data_300KXPREF5_publ

_pd_block_id
  2013-07-24T01:19|300KXPREF5|GSAS|Overall

_audit_creation_method  "from EXP file using GSAS2CIF"
_audit_creation_date                   2013-07-24T01:19
_audit_author_name                     GSAS
_audit_update_record
; 2013-07-24T01:19  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_300KXPREF5_overall

_refine_ls_shift/su_max                0.04
_refine_ls_shift/su_mean               0.01
_computing_structure_refinement        GSAS
_refine_ls_number_parameters           70
_refine_ls_goodness_of_fit_all         1.95
_refine_ls_number_restraints           0

# Overall powder R-factors

_pd_proc_ls_prof_R_factor              0.0365
_pd_proc_ls_prof_wR_factor             0.0455
_refine_ls_matrix_type                 full

# pointers to the phase blocks
loop_   _pd_phase_block_id
      2013-07-24T01:19|300KXPREF5_phase1|GSAS||
      2013-07-24T01:19|300KXPREF5_phase2|GSAS||
      2013-07-24T01:19|300KXPREF5_phase3|GSAS||
# pointers to the diffraction patterns
loop_   _pd_block_diffractogram_id
      2013-07-24T01:19|300KXPREF5_H_01|GSAS|HRPD
      2013-07-24T01:19|300KXPREF5_H_02|GSAS|HRPD

# Information for phase 1
data_300KXPREF5_phase_1

_pd_block_id
  2013-07-24T01:19|300KXPREF5_phase1|GSAS||

# Histograms for phase 1
loop_   _pd_block_diffractogram_id
  2013-07-24T01:19|300KXPREF5_H_01|GSAS|HRPD
  2013-07-24T01:19|300KXPREF5_H_02|GSAS|HRPD


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

# 8. Phase information from GSAS

_pd_phase_name
                   "from F:/University/MyWork/New/CsZrCu_SAR/cs2cu3zrf12rt.cif"
_cell_length_a                         7.13155(6)
_cell_length_b                         7.13155
_cell_length_c                         20.36095(34)
_cell_angle_alpha                      90.0
_cell_angle_beta                       90.0
_cell_angle_gamma                      120.0
_cell_volume                           896.800(17)
_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
F-
F1      0.20412(19) -0.20412(19)  0.98417(12)  1.0        Uiso   0.0163(7)    18
F-
F2      0.13038(20) -0.13038(20)  0.44695(14)  1.0        Uiso   0.0348(10)   18
Cs
Cs1     0.0          0.0          0.10564(25)  1.0        Uiso   0.0232(13)    6
Sn
Sn1     0.0          0.0          0.5          1.0        Uiso   0.0109(12)    3
Cu
Cu1    -0.5          0.0          0.0          1.0        Uiso   0.0058(6)     9

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   F- 36.0        
                   Cs  6.0        
                   Sn  3.0        
                   Cu  9.0        
 
# 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                3.532(4)  .      1_554  N
  Cs1       F1                3.532(4)  .      2_554  N
  Cs1       F1                3.532(4)  .      3_554  N
  Cs1       F1                3.115(4)  .     -1_556  N
  Cs1       F1                3.115(4)  .     -2_556  N
  Cs1       F1                3.115(4)  .     -3_556  N
  Cs1       F2               3.5975(4)  .    101_444  N
  Cs1       F2               3.5975(4)  .    101_554  N
  Cs1       F2               3.5975(4)  .    102_444  N
  Cs1       F2               3.5975(4)  .    102_544  N
  Cs1       F2               3.5975(4)  .    103_544  N
  Cs1       F2               3.5975(4)  .    103_554  N
  Cs1       F2                3.418(4)  .   -101_434  N
  Cs1       F2                3.418(4)  .   -102_444  N
  Cs1       F2                3.418(4)  .   -103_334  N
  Sn1       F2              1.9391(27)  .      1_555  N
  Sn1       F2              1.9391(27)  .      2_555  N
  Sn1       F2              1.9391(27)  .      3_555  N
  Sn1       F2              1.9391(27)  .     -1_556  N
  Sn1       F2              1.9391(27)  .     -2_556  N
  Sn1       F2              1.9391(27)  .     -3_556  N
  Cu1       F1               1.8984(8)  .      1_454  N
  Cu1       F1               1.8984(8)  .      3_554  N
  Cu1       F1               1.8984(8)  .     -1_556  N
  Cu1       F1               1.8984(8)  .     -3_456  N
  Cu1       F2              2.3564(28)  .    102_444  N
  Cu1       F2              2.3564(28)  .   -202_344  N


# Information for phase 2
data_300KXPREF5_phase_2

_pd_block_id
  2013-07-24T01:19|300KXPREF5_phase2|GSAS||

# Histograms for phase 2
loop_   _pd_block_diffractogram_id
  2013-07-24T01:19|300KXPREF5_H_01|GSAS|HRPD
  2013-07-24T01:19|300KXPREF5_H_02|GSAS|HRPD

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

# 8. Phase information from GSAS

_pd_phase_name
    "from F:/University/MyWork/New/CsSnCu/diamond1011/Cs2SnF6.cif"
_cell_length_a                         6.3262(5)
_cell_length_b                         6.3262
_cell_length_c                         5.0390(7)
_cell_angle_alpha                      90.0
_cell_angle_beta                       90.0
_cell_angle_gamma                      120.0
_cell_volume                           174.648(21)
_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   0.0126(24)    2
Sn
Sn1     0.0          0.0          0.0          1.0        Uiso   0.0126(24)    1
F-
F1      0.148       -0.148       -0.2163       1.0        Uiso   0.0126(24)    6

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   F-  6.0        
                   Cs  2.0        
                   Sn  1.0        
 
# 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_300KXPREF5_phase_3

_pd_block_id
  2013-07-24T01:19|300KXPREF5_phase3|GSAS||

# Histograms for phase 3
loop_   _pd_block_diffractogram_id
  2013-07-24T01:19|300KXPREF5_H_01|GSAS|HRPD
  2013-07-24T01:19|300KXPREF5_H_02|GSAS|HRPD

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

# 8. Phase information from GSAS

_pd_phase_name
                   "from F:/University/MyWork/New/CsSnCu/diamond0312/CuO.cif"
_cell_length_a                         4.6869(4)
_cell_length_b                         3.42396(25)
_cell_length_c                         5.1337(4)
_cell_angle_alpha                      90.0
_cell_angle_beta                       99.535(5)
_cell_angle_gamma                      90.0
_cell_volume                           81.247(6)
_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   0.0130(27)    4
O-
O1      0.0          0.4184       0.25         1.0        Uiso   0.0130(27)    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_300KXPREF5_p_01

_pd_block_id
  2013-07-24T01:19|300KXPREF5_H_01|GSAS|HRPD
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION
# phase table
loop_     _pd_phase_id
          _pd_phase_block_id
          _pd_phase_mass_%
  1  2013-07-24T01:19|300KXPREF5_phase1|GSAS||
           85.25999
;
           0.00100
  2  2013-07-24T01:19|300KXPREF5_phase2|GSAS||
           11.89(32)
;
           0.00100
  3  2013-07-24T01:19|300KXPREF5_phase3|GSAS||
            2.85(14)

loop_ _atom_type_symbol
      _atom_type_scat_length_neutron
      _atom_type_scat_source
  F-1   0.5654
  International_Tables_Vol_C
  Cs+1   0.5420
  International_Tables_Vol_C
  Sn+4   0.6225
  International_Tables_Vol_C
  Cu+2   0.7718
  International_Tables_Vol_C
  O-2   0.5803
  International_Tables_Vol_C
_diffrn_radiation_probe                neutron
_pd_proc_ls_prof_R_factor              0.0365
_pd_proc_ls_prof_wR_factor             0.0400
_pd_proc_ls_prof_wR_expected           0.0299
_refine_ls_R_Fsqd_factor               0.12633
