#------------------------------------------------------------------------------ #$Date: 2018-05-28 03:23:28 +0300 (Mon, 28 May 2018) $ #$Revision: 207993 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/94/1549467.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1549467 loop_ _publ_author_name 'Birger Dittrich' 'Justin Bergmann' 'Peter Roloff' 'Guido J. Reiss' _publ_section_title ; New Polymorphs of the Phase-Change Material Sodium Acetate ; _journal_name_full Crystals _journal_page_first 213 _journal_paper_doi 10.3390/cryst8050213 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C2 H3 Na O2' _chemical_formula_sum 'C2 H3 Na O2' _chemical_formula_weight 82.03 _chemical_name_common 'Sodium Acetate' _chemical_name_systematic 'Sodium Acetate' _space_group_crystal_system orthorhombic _space_group_IT_number 54 _space_group_name_Hall '-P 2a 2ac' _space_group_name_H-M_alt 'P c c a' _symmetry_space_group_name_Hall '-P 2a 2ac' _symmetry_space_group_name_H-M 'P c c a' _atom_sites_solution_hydrogens difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_date '14-Mar-03 T19:02:38-00:00' _audit_creation_method 'XD routine XDCIF' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.9482(7) _cell_length_b 10.0866(10) _cell_length_c 5.8984(6) _cell_measurement_reflns_used 9994 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 35.7848 _cell_measurement_theta_min 4.0571 _cell_volume 353.89(7) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS, 2014)' _computing_data_collection 'APEX2 v2014.11-0' _computing_data_reduction 'SAINT V8.38A (Bruker AXS, 2014)' _computing_molecular_graphics 'H\"ubschle, (2011)' _computing_publication_material 'enCIFer 1.5.1, CCDC, 2012' _computing_structure_refinement 'XDLSM, Volkov et al, (2006)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Huber Type 512 four circle diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_unetI/netI 0.0130 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 52457 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.515 _diffrn_reflns_theta_min 2.027 _diffrn_source 'Incoatec 3.0 microsource' _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_T_max 0.6499 _exptl_absorpt_correction_T_min 0.5303 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; SADABS version 2016/2, multi-scan. (G. M. Sheldrick, 2016) ; _exptl_crystal_density_diffrn 1.540 _exptl_crystal_description plate _exptl_crystal_F_000 168 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.227 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.5854 _refine_ls_matrix_type full _refine_ls_number_parameters 37 _refine_ls_number_reflns 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.029 _refine_ls_shift/su_max 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w2 = q/[s^2^(Fo^2^) + (0.03 P)^2^ + 0.08 P + 0.00 + 0.00 sin(th)] where P = (0.3333 Fo^2^ + 0.6667 Fc^2^) q = 1.0 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.081 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 704 _reflns_number_total 840 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file NaAc_pcca.cif _cod_data_source_block ortho _cod_database_code 1549467 _iucr_instruction_details ; !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! ! <<< X D MASTER FILE >>> $Revision: 6.03 (Jul 23 2008)$ 24-Jan-01! !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! TITLE ORTHO CELL 5.9482 10.0866 5.8984 90.000 90.000 90.000 WAVE 0.71073 CELLSD 0.0007 0.0010 0.0006 0.000 0.000 0.000 LATT C P SYMM 1/2-X, -Y, Z SYMM -X, Y, 1/2-Z SYMM 1/2+X, -Y, 1/2-Z BANK VM !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE *XDLSM SELECT *model 4 2 1 0 based_on F\^2 test SELECT cycle 10 dampk 1. cmin 0.6 cmax 1. eigcut 1.d-09 convcrit 0.0 SAVE deriv lsqmat *cormat SOLVE *inv diag *cond !------------------------------------------------------------------------------ SCAT CORE SPHV DEFV 1S 2S 3S 4S 2P 3P 4P 3D 4D 4F 5S 5P 6S 6P 5D 7S 6D 5F DELF' DELF'' NSCTL Na CHFW CHFW CSZD 2 2 -1 0 6 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0360 0.0250 0.363 O CHFW CHFW CSZD 2 -2 0 0 -4 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0110 0.0060 0.580 C CHFW CHFW CSZD 2 -2 0 0 -2 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0030 0.0020 0.665 H CHFW CHFW CSZD -1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0000 0.0000 -0.374 END SCAT !------------------------------------------------------------------------------ ATOM ATOM0 AX1 ATOM1 ATOM2 AX2 R/L TP TBL KAP LMX SITESYM CHEMCON Na(1) O(1) Z Na(1) C(1) Y R 2 1 1 4 _chemcon?? O(1) C(1) X O(1) DUM1 Y R 2 2 2 4 _mz O(2) C(1) X O(2) DUM2 Y R 2 2 2 4 _mz C(1) O(1) X C(1) DUM1 Y R 2 3 3 4 _mz C(2) C(1) Z C(2) H(2C) X R 2 3 4 4 _3my H(2A) C(2) Z H(2A) C(1) Y R 1 4 5 4 _6 H(2B) C(2) Z H(2B) C(1) Y R 1 4 5 4 _6 H(2C) C(2) Z H(2C) C(1) Y R 1 4 5 4 _6 DUM0 0.000000 0.000000 0.000000 DUM1 0.630835 0.643207 0.616691 DUM2 0.632025 0.645111 0.883309 END ATOM GROUP2 Na(1) O(2) O(1) C(1) C(2) H(2A) H(2B) H(2C) KEEP CHARGE GROUP2 !------------------------------------------------------------------------------ !GROUP2 atom1 atom2 ... KEEP kappa 1 2 3 4 KEEP charge group1 !KEEP rigid group1 !RESET bond C(1) H(1) 1.09 ... ! RESET BOND C(2) H(2A) 1.091370! it was 0.960002 A before. ! RESET BOND C(2) H(2B) 1.091370! it was 0.960004 A before. ! RESET BOND C(2) H(2C) 1.091370! it was 0.960001 A before. ! RESET BOND C(2) H(2C) 1.091370! it was 0.960001 A before. WEIGHT .03 .08 .0 .0 .0 0.3333 !SWAT g 0.00 U 0.00 SKIP *obs -500. 1.d10 *sigobs 2. 1.d06 sinthl 0. 2. PRINT sinthl .0 2. *obs -500. 15. delta 0. 10. *del% 80 100 extcn 80. 100. *abssc !EXTCN *iso aniso *type_1 type_2 type_3 distr_g *distr_l msc_0 msc_1 DMSDA 1.1 1.8 FOUR fmod1 4 2 0 0 fmod2 -1 2 0 0 !CON num1 par1/iat1 num2 par2/iat2 ... = num0 !These are riding hydrogen constraints. !CON 1.0 X/5 -1.0 X/6 = 0 CON 1.0 Y/5 -1.0 Y/6 = 0 !CON 1.0 Z/5 -1.0 Z/6 = 0! Atom 5 is C(2), atom 6 is H(2A) !CON 1.0 X/5 -1.0 X/7 = 0 CON 1.0 Y/5 -1.0 Y/7 = 0 !CON 1.0 Z/5 -1.0 Z/7 = 0! Atom 5 is C(2), atom 7 is H(2B) !CON 1.0 X/5 -1.0 X/8 = 0 CON 1.0 Y/5 -1.0 Y/8 = 0 !CON 1.0 Z/5 -1.0 Z/8 = 0! Atom 5 is C(2), atom 8 is H(2C) !Order u11 u22 u33 u12 u13 u23 ! Special position constraints for Na01 ! x = 0.5000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 ! Input constraints retained (at least in part) for sof ! Special position constraints for C1 ! x = 0.5000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 ! Input constraints retained (at least in part) for sof ! Special position constraints for C2 ! x = 0.5000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 ! Input constraints retained (at least in part) for sof !------------------------------------------------------------------------------ KEY XYZ --U2-- ----U3---- ------U4------- M- -D- --Q-- ---O--- ----H---- Na(1) 010 111010 0000000000 000000000000000 00 000 00000 0000000 000000000 O(1) 111 111111 0000000000 000000000000000 00 000 00000 0000000 000000000 O(2) 111 111111 0000000000 000000000000000 00 000 00000 0000000 000000000 C(1) 010 111010 0000000000 000000000000000 00 000 00000 0000000 000000000 C(2) 010 111010 0000000000 000000000000000 00 000 00000 0000000 000000000 H(2A) 010 100000 0000000000 000000000000000 00 000 00000 0000000 000000000 H(2B) 010 100000 0000000000 000000000000000 00 000 00000 0000000 000000000 H(2C) 010 100000 0000000000 000000000000000 00 000 00000 0000000 000000000 KAPPA 000000 KAPPA 000000 KAPPA 000000 KAPPA 000000 KAPPA 000000 EXTCN 0000000 OVTHP 0 SCALE 1 END KEY !------------------------------------------------------------------------------ END XDLSM !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDFFT SELECT *fobs *fmod1 fmod2 snlmin 0. snlmax 2. sig 3. phase 0. SELECT gridsize 0.2 scale 1. npeak 10 nhole 10 neutron gridf peakf END XDFFT !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE *XDFOUR SELECT *fobs *fmod1 fmod2 print snlmin 0. snlmax 2. GRID 3-points perp *cryst ATOM label ato(1) symm 1 trans 0 0 0 *mark on plot ATOM label ato(2) symm 1 trans 0 0 0 *mark on plot ATOM label ato(3) symm 1 trans 0 0 0 *mark on plot LIMITS xmin .0 xmax 1.0 nx 100 LIMITS ymin .0 ymax 1.0 ny 100 LIMITS zmin .0 zmax 1.0 nz 100 END XDFOUR !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDPROP ! !-----General section----- ! SIZE napl 8 MODEL iam *multipole ! *au will print results in a.u. but input is always given in Ang SELECT numdx esd au verbose 1 PROPERTY *rho gradrho d2rho nucpot core valence defden esp ef efg ! ! Define the cluster of atoms to be included: !CRYSTAL alim [amin] [amax] blim [bmin] [bmax] clim [cmin] [cmax] !APPLY symm 1 translations 0 0 0 ato(1) ato(2) ... !GROUP ato(1) ato(2) ... (atom label) !OMIT 1 2 ... 4 -8 (number in atom list) ! ! Parameters for topological analysis: SELECT cpcut 1.0d-6 lmax 4 nstep 20 rcut 4.0 SELECT scale 0.05 dx 0.001 ds 0.005 SELECT rEcrit 0.00001 rNcrit 0.00001 ! ! Parameters for the integration routine: ODESOLVE *rk bs eps 1.D-06 stepi 0.01 QUADINT iqt 2 Nrad 50 Nang 194 Becke *Stock ! ! Method for calculation of ESP/EF/EFG EPFG EP aMM mMM *EPMM rCrit1 6.0 rCrit2 15. ! Origin of the coordinate system for molecular moments ORIGIN *mass charge geom ucell ! ! Export atomic moments to Orient/MIN16 !EXPORT *orient *min16 lmax [4] nmol [k] natmol [i=1..k] ! !------End of General section----- ! ! Atomic/Molecular moments from pseudoatoms : MULTMOM ! ! Calculate d-orbital populations for transition metals !D-POP use *Pv *P00 ! ! Atomic/Molecular from STOCKHOLDER partitioning: !STOCKMOM atoms all *unique select ato(1) ato(2) ... ! ! Evaluation of intermolecular interaction energy and lattice energy: ! !ATATPOT *EXREP spack wilcox lj *saptP saptA !ATATPOT *DISPR spack wilcox lj *saptP saptA !ATATPOT INDUC saptP saptA !HBONDS atoH(1) ato(1) rHBOND(1) atoH(2) ato(2) rHBOND(2) ... !HPOLAR atoH(1) atoH(2) .... ! !INTEREN frag 1 nat1 -nat2 *neutral !INTEREN frag 2 nat3 -nat4 *neutral !INTEREN EP aMM mMM *EPMM rCrit1 4. rCrit2 15. ! !LATEN frag1 1 -10 *neutral !LATEN radii 0. 100. !LATEN EP aMM mMM *EPMM rCrit1 4. rCrit2 15. ! NUCPROP (*)all (*)selected [n1] [n2] [-n3] ... ! ! Atomic charges fitting electrostatic potential: !QFIT grid 11 length 7.0 width 1.0 constrain false !CONSTRAIN ato(1) ato(2) ... ! ! Function plots: !POINT x y z !LINE ato(1) ato(2) npts 50 !LINE points x1 y1 z1 x2 y2 z2 npts 50 !VECPLOT *labels *zcut 1.2 omitrad 0.2 *vcut 0.8 vscale 1. xytol 0.4 !MAP atoms ato(1) ato(2) ato(3) npts 50 stepsize 0.1 !MAP bvect1 x1 y1 z1 bvect2 x2 y2 z2 cen x0 y0 z0 npts 50 stepsize 0.1 !CUBE centre x y z npts 30 stepsize 0.1 !CUBE ato(1) ato(2) npts 20 stepsize 0.1 !CUBE hirshf xd_iam_mol.grd xd_iam_xtal.grd ! ! Gradient field plots (only for rho and esp functions): !TRAJPLT origin atom ato(1) !TRAJPLT xaxis atom ato(2) Xdim1 -3.0 Xdim2 3.0 !TRAJPLT yaxis point x y z Ydim1 -3.0 Ydim2 3.0 !TRAJPLT mark *atoms *labels *bonds *cps *basins *hbonds !TRAJPLT params Circle 0.1 ATrad 0.05 CPrad 0.08 CPgrid 0.3 CPlim 1.0d-4 !TRAJPLT *plot *plane npath 36 *zcut 0.3 *xytol 0.5 *all select ato(1) ! ! Local Source Function (only for rho and esp functions): !SOURCE refpoint x y z !SOURCE point x y z !SOURCE line ato(1) ato(2) npts 50 !SOURCE map atoms ato(1) ato(2) ato(3) npts 100 stepsize 0.1 !SOURCE cube ato(1) ato(2) ato(3) npts 20 stepsize 0.1 ! ! Topological analysis: !CPSEARCH bond ato(1) ato(2) !CPSEARCH bond rmin 1.2 rmax 1.6 !CPSEARCH ring ato(1) ato(2) ... !CPSEARCH shell ato(1) rmin 0.3 rmax 0.5 nrad 5 nang 11 11 cutoff 16.0 !CPSEARCH bubble ato(1) rmin 0.3 rmax 0.5 curv -3 ncps 3 !CPSEARCH point x y z !CPSEARCH line vec1 x1 y1 z1 vec2 x2 y2 z2 npts 15 !CPSEARCH start file.cps !BPATH ato(1) ato(2) algrithm 2 !MOLGR *auto level 1 rmin 0.8 rmax 3.5 algrithm 2 profile ! ! Atomic basin integration: !TOPINT step 0.01 accur 0.001 rmax 8.0 nmax 20 !TOPINT spheres ato(1) r1 ato(2) r2 ..... !TOPINT atoms all *unique select ato(1) ato(2) ... ! ! DFT Energy calculation: !DFTENERG *run rCrit 1.D-04 ! END XDPROP !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDGEOM SELECT rmin 0.8 rmax 1.8 tor *ato *bon *ang loc non *export END XDGEOM !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDVIB SELECT temp 100. scale 1. *nlinear linear MODES *all frqmin 0. frqmax 1500. !MODES include 1 2 3 ... !MODES exclude 1 2 3 ... DATAFILE *gaussian g98.out orient *standard input END XDVIB !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE TOPXD SIZE napl 2000 COMT just a comment for this run DEBG symeqv deriv check TRSH eigenvec 1.0d-10 nr 1.D-08 CGEN alim -0.5 1.5 blim -0.5 1.5 clim -0.5 1.5 MPAR rcut 4.0d0 dstep 5.d-3 au iam esp !DGRD *use *gen fra gstep 0.2 0.2 0.2 read *ascii fort.69 ! !TRHO *seed all ail debug nstep 12 nnb 15 rmax 3.0 th 2.7 ! fra 0. 0. 0. ! car 0. 0. 0. !TRHO *cluster all ail debug nstep 11 nnb 10 rmax 3.0 th 2.7 !TRHO *pairs nr ail debug nstep 11 nnb 9 rmax 5. th 2.2 pc 0.3 !TRHO *points nr ail debug nstep 20 nnb 9 rmax 5 fra ! 0.0 0.0 0.0 ! 0.5 0.5 0.5 !TRHO *line nr ail debug nstep 10 nnb 20 rmx 5. pc 0.3 ! point fra 0. 0. 0. 0.5 0.5 0.5 ! point car 0. 0. 0. 2. 2. 2. !TRHO *grid nr ail debug nstep 10 nnb 9 rmax 5 ncons 0 ! xmin 0. xmax 1. xstep 0.01 ! ymin 0. ymax 1. ystep 0.01 ! zmin 0. zmax 1. zstep 0.01 !TRHO *profile perstep 2. ! *atom ato(1) toneighbor 1 2 3 ! *point fra 0. 0. 0. 1. 1. 1. ! *point car 0. 0. 0. 2. 2. 2. ! !TLAP *auto ef CCCP ail debug nstep 15 nnb 10 rmax 3.0 ntheta 8 nphi 16 ! atoms ato(1) ato(2) ... nmax 0 rstar 0.d0 ! atoms ato(3) ato(4) ... nmax 2 rstar 0.d0 ! nna x 1. y 1. z 1. nmax 4 rstar 3.2 ! nna x 2. y 2. z 2. nmax 4 rstar 3.2 !TLAP *auto nr ail debug nstep 20 nnb 12 rmax 3.0 ntheta 16 nphi 8 ! atoms ato(1) ato(2) ... nmax 0 rstar 0.d0 !TLAP *points nr ail debug nstep 23 nnb 11 rmax 4.0 nmax 14 ! car 1. 1. 1. ! fra 0. 0. 0. !TLAP *line nr ail debug nstep 12 nnb 12 rmax 3.0 nmax 0 ! atom ato(1) toneighbor 1 2 3 ! points fra 0. 0. 0. 1. 1. 1. ! points car 0. 0. 0. 2. 2. 2. ! !ATBP Params PhInSph 48 ThInSp 32 *SavSurf !ATBP Spheres ato(1) 0.2 ato(2) 0.2 ... !ATBP AltGuess BigStep 0.5 Accur 0.002 MaxRInt 10.00 Rmax 10.0 Step0 0.025 A 0.0 B 0.0 !ATBP *atoms ato(1) iZFS nvi 100 IRsur 0 *IRSav Rest Debug Phi 32 Th 24 Rad 120 Accur 1.D-3 !ATBP nna 0 ! x 0. y 0. z 0. *integ sphere 0.2 iZFS nvi 5 irsur -1 irsav rest debug phi 8 th 4 rad 120 ncp 0 ! !VZ3D *plot ! files rays.dat ! basins ato(1) ato(2) ... ! range *default xmi 0. ymi 0. zmi 0. xma 1. yma 1. zma 1. ! grid *default dx 0.05 dy 0.05 dz 0.05 rvec *default 0.20 !END VZ3D ! !PL2D general ! point car 0. 0. 0. ! atom 1 0 -1 0 ! atom 2 -1 0 -1 ! plotdim xmin -2. xmax 2. xstep 0.5 ymin -2. ymax 2. ystep 0.5 ! origin ishift 5 origin 0. 0. 0. vmod 0.5 ! misc size a4 scale 0.4 name 'test2d' title 'TOPXD rulez!' !PL2D *rhoo nstar 10 rmax 3.0 test cut 0.5 0.2 !PL2D *lapp nstar 10 rmax 3.0 test cut 0.5 0.2 !PL2D *lapm nstar 10 rmax 3.0 test cut 0.5 0.2 !PL2D *grho nstar 10 rmax 3.0 test cut 0.5 0.2 !PL2D *trajgrad nstar 10 rmax 5.0 test cut 0.5 0.2 toler 0.5 0.5 *plane npath 36 nextr 0 !PL2D *molgraph nstar 10 rmax 5.0 test cut 0.5 0.2 toler 0.5 0.5 *plane thr 1.6 *tr1 *tr2 *tr3 !PL2D *trajmolg nstar 10 rmax 5.0 test cut 0.5 0.2 toler 0.5 0.5 *plane thr 1.6 *tr1 *tr2 *tr3 npath 36 nextr 0 ! !PL3D general fra ! xmin 0.0 xmax 0.5 xstep 0.05 ! ymin 0.0 ymax 0.5 ystep 0.05 ! zmin 0.0 zmax 0.5 zstep 0.05 ! name 'test3d' !PL3D *plot rhoo lapp grho ! !P2DCRY *diff rhoo file1 file2 !P2DCRY *diff lapm file3 file4 !P2DCRY diff test2d rhoo !P2DCRY diff test2d trajmolg ! END TOPXD !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDPDF SELECT atom atom(1) scale 1.0 orth CUMORD second third fourth GRID 3-points *cryst !ATOM label atom(2) symm 1 trans 0 0 0 !ATOM xyz 0. 0. 0. LIMITS xmin -0.8 xmax 0.8 nx 51 LIMITS ymin -0.8 ymax 0.8 ny 51 LIMITS zmin -0.8 zmax 0.8 nz 51 END XDPDF !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDHKL SELECT *merge zero remove crypher SELECT export stlmin 0.0 stlmax 1.1 nbatch -1 INPUT xd.hkl END XDHKL !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! MODULE XDSFR SELECT *resol hklim hklist print 100 Uiso 0.0 SELECT title UCELL 30.0 30.0 30.0 90.0 90.0 90.0 WFNFL file <wfn filename> INT3D iqt 1 Nr 70 Nang 590 RESOL stlmin 0 stlmax 1.1 HKLIM hmin -10 hmax 10 kmin -10 kmax 10 lmin -10 lmax 10 HKLIST file <hkl listfile> maxref -1 EXPORT *xd *shelx crystal nbatch -1 END XDSFR !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! ! <<< X D PARAMETER FILE >>> $Revision: 6.03 (Jul 23 2008)$ 14-Mar-03! !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!! XDPARFILE VERSION 2 ORTHO MODEL 4 2 1 0 LIMITS nat 8 ntx 31 lmx 4 nzz 5 nto 0 nsc 20 ntb 4 nov 71 USAGE 8 2 4 5 0 1 0 3 4 4 40 1 10 3 0.028664 0.034934 0.028664 0.034934 0.042550 0.081146 1.585371 0.167E+04 0.030000 0.080000 0.000000 0.000000 0.000000 0.333300 0.0000000000 0.0000000000 0.0000000000 0.6308350000 0.6432070000 0.6166910000 0.6320250000 0.6451110000 0.8833090000 Na(1) 3 2 2 1 4 2 1 1 4 1 0 0.500000 0.583754 0.250000 0.5000 0.009911 0.018720 0.008983 0.000000 0.000107 0.000000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 O(1) 1 2 4 2 10 2 2 2 4 1 0 0.367932 0.642460 0.884320 0.8581 0.010172 0.026476 0.007999 -0.002358 0.000322 0.002176 5.4103 0.0000 -0.0576 -0.0009 0.0000 -0.0462 0.0000 0.0000 -0.0522 0.0011 0.0000 -0.0106 -0.0013 0.0000 0.0000 0.0287 0.0044 -0.0033 0.0000 0.0000 -0.0008 0.0003 0.0000 0.0000 0.0060 0.0048 O(2) 1 2 4 3 11 2 2 2 4 1 0 0.368098 0.642602 0.614477 0.1419 0.021566 0.013082 0.032818 -0.003622 0.001506 -0.004284 0.8947 0.0000 -0.0095 -0.0002 0.0000 -0.0076 0.0000 0.0000 -0.0086 0.0002 0.0000 -0.0018 -0.0002 0.0000 0.0000 0.0048 0.0007 -0.0005 0.0000 0.0000 -0.0001 0.0001 0.0000 0.0000 0.0010 0.0008 C(1) 1 2 2 4 10 2 3 3 4 1 0 0.500000 0.701459 0.750000 0.5000 0.010500 0.016090 0.010133 0.000000 0.001463 0.000000 2.0444 0.0000 0.0070 0.0143 0.0000 -0.1148 0.0000 0.0000 0.0298 -0.0357 0.0000 0.0019 0.0048 0.0000 0.0000 0.1368 0.0335 0.0042 0.0000 0.0000 0.0072 -0.0080 0.0000 0.0000 -0.0043 -0.0226 C(2) 3 1 4 5 8 2 3 4 4 1 0 0.500000 0.852164 0.750000 0.5000 0.038447 0.015568 0.038198 0.000000 0.005860 0.000000 1.9079 0.0000 0.0000 0.0000 0.0050 -0.0021 0.0000 0.0000 0.0000 0.0000 0.1084 0.0000 0.0000 0.0000 0.0000 0.0841 0.0000 0.0131 0.0000 0.0000 0.0000 0.0000 -0.0374 0.0000 0.0000 0.0000 H(2A) 3 2 5 6 4 1 4 5 4 1 0 0.407265 0.888230 0.602739 0.5000 0.060526 0.000000 0.000000 0.000000 0.000000 0.000000 0.5809 0.0000 0.0000 0.0000 0.0756 0.0315 0.0000 0.0000 0.0000 0.0000 0.0081 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0019 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 H(2B) 3 2 5 7 4 1 4 5 4 1 0 0.672831 0.888231 0.742642 0.5000 0.055510 0.000000 0.000000 0.000000 0.000000 0.000000 0.5809 0.0000 0.0000 0.0000 0.0756 0.0315 0.0000 0.0000 0.0000 0.0000 0.0081 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0019 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 H(2C) 3 2 5 8 4 1 4 5 4 1 0 0.419903 0.888231 0.904619 0.5000 0.050902 0.000000 0.000000 0.000000 0.000000 0.000000 0.5809 0.0000 0.0000 0.0000 0.0756 0.0315 0.0000 0.0000 0.0000 0.0000 0.0081 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0019 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 1 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 2 0.989501 1.078251 1.078251 1.078251 1.078251 1.078251 3 1.000202 1.000000 1.000000 1.000000 1.000000 1.000000 3 1.018393 1.000000 1.000000 1.000000 1.000000 1.000000 4 1.114404 1.200000 1.200000 1.200000 1.200000 1.200000 0.0000E+00 0.0000E+00 0.0000E+00 0.0000E+00 0.0000E+00 0.0000E+00 0.0000E+00 0.0000E+00 0.139318E+01 ; _xd_hkl_file ; ortho F\^2 NDAT 7 2 1 0 1 983.114 18.5664 1.0000 4 1 0 1 59.7985 5.31345 1.0000 6 1 0 1 392.347 23.8421 1.0000 0 2 0 1 410.157 6.59083 1.0000 2 2 0 1 13.5117 0.69269 1.0000 4 2 0 1 104.863 1.97274 1.0000 6 2 0 1 0.87220 3.40174 1.0000 8 2 0 1 11.1405 4.41569 1.0000 0 3 0 1 3121.86 48.0694 1.0000 2 3 0 1 59.9627 0.84244 1.0000 4 3 0 1 754.119 11.2667 1.0000 6 3 0 1 42.3799 1.80628 1.0000 8 3 0 1 180.882 8.79408 1.0000 0 4 0 1 9109.14 118.478 1.0000 2 4 0 1 604.230 5.74407 1.0000 4 4 0 1 100.615 1.70134 1.0000 6 4 0 1 179.193 4.36271 1.0000 8 4 0 1 240.705 11.4581 1.0000 0 5 0 1 549.452 6.72600 1.0000 2 5 0 1 263.866 2.56083 1.0000 4 5 0 1 44.5695 0.99866 1.0000 6 5 0 1 46.0213 1.63288 1.0000 8 5 0 1 35.9211 2.31991 1.0000 0 6 0 1 1.58147 0.38704 1.0000 2 6 0 1 512.717 4.68600 1.0000 4 6 0 1 806.025 8.62771 1.0000 6 6 0 1 44.4386 1.38743 1.0000 8 6 0 1 1.03009 1.36584 1.0000 0 7 0 1 180.926 2.59007 1.0000 2 7 0 1 1693.95 14.9193 1.0000 4 7 0 1 2293.35 20.7717 1.0000 6 7 0 1 248.883 4.35320 1.0000 8 7 0 1 8.97157 1.79072 1.0000 0 8 0 1 7.84904 0.62780 1.0000 2 8 0 1 209.604 1.90472 1.0000 4 8 0 1 484.622 4.63706 1.0000 6 8 0 1 51.3455 1.37610 1.0000 8 8 0 1 -0.7301 1.05768 1.0000 0 9 0 1 -3.5657 0.43406 1.0000 2 9 0 1 51.3780 0.67096 1.0000 4 9 0 1 67.9521 0.99187 1.0000 6 9 0 1 2.62692 0.69632 1.0000 8 9 0 1 -0.1795 1.10396 1.0000 0 10 0 1 35.6527 0.75698 1.0000 2 10 0 1 111.073 1.07088 1.0000 4 10 0 1 348.441 3.44182 1.0000 6 10 0 1 16.7936 0.92110 1.0000 0 11 0 1 83.6499 1.28179 1.0000 2 11 0 1 321.948 2.60638 1.0000 4 11 0 1 524.191 5.20888 1.0000 6 11 0 1 64.9000 1.68343 1.0000 0 12 0 1 9.96417 0.93393 1.0000 2 12 0 1 53.2180 0.81008 1.0000 4 12 0 1 63.3548 1.14670 1.0000 6 12 0 1 12.2760 0.99188 1.0000 0 13 0 1 47.9484 1.15166 1.0000 2 13 0 1 -0.1975 0.42168 1.0000 4 13 0 1 16.3826 0.77366 1.0000 6 13 0 1 2.68829 0.97520 1.0000 0 14 0 1 316.713 4.19367 1.0000 2 14 0 1 70.7887 1.11556 1.0000 4 14 0 1 -1.4337 0.63426 1.0000 0 15 0 1 59.3944 1.55061 1.0000 2 15 0 1 6.73164 0.62975 1.0000 4 15 0 1 -1.1776 0.78203 1.0000 0 16 0 1 31.6022 1.29749 1.0000 2 16 0 1 13.8004 0.84143 1.0000 1 1 1 1 2457.99 17.7615 1.0000 2 1 1 1 652.638 5.92030 1.0000 3 1 1 1 243.327 2.50787 1.0000 4 1 1 1 7.76218 0.45097 1.0000 5 1 1 1 33.5914 1.60914 1.0000 6 1 1 1 89.3632 3.89746 1.0000 7 1 1 1 82.5105 3.09156 1.0000 1 2 1 1 661.455 4.89531 1.0000 2 2 1 1 979.179 9.02111 1.0000 3 2 1 1 3411.66 30.2771 1.0000 4 2 1 1 8.05095 0.34640 1.0000 5 2 1 1 885.634 15.3640 1.0000 6 2 1 1 122.846 3.74236 1.0000 7 2 1 1 8.65892 1.04867 1.0000 8 2 1 1 7.86627 1.14369 1.0000 1 3 1 1 1095.93 7.01119 1.0000 2 3 1 1 156.070 1.25477 1.0000 3 3 1 1 2499.10 18.9315 1.0000 4 3 1 1 -0.0279 0.26897 1.0000 5 3 1 1 872.484 13.3351 1.0000 6 3 1 1 22.3749 0.84848 1.0000 7 3 1 1 159.356 4.87402 1.0000 8 3 1 1 -1.7206 0.98064 1.0000 9 3 1 1 85.6711 4.45851 1.0000 1 4 1 1 2684.02 16.1153 1.0000 2 4 1 1 115.018 0.87176 1.0000 3 4 1 1 583.303 4.14055 1.0000 4 4 1 1 1.02018 0.27870 1.0000 5 4 1 1 366.817 4.76377 1.0000 6 4 1 1 15.6924 0.74623 1.0000 7 4 1 1 333.998 7.54099 1.0000 8 4 1 1 0.25391 1.09564 1.0000 9 4 1 1 112.891 4.94515 1.0000 1 5 1 1 2540.69 15.0272 1.0000 2 5 1 1 377.799 2.45871 1.0000 3 5 1 1 36.4292 0.46771 1.0000 4 5 1 1 5.67637 0.33040 1.0000 5 5 1 1 50.3687 0.79132 1.0000 6 5 1 1 78.9786 1.44767 1.0000 7 5 1 1 237.929 4.81747 1.0000 8 5 1 1 3.35602 0.91923 1.0000 9 5 1 1 42.9594 3.30981 1.0000 1 6 1 1 64.3358 0.60810 1.0000 2 6 1 1 177.025 1.32408 1.0000 3 6 1 1 595.205 4.13017 1.0000 4 6 1 1 0.50425 0.25175 1.0000 5 6 1 1 235.312 2.26657 1.0000 6 6 1 1 39.3649 0.83170 1.0000 7 6 1 1 3.02952 0.57481 1.0000 8 6 1 1 1.83609 1.01411 1.0000 9 6 1 1 7.27972 2.85642 1.0000 1 7 1 1 372.793 2.44084 1.0000 2 7 1 1 -0.5021 0.25675 1.0000 3 7 1 1 321.325 2.10498 1.0000 4 7 1 1 -0.8996 0.24801 1.0000 5 7 1 1 173.199 1.62864 1.0000 6 7 1 1 -2.3979 0.39240 1.0000 7 7 1 1 68.7041 1.39412 1.0000 8 7 1 1 -0.3692 1.05474 1.0000 1 8 1 1 258.623 1.84360 1.0000 2 8 1 1 80.8092 0.62454 1.0000 3 8 1 1 3.20014 0.21303 1.0000 4 8 1 1 0.66757 0.24023 1.0000 5 8 1 1 0.23369 0.27616 1.0000 6 8 1 1 17.8672 0.62987 1.0000 7 8 1 1 56.7242 1.30999 1.0000 8 8 1 1 1.39923 0.84144 1.0000 1 9 1 1 733.505 3.69996 1.0000 2 9 1 1 84.0800 0.62501 1.0000 3 9 1 1 47.8233 0.48801 1.0000 4 9 1 1 1.06465 0.24876 1.0000 5 9 1 1 32.9834 0.58356 1.0000 6 9 1 1 31.5076 0.83181 1.0000 7 9 1 1 119.467 2.08510 1.0000 8 9 1 1 0.22696 0.87815 1.0000 1 10 1 1 263.381 1.43192 1.0000 2 10 1 1 10.4338 0.26311 1.0000 3 10 1 1 71.2802 0.64725 1.0000 4 10 1 1 -1.7295 0.27064 1.0000 5 10 1 1 42.4356 0.71340 1.0000 6 10 1 1 4.42273 0.53748 1.0000 7 10 1 1 67.2368 1.48076 1.0000 1 11 1 1 40.0847 0.43697 1.0000 2 11 1 1 3.74410 0.26479 1.0000 3 11 1 1 97.9987 0.84322 1.0000 4 11 1 1 -0.7130 0.34557 1.0000 5 11 1 1 51.7667 0.81557 1.0000 6 11 1 1 0.94128 0.55496 1.0000 7 11 1 1 11.0282 0.81567 1.0000 1 12 1 1 9.76897 0.30783 1.0000 2 12 1 1 24.8814 0.41627 1.0000 3 12 1 1 134.298 1.10093 1.0000 4 12 1 1 0.61166 0.36808 1.0000 5 12 1 1 52.7328 0.90001 1.0000 6 12 1 1 9.73150 0.65665 1.0000 1 13 1 1 190.797 1.29401 1.0000 2 13 1 1 11.5279 0.37902 1.0000 3 13 1 1 32.3390 0.58695 1.0000 4 13 1 1 -0.2174 0.41076 1.0000 5 13 1 1 21.9599 0.65694 1.0000 6 13 1 1 4.86277 0.74221 1.0000 1 14 1 1 176.540 1.28234 1.0000 2 14 1 1 -1.0136 0.35290 1.0000 3 14 1 1 127.342 1.20211 1.0000 4 14 1 1 -1.0931 0.44269 1.0000 5 14 1 1 69.5485 1.29254 1.0000 1 15 1 1 -1.3016 0.37988 1.0000 2 15 1 1 3.30865 0.41144 1.0000 3 15 1 1 18.2386 0.59511 1.0000 4 15 1 1 -1.6641 0.57403 1.0000 1 16 1 1 0.49916 0.46619 1.0000 2 16 1 1 4.36035 0.53470 1.0000 0 0 2 1 7011.73 99.9938 1.0000 1 0 2 1 1080.33 11.8161 1.0000 2 0 2 1 5190.96 48.5564 1.0000 3 0 2 1 352.913 4.34540 1.0000 4 0 2 1 2535.28 30.8905 1.0000 5 0 2 1 301.351 11.2214 1.0000 6 0 2 1 854.646 21.5847 1.0000 7 0 2 1 37.6655 1.92668 1.0000 8 0 2 1 297.136 12.7618 1.0000 0 1 2 1 756.513 6.70032 1.0000 1 1 2 1 414.028 2.94049 1.0000 2 1 2 1 1071.06 7.21165 1.0000 3 1 2 1 146.524 1.41404 1.0000 4 1 2 1 671.788 6.28529 1.0000 5 1 2 1 93.9658 2.19264 1.0000 6 1 2 1 230.836 4.39893 1.0000 7 1 2 1 11.0810 0.95209 1.0000 8 1 2 1 85.2082 3.65206 1.0000 9 1 2 1 18.1354 2.46500 1.0000 0 2 2 1 15.0763 0.44631 1.0000 1 2 2 1 46.7956 0.51628 1.0000 2 2 2 1 6.09445 0.23993 1.0000 3 2 2 1 10.8453 0.32895 1.0000 4 2 2 1 5.25657 0.34012 1.0000 5 2 2 1 12.3326 0.58737 1.0000 6 2 2 1 4.11728 0.52541 1.0000 7 2 2 1 0.43041 0.49519 1.0000 8 2 2 1 1.12012 0.67990 1.0000 9 2 2 1 9.83700 1.89463 1.0000 0 3 2 1 82.0932 0.93408 1.0000 1 3 2 1 632.832 3.99686 1.0000 2 3 2 1 0.23964 0.17122 1.0000 3 3 2 1 221.002 1.81904 1.0000 4 3 2 1 22.3724 0.52605 1.0000 5 3 2 1 156.945 2.17378 1.0000 6 3 2 1 3.29848 0.41307 1.0000 7 3 2 1 15.9785 0.85945 1.0000 8 3 2 1 1.47615 1.03154 1.0000 9 3 2 1 60.4123 3.47372 1.0000 0 4 2 1 478.011 4.15130 1.0000 1 4 2 1 466.177 2.90320 1.0000 2 4 2 1 417.149 2.69163 1.0000 3 4 2 1 169.419 1.41437 1.0000 4 4 2 1 262.757 2.38355 1.0000 5 4 2 1 147.566 1.79561 1.0000 6 4 2 1 62.0378 1.20002 1.0000 7 4 2 1 20.9245 0.99574 1.0000 8 4 2 1 10.6319 0.99630 1.0000 9 4 2 1 46.6338 3.16576 1.0000 0 5 2 1 234.921 2.22211 1.0000 1 5 2 1 17.6034 0.33960 1.0000 2 5 2 1 235.855 1.62341 1.0000 3 5 2 1 8.01088 0.31030 1.0000 4 5 2 1 128.689 1.17051 1.0000 5 5 2 1 6.12348 0.34656 1.0000 6 5 2 1 36.7857 0.82471 1.0000 7 5 2 1 1.92750 0.63287 1.0000 8 5 2 1 9.86680 0.98552 1.0000 9 5 2 1 1.71291 2.05451 1.0000 0 6 2 1 495.663 4.38256 1.0000 1 6 2 1 111.338 0.90248 1.0000 2 6 2 1 287.072 1.98065 1.0000 3 6 2 1 36.8017 0.49404 1.0000 4 6 2 1 129.330 1.08644 1.0000 5 6 2 1 47.2624 0.70121 1.0000 6 6 2 1 89.9983 1.33676 1.0000 7 6 2 1 4.20411 0.54120 1.0000 8 6 2 1 48.0560 1.87263 1.0000 0 7 2 1 1643.30 14.0682 1.0000 1 7 2 1 201.837 1.49572 1.0000 2 7 2 1 1079.56 6.54661 1.0000 3 7 2 1 90.9415 0.71441 1.0000 4 7 2 1 535.934 3.61858 1.0000 5 7 2 1 88.0552 0.96859 1.0000 6 7 2 1 323.504 3.74433 1.0000 7 7 2 1 10.3263 0.69420 1.0000 8 7 2 1 156.277 3.73292 1.0000 0 8 2 1 210.853 1.79029 1.0000 1 8 2 1 50.1427 0.47403 1.0000 2 8 2 1 166.857 1.04103 1.0000 3 8 2 1 24.8411 0.36334 1.0000 4 8 2 1 90.3444 0.82084 1.0000 5 8 2 1 25.7812 0.51685 1.0000 6 8 2 1 60.7108 1.04112 1.0000 7 8 2 1 5.74837 0.67500 1.0000 8 8 2 1 35.3171 1.45132 1.0000 0 9 2 1 50.3094 0.64268 1.0000 1 9 2 1 3.82452 0.20789 1.0000 2 9 2 1 33.3582 0.39060 1.0000 3 9 2 1 0.40118 0.21947 1.0000 4 9 2 1 18.0461 0.39886 1.0000 5 9 2 1 2.08401 0.34059 1.0000 6 9 2 1 13.9977 0.64333 1.0000 7 9 2 1 -0.3727 0.64191 1.0000 8 9 2 1 6.30348 1.10685 1.0000 0 10 2 1 107.078 1.03113 1.0000 1 10 2 1 47.1143 0.45704 1.0000 2 10 2 1 63.0535 0.55452 1.0000 3 10 2 1 16.8353 0.36372 1.0000 4 10 2 1 34.6576 0.55325 1.0000 5 10 2 1 35.7466 0.67874 1.0000 6 10 2 1 44.5784 0.99186 1.0000 7 10 2 1 2.67956 0.70152 1.0000 0 11 2 1 313.231 2.39820 1.0000 1 11 2 1 34.8663 0.42418 1.0000 2 11 2 1 228.954 1.41854 1.0000 3 11 2 1 18.1253 0.41043 1.0000 4 11 2 1 123.914 1.13612 1.0000 5 11 2 1 19.2790 0.55704 1.0000 6 11 2 1 74.9162 1.29539 1.0000 7 11 2 1 4.26700 0.90136 1.0000 0 12 2 1 50.5412 0.76090 1.0000 1 12 2 1 1.24787 0.27243 1.0000 2 12 2 1 44.3554 0.55617 1.0000 3 12 2 1 0.75220 0.33429 1.0000 4 12 2 1 24.7215 0.56596 1.0000 5 12 2 1 0.18757 0.43826 1.0000 6 12 2 1 8.19953 0.69188 1.0000 0 13 2 1 0.53402 0.43938 1.0000 1 13 2 1 5.61762 0.34677 1.0000 2 13 2 1 -0.0705 0.31955 1.0000 3 13 2 1 1.90558 0.38930 1.0000 4 13 2 1 0.58102 0.43281 1.0000 5 13 2 1 4.52184 0.52325 1.0000 0 14 2 1 62.2463 1.04436 1.0000 1 14 2 1 11.6516 0.43351 1.0000 2 14 2 1 70.4063 0.81311 1.0000 3 14 2 1 5.04740 0.45889 1.0000 4 14 2 1 55.1555 0.93582 1.0000 5 14 2 1 9.84026 0.81758 1.0000 0 15 2 1 7.18455 0.63298 1.0000 1 15 2 1 3.02473 0.41993 1.0000 2 15 2 1 7.00730 0.45213 1.0000 3 15 2 1 1.64348 0.48913 1.0000 4 15 2 1 9.74286 6.43773 1.0000 0 16 2 1 12.1370 0.78275 1.0000 1 16 2 1 -0.1985 0.51642 1.0000 2 16 2 1 12.8717 0.67125 1.0000 1 1 3 1 264.187 1.78117 1.0000 2 1 3 1 185.445 1.36423 1.0000 3 1 3 1 349.457 2.45809 1.0000 4 1 3 1 2.18671 0.28188 1.0000 5 1 3 1 70.8877 1.00232 1.0000 6 1 3 1 40.2398 0.90250 1.0000 7 1 3 1 55.2371 1.42269 1.0000 8 1 3 1 1.35074 0.65028 1.0000 9 1 3 1 4.23279 1.19848 1.0000 1 2 3 1 3327.63 19.0422 1.0000 2 2 3 1 285.069 2.01529 1.0000 3 2 3 1 31.9981 0.49365 1.0000 4 2 3 1 1.32247 0.25289 1.0000 5 2 3 1 71.2699 1.00005 1.0000 6 2 3 1 44.3048 0.93440 1.0000 7 2 3 1 405.764 6.70794 1.0000 8 2 3 1 6.15885 0.80797 1.0000 9 2 3 1 73.7120 3.13820 1.0000 1 3 3 1 2416.73 14.6274 1.0000 2 3 3 1 52.7453 0.59076 1.0000 3 3 3 1 564.849 3.95851 1.0000 4 3 3 1 1.15050 0.22453 1.0000 5 3 3 1 321.170 3.31055 1.0000 6 3 3 1 9.33567 0.54256 1.0000 7 3 3 1 350.386 6.12819 1.0000 8 3 3 1 0.29990 0.64248 1.0000 9 3 3 1 121.292 5.43816 1.0000 1 4 3 1 540.811 3.39041 1.0000 2 4 3 1 34.0187 0.48264 1.0000 3 4 3 1 1152.45 7.82095 1.0000 4 4 3 1 -0.1708 0.19951 1.0000 5 4 3 1 494.073 4.59351 1.0000 6 4 3 1 4.62982 0.42659 1.0000 7 4 3 1 86.1380 1.73626 1.0000 8 4 3 1 0.54983 0.73466 1.0000 9 4 3 1 72.0175 4.69522 1.0000 1 5 3 1 28.8158 0.47288 1.0000 2 5 3 1 126.345 1.05437 1.0000 3 5 3 1 1028.79 6.36037 1.0000 4 5 3 1 2.12727 0.23272 1.0000 5 5 3 1 341.036 3.10259 1.0000 6 5 3 1 37.7137 0.84007 1.0000 7 5 3 1 4.33153 0.62403 1.0000 8 5 3 1 2.07543 0.81707 1.0000 1 6 3 1 598.811 3.86106 1.0000 2 6 3 1 66.8539 0.62219 1.0000 3 6 3 1 -0.4425 0.20561 1.0000 4 6 3 1 -0.6496 0.22321 1.0000 5 6 3 1 12.1097 0.40351 1.0000 6 6 3 1 15.3423 0.62380 1.0000 7 6 3 1 162.714 2.43002 1.0000 8 6 3 1 1.72467 0.79199 1.0000 1 7 3 1 307.484 1.77067 1.0000 2 7 3 1 -0.1157 0.18596 1.0000 3 7 3 1 229.852 1.45870 1.0000 4 7 3 1 -0.6482 0.22272 1.0000 5 7 3 1 98.9964 1.06742 1.0000 6 7 3 1 0.42990 0.41547 1.0000 7 7 3 1 52.5515 1.33737 1.0000 8 7 3 1 0.92219 0.82929 1.0000 1 8 3 1 4.21829 0.21212 1.0000 2 8 3 1 29.2803 0.36775 1.0000 3 8 3 1 178.050 1.15687 1.0000 4 8 3 1 0.04882 0.25864 1.0000 5 8 3 1 54.2987 0.75067 1.0000 6 8 3 1 7.02103 0.52891 1.0000 7 8 3 1 8.28099 0.80388 1.0000 8 8 3 1 0.58304 1.08136 1.0000 1 9 3 1 41.7774 0.42843 1.0000 2 9 3 1 34.9890 0.42252 1.0000 3 9 3 1 420.060 2.55402 1.0000 4 9 3 1 0.78665 0.30031 1.0000 5 9 3 1 166.161 1.62981 1.0000 6 9 3 1 15.4032 0.66769 1.0000 7 9 3 1 -0.3430 0.69183 1.0000 1 10 3 1 69.4237 0.58394 1.0000 2 10 3 1 7.04658 0.28453 1.0000 3 10 3 1 171.164 1.24482 1.0000 4 10 3 1 -0.9227 0.31554 1.0000 5 10 3 1 100.312 1.14111 1.0000 6 10 3 1 2.39915 0.58021 1.0000 7 10 3 1 10.3412 0.94905 1.0000 1 11 3 1 98.6618 0.75828 1.0000 2 11 3 1 1.92653 0.30203 1.0000 3 11 3 1 13.4975 0.42148 1.0000 4 11 3 1 -0.0218 0.34974 1.0000 5 11 3 1 24.8144 0.67285 1.0000 6 11 3 1 -0.2743 0.56229 1.0000 1 12 3 1 132.681 0.99407 1.0000 2 12 3 1 12.2561 0.39915 1.0000 3 12 3 1 -7.5459 0.37604 1.0000 4 12 3 1 -0.5123 0.39246 1.0000 5 12 3 1 0.25440 0.45652 1.0000 6 12 3 1 2.45169 0.76084 1.0000 1 13 3 1 28.6640 0.52079 1.0000 2 13 3 1 6.33711 0.40439 1.0000 3 13 3 1 135.684 1.24886 1.0000 4 13 3 1 -0.5738 0.43743 1.0000 5 13 3 1 75.9855 1.22637 1.0000 1 14 3 1 122.766 1.06840 1.0000 2 14 3 1 -0.0433 0.39861 1.0000 3 14 3 1 93.3001 1.05476 1.0000 4 14 3 1 -2.1025 0.52713 1.0000 1 15 3 1 20.5589 0.57236 1.0000 2 15 3 1 0.58984 0.45706 1.0000 3 15 3 1 -8.0493 0.63385 1.0000 0 0 4 1 279.577 3.85388 1.0000 1 0 4 1 21.1414 0.62132 1.0000 2 0 4 1 2416.80 21.7375 1.0000 3 0 4 1 8.65628 0.44211 1.0000 4 0 4 1 3210.50 28.3371 1.0000 5 0 4 1 8.22815 0.55162 1.0000 6 0 4 1 371.930 6.24483 1.0000 7 0 4 1 -0.2629 0.63925 1.0000 8 0 4 1 33.7564 2.00331 1.0000 0 1 4 1 19.0213 0.62054 1.0000 1 1 4 1 6.36368 0.30930 1.0000 2 1 4 1 652.920 4.37358 1.0000 3 1 4 1 1.67829 0.22272 1.0000 4 1 4 1 1006.90 6.72066 1.0000 5 1 4 1 4.88251 0.32648 1.0000 6 1 4 1 105.196 1.55770 1.0000 7 1 4 1 1.31871 0.46694 1.0000 8 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8 7 1 1.77441 0.41640 1.0000 3 8 7 1 9.40938 0.50642 1.0000 4 8 7 1 0.58427 0.49796 1.0000 5 8 7 1 1.46250 0.84839 1.0000 1 9 7 1 129.174 1.13846 1.0000 2 9 7 1 5.89512 0.46463 1.0000 3 9 7 1 1.30562 0.46423 1.0000 4 9 7 1 -0.6956 0.59735 1.0000 1 10 7 1 67.9983 0.87049 1.0000 2 10 7 1 1.83005 0.45765 1.0000 3 10 7 1 11.0038 0.62432 1.0000 1 11 7 1 11.3121 0.58161 1.0000 2 11 7 1 -0.0466 0.56189 1.0000 0 0 8 1 1012.50 11.4143 1.0000 1 0 8 1 16.1043 0.65876 1.0000 2 0 8 1 300.852 2.84584 1.0000 3 0 8 1 8.46314 0.63606 1.0000 4 0 8 1 33.2551 1.04470 1.0000 5 0 8 1 17.5306 1.05849 1.0000 0 1 8 1 334.600 2.98816 1.0000 1 1 8 1 6.22550 0.38383 1.0000 2 1 8 1 91.9602 0.92130 1.0000 3 1 8 1 3.97674 0.41656 1.0000 4 1 8 1 6.34770 0.50024 1.0000 5 1 8 1 4.84032 0.58371 1.0000 0 2 8 1 4.23105 0.53857 1.0000 1 2 8 1 1.12224 0.34836 1.0000 2 2 8 1 0.49520 0.36252 1.0000 3 2 8 1 -0.0194 0.39174 1.0000 4 2 8 1 4.77061 0.46944 1.0000 5 2 8 1 1.80218 0.55931 1.0000 0 3 8 1 160.210 1.77907 1.0000 1 3 8 1 12.6106 0.46248 1.0000 2 3 8 1 2.10365 0.39357 1.0000 3 3 8 1 7.85001 0.46965 1.0000 4 3 8 1 36.2890 0.75111 1.0000 5 3 8 1 7.36311 0.67320 1.0000 0 4 8 1 227.778 2.38837 1.0000 1 4 8 1 7.51262 0.42737 1.0000 2 4 8 1 15.2059 0.50612 1.0000 3 4 8 1 3.70604 0.42951 1.0000 4 4 8 1 21.5689 0.65109 1.0000 5 4 8 1 9.08008 0.75785 1.0000 0 5 8 1 38.5514 0.90749 1.0000 1 5 8 1 0.44176 0.37420 1.0000 2 5 8 1 9.54324 0.47886 1.0000 3 5 8 1 1.00939 0.41094 1.0000 4 5 8 1 -0.1504 0.47623 1.0000 0 6 8 1 0.72226 0.55509 1.0000 1 6 8 1 4.30737 0.42680 1.0000 2 6 8 1 50.4399 0.79070 1.0000 3 6 8 1 2.87478 0.45787 1.0000 4 6 8 1 94.7305 1.39073 1.0000 0 7 8 1 13.6548 0.72440 1.0000 1 7 8 1 6.56894 0.47702 1.0000 2 7 8 1 159.776 1.48858 1.0000 3 7 8 1 5.53600 0.53134 1.0000 0 8 8 1 0.68419 0.66184 1.0000 1 8 8 1 1.42686 0.48208 1.0000 2 8 8 1 37.7685 0.81059 1.0000 3 8 8 1 0.97127 0.60508 1.0000 0 9 8 1 1.70486 0.72259 1.0000 1 9 8 1 1.96498 0.54567 1.0000 2 9 8 1 4.38633 1.76032 1.0000 1 1 9 1 5.12408 0.46533 1.0000 2 1 9 1 54.0032 0.86760 1.0000 3 1 9 1 0.57711 0.50073 1.0000 1 2 9 1 19.9814 0.60802 1.0000 2 2 9 1 85.3530 1.05177 1.0000 3 2 9 1 56.5985 0.97583 1.0000 1 3 9 1 95.3985 1.08749 1.0000 2 3 9 1 16.5386 0.60730 1.0000 3 3 9 1 123.550 1.46670 1.0000 1 4 9 1 117.532 1.19990 1.0000 2 4 9 1 13.3611 0.58998 1.0000 3 4 9 1 84.5205 1.37851 1.0000 1 5 9 1 37.8115 0.79304 1.0000 2 5 9 1 52.0072 0.96692 1.0000 1 6 9 1 10.9055 0.64026 1.0000 ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL solve_a.res in Pcca CELL 0.71073 5.9136 10.0457 5.8572 90.000 90.000 90.000 ZERR 8.000 0.0005 0.0008 0.0004 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, Z SYMM -X, Y, 1/2-Z SYMM 1/2+X, -Y, 1/2-Z SFAC C H O NA UNIT 8 12 8 4 TEMP -173.000 L.S. 10 REM SHEL 10 0.7 BOND $H LIST 6 ACTA FMAP 2 PLAN 20 WGHT 0.075300 0.099900 FVAR 1.36908 0.88305 NA1 4 0.500000 0.583700 0.250000 10.50000 0.00882 0.01816 = 0.00767 0.00000 0.00014 0.00000 C1 1 0.500000 0.701417 0.750000 10.50000 0.00948 0.01547 = 0.00894 0.00000 -0.00032 0.00000 C2 1 0.500000 0.852243 0.750000 10.50000 0.03693 0.01581 = 0.03538 0.00000 0.00562 0.00000 AFIX 137 H2A 2 0.343843 0.884761 0.755213 10.50000 -1.50000 H2B 2 0.573607 0.884761 0.610856 10.50000 -1.50000 H2C 2 0.582550 0.884762 0.883931 10.50000 -1.50000 AFIX 0 O1 3 0.367669 0.642556 0.884658 21.00000 0.00967 0.02701 = 0.00721 0.00239 -0.00036 -0.00249 PART 2 O2 3 0.633849 0.643433 0.886774 -21.00000 0.01276 PART 0 HKLF 4 REM solve_a.res in Pcca REM R1 = 0.0458 for 707 Fo > 4sig(Fo) and 0.0540 for all 840 data REM 31 parameters refined using 0 restraints END WGHT 0.0753 0.0999 REM Highest difference peak 0.548, deepest hole -0.508, 1-sigma level 0.246 Q1 1 0.5000 0.7752 0.7500 10.50000 0.05 0.55 Q2 1 0.6032 0.9635 0.3902 11.00000 0.05 0.46 Q3 1 0.6230 0.9595 0.5373 11.00000 0.05 0.44 Q4 1 0.6370 0.9552 1.0418 11.00000 0.05 0.44 Q5 1 0.3731 1.0320 0.7799 11.00000 0.05 0.44 Q6 1 0.3652 0.8931 0.8200 11.00000 0.05 0.43 Q7 1 0.6903 0.9676 0.8577 11.00000 0.05 0.42 Q8 1 0.3357 0.8931 0.6623 11.00000 0.05 0.42 Q9 1 0.3791 0.9584 0.7715 11.00000 0.05 0.41 Q10 1 0.1438 0.9328 0.8618 11.00000 0.05 0.41 Q11 1 0.2406 0.9708 0.7605 11.00000 0.05 0.40 Q12 1 0.5099 0.8814 0.9442 11.00000 0.05 0.39 Q13 1 0.5174 0.8570 0.8368 11.00000 0.05 0.39 Q14 1 0.5840 0.9706 0.9591 11.00000 0.05 0.38 Q15 1 0.7003 0.9577 0.6152 11.00000 0.05 0.37 Q16 1 0.6071 0.8798 0.3789 11.00000 0.05 0.34 Q17 1 0.1271 0.8888 0.7700 11.00000 0.05 0.33 Q18 1 0.1666 0.8725 0.8059 11.00000 0.05 0.33 Q19 1 0.5000 0.9860 0.7500 10.50000 0.05 0.33 Q20 1 0.7011 0.8927 0.4374 11.00000 0.05 0.32 ; _shelx_res_checksum 67528 _shelx_hkl_file ; 0 -1 0 4.96246 1.64127 1 1 -1 0 0.29403 0.84065 2 1 -1 0 0.72670 1.07105 3 1 -1 0 0.94377 0.93899 3 1 -1 0 0.90342 1.05512 11 -1 1 0 0.77318 1.09797 3 1 -1 0 1.21952 1.14053 2 1 -1 0 1.06687 2.96099 1 1 -1 0 -1.7148 3.28740 1 -1 1 0 0.54808 0.85180 3 -1 1 0 0.38816 0.86646 2 -1 1 0 0.70667 1.01282 2 -1 1 0 -0.5959 2.41491 1 -1 1 0 2.71412 3.56881 1 -2 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7.76679 2.17459 7 3 -5 -2 8.30540 2.05445 5 3 -5 -2 9.14476 2.58809 8 -3 -5 2 5.88379 1.77492 5 3 5 2 9.59746 2.77227 8 3 5 2 -1.5404 5.18159 1 -3 -5 2 4.66506 3.17287 3 -3 5 -2 8.21834 2.48629 4 3 5 2 10.5455 3.59234 2 3 -5 -2 4.90692 3.00961 10 3 -5 -2 10.2426 2.96639 9 3 5 2 6.04333 2.57413 7 -3 5 -2 6.75086 2.30741 6 3 5 2 11.0481 2.70491 6 3 5 2 8.44766 2.82628 9 -3 -5 2 7.72808 2.05608 6 -3 -5 2 4.30103 1.43050 10 -3 5 -2 8.48551 2.37419 7 3 -5 -2 7.39175 5.79502 1 3 -5 -2 10.9781 2.56473 4 -4 -5 -2 130.479 8.24106 4 -4 5 2 123.563 11.0653 2 -4 5 2 127.403 8.84370 6 4 -5 2 123.410 11.6080 3 4 -5 2 128.638 9.12506 5 -4 5 2 134.651 8.97532 5 -4 5 2 122.949 8.61645 7 -4 5 2 138.173 8.18696 15 4 5 -2 126.703 8.77071 7 4 -5 2 111.401 8.64768 9 4 5 -2 129.972 9.15293 8 4 -5 2 135.203 9.42001 8 -4 5 2 139.480 8.14166 13 -4 5 2 130.905 9.38265 9 4 -5 2 138.164 8.16157 19 4 5 -2 130.051 13.8554 1 -4 5 2 139.297 8.29721 14 4 -5 2 130.749 19.0292 1 4 -5 2 127.612 9.20297 6 -4 5 2 141.402 9.62355 4 -4 -5 -2 123.994 8.82904 10 4 -5 2 109.529 10.1752 2 -4 5 2 131.689 9.58428 10 4 -5 2 129.482 9.12544 7 4 5 -2 138.023 9.04217 11 4 -5 2 133.777 8.17887 20 4 5 -2 141.079 7.94580 21 4 -5 2 129.714 10.9033 11 -4 5 2 122.744 10.6839 3 -4 5 -2 112.589 8.36075 9 4 -5 -2 122.441 8.42332 7 -4 5 -2 117.475 8.14039 14 4 -5 -2 131.458 8.80107 8 4 5 2 134.421 8.53449 8 4 -5 -2 129.575 11.8687 2 4 -5 -2 122.881 8.39579 5 -4 5 -2 121.798 8.55855 5 -4 -5 2 137.378 9.03657 4 -4 5 -2 104.609 9.53455 2 -4 -5 2 133.375 8.66538 5 -4 5 -2 128.336 11.2120 3 4 -5 -2 125.371 9.91723 3 4 -5 -2 139.650 10.0050 10 -4 -5 2 121.047 8.02500 10 4 -5 -2 154.212 11.4789 11 4 -5 -2 125.767 7.83973 19 4 5 2 133.522 8.21217 21 -4 -5 2 138.496 8.23275 13 4 -5 -2 120.324 8.29712 6 -4 5 -2 126.622 8.93944 4 -4 5 -2 129.627 7.98439 15 -4 5 -2 128.046 8.79581 6 -4 5 -2 119.008 8.57418 10 4 -5 -2 129.112 8.12313 20 4 5 2 110.753 8.88270 11 4 -5 -2 129.318 14.9398 1 4 -5 -2 134.660 9.50138 9 -4 5 -2 132.078 9.10024 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6.12874 20 -3 -7 2 96.9649 6.65950 9 -3 7 -2 100.312 6.59788 14 3 -7 -2 84.7056 7.95140 10 -3 7 -2 71.6123 8.26835 2 3 7 2 99.7342 7.59582 9 -3 -7 2 76.0686 6.10384 14 3 -7 -2 89.4137 7.17264 8 3 -7 -2 85.5510 5.87232 17 3 7 2 105.086 9.24856 2 -3 7 -2 110.312 6.79288 13 3 7 2 98.4243 7.08862 6 3 -7 -2 87.1488 5.99496 19 -3 -7 2 71.4333 5.83986 15 3 -7 -2 88.0535 7.27395 4 -3 7 -2 106.935 6.05978 17 3 -7 -2 88.3993 8.76539 3 -3 7 -2 89.8489 7.78978 8 -3 7 -2 94.4439 7.22241 6 -3 7 -2 96.4911 7.23024 10 -3 7 -2 111.127 6.34901 16 3 -7 -2 84.5482 5.83976 18 3 -7 -2 98.5219 15.0518 1 3 7 2 105.808 7.07478 7 -3 -7 2 78.9197 7.25994 4 3 7 2 93.0662 6.11058 20 -3 7 -2 97.0678 6.14616 12 -3 7 -2 87.6673 7.30632 7 -3 7 -2 102.086 7.24195 5 -3 -7 2 89.5980 6.33881 10 3 7 2 101.610 7.21552 8 -3 -7 2 76.9478 6.67906 5 -3 -7 2 93.1561 7.94186 2 -3 7 -2 104.074 6.34357 15 3 7 2 99.8652 11.2035 1 3 -7 -2 85.6662 6.76905 5 -3 -7 2 74.3184 6.80789 6 3 -7 -2 88.7755 6.00465 12 3 -7 -2 71.5839 9.58007 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139.670 1 1 3 -3 2417.67 134.982 8 -1 3 3 2398.26 134.565 10 1 3 -3 2469.76 134.293 5 1 3 -3 2413.61 134.427 6 -1 3 3 2332.79 134.736 11 1 3 -3 2461.34 134.616 7 -1 -3 -3 2338.95 133.953 5 -1 3 3 2358.16 134.347 6 1 -3 3 2391.77 140.496 1 -1 3 3 2598.95 141.787 1 1 3 -3 2457.37 134.441 4 -1 3 3 2422.54 134.348 5 -1 -3 -3 2339.77 135.934 3 1 -3 3 2244.22 134.530 11 1 3 -3 2444.81 134.253 10 -1 3 3 2418.03 134.422 8 1 -3 3 2451.44 134.210 10 1 -3 3 2404.38 134.758 4 -1 3 3 2320.60 136.160 2 1 3 -3 2482.97 137.093 3 1 -3 3 2354.94 135.601 2 1 3 -3 2611.68 141.107 1 -1 -3 -3 2279.18 134.724 11 1 3 -3 2441.53 134.235 9 1 -3 3 2328.83 134.039 9 -1 3 3 2531.33 134.647 4 1 -3 3 2365.97 134.531 6 1 3 -3 2503.85 136.299 2 -1 3 3 2383.01 134.307 7 1 3 -3 2462.12 134.697 11 1 -3 3 2406.43 134.685 8 1 -3 3 2413.75 137.328 3 1 3 -3 2404.15 139.622 1 1 -3 3 2401.88 134.511 7 -1 -3 -3 2379.89 136.475 2 -1 -3 -3 2313.21 134.028 6 -1 -3 -3 2420.84 134.436 9 -1 3 3 2490.46 137.005 3 -1 -3 -3 2425.18 134.497 10 1 -3 3 2379.69 134.470 5 1 -3 3 2380.90 140.057 1 -1 3 3 2355.02 134.315 9 -1 -3 3 2411.10 134.778 4 -1 3 -3 2463.75 134.960 8 1 3 3 2415.06 134.514 8 1 3 3 2322.57 134.604 11 -1 3 -3 2506.10 134.321 10 -1 -3 3 2370.82 135.708 2 1 -3 -3 2387.12 136.125 3 1 -3 -3 2344.02 134.975 11 1 3 3 2622.56 134.532 4 1 -3 -3 2367.67 134.029 4 -1 -3 3 2401.13 134.506 7 -1 -3 3 2361.47 134.413 5 -1 3 -3 2400.97 134.420 4 -1 3 -3 2367.57 139.632 1 -1 3 -3 2568.16 134.523 11 1 3 3 2409.78 134.356 7 1 -3 -3 2388.83 134.520 9 1 -3 -3 2419.81 136.847 2 1 3 3 2463.78 136.903 3 1 3 3 2414.57 134.279 9 -1 -3 3 2401.78 134.682 8 1 3 3 2435.75 140.528 1 1 3 3 2322.95 139.052 1 -1 -3 3 2419.43 134.298 10 1 3 3 2562.36 134.339 5 -1 3 -3 2354.27 134.203 5 -1 -3 3 2266.92 134.346 11 -1 -3 3 2393.82 134.520 6 -1 3 -3 2647.12 141.479 1 1 -3 -3 2451.71 134.652 10 -1 3 -3 2529.70 136.204 2 -1 -3 3 2400.75 137.219 3 1 -3 -3 2569.54 141.170 1 -1 -3 3 2419.42 140.376 1 1 3 3 2430.17 134.471 10 -1 3 -3 2381.44 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10.1424 19 -3 -4 9 85.8588 12.0418 5 3 -4 -9 111.552 13.4139 8 3 -4 -9 83.5080 8.75325 12 3 -4 -9 78.3090 7.37768 16 3 -4 -9 82.7497 8.04063 17 -3 4 -9 83.0736 11.6283 12 -3 4 -9 84.6554 9.66024 14 -3 -4 9 104.063 12.1824 12 -3 -4 9 83.7586 9.22490 13 3 4 9 83.6352 9.84976 6 -3 -4 9 97.6084 12.9555 15 -3 -4 9 86.3935 12.7960 16 -3 -4 9 85.8625 11.2622 17 -3 4 -9 98.9577 13.4664 4 -3 4 -9 102.392 12.5755 5 -3 4 -9 98.1697 12.7625 6 3 -4 -9 90.8823 9.11622 18 0 -5 -9 -0.5503 2.91595 15 0 5 -9 -4.5780 4.17885 12 0 5 -9 1.27615 2.76219 15 0 5 -9 3.33694 4.35557 18 0 5 -9 1.52607 3.28732 19 0 5 9 3.70458 5.12012 5 0 -5 -9 -4.0010 3.24373 16 0 -5 -9 -1.1146 2.49530 14 0 -5 9 0.21504 3.46000 15 0 -5 9 -1.9060 4.89517 16 0 -5 -9 5.74489 5.17671 7 0 -5 -9 -1.4186 17.3382 9 0 -5 -9 5.36007 14.4911 10 0 -5 -9 -2.1771 4.11260 12 0 -5 9 -1.7134 5.32949 7 0 -5 9 0.97093 5.94185 8 0 -5 9 -3.3336 12.7804 9 0 5 9 5.35943 5.34279 6 0 5 9 8.97806 6.23060 7 0 5 9 3.99513 6.04273 8 0 5 9 -1.1368 2.78473 15 0 5 -9 -0.1805 3.98698 4 0 5 -9 4.09840 4.75668 5 0 5 9 2.89236 5.39625 18 0 5 9 1.23625 5.41936 19 0 5 9 3.13735 4.20015 20 0 5 -9 -0.2600 5.47991 6 0 5 -9 -4.6726 4.83549 7 0 5 -9 -6.7735 5.05290 8 0 5 -9 3.51104 14.6734 9 0 5 -9 -3.6903 10.6660 10 0 -5 9 3.71613 6.02450 4 0 -5 9 3.75488 9.58906 10 0 -5 9 -6.4669 5.86248 6 0 -5 -9 11.5735 5.19125 4 0 -5 -9 12.5940 5.53592 5 0 5 -9 -1.3560 3.35846 16 0 5 -9 -4.2357 3.63131 17 0 -5 9 2.55148 4.37743 19 0 -5 9 -4.9866 6.22234 5 0 5 9 -1.8798 5.15615 12 0 -5 -9 -1.4779 3.26260 17 0 5 9 8.09585 13.3949 9 0 -5 9 -0.9924 5.69699 12 0 -5 -9 6.53423 5.33612 6 0 -5 9 2.95065 5.47766 17 0 5 9 -3.5449 3.26910 16 0 5 9 -1.5171 5.01058 17 0 5 9 7.86151 11.9711 10 0 -5 -9 1.98895 2.98955 18 0 -5 9 -7.3292 5.26091 18 -1 -5 -9 35.6307 4.94723 18 1 5 -9 36.7817 6.76692 12 -1 5 9 21.5981 4.63951 15 1 5 -9 48.5004 9.97629 8 -1 5 9 34.3024 7.35473 17 -1 -5 -9 41.0677 6.74783 12 1 5 -9 37.9625 11.8205 10 -1 5 9 39.4111 7.49475 18 -1 5 9 28.6688 6.31645 16 -1 5 9 29.3116 7.59917 6 -1 5 9 41.9687 8.36575 7 -1 5 9 43.7055 9.11504 8 -1 5 9 49.1424 15.2737 10 -1 5 9 38.1881 7.71214 12 -1 -5 -9 47.1613 6.24615 15 -1 -5 -9 40.8590 6.10317 16 -1 -5 -9 48.1161 6.10123 17 -1 -5 -9 48.4349 6.73782 14 -1 -5 -9 35.1836 6.81891 5 1 -5 9 24.8958 8.63652 4 1 -5 9 54.6228 10.9613 5 1 -5 9 26.3791 8.91149 6 1 -5 9 33.1220 9.10328 7 1 -5 9 54.9311 11.2073 8 1 -5 9 28.9965 10.2719 10 1 -5 9 49.6539 8.39388 12 1 -5 9 23.0229 5.56296 15 1 -5 9 42.7945 7.45091 16 -1 5 9 42.9718 6.97422 19 -1 -5 -9 32.4240 19.4639 9 1 -5 9 36.1421 7.49709 17 -1 -5 -9 53.5532 8.02509 6 -1 -5 -9 55.5572 8.04069 7 -1 -5 -9 39.1112 7.27351 4 1 5 -9 32.3684 5.99620 16 1 5 -9 35.1612 6.26367 17 1 5 -9 33.4054 6.48936 18 1 5 -9 34.5692 7.13483 19 1 5 -9 26.5501 5.80919 20 1 5 -9 45.6175 8.27941 5 1 5 -9 30.9097 8.91854 7 1 -5 9 36.6438 8.11642 18 -1 5 9 21.8230 6.56612 5 1 5 -9 46.4173 9.55867 6 1 -5 9 30.7075 8.08935 19 -1 5 -9 37.1906 6.54972 18 1 -5 -9 42.0810 6.67096 12 1 5 9 42.5671 6.74678 17 1 -5 -9 36.2711 5.23251 15 -1 5 -9 37.2104 7.11178 17 1 5 9 33.6999 6.84470 20 1 -5 -9 56.5672 8.94584 8 1 -5 -9 48.2204 16.3380 10 1 -5 -9 51.2749 7.65157 5 1 -5 -9 40.0834 7.87963 6 1 5 9 36.2476 14.5963 9 1 5 9 45.2522 7.11294 12 -1 -5 9 36.6471 8.93310 4 1 5 9 38.5196 7.68419 5 -1 -5 9 39.2212 7.21765 14 -1 -5 9 37.4197 7.69649 15 -1 -5 9 30.1650 7.73450 16 -1 -5 9 36.3031 8.16972 17 -1 -5 9 36.6880 6.77539 18 -1 5 -9 43.3721 8.37008 4 -1 5 -9 47.8786 8.64003 5 -1 5 -9 49.8962 10.1025 6 -1 5 -9 37.0141 8.49542 7 1 5 9 25.9414 6.93667 18 1 5 9 46.0079 8.49617 19 1 -5 -9 39.9273 5.77763 19 1 -5 -9 38.2772 5.78340 18 1 -5 -9 34.9695 6.85997 4 -1 5 -9 47.1951 7.14178 16 1 -5 -9 40.2656 8.11585 7 -1 -5 9 37.5793 8.61523 5 -1 -5 9 34.4985 9.77233 6 -1 -5 9 46.4347 8.84923 7 -1 -5 9 40.6357 8.60984 12 1 -5 -9 36.3525 5.45242 16 1 -5 -9 31.0731 5.43971 17 -1 5 -9 34.6262 16.3873 10 -1 5 -9 38.5867 7.62028 12 -1 5 -9 34.6862 5.67865 15 1 5 9 37.5922 8.10415 6 1 5 9 48.3324 9.10297 7 1 5 9 45.6547 9.61324 8 -1 5 -9 51.4269 11.4983 8 2 -5 9 61.2208 10.0194 18 -2 5 9 39.8312 8.81324 17 -2 5 9 47.6264 8.34480 18 2 5 -9 52.0018 7.73404 12 2 5 -9 63.9691 8.38657 16 2 5 -9 51.8047 7.24161 17 2 5 -9 37.7686 7.31853 18 -2 5 9 46.4009 8.52219 16 -2 5 9 38.1915 8.37399 6 -2 5 9 49.9001 8.59545 7 -2 5 9 50.8174 9.67053 12 -2 5 9 37.1507 6.49748 15 2 5 -9 35.5494 8.39165 19 2 -5 9 66.2238 11.1353 5 2 -5 9 47.3652 9.84324 6 2 -5 9 65.1552 11.5174 19 2 -5 9 51.5866 9.31556 20 2 5 -9 56.6086 8.72731 5 2 5 -9 45.7536 8.99555 6 2 5 -9 46.5251 9.37675 7 2 5 -9 39.0647 10.4959 8 -2 5 9 36.2147 7.99381 5 -2 -5 -9 49.8732 7.69527 4 -2 -5 -9 60.9184 7.92433 5 -2 -5 -9 86.1125 8.43567 6 -2 -5 -9 56.2712 7.35780 12 -2 -5 -9 59.2885 6.89236 13 -2 -5 -9 71.3937 7.65581 14 -2 -5 -9 67.1833 7.93288 15 -2 -5 -9 56.6417 7.41433 16 -2 -5 -9 63.3215 7.09107 17 2 -5 9 36.7250 9.82246 7 2 -5 9 65.7115 12.2699 8 2 5 -9 37.6053 8.71165 20 2 -5 9 63.1750 9.66404 12 2 -5 9 46.8179 7.19043 16 2 -5 9 51.5598 8.86064 17 -2 5 -9 51.8238 9.45106 4 -2 5 -9 65.7020 9.65840 5 -2 5 -9 52.4457 9.66486 6 -2 5 -9 50.2176 9.21562 7 -2 5 -9 49.0264 9.42453 12 2 -5 -9 64.4044 9.72576 8 2 -5 -9 49.0117 20.7343 10 2 -5 -9 45.3791 6.91697 12 2 -5 -9 58.3401 6.47552 16 2 -5 -9 49.3738 6.37257 17 2 -5 -9 42.8101 6.58493 18 2 -5 -9 52.9499 7.53148 19 2 5 9 43.5445 6.60042 17 2 5 9 42.8590 8.13927 18 2 5 9 50.0596 17.7199 11 2 5 9 62.2225 7.45260 12 2 5 9 36.3833 7.77283 6 2 5 9 32.0442 7.89834 7 2 5 9 62.8118 10.2872 8 2 -5 -9 92.1299 9.07124 5 2 -5 -9 62.7338 8.39460 6 2 -5 -9 73.1241 10.0040 7 -2 -5 9 67.4453 10.2754 5 2 5 9 58.5374 9.84956 19 2 5 9 49.0408 9.69846 20 -2 5 -9 66.1894 7.00042 14 -2 5 -9 50.1585 7.54123 15 -2 5 -9 53.9431 8.24091 16 -2 5 -9 54.3584 8.90578 17 -2 5 -9 45.5143 7.19253 18 -2 -5 9 32.6838 8.48950 4 -2 -5 9 42.7601 8.00015 14 -2 -5 9 50.8491 9.81034 15 -2 -5 9 43.2736 10.1508 16 -2 -5 9 50.0430 9.81502 17 -2 -5 9 65.5026 7.42233 18 -2 -5 9 29.2707 8.23438 7 -2 -5 9 53.1144 10.0803 12 -2 -5 9 52.3648 9.92261 6 0 -6 9 2.14959 6.36982 5 0 -6 9 -5.9578 5.62441 7 0 -6 9 0.27103 6.20395 8 0 6 9 7.23975 5.58905 20 0 -6 9 2.21871 6.48018 6 0 -6 -9 -4.2839 3.52697 18 0 -6 9 10.5425 6.66341 4 0 -6 -9 -2.6439 5.21360 12 0 -6 -9 -5.1717 3.28442 14 0 -6 -9 3.45189 3.61403 15 0 -6 -9 0.56552 4.17016 16 0 -6 -9 -1.6946 4.33749 17 0 6 9 0.64979 3.97091 16 0 6 9 -3.6464 5.93736 17 0 6 9 1.63738 6.59264 18 0 6 9 8.06909 7.33174 19 0 -6 -9 10.8145 5.23334 4 0 -6 -9 7.69876 5.11718 5 0 -6 -9 10.9650 4.96991 6 0 -6 -9 5.88635 4.88434 7 0 6 -9 0.91636 4.14460 4 0 6 -9 1.78431 3.82571 5 0 6 -9 -6.4340 4.83485 6 0 6 -9 1.43551 4.83248 7 0 6 -9 -0.9846 5.84181 8 0 6 -9 6.49185 6.04752 12 0 6 -9 1.33665 2.58186 15 0 6 -9 5.33018 4.96770 16 0 6 -9 5.91667 5.34896 17 0 6 -9 -2.1061 5.70585 18 0 6 -9 -5.1299 4.43226 19 0 6 9 -3.4417 4.46651 5 0 6 9 1.29253 5.45341 6 0 6 9 4.71108 6.06606 7 0 6 9 4.63836 5.91905 8 0 6 9 0.85882 13.3108 10 0 6 9 3.87660 6.41077 12 0 -6 9 3.15583 7.41229 18 0 -6 9 4.35318 4.85777 19 0 -6 9 -11.729 6.44751 16 0 -6 9 -2.8964 7.03918 17 0 -6 9 -3.4506 4.16854 15 0 -6 9 -0.1898 7.60184 12 -1 6 9 17.5583 5.98052 5 -1 6 9 15.0757 6.39347 6 -1 6 9 21.5842 6.73418 7 -1 6 9 21.6930 6.72686 8 -1 6 9 2.97200 7.54065 12 -1 6 9 3.28523 4.25234 4 -1 -6 -9 7.03712 6.05187 12 -1 -6 -9 9.80174 5.53988 6 -1 -6 -9 22.8965 5.68866 7 -1 6 9 16.4203 6.55008 19 -1 -6 -9 5.40013 5.32935 5 -1 -6 -9 9.90618 5.54988 17 -1 -6 -9 7.14820 3.27097 18 1 6 -9 8.53554 7.20352 19 1 6 -9 12.2283 4.88709 20 1 6 -9 13.0799 13.1184 10 -1 6 9 13.3782 3.84281 15 -1 6 9 13.2392 6.11949 16 -1 -6 -9 16.4496 4.83922 14 -1 -6 -9 11.5456 4.91231 15 -1 -6 -9 8.81106 4.91618 16 1 -6 9 4.69000 5.79317 4 1 -6 9 8.57825 6.40708 5 1 -6 9 -3.4081 6.49439 6 1 -6 9 10.2282 7.67917 7 1 -6 9 8.39825 7.06982 8 1 -6 9 9.31521 8.37051 12 1 -6 9 8.03036 6.40877 16 1 -6 9 10.7908 7.87557 17 1 -6 9 10.2037 8.58757 18 1 -6 9 0.55747 8.39869 19 1 6 -9 7.16691 4.32050 5 1 6 -9 3.18683 5.88293 6 1 6 -9 10.5634 6.66830 7 1 6 -9 7.87010 6.48693 8 -1 6 9 -4.5637 7.25759 18 1 6 -9 11.9026 6.33497 12 1 6 -9 11.7542 4.84972 16 1 6 -9 10.6943 5.70199 17 1 6 -9 8.61175 6.17970 18 -1 6 9 15.5184 7.60940 17 -1 -6 -9 5.58276 4.32943 4 1 6 9 8.72356 5.34376 5 1 -6 -9 23.4605 7.03521 7 1 6 9 6.73480 5.83966 7 1 6 9 21.1615 8.04469 8 1 6 9 9.87069 6.15655 12 1 6 9 4.13144 3.50265 16 1 6 9 10.7935 5.70324 17 1 6 9 21.6094 7.46983 18 1 6 9 14.2877 8.32024 19 1 6 9 5.44129 6.74856 20 1 -6 -9 9.41743 3.99667 15 1 -6 -9 16.3851 4.86006 16 1 6 9 26.0772 6.91033 6 1 -6 -9 10.8869 5.64773 12 1 -6 -9 19.5529 6.12088 8 1 -6 -9 10.8128 5.02662 4 1 -6 -9 17.0375 6.11089 5 1 -6 -9 13.9905 5.62080 6 -1 -6 9 5.35422 5.34124 4 -1 -6 9 21.8608 7.34132 5 -1 -6 9 15.2478 8.28538 6 -1 -6 9 15.3869 7.34648 7 -1 -6 9 1.68714 8.31641 12 -1 -6 9 15.3776 5.50718 14 -1 -6 9 11.1344 7.29307 15 -1 -6 9 9.42400 8.59139 16 -1 -6 9 9.99178 8.48322 17 -1 -6 9 14.0038 7.68920 18 -1 6 -9 10.2656 5.83048 4 -1 6 -9 14.3244 5.32191 5 -1 6 -9 9.72735 6.88081 6 -1 6 -9 11.0681 6.05195 7 -1 6 -9 16.6627 8.79091 8 -1 6 -9 9.76744 7.21855 12 -1 6 -9 16.1544 4.77897 15 -1 6 -9 22.5111 6.55412 16 -1 6 -9 0.29924 6.19334 17 -1 6 -9 7.64825 6.68829 18 1 -6 -9 11.6726 4.78075 17 1 -6 -9 14.5501 5.32717 18 1 -6 -9 13.6775 4.23179 19 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.6499 _exptl_absorpt_correction_T_min 0.5303 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 5.911 10.053 5.862 90.013 90.023 89.991 ) ; _shelx_hkl_checksum 13800 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,-Y,+Z 3 -X,+Y,1/2-Z 4 1/2+X,-Y,1/2-Z 5 -X,-Y,-Z 6 1/2+X,+Y,-Z 7 +X,-Y,1/2+Z 8 1/2-X,+Y,1/2+Z loop_ _atom_local_axes_atom_label _atom_local_axes_atom0 _atom_local_axes_ax1 _atom_local_axes_atom1 _atom_local_axes_atom2 _atom_local_axes_ax2 NA(1) O(1) Z NA(1) C(1) Y O(1) C(1) X O(1) DUM1 Y O(2) C(1) X O(2) DUM2 Y C(1) O(1) X C(1) DUM1 Y C(2) C(1) Z C(2) H(2C) X H(2A) C(2) Z H(2A) C(1) Y H(2B) C(2) Z H(2B) C(1) Y H(2C) C(2) Z H(2C) C(1) Y loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Na(1) Na 0.5 0.58375(4) 0.25 0.013 Uani 1 4 O(1) O 0.36793(10) 0.64246(6) 0.88432(9) 0.015 Uani 0.8581 8 O(2) O 0.3681(8) 0.6426(4) 0.6145(8) 0.022 Uani 0.1419 8 C(1) C 0.5 0.70146(9) 0.75 0.012 Uani 1 4 C(2) C 0.5 0.85216(12) 0.75 0.031 Uani 1 4 H(2A) H 0.4073 0.8882 0.6027 0.061(11) Uiso 0.5 8 H(2B) H 0.6728 0.8882 0.7426 0.056(11) Uiso 0.5 8 H(2C) H 0.4199 0.8882 0.9046 0.051(10) Uiso 0.5 8 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na(1) 0.0099(2) 0.0187(2) 0.00898(18) 0 0.00011(12) 0 O(1) 0.0102(3) 0.0265(3) 0.0080(2) 0.00218(19) 0.00032(17) -0.0024(2) O(2) 0.022(2) 0.0131(14) 0.033(2) -0.0043(15) 0.0015(16) -0.0036(14) C(1) 0.0105(4) 0.0161(3) 0.0101(3) 0 0.0015(3) 0 C(2) 0.0384(8) 0.0156(4) 0.0382(7) 0 0.0059(5) 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag NA(1) NA(1) NA(1) 120.80(2) 2_565 1_555 2_665 yes NA(1) NA(1) NA(1) 75.786(11) 2_565 1_555 5_665 yes NA(1) NA(1) O(1) 80.518(14) 2_565 1_555 1_554 yes NA(1) NA(1) O(1) 114.299(15) 2_565 1_555 3_656 yes NA(1) NA(1) O(1) 156.080(19) 2_565 1_555 6_556 yes NA(1) NA(1) O(2) 155.98(10) 2_565 1_555 6_556 yes O(1) NA(1) O(1) 151.07(4) 1_554 1_555 3_656 yes O(1) NA(1) O(1) 86.574(14) 1_554 1_555 6_556 yes O(1) NA(1) O(1) 86.365(14) 1_554 1_555 8_554 yes O(1) NA(1) O(2) 130.89(11) 1_554 1_555 1_555 yes O(1) NA(1) O(2) 122.85(10) 1_554 1_555 6_556 yes NA(1) O(1) NA(1) 122.72(3) 1_556 1_555 6_456 yes NA(1) O(1) C(1) 118.80(4) 1_556 1_555 1_555 yes NA(1) O(2) NA(1) 122.84(18) 1_555 1_555 6_456 yes NA(1) O(2) C(1) 119.1(3) 1_555 1_555 1_555 yes O(1) C(1) O(1) 123.85(9) 1_555 1_555 3_656 yes O(1) C(1) C(2) 118.07(5) 1_555 1_555 1_555 yes O(2) C(1) O(2) 124.2(4) 1_555 1_555 3_656 yes O(2) C(1) C(2) 117.92(19) 1_555 1_555 1_555 yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag NA(1) NA(1) 3.4205(4) 1_555 2_565 yes NA(1) NA(1) 3.3989(4) 1_555 5_665 yes NA(1) O(1) 2.3707(5) 1_555 1_554 yes NA(1) O(1) 2.4017(6) 1_555 6_556 yes NA(1) O(2) 2.364(4) 1_555 1_555 yes NA(1) O(2) 2.405(4) 1_555 6_556 yes O(1) C(1) 1.2645(7) 1_555 1_555 yes O(2) C(1) 1.268(4) 1_555 1_555 yes C(1) C(2) 1.5201(15) 1_555 1_555 yes