data_NiBr2(3-cypy)2-alpha

_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.

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
;
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)4]. 
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.  
;

_chemical_name_mineral ??
_cell_length_a     3.709(1)
_cell_length_b    26.801(4)
_cell_length_c    13.706(8)
_cell_angle_alpha 90
_cell_angle_beta  97.678(6)
_cell_angle_gamma 90
_cell_volume      1350.58(5)
_space_group C1c1
_cell_formula_units_Z 4
loop_
_symmetry_equiv_pos_as_xyz
	'x, -y, z+1/2'
	'x, y, z'
	'x+1/2, -y+1/2, z+1/2'
	'x+1/2, y+1/2, 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 0.849(4)    0.876(1) -0.127(8) 1 1.55095     0.01964
Br2 Br  0 0.345(4)    0.939(5) -0.081(3) 1 1.55095     0.01964
Br3 Br  0 1.331(7)    0.815(3) -0.175(9) 1 1.55095     0.01964
N4 N    0 0.899(1)    0.853(4)  0.019(3) 1 1.55095     0.01964
N5 N    0 0.760(7)    0.909(6) -0.273(5) 1 1.55095     0.01964
C6 C    0 0.915(8)    0.888(2)  0.091(9) 1 1.55095     0.01964
C7 C    0 0.901(9)    0.804(1)  0.040(3) 1 1.55095     0.01964
C8 C    0 0.703(5)    0.878(1) -0.350(8) 1 1.55095     0.01964
C9 C    0 0.743(2)    0.959(4) -0.286(7) 1 1.55095     0.01964
C10 C   0 0.948(9)    0.873(5)  0.189(9) 1 1.55095     0.01964
H11 H   0 0.907(6)    0.925(2)  0.077(7) 1 1.86114     0.02357
C12 C   0 0.927(5)    0.789(4)  0.136(4) 1 1.55095     0.01964
H13 H   0 0.889(1)    0.776(4) -0.006(4) 1 1.86114     0.02357
C14 C   0 0.636(2)    0.895(4) -0.446(4) 1 1.55095     0.01964
H15 H   0 0.707(8)    0.841(1) -0.341(1) 1 1.86114     0.02357
C16 C   0 0.675(6)    0.978(1) -0.378(8) 1 1.55095     0.01964
H17 H   0 0.780(4)    0.984(9) -0.236(3) 1 1.86114     0.02357
C18 C   0 0.951(3)    0.823(1)  0.210(4) 1 1.55095     0.01964
C19 C   0 0.964(8)    0.909(2)  0.268(7) 1 1.55095     0.01964
H20 H   0 0.931(5)    0.754(3)  0.150(9) 1 1.86114     0.02357
C21 C   0 0.622(6)    0.946(8) -0.457(4) 1 1.55095     0.01964
C22 C   0 0.570(9)    0.859(2) -0.524(8) 1 1.55095     0.01964
H23 H   0 0.675(4)    1.013(7) -0.387(7) 1 1.86114     0.02357
H24 H   0 0.975(6)    0.811(1)  0.278(5) 1 1.86114     0.02357
N25 N   0 0.972(1)    0.938(3)  0.329(5) 1 1.55095     0.01964
H26 H   0 0.582(1)    0.962(5) -0.521(1) 1 1.86114     0.02357
N27 N   0 0.508(6)    0.827(5) -0.580(2) 1 1.55095     0.01964



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   	   2.669(2)     . ?
Ni1     Br3  	   2.549(5)     . ?
Ni1     N4   	   2.162(1)     . ?
Ni1     N5   	   2.154(4)     . ?
N4      C6   	   1.358(8)     . ?
N4      C7   	   1.354(5)     . ?
N5      C8   	   1.350(9)     . ?
N5      C9   	   1.345(3)     . ?
C6      C10  	   1.389(8)     . ?
C6      H11  	   1.009(4)     . ?
C7      C12  	   1.366(1)     . ?
C7      H13  	   0.976(8)     . ?
C8      C14  	   1.381(7)     . ?
C8      H15  	   0.997(8)     . ?
C9      C16  	   1.349(5)     . ?
C9      H17  	   0.968(4)     . ?
C10     C18  	   1.380(1)     . ?
C10     C19  	   1.439(7)     . ?
C12     C18  	   1.351(5)     . ?
C14     C21  	   1.386(2)     . ?
C14     C22  	   1.443(4)     . ?
C16     C21  	   1.356(9)     . ?
C12     H20  	   0.960(1)     . ?
C16     H23  	   0.965(6)     . ?
C18     H24  	   0.979(7)     . ?
C21     H26  	   0.963(3)     . ?
C19     N25  	   1.138(4)     . ?
C22     N27  	   1.144(1)     . ?




				
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     Br3          178.292(1)     . . ?
Br2     Ni1     N4   	      86.131(1)	    . . ?
Br2     Ni1     N5   	      86.186(5)	    . . ?
Br3     Ni1     N4   	      95.154(2)	    . . ?
Br3     Ni1     N5   	      88.907(6)	    . . ?
N4      Ni1     N5   	     174.232(4)	    . . ?
Ni1     N4      C6   	     119.847(8)	    . . ?
Ni1     N4      C7   	     119.040(1)	    . . ?
C6      N4      C7   	     121.076(1)	    . . ?
Ni1     N5      C8   	     116.598(9)	    . . ?
Ni1     N5      C9   	     122.166(5)	    . . ?
C8      N5      C9   	     121.137(8)	    . . ?
N4      C6      C10  	     120.177(4)	    . . ?
N4      C6      H11  	     122.407(2)	    . . ?
C10     C6      H11  	     117.412(5)	    . . ?
N4      C7      C12  	     118.922(5)	    . . ?
N4      C7      H13  	     127.088(1)	    . . ?
C12     C7      H13  	     113.988(1)	    . . ?
N5      C8      C14  	     121.389(9)	    . . ?
N5      C8      H15  	     121.247(3)	    . . ?
C14     C8      H15  	     117.362(5)	    . . ?
N5      C9      C16  	     119.455(2)	    . . ?
N5      C9      H17  	     127.118(2)	    . . ?
C16     C9      H17  	     113.408(4)	    . . ?
C6      C10     C18  	     118.204(2)	    . . ?
C6      C10     C19  	     121.756(1)	    . . ?
C18     C10     C19  	     119.987(1)	    . . ?
C7      C12     C18  	     121.416(2)	    . . ?
C7      C12     H20  	     118.542(9)	    . . ?
C18     C12     H20  	     120.036(4)	    . . ?
C8      C14     C21  	     115.972(6)	    . . ?
C8      C14     C22  	     118.085(2)	    . . ?
C21     C14     C22  	     125.881(9)	    . . ?
C9      C16     C21  	     120.225(6)	    . . ?
C9      C16     H23  	     118.859(8)	    . . ?
C21     C16     H23  	     120.868(6)	    . . ?
C10     C18     C12  	     120.166(3)	    . . ?
C10     C18     H24  	     120.972(7)	    . . ?
C12     C18     H24  	     118.847(1)	    . . ?
C10     C19     N25  	     178.232(1)	    . . ?
C14     C21     C16  	     121.792(4)	    . . ?
C14     C21     H26  	     122.089(9)	    . . ?
C16     C21     H26  	     115.001(1)	    . . ?
C14     C22     N27  	     173.290(1)	    . . ?




_chemical_name_systematic                  
; 
alpha-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            monoclinic        
_symmetry_space_group_name_H-M    'C 1 c 1'        
_symmetry_space_group_name_Hall   'C -2 y c'


_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 2.099

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

# 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       198             
_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         8700
_pd_meas_2theta_range_min         3        
_pd_meas_2theta_range_max         90
_pd_meas_2theta_range_inc         ?        

_cell_measurement_temperature     198


#==============================================================================
# 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         0.03547        
_pd_proc_ls_prof_wR_factor        0.05026        
_pd_proc_ls_prof_wR_expected      0.02753        
_refine_ls_R_I_factor             0.00446	  



_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      167      		
_refine_ls_number_restraints      69        		
_refine_ls_number_constraints     3 			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.825      
      
_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         90        
_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_NiBr23-cypy2-alpha
;
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-alpha
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.136 Ang.  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT411_NiBr23-cypy2-alpha
;
PROBLEM: Short Inter H...H Contact  H11      ..H23              1.96 Ang.   
RESPONSE: structure was solved from powder data
;
_vrf_PLAT752_NiBr23-cypy2-alpha
;
PROBLEM: Angle   Calc      115.00, Rep      115.00 ......  Senseless s.u. 
RESPONSE: coincidence
;
_vrf_PLAT920_NiBr23-cypy2-alpha
;
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-alpha
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         69       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT790_NiBr23-cypy2-alpha
;
PROBLEM: centre of Gravity not Within Unit Cell 
RESPONSE: for reason of comparison
;
_vrf_PLAT971_NiBr23-cypy2-alpha
;
PROBLEM: Check Calcd Resid. Dens.  1.04A   From Br2             5.13 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_NiBr23-cypy2-alpha
;
PROBLEM: Check Calcd Resid. Dens.  0.15A   From Br3           -53.97 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_NiBr23-cypy2-alpha
;
PROBLEM: Check Calcd Negative Resid. Density on       Ni1     -40.66 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_NiBr23-cypy2-alpha
;
PROBLEM: Check Calcd Negative Resid. Density on       H11     -1.27 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_NiBr23-cypy2-alpha
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form