******************************************************* *** PROGRAM FULLPROF (Version 3.5 - Dec97-LLB JRC) *** ******************************************************* Rietveld, Profile Matching & Integrated Intensity Refinement of X-ray and/or Neutron Data Date: 04/24/98 Time: 11:20:46.38 => PCR file code: termycr1 => DAT file code: termycr1 => Title: Tetracycline Hydrochloride Siemens D501 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: 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: 7.0000 2Thmax: 100.0000 Step: 0.0200 No. of points: 4651 => 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: 4.2118 ==> RESULTS OF REFINEMENT: => No. of fitted parameters: 113 ------------------------------------------------------------------------------ => Phase No. 1 Tetracycline hydrochloride P 21 21 21 ------------------------------------------------------------------------------ => No. of reflections: 2657 ==> ATOM PARAMETERS: Name x sx y sy z sz B sB occ. socc. CL 0.06977( 52) 0.07951( 49) 0.00208( 37) 4.676(183) 1.000( 0) C1 0.03096( 145) -0.33147( 130) 0.18567( 125) 3.183(114) 1.000( 0) C10 0.48413( 174) -0.67505( 137) 0.35612( 94) 3.183(114) 1.000( 0) C20 0.38706( 166) -0.64139( 135) 0.29250( 92) 3.183(114) 1.000( 0) C11 0.31812( 182) -0.54582( 159) 0.32806( 128) 3.183(114) 1.000( 0) C21 0.21174( 153) -0.54446( 129) 0.26297( 108) 3.183(114) 1.000( 0) C12 0.13341( 143) -0.45197( 136) 0.28489( 116) 3.183(114) 1.000( 0) C22 0.00532( 123) -0.43271( 108) 0.24218( 88) 3.183(114) 1.000( 0) C13 -0.06265( 144) -0.21094( 128) 0.07736( 139) 3.183(114) 1.000( 0) C14 -0.30944( 185) -0.52059( 156) 0.22737( 100) 3.183(114) 1.000( 0) C15 -0.22116( 225) -0.66986( 120) 0.13435( 129) 3.183(114) 1.000( 0) C16 0.27750( 191) -0.70513( 148) 0.05947( 103) 3.183(114) 1.000( 0) C2 -0.07688( 169) -0.31054( 125) 0.12804( 126) 3.183(114) 1.000( 0) C3 -0.16434( 154) -0.39755( 100) 0.11479( 139) 3.183(114) 1.000( 0) C4 -0.14491( 123) -0.50986( 113) 0.12840( 124) 3.183(114) 1.000( 0) C40 -0.03341( 126) -0.52550( 131) 0.17877( 107) 3.183(114) 1.000( 0) C5 0.07075( 147) -0.57520( 178) 0.13721( 113) 3.183(114) 1.000( 0) C50 0.18439( 128) -0.61191( 154) 0.18903( 100) 3.183(114) 1.000( 0) C6 0.30079( 129) -0.64600( 112) 0.13949( 89) 3.183(114) 1.000( 0) C60 0.39080( 181) -0.68860( 147) 0.20485( 93) 3.183(114) 1.000( 0) C7 0.47701( 192) -0.76809( 138) 0.19207( 108) 3.183(114) 1.000( 0) C8 0.53645( 204) -0.81752( 139) 0.25865( 97) 3.183(114) 1.000( 0) C9 0.55588( 200) -0.76495( 131) 0.33441( 110) 3.183(114) 1.000( 0) N2 0.05404( 155) -0.13673( 108) 0.08561( 116) 3.458(465) 1.000( 0) N4 -0.26964( 121) -0.56195( 99) 0.14381( 87) 3.458(465) 1.000( 0) O1 0.13250( 119) -0.27704( 116) 0.18816( 90) 3.266(137) 1.000( 0) O10 0.49341( 128) -0.62260( 91) 0.43437( 75) 3.266(137) 1.000( 0) O11 0.33646( 127) -0.49031( 105) 0.38751( 82) 3.266(137) 1.000( 0) O12 0.15569( 111) -0.38334( 92) 0.35238( 75) 3.266(137) 1.000( 0) O13 -0.08502( 116) -0.39769( 112) 0.30521( 73) 3.266(137) 1.000( 0) O2 -0.15762( 121) -0.18624( 108) 0.03340( 84) 3.266(137) 1.000( 0) O3 -0.25763( 122) -0.35460( 109) 0.07129( 88) 3.266(137) 1.000( 0) O6 0.35617( 117) -0.54284( 86) 0.12457( 90) 3.266(137) 1.000( 0) => Slack Constraints(dist): Sum{W(Dobs-Dcal)**2}/35 = 812. SM/S2 = 6.26115 SM=Chi2*Sum{W(Dobs-Dcal)**2} = 0.925E+06 S2= Sum{w(yobs-ycal)**2} = 0.148E+06 Rms=Sqrt{Sum[Dobs-Dcal]**2/35}= 0.0998 ==> PROFILE PARAMETERS: => Cell parameters : 10.98676 0.00054 12.86425 0.00060 15.73084 0.00072 90.00000 0.00000 90.00000 0.00000 90.00000 0.00000 => Overall scale factor : 0.002714216 0.000011502 => ETA(p-V) or M(P-VII) : 0.55978 0.00677 => Overall Tem. factor : 0.00000 0.00000 => Halfwidth parameters : 0.06000 0.00000 0.01518 0.00255 0.01950 0.00047 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : 0.10219 0.00176 0.05856 0.00055 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: -0.0589 0.0013 => 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: 4537 => Rp: 6.60 Rwp: 9.36 Rexp: 1.64 Chi2: 32.5 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 9.32 Rwp: 12.5 Rexp: 2.19 Chi2: 32.5 => Deviance: 0.147E+06 Dev* : 32.35 => DW-Stat.: 0.2040 DW-exp: 1.9588 => N-sigma of the GoF: 1502.561 ==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS: => N-P+C: 4533 => Rp: 6.60 Rwp: 9.36 Rexp: 1.64 Chi2: 32.6 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 9.32 Rwp: 12.5 Rexp: 2.19 Chi2: 32.6 => Deviance: 0.147E+06 Dev* : 32.38 => DW-Stat.: 0.2040 DW-exp: 1.9588 => N-sigma of the GoF: 1503.229 => Phase: 1 => Bragg R-factor: 4.56 Vol: 2223.342( 0.181) Fract(%): 0.00( 0.00) => Rf-factor= 6.58 ATZ: 0.000 Brindley: 1.0000 => Run finished at Date: 04/24/98 Time: 13:07:22.78