data_NONCAL_publ

_pd_block_id
  2016-01-06T13:43|NONREF|ceak|combi

_audit_creation_method  "from EXP file using GSAS2CIF"
_audit_creation_date                   2016-01-06T13:43
_audit_author_name                     ceak
_audit_update_record
; 2016-01-06T13:43  Initial CIF as created by GSAS2CIF
;

#=============================================================================
# Rietveld refinement of NON obtained from synthesis using                   #
# azonia-spiro [4, 5] decane as structure directing agent                    #
#                                                                            #
#                                                                            #
#   Ge was assumed to occupy sites 1-4 in a ratio according to observed      #
#   content. Si-O bonds and O-O distances were constrained to 1.6            #
#   and 2.7A , respectively (weight 0.5)                                     #
#   Measurement occurred at BM01B (Swiss Norwegian Beam Lines, SNBL)         #
#   at the European Synchrotron Radiation Facility (ESRF), Grenoble, France  #
#   with a wavelength of  0.50493A                                           # 
#=============================================================================

_refine_ls_shift/su_max                0.04
_refine_ls_shift/su_mean               0.01
_computing_structure_refinement        GSAS
_refine_ls_number_parameters           51
_refine_ls_goodness_of_fit_all         1.41
_refine_ls_number_restraints           45
_refine_ls_matrix_type                 full
#==============================================================================

_pd_phase_name
    "NON azonia spiro templated, calcined"
_cell_length_a                         22.1062(23)
_cell_length_b                         15.0195(18)
_cell_length_c                         13.6153(16)
_cell_angle_alpha                      90.0
_cell_angle_beta                       90.0
_cell_angle_gamma                      90.0
_cell_volume                           4520.6(10)
_symmetry_cell_setting                 orthorhombic
_symmetry_space_group_name_H-M         "F m m m"
loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz
       1 +x,+y,+z 
       2 -x,+y,+z 
       3 +x,-y,+z 
       4 -x,-y,+z 
      -1 -x,-y,-z 
      -2 +x,-y,-z 
      -3 -x,+y,-z 
      -4 +x,+y,-z 
     101 +x,+y+1/2,+z+1/2 
     102 -x,+y+1/2,+z+1/2 
     103 +x,-y+1/2,+z+1/2 
     104 -x,-y+1/2,+z+1/2 
    -101 -x,-y+1/2,-z+1/2 
    -102 +x,-y+1/2,-z+1/2 
    -103 -x,+y+1/2,-z+1/2 
    -104 +x,+y+1/2,-z+1/2 
     201 +x+1/2,+y,+z+1/2 
     202 -x+1/2,+y,+z+1/2 
     203 +x+1/2,-y,+z+1/2 
     204 -x+1/2,-y,+z+1/2 
    -201 -x+1/2,-y,-z+1/2 
    -202 +x+1/2,-y,-z+1/2 
    -203 -x+1/2,+y,-z+1/2 
    -204 +x+1/2,+y,-z+1/2 
     301 +x+1/2,+y+1/2,+z 
     302 -x+1/2,+y+1/2,+z 
     303 +x+1/2,-y+1/2,+z 
     304 -x+1/2,-y+1/2,+z 
    -301 -x+1/2,-y+1/2,-z 
    -302 +x+1/2,-y+1/2,-z 
    -303 -x+1/2,+y+1/2,-z 
    -304 +x+1/2,+y+1/2,-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
O 
O1      0.34583(29)  0.09189(23)  0.2422(5)    1.0        Uiso   0.025        32
O 
O2      0.44022(15)  0.1151(5)    0.3433(5)    1.0        Uiso   0.025        32
O 
O3      0.4001(4)    0.25         0.25         1.0        Uiso   0.025        16
O 
O4      0.33830(28)  0.1896(5)    0.40197(25)  1.0        Uiso   0.025        32
O 
O5      0.25         0.25         0.0          1.0        Uiso   0.025         8
O 
O6      0.2662(4)    0.41678(20)  0.0          1.0        Uiso   0.025        16
O 
O7      0.5          0.1723(4)    0.5          1.0        Uiso   0.025         8
O 
O8      0.5          0.0          0.5527(11)   1.0        Uiso   0.025         8
O 
O9      0.3235(4)    0.5          0.40464(24)  1.0        Uiso   0.025        16
O 
O10     0.25         0.5          0.25         1.0        Uiso   0.025         8
Si
T1      0.37621(27)  0.1639(4)    0.3080(5)    1.0        Uiso   0.025        32
Si
T2      0.30004(31)  0.3252(4)    0.0          1.0        Uiso   0.025        16
Si
T3      0.5          0.1032(4)    0.5933(6)    1.0        Uiso   0.025        16
Si
T4      0.31775(25)  0.5          0.2876(5)    1.0        Uiso   0.025        16
Si
T5      0.2802(5)    0.5          0.5          1.0        Uiso   0.025         8
 
_chemical_formula_sum                  "O22 Si11"
_cell_formula_units_Z                  8


_diffrn_radiation_probe                x-ray
_diffrn_radiation_polarisn_ratio       0.95
_diffrn_radiation_wavelength           0.504934
_pd_proc_ls_prof_R_factor              0.0607
_pd_proc_ls_prof_wR_factor             0.0912
_pd_proc_ls_prof_wR_expected           0.0385
_refine_ls_R_Fsqd_factor               0.05641


_pd_proc_ls_background_function
;   GSAS Background function number 1 with 20 terms.
 Shifted Chebyshev function of 1st kind
      1:    226.029     2:   -100.731     3:   -6.90582     4:    11.3554    
      5:   -13.3957     6:   -6.29712     7:    41.8685     8:   -18.7660    
      9:   -15.5347    10:    18.3154    11:   -12.3803    12:    1.24864    
     13:    5.86324    14:   -9.72239    15:    3.94252    16:    3.87432    
     17:   -9.85962    18:    4.49488    19:   -2.54192    20:   -3.09971    
;

_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 Debye-Scherrer absorption correction
Term (= MU.r/wave) =      2.4207    
Correction is not refined.
;
_exptl_absorpt_correction_T_min        0.14037
_exptl_absorpt_correction_T_max        0.14798

_pd_proc_ls_profile_function
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =  387.238 #2(GV)   =  -35.226 #3(GW)   =    1.041
 #4(GP)   =    0.192 #5(LX)   =    1.374 #6(LY)   =    0.119
 #7(S/L)  =   0.0012 #8(H/L)  =   0.0024
 #9(trns) =     0.00 #10(shft)=   0.0000
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.096 #15(L22) =    0.287 #16(L33) =    0.174
 #17(L12) =    0.000 #18(L13) =    0.000 #19(L23) =    0.000
 Peak tails are ignored  where the intensity is below 0.0010 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff 0.00100
_pd_proc_info_datetime                 2016-01-06T13:43:33
_pd_calc_method                        "Rietveld Refinement"

_pd_meas_2theta_range_min              1.0
_pd_meas_2theta_range_max              50.149
_pd_meas_2theta_range_inc              0.003
_pd_proc_2theta_range_min              0.995558
_pd_proc_2theta_range_max              50.14456
_pd_proc_2theta_range_inc              0.003
_pd_meas_number_of_points              16384
_pd_proc_number_of_points              16384
_reflns_number_total                   734
_reflns_limit_h_min                    0
_reflns_limit_h_max                    23
_reflns_limit_k_min                    0
_reflns_limit_k_max                    15
_reflns_limit_l_min                    0
_reflns_limit_l_max                    14
_reflns_d_resolution_high              0.974
_reflns_d_resolution_low               11.053
#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
