 
######################################################################
data_marchettiite

# phase info for marchettiite follows
_pd_phase_name  marchettiite
_cell_measurement_temperature  298
_cell_length_a  3.6533(2)
_cell_length_b  10.2046(7)
_cell_length_c  10.5837(7)
_cell_angle_alpha  113.809(5)
_cell_angle_beta   91.313(8)
_cell_angle_gamma  92.44(1)
_cell_volume  360.312
_exptl_crystal_density_diffrn  1.7065
_symmetry_cell_setting  triclinic
_symmetry_space_group_name_H-M  "P -1"
loop_
    _space_group_symop_id
    _space_group_symop_operation_xyz
     1  x,y,z
     2  -x,-y,-z

_pd_spec_size_axial                      0.1
_pd_spec_size_equat                      0.1
_pd_spec_size_thick                      0.1
_pd_spec_mounting        'borosilicate glass fiber'
_pd_spec_mount_mode                  'transmission'
_pd_spec_shape                         'irregular'
_pd_char_particle_morphology        'needle'
_pd_char_colour                        'pink'
_pd_prep_cool_rate                       ?
_pd_prep_pressure                      'ambient'
_pd_prep_temperature                     'ambient'

_exptl_absorpt_coefficient_mu            ?
_exptl_absorpt_correction_type          'none'
_diffrn_ambient_temperature              298
_diffrn_source                      'microfocus X-ray tube'
_diffrn_source_target                    Mo
_diffrn_source_type                      ?
_diffrn_radiation_type  'Mo K\a~1,2~'
loop_
   _diffrn_radiation_wavelength
   _diffrn_radiation_wavelength_wt
   _diffrn_radiation_wavelength_id
  0.70926         1.0             1     
  0.71354         0.5000          2     
_refine_ls_R_F_factor        0.13003
_refine_ls_R_Fsqd_factor     0.14753
_pd_proc_ls_prof_R_factor     0.03242
_pd_proc_ls_prof_wR_factor    0.04515
_gsas_proc_ls_prof_R_B_factor   0.04475
_gsas_proc_ls_prof_wR_B_factor  0.05853
_pd_proc_ls_prof_wR_expected  0.49364
_diffrn_radiation_probe  x-ray
_diffrn_radiation_polarisn_ratio  0.7000
_pd_proc_ls_background_function
;
Background function: "chebyschev" function with 20 terms:
    2.714, -3.778, 4.290, -1.997, -33.974, 72.644, 393.575, -726.087, 
    -2154.532, 3392.954, 6456.271, -8917.277, -11267.191, 13929.380, 
    11408.182, -12806.036, -6209.021, 6392.748, 1404.058, -1335.760, 
;

_diffrn_radiation_monochromator         'Mirror'
_diffrn_measurement_device            diffractometer
_diffrn_measurement_device_type   'Rigaku Oxford diffraction Supernova'
_diffrn_detector                       'area detector'
_diffrn_detector_type              'Dectris Pilatus'

_pd_meas_scan_method                     ?
_pd_meas_special_details
; total 2theta range 0.000--58.400, 5841 points.
;
_pd_meas_number_of_points                2727
_pd_meas_2theta_range_min                3.2
_pd_meas_2theta_range_max                30.4593
_pd_meas_2theta_range_inc                0.01


_pd_proc_info_datetime  2022-01-10T09:01
_pd_calc_method  "Rietveld Refinement"
_computing_structure_refinement
   "GSAS-II (Toby & Von Dreele, J. Appl. Cryst. 46, 544-549, 2013)"
_refine_ls_matrix_type  full
_refine_ls_number_parameters  14
_refine_ls_goodness_of_fit_all  0.092
_refine_ls_shift/su_max  2.4649

# OVERALL WEIGHTED R-FACTOR
_refine_ls_wR_factor_obs  0.04515

_pd_proc_ls_pref_orient_corr
;
none  
;
_pd_proc_ls_profile_function
;
Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L:
  peak variance(Gauss) = Utan(Th)^2^+Vtan(Th)+W:
  peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L
  U, V, W in (centideg)^2^, X & Y in centideg
    1400.000, 179.799, 118(14), -8.5(21), 162(17), 0.002, 

;


# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_ 
   _atom_site_label
   _atom_site_type_symbol
   _atom_site_fract_x
   _atom_site_fract_y
   _atom_site_fract_z
   _atom_site_occupancy
   _atom_site_adp_type
   _atom_site_U_iso_or_equiv
   _atom_site_site_symmetry_multiplicity
N1     N    0.55789     0.58386     0.40871     1.0000     Uiso 0.0560     2   
H1     H    0.59426     0.49790     0.43794     1.0000     Uiso 0.0560     2   
C2     C    0.67493     0.72269     0.49831     1.0000     Uiso 0.0560     2   
N3     N    0.62782     0.83669     0.46061     1.0000     Uiso 0.0560     2   
C4     C    0.46448     0.81041     0.33286     1.0000     Uiso 0.0560     2   
C5     C    0.34998     0.67958     0.24473     1.0000     Uiso 0.0560     2   
C6     C    0.39346     0.55738     0.28083     1.0000     Uiso 0.0560     2   
N7     N    0.19685     0.67857     0.12451     1.0000     Uiso 0.0560     2   
H7     H    0.08346     0.59126     0.03662     1.0000     Uiso 0.0560     2   
C8     C    0.23343     0.82367     0.15137     1.0000     Uiso 0.0560     2   
N9     N    0.39837     0.91021     0.27963     1.0000     Uiso 0.0560     2   
H9     H    0.45782     1.02205     0.32472     1.0000     Uiso 0.0560     2   
O8     O    0.13004     0.87108     0.06961     1.0000     Uiso 0.0560     2   
O6     O    0.28990     0.43711     0.20195     1.0000     Uiso 0.0560     2   
O2     O    0.81826     0.74422     0.60963     1.0000     Uiso 0.0560     2   
N10    N    0.13918     0.84428     0.84885     1.0000     Uiso 0.0756     2   
H14    H    0.02436     0.93942     0.90257     1.0000     Uiso 0.0756     2   
H13    H    0.40986     0.85409     0.83484     1.0000     Uiso 0.0756     2   
H11    H    0.02700     0.78947     0.75267     1.0000     Uiso 0.0756     2   
H12    H    0.11992     0.77418     0.89408     1.0000     Uiso 0.0756     2   

# RIGID BODY DETAILS
loop_
    _restr_rigid_body_class.class_id
    _restr_rigid_body_class.details
  1
;
GSAS-II residue rigid body "UA:1" with 17 atoms
  Site symmetry @ origin: 1, multiplicity: 2
    At name       x          y          z
         C     3.2361     0.0038     0.0009
         N     2.4931    -1.1711     0.0014
         N     2.4801     1.1715    -0.0000
         C     1.2160    -0.6638     0.0002
         C     1.2031     0.6616    -0.0005
         C    -0.0366    -1.4096    -0.0015
         N    -1.2160    -0.6827     0.0009
         N     0.0247     1.3856    -0.0011
         C    -1.1883     0.7079     0.0019
         O     4.4461     0.0112     0.0015
         O    -2.2261     1.3296     0.0048
         O    -0.0463    -2.6199    -0.0043
         H     2.8121    -2.1765     0.0024
         H     2.7921     2.1787    -0.0000
         H    -2.1390    -1.1905     0.0027
         B     2.1251     0.0000     0.0000
         A     0.0000     0.0000     0.0000
  Orientation defined by: A -> B & A -> N

 Location:
  names :       Pos x       Pos y       Pos z       Ori a       Ori i       Ori j       Ori k        Frac
  values:     0.51148     0.69843     0.37105     0.50252     0.30141     0.78534     0.21515     1.00000
  esds  :     0.00160     0.00123     0.00093                 0.00299     0.00272     0.00197            
 Thermal motion:
  names :        Uiso
  values:     0.05599
  esds  :     0.00227
;
  2
;
GSAS-II residue rigid body "NH4:0" with 5 atoms
  Site symmetry @ origin: 1, multiplicity: 2
    At name       x          y          z
         N     0.0000     0.0000     0.0000
         H     1.0093    -0.0000    -0.0000
         H    -0.2532     0.9775     0.0000
         H    -0.2534    -0.3265    -0.9216
         H    -0.4162    -0.5380     0.7609
  Orientation defined by: N -> H & N -> H

 Location:
  names :       Pos x       Pos y       Pos z       Ori a       Ori i       Ori j       Ori k        Frac
  values:     0.13918     0.84428     0.84885     0.00000     0.56596    -0.12823    -0.81440     1.00000
  esds  :     0.00739     0.00290     0.00286                                                            
 Thermal motion:
  names :        Uiso
  values:     0.07560
  esds  :
;
loop_
    _restr_rigid_body.id
    _restr_rigid_body.atom_site_label
    _restr_rigid_body.site_symmetry
    _restr_rigid_body.class_id
    _restr_rigid_body.details
       1 C8      1_555   1 ?
       2 N7      1_555   1 ?
       3 N9      1_555   1 ?
       4 C5      1_555   1 ?
       5 C4      1_555   1 ?
       6 C6      1_555   1 ?
       7 N1      1_555   1 ?
       8 N3      1_555   1 ?
       9 C2      1_555   1 ?
      10 O8      1_555   1 ?
      11 O2      1_555   1 ?
      12 O6      1_555   1 ?
      13 H7      1_555   1 ?
      14 H9      1_555   1 ?
      15 H1      1_555   1 ?
      16 B26     1_555   1 ?
      17 B25     1_555   1 ?
      18 N10     1_555   2 ?
      19 H11     1_555   2 ?
      20 H12     1_555   2 ?
      21 H13     1_555   2 ?
      22 H14     1_555   2 ?


loop_  _atom_type_symbol _atom_type_number_in_cell
  C       10
  H       14
  B       0
  N       10
  O       6

# Note that Z affects _cell_formula_sum and _weight
_cell_formula_units_Z  2
_chemical_formula_sum  "C5 H7 B0 N5 O3"
_chemical_formula_weight  185.14

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
  N1     C2     1.39081      1_555    1_555 yes
  N1     C6     1.38543      1_555    1_555 yes
  H1     N1     1.05349      1_555    1_555 yes
  C2     N1     1.39081      1_555    1_555 yes
  C2     N3     1.38948      1_555    1_555 yes
  C2     O2     1.20978      1_555    1_555 yes
  N3     C2     1.38948      1_555    1_555 yes
  N3     C4     1.38302      1_555    1_555 yes
  C4     N3     1.38302      1_555    1_555 yes
  C4     C5     1.32537      1_555    1_555 yes
  C4     N9     1.37505      1_555    1_555 yes
  C5     C4     1.32537      1_555    1_555 yes
  C5     C6     1.45781      1_555    1_555 yes
  C5     N7     1.37416      1_555    1_555 yes
  C6     N1     1.38543      1_555    1_555 yes
  C6     C5     1.45781      1_555    1_555 yes
  C6     O6     1.21038      1_555    1_555 yes
  N7     C5     1.37416      1_555    1_555 yes
  N7     C8     1.39012      1_555    1_555 yes
  H7     N7     1.05475      1_555    1_555 yes
  C8     N7     1.39012      1_555    1_555 yes
  C8     N9     1.39108      1_555    1_555 yes
  C8     O8     1.21002      1_555    1_555 yes
  N9     C4     1.37505      1_555    1_555 yes
  N9     C8     1.39108      1_555    1_555 yes
  O8     C8     1.21002      1_555    1_555 yes
  O6     C6     1.21038      1_555    1_555 yes
  O2     C2     1.20978      1_555    1_555 yes

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
  C2     N1     C6     120.507       1_555  1_555    1_555 yes
  N1     C2     N3     120.331       1_555  1_555    1_555 yes
  N1     C2     O2     119.786       1_555  1_555    1_555 yes
  N3     C2     O2     119.882       1_555  1_555    1_555 yes
  C2     N3     C4     119.242       1_555  1_555    1_555 yes
  N3     C4     C5     122.126       1_555  1_555    1_555 yes
  N3     C4     N9     126.664       1_555  1_555    1_555 yes
  C5     C4     N9     111.21        1_555  1_555    1_555 yes
  C4     C5     C6     120.213       1_555  1_555    1_555 yes
  C4     C5     N7     112.225       1_555  1_555    1_555 yes
  C6     C5     N7     127.562       1_555  1_555    1_555 yes
  N1     C6     C5     117.581       1_555  1_555    1_555 yes
  N1     C6     O6     121.186       1_555  1_555    1_555 yes
  C5     C6     O6     121.233       1_555  1_555    1_555 yes
  C5     N7     C8     100.643       1_555  1_555    1_555 yes
  H7     N7     C8     130.085       1_555  1_555    1_555 yes
  N7     C8     N9     114.771       1_555  1_555    1_555 yes
  N7     C8     O8     122.66        1_555  1_555    1_555 yes
  N9     C8     O8     122.57        1_555  1_555    1_555 yes
  C4     N9     C8     101.151       1_555  1_555    1_555 yes
  C4     N9     H9     128.979       1_555  1_555    1_555 yes
  C8     N9     H9     129.869       1_555  1_555    1_555 yes

# start Validation Reply Form
_vrf_PLAT080_marchettiite
;
PROBLEM: Maximum Shift/Error ............................       2.46 Why ? 
RESPONSE: The data has low resolution and high peak overlap, 
preventing the refinement to reach full convergence.
;

_vrf_PLAT417_marchettiite
;
PROBLEM: Short Inter D-H..H-D       H1       ..H1       .       1.48 Ang.  
RESPONSE: The structure model is approximate as 
the available data has low resolution and high peak overlap,
and does not allow a full Rietveld refinement.
;
_vrf_SHFSU01_marchettiite
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: The data has low resolution and high peak overlap, 
preventing the refinement to reach full convergence.
;
# end Validation Reply Form

