data_300KXPL3_publ

_pd_block_id
  2014-04-15T11:24|300KXPL3|gsas|Overall

_audit_creation_method  "from EXP file using GSAS2CIF"
_audit_creation_date                   2014-04-15T11:24
_audit_author_name                     gsas
_audit_update_record
; 2014-04-15T11:24  Initial CIF as created by GSAS2CIF
;
# 1. SUBMISSION DETAILS

_publ_contact_author_name        
'Philip Lightfoot' # Name of author for correspondence
_publ_contact_author_address     # Address of author for correspondence
;School of Chemistry,
University of St Andrews,
North Haugh,
St Andrews,
Fife,
Scotland,
KY16 9ST
;
_publ_contact_author_email       pl@st-andrews.ac.uk
_publ_contact_author_phone       ?
_publ_contact_author_fax         ?
_journal_coden_cambridge         ?
_journal_name_full               ?
_journal_page_first              ?
_journal_volume                  ?
_journal_year                    ?
loop_
_publ_author_name
_publ_author_address
'Downie, L. J.'
; ?
;
'Black, C.'
; ?
;
'Ardashnikova, E. I.'
; ?
;
'Tang, C. C.'
; ?             
;
'Vasiliev, A. N.'
; ?
;
'Golovanov, A.'
; ?
;
'Berdonosov, P. S.'
; ?
;
'Dolgikh, V. A.'
; ?
;
'Lightfoot, P.'
; ?

#==============================================================================

# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate                ?
_pd_prep_pressure                 ?
_pd_prep_temperature              ?

_pd_char_colour                   ?       # use ICDD colour descriptions
data_300KXPL3_overall

_refine_ls_shift/su_max                0.04
_refine_ls_shift/su_mean               0.01
_computing_structure_refinement        GSAS
_refine_ls_number_parameters           48
_refine_ls_goodness_of_fit_all         2.33
_refine_ls_number_restraints           0
_refine_ls_matrix_type                 full

# pointers to the phase blocks
loop_   _pd_phase_block_id
      2014-04-15T11:24|300KXPL3_phase1|gsas||
      2014-04-15T11:24|300KXPL3_phase2|gsas||
      2014-04-15T11:24|300KXPL3_phase3|gsas||
# pointers to the diffraction patterns
loop_   _pd_block_diffractogram_id
      2014-04-15T11:24|300KXPL3_H_01|gsas|I11

# Information for phase 1
data_300KXPL3_phase_1

_pd_block_id
  2014-04-15T11:24|300KXPL3_phase1|gsas||

# Histograms for phase 1
loop_   _pd_block_diffractogram_id
  2014-04-15T11:24|300KXPL3_H_01|gsas|I11

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name
    "from C:/gsas/MyWork/New_School/CsSnCu/diamond0411/icsd_79114.cif"
_cell_length_a                         7.131778(10)
_cell_length_b                         7.131778
_cell_length_c                         20.36703(4)
_cell_angle_alpha                      90.0
_cell_angle_beta                       90.0
_cell_angle_gamma                      120.0
_cell_volume                           897.1270(30)
_symmetry_cell_setting                 trigonal
_symmetry_space_group_name_H-M         "R -3 m"
loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz
       1 +x,+y,+z 
       2 -y,x-y,+z 
       3 y-x,-x,+z 
       4 y-x,+y,+z 
       5 -y,-x,+z 
       6 +x,x-y,+z 
      -1 -x,-y,-z 
      -2 +y,y-x,-z 
      -3 x-y,+x,-z 
      -4 x-y,-y,-z 
      -5 +y,+x,-z 
      -6 -x,y-x,-z 
     101 +x+1/3,+y+2/3,+z+2/3 
     102 -y+1/3,x-y+2/3,+z+2/3 
     103 y-x+1/3,-x+2/3,+z+2/3 
     104 y-x+1/3,+y+2/3,+z+2/3 
     105 -y+1/3,-x+2/3,+z+2/3 
     106 +x+1/3,x-y+2/3,+z+2/3 
    -101 -x+2/3,-y+1/3,-z+1/3 
    -102 +y+2/3,y-x+1/3,-z+1/3 
    -103 x-y+2/3,+x+1/3,-z+1/3 
    -104 x-y+2/3,-y+1/3,-z+1/3 
    -105 +y+2/3,+x+1/3,-z+1/3 
    -106 -x+2/3,y-x+1/3,-z+1/3 
     201 +x+2/3,+y+1/3,+z+1/3 
     202 -y+2/3,x-y+1/3,+z+1/3 
     203 y-x+2/3,-x+1/3,+z+1/3 
     204 y-x+2/3,+y+1/3,+z+1/3 
     205 -y+2/3,-x+1/3,+z+1/3 
     206 +x+2/3,x-y+1/3,+z+1/3 
    -201 -x+1/3,-y+2/3,-z+2/3 
    -202 +y+1/3,y-x+2/3,-z+2/3 
    -203 x-y+1/3,+x+2/3,-z+2/3 
    -204 x-y+1/3,-y+2/3,-z+2/3 
    -205 +y+1/3,+x+2/3,-z+2/3 
    -206 -x+1/3,y-x+2/3,-z+2/3 

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
Cs
Cs1     0.0          0.0          0.106266(25  1.0        Uiso   0.02096(16)   6
Sn
Sn1     0.0          0.0          0.5          1.0        Uiso   0.00404(16)   3
Cu
Cu1     0.5          0.0          0.0          1.0        Uiso  -0.00062(15)   9
F-
F1      0.20541(15) -0.20541(15)  0.98475(10)  1.0        Uiso   0.0173(5)    18
F-
F2      0.13211(15)  0.86789(15)  0.44676(10)  1.0        Uiso   0.0173(5)    18

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   Cs  6.0        
                   Sn  3.0        
                   Cu  9.0        
                   F- 36.0        
 
# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum                  "Cs2 Cu3 F12 Sn"
_chemical_formula_weight               803.11
_cell_formula_units_Z                  3

# MOLECULAR GEOMETRY

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
  Cs1       F1              3.5446(19)  .      1_554  N
  Cs1       F1              3.5446(19)  .      2_554  N
  Cs1       F1              3.5446(19)  .      3_554  N
  Cs1       F1              3.1423(20)  .     -1_556  N
  Cs1       F1              3.1423(20)  .     -2_556  N
  Cs1       F1              3.1423(20)  .     -3_556  N
  Cs1       F2             3.59431(23)  .    101_434  N
  Cs1       F2             3.59432(23)  .    101_544  N
  Cs1       F2             3.59432(23)  .    102_554  N
  Cs1       F2             3.59431(23)  .    102_654  N
  Cs1       F2             3.59432(23)  .    103_444  N
  Cs1       F2             3.59431(23)  .    103_454  N
  Cs1       F2              3.3964(21)  .   -101_444  N
  Cs1       F2              3.3964(21)  .   -102_334  N
  Cs1       F2              3.3964(21)  .   -103_434  N
  Sn1       F2              1.9592(18)  .      1_545  N
  Sn1       F2              1.9592(18)  .      2_665  N
  Sn1       F2              1.9592(18)  .      3_455  N
  Sn1       F2              1.9592(18)  .     -1_566  N
  Sn1       F2              1.9592(18)  .     -2_446  N
  Sn1       F2              1.9592(18)  .     -3_656  N
  Cu1       F1               1.8918(6)  .      1_554  N
  Cu1       F1               1.8918(6)  .      3_654  N
  Cu1       F1               1.8918(6)  .     -1_656  N
  Cu1       F1               1.8918(6)  .     -3_556  N
  Cu1       F2              2.3493(20)  .    102_654  N
  Cu1       F2              2.3493(20)  .   -202_334  N

# Information for phase 2
data_300KXPL3_phase_2

_pd_block_id
  2014-04-15T11:24|300KXPL3_phase2|gsas||

# Histograms for phase 2
loop_   _pd_block_diffractogram_id
  2014-04-15T11:24|300KXPL3_H_01|gsas|I11

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name
    "from C:/gsas/MyWork/New_School/CsSnCu/diamond0312/Cs2SnF6.cif"
_cell_length_a                         6.32825(10)
_cell_length_b                         6.32825
_cell_length_c                         5.04171(12)
_cell_angle_alpha                      90.0
_cell_angle_beta                       90.0
_cell_angle_gamma                      120.0
_cell_volume                           174.854(4)
_symmetry_cell_setting                 trigonal
_symmetry_space_group_name_H-M         "P -3 m 1"
loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz
       1 +x,+y,+z 
       2 -y,x-y,+z 
       3 y-x,-x,+z 
       4 y-x,+y,+z 
       5 -y,-x,+z 
       6 +x,x-y,+z 
      -1 -x,-y,-z 
      -2 +y,y-x,-z 
      -3 x-y,+x,-z 
      -4 x-y,-y,-z 
      -5 +y,+x,-z 
      -6 -x,y-x,-z 

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
Cs
Cs1     0.3333       0.6667       0.309        1.0        Uiso   0.0007(4)     2
Sn
Sn1     0.0          0.0          0.0          1.0        Uiso   0.0007(4)     1
F-
F1      0.148       -0.148       -0.2163       1.0        Uiso   0.0007(4)     6

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   Cs  2.0        
                   Sn  1.0        
                   F-  6.0        
 
# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum                  "Cs2 F6 Sn"
_chemical_formula_weight               498.49
_cell_formula_units_Z                  1


# Information for phase 3
data_300KXPL3_phase_3

_pd_block_id
  2014-04-15T11:24|300KXPL3_phase3|gsas||

# Histograms for phase 3
loop_   _pd_block_diffractogram_id
  2014-04-15T11:24|300KXPL3_H_01|gsas|I11

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name
                   "from C:/gsas/MyWork/New_School/CsSnCu/diamond0312/CuO.cif"
_cell_length_a                         4.68685(26)
_cell_length_b                         3.42432(15)
_cell_length_c                         5.13223(25)
_cell_angle_alpha                      90.0
_cell_angle_beta                       99.5422(34)
_cell_angle_gamma                      90.0
_cell_volume                           81.229(4)
_symmetry_cell_setting                 monoclinic
_symmetry_space_group_name_H-M         "C 1 2/c 1"
loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz
       1 +x,+y,+z 
       2 -x,+y,-z+1/2 
      -1 -x,-y,-z 
      -2 +x,-y,+z+1/2 
     101 +x+1/2,+y+1/2,+z 
     102 -x+1/2,+y+1/2,-z+1/2 
    -101 -x+1/2,-y+1/2,-z 
    -102 +x+1/2,-y+1/2,+z+1/2 

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
Cu
CU1     0.25         0.25         0.0          1.0        Uiso  -0.0066(10)    4
O 
O1      0.0          0.4184       0.25         1.0        Uiso  -0.0066(10)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   Cu  4.0        
                   O   4.0        
 
# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum                  "Cu O"
_chemical_formula_weight               79.54
_cell_formula_units_Z                  4


# Powder diffraction data for histogram  1
data_300KXPL3_p_01

_pd_block_id
  2014-04-15T11:24|300KXPL3_H_01|gsas|I11
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

# phase table
loop_     _pd_phase_id
          _pd_phase_block_id
          _pd_phase_mass_%
  1  2014-04-15T11:24|300KXPL3_phase1|gsas||
           87.43
;
  2  2014-04-15T11:24|300KXPL3_phase2|gsas||
            9.33(5)
;
  3  2014-04-15T11:24|300KXPL3_phase3|gsas||
            3.23(5)
;

loop_ _atom_type_symbol
      _atom_type_scat_dispersion_real
      _atom_type_scat_dispersion_imag
      _atom_type_scat_Cromer_Mann_a1
      _atom_type_scat_Cromer_Mann_a2
      _atom_type_scat_Cromer_Mann_a3
      _atom_type_scat_Cromer_Mann_a4
      _atom_type_scat_Cromer_Mann_b1
      _atom_type_scat_Cromer_Mann_b2
      _atom_type_scat_Cromer_Mann_b3
      _atom_type_scat_Cromer_Mann_b4
      _atom_type_scat_Cromer_Mann_c
      _atom_type_scat_source
  Cs+1    0.000    0.000
 20.3524 3.55200 19.1278 0.30860 10.2821 23.7128 0.96150 59.4565 3.27910 
  International_Tables_Vol_C
  Sn+4    0.000    0.000
 18.9333 5.76400 19.7131 0.46550 3.41820 14.0049 0.01930 -0.7583 3.91820 
  International_Tables_Vol_C
  Cu+2    0.000    0.000
 11.8168 3.37484 7.11181 0.24408 5.78135 7.98760 1.14523 19.8970 1.14431 
  International_Tables_Vol_C
  F-1    0.000    0.000
 3.63220 5.27756 3.51057 14.7353 1.26064 0.44226 0.94071 47.3437 0.65340 
  International_Tables_Vol_C
  Cu    0.000    0.000
 13.3380 3.58280 7.16760 0.24700 5.61580 11.3966 1.67350 64.8126 1.19100 
  International_Tables_Vol_C
  O    0.000    0.000
 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 
  International_Tables_Vol_C
_diffrn_radiation_probe                x-ray
_diffrn_radiation_polarisn_ratio       0.93
_diffrn_radiation_wavelength           0.827168
_diffrn_radiation_type                 ?
_pd_proc_ls_prof_R_factor              0.0655
_pd_proc_ls_prof_wR_factor             0.0837
_pd_proc_ls_prof_wR_expected           0.0360
_refine_ls_R_Fsqd_factor               0.07403

