data_MnCl2(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
;
[MnCl2(3cypy)2]n was prepared from alcoholic solution.
;
_publ_section_exptl_refinement
;
The first 20 peaks were selected for indexing in DASH (David et al. , 2004), 
which resulted in an orthorhombic unit cell with Z = 2. 
Structure solution was then carried out using simulated annealing 
with DASH (David et al. , 2004).  
The molecular fragment (MnCl2(3cypy)1) was restricted to rotate around the Mn atom on special position (0,0,0).
Rietveld refinement was carried out with TOPAS (Coelho, 2018). 
The Cl atom was fixed on x = 0.5 during the refinement.
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 to those of 
the non-hydrogen atoms.
;

_chemical_name_mineral ??
_cell_length_a  3.702978(44)
_cell_length_b  15.43091(37)
_cell_length_c  11.57802(31)
_cell_angle_alpha 90
_cell_angle_beta  91.4375(16)
_cell_angle_gamma 90
_cell_volume 661.364(25)
_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 0.01782(63)  -0.09293(18) 0.15564(25) 1 3.179(46)     0.04026
Mn2 Mn   0               0           0           0 1 3.179(46)     0.04026
C3 C     0 -0.07355(62) -0.17562(15) 0.13349(21) 1 3.179(46)     0.04026
C4 C     0 0.12119(70)  -0.07037(16) 0.26161(20) 1 3.179(46)     0.04026
Cl5 Cl   0 0.5(01)          0.08484(14) 0.09582(21) 1 3.179(46)     0.04026
C6 C     0 -0.06739(68) -0.24028(15) 0.21687(21) 1 3.179(46)     0.04026
H7 H     0 -0.1503(19)  -0.19144(57) 0.05399(89) 1 3.814(55)     0.04831
C8 C     0 0.13193(70)  -0.13292(16) 0.34733(21) 1 3.179(46)     0.04026
H9 H     0 0.1860(19)   -0.00912(58) 0.27800(74) 1 3.814(55)     0.04831
C10 C    0 0.03938(73)  -0.21787(15) 0.32675(20) 1 3.179(46)     0.04026
H11 H    0 -0.1347(22)  -0.30120(58) 0.1978(10)  1 3.814(55)     0.04831
C12 C    0 0.24795(86)  -0.10938(25) 0.46158(22) 1 3.179(46)     0.04026
H13 H    0 0.0470(22)   -0.26129(53) 0.38919(85) 1 3.814(55)     0.04831
N14 N    0 0.35777(95)  -0.09094(31) 0.55165(30) 1 3.179(46)     0.04026

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      Mn2     2.3026(29)   .  ?
N1      C3      1.3431(37)     .  ?
N1      C4      1.3227(37)   .  ?
Mn2     Cl5     2.5039(16)   .  ? 
C3      C6      1.3882(34)   .  ?
C3      H7      0.987(10)    .  ?
C4      C8      1.3842(34)   .  ?
C4      H9      0.9922(93)   .  ?
C6      C10     1.3672(34)    .  ?
C6      H11     0.9957(91)     .  ?
C8      C10     1.3743(34)   .  ?
C10     H13     0.9856(94)   .  ?
C8      C12     1.4276(37)    .  ?
C12     N14     1.1456(45)     .  ?
    

				
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 
 
 
Mn2     N1      C3       116.1(2) 	 . . ?
Mn2     N1      C4       124.3(2)      . . ?
C3      N1      C4       119.5(3) 	  . . ?
N1      Mn2     Cl5      88.44(12)  	. . ?
N1      C3      C6      123.39(24)  . . ?
N1      C3      H7      118.58(58)   . . ?
C6      C3      H7      118.03(57)  . . ?
N1      C4      C8      118.94(24)  . . ?
N1      C4      H9      119.41(54)   . . ?
C8      C4      H9      121.64(54)  . . ?
C3      C6      C10     117.69(22)     . . ?
C3      C6      H11     121.67(71)    . . ?
C10     C6      H11     120.63(71)    . . ?
C4      C8      C10     122.57(23)  . . ?
C4      C8      C12     119.31(25)     . . ?
C8      C10     H13     121.26(56)    . . ?
C6      C10     H13     120.86(56)     . . ?
C10     C8      C12     118.12(25)      . . ?
C6      C10     C8      117.88(22)      . . ?
C8      C12     N14     176.72(35)    . . ?

	        				        
_chemical_name_systematic                  
; 
catena-bis-chloro-di(3-cyanopyridine)manganat(II)
;				  
_chemical_name_common             'Catena-bis-chloro-di(3-cyanopyridine)manganat(II)'		 
_chemical_formula_iupac           'C12 H8 Cl2 Mn N4 '				 
_chemical_formula_moiety          'C12 H8 Cl2 Mn N4 '				 
_chemical_formula_structural      'C12 H8 Cl2 Mn N4 '				 
_chemical_formula_analytical      ?              
_chemical_formula_sum             'C12 H8 Cl2 Mn N4 '
_chemical_formula_weight          334.06 
_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'
   Mn Mn '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 measured 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 1.677

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

# 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         7800
_pd_meas_2theta_range_min         3        
_pd_meas_2theta_range_max         80.99       
_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         0.01411        
_pd_proc_ls_prof_wR_factor        0.01805       
_pd_proc_ls_prof_wR_expected      0.01561        
_refine_ls_R_I_factor             0.01167	  



_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      28       		
_refine_ls_number_constraints     2			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.156  
      
_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         80.99       
_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_PLAT004_MnCl23-cypy2
;
PROBLEM: Polymeric Structure Found with Maximum Dimension   
RESPONSE: The structure is polymeric.
;
_vrf_PLAT041_MnCl23-cypy2
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ   
RESPONSE: The sumformula is [MnCl2C12H8N4]n.
;
_vrf_PLAT042_MnCl23-cypy2
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ   
RESPONSE: The sumformula is [MnCl2C12H8N4]n.
;
_vrf_PLAT920_MnCl23-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_MnCl23-cypy2
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         57       
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT971_MnCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT972_MnCl23-cypy2
;
PROBLEM: Check Calcd Resid. Dens.  0.10A   From Cl5           -14.76 eA-3  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT974_MnCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density on       Mn2     -23.19 eA-3  
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT977_MnCl23-cypy2
;
PROBLEM: Check Calcd Negative Resid. Density.
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT978_MnCl23-cypy2
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info    
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT802_MnCl23-cypy2
;
PROBLEM: CIF Input Record(s) with more than 80 Characters   
RESPONSE: The structure was solved from powder data.
;
_vrf_PLAT860_MnCl23-cypy2
;
PROBLEM: Number of Least-Squares Restraints: 28.   
RESPONSE: The structure was solved from powder data.
;
# end Validation Reply Form






