data_CoCl2(3-cypy)1

_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 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
;
'Coordination compounds built up from MCl2 and 3-cyanopyridine - double chains, single chains and isolated complexes.'
;

_publ_section_references
;
Boultif, A. & Louër, D. (1991). J. Appl. Cryst., 24, 987-993.

Coelho, A. (2018). J. Appl. Cryst., 51, 210-218.


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.

Oishi-Tomiyasu, R. (2014).J. Appl. Cryst., 47, 593-598. 

Oishi-Tomiyasu, R. (2014).J. Appl. Cryst., 47, 20552059. 

STOE & Cie (2004). WinXPOW. STOE and Cie, Darmstadt, Germany.
;

_publ_section_exptl_prep
;
[CoCl2(3cypy)1]n was prepared by thermal decomposition of [CoCl2(3cypy)2]n.
;
_publ_section_exptl_refinement
;
 
At first, a Pawley fit was performed in TOPAS (Coelho, 2018), refining background and instrumental parameters (zero point, axial divergence). 
Next, size and strain parameters were refined.
The crystal structure of [NiCl2(3cypy)1]n was used as starting point for the subsequent structure refinement. 
Rietveld refinement was carried out with TOPAS Coelho, 2018). All C-C and C-H angles of the pyridine ring were restrained to be 120°. 
Thermal parameters of hydrogen atoms were constrained to be 1.2 times of those of the non-hydrogen atoms.
;

_chemical_name_mineral ??
_cell_length_a  16.08629(49)
_cell_length_b  3.587370(97)
_cell_length_c  14.19096(54)
_cell_angle_alpha 90
_cell_angle_beta  90
_cell_angle_gamma 90
_cell_volume 818.93(4)
_cell_formula_units_Z 4
_space_group Pnma



loop_
_symmetry_equiv_pos_as_xyz
	'-x, -y, -z'
	'-x, y+1/2, -z'
	'-x+1/2, -y, z+1/2'
	'-x+1/2, y+1/2, z+1/2'
	'x, -y+1/2, z'
	'x, y, z'
	'x+1/2, -y+1/2, -z+1/2'
	'x+1/2, y, -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 0.61411(34) 0.25 0.28669(38) 1 2.08906     0.02646
Co2 Co 0 0.51423(16) 0.25 0.38769(17) 1 2.08906     0.02646
C3 C   0 0.59377(28) 0.25 0.19684(34) 1 2.08906     0.02646
C4 C   0 0.69264(28) 0.25 0.31730(33) 1 2.08906     0.02646
Cl5 Cl 0 0.43982(29) 0.75 0.30674(33) 1 2.08906     0.02646
Cl6 Cl 0 0.58802(26) 0.75 0.47830(30) 1 2.08906     0.02646
H7 H   0 0.5339(12) 0.25 0.1774(12) 1 2.506872     0.03175
C8 C   0 0.65724(30) 0.25 0.13143(33) 1 2.08906     0.02646
C9 C   0 0.7572(29) 0.25 0.25330(32) 1 2.08906     0.02646
H10 H  0 0.7038(11) 0.25 0.3870(16) 1 2.506872     0.03175
C11 C  0 0.63473(52) 0.25 0.03397(34) 1 2.08906     0.02646
C12 C  0 0.73961(29) 0.25 0.15693(32) 1 2.08906     0.02646
H13 H  0 0.8153(12) 0.25 0.2754(15) 1 2.506872     0.03175
N14 N  0 0.61086(56) 0.25 -0.04268(44) 1 2.08906     0.02646
H15 H  0 0.7842(10) 0.25 0.1074(15) 1 2.506872     0.03175


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    2.1531(60)   . ?
N1      C3     1.3164(72) . ?
N1      C4     1.3359(72)  . ?
Co2     Cl5    2.4433(35)  . ?
Co2     Cl6    2.5059(35) . ?
C3      H7     1.002(19) . ?
C3      C8     1.3798(67)  .  ?
C4      C9     1.3796(66)   .  ?
C4      H10    1.006(23)     .  ?
C8      C11    1.4297(68)   .  ?
C8      C12    1.3736(67)   .  ?
C9      C12    1.3965(65)   .  ?
C9      H13    0.985(20)   .  ?
C11     N14    1.1536(85)   .  ?
C12     H15    1.005(19)    .  ?

				
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         117.4(4)	 . . ?
Co2     N1      C4         119.3(4) . . ?
C3      N1      C4         123.36(50)  . . ?
N1      Co2     Cl5        93.01(16)    	. . ?
N1      Co2     Cl6        89.32(16) 	 . . ?
Cl5     Co2     Cl6        87.02(11)  . . ?
N1      C3      H7         120.4(11) . . ?
N1      C3      C8         117.89(46) . . ?
H7      C3      C8         121.7(11) . . ?
N1      C4      C9         119.85(45)  . . ?
N1      C4      H10        119.2(11)  . . ?
C9      C4      H10        120.9(11)  . . ?
C3      C8      C11        117.60(51)   . . ?
C3      C8      C12        122.45(44)  . . ?
C11     C8      C12        119.95(51)    . . ?
C4      C9      C12        119.48(43)  . . ?
C4      C9      H13        120.3(12)     . . ?
C12     C9      H13        120.2(12)   . . ?
C8      C11     N14        175.23(86)    . . ?
C8      C12     C9         116.96(42)    . . ?
C8      C12     H15        120.3(12)    . . ?
C9      C12     H15        122.7(12)       . . ?
	        				        
_chemical_name_systematic                  
; 
catena-bis-chloro-(3-cyanopyridine)cobaltat(II)
;				  
_chemical_name_common             'Catena-bis-chloro-(3-cyanopyridine)cobaltat(II)'		 
_chemical_formula_iupac           'C6 H4 Cl2 Co N2 '				 
_chemical_formula_moiety          'C6 H4 Cl2 Co N2 '				 
_chemical_formula_structural      'C6 H4 Cl2 Co N2 '				 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C6 H4 Cl2 Co N2'
_chemical_formula_weight          233.94 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   'light violet' 
 
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'
   Cl Cl '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 m a'        
_symmetry_space_group_name_Hall   '-P 2ac 2n'


#_pd_spec_size_axial   12

#_pd_spec_size_equat   0.7

# _pd_spec_size_thick   0.7


# The next four fields are character fields that describe the specimen.

_pd_spec_mounting                         
;
Specimen was measured in a boro silicate glass capillary (Hilgenberg).
;

_pd_spec_mount_mode               'transmission'

_pd_spec_shape                    ?

_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 1.898

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

# 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             STOE
_diffrn_source_type               STOE
_diffrn_radiation_type            'Mo K\a~1~'       
_diffrn_measurement_device_type   'STOE Stadi-P'       
_diffrn_detector	          Dectris      
_diffrn_detector_type             'Mythen silicon strip detector'
_diffrn_radiation_source   	     'X-ray tube'
_exptl_crystal_F_000        	  ?	    			    

_pd_meas_scan_method              step       


_diffrn_radiation_wavelength      0.70930        
_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         3906
_pd_meas_2theta_range_min         1.5        
_pd_meas_2theta_range_max         60.075      
_pd_meas_2theta_range_inc         0.21       

_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, 2018)
;        
_pd_proc_ls_background_function   'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr      'none'     


_pd_proc_ls_prof_R_factor         0.03103        
_pd_proc_ls_prof_wR_factor        0.04133       
_pd_proc_ls_prof_wR_expected      0.03416        
_refine_ls_R_I_factor             1.6026	  



_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      71      		
_refine_ls_number_restraints      29       		
_refine_ls_number_constraints     1			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.210   
      
_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         1.92        
_pd_proc_2theta_range_max         60.075       
_pd_proc_2theta_range_inc         0.21               
_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, 2018)'
_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_PUBL012_GLOBAL
;
PROBLEM: _publ_section_abstract is missing.
RESPONSE: Abstract will be given later.
;
_vrf_PLAT341_CoCl23-cypy1
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0142 Ang. 
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT802_CoCl23-cypy1
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT860_CoCl23-cypy1
;
PROBLEM: Number of Least-Squares Restraints: 29.   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT920_CoCl23-cypy1
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by 0.25 Degree.
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2018).
;
_vrf_PLAT962_CoCl23-cypy1
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0       1145       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_CoCl23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  0.11A   From Cl5 (-46.70 eA-3) and other atoms.             
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT971_CoCl23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  1.19A   From Cl5 (2.47 eA-3) and other atoms.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT974_CoCl23-cypy1
;
PROBLEM: Check Calcd Negative Resid. Density on       Co2 (-81.79 eA-3) and other atoms.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT978_CoCl23-cypy1
;
PROBLEM: Number C-C Bonds with Positive Residual Density.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT977_CoCl23-cypy1
;
PROBLEM: Check Negative Difference Density on H7 (-0.51 eA-3) and other atoms.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT004_CoCl23-cypy1
;
PROBLEM: Polymeric Structure Found with Maximum Dimension
RESPONSE: The structure is polymeric.
;
# end Validation Reply Form







