# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Fe(C4N2H6)2[Fe(CN)5NO]
_database_code_depnum_ccdc_archive 'CCDC 2013009'
loop_
_audit_author_name
_audit_author_address
'Joelis Rodriguez Hernandez'
;Centro de Investigacion en Quimica Aplicada
Mexico
;
_audit_update_record             
;
2020-06-29 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;

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

# 5. CHEMICAL DATA

_chemical_name_systematic        
; iron methylimidazole pentacyanonitrosilferrates (II)
;
_chemical_name_common            'pentacyanonitrosilferrates (II)'
_chemical_formula_moiety         'Fe2 C13 O N10'
_chemical_formula_structural     Fe(C4N2)2[Fe(CN)5NO]
_chemical_formula_analytical     ?
_chemical_formula_iupac          Fe(C4N2)2[Fe(CN)5NO]
_chemical_formula_sum            'Fe2 C13 O N10'
_chemical_formula_weight         423.93
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
fe 11.76950 4.76110 7.35730 0.30720 3.52220 15.35350 2.30450 76.88050 1.03690
-1.17900 3.20400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.02900 0.01800
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

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

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x,y+1/2,-z+1/2
-x,-y,-z
x,-y+1/2,z+1/2

_cell_length_a                   8.386(2)
_cell_length_b                   14.787(4)
_cell_length_c                   14.458(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.9(1)
_cell_angle_gamma                90.0000
_cell_volume                     1779.99
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              25 # perpendicular to 
# equatorial plane
_pd_spec_size_equat              25 # parallel to 
# scattering vector
# in transmission
_pd_spec_size_thick              1 # parallel to 
# scattering vector
# in reflection

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

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
; ?
;
_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'
_pd_spec_shape                   flat_sheet # options are 'cylinder' 
# 'flat_sheet' or 'irregular'
_pd_char_particle_morphology     ?
_pd_char_colour                  ? # use ICDD colour descriptions
_exptl_crystal_description       powder

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

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

# 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                   'sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_source_target            
Cu # Put here the chemical symbol of the anode
_diffrn_radiation_wavelength     1.54056
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'q/2q scans'
_diffrn_detector_area_resol_mean ?
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector
_pd_meas_scan_method             cont # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        2800
_pd_meas_2theta_range_min        4.00000
_pd_meas_2theta_range_max        59.98000
_pd_meas_2theta_range_inc        0.020000

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

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_background_function  'linear extrapolation'
_pd_proc_ls_pref_orient_corr     
; ?
;

#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        13.4276
_pd_proc_ls_prof_wR_factor       17.7629
_pd_proc_ls_prof_wR_expected     10.6071

#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       26.5004
_pd_proc_ls_prof_cwR_factor      29.0394
_pd_proc_ls_prof_cwR_expected    17.3408

#  The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            2.8044
_pd_proc_ls_prof_echi2           2.9000

#  Items related to LS refinement

_refine_ls_R_I_factor            12.7212
_refine_ls_number_reflns         634
_refine_ls_number_parameters     1
_refine_ls_number_restraints     0

# 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        4.0000
_pd_proc_2theta_range_max        59.9800
_pd_proc_2theta_range_inc        0.020000
_pd_proc_wavelength              1.540562

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   'No regions were excluded'
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_type_symbol
Fe1 0.50000 0.50000 0.50000 0.018(3) 1.00000 Uiso Fe
Fe2 0.50000 0.00000 0.50000 0.018(3) 1.00000 Uiso Fe
Fe 0.478(2) 0.243(2) 0.749(4) 0.018(3) 1.00000 Uiso Fe
C1 0.493(6) 0.336(2) 0.658(0) 0.021(3) 1.00000 Uiso C
N1 0.504(3) 0.390(6) 0.605(3) 0.021(3) 1.00000 Uiso N
C2 0.430(3) 0.155(3) 0.652(5) 0.021(3) 1.00000 Uiso C
N2 0.415(4) 0.101(7) 0.597(4) 0.021(3) 1.00000 Uiso N
C3 0.425(5) 0.153(4) 0.837(4) 0.021(3) 1.00000 Uiso C
N3 0.402(5) 0.098(4) 0.889(4) 0.021(3) 1.00000 Uiso N
C4 0.497(6) 0.334(4) 0.846(3) 0.021(3) 1.00000 Uiso C
N4 0.512(4) 0.387(7) 0.900(4) 0.021(3) 1.00000 Uiso N
C5 0.251(4) 0.272(4) 0.735(4) 0.021(3) 1.00000 Uiso C
N5 0.119(6) 0.290(3) 0.728(3) 0.021(3) 1.00000 Uiso N
N 0.671(6) 0.221(6) 0.761(7) 0.021(3) 1.00000 Uiso N
O 0.803(2) 0.209(2) 0.769(3) 0.021(3) 1.00000 Uiso O
C11 0.826(3) 0.487(4) 0.399(4) 0.023(3) 1.00000 Uiso C
C12 0.955(6) 0.434(6) 0.394(7) 0.023(3) 1.00000 Uiso C
C13 0.825(4) 0.386(6) 0.503(4) 0.023(3) 1.00000 Uiso C
C14 1.074(6) 0.300(3) 0.482(5) 0.023(3) 1.00000 Uiso C
N11 0.739(6) 0.456(4) 0.466(5) 0.023(3) 1.00000 Uiso N
N12 0.955(5) 0.371(3) 0.460(5) 0.023(3) 1.00000 Uiso N
C21 0.164(3) -0.102(4) 0.437(4) 0.023(3) 1.00000 Uiso C
C22 0.016(6) -0.090(5) 0.391(4) 0.023(3) 1.00000 Uiso C
C23 0.154(4) 0.031(3) 0.391(4) 0.023(3) 1.00000 Uiso C
C24 -0.126(7) 0.042(4) 0.311(3) 0.023(3) 1.00000 Uiso C
N21 0.250(5) -0.026(5) 0.436(3) 0.023(3) 1.00000 Uiso N
N22 0.010(5) -0.005(4) 0.362(2) 0.023(3) 1.00000 Uiso N

# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

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

# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 . . 2.217(1) y
Fe1 N11 . . 2.218(2) y
Fe2 N2 . . 2.231(1) y
Fe2 N21 . . 2.218(2) y
Fe C1 . . 1.923(1) y
Fe C2 . . 1.917(1) y
Fe C3 . . 1.923(1) y
Fe C4 . . 1.933(1) y
Fe C5 . . 1.937(2) y
Fe N . . 1.645(2) y
C1 N1 . . 1.123(1) y
C2 N2 . . 1.124(1) y
C3 N3 . . 1.136(1) y
C4 N4 . . 1.110(1) y
C5 N5 . . 1.126(1) y
N O . . 1.111(1) y
N11 C11 . . 1.361(1) y
C11 C12 . . 1.341(1) y
C12 N12 . . 1.338(1) y
N12 C13 . . 1.338(1) y
C13 N11 . . 1.329(1) y
C14 N12 . . 1.457(1) y
N21 C21 . . 1.337(1) y
C21 C22 . . 1.344(1) y
C22 N22 . . 1.331(1) y
N22 C23 . . 1.337(1) y
C23 N21 . . 1.299(1) y
C24 N22 . . 1.467(1) y


loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Fe2 N21 . . . 91.38(3) y
N1 Fe1 N11 . . . 89.88(3) y
N Fe C3 . . . 95.50(4) y
N Fe C1 . . . 93.61(4) y
N Fe C4 . . . 93.34(4) y
N Fe C5 . . . 178.32(6) y
N Fe C2 . . . 93.78(4) y
C3 Fe C1 . . . 170.85(3) y
C3 Fe C4 . . . 90.99(3) y
C3 Fe C5 . . . 85.76(3) y
C3 Fe C2 . . . 88.15(3) y
C1 Fe C4 . . . 89.22(3) y
C1 Fe C5 . . . 85.14(4) y
C1 Fe C2 . . . 90.51(3) y
C4 Fe C5 . . . 85.51(4) y
C4 Fe C2 . . . 172.87(3) y
C5 Fe C2 . . . 87.37(4) y
N1 C1 Fe . . . 179.51(5) y
N2 C2 Fe . . . 174.21(5) y
N3 C3 Fe . . . 176.57(5) y
N4 C4 Fe . . . 178.33(5) y
N5 C5 Fe . . . 178.60(8) y
O N Fe . . . 178.31(8) y
C1 N1 Fe1 . . . 174.64(5) y
C2 N2 Fe2 . . . 155.11(4) y
Fe1 N11 C11 . . . 129.41(5) y
N11 C11 C12 . . . 110.24(6) y
C11 C12 N12 . . . 107.63(5) y
C12 N12 C13 . . . 106.00(5) y
N12 C13 N11 . . . 112.53(6) y
C13 N11 Fe1 . . . 126.74(5) y
C14 N12 C12 . . . 127.04(5) y
C14 N12 C13 . . . 126.95(6) y
Fe2 N21 C21 . . . 128.90(5) y
N21 C21 C22 . . . 110.57(6) y
C21 C22 N22 . . . 106.22(5) y
C22 N22 C23 . . . 106.53(5) y
N22 C23 N21 . . . 112.01(6) y
C23 N21 Fe2 . . . 126.41(5) y
C24 N22 C22 . . . 127.44(5) y
C24 N22 C23 . . . 126.00(6) y


loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?

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

#=============================================================================
# Additional structures (last six sections and associated data_? identifiers) 
# may be added at this point.                                                 
#=============================================================================

# The following lines are used to test the character set of files sent by     
# network email or other means. They are not part of the CIF data set.        
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789              
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2014754'
loop_
_audit_author_name
_audit_author_address
'Oscar Enrique Piro'
;Universidad Nacional de La Plata
Argentina
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
catena-[bis(u-cyano)-cyano-tetrakis(1-methylimidazole)-nitrosyl-iron-copper]
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H24 Cu Fe N14 O'
_chemical_formula_weight         607.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1670(5)
_cell_length_b                   10.2296(5)
_cell_length_c                   15.6179(8)
_cell_angle_alpha                73.752(4)
_cell_angle_beta                 80.350(4)
_cell_angle_gamma                84.476(4)
_cell_volume                     1384.29(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    3119
_cell_measurement_theta_min      3.3980
_cell_measurement_theta_max      26.5470
_exptl_crystal_description       plate
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             622
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    1.334
_shelx_estimated_absorpt_T_min   0.661
_shelx_estimated_absorpt_T_max   0.927
_exptl_absorpt_correction_T_min  0.93589
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.890
_oxdiff_exptl_absorpt_empirical_full_max 1.212
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            11398
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.965
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5585
_reflns_number_gt                4212
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement. 
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+0.3851P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5585
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0828
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3216(3) 0.2906(3) 0.70251(19) 0.0378(6) Uani 1 1 d . . . . .
C2 C 0.1106(3) 0.1365(3) 0.7110(2) 0.0442(7) Uani 1 1 d . . . . .
C3 C 0.1058(3) 0.2852(3) 0.83860(19) 0.0385(6) Uani 1 1 d . . . . .
C4 C 0.3803(3) 0.1789(3) 0.8657(2) 0.0454(7) Uani 1 1 d . . . . .
C5 C 0.3844(3) 0.0275(3) 0.7499(2) 0.0449(7) Uani 1 1 d . . . . .
C11 C 0.3662(4) 0.6995(4) 0.6069(2) 0.0620(9) Uani 1 1 d . . . . .
H11 H 0.3728 0.6346 0.6615 0.074 Uiso 1 1 calc R U . . .
C12 C 0.3095(4) 0.8272(4) 0.5979(3) 0.0655(10) Uani 1 1 d . . . . .
H12 H 0.2699 0.8664 0.6443 0.079 Uiso 1 1 calc R U . . .
C13 C 0.3829(4) 0.7943(3) 0.4670(2) 0.0689(11) Uani 1 1 d . . . . .
H13 H 0.4024 0.8098 0.4047 0.083 Uiso 1 1 calc R U . . .
C14 C 0.2735(6) 1.0292(4) 0.4659(4) 0.145(3) Uani 1 1 d . . . . .
H14A H 0.3348 1.0611 0.4088 0.217 Uiso 1 1 calc R U . . .
H14B H 0.2828 1.0862 0.5040 0.217 Uiso 1 1 calc R U . . .
H14C H 0.1720 1.0327 0.4568 0.217 Uiso 1 1 calc R U . . .
C15 C 0.7140(4) 0.4327(3) 0.6409(2) 0.0600(9) Uani 1 1 d . . . . .
H15 H 0.6601 0.3619 0.6803 0.072 Uiso 1 1 calc R U . . .
C16 C 0.8422(4) 0.4734(4) 0.6539(3) 0.0660(10) Uani 1 1 d . . . . .
H16 H 0.8925 0.4362 0.7029 0.079 Uiso 1 1 calc R U . . .
C17 C 0.7806(3) 0.5987(3) 0.5280(2) 0.0447(7) Uani 1 1 d . . . . .
H17 H 0.7831 0.6662 0.4737 0.054 Uiso 1 1 calc R U . . .
C18 C 1.0149(4) 0.6570(4) 0.5668(3) 0.0767(12) Uani 1 1 d . . . . .
H18A H 1.0343 0.7060 0.5042 0.115 Uiso 1 1 calc R U . . .
H18B H 1.0985 0.5963 0.5829 0.115 Uiso 1 1 calc R U . . .
H18C H 0.9981 0.7204 0.6030 0.115 Uiso 1 1 calc R U . . .
C21 C 0.2751(3) 0.6400(3) 0.9972(2) 0.0505(8) Uani 1 1 d . . . . .
H21 H 0.2321 0.6714 1.0466 0.061 Uiso 1 1 calc R U . . .
C22 C 0.4113(3) 0.6668(3) 0.9519(2) 0.0542(8) Uani 1 1 d . . . . .
H22 H 0.4788 0.7196 0.9636 0.065 Uiso 1 1 calc R U . . .
C23 C 0.3080(3) 0.5386(3) 0.8933(2) 0.0470(7) Uani 1 1 d . . . . .
H23 H 0.2935 0.4858 0.8560 0.056 Uiso 1 1 calc R U . . .
C24 C 0.5637(3) 0.6018(4) 0.8195(2) 0.0683(10) Uani 1 1 d . . . . .
H24A H 0.5606 0.5300 0.7915 0.103 Uiso 1 1 calc R U . . .
H24B H 0.6502 0.5875 0.8488 0.103 Uiso 1 1 calc R U . . .
H24C H 0.5673 0.6879 0.7745 0.103 Uiso 1 1 calc R U . . .
C25 C -0.0205(3) 0.7093(3) 0.8205(2) 0.0528(8) Uani 1 1 d . . . . .
H25 H 0.0469 0.6612 0.7875 0.063 Uiso 1 1 calc R U . . .
C26 C -0.0847(4) 0.8327(3) 0.7863(2) 0.0556(8) Uani 1 1 d . . . . .
H26 H -0.0701 0.8850 0.7267 0.067 Uiso 1 1 calc R U . . .
C27 C -0.1624(3) 0.7625(3) 0.9290(2) 0.0458(7) Uani 1 1 d . . . . .
H27 H -0.2137 0.7596 0.9862 0.055 Uiso 1 1 calc R U . . .
C28 C -0.2645(4) 0.9931(3) 0.8529(3) 0.0760(11) Uani 1 1 d . . . . .
H28A H -0.3295 0.9848 0.9089 0.114 Uiso 1 1 calc R U . . .
H28B H -0.3220 1.0116 0.8044 0.114 Uiso 1 1 calc R U . . .
H28C H -0.2004 1.0664 0.8430 0.114 Uiso 1 1 calc R U . . .
N N 0.1592(3) 0.0178(2) 0.88076(17) 0.0444(6) Uani 1 1 d . . . . .
N1 N 0.3734(3) 0.3760(3) 0.64498(17) 0.0506(6) Uani 1 1 d . . . . .
N2 N 0.0432(3) 0.1327(3) 0.6563(2) 0.0649(8) Uani 1 1 d . . . . .
N3 N 0.0383(3) 0.3677(3) 0.86662(19) 0.0569(7) Uani 1 1 d . . . . .
N4 N 0.4645(3) 0.2016(3) 0.9046(2) 0.0736(9) Uani 1 1 d . . . . .
N5 N 0.4761(3) -0.0410(3) 0.7231(2) 0.0672(8) Uani 1 1 d . . . . .
N11 N 0.4127(2) 0.6789(2) 0.52381(17) 0.0419(6) Uani 1 1 d . . . . .
N12 N 0.3207(3) 0.8882(3) 0.5089(2) 0.0714(9) Uani 1 1 d . . . . .
N13 N 0.6756(2) 0.5119(2) 0.56074(16) 0.0401(5) Uani 1 1 d . . . . .
N14 N 0.8834(3) 0.5782(3) 0.58228(19) 0.0502(6) Uani 1 1 d . . . . .
N21 N 0.2092(2) 0.5600(2) 0.95996(17) 0.0440(6) Uani 1 1 d . . . . .
N22 N 0.4316(2) 0.6021(2) 0.88598(17) 0.0440(6) Uani 1 1 d . . . . .
N23 N -0.0692(2) 0.6654(2) 0.91074(15) 0.0401(5) Uani 1 1 d . . . . .
N24 N -0.1752(3) 0.8657(2) 0.85631(17) 0.0461(6) Uani 1 1 d . . . . .
O O 0.1075(3) -0.0682(2) 0.93761(17) 0.0789(8) Uani 1 1 d . . . . .
Fe Fe 0.23401(4) 0.14354(4) 0.79933(3) 0.03440(12) Uani 1 1 d . . . . .
Cu1 Cu 0.5000 0.5000 0.5000 0.03677(13) Uani 1 2 d S . P . .
Cu2 Cu 0.0000 0.5000 1.0000 0.05386(17) Uani 1 2 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.137(3) . ?
C1 Fe 1.936(3) . ?
C2 N2 1.147(4) . ?
C2 Fe 1.944(3) . ?
C3 N3 1.142(3) . ?
C3 Fe 1.945(3) . ?
C4 N4 1.136(4) . ?
C4 Fe 1.942(3) . ?
C5 N5 1.143(3) . ?
C5 Fe 1.936(3) . ?
C11 C12 1.336(4) . ?
C11 N11 1.364(4) . ?
C12 N12 1.346(5) . ?
C13 N11 1.299(4) . ?
C13 N12 1.340(4) . ?
C14 N12 1.468(5) . ?
C15 C16 1.348(4) . ?
C15 N13 1.369(4) . ?
C16 N14 1.345(4) . ?
C17 N13 1.312(4) . ?
C17 N14 1.334(4) . ?
C18 N14 1.463(4) . ?
C21 C22 1.341(4) . ?
C21 N21 1.362(4) . ?
C22 N22 1.351(4) . ?
C23 N21 1.313(4) . ?
C23 N22 1.332(4) . ?
C24 N22 1.457(4) . ?
C25 C26 1.345(4) . ?
C25 N23 1.365(4) . ?
C26 N24 1.359(4) . ?
C27 N23 1.308(3) . ?
C27 N24 1.330(4) . ?
C28 N24 1.464(4) . ?
N O 1.136(3) . ?
N Fe 1.644(3) . ?
N1 Cu1 2.425(3) . ?
N11 Cu1 2.032(2) . ?
N13 Cu1 2.030(2) . ?
N21 Cu2 2.013(2) . ?
N23 Cu2 1.995(2) . ?
Cu1 N13 2.030(2) 2_666 ?
Cu1 N11 2.032(2) 2_666 ?
Cu1 N1 2.425(3) 2_666 ?
Cu2 N23 1.995(2) 2_567 ?
Cu2 N21 2.013(2) 2_567 ?

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
N1 C1 Fe 179.1(2) . . ?
N2 C2 Fe 177.1(3) . . ?
N3 C3 Fe 174.4(3) . . ?
N4 C4 Fe 178.8(3) . . ?
N5 C5 Fe 177.5(3) . . ?
C12 C11 N11 109.7(3) . . ?
C11 C12 N12 107.0(3) . . ?
N11 C13 N12 112.0(3) . . ?
C16 C15 N13 109.3(3) . . ?
N14 C16 C15 106.8(3) . . ?
N13 C17 N14 111.6(3) . . ?
C22 C21 N21 109.6(3) . . ?
C21 C22 N22 106.7(3) . . ?
N21 C23 N22 111.4(3) . . ?
C26 C25 N23 109.7(3) . . ?
C25 C26 N24 106.3(3) . . ?
N23 C27 N24 112.0(3) . . ?
O N Fe 179.3(2) . . ?
C1 N1 Cu1 162.0(2) . . ?
C13 N11 C11 105.0(3) . . ?
C13 N11 Cu1 129.5(2) . . ?
C11 N11 Cu1 125.4(2) . . ?
C13 N12 C12 106.3(3) . . ?
C13 N12 C14 126.7(4) . . ?
C12 N12 C14 127.0(3) . . ?
C17 N13 C15 105.1(3) . . ?
C17 N13 Cu1 125.7(2) . . ?
C15 N13 Cu1 129.2(2) . . ?
C17 N14 C16 107.2(3) . . ?
C17 N14 C18 126.0(3) . . ?
C16 N14 C18 126.8(3) . . ?
C23 N21 C21 105.2(2) . . ?
C23 N21 Cu2 129.9(2) . . ?
C21 N21 Cu2 124.8(2) . . ?
C23 N22 C22 107.0(3) . . ?
C23 N22 C24 126.6(3) . . ?
C22 N22 C24 126.4(3) . . ?
C27 N23 C25 105.1(2) . . ?
C27 N23 Cu2 126.2(2) . . ?
C25 N23 Cu2 128.39(19) . . ?
C27 N24 C26 106.9(2) . . ?
C27 N24 C28 126.7(3) . . ?
C26 N24 C28 126.4(3) . . ?
N Fe C1 179.39(12) . . ?
N Fe C5 94.58(12) . . ?
C1 Fe C5 85.10(12) . . ?
N Fe C4 95.99(13) . . ?
C1 Fe C4 84.53(12) . . ?
C5 Fe C4 87.59(11) . . ?
N Fe C2 96.34(12) . . ?
C1 Fe C2 83.14(11) . . ?
C5 Fe C2 89.82(12) . . ?
C4 Fe C2 167.57(12) . . ?
N Fe C3 94.56(11) . . ?
C1 Fe C3 85.79(11) . . ?
C5 Fe C3 170.14(12) . . ?
C4 Fe C3 87.79(11) . . ?
C2 Fe C3 92.82(12) . . ?
N13 Cu1 N13 180.0 . 2_666 ?
N13 Cu1 N11 90.46(9) . 2_666 ?
N13 Cu1 N11 89.54(9) 2_666 2_666 ?
N13 Cu1 N11 89.54(9) . . ?
N13 Cu1 N11 90.46(9) 2_666 . ?
N11 Cu1 N11 180.00(12) 2_666 . ?
N13 Cu1 N1 90.95(9) . 2_666 ?
N13 Cu1 N1 89.05(9) 2_666 2_666 ?
N11 Cu1 N1 90.09(9) 2_666 2_666 ?
N11 Cu1 N1 89.91(9) . 2_666 ?
N13 Cu1 N1 89.05(9) . . ?
N13 Cu1 N1 90.95(9) 2_666 . ?
N11 Cu1 N1 89.91(9) 2_666 . ?
N11 Cu1 N1 90.09(9) . . ?
N1 Cu1 N1 180.0 2_666 . ?
N23 Cu2 N23 180.0 2_567 . ?
N23 Cu2 N21 90.72(9) 2_567 . ?
N23 Cu2 N21 89.28(9) . . ?
N23 Cu2 N21 89.28(9) 2_567 2_567 ?
N23 Cu2 N21 90.72(9) . 2_567 ?
N21 Cu2 N21 180.00(13) . 2_567 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14A N5 0.96 2.50 3.402(6) 156.2 2_666
C17 H17 N1 0.93 2.67 3.190(4) 115.9 2_666
C21 H21 N3 0.93 2.63 3.268(4) 126.6 2_567
C22 H22 N4 0.93 2.55 3.312(4) 138.8 2_667
C23 H23 N3 0.93 2.70 3.306(4) 123.9 .
C26 H26 N2 0.93 2.70 3.365(4) 129.4 1_565
C27 H27 N4 0.93 2.69 3.532(4) 150.9 2_567
C28 H28B N5 0.96 2.59 3.472(5) 153.6 1_465

_refine_diff_density_max         0.312
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.056


_exptl_crystal_recrystallization_method 
'Crystals obtained from a DMF solution of the reactants by very slow evaporation of the solvent.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2014752'
loop_
_audit_author_name
_audit_author_address
'Oscar Enrique Piro'
;Universidad Nacional de La Plata
Argentina
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
catena-[tetrakis(u-cyano)-cyano-bis(1-methylimidazole)-nitrosyl-iron-zinc]
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H12 Fe N10 O Zn'
_chemical_formula_weight         445.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   14.8493(11)
_cell_length_b                   14.4980(10)
_cell_length_c                   16.5461(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3562.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1136
_cell_measurement_theta_min      3.6480
_cell_measurement_theta_max      28.5230
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 1.0004 0.0012 0.0008 -0.0069 -0.9972 0.0328 0.0026 -0.0512 -0.9998
_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    2.186
_shelx_estimated_absorpt_T_min   0.776
_shelx_estimated_absorpt_T_max   0.882
_exptl_absorpt_correction_T_min  0.78636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            7971
_diffrn_reflns_av_unetI/netI     0.1318
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.810
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measured_fraction_theta_full 0.851
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_Laue_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_point_group_measured_fraction_full 0.851
_reflns_number_total             2946
_reflns_number_gt                1267
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement. 
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          Twin,Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0426P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2946
_refine_ls_number_parameters     237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   0.762
_refine_ls_restrained_S_all      0.762
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form 
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.851 Why?  
RESPONSE:The X-ray diffraction pattern can be mainly described in terms of
two crystal domains (twin). The Bragg reflection intensities of the dominant 
domain were perturbed due to their overlapping with the ones of a second domain 
(of about 23 percent scattering power) that integrates the sample and it is 
rotated in about 180 degrees around the reciprocal a*-axis of the dominant 
domain. Reflections of this domain having a degree of overlapping higher than 
80 percent with the minor domain were removed from the diffraction data set. 
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        477 Report
RESPONSE: Same as for _vrf_PLAT029_shelx. 
;
# end Validation Reply Form 
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3376(5) 0.3812(4) 0.2447(3) 0.0162(14) Uani 1 1 d . . . . .
C2 C 0.3377(5) 0.1931(4) 0.2496(3) 0.0175(15) Uani 1 1 d . . . . .
C3 C 0.1527(5) 0.1950(4) 0.2141(3) 0.0185(16) Uani 1 1 d . . . . .
C4 C 0.1567(5) 0.3811(4) 0.2124(3) 0.0167(16) Uani 1 1 d . . . . .
C5 C 0.2728(5) 0.2822(4) 0.1239(3) 0.0205(16) Uani 1 1 d . . . . .
C11 C 0.5110(5) 0.4111(5) 0.0914(4) 0.037(2) Uani 1 1 d . . . . .
H11 H 0.4624 0.3747 0.1067 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5621(5) 0.3973(5) 0.0252(4) 0.0310(19) Uani 1 1 d . . . . .
H12 H 0.5553 0.3503 -0.0126 0.037 Uiso 1 1 calc R U . . .
C13 C 0.6096(6) 0.5158(4) 0.0899(3) 0.0311(19) Uani 1 1 d . . . . .
H13 H 0.6445 0.5669 0.1032 0.037 Uiso 1 1 calc R U . . .
C14 C 0.6969(6) 0.4760(5) -0.0369(4) 0.049(2) Uani 1 1 d . . . . .
H14A H 0.7287 0.4189 -0.0439 0.074 Uiso 1 1 calc R U . . .
H14B H 0.7379 0.5226 -0.0185 0.074 Uiso 1 1 calc R U . . .
H14C H 0.6710 0.4946 -0.0875 0.074 Uiso 1 1 calc R U . . .
C21 C 0.3943(6) 0.5798(5) 0.4065(4) 0.041(2) Uani 1 1 d . . . . .
H21 H 0.3396 0.5600 0.3852 0.049 Uiso 1 1 calc R U . . .
C22 C 0.4045(7) 0.6124(6) 0.4812(4) 0.047(2) Uani 1 1 d . . . . .
H22 H 0.3598 0.6199 0.5200 0.056 Uiso 1 1 calc R U . . .
C23 C 0.5322(6) 0.6108(5) 0.4171(3) 0.035(2) Uani 1 1 d . . . . .
H23 H 0.5932 0.6179 0.4060 0.042 Uiso 1 1 calc R U . . .
C24 C 0.5399(6) 0.6683(5) 0.5596(3) 0.049(3) Uani 1 1 d . . . . .
H24A H 0.5827 0.7140 0.5428 0.073 Uiso 1 1 calc R U . . .
H24B H 0.5707 0.6189 0.5866 0.073 Uiso 1 1 calc R U . . .
H24C H 0.4971 0.6957 0.5959 0.073 Uiso 1 1 calc R U . . .
N N 0.2232(4) 0.2892(4) 0.3357(2) 0.0267(14) Uani 1 1 d . . . . .
N1 N 0.3920(4) 0.4354(4) 0.2500(2) 0.0244(14) Uani 1 1 d . . . . .
N2 N 0.3922(4) 0.1401(4) 0.2578(2) 0.0254(14) Uani 1 1 d . . . . .
N3 N 0.0988(4) 0.1415(4) 0.2045(3) 0.0254(14) Uani 1 1 d . . . . .
N4 N 0.1036(5) 0.4364(4) 0.2023(3) 0.0290(15) Uani 1 1 d . . . . .
N5 N 0.2939(4) 0.2795(4) 0.0575(3) 0.0395(17) Uani 1 1 d . . . . .
N11 N 0.5415(4) 0.4870(3) 0.1330(3) 0.0209(14) Uani 1 1 d . . . . .
N12 N 0.6237(4) 0.4633(4) 0.0243(2) 0.0269(14) Uani 1 1 d . . . . .
N21 N 0.4729(4) 0.5788(3) 0.3655(3) 0.0246(15) Uani 1 1 d . . . . .
N22 N 0.4929(5) 0.6322(4) 0.4890(3) 0.0341(16) Uani 1 1 d . . . . .
O O 0.2129(4) 0.2899(4) 0.4032(2) 0.066(2) Uani 1 1 d . . . . .
Fe Fe 0.24470(7) 0.28717(5) 0.23834(3) 0.0141(2) Uani 1 1 d . . . . .
Zn Zn 0.50110(7) 0.53730(4) 0.24679(4) 0.0181(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.131(8) . ?
C1 Fe 1.942(7) . ?
C2 N2 1.125(8) . ?
C2 Fe 1.950(7) . ?
C3 N3 1.126(8) . ?
C3 Fe 1.953(7) . ?
C4 N4 1.137(7) . ?
C4 Fe 1.935(7) . ?
C5 N5 1.142(6) . ?
C5 Fe 1.941(5) . ?
C11 C12 1.347(9) . ?
C11 N11 1.374(7) . ?
C12 N12 1.324(8) . ?
C13 N11 1.307(8) . ?
C13 N12 1.343(7) . ?
C14 N12 1.496(9) . ?
C21 C22 1.331(9) . ?
C21 N21 1.351(9) . ?
C22 N22 1.350(10) . ?
C23 N21 1.312(8) . ?
C23 N22 1.362(8) . ?
C24 N22 1.458(8) . ?
N O 1.127(5) . ?
N Fe 1.643(4) . ?
N1 Zn 2.192(6) . ?
N2 Zn 2.176(6) 3_645 ?
N3 Zn 2.230(6) 8_655 ?
N4 Zn 2.273(6) 6_556 ?
N11 Zn 2.106(5) . ?
N21 Zn 2.096(5) . ?
Zn N2 2.176(6) 3_655 ?
Zn N3 2.230(6) 8_665 ?
Zn N4 2.273(6) 6_656 ?

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
N1 C1 Fe 178.6(5) . . ?
N2 C2 Fe 178.3(6) . . ?
N3 C3 Fe 176.2(5) . . ?
N4 C4 Fe 175.5(5) . . ?
N5 C5 Fe 176.5(6) . . ?
C12 C11 N11 110.0(7) . . ?
N12 C12 C11 106.9(5) . . ?
N11 C13 N12 112.4(6) . . ?
C22 C21 N21 111.8(7) . . ?
C21 C22 N22 106.0(7) . . ?
N21 C23 N22 111.2(7) . . ?
O N Fe 176.6(5) . . ?
C1 N1 Zn 173.9(5) . . ?
C2 N2 Zn 171.1(4) . 3_645 ?
C3 N3 Zn 153.6(5) . 8_655 ?
C4 N4 Zn 149.8(4) . 6_556 ?
C13 N11 C11 103.7(5) . . ?
C13 N11 Zn 126.7(4) . . ?
C11 N11 Zn 129.1(5) . . ?
C12 N12 C13 107.1(6) . . ?
C12 N12 C14 126.8(5) . . ?
C13 N12 C14 126.2(6) . . ?
C23 N21 C21 104.5(5) . . ?
C23 N21 Zn 125.2(5) . . ?
C21 N21 Zn 130.3(5) . . ?
C23 N22 C22 106.5(6) . . ?
C23 N22 C24 125.2(8) . . ?
C22 N22 C24 128.2(6) . . ?
N Fe C2 93.2(2) . . ?
N Fe C1 94.2(2) . . ?
C2 Fe C1 89.0(3) . . ?
N Fe C3 94.5(3) . . ?
C2 Fe C3 92.1(3) . . ?
C1 Fe C3 171.2(2) . . ?
N Fe C4 94.3(2) . . ?
C2 Fe C4 172.5(2) . . ?
C1 Fe C4 89.9(2) . . ?
C3 Fe C4 87.9(2) . . ?
N Fe C5 178.4(3) . . ?
C2 Fe C5 85.2(2) . . ?
C1 Fe C5 85.8(2) . . ?
C3 Fe C5 85.7(2) . . ?
C4 Fe C5 87.4(2) . . ?
N21 Zn N11 173.6(2) . . ?
N21 Zn N2 88.94(19) . 3_655 ?
N11 Zn N2 89.93(19) . 3_655 ?
N21 Zn N1 91.33(19) . . ?
N11 Zn N1 89.92(19) . . ?
N2 Zn N1 178.9(2) 3_655 . ?
N21 Zn N3 88.06(19) . 8_665 ?
N11 Zn N3 98.26(18) . 8_665 ?
N2 Zn N3 90.5(2) 3_655 8_665 ?
N1 Zn N3 88.4(2) . 8_665 ?
N21 Zn N4 88.39(19) . 6_656 ?
N11 Zn N4 85.28(19) . 6_656 ?
N2 Zn N4 88.0(2) 3_655 6_656 ?
N1 Zn N4 93.0(2) . 6_656 ?
N3 Zn N4 176.19(18) 8_665 6_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C13 H13 N2 0.93 2.59 3.098(7) 114.8 3_655
C24 H24A N5 0.96 2.65 3.529(10) 152.6 3_655

_refine_diff_density_max         1.301
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.113


_exptl_crystal_recrystallization_method 
'Crystals obtained employing a U-shaped tube by inter-diffusion of a sodium nitroprusside aqueous solution in one arm of the tube with a 1-methylimidazole solution of the metal chloride salt in the other arm.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2014751'
loop_
_audit_author_name
_audit_author_address
'Oscar Enrique Piro'
;Universidad Nacional de La Plata
Argentina
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
catena-[tetrakis(u-cyano)-cyano-bis(1-methylimidazole)-nitrosyl-iron-manganese]
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H12 Fe Mn N10 O'
_chemical_formula_weight         435.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4311(10)
_cell_length_b                   14.9364(15)
_cell_length_c                   14.6337(16)
_cell_angle_alpha                90
_cell_angle_beta                 97.228(11)
_cell_angle_gamma                90
_cell_volume                     1828.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1086
_cell_measurement_theta_min      3.9450
_cell_measurement_theta_max      26.7220
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 1.0014 -0.0004 0.1462 -0.0017 -1.0009 0.0003 0.0013 -0.0004 -1.0009
_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    1.509
_shelx_estimated_absorpt_T_min   0.730
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_T_min  0.95751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            8308
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.983
_diffrn_reflns_theta_max         25.985
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.798
_diffrn_measured_fraction_theta_full 0.805
_diffrn_reflns_Laue_measured_fraction_max 0.798
_diffrn_reflns_Laue_measured_fraction_full 0.805
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_point_group_measured_fraction_full 0.805
_reflns_number_total             2866
_reflns_number_gt                1388
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement. 
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          Twin,Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0444P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2866
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_restrained_S_all      0.813
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.805 Why?  
RESPONSE: The X-ray diffraction pattern can be mainly described in terms of
two crystal domains (twin). The Bragg reflection intensities of the dominant 
domain were perturbed due to overlapping with the ones of a second domain 
(of about 34 percent scattering power) that integrates the sample and it is 
rotated in about 180 degrees around the reciprocal a*-axis of the dominant 
domain. Reflections of this domain having a degree of overlapping higher than 
80 percent with the minor domain were removed from the diffraction data set.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        639 Report
RESPONSE: Same as for _vrf_PLAT029_shelx.
;
# end Validation Reply Form
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4936(6) 0.3362(4) 0.6582(4) 0.0208(13) Uani 1 1 d . . . . .
C2 C 0.4299(6) 0.1553(3) 0.6525(3) 0.0173(12) Uani 1 1 d . . . . .
C3 C 0.4255(6) 0.1529(4) 0.8369(4) 0.0206(13) Uani 1 1 d . . . . .
C4 C 0.4976(6) 0.3344(4) 0.8458(4) 0.0191(13) Uani 1 1 d . . . . .
C5 C 0.2509(6) 0.2720(4) 0.7350(3) 0.0226(12) Uani 1 1 d . . . . .
C11 C 0.8263(8) 0.4871(4) 0.3992(4) 0.0471(19) Uani 1 1 d . . . . .
H11 H 0.7998 0.5368 0.3622 0.057 Uiso 1 1 calc R U . . .
C12 C 0.9556(7) 0.4346(5) 0.3947(4) 0.0458(17) Uani 1 1 d . . . . .
H12 H 1.0309 0.4410 0.3539 0.055 Uiso 1 1 calc R U . . .
C13 C 0.8250(6) 0.3866(4) 0.5030(4) 0.0386(16) Uani 1 1 d . . . . .
H13 H 0.7976 0.3529 0.5521 0.046 Uiso 1 1 calc R U . . .
C14 C 1.0746(7) 0.3001(5) 0.4825(5) 0.058(2) Uani 1 1 d . . . . .
H14A H 1.0530 0.2692 0.5371 0.088 Uiso 1 1 calc R U . . .
H14B H 1.1795 0.3261 0.4926 0.088 Uiso 1 1 calc R U . . .
H14C H 1.0693 0.2586 0.4321 0.088 Uiso 1 1 calc R U . . .
C21 C 0.1641(7) -0.1024(4) 0.4374(5) 0.0502(19) Uani 1 1 d . . . . .
H21 H 0.2010 -0.1554 0.4659 0.060 Uiso 1 1 calc R U . . .
C22 C 0.0166(7) -0.0905(4) 0.3914(5) 0.058(2) Uani 1 1 d . . . . .
H22 H -0.0646 -0.1328 0.3818 0.069 Uiso 1 1 calc R U . . .
C23 C 0.1539(7) 0.0313(4) 0.3909(4) 0.0404(17) Uani 1 1 d . . . . .
H23 H 0.1811 0.0903 0.3799 0.048 Uiso 1 1 calc R U . . .
C24 C -0.1267(6) 0.0419(5) 0.3109(4) 0.0503(19) Uani 1 1 d . . . . .
H24A H -0.1905 -0.0001 0.2725 0.075 Uiso 1 1 calc R U . . .
H24B H -0.0885 0.0877 0.2732 0.075 Uiso 1 1 calc R U . . .
H24C H -0.1903 0.0686 0.3536 0.075 Uiso 1 1 calc R U . . .
N N 0.6716(5) 0.2216(3) 0.7617(3) 0.0296(11) Uani 1 1 d . . . . .
N1 N 0.5040(5) 0.3906(3) 0.6051(3) 0.0300(12) Uani 1 1 d . . . . .
N2 N 0.4149(5) 0.1017(3) 0.5970(3) 0.0294(12) Uani 1 1 d . . . . .
N3 N 0.4025(5) 0.0984(3) 0.8891(3) 0.0293(12) Uani 1 1 d . . . . .
N4 N 0.5120(5) 0.3877(3) 0.9002(3) 0.0284(12) Uani 1 1 d . . . . .
N5 N 0.1196(6) 0.2900(4) 0.7281(3) 0.0434(14) Uani 1 1 d . . . . .
N11 N 0.7396(5) 0.4564(3) 0.4665(3) 0.0298(12) Uani 1 1 d . . . . .
N12 N 0.9555(5) 0.3710(3) 0.4605(3) 0.0355(12) Uani 1 1 d . . . . .
N21 N 0.2505(5) -0.0265(3) 0.4361(3) 0.0265(11) Uani 1 1 d . . . . .
N22 N 0.0105(5) -0.0051(3) 0.3622(3) 0.0350(14) Uani 1 1 d . . . . .
O O 0.8032(5) 0.2092(4) 0.7693(4) 0.0765(17) Uani 1 1 d . . . . .
Mn1 Mn 0.5000 0.5000 0.5000 0.0196(3) Uani 1 2 d S . P . .
Mn2 Mn 0.5000 0.0000 0.5000 0.0156(3) Uani 1 2 d S . P . .
Fe Fe 0.47774(8) 0.24302(5) 0.74945(5) 0.0157(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.135(6) . ?
C1 Fe 1.945(6) . ?
C2 N2 1.136(6) . ?
C2 Fe 1.936(5) . ?
C3 N3 1.149(6) . ?
C3 Fe 1.945(6) . ?
C4 N4 1.122(6) . ?
C4 Fe 1.954(6) . ?
C5 N5 1.131(6) . ?
C5 Fe 1.946(5) . ?
C11 C12 1.351(8) . ?
C11 N11 1.376(7) . ?
C12 N12 1.353(7) . ?
C13 N11 1.339(7) . ?
C13 N12 1.351(7) . ?
C14 N12 1.467(7) . ?
C21 N21 1.349(7) . ?
C21 C22 1.350(7) . ?
C22 N22 1.344(7) . ?
C23 N21 1.308(7) . ?
C23 N22 1.343(6) . ?
C24 N22 1.474(7) . ?
N O 1.117(5) . ?
N Fe 1.653(5) . ?
N1 Mn1 2.242(5) . ?
N2 Mn2 2.256(5) . ?
N3 Mn1 2.267(4) 2_646 ?
N4 Mn2 2.235(5) 2_656 ?
N11 Mn1 2.235(4) . ?
N21 Mn2 2.227(4) . ?
Mn1 N11 2.235(4) 3_666 ?
Mn1 N1 2.242(5) 3_666 ?
Mn1 N3 2.267(4) 2_656 ?
Mn1 N3 2.267(4) 4_565 ?
Mn2 N21 2.227(4) 3_656 ?
Mn2 N4 2.235(5) 4_565 ?
Mn2 N4 2.235(5) 2_646 ?
Mn2 N2 2.256(5) 3_656 ?

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
N1 C1 Fe 179.5(5) . . ?
N2 C2 Fe 174.3(5) . . ?
N3 C3 Fe 176.6(5) . . ?
N4 C4 Fe 178.4(5) . . ?
N5 C5 Fe 178.6(5) . . ?
C12 C11 N11 110.3(6) . . ?
C11 C12 N12 107.4(6) . . ?
N11 C13 N12 112.3(5) . . ?
N21 C21 C22 110.3(5) . . ?
N22 C22 C21 106.3(5) . . ?
N21 C23 N22 111.8(5) . . ?
O N Fe 178.3(5) . . ?
C1 N1 Mn1 174.6(5) . . ?
C2 N2 Mn2 155.2(4) . . ?
C3 N3 Mn1 149.2(4) . 2_646 ?
C4 N4 Mn2 170.7(4) . 2_656 ?
C13 N11 C11 103.7(5) . . ?
C13 N11 Mn1 126.5(4) . . ?
C11 N11 Mn1 129.5(4) . . ?
C13 N12 C12 106.2(5) . . ?
C13 N12 C14 126.8(5) . . ?
C12 N12 C14 126.9(5) . . ?
C23 N21 C21 105.0(5) . . ?
C23 N21 Mn2 126.2(4) . . ?
C21 N21 Mn2 128.8(4) . . ?
C22 N22 C23 106.7(5) . . ?
C22 N22 C24 127.6(5) . . ?
C23 N22 C24 125.8(5) . . ?
N11 Mn1 N11 180.0 . 3_666 ?
N11 Mn1 N1 89.88(17) . 3_666 ?
N11 Mn1 N1 90.12(17) 3_666 3_666 ?
N11 Mn1 N1 90.12(17) . . ?
N11 Mn1 N1 89.88(17) 3_666 . ?
N1 Mn1 N1 180.0 3_666 . ?
N11 Mn1 N3 95.16(16) . 2_656 ?
N11 Mn1 N3 84.84(16) 3_666 2_656 ?
N1 Mn1 N3 89.51(16) 3_666 2_656 ?
N1 Mn1 N3 90.49(16) . 2_656 ?
N11 Mn1 N3 84.84(16) . 4_565 ?
N11 Mn1 N3 95.16(16) 3_666 4_565 ?
N1 Mn1 N3 90.49(16) 3_666 4_565 ?
N1 Mn1 N3 89.51(16) . 4_565 ?
N3 Mn1 N3 180.00(18) 2_656 4_565 ?
N21 Mn2 N21 180.0 . 3_656 ?
N21 Mn2 N4 88.69(16) . 4_565 ?
N21 Mn2 N4 91.31(16) 3_656 4_565 ?
N21 Mn2 N4 91.31(16) . 2_646 ?
N21 Mn2 N4 88.69(16) 3_656 2_646 ?
N4 Mn2 N4 180.0 4_565 2_646 ?
N21 Mn2 N2 91.43(16) . . ?
N21 Mn2 N2 88.56(16) 3_656 . ?
N4 Mn2 N2 87.12(17) 4_565 . ?
N4 Mn2 N2 92.88(17) 2_646 . ?
N21 Mn2 N2 88.57(16) . 3_656 ?
N21 Mn2 N2 91.44(16) 3_656 3_656 ?
N4 Mn2 N2 92.88(17) 4_565 3_656 ?
N4 Mn2 N2 87.12(17) 2_646 3_656 ?
N2 Mn2 N2 180.00(17) . 3_656 ?
N Fe C2 93.4(2) . . ?
N Fe C3 95.6(2) . . ?
C2 Fe C3 88.3(2) . . ?
N Fe C4 93.6(2) . . ?
C2 Fe C4 172.9(2) . . ?
C3 Fe C4 90.8(2) . . ?
N Fe C5 178.3(2) . . ?
C2 Fe C5 87.7(2) . . ?
C3 Fe C5 85.7(2) . . ?
C4 Fe C5 85.2(2) . . ?
N Fe C1 93.5(2) . . ?
C2 Fe C1 90.4(2) . . ?
C3 Fe C1 170.9(2) . . ?
C4 Fe C1 89.3(2) . . ?
C5 Fe C1 85.3(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C24 H24B N5 0.96 2.67 3.566(8) 155.2 4_565

_refine_diff_density_max         1.175
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.100


_exptl_crystal_recrystallization_method 
'Crystals obtained employing a U-shaped tube by inter-diffusion of a sodium nitroprusside aqueous solution in one arm of the tube with a 1-methylimidazole solution of the metal chloride salt in the other arm.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2014753'
loop_
_audit_author_name
_audit_author_address
'Oscar Enrique Piro'
;Universidad Nacional de La Plata
Argentina
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
catena-[tetrakis(u-cyano)-cyano-bis(1-methylimidazole)-nitrosyl-iron-cadmium]
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H12 Cd Fe N10 O'
_chemical_formula_weight         492.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4002(3)
_cell_length_b                   15.2133(5)
_cell_length_c                   14.8960(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.048(3)
_cell_angle_gamma                90
_cell_volume                     1884.88(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1711
_cell_measurement_theta_min      4.0010
_cell_measurement_theta_max      28.2600
_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.062
_exptl_absorpt_coefficient_mu    1.922
_shelx_estimated_absorpt_T_min   0.698
_shelx_estimated_absorpt_T_max   0.890
_exptl_absorpt_correction_T_min  0.97437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            7780
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3693
_reflns_number_gt                2541
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement. 
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+0.7299P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3693
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4942(5) 0.3341(3) 0.6605(3) 0.0298(10) Uani 1 1 d . . . . .
C2 C 0.4250(5) 0.1576(3) 0.6528(3) 0.0313(10) Uani 1 1 d . . . . .
C3 C 0.4209(5) 0.1540(3) 0.8336(3) 0.0299(10) Uani 1 1 d . . . . .
C4 C 0.4982(5) 0.3304(3) 0.8446(3) 0.0297(10) Uani 1 1 d . . . . .
C5 C 0.2486(6) 0.2731(3) 0.7341(3) 0.0311(10) Uani 1 1 d . . . . .
C11 C 0.8304(7) 0.4840(3) 0.4012(4) 0.0526(14) Uani 1 1 d . . . . .
H11 H 0.8030 0.5327 0.3645 0.063 Uiso 1 1 calc R U . . .
C12 C 0.9610(7) 0.4327(3) 0.3976(4) 0.0551(15) Uani 1 1 d . . . . .
H12 H 1.0378 0.4393 0.3587 0.066 Uiso 1 1 calc R U . . .
C13 C 0.8272(6) 0.3841(3) 0.5021(3) 0.0503(14) Uani 1 1 d . . . . .
H13 H 0.7982 0.3499 0.5488 0.060 Uiso 1 1 calc R U . . .
C14 C 1.0774(7) 0.2990(4) 0.4816(4) 0.0678(17) Uani 1 1 d . . . . .
H14A H 1.0548 0.2662 0.5335 0.102 Uiso 1 1 calc R U . . .
H14B H 1.1830 0.3241 0.4941 0.102 Uiso 1 1 calc R U . . .
H14C H 1.0724 0.2605 0.4302 0.102 Uiso 1 1 calc R U . . .
C21 C 0.1566(6) -0.0990(3) 0.4342(4) 0.0637(17) Uani 1 1 d . . . . .
H21 H 0.1918 -0.1510 0.4633 0.076 Uiso 1 1 calc R U . . .
C22 C 0.0096(7) -0.0861(4) 0.3875(4) 0.0743(19) Uani 1 1 d . . . . .
H22 H -0.0731 -0.1272 0.3783 0.089 Uiso 1 1 calc R U . . .
C23 C 0.1490(6) 0.0296(3) 0.3849(4) 0.0513(14) Uani 1 1 d . . . . .
H23 H 0.1788 0.0865 0.3719 0.062 Uiso 1 1 calc R U . . .
C24 C -0.1317(6) 0.0405(4) 0.3052(4) 0.0626(16) Uani 1 1 d . . . . .
H24A H -0.2031 0.0613 0.3455 0.094 Uiso 1 1 calc R U . . .
H24B H -0.1880 0.0001 0.2624 0.094 Uiso 1 1 calc R U . . .
H24C H -0.0940 0.0894 0.2733 0.094 Uiso 1 1 calc R U . . .
N N 0.6719(5) 0.2191(2) 0.7628(3) 0.0395(10) Uani 1 1 d . . . . .
N1 N 0.5043(5) 0.3877(2) 0.6085(3) 0.0425(10) Uani 1 1 d . . . . .
N2 N 0.4050(5) 0.1056(3) 0.5972(3) 0.0438(10) Uani 1 1 d . . . . .
N3 N 0.3926(5) 0.1016(2) 0.8829(3) 0.0422(10) Uani 1 1 d . . . . .
N4 N 0.5155(5) 0.3824(3) 0.8994(3) 0.0429(10) Uani 1 1 d . . . . .
N5 N 0.1166(5) 0.2927(3) 0.7247(3) 0.0529(11) Uani 1 1 d . . . . .
N11 N 0.7438(5) 0.4536(3) 0.4669(3) 0.0410(10) Uani 1 1 d . . . . .
N12 N 0.9578(5) 0.3697(3) 0.4619(3) 0.0463(10) Uani 1 1 d . . . . .
N21 N 0.2451(4) -0.0258(2) 0.4325(3) 0.0362(9) Uani 1 1 d . . . . .
N22 N 0.0040(5) -0.0037(3) 0.3569(3) 0.0425(10) Uani 1 1 d . . . . .
O O 0.8026(5) 0.2058(3) 0.7701(3) 0.0910(15) Uani 1 1 d . . . . .
Fe Fe 0.47669(7) 0.24272(3) 0.74949(4) 0.02312(15) Uani 1 1 d . . . . .
Cd1 Cd 0.5000 0.5000 0.5000 0.02993(15) Uani 1 2 d S . P . .
Cd2 Cd 0.5000 0.0000 0.5000 0.02394(14) Uani 1 2 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.136(5) . ?
C1 Fe 1.940(4) . ?
C2 N2 1.140(5) . ?
C2 Fe 1.940(5) . ?
C3 N3 1.132(5) . ?
C3 Fe 1.943(4) . ?
C4 N4 1.131(5) . ?
C4 Fe 1.936(5) . ?
C5 N5 1.138(5) . ?
C5 Fe 1.953(5) . ?
C11 C12 1.353(7) . ?
C11 N11 1.379(6) . ?
C12 N12 1.359(6) . ?
C13 N11 1.333(6) . ?
C13 N12 1.338(6) . ?
C14 N12 1.473(6) . ?
C21 N21 1.341(6) . ?
C21 C22 1.345(7) . ?
C22 N22 1.332(6) . ?
C23 N21 1.306(6) . ?
C23 N22 1.331(6) . ?
C24 N22 1.449(6) . ?
N O 1.107(5) . ?
N Fe 1.663(4) . ?
N1 Cd1 2.349(4) . ?
N2 Cd2 2.375(4) . ?
N3 Cd1 2.409(4) 2_646 ?
N4 Cd2 2.349(4) 2_656 ?
N11 Cd1 2.284(4) . ?
N21 Cd2 2.269(4) . ?
Cd1 N11 2.285(4) 3_666 ?
Cd1 N1 2.349(4) 3_666 ?
Cd1 N3 2.409(4) 2_656 ?
Cd1 N3 2.409(4) 4_565 ?
Cd2 N21 2.269(4) 3_656 ?
Cd2 N4 2.349(4) 4_565 ?
Cd2 N4 2.349(4) 2_646 ?
Cd2 N2 2.375(4) 3_656 ?

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
N1 C1 Fe 179.9(4) . . ?
N2 C2 Fe 175.4(4) . . ?
N3 C3 Fe 178.1(4) . . ?
N4 C4 Fe 177.7(4) . . ?
N5 C5 Fe 178.4(4) . . ?
C12 C11 N11 110.3(5) . . ?
C11 C12 N12 106.4(4) . . ?
N11 C13 N12 111.9(4) . . ?
N21 C21 C22 109.9(5) . . ?
N22 C22 C21 107.5(5) . . ?
N21 C23 N22 113.2(4) . . ?
O N Fe 177.6(4) . . ?
C1 N1 Cd1 174.9(4) . . ?
C2 N2 Cd2 152.2(4) . . ?
C3 N3 Cd1 146.1(4) . 2_646 ?
C4 N4 Cd2 168.5(4) . 2_656 ?
C13 N11 C11 104.1(4) . . ?
C13 N11 Cd1 126.7(3) . . ?
C11 N11 Cd1 128.9(3) . . ?
C13 N12 C12 107.3(4) . . ?
C13 N12 C14 127.6(5) . . ?
C12 N12 C14 125.1(4) . . ?
C23 N21 C21 104.1(4) . . ?
C23 N21 Cd2 127.1(3) . . ?
C21 N21 Cd2 128.8(3) . . ?
C23 N22 C22 105.3(4) . . ?
C23 N22 C24 127.4(4) . . ?
C22 N22 C24 127.3(5) . . ?
N Fe C4 94.13(19) . . ?
N Fe C2 93.37(18) . . ?
C4 Fe C2 172.49(18) . . ?
N Fe C1 93.93(18) . . ?
C4 Fe C1 89.89(17) . . ?
C2 Fe C1 90.09(18) . . ?
N Fe C3 95.48(18) . . ?
C4 Fe C3 90.72(17) . . ?
C2 Fe C3 88.08(17) . . ?
C1 Fe C3 170.50(19) . . ?
N Fe C5 178.81(18) . . ?
C4 Fe C5 85.00(18) . . ?
C2 Fe C5 87.51(18) . . ?
C1 Fe C5 85.26(18) . . ?
C3 Fe C5 85.35(18) . . ?
N11 Cd1 N11 180.0 . 3_666 ?
N11 Cd1 N1 89.75(14) . . ?
N11 Cd1 N1 90.25(14) 3_666 . ?
N11 Cd1 N1 90.25(14) . 3_666 ?
N11 Cd1 N1 89.75(14) 3_666 3_666 ?
N1 Cd1 N1 180.0(2) . 3_666 ?
N11 Cd1 N3 95.65(13) . 2_656 ?
N11 Cd1 N3 84.35(13) 3_666 2_656 ?
N1 Cd1 N3 90.00(13) . 2_656 ?
N1 Cd1 N3 90.00(13) 3_666 2_656 ?
N11 Cd1 N3 84.35(13) . 4_565 ?
N11 Cd1 N3 95.65(13) 3_666 4_565 ?
N1 Cd1 N3 90.00(13) . 4_565 ?
N1 Cd1 N3 90.00(13) 3_666 4_565 ?
N3 Cd1 N3 180.00(14) 2_656 4_565 ?
N21 Cd2 N21 180.0 3_656 . ?
N21 Cd2 N4 91.01(14) 3_656 4_565 ?
N21 Cd2 N4 88.99(14) . 4_565 ?
N21 Cd2 N4 88.99(14) 3_656 2_646 ?
N21 Cd2 N4 91.01(14) . 2_646 ?
N4 Cd2 N4 180.0 4_565 2_646 ?
N21 Cd2 N2 89.41(14) 3_656 . ?
N21 Cd2 N2 90.59(14) . . ?
N4 Cd2 N2 85.83(14) 4_565 . ?
N4 Cd2 N2 94.17(14) 2_646 . ?
N21 Cd2 N2 90.59(14) 3_656 3_656 ?
N21 Cd2 N2 89.41(14) . 3_656 ?
N4 Cd2 N2 94.17(14) 4_565 3_656 ?
N4 Cd2 N2 85.83(14) 2_646 3_656 ?
N2 Cd2 N2 180.0 . 3_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C24 H24C N5 0.96 2.69 3.595(7) 157.7 4_565

_refine_diff_density_max         0.722
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.095


_exptl_crystal_recrystallization_method 
'Crystals obtained employing a U-shaped tube by inter-diffusion of a sodium nitroprusside aqueous solution in one arm of the tube with a 1-methylimidazole solution of the metal chloride salt in the other arm.'
