
data_NMPDI
_audit_creation_method              TOPAS_Academic
_publ_contact_author               'Masciocchi, Norberto'
_publ_contact_author_email          norberto.masciocchi@uninsubra.it
_journal_name_full                 'Journal of Materials Chemistry C'


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

# CHEMICAL DATA
 
_chemical_name_systematic
;
1,4,5,8-Naphthalenetetracarboxylic m-aminophenylenedimide

;
_chemical_formula_sum             'C26 H16 N4 O4'
_chemical_formula_weight          448.43 
_chemical_name_common  '1,4,5,8-Naphthalenetetracarboxylic m-aminophenylenedimide'
_chemical_melting_point           ?
_chemical_formula_moiety          'C26 H16 N4 O4'

 
#==============================================================================
# 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'
 'N'  'N'   
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'    
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting            'Orthorhombic'
_symmetry_space_group_name_H-M    'Pbca'

_chemical_name_mineral ?
_cell_length_a 32.012(9)
_cell_length_b 8.5412(8)
_cell_length_c 7.4427(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2035.0(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

loop_
	_symmetry_equiv_pos_as_xyz
	 'x, y, z '
	 '-x, y+1/2, -z+1/2 '
	 '-x+1/2, -y, z+1/2 '
	 '-x+1/2, y+1/2, z '
	 'x, -y+1/2, z+1/2 '
	 '-x, -y, -z '
	 'x+1/2, -y+1/2, -z '
	 'x+1/2, y, -z+1/2 '

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

_exptl_crystal_density_diffrn     1.464
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              ?

# 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               0.02    # 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 'unknown'                      
_pd_char_colour             'brown'       # use ICDD colour descriptions



# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu     0.84 #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      293                    
_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       5001                                     
_pd_meas_2theta_range_min          5                   
_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(@ -51.08653`_10.80054 val_on_continue = Val + Rand(-60,60);, C10 , N2 , " H10 H11")
Rotate_about_points(@ -133.68871`_42.65313 val_on_continue = Val + Rand(-60,60);, C10 , N3 , " H12 H13")
Rotate_about_points(@  -78.40656`_0.33450 val_on_continue = Val + Rand(-60,60);, C8 , N1 , " C9 C10 C11 C12 C13 N2 H6 H7 H8 H9 H10 H11 N3 H12 H13 H14")       
Rotate_about_axies (@ -38.47910`_0.09877, @  128.28671`_0.06246 , @  141.17747`_0.10204)
Translate(0.5, 0.5, 0.5)
      
for the rigid body described by:
	
rigid             
     

z_matrix H
z_matrix C1   H   0.70
z_matrix C2   C1  1.40   H  120
z_matrix C3   C2  1.40   C1 120   H   0
z_matrix H3   C3  0.95   C2 120   C1 180
z_matrix C4   C1  1.40   C2 120   C3 180
z_matrix C5   C4  1.40   C1 120   C2 180
z_matrix H5   C5  0.95   C4 120   C1 180
z_matrix C6   C2  1.48   C1 120   H  180
z_matrix C7   C4  1.48   C1 120   H  180
z_matrix O1   C6  1.21   C2 120   C1 180
z_matrix O2   C7  1.21   C4 120   C1 180
z_matrix N1   C6  1.40   C2 120   C1   0
z_matrix C8   N1  1.43   C6 120   C2 180
z_matrix C9   C8  1.39   N1 120   C6 180
z_matrix C10  C9  1.39   C8 120   N1 180
z_matrix C11  C10 1.39   C9 120   C8   0
z_matrix C12  C11 1.39   C10 120  C9   0
z_matrix C13  C12 1.39   C11 120  C10  0
z_matrix N2   C10 1.39   C9  120  C8 180
z_matrix H6   C9  0.95   C8  120  N1   0 
z_matrix H7   C11 0.95   C10 120  C9  180  
z_matrix H8   C12 0.95   C11 120  C10 180  
z_matrix H9   C13 0.95   C12 120  C8 180  
z_matrix H10   N2 0.95   C10 109.5 C9 60 
z_matrix H11   N2 0.95   C10 109.5 C9 180  
z_matrix N3   C12 1.39   C11 120  C10 180
z_matrix H12   N3 0.95   C11 109.5 C10  60 
z_matrix H13   N3 0.95   C11 109.5 C10 180  
z_matrix H14   C10 0.95  C9 120    C8  180  
;
 
# 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         0.072         
_pd_proc_ls_prof_wR_factor        0.102         
_pd_proc_ls_prof_wR_expected      0.008        

_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         32
_refine_ls_number_restraints         0
_refine_ls_number_constraints        ?
# The following item is 'CHI squared'
_refine_ls_goodness_of_fit_all       12.6

_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          5             
_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
H H   4 0.5 0.5 0.5 0 5.9(3) # Center of Mass
C1 C   8 0.481002(11) 0.49184(18) 0.45438(9) 1 5.9(3)
C2 C   8 0.48029(6) 0.4285(3) 0.28090(12) 1 5.9(3)
C3 C   8 0.51757(8) 0.3816(3) 0.19865(17) 1 5.9(3)
H3 H   8 0.51708(11) 0.3386(4) 0.0809(2) 1 5.9(3)
C4 C   8 0.44372(2) 0.5388(5) 0.5366(3) 1 5.9(3)
C5 C   8 0.44444(6) 0.6021(4) 0.7101(3) 1 5.9(3)
H5 H   8 0.41914(8) 0.6340(6) 0.7659(4) 1 5.9(3)
C6 C   8 0.44012(8) 0.4113(7) 0.1844(3) 1 5.9(3)
C7 C   8 0.40355(2) 0.5216(8) 0.4402(4) 1 5.9(3)
O1 O   8 0.43950(12) 0.3566(8) 0.0345(3) 1 5.9(3)
O2 O   8 0.37133(4) 0.5622(11) 0.5113(6) 1 5.9(3)
N1 N   8 0.40284(6) 0.4583(9) 0.2667(4) 1 5.9(3)
C8 C   8 0.36403(8) 0.4416(13) 0.1735(6) 1 5.9(3)
C9 C   8 0.34558(17) 0.5710(15) 0.0926(11) 1 5.9(3)
C10 C   8 0.30786(18) 0.5548(19) 0.0020(12) 1 5.9(3)
C11 C   8 0.28858(12) 0.409(2) -0.0077(10) 1 5.9(3)
C12 C   8 0.30703(18) 0.2798(18) 0.0732(12) 1 5.9(3)
C13 C   8 0.34475(16) 0.2960(15) 0.1638(11) 1 5.9(3)
N2 N   8 0.2894(3) 0.684(2) -0.0788(19) 0.733(12) 5.9(3)
H6 H   8 0.3588(2) 0.6705(14) 0.0993(15) 1 5.9(3)
H7 H   8 0.26280(14) 0.398(2) -0.0696(11) 1 5.9(3)
H8 H   8 0.2939(3) 0.180(2) 0.0665(17) 0.733(12) 5.9(3)
H9 H   8 0.3574(2) 0.2076(14) 0.2190(15) 1 5.9(3)
H10 H   8 0.308(2) 0.770(6) -0.08(2) 0.733(12) 5.9(3)
H11 H   8 0.283(5) 0.660(7) -0.200(7) 0.733(12) 5.9(3)
N3 N   8 0.2878(3) 0.134(2) 0.0635(19) 0.267(12) 5.9(3)
H12 H   8 0.306(15) 0.085(4) -0.02(7) 0.267(12) 5.9(3)
H13 H   8 0.291(18) 0.087(14) 0.178(17) 0.267(12) 5.9(3)
H14 H   8 0.2952(3) 0.643(2) -0.0532(17) 0.267(12) 5.9(3)


