data_beta-ZnCl2(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
;
Beta-ZnCl2(3cypy)2 was prepared from alcoholic solution. Beta-ZnCl2(3cypy)2 is the thermodynamically stable polymorph.
;
_publ_section_exptl_refinement
;

The first 20 peaks were selected for indexing in CONOGRAPH (Esmaeili et al. , 2017), 
which resulted in an monoclinic unit cell with Z = 4. 
Structure solution was carried out using simulated annealing 
in DASH (David et al. , 2004) using a starting molecular model derived from the crystal structure of alpha[ZnCl2(3cypy)2]. 
The molecular fragment was restricted to rotate around the Zn atom. 
Rietveld refinement was carried out with TOPAS (Coelho, 2018). The Zn and Cl atoms were fixed on y = 1/4.
All C-C and C-H angels of the pyridine ring were restraint 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  11.66192(15)
_cell_length_b  15.07309(18)
_cell_length_c  8.057182(98)
_cell_angle_alpha 90
_cell_angle_beta  91.01108(86)
_cell_angle_gamma 90
_cell_volume 1416.081(31)
_cell_formula_units_Z 4
_space_group P21/c



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


Zn1 Zn   0 0.25131(11) 0.408886(85) 0.82136(17) 1 3.69474     0.0467
N2 N     0 0.12653(19) 0.31903(15) 0.87470(26) 1 3.69474     0.04679
N3 N     0 0.36803(19) 0.41117(14) 1.01483(29) 1 3.69474     0.04679
Cl4 Cl   0 0.34988(22) 0.35280(14) 0.61822(32) 1 3.69474     0.04679
Cl5 Cl   0 0.17587(20) 0.54098(15) 0.82143(28) 1 3.69474     0.04679
C6 C     0 0.15120(17) 0.23463(12) 0.85303(32) 1 3.69474     0.04679
C7 C     0 0.02465(16) 0.34316(13) 0.93056(26) 1 3.69474     0.04679
C8 C     0 0.44511(18) 0.34588(13) 1.01463(26) 1 3.69474     0.04679
C9 C     0 0.37025(18) 0.47301(14) 1.13326(24) 1 3.69474     0.04679
H10 H    0 0.2258(14)  0.21886(73) 0.8118(18) 1 4.433688     0.05615
C11 C    0 0.07552(17) 0.16773(13) 0.88551(33) 1 3.69474     0.04679
C12 C   0 -0.05642(16) 0.27846(13) 0.96578(30) 1 3.69474     0.04679
H13 H    0 0.00869(99) 0.40807(91) 0.9447(16) 1 4.433688     0.05615
H14 H    0 0.4411(11)  0.30185(90) 0.9224(17) 1 4.433688     0.05615
C15 C    0 0.52858(18) 0.34240(14) 1.14057(26) 1 3.69474     0.04679
C16 C    0 0.45206(17) 0.47167(14) 1.25965(26) 1 3.69474     0.04679
H17 H    0 0.3123(11)  0.52125(79) 1.1311(14) 1 4.433688     0.05615
C18 C    0 0.09975(32) 0.07526(13) 0.86185(51) 1 3.69474     0.04679
C19 C   0 -0.02920(17) 0.19014(12) 0.94183(33) 1 3.69474     0.04679
H20 H   0 -0.1332(11)  0.29460(87) 1.0082(16) 1 4.433688     0.05615
C21 C    0 0.61478(20) 0.27379(16) 1.15242(51) 1 3.69474     0.04679
C22 C   0  0.53254(17) 0.40550(14) 1.26326(27) 1 3.69474     0.04679
H23 H   0 0.4539(12) 0.51643(97) 1.3495(13) 1 4.433688     0.05615
N24 N   0 0.12009(48) 0.00174(16) 0.84012(62) 1 3.69474     0.04679
H25 H   0 -0.0797(11) 0.13994(87) 0.9624(15) 1 4.433688     0.05615
N26 N   0 0.68464(30) 0.21963(22) 1.15874(57) 1 3.69474     0.04679
H27 H   0 0.5916(10) 0.40377(98) 1.3521(15) 1 4.433688     0.05615


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
 

 Zn1     N2      2.0393(25)    .  ?
 Zn1     N3      2.0516(26)    .  ?
 Zn1     Cl4     2.1866(29)    .  ?
 Zn1     Cl5     2.1768(26)    .  ?
 N2      C6      1.3167(29)    .  ?
 N2      C7      1.3286(29)    .  ?
 N3      C8      1.3329(29)    .  ?
 N3      C9      1.3339(30)    .  ?
 C6      H10     0.9666(63)     .  ?
 C6      C11     1.3684(28)    .  ?
 C7      C12     1.3910(28)    .  ?
 C7      H13     1.003(14)     .  ?
 C8      H14     0.997(13)     .  ?
 C8      C15     1.3946(29)    .  ?
 C9      C16     1.3833(29)    .  ?
 C9      H17     0.992(13)     .  ?
 C11     C18     1.4356(29)    .  ?
 C11     C19     1.3532(30)    .  ?
 C12     C19     1.3829(28)    .  ?
 C12     H20     0.994(14)     .  ?
 C15     C21     1.4442(32)    .  ?
 C15     C22     1.3720(30)    .  ?
 C16     C22     1.3695(30)    .  ?
 C16     H23     0.989(13)     .  ?
 C18     N24     1.1473(35)    .  ?
 C19     H25     0.975(13)     .  ?
 C21     N26     1.1539(42)    .  ?
 C22     H27     0.985(12)     .  ?
 
 			
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 
 
 
 N2      Zn1     N3      108.48(11)               .  .  ?
 N2      Zn1     Cl4     106.68(11)               .  .  ?
 N2      Zn1     Cl5     108.57(10)               .  .  ?
 N3      Zn1     Cl4     102.92(10)               .  .  ?
 N3      Zn1     Cl5     104.37(10)               .  .  ?
 Cl4     Zn1     Cl5     124.88(11)               .  .  ?
 Zn1     N2      C6      117.19(17)               .  .  ?
 Zn1     N2      C7      122.38(17)               .  .  ?
 C6      N2      C7      120.54(20)              .  .  ?
 Zn1     N3      C8      115.22(17)               .  .  ?
 Zn1     N3      C9      123.97(17)               .  .  ?
 C8      N3      C9       120.82(21)             .  .  ?
 N2      C6      H10      118.90(72)             .  .  ?
 N2      C6      C11      122.93(19)             .  .  ?
 H10     C6      C11      118.17(71)             .  .  ?
 N2      C7      C12      119.49(19)             .  .  ?
 N2      C7      H13      118.31(71)             .  .  ?
 C12     C7      H13      122.19(71)             .  .  ?
 N3      C8      H14      118.02(79)             .  .  ?
 N3      C8      C15      119.27(19)             .  .  ?
 H14     C8      C15      122.70(80)             .  .  ?
 N3      C9      C16      121.39(20)             .  .  ?
 N3      C9      H17      119.68(68)             .  .  ?
 C16     C9      H17      118.93(69)             .  .  ?
 C6      C11     C18      124.13(23)             .  .  ?
 C6      C11     C19      117.98(18)             .  .  ?
 C18     C11     C19      117.89(22)             .  .  ?
 C7      C12     C19      119.21(19)             .  .  ?
 C7      C12     H20      121.20(77)             .  .  ?
 C19     C12     H20      119.59(77)             .  .  ?
 C8      C15     C21      123.45(22)             .  .  ?
 C8      C15     C22      120.82(19)             .  .  ?
 C21     C15     C22      115.73(22)             .  .  ?
 C9      C16     C22      119.33(20)             .  .  ?
 C9      C16     H23      122.28(78)             .  .  ?
 C22     C16     H23      118.38(78)             .  .  ?
 C11     C18     N24      178.69(53)             .  .  ?
 C11     C19     C12      119.85(19)             .  .  ?
 C11     C19     H25      114.49(82)             .  .  ?
 C12     C19     H25      125.65(83)             .  .  ?
 C15     C21     N26      178.53(43)             .  .  ?
 C15     C22     C16      118.37(19)             .  .  ?
 C15     C22     H27      121.29(81)             .  .  ?
 C16     C22     H27      120.34(83)             .  .  ?
 
 

_chemical_name_systematic                  
; 
Beta-dichlorido-di(3-cyanopyridine)zinc
;				  
_chemical_name_common             'Beta-dichlorido-di(3-cyanopyridine)zinc'		 
_chemical_formula_iupac           'C12 H8 Cl2 N4 Zn'				 
_chemical_formula_moiety          'C12 H8 Cl2 N4 Zn'				 
_chemical_formula_structural      'C12 H8 Cl2 N4 Zn'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C12 H8 Cl2 N4 Zn'
_chemical_formula_weight          344.51 
_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'
   Zn Zn '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    'P 1 21/c 1'        
_symmetry_space_group_name_Hall   '-P 2ybc'


#_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 placed in a 0.7 mm diameter borosilicate 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 1.616

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

# 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         9700
_pd_meas_2theta_range_min         4        
_pd_meas_2theta_range_max         100       
_pd_meas_2theta_range_inc         0.1       

_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         0.02172        
_pd_proc_ls_prof_wR_factor        0.02791     
_pd_proc_ls_prof_wR_expected      0.02109       
_refine_ls_R_I_factor             0.00868	  



_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      156     		
_refine_ls_number_restraints      58      		
_refine_ls_number_constraints     3		
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.323    
      
_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         4        
_pd_proc_2theta_range_max         100        
_pd_proc_2theta_range_inc         0.1               
_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_beta-ZnCl23-cypy2
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.23 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2018).
;
_vrf_PLAT962_beta-ZnCl23-cypy2
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0        243       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT971_beta-ZnCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  1.02A   From Zn1 and other atoms.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_beta-ZnCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  0.23A   From Cl5  and other atoms         -19.48 eA-3  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT974_beta-ZnCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density on       Zn1 and other atoms     -40.24 eA-3  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT977_beta-ZnCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density on       H10     and other atoms.  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT978_beta-ZnCl23-cypy2
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info    
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT802_beta-ZnCl23-cypy2
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT860_beta-ZnCl23-cypy2
;
PROBLEM: Number of Least-Squares Restraints .............         58 Note  
RESPONSE: The structure was solved from powder data.
;
# end Validation Reply Form


