data_NiCl2(3-cypy)2

_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)2]n was prepared from alcoholic solution.
;
_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 [NiBr2(3cypy)2]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 1.2 times of those of the non-hydrogen atoms.
;

_chemical_name_mineral ??
_cell_length_a  3.583700(33)
_cell_length_b  27.28886(29)
_cell_length_c  13.18148(26)
_cell_angle_alpha 90
_cell_angle_beta  97.7149(35)
_cell_angle_gamma 90
_cell_volume 1277.416(32)
_cell_formula_units_Z 4
_space_group C1c1



loop_
_symmetry_equiv_pos_as_xyz
	'x, -y, z+1/2'
	'x, y, z'
	'x+1/2, -y+1/2, z+1/2'
	'x+1/2, y+1/2, 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


Ni1 Ni   0 0.03926(82) 0.87650(17) 0.10048(76) 1 2.32234     0.02941
Cl2 Cl   0 0.4840(20) 0.90106(18) -0.01477(80) 1 2.32234     0.02941
Cl3 Cl   0 -0.3933(17) 0.85396(17) 0.22231(81) 1 2.32234     0.02941
N4 N     0 0.0365(10) 0.80372(16) 0.03739(29) 1 2.32234     0.02941
N5 N     0 0.0833(10) 0.94642(16) 0.15988(29) 1 2.32234     0.02941
C6 C     0 0.0646(11) 0.76658(12) 0.10247(27) 1 2.32234     0.02941
C7 C     0 0.0249(11) 0.79443(13) -0.06275(26) 1 2.32234     0.02941
C8 C     0 0.1782(11) 0.95400(13) 0.26048(26) 1 2.32234     0.02941
C9 C    0 0.0305(12) 0.98426(12) 0.09643(27) 1 2.32234     0.02941
C10 C   0 0.0829(11) 0.71771(13) 0.07210(27) 1 2.32234     0.02941
H11 H   0 0.0759(58) 0.77469(54) 0.1741(13) 1 2.786808     0.03530
C12 C   0 0.0459(11) 0.74740(13) -0.09706(27) 1 2.32234     0.02941
H13 H   0 -0.0100(67) 0.82103(60) -0.1123(14) 1 2.786808     0.03530
C14 C   0 0.2282(11) 1.00037(13) 0.29967(26) 1 2.32234     0.02941
H15 H   0 0.2054(66) 0.92657(60) 0.3073(13) 1 2.786808     0.03530
C16 C   0 0.0722(11) 1.03189(13) 0.13002(27) 1 2.32234     0.02941
H17 H   0 -0.0345(55) 0.97774(57) 0.0243(12) 1 2.786808     0.03530
C18 C   0 0.0783(12) 0.70795(12) -0.03008(26) 1 2.32234     0.02941
C19 C   0 0.1181(15) 0.67815(15) 0.14371(36) 1 2.32234     0.02941
H20 H   0 0.0446(53) 0.74297(91) -0.1698(13) 1 2.786808     0.03530
C21 C   0 0.1740(12) 1.04058(12) 0.23339(27) 1 2.32234     0.02941
H22 H   0 0.3045(52) 1.00334(95) 0.3734(13) 1 2.786808     0.03530
C23 C   0 0.0134(15) 1.07019(15) 0.05610(35) 1 2.32234     0.02941
H24 H   0 0.0870(68) 0.67346(52) -0.0517(16) 1 2.786808     0.03530
N25 N   0 0.1649(26) 0.64795(19) 0.20303(44) 1 2.32234     0.02941
H26 H   0 0.1968(60) 1.07498(53) 0.2559(16) 1 2.786808     0.03530
N27 N   0 -0.0304(24) 1.09999(21) -0.00531(50) 1 2.32234     0.02941

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
 
Ni1     Cl2     2.439(12)    . ?
Ni1     Cl3     2.455(12)    . ?
Ni1     N4      2.153(7)    . ?
Ni1     N5      2.060(7)    . ?
N4      C6      1.3229(54)    . ?
N4      C7      1.3390(52)    . ?
N5      C8      1.3398(51)    . ?
N5      C9      1.3264(53)    . ?
C6      C10     1.3964(48)    . ?
C6      H11     0.965(18)    . ?
C7      C12     1.3658(50)    . ?
C7      H13     0.974(17)    . ?
C8      C14     1.3693(49)    . ?
C8      H15     0.967(17)    . ?
C9      C16     1.3748(48)    . ?
C9      H17     0.964(16)    . ?
C10     C18     1.3708(50)    . ?
C10     C19     1.4286(56)    . ?
C12     C18     1.3871(49)    . ?
C12     H20     0.966(17)    . ?
C14     C21     1.3998(48)    . ?
C14     H22     0.977(18)    . ?
C16     C21     1.3830(49)    . ?
C16     C23     1.4250(55)    . ?
C18     H24     0.985(15)    . ?
C19     N25     1.1325(69)    . ?
C21     H26     0.984(16)    . ?
C23     N27     1.1437(74)    . ?
 
 
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 
 
 Cl2     Ni1     Cl3         177.33(17)    . . ?
 Cl2     Ni1     N4           88.84(16)     . . ?
 Cl2     Ni1     N5           87.7(2)    . . ?
 Cl3     Ni1     N4           92.9(2)     . . ?
 Cl3     Ni1     N5           90.69(16)       . . ?
 N4      Ni1     N5          175.8(2)      . . ?
 Ni1     N4      C6          117.42(23)     . . ?
 Ni1     N4      C7          123.6(4)    . . ?
 C6      N4      C7          118.93(38)     . . ?
 Ni1     N5      C8          121.0(4)    . . ?
 Ni1     N5      C9          118.9(4)     . . ?
 C8      N5      C9          119.96(38)     . . ?
 N4      C6      C10         123.22(37)     . . ?
 N4      C6      H11         116.64(93)        . . ?
 C10     C6      H11         120.13(93)      . . ?
 N4      C7      C12         120.57(35)      . . ?
 N4      C7      H13         120.3(11)          . . ?
 C12     C7      H13         119.1(11)          . . ?
 N5      C8      C14         121.28(34)      . . ?
 N5      C8      H15         120.1(10)        . . ?
 C14     C8      H15         118.6(11)          . . ?
 N5      C9      C16         122.19(34)      . . ?
 N5      C9      H17         118.3(10)        . . ?
 C16     C9      H17         119.5(10)       . . ?
 C6      C10     C18         118.20(32)      . . ?
 C6      C10     C19         122.38(35)      . . ?
 C18     C10     C19         119.39(33)      . . ?
 C7      C12     C18         121.46(33)      . . ?
 C7      C12     H20         117.0(15)         . . ?
 C18     C12     H20         121.6(15)         . . ?
 C8      C14     C21         119.26(32)      . . ?
 C9      C16     C21         118.85(32)      . . ?
 C9      C16     C23         118.27(33)      . . ?
 C21     C16     C23         122.88(33)      . . ?
 C10     C18     C12         117.61(32)      . . ?
 C10     C18     H24         118.2(12)         . . ?
 C12     C18     H24         124.1(12)        . . ?
 C10     C19     N25         176.04(53)     . . ?
 C14     C21     C16         118.45(31)     . . ?
 C8      C14     H22         117.2(15)         . . ?
 C21     C14     H22         123.5(15)        . . ?
 C14     C21     H26         124.1(12)        . . ?
 C16     C21     H26         117.4(11)         . . ?
 C16     C23     N27         177.94(64)     . . ?
 

	        				        
_chemical_name_systematic                  
; 
catena-bis-chloro-di(3-cyanopyridine)nickelat(II)
;				  
_chemical_name_common             'Catena-bis-chloro-di(3-cyanopyridine)nickelat(II)'		 
_chemical_formula_iupac           'C12 H8 Cl2  N4 Ni'				 
_chemical_formula_moiety          'C12 H8 Cl2  N4 Ni'				 
_chemical_formula_structural      'C12 H8 Cl2  N4 Ni'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C12 H8 Cl2  N4 Ni'
_chemical_formula_weight          337.81
_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            monoclinic        
_symmetry_space_group_name_H-M    'C c'        
_symmetry_space_group_name_Hall   'C -2yc'


#_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 1.757

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

# 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         5900
_pd_meas_2theta_range_min         1        
_pd_meas_2theta_range_max         59.99      
_pd_meas_2theta_range_inc         0.01       

_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      '[001]'     


_pd_proc_ls_prof_R_factor         0.02348        
_pd_proc_ls_prof_wR_factor        0.03179       
_pd_proc_ls_prof_wR_expected      0.02468        
_refine_ls_R_I_factor             1.9061	  



_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      181      		
_refine_ls_number_restraints      56       		
_refine_ls_number_constraints     3			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.288   
      
_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        
_pd_proc_2theta_range_max         59.99       
_pd_proc_2theta_range_inc         0.01               
_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_PLAT041_NiCl23-cypy2
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: The sumformula is [NiCl2C12H8N4]n
;
_vrf_PLAT112_NiCl23-cypy2
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem 
RESPONSE: The structure has no higher symmetry.
;
_vrf_PLAT113_NiCl23-cypy2
;
PROBLEM: ADDSYM suggests new space group Fdd2 
RESPONSE: The structure crystallizes in Cc. 
;
_vrf_PLAT314_NiCl23-cypy2
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0142 Ang. 
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT341_NiCl23-cypy2
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0061 Ang.
RESPONSE: The structure was solved from powder data, collected with Mo radiation.
;
_vrf_PLAT802_NiCl23-cypy2
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT860_NiCl23-cypy2
;
PROBLEM: Number of Least-Squares Restraints: 56.   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT920_NiCl23-cypy2
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by 0.24 Degree.
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2018).
;
_vrf_PLAT962_NiCl23-cypy2
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0       1145       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_NiCl23-cypy2
;
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_NiCl23-cypy2
;
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_NiCl23-cypy2
;
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_NiCl23-cypy2
;
PROBLEM: Number C-C Bonds with Positive Residual Density.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT977_NiCl23-cypy2
;
PROBLEM: Check Negative Difference Density on H7 (-0.51 eA-3) and other atoms.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT004_NiCl23-cypy2
;
PROBLEM: Polymeric Structure Found with Maximum Dimension
RESPONSE: The structure is polymeric.
;
# end Validation Reply Form







