data_FeBr2(3-cypy)1

_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
;
FeBr2(3cypy)1 was prepared by thermal decomposition of FeBr2(3cypy)4.
;
_publ_section_exptl_refinement
;

The first 20 peaks were selected for indexing in CONOGRAPH (Esmaeili et al. , 2017), 
which resulted in an 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 cyanopyrdine were placed on a special position ((0,y,z)) during the simulated annealing.
The Rietveld refinement was carried out with TOPAS (Coelho, 2007). The bromine atoms were fixed on y= -0.5 and y= 0.5 during the refinement.
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.Reflections of a foreign phase were excluded during the refinement.  
;

_chemical_name_mineral ??
_cell_length_a     3.772(2)
_cell_length_b     7.251(2)
_cell_length_c    16.310(8)
_cell_angle_alpha 90
_cell_angle_beta  90
_cell_angle_gamma 90
_cell_volume      446.18(4)
_cell_formula_units_Z 2
_space_group Pmc21

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

N1 N   	0 0 	0.2381(1)     0.9806(1)    1 3.19139     0.04042
Fe2 Fe  0 0 	0.3932(5)     0.8640(5)    1 3.19139     0.04042
C3 C    0 0 	0.3316(6)     1.0503(1)    1 3.19139     0.04042
C4 C    0 0 	0.0530(1)     0.9814(1)    1 3.19139     0.04042
Br5 Br  0 0.5 	0.6134(8)     0.9225(9)    1 3.19139     0.04042
Br6 Br  0 -0.5  0.1846(1)     0.8003(9)    1 3.19139     0.04042
H7 H    0 0 	0.4639(2)     1.0484(1)    1 3.829668     0.04850
C8 C    0 0 	0.2468(1)     1.1251(1)    1 3.19139     0.04042
C9 C    0 0    -0.0385(3)     1.0552(3)    1 3.19139     0.04042
H10 H   0 0    -0.0194(9)     0.9305(7)    1 3.829668     0.04850
C11 C   0 0 	0.0613(2)     1.1270(7)    1 3.19139     0.04042
C12 C   0 0 	0.3437(3)     1.2020(1)    1 3.19139     0.04042
H13 H   0 0    -0.1742(8)     1.0568(8)    1 3.829668     0.04850
H14 H   0 0 	0.0047(3)     1.1806(5)    1 3.829668     0.04850
N15 N   0 0 	0.4283(5)     1.2615(1)    1 3.19139     0.04042


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
 

N1      Fe2   	2.2098(2)   . ?
N1      C3    	1.3238(7)  . ?
N1      C4    	1.3423(4)  . ?
Fe2     Br5   	2.6498(9)   . ?
Fe2     Br6   	2.6318(5)  . ?
C3      H7    	0.9595(5)  . ?
C3      C8    	1.3664(4)  . ?
C4      C9    	1.3750(2)  . ?
C4      H10   	0.9816(7)  . ?
C8      C11   	1.3453(4)  . ?
C8      C12   	1.4379(5)  . ?
C9      C11   	1.3774(2)  . ?
C9      H13   	0.9847(2)  . ?
C11     H14   	0.9654(8)  . ?
C12     N15   	1.1480(6)  . ?

				
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 
 
 
Fe2     N1      C3   118.6292(7)    	 . . ?
Fe2     N1      C4   121.1618(8)    	 . . ?
C3      N1      C4   120.2669(8)   	  . . ?
N1      Fe2     Br5   89.8420(7)     	. . ?
N1      Fe2     Br6   92.7317(5)     	 . . ?
Br5     Fe2     Br6  177.4512(6)    . . ?
N1      C3      H7   118.9731(4)   . . ?
N1      C3      C8   122.4117(2)   . . ?
H7      C3      C8   118.6151(4)    . . ?
N1      C4      C9   119.4181(1)     . . ?
N1      C4      H10  121.8179(5)     . . ?
C9      C4      H10  118.7639(5)     . . ?
C3      C8      C11  118.1329(2)      . . ?
C3      C8      C12  123.9743(3)      . . ?
C11     C8      C12  117.8927(5)      . . ?
C4      C9      C11  119.4270(4)      . . ?
C4      C9      H13  120.4272(4)       . . ?
C11     C9      H13  120.1457(2)       . . ?
C8      C11     C9   120.3432(5)        . . ?
C8      C11     H14  116.5205(1)        . . ?
C9      C11     H14  123.1362(5)        . . ?
C8      C12     N15  176.9537(3)          . . ?
	        				        
_chemical_name_systematic                  
; 
catena-dibromo-(3-cyanopyridine)ferrat
;				  
_chemical_name_common             'catena-dibromo-bis(3-cyanopyridine)ferrat'		 
_chemical_formula_iupac           'C6 H4 Br2 Fe N2'				 
_chemical_formula_moiety          'C6 H4 Br2 Fe N2'				 
_chemical_formula_structural      'C6 H4 Br2 Fe N2'				 
_chemical_formula_analytical      ? 	      
_chemical_formula_sum             'C6 H4 Br2 Fe N2'
_chemical_formula_weight          319.76 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   'brown-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  m c 21'        
_symmetry_space_group_name_Hall   'P 2 c -2'


_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 2.381

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

# 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         7600
_pd_meas_2theta_range_min         4        
_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      'no correction'     


_pd_proc_ls_prof_R_factor         0.01633        
_pd_proc_ls_prof_wR_factor        0.02077        
_pd_proc_ls_prof_wR_expected      0.01714        
_refine_ls_R_I_factor             0.01075	  



_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      71      		
_refine_ls_number_restraints      28       		
_refine_ls_number_constraints     1 			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.218      
      
_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         4        
_pd_proc_2theta_range_max         80        
_pd_proc_2theta_range_inc         ?               
_pd_proc_info_excluded_regions    '11.51-11.85; 12.40-12.71; 24.30-24.54'        


# 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-cypy1
;
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_PLAT920_FeBr23-cypy1
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.12 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_FeBr23-cypy1
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         49       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_FeBr23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  1.25A   From Br6             3.85 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_FeBr23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  0.03A   From Br6           -36.16 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_FeBr23-cypy1
;
PROBLEM: Check Calcd Negative Resid. Density on       Fe2     -22.69 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_FeBr23-cypy1
;
PROBLEM: Check Negative Difference Density on H7 -0.85 eA-3 and H14  -1.02 eA-3
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_FeBr23-cypy1
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form
