data_CoBr2(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              '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 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
;
CoBr2(3cypy)2 was prepared by thermal decomposition of CoBr2(3cypy)4.
;
_publ_section_exptl_refinement
; 
A starting molecular model was derived from the known crystal structure of [CoBr2(3cypy)2]n. 
The molecular fragment was restricted to rotate around the Co-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     3.757(1)
_cell_length_b    13.625(1)
_cell_length_c    13.868(7)
_cell_angle_alpha 87.377(2)
_cell_angle_beta  82.344(2)
_cell_angle_gamma 82.405(1)
_cell_volume      697.22(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

Co1 Co   0  0 		0.5 	   0.5 		1 3.6824     0.04662
Br2 Br   0  0.420(8)   0.623(7)   0.545(8)     	1 3.6824     0.04662
N5 N     0  0.070(1)   0.555(2)   0.371(1)    	1 3.6824     0.04662
C8 C     0  0.126(1)   0.493(3)   0.297(5)      1 3.6824     0.04662
C9 C     0  0.046(1)   0.654(1)   0.359(8)    	1 3.6824     0.04662
C14 C    0  0.157(1)   0.536(1)   0.205(7)      1 3.6824     0.04662
H15 H    0  0.175(9)   0.418(9)   0.305(4)    	1 4.4229     0.05594
C16 C    0  0.065(1)   0.704(3)   0.267(3)    	1 3.30105    0.04181
H17 H    0  0.033(8)   0.687(8)   0.423(5)    	1 4.4229     0.05594
C21 C    0  0.129(1)   0.638(6)   0.188(9)    	1 3.6824     0.04662
C22 C    0  0.204(1)   0.465(3)   0.131(6)    	1 3.6824     0.04662
H23 H    0  0.021(1)   0.783(1)   0.260(1)    	1 4.4229     0.05594
H26 H    0  0.166(9)   0.662(7)   0.120(2)    	1 4.4229     0.05594
N27 N    0  0.243(1)   0.405(1)   0.075(7)    	1 3.6824     0.04662

Co102 Co 0   1 		 0 	      0 	1 3.6824     0.04662
Br202 Br 0   0.531(6)    -0.123(7)     0.047(7)  1 3.6824     0.04662
N402 N   0   0.942(9)     0.057(5)     0.140(2)	1 3.6824     0.04662
C602 C   0   0.933(1)    -0.008(2)     0.213(6)  1 3.6824     0.04662
C702 C   0   0.893(1)     0.152(7)     0.159(9)	1 3.6824     0.04662
C1002 C  0   0.875(1)     0.019(8)     0.308(3)  1 3.6824     0.04662
H1102 H  0   0.959(02)   -0.079(5)     0.201(9)	1 4.4229     0.05594
C1202 C  0   0.837(1)     0.182(4)     0.254(1)	1 3.30105    0.04181
H1302 H  0   0.909(6)     0.201(7)     0.106(9)	1 4.4229     0.05594
C1802 C  0   0.826(6)     0.117(4)     0.329(7)	1 3.6824     0.04662
C1902 C  0   0.864(1)    -0.056(1)     0.381(9)	1 3.6824     0.04662
H2002 H  0   0.812(7)     0.251(1)     0.271(1)	1 4.4229     0.05594
H2402 H  0   0.774(6)     0.142(3)     0.395(9)	1 4.4229     0.05594
N2502 N  0   0.85(1)    -0.118(8)     0.438(7)	1 3.6824     0.04662


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
 

Co1     Br2    2.574(5)   	. ?
Co1     N5     1.913(8)    	. ?
N5      C8     1.330(3)   	. ?
N5      C9     1.341(1)   	. ?
C8      C14    1.371(6)   	. ?
C8      H15    1.009(1)   	. ?
C9      C16    1.423(1)   	. ?
C9      H17    1.006(1)   	. ?
C14     C21    1.398(4)   	. ?
C14     C22    1.421(2)   	. ?
C16     C21    1.415(1)   	. ?
C16     H23    1.069(1)   	. ?
C21     H26    0.991(1)   	. ?
C22     N27    1.135(4)   	. ?


Co102    Br202     2.573(6)     . ?
Co102    N402      2.119(8)     . ?
N402     C602      1.325(3)     . ?
N402     C702      1.321(4)     . ?
C602     C1002     1.365(4)     . ?
C602     H1102     0.981(7)     . ?
C702     C1202     1.366(1)     . ?
C702     H1302     0.970(2)     . ?
C1002    C1802     1.359(1)     . ?
C1002    C1902     1.419(4)     . ?
C1202    C1802     1.342(3)     . ?
C1202    H2002     0.957(4)     . ?
C1802    H2402     0.978(7)     . ?
C1902    N2502     1.137(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 
 
Br2     Co1     N5 	 87.212(1)    . . ?
Co1     N5      C8 	117.135(9)   . . ?
Co1     N5      C9 	119.369(1)   . . ?
C8      N5      C9 	124.018(8)   . . ?
N5      C8      C14	116.116(6)    . . ?
N5      C8      H15	124.164(7)    . . ?
C14     C8      H15	119.340(1)	 . . ?
N5      C9      C16	123.308(9)    	 . . ?
N5      C9      H17	112.323(6)      . . ?
C16     C9      H17	124.199(3)	   . . ?
C8      C14     C21	122.802(8)	   . . ?
C8      C14     C22	112.608(6)      . . ?
C21     C14     C22	124.541(6)	    . . ?
C9      C16     C21	112.810(4)	    . . ?
C9      C16     H23	122.163(1)       . . ?
C21     C16     H23	124.913(4)	    . . ?
C14     C21     C16	120.884(3)     	     . . ?
C14     C21     H26	117.108(1)        . . ?
C16     C21     H26	121.972(8)         . . ?
C14     C22     N27	176.615(7)         . . ?


Br202    Co102    N402        92.395(7) 	      . . ?
Co102     N402     C602      118.385(2) 	     . . ?
Co102     N402     C702      121.654(3) 	     . . ?
C602      N402     C702      118.635(2) 	     . . ?
N402     C602     C1002      121.851(3) 	      . . ?
N402     C602     H1102      120.925(7) 	      . . ?
C1002     C602     H1102     117.209(2) 	      . . ?
N402      C702     C1202     120.504(1) 	      	 . . ?
N402      C702     H1302     119.559(7) 	        . . ?
C1202     C702     H1302     119.868(5) 	        . . ?
C602      C1002    C1802     120.229(5) 	        . . ?
C602      C1002    C1902     117.661(3) 	        . . ?
C1802     C1002    C1902     122.099(5) 	         . . ?
C702      C1202    C1802     122.064(5) 	         . . ?
C702      C1202    H2002     122.578(2) 	         . . ?
C1802     C1202    H2002     115.325(6) 	         . . ?
C1002    C1802    C1202      116.711(4) 	       	     . . ?
C1002    C1802    H2402      124.140(5) 	          . . ?
C1202    C1802    H2402      119.117(6) 	           . . ?
C1002    C1902    N2502      177.594(2) 	           . . ?


_chemical_name_systematic                  
; 
beta-Catena-dibromo-di(3-cyanopyridine)cobaltat
;				  
_chemical_name_common             'Dibromo-bis(3-cyanopyridine)cobaltat'		 
_chemical_formula_iupac           'C12 H8 Br2 Co N4'				 
_chemical_formula_moiety          'C12 H8 Br2 Co N4'				 
_chemical_formula_structural      'C12 H8 Br2 Co N4'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum              'C12 H8 Br2 Co N4'
_chemical_formula_weight          426.95 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   'green' 
 
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            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 2.034

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

# 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         8200
_pd_meas_2theta_range_min         3        
_pd_meas_2theta_range_max         85
_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         0.01388        
_pd_proc_ls_prof_wR_factor        0.01823        
_pd_proc_ls_prof_wR_expected      0.01286        
_refine_ls_R_I_factor             0.00780	  



_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      155      		
_refine_ls_number_restraints      70        		
_refine_ls_number_constraints     3 			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.417      
      
_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         85        
_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-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_PLAT112_CoBr23-cypy2-beta
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         m
RESPONSE: symmetry was checked, no additional symmetry element
;
_vrf_PLAT113_CoBr23-cypy2-beta
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       I2/m
RESPONSE: symmetry was checked, no higher symmetry
;
_vrf_PLAT341_CoBr23-cypy2-beta
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.106 Ang.  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT411_CoBr23-cypy2-beta
;
PROBLEM: Short Inter H...H Contact  H1102    ..H23              2.01 Ang.
RESPONSE: structure was solved from powder data
;
_vrf_PLAT920_CoBr23-cypy2-beta
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.22 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_CoBr23-cypy2-beta
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         27       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_CoBr23-cypy2-beta
;
PROBLEM: Check Calcd Resid. Dens.  1.12A   From Br2             3.52 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_CoBr23-cypy2-beta
;
PROBLEM: Check Calcd Resid. Dens.  0.02A   From Br2           -39.83 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_CoBr23-cypy2-beta
;
PROBLEM: Check Calcd Negative Resid. Density on       Co1     -26.90 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_CoBr23-cypy2-beta
;
PROBLEM: Check Negative Difference Density on H1102 -1.13 eA-3 
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_CoBr23-cypy2-beta
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form


