data_FeBr2(3-cypy)2

_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 XXX.
;


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


# 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
;
The compound was prepared by thermal decomoposition of [Fe(3cypy)4]
;
_publ_section_exptl_refinement
;
The first 25 peaks were selected for indexing in CONOGRAPH (Esmaeili et al. , 2017), which resulted in a orthorhombic 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 [FeBr2(3cypy)4]. 
The molecular fragment was restricted to rotate around the Fe-atom, Fe-atom and 3-cyanopyridine were fixed on a special position (0,0,0) during the simulated annealing.
The Rietveld refinement was carried out with TOPAS (Coelho, 2007). 
The Fe atom was restraint on the origin, the 3-cyanopyridine was 
restrained flat in the mirror plane.
All C-C and C-H angels of the pyridine ring were restraint to be 120°. 
Thermal parameters of hydrogen atoms were constrained to those of 
the non-hydrogen atoms. 
;

_chemical_name_mineral ??
_cell_length_a  27.1280(50)
_cell_length_b  7.1722(14)
_cell_length_c  3.7881(06)
_cell_angle_alpha 90
_cell_angle_beta  90
_cell_angle_gamma 90
_cell_volume 737.0(2)
 _cell_formula_units_Z 2
_space_group Pnnm
loop_
_symmetry_equiv_pos_as_xyz
	'-x, -y, -z'
	'-x, -y, z'
	'-x+1/2, y+1/2, -z+1/2'
	'-x+1/2, y+1/2, z+1/2'
	'x, y, -z'
	'x, y, z'
	'x+1/2, -y+1/2, -z+1/2'
	'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

C1 C  		 0 0.65982(15)  0.6193(57)  0.5 	1 1.493(39)     0.01891
C2 C  		 0 0.70248(17)  0.5012(75)  0.5 	1 1.493(39)     0.01891
C3 C   		 0 0.61325(15)  0.54182(58) 0.5 	1 1.493(39)     0.01891
C4 C   		 0 0.66509(14)  0.80884(56) 0.5 	1 1.493(39)     0.01891
N5 N  		 0 0.73613(20)  0.40796(78) 0.5 	1 1.493(39)     0.01891
N6 N  		 0 0.57197(18)  0.64131(56) 0.5 	1 1.493(39)     0.01891
H7 H  		 0 0.61151(58)  0.4065(23)  0.5 	1 1.791(46)     0.02269
C8 C   		 0 0.62304(15)  0.91558(57) 0.5 	1 1.493(39)     0.01891
H9 H   		 0 0.69896(55)  0.8653(23)  0.5 	1 1.791(46)     0.02269
Fe10 Fe   	 0 0.5 		0.5   	    0.5 	1 1.493(39)     0.01891
C11 C   	 0 0.57691(15)  0.83287(54) 0.5 	1 1.493(39)     0.01891
H12 H   	 0 0.62727(60)  1.0512(26)  0.5 	1 1.791(46)     0.02269
Br13 Br	 	 0 0.532130(53) 0.27245(20) 1.0 	1 1.493(39)     0.01891
H14 H   	 0 0.54712(59)  0.9097(21)  0.5 	1 1.791(46)     0.02269


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
 

C1      C2     	1.4337(7)   . ?
C1      C3     	1.3793(9)   . ?
C1      C4     	1.3688(5)   . ?
C2      N5     	1.1313(5)   . ?
C3      N6     	1.3278(7)   . ?
C3      H7     	0.9715(6)   . ?
C4      C8     	1.3738(2)   . ?
C4      H9     	1.0039(9)   . ?
N6      Fe10   	2.2005(9)   . ?
N6      C11    	1.3804(4)   . ?
C8      C11    	1.3856(2)   . ?
C8      H12    	0.9795(2)   . ?
Fe10    Br13   	2.6484(2)   . ?
C11     H14    	0.9780(9)   . ?
	 
				
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 
 
 
C2      C1      C3     	120.1499(3)   . . ?
C2      C1      C4     	120.2456(2)  . . ?
C3      C1      C4     	119.6644(7)  . . ?
C1      C2      N5     	179.9723(6)  . . ?
C1      C3      N6     	123.8250(7)   . . ?
C1      C3      H7     	116.5143(2)   . . ?
N6      C3      H7     	119.7206(3)  	 . . ?
C1      C4      C8     	117.8713(5)  	 . . ?
C1      C4      H9     	119.7941(2)    . . ?
C8      C4      H9     	122.3645(6)  	   . . ?
C3      N6      Fe10   	120.3457(8)  	   . . ?
C3      N6      C11    	116.9344(1)     . . ?
Fe10    N6      C11    	123.0311(2)  	    . . ?
C4      C8      C11    	120.7709(7)  	    . . ?
C4      C8      H12    	117.1386(2)      . . ?
C11     C8      H12    	122.0904(2)  	    . . ?
N6      Fe10    Br13   	 89.5428(1)  	     . . ?
N6      C11     C8     	120.9337(4)       . . ?
N6      C11     H14    	118.7142(4)        . . ?
C8      C11     H14    	120.3520(3)        . . ?
				 
				 


_chemical_name_systematic                  
; 
Catena-dibromo-bis(3-cyanopyridine)iron
;				  
_chemical_name_common             'Dibromo-bis(3-cyanopyridine)iron'		 
_chemical_formula_iupac          'C12 H8 Br2 Fe N4'				 
_chemical_formula_moiety          'C12 H8 Br2 Fe N4'				 
_chemical_formula_structural      'C12 H8 Br2 Fe N4'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum              'C12 H8 Br2 Fe N4'
_chemical_formula_weight          423.87 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   'red' 
 
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            orthorhombic        
_symmetry_space_group_name_H-M    'P  n n m'        
_symmetry_space_group_name_Hall   '-P 2 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 0.5 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 1.91

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

# 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         9200
_pd_meas_2theta_range_min         3        
_pd_meas_2theta_range_max         95       
_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      'no correction'     


_pd_proc_ls_prof_R_factor         0.01315        
_pd_proc_ls_prof_wR_factor        0.01674        
_pd_proc_ls_prof_wR_expected      0.01484        
_refine_ls_R_I_factor             0.01191	  



_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      67      		
_refine_ls_number_restraints      29        		
_refine_ls_number_constraints     1 			
_refine_ls_number_reflns	  ?			
     

_refine_ls_goodness_of_fit_all     1.127      
      
_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         95        
_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-cypy2
;
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-cypy2
;
PROBLEM:Low Bond Precision on  C-C Bonds ...............     0.0222 Ang. 
RESPONSE: X-ray powder data
;
_vrf_PLAT962_FeBr23-cypy2
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         16       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_FeBr23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  0.99A   From Br13            4.51 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_FeBr23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  0.09A   From Br13          -59.87 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_FeBr23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density on      Fe10     -40.48 eA-3  
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form
