##############################################################################
### CIF submission form for results of Rietveld refinements (IUCr journals)###
###                                              Version 10 February 2005  ###
##############################################################################

# This is an electronic "form" for submitting the results of a Rietveld 
# refinement of a model against powder diffraction data to an
# IUCr journal as a Crystallographic Information File (CIF). Full details  
# of the CIF format are given in the paper "The Crystallographic Information 
# File (CIF): a New Standard Archive File for Crystallography" by S. R. Hall,
# F. H. Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. 
#
# The current version of the powder CIF dictionary, which contains definitions
# of the terms staring _pd_,  may be obtained from
# http://www.iucr.org/iucr-top/cif/pd/index.html. Other terms are defined in
# the core CIF dictionary at http://www.iucr.org/iucr-top/cif/core/index.html.
#
# Note that all fields should be numeric or character type EXCEPT those which
# are flagged as 'text' - free-form text of any length may be included in
# these latter fields provided the text block begins and ends with a semicolon
# as the first character of a new line.  Note also that the query marks
# '?' are significant as placeholders, and should not be deleted where a data
# item is not given, UNLESS the accompanying data name is also deleted.
# Lines should not exceed 80 characters in length.  The comments following
# a hash symbol '#' may be deleted if wished.
  
#=============================================================================
data_znvo
#=============================================================================

loop_
  _audit_conform_dict_name
  _audit_conform_dict_version
  _audit_conform_dict_location
     cif_core.dic .  ftp://ftp.iucr.org/pub/cif_core.dic
     cif_pd.dic .  ftp://ftp.iucr.org/pub/cif_pd.dic

# 1. SUBMISSION DETAILS

_publ_contact_author_name         'Dr Peter Y. Zavalij'
_publ_contact_author_address
;
      Materials Research Center
      State University of New York at Binghamton
      Binghamton, NY 13902-6016
      USA
;
_publ_contact_author_email        med@iucr.org
_publ_contact_author_fax          '607 777 4623'
_publ_contact_author_phone        '607 777 4623'

_publ_requested_journal           'Acta Cryst. C'
_publ_requested_category          FI

_publ_contact_letter
; Please consider this CIF submission for publication as a full paper in Acta
  Cryst. Section C. The figures, Transfer of Copyright Agreement form and
  powder profile will be sent on receipt of your acknowledgment letter.
;

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

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     97-04-14
_journal_date_to_coeditor         ?
_journal_date_from_coeditor       97-06-30
_journal_date_accepted            97-06-30
_journal_date_printers_first      97-09-18
_journal_date_printers_final      ?
_journal_date_proofs_out          97-10-06
_journal_date_proofs_in           97-10-14
_journal_coeditor_name            ?
_journal_coeditor_code            BR1188
_journal_coeditor_notes
; ?
;
_journal_techeditor_code          C970970
_journal_paper_category           FI
_iucr_compatibility_tag           ?
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM               ACSCEE
_journal_name_full                'Acta Crystallographica, Section C'
_journal_year                     1997 
_journal_volume                   C53
_journal_issue                    DEC97
_journal_page_first               1738 
_journal_page_last                1739
_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

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

# 3. TITLE AND AUTHOR LIST

_publ_section_title
;
Example CIF - Not for publication
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary. 

loop_
    _publ_author_name
    _publ_author_address
    'Zavalij, Peter Y.'
;     Materials Research Center
      State University of New York at Binghamton
      Binghamton, NY 13902-6016
      USA
;
    'Zhang, Fan'
;     Materials Research Center
      State University of New York at Binghamton
      Binghamton, NY 13902-6016
      USA
;
    'Whittingham, M. Stanley'
;     Materials Research Center
      State University of New York at Binghamton
      Binghamton, NY 13902-6016
      USA
;

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

# 4. TEXT

_publ_section_synopsis
;
Rietveld refinement of a new zinc divanadate, Zn₃(OH)₂V₂O₇.2H₂O, 
shows that it has a porous framework structure assembled from layers of 
Zn--O octahedra joined by pyrovanadate groups. Water molecules fill the 
large cavities.
;

_publ_section_abstract                           
; Hydrothermally prepared zinc dihydroxide divanadate dihydrate crystallizes 
in the trigonal system (space group P\=3m1). Its structure was solved ...
;

_publ_section_comment
; Recently, mild hydrothermal reactions driven by template cations
such as ...
;
_publ_section_exptl_prep     
; The title compound was prepared by hydrothermal treatment of ZnCl₂,
V₂O₅ and tetramethylammonium hydroxide, [N(CH₃)₄]OH, in a 1:1:3 
molar ratio at pH = 5.6. The reaction mixture was heated in a Teflon-lined 
Parr reactor for 2.5 d at 438 K. White crystalline powder resulted.
;

_publ_section_exptl_refinement  
;
The powder diffraction pattern was indexed in a hexagonal system ...
;
_publ_section_references   
;
Akselrud, L. G., Zavalij, P. Y., Grin, Yu. N., Pecharskii, V. K., 
Baumgartner, B. & Wolfel, E. (1993). Mater. Sci. Forum, 133/136, 335-340.

Basso, R., Palenzona, A. & Zefiro, L. (1988). Neues Jahrb. Miner. 
pp. 385-394.

...

;
_publ_section_figure_captions
; Fig. 1. Polyhedral representation of Zn₃(OH)₂V₂O₇.2H₂O.

Fig. 2. Comparison of observed (circles) and calculated (solid line) 
intensities for Zn₃(OH)₂V₂O₇.2H₂O. The difference pattern 
appears below.
;
_publ_section_acknowledgements
; The work at Binghamton was supported by the National Science Foundation
through grant DMR 9422667.
;

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

# If more than one structure is reported, sections 5-10 should be filled in
# per structure. For each data set, replace the '?' in the data_? line below
# by a unique identifier.

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

data_znvodata

# 5. CHEMICAL DATA

_chemical_name_systematic                           
;
zinc dihydroxide divanadate dihydrate
;
_chemical_name_common             ?
_chemical_formula_moiety          'H2 O9 V2 Zn3, 2(H2 O)'
_chemical_formula_structural      'Zn3 (O H)2 (V2 O7) (H2 O)2'
_chemical_formula_analytical      ?
_chemical_formula_iupac           'Zn3 (O H)2 V2 O7 ,2H2 O'  
_chemical_formula_sum             'H6 O11 V2 Zn3'
_chemical_formula_weight          480.05
_chemical_melting_point           ?
_chemical_compound_source         ?

loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    Zn Zn -1.612  .678 'International Tables for Crystallography (Vol. IV)'
    V V  .035 2.110 'International Tables for Crystallography (Vol. IV)'
    O O  .047  .032 'International Tables for Crystallography (Vol. IV)'
    H H  .000  .000 'International Tables for Crystallography (Vol. IV)'

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

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system             trigonal      
_space_group_name_H-M_alt               'P -3 m 1'
_space_group_name_Hall                  '-P 3 2"'

loop_                                            
    _symmetry_equiv_pos_site_id
    _symmetry_equiv_pos_as_xyz
    1    x,y,z
    2    -y,x-y,z
    3    -x+y,-x,z
    4    -y,-x,z
    5    -x+y,y,z
    6    x,x-y,z
    7    -x,-y,-z
    8    y,-x+y,-z
    9    x-y,x,-z
   10    y,x,-z
   11    x-y,-y,-z
   12    -x,-x+y,-z

_cell_length_a     6.05098(5)                
_cell_length_b     6.05098(5)                 
_cell_length_c     7.19498(9)                
_cell_angle_alpha  90.0                      
_cell_angle_beta   90.0                       
_cell_angle_gamma  120.0                     
_cell_volume       228.145(7)                
_cell_formula_units_Z     1                  
_cell_measurement_temperature     295        

_pd_calibration_special_details      
; ?
;
_cell_special_details
; ?
;

_exptl_crystal_density_diffrn     3.4937(1)
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000               230

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial               25       # perpendicular to 
                                           # equatorial plane

_pd_spec_size_equat               25       # parallel to 
                                           # scattering vector 
                                           # in transmission

_pd_spec_size_thick                1       # parallel to 
                                           # scattering vector 
                                           # in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                          
; packed powder pellet
;
_pd_spec_mount_mode         reflection    # options are 'reflection' 
                                          # or 'transmission'

_pd_spec_shape              flat_sheet    # options are 'cylinder',
                                          # 'flat_sheet' or 'irregular'
						       

_pd_char_particle_morphology      plate-like                      
_pd_char_colour              white        # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen. 
# 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            438        



# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu     27.4
_exptl_absorpt_correction_type    ?        
_exptl_absorpt_correction_T_min   ?        
_exptl_absorpt_correction_T_max   ?     

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

# 7. EXPERIMENTAL DATA

_exptl_special_details
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location
; ?
;

_diffrn_ambient_temperature     295                    
_diffrn_source              'sealed X-ray tube'        
_diffrn_source_target            Cu                                     
_diffrn_source_type               ?
_diffrn_measurement_device_type  'Scintag XDS2000'       
_diffrn_detector               'Ge solid-state'               
_diffrn_detector_type             ?        
_pd_meas_scan_method              step        # options are 'step', 'cont',
                                              # 'tof', 'fixed' or
                                              # 'disp' (= dispersive)
_pd_meas_special_details
;  ?
;

# The following six items are used for angular dispersive measurements only.

loop_
    _diffrn_radiation_type                   
    _diffrn_radiation_wavelength             
       CuK\a~1~ 1.54056
       CuK\a~2~ 1.54439
_diffrn_radiation_monochromator   none                 

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points       3667                                     
_pd_meas_2theta_range_min         10                   
_pd_meas_2theta_range_max        120                   
_pd_meas_2theta_range_inc          0.03

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec           ?                    
_pd_instr_dist_spec/detc          ?                    
_pd_meas_2theta_fixed             ?                    

# The following fields are used to identify the programs used.

_computing_data_collection        'DMS software (Scintag Inc., 1994)'
_computing_cell_refinement        'CSD (Akselrud et al., 1993)'
_computing_data_reduction         'CSD'
_computing_structure_solution     'CSD'
_computing_structure_refinement   'CSD'
_computing_molecular_graphics
   'STRUVIR [VRML version of STRUPLO (Fisher, 1985) created by A. LeBail]'
_computing_publication_material   'CSD'

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

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details
; ?
;

# The next three items are given as text
_pd_proc_ls_profile_function      pseudo-Voigt   
_pd_proc_ls_background_function   'square polynomial for each range'     
_pd_proc_ls_pref_orient_corr                      
; I~corr~ = I~obs~/[1 + (\t^2^-1)sin^2^\f]^1/2^, 
   axis (001), \t = 0.702(5), 
   (Pecharskii et al., 1987)
;

_pd_proc_ls_prof_R_factor         0.052          
_pd_proc_ls_prof_wR_factor        0.085         
_pd_proc_ls_prof_wR_expected      0.020         

_refine_special_details
; ?
;

_refine_ls_structure_factor_coef     Inet
_refine_ls_matrix_type               fullcycle
_refine_ls_weighting_scheme          sigma
_refine_ls_weighting_details          '1/[Yi+σ(Yi)]'
_refine_ls_hydrogen_treatment        noref
_refine_ls_extinction_method         none        
_refine_ls_extinction_coef           ?           
_refine_ls_number_parameters         18
_refine_ls_number_restraints         ?
_refine_ls_number_constraints        ?

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all       1.30      

_refine_ls_R_I_factor                 .053
_refine_ls_restrained_S_all          ?           
_refine_ls_shift/su_max               .01
_refine_ls_shift/su_mean             ?


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.
_pd_proc_2theta_range_min         10             
_pd_proc_2theta_range_max        120             
_pd_proc_2theta_range_inc          0.03

loop_
      _pd_proc_wavelength       1.540562    1.544390   

# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id      znvoprofile    

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions    ?             
_pd_proc_info_data_reduction      ?

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
    _atom_site_label               
    _atom_site_fract_x             
    _atom_site_fract_y             
    _atom_site_fract_z             
    _atom_site_U_iso_or_equiv      
    _atom_site_adp_type
    _atom_site_occupancy           
    _atom_site_type_symbol
    Zn  .5       0         0         .0210(5)  Uani 1     Zn
    V   0        0         .2525(2)  .0112(5)  Uani 1     V
    O1  .66667   .33333    .8823(7)  .011(2)   Uiso 1     O
    O2  .1534(3) .3068(6)  .8219(4)  .0141(11) Uiso 1     O
    O3  0        0         .5        .031(2)   Uiso 1     O 
    Ow  .736(2)  .3680(10) .491(2)   .012(3)   Uiso .3333 O
    H1  .66667   .33333    .75000    .07599    Uiso 1     H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Zn  .0198(6)  .0163(7)  .0256(7)  .0082(3)  .0009(10)  .002(2)
    V  .0144(7)  .0144(7)  .0049(8)  .0072(3) 0 0

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

# 10. MOLECULAR GEOMETRY

_geom_special_details             ?

loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Zn O1 1_554 1.941(2)    yes
    Zn O1 7_656 1.941(2)    yes
    Zn O2 2_654 2.226(2)    yes
    Zn O2 3_554 2.226(2)    yes
    Zn O2 8_556 2.226(2)    yes
    Zn O2 9_656 2.226(2)    yes
    V  O2 7_556 1.695(2)    yes
    V  O2 8_556 1.695(2)    yes
    V  O2 9_556 1.695(2)    yes
    V  O3 .     1.781(1)  yes
    O1 H1 .      .952       no

loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O2 V  O2 7_556 8_556 110.52(12) no
    O2 V  O2 7_556 9_556 110.52(12) no
    O2 V  O3 7_556 .     108.40(9)  no
    O2 V  O2 8_556 9_556 110.52(12) no
    O2 V  O3 8_556 .     108.40(9)  no
    O2 V  O3 9_556 .     108.40(9)  no
    V  O3 V  .     7_556 180.00(3)  no

loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    O1 H1 Ow   .  .95 1.90 2.84(2) 169

#==============================================================================
# Additional structures (sections 5-10 and associated data_? identifiers)
# may be added at this point.
#==============================================================================

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./                 





