data_NiCl2(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
;
[NiCl2(3cypy)1]n was prepared by thermal decomposition of [NiCl2(3cypy)2]n
;
_publ_section_exptl_refinement
;

The first 20 peaks were selected for indexing in CONOGRAPH (Esmaeili et al. , 2017), 
which resulted in an orthorhombic unit cell with Z = 4. 
Structure solution was carried out using simulated annealing in DASH (David et al. , 2004). 
A  molecular starting model was derived from the crystal structure of [NiCl2(3cypy)2]n. 
The Ni atom and the pyridine ring were placed on special position ((x,1/4,z)) and 
the molecular fragment (NiCl2(3cypy)1) was restricted to rotate around the Ni atom during the simulated annealing. 
Rietveld refinement was carried out with TOPAS (Coelho, 2018). 
The Ni atom and the pyridine ring were fixed on y = 1/4 and the Cl atoms were fixed on y = 3/4 during the refinement.
All C-C and C-H angels of the pyridine ring were restrained to be 120°. 
Thermal parameters of hydrogen atoms were constrained to 1.2 times of those of 
the non-hydrogen atoms. 
;

_chemical_name_mineral ??
_cell_length_a  15.90267(41)
_cell_length_b  3.532780(61)
_cell_length_c  14.08069(37)
_cell_angle_alpha 90
_cell_angle_beta  90
_cell_angle_gamma 90
_cell_volume 791.062(32)
_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   0.38823(23) 0.25 0.71487(25) 1 1.24075     0.01571
Ni2 Ni   0 0.48374(10) 0.25 0.61131(11) 1 1.24075     0.01571
C3 C   0   0.40647(19) 0.25 0.80586(22) 1 1.24075     0.01571
C4 C   0   0.30985(19) 0.25 0.68245(22) 1 1.24075     0.01571
Cl5 Cl   0 0.55995(14) 0.75 0.69214(20) 1 1.24075     0.01571
Cl6 Cl   0 0.41173(13) 0.75 0.52102(17) 1 1.24075     0.01571
H7 H   0   0.46632(75) 0.25 0.82680(90) 1 1.4889     0.01886
C8 C   0   0.34189(20) 0.25 0.87133(22) 1 1.24075     0.01571
C9 C   0   0.24368(19) 0.25 0.74574(21) 1 1.24075     0.01571
H10 H   0  0.29936(75) 0.25 0.6121(10) 1 1.4889     0.01886
C11 C   0  0.36517(30) 0.25 0.96962(23) 1 1.24075     0.01571
C12 C   0  0.25955(19) 0.25 0.84457(21) 1 1.24075     0.01571
H13 H   0  0.18628(75) 0.25 0.71957(98) 1 1.4889     0.01886
N14 N   0  0.39487(31) 0.25 1.04463(29) 1 1.24075     0.01571
H15 H   0  0.21515(71) 0.25 0.89448(95) 1 1.4889     0.01886



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      Ni2    2.1055(39)   . ?
N1      C3     1.3136(46) . ?
N1      C4     1.3274(47)  . ?
Ni2     Cl5    2.4258(21)  . ?
Ni2     Cl6    2.4592(19) . ?
C3      H7     0.996(13) . ?
C3      C8     1.3801(43)   .  ?
C4      C9     1.3789(43)   .  ?
C4      H10    1.005(14)    .  ?
C8      C11    1.4327(46)   .  ?
C8      C12    1.3626(43)   .  ?
C9      C12    1.4143(42)   .  ?
C9      H13    0.984(12)    .  ?
C11     N14    1.1570(55)   .  ?
C12     H15    0.996(13)    .  ?

				
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 
 
 
Ni2     N1      C3         121.1(2)  	 . . ?
Ni2     N1      C4         116.1(3) . . ?
C3      N1      C4         122.87(33)	  . . ?
N1      Ni2     Cl5        92.04(10)    	. . ?
N1      Ni2     Cl6        91.27(10) 	 . . ?
Cl5     Ni2     Cl6        87.25(6)   . . ?
N1      C3      H7         119.97(77) . . ?
N1      C3      C8         119.16(30) . . ?
H7      C3      C8         120.88(76)  . . ?
N1      C4      C9         119.62(30)   . . ?
N1      C4      H10        119.67(76)   . . ?
C9      C4      H10        120.70(75)   . . ?
C3      C8      C11        116.94(31)    . . ?
C3      C8      C12        122.03(28)   . . ?
C11     C8      C12        121.03(31)    . . ?
C4      C9      C12        119.98(28)   . . ?
C4      C9      H13        117.76(87)     . . ?
C12     C9      H13        122.26(87)    . . ?
C8      C11     N14        170.88(49)     . . ?
C8      C12     C9         116.33(27)     . . ?
C8      C12     H15        119.08(77)     . . ?
C9      C12     H15        124.57(76)        . . ?
	        				        
_chemical_name_systematic                  
; 
catena-bis-chloro-(3-cyanopyridine)nickelat(II)
;				  
_chemical_name_common             'Catena-bis-chloro-(3-cyanopyridine)nickelat(II)'		 
_chemical_formula_iupac           'C6 H4 Cl2 N2 Ni'				 
_chemical_formula_moiety          'C6 H4 Cl2 N2 Ni'				 
_chemical_formula_structural      'C6 H4 Cl2 N2 Ni'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C6 H4 Cl2 N2 Ni'
_chemical_formula_weight          233.70 
_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'
   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 1.962

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

# 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            'Cu K\a~1~'       
_diffrn_measurement_device_type   'STOE Stadi-P'       
_diffrn_detector                  STOE      
_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         7700
_pd_meas_2theta_range_min         3        
_pd_meas_2theta_range_max         80       
_pd_meas_2theta_range_inc         0.2       

_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         0.02896        
_pd_proc_ls_prof_wR_factor        0.03961       
_pd_proc_ls_prof_wR_expected      0.02235        
_refine_ls_R_I_factor             1.8494	  



_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     1.772   
      
_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         80        
_pd_proc_2theta_range_inc         0.2               
_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_PLAT920_NiCl23-cypy1
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.11 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2018).
;
_vrf_PLAT962_NiCl23-cypy1
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0          4       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT971_NiCl23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  1.19A   From Ni2  (3.41 eA-3) and other atoms.  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_NiCl23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  0.08A   From Cl5   (-16.89 eA-3) and other atoms.  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT974_NiCl23-cypy1
;
PROBLEM: Check Calcd Negative Resid. Density on       Ni2     (-29.44 eA-3) and other atoms.  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT977_NiCl23-cypy1
;
PROBLEM: Check Calcd Negative Resid. Density on  H7 (-0.99 eA-3) and other atoms.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT978_NiCl23-cypy1
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info    
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT860_NiCl23-cypy1
;
PROBLEM: Number of Least-Squares Restraints: 29.   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT004_NiCl23-cypy1
;
PROBLEM: Polymeric Structure Found with Maximum Dimension   
RESPONSE: The structure is polymeric.
;
_vrf_PLAT802_NiCl23-cypy1
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
# end Validation Reply Form






