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 ### CCP4 7.0.078: Refmac          version 5.8.0258 : 09/10/19##
 ###############################################################
 User: malyma  Run date: 11/ 3/2021 Run time: 15:57:57 


 Please reference: Collaborative Computational Project, Number 4. 2011.
 "Overview of the CCP4 suite and current developments". Acta Cryst. D67, 235-242.
 as well as any specific reference in the program write-up.


 $TEXT:Reference1: $$ Primary reference $$ 
   "Overview of refinement procedures within REFMAC5: utilizing data from different sources"
   O.Kovalevskiy, R.A.Nicholls, F.Long, G.N.Murshudov,(2018) 
   Acta Crystallogr. D74, 492-505

 $$
 $SUMMARY :Reference1:  $$ Refmac: $$
 :TEXT:Reference1: $$

 $TEXT:Reference1: $$ Primary reference for EM $$ 
   "Current approaches for the fitting and refinement of atomic models into cryo-EM maps using CCP-EM
   R.A. Nicholls, M. Tykac, O.Kovalevskiy, G.N.Murshudov,(2018) 
   Acta Crystallogr. D74, 215-227

 $$
 $SUMMARY :Reference2:  $$ Refmac: $$
 :TEXT:Reference1: $$

 $TEXT:Reference1: $$ Secondary reference $$ 
   "REFMAC5 for the refinement of macromolecular crystal structures:"
   G.N.Murshudov, P.Skubak, A.A.Lebedev, N.S.Pannu, R.A.Steiner, R.A.Nicholls, M.D.Winn, F.Long and A.A.Vagin,(2011) 
   Acta Crystallogr. D67, 355-367

 $$
 $SUMMARY :Reference3:  $$ Refmac: $$
 :TEXT:Reference1: $$

 $TEXT:Reference2: $$ Secondary reference $$ 
   "Refinement of Macromolecular Structures by the  Maximum-Likelihood Method:"
   G.N. Murshudov, A.A.Vagin and E.J.Dodson,(1997)
   Acta Crystallogr. D53, 240-255
   EU  Validation contract: BIO2CT-92-0524

 $$
 $SUMMARY :Reference4:  $$ Refmac: $$
 :TEXT:Reference2: $$

  Data line--- make     check NONE
  Data line--- refi     type REST reso 47.32 2.00     resi MLKF     meth CGMAT     bref MIXED
  Data line--- scal     type SIMP     LSSC     ANISO     EXPE
  Data line--- solvent YES
  Data line--- bins 5
  Data line--- ncyc 10
  Data line--- weight matrix 0.0600
  Data line--- monitor MEDIum
  Data line--- free 0
  Data line--- END

 OPENED INPUT MTZ FILE 
 Logical Name: HKLIN   Filename: poli67_1-9A.mtz 

 LABIN FP=F_XDSdataset SIGFP=SIGF_XDSdataset FREE=FreeR_flag

    ****                     Input and Default parameters#                      ****


Input coordinate file.  Logical name - XYZIN actual file name  - poli_R00_2-10A.pdb
Output coordinate file. Logical name - XYZOUT actual file name - poli_R00_2-00A.pdb
Input reflection file.  Logical name - HKLIN actual file name  - poli67_1-9A.mtz
Output reflection file. Logical name - HKLOUT actual file name - poli_R00_2-00A.mtz

Cell from mtz :    58.265    79.758    94.643    90.000    90.000    90.000
Space group from mtz: number -   19; name - P 21 21 21

  Refinement type                        : Restrained

    ****                           Makecif parameters                           ****

Dictionary files for restraints : /protein2/ccp4/ccp4-7.0/ccp4-7.0/lib/data/monomers/mon*cif
Parameters for new entry and VDW: /protein2/ccp4/ccp4-7.0/ccp4-7.0/lib/data/monomers/ener_lib.cif
    Program will rely on residue and atom names. No checking
    If this option is used then monomers should be checked carefully before using
    Hydrogens will be restored in their riding positions
    Links between monomers will be checked. Only those links present in the coordinate file will be used
    Standard sugar links will be analysed and used
    For new ligands "ideal restraint" values will be taken from the energetic libary ener_lib.cif
    Symmetry related links will be analysed and used
    Cis peptides will be found and used automatically


  Residual                               : Rice Maximum Likelihood for Fs

    ****                    Least-square scaling parameters                     ****

Overall scale
Overall B value
Overall anisotropic B with tr(B) = 0.0
Constant bulk solvent in non protein region
Probe radii for non-ions     1.200
Probe radii for ions         0.800
Shrinkage of the mask  by    0.800


    ****                 Map sharpening parameters and methods                  ****

No map sharpening will be performed

  Method of minimisation                 : Sparse Matrix
  Experimental sigmas used for weighting
  Number of Bins and width:     5       0.0500
  Refinement of mixed isotropic and anisotropic Bfactors
  Refinement resln        :    47.3245  2.0000
  Estimated number of reflections :      40320
  Free R exclusion - flag equals:     0
  Weighting by comparison of trace of matrix
  Weighting parameters   :     0.0600
  Refinement cycles       :    10
  Scaling type                           :
          Wilson scaling type with Guassians

  Estimation of D/Sigma in resolution bins
  using  free set of reflns with experimental sigmas
  using  free set of reflns with experimental sigmas

  Scaling and SigmaA resln:    47.3245  2.0000

  Damping factors:     1.0000  1.0000  1.0000


    ****                    Geometry restraints and weights                     ****


                                              Sigma:
 Bonding distances
          Weight =  1.00

 Bond angles
          Weight =  1.00

 Planar groups (all and main chain)
          WEIGHT= 1.00 1.00

 Chiral centers
          Weight= 1.00

 NON-BONDED CONTACTS
          Overall weight                          =  1.00
          Sigma for simple VDW                    =  0.20
          Sigma for VDW trhough torsion angle     =  0.20
          Sigma for HBOND                         =  0.20
          Sigma for metal-ion                     =  0.20
          Sigma for DUMMY and other atom          =  0.30
          Distance for donor-accepetor = vdw1+vdw2+(-0.30)
          Distance for acceptor - H    = vdw1+     ( 0.10)
          VDW distance through torsion = vdw1+vdw2+(-0.30)
          Distance for DUMMY-others    = vdw1+vdw2+(-0.70)

 TORSION ANGLES
          Weight= 1.00

 THERMAL FACTORS
          Weight= 1.00
     Main chain bond (1-2 neighbour)          1.5A**2
     Main chain angle (1-3 neighbour)         2.0A**2
     Side chain bond                          3.0A**2
     Side chain angle                         4.5A**2

 RESTRAINTS AGAINST EXCESSIVE SHIFTS
     Positional parameters                   0.00A
     Thermal parameters                      0.00A
     Occupancy parameters                    0.00

 RADIUS OF CONFIDENCE
     Positional parameters 0.00A
     Thermal parameters    0.00A**2
     Occupancy parameters  0.00

Monitoring style is "MEDIUM". Complete information will be printed out in the
first and last cycle. In all other cycles minimum information will be printed out
Sigma cutoffs for printing out outliers
If deviation of restraint parameter > alpha*sigma then information will be printed out
Distance outliers      10.000
Angle outliers         10.000
Torsion outliers       10.000
Chiral volume outliers 10.000
Plane outliers         10.000
Non-bonding outliers   10.000
B value  outliers      10.000
Rigid bond outliers    10.000
Sphericity outliers    10.000
---------------------------------------------------------------

 Input file :poli_R00_2-10A.pdb
  ------------------------------
  ---  LIBRARY OF MONOMERS   ---
 _lib_name         mon_lib
 _lib_version      5.51
 _lib_update       11/07/18
  ------------------------------
  NUMBER OF MONOMERS IN THE LIBRARY          : 24624
                with complete description    : 24624
  NUMBER OF MODIFICATIONS                    :    70
  NUMBER OF LINKS                            :    77
  I am reading libraries. Please wait.
      - energy parameters
      - monomer"s description (links & mod )
  Number of atoms    :    2286
  Number of residues :     307
  Number of chains   :       3
  I am reading library. Please wait.
                mon_lib.cif
  --------------------------------
  --- title of input coord file ---

  PDB_code:xxxx
  PDB_name:----
  PDB_date:24-OCT-17
  --------------------------------
  ATTENTION: atom:OXT  ASN                69  AAA  is missing in the structure
  ATTENTION: atom:OXT  ARG               164  AAA  is missing in the structure
  ATTENTION: atom:OXT  PRO                36  BBB  is missing in the structure
  ATTENTION: atom:OXT  THR                70  BBB  is missing in the structure
  ATTENTION: atom:OXT  ASN               153  BBB  is missing in the structure
  Number of chains                  :       3
  Total number of monomers          :     307
  Number of atoms                   :    4696
  Number of missing atoms           :       5
  Number of rebuilt atoms           :    2331
  Number of unknown atoms           :       0
  Number of deleted atoms           :       0

_ccp4_form_factor.scat_method    'Sum of Gaussians'
_ccp4_form_factor.scat_data_source  X-ray


 loop_
     _atom_type_symbol
     _atom_type_scat_Cromer_Mann_a1
     _atom_type_scat_Cromer_Mann_b1
     _atom_type_scat_Cromer_Mann_a2
     _atom_type_scat_Cromer_Mann_b2
     _atom_type_scat_Cromer_Mann_a3
     _atom_type_scat_Cromer_Mann_b3
     _atom_type_scat_Cromer_Mann_a4
     _atom_type_scat_Cromer_Mann_b4
     _atom_type_scat_Cromer_Mann_c


  N     12.2220   0.0057   3.1346   9.8933   2.0141  28.9975   1.1672   0.5826 -11.5379
  H      0.4930  10.5109   0.3229  26.1257   0.1402   3.1424   0.0408  57.7997   0.0030
  C      2.3103  20.8439   1.0201  10.2075   1.5888   0.5687   0.8651  51.6512   0.2156
  O      3.0487  13.2771   2.2870   5.7011   1.5464   0.3239   0.8671  32.9089   0.2508
  S      6.9054   1.4679   5.2035  22.2151   1.4379   0.2536   1.5863  56.1720   1.0317


 Number of distances         :           0
 Number of angles            :           0
 Number of torsions          :           0
 Number of planes            :           0
 Number of chirals           :           0
 Number of intervals         :           0
--------------------------------------------------------------------------------
--------------------------------------------------------------------------------
                        Standard  External       All
                Bonds:      4485         0      4485
               Angles:      8175         0      8175
              Chirals:       284         0       284
               Planes:       646         0       646
             Torsions:      2321         0      2321
            Intervals:         0         0         0
--------------------------------------------------------------------------------


  Number of harmonic restraints       =            0
  Number of atoms in special position =            0
 -----------------------------------------------------


    ****                           Info from mtz file                           ****

FreeR flag                            0
Number of "free" reflections       1483
Number of   all  reflections      30492
--------------------------------------------------------------------------------
 Number of reflections in file      35470
 Number of reflections read          30492

   Current auto weighting coefficient =    7.4995480    

 mode : HKRF


######  TLS Group Definitions ######



     CGMAT cycle number =      1

 Limits of asymmetric unit      : 1.00 1.00 0.25
 Grid spacing to be used        :   108  160  176
 Maximuum H,K,L                 :    30   40   48
 Minimum acceptable grid spacing:    71   97  115
 Limits of asymmetric unit      : 1.00 1.00 0.25
 Grid spacing to be used        :   108  160  176
 Maximuum H,K,L                 :    30   40   48
 Minimum acceptable grid spacing:    71   97  115
 Weight matrix   5.99999949E-02
 Actual weight    21.373104      is applied to the X-ray term
Norm of X_ray positional gradient                33.9
Norm of Geom. positional gradient                77.4
Norm of X_ray B-factor gradient                  36.0
Norm of Geom. B-factor gradient                  31.0
Product of X_ray and Geom posit. gradients     -0.127E+08
 Cosine of angle between them                      -0.359
Product of X_ray and Geom B-fact gradients     -0.375E+07
 Cosine of angle between them                      -0.749


Residuals: XRAY=     0.2538E+07 GEOM=     0.1839E+05 TOTAL=     0.2557E+07
 function value    2556761.5    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.034     0.017
Bond angles  : refined atoms                   3054     1.962     1.648
Bond angles  : others                          5121     2.283     1.582
Torsion angles, period  1. refined              265     7.641     5.000
Torsion angles, period  2. refined              135    32.900    22.370
Torsion angles, period  3. refined              475    20.696    15.000
Torsion angles, period  4. refined               19    20.956    15.000
Chiral centres: refined atoms                   284     0.087     0.200
Planar groups: refined atoms                   2462     0.011     0.020
Planar groups: others                           467     0.014     0.020
VDW repulsions: refined_atoms                   540     0.234     0.200
VDW repulsions.others                          1997     0.227     0.200
VDW; torsion: refined_atoms                    1096     0.175     0.200
VDW; torsion.others                            1063     0.082     0.200
HBOND: refined_atoms                             56     0.196     0.200
HBOND.others                                      1     0.022     0.200
VDW repulsions: symmetry: refined_atoms          11     0.218     0.200
VDW repulsions: symmetry: others                 35     0.235     0.200
HBOND: symmetry: refined_atoms                    2     0.146     0.200
M. chain bond B values: refined atoms          1075     7.839     6.973
M. chain bond B values: others                 1074     7.812     6.964
M. chain angle B values: refined atoms         1335     9.951    10.408
M. chain angle B values: others                1336     9.951    10.417
S. chain bond B values: refined atoms          1209     9.175     7.773
S. chain bond B values: others                 1207     9.176     7.765
S. chain angle B values: refined atoms         1719    12.686    11.321
S. chain angle B values: others                1719    12.681    11.321
Long range B values: refined atoms             2620    14.615    79.933
Long range B values: others                    2619    14.631    79.955
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5151, B  =   -1.1710
Partial structure    1: scale =     0.3856, B  =   55.1115
Overall anisotropic scale factors
   B11 =   5.07 B22 =  -1.59 B33 =  -3.48 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------

    ****                Things for loggraph, R factor and others                ****


$TABLE: Cycle    1. Rfactor analysis, F distribution v resln  :
$GRAPHS:Cycle    1.  v. resln :N:1,6,7,11,12:
:Cycle    1.  and  v. resln :N:1,4,5,9,10:
:Cycle    1. % observed v. resln :N:1,3:
$$
M(4SSQ/LL) NR_used %_obs M(Fo_used) M(Fc_used) Rf_used WR_used
NR_free M(Fo_free) M(Fc_free) Rf_free   WR_free $$
$$
 0.025    2782  99.45   272.2   270.7  0.20  0.21     125   261.5   261.0  0.30  0.31
 0.075    4806  99.90   156.0   144.3  0.20  0.19     260   158.1   146.2  0.27  0.25
 0.125    6062  99.74    54.4    53.6  0.25  0.21     344    54.3    54.8  0.35  0.32
 0.175    7199  99.91    28.2    26.5  0.36  0.33     331    28.8    27.6  0.39  0.36
 0.225    8050  99.26    20.0    12.8  0.48  0.49     417    19.7    12.3  0.48  0.48
$$

    ****                      Fom and SigmaA vs resolution                      ****

 $TABLE: Cycle    1. FSC and  Fom(-acentric, centric, overall v resln:
 $GRAPHS:Cycle    1. M(Fom) v. resln :N:1,3,5,7,8,9,10,11,12:
 $$
 <4SSQ/LL> NREFa  FOMa  NREFc FOMc NREFall FOMall  SigmaA_Fc1 FSCfree  FSCwork CorrFoFcFree CorrFoFcWork$$
 $$
  0.0254   2157   0.813    625   0.746   2782   0.798  0.921  0.9082  0.9431  0.8509  0.9293
  0.0753   4157   0.823    649   0.742   4806   0.812  1.005  0.9125  0.9359  0.8497  0.9327
  0.1252   5428   0.706    634   0.640   6062   0.699  0.876  0.8314  0.8707  0.7285  0.8885
  0.1751   6547   0.496    652   0.450   7199   0.492  0.654  0.6224  0.6387  0.7046  0.7748
  0.2250   7412   0.339    645   0.305   8057   0.337  0.594  0.3580  0.3593  0.5885  0.5587
 $$
Resolution limits                    =     47.324     2.000
Number of used reflections           =      28906
Percentage observed                  =    99.6360
Percentage of free reflections       =     4.8613
Overall R factor                     =     0.2419
Free R factor                        =     0.3171
Average Fourier shell correlation    =     0.6882
AverageFree Fourier shell correlation=     0.6717
Overall weighted R factor            =     0.2141
Free weighted R factor               =     0.2918
Overall weighted R2 factor           =     0.2276
Free weighted R2 factor              =     0.3169
Average correlation coefficient      =     0.7796
Overall correlation coefficient      =     0.9615
Free correlation coefficient         =     0.9196
Cruickshanks DPI for coordinate error=     0.1675
DPI based on free R factor           =     0.1816
Overall figure of merit              =     0.5747
ML based su of positional parameters =     0.2638
ML based su of thermal parameters    =    11.3750
-----------------------------------------------------------------------------
 Trying gamma equal    0.0000000    
 Not converging with gamma equal    0.0000000    
 Trying gamma equal   5.24999984E-02
 Gamma decreased to   4.19999994E-02
 fvalues    118764.84       18388.158       2556761.5      1.00000003E+32


     CGMAT cycle number =      2

 Weight matrix   5.99999987E-02
 Actual weight    21.844925      is applied to the X-ray term


 function value    2602949.5    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.002     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5163, B  =   -0.2601
Partial structure    1: scale =     0.3854, B  =   54.9203
Overall anisotropic scale factors
   B11 =   5.02 B22 =  -1.59 B33 =  -3.43 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2417
Free R factor                        =     0.3157
Average Fourier shell correlation    =     0.6650
AverageFree Fourier shell correlation=     0.6523
Average correlation coefficient      =     0.7840
Overall figure of merit              =     0.5501
-----------------------------------------------------------------------------
 Trying gamma equal   4.19999994E-02
 Gamma decreased to   3.24545428E-02


 fvalues    118512.91       12112.767       2601419.0       2556761.5    

 fvalues    118512.91       12112.767       2601477.5       2601018.3    
 fvalues    118512.91       12112.767       2601477.5       2601018.3    


     CGMAT cycle number =      3

 Weight matrix   5.99999987E-02
 Actual weight    21.205545      is applied to the X-ray term


 function value    2526581.8    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.002     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5166, B  =   -0.1437
Partial structure    1: scale =     0.3854, B  =   54.7921
Overall anisotropic scale factors
   B11 =   5.01 B22 =  -1.58 B33 =  -3.42 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2416
Free R factor                        =     0.3159
Average Fourier shell correlation    =     0.6740
AverageFree Fourier shell correlation=     0.6623
Average correlation coefficient      =     0.7834
Overall figure of merit              =     0.5592
-----------------------------------------------------------------------------
 Trying gamma equal   3.24545428E-02
 Gamma decreased to   2.37768572E-02
 fvalues    118570.84       12222.451       2526581.8       2601018.3    


     CGMAT cycle number =      4

 Weight matrix   6.00000024E-02
 Actual weight    20.715912      is applied to the X-ray term


 function value    2466365.8    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5181, B  =   -0.0315
Partial structure    1: scale =     0.3856, B  =   54.7398
Overall anisotropic scale factors
   B11 =   4.99 B22 =  -1.58 B33 =  -3.42 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2416
Free R factor                        =     0.3163
Average Fourier shell correlation    =     0.6777
AverageFree Fourier shell correlation=     0.6654
Average correlation coefficient      =     0.7831
Overall figure of merit              =     0.5654
-----------------------------------------------------------------------------
 Trying gamma equal   2.37768572E-02
 Gamma decreased to   1.58880539E-02
 fvalues    118462.59       12305.076       2466365.8       2526581.8    


     CGMAT cycle number =      5

 Weight matrix   5.99999949E-02
 Actual weight    21.230045      is applied to the X-ray term


 function value    2528938.0    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5178, B  =   -0.0134
Partial structure    1: scale =     0.3854, B  =   54.6490
Overall anisotropic scale factors
   B11 =   4.99 B22 =  -1.57 B33 =  -3.42 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2416
Free R factor                        =     0.3160
Average Fourier shell correlation    =     0.6740
AverageFree Fourier shell correlation=     0.6619
Average correlation coefficient      =     0.7831
Overall figure of merit              =     0.5588
-----------------------------------------------------------------------------
 Trying gamma equal   1.58880539E-02
 Gamma decreased to   8.71641375E-03


 fvalues    118463.56       12304.552       2528817.8       2466365.8    

 fvalues    118463.56       12304.552       2528895.5       2527291.3    
 fvalues    118463.56       12304.552       2528895.5       2527291.3    


     CGMAT cycle number =      6

 Weight matrix   6.00000024E-02
 Actual weight    21.274906      is applied to the X-ray term


 function value    2534282.5    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5177, B  =   -0.0011
Partial structure    1: scale =     0.3854, B  =   54.6177
Overall anisotropic scale factors
   B11 =   4.98 B22 =  -1.57 B33 =  -3.42 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2415
Free R factor                        =     0.3160
Average Fourier shell correlation    =     0.6737
AverageFree Fourier shell correlation=     0.6616
Average correlation coefficient      =     0.7830
Overall figure of merit              =     0.5584
-----------------------------------------------------------------------------
 Trying gamma equal   8.71641375E-03
 Not converging with gamma equal   8.71641375E-03
 Trying gamma equal   4.29446921E-02
 Gamma decreased to   3.60990353E-02


 fvalues    118471.20       12318.942       2534445.5       2527291.3    

 fvalues    118471.20       12318.942       2534465.8       2532782.8    
 fvalues    118471.20       12318.942       2534465.8       2532782.8    


     CGMAT cycle number =      7

 Weight matrix   5.99999987E-02
 Actual weight    21.293957      is applied to the X-ray term


 function value    2536754.0    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5173, B  =   -0.0004
Partial structure    1: scale =     0.3853, B  =   54.5798
Overall anisotropic scale factors
   B11 =   4.97 B22 =  -1.56 B33 =  -3.41 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2416
Free R factor                        =     0.3160
Average Fourier shell correlation    =     0.6738
AverageFree Fourier shell correlation=     0.6616
Average correlation coefficient      =     0.7829
Overall figure of merit              =     0.5584
-----------------------------------------------------------------------------
 Trying gamma equal   3.60990353E-02
 Gamma decreased to   2.98757106E-02


 fvalues    118479.05       12324.650       2537026.3       2532782.8    

 fvalues    118479.05       12324.650       2537081.0       2535212.5    
 fvalues    118479.05       12324.650       2537081.0       2535212.5    


     CGMAT cycle number =      8

 Weight matrix   6.00000024E-02
 Actual weight    21.280476      is applied to the X-ray term


 function value    2535517.0    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5164, B  =   -0.0313
Partial structure    1: scale =     0.3854, B  =   54.6108
Overall anisotropic scale factors
   B11 =   4.97 B22 =  -1.56 B33 =  -3.41 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2416
Free R factor                        =     0.3161
Average Fourier shell correlation    =     0.6740
AverageFree Fourier shell correlation=     0.6617
Average correlation coefficient      =     0.7829
Overall figure of merit              =     0.5585
-----------------------------------------------------------------------------
 Trying gamma equal   2.98757106E-02
 Gamma decreased to   2.42181439E-02

 fvalues    118497.77       12327.005       2534016.0       2535212.5    


     CGMAT cycle number =      9

 Weight matrix   5.99999987E-02
 Actual weight    21.320093      is applied to the X-ray term


 function value    2540373.8    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5161, B  =   -0.0162
Partial structure    1: scale =     0.3854, B  =   54.6165
Overall anisotropic scale factors
   B11 =   4.97 B22 =  -1.56 B33 =  -3.41 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall R factor                     =     0.2416
Free R factor                        =     0.3162
Average Fourier shell correlation    =     0.6738
AverageFree Fourier shell correlation=     0.6615
Average correlation coefficient      =     0.7828
Overall figure of merit              =     0.5582
-----------------------------------------------------------------------------
 Trying gamma equal   2.42181439E-02
 Gamma decreased to   1.90749019E-02


 fvalues    118497.84       12330.905       2540374.0       2534016.0    

 fvalues    118497.84       12330.905       2540350.3       2538716.0    
 fvalues    118497.84       12330.905       2540350.3       2538716.0    


     CGMAT cycle number =     10

 Limits of asymmetric unit      : 1.00 1.00 0.25
 Grid spacing to be used        :   108  160  176
 Maximuum H,K,L                 :    30   40   48
 Minimum acceptable grid spacing:    71   97  115
 Limits of asymmetric unit      : 1.00 1.00 0.25
 Grid spacing to be used        :   108  160  176
 Maximuum H,K,L                 :    30   40   48
 Minimum acceptable grid spacing:    71   97  115
 Weight matrix   5.99999987E-02
 Actual weight    21.489595      is applied to the X-ray term
Norm of X_ray positional gradient                34.7
Norm of Geom. positional gradient                33.6
Norm of X_ray B-factor gradient                  37.4
Norm of Geom. B-factor gradient                  34.0
Product of X_ray and Geom posit. gradients     -0.156E+08
 Cosine of angle between them                      -0.995
Product of X_ray and Geom B-fact gradients     -0.557E+07
 Cosine of angle between them                      -0.976


Residuals: XRAY=     0.2548E+07 GEOM=     0.1233E+05 TOTAL=     0.2561E+07
 function value    2560503.5    

-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
Bond angles  : refined atoms                   3054     1.987     1.648
Bond angles  : others                          5121     1.410     1.582
Torsion angles, period  1. refined              265     7.687     5.000
Torsion angles, period  2. refined              135    32.913    22.370
Torsion angles, period  3. refined              475    20.795    15.000
Torsion angles, period  4. refined               19    21.097    15.000
Chiral centres: refined atoms                   284     0.088     0.200
Planar groups: refined atoms                   2462     0.011     0.020
Planar groups: others                           467     0.001     0.020
VDW repulsions: refined_atoms                   548     0.234     0.200
VDW repulsions.others                          2001     0.207     0.200
VDW; torsion: refined_atoms                    1098     0.175     0.200
VDW; torsion.others                            1057     0.095     0.200
HBOND: refined_atoms                             58     0.197     0.200
VDW repulsions: symmetry: refined_atoms          11     0.219     0.200
VDW repulsions: symmetry: others                 34     0.231     0.200
HBOND: symmetry: refined_atoms                    2     0.131     0.200
M. chain bond B values: refined atoms          1075     7.972     6.870
M. chain bond B values: others                 1074     7.959     6.862
M. chain angle B values: refined atoms         1335    10.146    10.250
M. chain angle B values: others                1336    10.147    10.258
S. chain bond B values: refined atoms          1209     9.352     7.701
S. chain bond B values: others                 1207     9.352     7.694
S. chain angle B values: refined atoms         1719    12.952    11.199
S. chain angle B values: others                1719    12.945    11.199
Long range B values: refined atoms             2628    14.940    78.890
Long range B values: others                    2628    14.948    78.930
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5162, B  =   -0.0113
Partial structure    1: scale =     0.3854, B  =   54.6183
Overall anisotropic scale factors
   B11 =   4.97 B22 =  -1.56 B33 =  -3.41 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------

    ****                Things for loggraph, R factor and others                ****


$TABLE: Cycle   10. Rfactor analysis, F distribution v resln  :
$GRAPHS:Cycle   10.  v. resln :N:1,6,7,11,12:
:Cycle   10.  and  v. resln :N:1,4,5,9,10:
:Cycle   10. % observed v. resln :N:1,3:
$$
M(4SSQ/LL) NR_used %_obs M(Fo_used) M(Fc_used) Rf_used WR_used
NR_free M(Fo_free) M(Fc_free) Rf_free   WR_free $$
$$
 0.025    2782  99.45   272.0   270.7  0.20  0.21     125   261.3   261.0  0.30  0.31
 0.075    4806  99.90   155.9   144.1  0.19  0.18     260   158.0   146.1  0.26  0.25
 0.125    6062  99.74    54.4    53.5  0.25  0.22     344    54.2    54.8  0.35  0.32
 0.175    7199  99.91    28.1    26.5  0.36  0.33     331    28.7    27.7  0.39  0.36
 0.225    8050  99.26    19.9    12.7  0.48  0.48     417    19.7    12.3  0.47  0.48
$$

    ****                      Fom and SigmaA vs resolution                      ****

 $TABLE: Cycle   10. FSC and  Fom(-acentric, centric, overall v resln:
 $GRAPHS:Cycle   10. M(Fom) v. resln :N:1,3,5,7,8,9,10,11,12:
 $$
 <4SSQ/LL> NREFa  FOMa  NREFc FOMc NREFall FOMall  SigmaA_Fc1 FSCfree  FSCwork CorrFoFcFree CorrFoFcWork$$
 $$
  0.0254   2157   0.825    625   0.756   2782   0.809  0.921  0.9104  0.9449  0.8510  0.9283
  0.0753   4157   0.824    649   0.741   4806   0.813  1.005  0.9137  0.9372  0.8523  0.9348
  0.1252   5428   0.728    634   0.659   6062   0.720  0.881  0.8400  0.8784  0.7231  0.8855
  0.1751   6547   0.459    652   0.419   7199   0.455  0.605  0.6054  0.6231  0.7110  0.7800
  0.2250   7412   0.283    645   0.261   8057   0.281  0.499  0.3209  0.3077  0.5915  0.5670
 $$
Resolution limits                    =     47.324     2.000
Number of used reflections           =      28906
Percentage observed                  =    99.6360
Percentage of free reflections       =     4.8613
Overall R factor                     =     0.2416
Free R factor                        =     0.3161
Average Fourier shell correlation    =     0.6719
AverageFree Fourier shell correlation=     0.6598
Overall weighted R factor            =     0.2139
Free weighted R factor               =     0.2911
Overall weighted R2 factor           =     0.2275
Free weighted R2 factor              =     0.3165
Average correlation coefficient      =     0.7828
Overall correlation coefficient      =     0.9615
Free correlation coefficient         =     0.9200
Cruickshanks DPI for coordinate error=     0.1673
DPI based on free R factor           =     0.1810
Overall figure of merit              =     0.5557
ML based su of positional parameters =     0.2642
ML based su of thermal parameters    =    11.5140
-----------------------------------------------------------------------------
 Trying gamma equal   1.90749019E-02
 Gamma decreased to   1.43992268E-02


 fvalues    118530.83       12331.902       2560401.5       2538716.0    

 fvalues    118530.83       12331.902       2560407.8       2559511.5    
 fvalues    118530.83       12331.902       2560407.8       2559511.5    

 LABOUT FreeR_flag=FreeR_flag F_XDSdataset=F_XDSdataset SIGF_XDSdataset=SIGF_XDSdataset FC=FC PHIC=PHIC FC_ALL=FC_ALL PHIC_ALL=PHIC_ALL FWT=FWT PHWT=PHWT DELFWT=DELFWT PHDELWT=PHDELWT FOM=FOM FC_ALL_LS=FC_ALL_LS PHIC_ALL_LS=PHIC_ALL_LS

 WRITTEN OUTPUT MTZ FILE 
 Logical Name: HKLOUT   Filename: poli_R00_2-00A.mtz 




-------------------------------------------------------------------------------
             Restraint type              N restraints   Rms Delta   Av(Sigma)
Bond distances: refined atoms                  2284     0.013     0.013
Bond distances: others                         2201     0.001     0.017
Bond angles  : refined atoms                   3054     1.987     1.648
Bond angles  : others                          5121     1.410     1.582
Torsion angles, period  1. refined              265     7.688     5.000
Torsion angles, period  2. refined              135    32.913    22.370
Torsion angles, period  3. refined              475    20.796    15.000
Torsion angles, period  4. refined               19    21.096    15.000
Chiral centres: refined atoms                   284     0.088     0.200
Planar groups: refined atoms                   2462     0.011     0.020
Planar groups: others                           467     0.001     0.020
VDW repulsions: refined_atoms                   548     0.234     0.200
VDW repulsions.others                          2001     0.207     0.200
VDW; torsion: refined_atoms                    1098     0.175     0.200
VDW; torsion.others                            1057     0.095     0.200
HBOND: refined_atoms                             58     0.197     0.200
VDW repulsions: symmetry: refined_atoms          11     0.219     0.200
VDW repulsions: symmetry: others                 34     0.231     0.200
HBOND: symmetry: refined_atoms                    2     0.131     0.200
M. chain bond B values: refined atoms          1075     7.972     6.870
M. chain bond B values: others                 1074     7.960     6.862
M. chain angle B values: refined atoms         1335    10.146    10.250
M. chain angle B values: others                1336    10.147    10.258
S. chain bond B values: refined atoms          1209     9.352     7.701
S. chain bond B values: others                 1207     9.353     7.694
S. chain angle B values: refined atoms         1719    12.952    11.198
S. chain angle B values: others                1719    12.945    11.199
Long range B values: refined atoms             2628    14.940    78.889
Long range B values: others                    2628    14.948    78.930
-------------------------------------------------------------------------------

-----------------------------------------------------------------------------
Overall scale should be multiplied by       1.0000
Overall               : scale =     1.5163, B  =   -0.0056
Partial structure    1: scale =     0.3854, B  =   54.6283
Overall anisotropic scale factors
   B11 =   4.97 B22 =  -1.56 B33 =  -3.41 B12 =   0.00 B13 =   0.00 B23 =   0.00
-----------------------------------------------------------------------------

-----------------------------------------------------------------------------

    ****                Things for loggraph, R factor and others                ****


$TABLE: Cycle   11. Rfactor analysis, F distribution v resln  :
$GRAPHS:Cycle   11.  v. resln :N:1,6,7,11,12:
:Cycle   11.  and  v. resln :N:1,4,5,9,10:
:Cycle   11. % observed v. resln :N:1,3:
$$
M(4SSQ/LL) NR_used %_obs M(Fo_used) M(Fc_used) Rf_used WR_used
NR_free M(Fo_free) M(Fc_free) Rf_free   WR_free $$
$$
 0.025    2782  99.45   272.0   270.7  0.20  0.21     125   261.3   261.0  0.30  0.31
 0.075    4806  99.90   155.9   144.1  0.19  0.18     260   158.0   146.1  0.26  0.25
 0.125    6062  99.74    54.4    53.5  0.25  0.22     344    54.2    54.8  0.35  0.32
 0.175    7199  99.91    28.1    26.5  0.35  0.33     331    28.7    27.7  0.39  0.36
 0.225    8050  99.26    19.9    12.7  0.48  0.48     417    19.7    12.3  0.47  0.48
$$

    ****                      Fom and SigmaA vs resolution                      ****

 $TABLE: Cycle   11. FSC and  Fom(-acentric, centric, overall v resln:
 $GRAPHS:Cycle   11. M(Fom) v. resln :N:1,3,5,7,8,9,10,11,12:
 $$
 <4SSQ/LL> NREFa  FOMa  NREFc FOMc NREFall FOMall  SigmaA_Fc1 FSCfree  FSCwork CorrFoFcFree CorrFoFcWork$$
 $$
  0.0254   2157   0.825    625   0.756   2782   0.809  0.921  0.9104  0.9449  0.8510  0.9283
  0.0753   4157   0.824    649   0.741   4806   0.813  1.005  0.9137  0.9372  0.8523  0.9348
  0.1252   5428   0.728    634   0.659   6062   0.720  0.881  0.8400  0.8784  0.7231  0.8855
  0.1751   6547   0.464    652   0.424   7199   0.461  0.616  0.6084  0.6258  0.7110  0.7800
  0.2250   7412   0.287    645   0.264   8057   0.285  0.506  0.3246  0.3119  0.5915  0.5670
 $$
Resolution limits                    =     47.324     2.000
Number of used reflections           =      28906
Percentage observed                  =    99.6360
Percentage of free reflections       =     4.8613
Overall R factor                     =     0.2416
Free R factor                        =     0.3161
Average Fourier shell correlation    =     0.6738
AverageFree Fourier shell correlation=     0.6615
Overall weighted R factor            =     0.2139
Free weighted R factor               =     0.2911
Overall weighted R2 factor           =     0.2275
Free weighted R2 factor              =     0.3165
Average correlation coefficient      =     0.7828
Overall correlation coefficient      =     0.9615
Free correlation coefficient         =     0.9200
Cruickshanks DPI for coordinate error=     0.1673
DPI based on free R factor           =     0.1810
Overall figure of merit              =     0.5582
ML based su of positional parameters =     0.2642
ML based su of thermal parameters    =    11.5140
-----------------------------------------------------------------------------
  Time in seconds: CPU =        45.51
             Elapsed =         128.00

    ****           Things for loggraph, R factor and others vs cycle            ****


$TABLE: Rfactor analysis, stats vs cycle  :
$GRAPHS: vs cycle :N:1,2,3:
:FOM vs cycle :N:1,4:
:-LL vs cycle :N:1,5:
:-LLfree vs cycle :N:1,6:
:Geometry vs cycle:N:1,7,8,9,10,11:
$$
    Ncyc    Rfact    Rfree     FOM      -LL     -LLfree  rmsBOND  zBOND rmsANGL  zANGL rmsCHIRAL $$
$$
       0   0.2419   0.3171   0.575      118765.    6212.8   0.0127  0.880   1.962  1.163   0.087
       1   0.2417   0.3157   0.550      118601.    6209.9   0.0129  0.898   1.959  1.161   0.087
       2   0.2416   0.3159   0.559      118571.    6209.0   0.0130  0.906   1.970  1.168   0.088
       3   0.2416   0.3163   0.565      118463.    6205.8   0.0131  0.909   1.980  1.174   0.088
       4   0.2416   0.3160   0.559      118541.    6209.2   0.0131  0.906   1.983  1.176   0.088
       5   0.2415   0.3160   0.558      118542.    6209.3   0.0131  0.907   1.985  1.177   0.088
       6   0.2416   0.3160   0.558      118551.    6209.8   0.0131  0.907   1.986  1.177   0.088
       7   0.2416   0.3161   0.558      118568.    6210.7   0.0131  0.908   1.986  1.178   0.088
       8   0.2416   0.3162   0.558      118576.    6211.0   0.0131  0.908   1.986  1.178   0.088
       9   0.2416   0.3161   0.556      118577.    6211.2   0.0131  0.908   1.987  1.178   0.088
      10   0.2416   0.3161   0.558      118572.    6210.8   0.0131  0.908   1.987  1.178   0.088
 $$
 $TEXT:Result: $$ Final results $$
                      Initial    Final
           R factor    0.2419   0.2416
             R free    0.3171   0.3161
     Rms BondLength    0.0127   0.0131
      Rms BondAngle    1.9622   1.9866
     Rms ChirVolume    0.0867   0.0879
 $$
 Harvest: NO PNAME_KEYWRD given - no deposit file created

 Refmac:  End of Refmac_5.8.0258   
Times: User:      86.5s System:    0.3s Elapsed:     1:34