data_NiBr2(3-cypy)2-beta

_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              'CrystEngNimm'

_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 Universitaet Frankfurt am Main
Institute of Inorganic and Analytical Chemistry
Max-von-Laue-Str. 7
60438 Frankfurt am Main
Germany
;

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

'Schmidt, Martin U.'
;
Goethe Universitaet 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.

Nielho, A. A. (2007). TOPAS Academic User Manual. Nielho 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
;
NiBr2(3cypy)2 was prepared by thermal decomposition of NiBr2(3cypy)4.
;
_publ_section_exptl_refinement
; 
A starting molecular model was derived from the known crystal structure of [NiBr2(3cypy)2]n. 
The molecular fragment was restricted to rotate around the Ni-atom during the structre solution. 
All C-C and C-H angels of the pyridine ring were restraint to be 120°, the pyridine ring was constrained to be flat. 
Thermal parameters of hydrogen atoms were constrained to those of 
the non-hydrogen atoms.  
The final crystallographic data of the beta form were taken from the simultaneous Rietveld refinement of the two polymorphic structures.
;

_chemical_name_mineral ??
_cell_length_a     3.7274(2)
_cell_length_b    13.574(9)
_cell_length_c    13.761(6)
_cell_angle_alpha 86.862(2)
_cell_angle_beta  82.401(9)
_cell_angle_gamma 82.120(1)
_cell_volume      683.15(1)
_space_group P-1
_cell_formula_units_Z 2
loop_
_symmetry_equiv_pos_as_xyz
	'-x, -y, -z'
	'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

Ni1 Ni  0  0 	        0.5 	     0.5 		1 1.25764     0.01593
Br2 Br  0  0.400(2)     0.624(8)     0.541(8)     	1 1.25764     0.01593
N5 N    0  0.032(1)     0.561(2)     0.348(5)     	1 1.25764     0.01593
C8 C    0  0.119(5)     0.489(5)     0.279(9)     	1 1.25764     0.01593
C9 C    0 -0.015(3)     0.658(3)     0.323(4)     	1 1.25764     0.01593
C14 C   0  0.161(3)     0.515(9)     0.180(1)     	1 1.25764     0.01593
H15 H   0  0.142(1)     0.419(4)     0.300(9)    	1 1.509168     0.01911
C16 C   0  0.026(2)     0.686(1)     0.223(5)    	1 1.25764     0.01593
H17 H   0 -0.076(1)     0.709(5)     0.374(4)    	1 1.509168     0.01911
C21 C   0  0.115(3)     0.614(9)     0.152(3)     	1 1.25764     0.01593
C22 C   0  0.264(1)     0.444(3)     0.106(1)     	1 1.25764     0.01593
H23 H   0 -0.011(1)     0.757(1)     0.202(8)    	1 1.509168     0.01911
H26 H   0  0.148(1)     0.633(5)     0.080(7)    	1 1.509168     0.01911
N27 N   0  0.370(4)     0.386(6)     0.049(5)     	1 1.25764     0.01593


Ni102 Ni  0  1 	 	  0 	       0 	        1 1.25764     0.01593
Br202 Br  0  0.525(3)    -0.124(7)     0.055(2)     	1 1.25764     0.01593
N402 N    0  0.881(1)     0.063(8)     0.145(8)     	1 1.25764     0.01593
C602 C    0  0.875(9)    -0.000(8)     0.225(4)     	1 1.25764     0.01593
C702 C    0  0.834(6)     0.159(9)     0.161(8)     	1 1.25764     0.01593
C1002 C   0  0.820(6)     0.026(6)     0.321(3)     	1 1.25764     0.01593
H1102 H   0  0.909(1)    -0.073(1)     0.214(1)    	1 1.509168     0.01911
C1202 C   0  0.780(2)     0.190(2)     0.255(6)     	1 1.25764     0.01593
H1302 H   0  0.832(1)     0.210(9)     0.107(5)    	1 1.509168     0.01911
C1802 C   0  0.775(3)     0.124(2)     0.336(2)     	1 1.25764     0.01593
C1902 C   0  0.827(1)    -0.047(3)     0.398(1)     	1 1.25764     0.01593
H2002 H   0  0.743(2)     0.261(3)     0.263(3)    	1 1.509168     0.01911
H2402 H   0  0.735(1)     0.146(5)     0.403(6)    	1 1.509168     0.01911
N2502 N   0  0.848(8)    -0.107(9)     0.456(4)     	1 1.25764     0.01593


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
 

Ni1     Br2    2.581(4)    	. ?
Ni1     N5     2.147(8)    	. ?
N5      C8     1.370(1)    	. ?
N5      C9     1.338(2)    	. ?
C8      C14    1.393(8)    	. ?
C8      H15    0.975(7)    	. ?
C9      C16    1.400(4)    	. ?
C9      H17    0.995(8)    	. ?
C14     C21    1.371(1)    	. ?
C14     C22    1.427(5)    	. ?
C16     C21    1.390(4)    	. ?
C16     H23    0.985(1)    	. ?
C21     H26    0.999(5)    	. ?
C22     N27    1.132(7)    	. ?


Ni102    Br202     2.583(4)    . ?
Ni102    N402      2.151(5)    . ?
N402     C602      1.365(6)    . ?
N402     C702      1.318(6)    . ?
C602     C1002     1.371(9)    . ?
C602     H1102     0.990(3)    . ?
C702     C1202     1.358(5)    . ?
C702     H1302     0.990(5)    . ?
C1002    C1802     1.336(1)    . ?
C1002    C1902     1.417(7)    . ?
C1202    C1802     1.384(1)    . ?
C1202    H2002     0.965(1)     . ?
C1802    H2402     0.979(6)    . ?
C1902    N2502     1.119(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 
 
Br2     Ni1     N5 	 91.095(3)    . . ?
Ni1     N5      C8 	113.571(8)   . . ?
Ni1     N5      C9 	125.452(2)   . . ?
C8      N5      C9 	122.106(5)   . . ?
N5      C8      C14	120.580(4)    . . ?
N5      C8      H15	119.775(2)    . . ?
C14     C8      H15	119.586(3)	 . . ?
N5      C9      C16	118.050(6)    	 . . ?
N5      C9      H17	121.038(6)      . . ?
C16     C9      H17	120.908(8)	   . . ?
C8      C14     C21	118.548(8)	   . . ?
C8      C14     C22	122.547(6)      . . ?
C21     C14     C22	118.856(4)	    . . ?
C9      C16     C21	121.013(1)	    . . ?
C9      C16     H23	119.832(8)       . . ?
C21     C16     H23	119.150(4)	    . . ?
C14     C21     C16	119.698(1)        . . ?
C14     C21     H26	118.313(4)        . . ?
C16     C21     H26	121.988(1)         . . ?
C14     C22     N27	175.043(6)         . . ?


Br202    Ni102    N402        88.887(6)	      . . ?
Ni102     N402     C602      121.956(8)	     . . ?
Ni102     N402     C702      121.843(2)	     . . ?
C602      N402     C702      117.907(8)	     . . ?
N402     C602     C1002      124.874(6)	      . . ?
N402     C602     H1102      118.337(6)	      . . ?
C1002     C602     H1102     116.785(7)	      . . ?
N402      C702     C1202     119.072(1)	      	 . . ?
N402      C702     H1302     122.140(6)	        . . ?
C1202     C702     H1302     118.782(4)	        . . ?
C602      C1002    C1802     116.352(7)	        . . ?
C602      C1002    C1902     119.887(1)	        . . ?
C1802     C1002    C1902     123.712(1)	         . . ?
C702      C1202    C1802     122.703(6)	         . . ?
C702      C1202    H2002     115.794(3)	         . . ?
C1802     C1202    H2002     121.500(2)	         . . ?
C1002    C1802    C1202      119.080(9)	       	     . . ?
C1002    C1802    H2402      118.527(4)	          . . ?
C1202    C1802    H2402      122.384(1)	           . . ?
C1002    C1902    N2502      176.757(7)	           . . ?


_chemical_name_systematic                  
; 
beta-Catena-dibromo-di(3-cyanopyridine)nickelat
;				  
_chemical_name_common             'Dibromo-bis(3-cyanopyridine)nickelat'		 
_chemical_formula_iupac           'C12 H8 Br2 N4 Ni'				 
_chemical_formula_moiety          'C12 H8 Br2 N4 Ni'				 
_chemical_formula_structural      'C12 H8 Br2 N4 Ni'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum              'C12 H8 Br2 N4 Ni'
_chemical_formula_weight          426.71 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   'light yellow' 
 
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'
   Ni Ni '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            triclinic        
_symmetry_space_group_name_H-M    'P  -1'        
_symmetry_space_group_name_Hall   '-P 1'


_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 2.075

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

# 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         6600
_pd_meas_2theta_range_min         4        
_pd_meas_2theta_range_max         70
_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         0.03277       
_pd_proc_ls_prof_wR_factor        0.04294        
_pd_proc_ls_prof_wR_expected      0.02473        
_refine_ls_R_I_factor             0.00498	  



_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      165      		
_refine_ls_number_restraints      70        		
_refine_ls_number_constraints     3 			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.737      
      
_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         70        
_pd_proc_2theta_range_inc         ?               
_pd_proc_info_excluded_regions    '15.4 - 15.74'        


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

_computing_molecular_graphics   'MERCURY (Macrea et al.)'
_computing_structure_refinement   'TOPAS (Nielho, 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_NiBr23-cypy2-beta
;
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_NiBr23-cypy2-beta
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............        0.1 Ang.  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT920_NiBr23-cypy2-beta
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.20 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_NiBr23-cypy2-beta
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0          8       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_NiBr23-cypy2-beta
;
PROBLEM: Check Calcd Resid. Dens.  1.29A   From Ni1             5.65 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_NiBr23-cypy2-beta
;
PROBLEM: Check Calcd Resid. Dens.  0.09A   From Br2           -33.71 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_NiBr23-cypy2-beta
;
PROBLEM: Check Calcd Negative Resid. Density on       Ni1     -23.04 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_NiBr23-cypy2-beta
;
PROBLEM: Check Negative Difference Density on H1102 -1.13 eA-3 
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_NiBr23-cypy2-beta
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form