 153) 4.411(184) 1.000( 0) OW 0.58879( 123) 0.14714( 110) 0.88460( 131) 1.430(304) 1.000( 0) ==> PROFILE PARAMETERS: => Cell parameters : 7.67341 0.00036 9.63964 0.00052 7.08511 0.00033 90.00000 0.00000 106.19501 0.00285 90.00000 0.00000 => Overall scale factor : 0.010182448 0.000058541 => ETA(p-V) or M(P-VII) : 0.35426 0.01395 => Overall Tem. factor : 0.00000 0.00000 => Halfwidth parameters : 0.25000 0.00000 -0.26833 0.00487 0.11298 0.00162 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : 0.14360 0.00179 0.03521 0.00069 0.00000 0.00000 0.00000 0.00000 => X and Y parameters : 0.00000 0.00000 0.00000 0.00000 => Strain parameters : 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 => Size parameters : 0.00000 0.00000 0.00000 0.00000 ==> GLOBAL PARAMETERS: => Zero-point: 0.0067 0.0020 => Background Polynomial Parameters ==> 320.144 2.86595 -174.339 14.3120 2548.87 62.9737 641.152 154.390 -14609.2 519.800 -15140.9 399.019 => Cos( theta)-shift parameter : 0.0000 0.0000 => Sin(2theta)-shift parameter : 0.0000 0.0000 ==> RELIABILITY FACTORS WITH ALL NON-EXCLUDED POINTS: => Cycle: 20 => MaxCycle: 20 => N-P+C: 5413 => Rp: 6.30 Rwp: 8.25 Rexp: 2.77 Chi2: 8.85 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 10.1 Rwp: 12.0 Rexp: 4.05 Chi2: 8.85 => Deviance: 0.494E+05 Dev* : 9.124 => DW-Stat.: 0.2573 DW-exp: 1.9413 => N-sigma of the GoF: 408.526 ==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS: => N-P+C: 5413 => Rp: 6.30 Rwp: 8.25 Rexp: 2.77 Chi2: 8.85 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 10.1 Rwp: 12.0 Rexp: 4.05 Chi2: 8.85 => Deviance: 0.494E+05 Dev* : 9.124 => DW-Stat.: 0.2573 DW-exp: 1.9413 => N-sigma of the GoF: 408.526 => Phase: 1 => Bragg R-factor: 5.52 Vol: 503.281( 0.043) Fract(%): 0.00( 0.00) => Rf-factor= 5.84 ATZ: 0.000 Brindley: 1.0000 => Phase: 2 => Bragg R-factor: 2.17 Vol: 503.281( 0.043) Fract(%): 0.00( 0.00) => Rf-factor= 3.41 ATZ: 0.000 Brindley: 1.0000 => Run finished at Date: 05/16/98 Time: 20:09:52.71