# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_DMAFeFe_H2O-4
_database_code_depnum_ccdc_archive 'CCDC 1979650'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-01-23 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.04747(16)
_cell_length_b                   12.04747(16)
_cell_length_c                   12.04747(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1748.59(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4144
_cell_measurement_theta_min      4.0780
_cell_measurement_theta_max      28.5720

_exptl_crystal_description       cube
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.713
_shelx_estimated_absorpt_T_min   0.834
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10362
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.382
_diffrn_reflns_theta_max         29.227
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             445
_reflns_number_gt                348
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2014)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0493P)²+3.9725P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         445
_refine_ls_number_parameters     47
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.086
_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 0.250000 0.250000 0.250000 0.0218(3) Uani 1 6 d S T P . .
O1 O 0.40847(14) 0.30702(15) 0.20458(16) 0.0390(5) Uani 1 1 d . . . . .
C1 C 0.500000 0.2797(4) 0.2413(3) 0.0363(8) Uani 1 2 d S T P . .
H1 H 0.500000 0.233549 0.303211 0.044 Uiso 1 2 calc R U P . .
C2 C 0.500000 -0.0971(10) 0.000000 0.084(3) Uani 1 4 d DS TU P . .
H2A H 0.561(5) -0.153(5) 0.000000 0.101 Uiso 0.75 2 d DS U P . .
H2B H 0.500000 -0.1515(17) 0.0624(4) 0.101 Uiso 0.75 2 d DS U P . .
N1 N 0.437(3) 0.000000 0.000000 0.079(5) Uani 0.25 4 d DS TU P A 1
H3 H 0.395(6) 0.000000 0.062(4) 0.095 Uiso 0.25 2 d DS U P B 1
H4 H 0.442(4) 0.000000 -0.104(6) 0.095 Uiso 0.25 2 d DS U P C 2
N2 N 0.500000 -0.0262(13) -0.0643(15) 0.020(4) Uiso 0.125 2 d DS U P A 2
O2 O 0.552(3) 0.500000 0.500000 0.11(2) Uiso 0.1667 4 d DS . P . .
H5 H 0.602(6) 0.445(4) 0.500000 0.138 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0218(3) 0.0218(3) 0.0218(3) 0.00065(15) 0.00065(15) 0.00065(15)
O1 0.0275(9) 0.0424(10) 0.0470(11) 0.0093(9) -0.0005(8) 0.0002(7)
C1 0.0294(18) 0.0381(18) 0.042(2) 0.0130(15) 0.000 0.000
C2 0.051(4) 0.127(8) 0.074(5) 0.000 0.000 0.000
N1 0.060(13) 0.126(12) 0.053(12) 0.000 0.000 0.000

_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 2.1014(17) 45 ?
Fe1 O1 2.1014(17) 9 ?
Fe1 O1 2.1014(17) 41 ?
Fe1 O1 2.1014(17) 5 ?
Fe1 O1 2.1014(17) 37 ?
Fe1 O1 2.1014(17) . ?
O1 C1 1.233(2) . ?
C2 N2 1.154(18) 26 ?
C2 N2 1.154(18) . ?
C2 N1 1.397(18) 2_655 ?
C2 N1 1.397(18) . ?
C2 N2 1.68(2) 2_655 ?
C2 N2 1.68(2) 4 ?
N2 N2 0.63(3) 2_655 ?
N2 N2 1.55(4) 26 ?
O2 O2 0.88(6) 33_666 ?
O2 O2 0.88(6) 29_666 ?
O2 O2 0.88(6) 9 ?
O2 O2 0.88(6) 5 ?
O2 O2 1.24(8) 25_666 ?

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(4) 45 9 ?
O1 Fe1 O1 91.42(7) 45 41 ?
O1 Fe1 O1 88.58(7) 9 41 ?
O1 Fe1 O1 88.58(7) 45 5 ?
O1 Fe1 O1 91.42(7) 9 5 ?
O1 Fe1 O1 180.00(9) 41 5 ?
O1 Fe1 O1 91.42(7) 45 37 ?
O1 Fe1 O1 88.58(7) 9 37 ?
O1 Fe1 O1 91.42(7) 41 37 ?
O1 Fe1 O1 88.58(8) 5 37 ?
O1 Fe1 O1 88.58(7) 45 . ?
O1 Fe1 O1 91.42(8) 9 . ?
O1 Fe1 O1 88.58(7) 41 . ?
O1 Fe1 O1 91.42(8) 5 . ?
O1 Fe1 O1 180.0 37 . ?
C1 O1 Fe1 129.2(2) . . ?
O1 C1 O1 126.8(3) . 28_655 ?
N2 C2 N2 84.3(19) 26 . ?
N1 C2 N1 66(2) 2_655 . ?
C2 N1 C2 114(2) . 25_655 ?
N2 N2 C2 137.8(10) 2_655 . ?
C2 N2 N2 47.8(10) . 26 ?
C2 N2 C2 110.3(15) . 25_655 ?
O2 O2 O2 60.002(8) 33_666 29_666 ?
O2 O2 O2 90.004(1) 33_666 9 ?
O2 O2 O2 60.002(3) 29_666 9 ?
O2 O2 O2 60.002(1) 33_666 5 ?
O2 O2 O2 90.0 29_666 5 ?
O2 O2 O2 60.002(1) 9 5 ?
O2 O2 O2 45.002(10) 33_666 25_666 ?
O2 O2 O2 45.002(11) 29_666 25_666 ?
O2 O2 O2 45.002(10) 9 25_666 ?
O2 O2 O2 45.002(7) 5 25_666 ?

_refine_diff_density_max         0.444
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.077

_shelx_res_file                  
;
TITL empirical_absorption in Im-3
    empirical_absorption_disorder.res
    created by SHELXL-2018/3 at 11:39:49 on 09-Jan-2020
REM Im-3 (#204 in standard setting)
CELL 0.71073  12.047473  12.047473  12.047473  90.0000  90.0000  90.0000
ZERR    8.00   0.000159   0.000159   0.000159   0.0000   0.0000   0.0000
LATT  2
SYMM -x,-y, z
SYMM -x, y,-z
SYMM  x,-y,-z
SYMM  z, x, y
SYMM  z,-x,-y
SYMM -z,-x, y
SYMM -z, x,-y
SYMM  y, z, x
SYMM -y, z,-x
SYMM  y,-z,-x
SYMM -y,-z, x
SFAC C H O Fe N
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
UNIT 36 76.0 50.0 8.00 6.0
LIST 4! automatically inserted. Change 6 to 4 for CHECKCIF!!
ACTA
size 0.08 0.11 0.11
temp 25
L.S. 50
EQIV $1 +x, -y, -z
EQIV $2 1-x, -y, +z
EQIV $3 +x, +y, -z
EQIV $4 +x, 1-y, 1-z

FREE N2 N2_$1
FREE N1 N1_$2
DELU C2 N1 N2
SIMU C2 N1 N2
RIGU C2 N1 N2
BOND
FMAP 2
PLAN 20
WGHT    0.049300    3.972500
FVAR       0.89901   0.21793   0.28207   0.69877   0.80123   0.34570   0.35682
FE1   4    0.250000    0.250000    0.250000    10.16667    0.02177    0.02177 =
         0.02177    0.00065    0.00065    0.00065
O1    3    0.408466    0.307015    0.204576    11.00000    0.02747    0.04243 =
         0.04700    0.00926   -0.00053    0.00024
C1    1    0.500000    0.279661    0.241302    10.50000    0.02936    0.03806 =
         0.04162    0.01304    0.00000    0.00000
AFIX  43
H1    2    0.500000    0.233549    0.303211    10.50000   -1.20000
AFIX   0
C2    1    0.500000   -0.097127    0.000000    10.25000    0.05056    0.12730 =
         0.07376    0.00000    0.00000    0.00000
DFIX H2A C2 1.0 0.01
DFIX H2B C2 1.0 0.01
DFIX H2A H2B 1.0 0.1
DFIX H2B H2B_$3 1.5 0.01
H2A   2    0.561058   -0.153408    0.000000    10.37500   -1.20000
H2B   2    0.500000   -0.151507    0.062374    10.37500   -1.20000
PART 1
N1    5    0.436591    0.000000    0.000000    10.06250    0.06013    0.12553 =
         0.05256    0.00000    0.00000    0.00000
DFIX N1 H3 0.9 0.01
DFIX H3 H3_$1 1.5 0.1
H3    2    0.394902    0.000000    0.062132    10.12500   -1.20000
PART 2
H4    2    0.442303    0.000000   -0.104290    10.12500   -1.20000
N2    5    0.500000   -0.026162   -0.064289    10.06250    0.02024
DFIX N2 H4 0.9 0.01
DFIX H4 H4_$2 1.5 0.1
PART 0
O2    3    0.551647    0.500000    0.500000    10.04167    0.11498
DFIX O2 H5 0.9 0.01
DFIX H5 H5_$4 1.3 0.1
H5    2    0.602229    0.445308    0.500000    10.08333   -1.20000
HKLF 4




REM  empirical_absorption in Im-3
REM wR2 = 0.1066, GooF = S = 1.104, Restrained GooF = 1.086 for all data
REM R1 = 0.0373 for 348 Fo > 4sig(Fo) and 0.0500 for all 445 data
REM 47 parameters refined using 32 restraints

END

WGHT      0.0507      3.6345

REM Highest difference peak  0.444,  deepest hole -0.290,  1-sigma level  0.077
Q1    1   0.6142  0.5000  0.5000  10.25000  0.05    0.44
Q2    1   0.5000 -0.1467  0.0000  10.25000  0.05    0.26
Q3    1   0.3424  0.2503  0.2003  11.00000  0.05    0.23
Q4    1   0.5000 -0.0690 -0.0813  10.50000  0.05    0.22
Q5    1   0.4063  0.3156  0.2782  11.00000  0.05    0.22
Q6    1   0.4075  0.1974  0.1999  11.00000  0.05    0.20
Q7    1   0.5711 -0.0840 -0.0392  11.00000  0.05    0.18
Q8    1   0.5512 -0.0916  0.0687  11.00000  0.05    0.17
Q9    1   0.4216  0.3282  0.2559  11.00000  0.05    0.16
Q10   1   0.3939  0.1936  0.3206  11.00000  0.05    0.16
Q11   1   0.5722 -0.1371  0.1311  11.00000  0.05    0.15
Q12   1   0.4399 -0.0608 -0.1413  11.00000  0.05    0.14
Q13   1   0.5000 -0.0776 -0.1902  10.50000  0.05    0.14
Q14   1   0.4066  0.0000 -0.2018  10.50000  0.05    0.13
Q15   1   0.5000  0.0000 -0.1501  10.25000  0.05    0.13
Q16   1   0.5000  0.0000 -0.0797  10.25000  0.05    0.12
Q17   1   0.5000  0.1914  0.2584  10.50000  0.05    0.12
Q18   1   0.2590  0.1942  0.1636  11.00000  0.05    0.12
Q19   1   0.5000  0.2748  0.3620  10.50000  0.05    0.12
Q20   1   0.3071  0.2562  0.1613  11.00000  0.05    0.12
;
_shelx_res_checksum              2280

# start Validation Reply Form
_vrf_PLAT088_DMAFeFe_H2O-4       
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.47 Note  
RESPONSE: Due to the disorder in the DMA cation and water molecule, the H
atoms had to be restrained with distance restraints and not the usual riding
constraints applied to H atoms. This considerably increases the number of 
parameters.
;
_vrf_PLAT241_DMAFeFe_H2O-4       
;
PROBLEM: High   MainMol Ueq as Compared to Neighbors of         C2 Check   
RESPONSE: C2 is part of the DMA cation which exhibits disorder. The neighbouring
N atoms are split over several sites, therefore their thermal parameters
are smaller than the ones from C that are fixed on one site.
;
_vrf_PLAT329_DMAFeFe_H2O-4       
;
PROBLEM: Carbon Atom Hybridisation Unclear for ..........         C2 Check 
RESPONSE: This C atom is part of the DMA cation, and is connected to 4
main disordered N sites, of which two are further split along the bonding
direction.
;
_vrf_PLAT906_DMAFeFe_H2O-4       
;
PROBLEM: Large K Value in the Analysis of Variance ......      6.785 Check 
RESPONSE: This is observed only for the highest resolution data at 0.73A.
;
_vrf_PLAT975_DMAFeFe_H2O-4       
;
PROBLEM: Check Calcd Resid. Dens.  0.66A   From O2              0.46 eA-3  
RESPONSE: This was checked, but since the O2 is the disordered water molecule,
the modelled position may be an approximation to a more complex disordering 
pattern.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_18_PJS055_07_240_00
_database_code_depnum_ccdc_archive 'CCDC 1990950'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0219(8)
_cell_length_b                   12.0219(8)
_cell_length_c                   12.0219(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1737.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    240.0(4)
_cell_measurement_reflns_used    423
_cell_measurement_theta_min      4.1210
_cell_measurement_theta_max      29.1250

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.724
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.784
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      240.0(4)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            896
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.152
_diffrn_reflns_theta_max         29.529
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             395
_reflns_number_gt                333
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0484P)²+2.6877P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         395
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.077
_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 0.750000 0.250000 0.250000 0.0121(3) Uani 1 6 d S T P . .
O1 O 0.79555(19) 0.40828(16) 0.3072(2) 0.0267(5) Uani 1 1 d . . . . .
C1 C 0.7588(4) 0.500000 0.2804(4) 0.0254(10) Uani 1 2 d S T P . .
H1 H 0.696263 0.500000 0.234880 0.030 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3945(11) 0.500000 0.074(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.572(4) 0.100(11) Uiso 0.25 4 d S U P . .
N2 N 0.950(4) 0.500000 0.500000 0.100(11) Uiso 0.25 4 d S U P . .
O2 O 0.551(3) 0.500000 0.500000 0.069(16) Uiso 0.1667 4 d DS . P . .
H3 H 0.608(10) 0.500000 0.532(4) 0.082 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0121(3) 0.0121(3) 0.0121(3) 0.0009(2) -0.0009(2) -0.0009(2)
O1 0.0336(14) 0.0171(10) 0.0295(12) 0.0005(8) -0.0053(10) 0.0010(9)
C1 0.028(2) 0.0165(19) 0.031(3) 0.000 -0.0162(18) 0.000
C2 0.030(5) 0.118(10) 0.073(7) 0.000 0.000 0.000

_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 2.096(2) . ?
Fe1 O1 2.096(2) 37_655 ?
Fe1 O1 2.096(2) 46_554 ?
Fe1 O1 2.096(2) 10_656 ?
Fe1 O1 2.096(2) 7_665 ?
Fe1 O1 2.096(2) 43_545 ?
O1 C1 1.231(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.40(3) . ?
C2 N2 1.40(3) 25_766 ?
C2 N1 1.53(3) . ?
C2 N1 1.53(3) 25_766 ?
N1 N2 1.05(5) . ?
N1 N2 1.05(5) 25_766 ?
N1 N1 1.72(11) 25_766 ?
N2 N2 1.21(11) 25_766 ?
O2 O2 0.87(4) 33_666 ?
O2 O2 0.87(4) 29_666 ?
O2 O2 0.87(4) 9 ?
O2 O2 0.87(4) 5 ?
O2 O2 1.23(6) 25_666 ?
O2 H3 0.79(10) . ?
O2 H3 0.79(10) 4_566 ?

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 180.0 . 37_655 ?
O1 Fe1 O1 88.57(9) . 46_554 ?
O1 Fe1 O1 91.43(9) 37_655 46_554 ?
O1 Fe1 O1 91.43(9) . 10_656 ?
O1 Fe1 O1 88.57(9) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 91.43(9) . 7_665 ?
O1 Fe1 O1 88.57(9) 37_655 7_665 ?
O1 Fe1 O1 88.57(9) 46_554 7_665 ?
O1 Fe1 O1 91.43(9) 10_656 7_665 ?
O1 Fe1 O1 88.57(9) . 43_545 ?
O1 Fe1 O1 91.43(9) 37_655 43_545 ?
O1 Fe1 O1 91.43(9) 46_554 43_545 ?
O1 Fe1 O1 88.57(9) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
C1 O1 Fe1 129.3(2) . . ?
O1 C1 O1 127.2(4) 27_565 . ?
O1 C1 H1 116.4 27_565 . ?
O1 C1 H1 116.4 . . ?
N2 C2 N2 51(4) . 25_766 ?
N2 C2 N1 41.6(15) . . ?
N2 C2 N1 41.6(15) 25_766 . ?
N2 C2 N1 41.6(15) . 25_766 ?
N2 C2 N1 41.6(15) 25_766 25_766 ?
N1 C2 N1 68(3) . 25_766 ?
N2 N1 N2 70(6) . 25_766 ?
N2 N1 C2 63(2) . 25_766 ?
N2 N1 C2 63(2) 25_766 25_766 ?
N2 N1 C2 63(2) . . ?
N2 N1 C2 63(2) 25_766 . ?
C2 N1 C2 112(3) 25_766 . ?
N2 N1 N1 35(3) . 25_766 ?
N2 N1 N1 35(3) 25_766 25_766 ?
C2 N1 N1 55.9(17) 25_766 25_766 ?
C2 N1 N1 55.9(17) . 25_766 ?
N1 N2 N1 110(6) . 25_766 ?
N1 N2 N2 55(3) . 25_766 ?
N1 N2 N2 55(3) 25_766 25_766 ?
N1 N2 C2 76(2) . 25_766 ?
N1 N2 C2 76(2) 25_766 25_766 ?
N2 N2 C2 65(2) 25_766 25_766 ?
N1 N2 C2 76(2) . . ?
N1 N2 C2 76(2) 25_766 . ?
N2 N2 C2 65(2) 25_766 . ?
C2 N2 C2 129(4) 25_766 . ?
O2 O2 O2 60.001(7) 33_666 29_666 ?
O2 O2 O2 90.0 33_666 9 ?
O2 O2 O2 60.001(3) 29_666 9 ?
O2 O2 O2 60.001(1) 33_666 5 ?
O2 O2 O2 90.0 29_666 5 ?
O2 O2 O2 60.001(1) 9 5 ?
O2 O2 O2 45.001(7) 33_666 25_666 ?
O2 O2 O2 45.001(7) 29_666 25_666 ?
O2 O2 O2 45.001(7) 9 25_666 ?
O2 O2 O2 45.001(5) 5 25_666 ?
O2 O2 H3 165(6) 33_666 . ?
O2 O2 H3 128(3) 29_666 . ?
O2 O2 H3 105(6) 9 . ?
O2 O2 H3 128(3) 5 . ?
O2 O2 H3 150(6) 25_666 . ?
O2 O2 H3 105(6) 33_666 4_566 ?
O2 O2 H3 128(3) 29_666 4_566 ?
O2 O2 H3 165(6) 9 4_566 ?
O2 O2 H3 128(3) 5 4_566 ?
O2 O2 H3 150(6) 25_666 4_566 ?
H3 O2 H3 59(10) . 4_566 ?

_refine_diff_density_max         0.648
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.087

_shelx_res_file                  
;
TITL 18_PJS055_07_240_00 in Pn-3n
    18_PJS055_07_240_00.res
    created by SHELXL-2018/3 at 13:38:10 on 25-Sep-2019
REM Pn-3n (#222 in standard setting)
CELL 0.71073  12.021881  12.021881  12.021881  90.0000  90.0000  90.0000
ZERR    8.00   0.000809   0.000809   0.000809   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.048400    2.687700
BASF   0.52346
FVAR       1.40309   0.10047
FE1   5    0.750000    0.250000    0.250000    10.16667    0.01212    0.01212 =
         0.01212    0.00087   -0.00087   -0.00087
O1    4    0.795549    0.408284    0.307230    11.00000    0.03362    0.01705 =
         0.02949    0.00054   -0.00533    0.00099
C1    1    0.758784    0.500000    0.280439    10.50000    0.02826    0.01654 =
         0.03145    0.00000   -0.01623    0.00000
AFIX  43
H1    2    0.696263    0.500000    0.234880    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.394498    0.500000    10.25000    0.03045    0.11758 =
         0.07311    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.571532    10.06250   21.00000
N2    3    0.949809    0.500000    0.500000    10.06250   21.00000
O2    4    0.551008    0.500000    0.500000    10.04167    0.06853
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.607869    0.500000    0.532377    10.08333   -1.20000
HKLF 4




REM  18_PJS055_07_240_00 in Pn-3n
REM wR2 = 0.0961, GooF = S = 1.078, Restrained GooF = 1.077 for all data
REM R1 = 0.0361 for 333 Fo > 4sig(Fo) and 0.0429 for all 395 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0487      2.6748

REM Highest difference peak  0.648,  deepest hole -0.989,  1-sigma level  0.087
Q1    1   1.0000  0.5282  0.5702  10.50000  0.05    0.57
Q2    1   0.5849  0.5521  0.5000  10.50000  0.05    0.37
Q3    1   1.0000  0.4252  0.5000  10.25000  0.05    0.36
Q4    1   0.9227  0.5000  0.5000  10.25000  0.05    0.29
Q5    1   1.0565  0.3981  0.4423  11.00000  0.05    0.27
Q6    1   0.8179  0.3165  0.2514  11.00000  0.05    0.26
Q7    1   0.6797  0.3174  0.2476  11.00000  0.05    0.25
Q8    1   1.0522  0.3235  0.5000  10.50000  0.05    0.24
Q9    1   0.7488  0.4206  0.3171  11.00000  0.05    0.23
Q10   1   1.0000  0.5822  0.6399  10.50000  0.05    0.21
Q11   1   1.0453  0.2928  0.5000  10.50000  0.05    0.19
Q12   1   0.9253  0.5394  0.5000  10.50000  0.05    0.18
Q13   1   0.8162  0.4262  0.2562  11.00000  0.05    0.17
Q14   1   0.7765  0.3559  0.2952  11.00000  0.05    0.17
Q15   1   0.9116  0.5000  0.5895  10.50000  0.05    0.16
Q16   1   0.7978  0.4341  0.3578  11.00000  0.05    0.16
Q17   1   0.7324  0.3956  0.1696  11.00000  0.05    0.15
Q18   1   0.6695  0.5883  0.2552  11.00000  0.05    0.15
Q19   1   0.7530  0.3892  0.2185  11.00000  0.05    0.13
Q20   1   0.7694  0.5000  0.1524  10.50000  0.05    0.13
;
_shelx_res_checksum              48971

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_07_240_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_07_240_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_07_240_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT242_18_PJS055_07_240_00 
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of         C2 Check 
RESPONSE: The C2 atom is part of the DMA cation and neighbours the N position,
which is dynamically disordered.
;
_vrf_PLAT911_18_PJS055_07_240_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
####################################################################### 
# 
# 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_exp18_PJS054_01_80_00
_database_code_depnum_ccdc_archive 'CCDC 1990943'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3



_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   11.9923(3)
_cell_length_b                   11.9923(3)
_cell_length_c                   11.9923(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1724.67(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    80.0(9)
_cell_measurement_reflns_used    2876
_cell_measurement_theta_min      3.7820
_cell_measurement_theta_max      29.4340

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.737
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.680
_oxdiff_exptl_absorpt_empirical_full_max 1.404
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80.0(9)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6214
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.398
_diffrn_reflns_theta_max         29.609
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             444
_reflns_number_gt                398
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0333P)²+10.0332P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         444
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1051
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_restrained_S_all      1.233
_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 0.750000 0.250000 0.250000 0.0076(3) Uani 1 6 d S T P . .
O1 O 0.7958(3) 0.40775(19) 0.3084(3) 0.0204(6) Uani 1 1 d . . . . .
C1 C 0.7586(5) 0.500000 0.2809(4) 0.0157(11) Uani 1 2 d S T P . .
H1 H 0.696133 0.499999 0.234926 0.019 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3942(15) 0.500000 0.069(4) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.563(4) 0.057(8) Uiso 0.25 4 d S U P . .
N2 N 0.937(4) 0.500000 0.500000 0.057(8) Uiso 0.25 4 d S U P . .
O2 O 0.563(4) 0.500000 0.500000 0.09(3) Uiso 0.1667 4 d DS . P . .
H3 H 0.620(11) 0.500000 0.533(4) 0.103 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0076(3) 0.0076(3) 0.0076(3) 0.0004(3) -0.0004(3) -0.0004(3)
O1 0.0314(17) 0.0110(11) 0.0187(13) 0.0011(10) -0.0050(12) -0.0006(11)
C1 0.019(3) 0.0127(19) 0.015(2) 0.000 -0.004(2) 0.000
C2 0.024(6) 0.156(15) 0.027(6) 0.000 0.000 0.000

_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 2.090(2) 37_655 ?
Fe1 O1 2.090(2) 46_554 ?
Fe1 O1 2.090(2) 10_656 ?
Fe1 O1 2.090(2) 7_665 ?
Fe1 O1 2.090(2) 43_545 ?
Fe1 O1 2.090(2) . ?
O1 C1 1.237(3) . ?
C1 H1 0.9300 . ?
C2 N1 1.47(3) 25_766 ?
C2 N1 1.47(3) . ?
C2 N2 1.48(3) . ?
C2 N2 1.48(3) 25_766 ?
N1 N2 1.07(4) . ?
N1 N2 1.07(4) 25_766 ?
N1 N1 1.50(9) 25_766 ?
N2 N2 1.52(10) 25_766 ?
O2 O2 1.06(7) 33_666 ?
O2 O2 1.06(7) 29_666 ?
O2 O2 1.06(7) 9 ?
O2 O2 1.06(7) 5 ?
O2 O2 1.50(10) 25_666 ?
O2 H3 0.80(10) . ?
O2 H3 0.80(10) 4_566 ?

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 91.29(13) 37_655 46_554 ?
O1 Fe1 O1 88.71(13) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 88.71(13) 37_655 7_665 ?
O1 Fe1 O1 88.71(13) 46_554 7_665 ?
O1 Fe1 O1 91.29(13) 10_656 7_665 ?
O1 Fe1 O1 91.29(13) 37_655 43_545 ?
O1 Fe1 O1 91.29(13) 46_554 43_545 ?
O1 Fe1 O1 88.71(13) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.0 37_655 . ?
O1 Fe1 O1 88.71(13) 46_554 . ?
O1 Fe1 O1 91.29(13) 10_656 . ?
O1 Fe1 O1 91.28(13) 7_665 . ?
O1 Fe1 O1 88.72(13) 43_545 . ?
C1 O1 Fe1 128.7(3) . . ?
O1 C1 O1 126.8(5) 27_565 . ?
O1 C1 H1 116.6 27_565 . ?
O1 C1 H1 116.6 . . ?
N1 C2 N1 61(3) 25_766 . ?
N1 C2 N2 42.4(13) 25_766 . ?
N1 C2 N2 42.4(13) . . ?
N1 C2 N2 42.4(13) 25_766 25_766 ?
N1 C2 N2 42.4(13) . 25_766 ?
N2 C2 N2 62(3) . 25_766 ?
N2 N1 N2 91(6) . 25_766 ?
N2 N1 C2 69(2) . . ?
N2 N1 C2 69(2) 25_766 . ?
N2 N1 C2 69(2) . 25_766 ?
N2 N1 C2 69(2) 25_766 25_766 ?
C2 N1 C2 119(3) . 25_766 ?
N2 N1 N1 45(3) . 25_766 ?
N2 N1 N1 45(3) 25_766 25_766 ?
C2 N1 N1 59.4(17) . 25_766 ?
C2 N1 N1 59.4(17) 25_766 25_766 ?
N1 N2 N1 89(6) 25_766 . ?
N1 N2 C2 69(2) 25_766 . ?
N1 N2 C2 69(2) . . ?
N1 N2 C2 69(2) 25_766 25_766 ?
N1 N2 C2 69(2) . 25_766 ?
C2 N2 C2 118(3) . 25_766 ?
N1 N2 N2 45(3) 25_766 25_766 ?
N1 N2 N2 45(3) . 25_766 ?
C2 N2 N2 59.1(17) . 25_766 ?
C2 N2 N2 59.1(17) 25_766 25_766 ?
O2 O2 O2 60.002(11) 33_666 29_666 ?
O2 O2 O2 90.003(3) 33_666 9 ?
O2 O2 O2 60.002(4) 29_666 9 ?
O2 O2 O2 60.002(2) 33_666 5 ?
O2 O2 O2 90.003(1) 29_666 5 ?
O2 O2 O2 60.002(3) 9 5 ?
O2 O2 O2 45.002(7) 33_666 25_666 ?
O2 O2 O2 45.002(8) 29_666 25_666 ?
O2 O2 O2 45.002(7) 9 25_666 ?
O2 O2 O2 45.002(4) 5 25_666 ?
O2 O2 H3 165(6) 33_666 . ?
O2 O2 H3 128(3) 29_666 . ?
O2 O2 H3 105(6) 9 . ?
O2 O2 H3 128(3) 5 . ?
O2 O2 H3 150(6) 25_666 . ?
O2 O2 H3 105(6) 33_666 4_566 ?
O2 O2 H3 128(3) 29_666 4_566 ?
O2 O2 H3 165(6) 9 4_566 ?
O2 O2 H3 128(3) 5 4_566 ?
O2 O2 H3 150(6) 25_666 4_566 ?
H3 O2 H3 59(10) . 4_566 ?

_refine_diff_density_max         0.715
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.120

_shelx_res_file                  
;
TITL exp18_PJS054_01_80_00 in Pm-3m
    exp18_PJS054_01_80_00.res
    created by SHELXL-2018/3 at 11:48:06 on 25-Sep-2019
REM Pm-3m (#221 in standard setting)
CELL 0.71073  11.992277  11.992277  11.992277  90.0000  90.0000  90.0000
ZERR    8.00   0.000306   0.000306   0.000306   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.033300   10.033200
BASF   0.52684
FVAR       1.74009   0.05692
FE1   5    0.750000    0.250000    0.250000    10.16667    0.00762    0.00762 =
         0.00762    0.00044   -0.00044   -0.00044
O1    4    0.795765    0.407751    0.308376    11.00000    0.03139    0.01101 =
         0.01868    0.00111   -0.00495   -0.00063
C1    1    0.758554    0.500000    0.280944    10.50000    0.01945    0.01266 =
         0.01501    0.00000   -0.00422    0.00000
AFIX  43
H1    2    0.696133    0.499999    0.234926    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.394183    0.500000    10.25000    0.02372    0.15624 =
         0.02725    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.562662    10.06250   21.00000
N2    3    0.936694    0.500000    0.500000    10.06250   21.00000
O2    4    0.562588    0.500000    0.500000    10.04167    0.08543
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.620282    0.500000    0.532739    10.08333   -1.20000
HKLF 4




REM  exp18_PJS054_01_80_00 in Pm-3m
REM wR2 = 0.1051, GooF = S = 1.234, Restrained GooF = 1.233 for all data
REM R1 = 0.0437 for 398 Fo > 4sig(Fo) and 0.0499 for all 444 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0324     10.3193

REM Highest difference peak  0.715,  deepest hole -0.347,  1-sigma level  0.120
Q1    1   0.6176  0.5000  0.5000  10.25000  0.05    0.71
Q2    1   0.9245  0.5526  0.5000  10.50000  0.05    0.57
Q3    1   1.0000  0.5524  0.5684  10.50000  0.05    0.53
Q4    1   1.0491  0.3897  0.4436  11.00000  0.05    0.51
Q5    1   0.5000  0.5000  0.5000  10.04167  0.05    0.46
Q6    1   0.5832  0.5000  0.5694  10.50000  0.05    0.45
Q7    1   0.5703  0.5252  0.5598  11.00000  0.05    0.44
Q8    1   1.0000  0.5000  0.6381  10.25000  0.05    0.43
Q9    1   1.0000  0.4398  0.5000  10.25000  0.05    0.42
Q10   1   1.0000  0.6002  0.6541  10.50000  0.05    0.37
Q11   1   1.0429  0.3388  0.5000  10.50000  0.05    0.36
Q12   1   1.0000  0.3492  0.5000  10.25000  0.05    0.36
Q13   1   0.9114  0.5000  0.5758  10.50000  0.05    0.30
Q14   1   1.0681  0.3491  0.5000  10.50000  0.05    0.29
Q15   1   0.7735  0.5000  0.3704  10.50000  0.05    0.23
Q16   1   0.6433  0.5000  0.2497  10.50000  0.05    0.22
Q17   1   0.7340  0.5000  0.4053  10.50000  0.05    0.21
Q18   1   1.0000  0.2447  0.5000  10.25000  0.05    0.21
Q19   1   0.8479  0.4162  0.2900  11.00000  0.05    0.20
Q20   1   0.7629  0.4320  0.3534  11.00000  0.05    0.20
;
_shelx_res_checksum              23648

# start Validation Reply Form
_vrf_PLAT043_exp18_PJS054_01_80_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_exp18_PJS054_01_80_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_exp18_PJS054_01_80_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT094_exp18_PJS054_01_80_00 
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.06 Report
RESPONSE: This arises from the aproximations used in modelling the disorder 
of the water and DMA. 
;
_vrf_PLAT906_exp18_PJS054_01_80_00 
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.038 Check 
RESPONSE: This is observed only for the highest resolution data at 0.72 A.
;
####################################################################### 
# 
# 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_18_PJS055_08_260_00
_database_code_depnum_ccdc_archive 'CCDC 1990951'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0296(7)
_cell_length_b                   12.0296(7)
_cell_length_c                   12.0296(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1740.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    260.0(6)
_cell_measurement_reflns_used    429
_cell_measurement_theta_min      4.0690
_cell_measurement_theta_max      29.1090

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.721
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.784
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      260.0(6)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            901
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.150
_diffrn_reflns_theta_max         29.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             396
_reflns_number_gt                332
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0447P)²+2.0810P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         396
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.160
_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 0.750000 0.250000 0.250000 0.0140(3) Uani 1 6 d S T P . .
O1 O 0.79569(19) 0.40818(16) 0.3071(2) 0.0285(5) Uani 1 1 d . . . . .
C1 C 0.7587(4) 0.500000 0.2799(5) 0.0295(11) Uani 1 2 d S T P . .
H1 H 0.696446 0.499999 0.234048 0.035 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3942(12) 0.500000 0.081(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.575(5) 0.106(12) Uiso 0.25 4 d S U P . .
N2 N 0.956(5) 0.500000 0.500000 0.106(12) Uiso 0.25 4 d S U P . .
O2 O 0.549(4) 0.500000 0.500000 0.10(3) Uiso 0.1667 4 d DS . P . .
H3 H 0.604(10) 0.500000 0.533(4) 0.115 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0140(3) 0.0140(3) 0.0140(3) 0.0009(2) -0.0009(2) -0.0009(2)
O1 0.0344(15) 0.0196(10) 0.0315(12) 0.0014(9) -0.0059(11) 0.0019(9)
C1 0.035(3) 0.018(2) 0.035(3) 0.000 -0.0153(19) 0.000
C2 0.039(6) 0.123(11) 0.082(8) 0.000 0.000 0.000

_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 2.096(2) 37_655 ?
Fe1 O1 2.096(2) 46_554 ?
Fe1 O1 2.096(2) 10_656 ?
Fe1 O1 2.096(2) 7_665 ?
Fe1 O1 2.096(2) 43_545 ?
Fe1 O1 2.096(2) . ?
O1 C1 1.235(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.38(3) 25_766 ?
C2 N2 1.38(3) . ?
C2 N1 1.56(3) 25_766 ?
C2 N1 1.56(3) . ?
N1 N2 1.04(5) 25_766 ?
N1 N2 1.04(5) . ?
N1 N1 1.79(11) 25_766 ?
N2 N2 1.05(12) 25_766 ?
O2 O2 0.83(7) 33_666 ?
O2 O2 0.83(7) 29_666 ?
O2 O2 0.83(7) 9 ?
O2 O2 0.83(7) 5 ?
O2 O2 1.17(9) 25_666 ?
O2 H3 0.78(10) . ?
O2 H3 0.78(10) 4_566 ?

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 91.51(9) 37_655 46_554 ?
O1 Fe1 O1 88.49(9) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 88.49(9) 37_655 7_665 ?
O1 Fe1 O1 88.49(9) 46_554 7_665 ?
O1 Fe1 O1 91.51(9) 10_656 7_665 ?
O1 Fe1 O1 91.51(9) 37_655 43_545 ?
O1 Fe1 O1 91.51(9) 46_554 43_545 ?
O1 Fe1 O1 88.49(9) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.0 37_655 . ?
O1 Fe1 O1 88.49(9) 46_554 . ?
O1 Fe1 O1 91.51(9) 10_656 . ?
O1 Fe1 O1 91.51(9) 7_665 . ?
O1 Fe1 O1 88.49(9) 43_545 . ?
C1 O1 Fe1 129.1(3) . . ?
O1 C1 O1 126.9(5) . 27_565 ?
O1 C1 H1 116.6 . . ?
O1 C1 H1 116.6 27_565 . ?
N2 C2 N2 45(4) 25_766 . ?
N2 C2 N1 40.9(16) 25_766 25_766 ?
N2 C2 N1 40.9(16) . 25_766 ?
N2 C2 N1 40.9(16) 25_766 . ?
N2 C2 N1 40.9(16) . . ?
N1 C2 N1 70(3) 25_766 . ?
N2 N1 N2 61(7) 25_766 . ?
N2 N1 C2 60(2) 25_766 25_766 ?
N2 N1 C2 60(2) . 25_766 ?
N2 N1 C2 60(2) 25_766 . ?
N2 N1 C2 60(2) . . ?
C2 N1 C2 110(3) 25_766 . ?
N2 N1 N1 30(3) 25_766 25_766 ?
N2 N1 N1 30(3) . 25_766 ?
C2 N1 N1 54.8(17) 25_766 25_766 ?
C2 N1 N1 54.8(17) . 25_766 ?
N2 N2 N1 60(3) 25_766 25_766 ?
N2 N2 N1 60(3) 25_766 . ?
N1 N2 N1 119(7) 25_766 . ?
N2 N2 C2 68(2) 25_766 25_766 ?
N1 N2 C2 79(2) 25_766 25_766 ?
N1 N2 C2 79(2) . 25_766 ?
N2 N2 C2 68(2) 25_766 . ?
N1 N2 C2 79(2) 25_766 . ?
N1 N2 C2 79(2) . . ?
C2 N2 C2 135(4) 25_766 . ?
O2 O2 O2 60.002(11) 33_666 29_666 ?
O2 O2 O2 90.0 33_666 9 ?
O2 O2 O2 60.002(5) 29_666 9 ?
O2 O2 O2 60.002(2) 33_666 5 ?
O2 O2 O2 90.0 29_666 5 ?
O2 O2 O2 60.002(1) 9 5 ?
O2 O2 O2 45.002(12) 33_666 25_666 ?
O2 O2 O2 45.002(11) 29_666 25_666 ?
O2 O2 O2 45.002(12) 9 25_666 ?
O2 O2 O2 45.002(8) 5 25_666 ?
O2 O2 H3 166(6) 33_666 . ?
O2 O2 H3 127(3) 29_666 . ?
O2 O2 H3 104(6) 9 . ?
O2 O2 H3 127(3) 5 . ?
O2 O2 H3 149(6) 25_666 . ?
O2 O2 H3 104(6) 33_666 4_566 ?
O2 O2 H3 127(3) 29_666 4_566 ?
O2 O2 H3 166(6) 9 4_566 ?
O2 O2 H3 127(3) 5 4_566 ?
O2 O2 H3 149(6) 25_666 4_566 ?
H3 O2 H3 61(10) . 4_566 ?

_refine_diff_density_max         0.752
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.101

_shelx_res_file                  
;
TITL 18_PJS055_08_260_00 in Im-3m
    18_PJS055_08_260_00.res
    created by SHELXL-2018/3 at 13:39:49 on 25-Sep-2019
REM Im-3m (#229 in standard setting)
CELL 0.71073  12.029648  12.029648  12.029648  90.0000  90.0000  90.0000
ZERR    8.00   0.000733   0.000733   0.000733   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.044700    2.081000
BASF   0.53007
FVAR       1.45223   0.10635
FE1   5    0.750000    0.250000    0.250000    10.16667    0.01405    0.01405 =
         0.01405    0.00087   -0.00087   -0.00087
O1    4    0.795690    0.408185    0.307111    11.00000    0.03438    0.01962 =
         0.03146    0.00139   -0.00589    0.00186
C1    1    0.758703    0.500000    0.279882    10.50000    0.03534    0.01762 =
         0.03547    0.00000   -0.01533    0.00000
AFIX  43
H1    2    0.696446    0.499999    0.234048    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.394214    0.500000    10.25000    0.03938    0.12265 =
         0.08155    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.574529    10.06250   21.00000
N2    3    0.956493    0.500000    0.500000    10.06250   21.00000
O2    4    0.548657    0.500000    0.500000    10.04167    0.09611
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.604458    0.500000    0.533172    10.08333   -1.20000
HKLF 4




REM  18_PJS055_08_260_00 in Im-3m
REM wR2 = 0.1040, GooF = S = 1.161, Restrained GooF = 1.160 for all data
REM R1 = 0.0382 for 332 Fo > 4sig(Fo) and 0.0460 for all 396 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0447      2.1078

REM Highest difference peak  0.752,  deepest hole -1.486,  1-sigma level  0.101
Q1    1   1.0000  0.4276  0.5000  10.25000  0.05    0.59
Q2    1   1.0000  0.5265  0.5676  10.50000  0.05    0.58
Q3    1   0.9275  0.5000  0.5000  10.25000  0.05    0.48
Q4    1   0.5759  0.5000  0.5353  10.50000  0.05    0.43
Q5    1   1.0000  0.2507  0.5000  10.25000  0.05    0.34
Q6    1   1.0589  0.3972  0.4433  11.00000  0.05    0.33
Q7    1   0.7549  0.5000  0.5000  10.25000  0.05    0.30
Q8    1   0.7476  0.4339  0.3065  11.00000  0.05    0.23
Q9    1   1.0000  0.3300  0.5000  10.25000  0.05    0.23
Q10   1   0.7550  0.3629  0.2598  11.00000  0.05    0.22
Q11   1   0.7711  0.3285  0.3190  11.00000  0.05    0.20
Q12   1   0.8000  0.5000  0.2430  10.50000  0.05    0.20
Q13   1   0.8369  0.3240  0.2448  11.00000  0.05    0.19
Q14   1   1.0557  0.3588  0.5000  10.50000  0.05    0.18
Q15   1   0.8138  0.4256  0.2480  11.00000  0.05    0.18
Q16   1   0.6599  0.5608  0.2486  11.00000  0.05    0.17
Q17   1   1.0876  0.2820  0.5000  10.50000  0.05    0.16
Q18   1   0.8450  0.4429  0.2778  11.00000  0.05    0.16
Q19   1   0.7420  0.1763  0.3017  11.00000  0.05    0.16
Q20   1   1.0474  0.2889  0.4704  11.00000  0.05    0.16
;
_shelx_res_checksum              50619

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_08_260_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_08_260_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_08_260_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT242_18_PJS055_08_260_00 
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of         C2 Check 
RESPONSE: The C2 atom is part of the DMA cation and neighbours the N position,
which is dynamically disordered.
;
_vrf_PLAT911_18_PJS055_08_260_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
####################################################################### 
# 
# 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_18_PJS055_04_180_00
_database_code_depnum_ccdc_archive 'CCDC 1990947'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0082(7)
_cell_length_b                   12.0082(7)
_cell_length_c                   12.0082(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1731.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    180.0(3)
_cell_measurement_reflns_used    427
_cell_measurement_theta_min      4.1330
_cell_measurement_theta_max      28.6840

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.730
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.916
_oxdiff_exptl_absorpt_empirical_full_max 1.117
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180.0(3)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            885
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.157
_diffrn_reflns_theta_max         29.566
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             389
_reflns_number_gt                338
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0288P)²+4.5699P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         389
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_restrained_S_all      1.214
_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 0.750000 0.250000 0.250000 0.0099(3) Uani 1 6 d S T P . .
O1 O 0.7956(2) 0.40801(18) 0.3075(2) 0.0247(5) Uani 1 1 d . . . . .
C1 C 0.7589(5) 0.500000 0.2801(4) 0.0217(11) Uani 1 2 d S T P . .
H1 H 0.696931 0.500000 0.233637 0.026 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3936(12) 0.500000 0.063(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.567(4) 0.068(8) Uiso 0.25 4 d S U P . .
N2 N 0.938(4) 0.500000 0.500000 0.068(8) Uiso 0.25 4 d S U P . .
O2 O 0.555(3) 0.500000 0.500000 0.08(2) Uiso 0.1667 4 d DS . P . .
H3 H 0.610(10) 0.500000 0.533(4) 0.100 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0099(3) 0.0099(3) 0.0099(3) 0.0004(3) -0.0004(3) -0.0004(3)
O1 0.0339(17) 0.0131(11) 0.0271(14) 0.0012(10) -0.0073(11) 0.0001(10)
C1 0.028(3) 0.014(2) 0.023(3) 0.000 -0.0094(19) 0.000
C2 0.030(6) 0.109(10) 0.051(7) 0.000 0.000 0.000

_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 2.092(2) 37_655 ?
Fe1 O1 2.092(2) 46_554 ?
Fe1 O1 2.092(2) 10_656 ?
Fe1 O1 2.092(2) 7_665 ?
Fe1 O1 2.092(2) 43_545 ?
Fe1 O1 2.092(2) . ?
O1 C1 1.234(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.48(3) 25_766 ?
C2 N2 1.48(3) . ?
C2 N1 1.51(3) . ?
C2 N1 1.51(3) 25_766 ?
N1 N2 1.10(3) . ?
N1 N2 1.10(4) 25_766 ?
N1 N1 1.62(9) 25_766 ?
N2 N2 1.49(9) 25_766 ?
O2 O2 0.93(6) 33_666 ?
O2 O2 0.93(6) 29_666 ?
O2 O2 0.93(6) 9 ?
O2 O2 0.93(6) 5 ?
O2 O2 1.31(8) 25_666 ?
O2 H3 0.77(10) . ?
O2 H3 0.77(10) 4_566 ?

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 91.39(11) 37_655 46_554 ?
O1 Fe1 O1 88.61(11) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 88.61(11) 37_655 7_665 ?
O1 Fe1 O1 88.61(11) 46_554 7_665 ?
O1 Fe1 O1 91.39(11) 10_656 7_665 ?
O1 Fe1 O1 91.39(11) 37_655 43_545 ?
O1 Fe1 O1 91.39(11) 46_554 43_545 ?
O1 Fe1 O1 88.61(11) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.0 37_655 . ?
O1 Fe1 O1 88.61(11) 46_554 . ?
O1 Fe1 O1 91.39(11) 10_656 . ?
O1 Fe1 O1 91.39(11) 7_665 . ?
O1 Fe1 O1 88.61(11) 43_545 . ?
C1 O1 Fe1 129.1(3) . . ?
O1 C1 O1 127.1(5) . 27_565 ?
O1 C1 H1 116.5 . . ?
O1 C1 H1 116.5 27_565 . ?
N2 C2 N2 60(3) 25_766 . ?
N2 C2 N1 43.1(11) 25_766 . ?
N2 C2 N1 43.1(11) . . ?
N2 C2 N1 43.1(11) 25_766 25_766 ?
N2 C2 N1 43.1(11) . 25_766 ?
N1 C2 N1 65(3) . 25_766 ?
N2 N1 N2 85(5) . 25_766 ?
N2 N1 C2 66.8(19) . 25_766 ?
N2 N1 C2 66.8(19) 25_766 25_766 ?
N2 N1 C2 66.8(19) . . ?
N2 N1 C2 66.8(19) 25_766 . ?
C2 N1 C2 115(3) 25_766 . ?
N2 N1 N1 43(3) . 25_766 ?
N2 N1 N1 43(3) 25_766 25_766 ?
C2 N1 N1 57.6(14) 25_766 25_766 ?
C2 N1 N1 57.6(14) . 25_766 ?
N1 N2 N1 95(5) . 25_766 ?
N1 N2 C2 70.1(19) . 25_766 ?
N1 N2 C2 70.1(19) 25_766 25_766 ?
N1 N2 C2 70.1(19) . . ?
N1 N2 C2 70.1(19) 25_766 . ?
C2 N2 C2 120(3) 25_766 . ?
N1 N2 N2 47(3) . 25_766 ?
N1 N2 N2 47(3) 25_766 25_766 ?
C2 N2 N2 59.8(15) 25_766 25_766 ?
C2 N2 N2 59.8(15) . 25_766 ?
O2 O2 O2 59.999(9) 33_666 29_666 ?
O2 O2 O2 89.998(2) 33_666 9 ?
O2 O2 O2 59.999(5) 29_666 9 ?
O2 O2 O2 59.999(2) 33_666 5 ?
O2 O2 O2 89.998(1) 29_666 5 ?
O2 O2 O2 59.999(3) 9 5 ?
O2 O2 O2 44.999(8) 33_666 25_666 ?
O2 O2 O2 44.999(8) 29_666 25_666 ?
O2 O2 O2 44.999(7) 9 25_666 ?
O2 O2 O2 44.999(5) 5 25_666 ?
O2 O2 H3 166(6) 33_666 . ?
O2 O2 H3 127(3) 29_666 . ?
O2 O2 H3 104(6) 9 . ?
O2 O2 H3 127(3) 5 . ?
O2 O2 H3 149(6) 25_666 . ?
O2 O2 H3 104(6) 33_666 4_566 ?
O2 O2 H3 127(3) 29_666 4_566 ?
O2 O2 H3 166(6) 9 4_566 ?
O2 O2 H3 127(3) 5 4_566 ?
O2 O2 H3 149(6) 25_666 4_566 ?
H3 O2 H3 62(10) . 4_566 ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.080

_shelx_res_file                  
;
TITL 18_PJS055_04_180_00 in P4(2)32
    18_PJS055_04_180_00.res
    created by SHELXL-2018/3 at 13:32:34 on 25-Sep-2019
REM P4(2)32 (#208 in standard setting)
CELL 0.71073  12.008237  12.008237  12.008237  90.0000  90.0000  90.0000
ZERR    8.00   0.000698   0.000698   0.000698   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.028800    4.569900
BASF   0.52373
FVAR       1.38992   0.06790
FE1   5    0.750000    0.250000    0.250000    10.16667    0.00988    0.00988 =
         0.00988    0.00044   -0.00044   -0.00044
O1    4    0.795592    0.408008    0.307526    11.00000    0.03386    0.01308 =
         0.02713    0.00124   -0.00726    0.00009
C1    1    0.758921    0.500000    0.280063    10.50000    0.02779    0.01434 =
         0.02311    0.00000   -0.00941    0.00000
AFIX  43
H1    2    0.696931    0.500000    0.233637    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.393572    0.500000    10.25000    0.02964    0.10859 =
         0.05110    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.567420    10.06250   21.00000
N2    3    0.938055    0.500000    0.500000    10.06250   21.00000
O2    4    0.554660    0.500000    0.500000    10.04167    0.08322
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.609711    0.500000    0.533239    10.08333   -1.20000
HKLF 4




REM  18_PJS055_04_180_00 in P4(2)32
REM wR2 = 0.0883, GooF = S = 1.215, Restrained GooF = 1.214 for all data
REM R1 = 0.0348 for 338 Fo > 4sig(Fo) and 0.0413 for all 389 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0288      4.5627

REM Highest difference peak  0.397,  deepest hole -0.525,  1-sigma level  0.080
Q1    1   0.5718  0.5000  0.5792  10.50000  0.05    0.39
Q2    1   1.0000  0.4243  0.5000  10.25000  0.05    0.28
Q3    1   1.0000  0.5322  0.5626  10.50000  0.05    0.28
Q4    1   1.0566  0.3924  0.4431  11.00000  0.05    0.28
Q5    1   0.7508  0.3645  0.2479  11.00000  0.05    0.24
Q6    1   1.0764  0.3287  0.5000  10.50000  0.05    0.22
Q7    1   0.7653  0.3378  0.2961  11.00000  0.05    0.22
Q8    1   0.7831  0.3497  0.2893  11.00000  0.05    0.21
Q9    1   1.0000  0.2644  0.5000  10.25000  0.05    0.18
Q10   1   0.6410  0.5000  0.5000  10.25000  0.05    0.18
Q11   1   0.8533  0.3897  0.2499  11.00000  0.05    0.18
Q12   1   0.7701  0.4478  0.3918  11.00000  0.05    0.17
Q13   1   1.0371  0.2887  0.5000  10.50000  0.05    0.17
Q14   1   0.9058  0.5000  0.5867  10.50000  0.05    0.17
Q15   1   0.8386  0.4325  0.2917  11.00000  0.05    0.16
Q16   1   0.8000  0.2461  0.3263  11.00000  0.05    0.16
Q17   1   1.0000  0.5778  0.6226  10.50000  0.05    0.16
Q18   1   0.7935  0.5000  0.2458  10.50000  0.05    0.16
Q19   1   1.0000  0.6136  0.6632  10.50000  0.05    0.15
Q20   1   0.7494  0.4278  0.3155  11.00000  0.05    0.15
;
_shelx_res_checksum              1443

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_04_180_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_04_180_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_04_180_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT906_18_PJS055_04_180_00 
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.879 Check 
RESPONSE: This is observed only for the highest resolution data at 0.72 A.
;
_vrf_PLAT911_18_PJS055_04_180_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
####################################################################### 
# 
# 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_18_PJS055_03_160_00
_database_code_depnum_ccdc_archive 'CCDC 1990946'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0051(6)
_cell_length_b                   12.0051(6)
_cell_length_c                   12.0051(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1730.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    160.0(3)
_cell_measurement_reflns_used    436
_cell_measurement_theta_min      4.0920
_cell_measurement_theta_max      28.6860

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.731
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.907
_oxdiff_exptl_absorpt_empirical_full_max 1.127
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160.0(3)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            886
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.158
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             387
_reflns_number_gt                342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0330P)²+4.2926P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         387
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0977
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_restrained_S_all      1.237
_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 0.750000 0.250000 0.250000 0.0086(3) Uani 1 6 d S T P . .
O1 O 0.7955(2) 0.40782(19) 0.3080(2) 0.0229(6) Uani 1 1 d . . . . .
C1 C 0.7591(5) 0.500000 0.2795(5) 0.0206(12) Uani 1 2 d S T P . .
H1 H 0.698143 0.500000 0.231687 0.025 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3933(13) 0.500000 0.063(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.567(4) 0.065(8) Uiso 0.25 4 d S U P . .
N2 N 0.936(4) 0.500000 0.500000 0.065(8) Uiso 0.25 4 d S U P . .
O2 O 0.552(4) 0.500000 0.500000 0.09(3) Uiso 0.1667 4 d DS . P . .
H3 H 0.609(10) 0.500000 0.533(4) 0.103 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0086(3) 0.0086(3) 0.0086(3) 0.0006(3) -0.0006(3) -0.0006(3)
O1 0.0319(18) 0.0125(12) 0.0241(15) 0.0012(10) -0.0080(11) 0.0009(11)
C1 0.027(3) 0.016(2) 0.019(3) 0.000 -0.010(2) 0.000
C2 0.025(6) 0.113(11) 0.052(8) 0.000 0.000 0.000

_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 2.091(2) 37_655 ?
Fe1 O1 2.091(2) 46_554 ?
Fe1 O1 2.091(2) 10_656 ?
Fe1 O1 2.091(2) 7_665 ?
Fe1 O1 2.091(2) 43_545 ?
Fe1 O1 2.091(2) . ?
O1 C1 1.238(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.50(3) 25_766 ?
C2 N2 1.50(3) . ?
C2 N1 1.51(3) . ?
C2 N1 1.51(3) 25_766 ?
N1 N2 1.12(4) 25_766 ?
N1 N2 1.12(4) . ?
N1 N1 1.61(9) 25_766 ?
N2 N2 1.55(9) 25_766 ?
O2 O2 0.88(6) 29_666 ?
O2 O2 0.88(6) 33_666 ?
O2 O2 0.88(6) 5 ?
O2 O2 0.88(6) 9 ?
O2 O2 1.25(9) 25_666 ?
O2 H3 0.79(10) . ?
O2 H3 0.79(10) 4_566 ?

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 91.26(12) 37_655 46_554 ?
O1 Fe1 O1 88.74(12) 37_655 10_656 ?
O1 Fe1 O1 180.00(15) 46_554 10_656 ?
O1 Fe1 O1 88.74(12) 37_655 7_665 ?
O1 Fe1 O1 88.74(12) 46_554 7_665 ?
O1 Fe1 O1 91.26(12) 10_656 7_665 ?
O1 Fe1 O1 91.26(12) 37_655 43_545 ?
O1 Fe1 O1 91.26(12) 46_554 43_545 ?
O1 Fe1 O1 88.74(12) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.00(15) 37_655 . ?
O1 Fe1 O1 88.74(12) 46_554 . ?
O1 Fe1 O1 91.26(12) 10_656 . ?
O1 Fe1 O1 91.26(12) 7_665 . ?
O1 Fe1 O1 88.74(12) 43_545 . ?
C1 O1 Fe1 128.8(3) . . ?
O1 C1 O1 126.8(5) . 27_565 ?
O1 C1 H1 116.6 . . ?
O1 C1 H1 116.6 27_565 . ?
N2 C2 N2 62(3) 25_766 . ?
N2 C2 N1 43.5(12) 25_766 . ?
N2 C2 N1 43.5(12) . . ?
N2 C2 N1 43.5(12) 25_766 25_766 ?
N2 C2 N1 43.5(12) . 25_766 ?
N1 C2 N1 64(3) . 25_766 ?
N2 N1 N2 88(5) 25_766 . ?
N2 N1 C2 67.5(19) 25_766 25_766 ?
N2 N1 C2 67.5(19) . 25_766 ?
N2 N1 C2 67.5(19) 25_766 . ?
N2 N1 C2 67.5(19) . . ?
C2 N1 C2 116(3) 25_766 . ?
N2 N1 N1 44(3) 25_766 25_766 ?
N2 N1 N1 44(3) . 25_766 ?
C2 N1 N1 57.9(15) 25_766 25_766 ?
C2 N1 N1 57.9(15) . 25_766 ?
N1 N2 N1 92(5) . 25_766 ?
N1 N2 C2 69(2) . 25_766 ?
N1 N2 C2 69(2) 25_766 25_766 ?
N1 N2 C2 69(2) . . ?
N1 N2 C2 69(2) 25_766 . ?
C2 N2 C2 118(3) 25_766 . ?
N1 N2 N2 46(3) . 25_766 ?
N1 N2 N2 46(3) 25_766 25_766 ?
C2 N2 N2 58.9(16) 25_766 25_766 ?
C2 N2 N2 58.9(16) . 25_766 ?
O2 O2 O2 59.999(6) 29_666 33_666 ?
O2 O2 O2 89.999(2) 29_666 5 ?
O2 O2 O2 59.999(3) 33_666 5 ?
O2 O2 O2 59.999(4) 29_666 9 ?
O2 O2 O2 89.999(1) 33_666 9 ?
O2 O2 O2 59.999(5) 5 9 ?
O2 O2 O2 44.999(12) 29_666 25_666 ?
O2 O2 O2 44.999(11) 33_666 25_666 ?
O2 O2 O2 44.999(8) 5 25_666 ?
O2 O2 O2 44.999(11) 9 25_666 ?
O2 O2 H3 128(3) 29_666 . ?
O2 O2 H3 165(6) 33_666 . ?
O2 O2 H3 128(3) 5 . ?
O2 O2 H3 105(6) 9 . ?
O2 O2 H3 150(6) 25_666 . ?
O2 O2 H3 128(3) 29_666 4_566 ?
O2 O2 H3 105(6) 33_666 4_566 ?
O2 O2 H3 128(3) 5 4_566 ?
O2 O2 H3 165(6) 9 4_566 ?
O2 O2 H3 150(6) 25_666 4_566 ?
H3 O2 H3 60(10) . 4_566 ?

_refine_diff_density_max         0.376
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.087

_shelx_res_file                  
;
TITL 18_PJS055_03_160_00 in P4(2)32
    18_PJS055_03_160_00.res
    created by SHELXL-2018/3 at 13:30:45 on 25-Sep-2019
REM P4(2)32 (#208 in standard setting)
CELL 0.71073  12.005147  12.005147  12.005147  90.0000  90.0000  90.0000
ZERR    8.00   0.000588   0.000588   0.000588   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.033000    4.292600
BASF   0.52617
FVAR       1.35842   0.06490
FE1   5    0.750000    0.250000    0.250000    10.16667    0.00860    0.00860 =
         0.00860    0.00058   -0.00058   -0.00058
O1    4    0.795479    0.407817    0.307950    11.00000    0.03194    0.01255 =
         0.02412    0.00115   -0.00799    0.00094
C1    1    0.759121    0.500000    0.279465    10.50000    0.02650    0.01605 =
         0.01923    0.00000   -0.00997    0.00000
AFIX  43
H1    2    0.698143    0.500000    0.231687    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.393294    0.500000    10.25000    0.02474    0.11263 =
         0.05247    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.566985    10.06250   21.00000
N2    3    0.935514    0.500000    0.500000    10.06250   21.00000
O2    4    0.551980    0.500000    0.500000    10.04167    0.08591
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.608672    0.500000    0.532868    10.08333   -1.20000
HKLF 4




REM  18_PJS055_03_160_00 in P4(2)32
REM wR2 = 0.0977, GooF = S = 1.238, Restrained GooF = 1.237 for all data
REM R1 = 0.0368 for 342 Fo > 4sig(Fo) and 0.0432 for all 387 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0327      4.3679

REM Highest difference peak  0.376,  deepest hole -0.497,  1-sigma level  0.087
Q1    1   1.0641  0.3909  0.4478  11.00000  0.05    0.38
Q2    1   0.5878  0.5534  0.5000  10.50000  0.05    0.37
Q3    1   1.0000  0.4349  0.5000  10.25000  0.05    0.36
Q4    1   1.0654  0.3262  0.5000  10.50000  0.05    0.29
Q5    1   0.7567  0.3220  0.3039  11.00000  0.05    0.24
Q6    1   0.7550  0.3698  0.2557  11.00000  0.05    0.23
Q7    1   1.0000  0.3419  0.4505  10.50000  0.05    0.23
Q8    1   1.0589  0.3536  0.5000  10.50000  0.05    0.23
Q9    1   0.8248  0.3092  0.2513  11.00000  0.05    0.23
Q10   1   1.0000  0.6167  0.6639  10.50000  0.05    0.22
Q11   1   0.7999  0.5000  0.5000  10.25000  0.05    0.20
Q12   1   0.8172  0.4283  0.2550  11.00000  0.05    0.18
Q13   1   0.9083  0.5511  0.5871  11.00000  0.05    0.16
Q14   1   1.0000  0.5685  0.6140  10.50000  0.05    0.16
Q15   1   0.7443  0.4360  0.3096  11.00000  0.05    0.16
Q16   1   0.7477  0.4282  0.1896  11.00000  0.05    0.15
Q17   1   1.0000  0.5371  0.6405  10.50000  0.05    0.14
Q18   1   0.7119  0.5518  0.5000  10.50000  0.05    0.14
Q19   1   0.8225  0.3583  0.3555  11.00000  0.05    0.14
Q20   1   0.8922  0.3264  0.3243  11.00000  0.05    0.13
;
_shelx_res_checksum              71391

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_03_160_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_03_160_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_03_160_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT906_18_PJS055_03_160_00 
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.445 Check 
RESPONSE: This is observed only for the highest resolution data at 0.72 A.
;
_vrf_PLAT911_18_PJS055_03_160_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
####################################################################### 
# 
# 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_18_PJS055_10_300_00_SW_r2f28_78
_database_code_depnum_ccdc_archive 'CCDC 1990952'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0350(6)
_cell_length_b                   12.0350(6)
_cell_length_c                   12.0350(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1743.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    300.0(7)
_cell_measurement_reflns_used    767
_cell_measurement_theta_min      4.0820
_cell_measurement_theta_max      29.5420

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.718
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.715
_oxdiff_exptl_absorpt_empirical_full_max 1.408
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300.0(7)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1203
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.148
_diffrn_reflns_theta_max         29.610
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             388
_reflns_number_gt                292
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.1211P)²+2.3344P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         388
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.2185
_refine_ls_wR_factor_gt          0.1784
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_restrained_S_all      1.174
_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 0.750000 0.250000 0.250000 0.0224(7) Uani 1 6 d S T P . .
O1 O 0.7959(3) 0.4081(3) 0.3070(4) 0.0405(11) Uani 1 1 d . . . . .
C1 C 0.7593(7) 0.500000 0.2779(9) 0.0395(18) Uani 1 2 d S T P . .
H1 H 0.698830 0.500000 0.229863 0.047 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.396(2) 0.500000 0.099(7) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.568(6) 0.084(14) Uiso 0.25 4 d S U P . .
N2 N 0.926(6) 0.500000 0.500000 0.084(14) Uiso 0.25 4 d S U P . .
O2 O 0.550(4) 0.500000 0.500000 0.056(19) Uiso 0.1667 4 d DS . P . .
H3 H 0.613(10) 0.500000 0.533(4) 0.067 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0224(7) 0.0224(7) 0.0224(7) 0.0007(3) -0.0007(3) -0.0007(3)
O1 0.048(3) 0.029(2) 0.045(2) -0.0003(14) -0.0075(17) 0.0029(16)
C1 0.044(5) 0.033(4) 0.042(4) 0.000 -0.016(3) 0.000
C2 0.034(8) 0.17(2) 0.097(15) 0.000 0.000 0.000

_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 2.096(4) . ?
Fe1 O1 2.096(4) 37_655 ?
Fe1 O1 2.096(4) 46_554 ?
Fe1 O1 2.096(4) 10_656 ?
Fe1 O1 2.096(4) 7_665 ?
Fe1 O1 2.096(4) 43_545 ?
O1 C1 1.240(6) . ?
C1 H1 0.9300 . ?
C2 N1 1.49(5) 25_766 ?
C2 N1 1.49(5) . ?
C2 N2 1.53(5) 25_766 ?
C2 N2 1.53(5) . ?
N1 N2 1.21(8) 25_766 ?
N1 N2 1.21(8) . ?
N1 N1 1.63(15) 25_766 ?
N2 N2 1.79(15) 25_766 ?
O2 O2 0.86(6) 33_666 ?
O2 O2 0.86(6) 29_666 ?
O2 O2 0.86(6) 9 ?
O2 O2 0.86(6) 5 ?
O2 O2 1.21(9) 25_666 ?
O2 H3 0.85(10) . ?
O2 H3 0.85(10) 4_566 ?

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 180.0 . 37_655 ?
O1 Fe1 O1 88.38(17) . 46_554 ?
O1 Fe1 O1 91.62(17) 37_655 46_554 ?
O1 Fe1 O1 91.62(17) . 10_656 ?
O1 Fe1 O1 88.38(17) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 91.62(17) . 7_665 ?
O1 Fe1 O1 88.38(17) 37_655 7_665 ?
O1 Fe1 O1 88.38(17) 46_554 7_665 ?
O1 Fe1 O1 91.62(17) 10_656 7_665 ?
O1 Fe1 O1 88.38(17) . 43_545 ?
O1 Fe1 O1 91.62(17) 37_655 43_545 ?
O1 Fe1 O1 91.62(17) 46_554 43_545 ?
O1 Fe1 O1 88.38(17) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
C1 O1 Fe1 128.6(5) . . ?
O1 C1 O1 126.2(8) 27_565 . ?
O1 C1 H1 116.9 27_565 . ?
O1 C1 H1 116.9 . . ?
N1 C2 N1 66(5) 25_766 . ?
N1 C2 N2 47(2) 25_766 25_766 ?
N1 C2 N2 47(2) . 25_766 ?
N1 C2 N2 47(2) 25_766 . ?
N1 C2 N2 47(2) . . ?
N2 C2 N2 71(5) 25_766 . ?
N2 N1 N2 95(7) 25_766 . ?
N2 N1 C2 68(3) 25_766 . ?
N2 N1 C2 68(3) . . ?
N2 N1 C2 68(3) 25_766 25_766 ?
N2 N1 C2 68(3) . 25_766 ?
C2 N1 C2 114(5) . 25_766 ?
N2 N1 N1 48(3) 25_766 25_766 ?
N2 N1 N1 48(3) . 25_766 ?
C2 N1 N1 57(2) . 25_766 ?
C2 N1 N1 57(2) 25_766 25_766 ?
N1 N2 N1 85(7) 25_766 . ?
N1 N2 C2 64(3) 25_766 . ?
N1 N2 C2 64(3) . . ?
N1 N2 C2 64(3) 25_766 25_766 ?
N1 N2 C2 64(3) . 25_766 ?
C2 N2 C2 109(5) . 25_766 ?
N1 N2 N2 42(3) 25_766 25_766 ?
N1 N2 N2 42(3) . 25_766 ?
C2 N2 N2 54(2) . 25_766 ?
C2 N2 N2 54(2) 25_766 25_766 ?
O2 O2 O2 59.998(10) 33_666 29_666 ?
O2 O2 O2 89.997(1) 33_666 9 ?
O2 O2 O2 59.998(6) 29_666 9 ?
O2 O2 O2 59.998(1) 33_666 5 ?
O2 O2 O2 89.997(1) 29_666 5 ?
O2 O2 O2 59.998(2) 9 5 ?
O2 O2 O2 44.999(11) 33_666 25_666 ?
O2 O2 O2 44.999(11) 29_666 25_666 ?
O2 O2 O2 44.999(11) 9 25_666 ?
O2 O2 O2 44.999(7) 5 25_666 ?
O2 O2 H3 163(5) 33_666 . ?
O2 O2 H3 129(2) 29_666 . ?
O2 O2 H3 107(5) 9 . ?
O2 O2 H3 129(2) 5 . ?
O2 O2 H3 152(5) 25_666 . ?
O2 O2 H3 107(5) 33_666 4_566 ?
O2 O2 H3 129(2) 29_666 4_566 ?
O2 O2 H3 163(5) 9 4_566 ?
O2 O2 H3 129(2) 5 4_566 ?
O2 O2 H3 152(5) 25_666 4_566 ?
H3 O2 H3 55(10) . 4_566 ?

_refine_diff_density_max         0.498
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.141

_shelx_res_file                  
;
TITL 18_PJS055_10_300_00_SW_r2f28_78 in Im-3
    18_PJS055_10_300_00_SW_r2f28_78.res
    created by SHELXL-2018/3 at 13:48:03 on 25-Sep-2019
REM Im-3 (#204 in standard setting)
CELL 0.71073  12.034985  12.034985  12.034985  90.0000  90.0000  90.0000
ZERR    8.00   0.000576   0.000576   0.000576   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.121100    2.334400
BASF   0.53559
FVAR       1.57250   0.08394
FE1   5    0.750000    0.250000    0.250000    10.16667    0.02243    0.02243 =
         0.02243    0.00066   -0.00066   -0.00066
O1    4    0.795860    0.408103    0.306961    11.00000    0.04777    0.02880 =
         0.04505   -0.00030   -0.00746    0.00286
C1    1    0.759331    0.500000    0.277936    10.50000    0.04351    0.03291 =
         0.04223    0.00000   -0.01627    0.00000
AFIX  43
H1    2    0.698830    0.500000    0.229863    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.396433    0.500000    10.25000    0.03380    0.16664 =
         0.09660    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.567865    10.06250   21.00000
N2    3    0.925658    0.500000    0.500000    10.06250   21.00000
O2    4    0.550265    0.500000    0.500000    10.04167    0.05571
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.612592    0.500000    0.532587    10.08333   -1.20000
HKLF 4




REM  18_PJS055_10_300_00_SW_r2f28_78 in Im-3
REM wR2 = 0.2185, GooF = S = 1.177, Restrained GooF = 1.174 for all data
REM R1 = 0.0567 for 292 Fo > 4sig(Fo) and 0.0744 for all 388 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.1139      2.9297

REM Highest difference peak  0.498,  deepest hole -0.862,  1-sigma level  0.141
Q1    1   0.8027  0.5000  0.1183  10.50000  0.05    0.50
Q2    1   0.7486  0.4387  0.3433  11.00000  0.05    0.42
Q3    1   0.8361  0.5000  0.3344  10.50000  0.05    0.41
Q4    1   0.8195  0.5000  0.2282  10.50000  0.05    0.39
Q5    1   0.7517  0.3476  0.2857  11.00000  0.05    0.38
Q6    1   1.0618  0.4203  0.5000  10.50000  0.05    0.36
Q7    1   0.8193  0.5000  0.1862  10.50000  0.05    0.36
Q8    1   0.7864  0.5000  0.5000  10.25000  0.05    0.36
Q9    1   1.0654  0.3784  0.4537  11.00000  0.05    0.35
Q10   1   0.8715  0.3625  0.2561  11.00000  0.05    0.34
Q11   1   1.0597  0.3416  0.4562  11.00000  0.05    0.32
Q12   1   0.7538  0.3619  0.2164  11.00000  0.05    0.30
Q13   1   0.7799  0.5210  0.5376  11.00000  0.05    0.30
Q14   1   1.0377  0.2790  0.5000  10.50000  0.05    0.30
Q15   1   1.0788  0.2701  0.5000  10.50000  0.05    0.30
Q16   1   0.8329  0.5000  0.1649  10.50000  0.05    0.30
Q17   1   0.9103  0.3879  0.3039  11.00000  0.05    0.29
Q18   1   1.0000  0.5755  0.6560  10.50000  0.05    0.29
Q19   1   0.9231  0.3760  0.2842  11.00000  0.05    0.29
Q20   1   0.6873  0.4306  0.1231  11.00000  0.05    0.29
;
_shelx_res_checksum              85650

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_10_300_00_SW_r2f28_78 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT029_18_PJS055_10_300_00_SW_r2f28_78 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.971 Why?
RESPONSE: 22 frames were exlcuded from integration due the movement of 
the crystal.
;
_vrf_PLAT041_18_PJS055_10_300_00_SW_r2f28_78 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_10_300_00_SW_r2f28_78 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT241_18_PJS055_10_300_00_SW_r2f28_78 
;
PROBLEM: High   MainMol Ueq as Compared to Neighbors of         C2 Check   
RESPONSE: The C2 atom is part of the DMA cation and neighbours the N position,
which is dynamically disordered.
;
_vrf_PLAT911_18_PJS055_10_300_00_SW_r2f28_78 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          7 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
# end Validation Reply Form

#==============================================================================
####################################################################### 
# 
# 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_18_PJS055_05_200_00
_database_code_depnum_ccdc_archive 'CCDC 1990948'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0077(3)
_cell_length_b                   12.0077(3)
_cell_length_c                   12.0077(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1731.33(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    200.0(4)
_cell_measurement_reflns_used    3235
_cell_measurement_theta_min      3.7980
_cell_measurement_theta_max      29.3850

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.730
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.857
_oxdiff_exptl_absorpt_empirical_full_max 1.206
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200.0(4)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6495
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.157
_diffrn_reflns_theta_max         29.567
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             454
_reflns_number_gt                433
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0307P)²+5.0464P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         454
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_restrained_S_all      1.206
_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 0.750000 0.250000 0.250000 0.0110(2) Uani 1 6 d S T P . .
O1 O 0.79547(19) 0.40813(14) 0.30780(19) 0.0253(4) Uani 1 1 d . . . . .
C1 C 0.7591(4) 0.500000 0.2802(4) 0.0228(8) Uani 1 2 d S T P . .
H1 H 0.697396 0.499999 0.233326 0.027 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3953(10) 0.500000 0.067(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.566(3) 0.060(5) Uiso 0.25 4 d S U P . .
N2 N 0.936(3) 0.500000 0.500000 0.060(5) Uiso 0.25 4 d S U P . .
O2 O 0.550(3) 0.500000 0.500000 0.08(2) Uiso 0.1667 4 d DS . P . .
H3 H 0.601(10) 0.500000 0.534(4) 0.098 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0110(2) 0.0110(2) 0.0110(2) 0.00034(18) -0.00034(18) -0.00034(18)
O1 0.0344(13) 0.0153(8) 0.0261(10) 0.0005(7) -0.0072(9) -0.0004(8)
C1 0.027(2) 0.0165(15) 0.025(2) 0.000 -0.0080(15) 0.000
C2 0.036(5) 0.122(9) 0.043(5) 0.000 0.000 0.000

_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 2.0941(18) 37_655 ?
Fe1 O1 2.0941(18) 46_554 ?
Fe1 O1 2.0941(18) 10_656 ?
Fe1 O1 2.0941(18) 7_665 ?
Fe1 O1 2.0941(18) 43_545 ?
Fe1 O1 2.0941(18) . ?
O1 C1 1.232(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.47(2) . ?
C2 N2 1.47(2) 25_766 ?
C2 N1 1.48(2) . ?
C2 N1 1.48(2) 25_766 ?
N1 N2 1.10(3) . ?
N1 N2 1.10(3) 25_766 ?
N1 N1 1.58(7) 25_766 ?
N2 N2 1.53(7) 25_766 ?
O2 O2 0.86(5) 33_666 ?
O2 O2 0.86(5) 29_666 ?
O2 O2 0.86(5) 9 ?
O2 O2 0.86(5) 5 ?
O2 O2 1.21(7) 25_666 ?
O2 H3 0.72(10) . ?
O2 H3 0.72(10) 4_566 ?

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 91.28(9) 37_655 46_554 ?
O1 Fe1 O1 88.72(9) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 88.72(9) 37_655 7_665 ?
O1 Fe1 O1 88.72(9) 46_554 7_665 ?
O1 Fe1 O1 91.28(9) 10_656 7_665 ?
O1 Fe1 O1 91.28(9) 37_655 43_545 ?
O1 Fe1 O1 91.28(9) 46_554 43_545 ?
O1 Fe1 O1 88.72(9) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.0 37_655 . ?
O1 Fe1 O1 88.72(9) 46_554 . ?
O1 Fe1 O1 91.28(9) 10_656 . ?
O1 Fe1 O1 91.28(9) 7_665 . ?
O1 Fe1 O1 88.72(9) 43_545 . ?
C1 O1 Fe1 129.1(2) . . ?
O1 C1 O1 127.1(4) 27_565 . ?
O1 C1 H1 116.4 27_565 . ?
O1 C1 H1 116.4 . . ?
N2 C2 N2 63(2) . 25_766 ?
N2 C2 N1 43.6(10) . . ?
N2 C2 N1 43.6(10) 25_766 . ?
N2 C2 N1 43.6(10) . 25_766 ?
N2 C2 N1 43.6(10) 25_766 25_766 ?
N1 C2 N1 64(2) . 25_766 ?
N2 N1 N2 88(4) . 25_766 ?
N2 N1 C2 67.6(15) . 25_766 ?
N2 N1 C2 67.6(15) 25_766 25_766 ?
N2 N1 C2 67.6(15) . . ?
N2 N1 C2 67.6(15) 25_766 . ?
C2 N1 C2 116(2) 25_766 . ?
N2 N1 N1 44(2) . 25_766 ?
N2 N1 N1 44(2) 25_766 25_766 ?
C2 N1 N1 57.9(12) 25_766 25_766 ?
C2 N1 N1 57.9(12) . 25_766 ?
N1 N2 N1 92(4) . 25_766 ?
N1 N2 C2 68.8(15) . 25_766 ?
N1 N2 C2 68.8(15) 25_766 25_766 ?
N1 N2 C2 68.8(15) . . ?
N1 N2 C2 68.8(15) 25_766 . ?
C2 N2 C2 117(2) 25_766 . ?
N1 N2 N2 46(2) . 25_766 ?
N1 N2 N2 46(2) 25_766 25_766 ?
C2 N2 N2 58.7(12) 25_766 25_766 ?
C2 N2 N2 58.7(12) . 25_766 ?
O2 O2 O2 60.001(8) 33_666 29_666 ?
O2 O2 O2 90.002(1) 33_666 9 ?
O2 O2 O2 60.001(5) 29_666 9 ?
O2 O2 O2 60.001(2) 33_666 5 ?
O2 O2 O2 90.002(1) 29_666 5 ?
O2 O2 O2 60.001(2) 9 5 ?
O2 O2 O2 45.001(9) 33_666 25_666 ?
O2 O2 O2 45.001(10) 29_666 25_666 ?
O2 O2 O2 45.001(9) 9 25_666 ?
O2 O2 O2 45.001(6) 5 25_666 ?
O2 O2 H3 169(7) 33_666 . ?
O2 O2 H3 126(3) 29_666 . ?
O2 O2 H3 101(7) 9 . ?
O2 O2 H3 126(3) 5 . ?
O2 O2 H3 146(7) 25_666 . ?
O2 O2 H3 101(7) 33_666 4_566 ?
O2 O2 H3 126(3) 29_666 4_566 ?
O2 O2 H3 169(7) 9 4_566 ?
O2 O2 H3 126(3) 5 4_566 ?
O2 O2 H3 146(7) 25_666 4_566 ?
H3 O2 H3 68(10) . 4_566 ?

_refine_diff_density_max         0.499
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.083

_shelx_res_file                  
;
TITL 18_PJS055_05_200_00 in Pm-3m
    18_PJS055_05_200_00.res
    created by SHELXL-2018/3 at 13:33:59 on 25-Sep-2019
REM Pm-3m (#221 in standard setting)
CELL 0.71073  12.007696  12.007696  12.007696  90.0000  90.0000  90.0000
ZERR    8.00   0.000300   0.000300   0.000300   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.030700    5.046400
BASF   0.52571
FVAR       1.43218   0.06014
FE1   5    0.750000    0.250000    0.250000    10.16667    0.01098    0.01098 =
         0.01098    0.00034   -0.00034   -0.00034
O1    4    0.795475    0.408128    0.307800    11.00000    0.03439    0.01529 =
         0.02615    0.00052   -0.00722   -0.00037
C1    1    0.759079    0.500000    0.280164    10.50000    0.02717    0.01651 =
         0.02485    0.00000   -0.00803    0.00000
AFIX  43
H1    2    0.697396    0.499999    0.233326    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.395254    0.500000    10.25000    0.03554    0.12159 =
         0.04285    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.565619    10.06250   21.00000
N2    3    0.936232    0.500000    0.500000    10.06250   21.00000
O2    4    0.550428    0.500000    0.500000    10.04167    0.08136
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.600537    0.500000    0.533638    10.08333   -1.20000
HKLF 4




REM  18_PJS055_05_200_00 in Pm-3m
REM wR2 = 0.0855, GooF = S = 1.205, Restrained GooF = 1.206 for all data
REM R1 = 0.0335 for 433 Fo > 4sig(Fo) and 0.0358 for all 454 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0307      5.0460

REM Highest difference peak  0.499,  deepest hole -0.540,  1-sigma level  0.083
Q1    1   1.0000  0.5488  0.5711  10.50000  0.05    0.50
Q2    1   0.5668  0.5000  0.5750  10.50000  0.05    0.40
Q3    1   1.0530  0.3949  0.4436  11.00000  0.05    0.40
Q4    1   0.6045  0.5000  0.5000  10.25000  0.05    0.35
Q5    1   0.9189  0.5550  0.5000  10.50000  0.05    0.29
Q6    1   0.7685  0.3457  0.2825  11.00000  0.05    0.24
Q7    1   1.0000  0.3553  0.4355  10.50000  0.05    0.22
Q8    1   1.0546  0.3301  0.5000  10.50000  0.05    0.21
Q9    1   0.5000  0.5000  0.5000  10.04167  0.05    0.20
Q10   1   0.6796  0.3204  0.3204  10.33333  0.05    0.19
Q11   1   1.0000  0.4242  0.5000  10.25000  0.05    0.18
Q12   1   0.8926  0.5000  0.5677  10.50000  0.05    0.17
Q13   1   0.8149  0.4289  0.2506  11.00000  0.05    0.17
Q14   1   1.0000  0.5000  0.6449  10.25000  0.05    0.16
Q15   1   0.5940  0.5940  0.5941  10.33333  0.05    0.15
Q16   1   1.0000  0.6122  0.6677  10.50000  0.05    0.15
Q17   1   0.7329  0.4072  0.3231  11.00000  0.05    0.14
Q18   1   0.8578  0.4084  0.2456  11.00000  0.05    0.14
Q19   1   0.8408  0.3349  0.3667  11.00000  0.05    0.13
Q20   1   0.9256  0.5000  0.5896  10.50000  0.05    0.13
;
_shelx_res_checksum              20567

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_05_200_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_05_200_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_05_200_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT906_18_PJS055_05_200_00 
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.651 Check 
RESPONSE: This is observed only for the highest resolution data at 0.72 A.
;
####################################################################### 
# 
# 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_18_PJS055_01_120_00
_database_code_depnum_ccdc_archive 'CCDC 1990944'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   11.9986(7)
_cell_length_b                   11.9986(7)
_cell_length_c                   11.9986(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1727.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120.0(3)
_cell_measurement_reflns_used    423
_cell_measurement_theta_min      3.7800
_cell_measurement_theta_max      28.7100

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.734
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.883
_oxdiff_exptl_absorpt_empirical_full_max 1.159
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120.0(3)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            875
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.160
_diffrn_reflns_theta_max         29.239
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             384
_reflns_number_gt                331
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0278P)²+4.0129P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         384
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.229
_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 0.750000 0.250000 0.250000 0.0069(3) Uani 1 6 d S T P . .
O1 O 0.7957(2) 0.40763(19) 0.3081(2) 0.0208(6) Uani 1 1 d . . . . .
C1 C 0.7589(5) 0.500000 0.2803(5) 0.0172(12) Uani 1 2 d S T P . .
H1 H 0.697048 0.500001 0.233499 0.021 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3939(12) 0.500000 0.061(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.566(4) 0.064(8) Uiso 0.25 4 d S U P . .
N2 N 0.940(4) 0.500000 0.500000 0.064(8) Uiso 0.25 4 d S U P . .
O2 O 0.558(3) 0.500000 0.500000 0.07(2) Uiso 0.1667 4 d DS . P . .
H3 H 0.617(10) 0.500000 0.532(4) 0.086 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0069(3) 0.0069(3) 0.0069(3) 0.0006(3) -0.0006(3) -0.0006(3)
O1 0.0298(18) 0.0119(12) 0.0207(16) 0.0017(10) -0.0066(12) 0.0010(11)
C1 0.022(3) 0.013(2) 0.017(3) 0.000 -0.007(2) 0.000
C2 0.025(6) 0.106(11) 0.052(8) 0.000 0.000 0.000

_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 2.089(2) 37_655 ?
Fe1 O1 2.089(2) 46_554 ?
Fe1 O1 2.089(2) 10_656 ?
Fe1 O1 2.089(2) 7_665 ?
Fe1 O1 2.089(2) 43_545 ?
Fe1 O1 2.089(2) . ?
O1 C1 1.239(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.46(3) . ?
C2 N2 1.46(3) 25_766 ?
C2 N1 1.50(3) 25_766 ?
C2 N1 1.50(3) . ?
N1 N2 1.07(4) . ?
N1 N2 1.07(4) 25_766 ?
N1 N1 1.58(9) 25_766 ?
N2 N2 1.44(9) 25_766 ?
O2 O2 0.98(5) 33_666 ?
O2 O2 0.98(5) 29_666 ?
O2 O2 0.98(5) 9 ?
O2 O2 0.98(5) 5 ?
O2 O2 1.39(8) 25_666 ?
O2 H3 0.81(10) . ?
O2 H3 0.81(10) 4_566 ?

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 91.31(12) 37_655 46_554 ?
O1 Fe1 O1 88.69(12) 37_655 10_656 ?
O1 Fe1 O1 180.00(15) 46_554 10_656 ?
O1 Fe1 O1 88.69(12) 37_655 7_665 ?
O1 Fe1 O1 88.69(12) 46_554 7_665 ?
O1 Fe1 O1 91.31(12) 10_656 7_665 ?
O1 Fe1 O1 91.31(12) 37_655 43_545 ?
O1 Fe1 O1 91.31(12) 46_554 43_545 ?
O1 Fe1 O1 88.69(12) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.0 37_655 . ?
O1 Fe1 O1 88.69(12) 46_554 . ?
O1 Fe1 O1 91.31(12) 10_656 . ?
O1 Fe1 O1 91.31(12) 7_665 . ?
O1 Fe1 O1 88.69(12) 43_545 . ?
C1 O1 Fe1 128.8(3) . . ?
O1 C1 O1 126.9(5) . 27_565 ?
O1 C1 H1 116.6 . . ?
O1 C1 H1 116.6 27_565 . ?
N2 C2 N2 59(3) . 25_766 ?
N2 C2 N1 42.4(12) . 25_766 ?
N2 C2 N1 42.4(12) 25_766 25_766 ?
N2 C2 N1 42.4(12) . . ?
N2 C2 N1 42.4(12) 25_766 . ?
N1 C2 N1 64(3) 25_766 . ?
N2 N1 N2 85(6) . 25_766 ?
N2 N1 C2 67(2) . . ?
N2 N1 C2 67(2) 25_766 . ?
N2 N1 C2 67(2) . 25_766 ?
N2 N1 C2 67(2) 25_766 25_766 ?
C2 N1 C2 116(3) . 25_766 ?
N2 N1 N1 42(3) . 25_766 ?
N2 N1 N1 42(3) 25_766 25_766 ?
C2 N1 N1 58.1(15) . 25_766 ?
C2 N1 N1 58.1(15) 25_766 25_766 ?
N1 N2 N1 95(6) 25_766 . ?
N1 N2 N2 48(3) 25_766 25_766 ?
N1 N2 N2 48(3) . 25_766 ?
N1 N2 C2 71(2) 25_766 . ?
N1 N2 C2 71(2) . . ?
N2 N2 C2 60.5(16) 25_766 . ?
N1 N2 C2 71(2) 25_766 25_766 ?
N1 N2 C2 71(2) . 25_766 ?
N2 N2 C2 60.5(16) 25_766 25_766 ?
C2 N2 C2 121(3) . 25_766 ?
O2 O2 O2 60.001(9) 33_666 29_666 ?
O2 O2 O2 90.002(2) 33_666 9 ?
O2 O2 O2 60.001(3) 29_666 9 ?
O2 O2 O2 60.001(2) 33_666 5 ?
O2 O2 O2 90.002(2) 29_666 5 ?
O2 O2 O2 60.001(2) 9 5 ?
O2 O2 O2 45.001(6) 33_666 25_666 ?
O2 O2 O2 45.001(7) 29_666 25_666 ?
O2 O2 O2 45.001(6) 9 25_666 ?
O2 O2 O2 45.001(3) 5 25_666 ?
O2 O2 H3 164(6) 33_666 . ?
O2 O2 H3 128(2) 29_666 . ?
O2 O2 H3 106(6) 9 . ?
O2 O2 H3 128(3) 5 . ?
O2 O2 H3 151(6) 25_666 . ?
O2 O2 H3 106(6) 33_666 4_566 ?
O2 O2 H3 128(2) 29_666 4_566 ?
O2 O2 H3 164(6) 9 4_566 ?
O2 O2 H3 128(3) 5 4_566 ?
O2 O2 H3 151(6) 25_666 4_566 ?
H3 O2 H3 58(10) . 4_566 ?

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.086

_shelx_res_file                  
;
TITL 18_PJS055_01_120_00 in P4(2)32
    18_PJS055_01_120_00.res
    created by SHELXL-2018/3 at 12:11:03 on 25-Sep-2019
REM P4(2)32 (#208 in standard setting)
CELL 0.71073  11.998613  11.998613  11.998613  90.0000  90.0000  90.0000
ZERR    8.00   0.000744   0.000744   0.000744   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
EQIV $2 2-x, +y, +z
EQIV $3 +x, +y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.027800    4.012900
BASF   0.52247
FVAR       1.30499   0.06351
FE1   5    0.750000    0.250000    0.250000    10.16667    0.00688    0.00688 =
         0.00688    0.00056   -0.00056   -0.00056
O1    4    0.795689    0.407626    0.308134    11.00000    0.02983    0.01187 =
         0.02068    0.00172   -0.00660    0.00103
C1    1    0.758858    0.500000    0.280266    10.50000    0.02155    0.01270 =
         0.01730    0.00000   -0.00698    0.00000
AFIX  43
H1    2    0.697048    0.500001    0.233499    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.393937    0.500000    10.25000    0.02489    0.10603 =
         0.05192    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.565959    10.06250   21.00000
N2    3    0.939959    0.500000    0.500000    10.06250   21.00000
O2    4    0.557783    0.500000    0.500000    10.04167    0.07153
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.616849    0.500000    0.532412    10.08333   -1.20000
HKLF 4




REM  18_PJS055_01_120_00 in P4(2)32
REM wR2 = 0.0917, GooF = S = 1.231, Restrained GooF = 1.229 for all data
REM R1 = 0.0366 for 331 Fo > 4sig(Fo) and 0.0441 for all 384 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0283      4.0355

REM Highest difference peak  0.382,  deepest hole -0.704,  1-sigma level  0.086
Q1    1   1.0000  0.5000  0.6432  10.25000  0.05    0.38
Q2    1   1.0596  0.3961  0.4345  11.00000  0.05    0.37
Q3    1   0.6372  0.5000  0.5000  10.25000  0.05    0.33
Q4    1   0.5809  0.5566  0.5000  10.50000  0.05    0.32
Q5    1   0.5864  0.5528  0.5296  11.00000  0.05    0.31
Q6    1   0.6905  0.3095  0.3095  10.33333  0.05    0.28
Q7    1   0.6018  0.5437  0.5495  11.00000  0.05    0.27
Q8    1   1.0000  0.4350  0.5000  10.25000  0.05    0.27
Q9    1   0.5728  0.5000  0.5597  10.50000  0.05    0.26
Q10   1   1.0000  0.5459  0.5472  10.50000  0.05    0.26
Q11   1   1.0564  0.3323  0.5000  10.50000  0.05    0.24
Q12   1   0.7489  0.3287  0.3077  11.00000  0.05    0.23
Q13   1   0.6604  0.5000  0.3067  10.50000  0.05    0.21
Q14   1   0.7408  0.4360  0.3093  11.00000  0.05    0.21
Q15   1   1.0000  0.6092  0.6475  10.50000  0.05    0.21
Q16   1   1.0000  0.3384  0.4515  10.50000  0.05    0.20
Q17   1   0.7956  0.4235  0.3385  11.00000  0.05    0.20
Q18   1   0.8205  0.4405  0.2473  11.00000  0.05    0.19
Q19   1   0.8220  0.4069  0.3027  11.00000  0.05    0.18
Q20   1   0.7153  0.4075  0.1591  11.00000  0.05    0.18
;
_shelx_res_checksum              18323

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_01_120_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_01_120_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_01_120_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT906_18_PJS055_01_120_00 
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.991 Check 
RESPONSE: This is observed only for the highest resolution data at 0.73 A.
;
_vrf_PLAT911_18_PJS055_01_120_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
####################################################################### 
# 
# 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_18_PJS055_06_220_00
_database_code_depnum_ccdc_archive 'CCDC 1990949'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0121(9)
_cell_length_b                   12.0121(9)
_cell_length_c                   12.0121(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1733.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    220.0(4)
_cell_measurement_reflns_used    434
_cell_measurement_theta_min      4.1260
_cell_measurement_theta_max      29.1310

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.728
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.22701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.775
_oxdiff_exptl_absorpt_empirical_full_max 3.113
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220.0(4)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            890
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.156
_diffrn_reflns_theta_max         29.555
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             393
_reflns_number_gt                338
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0416P)²+4.2080P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         393
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0933
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.105
_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 0.750000 0.250000 0.250000 0.0119(3) Uani 1 6 d S T P . .
O1 O 0.7956(2) 0.40799(17) 0.3075(2) 0.0264(5) Uani 1 1 d . . . . .
C1 C 0.7587(4) 0.500000 0.2799(4) 0.0248(10) Uani 1 2 d S T P . .
H1 H 0.696751 0.500000 0.233458 0.030 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3943(12) 0.500000 0.073(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.569(3) 0.070(7) Uiso 0.25 4 d S U P . .
N2 N 0.939(4) 0.500000 0.500000 0.070(7) Uiso 0.25 4 d S U P . .
O2 O 0.551(3) 0.500000 0.500000 0.09(2) Uiso 0.1667 4 d DS . P . .
H3 H 0.607(10) 0.500000 0.533(4) 0.105 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0119(3) 0.0119(3) 0.0119(3) 0.0006(2) -0.0006(2) -0.0006(2)
O1 0.0342(15) 0.0166(10) 0.0284(13) 0.0010(9) -0.0064(11) 0.0015(10)
C1 0.029(3) 0.018(2) 0.028(3) 0.000 -0.0123(19) 0.000
C2 0.029(5) 0.127(11) 0.063(7) 0.000 0.000 0.000

_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 2.093(2) 37_655 ?
Fe1 O1 2.093(2) 46_554 ?
Fe1 O1 2.093(2) 10_656 ?
Fe1 O1 2.093(2) 7_665 ?
Fe1 O1 2.093(2) 43_545 ?
Fe1 O1 2.093(2) . ?
O1 C1 1.236(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.47(3) 25_766 ?
C2 N2 1.47(3) . ?
C2 N1 1.51(3) . ?
C2 N1 1.51(3) 25_766 ?
N1 N2 1.11(4) 25_766 ?
N1 N2 1.11(4) . ?
N1 N1 1.65(8) 25_766 ?
N2 N2 1.47(9) 25_766 ?
O2 O2 0.86(6) 33_666 ?
O2 O2 0.86(6) 29_666 ?
O2 O2 0.86(6) 9 ?
O2 O2 0.86(6) 5 ?
O2 O2 1.22(8) 25_666 ?
O2 H3 0.78(10) . ?
O2 H3 0.78(10) 4_566 ?

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 91.38(10) 37_655 46_554 ?
O1 Fe1 O1 88.62(10) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 88.62(10) 37_655 7_665 ?
O1 Fe1 O1 88.62(10) 46_554 7_665 ?
O1 Fe1 O1 91.38(10) 10_656 7_665 ?
O1 Fe1 O1 91.38(10) 37_655 43_545 ?
O1 Fe1 O1 91.38(10) 46_554 43_545 ?
O1 Fe1 O1 88.62(10) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.0 37_655 . ?
O1 Fe1 O1 88.62(10) 46_554 . ?
O1 Fe1 O1 91.38(10) 10_656 . ?
O1 Fe1 O1 91.38(10) 7_665 . ?
O1 Fe1 O1 88.62(10) 43_545 . ?
C1 O1 Fe1 128.9(3) . . ?
O1 C1 O1 126.8(4) . 27_565 ?
O1 C1 H1 116.6 . . ?
O1 C1 H1 116.6 27_565 . ?
N2 C2 N2 60(3) 25_766 . ?
N2 C2 N1 43.5(12) 25_766 . ?
N2 C2 N1 43.5(12) . . ?
N2 C2 N1 43.5(12) 25_766 25_766 ?
N2 C2 N1 43.5(12) . 25_766 ?
N1 C2 N1 66(3) . 25_766 ?
N2 N1 N2 84(5) 25_766 . ?
N2 N1 C2 66.0(18) 25_766 . ?
N2 N1 C2 66.0(18) . . ?
N2 N1 C2 66.0(18) 25_766 25_766 ?
N2 N1 C2 66.0(18) . 25_766 ?
C2 N1 C2 114(3) . 25_766 ?
N2 N1 N1 42(3) 25_766 25_766 ?
N2 N1 N1 42(3) . 25_766 ?
C2 N1 N1 57.0(14) . 25_766 ?
C2 N1 N1 57.0(14) 25_766 25_766 ?
N1 N2 N1 96(5) . 25_766 ?
N1 N2 C2 70.5(18) . . ?
N1 N2 C2 70.5(18) 25_766 . ?
N1 N2 C2 70.5(18) . 25_766 ?
N1 N2 C2 70.5(18) 25_766 25_766 ?
C2 N2 C2 120(3) . 25_766 ?
N1 N2 N2 48(3) . 25_766 ?
N1 N2 N2 48(3) 25_766 25_766 ?
C2 N2 N2 59.9(15) . 25_766 ?
C2 N2 N2 59.9(15) 25_766 25_766 ?
O2 O2 O2 59.998(10) 33_666 29_666 ?
O2 O2 O2 90.0 33_666 9 ?
O2 O2 O2 59.998(4) 29_666 9 ?
O2 O2 O2 59.998(2) 33_666 5 ?
O2 O2 O2 89.997(1) 29_666 5 ?
O2 O2 O2 59.998(2) 9 5 ?
O2 O2 O2 44.999(10) 33_666 25_666 ?
O2 O2 O2 44.999(10) 29_666 25_666 ?
O2 O2 O2 44.999(10) 9 25_666 ?
O2 O2 O2 44.999(7) 5 25_666 ?
O2 O2 H3 165(6) 33_666 . ?
O2 O2 H3 128(3) 29_666 . ?
O2 O2 H3 105(6) 9 . ?
O2 O2 H3 128(3) 5 . ?
O2 O2 H3 150(6) 25_666 . ?
O2 O2 H3 105(6) 33_666 4_566 ?
O2 O2 H3 128(3) 29_666 4_566 ?
O2 O2 H3 165(6) 9 4_566 ?
O2 O2 H3 128(3) 5 4_566 ?
O2 O2 H3 150(6) 25_666 4_566 ?
H3 O2 H3 61(10) . 4_566 ?

_refine_diff_density_max         0.429
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.084

_shelx_res_file                  
;
TITL 18_PJS055_06_220_00 in Pn-3n
    18_PJS055_06_220_00.res
    created by SHELXL-2018/3 at 13:35:59 on 25-Sep-2019
REM Pn-3n (#222 in standard setting)
CELL 0.71073  12.012127  12.012127  12.012127  90.0000  90.0000  90.0000
ZERR    8.00   0.000877   0.000877   0.000877   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.041600    4.208000
BASF   0.47555
FVAR       1.41699   0.07019
FE1   5    0.750000    0.250000    0.250000    10.16667    0.01191    0.01191 =
         0.01191    0.00057   -0.00057   -0.00057
O1    4    0.795577    0.407992    0.307547    11.00000    0.03420    0.01665 =
         0.02837    0.00096   -0.00640    0.00152
C1    1    0.758698    0.500000    0.279899    10.50000    0.02880    0.01769 =
         0.02800    0.00000   -0.01231    0.00000
AFIX  43
H1    2    0.696751    0.500000    0.233458    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.394272    0.500000    10.25000    0.02896    0.12664 =
         0.06250    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.568715    10.06250   21.00000
N2    3    0.938621    0.500000    0.500000    10.06250   21.00000
O2    4    0.550696    0.500000    0.500000    10.04167    0.08725
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.606631    0.500000    0.532896    10.08333   -1.20000
HKLF 4




REM  18_PJS055_06_220_00 in Pn-3n
REM wR2 = 0.0933, GooF = S = 1.106, Restrained GooF = 1.105 for all data
REM R1 = 0.0358 for 338 Fo > 4sig(Fo) and 0.0416 for all 393 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0415      4.2075

REM Highest difference peak  0.429,  deepest hole -0.741,  1-sigma level  0.084
Q1    1   1.0000  0.5342  0.5685  10.50000  0.05    0.43
Q2    1   1.0527  0.3909  0.4498  11.00000  0.05    0.37
Q3    1   0.5880  0.5566  0.5000  10.50000  0.05    0.32
Q4    1   1.0000  0.4244  0.5000  10.25000  0.05    0.25
Q5    1   0.6833  0.3137  0.2544  11.00000  0.05    0.23
Q6    1   0.8799  0.3649  0.2462  11.00000  0.05    0.22
Q7    1   0.8294  0.4218  0.2523  11.00000  0.05    0.21
Q8    1   0.7136  0.3173  0.3434  11.00000  0.05    0.21
Q9    1   0.7838  0.3543  0.2936  11.00000  0.05    0.21
Q10   1   1.0000  0.5000  0.6552  10.25000  0.05    0.20
Q11   1   0.8248  0.3166  0.2562  11.00000  0.05    0.20
Q12   1   0.9137  0.5558  0.5000  10.50000  0.05    0.19
Q13   1   0.7511  0.5000  0.4109  10.50000  0.05    0.19
Q14   1   1.0000  0.6140  0.6555  10.50000  0.05    0.18
Q15   1   0.7496  0.3920  0.2509  11.00000  0.05    0.18
Q16   1   1.0544  0.3225  0.5000  10.50000  0.05    0.17
Q17   1   0.7544  0.4235  0.3242  11.00000  0.05    0.17
Q18   1   0.8006  0.2992  0.3718  11.00000  0.05    0.15
Q19   1   0.8145  0.3726  0.2019  11.00000  0.05    0.14
Q20   1   1.0000  0.2324  0.5000  10.25000  0.05    0.14
;
_shelx_res_checksum              13737

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_06_220_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_06_220_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_06_220_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT911_18_PJS055_06_220_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
####################################################################### 
# 
# 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_18_PJS055_02_140_00
_database_code_depnum_ccdc_archive 'CCDC 1990945'
loop_
_audit_author_name
_audit_author_address
'Ines Collings'
;Empa, Swiss Federal Laboratories for Materials Science and Technology
Switzerland
;
_audit_update_record             
;
2020-03-17 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.50 H9.50 Fe N0.75 O6.25'
_chemical_formula_weight         229.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 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'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

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

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

_cell_length_a                   12.0016(7)
_cell_length_b                   12.0016(7)
_cell_length_c                   12.0016(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1728.7(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    140.0(3)
_cell_measurement_reflns_used    423
_cell_measurement_theta_min      3.8090
_cell_measurement_theta_max      29.1650

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_F_000             942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.733
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.882
_oxdiff_exptl_absorpt_empirical_full_max 1.172
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      140.0(3)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            882
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.159
_diffrn_reflns_theta_max         29.584
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             386
_reflns_number_gt                342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0275P)²+5.9748P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         386
_refine_ls_number_parameters     30
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0893
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.182
_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 0.750000 0.250000 0.250000 0.0066(3) Uani 1 6 d S T P . .
O1 O 0.7958(2) 0.40779(19) 0.3080(2) 0.0207(5) Uani 1 1 d . . . . .
C1 C 0.7594(5) 0.500000 0.2803(4) 0.0171(11) Uani 1 2 d S T P . .
H1 H 0.697801 0.500000 0.233331 0.021 Uiso 1 2 calc R U P . .
C2 C 1.000000 0.3923(13) 0.500000 0.062(3) Uani 1 4 d S T P . .
N1 N 1.000000 0.500000 0.566(4) 0.058(7) Uiso 0.25 4 d S U P . .
N2 N 0.938(4) 0.500000 0.500000 0.058(7) Uiso 0.25 4 d S U P . .
O2 O 0.555(4) 0.500000 0.500000 0.09(3) Uiso 0.1667 4 d DS . P . .
H3 H 0.611(11) 0.500000 0.533(4) 0.105 Uiso 0.1667 2 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0066(3) 0.0066(3) 0.0066(3) 0.0006(3) -0.0006(3) -0.0006(3)
O1 0.0291(17) 0.0095(11) 0.0235(15) 0.0012(10) -0.0075(12) -0.0001(11)
C1 0.020(3) 0.013(2) 0.018(3) 0.000 -0.0073(19) 0.000
C2 0.033(6) 0.115(11) 0.038(7) 0.000 0.000 0.000

_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 2.091(2) 37_655 ?
Fe1 O1 2.091(2) 46_554 ?
Fe1 O1 2.091(2) 10_656 ?
Fe1 O1 2.091(2) 7_665 ?
Fe1 O1 2.091(2) 43_545 ?
Fe1 O1 2.091(2) . ?
O1 C1 1.235(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.49(3) . ?
C2 N2 1.49(3) 25_766 ?
C2 N1 1.51(2) . ?
C2 N1 1.51(2) 25_766 ?
N1 N2 1.09(3) . ?
N1 N2 1.09(3) 25_766 ?
N1 N1 1.57(8) 25_766 ?
N2 N2 1.50(9) 25_766 ?
O2 O2 0.93(6) 33_666 ?
O2 O2 0.93(6) 29_666 ?
O2 O2 0.93(6) 9 ?
O2 O2 0.93(6) 5 ?
O2 O2 1.32(9) 25_666 ?
O2 H3 0.78(10) . ?
O2 H3 0.78(10) 4_566 ?

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 91.38(12) 37_655 46_554 ?
O1 Fe1 O1 88.62(12) 37_655 10_656 ?
O1 Fe1 O1 180.0 46_554 10_656 ?
O1 Fe1 O1 88.62(12) 37_655 7_665 ?
O1 Fe1 O1 88.62(12) 46_554 7_665 ?
O1 Fe1 O1 91.38(12) 10_656 7_665 ?
O1 Fe1 O1 91.38(12) 37_655 43_545 ?
O1 Fe1 O1 91.38(12) 46_554 43_545 ?
O1 Fe1 O1 88.62(12) 10_656 43_545 ?
O1 Fe1 O1 180.0 7_665 43_545 ?
O1 Fe1 O1 180.00(16) 37_655 . ?
O1 Fe1 O1 88.62(12) 46_554 . ?
O1 Fe1 O1 91.38(12) 10_656 . ?
O1 Fe1 O1 91.38(12) 7_665 . ?
O1 Fe1 O1 88.62(12) 43_545 . ?
C1 O1 Fe1 129.0(3) . . ?
O1 C1 O1 127.3(5) . 27_565 ?
O1 C1 H1 116.4 . . ?
O1 C1 H1 116.4 27_565 . ?
N2 C2 N2 60(3) . 25_766 ?
N2 C2 N1 42.3(11) . . ?
N2 C2 N1 42.3(11) 25_766 . ?
N2 C2 N1 42.3(11) . 25_766 ?
N2 C2 N1 42.3(11) 25_766 25_766 ?
N1 C2 N1 63(3) . 25_766 ?
N2 N1 N2 87(5) . 25_766 ?
N2 N1 C2 67.9(19) . . ?
N2 N1 C2 67.9(19) 25_766 . ?
N2 N1 C2 67.9(19) . 25_766 ?
N2 N1 C2 67.9(19) 25_766 25_766 ?
C2 N1 C2 117(3) . 25_766 ?
N2 N1 N1 44(3) . 25_766 ?
N2 N1 N1 44(3) 25_766 25_766 ?
C2 N1 N1 58.7(14) . 25_766 ?
C2 N1 N1 58.7(14) 25_766 25_766 ?
N1 N2 N1 93(5) . 25_766 ?
N1 N2 N2 46(3) . 25_766 ?
N1 N2 N2 46(3) 25_766 25_766 ?
N1 N2 C2 69.8(19) . . ?
N1 N2 C2 69.8(19) 25_766 . ?
N2 N2 C2 59.9(15) 25_766 . ?
N1 N2 C2 69.8(19) . 25_766 ?
N1 N2 C2 69.8(19) 25_766 25_766 ?
N2 N2 C2 59.9(15) 25_766 25_766 ?
C2 N2 C2 120(3) . 25_766 ?
O2 O2 O2 59.998(10) 33_666 29_666 ?
O2 O2 O2 89.997(3) 33_666 9 ?
O2 O2 O2 59.998(6) 29_666 9 ?
O2 O2 O2 59.998(2) 33_666 5 ?
O2 O2 O2 89.997(2) 29_666 5 ?
O2 O2 O2 59.998(3) 9 5 ?
O2 O2 O2 44.998(9) 33_666 25_666 ?
O2 O2 O2 44.998(9) 29_666 25_666 ?
O2 O2 O2 44.998(9) 9 25_666 ?
O2 O2 O2 44.998(6) 5 25_666 ?
O2 O2 H3 166(6) 33_666 . ?
O2 O2 H3 127(3) 29_666 . ?
O2 O2 H3 104(6) 9 . ?
O2 O2 H3 127(3) 5 . ?
O2 O2 H3 149(6) 25_666 . ?
O2 O2 H3 104(6) 33_666 4_566 ?
O2 O2 H3 127(3) 29_666 4_566 ?
O2 O2 H3 166(6) 9 4_566 ?
O2 O2 H3 127(3) 5 4_566 ?
O2 O2 H3 149(6) 25_666 4_566 ?
H3 O2 H3 62(10) . 4_566 ?

_refine_diff_density_max         0.379
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.091

_shelx_res_file                  
;
TITL 18_PJS055_02_140_00 in P4(2)32
    18_PJS055_02_140_00.res
    created by SHELXL-2018/3 at 13:29:03 on 25-Sep-2019
REM P4(2)32 (#208 in standard setting)
CELL 0.71073  12.001594  12.001594  12.001594  90.0000  90.0000  90.0000
ZERR    8.00   0.000714   0.000714   0.000714   0.0000   0.0000   0.0000
LATT  2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SFAC C H N O FE
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $N  0.00664  0.00342 19.38436!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Fe  0.34859  0.85311 3471.86072!source kissel
UNIT 36.00 76.00 6.00 50.00 8.00
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
EQIV $1 +x, 1-y, 1-z
TWIN  0 1 0  1 0 0  0 0 -1  2
WGHT    0.027500    5.974801
BASF   0.47555
FVAR       1.30701   0.05822
FE1   5    0.750000    0.250000    0.250000    10.16667    0.00660    0.00660 =
         0.00660    0.00058   -0.00058   -0.00058
O1    4    0.795770    0.407793    0.307970    11.00000    0.02914    0.00949 =
         0.02347    0.00125   -0.00746   -0.00014
C1    1    0.759440    0.500000    0.280291    10.50000    0.02012    0.01320 =
         0.01794    0.00000   -0.00733    0.00000
AFIX  43
H1    2    0.697801    0.500000    0.233331    10.50000   -1.20000
AFIX   0
C2    1    1.000000    0.392326    0.500000    10.25000    0.03270    0.11488 =
         0.03754    0.00000    0.00000    0.00000
N1    3    1.000000    0.500000    0.565532    10.06250   21.00000
N2    3    0.937650    0.500000    0.500000    10.06250   21.00000
O2    4    0.555078    0.500000    0.500000    10.04167    0.08778
DFIX O2 H3 0.9 0.1
DFIX H3 H3_$1 0.8 0.1
H3    2    0.610660    0.500000    0.533202    10.08333   -1.20000
HKLF 4




REM  18_PJS055_02_140_00 in P4(2)32
REM wR2 = 0.0893, GooF = S = 1.183, Restrained GooF = 1.182 for all data
REM R1 = 0.0367 for 342 Fo > 4sig(Fo) and 0.0422 for all 386 data
REM 30 parameters refined using 2 restraints

END

WGHT      0.0281      5.3240

REM Highest difference peak  0.379,  deepest hole -0.657,  1-sigma level  0.091
Q1    1   1.0000  0.5530  0.5579  10.50000  0.05    0.38
Q2    1   0.5760  0.5000  0.5723  10.50000  0.05    0.33
Q3    1   0.5000  0.5000  0.5000  10.04167  0.05    0.32
Q4    1   0.8214  0.2341  0.2981  11.00000  0.05    0.32
Q5    1   0.7584  0.3191  0.3065  11.00000  0.05    0.31
Q6    1   1.0538  0.3884  0.4501  11.00000  0.05    0.30
Q7    1   1.0000  0.3603  0.4431  10.50000  0.05    0.29
Q8    1   0.6774  0.2641  0.3045  11.00000  0.05    0.26
Q9    1   1.0592  0.3149  0.5000  10.50000  0.05    0.26
Q10   1   1.0000  0.4329  0.5000  10.25000  0.05    0.25
Q11   1   1.0000  0.6029  0.6641  10.50000  0.05    0.23
Q12   1   0.8198  0.4303  0.2554  11.00000  0.05    0.22
Q13   1   1.0000  0.5000  0.6514  10.25000  0.05    0.21
Q14   1   1.0000  0.2579  0.5000  10.25000  0.05    0.21
Q15   1   0.7299  0.5000  0.5835  10.50000  0.05    0.20
Q16   1   0.7511  0.4272  0.3270  11.00000  0.05    0.20
Q17   1   0.8798  0.3143  0.3416  11.00000  0.05    0.19
Q18   1   0.9128  0.5468  0.6086  11.00000  0.05    0.17
Q19   1   0.7059  0.5394  0.5000  10.50000  0.05    0.17
Q20   1   0.9135  0.5507  0.5000  10.50000  0.05    0.17
;
_shelx_res_checksum              75052

# start Validation Reply Form
_vrf_PLAT043_18_PJS055_02_140_00 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT041_18_PJS055_02_140_00 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted due to the
disorder and to improve the data/parameter ratio, since AFIX commands could
not be implemented.
;
_vrf_PLAT068_18_PJS055_02_140_00 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check 
RESPONSE: The hydrogen positions for the DMA cation were omitted in the 
refinement, while the formula given includes all H atoms, giving rise to the 
discrepency.
;
_vrf_PLAT906_18_PJS055_02_140_00 
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.477 Check 
RESPONSE: This is observed only for the highest resolution data at 0.72 A.
;
_vrf_PLAT911_18_PJS055_02_140_00 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: These reflections were treated as outliers during the integration 
procedure in CrysAlisPro.
;
