 
data_PRSHPBI3_beta
 
_audit_creation_method              TOPAS_Academic
_publ_contact_author               'Masciocchi, Norberto'
_publ_contact_author_email          norberto.masciocchi@uninsubra.it
_journal_name_full                 ?




#==============================================================================
 
# CHEMICAL DATA
 
_chemical_name_systematic
;
(Protonated proton sponge) triiodoplumbate, beta phase

;
_chemical_formula_sum             'C14 H19 I3 N2 Pb'
_chemical_formula_weight          803.23
_chemical_name_common  '(Protonated proton sponge) triiodoplumbate, beta phase'
_chemical_melting_point           ?
_chemical_formula_moiety          ?

 
#==============================================================================
 
# POWDER SPECIMEN AND CRYSTAL DATA

loop_
 _atom_type_symbol
 _atom_type_description

 _atom_type_scat_source
 'C'  'C'    
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'    
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'   
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'    
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'   
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            'Orthorhombic'
_symmetry_space_group_name_H-M    'Pca21'

 
loop_
	_symmetry_equiv_pos_as_xyz
	 'x, y, z '
	 '-x+1/2, y, z+1/2 '
	 '-x, -y, z+1/2 '
	 'x+1/2, -y, z '
 
_cell_length_a 25.0530(12)
_cell_length_b 10.4016(5)
_cell_length_c 8.0082(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2086.86(16)

_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

 
#==============================================================================
 
_pd_calibration_special_details      
; ?
;
_cell_special_details
; ?
;

_exptl_crystal_density_diffrn     2.556
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1432

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial               15      # perpendicular to 
                                          # equatorial plane

_pd_spec_size_equat               20      # parallel to 
                                          # scattering vector 
                                          # in transmission

_pd_spec_size_thick               0.05    # 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             'light yellow'       # use ICDD colour descriptions



# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu     49.98 #mm-1
_exptl_absorpt_correction_type    'none'        
_exptl_absorpt_correction_T_min   ?        
_exptl_absorpt_correction_T_max   ?        

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

# 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      298                    
_diffrn_source_target            Cu                                     
_diffrn_source_type              'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Advance'       
_diffrn_detector_type            'Bruker AXS Lynxeye linear PSD'        
_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  'Cu K\a'                 
    _diffrn_radiation_wavelength   1.5418          
 #      CuK\a~1~ 1.54056
 #      CuK\a~2~ 1.54439
_diffrn_radiation_monochromator   'Nickel filter'                

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

_pd_meas_number_of_points       5051                                     
_pd_meas_2theta_range_min          4                   
_pd_meas_2theta_range_max        105                   
_pd_meas_2theta_range_inc          0.02

# 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        ?
_computing_cell_refinement        
;
 TOPAS-R v. 3.0, Bruker AXS, 2005, Karlsruhe, Germany
;
_computing_data_reduction         ?
_computing_structure_solution     
;
 TOPAS-R v. 3.0, Bruker AXS, 2005, Karlsruhe, Germany
;
_computing_structure_refinement   
;
 TOPAS-Academic A.A.Coelho
;
_computing_molecular_graphics     ?
_computing_publication_material   ?

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

# REFINEMENT DATA

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

_pd_proc_ls_special_details

;   

Rotate_about_points(60, N2, C12, "H10 H11 H12")
Rotate_about_points(70, N1, C13, "H13 H14 H15")
Rotate_about_points(70, N1, C14, "H16 H17 H18")
Rotate_about_axies (@ -140.20476`_0.58472,  @ -215.20268`_0.64512 ,  22.64414 )
Translate(@  0.45746`_0.00099,  @  -0.20369`_0.00149,  @   0.29591`_0.00379)   

      
for the rigid body described by:
	
rigid
prm !cn  1.50
prm !cc  1.39
z_matrix C1 
z_matrix C2  C1  =cc;
z_matrix C3  C2  =cc; C1  120 
z_matrix C4  C3  =cc; C2  120 C1 0
z_matrix C5  C4  =cc; C3  120 C2 0
z_matrix C6  C5  =cc; C4  120 C3 0
z_matrix C7  C1  =cc; C2  120 C5 180
z_matrix C8  C7  =cc; C1  120 C2 0
z_matrix C9  C8  =cc; C7  120 C1 0
z_matrix C10 C9  =cc; C8  120 C7 0
z_matrix H1  C10 0.95 C2  120 C8 180
z_matrix H2  C9  0.95 C10 120 H1 0
z_matrix H3  C8  0.95 C9  120 H2 0
z_matrix H4  C5  0.95 C6  120 C1 180
z_matrix H5  C4  0.95 C5  120 H4 0
z_matrix H6  C3  0.95 C4  120 H5 0
z_matrix N1  C7  =cn-0.04; C1  120 C6 0
z_matrix N2  C6  =cn-0.04; C1  120 C7 0
z_matrix C11 N2  =cn; C1  120 C5 60
z_matrix C12 N2  =cn; C1  120 C5 -60
z_matrix C13 N1  =cn; C1  120 C8 60
z_matrix C14 N1  =cn; C1  120 C8 -60
z_matrix H7  C11 0.95 N2  110 C6 -30
z_matrix H8  C11 0.95 N2  110 C6 120
z_matrix H9  C11 0.95 N2  110 C6 210
z_matrix H10 C12 0.95 N2  110 C6 -30
z_matrix H11 C12 0.95 N2  110 C6 120
z_matrix H12 C12 0.95 N2  110 C6 210
z_matrix H13 C13 0.95 N1  110 C7 -30
z_matrix H14 C13 0.95 N1  110 C7 120
z_matrix H15 C13 0.95 N1  110 C7 210
z_matrix H16 C14 0.95 N1  110 C7 -30
z_matrix H17 C14 0.95 N1  110 C7 120
z_matrix H18 C14 0.95 N1  110 C7 210
z_matrix H19 N1  1.25 C7  110 C1 0 
;
 
# The next three items are given as text
_pd_proc_ls_profile_function      'fundamental parameters approach'  
_pd_proc_ls_background_function   'Chebychev polynomial'     
_pd_proc_ls_pref_orient_corr      ?
_pd_proc_ls_prof_R_factor         0.070         
_pd_proc_ls_prof_wR_factor        0.102         
_pd_proc_ls_prof_wR_expected      0.009        

_refine_special_details
; ?
;

_refine_ls_structure_factor_coef     Inet
_refine_ls_matrix_type               fullcycle
_refine_ls_weighting_scheme          ?   # '1/[Y~i~]'
_refine_ls_hydrogen_treatment        ?
_refine_ls_extinction_method         none        
_refine_ls_extinction_coef           ?           
_refine_ls_number_parameters         46
_refine_ls_number_restraints         0
_refine_ls_number_constraints        ?
# The following item is 'CHI squared'
_refine_ls_goodness_of_fit_all       12.0

_refine_ls_restrained_S_all          ?           
_refine_ls_restrained_S_obs          ?
_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          6             
_pd_proc_2theta_range_max        105             
_pd_proc_2theta_range_inc          0.02

loop_
      _pd_proc_wavelength       1.540562    1.544390   

_pd_block_diffractogram_id        ?            # The id used for the block
                                               # containing the powder 
                                               # pattern profile (section 11).

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

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


 
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Pb Pb   4 0.2536(5)   0.2970(5)  0        1 2.21(11)
I1 I    4 0.1482(3)   0.2862(8) -0.232(3) 1 2.21(11)
I2 I    4 0.3052(3)   0.5068(8) -0.258(3) 1 2.21(11)
I3 I    4 0.2891(3)   0.0746(7) -0.251(4) 1 2.21(11)
C1 C    4 0.4575(10) -0.2037(15) 0.296(4) 1 2.21(11)
C2 C    4 0.4211(11) -0.1475(19) 0.405(4) 1 2.21(11)
C3 C    4 0.3667(10) -0.156(2)   0.373(5) 1 2.21(11)
C4 C    4 0.3486(10) -0.2204(19) 0.232(5) 1 2.21(11)
C5 C    4 0.3850(11) -0.2765(16) 0.123(5) 1 2.21(11)
C6 C    4 0.4394(11) -0.2682(17) 0.155(4) 1 2.21(11)
C7 C    4 0.5119(10) -0.1954(16) 0.328(4) 1 2.21(11)
C8 C    4 0.5299(11) -0.1309(16) 0.469(5) 1 2.21(11)
C9 C    4 0.4936(14) -0.075(2)   0.578(4) 1 2.21(11)
C10 C   4 0.4392(13) -0.083(2)   0.546(4) 1 2.21(11)
N1 N    4 0.5501(10) -0.254(2)   0.214(5) 1 2.21(11)
N2 N    4 0.4776(13) -0.327(2)   0.040(4) 1 2.21(11)
C11 C   4 0.4604(17) -0.277(3)  -0.127(4) 1 2.21(11)
C12 C   4 0.4563(14) -0.461(2)   0.020(5) 1 2.21(11)
C13 C   4 0.5850(11) -0.332(2)   0.328(6) 1 2.21(11)
C14 C   4 0.5890(11) -0.148(3)   0.181(6) 1 2.21(11)
H1 H    4 0.4143(15) -0.045(3)   0.620(4) 1 2.21(11)
H2 H    4 0.5059(16) -0.031(2)   0.675(5) 1 2.21(11)
H3 H    4 0.5671(12) -0.1252(17) 0.491(6) 1 2.21(11)
H4 H    4 0.3726(13) -0.3206(18) 0.026(5) 1 2.21(11)
H5 H    4 0.3114(10) -0.226(2)   0.210(6) 1 2.21(11)
H6 H    4 0.3419(11) -0.117(3)   0.447(5) 1 2.21(11)
H7 H    4 0.4230(17) -0.262(3)  -0.127(4) 1 2.21(11)
H8 H    4 0.4783(18) -0.199(4)  -0.151(4) 1 2.21(11)
H9 H    4 0.469(2)   -0.338(4)  -0.211(4) 1 2.21(11)
H10 H   4 0.4186(14) -0.461(2)   0.032(5) 1 2.21(11)
H11 H   4 0.4652(16) -0.493(3)  -0.087(5) 1 2.21(11)
H12 H   4 0.4714(13) -0.516(2)   0.102(5) 1 2.21(11)
H13 H   4 0.5639(12) -0.3718(17) 0.412(5) 1 2.21(11)
H14 H   4 0.6031(11) -0.396(3)   0.266(6) 1 2.21(11)
H15 H   4 0.6106(11) -0.278(2)   0.380(6) 1 2.21(11)
H16 H   4 0.5958(10) -0.102(3)   0.281(6) 1 2.21(11)
H17 H   4 0.6216(11) -0.182(4)   0.140(7) 1 2.21(11)
H18 H   4 0.5748(13) -0.090(3)   0.100(6) 1 2.21(11)
H19 H   4 0.5259(12) -0.307(3)   0.096(4) 1 2.21(11)
