data_CoBr2(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              '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
;
20 reflections in the low angle range were selected for indexing in DASH (Louër et al. , 2017),
which led in an orthorhombic unit cell with Z = 2 and lattice parameters similar to those of MnBr2(3cypy)2. 
A starting molecular model was derived from the known crystal structure of [CoBr2(3cypy)4]. 
The molecular fragment was restricted to rotate around the Co-atom; Co-atom and 3-cyanopyridine were fixed on a special position (0,0,0) during the simulated annealing. 
The Rietveld refinement was carried out with TOPAS (Coelho, 2007). 
The Co atom was restraint on the origin, the 3-cyanopyridine was 
restrained flat in the mirror plane, the Br atom was fixed on (0/0.5/0).
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.  
The final crystallographic data of (a-3b) were taken from the simultaneous Rietveld refinement of the two polymorphic structures.
;

_chemical_name_mineral ??
_cell_length_a    27.0190(16)
_cell_length_b     7.1242(9)
_cell_length_c     3.7597(5)
_cell_angle_alpha  90
_cell_angle_beta   90
_cell_angle_gamma  90
_cell_volume       723.70(14)
_cell_formula_units_Z 2
_space_group Pnnm
loop_
_symmetry_equiv_pos_as_xyz
	'-x, -y, -z'
	'-x, -y, z'
	'-x+1/2, y+1/2, -z+1/2'
	'-x+1/2, y+1/2, z+1/2'
	'x, y, -z'
	'x, y, z'
	'x+1/2, -y+1/2, -z+1/2'
	'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


C1 C         0 0.665(7)  0.394(6)    0.5   1 3.30105     0.04181
C2 C         0 0.708(1)  0.519(5)    0.5   1 3.30105     0.04181
C3 C         0 0.618(6)  0.469(8)    0.5   1 3.30105     0.04181
C4 C         0 0.671(5)  0.201(5)    0.5   1 3.30105     0.04181
N5 N         0 0.741(4)  0.618(6)    0.5   1 3.30105     0.04181
N6 N         0 0.578(5)  0.362(4)    0.5   1 3.30105     0.04181
H7 H         0 0.614(3)  0.607(1)    0.5   1 3.96126     0.05017
C8 C         0 0.629(1)  0.091(9)    0.5   1 3.30105     0.04181
H9 H         0 0.705(4)  0.142(6)    0.5   1 3.96126     0.05017
Co10 Co      0 0.5 	 0.5   	     0.5   1 3.30105     0.04181
C11 C        0 0.582(3)  0.171(4)    0.5   1 3.30105     0.04181
H12 H        0 0.632(3) -0.045(4)    0.5   1 3.96126     0.05017
Br13 Br      0 0.530(1)  0.723(3)    1.0   1 3.30105     0.04181
H14 H        0 0.551(6)  0.095(6)    0.5   1 3.96126     0.05017


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
 

C1      C2    	1.4521(1)   . ?
C1      C3    	1.3808(6)   . ?
C1      C4    	1.3850(6)   . ?
C2      N5    	1.1416(9)   . ?
C3      N6    	1.3259(4)   . ?
C3      H7    	0.9854(8)   . ?
C4      C8    	1.3870(9)   . ?
C4      H9    	1.0074(9)   . ?
N6      Co10  	2.3366(2)   . ?
N6      C11   	1.3648(4)   . ?
C8      C11   	1.3844(6)   . ?
C8      H12   	0.9791(1)   . ?
Co10    Br13  	2.5933(6)   . ?
C11     H14   	0.9921(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 
 
 
C2      C1      C3     119.3738(9)  . . ?
C2      C1      C4     121.2710(3) . . ?
C3      C1      C4     119.3550(9) . . ?
C1      C2      N5     179.6226(6) . . ?
C1      C3      N6     121.9437(1)  . . ?
C1      C3      H7     119.6116(6)  . . ?
N6      C3      H7     118.4445(3) 	 . . ?
C1      C4      C8     117.7380(9)  	 . . ?
C1      C4      H9     121.1127(1)    . . ?
C8      C4      H9     121.1492(1) 	   . . ?
C3      N6      Co10   119.9657(9) 	   . . ?
C3      N6      C11    120.8599(7)    . . ?
Co10    N6      C11    119.1743(5) 	    . . ?
C4      C8      C11    121.5547(8) 	    . . ?
C4      C8      H12    119.1705(8)     . . ?
C11     C8      H12    119.2747(4) 	    . . ?
N6      Co10    Br13    88.4748(6)   	     . . ?
N6      C11     C8     118.5484(8)      . . ?
N6      C11     H14    118.6554(1)       . . ?
C8      C11     H14    122.7961(2)       . . ?
				 
				 


_chemical_name_systematic                  
; 
alpha-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   '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            orthorhombic        
_symmetry_space_group_name_H-M    'P  n n m'        
_symmetry_space_group_name_Hall   '-P 2 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 0.5 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 1.941

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

# 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         4960
_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      70      		
_refine_ls_number_restraints      34        		
_refine_ls_number_constraints     1 			
_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-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_CoBr23-cypy2-alpha
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0176 Ang. 
RESPONSE: X-ray powder data
;
_vrf_PLAT920_CoBr23-cypy2-alpha
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.25 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_CoBr23-cypy2-alpha
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0        162       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_CoBr23-cypy2-alpha
;
PROBLEM: Check Calcd Resid. Dens.   From Br13          2.34 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_CoBr23-cypy2-alpha
;
PROBLEM: Check Calcd Resid. Dens.  1.76A   From Br13          -39.17 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_CoBr23-cypy2-alpha
;
PROBLEM: Check Calcd Negative Resid. Density on      Co10     -25.60 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_CoBr23-cypy2-alpha
;
PROBLEM: Check Negative Difference Density on H7 -0.50 eA-3 and H14  -1.02 eA-3
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_CoBr23-cypy2-alpha
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form


