# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_JOU-22
_database_code_depnum_ccdc_archive 'CCDC 2026455'
loop_
_audit_author_name
_audit_author_address
'Yuhui Luo'
;JOU
China
;
_audit_update_record             
;
2021-01-30 deposited with the CCDC.	2021-06-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Fe2(OH)2(C16H6O8)]^2(C3H7ON)^2(H2O)'
_chemical_formula_sum            'C11 H13 Fe N O7'
_chemical_formula_weight         327.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_H-M_alt        'I 41 2 2'
_space_group_name_Hall           'I 4bw 2bw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'-x+1/2, y, -z+3/4'
'x, -y+1/2, -z+1/4'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'-x+1, y+1/2, -z+5/4'
'x+1/2, -y+1, -z+3/4'
'y+1, x+1, -z+1'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   15.14940(10)
_cell_length_b                   15.14940(10)
_cell_length_c                   12.0558(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2766.86(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2185
_cell_measurement_theta_min      4.6960
_cell_measurement_theta_max      67.8790

_exptl_crystal_description       block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    9.050
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3318
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.127
_diffrn_reflns_theta_max         68.227
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1239
_reflns_number_gt                1203
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.684
_reflns_Friedel_fraction_max     0.979
_reflns_Friedel_fraction_full    0.990

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.507(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1239
_refine_ls_number_parameters     72
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.028
_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
Fe1 Fe 0.19187(4) 0.30813(4) 0.750000 0.0070(3) Uani 1 2 d S T P . .
C1 C 0.0891(3) 0.1396(3) 0.7045(3) 0.0090(8) Uani 1 1 d . . . . .
C2 C 0.000000 0.000000 0.7057(4) 0.0136(10) Uani 1 2 d S T P . .
H2 H -0.000001 0.000001 0.628524 0.016 Uiso 1 2 calc R U P . .
C3 C 0.0407(2) 0.0685(3) 0.7642(4) 0.0140(9) Uani 1 1 d . . . . .
C4 C 0.0386(3) 0.0693(3) 0.8793(4) 0.0163(9) Uani 1 1 d . . . . .
H4 H 0.063215 0.116440 0.917925 0.020 Uiso 1 1 calc R U . . .
C5 C 0.000000 0.000000 0.9372(4) 0.0149(11) Uani 1 2 d S T P . .
O1 O 0.2499(3) 0.250000 0.625000 0.0092(6) Uani 1 2 d S T P . .
H1 H 0.303909 0.250000 0.625000 0.011 Uiso 1 2 d R U P . .
O2 O 0.1179(2) 0.1213(2) 0.6084(2) 0.0126(6) Uani 1 1 d . U . . .
O3 O 0.09880(16) 0.21250(16) 0.7546(2) 0.0117(6) Uani 1 1 d . . . . .
O1W O 0.4287(6) 0.250000 0.625000 0.100(4) Uani 1 2 d S 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 1.954(2) 12_454 ?
Fe1 O1 1.954(2) . ?
Fe1 O3 2.022(2) . ?
Fe1 O3 2.022(2) 16_556 ?
Fe1 O2 2.026(3) 12_454 ?
Fe1 O2 2.026(3) 6_556 ?
C1 O2 1.269(5) . ?
C1 O3 1.267(5) . ?
C1 C3 1.488(5) . ?
C2 C3 1.399(5) 10_444 ?
C2 C3 1.399(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(7) . ?
C4 C5 1.390(5) . ?
C4 H4 0.9300 . ?
C5 C5 1.513(11) 15_446 ?
O1 H1 0.8186 . ?

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 100.91(14) 12_454 . ?
O1 Fe1 O3 88.33(12) 12_454 . ?
O1 Fe1 O3 90.68(12) . . ?
O1 Fe1 O3 90.68(12) 12_454 16_556 ?
O1 Fe1 O3 88.32(12) . 16_556 ?
O3 Fe1 O3 178.44(15) . 16_556 ?
O1 Fe1 O2 89.37(10) 12_454 12_454 ?
O1 Fe1 O2 169.66(9) . 12_454 ?
O3 Fe1 O2 90.62(13) . 12_454 ?
O3 Fe1 O2 90.57(12) 16_556 12_454 ?
O1 Fe1 O2 169.66(9) 12_454 6_556 ?
O1 Fe1 O2 89.37(10) . 6_556 ?
O3 Fe1 O2 90.57(12) . 6_556 ?
O3 Fe1 O2 90.62(13) 16_556 6_556 ?
O2 Fe1 O2 80.36(15) 12_454 6_556 ?
O2 C1 O3 125.8(4) . . ?
O2 C1 C3 116.9(4) . . ?
O3 C1 C3 117.2(4) . . ?
C3 C2 C3 119.4(5) 10_444 . ?
C3 C2 H2 120.3 10_444 . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 C1 119.2(4) . . ?
C2 C3 C1 120.7(4) . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C4 119.7(5) . 10_444 ?
C4 C5 C5 120.1(3) . 15_446 ?
C4 C5 C5 120.1(3) 10_444 15_446 ?
Fe1 O1 Fe1 126.6(2) 11_544 . ?
Fe1 O1 H1 116.7 11_544 . ?
Fe1 O1 H1 116.7 . . ?
C1 O2 Fe1 131.6(3) . 11_544 ?
C1 O3 Fe1 133.8(2) . . ?

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
C3 C2 C3 C4 -1.6(3) 10_444 . . . ?
C3 C2 C3 C1 176.4(4) 10_444 . . . ?
O2 C1 C3 C4 154.4(4) . . . . ?
O3 C1 C3 C4 -24.7(6) . . . . ?
O2 C1 C3 C2 -23.7(5) . . . . ?
O3 C1 C3 C2 157.2(3) . . . . ?
C2 C3 C4 C5 3.2(5) . . . . ?
C1 C3 C4 C5 -174.9(3) . . . . ?
C3 C4 C5 C4 -1.6(3) . . . 10_444 ?
C3 C4 C5 C5 178.4(3) . . . 15_446 ?
O3 C1 O2 Fe1 2.9(6) . . . 11_544 ?
C3 C1 O2 Fe1 -176.1(3) . . . 11_544 ?
O2 C1 O3 Fe1 -28.6(6) . . . . ?
C3 C1 O3 Fe1 150.5(3) . . . . ?

_refine_diff_density_max         0.716
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.073



