# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_fenb_0008
_database_code_depnum_ccdc_archive 'CCDC 2326495'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0008           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.659 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0008           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        496 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 02:46 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.4750(3)
_cell_length_b                   21.4750(3)
_cell_length_c                   9.4576(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4361.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1297
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.9640
_cell_measurement_theta_min      1.7440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.659
_diffrn_reflns_Laue_measured_fraction_max 0.389
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4490
_diffrn_reflns_point_group_measured_fraction_full 0.659
_diffrn_reflns_point_group_measured_fraction_max 0.389
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.963
_diffrn_reflns_theta_min         1.744
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         370000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.659
_diffrn_measured_fraction_theta_max 0.389
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004027000
_diffrn_orient_matrix_UB_12      0.0081451000
_diffrn_orient_matrix_UB_13      -0.0392035000
_diffrn_orient_matrix_UB_21      -0.0023297000
_diffrn_orient_matrix_UB_22      0.0171607000
_diffrn_orient_matrix_UB_23      0.0182559000
_diffrn_orient_matrix_UB_31      0.0189517000
_diffrn_orient_matrix_UB_32      0.0019424000
_diffrn_orient_matrix_UB_33      0.0030861000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15b'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1824
_reflns_number_total             2053
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+0.8230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0956
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Free rotating group:
 O1(H1,H2)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C5(H4), C8(H8), C7(H9), C3(H6), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.750000 0.625000 0.01371(15) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0181(2) Uani 1 2 d S . P . .
N2 N 0.48320(9) 0.59921(9) 0.5201(3) 0.0229(8) Uani 1 1 d . . . . .
N4 N 0.45248(10) 0.53569(9) 0.7968(4) 0.0262(9) Uani 1 1 d . . . . .
H3 H 0.465602 0.573611 0.777983 0.031 Uiso 1 1 calc R U . . .
N3 N 0.45459(9) 0.48793(8) 0.7028(4) 0.0220(8) Uani 1 1 d . . . . .
N5 N 0.41474(9) 0.48329(8) 0.3870(3) 0.0251(8) Uani 1 1 d . . . . .
N1 N 0.51467(10) 0.83898(10) 0.9189(4) 0.0293(9) Uani 1 1 d . . . . .
N6 N 0.38987(9) 0.52231(9) 0.2909(4) 0.0255(8) Uani 1 1 d . . . . .
H7 H 0.407380 0.557330 0.263441 0.031 Uiso 1 1 calc R U . . .
C2 C 0.48672(9) 0.65055(9) 0.5554(4) 0.0203(8) Uani 1 1 d . . . . .
C6 C 0.37413(11) 0.43609(10) 0.3990(4) 0.0275(10) Uani 1 1 d . . . . .
H10 H 0.379350 0.401067 0.459267 0.033 Uiso 1 1 calc R U . . .
C1 C 0.50952(9) 0.80998(9) 0.8192(4) 0.0206(9) Uani 1 1 d . . . . .
C5 C 0.42837(13) 0.51879(12) 0.9205(5) 0.0315(11) Uani 1 1 d . . . . .
H4 H 0.422639 0.544679 1.000933 0.038 Uiso 1 1 calc R U . . .
C8 C 0.33491(12) 0.50115(12) 0.2420(5) 0.0313(11) Uani 1 1 d . . . . .
H8 H 0.309153 0.520651 0.173340 0.038 Uiso 1 1 calc R U . . .
C7 C 0.32324(11) 0.44584(11) 0.3106(5) 0.0315(11) Uani 1 1 d . . . . .
H9 H 0.287838 0.419742 0.299750 0.038 Uiso 1 1 calc R U . . .
C3 C 0.43043(11) 0.44000(10) 0.7755(4) 0.0265(10) Uani 1 1 d . . . . .
H6 H 0.425734 0.399207 0.738076 0.032 Uiso 1 1 calc R U . . .
C4 C 0.41330(12) 0.45670(11) 0.9099(4) 0.0314(11) Uani 1 1 d . . . . .
H5 H 0.395021 0.431006 0.980364 0.038 Uiso 1 1 calc R U . . .
O1 O 0.44021(9) 0.63380(8) 0.1953(4) 0.0292(8) Uani 1 1 d DG . . . .
H1 H 0.451668 0.644206 0.112572 0.044 Uiso 1 1 d DG U . . .
H2 H 0.442239 0.667313 0.242945 0.044 Uiso 1 1 d DG U . . .


_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
Nb1 C2 2.253(2) 12_767 ?
Nb1 C2 2.253(2) 15_566 ?
Nb1 C2 2.253(2) 6_564 ?
Nb1 C2 2.253(2) . ?
Nb1 C1 2.253(3) . ?
Nb1 C1 2.253(3) 15_566 ?
Nb1 C1 2.253(3) 12_767 ?
Nb1 C1 2.253(3) 6_564 ?
Fe1 N2 2.1693(19) 9_666 ?
Fe1 N2 2.1692(19) . ?
Fe1 N3 2.167(3) 9_666 ?
Fe1 N3 2.167(3) . ?
Fe1 N5 2.150(2) 9_666 ?
Fe1 N5 2.150(2) . ?
N2 C2 1.154(3) . ?
N4 H3 0.8800 . ?
N4 N3 1.358(4) . ?
N4 C5 1.330(5) . ?
N3 C3 1.342(4) . ?
N5 N6 1.347(4) . ?
N5 C6 1.342(3) . ?
N1 C1 1.135(5) . ?
N6 H7 0.8800 . ?
N6 C8 1.347(3) . ?
C6 H10 0.9500 . ?
C6 C7 1.392(4) . ?
C5 H4 0.9500 . ?
C5 C4 1.376(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.376(4) . ?
C7 H9 0.9500 . ?
C3 H6 0.9500 . ?
C3 C4 1.372(5) . ?
C4 H5 0.9500 . ?
O1 H1 0.8499 . ?
O1 H2 0.8503 . ?

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
C2 Nb1 C2 94.90(5) 12_767 6_564 ?
C2 Nb1 C2 94.90(5) 6_564 15_566 ?
C2 Nb1 C2 146.01(19) 12_767 15_566 ?
C2 Nb1 C2 94.90(5) 12_767 . ?
C2 Nb1 C2 94.90(5) 15_566 . ?
C2 Nb1 C2 146.01(19) 6_564 . ?
C1 Nb1 C2 77.02(10) 15_566 6_564 ?
C1 Nb1 C2 142.36(12) . . ?
C1 Nb1 C2 75.41(10) 12_767 6_564 ?
C1 Nb1 C2 142.36(12) 6_564 6_564 ?
C1 Nb1 C2 75.41(10) 15_566 . ?
C1 Nb1 C2 75.41(10) . 12_767 ?
C1 Nb1 C2 71.63(12) . 6_564 ?
C1 Nb1 C2 142.36(12) 12_767 12_767 ?
C1 Nb1 C2 77.02(10) 12_767 . ?
C1 Nb1 C2 71.62(12) 15_566 12_767 ?
C1 Nb1 C2 71.62(12) 6_564 . ?
C1 Nb1 C2 142.36(12) 15_566 15_566 ?
C1 Nb1 C2 77.02(10) 6_564 12_767 ?
C1 Nb1 C2 77.02(10) . 15_566 ?
C1 Nb1 C2 71.62(12) 12_767 15_566 ?
C1 Nb1 C2 75.41(10) 6_564 15_566 ?
C1 Nb1 C1 70.76(15) . 6_564 ?
C1 Nb1 C1 131.67(9) . 15_566 ?
C1 Nb1 C1 131.67(9) . 12_767 ?
C1 Nb1 C1 131.67(9) 12_767 6_564 ?
C1 Nb1 C1 70.76(15) 12_767 15_566 ?
C1 Nb1 C1 131.67(9) 15_566 6_564 ?
N2 Fe1 N2 180.0 . 9_666 ?
N3 Fe1 N2 91.99(9) . 9_666 ?
N3 Fe1 N2 88.01(9) 9_666 9_666 ?
N3 Fe1 N2 91.99(9) 9_666 . ?
N3 Fe1 N2 88.01(9) . . ?
N3 Fe1 N3 180.0 9_666 . ?
N5 Fe1 N2 86.23(8) . 9_666 ?
N5 Fe1 N2 93.77(8) . . ?
N5 Fe1 N2 86.23(8) 9_666 . ?
N5 Fe1 N2 93.77(8) 9_666 9_666 ?
N5 Fe1 N3 92.10(10) 9_666 9_666 ?
N5 Fe1 N3 87.90(10) 9_666 . ?
N5 Fe1 N3 92.10(10) . . ?
N5 Fe1 N3 87.90(10) . 9_666 ?
N5 Fe1 N5 180.0 9_666 . ?
C2 N2 Fe1 162.2(2) . . ?
N3 N4 H3 123.7 . . ?
C5 N4 H3 123.7 . . ?
C5 N4 N3 112.5(2) . . ?
N4 N3 Fe1 120.28(17) . . ?
C3 N3 Fe1 136.0(2) . . ?
C3 N3 N4 103.3(3) . . ?
N6 N5 Fe1 124.70(14) . . ?
C6 N5 Fe1 129.6(2) . . ?
C6 N5 N6 105.6(2) . . ?
N5 N6 H7 124.2 . . ?
C8 N6 N5 111.7(2) . . ?
C8 N6 H7 124.2 . . ?
N2 C2 Nb1 176.48(17) . . ?
N5 C6 H10 124.9 . . ?
N5 C6 C7 110.2(3) . . ?
C7 C6 H10 124.9 . . ?
N1 C1 Nb1 178.4(3) . . ?
N4 C5 H4 126.5 . . ?
N4 C5 C4 107.0(3) . . ?
C4 C5 H4 126.5 . . ?
N6 C8 H8 126.6 . . ?
N6 C8 C7 106.8(3) . . ?
C7 C8 H8 126.6 . . ?
C6 C7 H9 127.2 . . ?
C8 C7 C6 105.7(2) . . ?
C8 C7 H9 127.2 . . ?
N3 C3 H6 123.9 . . ?
N3 C3 C4 112.2(2) . . ?
C4 C3 H6 123.9 . . ?
C5 C4 H5 127.5 . . ?
C3 C4 C5 104.9(3) . . ?
C3 C4 H5 127.5 . . ?
H1 O1 H2 104.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 172.7(2) . . . . ?
Fe1 N5 N6 C8 -177.2(2) . . . . ?
Fe1 N5 C6 C7 176.5(2) . . . . ?
N4 N3 C3 C4 0.4(3) . . . . ?
N4 C5 C4 C3 0.3(4) . . . . ?
N3 N4 C5 C4 -0.1(4) . . . . ?
N3 C3 C4 C5 -0.4(4) . . . . ?
N5 N6 C8 C7 0.5(4) . . . . ?
N5 C6 C7 C8 0.7(4) . . . . ?
N6 N5 C6 C7 -0.4(4) . . . . ?
N6 C8 C7 C6 -0.7(4) . . . . ?
C6 N5 N6 C8 0.0(4) . . . . ?
C5 N4 N3 Fe1 -173.9(2) . . . . ?
C5 N4 N3 C3 -0.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   238
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.718
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0014
_database_code_depnum_ccdc_archive 'CCDC 2326501'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0014           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.660 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0014           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        496 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 03:58 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.4722(3)
_cell_length_b                   21.4722(3)
_cell_length_c                   9.4522(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4358.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1317
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.8630
_cell_measurement_theta_min      1.7420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.660
_diffrn_reflns_Laue_measured_fraction_max 0.386
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4513
_diffrn_reflns_point_group_measured_fraction_full 0.660
_diffrn_reflns_point_group_measured_fraction_max 0.386
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.966
_diffrn_reflns_theta_min         1.744
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         280000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.660
_diffrn_measured_fraction_theta_max 0.386
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003879000
_diffrn_orient_matrix_UB_12      -0.0080441000
_diffrn_orient_matrix_UB_13      -0.0393195000
_diffrn_orient_matrix_UB_21      0.0023288000
_diffrn_orient_matrix_UB_22      -0.0172071000
_diffrn_orient_matrix_UB_23      0.0180495000
_diffrn_orient_matrix_UB_31      -0.0189611000
_diffrn_orient_matrix_UB_32      -0.0019560000
_diffrn_orient_matrix_UB_33      0.0030361000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1767
_reflns_number_total             2039
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2039
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0386P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0930
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C5(H4), C8(H8), C7(H9), C3(H6), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.750000 0.625000 0.01272(17) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0148(2) Uani 1 2 d S . P . .
O1 O 0.44020(8) 0.63426(8) 0.1952(4) 0.0203(8) Uani 1 1 d D . . . .
N2 N 0.48329(9) 0.59903(9) 0.5200(4) 0.0183(8) Uani 1 1 d . . . . .
N4 N 0.45276(9) 0.53567(9) 0.7973(4) 0.0189(9) Uani 1 1 d . . . . .
H3 H 0.466019 0.573539 0.778347 0.023 Uiso 1 1 calc R U . . .
N5 N 0.41472(8) 0.48314(8) 0.3865(3) 0.0193(9) Uani 1 1 d . . . . .
N3 N 0.45470(9) 0.48789(8) 0.7035(4) 0.0184(8) Uani 1 1 d . . . . .
N1 N 0.51429(9) 0.83938(9) 0.9198(4) 0.0212(9) Uani 1 1 d . . . . .
N6 N 0.38989(9) 0.52256(9) 0.2908(4) 0.0184(9) Uani 1 1 d . . . . .
H7 H 0.407460 0.557529 0.263210 0.022 Uiso 1 1 calc R U . . .
C2 C 0.48685(10) 0.65037(10) 0.5552(4) 0.0167(9) Uani 1 1 d . . . . .
C6 C 0.37410(11) 0.43611(10) 0.3979(4) 0.0201(10) Uani 1 1 d . . . . .
H10 H 0.379573 0.400962 0.457675 0.024 Uiso 1 1 calc R U . . .
C5 C 0.42846(11) 0.51878(11) 0.9214(4) 0.0205(10) Uani 1 1 d . . . . .
H4 H 0.422602 0.544647 1.001861 0.025 Uiso 1 1 calc R U . . .
C8 C 0.33455(10) 0.50137(11) 0.2430(4) 0.0216(11) Uani 1 1 d . . . . .
H8 H 0.308528 0.521199 0.175303 0.026 Uiso 1 1 calc R U . . .
C1 C 0.50943(10) 0.80972(10) 0.8196(4) 0.0168(10) Uani 1 1 d . . . . .
C7 C 0.32277(11) 0.44556(11) 0.3105(4) 0.0219(10) Uani 1 1 d . . . . .
H9 H 0.287420 0.419383 0.299631 0.026 Uiso 1 1 calc R U . . .
C3 C 0.43064(10) 0.43976(11) 0.7752(4) 0.0199(10) Uani 1 1 d . . . . .
H6 H 0.425929 0.399019 0.737552 0.024 Uiso 1 1 calc R U . . .
C4 C 0.41355(11) 0.45665(11) 0.9104(4) 0.0240(11) Uani 1 1 d . . . . .
H5 H 0.395364 0.430894 0.980916 0.029 Uiso 1 1 calc R U . . .
H1 H 0.4540(13) 0.6413(13) 0.103(2) 0.020(9) Uiso 1 1 d D . . . .
H2 H 0.4404(18) 0.6660(15) 0.254(4) 0.067(14) Uiso 1 1 d 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
Nb1 C2 2.256(2) . ?
Nb1 C2 2.257(2) 15_566 ?
Nb1 C2 2.257(2) 6_564 ?
Nb1 C2 2.257(2) 12_767 ?
Nb1 C1 2.252(4) . ?
Nb1 C1 2.252(4) 6_564 ?
Nb1 C1 2.252(4) 12_767 ?
Nb1 C1 2.252(4) 15_566 ?
Fe1 N2 2.1647(19) . ?
Fe1 N2 2.1647(19) 9_666 ?
Fe1 N5 2.153(2) . ?
Fe1 N5 2.153(2) 9_666 ?
Fe1 N3 2.171(3) . ?
Fe1 N3 2.171(3) 9_666 ?
O1 H1 0.932(18) . ?
O1 H2 0.880(18) . ?
N2 C2 1.154(3) . ?
N4 H3 0.8800 . ?
N4 N3 1.356(4) . ?
N4 C5 1.335(5) . ?
N5 N6 1.348(4) . ?
N5 C6 1.339(3) . ?
N3 C3 1.340(4) . ?
N1 C1 1.146(5) . ?
N6 H7 0.8800 . ?
N6 C8 1.350(3) . ?
C6 H10 0.9500 . ?
C6 C7 1.393(4) . ?
C5 H4 0.9500 . ?
C5 C4 1.376(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.381(4) . ?
C7 H9 0.9500 . ?
C3 H6 0.9500 . ?
C3 C4 1.378(5) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 94.90(6) . 12_767 ?
C2 Nb1 C2 94.90(6) 6_564 15_566 ?
C2 Nb1 C2 146.0(2) 12_767 15_566 ?
C2 Nb1 C2 146.0(2) . 6_564 ?
C2 Nb1 C2 94.91(6) . 15_566 ?
C2 Nb1 C2 94.90(6) 12_767 6_564 ?
C1 Nb1 C2 142.19(12) . . ?
C1 Nb1 C2 71.80(12) . 6_564 ?
C1 Nb1 C2 77.00(10) . 15_566 ?
C1 Nb1 C2 77.00(10) 12_767 . ?
C1 Nb1 C2 77.00(10) 15_566 6_564 ?
C1 Nb1 C2 75.36(10) 15_566 . ?
C1 Nb1 C2 75.36(10) 6_564 15_566 ?
C1 Nb1 C2 71.80(12) 6_564 . ?
C1 Nb1 C2 75.36(10) 12_767 6_564 ?
C1 Nb1 C2 75.36(10) . 12_767 ?
C1 Nb1 C2 142.20(12) 6_564 6_564 ?
C1 Nb1 C2 142.20(13) 12_767 12_767 ?
C1 Nb1 C2 71.80(13) 12_767 15_566 ?
C1 Nb1 C2 71.80(13) 15_566 12_767 ?
C1 Nb1 C2 77.00(10) 6_564 12_767 ?
C1 Nb1 C2 142.20(13) 15_566 15_566 ?
C1 Nb1 C1 131.88(10) . 15_566 ?
C1 Nb1 C1 131.88(10) . 12_767 ?
C1 Nb1 C1 131.88(10) 12_767 6_564 ?
C1 Nb1 C1 131.88(10) 15_566 6_564 ?
C1 Nb1 C1 70.42(15) 12_767 15_566 ?
C1 Nb1 C1 70.42(15) . 6_564 ?
N2 Fe1 N2 180.00(10) 9_666 . ?
N2 Fe1 N3 88.06(10) . . ?
N2 Fe1 N3 91.94(10) . 9_666 ?
N2 Fe1 N3 91.94(10) 9_666 . ?
N2 Fe1 N3 88.06(10) 9_666 9_666 ?
N5 Fe1 N2 86.12(8) 9_666 . ?
N5 Fe1 N2 93.88(8) 9_666 9_666 ?
N5 Fe1 N2 86.12(8) . 9_666 ?
N5 Fe1 N2 93.88(8) . . ?
N5 Fe1 N5 180.0 . 9_666 ?
N5 Fe1 N3 87.69(10) 9_666 . ?
N5 Fe1 N3 92.31(10) . . ?
N5 Fe1 N3 92.31(10) 9_666 9_666 ?
N5 Fe1 N3 87.69(10) . 9_666 ?
N3 Fe1 N3 180.0 . 9_666 ?
H1 O1 H2 118(3) . . ?
C2 N2 Fe1 162.3(2) . . ?
N3 N4 H3 123.8 . . ?
C5 N4 H3 123.8 . . ?
C5 N4 N3 112.4(2) . . ?
N6 N5 Fe1 124.39(14) . . ?
C6 N5 Fe1 129.9(2) . . ?
C6 N5 N6 105.7(2) . . ?
N4 N3 Fe1 120.14(17) . . ?
C3 N3 Fe1 135.5(2) . . ?
C3 N3 N4 103.9(3) . . ?
N5 N6 H7 124.4 . . ?
N5 N6 C8 111.2(2) . . ?
C8 N6 H7 124.4 . . ?
N2 C2 Nb1 176.59(18) . . ?
N5 C6 H10 124.5 . . ?
N5 C6 C7 111.0(3) . . ?
C7 C6 H10 124.5 . . ?
N4 C5 H4 126.6 . . ?
N4 C5 C4 106.7(3) . . ?
C4 C5 H4 126.6 . . ?
N6 C8 H8 126.3 . . ?
N6 C8 C7 107.4(3) . . ?
C7 C8 H8 126.3 . . ?
N1 C1 Nb1 179.0(3) . . ?
C6 C7 H9 127.6 . . ?
C8 C7 C6 104.8(2) . . ?
C8 C7 H9 127.6 . . ?
N3 C3 H6 124.2 . . ?
N3 C3 C4 111.7(2) . . ?
C4 C3 H6 124.2 . . ?
C5 C4 C3 105.3(3) . . ?
C5 C4 H5 127.4 . . ?
C3 C4 H5 127.4 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N5 N6 C8 -176.5(2) . . . . ?
Fe1 N5 C6 C7 176.0(2) . . . . ?
Fe1 N3 C3 C4 172.8(2) . . . . ?
N4 N3 C3 C4 0.4(3) . . . . ?
N4 C5 C4 C3 0.1(3) . . . . ?
N5 N6 C8 C7 0.0(4) . . . . ?
N5 C6 C7 C8 0.6(4) . . . . ?
N3 N4 C5 C4 0.1(3) . . . . ?
N3 C3 C4 C5 -0.3(3) . . . . ?
N6 N5 C6 C7 -0.6(4) . . . . ?
N6 C8 C7 C6 -0.3(4) . . . . ?
C6 N5 N6 C8 0.4(4) . . . . ?
C5 N4 N3 Fe1 -174.19(18) . . . . ?
C5 N4 N3 C3 -0.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   274
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.847
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0012
_database_code_depnum_ccdc_archive 'CCDC 2326497'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0012           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.656 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0012           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        503 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 03:53 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.4595(4)
_cell_length_b                   21.4595(4)
_cell_length_c                   9.4491(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4351.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1355
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.9730
_cell_measurement_theta_min      2.0570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.656
_diffrn_reflns_Laue_measured_fraction_max 0.384
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4496
_diffrn_reflns_point_group_measured_fraction_full 0.656
_diffrn_reflns_point_group_measured_fraction_max 0.384
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.978
_diffrn_reflns_theta_min         1.745
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         280000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.656
_diffrn_measured_fraction_theta_max 0.384
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003951000
_diffrn_orient_matrix_UB_12      -0.0080469000
_diffrn_orient_matrix_UB_13      -0.0393474000
_diffrn_orient_matrix_UB_21      0.0023251000
_diffrn_orient_matrix_UB_22      -0.0172162000
_diffrn_orient_matrix_UB_23      0.0180476000
_diffrn_orient_matrix_UB_31      -0.0189701000
_diffrn_orient_matrix_UB_32      -0.0019543000
_diffrn_orient_matrix_UB_33      0.0030428000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1789
_reflns_number_total             2028
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2028
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0370
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0443P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1001
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C8(H8), C5(H4), C7(H9), C3(H6), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.750000 0.625000 0.01262(17) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0146(2) Uani 1 2 d S . P . .
N2 N 0.48322(9) 0.59897(9) 0.5205(3) 0.0187(8) Uani 1 1 d . . . . .
O1 O 0.44018(8) 0.63406(8) 0.1964(4) 0.0225(8) Uani 1 1 d D . . . .
N4 N 0.45271(9) 0.53545(9) 0.7973(4) 0.0207(9) Uani 1 1 d . . . . .
H3 H 0.465908 0.573378 0.778445 0.025 Uiso 1 1 calc R U . . .
N3 N 0.45469(8) 0.48784(8) 0.7029(4) 0.0167(8) Uani 1 1 d . . . . .
N5 N 0.41482(9) 0.48313(8) 0.3866(3) 0.0201(8) Uani 1 1 d . . . . .
N1 N 0.51458(10) 0.83900(9) 0.9201(4) 0.0221(9) Uani 1 1 d . . . . .
N6 N 0.38981(9) 0.52243(9) 0.2915(4) 0.0190(8) Uani 1 1 d . . . . .
H7 H 0.407300 0.557472 0.263904 0.023 Uiso 1 1 calc R U . . .
C2 C 0.48679(10) 0.65036(10) 0.5549(4) 0.0176(9) Uani 1 1 d . . . . .
C6 C 0.37432(11) 0.43620(10) 0.3988(4) 0.0210(9) Uani 1 1 d . . . . .
H10 H 0.379753 0.401175 0.459081 0.025 Uiso 1 1 calc R U . . .
C8 C 0.33456(11) 0.50130(11) 0.2439(4) 0.0230(10) Uani 1 1 d . . . . .
H8 H 0.308453 0.521194 0.176501 0.028 Uiso 1 1 calc R U . . .
C1 C 0.50955(10) 0.81001(10) 0.8190(4) 0.0174(9) Uani 1 1 d . . . . .
C5 C 0.42875(12) 0.51868(11) 0.9208(5) 0.0240(10) Uani 1 1 d . . . . .
H4 H 0.423190 0.544667 1.001178 0.029 Uiso 1 1 calc R U . . .
C7 C 0.32290(11) 0.44564(11) 0.3109(4) 0.0240(10) Uani 1 1 d . . . . .
H9 H 0.287600 0.419370 0.299825 0.029 Uiso 1 1 calc R U . . .
C3 C 0.43069(11) 0.43974(10) 0.7750(4) 0.0216(10) Uani 1 1 d . . . . .
H6 H 0.426109 0.398964 0.737259 0.026 Uiso 1 1 calc R U . . .
C4 C 0.41338(11) 0.45636(11) 0.9107(4) 0.0230(10) Uani 1 1 d . . . . .
H5 H 0.395031 0.430688 0.981239 0.028 Uiso 1 1 calc R U . . .
H2 H 0.4401(17) 0.6689(13) 0.248(4) 0.059(13) Uiso 1 1 d D . . . .
H1 H 0.4549(14) 0.6407(14) 0.105(2) 0.024(9) Uiso 1 1 d 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
Nb1 C2 2.256(2) 12_767 ?
Nb1 C2 2.256(2) . ?
Nb1 C2 2.256(2) 6_564 ?
Nb1 C2 2.256(2) 15_566 ?
Nb1 C1 2.250(4) 12_767 ?
Nb1 C1 2.250(4) . ?
Nb1 C1 2.250(4) 15_566 ?
Nb1 C1 2.250(4) 6_564 ?
Fe1 N2 2.1628(19) . ?
Fe1 N2 2.1628(19) 9_666 ?
Fe1 N3 2.166(3) 9_666 ?
Fe1 N3 2.166(3) . ?
Fe1 N5 2.149(2) . ?
Fe1 N5 2.149(2) 9_666 ?
N2 C2 1.152(3) . ?
O1 H2 0.893(18) . ?
O1 H1 0.934(18) . ?
N4 H3 0.8800 . ?
N4 N3 1.356(4) . ?
N4 C5 1.325(5) . ?
N3 C3 1.340(3) . ?
N5 N6 1.344(4) . ?
N5 C6 1.335(3) . ?
N1 C1 1.145(5) . ?
N6 H7 0.8800 . ?
N6 C8 1.347(3) . ?
C6 H10 0.9500 . ?
C6 C7 1.396(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.375(4) . ?
C5 H4 0.9500 . ?
C5 C4 1.381(3) . ?
C7 H9 0.9500 . ?
C3 H6 0.9500 . ?
C3 C4 1.382(5) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 94.94(6) 12_767 6_564 ?
C2 Nb1 C2 94.94(6) 15_566 . ?
C2 Nb1 C2 145.87(19) 6_564 . ?
C2 Nb1 C2 145.87(19) 12_767 15_566 ?
C2 Nb1 C2 94.94(6) 12_767 . ?
C2 Nb1 C2 94.94(6) 6_564 15_566 ?
C1 Nb1 C2 142.47(12) 12_767 12_767 ?
C1 Nb1 C2 71.65(13) 12_767 15_566 ?
C1 Nb1 C2 77.01(10) 12_767 . ?
C1 Nb1 C2 71.65(13) 15_566 12_767 ?
C1 Nb1 C2 75.31(10) 6_564 15_566 ?
C1 Nb1 C2 77.01(10) 6_564 12_767 ?
C1 Nb1 C2 142.47(12) . . ?
C1 Nb1 C2 75.31(10) . 12_767 ?
C1 Nb1 C2 142.47(12) 15_566 15_566 ?
C1 Nb1 C2 75.31(10) 12_767 6_564 ?
C1 Nb1 C2 77.01(10) . 15_566 ?
C1 Nb1 C2 77.01(10) 15_566 6_564 ?
C1 Nb1 C2 75.31(10) 15_566 . ?
C1 Nb1 C2 142.47(12) 6_564 6_564 ?
C1 Nb1 C2 71.65(12) . 6_564 ?
C1 Nb1 C2 71.65(12) 6_564 . ?
C1 Nb1 C1 131.61(10) 12_767 6_564 ?
C1 Nb1 C1 131.61(10) 15_566 . ?
C1 Nb1 C1 131.61(10) 12_767 . ?
C1 Nb1 C1 70.84(15) 6_564 . ?
C1 Nb1 C1 131.61(10) 15_566 6_564 ?
C1 Nb1 C1 70.84(15) 12_767 15_566 ?
N2 Fe1 N2 180.0 9_666 . ?
N2 Fe1 N3 87.95(9) . . ?
N2 Fe1 N3 92.05(9) . 9_666 ?
N2 Fe1 N3 92.05(9) 9_666 . ?
N2 Fe1 N3 87.95(9) 9_666 9_666 ?
N3 Fe1 N3 180.0 . 9_666 ?
N5 Fe1 N2 86.08(8) . 9_666 ?
N5 Fe1 N2 93.92(8) . . ?
N5 Fe1 N2 93.92(8) 9_666 9_666 ?
N5 Fe1 N2 86.08(8) 9_666 . ?
N5 Fe1 N3 92.24(10) . . ?
N5 Fe1 N3 92.24(10) 9_666 9_666 ?
N5 Fe1 N3 87.76(10) 9_666 . ?
N5 Fe1 N3 87.76(10) . 9_666 ?
N5 Fe1 N5 180.0 . 9_666 ?
C2 N2 Fe1 162.5(2) . . ?
H2 O1 H1 112(3) . . ?
N3 N4 H3 123.6 . . ?
C5 N4 H3 123.6 . . ?
C5 N4 N3 112.7(2) . . ?
N4 N3 Fe1 120.34(17) . . ?
C3 N3 Fe1 135.7(2) . . ?
C3 N3 N4 103.5(3) . . ?
N6 N5 Fe1 124.55(14) . . ?
C6 N5 Fe1 129.6(2) . . ?
C6 N5 N6 105.7(2) . . ?
N5 N6 H7 124.3 . . ?
N5 N6 C8 111.3(2) . . ?
C8 N6 H7 124.3 . . ?
N2 C2 Nb1 176.50(18) . . ?
N5 C6 H10 124.6 . . ?
N5 C6 C7 110.7(3) . . ?
C7 C6 H10 124.6 . . ?
N6 C8 H8 126.3 . . ?
N6 C8 C7 107.4(3) . . ?
C7 C8 H8 126.3 . . ?
N1 C1 Nb1 178.0(3) . . ?
N4 C5 H4 126.4 . . ?
N4 C5 C4 107.2(3) . . ?
C4 C5 H4 126.4 . . ?
C6 C7 H9 127.6 . . ?
C8 C7 C6 104.8(2) . . ?
C8 C7 H9 127.6 . . ?
N3 C3 H6 124.0 . . ?
N3 C3 C4 112.1(2) . . ?
C4 C3 H6 124.0 . . ?
C5 C4 C3 104.5(3) . . ?
C5 C4 H5 127.8 . . ?
C3 C4 H5 127.8 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 172.71(19) . . . . ?
Fe1 N5 N6 C8 -176.3(2) . . . . ?
Fe1 N5 C6 C7 176.0(2) . . . . ?
N4 N3 C3 C4 0.6(3) . . . . ?
N4 C5 C4 C3 0.4(3) . . . . ?
N3 N4 C5 C4 -0.1(3) . . . . ?
N3 C3 C4 C5 -0.6(3) . . . . ?
N5 N6 C8 C7 0.0(4) . . . . ?
N5 C6 C7 C8 0.1(4) . . . . ?
N6 N5 C6 C7 -0.1(4) . . . . ?
N6 C8 C7 C6 -0.1(4) . . . . ?
C6 N5 N6 C8 0.1(4) . . . . ?
C5 N4 N3 Fe1 -173.92(19) . . . . ?
C5 N4 N3 C3 -0.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   265
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.747
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0009
_database_code_depnum_ccdc_archive 'CCDC 2326507'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0009           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.660 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0009           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        495 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 03:37 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C14 N8 O4 Fe2 Nb1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.4180(3)
_cell_length_b                   21.4180(3)
_cell_length_c                   9.4229(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4322.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1390
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      20.0230
_cell_measurement_theta_min      1.7470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.660
_diffrn_reflns_Laue_measured_fraction_max 0.384
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4459
_diffrn_reflns_point_group_measured_fraction_full 0.660
_diffrn_reflns_point_group_measured_fraction_max 0.384
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.019
_diffrn_reflns_theta_min         1.749
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         510000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.660
_diffrn_measured_fraction_theta_max 0.384
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004042000
_diffrn_orient_matrix_UB_12      -0.0081915000
_diffrn_orient_matrix_UB_13      -0.0393114000
_diffrn_orient_matrix_UB_21      0.0023395000
_diffrn_orient_matrix_UB_22      -0.0171927000
_diffrn_orient_matrix_UB_23      0.0183898000
_diffrn_orient_matrix_UB_31      -0.0190051000
_diffrn_orient_matrix_UB_32      -0.0019508000
_diffrn_orient_matrix_UB_33      0.0031087000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1811
_reflns_number_total             2028
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2028
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+0.6937P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0917
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C8(H8), C3(H6), C7(H9), C5(H4), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.750000 0.625000 0.01531(15) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.01988(19) Uani 1 2 d S . P . .
O1 O 0.44034(8) 0.63364(8) 0.1966(4) 0.0301(8) Uani 1 1 d D . . . .
N2 N 0.48253(9) 0.59891(9) 0.5197(3) 0.0255(8) Uani 1 1 d . . . . .
N4 N 0.45246(10) 0.53536(9) 0.7980(4) 0.0291(9) Uani 1 1 d . . . . .
H3 H 0.465874 0.573316 0.779293 0.035 Uiso 1 1 calc R U . . .
N3 N 0.45457(8) 0.48785(8) 0.7041(3) 0.0243(8) Uani 1 1 d . . . . .
N5 N 0.41488(9) 0.48259(8) 0.3870(3) 0.0246(8) Uani 1 1 d . . . . .
N6 N 0.38960(9) 0.52179(9) 0.2911(4) 0.0270(8) Uani 1 1 d . . . . .
H7 H 0.406981 0.556895 0.262927 0.032 Uiso 1 1 calc R U . . .
N1 N 0.51519(10) 0.83898(9) 0.9204(4) 0.0308(9) Uani 1 1 d . . . . .
C2 C 0.48617(9) 0.65038(9) 0.5545(4) 0.0207(8) Uani 1 1 d . . . . .
C6 C 0.37428(11) 0.43549(10) 0.3989(4) 0.0278(9) Uani 1 1 d . . . . .
H10 H 0.380076 0.400222 0.458573 0.033 Uiso 1 1 calc R U . . .
C1 C 0.50962(9) 0.80993(9) 0.8194(4) 0.0195(8) Uani 1 1 d . . . . .
C8 C 0.33412(11) 0.50022(11) 0.2437(5) 0.0323(11) Uani 1 1 d . . . . .
H8 H 0.307960 0.519741 0.175431 0.039 Uiso 1 1 calc R U . . .
C3 C 0.43018(11) 0.43975(10) 0.7759(4) 0.0279(9) Uani 1 1 d . . . . .
H6 H 0.425424 0.398911 0.738086 0.034 Uiso 1 1 calc R U . . .
C7 C 0.32247(11) 0.44478(11) 0.3125(4) 0.0327(11) Uani 1 1 d . . . . .
H9 H 0.286889 0.418628 0.303104 0.039 Uiso 1 1 calc R U . . .
C5 C 0.42795(13) 0.51859(12) 0.9216(5) 0.0351(11) Uani 1 1 d . . . . .
H4 H 0.422033 0.544656 1.002077 0.042 Uiso 1 1 calc R U . . .
C4 C 0.41282(12) 0.45674(11) 0.9113(5) 0.0360(11) Uani 1 1 d . . . . .
H5 H 0.394381 0.431077 0.982068 0.043 Uiso 1 1 calc R U . . .
H1 H 0.4532(14) 0.6409(13) 0.104(2) 0.028(8) Uiso 1 1 d D . . . .
H2 H 0.437(2) 0.6664(17) 0.255(5) 0.11(2) Uiso 1 1 d 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
Nb1 C2 2.254(2) 12_767 ?
Nb1 C2 2.254(2) . ?
Nb1 C2 2.254(2) 6_564 ?
Nb1 C2 2.254(2) 15_566 ?
Nb1 C1 2.246(3) . ?
Nb1 C1 2.246(3) 6_564 ?
Nb1 C1 2.246(3) 12_767 ?
Nb1 C1 2.246(3) 15_566 ?
Fe1 N2 2.1594(18) . ?
Fe1 N2 2.1593(18) 9_666 ?
Fe1 N3 2.171(3) 9_666 ?
Fe1 N3 2.171(3) . ?
Fe1 N5 2.144(2) . ?
Fe1 N5 2.144(2) 9_666 ?
O1 H1 0.929(18) . ?
O1 H2 0.896(19) . ?
N2 C2 1.153(3) . ?
N4 H3 0.8800 . ?
N4 N3 1.349(4) . ?
N4 C5 1.327(5) . ?
N3 C3 1.338(3) . ?
N5 N6 1.347(4) . ?
N5 C6 1.337(3) . ?
N6 H7 0.8800 . ?
N6 C8 1.351(3) . ?
N1 C1 1.144(5) . ?
C6 H10 0.9500 . ?
C6 C7 1.390(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.376(4) . ?
C3 H6 0.9500 . ?
C3 C4 1.378(5) . ?
C7 H9 0.9500 . ?
C5 H4 0.9500 . ?
C5 C4 1.367(3) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 94.98(5) 12_767 6_564 ?
C2 Nb1 C2 94.98(5) 15_566 . ?
C2 Nb1 C2 145.73(18) 6_564 . ?
C2 Nb1 C2 145.73(18) 12_767 15_566 ?
C2 Nb1 C2 94.98(5) 12_767 . ?
C2 Nb1 C2 94.98(5) 6_564 15_566 ?
C1 Nb1 C2 75.40(9) . 12_767 ?
C1 Nb1 C2 76.79(9) . 15_566 ?
C1 Nb1 C2 142.48(11) . . ?
C1 Nb1 C2 142.48(12) 12_767 12_767 ?
C1 Nb1 C2 142.48(12) 15_566 15_566 ?
C1 Nb1 C2 71.78(12) 15_566 12_767 ?
C1 Nb1 C2 71.78(12) 6_564 . ?
C1 Nb1 C2 76.79(9) 6_564 12_767 ?
C1 Nb1 C2 71.78(12) 12_767 15_566 ?
C1 Nb1 C2 71.78(12) . 6_564 ?
C1 Nb1 C2 75.40(9) 6_564 15_566 ?
C1 Nb1 C2 75.40(9) 12_767 6_564 ?
C1 Nb1 C2 76.79(9) 12_767 . ?
C1 Nb1 C2 76.79(9) 15_566 6_564 ?
C1 Nb1 C2 142.48(11) 6_564 6_564 ?
C1 Nb1 C2 75.40(9) 15_566 . ?
C1 Nb1 C1 131.69(9) . 15_566 ?
C1 Nb1 C1 131.69(9) 12_767 6_564 ?
C1 Nb1 C1 70.72(14) . 6_564 ?
C1 Nb1 C1 131.69(9) 15_566 6_564 ?
C1 Nb1 C1 70.72(14) 12_767 15_566 ?
C1 Nb1 C1 131.69(9) . 12_767 ?
N2 Fe1 N2 180.0 9_666 . ?
N2 Fe1 N3 87.92(9) . . ?
N2 Fe1 N3 92.09(9) . 9_666 ?
N2 Fe1 N3 92.08(9) 9_666 . ?
N2 Fe1 N3 87.91(9) 9_666 9_666 ?
N3 Fe1 N3 180.0 . 9_666 ?
N5 Fe1 N2 86.21(8) . 9_666 ?
N5 Fe1 N2 93.79(8) . . ?
N5 Fe1 N2 93.79(8) 9_666 9_666 ?
N5 Fe1 N2 86.21(8) 9_666 . ?
N5 Fe1 N3 92.18(10) . . ?
N5 Fe1 N3 92.18(10) 9_666 9_666 ?
N5 Fe1 N3 87.82(10) 9_666 . ?
N5 Fe1 N3 87.82(10) . 9_666 ?
N5 Fe1 N5 180.0 . 9_666 ?
H1 O1 H2 118(3) . . ?
C2 N2 Fe1 162.0(2) . . ?
N3 N4 H3 123.7 . . ?
C5 N4 H3 123.7 . . ?
C5 N4 N3 112.6(2) . . ?
N4 N3 Fe1 120.36(17) . . ?
C3 N3 Fe1 135.6(2) . . ?
C3 N3 N4 103.7(3) . . ?
N6 N5 Fe1 124.51(14) . . ?
C6 N5 Fe1 130.0(2) . . ?
C6 N5 N6 105.4(2) . . ?
N5 N6 H7 124.4 . . ?
N5 N6 C8 111.2(2) . . ?
C8 N6 H7 124.4 . . ?
N2 C2 Nb1 176.26(17) . . ?
N5 C6 H10 124.4 . . ?
N5 C6 C7 111.2(3) . . ?
C7 C6 H10 124.4 . . ?
N1 C1 Nb1 178.0(3) . . ?
N6 C8 H8 126.3 . . ?
N6 C8 C7 107.4(3) . . ?
C7 C8 H8 126.3 . . ?
N3 C3 H6 124.1 . . ?
N3 C3 C4 111.7(2) . . ?
C4 C3 H6 124.1 . . ?
C6 C7 H9 127.6 . . ?
C8 C7 C6 104.8(2) . . ?
C8 C7 H9 127.6 . . ?
N4 C5 H4 126.5 . . ?
N4 C5 C4 107.1(3) . . ?
C4 C5 H4 126.5 . . ?
C3 C4 H5 127.5 . . ?
C5 C4 C3 104.9(3) . . ?
C5 C4 H5 127.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 173.2(2) . . . . ?
Fe1 N5 N6 C8 -176.3(2) . . . . ?
Fe1 N5 C6 C7 175.4(2) . . . . ?
N4 N3 C3 C4 0.4(3) . . . . ?
N4 C5 C4 C3 0.1(4) . . . . ?
N3 N4 C5 C4 0.1(4) . . . . ?
N3 C3 C4 C5 -0.3(4) . . . . ?
N5 N6 C8 C7 0.5(4) . . . . ?
N5 C6 C7 C8 1.2(4) . . . . ?
N6 N5 C6 C7 -1.0(4) . . . . ?
N6 C8 C7 C6 -1.0(4) . . . . ?
C6 N5 N6 C8 0.3(4) . . . . ?
C5 N4 N3 Fe1 -174.5(2) . . . . ?
C5 N4 N3 C3 -0.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   252
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.778
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0043
_database_code_depnum_ccdc_archive 'CCDC 2326694'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0043           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.486 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0043           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        547 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 06:23 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         Fe2NbC10N10OH10
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.6050(4)
_cell_length_b                   21.6050(4)
_cell_length_c                   9.5533(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4459.3(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    563
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.7630
_cell_measurement_theta_min      2.3120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.486
_diffrn_reflns_Laue_measured_fraction_max 0.267
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2238
_diffrn_reflns_point_group_measured_fraction_full 0.486
_diffrn_reflns_point_group_measured_fraction_max 0.267
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.155
_diffrn_reflns_theta_min         2.043
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         80000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.486
_diffrn_measured_fraction_theta_max 0.267
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.50  32.00   0.50    0.20    --    0.00   0.00   0.00   63
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0001607000
_diffrn_orient_matrix_UB_12      -0.0048350000
_diffrn_orient_matrix_UB_13      0.0415074000
_diffrn_orient_matrix_UB_21      -0.0062213000
_diffrn_orient_matrix_UB_22      -0.0173579000
_diffrn_orient_matrix_UB_23      -0.0101984000
_diffrn_orient_matrix_UB_31      0.0179292000
_diffrn_orient_matrix_UB_32      -0.0059776000
_diffrn_orient_matrix_UB_33      -0.0039328000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1228
_reflns_number_total             1481
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1481
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0401
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0960
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H2
 0.95 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C6(H10), C5(H4), C7(H9), C3(H6), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0142(4) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0191(5) Uani 1 2 d S . P . .
O1 O 0.43995(14) 0.36514(13) 0.8108(8) 0.0330(19) Uani 1 1 d D . . . .
N4 N 0.45290(15) 0.46438(13) 0.2042(7) 0.026(2) Uani 1 1 d . . . . .
H3 H 0.465888 0.426624 0.222459 0.032 Uiso 1 1 calc R U . . .
N3 N 0.45517(13) 0.51144(12) 0.2982(6) 0.020(2) Uani 1 1 d . . . . .
N2 N 0.48464(13) 0.40061(12) 0.4784(6) 0.025(2) Uani 1 1 d . . . . .
N5 N 0.41486(12) 0.51503(12) 0.6125(6) 0.025(2) Uani 1 1 d . . . . .
N6 N 0.39111(13) 0.47614(13) 0.7098(7) 0.029(2) Uani 1 1 d . . . . .
H7 H 0.408909 0.441462 0.736593 0.035 Uiso 1 1 calc R U . . .
N1 N 0.51391(15) 0.16118(14) 0.0844(7) 0.035(2) Uani 1 1 d . . . . .
C2 C 0.48809(14) 0.34936(15) 0.4452(8) 0.023(2) Uani 1 1 d . . . . .
C8 C 0.33702(17) 0.49707(18) 0.7604(8) 0.034(3) Uani 1 1 d . . . . .
H8 H 0.312128 0.477755 0.829814 0.041 Uiso 1 1 calc R U . . .
C6 C 0.37447(15) 0.56154(15) 0.6034(8) 0.028(3) Uani 1 1 d . . . . .
H10 H 0.379339 0.596469 0.544043 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4294(2) 0.48094(17) 0.0840(9) 0.033(3) Uani 1 1 d . . . . .
H4 H 0.423605 0.454990 0.004867 0.040 Uiso 1 1 calc R U . . .
C7 C 0.32447(17) 0.55232(17) 0.6920(8) 0.029(3) Uani 1 1 d . . . . .
H9 H 0.289266 0.578189 0.703305 0.035 Uiso 1 1 calc R U . . .
C1 C 0.50896(13) 0.19052(15) 0.1831(8) 0.022(2) Uani 1 1 d . . . . .
C3 C 0.43151(17) 0.55953(16) 0.2263(8) 0.026(3) Uani 1 1 d . . . . .
H6 H 0.427033 0.600056 0.263487 0.032 Uiso 1 1 calc R U . . .
C4 C 0.41461(19) 0.54305(17) 0.0927(9) 0.033(3) Uani 1 1 d . . . . .
H5 H 0.396794 0.568533 0.022428 0.039 Uiso 1 1 calc R U . . .
H1 H 0.454(2) 0.348(3) 0.894(3) 0.06(2) Uiso 1 1 d D . . . .
H2 H 0.439(2) 0.342(2) 0.732(3) 0.035(15) Uiso 1 1 d 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
Nb1 C2 2.264(4) 16_656 ?
Nb1 C2 2.264(4) . ?
Nb1 C2 2.264(4) 11_666 ?
Nb1 C2 2.264(4) 6_554 ?
Nb1 C1 2.247(6) . ?
Nb1 C1 2.247(6) 6_554 ?
Nb1 C1 2.247(6) 16_656 ?
Nb1 C1 2.247(6) 11_666 ?
Fe1 N3 2.172(5) . ?
Fe1 N3 2.172(5) 9_666 ?
Fe1 N2 2.183(3) . ?
Fe1 N2 2.183(3) 9_666 ?
Fe1 N5 2.155(4) 9_666 ?
Fe1 N5 2.155(4) . ?
O1 H1 0.923(19) . ?
O1 H2 0.905(19) . ?
N4 H3 0.8800 . ?
N4 N3 1.357(6) . ?
N4 C5 1.305(10) . ?
N3 C3 1.346(6) . ?
N2 C2 1.154(5) . ?
N5 N6 1.354(7) . ?
N5 C6 1.334(4) . ?
N6 H7 0.8800 . ?
N6 C8 1.343(5) . ?
N1 C1 1.141(9) . ?
C8 H8 0.9500 . ?
C8 C7 1.388(8) . ?
C6 H10 0.9500 . ?
C6 C7 1.386(8) . ?
C5 H4 0.9500 . ?
C5 C4 1.382(5) . ?
C7 H9 0.9500 . ?
C3 H6 0.9500 . ?
C3 C4 1.374(10) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 145.5(3) 16_656 11_666 ?
C2 Nb1 C2 145.5(3) 6_554 . ?
C2 Nb1 C2 95.03(10) 11_666 . ?
C2 Nb1 C2 95.03(10) 16_656 6_554 ?
C2 Nb1 C2 95.03(10) 16_656 . ?
C2 Nb1 C2 95.04(10) 11_666 6_554 ?
C1 Nb1 C2 77.00(16) . 16_656 ?
C1 Nb1 C2 71.9(2) . 6_554 ?
C1 Nb1 C2 142.5(2) . . ?
C1 Nb1 C2 142.5(2) 16_656 16_656 ?
C1 Nb1 C2 75.03(17) 11_666 6_554 ?
C1 Nb1 C2 71.9(2) 11_666 16_656 ?
C1 Nb1 C2 71.9(2) 6_554 . ?
C1 Nb1 C2 75.03(17) 6_554 16_656 ?
C1 Nb1 C2 76.99(16) 16_656 6_554 ?
C1 Nb1 C2 75.03(17) . 11_666 ?
C1 Nb1 C2 142.5(2) 6_554 6_554 ?
C1 Nb1 C2 71.9(2) 16_656 11_666 ?
C1 Nb1 C2 75.03(17) 16_656 . ?
C1 Nb1 C2 142.5(2) 11_666 11_666 ?
C1 Nb1 C2 76.99(16) 6_554 11_666 ?
C1 Nb1 C2 76.99(16) 11_666 . ?
C1 Nb1 C1 131.72(16) . 11_666 ?
C1 Nb1 C1 131.72(16) 16_656 6_554 ?
C1 Nb1 C1 70.7(3) . 6_554 ?
C1 Nb1 C1 131.72(16) 11_666 6_554 ?
C1 Nb1 C1 70.7(3) 16_656 11_666 ?
C1 Nb1 C1 131.72(16) . 16_656 ?
N3 Fe1 N3 180.0 9_666 . ?
N3 Fe1 N2 92.28(16) . 9_666 ?
N3 Fe1 N2 87.72(16) . . ?
N3 Fe1 N2 87.72(16) 9_666 9_666 ?
N3 Fe1 N2 92.28(16) 9_666 . ?
N2 Fe1 N2 180.0 9_666 . ?
N5 Fe1 N3 87.42(16) . 9_666 ?
N5 Fe1 N3 92.58(16) . . ?
N5 Fe1 N3 92.58(16) 9_666 9_666 ?
N5 Fe1 N3 87.42(16) 9_666 . ?
N5 Fe1 N2 86.23(12) . 9_666 ?
N5 Fe1 N2 86.23(12) 9_666 . ?
N5 Fe1 N2 93.77(12) 9_666 9_666 ?
N5 Fe1 N2 93.77(12) . . ?
N5 Fe1 N5 180.0 . 9_666 ?
H1 O1 H2 120(4) . . ?
N3 N4 H3 123.5 . . ?
C5 N4 H3 123.5 . . ?
C5 N4 N3 113.0(3) . . ?
N4 N3 Fe1 121.2(3) . . ?
C3 N3 Fe1 135.2(4) . . ?
C3 N3 N4 103.1(5) . . ?
C2 N2 Fe1 163.7(4) . . ?
N6 N5 Fe1 124.9(2) . . ?
C6 N5 Fe1 129.8(4) . . ?
C6 N5 N6 105.3(4) . . ?
N5 N6 H7 124.2 . . ?
C8 N6 N5 111.6(4) . . ?
C8 N6 H7 124.2 . . ?
N2 C2 Nb1 176.9(3) . . ?
N6 C8 H8 126.6 . . ?
N6 C8 C7 106.9(5) . . ?
C7 C8 H8 126.6 . . ?
N5 C6 H10 124.4 . . ?
N5 C6 C7 111.2(5) . . ?
C7 C6 H10 124.4 . . ?
N4 C5 H4 126.2 . . ?
N4 C5 C4 107.7(6) . . ?
C4 C5 H4 126.2 . . ?
C8 C7 H9 127.5 . . ?
C6 C7 C8 105.0(4) . . ?
C6 C7 H9 127.5 . . ?
N1 C1 Nb1 178.8(5) . . ?
N3 C3 H6 124.0 . . ?
N3 C3 C4 112.0(4) . . ?
C4 C3 H6 124.0 . . ?
C5 C4 H5 127.9 . . ?
C3 C4 C5 104.2(6) . . ?
C3 C4 H5 127.9 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 172.6(4) . . . . ?
Fe1 N5 N6 C8 -178.9(4) . . . . ?
Fe1 N5 C6 C7 178.2(4) . . . . ?
N4 N3 C3 C4 0.5(5) . . . . ?
N4 C5 C4 C3 0.0(6) . . . . ?
N3 N4 C5 C4 0.4(6) . . . . ?
N3 C3 C4 C5 -0.3(6) . . . . ?
N5 N6 C8 C7 0.4(7) . . . . ?
N5 C6 C7 C8 1.4(7) . . . . ?
N6 N5 C6 C7 -1.2(6) . . . . ?
N6 C8 C7 C6 -1.1(7) . . . . ?
C6 N5 N6 C8 0.4(6) . . . . ?
C5 N4 N3 Fe1 -174.0(4) . . . . ?
C5 N4 N3 C3 -0.5(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   155
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.825
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0019
_database_code_depnum_ccdc_archive 'CCDC 2326523'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0019           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.649 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0019           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        386 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 05:13 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.0746(7)
_cell_length_b                   21.0746(7)
_cell_length_c                   9.3334(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4145.3(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    879
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.4970
_cell_measurement_theta_min      2.2320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.649
_diffrn_reflns_Laue_measured_fraction_max 0.358
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4011
_diffrn_reflns_point_group_measured_fraction_full 0.649
_diffrn_reflns_point_group_measured_fraction_max 0.358
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.194
_diffrn_reflns_theta_min         1.772
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         870000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.649
_diffrn_measured_fraction_theta_max 0.358
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003993000
_diffrn_orient_matrix_UB_12      0.0079583000
_diffrn_orient_matrix_UB_13      0.0400065000
_diffrn_orient_matrix_UB_21      0.0023228000
_diffrn_orient_matrix_UB_22      0.0176745000
_diffrn_orient_matrix_UB_23      -0.0177861000
_diffrn_orient_matrix_UB_31      -0.0193174000
_diffrn_orient_matrix_UB_32      0.0019433000
_diffrn_orient_matrix_UB_33      -0.0029601000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1289
_reflns_number_total             1857
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1857
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0984
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C3(H6), C7(H9), C6(H10), C5(H4), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0306(3) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0307(3) Uani 1 2 d S . P . .
O1 O 0.44233(12) 0.36591(12) 0.7993(5) 0.0394(11) Uani 1 1 d D . . . .
N3 N 0.45540(12) 0.51329(12) 0.3004(5) 0.0348(13) Uani 1 1 d . . . . .
N2 N 0.48210(13) 0.40350(13) 0.4813(5) 0.0379(13) Uani 1 1 d . . . . .
N4 N 0.45365(14) 0.46532(13) 0.2038(5) 0.0384(14) Uani 1 1 d . . . . .
H3 H 0.467879 0.426835 0.221365 0.046 Uiso 1 1 calc R U . . .
N1 N 0.51569(13) 0.15997(14) 0.0770(6) 0.0395(15) Uani 1 1 d . . . . .
N5 N 0.41564(13) 0.51827(13) 0.6085(5) 0.0374(14) Uani 1 1 d . . . . .
N6 N 0.39007(13) 0.47890(14) 0.7057(5) 0.0438(15) Uani 1 1 d . . . . .
H7 H 0.407804 0.443291 0.734323 0.053 Uiso 1 1 calc R U . . .
C2 C 0.48539(15) 0.35120(17) 0.4466(6) 0.0368(16) Uani 1 1 d . . . . .
C8 C 0.33386(18) 0.50067(17) 0.7540(7) 0.0467(19) Uani 1 1 d . . . . .
H8 H 0.307446 0.481146 0.823669 0.056 Uiso 1 1 calc R U . . .
C3 C 0.42955(16) 0.56190(16) 0.2296(7) 0.0396(17) Uani 1 1 d . . . . .
H6 H 0.424061 0.603087 0.269039 0.048 Uiso 1 1 calc R U . . .
C1 C 0.51072(15) 0.18963(17) 0.1796(6) 0.0336(16) Uani 1 1 d . . . . .
C7 C 0.32205(18) 0.55707(17) 0.6823(6) 0.0443(19) Uani 1 1 d . . . . .
H9 H 0.285707 0.583493 0.690364 0.053 Uiso 1 1 calc R U . . .
C6 C 0.37449(16) 0.56643(15) 0.5968(6) 0.0387(16) Uani 1 1 d . . . . .
H10 H 0.380683 0.602417 0.537085 0.046 Uiso 1 1 calc R U . . .
C5 C 0.42812(18) 0.48271(17) 0.0797(7) 0.0435(19) Uani 1 1 d . . . . .
H4 H 0.422288 0.456729 -0.002415 0.052 Uiso 1 1 calc R U . . .
C4 C 0.41183(16) 0.54533(16) 0.0931(6) 0.0436(19) Uani 1 1 d . . . . .
H5 H 0.392438 0.571642 0.022964 0.052 Uiso 1 1 calc R U . . .
H1 H 0.459(2) 0.359(2) 0.892(3) 0.060(16) Uiso 1 1 d D . . . .
H2 H 0.421(4) 0.329(2) 0.772(9) 0.31(6) Uiso 1 1 d 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
Nb1 C2 2.256(4) 16_656 ?
Nb1 C2 2.256(4) 6_554 ?
Nb1 C2 2.256(4) 11_666 ?
Nb1 C2 2.256(4) . ?
Nb1 C1 2.235(5) . ?
Nb1 C1 2.235(5) 6_554 ?
Nb1 C1 2.235(5) 16_656 ?
Nb1 C1 2.235(5) 11_666 ?
Fe1 N3 2.105(4) 9_666 ?
Fe1 N3 2.105(4) . ?
Fe1 N2 2.076(3) 9_666 ?
Fe1 N2 2.076(3) . ?
Fe1 N5 2.082(3) . ?
Fe1 N5 2.082(3) 9_666 ?
O1 H1 0.949(19) . ?
O1 H2 0.93(2) . ?
N3 N4 1.355(5) . ?
N3 C3 1.335(5) . ?
N2 C2 1.151(5) . ?
N4 H3 0.8800 . ?
N4 C5 1.329(7) . ?
N1 C1 1.148(7) . ?
N5 N6 1.342(5) . ?
N5 C6 1.339(4) . ?
N6 H7 0.8800 . ?
N6 C8 1.348(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.386(6) . ?
C3 H6 0.9500 . ?
C3 C4 1.373(8) . ?
C7 H9 0.9500 . ?
C7 C6 1.378(6) . ?
C6 H10 0.9500 . ?
C5 H4 0.9500 . ?
C5 C4 1.369(5) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 145.5(3) 16_656 11_666 ?
C2 Nb1 C2 95.04(8) 11_666 6_554 ?
C2 Nb1 C2 95.04(8) 16_656 6_554 ?
C2 Nb1 C2 95.04(8) 16_656 . ?
C2 Nb1 C2 145.5(3) 6_554 . ?
C2 Nb1 C2 95.04(8) 11_666 . ?
C1 Nb1 C2 142.52(19) 11_666 11_666 ?
C1 Nb1 C2 142.52(18) . . ?
C1 Nb1 C2 71.94(18) 16_656 11_666 ?
C1 Nb1 C2 77.06(15) 6_554 11_666 ?
C1 Nb1 C2 77.06(15) 11_666 . ?
C1 Nb1 C2 77.06(15) . 16_656 ?
C1 Nb1 C2 74.95(15) . 11_666 ?
C1 Nb1 C2 142.52(19) 16_656 16_656 ?
C1 Nb1 C2 74.95(15) 16_656 . ?
C1 Nb1 C2 71.94(18) 11_666 16_656 ?
C1 Nb1 C2 71.94(18) 6_554 . ?
C1 Nb1 C2 142.52(18) 6_554 6_554 ?
C1 Nb1 C2 74.95(15) 6_554 16_656 ?
C1 Nb1 C2 77.06(15) 16_656 6_554 ?
C1 Nb1 C2 74.95(15) 11_666 6_554 ?
C1 Nb1 C2 71.94(18) . 6_554 ?
C1 Nb1 C1 70.6(2) . 6_554 ?
C1 Nb1 C1 131.74(14) . 11_666 ?
C1 Nb1 C1 70.6(2) 16_656 11_666 ?
C1 Nb1 C1 131.74(14) 16_656 6_554 ?
C1 Nb1 C1 131.74(14) 11_666 6_554 ?
C1 Nb1 C1 131.74(14) . 16_656 ?
N3 Fe1 N3 180.0 9_666 . ?
N2 Fe1 N3 88.56(15) . . ?
N2 Fe1 N3 88.56(15) 9_666 9_666 ?
N2 Fe1 N3 91.44(15) . 9_666 ?
N2 Fe1 N3 91.44(15) 9_666 . ?
N2 Fe1 N2 180.00(15) 9_666 . ?
N2 Fe1 N5 86.16(12) . 9_666 ?
N2 Fe1 N5 93.84(12) . . ?
N2 Fe1 N5 93.84(12) 9_666 9_666 ?
N2 Fe1 N5 86.16(12) 9_666 . ?
N5 Fe1 N3 91.42(14) . . ?
N5 Fe1 N3 91.41(14) 9_666 9_666 ?
N5 Fe1 N3 88.59(14) . 9_666 ?
N5 Fe1 N3 88.58(14) 9_666 . ?
N5 Fe1 N5 180.0 9_666 . ?
H1 O1 H2 108(4) . . ?
N4 N3 Fe1 120.1(3) . . ?
C3 N3 Fe1 136.2(3) . . ?
C3 N3 N4 103.4(4) . . ?
C2 N2 Fe1 162.0(3) . . ?
N3 N4 H3 123.7 . . ?
C5 N4 N3 112.6(3) . . ?
C5 N4 H3 123.7 . . ?
N6 N5 Fe1 123.9(2) . . ?
C6 N5 Fe1 130.8(3) . . ?
C6 N5 N6 105.3(3) . . ?
N5 N6 H7 124.2 . . ?
N5 N6 C8 111.6(3) . . ?
C8 N6 H7 124.2 . . ?
N2 C2 Nb1 175.5(3) . . ?
N6 C8 H8 126.6 . . ?
N6 C8 C7 106.8(4) . . ?
C7 C8 H8 126.6 . . ?
N3 C3 H6 124.0 . . ?
N3 C3 C4 112.0(4) . . ?
C4 C3 H6 124.0 . . ?
N1 C1 Nb1 178.2(4) . . ?
C8 C7 H9 127.5 . . ?
C6 C7 C8 105.0(3) . . ?
C6 C7 H9 127.5 . . ?
N5 C6 C7 111.3(4) . . ?
N5 C6 H10 124.3 . . ?
C7 C6 H10 124.3 . . ?
N4 C5 H4 126.6 . . ?
N4 C5 C4 106.7(5) . . ?
C4 C5 H4 126.6 . . ?
C3 C4 H5 127.4 . . ?
C5 C4 C3 105.2(4) . . ?
C5 C4 H5 127.4 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -175.3(3) . . . . ?
Fe1 N3 C3 C4 174.2(3) . . . . ?
Fe1 N5 N6 C8 -176.8(3) . . . . ?
Fe1 N5 C6 C7 175.3(3) . . . . ?
N3 N4 C5 C4 0.0(5) . . . . ?
N3 C3 C4 C5 -0.2(5) . . . . ?
N4 N3 C3 C4 0.2(4) . . . . ?
N4 C5 C4 C3 0.1(5) . . . . ?
N5 N6 C8 C7 0.8(6) . . . . ?
N6 N5 C6 C7 -1.9(6) . . . . ?
N6 C8 C7 C6 -1.9(5) . . . . ?
C8 C7 C6 N5 2.3(6) . . . . ?
C3 N3 N4 C5 -0.1(4) . . . . ?
C6 N5 N6 C8 0.6(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   413
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.689
_oxdiff_exptl_absorpt_empirical_full_min 0.722
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0018
_database_code_depnum_ccdc_archive 'CCDC 2326519'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0018           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.641 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0018           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        514 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 05:08 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   20.9186(13)
_cell_length_b                   20.9186(13)
_cell_length_c                   9.372(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4101.0(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    670
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.5460
_cell_measurement_theta_min      1.7740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.641
_diffrn_reflns_Laue_measured_fraction_max 0.346
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3764
_diffrn_reflns_point_group_measured_fraction_full 0.641
_diffrn_reflns_point_group_measured_fraction_max 0.346
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.274
_diffrn_reflns_theta_min         1.775
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         870000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.641
_diffrn_measured_fraction_theta_max 0.346
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0080720000
_diffrn_orient_matrix_UB_12      -0.0003622000
_diffrn_orient_matrix_UB_13      -0.0397790000
_diffrn_orient_matrix_UB_21      0.0177807000
_diffrn_orient_matrix_UB_22      0.0023023000
_diffrn_orient_matrix_UB_23      0.0178341000
_diffrn_orient_matrix_UB_31      0.0019427000
_diffrn_orient_matrix_UB_32      -0.0194792000
_diffrn_orient_matrix_UB_33      0.0028993000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1130
_reflns_number_total             1796
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1796
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      0.940
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1131
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C5(H4), C8(H8), C6(H10), C7(H9), C3(H6), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.750000 0.625000 0.0340(4) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0326(4) Uani 1 2 d S . P . .
O1 O 0.44440(15) 0.63494(15) 0.2011(6) 0.0379(14) Uani 1 1 d D . . . .
N4 N 0.45587(17) 0.53407(16) 0.7929(7) 0.0384(17) Uani 1 1 d . . . . .
H3 H 0.471466 0.572496 0.777121 0.046 Uiso 1 1 calc R U . . .
N3 N 0.45668(15) 0.48648(16) 0.6944(6) 0.0377(17) Uani 1 1 d . . . . .
N2 N 0.48313(15) 0.59484(17) 0.5189(6) 0.0381(16) Uani 1 1 d . . . . .
N5 N 0.41670(15) 0.48251(15) 0.3942(6) 0.0360(17) Uani 1 1 d . . . . .
N1 N 0.51520(16) 0.84078(18) 0.9237(7) 0.0377(18) Uani 1 1 d . . . . .
N6 N 0.39197(16) 0.52205(16) 0.2938(6) 0.0372(17) Uani 1 1 d . . . . .
H7 H 0.410273 0.557631 0.264766 0.045 Uiso 1 1 calc R U . . .
C5 C 0.4291(2) 0.5167(2) 0.9155(8) 0.041(2) Uani 1 1 d . . . . .
H4 H 0.423423 0.542710 0.997599 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3359(2) 0.4999(2) 0.2442(8) 0.041(2) Uani 1 1 d . . . . .
H8 H 0.309749 0.519499 0.173779 0.049 Uiso 1 1 calc R U . . .
C6 C 0.37488(19) 0.43443(19) 0.4047(7) 0.036(2) Uani 1 1 d . . . . .
H10 H 0.379988 0.398681 0.466152 0.043 Uiso 1 1 calc R U . . .
C2 C 0.48585(18) 0.6483(2) 0.5522(8) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.3233(2) 0.44327(19) 0.3149(8) 0.042(2) Uani 1 1 d . . . . .
H9 H 0.287088 0.416317 0.304003 0.050 Uiso 1 1 calc R U . . .
C3 C 0.4292(2) 0.4375(2) 0.7663(8) 0.040(2) Uani 1 1 d . . . . .
H6 H 0.423196 0.396069 0.726991 0.049 Uiso 1 1 calc R U . . .
C4 C 0.41135(19) 0.45393(19) 0.9004(8) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.390871 0.427616 0.969216 0.051 Uiso 1 1 calc R U . . .
C1 C 0.51057(19) 0.8108(2) 0.8228(8) 0.038(2) Uani 1 1 d . . . . .
H2 H 0.442(3) 0.670(2) 0.259(6) 0.11(3) Uiso 1 1 d D . . . .
H1 H 0.460(2) 0.642(2) 0.109(3) 0.06(2) Uiso 1 1 d 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
Nb1 C2 2.254(5) 12_767 ?
Nb1 C2 2.254(5) 15_566 ?
Nb1 C2 2.254(5) 6_564 ?
Nb1 C2 2.254(5) . ?
Nb1 C1 2.259(7) 12_767 ?
Nb1 C1 2.259(7) . ?
Nb1 C1 2.259(7) 6_564 ?
Nb1 C1 2.259(7) 15_566 ?
Fe1 N3 2.054(6) 9_666 ?
Fe1 N3 2.054(6) . ?
Fe1 N2 2.023(4) 9_666 ?
Fe1 N2 2.023(4) . ?
Fe1 N5 2.038(4) 9_666 ?
Fe1 N5 2.038(4) . ?
O1 H2 0.909(19) . ?
O1 H1 0.933(19) . ?
N4 H3 0.8800 . ?
N4 N3 1.358(7) . ?
N4 C5 1.328(8) . ?
N3 C3 1.354(6) . ?
N2 C2 1.163(6) . ?
N5 N6 1.356(6) . ?
N5 C6 1.337(5) . ?
N1 C1 1.138(8) . ?
N6 H7 0.8800 . ?
N6 C8 1.344(6) . ?
C5 H4 0.9500 . ?
C5 C4 1.372(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.382(7) . ?
C6 H10 0.9500 . ?
C6 C7 1.381(7) . ?
C7 H9 0.9500 . ?
C3 H6 0.9500 . ?
C3 C4 1.356(9) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 95.26(10) 12_767 6_564 ?
C2 Nb1 C2 144.8(3) 6_564 . ?
C2 Nb1 C2 95.25(10) 12_767 . ?
C2 Nb1 C2 144.8(3) 12_767 15_566 ?
C2 Nb1 C2 95.26(10) 6_564 15_566 ?
C2 Nb1 C2 95.26(10) 15_566 . ?
C2 Nb1 C1 142.5(2) 15_566 15_566 ?
C2 Nb1 C1 142.5(2) . . ?
C2 Nb1 C1 72.8(2) 6_564 . ?
C2 Nb1 C1 142.5(2) 6_564 6_564 ?
C2 Nb1 C1 76.71(18) 6_564 15_566 ?
C2 Nb1 C1 72.8(2) . 6_564 ?
C2 Nb1 C1 74.53(18) . 15_566 ?
C2 Nb1 C1 142.5(2) 12_767 12_767 ?
C2 Nb1 C1 74.53(18) 15_566 6_564 ?
C2 Nb1 C1 74.53(18) 6_564 12_767 ?
C2 Nb1 C1 74.53(18) 12_767 . ?
C2 Nb1 C1 72.8(2) 15_566 12_767 ?
C2 Nb1 C1 76.71(18) 15_566 . ?
C2 Nb1 C1 76.71(18) . 12_767 ?
C2 Nb1 C1 72.8(2) 12_767 15_566 ?
C2 Nb1 C1 76.71(18) 12_767 6_564 ?
C1 Nb1 C1 69.7(3) 12_767 15_566 ?
C1 Nb1 C1 69.7(3) 6_564 . ?
C1 Nb1 C1 132.31(19) 12_767 . ?
C1 Nb1 C1 132.31(19) 12_767 6_564 ?
C1 Nb1 C1 132.31(19) 15_566 6_564 ?
C1 Nb1 C1 132.31(19) 15_566 . ?
N3 Fe1 N3 180.00(15) . 9_666 ?
N2 Fe1 N3 88.88(18) 9_666 9_666 ?
N2 Fe1 N3 88.88(18) . . ?
N2 Fe1 N3 91.12(18) 9_666 . ?
N2 Fe1 N3 91.12(18) . 9_666 ?
N2 Fe1 N2 180.00(4) . 9_666 ?
N2 Fe1 N5 93.99(14) 9_666 9_666 ?
N2 Fe1 N5 86.01(14) 9_666 . ?
N2 Fe1 N5 86.01(14) . 9_666 ?
N2 Fe1 N5 93.99(14) . . ?
N5 Fe1 N3 88.31(18) . 9_666 ?
N5 Fe1 N3 88.31(18) 9_666 . ?
N5 Fe1 N3 91.69(18) . . ?
N5 Fe1 N3 91.69(18) 9_666 9_666 ?
N5 Fe1 N5 180.0 9_666 . ?
H2 O1 H1 116(4) . . ?
N3 N4 H3 123.4 . . ?
C5 N4 H3 123.4 . . ?
C5 N4 N3 113.1(4) . . ?
N4 N3 Fe1 120.5(3) . . ?
C3 N3 Fe1 137.1(4) . . ?
C3 N3 N4 102.2(5) . . ?
C2 N2 Fe1 163.4(4) . . ?
N6 N5 Fe1 123.7(3) . . ?
C6 N5 Fe1 131.2(4) . . ?
C6 N5 N6 105.1(4) . . ?
N5 N6 H7 124.4 . . ?
C8 N6 N5 111.3(4) . . ?
C8 N6 H7 124.4 . . ?
N4 C5 H4 126.7 . . ?
N4 C5 C4 106.7(6) . . ?
C4 C5 H4 126.7 . . ?
N6 C8 H8 126.4 . . ?
N6 C8 C7 107.2(5) . . ?
C7 C8 H8 126.4 . . ?
N5 C6 H10 124.3 . . ?
N5 C6 C7 111.5(5) . . ?
C7 C6 H10 124.3 . . ?
N2 C2 Nb1 174.8(4) . . ?
C8 C7 H9 127.5 . . ?
C6 C7 C8 105.0(4) . . ?
C6 C7 H9 127.5 . . ?
N3 C3 H6 123.6 . . ?
N3 C3 C4 112.7(5) . . ?
C4 C3 H6 123.6 . . ?
C5 C4 H5 127.4 . . ?
C3 C4 C5 105.3(5) . . ?
C3 C4 H5 127.4 . . ?
N1 C1 Nb1 178.8(5) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 175.5(4) . . . . ?
Fe1 N5 N6 C8 -178.3(4) . . . . ?
Fe1 N5 C6 C7 177.8(4) . . . . ?
N4 N3 C3 C4 1.1(5) . . . . ?
N4 C5 C4 C3 0.1(6) . . . . ?
N3 N4 C5 C4 0.6(6) . . . . ?
N3 C3 C4 C5 -0.8(6) . . . . ?
N5 N6 C8 C7 -0.2(7) . . . . ?
N5 C6 C7 C8 1.1(7) . . . . ?
N6 N5 C6 C7 -1.2(7) . . . . ?
N6 C8 C7 C6 -0.6(6) . . . . ?
C5 N4 N3 Fe1 -176.6(3) . . . . ?
C5 N4 N3 C3 -1.0(5) . . . . ?
C6 N5 N6 C8 0.9(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   497
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.453
_oxdiff_exptl_absorpt_empirical_full_min 0.610
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0022
_database_code_depnum_ccdc_archive 'CCDC 2327391'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;

# start Validation Reply Form
_vrf_PLAT029_fenb_0022           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.632 Why?  
RESPONSE: The generated Alerts A, B and C are the typical high-pressure crystallography warnings. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0022           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        531 Report
RESPONSE: The generated Alerts A, B and C are the typical high-pressure crystallography warnings. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# end Validation Reply Form

_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20N14O4Fe2Nb1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   20.9206(17)
_cell_length_b                   20.9206(17)
_cell_length_c                   9.371(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4101.3(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    802
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.5660
_cell_measurement_theta_min      1.7710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.1702
_diffrn_reflns_Laue_measured_fraction_full 0.632
_diffrn_reflns_Laue_measured_fraction_max 0.386
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3847
_diffrn_reflns_point_group_measured_fraction_full 0.632
_diffrn_reflns_point_group_measured_fraction_max 0.386
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.760
_diffrn_reflns_theta_min         1.775
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         870000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.632
_diffrn_measured_fraction_theta_max 0.386
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0080508000
_diffrn_orient_matrix_UB_12      -0.0004089000
_diffrn_orient_matrix_UB_13      0.0399210000
_diffrn_orient_matrix_UB_21      -0.0177653000
_diffrn_orient_matrix_UB_22      0.0026971000
_diffrn_orient_matrix_UB_23      -0.0176338000
_diffrn_orient_matrix_UB_31      -0.0022977000
_diffrn_orient_matrix_UB_32      -0.0193741000
_diffrn_orient_matrix_UB_33      -0.0032052000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1111
_reflns_number_total             1864
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0640
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.2054
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H2
 0.95 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3.a Free rotating group:
 O1(H1,H2)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C5(H4), C3(H6), C4(H5), C6(H10), C7(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0355(4) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0355(5) Uani 1 2 d S . P . .
N3 N 0.4562(2) 0.5135(2) 0.3042(8) 0.0405(18) Uani 1 1 d . . . . .
N4 N 0.4548(2) 0.4653(2) 0.2072(8) 0.047(2) Uani 1 1 d . . . . .
H3 H 0.469561 0.426571 0.223654 0.057 Uiso 1 1 calc R U . . .
N2 N 0.4830(2) 0.4049(2) 0.4810(8) 0.0419(18) Uani 1 1 d . . . . .
N5 N 0.4163(2) 0.5174(2) 0.6049(7) 0.0417(19) Uani 1 1 d . . . . .
N1 N 0.5160(2) 0.1599(2) 0.0768(9) 0.045(2) Uani 1 1 d . . . . .
N6 N 0.3921(2) 0.4775(2) 0.7045(9) 0.048(2) Uani 1 1 d . . . . .
H7 H 0.410287 0.441729 0.732588 0.057 Uiso 1 1 calc R U . . .
C1 C 0.5110(2) 0.1889(3) 0.1792(10) 0.039(2) Uani 1 1 d . . . . .
C2 C 0.4855(2) 0.3515(3) 0.4454(10) 0.042(2) Uani 1 1 d . . . . .
C8 C 0.3356(3) 0.5003(3) 0.7554(10) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.309742 0.480951 0.826521 0.057 Uiso 1 1 calc R U . . .
C5 C 0.4283(3) 0.4833(3) 0.0842(10) 0.048(3) Uani 1 1 d . . . . .
H4 H 0.421981 0.457503 0.001983 0.058 Uiso 1 1 calc R U . . .
C3 C 0.4299(3) 0.5622(3) 0.2334(10) 0.048(3) Uani 1 1 d . . . . .
H6 H 0.424395 0.603719 0.272775 0.057 Uiso 1 1 calc R U . . .
C4 C 0.4121(3) 0.5461(3) 0.0993(10) 0.052(3) Uani 1 1 d . . . . .
H5 H 0.392352 0.572840 0.030202 0.063 Uiso 1 1 calc R U . . .
C6 C 0.3747(3) 0.5658(3) 0.5951(10) 0.049(3) Uani 1 1 d . . . . .
H10 H 0.380074 0.601787 0.534427 0.059 Uiso 1 1 calc R U . . .
C7 C 0.3228(3) 0.5567(3) 0.6850(10) 0.053(3) Uani 1 1 d . . . . .
H9 H 0.286405 0.583426 0.695562 0.064 Uiso 1 1 calc R U . . .
O1 O 0.44365(19) 0.36531(18) 0.8006(7) 0.0471(17) Uani 1 1 d DG . . . .
H1 H 0.464934 0.355456 0.874666 0.071 Uiso 1 1 d DG U . . .
H2 H 0.433777 0.329595 0.763326 0.071 Uiso 1 1 d DG U . . .


_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
Nb1 C1 2.248(8) 16_656 ?
Nb1 C1 2.248(8) 11_666 ?
Nb1 C1 2.248(8) 6_554 ?
Nb1 C1 2.249(8) . ?
Nb1 C2 2.245(6) . ?
Nb1 C2 2.245(6) 6_554 ?
Nb1 C2 2.245(6) 16_656 ?
Nb1 C2 2.245(6) 11_666 ?
Fe1 N3 2.069(7) . ?
Fe1 N3 2.069(7) 9_666 ?
Fe1 N2 2.028(5) 9_666 ?
Fe1 N2 2.028(5) . ?
Fe1 N5 2.041(5) . ?
Fe1 N5 2.041(5) 9_666 ?
N3 N4 1.358(9) . ?
N3 C3 1.336(8) . ?
N4 H3 0.8800 . ?
N4 C5 1.334(11) . ?
N2 C2 1.167(8) . ?
N5 N6 1.351(8) . ?
N5 C6 1.338(7) . ?
N1 C1 1.140(11) . ?
N6 H7 0.8800 . ?
N6 C8 1.360(8) . ?
C8 H8 0.9500 . ?
C8 C7 1.377(9) . ?
C5 H4 0.9500 . ?
C5 C4 1.363(8) . ?
C3 H6 0.9500 . ?
C3 C4 1.354(12) . ?
C4 H5 0.9500 . ?
C6 H10 0.9500 . ?
C6 C7 1.388(10) . ?
C7 H9 0.9500 . ?
O1 H1 0.8501 . ?
O1 H2 0.8502 . ?

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
C1 Nb1 C1 131.7(2) 16_656 6_554 ?
C1 Nb1 C1 131.7(2) 6_554 11_666 ?
C1 Nb1 C1 70.6(4) 16_656 11_666 ?
C1 Nb1 C1 131.7(2) 16_656 . ?
C1 Nb1 C1 131.7(2) 11_666 . ?
C1 Nb1 C1 70.6(4) 6_554 . ?
C2 Nb1 C1 77.3(2) 11_666 6_554 ?
C2 Nb1 C1 142.4(3) . . ?
C2 Nb1 C1 74.9(2) 16_656 6_554 ?
C2 Nb1 C1 142.4(3) 6_554 6_554 ?
C2 Nb1 C1 74.9(2) 11_666 . ?
C2 Nb1 C1 74.9(2) . 16_656 ?
C2 Nb1 C1 71.8(3) . 6_554 ?
C2 Nb1 C1 142.4(3) 16_656 16_656 ?
C2 Nb1 C1 77.3(2) 16_656 . ?
C2 Nb1 C1 71.8(3) 11_666 16_656 ?
C2 Nb1 C1 71.8(3) 6_554 . ?
C2 Nb1 C1 74.9(2) 6_554 11_666 ?
C2 Nb1 C1 77.3(2) 6_554 16_656 ?
C2 Nb1 C1 71.8(3) 16_656 11_666 ?
C2 Nb1 C1 142.4(3) 11_666 11_666 ?
C2 Nb1 C1 77.3(2) . 11_666 ?
C2 Nb1 C2 145.8(5) . 6_554 ?
C2 Nb1 C2 94.95(13) . 11_666 ?
C2 Nb1 C2 145.8(5) 16_656 11_666 ?
C2 Nb1 C2 94.95(13) 16_656 6_554 ?
C2 Nb1 C2 94.95(13) 11_666 6_554 ?
C2 Nb1 C2 94.95(13) . 16_656 ?
N3 Fe1 N3 180.0 . 9_666 ?
N2 Fe1 N3 91.2(2) . 9_666 ?
N2 Fe1 N3 91.2(2) 9_666 . ?
N2 Fe1 N3 88.8(2) . . ?
N2 Fe1 N3 88.8(2) 9_666 9_666 ?
N2 Fe1 N2 180.0 9_666 . ?
N2 Fe1 N5 86.14(19) 9_666 . ?
N2 Fe1 N5 93.86(19) . . ?
N2 Fe1 N5 93.86(19) 9_666 9_666 ?
N2 Fe1 N5 86.14(19) . 9_666 ?
N5 Fe1 N3 91.3(2) 9_666 9_666 ?
N5 Fe1 N3 91.3(2) . . ?
N5 Fe1 N3 88.7(2) 9_666 . ?
N5 Fe1 N3 88.7(2) . 9_666 ?
N5 Fe1 N5 180.0(3) 9_666 . ?
N4 N3 Fe1 120.1(4) . . ?
C3 N3 Fe1 136.6(5) . . ?
C3 N3 N4 103.0(7) . . ?
N3 N4 H3 123.9 . . ?
C5 N4 N3 112.2(5) . . ?
C5 N4 H3 123.9 . . ?
C2 N2 Fe1 163.0(5) . . ?
N6 N5 Fe1 123.0(3) . . ?
C6 N5 Fe1 131.3(5) . . ?
C6 N5 N6 105.7(6) . . ?
N5 N6 H7 124.7 . . ?
N5 N6 C8 110.5(5) . . ?
C8 N6 H7 124.7 . . ?
N1 C1 Nb1 177.3(7) . . ?
N2 C2 Nb1 174.8(4) . . ?
N6 C8 H8 126.2 . . ?
N6 C8 C7 107.6(6) . . ?
C7 C8 H8 126.2 . . ?
N4 C5 H4 126.7 . . ?
N4 C5 C4 106.7(8) . . ?
C4 C5 H4 126.7 . . ?
N3 C3 H6 123.7 . . ?
N3 C3 C4 112.6(6) . . ?
C4 C3 H6 123.7 . . ?
C5 C4 H5 127.2 . . ?
C3 C4 C5 105.6(7) . . ?
C3 C4 H5 127.2 . . ?
N5 C6 H10 124.3 . . ?
N5 C6 C7 111.3(7) . . ?
C7 C6 H10 124.3 . . ?
C8 C7 C6 104.8(5) . . ?
C8 C7 H9 127.6 . . ?
C6 C7 H9 127.6 . . ?
H1 O1 H2 104.4 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -176.2(5) . . . . ?
Fe1 N3 C3 C4 174.9(5) . . . . ?
Fe1 N5 N6 C8 -179.1(5) . . . . ?
Fe1 N5 C6 C7 178.1(5) . . . . ?
N3 N4 C5 C4 0.6(9) . . . . ?
N3 C3 C4 C5 -0.3(9) . . . . ?
N4 N3 C3 C4 0.6(7) . . . . ?
N4 C5 C4 C3 -0.2(9) . . . . ?
N5 N6 C8 C7 0.6(9) . . . . ?
N5 C6 C7 C8 1.9(9) . . . . ?
N6 N5 C6 C7 -1.6(9) . . . . ?
N6 C8 C7 C6 -1.5(9) . . . . ?
C3 N3 N4 C5 -0.7(7) . . . . ?
C6 N5 N6 C8 0.6(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.445
_oxdiff_exptl_absorpt_empirical_full_min 0.705
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0042
_database_code_depnum_ccdc_archive 'CCDC 2326697'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0042           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.592 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0042           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        496 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 06:21 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.4558(4)
_cell_length_b                   21.4558(4)
_cell_length_c                   9.4642(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4356.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1080
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.2940
_cell_measurement_theta_min      1.7430
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.592
_diffrn_reflns_Laue_measured_fraction_max 0.333
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4054
_diffrn_reflns_point_group_measured_fraction_full 0.592
_diffrn_reflns_point_group_measured_fraction_max 0.333
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.301
_diffrn_reflns_theta_min         1.744
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         380000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.592
_diffrn_measured_fraction_theta_max 0.333
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0061184000
_diffrn_orient_matrix_UB_12      0.0003330000
_diffrn_orient_matrix_UB_13      0.0410453000
_diffrn_orient_matrix_UB_21      0.0171416000
_diffrn_orient_matrix_UB_22      -0.0062611000
_diffrn_orient_matrix_UB_23      -0.0128563000
_diffrn_orient_matrix_UB_31      0.0058364000
_diffrn_orient_matrix_UB_32      0.0180538000
_diffrn_orient_matrix_UB_33      -0.0052432000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1494
_reflns_number_total             1840
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1840
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1123
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H2
 0.95 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C3(H6), C8(H8), C5(H4), C4(H5), C7(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0194(3) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0243(4) Uani 1 2 d S . P . .
O1 O 0.44056(13) 0.36593(12) 0.8052(6) 0.0331(16) Uani 1 1 d D . . . .
N4 N 0.45250(14) 0.46479(12) 0.2035(7) 0.0343(18) Uani 1 1 d . . . . .
H3 H 0.465697 0.426806 0.221759 0.041 Uiso 1 1 calc R U . . .
N2 N 0.48319(12) 0.40078(12) 0.4813(6) 0.0290(16) Uani 1 1 d . . . . .
N3 N 0.45480(12) 0.51218(11) 0.2982(6) 0.0275(17) Uani 1 1 d . . . . .
N5 N 0.41489(12) 0.51656(11) 0.6137(5) 0.0292(16) Uani 1 1 d . . . . .
N6 N 0.39020(12) 0.47780(13) 0.7084(6) 0.0328(18) Uani 1 1 d . . . . .
H7 H 0.407662 0.442777 0.736265 0.039 Uiso 1 1 calc R U . . .
N1 N 0.51470(14) 0.16099(13) 0.0824(7) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.48691(13) 0.34957(13) 0.4453(7) 0.0263(18) Uani 1 1 d . . . . .
C1 C 0.50972(14) 0.19026(14) 0.1810(7) 0.0247(19) Uani 1 1 d . . . . .
C6 C 0.37422(16) 0.56364(15) 0.6015(7) 0.038(2) Uani 1 1 d . . . . .
H10 H 0.379922 0.598712 0.541615 0.045 Uiso 1 1 calc R U . . .
C3 C 0.43050(15) 0.56011(15) 0.2248(7) 0.033(2) Uani 1 1 d . . . . .
H6 H 0.425768 0.600901 0.262295 0.040 Uiso 1 1 calc R U . . .
C8 C 0.33497(17) 0.49922(16) 0.7561(8) 0.038(2) Uani 1 1 d . . . . .
H8 H 0.309029 0.479806 0.824492 0.046 Uiso 1 1 calc R U . . .
C5 C 0.42834(19) 0.48165(17) 0.0808(8) 0.044(3) Uani 1 1 d . . . . .
H4 H 0.422434 0.455616 0.000700 0.053 Uiso 1 1 calc R U . . .
C4 C 0.41331(17) 0.54396(15) 0.0904(8) 0.039(2) Uani 1 1 d . . . . .
H5 H 0.395176 0.569766 0.020006 0.047 Uiso 1 1 calc R U . . .
C7 C 0.32318(16) 0.55462(16) 0.6869(8) 0.040(2) Uani 1 1 d . . . . .
H9 H 0.287652 0.580726 0.696175 0.048 Uiso 1 1 calc R U . . .
H2 H 0.434(3) 0.3291(17) 0.761(6) 0.10(2) Uiso 1 1 d D . . . .
H1 H 0.455(2) 0.358(2) 0.899(3) 0.061(18) Uiso 1 1 d 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
Nb1 C2 2.255(3) 16_656 ?
Nb1 C2 2.255(3) . ?
Nb1 C2 2.255(3) 11_666 ?
Nb1 C2 2.255(3) 6_554 ?
Nb1 C1 2.249(6) 16_656 ?
Nb1 C1 2.249(6) . ?
Nb1 C1 2.249(6) 11_666 ?
Nb1 C1 2.249(6) 6_554 ?
Fe1 N2 2.166(3) 9_666 ?
Fe1 N2 2.166(3) . ?
Fe1 N3 2.158(5) . ?
Fe1 N3 2.158(5) 9_666 ?
Fe1 N5 2.149(3) . ?
Fe1 N5 2.149(3) 9_666 ?
O1 H2 0.903(19) . ?
O1 H1 0.96(2) . ?
N4 H3 0.8800 . ?
N4 N3 1.357(6) . ?
N4 C5 1.322(9) . ?
N2 C2 1.153(5) . ?
N3 C3 1.346(6) . ?
N5 N6 1.333(6) . ?
N5 C6 1.340(4) . ?
N6 H7 0.8800 . ?
N6 C8 1.349(5) . ?
N1 C1 1.130(8) . ?
C6 H10 0.9500 . ?
C6 C7 1.375(7) . ?
C3 H6 0.9500 . ?
C3 C4 1.368(9) . ?
C8 H8 0.9500 . ?
C8 C7 1.381(7) . ?
C5 H4 0.9500 . ?
C5 C4 1.378(5) . ?
C4 H5 0.9500 . ?
C7 H9 0.9500 . ?

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
C2 Nb1 C2 145.7(3) 16_656 11_666 ?
C2 Nb1 C2 95.00(9) 11_666 6_554 ?
C2 Nb1 C2 95.00(9) 16_656 6_554 ?
C2 Nb1 C2 95.00(9) 16_656 . ?
C2 Nb1 C2 145.7(3) 6_554 . ?
C2 Nb1 C2 95.00(9) 11_666 . ?
C1 Nb1 C2 77.05(15) 6_554 11_666 ?
C1 Nb1 C2 75.05(16) 16_656 . ?
C1 Nb1 C2 142.4(2) 11_666 11_666 ?
C1 Nb1 C2 75.06(16) . 11_666 ?
C1 Nb1 C2 71.9(2) 6_554 . ?
C1 Nb1 C2 142.4(2) 16_656 16_656 ?
C1 Nb1 C2 71.9(2) 16_656 11_666 ?
C1 Nb1 C2 71.9(2) 11_666 16_656 ?
C1 Nb1 C2 77.05(15) 11_666 . ?
C1 Nb1 C2 75.05(16) 6_554 16_656 ?
C1 Nb1 C2 142.4(2) . . ?
C1 Nb1 C2 142.4(2) 6_554 6_554 ?
C1 Nb1 C2 77.05(15) . 16_656 ?
C1 Nb1 C2 77.05(15) 16_656 6_554 ?
C1 Nb1 C2 75.05(16) 11_666 6_554 ?
C1 Nb1 C2 71.9(2) . 6_554 ?
C1 Nb1 C1 131.81(15) 16_656 . ?
C1 Nb1 C1 131.81(15) 16_656 6_554 ?
C1 Nb1 C1 70.5(2) 16_656 11_666 ?
C1 Nb1 C1 131.81(15) 11_666 . ?
C1 Nb1 C1 131.81(15) 11_666 6_554 ?
C1 Nb1 C1 70.5(2) 6_554 . ?
N2 Fe1 N2 180.0 . 9_666 ?
N3 Fe1 N2 91.62(15) . 9_666 ?
N3 Fe1 N2 88.38(15) 9_666 9_666 ?
N3 Fe1 N2 91.62(15) 9_666 . ?
N3 Fe1 N2 88.38(15) . . ?
N3 Fe1 N3 180.0 9_666 . ?
N5 Fe1 N2 86.44(11) . 9_666 ?
N5 Fe1 N2 93.55(11) . . ?
N5 Fe1 N2 86.44(11) 9_666 . ?
N5 Fe1 N2 93.56(11) 9_666 9_666 ?
N5 Fe1 N3 92.37(15) 9_666 9_666 ?
N5 Fe1 N3 92.37(15) . . ?
N5 Fe1 N3 87.63(15) . 9_666 ?
N5 Fe1 N3 87.63(15) 9_666 . ?
N5 Fe1 N5 180.0 9_666 . ?
H2 O1 H1 109(4) . . ?
N3 N4 H3 123.5 . . ?
C5 N4 H3 123.5 . . ?
C5 N4 N3 112.9(3) . . ?
C2 N2 Fe1 161.6(4) . . ?
N4 N3 Fe1 120.7(3) . . ?
C3 N3 Fe1 136.4(3) . . ?
C3 N3 N4 102.5(5) . . ?
N6 N5 Fe1 124.9(2) . . ?
N6 N5 C6 105.6(4) . . ?
C6 N5 Fe1 129.4(3) . . ?
N5 N6 H7 124.4 . . ?
N5 N6 C8 111.2(3) . . ?
C8 N6 H7 124.4 . . ?
N2 C2 Nb1 176.8(2) . . ?
N1 C1 Nb1 179.0(5) . . ?
N5 C6 H10 124.4 . . ?
N5 C6 C7 111.2(4) . . ?
C7 C6 H10 124.4 . . ?
N3 C3 H6 123.5 . . ?
N3 C3 C4 113.0(4) . . ?
C4 C3 H6 123.5 . . ?
N6 C8 H8 126.4 . . ?
N6 C8 C7 107.2(4) . . ?
C7 C8 H8 126.4 . . ?
N4 C5 H4 126.3 . . ?
N4 C5 C4 107.4(6) . . ?
C4 C5 H4 126.3 . . ?
C3 C4 C5 104.1(5) . . ?
C3 C4 H5 127.9 . . ?
C5 C4 H5 127.9 . . ?
C6 C7 C8 104.7(3) . . ?
C6 C7 H9 127.6 . . ?
C8 C7 H9 127.6 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 172.6(3) . . . . ?
Fe1 N5 N6 C8 -176.5(4) . . . . ?
Fe1 N5 C6 C7 175.6(4) . . . . ?
N4 N3 C3 C4 0.3(5) . . . . ?
N4 C5 C4 C3 0.0(6) . . . . ?
N3 N4 C5 C4 0.2(6) . . . . ?
N3 C3 C4 C5 -0.2(6) . . . . ?
N5 N6 C8 C7 0.7(6) . . . . ?
N5 C6 C7 C8 1.2(6) . . . . ?
N6 N5 C6 C7 -0.8(6) . . . . ?
N6 C8 C7 C6 -1.1(6) . . . . ?
C6 N5 N6 C8 0.1(6) . . . . ?
C5 N4 N3 Fe1 -174.1(3) . . . . ?
C5 N4 N3 C3 -0.3(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   423
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.908
_oxdiff_exptl_absorpt_empirical_full_min 0.727
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0031
_database_code_depnum_ccdc_archive 'CCDC 2326557'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0031           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.626 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0031           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        425 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 05:46 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.1680(7)
_cell_length_b                   21.1680(7)
_cell_length_c                   9.3545(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4191.6(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    810
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.8080
_cell_measurement_theta_min      1.7640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.1218
_diffrn_reflns_Laue_measured_fraction_full 0.626
_diffrn_reflns_Laue_measured_fraction_max 0.368
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3895
_diffrn_reflns_point_group_measured_fraction_full 0.626
_diffrn_reflns_point_group_measured_fraction_max 0.368
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.860
_diffrn_reflns_theta_min         1.766
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         820000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.626
_diffrn_measured_fraction_theta_max 0.368
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003524000
_diffrn_orient_matrix_UB_12      0.0071896000
_diffrn_orient_matrix_UB_13      0.0405194000
_diffrn_orient_matrix_UB_21      0.0028841000
_diffrn_orient_matrix_UB_22      0.0178363000
_diffrn_orient_matrix_UB_23      -0.0160759000
_diffrn_orient_matrix_UB_31      -0.0191862000
_diffrn_orient_matrix_UB_32      0.0025411000
_diffrn_orient_matrix_UB_33      -0.0031800000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1235
_reflns_number_total             1832
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1657
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C5(H4), C6(H10), C4(H5), C3(H6), C7(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0304(4) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0310(5) Uani 1 2 d S . P . .
O1 O 0.44193(18) 0.36616(19) 0.7995(8) 0.0370(19) Uani 1 1 d D . . . .
N3 N 0.45477(18) 0.51359(19) 0.2997(8) 0.034(2) Uani 1 1 d . . . . .
N4 N 0.4534(2) 0.4651(2) 0.2032(9) 0.040(2) Uani 1 1 d . . . . .
H3 H 0.467777 0.426845 0.220815 0.047 Uiso 1 1 calc R U . . .
N2 N 0.4818(2) 0.4033(2) 0.4832(8) 0.036(2) Uani 1 1 d . . . . .
N1 N 0.5158(2) 0.1604(2) 0.0756(9) 0.042(2) Uani 1 1 d . . . . .
N5 N 0.4154(2) 0.51828(19) 0.6099(8) 0.037(2) Uani 1 1 d . . . . .
N6 N 0.3899(2) 0.4788(2) 0.7070(8) 0.041(2) Uani 1 1 d . . . . .
H7 H 0.407571 0.443457 0.736425 0.049 Uiso 1 1 calc R U . . .
C8 C 0.3333(3) 0.5007(3) 0.7534(10) 0.042(3) Uani 1 1 d . . . . .
H8 H 0.306520 0.480977 0.821587 0.050 Uiso 1 1 calc R U . . .
C2 C 0.4852(2) 0.3511(3) 0.4464(10) 0.037(2) Uani 1 1 d . . . . .
C5 C 0.4276(3) 0.4824(3) 0.0792(11) 0.042(3) Uani 1 1 d . . . . .
H4 H 0.421186 0.456340 -0.002187 0.050 Uiso 1 1 calc R U . . .
C6 C 0.3745(3) 0.5662(2) 0.5968(10) 0.039(3) Uani 1 1 d . . . . .
H10 H 0.380584 0.601762 0.536495 0.047 Uiso 1 1 calc R U . . .
C1 C 0.5102(2) 0.1896(3) 0.1794(10) 0.032(3) Uani 1 1 d . . . . .
C4 C 0.4122(3) 0.5446(2) 0.0912(10) 0.043(3) Uani 1 1 d . . . . .
H5 H 0.393299 0.570736 0.020424 0.051 Uiso 1 1 calc R U . . .
C3 C 0.4297(2) 0.5618(2) 0.2274(10) 0.040(3) Uani 1 1 d . . . . .
H6 H 0.424619 0.603050 0.265452 0.048 Uiso 1 1 calc R U . . .
C7 C 0.3218(3) 0.5567(3) 0.6836(10) 0.045(3) Uani 1 1 d . . . . .
H9 H 0.285797 0.583207 0.692572 0.054 Uiso 1 1 calc R U . . .
H1 H 0.454(3) 0.364(3) 0.898(3) 0.033(19) Uiso 1 1 d D . . . .
H2 H 0.427(6) 0.325(2) 0.780(10) 0.28(8) Uiso 1 1 d 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
Nb1 C2 2.265(6) . ?
Nb1 C2 2.265(6) 11_666 ?
Nb1 C2 2.265(6) 16_656 ?
Nb1 C2 2.265(6) 6_554 ?
Nb1 C1 2.243(8) 16_656 ?
Nb1 C1 2.243(8) . ?
Nb1 C1 2.243(8) 11_666 ?
Nb1 C1 2.243(8) 6_554 ?
Fe1 N3 2.124(7) 9_666 ?
Fe1 N3 2.124(7) . ?
Fe1 N2 2.089(4) . ?
Fe1 N2 2.089(4) 9_666 ?
Fe1 N5 2.101(5) . ?
Fe1 N5 2.100(5) 9_666 ?
O1 H1 0.96(2) . ?
O1 H2 0.95(2) . ?
N3 N4 1.368(8) . ?
N3 C3 1.333(8) . ?
N4 H3 0.8800 . ?
N4 C5 1.334(11) . ?
N2 C2 1.158(8) . ?
N1 C1 1.157(11) . ?
N5 N6 1.348(8) . ?
N5 C6 1.339(7) . ?
N6 H7 0.8800 . ?
N6 C8 1.355(7) . ?
C8 H8 0.9500 . ?
C8 C7 1.376(9) . ?
C5 H4 0.9500 . ?
C5 C4 1.361(8) . ?
C6 H10 0.9500 . ?
C6 C7 1.394(10) . ?
C4 H5 0.9500 . ?
C4 C3 1.376(12) . ?
C3 H6 0.9500 . ?
C7 H9 0.9500 . ?

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
C2 Nb1 C2 94.99(13) . 16_656 ?
C2 Nb1 C2 145.7(5) 16_656 11_666 ?
C2 Nb1 C2 95.00(13) . 11_666 ?
C2 Nb1 C2 145.7(5) . 6_554 ?
C2 Nb1 C2 95.00(13) 11_666 6_554 ?
C2 Nb1 C2 95.00(13) 16_656 6_554 ?
C1 Nb1 C2 75.3(2) 6_554 16_656 ?
C1 Nb1 C2 76.8(2) 16_656 6_554 ?
C1 Nb1 C2 71.9(3) 11_666 16_656 ?
C1 Nb1 C2 76.8(2) . 16_656 ?
C1 Nb1 C2 142.5(3) 6_554 6_554 ?
C1 Nb1 C2 75.3(2) 16_656 . ?
C1 Nb1 C2 142.5(3) 16_656 16_656 ?
C1 Nb1 C2 76.8(2) 11_666 . ?
C1 Nb1 C2 75.3(2) 11_666 6_554 ?
C1 Nb1 C2 71.9(3) 6_554 . ?
C1 Nb1 C2 71.9(3) . 6_554 ?
C1 Nb1 C2 75.3(2) . 11_666 ?
C1 Nb1 C2 142.5(3) . . ?
C1 Nb1 C2 142.5(3) 11_666 11_666 ?
C1 Nb1 C2 76.8(2) 6_554 11_666 ?
C1 Nb1 C2 71.9(3) 16_656 11_666 ?
C1 Nb1 C1 131.7(2) 16_656 . ?
C1 Nb1 C1 131.7(2) 16_656 6_554 ?
C1 Nb1 C1 131.7(2) 11_666 6_554 ?
C1 Nb1 C1 131.7(2) 11_666 . ?
C1 Nb1 C1 70.6(4) 6_554 . ?
C1 Nb1 C1 70.6(4) 16_656 11_666 ?
N3 Fe1 N3 180.0 9_666 . ?
N2 Fe1 N3 91.0(2) 9_666 . ?
N2 Fe1 N3 91.0(2) . 9_666 ?
N2 Fe1 N3 89.0(2) 9_666 9_666 ?
N2 Fe1 N3 89.0(2) . . ?
N2 Fe1 N2 180.0 . 9_666 ?
N2 Fe1 N5 93.45(18) 9_666 9_666 ?
N2 Fe1 N5 86.55(18) 9_666 . ?
N2 Fe1 N5 86.55(18) . 9_666 ?
N2 Fe1 N5 93.45(18) . . ?
N5 Fe1 N3 91.3(2) . . ?
N5 Fe1 N3 91.3(2) 9_666 9_666 ?
N5 Fe1 N3 88.7(2) . 9_666 ?
N5 Fe1 N3 88.7(2) 9_666 . ?
N5 Fe1 N5 180.0(2) 9_666 . ?
H1 O1 H2 103(4) . . ?
N4 N3 Fe1 119.4(4) . . ?
C3 N3 Fe1 136.9(5) . . ?
C3 N3 N4 103.3(7) . . ?
N3 N4 H3 124.0 . . ?
C5 N4 N3 112.1(5) . . ?
C5 N4 H3 124.0 . . ?
C2 N2 Fe1 160.9(5) . . ?
N6 N5 Fe1 123.9(3) . . ?
C6 N5 Fe1 130.2(5) . . ?
C6 N5 N6 105.8(6) . . ?
N5 N6 H7 124.5 . . ?
N5 N6 C8 110.9(5) . . ?
C8 N6 H7 124.5 . . ?
N6 C8 H8 126.3 . . ?
N6 C8 C7 107.4(6) . . ?
C7 C8 H8 126.3 . . ?
N2 C2 Nb1 175.5(4) . . ?
N4 C5 H4 126.5 . . ?
N4 C5 C4 107.1(8) . . ?
C4 C5 H4 126.5 . . ?
N5 C6 H10 124.6 . . ?
N5 C6 C7 110.8(7) . . ?
C7 C6 H10 124.6 . . ?
N1 C1 Nb1 177.6(7) . . ?
C5 C4 H5 127.3 . . ?
C5 C4 C3 105.4(7) . . ?
C3 C4 H5 127.3 . . ?
N3 C3 C4 112.1(5) . . ?
N3 C3 H6 124.0 . . ?
C4 C3 H6 124.0 . . ?
C8 C7 C6 105.0(5) . . ?
C8 C7 H9 127.5 . . ?
C6 C7 H9 127.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -175.3(4) . . . . ?
Fe1 N3 C3 C4 173.3(5) . . . . ?
Fe1 N5 N6 C8 -175.9(5) . . . . ?
Fe1 N5 C6 C7 175.2(5) . . . . ?
N3 N4 C5 C4 1.1(8) . . . . ?
N4 N3 C3 C4 0.9(7) . . . . ?
N4 C5 C4 C3 -0.5(8) . . . . ?
N5 N6 C8 C7 -0.1(9) . . . . ?
N5 C6 C7 C8 1.2(9) . . . . ?
N6 N5 C6 C7 -1.3(9) . . . . ?
N6 C8 C7 C6 -0.7(9) . . . . ?
C5 C4 C3 N3 -0.2(8) . . . . ?
C6 N5 N6 C8 0.9(8) . . . . ?
C3 N3 N4 C5 -1.2(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   485
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.495
_oxdiff_exptl_absorpt_empirical_full_min 0.459
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0020
_database_code_depnum_ccdc_archive 'CCDC 2326553'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0020           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.648 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0020           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        388 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 05:15 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.0773(6)
_cell_length_b                   21.0773(6)
_cell_length_c                   9.3291(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4144.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    931
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.5530
_cell_measurement_theta_min      1.7700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.648
_diffrn_reflns_Laue_measured_fraction_max 0.359
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4037
_diffrn_reflns_point_group_measured_fraction_full 0.648
_diffrn_reflns_point_group_measured_fraction_max 0.359
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.192
_diffrn_reflns_theta_min         1.772
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         870000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.648
_diffrn_measured_fraction_theta_max 0.359
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004002000
_diffrn_orient_matrix_UB_12      0.0079587000
_diffrn_orient_matrix_UB_13      0.0400345000
_diffrn_orient_matrix_UB_21      0.0023214000
_diffrn_orient_matrix_UB_22      0.0176698000
_diffrn_orient_matrix_UB_23      -0.0177798000
_diffrn_orient_matrix_UB_31      -0.0193152000
_diffrn_orient_matrix_UB_32      0.0019400000
_diffrn_orient_matrix_UB_33      -0.0029736000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1322
_reflns_number_total             1862
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1862
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1030
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C5(H4), C8(H8), C3(H6), C7(H9), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0298(3) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0295(3) Uani 1 2 d S . P . .
O1 O 0.44238(13) 0.36640(12) 0.7996(5) 0.0377(11) Uani 1 1 d D . . . .
N4 N 0.45368(14) 0.46546(13) 0.2024(6) 0.0358(14) Uani 1 1 d . . . . .
H3 H 0.468267 0.427068 0.219349 0.043 Uiso 1 1 calc R U . . .
N3 N 0.45556(13) 0.51337(12) 0.3009(5) 0.0360(13) Uani 1 1 d . . . . .
N2 N 0.48218(13) 0.40333(14) 0.4808(5) 0.0358(13) Uani 1 1 d . . . . .
N5 N 0.41566(13) 0.51801(13) 0.6087(5) 0.0351(13) Uani 1 1 d . . . . .
N1 N 0.51572(14) 0.15996(14) 0.0770(6) 0.0382(15) Uani 1 1 d . . . . .
N6 N 0.39010(14) 0.47885(13) 0.7063(5) 0.0399(14) Uani 1 1 d . . . . .
H7 H 0.407828 0.443337 0.735574 0.048 Uiso 1 1 calc R U . . .
C2 C 0.48555(15) 0.35117(16) 0.4464(6) 0.0352(16) Uani 1 1 d . . . . .
C6 C 0.37464(16) 0.56628(15) 0.5972(6) 0.0359(16) Uani 1 1 d . . . . .
H10 H 0.380920 0.602215 0.537364 0.043 Uiso 1 1 calc R U . . .
C5 C 0.42798(18) 0.48232(18) 0.0800(7) 0.0439(19) Uani 1 1 d . . . . .
H4 H 0.421882 0.456085 -0.001632 0.053 Uiso 1 1 calc R U . . .
C1 C 0.51056(15) 0.18964(16) 0.1785(6) 0.0305(15) Uani 1 1 d . . . . .
C8 C 0.33366(17) 0.50086(17) 0.7540(7) 0.0432(19) Uani 1 1 d . . . . .
H8 H 0.307050 0.481227 0.823231 0.052 Uiso 1 1 calc R U . . .
C3 C 0.42965(16) 0.56177(17) 0.2279(7) 0.0366(17) Uani 1 1 d . . . . .
H6 H 0.424465 0.603168 0.266356 0.044 Uiso 1 1 calc R U . . .
C7 C 0.32195(18) 0.55722(17) 0.6833(6) 0.0414(19) Uani 1 1 d . . . . .
H9 H 0.285784 0.583852 0.691914 0.050 Uiso 1 1 calc R U . . .
C4 C 0.41158(16) 0.54523(16) 0.0926(6) 0.0423(19) Uani 1 1 d . . . . .
H5 H 0.391976 0.571398 0.022511 0.051 Uiso 1 1 calc R U . . .
H1 H 0.458(2) 0.3575(19) 0.892(3) 0.050(15) Uiso 1 1 d D . . . .
H2 H 0.434(3) 0.334(2) 0.740(5) 0.11(2) Uiso 1 1 d 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
Nb1 C2 2.255(4) . ?
Nb1 C2 2.255(4) 6_554 ?
Nb1 C2 2.255(4) 11_666 ?
Nb1 C2 2.255(4) 16_656 ?
Nb1 C1 2.242(5) . ?
Nb1 C1 2.242(5) 6_554 ?
Nb1 C1 2.242(5) 16_656 ?
Nb1 C1 2.242(5) 11_666 ?
Fe1 N3 2.099(5) 9_666 ?
Fe1 N3 2.099(5) . ?
Fe1 N2 2.080(3) 9_666 ?
Fe1 N2 2.080(3) . ?
Fe1 N5 2.081(3) . ?
Fe1 N5 2.081(3) 9_666 ?
O1 H1 0.940(19) . ?
O1 H2 0.897(19) . ?
N4 H3 0.8800 . ?
N4 N3 1.366(5) . ?
N4 C5 1.313(7) . ?
N3 C3 1.343(5) . ?
N2 C2 1.148(5) . ?
N5 N6 1.342(5) . ?
N5 C6 1.339(4) . ?
N1 C1 1.140(7) . ?
N6 H7 0.8800 . ?
N6 C8 1.352(5) . ?
C6 H10 0.9500 . ?
C6 C7 1.384(6) . ?
C5 H4 0.9500 . ?
C5 C4 1.375(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.381(6) . ?
C3 H6 0.9500 . ?
C3 C4 1.363(8) . ?
C7 H9 0.9500 . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 95.01(8) . 16_656 ?
C2 Nb1 C2 145.6(3) 16_656 11_666 ?
C2 Nb1 C2 95.01(8) . 11_666 ?
C2 Nb1 C2 145.6(3) . 6_554 ?
C2 Nb1 C2 95.01(8) 11_666 6_554 ?
C2 Nb1 C2 95.01(8) 16_656 6_554 ?
C1 Nb1 C2 72.03(18) 11_666 16_656 ?
C1 Nb1 C2 72.03(18) . 6_554 ?
C1 Nb1 C2 142.33(19) 16_656 16_656 ?
C1 Nb1 C2 75.01(15) 6_554 16_656 ?
C1 Nb1 C2 75.01(15) 11_666 6_554 ?
C1 Nb1 C2 142.33(18) . . ?
C1 Nb1 C2 77.04(15) . 16_656 ?
C1 Nb1 C2 75.01(15) 16_656 . ?
C1 Nb1 C2 77.04(15) 16_656 6_554 ?
C1 Nb1 C2 77.04(15) 11_666 . ?
C1 Nb1 C2 142.33(19) 6_554 6_554 ?
C1 Nb1 C2 77.04(15) 6_554 11_666 ?
C1 Nb1 C2 72.03(18) 6_554 . ?
C1 Nb1 C2 72.03(18) 16_656 11_666 ?
C1 Nb1 C2 142.33(19) 11_666 11_666 ?
C1 Nb1 C2 75.01(15) . 11_666 ?
C1 Nb1 C1 70.3(2) . 6_554 ?
C1 Nb1 C1 131.93(15) . 11_666 ?
C1 Nb1 C1 70.3(2) 16_656 11_666 ?
C1 Nb1 C1 131.93(15) 16_656 6_554 ?
C1 Nb1 C1 131.93(15) 11_666 6_554 ?
C1 Nb1 C1 131.93(15) . 16_656 ?
N3 Fe1 N3 180.0 . 9_666 ?
N2 Fe1 N3 88.56(15) 9_666 9_666 ?
N2 Fe1 N3 88.56(15) . . ?
N2 Fe1 N3 91.44(15) 9_666 . ?
N2 Fe1 N3 91.44(15) . 9_666 ?
N2 Fe1 N2 180.0 . 9_666 ?
N2 Fe1 N5 86.20(12) 9_666 . ?
N2 Fe1 N5 93.80(12) 9_666 9_666 ?
N2 Fe1 N5 93.80(12) . . ?
N2 Fe1 N5 86.20(12) . 9_666 ?
N5 Fe1 N3 91.45(15) 9_666 9_666 ?
N5 Fe1 N3 91.45(15) . . ?
N5 Fe1 N3 88.55(15) 9_666 . ?
N5 Fe1 N3 88.55(15) . 9_666 ?
N5 Fe1 N5 180.0 . 9_666 ?
H1 O1 H2 119(4) . . ?
N3 N4 H3 123.3 . . ?
C5 N4 H3 123.3 . . ?
C5 N4 N3 113.4(3) . . ?
N4 N3 Fe1 120.6(3) . . ?
C3 N3 Fe1 137.1(3) . . ?
C3 N3 N4 102.0(4) . . ?
C2 N2 Fe1 162.1(3) . . ?
N6 N5 Fe1 124.1(2) . . ?
C6 N5 Fe1 130.6(3) . . ?
C6 N5 N6 105.2(4) . . ?
N5 N6 H7 124.3 . . ?
N5 N6 C8 111.4(3) . . ?
C8 N6 H7 124.3 . . ?
N2 C2 Nb1 175.7(3) . . ?
N5 C6 H10 124.2 . . ?
N5 C6 C7 111.5(4) . . ?
C7 C6 H10 124.2 . . ?
N4 C5 H4 126.6 . . ?
N4 C5 C4 106.9(5) . . ?
C4 C5 H4 126.6 . . ?
N1 C1 Nb1 178.7(5) . . ?
N6 C8 H8 126.4 . . ?
N6 C8 C7 107.2(4) . . ?
C7 C8 H8 126.4 . . ?
N3 C3 H6 123.5 . . ?
N3 C3 C4 112.9(4) . . ?
C4 C3 H6 123.5 . . ?
C6 C7 H9 127.7 . . ?
C8 C7 C6 104.6(3) . . ?
C8 C7 H9 127.7 . . ?
C5 C4 H5 127.6 . . ?
C3 C4 C5 104.8(4) . . ?
C3 C4 H5 127.6 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 174.5(3) . . . . ?
Fe1 N5 N6 C8 -176.8(3) . . . . ?
Fe1 N5 C6 C7 175.7(3) . . . . ?
N4 N3 C3 C4 1.0(4) . . . . ?
N4 C5 C4 C3 0.0(5) . . . . ?
N3 N4 C5 C4 0.6(5) . . . . ?
N3 C3 C4 C5 -0.7(5) . . . . ?
N5 N6 C8 C7 0.1(6) . . . . ?
N5 C6 C7 C8 2.1(6) . . . . ?
N6 N5 C6 C7 -2.0(6) . . . . ?
N6 C8 C7 C6 -1.3(6) . . . . ?
C6 N5 N6 C8 1.1(6) . . . . ?
C5 N4 N3 Fe1 -175.8(3) . . . . ?
C5 N4 N3 C3 -1.0(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   435
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.311
_oxdiff_exptl_absorpt_empirical_full_min 0.590
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0037
_database_code_depnum_ccdc_archive 'CCDC 2327700'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;

# start Validation Reply Form
_vrf_PLAT029_fenb_0037           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.610 Why?  
RESPONSE: The generated Alerts A, B and C are the typical high-pressure crystallography warnings. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0037           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        562 Report
RESPONSE: The generated Alerts A, B and C are the typical high-pressure crystallography warnings. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# end Validation Reply Form

_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   20.6618(4)
_cell_length_b                   20.6618(4)
_cell_length_c                   9.2789(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3961.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    998
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.5020
_cell_measurement_theta_min      2.4100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_unetI/netI     0.3130
_diffrn_reflns_Laue_measured_fraction_full 0.610
_diffrn_reflns_Laue_measured_fraction_max 0.366
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3321
_diffrn_reflns_point_group_measured_fraction_full 0.610
_diffrn_reflns_point_group_measured_fraction_max 0.366
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.894
_diffrn_reflns_theta_min         1.795
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         1530000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.610
_diffrn_measured_fraction_theta_max 0.366
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003751000
_diffrn_orient_matrix_UB_12      0.0080410000
_diffrn_orient_matrix_UB_13      0.0403054000
_diffrn_orient_matrix_UB_21      0.0055425000
_diffrn_orient_matrix_UB_22      0.0174775000
_diffrn_orient_matrix_UB_23      -0.0170428000
_diffrn_orient_matrix_UB_31      -0.0190719000
_diffrn_orient_matrix_UB_32      0.0049047000
_diffrn_orient_matrix_UB_33      -0.0057933000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1411
_reflns_number_total             1743
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1743
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0959
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0479P)²+2.4197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2959
_refine_ls_wR_factor_ref         0.3270
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N5 \\sim N6 \\sim C8 \\sim C7 \\sim C6: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
N3 \\sim C3 \\sim C4 \\sim C5 \\sim N4: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.016
Uanis(C1) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(N2) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
4.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C5(H4), C3(H6), C7(H9), C6(H10), C4(H5), C8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0174(6) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0216(7) Uani 1 2 d S . P . .
O1 O 0.4455(2) 0.3645(2) 0.7959(11) 0.036(2) Uani 1 1 d D . . . .
N3 N 0.4578(3) 0.5136(2) 0.3094(10) 0.0254(17) Uani 1 1 d . U . . .
N2 N 0.4834(2) 0.4073(2) 0.4794(9) 0.0221(16) Uani 1 1 d . U . . .
N4 N 0.4566(3) 0.4662(3) 0.2088(10) 0.0298(18) Uani 1 1 d . U . . .
H3 H 0.472274 0.427159 0.223555 0.036 Uiso 1 1 calc R U . . .
N1 N 0.5165(3) 0.1586(3) 0.0763(12) 0.034(3) Uani 1 1 d . . . . .
N5 N 0.4176(3) 0.5179(3) 0.6008(10) 0.0285(16) Uani 1 1 d . U . . .
C2 C 0.4848(3) 0.3538(3) 0.4481(12) 0.024(2) Uani 1 1 d . . . . .
N6 N 0.3933(3) 0.4776(3) 0.7049(11) 0.0306(16) Uani 1 1 d . U . . .
H7 H 0.412428 0.442007 0.735197 0.037 Uiso 1 1 calc R U . . .
C1 C 0.5112(3) 0.1885(3) 0.1772(13) 0.0250(19) Uani 1 1 d . U . . .
C5 C 0.4296(4) 0.4841(3) 0.0870(14) 0.0334(19) Uani 1 1 d . U . . .
H4 H 0.423956 0.458040 0.003651 0.040 Uiso 1 1 calc R U . . .
C3 C 0.4291(3) 0.5631(3) 0.2399(13) 0.031(2) Uani 1 1 d . U . . .
H6 H 0.421863 0.604595 0.281095 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3228(3) 0.5588(3) 0.6799(12) 0.0328(19) Uani 1 1 d . U . . .
H9 H 0.286347 0.586430 0.689578 0.039 Uiso 1 1 calc R U . . .
C6 C 0.3747(3) 0.5667(3) 0.5904(12) 0.0298(18) Uani 1 1 d . U . . .
H10 H 0.379997 0.602737 0.527849 0.036 Uiso 1 1 calc R U . . .
C4 C 0.4115(4) 0.5463(4) 0.1021(13) 0.033(2) Uani 1 1 d . U . . .
H5 H 0.390958 0.572976 0.032250 0.039 Uiso 1 1 calc R U . . .
C8 C 0.3354(4) 0.5001(4) 0.7554(14) 0.0354(19) Uani 1 1 d . U . . .
H8 H 0.308791 0.480491 0.826639 0.042 Uiso 1 1 calc R U . . .
H2 H 0.428(7) 0.326(3) 0.760(15) 0.13(6) Uiso 1 1 d D . . . .
H1 H 0.454(6) 0.357(7) 0.895(4) 0.10(6) Uiso 1 1 d 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
Nb1 C2 2.272(6) . ?
Nb1 C2 2.272(6) 11_666 ?
Nb1 C2 2.272(6) 16_656 ?
Nb1 C2 2.272(6) 6_554 ?
Nb1 C1 2.244(10) . ?
Nb1 C1 2.244(10) 6_554 ?
Nb1 C1 2.244(10) 16_656 ?
Nb1 C1 2.244(10) 11_666 ?
Fe1 N3 1.992(9) 9_666 ?
Fe1 N3 1.992(9) . ?
Fe1 N2 1.954(5) 9_666 ?
Fe1 N2 1.954(5) . ?
Fe1 N5 1.977(7) . ?
Fe1 N5 1.977(7) 9_666 ?
O1 H2 0.94(2) . ?
O1 H1 0.95(2) . ?
N3 N4 1.354(10) . ?
N3 C3 1.347(10) . ?
N2 C2 1.143(8) . ?
N4 H3 0.8800 . ?
N4 C5 1.313(14) . ?
N1 C1 1.127(14) . ?
N5 N6 1.371(11) . ?
N5 C6 1.347(9) . ?
N6 H7 0.8800 . ?
N6 C8 1.367(10) . ?
C5 H4 0.9500 . ?
C5 C4 1.346(10) . ?
C3 H6 0.9500 . ?
C3 C4 1.374(15) . ?
C7 H9 0.9500 . ?
C7 C6 1.365(13) . ?
C7 C8 1.425(12) . ?
C6 H10 0.9500 . ?
C4 H5 0.9500 . ?
C8 H8 0.9500 . ?

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
C2 Nb1 C2 95.12(15) . 16_656 ?
C2 Nb1 C2 145.3(5) 16_656 11_666 ?
C2 Nb1 C2 95.12(16) . 11_666 ?
C2 Nb1 C2 145.3(5) . 6_554 ?
C2 Nb1 C2 95.12(15) 11_666 6_554 ?
C2 Nb1 C2 95.12(16) 16_656 6_554 ?
C1 Nb1 C2 72.2(4) 11_666 16_656 ?
C1 Nb1 C2 72.2(3) . 6_554 ?
C1 Nb1 C2 142.5(3) 16_656 16_656 ?
C1 Nb1 C2 74.7(3) 6_554 16_656 ?
C1 Nb1 C2 74.7(3) 11_666 6_554 ?
C1 Nb1 C2 142.5(3) . . ?
C1 Nb1 C2 77.0(3) . 16_656 ?
C1 Nb1 C2 74.7(3) 16_656 . ?
C1 Nb1 C2 77.0(3) 16_656 6_554 ?
C1 Nb1 C2 77.0(3) 11_666 . ?
C1 Nb1 C2 142.5(3) 6_554 6_554 ?
C1 Nb1 C2 77.0(3) 6_554 11_666 ?
C1 Nb1 C2 72.2(4) 6_554 . ?
C1 Nb1 C2 72.2(4) 16_656 11_666 ?
C1 Nb1 C2 142.5(3) 11_666 11_666 ?
C1 Nb1 C2 74.7(3) . 11_666 ?
C1 Nb1 C1 70.3(4) . 6_554 ?
C1 Nb1 C1 131.9(3) . 11_666 ?
C1 Nb1 C1 70.3(4) 16_656 11_666 ?
C1 Nb1 C1 131.9(3) 16_656 6_554 ?
C1 Nb1 C1 131.9(3) 11_666 6_554 ?
C1 Nb1 C1 132.0(3) . 16_656 ?
N3 Fe1 N3 180.0 9_666 . ?
N2 Fe1 N3 88.6(3) . . ?
N2 Fe1 N3 88.6(3) 9_666 9_666 ?
N2 Fe1 N3 91.4(3) . 9_666 ?
N2 Fe1 N3 91.4(3) 9_666 . ?
N2 Fe1 N2 180.0 9_666 . ?
N2 Fe1 N5 85.5(2) 9_666 . ?
N2 Fe1 N5 85.5(2) . 9_666 ?
N2 Fe1 N5 94.5(2) 9_666 9_666 ?
N2 Fe1 N5 94.5(2) . . ?
N5 Fe1 N3 90.9(3) . . ?
N5 Fe1 N3 90.9(3) 9_666 9_666 ?
N5 Fe1 N3 89.1(3) . 9_666 ?
N5 Fe1 N3 89.1(3) 9_666 . ?
N5 Fe1 N5 180.00(18) 9_666 . ?
H2 O1 H1 106(5) . . ?
N4 N3 Fe1 121.2(5) . . ?
C3 N3 Fe1 136.5(6) . . ?
C3 N3 N4 102.2(8) . . ?
C2 N2 Fe1 165.4(6) . . ?
N3 N4 H3 123.3 . . ?
C5 N4 N3 113.4(6) . . ?
C5 N4 H3 123.3 . . ?
N6 N5 Fe1 122.4(4) . . ?
C6 N5 Fe1 132.3(7) . . ?
C6 N5 N6 105.4(7) . . ?
N2 C2 Nb1 172.9(5) . . ?
N5 N6 H7 124.6 . . ?
C8 N6 N5 110.8(6) . . ?
C8 N6 H7 124.6 . . ?
N1 C1 Nb1 178.6(9) . . ?
N4 C5 H4 126.3 . . ?
N4 C5 C4 107.4(9) . . ?
C4 C5 H4 126.3 . . ?
N3 C3 H6 124.1 . . ?
N3 C3 C4 111.8(7) . . ?
C4 C3 H6 124.1 . . ?
C6 C7 H9 127.5 . . ?
C6 C7 C8 105.0(6) . . ?
C8 C7 H9 127.5 . . ?
N5 C6 C7 112.5(8) . . ?
N5 C6 H10 123.7 . . ?
C7 C6 H10 123.7 . . ?
C5 C4 C3 105.3(8) . . ?
C5 C4 H5 127.3 . . ?
C3 C4 H5 127.3 . . ?
N6 C8 C7 106.3(8) . . ?
N6 C8 H8 126.9 . . ?
C7 C8 H8 126.9 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -176.9(6) . . . . ?
Fe1 N3 C3 C4 175.9(6) . . . . ?
Fe1 N5 N6 C8 -178.8(6) . . . . ?
Fe1 N5 C6 C7 178.7(6) . . . . ?
N3 N4 C5 C4 0.3(11) . . . . ?
N3 C3 C4 C5 0.5(10) . . . . ?
N4 N3 C3 C4 -0.3(9) . . . . ?
N4 C5 C4 C3 -0.5(10) . . . . ?
N5 N6 C8 C7 -0.9(11) . . . . ?
N6 N5 C6 C7 -1.9(10) . . . . ?
C3 N3 N4 C5 0.0(9) . . . . ?
C6 N5 N6 C8 1.7(10) . . . . ?
C6 C7 C8 N6 -0.3(11) . . . . ?
C8 C7 C6 N5 1.4(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   386
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 10.180
_oxdiff_exptl_absorpt_empirical_full_min 0.492
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0030
_database_code_depnum_ccdc_archive 'CCDC 2327702'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;

# start Validation Reply Form
_vrf_PLAT029_fenb_0030           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.600 Why?  
RESPONSE: The generated Alerts A, B and C are the typical high-pressure crystallography warnings. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0030           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        473 Report
RESPONSE: The generated Alerts A, B and C are the typical high-pressure crystallography warnings. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# end Validation Reply Form

_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.0910(10)
_cell_length_b                   21.0910(10)
_cell_length_c                   9.378(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4171.8(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    792
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.8400
_cell_measurement_theta_min      1.7660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.1281
_diffrn_reflns_Laue_measured_fraction_full 0.600
_diffrn_reflns_Laue_measured_fraction_max 0.338
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3566
_diffrn_reflns_point_group_measured_fraction_full 0.600
_diffrn_reflns_point_group_measured_fraction_max 0.338
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.275
_diffrn_reflns_theta_min         1.767
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         820000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.600
_diffrn_measured_fraction_theta_max 0.338
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003739000
_diffrn_orient_matrix_UB_12      0.0072572000
_diffrn_orient_matrix_UB_13      0.0405108000
_diffrn_orient_matrix_UB_21      0.0029107000
_diffrn_orient_matrix_UB_22      0.0178649000
_diffrn_orient_matrix_UB_23      -0.0160454000
_diffrn_orient_matrix_UB_31      -0.0192294000
_diffrn_orient_matrix_UB_32      0.0025583000
_diffrn_orient_matrix_UB_33      -0.0031677000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1177
_reflns_number_total             1782
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1782
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0655
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0787P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2052
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C6 \\sim N5 \\sim N6: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
N3 \\sim C3 \\sim C4 \\sim C5 \\sim N4: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
C2 \\sim N2: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016 within 2A
Uanis(C1) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
4.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C5(H4), C7(H9), C4(H5), C3(H6), C6(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0311(5) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0304(6) Uani 1 2 d S . P . .
O1 O 0.4422(2) 0.3660(2) 0.8003(8) 0.039(2) Uani 1 1 d D . . . .
N3 N 0.4551(2) 0.5131(2) 0.3015(9) 0.0362(17) Uani 1 1 d . U . . .
N4 N 0.4537(2) 0.4650(2) 0.2038(9) 0.0372(17) Uani 1 1 d . U . . .
H3 H 0.468292 0.426578 0.220551 0.045 Uiso 1 1 calc R U . . .
N2 N 0.4821(2) 0.4038(2) 0.4813(9) 0.0372(19) Uani 1 1 d . U . . .
N1 N 0.5157(2) 0.1603(2) 0.0770(10) 0.038(2) Uani 1 1 d . . . . .
N5 N 0.4158(2) 0.5187(2) 0.6092(8) 0.0366(17) Uani 1 1 d . U . . .
N6 N 0.3907(2) 0.4789(2) 0.7062(9) 0.0396(18) Uani 1 1 d . U . . .
H7 H 0.408981 0.443759 0.735606 0.048 Uiso 1 1 calc R U . . .
C2 C 0.4852(3) 0.3513(3) 0.4466(11) 0.037(2) Uani 1 1 d . U . . .
C8 C 0.3336(3) 0.5000(3) 0.7525(11) 0.041(2) Uani 1 1 d . U . . .
H8 H 0.306540 0.479670 0.819274 0.050 Uiso 1 1 calc R U . . .
C1 C 0.5099(3) 0.1893(3) 0.1792(11) 0.034(2) Uani 1 1 d . U . . .
C5 C 0.4280(3) 0.4824(3) 0.0815(11) 0.041(2) Uani 1 1 d . U . . .
H4 H 0.421962 0.456147 0.000337 0.050 Uiso 1 1 calc R U . . .
C7 C 0.3223(3) 0.5568(3) 0.6841(11) 0.043(2) Uani 1 1 d . U . . .
H9 H 0.286468 0.583626 0.694311 0.052 Uiso 1 1 calc R U . . .
C4 C 0.4118(3) 0.5450(3) 0.0923(10) 0.039(2) Uani 1 1 d . U . . .
H5 H 0.392675 0.571164 0.021991 0.047 Uiso 1 1 calc R U . . .
C3 C 0.4296(3) 0.5614(3) 0.2300(10) 0.0365(19) Uani 1 1 d . U . . .
H6 H 0.424277 0.602633 0.268983 0.044 Uiso 1 1 calc R U . . .
C6 C 0.3750(3) 0.5662(3) 0.5964(11) 0.0383(19) Uani 1 1 d . U . . .
H10 H 0.380769 0.601882 0.535868 0.046 Uiso 1 1 calc R U . . .
H2 H 0.440(4) 0.3244(19) 0.766(9) 0.09(3) Uiso 1 1 d D . . . .
H1 H 0.460(4) 0.363(4) 0.893(4) 0.08(3) Uiso 1 1 d 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
Nb1 C2 2.261(7) 16_656 ?
Nb1 C2 2.261(7) 6_554 ?
Nb1 C2 2.261(7) 11_666 ?
Nb1 C2 2.261(7) . ?
Nb1 C1 2.248(9) 16_656 ?
Nb1 C1 2.248(9) . ?
Nb1 C1 2.248(9) 11_666 ?
Nb1 C1 2.248(9) 6_554 ?
Fe1 N3 2.106(8) . ?
Fe1 N3 2.106(8) 9_666 ?
Fe1 N2 2.072(5) . ?
Fe1 N2 2.072(5) 9_666 ?
Fe1 N5 2.087(6) . ?
Fe1 N5 2.087(6) 9_666 ?
O1 H2 0.94(2) . ?
O1 H1 0.95(2) . ?
N3 N4 1.369(9) . ?
N3 C3 1.333(9) . ?
N4 H3 0.8800 . ?
N4 C5 1.321(12) . ?
N2 C2 1.156(8) . ?
N1 C1 1.145(12) . ?
N5 N6 1.346(9) . ?
N5 C6 1.328(7) . ?
N6 H7 0.8800 . ?
N6 C8 1.356(8) . ?
C8 H8 0.9500 . ?
C8 C7 1.378(10) . ?
C5 H4 0.9500 . ?
C5 C4 1.367(8) . ?
C7 H9 0.9500 . ?
C7 C6 1.395(11) . ?
C4 H5 0.9500 . ?
C4 C3 1.389(13) . ?
C3 H6 0.9500 . ?
C6 H10 0.9500 . ?

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
C2 Nb1 C2 145.4(5) 16_656 11_666 ?
C2 Nb1 C2 95.06(15) 11_666 6_554 ?
C2 Nb1 C2 95.06(15) 16_656 6_554 ?
C2 Nb1 C2 95.06(15) 16_656 . ?
C2 Nb1 C2 145.4(5) 6_554 . ?
C2 Nb1 C2 95.06(15) 11_666 . ?
C1 Nb1 C2 76.5(3) 6_554 11_666 ?
C1 Nb1 C2 75.4(3) 16_656 . ?
C1 Nb1 C2 142.5(3) 11_666 11_666 ?
C1 Nb1 C2 75.4(3) . 11_666 ?
C1 Nb1 C2 72.1(3) 6_554 . ?
C1 Nb1 C2 142.5(3) 16_656 16_656 ?
C1 Nb1 C2 72.1(3) 16_656 11_666 ?
C1 Nb1 C2 72.1(3) 11_666 16_656 ?
C1 Nb1 C2 76.5(3) 11_666 . ?
C1 Nb1 C2 75.4(3) 6_554 16_656 ?
C1 Nb1 C2 142.5(3) . . ?
C1 Nb1 C2 72.1(3) . 6_554 ?
C1 Nb1 C2 76.5(3) . 16_656 ?
C1 Nb1 C2 75.4(3) 11_666 6_554 ?
C1 Nb1 C2 142.5(3) 6_554 6_554 ?
C1 Nb1 C2 76.5(3) 16_656 6_554 ?
C1 Nb1 C1 131.9(2) 16_656 . ?
C1 Nb1 C1 131.9(2) 16_656 6_554 ?
C1 Nb1 C1 131.9(2) 11_666 6_554 ?
C1 Nb1 C1 131.9(2) 11_666 . ?
C1 Nb1 C1 70.5(4) 6_554 . ?
C1 Nb1 C1 70.5(4) 16_656 11_666 ?
N3 Fe1 N3 180.0(2) . 9_666 ?
N2 Fe1 N3 88.4(2) 9_666 9_666 ?
N2 Fe1 N3 88.4(2) . . ?
N2 Fe1 N3 91.6(2) 9_666 . ?
N2 Fe1 N3 91.6(2) . 9_666 ?
N2 Fe1 N2 180.0 . 9_666 ?
N2 Fe1 N5 94.1(2) 9_666 9_666 ?
N2 Fe1 N5 85.9(2) 9_666 . ?
N2 Fe1 N5 85.9(2) . 9_666 ?
N2 Fe1 N5 94.1(2) . . ?
N5 Fe1 N3 88.5(2) . 9_666 ?
N5 Fe1 N3 88.5(2) 9_666 . ?
N5 Fe1 N3 91.5(2) . . ?
N5 Fe1 N3 91.5(2) 9_666 9_666 ?
N5 Fe1 N5 180.0 9_666 . ?
H2 O1 H1 105(4) . . ?
N4 N3 Fe1 120.3(4) . . ?
C3 N3 Fe1 136.6(5) . . ?
C3 N3 N4 102.8(8) . . ?
N3 N4 H3 123.7 . . ?
C5 N4 N3 112.6(5) . . ?
C5 N4 H3 123.7 . . ?
C2 N2 Fe1 162.1(6) . . ?
N6 N5 Fe1 123.2(4) . . ?
C6 N5 Fe1 130.6(5) . . ?
C6 N5 N6 106.1(6) . . ?
N5 N6 H7 124.4 . . ?
N5 N6 C8 111.2(5) . . ?
C8 N6 H7 124.4 . . ?
N2 C2 Nb1 175.2(5) . . ?
N6 C8 H8 126.6 . . ?
N6 C8 C7 106.8(7) . . ?
C7 C8 H8 126.6 . . ?
N1 C1 Nb1 177.6(7) . . ?
N4 C5 H4 126.1 . . ?
N4 C5 C4 107.9(8) . . ?
C4 C5 H4 126.1 . . ?
C8 C7 H9 127.4 . . ?
C8 C7 C6 105.2(6) . . ?
C6 C7 H9 127.4 . . ?
C5 C4 H5 128.0 . . ?
C5 C4 C3 104.0(7) . . ?
C3 C4 H5 128.0 . . ?
N3 C3 C4 112.8(6) . . ?
N3 C3 H6 123.6 . . ?
C4 C3 H6 123.6 . . ?
N5 C6 C7 110.8(7) . . ?
N5 C6 H10 124.6 . . ?
C7 C6 H10 124.6 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -175.3(5) . . . . ?
Fe1 N3 C3 C4 173.5(5) . . . . ?
Fe1 N5 N6 C8 -175.1(5) . . . . ?
Fe1 N5 C6 C7 175.2(6) . . . . ?
N3 N4 C5 C4 1.0(9) . . . . ?
N4 N3 C3 C4 0.7(7) . . . . ?
N4 C5 C4 C3 -0.5(8) . . . . ?
N5 N6 C8 C7 -1.3(9) . . . . ?
N6 N5 C6 C7 -1.0(9) . . . . ?
N6 C8 C7 C6 0.6(9) . . . . ?
C8 C7 C6 N5 0.2(10) . . . . ?
C5 C4 C3 N3 -0.2(8) . . . . ?
C3 N3 N4 C5 -1.0(7) . . . . ?
C6 N5 N6 C8 1.4(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   468
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.480
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0038
_database_code_depnum_ccdc_archive 'CCDC 2327431'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0038           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.672 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0038           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        453 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT934_fenb_0038           
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          2 Check
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Monday 22 January 2024 02:25 PM
# end Validation Reply Form

_audit_creation_date             2024-01-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   20.7181(6)
_cell_length_b                   20.7181(6)
_cell_length_c                   9.3075(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3995.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1040
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.8590
_cell_measurement_theta_min      1.7860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.1765
_diffrn_reflns_Laue_measured_fraction_full 0.672
_diffrn_reflns_Laue_measured_fraction_max 0.397
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3742
_diffrn_reflns_point_group_measured_fraction_full 0.672
_diffrn_reflns_point_group_measured_fraction_max 0.397
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.838
_diffrn_reflns_theta_min         1.789
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         1360000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.672
_diffrn_measured_fraction_theta_max 0.397
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004458000
_diffrn_orient_matrix_UB_12      0.0089023000
_diffrn_orient_matrix_UB_13      0.0393111000
_diffrn_orient_matrix_UB_21      0.0058422000
_diffrn_orient_matrix_UB_22      0.0169687000
_diffrn_orient_matrix_UB_23      -0.0186993000
_diffrn_orient_matrix_UB_31      -0.0189010000
_diffrn_orient_matrix_UB_32      0.0049932000
_diffrn_orient_matrix_UB_33      -0.0067438000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1269
_reflns_number_total             1889
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0742
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2162
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 O1-H2
 0.95 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
 N6-H1
 3.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C6(H10), C5(H4), C3(H6), C4(H5), C7(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0209(4) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0245(5) Uani 1 2 d S . P . .
O1 O 0.4456(2) 0.3646(2) 0.7968(9) 0.0374(18) Uani 1 1 d D . . . .
N4 N 0.4564(3) 0.4663(3) 0.2091(10) 0.039(2) Uani 1 1 d . . . . .
H3 H 0.471548 0.427149 0.223784 0.047 Uiso 1 1 calc R U . . .
N3 N 0.4575(3) 0.5135(2) 0.3094(9) 0.0302(18) Uani 1 1 d . . . . .
N2 N 0.4841(2) 0.4070(2) 0.4803(8) 0.0293(19) Uani 1 1 d . . . . .
N5 N 0.4176(2) 0.5165(2) 0.6034(8) 0.030(2) Uani 1 1 d . . . . .
N6 N 0.3926(2) 0.4769(2) 0.7041(10) 0.038(2) Uani 1 1 d D . . . .
H7 H 0.411039 0.440911 0.733229 0.045 Uiso 1 1 calc R U . . .
N1 N 0.5157(3) 0.1577(3) 0.0779(10) 0.037(2) Uani 1 1 d . . . . .
C2 C 0.4853(3) 0.3523(3) 0.4466(10) 0.025(2) Uani 1 1 d . . . . .
C1 C 0.5102(3) 0.1899(3) 0.1782(11) 0.032(2) Uani 1 1 d . . . . .
C8 C 0.3363(4) 0.4993(3) 0.7539(12) 0.044(3) Uani 1 1 d . . . . .
H8 H 0.310024 0.479414 0.824831 0.053 Uiso 1 1 calc R U . . .
C6 C 0.3750(3) 0.5664(3) 0.5921(11) 0.036(2) Uani 1 1 d . . . . .
H10 H 0.380437 0.602409 0.530135 0.043 Uiso 1 1 calc R U . . .
C5 C 0.4302(4) 0.4851(4) 0.0868(13) 0.044(2) Uani 1 1 d . U . . .
H4 H 0.425668 0.459649 0.002575 0.053 Uiso 1 1 calc R U . . .
C3 C 0.4295(3) 0.5638(3) 0.2391(11) 0.039(3) Uani 1 1 d . . . . .
H6 H 0.423258 0.605579 0.278913 0.047 Uiso 1 1 calc R U . . .
C4 C 0.4114(4) 0.5460(4) 0.1023(12) 0.043(3) Uani 1 1 d . . . . .
H5 H 0.389919 0.572018 0.033199 0.051 Uiso 1 1 calc R U . . .
C7 C 0.3231(3) 0.5577(3) 0.6820(12) 0.040(3) Uani 1 1 d . . . . .
H9 H 0.286554 0.584873 0.693114 0.048 Uiso 1 1 calc R U . . .
H2 H 0.435(3) 0.3214(14) 0.780(9) 0.048 Uiso 1 1 d D U . . .
H1 H 0.455(5) 0.366(3) 0.897(4) 0.13(6) Uiso 1 1 d 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
Nb1 C2 2.243(6) 16_656 ?
Nb1 C2 2.243(6) . ?
Nb1 C2 2.243(6) 6_554 ?
Nb1 C2 2.243(6) 11_666 ?
Nb1 C1 2.225(9) 16_656 ?
Nb1 C1 2.225(9) . ?
Nb1 C1 2.225(9) 11_666 ?
Nb1 C1 2.225(9) 6_554 ?
Fe1 N3 2.000(8) 9_666 ?
Fe1 N3 2.000(8) . ?
Fe1 N2 1.963(5) 9_666 ?
Fe1 N2 1.963(5) . ?
Fe1 N5 1.990(6) . ?
Fe1 N5 1.990(6) 9_666 ?
O1 H2 0.94(2) . ?
O1 H1 0.95(2) . ?
N4 H3 0.8800 . ?
N4 N3 1.353(10) . ?
N4 C5 1.320(13) . ?
N3 C3 1.361(9) . ?
N2 C2 1.176(8) . ?
N5 N6 1.349(10) . ?
N5 C6 1.363(8) . ?
N6 H7 0.8800 . ?
N6 C8 1.339(9) . ?
N1 C1 1.153(12) . ?
C8 H8 0.9500 . ?
C8 C7 1.409(12) . ?
C6 H10 0.9500 . ?
C6 C7 1.374(12) . ?
C5 H4 0.9500 . ?
C5 C4 1.329(11) . ?
C3 H6 0.9500 . ?
C3 C4 1.377(13) . ?
C4 H5 0.9500 . ?
C7 H9 0.9500 . ?

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
C2 Nb1 C2 145.5(4) 16_656 11_666 ?
C2 Nb1 C2 95.06(13) 11_666 6_554 ?
C2 Nb1 C2 95.06(13) 16_656 6_554 ?
C2 Nb1 C2 95.06(13) 16_656 . ?
C2 Nb1 C2 145.5(4) 6_554 . ?
C2 Nb1 C2 95.06(13) 11_666 . ?
C1 Nb1 C2 76.6(3) 6_554 11_666 ?
C1 Nb1 C2 75.1(3) 16_656 . ?
C1 Nb1 C2 141.8(3) 11_666 11_666 ?
C1 Nb1 C2 75.1(3) . 11_666 ?
C1 Nb1 C2 72.7(3) 6_554 . ?
C1 Nb1 C2 141.8(3) 16_656 16_656 ?
C1 Nb1 C2 72.7(3) 16_656 11_666 ?
C1 Nb1 C2 72.7(3) 11_666 16_656 ?
C1 Nb1 C2 76.6(3) 11_666 . ?
C1 Nb1 C2 75.1(3) 6_554 16_656 ?
C1 Nb1 C2 141.8(3) . . ?
C1 Nb1 C2 72.7(3) . 6_554 ?
C1 Nb1 C2 76.6(3) . 16_656 ?
C1 Nb1 C2 75.1(3) 11_666 6_554 ?
C1 Nb1 C2 141.8(3) 6_554 6_554 ?
C1 Nb1 C2 76.6(3) 16_656 6_554 ?
C1 Nb1 C1 132.7(3) 16_656 . ?
C1 Nb1 C1 132.7(3) 16_656 6_554 ?
C1 Nb1 C1 132.7(3) 11_666 6_554 ?
C1 Nb1 C1 132.7(3) 11_666 . ?
C1 Nb1 C1 69.2(4) 6_554 . ?
C1 Nb1 C1 69.2(4) 16_656 11_666 ?
N3 Fe1 N3 180.0 . 9_666 ?
N2 Fe1 N3 88.9(3) 9_666 9_666 ?
N2 Fe1 N3 88.9(3) . . ?
N2 Fe1 N3 91.1(3) 9_666 . ?
N2 Fe1 N3 91.1(3) . 9_666 ?
N2 Fe1 N2 180.0 . 9_666 ?
N2 Fe1 N5 86.0(2) 9_666 . ?
N2 Fe1 N5 94.0(2) 9_666 9_666 ?
N2 Fe1 N5 94.0(2) . . ?
N2 Fe1 N5 86.0(2) . 9_666 ?
N5 Fe1 N3 91.6(3) 9_666 9_666 ?
N5 Fe1 N3 91.6(3) . . ?
N5 Fe1 N3 88.4(3) 9_666 . ?
N5 Fe1 N3 88.4(3) . 9_666 ?
N5 Fe1 N5 180.0 . 9_666 ?
H2 O1 H1 105(4) . . ?
N3 N4 H3 123.6 . . ?
C5 N4 H3 123.6 . . ?
C5 N4 N3 112.8(7) . . ?
N4 N3 Fe1 121.2(5) . . ?
N4 N3 C3 102.4(8) . . ?
C3 N3 Fe1 136.2(6) . . ?
C2 N2 Fe1 165.2(6) . . ?
N6 N5 Fe1 124.1(4) . . ?
N6 N5 C6 105.5(6) . . ?
C6 N5 Fe1 130.5(6) . . ?
N5 N6 H7 124.3 . . ?
C8 N6 N5 111.3(6) . . ?
C8 N6 H7 124.3 . . ?
N2 C2 Nb1 173.1(5) . . ?
N1 C1 Nb1 178.7(8) . . ?
N6 C8 H8 126.2 . . ?
N6 C8 C7 107.6(7) . . ?
C7 C8 H8 126.2 . . ?
N5 C6 H10 124.4 . . ?
N5 C6 C7 111.1(8) . . ?
C7 C6 H10 124.4 . . ?
N4 C5 H4 126.0 . . ?
N4 C5 C4 107.9(10) . . ?
C4 C5 H4 126.0 . . ?
N3 C3 H6 124.6 . . ?
N3 C3 C4 110.8(6) . . ?
C4 C3 H6 124.6 . . ?
C5 C4 C3 106.0(8) . . ?
C5 C4 H5 127.0 . . ?
C3 C4 H5 127.0 . . ?
C8 C7 H9 127.8 . . ?
C6 C7 C8 104.5(7) . . ?
C6 C7 H9 127.8 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 175.9(6) . . . . ?
Fe1 N5 N6 C8 -178.9(6) . . . . ?
Fe1 N5 C6 C7 178.5(6) . . . . ?
N4 N3 C3 C4 1.1(8) . . . . ?
N4 C5 C4 C3 1.9(11) . . . . ?
N3 N4 C5 C4 -1.3(11) . . . . ?
N3 C3 C4 C5 -1.9(10) . . . . ?
N5 N6 C8 C7 -0.2(10) . . . . ?
N5 C6 C7 C8 1.2(10) . . . . ?
N6 N5 C6 C7 -1.3(10) . . . . ?
N6 C8 C7 C6 -0.6(10) . . . . ?
C6 N5 N6 C8 0.9(9) . . . . ?
C5 N4 N3 Fe1 -175.7(6) . . . . ?
C5 N4 N3 C3 0.1(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   406
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 15.699
_oxdiff_exptl_absorpt_empirical_full_min 0.580
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0028
_database_code_depnum_ccdc_archive 'CCDC 2326556'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0028           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.642 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0028           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        388 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 05:31 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   20.7576(7)
_cell_length_b                   20.7576(7)
_cell_length_c                   9.3174(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4014.7(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    932
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      18.9300
_cell_measurement_theta_min      1.7860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.642
_diffrn_reflns_Laue_measured_fraction_max 0.358
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3719
_diffrn_reflns_point_group_measured_fraction_full 0.642
_diffrn_reflns_point_group_measured_fraction_max 0.358
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.165
_diffrn_reflns_theta_min         1.787
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         1250000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.642
_diffrn_measured_fraction_theta_max 0.358
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003925000
_diffrn_orient_matrix_UB_12      0.0076792000
_diffrn_orient_matrix_UB_13      0.0404988000
_diffrn_orient_matrix_UB_21      0.0028664000
_diffrn_orient_matrix_UB_22      0.0180580000
_diffrn_orient_matrix_UB_23      -0.0168179000
_diffrn_orient_matrix_UB_31      -0.0195378000
_diffrn_orient_matrix_UB_32      0.0024656000
_diffrn_orient_matrix_UB_33      -0.0032828000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1353
_reflns_number_total             1788
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1788
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      0.949
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0348P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1083
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H2
 0.95 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C3(H6), C6(H10), C5(H4), C8(H8), C7(H9), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0240(3) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0274(3) Uani 1 2 d S . P . .
O1 O 0.44497(14) 0.36425(14) 0.7971(6) 0.0407(13) Uani 1 1 d D . . . .
N3 N 0.45694(13) 0.51395(13) 0.3088(6) 0.0356(14) Uani 1 1 d . . . . .
N2 N 0.48367(13) 0.40659(13) 0.4809(5) 0.0307(13) Uani 1 1 d . . . . .
N4 N 0.45589(15) 0.46623(14) 0.2094(6) 0.0383(16) Uani 1 1 d . . . . .
H3 H 0.471665 0.427449 0.224238 0.046 Uiso 1 1 calc R U . . .
N5 N 0.41755(13) 0.51712(13) 0.6027(5) 0.0324(14) Uani 1 1 d . . . . .
N6 N 0.39306(14) 0.47757(14) 0.7037(6) 0.0392(15) Uani 1 1 d . . . . .
H7 H 0.411670 0.441804 0.732917 0.047 Uiso 1 1 calc R U . . .
N1 N 0.51644(15) 0.15930(15) 0.0768(6) 0.0398(16) Uani 1 1 d . . . . .
C2 C 0.48529(15) 0.35282(15) 0.4479(6) 0.0294(15) Uani 1 1 d . . . . .
C1 C 0.51068(15) 0.18876(16) 0.1807(6) 0.0257(16) Uani 1 1 d . . . . .
C3 C 0.42961(18) 0.56279(17) 0.2389(7) 0.039(2) Uani 1 1 d . . . . .
H6 H 0.423521 0.604326 0.279536 0.047 Uiso 1 1 calc R U . . .
C6 C 0.37528(17) 0.56638(17) 0.5922(7) 0.0404(19) Uani 1 1 d . . . . .
H10 H 0.380507 0.602673 0.531191 0.048 Uiso 1 1 calc R U . . .
C5 C 0.4287(2) 0.48428(19) 0.0882(8) 0.042(2) Uani 1 1 d . . . . .
H4 H 0.422441 0.458128 0.005662 0.050 Uiso 1 1 calc R U . . .
C8 C 0.33642(19) 0.49982(18) 0.7544(7) 0.045(2) Uani 1 1 d . . . . .
H8 H 0.310234 0.480332 0.825828 0.053 Uiso 1 1 calc R U . . .
C7 C 0.32390(19) 0.55675(18) 0.6816(7) 0.044(2) Uani 1 1 d . . . . .
H9 H 0.287119 0.583604 0.691793 0.053 Uiso 1 1 calc R U . . .
C4 C 0.41120(18) 0.54681(18) 0.1023(7) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.390785 0.573541 0.033189 0.052 Uiso 1 1 calc R U . . .
H1 H 0.462(2) 0.356(2) 0.890(3) 0.052(16) Uiso 1 1 d D . . . .
H2 H 0.417(5) 0.330(4) 0.774(11) 0.40(9) Uiso 1 1 d 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
Nb1 C2 2.260(4) . ?
Nb1 C2 2.260(4) 11_666 ?
Nb1 C2 2.260(4) 16_656 ?
Nb1 C2 2.260(4) 6_554 ?
Nb1 C1 2.223(5) . ?
Nb1 C1 2.223(5) 6_554 ?
Nb1 C1 2.223(5) 16_656 ?
Nb1 C1 2.223(5) 11_666 ?
Fe1 N3 2.014(5) . ?
Fe1 N3 2.014(5) 9_666 ?
Fe1 N2 1.976(3) 9_666 ?
Fe1 N2 1.976(3) . ?
Fe1 N5 1.993(3) 9_666 ?
Fe1 N5 1.993(3) . ?
O1 H1 0.95(2) . ?
O1 H2 0.94(2) . ?
N3 N4 1.357(6) . ?
N3 C3 1.332(6) . ?
N2 C2 1.158(5) . ?
N4 H3 0.8800 . ?
N4 C5 1.317(8) . ?
N5 N6 1.348(6) . ?
N5 C6 1.351(4) . ?
N6 H7 0.8800 . ?
N6 C8 1.348(5) . ?
N1 C1 1.151(7) . ?
C3 H6 0.9500 . ?
C3 C4 1.370(8) . ?
C6 H10 0.9500 . ?
C6 C7 1.368(7) . ?
C5 H4 0.9500 . ?
C5 C4 1.354(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.387(7) . ?
C7 H9 0.9500 . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 95.18(8) . 16_656 ?
C2 Nb1 C2 145.0(3) 16_656 11_666 ?
C2 Nb1 C2 95.18(8) . 11_666 ?
C2 Nb1 C2 145.0(3) . 6_554 ?
C2 Nb1 C2 95.18(8) 11_666 6_554 ?
C2 Nb1 C2 95.18(8) 16_656 6_554 ?
C1 Nb1 C2 72.01(18) 11_666 16_656 ?
C1 Nb1 C2 72.01(18) . 6_554 ?
C1 Nb1 C2 142.94(18) 16_656 16_656 ?
C1 Nb1 C2 74.84(15) 6_554 16_656 ?
C1 Nb1 C2 74.84(15) 11_666 6_554 ?
C1 Nb1 C2 142.94(18) . . ?
C1 Nb1 C2 76.84(15) . 16_656 ?
C1 Nb1 C2 74.84(15) 16_656 . ?
C1 Nb1 C2 76.84(15) 16_656 6_554 ?
C1 Nb1 C2 76.84(15) 11_666 . ?
C1 Nb1 C2 142.94(18) 6_554 6_554 ?
C1 Nb1 C2 76.84(15) 6_554 11_666 ?
C1 Nb1 C2 72.02(18) 6_554 . ?
C1 Nb1 C2 72.01(18) 16_656 11_666 ?
C1 Nb1 C2 142.94(18) 11_666 11_666 ?
C1 Nb1 C2 74.84(15) . 11_666 ?
C1 Nb1 C1 71.0(2) . 6_554 ?
C1 Nb1 C1 131.54(14) . 11_666 ?
C1 Nb1 C1 71.0(2) 16_656 11_666 ?
C1 Nb1 C1 131.54(14) 16_656 6_554 ?
C1 Nb1 C1 131.54(14) 11_666 6_554 ?
C1 Nb1 C1 131.54(14) . 16_656 ?
N3 Fe1 N3 180.0 . 9_666 ?
N2 Fe1 N3 90.84(15) . 9_666 ?
N2 Fe1 N3 90.84(15) 9_666 . ?
N2 Fe1 N3 89.16(15) . . ?
N2 Fe1 N3 89.16(15) 9_666 9_666 ?
N2 Fe1 N2 180.0 9_666 . ?
N2 Fe1 N5 94.06(12) . . ?
N2 Fe1 N5 85.94(12) . 9_666 ?
N2 Fe1 N5 85.94(12) 9_666 . ?
N2 Fe1 N5 94.06(12) 9_666 9_666 ?
N5 Fe1 N3 91.03(16) 9_666 9_666 ?
N5 Fe1 N3 91.03(16) . . ?
N5 Fe1 N3 88.97(16) 9_666 . ?
N5 Fe1 N3 88.97(16) . 9_666 ?
N5 Fe1 N5 180.00(15) . 9_666 ?
H1 O1 H2 107(4) . . ?
N4 N3 Fe1 120.4(3) . . ?
C3 N3 Fe1 137.0(3) . . ?
C3 N3 N4 102.4(5) . . ?
C2 N2 Fe1 164.6(4) . . ?
N3 N4 H3 123.7 . . ?
C5 N4 N3 112.6(4) . . ?
C5 N4 H3 123.7 . . ?
N6 N5 Fe1 123.4(2) . . ?
N6 N5 C6 105.5(4) . . ?
C6 N5 Fe1 131.1(3) . . ?
N5 N6 H7 124.3 . . ?
C8 N6 N5 111.4(3) . . ?
C8 N6 H7 124.3 . . ?
N2 C2 Nb1 173.5(3) . . ?
N1 C1 Nb1 177.2(4) . . ?
N3 C3 H6 123.6 . . ?
N3 C3 C4 112.9(4) . . ?
C4 C3 H6 123.6 . . ?
N5 C6 H10 124.7 . . ?
N5 C6 C7 110.6(4) . . ?
C7 C6 H10 124.7 . . ?
N4 C5 H4 126.2 . . ?
N4 C5 C4 107.7(5) . . ?
C4 C5 H4 126.2 . . ?
N6 C8 H8 126.7 . . ?
N6 C8 C7 106.5(4) . . ?
C7 C8 H8 126.7 . . ?
C6 C7 C8 106.0(4) . . ?
C6 C7 H9 127.0 . . ?
C8 C7 H9 127.0 . . ?
C3 C4 H5 127.8 . . ?
C5 C4 C3 104.4(5) . . ?
C5 C4 H5 127.8 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -176.9(3) . . . . ?
Fe1 N3 C3 C4 175.4(3) . . . . ?
Fe1 N5 N6 C8 -179.0(3) . . . . ?
Fe1 N5 C6 C7 178.1(4) . . . . ?
N3 N4 C5 C4 1.1(6) . . . . ?
N3 C3 C4 C5 -0.2(6) . . . . ?
N4 N3 C3 C4 0.8(5) . . . . ?
N4 C5 C4 C3 -0.5(6) . . . . ?
N5 N6 C8 C7 0.1(6) . . . . ?
N5 C6 C7 C8 2.2(6) . . . . ?
N6 N5 C6 C7 -2.1(6) . . . . ?
N6 C8 C7 C6 -1.3(6) . . . . ?
C3 N3 N4 C5 -1.2(5) . . . . ?
C6 N5 N6 C8 1.2(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   403
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.606
_oxdiff_exptl_absorpt_empirical_full_min 0.675
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0039
_database_code_depnum_ccdc_archive 'CCDC 2327450'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0039           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.589 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0039           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        494 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Monday 22 January 2024 03:02 PM
# end Validation Reply Form

_audit_creation_date             2024-01-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.1151(5)
_cell_length_b                   21.1151(5)
_cell_length_c                   9.3661(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4175.9(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    739
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.4620
_cell_measurement_theta_min      2.0850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.589
_diffrn_reflns_Laue_measured_fraction_max 0.334
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3895
_diffrn_reflns_point_group_measured_fraction_full 0.589
_diffrn_reflns_point_group_measured_fraction_max 0.334
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.147
_diffrn_reflns_theta_min         1.767
_diffrn_ambient_temperature      100.00
_diffrn_ambient_pressure         830000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.589
_diffrn_measured_fraction_theta_max 0.334
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0060022000
_diffrn_orient_matrix_UB_12      -0.0004277000
_diffrn_orient_matrix_UB_13      0.0416285000
_diffrn_orient_matrix_UB_21      -0.0174929000
_diffrn_orient_matrix_UB_22      0.0063589000
_diffrn_orient_matrix_UB_23      -0.0124834000
_diffrn_orient_matrix_UB_31      -0.0059274000
_diffrn_orient_matrix_UB_32      -0.0183461000
_diffrn_orient_matrix_UB_33      -0.0053134000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1185
_reflns_number_total             1737
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1737
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0543
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0582P)²+3.5958P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1473
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 O1-H2
 0.95 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
 H2-N6
 3.3 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C3(H6), C4(H5), C6(H10), C8(H8), C5(H4), C7(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.250000 0.375000 0.0373(5) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0403(7) Uani 1 2 d S . P . .
O1 O 0.44190(17) 0.36564(18) 0.8020(8) 0.049(2) Uani 1 1 d D . . . .
N3 N 0.45542(19) 0.51305(18) 0.3029(9) 0.046(3) Uani 1 1 d . . . . .
N2 N 0.4825(2) 0.40330(19) 0.4816(9) 0.046(3) Uani 1 1 d . . . . .
N1 N 0.5159(2) 0.1603(2) 0.0821(10) 0.051(3) Uani 1 1 d . . . . .
N5 N 0.4156(2) 0.51746(19) 0.6063(8) 0.045(3) Uani 1 1 d . . . . .
N4 N 0.4534(2) 0.4654(2) 0.2068(11) 0.056(3) Uani 1 1 d . . . . .
H3 H 0.467403 0.426882 0.224158 0.067 Uiso 1 1 calc R U . . .
N6 N 0.3908(2) 0.4784(2) 0.7066(10) 0.058(3) Uani 1 1 d D . . . .
H7 H 0.408949 0.443413 0.736773 0.069 Uiso 1 1 calc R U . . .
C1 C 0.5100(3) 0.1899(2) 0.1787(12) 0.051(4) Uani 1 1 d . . . . .
C2 C 0.4855(2) 0.3510(2) 0.4479(11) 0.039(3) Uani 1 1 d . . . . .
C3 C 0.4299(3) 0.5617(3) 0.2303(13) 0.059(4) Uani 1 1 d . . . . .
H6 H 0.425030 0.603066 0.268346 0.070 Uiso 1 1 calc R U . . .
C4 C 0.4119(3) 0.5449(3) 0.0961(12) 0.053(4) Uani 1 1 d . . . . .
H5 H 0.392192 0.570945 0.026369 0.064 Uiso 1 1 calc R U . . .
C6 C 0.3744(3) 0.5655(2) 0.5960(12) 0.053(4) Uani 1 1 d . . . . .
H10 H 0.380392 0.601528 0.536901 0.064 Uiso 1 1 calc R U . . .
C8 C 0.3348(3) 0.5002(3) 0.7540(12) 0.064(4) Uani 1 1 d . . . . .
H8 H 0.308534 0.480946 0.823996 0.077 Uiso 1 1 calc R U . . .
C5 C 0.4281(3) 0.4829(3) 0.0834(13) 0.057(4) Uani 1 1 d . . . . .
H4 H 0.422459 0.457015 0.001420 0.069 Uiso 1 1 calc R U . . .
C7 C 0.3227(3) 0.5561(3) 0.6809(12) 0.060(4) Uani 1 1 d . . . . .
H9 H 0.286217 0.582238 0.688417 0.071 Uiso 1 1 calc R U . . .
H1 H 0.467(3) 0.357(3) 0.885(5) 0.071 Uiso 1 1 d D U . . .
H2 H 0.414(4) 0.330(3) 0.801(17) 0.53(17) Uiso 1 1 d 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
Nb1 C1 2.244(10) 16_656 ?
Nb1 C1 2.244(10) 6_554 ?
Nb1 C1 2.244(10) 11_666 ?
Nb1 C1 2.244(10) . ?
Nb1 C2 2.261(6) 16_656 ?
Nb1 C2 2.261(6) 6_554 ?
Nb1 C2 2.261(6) 11_666 ?
Nb1 C2 2.261(6) . ?
Fe1 N3 2.090(8) . ?
Fe1 N3 2.090(8) 9_666 ?
Fe1 N2 2.082(4) . ?
Fe1 N2 2.082(4) 9_666 ?
Fe1 N5 2.075(5) . ?
Fe1 N5 2.074(5) 9_666 ?
O1 H1 0.96(2) . ?
O1 H2 0.95(2) . ?
N3 N4 1.351(10) . ?
N3 C3 1.344(9) . ?
N2 C2 1.150(7) . ?
N1 C1 1.107(13) . ?
N5 N6 1.355(10) . ?
N5 C6 1.339(6) . ?
N4 H3 0.8800 . ?
N4 C5 1.326(14) . ?
N6 H7 0.8800 . ?
N6 C8 1.343(8) . ?
C3 H6 0.9500 . ?
C3 C4 1.359(15) . ?
C4 H5 0.9500 . ?
C4 C5 1.358(8) . ?
C6 H10 0.9500 . ?
C6 C7 1.365(10) . ?
C8 H8 0.9500 . ?
C8 C7 1.389(11) . ?
C5 H4 0.9500 . ?
C7 H9 0.9500 . ?

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
C1 Nb1 C1 69.9(4) 16_656 11_666 ?
C1 Nb1 C1 132.2(3) 11_666 . ?
C1 Nb1 C1 132.2(3) 16_656 . ?
C1 Nb1 C1 132.2(3) 16_656 6_554 ?
C1 Nb1 C1 132.2(3) 11_666 6_554 ?
C1 Nb1 C1 69.9(4) 6_554 . ?
C1 Nb1 C2 76.4(2) 6_554 11_666 ?
C1 Nb1 C2 142.5(3) . . ?
C1 Nb1 C2 76.4(2) 11_666 . ?
C1 Nb1 C2 76.4(2) 16_656 6_554 ?
C1 Nb1 C2 142.5(3) 11_666 11_666 ?
C1 Nb1 C2 142.5(3) 6_554 6_554 ?
C1 Nb1 C2 75.0(3) . 11_666 ?
C1 Nb1 C2 142.5(3) 16_656 16_656 ?
C1 Nb1 C2 75.0(3) 11_666 6_554 ?
C1 Nb1 C2 72.6(3) 11_666 16_656 ?
C1 Nb1 C2 75.0(3) 16_656 . ?
C1 Nb1 C2 75.0(3) 6_554 16_656 ?
C1 Nb1 C2 72.6(3) 6_554 . ?
C1 Nb1 C2 76.4(2) . 16_656 ?
C1 Nb1 C2 72.6(3) 16_656 11_666 ?
C1 Nb1 C2 72.6(3) . 6_554 ?
C2 Nb1 C2 95.24(14) 16_656 6_554 ?
C2 Nb1 C2 144.8(5) 16_656 11_666 ?
C2 Nb1 C2 144.8(5) 6_554 . ?
C2 Nb1 C2 95.24(14) 11_666 6_554 ?
C2 Nb1 C2 95.24(14) 11_666 . ?
C2 Nb1 C2 95.24(14) 16_656 . ?
N3 Fe1 N3 180.00(19) 9_666 . ?
N2 Fe1 N3 88.6(2) 9_666 9_666 ?
N2 Fe1 N3 88.6(2) . . ?
N2 Fe1 N3 91.4(2) 9_666 . ?
N2 Fe1 N3 91.4(2) . 9_666 ?
N2 Fe1 N2 180.0 . 9_666 ?
N5 Fe1 N3 89.2(2) . 9_666 ?
N5 Fe1 N3 90.8(2) . . ?
N5 Fe1 N3 90.8(2) 9_666 9_666 ?
N5 Fe1 N3 89.2(2) 9_666 . ?
N5 Fe1 N2 86.47(19) 9_666 . ?
N5 Fe1 N2 86.47(19) . 9_666 ?
N5 Fe1 N2 93.53(19) . . ?
N5 Fe1 N2 93.53(19) 9_666 9_666 ?
N5 Fe1 N5 180.0 9_666 . ?
H1 O1 H2 102(4) . . ?
N4 N3 Fe1 120.3(4) . . ?
C3 N3 Fe1 136.7(6) . . ?
C3 N3 N4 102.6(8) . . ?
C2 N2 Fe1 162.6(6) . . ?
N6 N5 Fe1 123.9(3) . . ?
C6 N5 Fe1 131.1(6) . . ?
C6 N5 N6 105.0(6) . . ?
N3 N4 H3 123.7 . . ?
C5 N4 N3 112.7(5) . . ?
C5 N4 H3 123.7 . . ?
N5 N6 H7 124.4 . . ?
C8 N6 N5 111.2(5) . . ?
C8 N6 H7 124.4 . . ?
N1 C1 Nb1 178.8(5) . . ?
N2 C2 Nb1 175.1(5) . . ?
N3 C3 H6 123.8 . . ?
N3 C3 C4 112.4(6) . . ?
C4 C3 H6 123.8 . . ?
C3 C4 H5 127.4 . . ?
C5 C4 C3 105.2(8) . . ?
C5 C4 H5 127.4 . . ?
N5 C6 H10 124.2 . . ?
N5 C6 C7 111.6(7) . . ?
C7 C6 H10 124.2 . . ?
N6 C8 H8 126.6 . . ?
N6 C8 C7 106.8(7) . . ?
C7 C8 H8 126.6 . . ?
N4 C5 C4 107.1(9) . . ?
N4 C5 H4 126.5 . . ?
C4 C5 H4 126.5 . . ?
C6 C7 C8 105.2(5) . . ?
C6 C7 H9 127.4 . . ?
C8 C7 H9 127.4 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 N4 C5 -174.8(5) . . . . ?
Fe1 N3 C3 C4 174.0(5) . . . . ?
Fe1 N5 N6 C8 -177.8(6) . . . . ?
Fe1 N5 C6 C7 176.4(6) . . . . ?
N3 N4 C5 C4 -0.4(9) . . . . ?
N3 C3 C4 C5 -1.2(9) . . . . ?
N5 N6 C8 C7 0.0(10) . . . . ?
N5 C6 C7 C8 3.4(10) . . . . ?
N4 N3 C3 C4 1.0(8) . . . . ?
N6 N5 C6 C7 -3.4(10) . . . . ?
N6 C8 C7 C6 -2.0(10) . . . . ?
C3 N3 N4 C5 -0.4(8) . . . . ?
C3 C4 C5 N4 0.9(9) . . . . ?
C6 N5 N6 C8 2.1(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   572
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.999
_oxdiff_exptl_absorpt_empirical_full_min 0.253
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fenb_0016
_database_code_depnum_ccdc_archive 'CCDC 2326517'
loop_
_audit_author_name
_audit_author_address
'Gabriela Handzlik'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_fenb_0016           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.659 Why?
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
_vrf_PLAT911_fenb_0016           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        497 Report
RESPONSE: The generated alert is typical high pressure crystallography warning. Due to the construction of the diamond anvil cell access to the sample crystal is limited, which affects data collection.
;
# Added during the CSD deposition process: Thursday 18 January 2024 04:12 PM
# end Validation Reply Form

_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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'
Fe Fe 0.1482 0.3017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0016 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.0343 1.6958 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0014 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.4699(3)
_cell_length_b                   21.4699(3)
_cell_length_c                   9.4581(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4359.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1159
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.7080
_cell_measurement_theta_min      1.7410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.659
_diffrn_reflns_Laue_measured_fraction_max 0.385
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4499
_diffrn_reflns_point_group_measured_fraction_full 0.659
_diffrn_reflns_point_group_measured_fraction_max 0.385
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         19.968
_diffrn_reflns_theta_min         1.744
_diffrn_ambient_temperature      5.00
_diffrn_ambient_pressure         280000
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.659
_diffrn_measured_fraction_theta_max 0.385
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003898000
_diffrn_orient_matrix_UB_12      -0.0080440000
_diffrn_orient_matrix_UB_13      -0.0392836000
_diffrn_orient_matrix_UB_21      0.0023323000
_diffrn_orient_matrix_UB_22      -0.0172112000
_diffrn_orient_matrix_UB_23      0.0180512000
_diffrn_orient_matrix_UB_31      -0.0189634000
_diffrn_orient_matrix_UB_32      -0.0019567000
_diffrn_orient_matrix_UB_33      0.0030290000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_source                   'ESRF ID15B'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1708
_reflns_number_total             2033
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2033
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0408
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1078
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 H2-O1
 0.95 with sigma of 0.02
 H2-H1
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C6(H10), C8(H8), C7(H9), C3(H6), C5(H4), C4(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nb1 Nb 0.500000 0.750000 0.625000 0.0160(2) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0186(3) Uani 1 2 d S . P . .
O1 O 0.44030(10) 0.63432(10) 0.1956(4) 0.0253(9) Uani 1 1 d D . . . .
N2 N 0.48345(11) 0.59895(11) 0.5204(4) 0.0230(10) Uani 1 1 d . . . . .
N4 N 0.45278(11) 0.53539(10) 0.7976(4) 0.0239(10) Uani 1 1 d . . . . .
H3 H 0.466080 0.573255 0.778678 0.029 Uiso 1 1 calc R U . . .
N3 N 0.45486(10) 0.48772(10) 0.7036(4) 0.0217(9) Uani 1 1 d . . . . .
N5 N 0.41465(10) 0.48319(10) 0.3869(4) 0.0231(10) Uani 1 1 d . . . . .
N1 N 0.51439(11) 0.83933(11) 0.9200(5) 0.0251(11) Uani 1 1 d . . . . .
N6 N 0.38990(10) 0.52265(11) 0.2909(4) 0.0229(10) Uani 1 1 d . . . . .
H7 H 0.407497 0.557622 0.263382 0.028 Uiso 1 1 calc R U . . .
C2 C 0.48665(12) 0.65027(12) 0.5559(5) 0.0209(11) Uani 1 1 d . . . . .
C1 C 0.50938(12) 0.80988(12) 0.8198(5) 0.0203(11) Uani 1 1 d . . . . .
C6 C 0.37429(13) 0.43629(12) 0.3982(5) 0.0242(12) Uani 1 1 d . . . . .
H10 H 0.379737 0.401152 0.457946 0.029 Uiso 1 1 calc R U . . .
C8 C 0.33458(13) 0.50142(13) 0.2428(5) 0.0264(13) Uani 1 1 d . . . . .
H8 H 0.308623 0.521256 0.175054 0.032 Uiso 1 1 calc R U . . .
C7 C 0.32273(13) 0.44579(13) 0.3099(5) 0.0258(12) Uani 1 1 d . . . . .
H9 H 0.287396 0.419607 0.298826 0.031 Uiso 1 1 calc R U . . .
C3 C 0.43060(13) 0.43981(13) 0.7746(5) 0.0254(12) Uani 1 1 d . . . . .
H6 H 0.425730 0.399190 0.736337 0.030 Uiso 1 1 calc R U . . .
C5 C 0.42855(14) 0.51886(14) 0.9213(5) 0.0268(13) Uani 1 1 d . . . . .
H4 H 0.422717 0.544809 1.001538 0.032 Uiso 1 1 calc R U . . .
C4 C 0.41342(13) 0.45621(13) 0.9101(5) 0.0288(13) Uani 1 1 d . . . . .
H5 H 0.395238 0.430324 0.980345 0.035 Uiso 1 1 calc R U . . .
H2 H 0.439(2) 0.6691(16) 0.250(4) 0.070(16) Uiso 1 1 d D . . . .
H1 H 0.4535(17) 0.6429(17) 0.103(2) 0.032(11) Uiso 1 1 d 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
Nb1 C2 2.257(3) . ?
Nb1 C2 2.257(3) 15_566 ?
Nb1 C2 2.257(3) 12_767 ?
Nb1 C2 2.257(3) 6_564 ?
Nb1 C1 2.256(4) . ?
Nb1 C1 2.256(4) 6_564 ?
Nb1 C1 2.256(4) 12_767 ?
Nb1 C1 2.256(4) 15_566 ?
Fe1 N2 2.163(2) 9_666 ?
Fe1 N2 2.163(2) . ?
Fe1 N3 2.172(4) 9_666 ?
Fe1 N3 2.172(4) . ?
Fe1 N5 2.152(3) 9_666 ?
Fe1 N5 2.152(3) . ?
O1 H2 0.907(18) . ?
O1 H1 0.937(19) . ?
N2 C2 1.154(4) . ?
N4 H3 0.8800 . ?
N4 N3 1.356(4) . ?
N4 C5 1.329(6) . ?
N3 C3 1.334(4) . ?
N5 N6 1.350(4) . ?
N5 C6 1.333(3) . ?
N1 C1 1.144(6) . ?
N6 H7 0.8800 . ?
N6 C8 1.351(4) . ?
C6 H10 0.9500 . ?
C6 C7 1.401(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.376(5) . ?
C7 H9 0.9500 . ?
C3 H6 0.9500 . ?
C3 C4 1.379(6) . ?
C5 H4 0.9500 . ?
C5 C4 1.388(4) . ?
C4 H5 0.9500 . ?

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
C2 Nb1 C2 94.81(7) . 12_767 ?
C2 Nb1 C2 94.81(7) 6_564 15_566 ?
C2 Nb1 C2 146.3(2) 12_767 15_566 ?
C2 Nb1 C2 146.3(2) . 6_564 ?
C2 Nb1 C2 94.81(7) . 15_566 ?
C2 Nb1 C2 94.81(7) 12_767 6_564 ?
C1 Nb1 C2 142.05(15) . . ?
C1 Nb1 C2 71.61(15) . 6_564 ?
C1 Nb1 C2 77.04(12) . 15_566 ?
C1 Nb1 C2 77.04(12) 12_767 . ?
C1 Nb1 C2 77.04(12) 15_566 6_564 ?
C1 Nb1 C2 75.59(12) 15_566 . ?
C1 Nb1 C2 75.60(12) 6_564 15_566 ?
C1 Nb1 C2 71.61(15) 6_564 . ?
C1 Nb1 C2 75.60(12) 12_767 6_564 ?
C1 Nb1 C2 75.59(12) . 12_767 ?
C1 Nb1 C2 142.05(15) 6_564 6_564 ?
C1 Nb1 C2 142.05(15) 12_767 12_767 ?
C1 Nb1 C2 71.61(15) 12_767 15_566 ?
C1 Nb1 C2 71.61(15) 15_566 12_767 ?
C1 Nb1 C2 77.04(12) 6_564 12_767 ?
C1 Nb1 C2 142.05(15) 15_566 15_566 ?
C1 Nb1 C1 131.85(12) . 15_566 ?
C1 Nb1 C1 131.85(12) 12_767 6_564 ?
C1 Nb1 C1 70.47(19) . 6_564 ?
C1 Nb1 C1 131.85(12) 15_566 6_564 ?
C1 Nb1 C1 70.47(19) 12_767 15_566 ?
C1 Nb1 C1 131.85(12) . 12_767 ?
N2 Fe1 N2 180.0 . 9_666 ?
N2 Fe1 N3 91.91(11) 9_666 . ?
N2 Fe1 N3 88.09(11) 9_666 9_666 ?
N2 Fe1 N3 88.09(11) . . ?
N2 Fe1 N3 91.91(11) . 9_666 ?
N3 Fe1 N3 180.0 . 9_666 ?
N5 Fe1 N2 86.03(9) 9_666 . ?
N5 Fe1 N2 93.97(9) 9_666 9_666 ?
N5 Fe1 N2 93.97(9) . . ?
N5 Fe1 N2 86.03(9) . 9_666 ?
N5 Fe1 N3 87.68(12) 9_666 . ?
N5 Fe1 N3 87.68(12) . 9_666 ?
N5 Fe1 N3 92.32(12) . . ?
N5 Fe1 N3 92.32(12) 9_666 9_666 ?
N5 Fe1 N5 180.0 9_666 . ?
H2 O1 H1 112(3) . . ?
C2 N2 Fe1 162.6(3) . . ?
N3 N4 H3 123.6 . . ?
C5 N4 H3 123.6 . . ?
C5 N4 N3 112.9(3) . . ?
N4 N3 Fe1 120.3(2) . . ?
C3 N3 Fe1 135.6(3) . . ?
C3 N3 N4 103.8(4) . . ?
N6 N5 Fe1 124.32(17) . . ?
C6 N5 Fe1 129.8(3) . . ?
C6 N5 N6 105.8(3) . . ?
N5 N6 H7 124.4 . . ?
N5 N6 C8 111.1(3) . . ?
C8 N6 H7 124.4 . . ?
N2 C2 Nb1 176.1(2) . . ?
N1 C1 Nb1 178.8(3) . . ?
N5 C6 H10 124.6 . . ?
N5 C6 C7 110.8(3) . . ?
C7 C6 H10 124.6 . . ?
N6 C8 H8 126.3 . . ?
N6 C8 C7 107.4(3) . . ?
C7 C8 H8 126.3 . . ?
C6 C7 H9 127.6 . . ?
C8 C7 C6 104.8(3) . . ?
C8 C7 H9 127.6 . . ?
N3 C3 H6 124.0 . . ?
N3 C3 C4 112.0(3) . . ?
C4 C3 H6 124.0 . . ?
N4 C5 H4 126.8 . . ?
N4 C5 C4 106.5(4) . . ?
C4 C5 H4 126.8 . . ?
C3 C4 C5 104.8(3) . . ?
C3 C4 H5 127.6 . . ?
C5 C4 H5 127.6 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 173.1(2) . . . . ?
Fe1 N5 N6 C8 -176.7(3) . . . . ?
Fe1 N5 C6 C7 176.3(3) . . . . ?
N4 N3 C3 C4 0.0(4) . . . . ?
N4 C5 C4 C3 -0.1(4) . . . . ?
N3 N4 C5 C4 0.1(4) . . . . ?
N3 C3 C4 C5 0.0(4) . . . . ?
N5 N6 C8 C7 -0.1(5) . . . . ?
N5 C6 C7 C8 0.6(4) . . . . ?
N6 N5 C6 C7 -0.6(4) . . . . ?
N6 C8 C7 C6 -0.3(4) . . . . ?
C6 N5 N6 C8 0.4(4) . . . . ?
C5 N4 N3 Fe1 -174.4(2) . . . . ?
C5 N4 N3 C3 -0.1(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   295
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.691
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
