# Electronic Supplementary Material (ESI) for Materials Horizons.
# This journal is © The Royal Society of Chemistry 2021

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

data_Fe_BDC_Br
_audit_block_doi                 10.5517/ccdc.csd.cc28395w
_database_code_depnum_ccdc_archive 'CCDC 2088537'
loop_
_citation_id
_citation_doi
_citation_year
1 10.33774/chemrxiv-2021-lkt60 2021
loop_
_audit_author_name
_audit_author_address
'Claire Wilson'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-06-07 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
#mo_djb_07_18a_150k_0m_sq
_audit_creation_date             2020-08-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         Fe(III)2Fe(II)3(O)(C8H3O4Br)3(H2O)3
_chemical_formula_sum            'C24 H15 Br3 Fe3 O16'
_chemical_formula_weight         966.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 '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'

_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           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'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'

_cell_length_a                   16.3069(11)
_cell_length_b                   16.3069(11)
_cell_length_c                   52.852(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14054(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8291
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.872
_shelx_estimated_absorpt_T_min   0.511
_exptl_absorpt_coefficient_mu    2.350
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
 wR2(int) was 0.1261 before and 0.0811 after correction. The Ratio 
 of minimum to maximum transmission is 0.6536. The λ/2 correction 
 factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       tablet
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            35038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.409
_diffrn_reflns_theta_min         2.296
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3171
_reflns_number_total             4705
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         4705
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0843
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1523P)²+53.8512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.2759
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C4-C2 = C4-C3_$1 = C3_$1-C2_$1 = C6_$1-C2_$1 = C6_$1-C5 = C5-C2
 1.39 with sigma of 0.02
 Br2-C5 = Br2A-C5 = Br1A-C4 = Br1-C4 = Br3-C9 = Br3A-C9
 1.899 with sigma of 0.02
 C9A-C9_$2 = C9-C8 = C9A-C8
 1.39 with sigma of 0.02
2. Restrained planarity
 C2, C2_$1, C3_$1, C4, C5, C6_$1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Br1A \\sim Br2 \\sim Br2A \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Br3 \\sim Br3A \\sim C9 \\sim C9A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: Br1(0.125) Br1A(0.125) Br2(0.125) Br2A(0.125) Br3(0.125)
 Br3A(0.125) C3(0.5) C4(0.5) C5(0.5) C6(0.5) C9(0.5) C9A(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.6630(8) -0.0242(6) 0.4295(2) 0.137(4) Uani 0.125 1 d D U . A 2
Br1A Br 0.7193(8) 0.0094(7) 0.43733(15) 0.134(4) Uani 0.125 1 d D U . A 1
Br2 Br 0.6978(6) 0.1393(6) 0.32791(14) 0.111(3) Uani 0.125 1 d D U . B 1
Br2A Br 0.7342(6) 0.1742(5) 0.33617(17) 0.092(3) Uani 0.125 1 d D U . B 2
Br3 Br 0.6890(5) 0.0438(6) 0.4762(2) 0.107(3) Uani 0.125 1 d D U . . .
Br3A Br 0.6722(6) 0.0066(6) 0.46428(19) 0.109(3) Uani 0.125 1 d D U . . .
Fe1 Fe 0.500000 0.250000 0.37814(2) 0.0309(3) Uani 1 4 d S T P . .
Fe2 Fe 0.59983(5) 0.250000 0.43280(2) 0.0327(3) Uani 1 2 d S T P . .
O1 O 0.500000 0.250000 0.41599(10) 0.0291(11) Uani 1 4 d S T P . .
O2 O 0.5918(2) 0.1575(2) 0.37600(7) 0.0511(8) Uani 1 1 d . . . . .
O3 O 0.6557(2) 0.1628(2) 0.41285(7) 0.0623(11) Uani 1 1 d . . . . .
O4 O 0.5678(2) 0.1622(3) 0.45810(8) 0.0682(12) Uani 1 1 d . . . . .
O5 O 0.500000 0.250000 0.33858(14) 0.065(2) Uani 1 4 d S T P . .
O6 O 0.7112(3) 0.250000 0.45375(11) 0.0656(15) Uani 1 2 d S T P . .
C1 C 0.6451(3) 0.1368(3) 0.39075(10) 0.0459(11) Uani 1 1 d . . . . .
C2 C 0.7059(3) 0.0712(3) 0.38265(11) 0.0561(12) Uani 1 1 d D U . . .
C3 C 0.7045(7) 0.0392(6) 0.3588(2) 0.060(2) Uiso 0.5 1 d D U . . .
C4 C 0.7309(7) 0.0106(7) 0.40026(19) 0.067(3) Uiso 0.5 1 d D U . . .
C5 C 0.7351(8) 0.0745(7) 0.3574(2) 0.077(3) Uiso 0.5 1 d D U . . .
C6 C 0.7637(7) 0.0427(7) 0.4001(2) 0.063(3) Uiso 0.5 1 d D U . . .
C7 C 0.500000 0.1362(4) 0.46488(13) 0.0494(16) Uani 1 2 d S T P . .
C8 C 0.500000 0.0654(5) 0.48299(14) 0.061(2) Uani 1 2 d DS T P . .
C9 C 0.5750(7) 0.0163(9) 0.4859(3) 0.082(3) Uiso 0.5 1 d D U . . .
C9A C 0.5704(7) 0.0471(8) 0.4961(3) 0.068(3) Uiso 0.5 1 d D 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
Br1 C4 1.982(12) . ?
Br1A C4 1.969(12) . ?
Br2 C5 1.978(12) . ?
Br2A Br2A 2.471(15) 29 ?
Br2A C5 1.975(12) . ?
Br3 Br3A 0.917(13) . ?
Br3 C9 1.979(13) . ?
Br3A C9 1.961(13) . ?
Fe1 O1 2.000(6) . ?
Fe1 O2 2.128(3) 22_655 ?
Fe1 O2 2.128(3) . ?
Fe1 O2 2.128(3) 10_554 ?
Fe1 O2 2.128(3) 29 ?
Fe1 O5 2.090(7) . ?
Fe2 O1 1.855(3) . ?
Fe2 O3 1.991(3) 29 ?
Fe2 O3 1.991(3) . ?
Fe2 O4 2.028(3) 29 ?
Fe2 O4 2.028(3) . ?
Fe2 O6 2.128(5) . ?
O2 C1 1.216(6) . ?
O3 C1 1.254(6) . ?
O4 C7 1.237(5) . ?
C1 C2 1.519(6) . ?
C2 C3 1.364(11) . ?
C2 C4 1.418(11) . ?
C2 C5 1.420(11) . ?
C2 C6 1.397(11) . ?
C3 C4 1.404(13) 15_535 ?
C3 C6 1.569(16) 15_535 ?
C5 C6 1.421(13) 15_535 ?
C7 C8 1.501(9) . ?
C8 C9 1.470(12) . ?
C8 C9 1.470(12) 22_655 ?
C8 C9A 1.373(11) . ?
C8 C9A 1.373(11) 22_655 ?
C9 C9A 1.408(12) 6_556 ?

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
C5 Br2A Br2A 145.5(5) . 29 ?
Br3A Br3 C9 75.4(9) . . ?
Br3 Br3A C9 77.6(9) . . ?
O1 Fe1 O2 93.03(10) . 22_655 ?
O1 Fe1 O2 93.03(10) . . ?
O1 Fe1 O2 93.03(10) . 10_554 ?
O1 Fe1 O2 93.03(10) . 29 ?
O1 Fe1 O5 180.0 . . ?
O2 Fe1 O2 89.4(2) 22_655 . ?
O2 Fe1 O2 173.9(2) 22_655 29 ?
O2 Fe1 O2 173.9(2) 10_554 . ?
O2 Fe1 O2 90.3(2) 22_655 10_554 ?
O2 Fe1 O2 89.4(2) 29 10_554 ?
O2 Fe1 O2 90.3(2) 29 . ?
O5 Fe1 O2 86.97(10) . 29 ?
O5 Fe1 O2 86.97(10) . . ?
O5 Fe1 O2 86.97(10) . 22_655 ?
O5 Fe1 O2 86.97(10) . 10_554 ?
O1 Fe2 O3 98.50(15) . . ?
O1 Fe2 O3 98.50(15) . 29 ?
O1 Fe2 O4 95.16(15) . 29 ?
O1 Fe2 O4 95.16(15) . . ?
O1 Fe2 O6 177.3(2) . . ?
O3 Fe2 O3 91.2(3) . 29 ?
O3 Fe2 O4 166.30(16) 29 . ?
O3 Fe2 O4 166.30(16) . 29 ?
O3 Fe2 O4 87.84(19) 29 29 ?
O3 Fe2 O4 87.84(19) . . ?
O3 Fe2 O6 83.41(16) 29 . ?
O3 Fe2 O6 83.41(16) . . ?
O4 Fe2 O4 89.9(3) 29 . ?
O4 Fe2 O6 82.91(16) . . ?
O4 Fe2 O6 82.91(16) 29 . ?
Fe2 O1 Fe1 118.62(15) . . ?
Fe2 O1 Fe1 118.63(15) 10_554 . ?
Fe2 O1 Fe2 122.8(3) . 10_554 ?
C1 O2 Fe1 131.8(3) . . ?
C1 O3 Fe2 132.2(3) . . ?
C7 O4 Fe2 131.5(4) . . ?
O2 C1 O3 126.9(4) . . ?
O2 C1 C2 118.8(4) . . ?
O3 C1 C2 114.3(4) . . ?
C3 C2 C1 121.3(6) . . ?
C3 C2 C4 110.1(7) . . ?
C3 C2 C5 31.8(6) . . ?
C3 C2 C6 119.5(8) . . ?
C4 C2 C1 119.6(6) . . ?
C4 C2 C5 123.2(7) . . ?
C5 C2 C1 117.2(6) . . ?
C6 C2 C1 119.3(6) . . ?
C6 C2 C4 30.8(6) . . ?
C6 C2 C5 113.9(7) . . ?
C2 C3 C4 124.3(9) . 15_535 ?
C2 C3 C6 111.3(9) . 15_535 ?
C4 C3 C6 28.4(6) 15_535 15_535 ?
C2 C4 Br1 123.3(8) . . ?
C2 C4 Br1A 129.2(8) . . ?
C3 C4 Br1 117.2(8) 15_535 . ?
C3 C4 Br1A 113.5(8) 15_535 . ?
C3 C4 C2 115.2(8) 15_535 . ?
C2 C5 Br2 131.1(8) . . ?
C2 C5 Br2A 124.2(8) . . ?
C2 C5 C4 106.5(8) . 15_535 ?
C2 C5 C6 117.1(9) . 15_535 ?
C4 C5 Br2 112.6(8) 15_535 . ?
C4 C5 Br2A 129.2(8) 15_535 . ?
C6 C5 Br2 111.0(8) 15_535 . ?
C6 C5 Br2A 115.0(8) 15_535 . ?
C6 C5 C4 27.2(6) 15_535 15_535 ?
C2 C6 C5 120.6(9) . 15_535 ?
O4 C7 O4 126.7(7) . 22_655 ?
O4 C7 C8 116.6(3) . . ?
O4 C7 C8 116.6(3) 22_655 . ?
C9 C8 C7 119.1(6) . . ?
C9 C8 C7 119.1(6) 22_655 . ?
C9 C8 C9 112.7(12) 22_655 . ?
C9A C8 C7 119.2(6) 22_655 . ?
C9A C8 C7 119.2(6) . . ?
C9A C8 C9 29.8(7) . . ?
C9A C8 C9 29.8(7) 22_655 22_655 ?
C9A C8 C9 121.7(7) . 22_655 ?
C9A C8 C9 121.7(7) 22_655 . ?
C9A C8 C9A 113.6(12) 22_655 . ?
Br3A C9 Br3 26.9(4) . . ?
C8 C9 Br3 129.2(9) . . ?
C8 C9 Br3A 130.9(9) . . ?
C9A C9 Br3 113.0(9) 6_556 . ?
C9A C9 Br3A 112.2(9) 6_556 . ?
C9A C9 C8 115.2(10) 6_556 . ?
C8 C9A C9 123.0(11) . 6_556 ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.176 0.657 0.052 7120 623 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_MIL53_Fe_DMF
_audit_block_doi                 10.5517/ccdc.csd.cc28394v
_database_code_depnum_ccdc_archive 'CCDC 2088536'
loop_
_citation_id
_citation_doi
_citation_year
1 10.33774/chemrxiv-2021-lkt60 2021
loop_
_audit_author_name
_audit_author_address
'Claire Wilson'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
#mo_em_01_75a_150k_0m_4_sq
_audit_creation_date             2019-08-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

# start Validation Reply Form
_vrf_PLAT420_MIL53_Fe_DMF        
;
PROBLEM: D-H Without Acceptor       O3       --H3       .     Please Check 
RESPONSE: H3 points towards lattice solvent (DMF) which was accounted for
using SQUEEZE.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H5 Fe1 O5'
_chemical_formula_sum            'C8 H5 Fe1 O5'
_chemical_formula_weight         236.97
_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'
O O 0.0106 0.0060 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8403(12)
_cell_length_b                   10.7142(18)
_cell_length_c                   10.7928(18)
_cell_angle_alpha                117.292(6)
_cell_angle_beta                 94.188(7)
_cell_angle_gamma                103.254(6)
_cell_volume                     669.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2295
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.166
_cell_measurement_theta_min      3.127
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.841
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.745687
_exptl_absorpt_correction_T_min  0.637354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 13960 reflections, Rint = 0.0542
 (7774 with I > 3sig(I), Rint = 0.0432)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       column
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            13960
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.252
_diffrn_reflns_theta_min         2.228
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2479
_reflns_number_total             3285
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      1.040
_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)+(0.0458P)²+2.1623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1366
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C3A(H3AA), C4A(H4A)
;
_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
Fe1 Fe 0.500000 0.500000 0.500000 0.01572(19) Uani 1 2 d S T P . .
Fe2 Fe 1.000000 0.500000 0.500000 0.01766(19) Uani 1 2 d S T P . .
O1 O 0.6675(4) 0.6903(3) 0.6735(3) 0.0236(6) Uani 1 1 d . . . . .
O2 O 0.9736(4) 0.6499(3) 0.6932(3) 0.0251(6) Uani 1 1 d . . . . .
O3 O 0.2630(4) 0.5111(3) 0.5897(3) 0.0205(6) Uani 1 1 d . . . . .
C1 C 0.8507(6) 0.7254(4) 0.7351(4) 0.0222(8) Uani 1 1 d . . . . .
C2 C 0.9291(5) 0.8679(4) 0.8732(4) 0.0239(9) Uani 1 1 d . . . . .
C3 C 0.8011(6) 0.9559(5) 0.9245(4) 0.0304(10) Uani 1 1 d . . . . .
H3A H 0.665147 0.925482 0.872629 0.036 Uiso 1 1 calc R . . . .
C4 C 0.8717(6) 1.0882(4) 1.0515(4) 0.0316(10) Uani 1 1 d . . . . .
H4 H 0.784331 1.148427 1.086661 0.038 Uiso 1 1 calc R . . . .
O1A O 0.4282(4) 0.6223(3) 0.4178(3) 0.0230(6) Uani 1 1 d . . . . .
O2A O 1.1359(4) 0.6747(3) 0.4709(3) 0.0272(6) Uani 1 1 d . . . . .
C1A C 0.3174(6) 0.7079(4) 0.4551(4) 0.0210(8) Uani 1 1 d . . . . .
C2A C 0.4113(6) 0.8599(4) 0.4778(4) 0.0222(8) Uani 1 1 d . . . . .
C3A C 0.6241(6) 0.9166(5) 0.5104(5) 0.0296(9) Uani 1 1 d . . . . .
H3AA H 0.707816 0.859840 0.517835 0.036 Uiso 1 1 calc R . . . .
C4A C 0.7131(6) 1.0576(5) 0.5321(5) 0.0287(9) Uani 1 1 d . . . . .
H4A H 0.858228 1.097324 0.553614 0.034 Uiso 1 1 calc R . . . .
H3 H 0.302(6) 0.541(5) 0.678(5) 0.019(11) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.023(2) . ?
Fe1 O1 2.023(2) 2_666 ?
Fe1 O3 1.947(2) 2_666 ?
Fe1 O3 1.947(2) . ?
Fe1 O1A 2.011(3) . ?
Fe1 O1A 2.011(3) 2_666 ?
Fe2 O2 2.019(2) . ?
Fe2 O2 2.019(2) 2_766 ?
Fe2 O3 1.931(3) 1_655 ?
Fe2 O3 1.931(3) 2_666 ?
Fe2 O2A 2.062(3) 2_766 ?
Fe2 O2A 2.062(3) . ?
O1 C1 1.260(5) . ?
O2 C1 1.263(5) . ?
O3 H3 0.85(4) . ?
C1 C2 1.503(5) . ?
C2 C3 1.390(6) . ?
C2 C4 1.390(5) 2_777 ?
C3 H3A 0.9500 . ?
C3 C4 1.389(5) . ?
C4 H4 0.9500 . ?
O1A C1A 1.266(5) . ?
O2A C1A 1.258(4) 1_655 ?
C1A C2A 1.501(5) . ?
C2A C3A 1.391(5) . ?
C2A C4A 1.391(6) 2_676 ?
C3A H3AA 0.9500 . ?
C3A C4A 1.393(5) . ?
C4A H4A 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
O1 Fe1 O1 180.00(15) 2_666 . ?
O3 Fe1 O1 90.86(10) 2_666 . ?
O3 Fe1 O1 89.14(10) . . ?
O3 Fe1 O1 90.86(10) . 2_666 ?
O3 Fe1 O1 89.14(10) 2_666 2_666 ?
O3 Fe1 O3 180.0 . 2_666 ?
O3 Fe1 O1A 90.14(11) 2_666 2_666 ?
O3 Fe1 O1A 89.86(11) 2_666 . ?
O3 Fe1 O1A 89.86(11) . 2_666 ?
O3 Fe1 O1A 90.14(11) . . ?
O1A Fe1 O1 87.48(11) . . ?
O1A Fe1 O1 92.52(11) . 2_666 ?
O1A Fe1 O1 92.52(11) 2_666 . ?
O1A Fe1 O1 87.48(11) 2_666 2_666 ?
O1A Fe1 O1A 180.0 2_666 . ?
O2 Fe2 O2 180.0 . 2_766 ?
O2 Fe2 O2A 87.04(11) . . ?
O2 Fe2 O2A 92.96(11) 2_766 . ?
O2 Fe2 O2A 92.96(11) . 2_766 ?
O2 Fe2 O2A 87.04(11) 2_766 2_766 ?
O3 Fe2 O2 92.05(11) 2_666 . ?
O3 Fe2 O2 92.05(11) 1_655 2_766 ?
O3 Fe2 O2 87.95(11) 2_666 2_766 ?
O3 Fe2 O2 87.95(11) 1_655 . ?
O3 Fe2 O3 180.0 2_666 1_655 ?
O3 Fe2 O2A 89.36(11) 1_655 2_766 ?
O3 Fe2 O2A 90.64(11) 1_655 . ?
O3 Fe2 O2A 90.64(11) 2_666 2_766 ?
O3 Fe2 O2A 89.36(11) 2_666 . ?
O2A Fe2 O2A 180.0 . 2_766 ?
C1 O1 Fe1 128.6(2) . . ?
C1 O2 Fe2 133.8(3) . . ?
Fe1 O3 H3 109(3) . . ?
Fe2 O3 Fe1 123.73(14) 1_455 . ?
Fe2 O3 H3 126(3) 1_455 . ?
O1 C1 O2 125.9(3) . . ?
O1 C1 C2 117.2(3) . . ?
O2 C1 C2 116.8(3) . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 C4 120.2(3) . 2_777 ?
C4 C2 C1 120.3(3) 2_777 . ?
C2 C3 H3A 119.9 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3A 119.9 . . ?
C2 C4 H4 120.2 2_777 . ?
C3 C4 C2 119.6(4) . 2_777 ?
C3 C4 H4 120.2 . . ?
C1A O1A Fe1 130.3(2) . . ?
C1A O2A Fe2 125.4(3) 1_655 . ?
O1A C1A C2A 116.4(3) . . ?
O2A C1A O1A 125.4(3) 1_455 . ?
O2A C1A C2A 118.2(4) 1_455 . ?
C3A C2A C1A 118.7(4) . . ?
C4A C2A C1A 120.3(3) 2_676 . ?
C4A C2A C3A 120.9(4) 2_676 . ?
C2A C3A H3AA 120.4 . . ?
C2A C3A C4A 119.3(4) . . ?
C4A C3A H3AA 120.3 . . ?
C2A C4A C3A 119.8(3) 2_676 . ?
C2A C4A H4A 120.1 2_676 . ?
C3A C4A H4A 120.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Fe3ODMF3BDC3BF4
_audit_block_doi                 10.5517/ccdc.csd.cc28392s
_database_code_depnum_ccdc_archive 'CCDC 2088534'
loop_
_citation_id
_citation_doi
_citation_year
1 10.33774/chemrxiv-2021-lkt60 2021
loop_
_audit_author_name
_audit_author_address
'Claire Wilson'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-06-08 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
#mo_em_02_34g_150k_0m_sq
_audit_creation_date             2020-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '[Fe3O(C8H4O4)3(C3H7NO3)BF4]'
_chemical_formula_sum            'C33 H33 B F4 Fe3 N3 O16'
_chemical_formula_weight         981.98
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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      hexagonal
_space_group_IT_number           190
_space_group_name_H-M_alt        'P -6 2 c'
_space_group_name_Hall           'P -6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   12.6391(8)
_cell_length_b                   12.6391(8)
_cell_length_c                   18.3551(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2539.3(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8599
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.90
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.898
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0760 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.8788. 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    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16518
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.896
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2120
_reflns_number_total             2161
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2161
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0551
_refine_ls_restrained_S_all      1.200
_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)+(0.0428P)²+8.1639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1390
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.89(6)
 0.11(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 F2-B1 = F1-B1
 1.365 with sigma of 0.02
 F1_$2-F2_$2
 2.22 with sigma of 0.02
 F1-F2
 2.22 with sigma of 0.02
 O1S-C2S_$1
 1.236 with sigma of 0.02
 N3S_$1-C4S_$1 = N3S-C4T
 1.454 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C4S \\sim C4T \\sim N3S \\sim C2S \\sim O1S: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
F2 \\sim B1 \\sim F1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Others
 Fixed Sof: C2S(0.5) H2S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5) C4T(0.5)
 F1(0.33333) F2(0.33333) B1(0.16667)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C2S(H2S)
6.b Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC)
;
_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
Fe1 Fe 0.22205(10) 0.49391(9) 0.750000 0.0144(2) Uani 1 2 d S T P A .
O1 O 0.333333 0.666667 0.750000 0.0114(17) Uani 1 6 d S T P . .
O2 O 0.3057(4) 0.4550(4) 0.6695(2) 0.0339(11) Uani 1 1 d . . . . .
O3 O 0.1199(5) 0.5052(4) 0.6714(3) 0.0365(12) Uani 1 1 d . . . . .
C1 C 0.4078(6) 0.5201(6) 0.6422(3) 0.0316(14) Uani 1 1 d . . . . .
C2 C 0.4337(7) 0.4870(6) 0.5688(4) 0.0373(17) Uani 1 1 d . . . . .
C3 C 0.3517(7) 0.3793(6) 0.5345(3) 0.0399(17) Uani 1 1 d . . . . .
H3 H 0.276773 0.324096 0.557591 0.048 Uiso 1 1 calc R . . . .
C4 C 0.5429(8) 0.5707(8) 0.5344(4) 0.057(3) Uani 1 1 d . . . . .
H4 H 0.597710 0.645789 0.557491 0.068 Uiso 1 1 calc R . . . .
O1S O 0.0950(6) 0.3116(6) 0.750000 0.0398(19) Uani 1 2 d DS TU P . .
N3S N -0.0908(15) 0.1490(14) 0.750000 0.105(5) Uani 1 2 d DS TU P . .
C2S C 0.0112(18) 0.2477(15) 0.7184(9) 0.067(5) Uani 0.5 1 d D U . A -1
H2S H 0.009513 0.261472 0.667662 0.081 Uiso 0.5 1 calc R . . A -1
C4S C -0.171(3) 0.082(4) 0.6884(15) 0.144(12) Uani 0.5 1 d D U . A 1
H4SA H -0.256241 0.049562 0.702347 0.216 Uiso 0.5 1 calc GR . . A 1
H4SB H -0.158067 0.013584 0.675087 0.216 Uiso 0.5 1 calc GR . . A 1
H4SC H -0.151121 0.136566 0.646585 0.216 Uiso 0.5 1 calc GR . . A 1
C4T C -0.096(4) 0.085(4) 0.6838(18) 0.154(13) Uani 0.5 1 d D U . A 2
F1 F 0.036(4) 0.170(4) 0.554(2) 0.214(18) Uiso 0.3333 1 d D U . . .
F2 F 0.101(3) 0.088(3) 0.4719(18) 0.181(16) Uiso 0.3333 1 d D U . . .
B1 B 0.000000 0.085(5) 0.500000 0.12(2) Uiso 0.3333 2 d DS TU 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
Fe1 O1 1.9170(10) . ?
Fe1 O2 2.016(4) . ?
Fe1 O2 2.016(4) 4_556 ?
Fe1 O3 1.988(4) . ?
Fe1 O3 1.988(4) 4_556 ?
Fe1 O1S 2.047(7) . ?
O2 C1 1.237(8) . ?
O3 C1 1.270(8) 3_565 ?
C1 C2 1.496(8) . ?
C2 C3 1.383(9) . ?
C2 C4 1.401(10) . ?
C3 C3 1.402(11) 7_556 ?
C3 H3 0.9500 . ?
C4 C4 1.401(13) 7_556 ?
C4 H4 0.9500 . ?
O1S C2S 1.120(15) . ?
O1S C2S 1.120(15) 4_556 ?
N3S N3S 0.00000(12) 4_556 ?
N3S C2S 1.40(2) 4_556 ?
N3S C2S 1.40(2) . ?
N3S C4S 1.472(13) 4_556 ?
N3S C4S 1.472(13) . ?
N3S C4T 1.446(13) . ?
N3S C4T 1.447(13) 4_556 ?
C2S H2S 0.9500 . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
F1 F2 1.42(5) 7_556 ?
F1 B1 1.36(2) . ?
F2 F2 1.07(6) 7_556 ?
F2 B1 1.14(4) 3 ?
F2 B1 1.36(2) . ?
B1 B1 1.86(12) 2 ?
B1 B1 1.86(12) 3 ?

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
O1 Fe1 O2 95.87(13) . 4_556 ?
O1 Fe1 O2 95.87(14) . . ?
O1 Fe1 O3 92.95(13) . . ?
O1 Fe1 O3 92.95(13) . 4_556 ?
O1 Fe1 O1S 176.7(2) . . ?
O2 Fe1 O2 94.3(3) 4_556 . ?
O2 Fe1 O1S 86.38(18) . . ?
O2 Fe1 O1S 86.38(18) 4_556 . ?
O3 Fe1 O2 85.7(2) 4_556 4_556 ?
O3 Fe1 O2 171.13(19) . 4_556 ?
O3 Fe1 O2 171.13(19) 4_556 . ?
O3 Fe1 O2 85.7(2) . . ?
O3 Fe1 O3 93.0(3) . 4_556 ?
O3 Fe1 O1S 84.76(19) 4_556 . ?
O3 Fe1 O1S 84.76(19) . . ?
Fe1 O1 Fe1 120.0 3_565 2_665 ?
Fe1 O1 Fe1 120.0 2_665 . ?
Fe1 O1 Fe1 120.0 3_565 . ?
C1 O2 Fe1 129.4(4) . . ?
C1 O3 Fe1 134.5(4) 3_565 . ?
O2 C1 O3 125.4(5) . 2_665 ?
O2 C1 C2 118.7(6) . . ?
O3 C1 C2 115.9(6) 2_665 . ?
C3 C2 C1 121.6(6) . . ?
C3 C2 C4 120.6(6) . . ?
C4 C2 C1 117.8(6) . . ?
C2 C3 C3 119.9(4) . 7_556 ?
C2 C3 H3 120.1 . . ?
C3 C3 H3 120.1 7_556 . ?
C2 C4 H4 120.3 . . ?
C4 C4 C2 119.5(4) 7_556 . ?
C4 C4 H4 120.3 7_556 . ?
C2S O1S Fe1 137.6(9) 4_556 . ?
C2S O1S Fe1 137.6(9) . . ?
C2S O1S C2S 62.3(19) . 4_556 ?
N3S N3S C2S 0(10) 4_556 4_556 ?
N3S N3S C2S 0(10) 4_556 . ?
N3S N3S C4S 0(10) 4_556 4_556 ?
N3S N3S C4S 0(10) 4_556 . ?
N3S N3S C4T 0(10) 4_556 4_556 ?
N3S N3S C4T 0(10) 4_556 . ?
C2S N3S C2S 49.1(14) 4_556 . ?
C2S N3S C4S 105.0(17) 4_556 4_556 ?
C2S N3S C4S 153.8(19) . 4_556 ?
C2S N3S C4S 105.0(17) . . ?
C2S N3S C4S 153.8(19) 4_556 . ?
C2S N3S C4T 85.1(19) 4_556 4_556 ?
C2S N3S C4T 128(2) . 4_556 ?
C4S N3S C4S 100(3) . 4_556 ?
C4T N3S C4T 114(5) . 4_556 ?
O1S C2S N3S 123.2(13) . . ?
O1S C2S H2S 118.4 . . ?
N3S C2S H2S 118.4 . . ?
N3S C4S N3S 0.000(2) 4_556 . ?
N3S C4S H4SA 109.5 . . ?
N3S C4S H4SA 109.5 4_556 . ?
N3S C4S H4SB 109.5 . . ?
N3S C4S H4SB 109.5 4_556 . ?
N3S C4S H4SC 109.5 . . ?
N3S C4S H4SC 109.5 4_556 . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
N3S C4T N3S 0.0(15) 4_556 . ?
B1 F1 F2 48.6(16) . 7_556 ?
F2 F2 F1 125(6) 7_556 7_556 ?
F2 F2 B1 55(2) 7_556 . ?
F2 F2 B1 76(3) 7_556 3 ?
B1 F2 F1 155(6) . 7_556 ?
B1 F2 F1 63(3) 3 7_556 ?
B1 F2 B1 96(7) 3 . ?
F1 B1 F1 102(6) . 9_556 ?
F1 B1 B1 114(3) 9_556 2 ?
F1 B1 B1 133(2) 9_556 3 ?
F1 B1 B1 133(2) . 2 ?
F1 B1 B1 114(3) . 3 ?
F2 B1 F1 104(2) . 9_556 ?
F2 B1 F1 140(5) 2 . ?
F2 B1 F1 108.7(17) 9_556 9_556 ?
F2 B1 F1 68(3) 7_556 . ?
F2 B1 F1 104(2) 9_556 . ?
F2 B1 F1 68(3) 2 9_556 ?
F2 B1 F1 140(5) 7_556 9_556 ?
F2 B1 F1 108.7(17) . . ?
F2 B1 F2 50(3) 7_556 . ?
F2 B1 F2 112(5) 2 . ?
F2 B1 F2 144(9) 2 7_556 ?
F2 B1 F2 127(6) 9_556 . ?
F2 B1 F2 50(3) 2 9_556 ?
F2 B1 F2 112(5) 7_556 9_556 ?
F2 B1 B1 47(4) 2 2 ?
F2 B1 B1 38(3) . 3 ?
F2 B1 B1 38(3) 9_556 2 ?
F2 B1 B1 99(4) 2 3 ?
F2 B1 B1 99(4) 7_556 2 ?
F2 B1 B1 47(4) 7_556 3 ?
F2 B1 B1 91(3) . 2 ?
F2 B1 B1 91(3) 9_556 3 ?
B1 B1 B1 60.000(3) 2 3 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.89(6)
2 0.11(6)

####################################################################### 
# 
# 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_FeDMFBDC
_audit_block_doi                 10.5517/ccdc.csd.cc28391r
_database_code_depnum_ccdc_archive 'CCDC 2088533'
loop_
_citation_id
_citation_doi
_citation_year
1 10.33774/chemrxiv-2021-lkt60 2021
loop_
_audit_author_name
_audit_author_address
'Claire Wilson'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-06-07 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
# mo_djb_07_10g_150k_0m
_audit_creation_date             2019-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H11 Fe  N  O5'
_chemical_formula_sum            'C11 H11 Fe N O5'
_chemical_formula_weight         293.06
_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'
O O 0.0106 0.0060 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   19.4334(19)
_cell_length_b                   7.2431(7)
_cell_length_c                   8.7675(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1234.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.908
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0685 before and 0.0509 after correction. The Ratio of minimum to maximum transmission is 0.9388. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24397
_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         28.303
_diffrn_reflns_theta_min         2.549
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1477
_reflns_number_total             1654
_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       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1654
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²+1.0827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0967
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3S-C4S
 1.454 with sigma of 0.02
 N3S-C2S
 1.346 with sigma of 0.02
 O1S-C2S
 1.254 with sigma of 0.02
3. Others
 Fixed Sof: H4SA(0.5) H4SB(0.5) H4SC(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2S(H2S), C3(H3), C4(H4)
4.b Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.500000 0.500000 0.00971(13) Uani 1 2 d S T P . .
O1S O 0.49551(7) 0.750000 0.3611(2) 0.0156(3) Uani 1 2 d DS T P . .
O1 O 0.58348(6) 0.59553(16) 0.62110(14) 0.0196(3) Uani 1 1 d . . . . .
O2 O 0.92612(6) 0.90446(16) 0.84403(14) 0.0203(3) Uani 1 1 d . . . . .
N3S N 0.49284(12) 0.750000 0.1024(3) 0.0267(5) Uani 1 2 d DS T P . .
C1 C 0.61135(11) 0.750000 0.6387(2) 0.0146(4) Uani 1 2 d S T P . .
C6 C 0.89781(11) 0.750000 0.8264(2) 0.0143(4) Uani 1 2 d S T P . .
C5 C 0.82350(11) 0.750000 0.7773(3) 0.0158(4) Uani 1 2 d S T P . .
C2 C 0.68578(11) 0.750000 0.6879(3) 0.0156(4) Uani 1 2 d S T P . .
C2S C 0.52445(15) 0.750000 0.2325(3) 0.0235(5) Uani 1 2 d DS T P . .
H2S H 0.573324 0.750000 0.230774 0.028 Uiso 1 2 calc RS T P . .
C3 C 0.72036(9) 0.9148(2) 0.7093(3) 0.0295(4) Uani 1 1 d . . . . .
H3 H 0.697142 1.028491 0.693038 0.035 Uiso 1 1 calc R . . . .
C4 C 0.78903(9) 0.9150(2) 0.7546(3) 0.0294(4) Uani 1 1 d . . . . .
H4 H 0.812314 1.028768 0.770008 0.035 Uiso 1 1 calc R . . . .
C4S C 0.41735(17) 0.750000 0.0963(4) 0.0454(8) Uani 1 2 d DS T P . .
H4SA H 0.398934 0.794699 0.193548 0.068 Uiso 0.5 1 calc GR . . A -1
H4SB H 0.400842 0.624182 0.077551 0.068 Uiso 0.5 1 calc GR . . A -1
H4SC H 0.401893 0.831119 0.013634 0.068 Uiso 0.5 1 calc GR . . A -1
C5S C 0.5283(2) 0.750000 -0.0433(4) 0.0432(8) Uani 1 2 d S T P . .
H5SA H 0.522908 0.870835 -0.092120 0.065 Uiso 0.5 1 calc GR . . B -1
H5SB H 0.508700 0.654179 -0.109129 0.065 Uiso 0.5 1 calc GR . . B -1
H5SC H 0.577336 0.724986 -0.026963 0.065 Uiso 0.5 1 calc GR . . B -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
Fe1 O1S 2.1837(10) 5_666 ?
Fe1 O1S 2.1837(10) . ?
Fe1 O1 2.0587(11) . ?
Fe1 O1 2.0587(11) 5_666 ?
Fe1 O2 2.1001(11) 4_466 ?
Fe1 O2 2.1001(11) 8_755 ?
O1S C2S 1.260(3) . ?
O1 C1 1.2526(15) . ?
O2 C6 1.2563(15) . ?
N3S C2S 1.296(3) . ?
N3S C4S 1.468(4) . ?
N3S C5S 1.451(4) . ?
C1 C2 1.509(3) . ?
C6 C5 1.507(3) . ?
C5 C4 1.384(2) . ?
C5 C4 1.384(2) 7_575 ?
C2 C3 1.382(2) 7_575 ?
C2 C3 1.382(2) . ?
C2S H2S 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.392(2) . ?
C4 H4 0.9500 . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
C5S H5SA 0.9800 . ?
C5S H5SB 0.9800 . ?
C5S H5SC 0.9800 . ?

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
O1S Fe1 O1S 180.0 . 5_666 ?
O1 Fe1 O1S 87.69(5) 5_666 . ?
O1 Fe1 O1S 92.31(5) 5_666 5_666 ?
O1 Fe1 O1S 87.69(5) . 5_666 ?
O1 Fe1 O1S 92.31(5) . . ?
O1 Fe1 O1 180.0 5_666 . ?
O1 Fe1 O2 95.29(5) 5_666 8_755 ?
O1 Fe1 O2 95.29(5) . 4_466 ?
O1 Fe1 O2 84.71(5) 5_666 4_466 ?
O1 Fe1 O2 84.71(5) . 8_755 ?
O2 Fe1 O1S 93.58(5) 8_755 5_666 ?
O2 Fe1 O1S 93.58(5) 4_466 . ?
O2 Fe1 O1S 86.42(5) 8_755 . ?
O2 Fe1 O1S 86.42(5) 4_466 5_666 ?
O2 Fe1 O2 180.00(4) 8_755 4_466 ?
Fe1 O1S Fe1 112.03(8) 3_656 . ?
C2S O1S Fe1 118.76(6) . 3_656 ?
C2S O1S Fe1 118.76(6) . . ?
C1 O1 Fe1 134.78(12) . . ?
C6 O2 Fe1 132.31(12) . 4_566 ?
C2S N3S C4S 120.4(3) . . ?
C2S N3S C5S 123.3(3) . . ?
C5S N3S C4S 116.3(3) . . ?
O1 C1 O1 126.57(19) . 7_575 ?
O1 C1 C2 116.71(10) . . ?
O1 C1 C2 116.71(10) 7_575 . ?
O2 C6 O2 125.88(19) 7_575 . ?
O2 C6 C5 117.06(10) 7_575 . ?
O2 C6 C5 117.06(10) . . ?
C4 C5 C6 120.32(10) . . ?
C4 C5 C6 120.32(10) 7_575 . ?
C4 C5 C4 119.4(2) . 7_575 ?
C3 C2 C1 120.31(10) 7_575 . ?
C3 C2 C1 120.31(10) . . ?
C3 C2 C3 119.4(2) 7_575 . ?
O1S C2S N3S 125.2(3) . . ?
O1S C2S H2S 117.4 . . ?
N3S C2S H2S 117.4 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.37(16) . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 120.26(15) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N3S C4S H4SA 109.5 . . ?
N3S C4S H4SB 109.5 . . ?
N3S C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
N3S C5S H5SA 109.5 . . ?
N3S C5S H5SB 109.5 . . ?
N3S C5S H5SC 109.5 . . ?
H5SA C5S H5SB 109.5 . . ?
H5SA C5S H5SC 109.5 . . ?
H5SB C5S H5SC 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_MIL888Fe
_audit_block_doi                 10.5517/ccdc.csd.cc28393t
_database_code_depnum_ccdc_archive 'CCDC 2088535'
loop_
_citation_id
_citation_doi
_citation_year
1 10.33774/chemrxiv-2021-lkt60 2021
loop_
_audit_author_name
_audit_author_address
'Claire Wilson'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
#mo_djb_06_62d_150k_0m_sq
_audit_creation_date             2021-06-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '[Fe3O(C8H4O4)3(H2O)2(OH)]'
_chemical_formula_sum            'C24 H17 Fe3 O16'
_chemical_formula_weight         728.92
_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'
O O 0.0106 0.0060 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   13.9105(12)
_cell_length_b                   13.9105(12)
_cell_length_c                   17.6608(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2959.6(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.337
_cell_measurement_theta_min      2.860
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.907
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1067 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.8952.
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    0.818
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32529
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         2.306
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1056
_reflns_number_total             1175
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0830P)²+1.1060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1239
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6)
;
_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
Fe1 Fe 0.74639(2) 0.49278(4) 0.250000 0.0192(2) Uani 1 4 d S T P . .
O1 O 0.65368(13) 0.50626(11) 0.33240(8) 0.0366(4) Uani 1 1 d . . . . .
O2 O 0.666667 0.333333 0.250000 0.0184(8) Uani 1 12 d S T P . .
O3 O 0.83128(12) 0.6626(2) 0.250000 0.0363(6) Uani 1 4 d S T P . .
C4 C 0.56128(11) 0.43872(11) 0.35972(14) 0.0282(6) Uani 1 2 d S T P . .
C5 C 0.52905(14) 0.47095(14) 0.43197(15) 0.0336(7) Uani 1 2 d S T P . .
C6 C 0.4282(2) 0.3997(2) 0.46595(13) 0.0500(7) Uani 1 1 d . . . . .
H6 H 0.379513 0.332442 0.442962 0.060 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
Fe1 O1 2.0145(13) 16_556 ?
Fe1 O1 2.0145(13) . ?
Fe1 O1 2.0145(13) 19_655 ?
Fe1 O1 2.0145(13) 11_655 ?
Fe1 O2 1.9208(5) . ?
Fe1 O3 2.045(3) . ?
O1 C4 1.2489(18) . ?
C4 C5 1.494(3) . ?
C5 C6 1.386(3) . ?
C5 C6 1.386(3) 21_665 ?
C6 C6 1.385(4) 9_556 ?
C6 H6 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
O1 Fe1 O1 92.51(9) 16_556 . ?
O1 Fe1 O1 170.75(8) . 11_655 ?
O1 Fe1 O1 170.75(8) 16_556 19_655 ?
O1 Fe1 O1 92.50(9) 19_655 11_655 ?
O1 Fe1 O1 86.75(9) 16_556 11_655 ?
O1 Fe1 O1 86.75(9) . 19_655 ?
O1 Fe1 O3 85.37(4) 11_655 . ?
O1 Fe1 O3 85.37(4) 19_655 . ?
O1 Fe1 O3 85.37(4) . . ?
O1 Fe1 O3 85.37(4) 16_556 . ?
O2 Fe1 O1 94.63(4) . 11_655 ?
O2 Fe1 O1 94.63(4) . 19_655 ?
O2 Fe1 O1 94.63(4) . 16_556 ?
O2 Fe1 O1 94.63(4) . . ?
O2 Fe1 O3 180.00(3) . . ?
C4 O1 Fe1 132.45(14) . . ?
Fe1 O2 Fe1 120.0 14_666 3_655 ?
Fe1 O2 Fe1 120.000(1) . 3_655 ?
Fe1 O2 Fe1 120.0 14_666 . ?
O1 C4 O1 125.9(2) . 21_665 ?
O1 C4 C5 117.04(11) . . ?
O1 C4 C5 117.04(11) 21_665 . ?
C6 C5 C4 120.24(13) 21_665 . ?
C6 C5 C4 120.24(13) . . ?
C6 C5 C6 119.5(3) . 21_665 ?
C5 C6 H6 119.9 . . ?
C6 C6 C5 120.24(13) 9_556 . ?
C6 C6 H6 119.9 9_556 . ?

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 O1 C4 O1 -12.4(4) . . . 21_665 ?
Fe1 O1 C4 C5 167.02(18) . . . . ?
O1 C4 C5 C6 0.1(4) 21_665 . . . ?
O1 C4 C5 C6 -179.4(3) . . . . ?
O1 C4 C5 C6 179.4(3) 21_665 . . 21_665 ?
O1 C4 C5 C6 -0.1(4) . . . 21_665 ?
C4 C5 C6 C6 178.2(3) . . . 9_556 ?
C6 C5 C6 C6 -1.1(7) 21_665 . . 9_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
