******************************************************* *** 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: 11:25:43.97 => PCR file code: termycr2 => DAT file code: termycr2 => 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 => Scor: 4.0369 ==> 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 0.07165( 58) 0.07759( 61) 0.00334( 45) 5.210(208) 1.000( 0) C1 0.04618( 250) -0.32722( 192) 0.17937( 170) 2.717(113) 1.000( 0) C10 0.48875( 243) -0.66944( 196) 0.35653( 170) 2.717(113) 1.000( 0) C20 0.37770( 222) -0.64530( 180) 0.28073( 177) 2.717(113) 1.000( 0) C11 0.32605( 319) -0.53365( 239) 0.34217( 185) 2.717(113) 1.000( 0) C21 0.21372( 244) -0.54359( 202) 0.25477( 170) 2.717(113) 1.000( 0) C12 0.14491( 251) -0.46054( 204) 0.28786( 170) 2.717(113) 1.000( 0) C22 0.00588( 247) -0.42917( 201) 0.24512( 168) 2.717(113) 1.000( 0) C13 -0.05894( 252) -0.21395( 211) 0.07356( 170) 2.717(113) 1.000( 0) C14 -0.30425( 228) -0.51893( 196) 0.22425( 163) 2.717(113) 1.000( 0) C15 -0.21811( 277) -0.67027( 177) 0.13606( 142) 2.717(113) 1.000( 0) C16 0.27410( 198) -0.70609( 193) 0.06166( 138) 2.717(113) 1.000( 0) C2 -0.08205( 285) -0.31448( 227) 0.13491( 162) 2.717(113) 1.000( 0) C3 -0.17031( 269) -0.39785( 214) 0.10861( 178) 2.717(113) 1.000( 0) C4 -0.13702( 241) -0.51178( 190) 0.12853( 151) 2.717(113) 1.000( 0) C40 -0.03620( 243) -0.52755( 208) 0.18344( 161) 2.717(113) 1.000( 0) C5 0.07187( 232) -0.57069( 202) 0.12672( 174) 2.717(113) 1.000( 0) C50 0.17525( 228) -0.61608( 203) 0.20048( 169) 2.717(113) 1.000( 0) C6 0.30746( 244) -0.63661( 207) 0.12836( 189) 2.717(113) 1.000( 0) C60 0.38304( 258) -0.68979( 207) 0.19599( 183) 2.717(113) 1.000( 0) C7 0.48152( 262) -0.76357( 193) 0.19536( 170) 2.717(113) 1.000( 0) C8 0.53995( 228) -0.81210( 197) 0.25439( 198) 2.717(113) 1.000( 0) C9 0.54675( 261) -0.77000( 187) 0.33907( 160) 2.717(113) 1.000( 0) N2 0.05236( 211) -0.13422( 135) 0.08783( 144) 4.156(561) 1.000( 0) N4 -0.27706( 183) -0.55572( 164) 0.14978( 119) 4.156(561) 1.000( 0) O1 0.13607( 158) -0.27637( 150) 0.19320( 113) 3.951(175) 1.000( 0) O10 0.49470( 148) -0.62186( 110) 0.43390( 112) 3.951(175) 1.000( 0) O11 0.33774( 216) -0.49458( 150) 0.38238( 111) 3.951(175) 1.000( 0) O12 0.15220( 140) -0.38289( 116) 0.35289( 98) 3.951(175) 1.000( 0) O13 -0.08742( 162) -0.39741( 128) 0.30432( 97) 3.951(175) 1.000( 0) O2 -0.15932( 169) -0.19331( 137) 0.03670( 104) 3.951(175) 1.000( 0) O3 -0.25358( 162) -0.35302( 145) 0.07231( 117) 3.951(175) 1.000( 0) O6 0.36001( 147) -0.54439( 115) 0.12317( 112) 3.951(175) 1.000( 0) ==> PROFILE PARAMETERS: => Cell parameters : 10.98557 0.00051 12.86374 0.00058 15.73026 0.00069 90.00000 0.00000 90.00000 0.00000 90.00000 0.00000 => Overall scale factor : 0.002741672 0.000014006 => ETA(p-V) or M(P-VII) : 0.53622 0.00643 => Overall Tem. factor : 0.00000 0.00000 => Halfwidth parameters : 0.06000 0.00000 0.01626 0.00246 0.02010 0.00046 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : 0.09914 0.00172 0.05854 0.00052 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: -0.0614 0.0012 => 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: 6.18 Rwp: 8.79 Rexp: 1.64 Chi2: 28.7 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 8.73 Rwp: 11.7 Rexp: 2.19 Chi2: 28.7 => Deviance: 0.130E+06 Dev* : 28.70 => DW-Stat.: 0.2349 DW-exp: 1.9588 => N-sigma of the GoF: 1320.892 ==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS: => N-P+C: 4535 => Rp: 6.18 Rwp: 8.79 Rexp: 1.64 Chi2: 28.7 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 8.73 Rwp: 11.7 Rexp: 2.19 Chi2: 28.7 => Deviance: 0.130E+06 Dev* : 28.71 => DW-Stat.: 0.2349 DW-exp: 1.9588 => N-sigma of the GoF: 1321.195 => Phase: 1 => Bragg R-factor: 3.67 Vol: 2222.930( 0.173) Fract(%): 0.00( 0.00) => Rf-factor= 6.06 ATZ: 0.000 Brindley: 1.0000 => Run finished at Date: 04/24/98 Time: 13:05:21.56