# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 2155441'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2022-04-13 deposited with the CCDC.	2022-05-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Fe2W                
;
PROBLEM: Short Inter D...A Contact  O8A      ..N4       .       2.87 Ang.
RESPONSE: This results from disorder of solvent molecule.
;
# Added during the CSD deposition process: Wednesday 13 April 2022 04:51 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 Fe2 N12 O17 W'
_chemical_formula_weight         1108.24

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   12.9768(3)
_cell_length_b                   20.3701(5)
_cell_length_c                   15.7622(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.8440(10)
_cell_angle_gamma                90
_cell_volume                     4077.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    13203
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      24.48

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_F_000             2200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.601
_shelx_estimated_absorpt_T_min   0.466
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20717
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.313
_diffrn_reflns_theta_max         24.486
_diffrn_reflns_theta_full        24.486
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3363
_reflns_number_gt                3191
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL, Mercury'
_computing_publication_material  'Bruker SHELXTL, Mercury'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+21.0960P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3363
_refine_ls_number_parameters     315
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0448
_refine_ls_wR_factor_gt          0.0441
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.500000 0.44174(2) 0.250000 0.00670(6) Uani 1 2 d S T P . .
Fe02 Fe 0.58198(4) 0.65831(2) 0.45283(3) 0.00980(11) Uani 1 1 d . . . . .
O1 O 0.42349(18) 0.68502(11) 0.41474(15) 0.0168(5) Uani 1 1 d . . . . .
O3 O 0.62633(19) 0.75142(11) 0.51932(16) 0.0150(5) Uani 1 1 d D . . . .
H3A H 0.615(3) 0.7590(17) 0.5741(14) 0.018 Uiso 1 1 d D U . . .
H3B H 0.665(2) 0.7865(13) 0.507(2) 0.018 Uiso 1 1 d D U . . .
O2 O 0.24478(18) 1.13610(10) 0.50046(15) 0.0143(5) Uani 1 1 d . . . . .
O4 O 0.6181(2) 0.70400(12) 0.34186(16) 0.0206(6) Uani 1 1 d D . . . .
H4A H 0.642(3) 0.6767(14) 0.304(2) 0.025 Uiso 1 1 d D U . . .
H4B H 0.651(3) 0.7438(11) 0.340(2) 0.025 Uiso 1 1 d D U . . .
N2 N 0.4549(2) 0.38043(13) 0.43247(18) 0.0143(6) Uani 1 1 d . . . . .
N1 N 0.5505(2) 0.56981(13) 0.38155(17) 0.0130(6) Uani 1 1 d . . . . .
O7 O 0.2858(2) 0.63842(12) 0.27343(17) 0.0260(6) Uani 1 1 d D . . . .
H7A H 0.333(3) 0.6508(17) 0.3236(18) 0.031 Uiso 1 1 d D U . . .
H7B H 0.283(3) 0.5936(9) 0.271(2) 0.031 Uiso 1 1 d D U . . .
O6 O 0.6054(2) 0.79267(15) 0.68163(19) 0.0359(7) Uani 1 1 d D . . . .
H6A H 0.592(3) 0.7566(15) 0.713(2) 0.043 Uiso 1 1 d D U . . .
H6B H 0.668(2) 0.8118(19) 0.712(3) 0.043 Uiso 1 1 d D U . . .
C1 C 0.5341(3) 0.52389(16) 0.3383(2) 0.0109(7) Uani 1 1 d . . . . .
O5 O 0.6975(2) 0.82602(12) 0.32564(17) 0.0222(6) Uani 1 1 d D . . . .
H5A H 0.732(3) 0.8386(18) 0.3806(14) 0.027 Uiso 1 1 d D U . . .
H5B H 0.746(2) 0.8278(19) 0.290(2) 0.027 Uiso 1 1 d D U . . .
C2 C 0.4740(2) 0.40365(15) 0.3707(2) 0.0101(7) Uani 1 1 d . . . . .
N5 N 0.4053(2) 0.74848(13) 0.42945(18) 0.0136(6) Uani 1 1 d . . . . .
C3 C 0.3947(3) 0.36028(16) 0.2102(2) 0.0127(7) Uani 1 1 d . . . . .
C4 C 0.3441(3) 0.47607(15) 0.2561(2) 0.0121(7) Uani 1 1 d . . . . .
N4 N 0.2628(2) 0.49539(14) 0.26293(19) 0.0194(7) Uani 1 1 d . . . . .
N3 N 0.3419(2) 0.31487(14) 0.1919(2) 0.0206(7) Uani 1 1 d . . . . .
N6 N 0.2757(2) 1.07372(13) 0.49075(18) 0.0135(6) Uani 1 1 d . . . . .
C12 C 0.2291(3) 1.02440(16) 0.5258(2) 0.0175(8) Uani 1 1 d . . . . .
H12 H 0.176000 1.033775 0.557545 0.021 Uiso 1 1 calc R U . . .
C13 C 0.3512(2) 1.06238(17) 0.4458(2) 0.0146(7) Uani 1 1 d . . . . .
H13 H 0.382994 1.098017 0.421952 0.017 Uiso 1 1 calc R U . . .
C11 C 0.2584(3) 0.96094(16) 0.5158(2) 0.0184(8) Uani 1 1 d . . . . .
H11 H 0.225142 0.926236 0.540246 0.022 Uiso 1 1 calc R U . . .
C5 C 0.3783(3) 0.76549(17) 0.5044(2) 0.0155(8) Uani 1 1 d . . . . .
H5 H 0.373145 0.732991 0.546566 0.019 Uiso 1 1 calc R U . . .
C6 C 0.3582(3) 0.83000(17) 0.5196(2) 0.0166(8) Uani 1 1 d . . . . .
H6 H 0.339001 0.842205 0.572416 0.020 Uiso 1 1 calc R U . . .
C9 C 0.4169(3) 0.79340(17) 0.3698(2) 0.0173(8) Uani 1 1 d . . . . .
H9 H 0.438433 0.780138 0.318282 0.021 Uiso 1 1 calc R U . . .
C10 C 0.3364(3) 0.94684(16) 0.4700(2) 0.0137(7) Uani 1 1 d . . . . .
C7 C 0.3657(3) 0.87791(16) 0.4578(2) 0.0135(7) Uani 1 1 d . . . . .
C14 C 0.3825(3) 0.99902(16) 0.4344(2) 0.0144(7) Uani 1 1 d . . . . .
H14 H 0.435581 0.990850 0.402281 0.017 Uiso 1 1 calc R U . . .
C8 C 0.3977(3) 0.85809(17) 0.3830(2) 0.0168(8) Uani 1 1 d . . . . .
H8 H 0.406400 0.889753 0.340759 0.020 Uiso 1 1 calc R U . . .
O8A O 0.0636(6) 0.4941(4) 0.3152(5) 0.057(2) Uani 0.5 1 d . . P A 1
O8B O 0.0779(5) 0.4442(4) 0.3153(4) 0.0458(16) Uani 0.5 1 d . . P B 2
O9 O 0.4720(12) 0.9056(7) 0.6986(9) 0.179(6) Uani 0.5 1 d . U P C -1


_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 C2 2.144(3) 2_655 ?
W1 C2 2.144(3) . ?
W1 C3 2.159(3) . ?
W1 C3 2.159(3) 2_655 ?
W1 C4 2.161(3) 2_655 ?
W1 C4 2.161(3) . ?
W1 C1 2.163(3) . ?
W1 C1 2.164(3) 2_655 ?
Fe02 O1 2.093(2) . ?
Fe02 N2 2.115(3) 5_666 ?
Fe02 O4 2.117(2) . ?
Fe02 N1 2.119(3) . ?
Fe02 O2 2.140(2) 3_545 ?
Fe02 O3 2.186(2) . ?
O1 N5 1.343(3) . ?
O3 H3A 0.920(18) . ?
O3 H3B 0.916(18) . ?
O2 N6 1.350(3) . ?
O4 H4A 0.918(18) . ?
O4 H4B 0.920(18) . ?
N2 C2 1.155(4) . ?
N1 C1 1.151(4) . ?
O7 H7A 0.929(18) . ?
O7 H7B 0.914(18) . ?
O6 H6A 0.922(19) . ?
O6 H6B 0.938(19) . ?
O5 H5A 0.925(18) . ?
O5 H5B 0.921(18) . ?
N5 C9 1.343(4) . ?
N5 C5 1.345(4) . ?
C3 N3 1.152(4) . ?
C4 N4 1.151(4) . ?
N6 C13 1.342(4) . ?
N6 C12 1.348(4) . ?
C12 C11 1.366(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(5) . ?
C13 H13 0.9500 . ?
C11 C10 1.389(5) . ?
C11 H11 0.9500 . ?
C5 C6 1.370(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(5) . ?
C6 H6 0.9500 . ?
C9 C8 1.365(5) . ?
C9 H9 0.9500 . ?
C10 C14 1.393(5) . ?
C10 C7 1.478(5) . ?
C7 C8 1.387(5) . ?
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
C2 W1 C2 137.56(16) 2_655 . ?
C2 W1 C3 70.69(12) 2_655 . ?
C2 W1 C3 76.96(12) . . ?
C2 W1 C3 76.96(12) 2_655 2_655 ?
C2 W1 C3 70.69(12) . 2_655 ?
C3 W1 C3 79.56(17) . 2_655 ?
C2 W1 C4 76.04(12) 2_655 2_655 ?
C2 W1 C4 118.39(12) . 2_655 ?
C3 W1 C4 141.09(12) . 2_655 ?
C3 W1 C4 73.70(12) 2_655 2_655 ?
C2 W1 C4 118.39(12) 2_655 . ?
C2 W1 C4 76.04(12) . . ?
C3 W1 C4 73.70(12) . . ?
C3 W1 C4 141.08(12) 2_655 . ?
C4 W1 C4 142.24(17) 2_655 . ?
C2 W1 C1 143.33(12) 2_655 . ?
C2 W1 C1 75.99(12) . . ?
C3 W1 C1 144.60(12) . . ?
C3 W1 C1 111.95(12) 2_655 . ?
C4 W1 C1 73.05(12) 2_655 . ?
C4 W1 C1 77.93(12) . . ?
C2 W1 C1 75.99(12) 2_655 2_655 ?
C2 W1 C1 143.33(12) . 2_655 ?
C3 W1 C1 111.95(12) . 2_655 ?
C3 W1 C1 144.60(12) 2_655 2_655 ?
C4 W1 C1 77.93(12) 2_655 2_655 ?
C4 W1 C1 73.05(12) . 2_655 ?
C1 W1 C1 78.66(17) . 2_655 ?
O1 Fe02 N2 87.75(10) . 5_666 ?
O1 Fe02 O4 91.14(10) . . ?
N2 Fe02 O4 175.82(10) 5_666 . ?
O1 Fe02 N1 89.88(10) . . ?
N2 Fe02 N1 94.76(10) 5_666 . ?
O4 Fe02 N1 89.26(10) . . ?
O1 Fe02 O2 175.44(9) . 3_545 ?
N2 Fe02 O2 90.09(10) 5_666 3_545 ?
O4 Fe02 O2 90.73(10) . 3_545 ?
N1 Fe02 O2 94.30(10) . 3_545 ?
O1 Fe02 O3 93.36(9) . . ?
N2 Fe02 O3 89.85(10) 5_666 . ?
O4 Fe02 O3 86.19(9) . . ?
N1 Fe02 O3 174.47(10) . . ?
O2 Fe02 O3 82.62(9) 3_545 . ?
N5 O1 Fe02 113.47(18) . . ?
Fe02 O3 H3A 121(2) . . ?
Fe02 O3 H3B 132(2) . . ?
H3A O3 H3B 106(3) . . ?
N6 O2 Fe02 116.98(17) . 3_455 ?
Fe02 O4 H4A 116(2) . . ?
Fe02 O4 H4B 127(2) . . ?
H4A O4 H4B 107(3) . . ?
C2 N2 Fe02 177.7(3) . 5_666 ?
C1 N1 Fe02 175.7(3) . . ?
H7A O7 H7B 108(3) . . ?
H6A O6 H6B 107(3) . . ?
N1 C1 W1 176.3(3) . . ?
H5A O5 H5B 107(3) . . ?
N2 C2 W1 175.4(3) . . ?
O1 N5 C9 119.1(3) . . ?
O1 N5 C5 119.1(3) . . ?
C9 N5 C5 121.8(3) . . ?
N3 C3 W1 176.5(3) . . ?
N4 C4 W1 177.0(3) . . ?
C13 N6 C12 121.7(3) . . ?
C13 N6 O2 119.2(3) . . ?
C12 N6 O2 119.1(3) . . ?
N6 C12 C11 119.9(3) . . ?
N6 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
N6 C13 C14 119.8(3) . . ?
N6 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
N5 C5 C6 119.6(3) . . ?
N5 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 120.3(3) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
N5 C9 C8 120.0(3) . . ?
N5 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C14 118.1(3) . . ?
C11 C10 C7 120.0(3) . . ?
C14 C10 C7 121.9(3) . . ?
C8 C7 C6 117.7(3) . . ?
C8 C7 C10 121.2(3) . . ?
C6 C7 C10 121.0(3) . . ?
C13 C14 C10 120.0(3) . . ?
C13 C14 H14 120.0 . . ?
C10 C14 H14 120.0 . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?

_refine_diff_density_max         0.636
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.098



_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_Fe2Nb
_database_code_depnum_ccdc_archive 'CCDC 2155442'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2022-04-13 deposited with the CCDC.	2022-05-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Fe2Nb               
;
PROBLEM: Short Inter D...A Contact  O8B      ..N2       .       2.86 Ang.
RESPONSE: This results from disorder of solvent molecule.
;
# Added during the CSD deposition process: Wednesday 13 April 2022 04:51 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 Fe2 N12 Nb O17'
_chemical_formula_weight         1017.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3480 0.7730 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.9090 0.5830 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   13.0334(3)
_cell_length_b                   20.5187(3)
_cell_length_c                   16.0049(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.618(2)
_cell_angle_gamma                90
_cell_volume                     4176.79(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6692
_cell_measurement_theta_min      1.779
_cell_measurement_theta_max      32.258

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_F_000             2068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.901
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_T_max  1.480
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.6754
_diffrn_radiation_type           synchrotron
_diffrn_source                   'ESRF BM01'
_diffrn_measurement_device_type  
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16914
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.790
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_full        23.906
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             5886
_reflns_number_gt                4867
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL, Mercury'
_computing_publication_material  'Bruker SHELXTL, Mercury'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1026P)²+0.4578P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5886
_refine_ls_number_parameters     315
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1491
_refine_ls_wR_factor_gt          0.1409
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe02 Fe 0.58326(3) 0.83904(2) 0.45227(2) 0.02158(11) Uani 1 1 d . . . . .
O2 O 0.61991(19) 0.79466(9) 0.34291(12) 0.0311(4) Uani 1 1 d D . . . .
H2A H 0.646(3) 0.8237(14) 0.308(2) 0.037 Uiso 1 1 d D U . . .
H2B H 0.656(3) 0.7556(11) 0.339(2) 0.037 Uiso 1 1 d D U . . .
C2 C 0.6616(2) 0.97642(12) 0.74225(16) 0.0253(5) Uani 1 1 d . . . . .
N2 N 0.7422(2) 0.99614(12) 0.73480(16) 0.0319(5) Uani 1 1 d . . . . .
O3 O 0.42436(17) 0.81184(9) 0.41316(12) 0.0290(4) Uani 1 1 d . . . . .
N3 N 0.3387(2) 0.80943(12) 0.68872(16) 0.0337(5) Uani 1 1 d . . . . .
C3 C 0.3917(2) 0.85479(12) 0.70858(16) 0.0253(5) Uani 1 1 d . . . . .
Nb1 Nb 0.500000 0.94005(2) 0.750000 0.01885(10) Uani 1 2 d S T P . .
O1 O 0.62790(17) 0.74703(9) 0.51895(12) 0.0271(4) Uani 1 1 d D . . . .
H1A H 0.668(3) 0.7146(13) 0.505(2) 0.033 Uiso 1 1 d D U . . .
H1B H 0.620(3) 0.7413(16) 0.5741(14) 0.033 Uiso 1 1 d D U . . .
N1 N 0.5472(2) 0.87713(10) 0.56549(14) 0.0258(4) Uani 1 1 d . . . . .
C1 C 0.5289(2) 0.90030(11) 0.62669(15) 0.0230(5) Uani 1 1 d . . . . .
N4 N 0.55148(19) 0.92724(10) 0.38220(14) 0.0245(4) Uani 1 1 d . . . . .
O4 O 0.24628(16) 0.36284(8) 0.50151(12) 0.0264(4) Uani 1 1 d . . . . .
C4 C 0.5347(2) 0.97330(11) 0.34007(15) 0.0225(4) Uani 1 1 d . . . . .
N5 N 0.40583(19) 0.74897(10) 0.42769(15) 0.0265(4) Uani 1 1 d . . . . .
O5 O 0.69780(19) 0.67394(10) 0.32476(13) 0.0340(5) Uani 1 1 d D . . . .
H5A H 0.743(3) 0.6680(19) 0.288(2) 0.041 Uiso 1 1 d D U . . .
H5B H 0.732(3) 0.6569(17) 0.3770(15) 0.041 Uiso 1 1 d D U . . .
C5 C 0.3786(2) 0.73261(12) 0.50161(17) 0.0261(5) Uani 1 1 d . . . . .
H5 H 0.373717 0.764540 0.541789 0.031 Uiso 1 1 calc R U . . .
N6 N 0.27651(19) 0.42517(10) 0.49177(14) 0.0255(4) Uani 1 1 d . . . . .
O6 O 0.2879(2) 0.86052(10) 0.27192(14) 0.0376(5) Uani 1 1 d D . . . .
H6A H 0.296(3) 0.9053(9) 0.277(3) 0.045 Uiso 1 1 d D U . . .
H6B H 0.330(3) 0.8449(17) 0.3221(18) 0.045 Uiso 1 1 d D U . . .
C6 C 0.3581(2) 0.66818(12) 0.51740(17) 0.0260(5) Uani 1 1 d . . . . .
H6 H 0.338942 0.656818 0.568124 0.031 Uiso 1 1 calc R U . . .
C7 C 0.4183(2) 0.70368(13) 0.37000(17) 0.0300(6) Uani 1 1 d . . . . .
H7 H 0.440180 0.716194 0.320834 0.036 Uiso 1 1 calc R U . . .
O7 O 0.6059(2) 0.70464(12) 0.67950(16) 0.0475(6) Uani 1 1 d D . . . .
H7A H 0.594(3) 0.7395(15) 0.715(2) 0.057 Uiso 1 1 d D U . . .
H7B H 0.650(3) 0.6744(16) 0.714(2) 0.057 Uiso 1 1 d D U . . .
C8 C 0.3988(2) 0.63872(12) 0.38314(18) 0.0285(5) Uani 1 1 d . . . . .
H8 H 0.407332 0.607625 0.342918 0.034 Uiso 1 1 calc R U . . .
O9 O 0.5485(13) 0.4149(7) 0.3057(9) 0.176(6) Uani 0.5 1 d . U P A -1
C9 C 0.3662(2) 0.62000(12) 0.45716(16) 0.0247(5) Uani 1 1 d . . . . .
O8A O 0.5568(6) 0.5069(5) 0.3138(5) 0.077(2) Uani 0.5 1 d . . P B 2
C14 C 0.2604(2) 0.53785(13) 0.51630(18) 0.0289(5) Uani 1 1 d . . . . .
H14 H 0.228963 0.571686 0.540175 0.035 Uiso 1 1 calc R U . . .
C13 C 0.2314(3) 0.47389(13) 0.52680(18) 0.0303(6) Uani 1 1 d . . . . .
H13 H 0.180835 0.464738 0.558064 0.036 Uiso 1 1 calc R U . . .
C12 C 0.3502(2) 0.43620(12) 0.44598(17) 0.0263(5) Uani 1 1 d . . . . .
H12 H 0.379922 0.401491 0.422308 0.032 Uiso 1 1 calc R U . . .
C11 C 0.3813(2) 0.49943(12) 0.43438(17) 0.0259(5) Uani 1 1 d . . . . .
H11 H 0.432108 0.507292 0.402820 0.031 Uiso 1 1 calc R U . . .
C10 C 0.3367(2) 0.55135(12) 0.47000(16) 0.0247(5) Uani 1 1 d . . . . .
O8B O 0.5780(7) 0.5571(4) 0.3164(5) 0.076(2) Uani 0.5 1 d . . P C 1


_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
Fe02 O3 2.104(2) . ?
Fe02 O2 2.1180(19) . ?
Fe02 N1 2.118(2) . ?
Fe02 N4 2.122(2) . ?
Fe02 O4 2.155(2) 3 ?
Fe02 O1 2.1841(18) . ?
O2 H2A 0.927(18) . ?
O2 H2B 0.939(18) . ?
C2 N2 1.156(4) . ?
C2 Nb1 2.263(3) . ?
O3 N5 1.342(3) . ?
N3 C3 1.161(4) . ?
C3 Nb1 2.255(3) . ?
Nb1 C1 2.242(2) . ?
Nb1 C1 2.242(2) 2_656 ?
Nb1 C4 2.271(2) 6_576 ?
Nb1 C4 2.271(2) 5_676 ?
O1 H1A 0.906(17) . ?
O1 H1B 0.918(18) . ?
N1 C1 1.160(3) . ?
N4 C4 1.154(3) . ?
O4 N6 1.357(3) . ?
N5 C7 1.345(3) . ?
N5 C5 1.349(3) . ?
O5 H5A 0.924(18) . ?
O5 H5B 0.927(18) . ?
C5 C6 1.383(3) . ?
C5 H5 0.9300 . ?
N6 C13 1.343(4) . ?
N6 C12 1.348(4) . ?
O6 H6A 0.926(18) . ?
O6 H6B 0.928(18) . ?
C6 C9 1.401(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.382(3) . ?
C7 H7 0.9300 . ?
O7 H7A 0.949(18) . ?
O7 H7B 0.939(19) . ?
C8 C9 1.397(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.486(3) . ?
C14 C13 1.386(4) . ?
C14 C10 1.391(4) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C12 C11 1.384(3) . ?
C12 H12 0.9300 . ?
C11 C10 1.394(4) . ?
C11 H11 0.9300 . ?

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
O3 Fe02 O2 91.44(8) . . ?
O3 Fe02 N1 87.97(9) . . ?
O2 Fe02 N1 176.15(8) . . ?
O3 Fe02 N4 90.19(8) . . ?
O2 Fe02 N4 89.03(8) . . ?
N1 Fe02 N4 94.78(8) . . ?
O3 Fe02 O4 175.53(7) . 3 ?
O2 Fe02 O4 90.99(8) . 3 ?
N1 Fe02 O4 89.35(9) . 3 ?
N4 Fe02 O4 93.61(8) . 3 ?
O3 Fe02 O1 93.21(8) . . ?
O2 Fe02 O1 87.02(7) . . ?
N1 Fe02 O1 89.21(8) . . ?
N4 Fe02 O1 174.86(9) . . ?
O4 Fe02 O1 83.17(7) 3 . ?
Fe02 O2 H2A 113(2) . . ?
Fe02 O2 H2B 129(2) . . ?
H2A O2 H2B 105(3) . . ?
N2 C2 Nb1 177.0(2) . . ?
N5 O3 Fe02 113.96(16) . . ?
N3 C3 Nb1 177.6(2) . . ?
C1 Nb1 C1 137.33(12) . 2_656 ?
C1 Nb1 C3 70.95(9) . . ?
C1 Nb1 C3 76.23(9) 2_656 . ?
C1 Nb1 C3 76.23(9) . 2_656 ?
C1 Nb1 C3 70.95(9) 2_656 2_656 ?
C3 Nb1 C3 78.25(14) . 2_656 ?
C1 Nb1 C2 120.35(9) . 2_656 ?
C1 Nb1 C2 74.61(9) 2_656 2_656 ?
C3 Nb1 C2 75.02(9) . 2_656 ?
C3 Nb1 C2 140.37(9) 2_656 2_656 ?
C1 Nb1 C2 74.62(9) . . ?
C1 Nb1 C2 120.35(9) 2_656 . ?
C3 Nb1 C2 140.37(9) . . ?
C3 Nb1 C2 75.02(9) 2_656 . ?
C2 Nb1 C2 141.49(13) 2_656 . ?
C1 Nb1 C4 142.67(9) . 6_576 ?
C1 Nb1 C4 76.96(8) 2_656 6_576 ?
C3 Nb1 C4 144.97(9) . 6_576 ?
C3 Nb1 C4 113.31(9) 2_656 6_576 ?
C2 Nb1 C4 76.44(9) 2_656 6_576 ?
C2 Nb1 C4 73.63(9) . 6_576 ?
C1 Nb1 C4 76.96(8) . 5_676 ?
C1 Nb1 C4 142.67(9) 2_656 5_676 ?
C3 Nb1 C4 113.31(9) . 5_676 ?
C3 Nb1 C4 144.97(9) 2_656 5_676 ?
C2 Nb1 C4 73.63(9) 2_656 5_676 ?
C2 Nb1 C4 76.44(9) . 5_676 ?
C4 Nb1 C4 76.96(12) 6_576 5_676 ?
Fe02 O1 H1A 128(2) . . ?
Fe02 O1 H1B 120(2) . . ?
H1A O1 H1B 110(3) . . ?
C1 N1 Fe02 177.4(2) . . ?
N1 C1 Nb1 176.2(2) . . ?
C4 N4 Fe02 176.2(2) . . ?
N6 O4 Fe02 117.34(15) . 3_445 ?
N4 C4 Nb1 176.5(2) . 5_676 ?
O3 N5 C7 119.5(2) . . ?
O3 N5 C5 118.9(2) . . ?
C7 N5 C5 121.6(2) . . ?
H5A O5 H5B 106(3) . . ?
N5 C5 C6 119.8(2) . . ?
N5 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C13 N6 C12 122.0(2) . . ?
C13 N6 O4 119.3(2) . . ?
C12 N6 O4 118.7(2) . . ?
H6A O6 H6B 104(3) . . ?
C5 C6 C9 120.2(2) . . ?
C5 C6 H6 119.9 . . ?
C9 C6 H6 119.9 . . ?
N5 C7 C8 120.6(2) . . ?
N5 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
H7A O7 H7B 108(3) . . ?
C7 C8 C9 119.6(2) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C6 118.2(2) . . ?
C8 C9 C10 120.9(2) . . ?
C6 C9 C10 120.9(2) . . ?
C13 C14 C10 119.9(3) . . ?
C13 C14 H14 120.0 . . ?
C10 C14 H14 120.0 . . ?
N6 C13 C14 119.9(3) . . ?
N6 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
N6 C12 C11 119.7(2) . . ?
N6 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C14 C10 C11 118.4(2) . . ?
C14 C10 C9 120.0(2) . . ?
C11 C10 C9 121.6(2) . . ?

_refine_diff_density_max         1.246
_refine_diff_density_min         -2.285
_refine_diff_density_rms         0.130



_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_Fe2Mo
_database_code_depnum_ccdc_archive 'CCDC 2155443'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2022-04-13 deposited with the CCDC.	2022-05-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Fe2Mo               
;
PROBLEM: Short Inter D...A Contact  O8B      ..N2       .       2.87 Ang.
RESPONSE: This results from disorder of solvent molecule.
;
# Added during the CSD deposition process: Wednesday 13 April 2022 04:51 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 Fe2 Mo N12 O17'
_chemical_formula_weight         1020.33

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'
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'
Mo Mo -1.6832 0.6857 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   12.9910(6)
_cell_length_b                   20.3836(9)
_cell_length_c                   15.7673(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.721(2)
_cell_angle_gamma                90
_cell_volume                     4088.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    12670
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      24.71

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_F_000             2072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.087
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6466
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23780
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.311
_diffrn_reflns_theta_max         24.732
_diffrn_reflns_theta_full        24.732
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3488
_reflns_number_gt                3107
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL, Mercury'
_computing_publication_material  'Bruker SHELXTL, Mercury'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0281P)²+13.0873P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3488
_refine_ls_number_parameters     315
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.500000 0.05815(2) 0.250000 0.00873(10) Uani 1 2 d S T P . .
Fe1 Fe 0.41784(3) 0.15836(2) 0.54709(2) 0.01133(11) Uani 1 1 d . . . . .
O4 O 0.75538(15) 0.63600(9) 0.49967(13) 0.0166(4) Uani 1 1 d . . . . .
O1 O 0.37361(16) 0.25160(9) 0.48038(13) 0.0176(4) Uani 1 1 d D . . . .
H1A H 0.333(2) 0.2846(12) 0.4935(19) 0.021 Uiso 1 1 d D U . . .
H1B H 0.380(2) 0.2617(15) 0.4243(13) 0.021 Uiso 1 1 d D U . . .
O3 O 0.57612(15) 0.18493(9) 0.58489(13) 0.0183(4) Uani 1 1 d . . . . .
O2 O 0.38152(17) 0.20411(10) 0.65811(13) 0.0222(5) Uani 1 1 d D . . . .
H2A H 0.356(2) 0.1749(13) 0.6930(19) 0.027 Uiso 1 1 d D U . . .
H2B H 0.350(2) 0.2440(10) 0.659(2) 0.027 Uiso 1 1 d D U . . .
O5 O 0.71368(19) 0.13865(11) 0.72594(14) 0.0271(5) Uani 1 1 d D . . . .
H5A H 0.665(2) 0.1508(15) 0.6767(16) 0.032 Uiso 1 1 d D U . . .
H5B H 0.716(3) 0.0946(9) 0.727(2) 0.032 Uiso 1 1 d D U . . .
O6 O 0.30221(17) 0.32599(10) 0.67408(14) 0.0238(5) Uani 1 1 d D . . . .
H6A H 0.254(2) 0.3280(17) 0.7084(18) 0.029 Uiso 1 1 d D U . . .
H6B H 0.272(2) 0.3401(16) 0.6192(13) 0.029 Uiso 1 1 d D U . . .
N3 N 0.6584(2) 0.18468(12) 0.30843(16) 0.0221(6) Uani 1 1 d . . . . .
N1 N 0.45463(18) 0.11970(11) 0.43220(15) 0.0156(5) Uani 1 1 d . . . . .
N4 N 0.44926(18) 0.06980(11) 0.61835(14) 0.0151(5) Uani 1 1 d . . . . .
N6 N 0.72488(18) 0.57360(11) 0.50930(14) 0.0150(5) Uani 1 1 d . . . . .
N5 N 0.59456(18) 0.24838(11) 0.57014(15) 0.0164(5) Uani 1 1 d . . . . .
O7 O 0.3939(2) 0.29236(13) 0.31788(16) 0.0395(6) Uani 1 1 d D . . . .
H7A H 0.402(3) 0.2548(13) 0.287(2) 0.047 Uiso 1 1 d D U . . .
H7B H 0.332(2) 0.3120(17) 0.287(2) 0.047 Uiso 1 1 d D U . . .
C4 C 0.4661(2) 0.02415(13) 0.66162(17) 0.0122(6) Uani 1 1 d . . . . .
C2 C 0.3444(2) 0.02384(13) 0.25605(17) 0.0135(6) Uani 1 1 d . . . . .
C5 C 0.6213(2) 0.26538(14) 0.49504(18) 0.0178(6) Uani 1 1 d . . . . .
H5 H 0.625958 0.232965 0.452684 0.021 Uiso 1 1 calc R U . . .
C11 C 0.6178(2) 0.49888(14) 0.56513(18) 0.0165(6) Uani 1 1 d . . . . .
H11 H 0.564390 0.490664 0.596952 0.020 Uiso 1 1 calc R U . . .
C14 C 0.7421(2) 0.46085(14) 0.48404(19) 0.0200(6) Uani 1 1 d . . . . .
H14 H 0.775310 0.426234 0.459422 0.024 Uiso 1 1 calc R U . . .
C13 C 0.7713(2) 0.52441(14) 0.47424(18) 0.0190(6) Uani 1 1 d . . . . .
H13 H 0.824477 0.533842 0.442621 0.023 Uiso 1 1 calc R U . . .
C6 C 0.6418(2) 0.32982(14) 0.48016(19) 0.0179(6) Uani 1 1 d . . . . .
H6 H 0.661340 0.341926 0.427412 0.021 Uiso 1 1 calc R U . . .
N2 N 0.26295(19) 0.00482(12) 0.26336(16) 0.0208(5) Uani 1 1 d . . . . .
C1 C 0.4735(2) 0.09673(13) 0.37055(17) 0.0132(6) Uani 1 1 d . . . . .
C3 C 0.6051(2) 0.13958(14) 0.29009(17) 0.0158(6) Uani 1 1 d . . . . .
C8 C 0.6024(2) 0.35806(14) 0.61693(19) 0.0196(6) Uani 1 1 d . . . . .
H8 H 0.594167 0.389729 0.659255 0.024 Uiso 1 1 calc R U . . .
C9 C 0.6344(2) 0.37786(14) 0.54163(18) 0.0160(6) Uani 1 1 d . . . . .
C12 C 0.6490(2) 0.56230(14) 0.55417(18) 0.0166(6) Uani 1 1 d . . . . .
H12 H 0.617092 0.597853 0.578124 0.020 Uiso 1 1 calc R U . . .
C10 C 0.6640(2) 0.44669(13) 0.52989(17) 0.0153(6) Uani 1 1 d . . . . .
C7 C 0.5829(2) 0.29343(14) 0.63020(19) 0.0207(6) Uani 1 1 d . . . . .
H7 H 0.561253 0.280210 0.681627 0.025 Uiso 1 1 calc R U . . .
O9 O 0.5229(10) 0.4017(6) 0.3013(8) 0.166(5) Uani 0.5 1 d . U P A -1
O8A O 0.0784(4) 0.0565(3) 0.3149(4) 0.0441(13) Uani 0.5 1 d . . P B 1
O8B O 0.0642(4) 0.0044(4) 0.3156(4) 0.0537(15) Uani 0.5 1 d . . P C 2


_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
Mo1 C1 2.148(3) . ?
Mo1 C1 2.149(3) 2_655 ?
Mo1 C2 2.160(3) . ?
Mo1 C2 2.160(3) 2_655 ?
Mo1 C3 2.160(3) . ?
Mo1 C3 2.160(3) 2_655 ?
Mo1 C4 2.168(3) 6 ?
Mo1 C4 2.168(3) 5_656 ?
Fe1 O3 2.092(2) . ?
Fe1 N1 2.117(2) . ?
Fe1 O2 2.119(2) . ?
Fe1 N4 2.122(2) . ?
Fe1 O4 2.140(2) 3_445 ?
Fe1 O1 2.1917(19) . ?
O4 N6 1.350(3) . ?
O1 H1A 0.906(17) . ?
O1 H1B 0.928(17) . ?
O3 N5 1.344(3) . ?
O2 H2A 0.916(18) . ?
O2 H2B 0.914(18) . ?
O5 H5A 0.932(18) . ?
O5 H5B 0.899(18) . ?
O6 H6A 0.909(18) . ?
O6 H6B 0.919(18) . ?
N3 C3 1.153(4) . ?
N1 C1 1.149(4) . ?
N4 C4 1.148(4) . ?
N6 C12 1.345(4) . ?
N6 C13 1.346(4) . ?
N5 C5 1.346(4) . ?
N5 C7 1.349(4) . ?
O7 H7A 0.923(18) . ?
O7 H7B 0.942(18) . ?
C2 N2 1.154(4) . ?
C5 C6 1.370(4) . ?
C5 H5 0.9500 . ?
C11 C12 1.376(4) . ?
C11 C10 1.391(4) . ?
C11 H11 0.9500 . ?
C14 C13 1.367(4) . ?
C14 C10 1.390(4) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?
C6 C9 1.395(4) . ?
C6 H6 0.9500 . ?
C8 C7 1.366(4) . ?
C8 C9 1.395(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.476(4) . ?
C12 H12 0.9500 . ?
C7 H7 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 Mo1 C1 137.06(14) . 2_655 ?
C1 Mo1 C2 76.09(10) . . ?
C1 Mo1 C2 118.51(10) 2_655 . ?
C1 Mo1 C2 118.51(10) . 2_655 ?
C1 Mo1 C2 76.09(10) 2_655 2_655 ?
C2 Mo1 C2 142.22(14) . 2_655 ?
C1 Mo1 C3 70.44(10) . . ?
C1 Mo1 C3 76.84(10) 2_655 . ?
C2 Mo1 C3 141.02(10) . . ?
C2 Mo1 C3 73.75(10) 2_655 . ?
C1 Mo1 C3 76.84(10) . 2_655 ?
C1 Mo1 C3 70.44(10) 2_655 2_655 ?
C2 Mo1 C3 73.75(10) . 2_655 ?
C2 Mo1 C3 141.02(10) 2_655 2_655 ?
C3 Mo1 C3 79.59(15) . 2_655 ?
C1 Mo1 C4 143.48(10) . 6 ?
C1 Mo1 C4 76.28(10) 2_655 6 ?
C2 Mo1 C4 73.02(10) . 6 ?
C2 Mo1 C4 77.94(10) 2_655 6 ?
C3 Mo1 C4 144.73(10) . 6 ?
C3 Mo1 C4 111.87(10) 2_655 6 ?
C1 Mo1 C4 76.28(10) . 5_656 ?
C1 Mo1 C4 143.48(10) 2_655 5_656 ?
C2 Mo1 C4 77.94(10) . 5_656 ?
C2 Mo1 C4 73.02(10) 2_655 5_656 ?
C3 Mo1 C4 111.87(10) . 5_656 ?
C3 Mo1 C4 144.73(10) 2_655 5_656 ?
C4 Mo1 C4 78.62(13) 6 5_656 ?
O3 Fe1 N1 87.74(8) . . ?
O3 Fe1 O2 91.24(8) . . ?
N1 Fe1 O2 175.74(8) . . ?
O3 Fe1 N4 89.84(8) . . ?
N1 Fe1 N4 94.81(9) . . ?
O2 Fe1 N4 89.32(8) . . ?
O3 Fe1 O4 175.49(8) . 3_445 ?
N1 Fe1 O4 89.99(8) . 3_445 ?
O2 Fe1 O4 90.75(8) . 3_445 ?
N4 Fe1 O4 94.23(8) . 3_445 ?
O3 Fe1 O1 93.38(7) . . ?
N1 Fe1 O1 89.70(8) . . ?
O2 Fe1 O1 86.23(8) . . ?
N4 Fe1 O1 174.56(8) . . ?
O4 Fe1 O1 82.72(7) 3_445 . ?
N6 O4 Fe1 116.91(15) . 3 ?
Fe1 O1 H1A 130.0(19) . . ?
Fe1 O1 H1B 125.7(19) . . ?
H1A O1 H1B 103(2) . . ?
N5 O3 Fe1 113.53(15) . . ?
Fe1 O2 H2A 112(2) . . ?
Fe1 O2 H2B 126(2) . . ?
H2A O2 H2B 110(3) . . ?
H5A O5 H5B 107(3) . . ?
H6A O6 H6B 110(3) . . ?
C1 N1 Fe1 177.7(2) . . ?
C4 N4 Fe1 175.6(2) . . ?
C12 N6 C13 121.7(2) . . ?
C12 N6 O4 118.9(2) . . ?
C13 N6 O4 119.3(2) . . ?
O3 N5 C5 119.1(2) . . ?
O3 N5 C7 119.0(2) . . ?
C5 N5 C7 121.9(2) . . ?
H7A O7 H7B 105(3) . . ?
N4 C4 Mo1 176.6(2) . 5_656 ?
N2 C2 Mo1 176.8(2) . . ?
N5 C5 C6 119.4(3) . . ?
N5 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C14 C10 120.3(3) . . ?
C13 C14 H14 119.9 . . ?
C10 C14 H14 119.9 . . ?
N6 C13 C14 120.1(3) . . ?
N6 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C5 C6 C9 120.7(3) . . ?
C5 C6 H6 119.6 . . ?
C9 C6 H6 119.6 . . ?
N1 C1 Mo1 175.9(2) . . ?
N3 C3 Mo1 176.9(3) . . ?
C7 C8 C9 120.4(3) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C6 117.6(3) . . ?
C8 C9 C10 120.8(3) . . ?
C6 C9 C10 121.5(3) . . ?
N6 C12 C11 119.5(3) . . ?
N6 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C10 C11 117.9(3) . . ?
C14 C10 C9 119.9(3) . . ?
C11 C10 C9 122.1(3) . . ?
N5 C7 C8 119.9(3) . . ?
N5 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?

_refine_diff_density_max         0.850
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.076



_exptl_crystal_preparation       'Magnetic properties'
