data_CoBr2(3-cypy)4-Pulver

_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
;
CoBr2(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-Co-Br-axis, Co 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 Co 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 CoBr2(3cypy)4
_cell_length_a                    11.0587(4)   
_cell_length_b                    11.0587(4)   
_cell_length_c                    10.4149(5)    
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1273.70(4)
_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

N1 N    0 0.1145(6) 0.1580(1)  0.9452(1)    1 3.18929     0.04039
Co2 Co  0 0 	    0 	       0.9440(7)    1 3.18929     0.04039
C3 C    0 0.0956(5) 0.2536(1)  1.0217(1)    1 3.18929     0.04039
C4 C    0 0.2081(8) 0.1661(7)  0.8643(5)    1 3.18929     0.04039
Br5 Br  0 0 	    0 	       0.6964(6)    1 3.18929     0.04039
Br6 Br  0 0 	    0          1.1997(5)    1 3.18929     0.04039
H7 H    0 0.0255(8) 0.2507(4)  1.0781(2)    1 3.827148     0.04847
C8 C    0 0.1740(9) 0.3547(1)  1.0164(8)    1 3.18929     0.04039
C9 C    0 0.2878(2) 0.2631(9)  0.8542(1)    1 3.18929     0.04039
H10 H   0 0.2236(8) 0.0998(9)  0.8083(5)    1 3.827148     0.04847
C11 C   0 0.1516(2) 0.4600(9)  1.0908(2)    1 3.18929     0.04039
C12 C   0 0.2717(1) 0.3610(3)  0.9332(9)    1 3.18929     0.04039
H13 H   0 0.3518(9) 0.2599(4)  0.7890(9)    1 3.827148     0.04847
N14 N   0 0.1227(1) 0.5471(1)  1.1393(2)    1 3.18929     0.04039
H15 H   0 0.3249(3) 0.4332(2)  0.9363(9)    1 3.827148     0.04847

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      Co2     2.1584(5)    . ?
N1      C3      1.3401(5)    . ?
N1      C4      1.3375(6)    . ?
Co2     Br5     2.5790(1)    . ?
Co2     Br6     2.6639(8)    . ?
C3      H7      0.9729(4)    . ?
C3      C8      1.4161(3)    . ?
C4      C9      1.3922(1)    . ?
C4      H10     0.9522(6)    . ?
C8      C11     1.4210(2)    . ?
C8      C12     1.3859(2)    . ?
C9      C12     1.3727(3)    . ?
C9      H13     0.9800(5)    . ?
C11     N14     1.1328(9)    . ?
C12     H15     0.9924(2)    . ?


				
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 

Co2     N1      C3       123.4401(1)    . . ?
Co2     N1      C4     	 120.3491(7)    . . ?
C3      N1      C4     	 116.2212(5)    . . ?
N1      Co2     Br5    	  90.3260(6)    . . ?
N1      Co2     Br6    	  89.7239(4)    . . ?
Br5     Co2     Br6    	 180.0000(0)    . . ?
N1      C3      H7     	 117.2345(6)    . . ?
N1      C3      C8     	 120.2880(8)    . . ?
H7      C3      C8     	 122.5494(1)    . . ?
N1      C4      C9     	 126.1806(2)    . . ?
N1      C4      H10    	 118.2278(1)    . . ?
C9      C4      H10    	 115.5890(3)    . . ?
C3      C8      C11    	 121.3757(1)    . . ?
C3      C8      C12    	 122.8495(1)    . . ?
C11     C8      C12    	 115.8082(6)    . . ?
C4      C9      C12    	 118.6048(5)    . . ?
C4      C9      H13    	 118.8493(7)    . . ?
C12     C9      H13    	 122.5281(7)    . . ?
C8      C11     N14    	 171.4768(1)    . . ?
C8      C12     C9     	 115.9350(1)    . . ?
C8      C12     H15    	 118.8343(6)    . . ?
C9      C12     H15    	 125.2148(2)    . . ?

_chemical_name_systematic                  
; 
Dibromo-tetra(3-cyanopyridine)nickelat
;				  
_chemical_name_common             'Dibromo-tetra(3-cyanopyridine)nickelat'		 
_chemical_formula_iupac           'C24 H16 Br2 Co N8 '				 
_chemical_formula_moiety          'C24 H16 Br2 Co N8 '				 
_chemical_formula_structural      'C24 H16 Br2 Co N8 '				 
_chemical_formula_analytical      ? 
_chemical_formula_sum              'C24 H16 Br2 Co N8 '
_chemical_formula_weight          635.18 
_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'
   Co Co '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 1.656

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

# 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         9600
_pd_meas_2theta_range_min         4        
_pd_meas_2theta_range_max         100       
_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      '100'        


_pd_proc_ls_prof_R_factor         0.01039        
_pd_proc_ls_prof_wR_factor        0.01335        
_pd_proc_ls_prof_wR_expected      0.01150        
_refine_ls_R_I_factor             0.01015	  



_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      80      		
_refine_ls_number_restraints      29        		
_refine_ls_number_constraints     1 			
_refine_ls_number_reflns	  ?			
     

_refine_ls_goodness_of_fit_all     1.162      
      
_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         100        
_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_CoBr23-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_CoBr23-cypy4-Pulver
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0098 Ang. 
RESPONSE: X-ray powder data
;
_vrf_PLAT920_CoBr23-cypy4-Pulver
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.16 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_CoBr23-cypy4-Pulver
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0        206       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_CoBr23-cypy4-Pulver
;
PROBLEM: Check Calcd Resid. Dens.  from Br6 and others   
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_CoBr23-cypy4-Pulver
;
PROBLEM: Check Calcd Resid. Dens.  0.13A   From Br5           -49.65 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_CoBr23-cypy4-Pulver
;
PROBLEM: Check Calcd Negative Resid. Density on       Co2     -34.00 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_CoBr23-cypy4-Pulver
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structur was solved from powder data
;
# end Validation Reply Form

