data_MnBr2(3-cypy)4

_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 Crystal Engineering Communications.
;


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


# 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)4 was prepared from alcoholic solution. 
;
_publ_section_exptl_refinement
;
The first 20 peaks were selected for indexing in DASH (Louër et al. , 2017), which resulted in a tetragonal unit cell with Z = 2. 
Structure solution was then carried out using simulated annealing 
with DASH(David et al. , 2004). 
A starting molecular model was derived from the known crystal structure of [CoBr2(3cypy)4]. 
The molecular fragment was restricted to rotate around the Br-Mn-Br-axis, Mn and Br atoms were
fixed on the fourfold rotation axis (0,0,z) during the simulated annealing.
The Rietveld refinement was carried out with TOPAS (Coelho, 2007). 
The Mn and Br atoms were restraint on the the fourfold axis, the 3-cyanopyridine was 
restrained flat in the mirror plane.
All C-C and C-H angles of the pyridine ring were restraint to be 120°. 
Thermal parameters of H atoms were constrained to those of 
the non-H atoms. 
;

_chemical_name_mineral MnBr2(3-cypy)4
_cell_length_a                    11.2178(5)
_cell_length_b                    11.2178(5)
_cell_length_c                    10.3309(6)
_cell_angle_alpha                 90	
_cell_angle_beta                  90	
_cell_angle_gamma                 90	
_cell_volume                      1300.03(14)
_cell_formula_units_Z             2 
_space_group 			  P4nc
loop_ 
 _symmetry_equiv_pos_as_xyz 
 '-x, -y, z'
 '-x+1/2, y+1/2, z+1/2'
 '-y, x, z'
 '-y+1/2, -x+1/2, z+1/2'
 'y, -x, z'
 'y+1/2, x+1/2, z+1/2'
 'x, y, z'
 'x+1/2, -y+1/2, 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 0.1644(4)   0.1186(4)  0.5040(2) 	1 3.82723     0.04847
Mn2 Mn   0 0 	       0 	  0.5	  	1 3.82723     0.04847
C3 C     0 0.2580(5)   0.0976(6)  0.5813(8) 	1 3.82723     0.04847
C4 C     0 0.1734(2)   0.2093(8)  0.4196(4) 	1 3.82723     0.04847
Br5 Br   0 0 	       0 	  0.7588(1) 	1 3.82723     0.04847
Br6 Br   0 0 	       0 	  0.2429(3) 	1 3.82723     0.04847
H7 H     0 0.2559(9)   0.0306(1)  0.6437(8) 	1 4.592676     0.05817
C8 C     0 0.3603(5)   0.1687(1)  0.5737(2) 	1 3.82723     0.04847
C9 C     0 0.2725(1)   0.2843(6)  0.4079(5) 	1 3.82723     0.04847
H10 H    0 0.1071(9)   0.2282(6)  0.3601(9) 	1 4.592676     0.05817
C11 C    0 0.3693(7)   0.2635(2)  0.4883(1)	1 3.82723     0.04847
C12 C    0 0.4647(8)   0.1496(9)  0.6505(6) 	1 3.82723     0.04847
H13 H    0 0.2715(8)   0.3497(5)  0.3439(3) 	1 4.592676     0.05817
H14 H    0 0.4438(2)   0.3104(8)  0.4902(3) 	1 4.592676     0.05817
N15 N    0 0.5488(2)   0.1276(9)  0.7052(3) 	1 3.82723     0.04847 

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    2.2744(1) . ?	
N1      C3     1.3404(6) . ?
N1      C4     1.3439(5) . ?
Mn2     Br5    2.6736(1) . ?
Mn2     Br6    2.6581(1) . ?
C3      H7     0.9909(7) . ?
C3      C8     1.3994(5) . ?
C4      C9     1.3991(6) . ?
C4      H10    0.9869(4) . ?
C8      C11    1.3857(1) . ?
C8      C12    1.4311(1) . ?
C9      C11    1.3872(1) . ?
C9      H13    0.9877(3) . ?
C11     H14    0.9876(3) . ?
C12     N15    1.1263(5) . ?

				
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    122.9401(1)	. . ?
Mn2     N1      C4    119.5301(9)	. . ?
C3      N1      C4    117.5500(5)	. . ?
N1      Mn2     Br5    88.9650(5)	. . ?
N1      Mn2     Br6    91.0452(5)	. . ?
Br5     Mn2     Br6   180.0000(1)	. . ?
N1      C3      H7    120.1900(4)	. . ?
N1      C3      C8    120.5766(1)	. . ?
H7      C3      C8    119.2256(8)	. . ?
N1      C4      C9    124.8096(3)	. . ?
N1      C4      H10   120.6474(6)	. . ?
C9      C4      H10   114.5406(6)	. . ?
C3      C8      C11   122.2097(2)	. . ?
C3      C8      C12   123.7094(7)	. . ?
C11     C8      C12   114.0737(8)	. . ?
C4      C9      C11   117.9900(9)	. . ?
C4      C9      H13   119.7258(2)	. . ?
C11     C9      H13   122.2839(2)	. . ?
C8      C11     C9    116.9515(2)	. . ?
C8      C11     H14   117.2763(5)	. . ?
C9      C11     H14   125.7713(7)	. . ?
C8      C12     N15   174.8485(9)	. . ?

_chemical_name_systematic                  
; 
Dibromo-tetra(3-cyanopyridine)manganat
;				  
_chemical_name_common             'Dibromo-tetra(3-cyanopyridine)manganat'		 
_chemical_formula_iupac           'C24 H16 Br2 Mn N8'				 
_chemical_formula_moiety          'C24 H16 Br2 Mn N8'				 
_chemical_formula_structural      'C24 H16 Br2 Mn N8'				 
_chemical_formula_analytical      ? 
_chemical_formula_sum              'C24 H16 Br2 Mn N8'
_chemical_formula_weight          631.19 
_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'
   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            tetragonal        
_symmetry_space_group_name_H-M    'P  4 n c'        
_symmetry_space_group_name_Hall   'P 4 -2n'


_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 1.612

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

# 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      1.540598    
_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         3        
_pd_meas_2theta_range_max        100       
_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      '[002]'        


_pd_proc_ls_prof_R_factor         0.01587        
_pd_proc_ls_prof_wR_factor        0.02038        
_pd_proc_ls_prof_wR_expected      0.01959        
_refine_ls_R_I_factor             0.00933	  



_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      83      		
_refine_ls_number_restraints      29        		
_refine_ls_number_constraints     2 			
_refine_ls_number_reflns	  ?			
     

_refine_ls_goodness_of_fit_all     1.040      
      
_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         3        
_pd_proc_2theta_range_max         100        
_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-cypy4
;
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-cypy4
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.007 Ang. 
RESPONSE: X-ray powder data
;
_vrf_PLAT920_MnBr23-cypy4
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.18 Degree
RESPONSE: X-ray powder data, FCF calculated by program TOPAS (Coelho, 2007)
;
_vrf_PLAT962_MnBr23-cypy4
;
PROBLEM: Number of Input Relections with Sigma(Fo^2) =  0        193       
RESPONSE: structure was solved from powder data
;
_vrf_PLAT971_MnBr23-cypy4
;
PROBLEM: Check Calcd Resid. Dens. for all atoms 
RESPONSE: structure was solved from powder data
;
_vrf_PLAT972_MnBr23-cypy4
;
PROBLEM: Check Calcd Resid. Dens.  0.10A   From Br6           -47.84 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT974_MnBr23-cypy4
;
PROBLEM: Check Calcd Negative Resid. Density on       Mn2     -30.41 eA-3  
RESPONSE: structure was solved from powder data
;
_vrf_PLAT977_MnBr23-cypy4
;
PROBLEM: Check Negative Difference Density on H14              -0.51 eA-3
RESPONSE: structur was solved from powder data
;
_vrf_PLAT978_MnBr23-cypy4
;
PROBLEM: Number C-C Bonds with Positive Residual Density:          0 Info
RESPONSE: structur was solved from powder data
;
# end Validation Reply Form