data_alpha-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
;
alpha-ZnCl2(3cypy)2 was prepared from alcoholic solution. It easily transforms into beta-ZnCl2(3cypy)2
;
_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 then carried out using simulated annealing 
with DASH(David et al. , 2004). 
A starting molecular model was derived from the crystal structure of [ZnBr2(3cypy)2]. 
The Zn and Cl atoms were placed on special position ((x,1/4,z)); the molecular fragment 
was restricted to rotate around the Zn atom during simulated annealing.
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 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. Preferred orientation was observed and thus refined.
;

_chemical_name_mineral ??
_cell_length_a     10.66526(25)
_cell_length_b     20.39976(48)
_cell_length_c    6.61154(17)
_cell_angle_alpha 90
_cell_angle_beta  90
_cell_angle_gamma 90
_cell_volume      1438.464(61)
_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 0.40063(27) 0.32723(14) -0.03395(40) 1 6.35863     0.08053
C2 C   0 0.48807(24) 0.34822(13) 0.09281(36) 1 6.35863     0.08053
C3 C   0 0.38148(24) 0.35346(13) -0.21483(36) 1 6.35863     0.08053
Zn4 Zn   0 0.28771(21) 0.25 0.06990(35) 1 6.35863     0.08053
H5 H   0 0.4975(11) 0.32685(45) 0.2282(16) 1 7.630356     0.09664
C6 C   0 0.56470(23) 0.39932(12) 0.03855(36) 1 6.35863     0.08053
C7 C   0 0.45598(22) 0.40528(11) -0.27600(36) 1 6.35863     0.08053
H8 H   0 0.31360(99) 0.33523(47) -0.3055(15) 1 7.630356     0.09664
Cl9 Cl   0 0.11710(32) 0.25 -0.10284(58) 1 6.35863     0.08053
Cl10 Cl   0 0.27837(35) 0.25 0.39848(53) 1 6.35863     0.08053
C11 C   0 0.66207(26) 0.42319(16) 0.17381(45) 1 6.35863     0.08053
C12 C   0 0.54771(24) 0.42758(12) -0.14695(35) 1 6.35863     0.08053
H13 H   0 0.4446(11) 0.42604(44) -0.4124(20) 1 7.630356     0.09664
N14 N   0 0.74054(36) 0.44186(20) 0.28141(62) 1 6.35863     0.08053
H15 H   0 0.60220(97) 0.46473(51) -0.1891(17) 1 7.630356     0.09664

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      C2     1.3249(37)   . ?
N1      C3     1.3260(36) . ?
N1      Zn4    2.0986(32)  . ?
C2      H5     1.001(11)  . ?
C2      C6     1.3723(35) . ?
C3      C7     1.3829(34) . ?
C3      H8     1.011(10) . ?
Zn4     Cl9    2.1483(42)  . ?
Zn4     Cl10   2.1747(42)   . ?
C6      C11    1.4544(38) . ?
C6      C12    1.3672(34) . ?
C7      C12    1.3755(34) . ?
C7      H13    1.004(13) . ?
C11     N14    1.1626(50) . ?
C12     H15    0.995(11) . ?

				
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      N1      C3         123.265(261)    	 . . ?
C2      N1      Zn4        116.1(2)     	 . . ?
C3      N1      Zn4        120.7(2)    	  . . ?
N1      C2      H5         119.743(664)     	. . ?
N1      C2      C6         119.953(236)     	 . . ?
H5      C2      C6         120.301(673)    . . ?
N1      C3      C7         118.929(238)   . . ?
N1      C3      H8         119.785(638)   . . ?
C7      C3      H8         121.283(635)    . . ?
N1      Zn4     Cl9        108.303(124)      . . ?
N1      Zn4     Cl10       110.723(127)      . . ?
Cl9     Zn4     Cl10       119.489(167)      . . ?
C2      C6      C11        121.252(233)      . . ?
C2      C6      C12        118.415(230)      . . ?
C11     C6      C12        120.332(231)      . . ?
C3      C7      C12        118.688(220)      . . ?
C3      C7      H13        121.070(650)       . . ?
C12     C7      H13        120.234(667)       . . ?
C6      C11     N14        179.441(447)        . . ?
C6      C12     C7         120.745(230)        . . ?
C6      C12     H15        119.660(681)        . . ?
C7      C12     H15        119.594(670)          . . ?
	        				        
_chemical_name_systematic                  
; 
Alpha-dichlorido-di(3-cyanopyridine)zinc
;				  
_chemical_name_common             'Alpha-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            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 placed between foils. 
;

_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 1.591

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

# 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         9800
_pd_meas_2theta_range_min         2        
_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, 2018)
;        
_pd_proc_ls_background_function   'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr      '[010]'     


_pd_proc_ls_prof_R_factor         0.03768        
_pd_proc_ls_prof_wR_factor        0.05104       
_pd_proc_ls_prof_wR_expected      0.03188        
_refine_ls_R_I_factor             2.1680	  



_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      84      		
_refine_ls_number_restraints      29       		
_refine_ls_number_constraints     2			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.601     
      
_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         2        
_pd_proc_2theta_range_max         100        
_pd_proc_2theta_range_inc         0.1               
_pd_proc_info_excluded_regions    '9.44 - 9.74     4.34 - 14.84  19.10 - 19.40  22.22 - 22.47'
								 
				
# 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_PLAT962_alpha-ZnCl23-cypy2
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0        263       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_alpha-ZnCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  0.06A   From Cl10          -14.98 eA-3  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT974_alpha-ZnCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density on       Zn4     -30.32 eA-3  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT920_alpha-ZnCl23-cypy2
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.18 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2018).
;
_vrf_PLAT978_alpha-ZnCl23-cypy2
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info    
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT802_alpha-ZnCl23-cypy2
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
# end Validation Reply Form


