data_MnBr2(3-cypy)1

_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
;
'3-Cyanopyridine as bridging and terminal ligand in coordination polymers'
;

_publ_section_references
;
Boultif, A. & Louër, D. (1991). J. Appl. Cryst., 24, 987-993.

Coelho, A. A. (2007). TOPAS Academic User Manual. Coelho Software, B
risbane, Australia.

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.


STOE & Cie (2004). WinXPOW. STOE and Cie, Darmstadt, Germany.
;

_publ_section_exptl_prep
;
MnBr2(3cypy)1 was prepared by thermal decomposition of MnBr2(3cypy)4.
;
_publ_section_exptl_refinement
;

The first 20 peaks were selected for indexing in DASH (David et al. , 2004).
which resulted in a monoclinic unit cell with Z = 2. 
Structure solution was then carried out using simulated annealing 
with DASH.
A starting molecular model was derived from the known crystal structure of [MnBr2(3cypy)4]. 
The molecular fragment was restricted to rotate around the Mn-atom, 
The Rietveld refinement was carried out with TOPAS (Coelho, 2007).
All C-C and C-H angels of the pyridine ring were restraint to be 120°. 
Thermal parameters of hydrogen atoms were constrained to those of 
the non-hydrogen atoms.  
;

_chemical_name_mineral ??
_cell_length_a     3.8347(9)
_cell_length_b     7.2580(3)
_cell_length_c    16.5477(2)
_cell_angle_alpha 90
_cell_angle_beta  90
_cell_angle_gamma 93.410(8)
_cell_volume 	 459.75(7)
_space_group P1121
_cell_formula_units_Z 2

loop_
_symmetry_equiv_pos_as_xyz
	'-x, -y, 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  0.0035(4)    0.2367(6)    0.9876(5)   1 2.95709     0.03745
Mn2 Mn   0 -0.0192(7)    0.3896(1)    0.8640(8)   1 2.95709     0.03745
C3 C   	 0 -0.0109(7)    0.3395(1)    1.0560(3)   1 2.95709     0.03745
C4 C   	 0  0.0375(6)    0.0488(1)    0.9882(3)   1 2.95709     0.03745
Br5 Br   0 -0.4893(8)    0.6061(6)    0.9268(1)   1 2.95709     0.03745
Br6 Br   0  0.4803(5)    0.1760(1)    0.8020(1)   1 2.95709     0.03745
H7 H  	 0 -0.0360(3)    0.4751(9)    1.0526(4)   1 3.548508     0.04494
C8 C  	 0  0.0062(1)    0.2493(1)    1.1301(1)   1 2.95709     0.03745
C9 C  	 0  0.0570(5)   -0.0383(1)    1.0607(4)   1 2.95709     0.03745
H10 H    0  0.0458(5)   -0.0248(6)    0.9376(8)   1 3.548508     0.04494
C11 C    0 -0.0092(7)    0.3452(9)    1.2044(6)   1 2.95709     0.03745
C12 C    0  0.0420(2)    0.0655(1)    1.1307(7)   1 2.95709     0.03745
H13 H    0  0.0830(7)   -0.1735(7)    1.0605(9)   1 3.548508     0.04494
N14 N    0 -0.0198(9)    0.4283(9)    1.2651(1)   1 2.95709     0.03745
H15 H    0  0.0516(6)    0.0125(1)    1.1816(8)   1 3.548508     0.04494

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   	2.3309(9)    . ?
N1      C3    	1.3581(1)    . ?
N1      C4    	1.3781(8)    . ?
Mn2     Br5   	2.6716(2)    . ?
Mn2     Br6   	2.7356(9)    . ?
C3      H7    	0.9967(7)    . ?
C3      C8    	1.3929(7)    . ?
C4      C9    	1.3603(8)    . ?
C4      H10   	0.9942(7)    . ?
C8      C11   	1.4170(1)    . ?
C8      C12   	1.3491(6)    . ?
C9      C12   	1.3853(5)    . ?
C9      H13   	0.9926(7)    . ?
C12     H15   	0.9277(6)    . ?
C11     N14   	1.1727(2)    . ?

				
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     117.7596(5)    	 . . ?
Mn2     N1      C4     119.0351(2)    	 . . ?
C3      N1      C4     123.1672(7)   	  . . ?
N1      Mn2     Br5     89.3718(2)     	. . ?
N1      Mn2     Br6     90.6917(1)     	 . . ?
Br5     Mn2     Br6    178.0208(6)    . . ?
N1      C3      H7     120.3388(1)   . . ?
N1      C3      C8     118.0624(6)   . . ?
H7      C3      C8     121.5948(2)    . . ?
N1      C4      C9     118.5055(8)     . . ?
N1      C4      H10    122.2992(1)     . . ?
C9      C4      H10    119.2523(1)     . . ?
C3      C8      C11    121.9025(1)      . . ?
C3      C8      C12    118.8559(1)      . . ?
C11     C8      C12    119.2547(6)      . . ?
C4      C9      C12    118.6716(2)      . . ?
C4      C9      H13    117.9667(6)       . . ?
C12     C9      H13    123.3602(4)       . . ?
C8      C12     C9     122.7449(8)        . . ?
C8      C12     H15    115.2347(8)        . . ?
C9      C12     H15    122.0099(4)        . . ?
C8      C11     N14    178.4777(2)          . . ?
	        				        
_chemical_name_systematic                  
; 
catena-dibromo-(3-cyanopyridine)manganat
;				  
_chemical_name_common             'catena-dibromo-bis(3-cyanopyridine)manganat'		 
_chemical_formula_iupac           'C6 H4 Br2 Mn N2 '				 
_chemical_formula_moiety          'C6 H4 Br2 Mn N2 '				 
_chemical_formula_structural      'C6 H4 Br2 Mn N2 '				 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C6 H4 Br2 Mn N2 '
_chemical_formula_weight          318.85 
_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'
   Mn Mn 'International Tables Vol C Table 6.1.1.4'
   Br Br '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 1 21'        
_symmetry_space_group_name_Hall   'P  2 c '


_pd_spec_size_axial   12

_pd_spec_size_equat   0.7

_pd_spec_size_thick   0.7


# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                         
;
Specimen was sealed in a 0.7 mm diameter borosilicate glass capillary. 
;

_pd_spec_mount_mode               'transmission'

_pd_spec_shape                    'cylinder'

_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 2.303

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

# 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             ?
_diffrn_source_type               ?
_diffrn_radiation_type            'Cu K\a~1~'       
_diffrn_measurement_device_type   'STOE Stadi-P'       
_diffrn_detector                  ?      
_diffrn_detector_type             'lin psd'
_diffrn_radiation_source   	  'X-ray tube'
_exptl_crystal_F_000        	  ?	    			    

_pd_meas_scan_method              step       


_diffrn_radiation_wavelength      1.54060       
_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         ?
_pd_meas_2theta_range_min         5        
_pd_meas_2theta_range_max         80       
_pd_meas_2theta_range_inc         ?        

_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         0.01695        
_pd_proc_ls_prof_wR_factor        0.02147        
_pd_proc_ls_prof_wR_expected      0.01696        
_refine_ls_R_I_factor             0.00944	  



_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      90      		
_refine_ls_number_restraints      29       		
_refine_ls_number_constraints     2 			
_refine_ls_number_reflns	?			
     

_refine_ls_goodness_of_fit_all     1.266      
      
_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         5        
_pd_proc_2theta_range_max         80        
_pd_proc_2theta_range_inc         ?               
_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, 2007)'
_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_REFI015_MnBr23-cypy1
;
PROBLEM: refine_ls_shift/su_max is missing
         Maximum shift/s.u. ratio after final refinement cycle.
RESPONSE: structure was solved from powder data
;
_vrf_PLAT341_MnBr23-cypy1
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.00662 Ang. 
RESPONSE: X-ray powder data
;
_vrf_PLAT920_MnBr23-cypy1
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.24 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_MnBr23-cypy1
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0         93       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_MnBr23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  1.22A   From Br6             3.55 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_MnBr23-cypy1
;
PROBLEM: Check Calcd Resid. Dens.  0.01A   From Br6           -36.02 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_MnBr23-cypy1
;
PROBLEM: Check Calcd Negative Resid. Density on       Mn2     -22.26 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_MnBr23-cypy1
;
PROBLEM: Check Negative Difference Density on H15 -1.56 eA-3 and H14  -1.02 eA-3
RESPONSE: structure was solved from powder data
;
_vrf_PLAT978_MnBr23-cypy1
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structure was solved from powder data
;
# end Validation Reply Form
