data_FeCl2(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
;
[FeCl2(3cypy)2]n was prepared from alcoholic solution.
;
_publ_section_exptl_refinement
;
The first 20 peaks were selected for indexing in CONOGRAPH (Esmaeili et al. , 2017; Oishi-Tomiyasu, 2014), 
which resulted in a monoclinic unit cell with Z = 4. 
Structure solution was then carried out using simulated annealing 
with DASH (David et al. , 2004).  
The molecular fragment (FeCl2(3cypy)1) was restricted to rotate around the Fe atom on special position (0,0,0).
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  3.64403(18)
_cell_length_b  13.81346(76)
_cell_length_c  13.1192(11)
_cell_angle_alpha 90
_cell_angle_beta  98.5316(67)
_cell_angle_gamma 90
_cell_volume 653.068(75)
_cell_formula_units_Z 2
_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


N1 N     0  0.0079(12) -0.15375(32)  0.06335(35) 1   2.952(64)     0.03739
Fe2 Fe   0  0           0            0           1   2.952(64)     0.03739
C3 C     0 -0.1106(12) -0.22683(27) -0.00050(30) 1   2.952(64)     0.03739
C4 C     0  0.1230(11) -0.17127(29)  0.16446(31) 1   2.952(64)     0.03739
Cl5 Cl   0 -0.4236(13)  0.04356(22)  0.12452(27) 1   2.952(64)     0.03739
C6 C     0 -0.1171(12) -0.32137(29)  0.03200(32) 1   2.952(64)     0.03739
H7 H     0 -0.1945(52) -0.21322(96) -0.0726(12)  1   3.543(77)     0.04487
C8 C     0  0.1171(13) -0.26552(29)  0.20184(29) 1   2.952(64)     0.03739
H9 H     0  0.2153(58) -0.1184(12)   0.2130(12)  1   3.543(77)     0.04487
C10 C    0 -0.0043(13) -0.34194(28)  0.13437(31) 1   2.952(64)     0.03739
C11 C    0 -0.2597(15) -0.39301(35) -0.04419(40) 1   2.952(64)     0.03739
H12 H    0  0.1993(52) -0.2756(19)   0.2751(13)  1   3.543(77)     0.04487
H13 H    0 -0.0163(69) -0.4099(12)   0.1589(11)  1   3.543(77)     0.04487
N14 N    0 -0.3852(25) -0.44483(43) -0.10615(46) 1   2.952(64)     0.03739

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      Fe2       2.2793(45)   .  ?
N1      C3        1.3415(58)     .  ?
N1      C4        1.3524(60)   .  ?
Fe2     Cl5       2.4822(44)   .  ? 
C3      C6        1.3751(55)   .  ?
C3      H7        0.968(15)    .  ?
C4      C8        1.3925(57)   .  ?
C4      H9        0.994(18)   .  ?
C6      C10       1.3745(56)    .  ?
C6      C11       1.4472(63)     .  ?
C8      C10       1.4062(55)   .  ?
C8      H12       0.973(17)   .  ?
C10     H13       0.995(16)    .  ?
C11     N14       1.1278(77)     .  ?
    

				
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 
 
 
Fe2     N1      C3     119.2(3) . . ?
Fe2     N1      C4     120.6(3)   . . ?
C3      N1      C4     120.14(40)  . . ?
N1      Fe2     Cl5     87.79(13) 	. . ?
N1      C3      C6     122.67(38) . . ?
N1      C3      H7     119.31(88)  . . ?
C6      C3      H7     118.03(86) . . ?
N1      C4      C8     119.60(38) . . ?
N1      C4      H9     121.54(96) . . ?
C8      C4      H9     118.86(95) . . ?
C3      C6      C10    118.87(36)   . . ?
C3      C6      C11    117.14(38)   . . ?
C10     C6      C11    123.93(39)  . . ?
C4      C8      C10    120.1(4)  . . ?
C4      C8      H12    117.6(16)    . . ?
C10     C8      H12    122.4(16)    . . ?
C6      C10     C8     118.71(36)   . . ?
C6      C10     H13    119.31(91)    . . ?
C8      C10     H13    121.96(93)     . . ?
C6      C11     N14    175.93(55)   . . ?

	        				        
_chemical_name_systematic                  
; 
catena-bis-chloro-di(3-cyanopyridine)ferrat(II)
;				  
_chemical_name_common             'Catena-bis-chloro-di(3-cyanopyridine)ferrat(II)'		 
_chemical_formula_iupac           'C12 H8 Cl2 Fe N4 '				 
_chemical_formula_moiety          'C12 H8 Cl2 Fe N4 '				 
_chemical_formula_structural      'C12 H8 Cl2 Fe N4 '				 
_chemical_formula_analytical      ?              
_chemical_formula_sum             'C12 H8 Cl2 Fe N4 '
_chemical_formula_weight          334.97 
_chemical_melting_point           ? 
 
_exptl_crystal_colour   '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'
   Fe Fe '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   0.5


# 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 1.704

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

# 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         3942
_pd_meas_2theta_range_min         1        
_pd_meas_2theta_range_max         60.115       
_pd_meas_2theta_range_inc         0.015       

_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         0.02682        
_pd_proc_ls_prof_wR_factor        0.03448       
_pd_proc_ls_prof_wR_expected      0.02260        
_refine_ls_R_I_factor             1.6997	  



_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      85      		
_refine_ls_number_restraints      29       		
_refine_ls_number_constraints     2			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.525 
      
_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         2.11         
_pd_proc_2theta_range_max         60.1156       
_pd_proc_2theta_range_inc         0.015                
_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_PLAT004_FeCl23-cypy2
;
PROBLEM: Polymeric Structure Found with Maximum Dimension   
RESPONSE: The structure is polymeric.
;
_vrf_PLAT920_FeCl23-cypy2
;
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_FeCl23-cypy2
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         57       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT971_FeCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_FeCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.        
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT974_FeCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density      
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT977_FeCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT978_FeCl23-cypy2
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info    
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT802_FeCl23-cypy2
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT860_FeCl23-cypy2
;
PROBLEM: Number of Least-Squares Restraints: 29.   
RESPONSE: The structure was solved from powder data.
;
# end Validation Reply Form






