data_FeBr2(3-cypy)4

_publ_contact_author_name            
'Dr Lothar Fink'   
_publ_contact_author_address             
;
Institute of Inorganic and Analytical Chemistry
Max-von-Laue-Str. 7
60438 Frankfurt am Main
Germany
;


_publ_contact_author_email           fink@chemie.uni-frankfurt.de
_publ_contact_author_fax             '+49 69 798 29235'
_publ_contact_author_phone           '+49 69 798 29123'

_publ_requested_journal              'CrystEngComm'

_publ_contact_letter
;
Please consider this CIF submission as supplementary material for a
manuscript intended for publication in Crystal Engineering Communications.
;


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


# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     ?

_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?

_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
    
_journal_coeditor_name            ?
_journal_coeditor_code            ?
_journal_coeditor_notes
; ?
;

_journal_techeditor_code          ?
_journal_techeditor_notes
; ?
;

_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?

_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

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


loop_
_publ_author_name
_publ_author_address

'Heine, Miriam'
;
Goethe Universität Frankfurt am Main
Institute of Inorganic and Analytical Chemistry
Max-von-Laue-Str. 7
60438 Frankfurt am Main
Germany
;

'Fink, Lothar'
;
Goethe Universität Frankfurt am Main
Institute of Inorganic and Analytical Chemistry
Max-von-Laue-Str. 7
60438 Frankfurt am Main
Germany
;

'Schmidt, Martin U.'
;
Goethe Universität Frankfurt am Main
Institute of Inorganic and Analytical Chemistry
Max-von-Laue-Str. 7
60438 Frankfurt am Main
Germany
;

_publ_section_title
;
'3-Cyanopyridine as bridging and terminal ligand in coordination polymers'
;

_publ_section_references
;

Boultif, A. & Louër, D. (1991). J. Appl. Cryst., 24, 987-993.

Coelho, A. A. (2007). TOPAS Academic User Manual. Coelho Software, B
risbane, Australia.

David, W. I. F., Shankland, K., Van de Streek, J., Pidcock, E. & Motherwell, S.
(2004). DASH. Version 3.0. Cambridge Crystallographic Data Centre, 12
Union Road, Cambridge, England.

Esmaeili, A., Kamiyama, T., Oishi-Tomiyasu, R. (2017). J. Appl. Cryst.
50 , 651-659.

Macrea, C. F., Edingington, P. R., McCabe, P., Pidcock, E., Shields, G.,
Taylor, R., Towler, M. & Van de Streek, J. (2006). J. Appl. Cryst.
39 , 453-457.


STOE & Cie (2004). WinXPOW. STOE and Cie, Darmstadt, Germany.
;

_publ_section_exptl_prep
;
FeBr2(3cypy)4 was prepared from alcoholic solution. 
;
_publ_section_exptl_refinement
;
The first 20 peaks were selected for indexing in DASH (Louër et al. , 2017), which resulted in a tetragonal unit cell with Z = 2. 
Structure solution was then carried out using simulated annealing 
with DASH(David et al. , 2004). 
A starting molecular model was derived from the known crystal structure of [CoBr2(3cypy)4]. 
The molecular fragment was restricted to rotate around the Br-Fe-Br-axis, Fe and Br atoms were
fixed on the fourfold rotation axis (0,0,z) during the simulated annealing.
The Rietveld refinement was carried out with TOPAS (Coelho, 2007). 
The Fe and Br atoms were restraint on the the fourfold axis, the 3-cyanopyridine was 
restrained flat in the mirror plane.
All C-C and C-H angles of the pyridine ring were restraint to be 120°. 
Thermal parameters of H atoms were constrained to those of 
the non-H atoms. 
;

_chemical_name_mineral FeBr2(3-cypy)4
_cell_length_a                    11.14842(14)
_cell_length_b                    11.14842(14)
_cell_length_c                    10.32052(15)
_cell_angle_alpha                 90	
_cell_angle_beta                  90	
_cell_angle_gamma                 90	
_cell_volume                      1282.71(40)
_cell_formula_units_Z             2 
_space_group 			  P4nc
loop_ 
 _symmetry_equiv_pos_as_xyz 
 '-x, -y, z'
 '-x+1/2, y+1/2, z+1/2'
 '-y, x, z'
 '-y+1/2, -x+1/2, z+1/2'
 'y, -x, z'
 'y+1/2, x+1/2, z+1/2'
 'x, y, z'
 'x+1/2, -y+1/2, z+1/2'
  
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
_atom_site_U_iso_or_equiv

Fe1 Fe   0  0 		0 		 0.5373(1)    1 4.42236     0.05601
N3  N    0 -0.1584(4) -0.1195(8)	 0.5369(6)    1 4.42236     0.05601
Br4 Br   0  0 	       0 		 0.2839(6)    1 4.42236     0.05601
Br5 Br   0  0 	       0 		 0.7904(6)    1 4.42236     0.05601
C8  C    0 -0.1637(8) -0.2106(3) 	 0.6207(3)    1 4.42236     0.05601
C9  C    0 -0.2531(1) -0.0973(3) 	 0.4606(7)    1 4.42236     0.05601
C14 C    0 -0.2627(4) -0.2868(7) 	 0.6285(8)    1 4.42236     0.05601
H15 H    0 -0.1003(1) -0.2184(7) 	 0.6868(1)    1 5.306832     0.06721
C16 C    0 -0.3545(5) -0.1716(9) 	 0.4670(3)    1 4.42236     0.05601
H17 H    0 -0.2540(9) -0.0236(1)	 0.4085(1)    1 5.306832     0.06721
C21 C    0 -0.3622(9) -0.2649(3) 	 0.5541(5)    1 4.42236     0.05601
H22 H    0 -0.2624(1) -0.3501(7)    	 0.6816(1)    1 5.306832     0.06721
C23 C    0 -0.4591(1) -0.1495(1)    	 0.3915(3)    1 4.42236     0.05601
H26 H    0 -0.4320(1) -0.3209(2) 	 0.5526(()    1 5.306832     0.06721
N27 N    0 -0.5464(5) -0.1298(1) 	 0.3380(6)    1 4.42236     0.05601


loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
 
 Fe1     N3   2.2108(4)   . ?	
 Fe1     Br4  2.6156(1)   . ?
 Fe1     Br5  2.6126(1)   . ?
 N3      C8   1.3345(5)   . ?
 N3      C9   1.3398(5)   . ?
 C8      C14  1.3950(5)   . ?
 C8      H15  0.9863(8)   . ?
 C9      C16  1.4038(3)   . ?
 C9      H17  0.9826(9)   . ?
 C14     C21  1.3716(8)   . ?
 C14     H22  0.8929(9)   . ?
 C16     C21  1.3770(9)   . ?
 C16     C23  1.4236(7)   . ?
 C21     H26  0.9971(4)   . ?
 C23     N27  1.1406(7)   . ?

				
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_3 
 _geom_angle_publ_flag 

N3      Fe1     Br4    89.8916(8)     . . ?
N3      Fe1     Br5    90.1116(2)     . . ?
Br4     Fe1     Br5   180.0000(0)     . . ?
Fe1     N3      C8    119.6826(9)     . . ?
Fe1     N3      C9    121.3511(6)     . . ?
C8      N3      C9    119.1013(6)     . . ?
N3      C8      C14   122.4316(3)     . . ?
N3      C8      H15   118.8928(7)     . . ?
C14     C8      H15   118.2300(6)     . . ?
N3      C9      C16   119.8513(4)     . . ?
N3      C9      H17   119.0647(2)     . . ?
C16     C9      H17   120.6925(6)     . . ?
C8      C14     C21   119.9109(5)     . . ?
C8      C14     H22   120.9222(7)     . . ?
C21     C14     H22   119.1667(8)     . . ?
C9      C16     C21   121.7843(1)     . . ?
C9      C16     C23   122.1007(4)     . . ?
C21     C16     C23   115.9279(9)     . . ?
C14     C21     C16   116.7157(7)     . . ?
C14     C21     H26   121.8734(4)     . . ?
C16     C21     H26   120.7313(8)     . . ?
C16     C23     N27   175.6972(1)     . . ?

_chemical_name_systematic                  
; 
Dibromo-tetra(3-cyanopyridine)ferrat
;				  
_chemical_name_common             'Dibromo-tetra(3-cyanopyridine)ferrat'		 
_chemical_formula_iupac           'C24 H16 Br2 Fe N8'				 
_chemical_formula_moiety          'C24 H16 Br2 Fe N8'				 
_chemical_formula_structural      'C24 H16 Br2 Fe N8'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum              'C24 H16 Br2 Fe N8'
_chemical_formula_weight          632.10 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   'colorless' 
 
loop_                                       
     _atom_type_symbol                      
     _atom_type_description      
     _atom_type_scat_source                       
   C C 'International Tables Vol C Table 6.1.1.4'
   H H 'International Tables Vol C Table 6.1.1.4'
   Fe Fe 'International Tables Vol C Table 6.1.1.4'
   Br Br 'International Tables Vol C Table 6.1.1.4'
   N N 'International Tables Vol C Table 6.1.1.4'


_symmetry_cell_setting            tetragonal        
_symmetry_space_group_name_H-M    'P  4 n c'        
_symmetry_space_group_name_Hall   'P 4 -2n'


_pd_spec_size_axial   12

_pd_spec_size_equat   0.7

_pd_spec_size_thick   0.7


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

_pd_spec_mounting                         
;
Specimen was sealed in a 0.7 mm diameter borosilicate glass capillary 
;

_pd_spec_mount_mode               'transmission'

_pd_spec_shape                    'cylinder'

_pd_char_particle_morphology      ?
_pd_char_colour                   ?       




# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu     ?
_pd_char_atten_coef_mu_obs ?								
_exptl_crystal_density_diffrn 1.634

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

# 7. EXPERIMENTAL DATA

_exptl_special_details
; ?
;

# The 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
; ?
;
_pd_calibration_special_details           # description of the method used
                                          # to calibrate the instrument
; ?
;

_diffrn_ambient_temperature       298             
_diffrn_source_target             ?
_diffrn_source_type               ?
_diffrn_radiation_type            'Cu K\a~1~'   
_diffrn_measurement_device_type   'STOE Stadi-P'       
_diffrn_detector                  ?      
_diffrn_detector_type             'lin psd'
_diffrn_radiation_source   	  'X-ray tube'
_exptl_crystal_F_000              ?	    	

_pd_meas_scan_method              step       


_diffrn_radiation_wavelength      1.540598    
_diffrn_radiation_monochromator   'primary focussing, Ge 111'   

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

_pd_meas_number_of_points         7700
_pd_meas_2theta_range_min         3        
_pd_meas_2theta_range_max        80       
_pd_meas_2theta_range_inc         ?        

_cell_measurement_temperature     298


#==============================================================================
# 8. REFINEMENT DATA

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


_pd_proc_ls_profile_function      
;
modified spherical harmonics(Coelho, 2007)
;        
_pd_proc_ls_background_function   'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr      'none'        


_pd_proc_ls_prof_R_factor         0.01821        
_pd_proc_ls_prof_wR_factor        0.02315        
_pd_proc_ls_prof_wR_expected      0.02279        
_refine_ls_R_I_factor             0.01408	  



_refine_ls_matrix_type            fullcycle        	
_refine_ls_weighting_scheme       sigma        		
_refine_ls_weighting_details      w=1/σ(Yobs)²	
_refine_ls_hydrogen_treatment     'mixed'        	
_refine_ls_extinction_method      'none'        	
_refine_ls_extinction_coef        ?         		
_refine_ls_number_parameters      78      		
_refine_ls_number_restraints      28        		
_refine_ls_number_constraints     2 			
_refine_ls_number_reflns	  ?			
     

_refine_ls_goodness_of_fit_all     1.015      
      
_refine_ls_restrained_S_all       ?        
_refine_ls_restrained_S_obs       ?
_refine_ls_shift/su_max           ?        
_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         3        
_pd_proc_2theta_range_max         80        
_pd_proc_2theta_range_inc         ?               
_pd_proc_info_excluded_regions    'none'        


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

_computing_molecular_graphics   'MERCURY (Macrea et al.)'
_computing_structure_refinement   'TOPAS (Coelho, 2007)'
_computing_structure_solution   'DASH (David et al., 2004)'
_computing_data_reduction   'DASH (David et al., 2004)'
_computing_cell_refinement   'DASH (David  et al. , 2004)'
_computing_data_collection   'STOE WINXPOW (STOE & Cie GmbH, 2004)'

# start Validation Reply Form
_vrf_REFI015_FeBr23-cypy4
;
PROBLEM: refine_ls_shift/su_max is missing
         Maximum shift/s.u. ratio after final refinement cycle.
RESPONSE: structure was solved from powder data
;
_vrf_PLAT341_FeBr23-cypy4
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0086 Ang. 
RESPONSE: X-ray powder data
;
_vrf_PLAT920_FeBr23-cypy4
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.18 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_FeBr23-cypy4
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0        227       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_FeBr23-cypy4
;
PROBLEM: Check Calcd Resid. Dens.  1.07A   From Br4             1.90 eA-3    
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_FeBr23-cypy4
;
PROBLEM: Check Calcd Resid. Dens.  0.03A   From Br4           -43.48 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_FeBr23-cypy4
;
PROBLEM: Check Calcd Negative Resid. Density on       Fe1     -28.60 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_FeBr23-cypy4
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structur was solved from powder data
;
# end Validation Reply Form