# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_fe2w_200k_0m
_database_code_depnum_ccdc_archive 'CCDC 2240344'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2023-02-07 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_audit_creation_date             2022-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H32 Fe2 N24 W, 4(H2 O)'
_chemical_formula_sum            'C56 H40 Fe2 N24 O4 W'
_chemical_formula_weight         1408.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-y-1/4, x-1/4, -z-1/4'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z-1/4'
'-y+1/4, x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'

_cell_length_a                   19.7947(3)
_cell_length_b                   19.7947(3)
_cell_length_c                   16.0477(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6288.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   0.835
_shelx_estimated_absorpt_T_min   0.603
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0590 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8856.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30445
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.858
_diffrn_reflns_theta_min         2.628
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3458
_reflns_number_total             3744
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0201
_refine_ls_restrained_S_all      1.095
_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)+(0.0274P)²+8.2190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0535
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 O1-H1A
 0.95 with sigma of 0.02
 O1-H1B
 0.95 with sigma of 0.02
 H1A-H1B
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C13(H13), C12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
W1 W 0.5000 0.7500 0.6250 0.01676(5) Uani 1 4 d S T P . .
O1 O 0.4224(2) 0.9264(2) 0.9053(2) 0.1265(15) Uani 1 1 d D . . . .
H1A H 0.450(2) 0.926(3) 0.956(2) 0.152 Uiso 1 1 d D U . . .
H1B H 0.438(3) 0.891(2) 0.869(3) 0.152 Uiso 1 1 d D U . . .
N1 N 0.48987(11) 0.59432(9) 0.55576(12) 0.0377(5) Uani 1 1 d . . . . .
C1 C 0.49306(11) 0.64807(10) 0.58336(13) 0.0263(4) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.03312(10) Uani 1 2 d S . P . .
C2 C 0.50287(11) 0.81602(11) 0.73310(13) 0.0286(4) Uani 1 1 d . . . . .
N3 N 0.49382(12) 0.45210(10) 0.62645(12) 0.0398(5) Uani 1 1 d . . . . .
C3 C 0.50712(16) 0.48839(13) 0.69478(16) 0.0463(6) Uani 1 1 d . . . . .
H3 H 0.5225 0.5335 0.6877 0.056 Uiso 1 1 calc R U . . .
N4 N 0.4637(2) 0.35202(19) 0.93445(19) 0.0960(12) Uani 1 1 d . . . . .
C4 C 0.49991(17) 0.46455(15) 0.77447(17) 0.0519(7) Uani 1 1 d . . . . .
H4 H 0.5101 0.4922 0.8212 0.062 Uiso 1 1 calc R U . . .
C5 C 0.47739(17) 0.39894(15) 0.78463(17) 0.0529(7) Uani 1 1 d . . . . .
N5 N 0.38708(12) 0.49360(11) 0.48176(14) 0.0461(5) Uani 1 1 d . . . . .
N2 N 0.50343(13) 0.85172(11) 0.78936(14) 0.0462(5) Uani 1 1 d . . . . .
C6 C 0.4636(2) 0.35985(15) 0.71572(19) 0.0668(10) Uani 1 1 d . . . . .
H6 H 0.4481 0.3146 0.7213 0.080 Uiso 1 1 calc R U . . .
N6 N 0.1198(2) 0.4841(3) 0.4233(3) 0.1259(17) Uani 1 1 d . . . . .
C7 C 0.4730(2) 0.38855(14) 0.63834(17) 0.0590(9) Uani 1 1 d . . . . .
H7 H 0.4641 0.3616 0.5906 0.071 Uiso 1 1 calc R U . . .
C8 C 0.4691(2) 0.37210(19) 0.8682(2) 0.0691(10) Uani 1 1 d . . . . .
C9 C 0.3507(2) 0.54921(17) 0.4696(3) 0.0748(11) Uani 1 1 d . . . . .
H9 H 0.3733 0.5916 0.4713 0.090 Uiso 1 1 calc R U . . .
C10 C 0.2821(2) 0.5489(2) 0.4547(3) 0.0845(12) Uani 1 1 d . . . . .
H10 H 0.2585 0.5901 0.4461 0.101 Uiso 1 1 calc R U . . .
C11 C 0.24830(18) 0.48862(19) 0.4525(2) 0.0636(8) Uani 1 1 d . . . . .
C13 C 0.35284(17) 0.43530(16) 0.4781(2) 0.0648(9) Uani 1 1 d . . . . .
H13 H 0.3774 0.3945 0.4854 0.078 Uiso 1 1 calc R U . . .
C14 C 0.1764(2) 0.4862(2) 0.4365(3) 0.0871(13) Uani 1 1 d . . . . .
C12 C 0.28428(19) 0.43082(18) 0.4645(3) 0.0737(10) Uani 1 1 d . . . . .
H12 H 0.2625 0.3881 0.4636 0.088 Uiso 1 1 calc R 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
W1 C1 2.130(2) 15_656 ?
W1 C1 2.130(2) 10_577 ?
W1 C1 2.130(2) 4_665 ?
W1 C1 2.130(2) . ?
W1 C2 2.173(2) 10_577 ?
W1 C2 2.173(2) . ?
W1 C2 2.173(2) 4_665 ?
W1 C2 2.173(2) 15_656 ?
O1 H1A 0.982(19) . ?
O1 H1B 0.969(19) . ?
N1 C1 1.154(3) . ?
N1 Fe1 2.0800(18) . ?
Fe1 N1 2.0801(18) 9_666 ?
Fe1 N3 2.2431(19) . ?
Fe1 N3 2.2430(19) 9_666 ?
Fe1 N5 2.258(2) 9_666 ?
Fe1 N5 2.258(2) . ?
C2 N2 1.147(3) . ?
N3 C3 1.337(3) . ?
N3 C7 1.338(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(4) . ?
N4 C8 1.139(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(4) . ?
C5 C6 1.377(4) . ?
C5 C8 1.452(4) . ?
N5 C9 1.330(4) . ?
N5 C13 1.340(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(4) . ?
N6 C14 1.142(5) . ?
C7 H7 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.379(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.368(5) . ?
C11 C14 1.446(5) . ?
C11 C12 1.362(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.377(5) . ?
C12 H12 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 W1 C1 95.65(3) 15_656 4_665 ?
C1 W1 C1 143.44(11) 4_665 . ?
C1 W1 C1 95.65(3) 15_656 . ?
C1 W1 C1 143.44(11) 15_656 10_577 ?
C1 W1 C1 95.65(3) 4_665 10_577 ?
C1 W1 C1 95.65(3) 10_577 . ?
C1 W1 C2 145.28(8) 10_577 10_577 ?
C1 W1 C2 145.28(8) . . ?
C1 W1 C2 71.27(8) 4_665 . ?
C1 W1 C2 145.28(8) 4_665 4_665 ?
C1 W1 C2 74.66(8) 4_665 10_577 ?
C1 W1 C2 71.28(8) . 4_665 ?
C1 W1 C2 74.66(8) 15_656 4_665 ?
C1 W1 C2 145.28(8) 15_656 15_656 ?
C1 W1 C2 76.33(8) 10_577 4_665 ?
C1 W1 C2 76.33(8) 4_665 15_656 ?
C1 W1 C2 76.33(8) 15_656 . ?
C1 W1 C2 71.27(8) 10_577 15_656 ?
C1 W1 C2 74.66(8) 10_577 . ?
C1 W1 C2 74.66(8) . 15_656 ?
C1 W1 C2 71.27(8) 15_656 10_577 ?
C1 W1 C2 76.32(8) . 10_577 ?
C2 W1 C2 129.61(7) 10_577 4_665 ?
C2 W1 C2 74.03(11) 15_656 10_577 ?
C2 W1 C2 129.61(7) 10_577 . ?
C2 W1 C2 74.03(11) 4_665 . ?
C2 W1 C2 129.61(7) 15_656 . ?
C2 W1 C2 129.61(7) 15_656 4_665 ?
H1A O1 H1B 108(3) . . ?
C1 N1 Fe1 170.8(2) . . ?
N1 C1 W1 175.69(19) . . ?
N1 Fe1 N1 180.0 . 9_666 ?
N1 Fe1 N3 90.86(7) . 9_666 ?
N1 Fe1 N3 90.86(7) 9_666 . ?
N1 Fe1 N3 89.14(7) . . ?
N1 Fe1 N3 89.13(7) 9_666 9_666 ?
N1 Fe1 N5 90.62(8) . . ?
N1 Fe1 N5 89.38(8) . 9_666 ?
N1 Fe1 N5 89.38(8) 9_666 . ?
N1 Fe1 N5 90.62(8) 9_666 9_666 ?
N3 Fe1 N3 180.0 9_666 . ?
N3 Fe1 N5 87.73(9) . 9_666 ?
N3 Fe1 N5 92.27(9) . . ?
N3 Fe1 N5 87.73(9) 9_666 . ?
N3 Fe1 N5 92.27(9) 9_666 9_666 ?
N5 Fe1 N5 180.0 . 9_666 ?
N2 C2 W1 178.6(2) . . ?
C3 N3 Fe1 120.27(17) . . ?
C3 N3 C7 116.7(2) . . ?
C7 N3 Fe1 122.92(17) . . ?
N3 C3 H3 118.0 . . ?
N3 C3 C4 124.0(3) . . ?
C4 C3 H3 118.0 . . ?
C3 C4 H4 121.1 . . ?
C3 C4 C5 117.8(3) . . ?
C5 C4 H4 121.1 . . ?
C4 C5 C8 119.3(3) . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 C8 120.9(3) . . ?
C9 N5 Fe1 120.6(2) . . ?
C9 N5 C13 115.7(3) . . ?
C13 N5 Fe1 123.7(2) . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.7(3) . . ?
C7 C6 H6 121.1 . . ?
N3 C7 C6 123.9(3) . . ?
N3 C7 H7 118.0 . . ?
C6 C7 H7 118.0 . . ?
N4 C8 C5 178.4(5) . . ?
N5 C9 H9 118.2 . . ?
N5 C9 C10 123.7(3) . . ?
C10 C9 H9 118.2 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C14 120.9(4) . . ?
C12 C11 C10 118.2(3) . . ?
C12 C11 C14 120.8(4) . . ?
N5 C13 H13 117.9 . . ?
N5 C13 C12 124.1(3) . . ?
C12 C13 H13 117.9 . . ?
N6 C14 C11 179.5(6) . . ?
C11 C12 C13 118.9(3) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?

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 175.2(2) . . . . ?
Fe1 N3 C7 C6 -174.6(3) . . . . ?
Fe1 N5 C9 C10 177.3(4) . . . . ?
Fe1 N5 C13 C12 -178.0(3) . . . . ?
N3 C3 C4 C5 -0.1(5) . . . . ?
C3 N3 C7 C6 1.2(5) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C3 C4 C5 C8 -179.9(3) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C5 C6 C7 N3 -0.9(6) . . . . ?
N5 C9 C10 C11 0.4(7) . . . . ?
N5 C13 C12 C11 1.1(6) . . . . ?
C7 N3 C3 C4 -0.8(5) . . . . ?
C8 C5 C6 C7 -179.6(4) . . . . ?
C9 N5 C13 C12 -1.2(6) . . . . ?
C9 C10 C11 C14 -179.6(4) . . . . ?
C9 C10 C11 C12 -0.6(7) . . . . ?
C10 C11 C12 C13 -0.2(6) . . . . ?
C13 N5 C9 C10 0.4(6) . . . . ?
C14 C11 C12 C13 178.9(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_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_fe2wanh_80k_0m
_database_code_depnum_ccdc_archive 'CCDC 2240347'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2023-02-07 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_fe2wanh_80k_0m      
;
PROBLEM: NonSolvent   Resd 1  N   Ueq(max)/Ueq(min) Range        6.6 Ratio
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
_vrf_PLAT972_fe2wanh_80k_0m      
;
PROBLEM: Check Calcd Resid. Dens.  2.45Ang From N6             -3.23 eA-3
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
_vrf_PLAT973_fe2wanh_80k_0m      
;
PROBLEM: Check Calcd Positive Resid. Density on      W001       1.58 eA-3
RESPONSE: The small, unaccounted for electron density near tungsten is due to the anharmonic vibrations of this heavy metal ion.
;
# Added during the CSD deposition process: Tuesday 07 February 2023 06:09 AM
# end Validation Reply Form

_audit_creation_date             2022-09-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H32 Fe2 N24 W'
_chemical_formula_sum            'C56 H32 Fe2 N24 W'
_chemical_formula_weight         1336.60
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y, -z+3/4'
'-x+1/2, y, -z+3/4'
'-x, -y, z'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1, -y+1/2, -z+5/4'
'-x+1, y+1/2, -z+5/4'
'-x+1/2, -y+1/2, z+1/2'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   18.8695(4)
_cell_length_b                   18.8695(4)
_cell_length_c                   15.4503(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5501.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.75
_shelx_estimated_absorpt_T_max   0.856
_shelx_estimated_absorpt_T_min   0.740
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0746 before and 0.0610 after correction.
The Ratio of minimum to maximum transmission is 0.7687.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_min         2.750
_diffrn_ambient_temperature      80.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3241
_reflns_number_total             3429
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.737
_refine_diff_density_min         -2.457
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.473(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0340
_refine_ls_restrained_S_all      1.114
_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)+(0.0209P)²+27.7101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0674
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.527(14)
 0.473(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C11(H11), C7(H7), C12(H12), C14(H14), C8(H8)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
W001 W 0.5000 0.5000 1.0000 0.00807(10) Uani 1 4 d S T P . .
Fe1 Fe 0.2500 0.44172(8) 0.8750 0.0110(3) Uani 1 2 d S T P . .
C3 C 0.3658(3) 0.4156(3) 0.7442(5) 0.0176(12) Uani 1 1 d . . . . .
H3 H 0.3916 0.4012 0.7940 0.021 Uiso 1 1 calc R U . . .
C9 C 0.2500 0.6965(5) 0.8750 0.023(2) Uani 1 2 d S T P . .
C4 C 0.3622(3) 0.4312(3) 0.5919(4) 0.0182(13) Uani 1 1 d . . . . .
N2 N 0.5236(3) 0.3931(3) 0.8309(3) 0.0166(11) Uani 1 1 d . . . . .
N5 N 0.2991(2) 0.4406(2) 0.7552(4) 0.0156(10) Uani 1 1 d . . . . .
N1 N 0.3430(3) 0.4469(3) 0.9310(3) 0.0141(10) Uani 1 1 d . . . . .
C1 C 0.3973(3) 0.4650(3) 0.9581(4) 0.0145(12) Uani 1 1 d . . . . .
C5 C 0.2652(3) 0.4629(3) 0.6831(4) 0.0173(13) Uani 1 1 d . . . . .
H5 H 0.2190 0.4823 0.6894 0.021 Uiso 1 1 calc R U . . .
N3 N 0.2500 0.5486(5) 0.8750 0.022(2) Uani 1 2 d S T P . .
N7 N 0.2500 0.3326(4) 0.8750 0.0175(18) Uani 1 2 d S T P . .
N4 N 0.2500 0.0479(5) 0.8750 0.030(2) Uani 1 2 d S T P . .
N6 N 0.4150(3) 0.4161(4) 0.4384(4) 0.0305(14) Uani 1 1 d . . . . .
N8 N 0.2500 0.8322(6) 0.8750 0.095(7) Uani 1 2 d S T P . .
C6 C 0.3927(3) 0.4236(3) 0.5065(5) 0.0209(13) Uani 1 1 d . . . . .
C2 C 0.5173(3) 0.4321(3) 0.8871(4) 0.0130(12) Uani 1 1 d . . . . .
C10 C 0.3076(3) 0.5861(3) 0.8496(4) 0.0170(13) Uani 1 1 d . . . . .
H10 H 0.3484 0.5608 0.8310 0.020 Uiso 1 1 calc R U . . .
C11 C 0.3101(4) 0.6589(4) 0.8494(5) 0.0227(14) Uani 1 1 d . . . . .
H11 H 0.3519 0.6832 0.8321 0.027 Uiso 1 1 calc R U . . .
C7 C 0.2937(3) 0.4593(3) 0.6013(4) 0.0191(14) Uani 1 1 d . . . . .
H7 H 0.2678 0.4754 0.5525 0.023 Uiso 1 1 calc R U . . .
C12 C 0.1903(4) 0.2945(4) 0.8614(5) 0.0252(15) Uani 1 1 d . . . . .
H12 H 0.1476 0.3197 0.8506 0.030 Uiso 1 1 calc R U . . .
C13 C 0.2500 0.1844(7) 0.8750 0.026(2) Uani 1 2 d S T P . .
C14 C 0.1874(4) 0.2214(4) 0.8622(5) 0.0242(15) Uani 1 1 d . . . . .
H14 H 0.1438 0.1972 0.8542 0.029 Uiso 1 1 calc R U . . .
C15 C 0.2500 0.1081(5) 0.8750 0.0233(19) Uani 1 2 d S T P . .
C8 C 0.3984(3) 0.4101(3) 0.6647(4) 0.0196(13) Uani 1 1 d . . . . .
H8 H 0.4452 0.3920 0.6603 0.024 Uiso 1 1 calc R U . . .
C16 C 0.2500 0.7727(6) 0.8750 0.055(4) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W001 C1 2.147(6) 2_567 ?
W001 C1 2.147(6) 3_657 ?
W001 C1 2.147(6) 6_665 ?
W001 C1 2.147(6) . ?
W001 C2 2.189(6) 3_657 ?
W001 C2 2.189(6) . ?
W001 C2 2.189(6) 2_567 ?
W001 C2 2.189(6) 6_665 ?
Fe1 N5 2.070(6) 5_556 ?
Fe1 N5 2.070(6) . ?
Fe1 N1 1.958(5) 5_556 ?
Fe1 N1 1.958(5) . ?
Fe1 N3 2.016(9) . ?
Fe1 N7 2.059(8) . ?
C3 H3 0.9500 . ?
C3 N5 1.355(7) . ?
C3 C8 1.376(10) . ?
C9 C11 1.395(8) 5_556 ?
C9 C11 1.395(8) . ?
C9 C16 1.439(16) . ?
C4 C6 1.448(10) . ?
C4 C7 1.404(9) . ?
C4 C8 1.375(9) . ?
N2 C2 1.144(8) . ?
N5 C5 1.351(8) . ?
N1 C1 1.159(8) . ?
C5 H5 0.9500 . ?
C5 C7 1.375(9) . ?
N3 C10 1.355(8) 5_556 ?
N3 C10 1.356(8) . ?
N7 C12 1.353(8) . ?
N7 C12 1.353(8) 5_556 ?
N4 C15 1.136(13) . ?
N6 C6 1.142(10) . ?
N8 C16 1.123(15) . ?
C10 H10 0.9500 . ?
C10 C11 1.375(9) . ?
C11 H11 0.9500 . ?
C7 H7 0.9500 . ?
C12 H12 0.9500 . ?
C12 C14 1.380(10) . ?
C13 C14 1.386(10) 5_556 ?
C13 C14 1.386(10) . ?
C13 C15 1.440(16) . ?
C14 H14 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
C1 W001 C1 95.23(9) 2_567 6_665 ?
C1 W001 C1 144.9(3) 6_665 . ?
C1 W001 C1 95.23(9) 2_567 . ?
C1 W001 C1 144.9(3) 2_567 3_657 ?
C1 W001 C1 95.23(9) 6_665 3_657 ?
C1 W001 C1 95.23(9) 3_657 . ?
C1 W001 C2 144.6(2) 3_657 6_665 ?
C1 W001 C2 73.4(2) . . ?
C1 W001 C2 144.6(2) 2_567 . ?
C1 W001 C2 73.4(2) 2_567 2_567 ?
C1 W001 C2 73.4(2) 6_665 6_665 ?
C1 W001 C2 78.8(2) 3_657 2_567 ?
C1 W001 C2 78.8(2) . 6_665 ?
C1 W001 C2 78.8(2) 2_567 3_657 ?
C1 W001 C2 144.6(2) 6_665 2_567 ?
C1 W001 C2 70.5(2) 6_665 3_657 ?
C1 W001 C2 70.5(2) . 2_567 ?
C1 W001 C2 73.4(2) 3_657 3_657 ?
C1 W001 C2 70.5(2) 3_657 . ?
C1 W001 C2 144.6(2) . 3_657 ?
C1 W001 C2 70.5(2) 2_567 6_665 ?
C1 W001 C2 78.8(2) 6_665 . ?
C2 W001 C2 74.3(3) 3_657 2_567 ?
C2 W001 C2 129.42(18) 3_657 6_665 ?
C2 W001 C2 129.42(18) 2_567 . ?
C2 W001 C2 129.42(18) 6_665 2_567 ?
C2 W001 C2 129.42(18) 3_657 . ?
C2 W001 C2 74.3(3) 6_665 . ?
N5 Fe1 N5 178.8(3) . 5_556 ?
N1 Fe1 N5 90.4(2) . 5_556 ?
N1 Fe1 N5 90.4(2) 5_556 . ?
N1 Fe1 N5 89.7(2) 5_556 5_556 ?
N1 Fe1 N5 89.7(2) . . ?
N1 Fe1 N1 174.2(3) 5_556 . ?
N1 Fe1 N3 87.11(16) 5_556 . ?
N1 Fe1 N3 87.11(16) . . ?
N1 Fe1 N7 92.89(16) . . ?
N1 Fe1 N7 92.89(16) 5_556 . ?
N3 Fe1 N5 90.60(14) . 5_556 ?
N3 Fe1 N5 90.60(14) . . ?
N3 Fe1 N7 180.0 . . ?
N7 Fe1 N5 89.40(14) . 5_556 ?
N7 Fe1 N5 89.40(14) . . ?
N5 C3 H3 118.2 . . ?
N5 C3 C8 123.6(6) . . ?
C8 C3 H3 118.2 . . ?
C11 C9 C11 118.9(9) 5_556 . ?
C11 C9 C16 120.5(5) . . ?
C11 C9 C16 120.5(5) 5_556 . ?
C7 C4 C6 119.8(6) . . ?
C8 C4 C6 121.3(6) . . ?
C8 C4 C7 118.8(6) . . ?
C3 N5 Fe1 122.1(5) . . ?
C5 N5 Fe1 121.4(4) . . ?
C5 N5 C3 116.4(6) . . ?
C1 N1 Fe1 165.2(5) . . ?
N1 C1 W001 176.4(5) . . ?
N5 C5 H5 118.1 . . ?
N5 C5 C7 123.8(6) . . ?
C7 C5 H5 118.1 . . ?
C10 N3 Fe1 121.5(5) . . ?
C10 N3 Fe1 121.5(5) 5_556 . ?
C10 N3 C10 117.0(9) 5_556 . ?
C12 N7 Fe1 122.1(4) . . ?
C12 N7 Fe1 122.1(4) 5_556 . ?
C12 N7 C12 115.8(9) 5_556 . ?
N6 C6 C4 177.7(7) . . ?
N2 C2 W001 175.3(5) . . ?
N3 C10 H10 118.3 . . ?
N3 C10 C11 123.4(7) . . ?
C11 C10 H10 118.3 . . ?
C9 C11 H11 120.7 . . ?
C10 C11 C9 118.6(7) . . ?
C10 C11 H11 120.7 . . ?
C4 C7 H7 120.9 . . ?
C5 C7 C4 118.3(6) . . ?
C5 C7 H7 120.9 . . ?
N7 C12 H12 117.9 . . ?
N7 C12 C14 124.2(7) . . ?
C14 C12 H12 117.9 . . ?
C14 C13 C14 119.5(11) 5_556 . ?
C14 C13 C15 120.3(6) 5_556 . ?
C14 C13 C15 120.3(6) . . ?
C12 C14 C13 118.1(8) . . ?
C12 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
N4 C15 C13 180.0 . . ?
C3 C8 H8 120.5 . . ?
C4 C8 C3 119.0(6) . . ?
C4 C8 H8 120.5 . . ?
N8 C16 C9 180.0 . . ?

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 C5 C7 -175.9(5) . . . . ?
Fe1 N3 C10 C11 -179.4(5) . . . . ?
Fe1 N7 C12 C14 -178.9(6) . . . . ?
C3 N5 C5 C7 2.3(9) . . . . ?
N5 C3 C8 C4 0.4(10) . . . . ?
N5 C5 C7 C4 -0.4(9) . . . . ?
N3 C10 C11 C9 -1.2(9) . . . . ?
N7 C12 C14 C13 -2.2(11) . . . . ?
C6 C4 C7 C5 177.3(6) . . . . ?
C6 C4 C8 C3 -177.2(6) . . . . ?
C10 N3 C10 C11 0.6(5) 5_556 . . . ?
C11 C9 C11 C10 0.6(4) 5_556 . . . ?
C7 C4 C8 C3 1.5(9) . . . . ?
C12 N7 C12 C14 1.1(6) 5_556 . . . ?
C14 C13 C14 C12 1.0(5) 5_556 . . . ?
C15 C13 C14 C12 -179.0(5) . . . . ?
C8 C3 N5 Fe1 175.9(5) . . . . ?
C8 C3 N5 C5 -2.3(9) . . . . ?
C8 C4 C7 C5 -1.5(9) . . . . ?
C16 C9 C11 C10 -179.4(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.527(14)
2 0.473(14)

_chemical_properties_physical    Air-sensitive,Moisture-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_fe2wanh_200k_0m
_database_code_depnum_ccdc_archive 'CCDC 2240345'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2023-02-07 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_fe2wanh_200k_0m     
;
PROBLEM: NonSolvent   Resd 1  N   Ueq(max)/Ueq(min) Range        7.2 Ratio
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
_vrf_PLAT972_fe2wanh_200k_0m     
;
PROBLEM: Check Calcd Resid. Dens.  2.47Ang From N6             -3.11 eA-3
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
_vrf_PLAT973_fe2wanh_200k_0m     
;
PROBLEM: Check Calcd Positive Resid. Density on        W1       1.79 eA-3
RESPONSE: The small, unaccounted for electron density near tungsten is due to the anharmonic vibrations of this heavy metal ion.
;
# Added during the CSD deposition process: Tuesday 07 February 2023 06:09 AM
# end Validation Reply Form

_audit_creation_date             2022-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H32 Fe2 N24 W'
_chemical_formula_sum            'C56 H32 Fe2 N24 W'
_chemical_formula_weight         1336.60
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   19.1966(4)
_cell_length_b                   19.1966(4)
_cell_length_c                   15.8129(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5827.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.70
_shelx_estimated_absorpt_T_max   0.863
_shelx_estimated_absorpt_T_min   0.752
_exptl_absorpt_coefficient_mu    2.520
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.8209.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.006
_diffrn_reflns_theta_min         2.700
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2692
_reflns_number_total             2879
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.488
_refine_diff_density_min         -2.494
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.480(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2879
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.135
_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)+(0.0295P)²+20.6450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0747
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.520(18)
 0.480(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained planarity
 N3, C3, C4, C5, C6, N4
 with sigma of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
W1 W 0.5000 0.5000 0.5000 0.01255(14) Uani 1 4 d S T P . .
Fe1 Fe 0.2500 0.44044(11) 0.3750 0.0209(4) Uani 1 2 d S T P . .
N1 N 0.3470(3) 0.4445(4) 0.4342(4) 0.0237(15) Uani 1 1 d . . . . .
C1 C 0.4005(4) 0.4643(4) 0.4599(5) 0.0194(17) Uani 1 1 d . . . . .
N2 N 0.6043(4) 0.5253(4) 0.6650(4) 0.0313(17) Uani 1 1 d . . . . .
N4 N 0.2500 0.8312(11) 0.3750 0.171(16) Uani 1 2 d S T P . .
C2 C 0.5658(4) 0.5188(3) 0.6096(4) 0.0197(18) Uani 1 1 d . . . . .
C4 C 0.3087(5) 0.6630(5) 0.3514(5) 0.045(3) Uani 1 1 d . . . . .
H4 H 0.3498 0.6869 0.3349 0.054 Uiso 1 1 calc R U . . .
C3 C 0.3073(5) 0.5917(5) 0.3520(4) 0.035(2) Uani 1 1 d . . . . .
H3 H 0.3480 0.5669 0.3356 0.042 Uiso 1 1 calc R U . . .
N3 N 0.2500 0.5554(8) 0.3750 0.043(3) Uani 1 2 d S T P . .
N5 N 0.1960(3) 0.4404(4) 0.5015(5) 0.0281(14) Uani 1 1 d . . . . .
C5 C 0.2500 0.7002(9) 0.3750 0.054(5) Uani 1 2 d S T P . .
C7 C 0.2307(4) 0.4591(5) 0.5716(5) 0.030(2) Uani 1 1 d . . . . .
H7 H 0.2770 0.4758 0.5657 0.036 Uiso 1 1 calc R U . . .
N7 N 0.2500 0.3231(6) 0.3750 0.028(3) Uani 1 2 d S T P . .
C6 C 0.2500 0.7744(11) 0.3750 0.108(10) Uani 1 2 d S T P . .
N6 N 0.0845(5) 0.4169(6) 0.8101(6) 0.059(3) Uani 1 1 d . . . . .
C9 C 0.1353(4) 0.4309(5) 0.6591(5) 0.030(2) Uani 1 1 d . . . . .
C8 C 0.2032(5) 0.4555(5) 0.6507(5) 0.032(2) Uani 1 1 d . . . . .
H8 H 0.2294 0.4693 0.6987 0.038 Uiso 1 1 calc R U . . .
N8 N 0.2500 0.0455(7) 0.3750 0.061(4) Uani 1 2 d S T P . .
C10 C 0.0984(5) 0.4135(5) 0.5892(6) 0.036(2) Uani 1 1 d . . . . .
H10 H 0.0514 0.3984 0.5938 0.043 Uiso 1 1 calc R U . . .
C11 C 0.1302(4) 0.4183(5) 0.5110(6) 0.035(2) Uani 1 1 d . . . . .
H11 H 0.1044 0.4055 0.4621 0.042 Uiso 1 1 calc R U . . .
C12 C 0.1057(4) 0.4237(5) 0.7443(8) 0.039(2) Uani 1 1 d . . . . .
C13 C 0.1909(5) 0.2865(5) 0.3639(7) 0.041(2) Uani 1 1 d . . . . .
H13 H 0.1488 0.3115 0.3545 0.049 Uiso 1 1 calc R U . . .
C14 C 0.1882(6) 0.2151(5) 0.3653(8) 0.047(3) Uani 1 1 d . . . . .
H14 H 0.1450 0.1913 0.3598 0.057 Uiso 1 1 calc R U . . .
C15 C 0.2500 0.1784(10) 0.3750 0.050(5) Uani 1 2 d S T P . .
C16 C 0.2500 0.1035(9) 0.3750 0.052(4) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 2.126(8) 2_665 ?
W1 C1 2.126(8) 4_656 ?
W1 C1 2.126(8) 3_566 ?
W1 C1 2.126(8) . ?
W1 C2 2.174(7) 3_566 ?
W1 C2 2.174(7) 2_665 ?
W1 C2 2.174(7) 4_656 ?
W1 C2 2.174(7) . ?
Fe1 N1 2.085(7) 5 ?
Fe1 N1 2.085(7) . ?
Fe1 N3 2.207(13) . ?
Fe1 N5 2.252(7) 5 ?
Fe1 N5 2.252(7) . ?
Fe1 N7 2.252(12) . ?
N1 C1 1.168(10) . ?
N2 C2 1.153(10) . ?
N4 C6 1.09(2) . ?
C4 H4 0.9500 . ?
C4 C3 1.369(14) . ?
C4 C5 1.385(14) . ?
C3 H3 0.9500 . ?
C3 N3 1.353(11) . ?
N3 C3 1.353(11) 5 ?
N5 C7 1.344(11) . ?
N5 C11 1.341(10) . ?
C5 C4 1.385(14) 5 ?
C5 C6 1.42(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.359(12) . ?
N7 C13 1.347(11) . ?
N7 C13 1.347(11) 5 ?
N6 C12 1.126(15) . ?
C9 C8 1.393(12) . ?
C9 C10 1.355(12) . ?
C9 C12 1.468(14) . ?
C8 H8 0.9500 . ?
N8 C16 1.114(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(13) . ?
C11 H11 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.372(14) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(15) . ?
C15 C14 1.389(15) 5 ?
C15 C16 1.44(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C1 95.11(12) 2_665 3_566 ?
C1 W1 C1 95.11(12) 3_566 . ?
C1 W1 C1 145.3(4) 2_665 . ?
C1 W1 C1 95.11(12) 2_665 4_656 ?
C1 W1 C1 145.3(4) 3_566 4_656 ?
C1 W1 C1 95.11(12) 4_656 . ?
C1 W1 C2 70.3(3) 4_656 3_566 ?
C1 W1 C2 70.3(3) . 2_665 ?
C1 W1 C2 144.4(3) 2_665 2_665 ?
C1 W1 C2 74.0(3) 2_665 4_656 ?
C1 W1 C2 144.4(3) 3_566 3_566 ?
C1 W1 C2 144.4(3) 4_656 4_656 ?
C1 W1 C2 74.0(3) . 3_566 ?
C1 W1 C2 70.3(3) 2_665 . ?
C1 W1 C2 70.3(3) 3_566 4_656 ?
C1 W1 C2 78.5(3) 3_566 . ?
C1 W1 C2 78.5(3) . 4_656 ?
C1 W1 C2 74.0(3) 4_656 . ?
C1 W1 C2 78.5(3) 4_656 2_665 ?
C1 W1 C2 144.4(3) . . ?
C1 W1 C2 78.5(3) 2_665 3_566 ?
C1 W1 C2 74.0(3) 3_566 2_665 ?
C2 W1 C2 129.4(2) . 4_656 ?
C2 W1 C2 129.4(2) 4_656 2_665 ?
C2 W1 C2 129.4(2) . 3_566 ?
C2 W1 C2 74.3(4) 3_566 4_656 ?
C2 W1 C2 74.3(4) . 2_665 ?
C2 W1 C2 129.4(2) 3_566 2_665 ?
N1 Fe1 N1 175.8(4) 5 . ?
N1 Fe1 N3 87.9(2) . . ?
N1 Fe1 N3 87.9(2) 5 . ?
N1 Fe1 N5 90.7(2) . . ?
N1 Fe1 N5 89.3(2) 5 . ?
N1 Fe1 N5 90.7(2) 5 5 ?
N1 Fe1 N5 89.3(2) . 5 ?
N1 Fe1 N7 92.1(2) . . ?
N1 Fe1 N7 92.1(2) 5 . ?
N3 Fe1 N5 90.02(18) . 5 ?
N3 Fe1 N5 90.02(18) . . ?
N3 Fe1 N7 180.0 . . ?
N5 Fe1 N5 180.0(4) 5 . ?
N7 Fe1 N5 89.98(18) . . ?
N7 Fe1 N5 89.98(18) . 5 ?
C1 N1 Fe1 162.4(7) . . ?
N1 C1 W1 177.0(7) . . ?
N2 C2 W1 174.8(7) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 119.9(11) . . ?
C5 C4 H4 120.0 . . ?
C4 C3 H3 118.9 . . ?
N3 C3 C4 122.2(10) . . ?
N3 C3 H3 118.9 . . ?
C3 N3 Fe1 121.0(7) . . ?
C3 N3 Fe1 121.0(7) 5 . ?
C3 N3 C3 118.0(14) 5 . ?
C7 N5 Fe1 120.3(5) . . ?
C11 N5 Fe1 122.2(6) . . ?
C11 N5 C7 117.3(8) . . ?
C4 C5 C4 117.9(15) 5 . ?
C4 C5 C6 121.1(8) . . ?
C4 C5 C6 121.1(8) 5 . ?
N5 C7 H7 118.2 . . ?
N5 C7 C8 123.6(8) . . ?
C8 C7 H7 118.2 . . ?
C13 N7 Fe1 121.4(6) 5 . ?
C13 N7 Fe1 121.4(6) . . ?
C13 N7 C13 117.1(12) . 5 ?
N4 C6 C5 180.0 . . ?
C8 C9 C12 118.8(8) . . ?
C10 C9 C8 119.6(8) . . ?
C10 C9 C12 121.6(8) . . ?
C7 C8 C9 118.0(8) . . ?
C7 C8 H8 121.0 . . ?
C9 C8 H8 121.0 . . ?
C9 C10 H10 120.6 . . ?
C9 C10 C11 118.9(8) . . ?
C11 C10 H10 120.6 . . ?
N5 C11 C10 122.5(8) . . ?
N5 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
N6 C12 C9 178.0(11) . . ?
N7 C13 H13 118.3 . . ?
N7 C13 C14 123.4(11) . . ?
C14 C13 H13 118.3 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.4(12) . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C14 119.1(16) . 5 ?
C14 C15 C16 120.5(8) . . ?
C14 C15 C16 120.5(8) 5 . ?
N8 C16 C15 180.0 . . ?

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 C7 C8 -175.0(7) . . . . ?
Fe1 N5 C11 C10 175.3(7) . . . . ?
Fe1 N7 C13 C14 -178.5(9) . . . . ?
C4 C3 N3 Fe1 -179.99(8) . . . . ?
C4 C3 N3 C3 0.01(8) . . . 5 ?
C3 C4 C5 C4 0.01(8) . . . 5 ?
C3 C4 C5 C6 -179.99(8) . . . . ?
N5 C7 C8 C9 0.1(14) . . . . ?
C5 C4 C3 N3 -0.02(17) . . . . ?
C7 N5 C11 C10 -0.9(13) . . . . ?
N7 C13 C14 C15 -3.0(18) . . . . ?
C9 C10 C11 N5 -1.0(15) . . . . ?
C8 C9 C10 C11 2.4(14) . . . . ?
C10 C9 C8 C7 -2.0(13) . . . . ?
C11 N5 C7 C8 1.4(13) . . . . ?
C12 C9 C8 C7 177.4(8) . . . . ?
C12 C9 C10 C11 -177.0(9) . . . . ?
C13 N7 C13 C14 1.5(9) 5 . . . ?
C13 C14 C15 C14 1.4(8) . . . 5 ?
C13 C14 C15 C16 -178.6(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.520(18)
2 0.480(18)

_chemical_properties_physical    Air-sensitive,Moisture-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_fe2wanh_140k_0m
_database_code_depnum_ccdc_archive 'CCDC 2240346'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2023-02-07 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_fe2wanh_140k_0m     
;
PROBLEM: Atom N4              has ADP max/min Ratio .....        4.2 prolat
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
_vrf_PLAT220_fe2wanh_140k_0m     
;
PROBLEM: NonSolvent   Resd 1  N   Ueq(max)/Ueq(min) Range        8.0 Ratio
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
_vrf_PLAT972_fe2wanh_140k_0m     
;
PROBLEM: Check Calcd Resid. Dens.  2.46Ang From N8             -3.43 eA-3
RESPONSE: This is most likely due to the oscillation of the 4-cyanopyridine molecules, which is allowed by the appearance of small voids in the crystal structure as a result of dehydration.
;
# Added during the CSD deposition process: Tuesday 07 February 2023 06:09 AM
# end Validation Reply Form

_audit_creation_date             2022-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H32 Fe2 N24 W'
_chemical_formula_sum            'C56 H32 Fe2 N24 W'
_chemical_formula_weight         1336.60
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   19.1481(4)
_cell_length_b                   19.1481(4)
_cell_length_c                   15.7535(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5776.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.71
_shelx_estimated_absorpt_T_max   0.862
_shelx_estimated_absorpt_T_min   0.750
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0764 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.8279.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19498
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.013
_diffrn_reflns_theta_min         2.707
_diffrn_ambient_temperature      140.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2734
_reflns_number_total             2859
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.339
_refine_diff_density_min         -2.665
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.492(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2859
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0382
_refine_ls_restrained_S_all      1.157
_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)+(0.0308P)²+33.8137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0788
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.508(18)
 0.492(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C8(H8), C7(H7), C16(H16), C15(H15), C12(H12), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
W1 W 0.5000 0.5000 0.5000 0.00862(14) Uani 1 4 d S T P . .
Fe1 Fe 0.7500 0.56193(11) 0.3750 0.0141(4) Uani 1 2 d S T P . .
N1 N 0.6528(4) 0.5580(4) 0.4341(4) 0.0185(15) Uani 1 1 d . . . . .
C1 C 0.5992(4) 0.5373(4) 0.4598(5) 0.0158(17) Uani 1 1 d . . . . .
N8 N 0.9164(4) 0.5828(5) 0.8120(6) 0.042(2) Uani 1 1 d . . . . .
N2 N 0.6046(4) 0.5257(4) 0.6664(4) 0.0214(16) Uani 1 1 d . . . . .
C2 C 0.5663(4) 0.5185(3) 0.6100(5) 0.0153(18) Uani 1 1 d . . . . .
C4 C 0.8094(5) 0.3390(5) 0.3991(7) 0.033(2) Uani 1 1 d . . . . .
H4 H 0.8506 0.3149 0.4156 0.039 Uiso 1 1 calc R U . . .
N4 N 0.7500 0.1698(9) 0.3750 0.151(15) Uani 1 2 d S T P . .
N3 N 0.7500 0.4485(7) 0.3750 0.036(3) Uani 1 2 d S T P . .
C3 C 0.8073(5) 0.4104(5) 0.3988(5) 0.027(2) Uani 1 1 d . . . . .
H3 H 0.8479 0.4350 0.4160 0.033 Uiso 1 1 calc R U . . .
C5 C 0.7500 0.3025(10) 0.3750 0.049(6) Uani 1 2 d S T P . .
N7 N 0.7500 0.6795(7) 0.3750 0.021(3) Uani 1 2 d S T P . .
C6 C 0.7500 0.2268(9) 0.3750 0.088(9) Uani 1 2 d S T P . .
N6 N 0.7500 0.9571(7) 0.3750 0.045(3) Uani 1 2 d S T P . .
C9 C 0.7500 0.8239(10) 0.3750 0.038(4) Uani 1 2 d S T P . .
C8 C 0.8119(6) 0.7875(5) 0.3643(7) 0.034(2) Uani 1 1 d . . . . .
H8 H 0.8551 0.8113 0.3579 0.040 Uiso 1 1 calc R U . . .
C10 C 0.7500 0.8995(8) 0.3750 0.036(3) Uani 1 2 d S T P . .
C7 C 0.8090(5) 0.7161(5) 0.3632(7) 0.029(2) Uani 1 1 d . . . . .
H7 H 0.8511 0.6910 0.3535 0.035 Uiso 1 1 calc R U . . .
N5 N 0.8039(3) 0.5619(3) 0.5010(5) 0.0198(14) Uani 1 1 d . . . . .
C16 C 0.7683(4) 0.5420(4) 0.5710(5) 0.0204(18) Uani 1 1 d . . . . .
H16 H 0.7218 0.5255 0.5648 0.025 Uiso 1 1 calc R U . . .
C15 C 0.7974(5) 0.5449(4) 0.6513(5) 0.024(2) Uani 1 1 d . . . . .
H15 H 0.7714 0.5301 0.6994 0.029 Uiso 1 1 calc R U . . .
C14 C 0.8948(4) 0.5765(4) 0.7452(7) 0.0255(19) Uani 1 1 d . . . . .
C13 C 0.8650(4) 0.5698(5) 0.6604(5) 0.0202(18) Uani 1 1 d . . . . .
C12 C 0.9018(5) 0.5883(5) 0.5898(6) 0.026(2) Uani 1 1 d . . . . .
H12 H 0.9487 0.6040 0.5944 0.031 Uiso 1 1 calc R U . . .
C11 C 0.8698(4) 0.5836(5) 0.5115(6) 0.0245(19) Uani 1 1 d . . . . .
H11 H 0.8958 0.5965 0.4626 0.029 Uiso 1 1 calc R 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
W1 C1 2.125(8) 2_665 ?
W1 C1 2.125(8) 3_566 ?
W1 C1 2.125(8) 4_656 ?
W1 C1 2.126(8) . ?
W1 C2 2.178(8) 4_656 ?
W1 C2 2.178(8) . ?
W1 C2 2.178(8) 2_665 ?
W1 C2 2.178(8) 3_566 ?
Fe1 N1 2.082(7) . ?
Fe1 N1 2.082(7) 5_655 ?
Fe1 N3 2.171(13) . ?
Fe1 N7 2.251(13) . ?
Fe1 N5 2.237(7) 5_655 ?
Fe1 N5 2.237(7) . ?
N1 C1 1.173(11) . ?
N8 C14 1.136(14) . ?
N2 C2 1.159(10) . ?
C4 H4 0.9500 . ?
C4 C3 1.367(13) . ?
C4 C5 1.388(14) . ?
N4 C6 1.09(2) . ?
N3 C3 1.370(12) 5_655 ?
N3 C3 1.370(12) . ?
C3 H3 0.9500 . ?
C5 C4 1.388(14) 5_655 ?
C5 C6 1.45(3) . ?
N7 C7 1.343(11) . ?
N7 C7 1.343(11) 5_655 ?
N6 C10 1.103(18) . ?
C9 C8 1.387(14) . ?
C9 C8 1.387(14) 5_655 ?
C9 C10 1.45(2) . ?
C8 H8 0.9500 . ?
C8 C7 1.368(13) . ?
C7 H7 0.9500 . ?
N5 C16 1.351(11) . ?
N5 C11 1.339(10) . ?
C16 H16 0.9500 . ?
C16 C15 1.383(12) . ?
C15 H15 0.9500 . ?
C15 C13 1.388(12) . ?
C14 C13 1.458(13) . ?
C13 C12 1.364(12) . ?
C12 H12 0.9500 . ?
C12 C11 1.379(13) . ?
C11 H11 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 W1 C1 95.09(12) 2_665 4_656 ?
C1 W1 C1 95.09(12) 4_656 . ?
C1 W1 C1 145.3(4) 2_665 . ?
C1 W1 C1 95.09(12) 2_665 3_566 ?
C1 W1 C1 145.3(4) 4_656 3_566 ?
C1 W1 C1 95.09(12) 3_566 . ?
C1 W1 C2 144.4(3) 3_566 4_656 ?
C1 W1 C2 70.2(3) . . ?
C1 W1 C2 144.4(3) 2_665 . ?
C1 W1 C2 70.2(3) 2_665 2_665 ?
C1 W1 C2 70.2(3) 4_656 4_656 ?
C1 W1 C2 79.2(3) 3_566 2_665 ?
C1 W1 C2 73.3(3) . 4_656 ?
C1 W1 C2 73.3(3) 2_665 3_566 ?
C1 W1 C2 73.3(3) 4_656 2_665 ?
C1 W1 C2 144.4(3) 4_656 3_566 ?
C1 W1 C2 144.4(3) . 2_665 ?
C1 W1 C2 70.2(3) 3_566 3_566 ?
C1 W1 C2 73.3(3) 3_566 . ?
C1 W1 C2 79.2(3) . 3_566 ?
C1 W1 C2 79.2(3) 2_665 4_656 ?
C1 W1 C2 79.2(3) 4_656 . ?
C2 W1 C2 129.3(2) 3_566 2_665 ?
C2 W1 C2 74.5(4) 2_665 . ?
C2 W1 C2 74.5(4) 3_566 4_656 ?
C2 W1 C2 129.3(2) 4_656 2_665 ?
C2 W1 C2 129.3(2) 3_566 . ?
C2 W1 C2 129.3(2) 4_656 . ?
N1 Fe1 N1 175.8(4) . 5_655 ?
N1 Fe1 N3 87.9(2) 5_655 . ?
N1 Fe1 N3 87.9(2) . . ?
N1 Fe1 N7 92.1(2) 5_655 . ?
N1 Fe1 N7 92.1(2) . . ?
N1 Fe1 N5 89.1(2) 5_655 . ?
N1 Fe1 N5 89.1(2) . 5_655 ?
N1 Fe1 N5 90.9(2) 5_655 5_655 ?
N1 Fe1 N5 90.9(2) . . ?
N3 Fe1 N7 180.0 . . ?
N3 Fe1 N5 89.97(18) . 5_655 ?
N3 Fe1 N5 89.97(18) . . ?
N5 Fe1 N7 90.03(18) . . ?
N5 Fe1 N7 90.03(18) 5_655 . ?
N5 Fe1 N5 179.9(4) . 5_655 ?
C1 N1 Fe1 161.7(7) . . ?
N1 C1 W1 177.2(7) . . ?
N2 C2 W1 175.8(7) . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.6(11) . . ?
C5 C4 H4 120.7 . . ?
C3 N3 Fe1 122.2(6) 5_655 . ?
C3 N3 Fe1 122.2(6) . . ?
C3 N3 C3 115.5(13) 5_655 . ?
C4 C3 N3 123.9(10) . . ?
C4 C3 H3 118.0 . . ?
N3 C3 H3 118.0 . . ?
C4 C5 C4 119.5(16) 5_655 . ?
C4 C5 C6 120.3(8) . . ?
C4 C5 C6 120.3(8) 5_655 . ?
C7 N7 Fe1 121.5(6) 5_655 . ?
C7 N7 Fe1 121.5(6) . . ?
C7 N7 C7 117.0(13) . 5_655 ?
N4 C6 C5 180.0 . . ?
C8 C9 C8 119.5(16) . 5_655 ?
C8 C9 C10 120.2(8) . . ?
C8 C9 C10 120.2(8) 5_655 . ?
C9 C8 H8 121.0 . . ?
C7 C8 C9 118.0(11) . . ?
C7 C8 H8 121.0 . . ?
N6 C10 C9 180.0 . . ?
N7 C7 C8 123.7(10) . . ?
N7 C7 H7 118.2 . . ?
C8 C7 H7 118.2 . . ?
C16 N5 Fe1 119.4(5) . . ?
C11 N5 Fe1 123.0(6) . . ?
C11 N5 C16 117.5(7) . . ?
N5 C16 H16 118.9 . . ?
N5 C16 C15 122.2(8) . . ?
C15 C16 H16 118.9 . . ?
C16 C15 H15 120.5 . . ?
C16 C15 C13 118.9(8) . . ?
C13 C15 H15 120.5 . . ?
N8 C14 C13 178.0(10) . . ?
C15 C13 C14 119.4(8) . . ?
C12 C13 C15 119.1(8) . . ?
C12 C13 C14 121.5(8) . . ?
C13 C12 H12 120.5 . . ?
C13 C12 C11 118.9(8) . . ?
C11 C12 H12 120.5 . . ?
N5 C11 C12 123.3(8) . . ?
N5 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?

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 C3 C4 -179.6(7) . . . . ?
Fe1 N7 C7 C8 -178.7(8) . . . . ?
Fe1 N5 C16 C15 -176.0(6) . . . . ?
Fe1 N5 C11 C12 175.4(7) . . . . ?
C3 C4 C5 C4 0.4(6) . . . 5_655 ?
C3 C4 C5 C6 -179.6(6) . . . . ?
C3 N3 C3 C4 0.4(7) 5_655 . . . ?
C5 C4 C3 N3 -0.7(13) . . . . ?
C9 C8 C7 N7 -2.5(16) . . . . ?
C8 C9 C8 C7 1.2(8) 5_655 . . . ?
C10 C9 C8 C7 -178.8(8) . . . . ?
C7 N7 C7 C8 1.3(8) 5_655 . . . ?
N5 C16 C15 C13 0.8(13) . . . . ?
C16 N5 C11 C12 -1.7(13) . . . . ?
C16 C15 C13 C14 176.8(8) . . . . ?
C16 C15 C13 C12 -2.4(13) . . . . ?
C15 C13 C12 C11 2.0(13) . . . . ?
C14 C13 C12 C11 -177.2(8) . . . . ?
C13 C12 C11 N5 0.1(14) . . . . ?
C11 N5 C16 C15 1.2(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.508(18)
2 0.492(18)

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
