# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_pcn-250_beforeactivation
_database_code_depnum_ccdc_archive 'CCDC 1922881'
loop_
_audit_author_name
_audit_author_address
'Zhifeng Xiao'
;Texas A M University
United States of America
;
_audit_update_record             
;
2019-09-12 deposited with the CCDC.	2019-09-23 downloaded from the CCDC.
;
_audit_creation_date             2019-09-08
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            PCN-250
_chemical_name_systematic        
"catena-[hexakis(m-5,5'-((E)-diazenediyl)bis(benzene-1,3-dicarboxylato))-tetrakis(m-oxo)-dodeca-aqua-dodeca-iron unknown solvate]"
_chemical_formula_moiety         'C48 H29.639 Fe6 N6 O31.82'
_chemical_formula_sum            'C48 H29.64 Fe6 N6 O31.82'
_chemical_formula_weight         1534.64
_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 0.0037 0.0017 '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 0.3621 0.8896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0123 0.0065 '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      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/2, -x+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, z+1/2, -y+1/2'
'x, -y, -z'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, y, -z'
'z+1/2, -y+1/2, -x+1/2'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   21.9389(7)
_cell_length_b                   21.9389(7)
_cell_length_c                   21.9389(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10559.5(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9472
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0.5
_shelx_estimated_absorpt_T_max   0.956
_shelx_estimated_absorpt_T_min   0.914
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.965
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3081
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104626
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         28.268
_diffrn_reflns_theta_min         1.346
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source, Beamline 12.2.1'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3680
_reflns_number_total             4054
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.007(19)
_refine_ls_extinction_coef       0.0044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0263
_refine_ls_restrained_S_all      1.088
_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)+(0.0455P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0739
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.99276
 0.00724
2. Others
 Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(1)
3.a Rotating group:
 O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8)
;
_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 0.73995(2) 0.31990(2) 0.19632(2) 0.01694(12) Uani 1 1 d . . . . .
O1 O 0.74063(8) 0.25937(8) 0.25937(8) 0.0152(5) Uani 1 3 d S T P . .
O4 O 1.10775(8) 0.25549(10) 0.24900(9) 0.0298(5) Uani 1 1 d . . . . .
O5 O 1.14940(8) 0.29618(11) 0.16591(9) 0.0326(5) Uani 1 1 d . . . . .
O3 O 0.87494(9) 0.27366(10) 0.26235(9) 0.0307(5) Uani 1 1 d . . . . .
O2 O 0.82956(8) 0.31301(11) 0.18083(10) 0.0342(5) Uani 1 1 d . . . . .
C1 C 0.87515(11) 0.29305(13) 0.20907(13) 0.0228(5) Uani 1 1 d . . . . .
C2 C 1.10522(11) 0.27917(12) 0.19751(13) 0.0222(5) Uani 1 1 d . . . . .
C3 C 1.04322(12) 0.28752(15) 0.16891(13) 0.0283(6) Uani 1 1 d . . . . .
C4 C 1.04051(13) 0.2963(2) 0.10686(14) 0.0452(9) Uani 1 1 d . . . . .
H4 H 1.076878 0.297894 0.083413 0.054 Uiso 1 1 calc R U . . .
C6 C 0.93141(13) 0.3034(2) 0.11272(15) 0.0481(10) Uani 1 1 d . . . . .
H6 H 0.893258 0.310081 0.093371 0.058 Uiso 1 1 calc R U . . .
C8 C 0.99015(12) 0.28463(14) 0.20294(13) 0.0267(6) Uani 1 1 d . . . . .
H8 H 0.992064 0.276205 0.245374 0.032 Uiso 1 1 calc R U . . .
C7 C 0.93393(12) 0.29410(15) 0.17492(13) 0.0290(6) Uani 1 1 d . . . . .
C5 C 0.98406(14) 0.3029(2) 0.07879(15) 0.0565(13) Uani 1 1 d . . . . .
O6 O 0.73803(12) 0.38496(10) 0.12948(11) 0.0375(7) Uani 0.970(6) 1 d . . P . .
H6A H 0.758949 0.424265 0.128673 0.056 Uiso 0.970(6) 1 d R U P . .
H6B H 0.716360 0.384660 0.090498 0.056 Uiso 0.970(6) 1 d R U P . .
N1 N 0.97671(12) 0.3071(2) 0.01396(13) 0.0719(13) Uani 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 1.9177(3) . ?
Fe1 O4 2.019(2) 2_565 ?
Fe1 O5 2.0176(19) 21_455 ?
Fe1 O3 2.031(2) 15_656 ?
Fe1 O2 2.0007(18) . ?
Fe1 O6 2.0467(19) . ?
O4 C2 1.244(3) . ?
O5 C2 1.249(4) . ?
O3 C1 1.244(3) . ?
O2 C1 1.255(3) . ?
C1 C7 1.492(4) . ?
C2 C3 1.509(3) . ?
C3 C4 1.376(4) . ?
C3 C8 1.385(4) . ?
C4 C5 1.391(4) . ?
C6 C7 1.381(4) . ?
C6 C5 1.374(4) . ?
C8 C7 1.394(4) . ?
C5 N1 1.434(4) . ?
N1 N1 1.192(5) 9_755 ?

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 O4 96.57(8) . 2_565 ?
O1 Fe1 O5 93.19(9) . 21_455 ?
O1 Fe1 O3 97.23(8) . 15_656 ?
O1 Fe1 O2 93.59(9) . . ?
O1 Fe1 O6 179.16(12) . . ?
O4 Fe1 O3 166.13(7) 2_565 15_656 ?
O4 Fe1 O6 83.17(9) 2_565 . ?
O5 Fe1 O4 89.80(9) 21_455 2_565 ?
O5 Fe1 O3 90.79(9) 21_455 15_656 ?
O5 Fe1 O6 86.02(10) 21_455 . ?
O3 Fe1 O6 83.05(9) 15_656 . ?
O2 Fe1 O4 89.69(10) . 2_565 ?
O2 Fe1 O5 173.22(8) . 21_455 ?
O2 Fe1 O3 88.10(9) . 15_656 ?
O2 Fe1 O6 87.21(9) . . ?
Fe1 O1 Fe1 119.985(4) . 15_656 ?
Fe1 O1 Fe1 119.985(4) 16_665 15_656 ?
Fe1 O1 Fe1 119.985(4) . 16_665 ?
C2 O4 Fe1 130.17(17) . 4_645 ?
C2 O5 Fe1 134.67(18) . 21 ?
C1 O3 Fe1 129.58(17) . 16_665 ?
C1 O2 Fe1 136.50(18) . . ?
O3 C1 O2 125.5(2) . . ?
O3 C1 C7 118.7(2) . . ?
O2 C1 C7 115.8(3) . . ?
O4 C2 O5 126.4(2) . . ?
O4 C2 C3 117.9(2) . . ?
O5 C2 C3 115.6(2) . . ?
C4 C3 C2 117.9(2) . . ?
C4 C3 C8 120.2(2) . . ?
C8 C3 C2 121.9(2) . . ?
C3 C4 C5 119.4(3) . . ?
C5 C6 C7 120.0(3) . . ?
C3 C8 C7 120.0(3) . . ?
C6 C7 C1 117.6(2) . . ?
C6 C7 C8 119.6(3) . . ?
C8 C7 C1 122.8(3) . . ?
C4 C5 N1 123.1(3) . . ?
C6 C5 C4 120.6(3) . . ?
C6 C5 N1 116.2(3) . . ?
N1 N1 C5 114.4(3) 9_755 . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  
;
A solvent mask was calculated and 993 electrons were
found in a volume of 6055Å^3 in 1 void per unit cell.
This is consistent with the presence of 
6[C3H7NO(N,N-dimethylformamide] per Formula Unit 
which account for 960 electrons 
per unit cell.
;
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 -0.062 -0.046 -0.045 6055 993 '24 C3H7NO'

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id PCN-250_BeforeActivation
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.99276
2 0.00724

####################################################################### 
# 
# 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_pcn-250_afteractivation
_database_code_depnum_ccdc_archive 'CCDC 1922882'
loop_
_audit_author_name
_audit_author_address
'Zhifeng Xiao'
;Texas A M University
United States of America
;
_audit_update_record             
;
2019-09-12 deposited with the CCDC.	2019-09-23 downloaded from the CCDC.
;
_audit_creation_date             2019-09-09
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            PCN-250
_chemical_name_systematic        
"catena-[hexakis(m-5,5'-((E)-diazenediyl)bis(benzene-1,3-dicarboxylato))-tetrakis(m-oxo)-dodeca-aqua-dodeca-iron unknown solvate]"
_chemical_formula_moiety         'C48 H30 Fe6 N6 O32'
_chemical_formula_sum            'C48 H30 Fe6 N6 O32'
_chemical_formula_weight         1537.88
_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 0.0037 0.0017 '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 0.3621 0.8896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0123 0.0065 '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      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/2, -x+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, z+1/2, -y+1/2'
'x, -y, -z'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, y, -z'
'z+1/2, -y+1/2, -x+1/2'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   21.9834(5)
_cell_length_b                   21.9834(5)
_cell_length_c                   21.9834(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10623.9(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0.5
_shelx_estimated_absorpt_T_max   0.956
_shelx_estimated_absorpt_T_min   0.915
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.961
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2412
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67255
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.029
_diffrn_reflns_theta_min         1.343
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source, Beamline 12.2.1'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                3835
_reflns_number_total             4288
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_coef       0.118(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0414
_refine_ls_restrained_S_all      1.102
_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)+(0.0786P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1273
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.91(3)
 0.09(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Rotating group:
 O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C4(H4)
;
_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 0.76116(2) 0.82041(3) 0.69675(3) 0.0221(2) Uani 1 1 d . . . . .
O1 O 0.75974(12) 0.75974(12) 0.75974(12) 0.0199(8) Uani 1 3 d S T P . .
O2 O 0.67149(13) 0.81330(16) 0.68138(15) 0.0386(8) Uani 1 1 d . . . . .
O3 O 0.62591(13) 0.77469(16) 0.76291(14) 0.0352(7) Uani 1 1 d . . . . .
O4 O 0.39359(13) 0.75514(15) 0.74991(13) 0.0345(7) Uani 1 1 d . . . . .
O5 O 0.35134(13) 0.79558(17) 0.66656(14) 0.0359(7) Uani 1 1 d . . . . .
C2 C 0.39615(16) 0.77807(18) 0.69781(19) 0.0255(8) Uani 1 1 d . . . . .
C8 C 0.51108(17) 0.7837(2) 0.70386(19) 0.0290(8) Uani 1 1 d . . . . .
H8 H 0.509130 0.775689 0.746289 0.035 Uiso 1 1 calc R U . . .
C1 C 0.62557(17) 0.7936(2) 0.70993(19) 0.0278(8) Uani 1 1 d . . . . .
C7 C 0.56751(17) 0.7932(2) 0.67538(19) 0.0307(9) Uani 1 1 d . . . . .
C6 C 0.56922(19) 0.8031(3) 0.6124(2) 0.0452(13) Uani 1 1 d . . . . .
H6 H 0.606867 0.811703 0.592952 0.054 Uiso 1 1 calc R U . . .
C3 C 0.45743(18) 0.7861(2) 0.66889(19) 0.0317(9) Uani 1 1 d . . . . .
C4 C 0.45964(19) 0.7950(3) 0.6070(2) 0.0428(12) Uani 1 1 d . . . . .
H4 H 0.423208 0.797386 0.583872 0.051 Uiso 1 1 calc R U . . .
C5 C 0.5165(2) 0.8005(3) 0.5785(2) 0.0557(18) Uani 1 1 d . . . . .
O6 O 0.76330(18) 0.88628(16) 0.62783(16) 0.0436(8) Uani 1 1 d . . . . .
H6A H 0.767247 0.926892 0.631790 0.065 Uiso 1 1 d R U . . .
H6B H 0.760457 0.880392 0.587391 0.065 Uiso 1 1 d R U . . .
N1 N 0.52418(18) 0.8027(3) 0.51396(18) 0.0679(18) Uani 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 1.9229(5) . ?
Fe1 O2 2.006(3) . ?
Fe1 O3 2.028(3) 12 ?
Fe1 O4 2.023(3) 4_656 ?
Fe1 O5 2.010(3) 21_566 ?
Fe1 O6 2.096(3) . ?
O2 C1 1.265(5) . ?
O3 C1 1.237(5) . ?
O4 C2 1.253(5) . ?
O5 C2 1.261(5) . ?
C2 C3 1.500(5) . ?
C8 C7 1.405(5) . ?
C8 C3 1.409(6) . ?
C1 C7 1.485(5) . ?
C7 C6 1.403(6) . ?
C6 C5 1.379(6) . ?
C3 C4 1.376(6) . ?
C4 C5 1.403(6) . ?
C5 N1 1.429(6) . ?
N1 N1 1.228(8) 9_656 ?

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 92.94(14) . . ?
O1 Fe1 O3 97.07(13) . 12 ?
O1 Fe1 O4 97.54(13) . 4_656 ?
O1 Fe1 O5 93.12(14) . 21_566 ?
O1 Fe1 O6 179.59(12) . . ?
O2 Fe1 O3 88.07(15) . 12 ?
O2 Fe1 O4 89.17(15) . 4_656 ?
O2 Fe1 O5 173.90(13) . 21_566 ?
O2 Fe1 O6 87.37(14) . . ?
O3 Fe1 O6 82.66(14) 12 . ?
O4 Fe1 O3 165.25(12) 4_656 12 ?
O4 Fe1 O6 82.74(14) 4_656 . ?
O5 Fe1 O3 90.50(14) 21_566 12 ?
O5 Fe1 O4 90.73(14) 21_566 4_656 ?
O5 Fe1 O6 86.57(14) 21_566 . ?
Fe1 O1 Fe1 119.996(3) . 11 ?
Fe1 O1 Fe1 119.996(3) 12 11 ?
Fe1 O1 Fe1 119.997(3) . 12 ?
C1 O2 Fe1 136.7(3) . . ?
C1 O3 Fe1 129.9(3) . 11 ?
C2 O4 Fe1 129.6(3) . 2_466 ?
C2 O5 Fe1 135.9(3) . 21_466 ?
O4 C2 O5 125.9(3) . . ?
O4 C2 C3 118.4(4) . . ?
O5 C2 C3 115.8(4) . . ?
C7 C8 C3 119.4(4) . . ?
O2 C1 C7 115.7(4) . . ?
O3 C1 O2 125.3(4) . . ?
O3 C1 C7 119.0(4) . . ?
C8 C7 C1 122.1(4) . . ?
C6 C7 C8 119.1(4) . . ?
C6 C7 C1 118.7(4) . . ?
C5 C6 C7 120.3(4) . . ?
C8 C3 C2 121.1(4) . . ?
C4 C3 C2 117.9(4) . . ?
C4 C3 C8 121.0(4) . . ?
C3 C4 C5 119.1(4) . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 N1 115.8(4) . . ?
C4 C5 N1 123.5(4) . . ?
N1 N1 C5 113.2(5) 9_656 . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 2 2.327
2 2 2 3.292
0 2 3 3.426
0 3 3 4.033
2 3 3 4.459
0 0 4 3.802
0 1 4 3.919
1 2 4 4.356
0 4 4 5.380
2 4 4 5.708
4 4 4 6.595
0 1 5 4.849
0 2 5 5.121
0 3 5 5.547
1 3 5 5.628
2 3 5 5.865
0 5 5 6.731
0 1 6 5.787
1 2 6 6.093
0 3 6 6.384
2 3 6 6.663
0 5 6 7.439
2 5 6 7.680
0 6 6 8.086
6 6 6 9.919
0 1 7 6.731
0 2 7 6.931
1 1 8 7.739
2 2 8 8.086
0 3 8 8.142
2 3 8 8.364
1 4 8 8.580
0 5 8 8.997
2 5 8 9.198
0 6 8 9.541
0 7 8 10.149
0 0 10 9.541
0 1 10 9.590
1 2 10 9.779
0 3 10 9.966
3 3 10 10.373
1 4 10 10.329
2 4 10 10.462

_platon_squeeze_details          )
_platon_squeeze_special_details  
;
A solvent mask was calculated and 3939 electrons were
found in a volume of 6109Å^3 in 1 void per unit cell.
This is consistent with the presence of 
24[C3H7NO] per Formula Unit 
which account for 3840 electrons 
per unit cell.
;
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 -0.074 -0.031 -0.025 6109 3939 ' '

_platon_squeeze_void_probe_radius 1.20


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91(3)
2 0.09(3)

