data_100KXPREF2_publ

_pd_block_id
  2013-07-24T01:37|100KXPREF2|gsas|Overall

_audit_creation_method  "from EXP file using GSAS2CIF"
_audit_creation_date                   2013-07-24T01:37
_audit_author_name                     gsas
_audit_update_record
; 2013-07-24T01:37  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_100KXPREF2_overall

_refine_ls_shift/su_max                0.02
_refine_ls_shift/su_mean               0.00
_computing_structure_refinement        GSAS
_refine_ls_number_parameters           101
_refine_ls_goodness_of_fit_all         1.86
_refine_ls_number_restraints           0

# Overall powder R-factors

_pd_proc_ls_prof_R_factor              0.0350
_pd_proc_ls_prof_wR_factor             0.0433
_refine_ls_matrix_type                 full

# pointers to the phase blocks
loop_   _pd_phase_block_id
      2013-07-24T01:37|100KXPREF2_phase1|gsas||
      2013-07-24T01:37|100KXPREF2_phase2|gsas||
      2013-07-24T01:37|100KXPREF2_phase3|gsas||
# pointers to the diffraction patterns
loop_   _pd_block_diffractogram_id
      2013-07-24T01:37|100KXPREF2_H_01|gsas|HRPD
      2013-07-24T01:37|100KXPREF2_H_02|gsas|HRPD

# Information for phase 1
data_100KXPREF2_phase_1

_pd_block_id
  2013-07-24T01:37|100KXPREF2_phase1|gsas||

# Histograms for phase 1
loop_   _pd_block_diffractogram_id
  2013-07-24T01:37|100KXPREF2_H_01|gsas|HRPD
  2013-07-24T01:37|100KXPREF2_H_02|gsas|HRPD

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

# 8. Phase information from GSAS

_pd_phase_name
                   "from F:/University/MyWork/New/CsSnCu/cssncu_LT.cif"
_cell_length_a                         7.89656(16)
_cell_length_b                         7.09752(15)
_cell_length_c                         10.58758(25)
_cell_angle_alpha                      90.0
_cell_angle_beta                       97.8209(16)
_cell_angle_gamma                      90.0
_cell_volume                           587.872(16)
_symmetry_cell_setting                 monoclinic
_symmetry_space_group_name_H-M         "P 1 21/n 1"
loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz
       1 +x,+y,+z 
       2 -x+1/2,+y+1/2,-z+1/2 
      -1 -x,-y,-z 
      -2 +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
Cs
Cs1     0.2121(7)   -0.0100(11)   0.8927(6)    1.0        Uiso   0.0027(11)    4
Sn
Sn1     0.0          0.0          0.5          1.0        Uiso   0.0044(12)    2
Cu
Cu1     0.5          0.0          0.5          1.0        Uiso   0.0020(18)    2
Cu
Cu2     0.2493(7)    0.2668(7)    0.2560(5)    1.0        Uiso  -0.0009(10)    4
F-
F1      0.4214(9)    0.2047(10)   0.3965(7)    1.0        Uiso   0.0034(16)    4
F-
F2      0.9419(9)    0.6817(10)   0.8650(7)    1.0        Uiso   0.0023(16)    4
F-
F3      0.2407(9)    0.0099(12)   0.1834(8)    1.0        Uiso   0.0090(18)    4
F-
F4      0.4439(9)    0.7182(11)   0.0967(7)    1.0        Uiso   0.0089(18)    4
F-
F5     -0.0227(9)    0.1714(11)   0.6400(7)    1.0        Uiso   0.0091(18)    4
F-
F6      0.7614(8)    0.0412(11)   0.4302(7)    1.0        Uiso   0.0022(16)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   Cu  6.0        
                   Sn  2.0        
                   Cs  4.0        
                   F- 24.0        
 
# 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                  2

# 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                3.291(9)  .      2_546  N
  Cs1       F1               3.161(10)  .     -2_455  N
  Cs1       F2               3.042(10)  .      1_445  N
  Cs1       F2                3.787(8)  .     -1_667  N
  Cs1       F3               3.058(11)  .      1_556  N
  Cs1       F3                3.557(9)  .     -1_556  N
  Cs1       F4               3.265(11)  .      1_546  N
  Cs1       F4               3.406(10)  .     -1_666  N
  Cs1       F4               3.832(10)  .     -2_455  N
  Cs1       F5               3.303(11)  .      1_555  N
  Cs1       F5               3.388(10)  .      2_546  N
  Cs1       F5               3.940(11)  .     -2_555  N
  Cs1       F6                3.460(9)  .     -1_656  N
  Cs1       F6               3.805(11)  .     -2_445  N
  Cs1       F6               3.368(11)  .     -2_455  N
  Sn1       F4                1.940(7)  .      2_545  N
  Sn1       F4                1.940(7)  .     -2_455  N
  Sn1       F5                1.945(7)  .      1_555  N
  Sn1       F5                1.945(7)  .     -1_556  N
  Sn1       F6                1.950(6)  .      1_455  N
  Sn1       F6                1.950(6)  .     -1_656  N
  Cu1       F1                1.874(8)  .      1_555  N
  Cu1       F1                1.874(8)  .     -1_656  N
  Cu1       F2                1.934(8)  .      2_646  N
  Cu1       F2                1.934(8)  .     -2_454  N
  Cu1       F3                3.683(8)  .      1_555  N
  Cu1       F3                3.683(8)  .     -1_656  N
  Cu1       F6                2.304(7)  .      1_555  N
  Cu1       F6                2.304(7)  .     -1_656  N
  Cu2       F1                1.925(9)  .      1_555  N
  Cu2       F1                3.673(9)  .      2_555  N
  Cu2       F2               1.878(10)  .     -1_666  N
  Cu2       F2                3.647(8)  .     -2_454  N
  Cu2       F3               1.976(11)  .      1_555  N
  Cu2       F3               1.839(11)  .      2_555  N
  Cu2       F4                2.351(8)  .      2_545  N
  Cu2       F5                2.355(9)  .     -2_554  N
  Cu2       F6                3.723(9)  .     -2_454  N

# Information for phase 2
data_100KXPREF2_phase_2

_pd_block_id
  2013-07-24T01:37|100KXPREF2_phase2|gsas||

# Histograms for phase 2
loop_   _pd_block_diffractogram_id
  2013-07-24T01:37|100KXPREF2_H_01|gsas|HRPD
  2013-07-24T01:37|100KXPREF2_H_02|gsas|HRPD


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

# 8. Phase information from GSAS

_pd_phase_name
                   "from C:/gsas/MyWork/New/CsSnCu/diamond1011/Cs2SnF6.cif"
_cell_length_a                         6.2867(5)
_cell_length_b                         6.2867
_cell_length_c                         4.9881(8)
_cell_angle_alpha                      90.0
_cell_angle_beta                       90.0
_cell_angle_gamma                      120.0
_cell_volume                           170.731(23)
_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   0.0057(17)    2
Sn
Sn1     0.0          0.0          0.0          1.0        Uiso   0.0057(17)    1
F-
F1      0.148       -0.148       -0.2163       1.0        Uiso   0.0057(17)    6

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   Sn  1.0        
                   Cs  2.0        
                   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_100KXPREF2_phase_3

_pd_block_id
  2013-07-24T01:37|100KXPREF2_phase3|gsas||

# Histograms for phase 3
loop_   _pd_block_diffractogram_id
  2013-07-24T01:37|100KXPREF2_H_01|gsas|HRPD
  2013-07-24T01:37|100KXPREF2_H_02|gsas|HRPD

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


# 8. Phase information from GSAS

_pd_phase_name
                   "from C:/gsas/MyWork/New/CsSnCu/diamond1011/CuO.cif"
_cell_length_a                         4.6878(14)
_cell_length_b                         3.4045(9)
_cell_length_c                         5.1360(16)
_cell_angle_alpha                      90.0
_cell_angle_beta                       99.602(21)
_cell_angle_gamma                      90.0
_cell_volume                           80.822(25)
_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  -0.0076(23)    4
O-
O1      0.0          0.4184       0.25         1.0        Uiso  -0.0076(23)    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_100KXPREF2_p_01

_pd_block_id
  2013-07-24T01:37|100KXPREF2_H_01|gsas|HRPD
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

# phase table
loop_     _pd_phase_id
          _pd_phase_block_id
          _pd_phase_mass_%
  1  2013-07-24T01:37|100KXPREF2_phase1|gsas||
           81.7
;
  2  2013-07-24T01:37|100KXPREF2_phase2|gsas||
           14.78(32)
;
  3  2013-07-24T01:37|100KXPREF2_phase3|gsas||
            3.52(18)
;

loop_ _atom_type_symbol
      _atom_type_scat_length_neutron
      _atom_type_scat_source
  Cu+2   0.7718
  International_Tables_Vol_C
  Sn+4   0.6225
  International_Tables_Vol_C
  Cs+1   0.5420
  International_Tables_Vol_C
  F-1   0.5654
  International_Tables_Vol_C
  O-2   0.5803
  International_Tables_Vol_C
_diffrn_radiation_probe                neutron
_pd_proc_ls_prof_R_factor              0.0362
_pd_proc_ls_prof_wR_factor             0.0395
_pd_proc_ls_prof_wR_expected           0.0299
_refine_ls_R_Fsqd_factor               0.08902

