******************************************************* *** PROGRAM FULLPROF (Version 3.5 - Dec97-LLB JRC) *** ******************************************************* Rietveld, Profile Matching & Integrated Intensity Refinement of X-ray and/or Neutron Data Date: 06/06/98 Time: 15:38:09.95 => PCR file code: M33tetcyc => DAT file code: M33tetcyc => Title: Tetracycline Hydrochloride P212121 ==> 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: 0.69200 0.69200 => Cos(Monochromator angle)= 0.0000 => Absorption correction (muR-eff): 0.0000 => Base of peaks: 2.0*HW* 12.00 ==> Angular range, step and number of points: 2Thmin: 2.1150 2Thmax: 40.0000 Step: 0.0050 No. of points: 7578 => Crystal Structure Refinement for phase: 1 => Constraints on distances for phase 1 Distance between C1 and O1 is 1.22000 with standard error: 0.02000 Distance between C10 and O10 is 1.43000 with standard error: 0.02000 Distance between C10 and C9 is 1.40000 with standard error: 0.02000 Distance between C10 and C20 is 1.45000 with standard error: 0.02000 Distance between C20 and C11 is 1.43000 with standard error: 0.02000 Distance between C20 and C60 is 1.40000 with standard error: 0.02000 Distance between C11 and O11 is 1.22000 with standard error: 0.02000 Distance between C11 and C21 is 1.45000 with standard error: 0.02000 Distance between C21 and C12 is 1.40000 with standard error: 0.02000 Distance between C21 and C50 is 1.40000 with standard error: 0.02000 Distance between C12 and O12 is 1.43000 with standard error: 0.02000 Distance between C12 and C22 is 1.40000 with standard error: 0.02000 Distance between C22 and O13 is 1.43000 with standard error: 0.02000 Distance between C22 and C1 is 1.40000 with standard error: 0.02000 Distance between C22 and C40 is 1.40000 with standard error: 0.02000 Distance between C13 and O2 is 1.22000 with standard error: 0.02000 Distance between C13 and C2 is 1.40000 with standard error: 0.02000 Distance between C13 and N2 is 1.50000 with standard error: 0.02000 Distance between C14 and N4 is 1.50000 with standard error: 0.02000 Distance between C15 and N4 is 1.50000 with standard error: 0.02000 Distance between C16 and C6 is 1.40000 with standard error: 0.02000 Distance between C2 and C1 is 1.40000 with standard error: 0.02000 Distance between C2 and C3 is 1.40000 with standard error: 0.02000 Distance between C3 and O3 is 1.43000 with standard error: 0.02000 Distance between C3 and C4 is 1.40000 with standard error: 0.02000 Distance between C4 and N4 is 1.50000 with standard error: 0.02000 Distance between C4 and C40 is 1.40000 with standard error: 0.02000 Distance between C5 and C40 is 1.40000 with standard error: 0.02000 Distance between C5 and C50 is 1.40000 with standard error: 0.02000 Distance between C6 and C50 is 1.40000 with standard error: 0.02000 Distance between C6 and O6 is 1.43000 with standard error: 0.02000 Distance between C6 and C60 is 1.40000 with standard error: 0.02000 Distance between C60 and C7 is 1.40000 with standard error: 0.02000 Distance between C7 and C8 is 1.40000 with standard error: 0.02000 Distance between C8 and C9 is 1.40000 with standard error: 0.02000 (See output file *.OUT for symmetry details) => Scor: 3.6393 ==> RESULTS OF REFINEMENT: => No. of fitted parameters: 113 ------------------------------------------------------------------------------ => Phase No. 1 Tetracycline hydrochloride P 21 21 21 ------------------------------------------------------------------------------ => No. of reflections: 1307 ==> ATOM PARAMETERS: Name x sx y sy z sz B sB occ. socc. CL 0.07234( 30) 0.08051( 27) 0.00354( 21) 3.401( 89) 1.000( 0) C1 0.03724( 102) -0.32921( 84) 0.18279( 78) 3.341( 71) 1.000( 0) C10 0.49271( 108) -0.68443( 85) 0.35970( 69) 3.341( 71) 1.000( 0) C20 0.39007( 105) -0.63770( 88) 0.30549( 69) 3.341( 71) 1.000( 0) C11 0.30795( 118) -0.54928( 96) 0.32684( 79) 3.341( 71) 1.000( 0) C21 0.21197( 104) -0.54244( 86) 0.26032( 69) 3.341( 71) 1.000( 0) C12 0.13241( 97) -0.44678( 91) 0.28158( 71) 3.341( 71) 1.000( 0) C22 0.00815( 101) -0.42959( 83) 0.23451( 67) 3.341( 71) 1.000( 0) C13 -0.05822( 101) -0.21291( 83) 0.08145( 87) 3.341( 71) 1.000( 0) C14 -0.30144( 107) -0.51448( 91) 0.22655( 68) 3.341( 71) 1.000( 0) C15 -0.21936( 130) -0.67386( 78) 0.13017( 76) 3.341( 71) 1.000( 0) C16 0.28356( 107) -0.71577( 90) 0.06435( 69) 3.341( 71) 1.000( 0) C2 -0.08127( 115) -0.31283( 86) 0.12244( 74) 3.341( 71) 1.000( 0) C3 -0.15377( 102) -0.41168( 77) 0.11038( 79) 3.341( 71) 1.000( 0) C4 -0.13041( 95) -0.51841( 82) 0.12652( 77) 3.341( 71) 1.000( 0) C40 -0.02733( 97) -0.52712( 88) 0.18762( 73) 3.341( 71) 1.000( 0) C5 0.08018( 108) -0.57068( 101) 0.13666( 72) 3.341( 71) 1.000( 0) C50 0.18328( 94) -0.62239( 94) 0.19433( 73) 3.341( 71) 1.000( 0) C6 0.30064( 100) -0.64321( 84) 0.14215( 70) 3.341( 71) 1.000( 0) C60 0.39033( 109) -0.68093( 83) 0.21479( 68) 3.341( 71) 1.000( 0) C7 0.46781( 125) -0.77372( 89) 0.19159( 69) 3.341( 71) 1.000( 0) C8 0.51671( 133) -0.81726( 94) 0.25758( 75) 3.341( 71) 1.000( 0) C9 0.55030( 126) -0.77239( 86) 0.33330( 72) 3.341( 71) 1.000( 0) N2 0.04239( 98) -0.13820( 69) 0.08450( 67) 3.384(259) 1.000( 0) N4 -0.25558( 84) -0.56571( 69) 0.15106( 56) 3.384(259) 1.000( 0) O1 0.13445( 75) -0.26867( 76) 0.18497( 52) 4.611(100) 1.000( 0) O10 0.49114( 80) -0.62451( 56) 0.43855( 50) 4.611(100) 1.000( 0) O11 0.33478( 74) -0.49553( 67) 0.38937( 51) 4.611(100) 1.000( 0) O12 0.15679( 68) -0.38834( 63) 0.35294( 48) 4.611(100) 1.000( 0) O13 -0.07574( 74) -0.39147( 70) 0.30056( 49) 4.611(100) 1.000( 0) O2 -0.16042( 77) -0.18493( 66) 0.03852( 48) 4.611(100) 1.000( 0) O3 -0.24628( 78) -0.35319( 66) 0.07681( 55) 4.611(100) 1.000( 0) O6 0.35914( 77) -0.53912( 58) 0.12694( 54) 4.611(100) 1.000( 0) => Slack Constraints(dist): Sum{W(Dobs-Dcal)**2}/35 = 126. SM/S2 = 0.59849 SM=Chi2*Sum{W(Dobs-Dcal)**2} = 0.186E+05 S2= Sum{w(yobs-ycal)**2} = 0.311E+05 Rms=Sqrt{Sum[Dobs-Dcal]**2/35}= 0.1083 ==> PROFILE PARAMETERS: => Cell parameters : 10.98055 0.00022 12.85250 0.00026 15.73312 0.00030 90.00000 0.00000 90.00000 0.00000 90.00000 0.00000 => Overall scale factor : 0.000429481 0.000001255 => ETA(p-V) or M(P-VII) : 0.41390 0.00368 => Overall Tem. factor : 0.00000 0.00000 => Halfwidth parameters : 0.00600 0.00000 0.00516 0.00024 0.00251 0.00002 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : -0.00405 0.00082 -0.00333 0.00012 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: 0.0028 0.0003 => Cos( theta)-shift parameter : 0.0000 0.0000 => Sin(2theta)-shift parameter : 0.0000 0.0000 ==> RELIABILITY FACTORS WITH ALL NON-EXCLUDED POINTS: => Cycle: 10 => MaxCycle: 10 => N-P+C: 7386 => Rp: 1.38 Rwp: 1.77 Rexp: 0.86 Chi2: 4.21 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 9.21 Rwp: 7.42 Rexp: 3.62 Chi2: 4.21 => Deviance: 0.311E+05 Dev* : 4.214 => DW-Stat.: 0.2653 DW-exp: 1.9590 => N-sigma of the GoF: 195.118 ==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS: => N-P+C: 7214 => Rp: 1.39 Rwp: 1.78 Rexp: 0.86 Chi2: 4.28 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 9.11 Rwp: 7.40 Rexp: 3.58 Chi2: 4.28 => Deviance: 0.309E+05 Dev* : 4.286 => DW-Stat.: 0.2671 DW-exp: 1.9589 => N-sigma of the GoF: 197.154 => Phase: 1 => Bragg R-factor: 4.97 Vol: 2220.377( 0.075) Fract(%): 0.00( 0.00) => Rf-factor= 8.13 ATZ: 0.000 Brindley: 1.0000 => Run finished at Date: 06/06/98 Time: 15:55:32.76