# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_lmz_eakfecn6_300k_auto
_database_code_depnum_ccdc_archive 'CCDC 2285650'
loop_
_audit_author_name
_audit_author_address
'Xiaogang chen'
;Nanchang University
China
;
_audit_update_record             
;
2023-10-20 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT088_lmz_eakfecn6_300k_auto 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.03 Note
RESPONSE: The structure was refined with restraints to offset the effects of overfitting.
;
# Added during the CSD deposition process: Friday 20 October 2023 01:36 PM
# end Validation Reply Form

_audit_creation_date             2023-10-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 Fe2 K2 N12, 4(C2 H8 N)'
_chemical_formula_sum            'C20 H32.01 Fe2 K2 N16'
_chemical_formula_weight         686.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
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'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-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'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   11.78030(10)
_cell_length_b                   11.78030(10)
_cell_length_c                   11.78030(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1634.82(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2286
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      74.0260
_cell_measurement_theta_min      6.4940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.712
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'brownish black'
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.568
_diffrn_reflns_theta_min         6.508
_diffrn_ambient_temperature      295.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                121
_reflns_number_total             121
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.101
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.022
_refine_ls_extinction_coef       0.00060(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         121
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0166
_refine_ls_restrained_S_all      0.899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+0.8129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0454
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-N2
 1.48 with sigma of 0.02
 N2-C2
 1.5 with sigma of 0.02
 C2-C3
 1.53 with sigma of 0.02
 N2-C3
 2.4 with sigma of 0.02
 C3-C2 \\sim C2-N2
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C3 \\sim C2 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C3, C2, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: N1(0.125) C2(0.04167) H2A(0.04167) H2B(0.04167) N2(0.04167)
 H2C(0.04167) H2D(0.04167) H2E(0.04167) C3(0.04167) H3A(0.04167) H3B(0.04167)
 H3C(0.04167)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
6.b Me refined with riding coordinates:
 N2(H2C,H2D,H2E), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.000000 0.500000 0.500000 0.0482(4) Uani 1 48 d S T P . .
K1 K 0.500000 0.500000 0.500000 0.0575(5) Uani 1 48 d S T P . .
C1 C 0.1634(3) 0.500000 0.500000 0.0816(11) Uani 1 8 d S T P . .
N1 N 0.2590(3) 0.500000 0.5303(18) 0.099(7) Uani 0.25 2 d S T P . .
C2 C 0.226(4) 0.751(3) 0.787(3) 0.076(9) Uani 0.0417 1 d D U P A -1
H2A H 0.268315 0.786044 0.849120 0.091 Uiso 0.0417 1 calc R U P A -1
H2B H 0.150374 0.733375 0.814195 0.091 Uiso 0.0417 1 calc R U P A -1
N2 N 0.285(5) 0.646(3) 0.746(4) 0.092(14) Uani 0.0417 1 d D U P A -1
H2C H 0.290787 0.596484 0.802783 0.111 Uiso 0.0417 1 calc R U P A -1
H2D H 0.245812 0.615599 0.689501 0.111 Uiso 0.0417 1 calc R U P A -1
H2E H 0.354557 0.664161 0.721703 0.111 Uiso 0.0417 1 calc R U P A -1
C3 C 0.220(2) 0.831(4) 0.687(4) 0.072(13) Uani 0.0417 1 d D U P A -1
H3A H 0.183139 0.899581 0.709218 0.109 Uiso 0.0417 1 calc R U P A -1
H3B H 0.295981 0.847437 0.661711 0.109 Uiso 0.0417 1 calc R U P A -1
H3C H 0.178683 0.795055 0.626977 0.109 Uiso 0.0417 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 1.925(4) 153_565 ?
Fe1 C1 1.925(4) 173_556 ?
Fe1 C1 1.925(4) 77_455 ?
Fe1 C1 1.925(4) 57_455 ?
Fe1 C1 1.925(4) 97_566 ?
Fe1 C1 1.925(4) . ?
K1 N1 2.861(5) 109_665 ?
K1 N1 2.861(5) 98_556 ?
K1 N1 2.861(5) 2_665 ?
K1 N1 2.861(5) 102_655 ?
K1 N1 2.861(5) 18_655 ?
K1 N1 2.861(5) 106_565 ?
K1 N1 2.861(5) 6_566 ?
K1 N1 2.861(5) 117_665 ?
K1 N1 2.861(5) 13_556 ?
K1 N1 2.861(5) 21_556 ?
K1 N1 2.861(5) 114_566 ?
K1 N1 2.861(5) 10_656 ?
C1 N1 1.181(8) . ?
C1 N1 1.181(8) 114_566 ?
C1 N1 1.181(8) 17_556 ?
C1 N1 1.181(8) 98_556 ?
N1 N1 0.50(3) 17_556 ?
N1 N1 0.71(4) 98_556 ?
N1 N1 0.50(3) 114_566 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N2 1.504(12) . ?
C2 C3 1.505(12) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C1 180.0 153_565 57_455 ?
C1 Fe1 C1 90.000(1) 97_566 173_556 ?
C1 Fe1 C1 180.0 97_566 . ?
C1 Fe1 C1 90.000(1) 153_565 97_566 ?
C1 Fe1 C1 90.0 153_565 . ?
C1 Fe1 C1 90.0 57_455 97_566 ?
C1 Fe1 C1 90.0 57_455 173_556 ?
C1 Fe1 C1 90.0 153_565 77_455 ?
C1 Fe1 C1 180.0 77_455 173_556 ?
C1 Fe1 C1 90.0 57_455 77_455 ?
C1 Fe1 C1 90.000(1) 57_455 . ?
C1 Fe1 C1 90.0 97_566 77_455 ?
C1 Fe1 C1 90.000(1) 77_455 . ?
C1 Fe1 C1 90.0 153_565 173_556 ?
C1 Fe1 C1 90.0 173_556 . ?
N1 K1 N1 169.9(6) 21_556 106_565 ?
N1 K1 N1 97.1(4) 2_665 102_655 ?
N1 K1 N1 90.89(11) 2_665 13_556 ?
N1 K1 N1 90.89(11) 18_655 106_565 ?
N1 K1 N1 180.0 6_566 102_655 ?
N1 K1 N1 75.7(9) 13_556 106_565 ?
N1 K1 N1 169.9(6) 6_566 13_556 ?
N1 K1 N1 82.9(4) 2_665 10_656 ?
N1 K1 N1 104.3(9) 18_655 102_655 ?
N1 K1 N1 82.9(4) 6_566 10_656 ?
N1 K1 N1 97.1(4) 21_556 13_556 ?
N1 K1 N1 97.1(4) 98_556 6_566 ?
N1 K1 N1 97.1(4) 18_655 13_556 ?
N1 K1 N1 10.1(6) 109_665 6_566 ?
N1 K1 N1 90.89(11) 21_556 102_655 ?
N1 K1 N1 97.1(4) 2_665 106_565 ?
N1 K1 N1 180.0 117_665 21_556 ?
N1 K1 N1 97.1(4) 6_566 106_565 ?
N1 K1 N1 82.9(4) 117_665 114_566 ?
N1 K1 N1 10.1(6) 21_556 10_656 ?
N1 K1 N1 97.1(4) 21_556 114_566 ?
N1 K1 N1 89.11(11) 18_655 10_656 ?
N1 K1 N1 104.3(9) 117_665 2_665 ?
N1 K1 N1 104.3(9) 13_556 10_656 ?
N1 K1 N1 75.7(9) 21_556 2_665 ?
N1 K1 N1 75.7(9) 18_655 6_566 ?
N1 K1 N1 169.9(6) 114_566 2_665 ?
N1 K1 N1 89.11(11) 117_665 102_655 ?
N1 K1 N1 75.7(9) 117_665 98_556 ?
N1 K1 N1 75.7(9) 114_566 102_655 ?
N1 K1 N1 104.3(9) 21_556 98_556 ?
N1 K1 N1 82.9(4) 98_556 102_655 ?
N1 K1 N1 10.1(6) 114_566 98_556 ?
N1 K1 N1 169.9(6) 109_665 102_655 ?
N1 K1 N1 180.0 2_665 98_556 ?
N1 K1 N1 82.9(4) 117_665 13_556 ?
N1 K1 N1 97.1(4) 117_665 18_655 ?
N1 K1 N1 82.9(4) 114_566 13_556 ?
N1 K1 N1 82.9(4) 21_556 18_655 ?
N1 K1 N1 89.11(11) 98_556 13_556 ?
N1 K1 N1 180.0 114_566 18_655 ?
N1 K1 N1 180.0(9) 109_665 13_556 ?
N1 K1 N1 10.1(6) 2_665 18_655 ?
N1 K1 N1 10.1(6) 117_665 106_565 ?
N1 K1 N1 169.9(6) 98_556 18_655 ?
N1 K1 N1 89.11(11) 114_566 106_565 ?
N1 K1 N1 97.1(4) 117_665 109_665 ?
N1 K1 N1 82.9(4) 98_556 106_565 ?
N1 K1 N1 82.9(4) 21_556 109_665 ?
N1 K1 N1 104.3(9) 109_665 106_565 ?
N1 K1 N1 97.1(4) 114_566 109_665 ?
N1 K1 N1 82.9(4) 102_655 106_565 ?
N1 K1 N1 89.11(11) 2_665 109_665 ?
N1 K1 N1 169.9(6) 117_665 10_656 ?
N1 K1 N1 90.89(11) 98_556 109_665 ?
N1 K1 N1 90.89(11) 114_566 10_656 ?
N1 K1 N1 82.9(4) 18_655 109_665 ?
N1 K1 N1 97.1(4) 98_556 10_656 ?
N1 K1 N1 90.89(11) 117_665 6_566 ?
N1 K1 N1 75.7(9) 109_665 10_656 ?
N1 K1 N1 89.11(11) 21_556 6_566 ?
N1 K1 N1 97.1(4) 102_655 10_656 ?
N1 K1 N1 104.3(9) 114_566 6_566 ?
N1 K1 N1 180.0 106_565 10_656 ?
N1 K1 N1 82.9(4) 2_665 6_566 ?
N1 K1 N1 10.1(6) 102_655 13_556 ?
N1 C1 Fe1 162.4(10) 17_556 . ?
N1 C1 Fe1 162.4(10) 114_566 . ?
N1 C1 Fe1 162.4(10) 98_556 . ?
N1 C1 Fe1 162.4(10) . . ?
N1 C1 N1 35(2) 17_556 114_566 ?
N1 C1 N1 24.7(14) 17_556 98_556 ?
N1 C1 N1 24.7(14) . 114_566 ?
N1 C1 N1 24.7(14) 98_556 114_566 ?
N1 C1 N1 24.7(14) . 17_556 ?
N1 C1 N1 35(2) . 98_556 ?
C1 N1 K1 155.2(14) . . ?
N1 N1 K1 84.9(3) 114_566 . ?
N1 N1 K1 84.9(3) 17_556 . ?
N1 N1 K1 82.8(4) 98_556 . ?
N1 N1 C1 77.7(7) 17_556 . ?
N1 N1 C1 72.4(10) 98_556 . ?
N1 N1 C1 77.7(7) 114_566 . ?
N1 N1 N1 45.004(3) 114_566 98_556 ?
N1 N1 N1 45.004(3) 17_556 98_556 ?
N1 N1 N1 90.007(4) 114_566 17_556 ?
H2A C2 H2B 108.7 . . ?
N2 C2 H2A 110.5 . . ?
N2 C2 H2B 110.5 . . ?
N2 C2 C3 106.1(19) . . ?
C3 C2 H2A 110.5 . . ?
C3 C2 H2B 110.5 . . ?
C2 N2 H2C 109.5 . . ?
C2 N2 H2D 109.5 . . ?
C2 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 C1 N1 K1 180.000(2) . . . . ?
Fe1 C1 N1 N1 133.63(17) . . . 114_566 ?
Fe1 C1 N1 N1 180.000(4) . . . 98_556 ?
Fe1 C1 N1 N1 -133.63(15) . . . 17_556 ?
N1 C1 N1 K1 0.000(1) 98_556 . . . ?
N1 C1 N1 K1 -46.37(16) 17_556 . . . ?
N1 C1 N1 K1 46.37(16) 114_566 . . . ?
N1 C1 N1 N1 92.7(3) 114_566 . . 17_556 ?
N1 C1 N1 N1 -92.7(3) 17_556 . . 114_566 ?
N1 C1 N1 N1 -46.37(17) 98_556 . . 114_566 ?
N1 C1 N1 N1 46.37(15) 114_566 . . 98_556 ?
N1 C1 N1 N1 46.37(16) 98_556 . . 17_556 ?
N1 C1 N1 N1 -46.37(16) 17_556 . . 98_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_oh_ea_kfecn_403k_auto
_database_code_depnum_ccdc_archive 'CCDC 2285651'
loop_
_audit_author_name
_audit_author_address
'Xiaogang chen'
;Nanchang University
China
;
_audit_update_record             
;
2023-10-19 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT088_oh_ea_kfecn_403k_auto 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.29 Note
RESPONSE: The structure was refined with restraints to offset the effects of overfitting.
;
# Added during the CSD deposition process: Thursday 19 October 2023 12:57 PM
# end Validation Reply Form

_audit_creation_date             2023-10-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 Fe2 K2 N12, 4(C2 H8 N O)'
_chemical_formula_sum            'C20 H32.03 Fe2 K2 N16 O4'
_chemical_formula_weight         750.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
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'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-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'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   11.9312(5)
_cell_length_b                   11.9312(5)
_cell_length_c                   11.9312(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1698.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    390
_cell_measurement_temperature    403(2)
_cell_measurement_theta_max      26.4120
_cell_measurement_theta_min      2.9640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0105
_diffrn_reflns_av_unetI/netI     0.0053
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            643
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.070
_diffrn_reflns_theta_min         2.957
_diffrn_ambient_temperature      403.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                130
_reflns_number_total             148
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         148
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²+0.0429P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0932
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-C2
 1.38 with sigma of 0.02
 C2-C3
 1.53 with sigma of 0.02
 C3-N2
 1.35 with sigma of 0.02
 C2-N2
 2.4 with sigma of 0.04
 O1-C3
 2.415 with sigma of 0.04
 N2-C3 \\sim C3-C2 \\sim O1-C2
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
O1 \\sim C2 \\sim C3 \\sim N2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O1, C2, C3, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.04167) H1(0.04167) C2(0.04167) H2A(0.04167) H2B(0.04167)
 C3(0.04167) H3A(0.04167) H3B(0.04167) N2(0.04167) H2C(0.04167) H2D(0.04167)
 H2E(0.04167)
6.a Riding coordinates:
 O1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
6.c Me refined with riding coordinates:
 N2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.500000 0.500000 0.0568(6) Uani 1 48 d S T P . .
K1 K 0.500000 0.500000 1.000000 0.0738(7) Uani 1 48 d S T P . .
C1 C 0.500000 0.500000 0.6620(4) 0.0794(12) Uani 1 8 d S T P . .
N1 N 0.500000 0.500000 0.7575(3) 0.124(3) Uani 1 8 d S T P . .
O1 O 0.3757(17) 0.737(3) 0.787(3) 0.096(15) Uani 0.0417 1 d D U P A -1
H1 H 0.428885 0.751754 0.827805 0.144 Uiso 0.0417 1 d R U P A -1
C2 C 0.2674(17) 0.785(4) 0.803(4) 0.097(16) Uani 0.0417 1 d D U P A -1
H2A H 0.271915 0.864712 0.789264 0.117 Uiso 0.0417 1 calc R U P A -1
H2B H 0.245517 0.774101 0.880416 0.117 Uiso 0.0417 1 calc R U P A -1
C3 C 0.182(2) 0.739(3) 0.733(3) 0.087(13) Uani 0.0417 1 d D U P A -1
H3A H 0.118328 0.719601 0.778739 0.104 Uiso 0.0417 1 calc R U P A -1
H3B H 0.158586 0.796058 0.680082 0.104 Uiso 0.0417 1 calc R U P A -1
N2 N 0.215(4) 0.6419(18) 0.671(2) 0.089(16) Uani 0.0417 1 d D U P A -1
H2C H 0.157685 0.618483 0.629265 0.107 Uiso 0.0417 1 calc R U P A -1
H2D H 0.272567 0.658888 0.626493 0.107 Uiso 0.0417 1 calc R U P A -1
H2E H 0.235175 0.587873 0.718128 0.107 Uiso 0.0417 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 1.933(4) 105_666 ?
Fe1 C1 1.933(4) 101_666 ?
Fe1 C1 1.933(4) 5 ?
Fe1 C1 1.933(4) 9 ?
Fe1 C1 1.933(4) 97_666 ?
Fe1 C1 1.933(4) . ?
K1 N1 2.894(4) 129_666 ?
K1 N1 2.894(4) 149_666 ?
K1 N1 2.894(4) 53_455 ?
K1 N1 2.894(4) 33_545 ?
K1 N1 2.894(4) 97_667 ?
K1 N1 2.894(4) . ?
C1 N1 1.139(5) . ?
O1 H1 0.8200 . ?
O1 C2 1.424(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.425(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 N2 1.424(12) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C1 180.0 105_666 9 ?
C1 Fe1 C1 90.000(1) 97_666 101_666 ?
C1 Fe1 C1 180.0 97_666 . ?
C1 Fe1 C1 90.0 105_666 97_666 ?
C1 Fe1 C1 90.0 105_666 . ?
C1 Fe1 C1 90.0 9 97_666 ?
C1 Fe1 C1 90.0 9 101_666 ?
C1 Fe1 C1 90.0 105_666 5 ?
C1 Fe1 C1 180.0 5 101_666 ?
C1 Fe1 C1 90.000(1) 9 5 ?
C1 Fe1 C1 90.0 9 . ?
C1 Fe1 C1 90.0 97_666 5 ?
C1 Fe1 C1 90.0 5 . ?
C1 Fe1 C1 90.000(1) 105_666 101_666 ?
C1 Fe1 C1 90.000(1) 101_666 . ?
N1 K1 N1 180.0 129_666 33_545 ?
N1 K1 N1 90.000(1) 97_667 149_666 ?
N1 K1 N1 90.0 53_455 . ?
N1 K1 N1 90.0 129_666 97_667 ?
N1 K1 N1 90.0 33_545 . ?
N1 K1 N1 90.0 33_545 97_667 ?
N1 K1 N1 90.0 33_545 149_666 ?
N1 K1 N1 90.0 129_666 53_455 ?
N1 K1 N1 180.0 53_455 149_666 ?
N1 K1 N1 90.000(1) 33_545 53_455 ?
N1 K1 N1 180.0 97_667 . ?
N1 K1 N1 90.0 97_667 53_455 ?
N1 K1 N1 90.0 149_666 . ?
N1 K1 N1 90.000(1) 129_666 149_666 ?
N1 K1 N1 90.0 129_666 . ?
N1 C1 Fe1 180.0 . . ?
C1 N1 K1 180.0 . . ?
C2 O1 H1 122.5 . . ?
O1 C2 H2A 108.7 . . ?
O1 C2 H2B 108.7 . . ?
O1 C2 C3 114(2) . . ?
H2A C2 H2B 107.6 . . ?
C3 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
N2 C3 C2 115(3) . . ?
N2 C3 H3A 108.5 . . ?
N2 C3 H3B 108.5 . . ?
C3 N2 H2C 109.5 . . ?
C3 N2 H2D 109.5 . . ?
C3 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 N2 9(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lmz_yakfecn6_243k_auto
_database_code_depnum_ccdc_archive 'CCDC 2285652'
loop_
_audit_author_name
_audit_author_address
'Xiaogang chen'
;Nanchang University
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Fe K N6, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H16 Fe K N8'
_chemical_formula_weight         343.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   7.9025(6)
_cell_length_b                   8.5039(7)
_cell_length_c                   11.9308(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.407(7)
_cell_angle_gamma                90
_cell_volume                     801.53(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    243(2)
_cell_measurement_reflns_used    2224
_cell_measurement_theta_min      6.3240
_cell_measurement_theta_max      74.3610

_exptl_crystal_description       bulk
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_F_000             354
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    9.904
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_T_max  0.371
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      243(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6855
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         6.392
_diffrn_reflns_theta_max         76.648
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             1620
_reflns_number_gt                1309
_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       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_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)+(0.1200P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1620
_refine_ls_number_parameters     96
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.1066
_refine_ls_wR_factor_ref         0.2628
_refine_ls_wR_factor_gt          0.2539
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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 0.500000 1.000000 1.000000 0.0280(5) Uani 1 2 d S . P . .
K1 K 0.000000 0.500000 1.000000 0.0369(6) Uani 1 2 d S . P . .
N2 N 0.5405(10) 0.9658(8) 0.7444(5) 0.0476(16) Uani 1 1 d . . . . .
N1 N 0.2829(8) 0.6985(9) 1.0126(6) 0.0488(16) Uani 1 1 d . . . . .
C2 C 0.5186(9) 0.9802(8) 0.8390(6) 0.0347(15) Uani 1 1 d . . . . .
N4 N 0.5848(9) 0.6241(8) 0.6956(6) 0.0545(18) Uani 1 1 d . . . . .
H4A H 0.531661 0.617864 0.628127 0.082 Uiso 1 1 calc R U . . .
H4B H 0.686139 0.576143 0.692502 0.082 Uiso 1 1 calc R U . . .
H4C H 0.599771 0.725724 0.714264 0.082 Uiso 1 1 calc R U . . .
N3 N 0.1688(9) 1.1931(9) 0.9837(6) 0.0550(18) Uani 1 1 d . . . . .
C1 C 0.3666(8) 0.8093(8) 1.0073(5) 0.0337(14) Uani 1 1 d . . . . .
C3 C 0.2934(9) 1.1255(9) 0.9879(6) 0.0385(16) Uani 1 1 d . . . . .
C5 C 0.4426(14) 0.3822(12) 0.7472(9) 0.071(3) Uani 1 1 d . . . . .
H5A H 0.382396 0.382469 0.675356 0.107 Uiso 1 1 calc R U . . .
H5B H 0.372939 0.332758 0.802999 0.107 Uiso 1 1 calc R U . . .
H5C H 0.547516 0.324117 0.740831 0.107 Uiso 1 1 calc R U . . .
C4 C 0.4803(15) 0.5453(12) 0.7813(8) 0.064(3) Uani 1 1 d . . . . .
H4D H 0.541546 0.545374 0.853721 0.077 Uiso 1 1 calc R U . . .
H4E H 0.374361 0.603435 0.789954 0.077 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.937(7) 3_677 ?
Fe1 C2 1.937(7) . ?
Fe1 C1 1.937(7) . ?
Fe1 C1 1.937(7) 3_677 ?
Fe1 C3 1.953(7) . ?
Fe1 C3 1.953(7) 3_677 ?
K1 N1 2.802(6) . ?
K1 N1 2.802(6) 3_567 ?
K1 N3 2.939(7) 3_577 ?
K1 N3 2.939(7) 1_545 ?
K1 N2 2.940(6) 4_576 ?
K1 N2 2.940(6) 2_546 ?
N2 C2 1.153(9) . ?
N1 C1 1.154(9) . ?
N4 C4 1.489(12) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N4 H4C 0.9000 . ?
N3 C3 1.140(9) . ?
C5 C4 1.474(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Fe1 C2 180.0 3_677 . ?
C2 Fe1 C1 88.5(3) 3_677 . ?
C2 Fe1 C1 91.5(3) . . ?
C2 Fe1 C1 91.5(3) 3_677 3_677 ?
C2 Fe1 C1 88.5(3) . 3_677 ?
C1 Fe1 C1 180.0 . 3_677 ?
C2 Fe1 C3 86.7(3) 3_677 . ?
C2 Fe1 C3 93.3(3) . . ?
C1 Fe1 C3 90.3(3) . . ?
C1 Fe1 C3 89.7(3) 3_677 . ?
C2 Fe1 C3 93.3(3) 3_677 3_677 ?
C2 Fe1 C3 86.7(3) . 3_677 ?
C1 Fe1 C3 89.7(3) . 3_677 ?
C1 Fe1 C3 90.3(3) 3_677 3_677 ?
C3 Fe1 C3 180.0(4) . 3_677 ?
N1 K1 N1 180.0 . 3_567 ?
N1 K1 N3 79.9(2) . 3_577 ?
N1 K1 N3 100.1(2) 3_567 3_577 ?
N1 K1 N3 100.1(2) . 1_545 ?
N1 K1 N3 79.9(2) 3_567 1_545 ?
N3 K1 N3 180.0 3_577 1_545 ?
N1 K1 N2 79.6(2) . 4_576 ?
N1 K1 N2 100.4(2) 3_567 4_576 ?
N3 K1 N2 83.4(2) 3_577 4_576 ?
N3 K1 N2 96.6(2) 1_545 4_576 ?
N1 K1 N2 100.4(2) . 2_546 ?
N1 K1 N2 79.6(2) 3_567 2_546 ?
N3 K1 N2 96.6(2) 3_577 2_546 ?
N3 K1 N2 83.4(2) 1_545 2_546 ?
N2 K1 N2 180.0 4_576 2_546 ?
C2 N2 K1 161.0(6) . 2_556 ?
C1 N1 K1 161.1(6) . . ?
N2 C2 Fe1 175.5(7) . . ?
C4 N4 H4A 109.5 . . ?
C4 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C3 N3 K1 146.9(6) . 1_565 ?
N1 C1 Fe1 177.9(6) . . ?
N3 C3 Fe1 176.6(7) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C5 C4 N4 110.2(8) . . ?
C5 C4 H4D 109.6 . . ?
N4 C4 H4D 109.6 . . ?
C5 C4 H4E 109.6 . . ?
N4 C4 H4E 109.6 . . ?
H4D C4 H4E 108.1 . . ?


_refine_diff_density_max         2.181
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.206



####################################################################### 
# 
# 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_oh_ea_kfecn6_300k_auto
_database_code_depnum_ccdc_archive 'CCDC 2285653'
loop_
_audit_author_name
_audit_author_address
'Xiaogang chen'
;Nanchang University
China
;
_audit_update_record             
;
2023-10-19 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5-dev
(compiled 2023.09.12 svn.re1ec1418 for OlexSys, GUI svn.r6697)
;
_chemical_formula_moiety         'C6 Fe K N6, 2(C2 H8 N O)'
_chemical_formula_sum            'C10 H16 Fe K N8 O2'
_chemical_formula_weight         375.235
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Fe -1.13125 3.15233 11.76950 7.35730 3.52220 2.30450 4.76110 0.30720 15.35350
76.88050 1.03690 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
K 0.38695 1.06752 8.21860 7.43980 1.05190 0.86590 12.79490 0.77480 213.18700
41.68410 1.42280 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   11.7710(3)
_cell_length_b                   11.6695(3)
_cell_length_c                   11.9739(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.999(2)
_cell_angle_gamma                90
_cell_volume                     1643.75(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3418
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      71.3710
_cell_measurement_theta_min      3.7790
_exptl_absorpt_coefficient_mu    9.806
_exptl_absorpt_correction_T_max  0.189
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             772.232
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.9801
_diffrn_reflns_Laue_measured_fraction_max 0.9558
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7881
_diffrn_reflns_point_group_measured_fraction_full 0.9801
_diffrn_reflns_point_group_measured_fraction_max 0.9558
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         71.59
_diffrn_reflns_theta_min         5.18
_diffrn_ambient_temperature      300.15
_diffrn_measured_fraction_theta_full 0.9801
_diffrn_measured_fraction_theta_max 0.9558
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              -9
_reflns_number_gt                2588
_reflns_number_total             3073
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.1389
_refine_diff_density_min         -0.4985
_refine_diff_density_rms         0.0992
_refine_ls_d_res_high            0.8125
_refine_ls_d_res_low             8.5392
_refine_ls_extinction_coef       0.0037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3073
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.0181
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0906P)²+0.4314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1363
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O2-C10 \\sim O2a-C10a
 with sigma of 0.02
 N8-C10 \\sim N8-C10a
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N8, C9a, C10, C10a, O2, O2a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O2a)=Sof(H2a)=Sof(H9ac)=Sof(H9ad)=Sof(C10a)=Sof(H10c)=Sof(H10d)=1-FVAR(1)
 Sof(O2)=Sof(H2)=Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(H9aa)=Sof(H9ab)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7d,H7e), C8(H8d,H8e), C10(H10a,H10b), C9a(H9aa,H9ab), C9a(H9ac,H9ad),
 C10a(H10c,H10d)
5.b Idealised Me refined as rotating group:
 N7(H7a,H7b,H7c), N8(H8a,H8b,H8c)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O2a(H2a)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
Fe1 Fe 0.27437(3) 0.75269(3) 0.50953(3) 0.01446(18) Uani 1.000000 . . . .
K1 K 0.27451(4) 0.75546(4) 1.00385(4) 0.0225(2) Uani 1.000000 . . . .
O1 O 0.46069(18) 0.38792(18) 0.6836(2) 0.0480(6) Uani 1.000000 . . . .
H1 H 0.426(3) 0.4072(16) 0.6258(10) 0.0720(9) Uiso 1.000000 GR . . .
N2 N 0.2795(2) 0.75672(17) 0.2509(2) 0.0300(7) Uani 1.000000 . . . .
N6 N 0.2800(2) 0.74885(17) 0.7671(2) 0.0351(8) Uani 1.000000 . . . .
N7 N 0.64679(19) 0.5140(2) 0.7528(2) 0.0372(6) Uani 1.000000 . . . .
H7a H 0.6465(4) 0.4567(11) 0.7037(12) 0.0446(7) Uiso 1.000000 GR . . .
H7b H 0.6959(3) 0.5675(5) 0.7325(15) 0.0446(7) Uiso 1.000000 GR . . .
H7c H 0.6673(7) 0.4875(15) 0.8202(4) 0.0446(7) Uiso 1.000000 GR . . .
C2 C 0.2756(2) 0.75401(17) 0.3465(2) 0.0202(6) Uani 1.000000 . . . .
N8 N 0.46027(19) 1.1442(2) 0.73581(18) 0.0371(6) Uani 1.000000 D U . .
H8a H 0.5071(13) 1.1512(3) 0.6794(10) 0.0446(7) Uiso 1.000000 GR . . .
H8b H 0.3978(3) 1.1855(3) 0.7215(15) 0.0446(7) Uiso 1.000000 GR . . .
H8c H 0.4947(14) 1.1694(5) 0.7985(6) 0.0446(7) Uiso 1.000000 GR . . .
C1 C 0.2960(2) 0.5875(2) 0.50922(18) 0.0236(5) Uani 1.000000 . . . .
C6 C 0.2788(2) 0.75172(17) 0.6715(2) 0.0213(6) Uani 1.000000 . . . .
C4 C 0.2458(2) 0.9164(2) 0.50594(18) 0.0225(5) Uani 1.000000 . . . .
N5 N 0.0143(2) 0.7173(3) 0.5167(2) 0.0442(6) Uani 1.000000 . . . .
N3 N 0.53380(19) 0.7937(3) 0.5202(2) 0.0427(6) Uani 1.000000 . . . .
N1 N 0.3073(2) 0.4903(2) 0.5061(2) 0.0432(6) Uani 1.000000 . . . .
N4 N 0.2250(2) 1.0121(2) 0.4990(2) 0.0415(6) Uani 1.000000 . . . .
C3 C 0.4374(2) 0.7781(2) 0.5159(2) 0.0240(5) Uani 1.000000 . . . .
C5 C 0.1106(2) 0.7299(2) 0.5105(2) 0.0239(5) Uani 1.000000 . . . .
O2 O 0.6126(2) 0.9721(3) 0.6953(3) 0.0464(9) Uani 0.732(5) D U P 1
H2 H 0.600(3) 0.934(3) 0.6388(18) 0.0696(13) Uiso 0.732(5) GR . P 1
C7 C 0.5314(3) 0.5644(3) 0.7561(3) 0.0472(9) Uani 1.000000 . . . .
H7d H 0.5270(3) 0.6154(3) 0.8197(3) 0.0566(10) Uiso 1.000000 R . . .
H7e H 0.5155(3) 0.6085(3) 0.6887(3) 0.0566(10) Uiso 1.000000 R . . .
C8 C 0.4470(3) 0.4716(3) 0.7650(3) 0.0482(8) Uani 1.000000 . . . .
H8d H 0.3711(3) 0.5036(3) 0.7571(3) 0.0579(10) Uiso 1.000000 R . . .
H8e H 0.4548(3) 0.4367(3) 0.8384(3) 0.0579(10) Uiso 1.000000 R . . .
C10 C 0.5348(9) 0.9515(10) 0.7663(11) 0.049(2) Uani 0.732(5) D U P 1
H10a H 0.5136(9) 0.8713(10) 0.7611(11) 0.059(2) Uiso 0.732(5) R . P 1
H10b H 0.5661(9) 0.9649(10) 0.8412(11) 0.059(2) Uiso 0.732(5) R . P 1
O2a O 0.6164(6) 0.9974(6) 0.8300(7) 0.040(2) Uani 0.268(5) D U P 2
H2a H 0.623(6) 0.971(8) 0.893(4) 0.059(3) Uiso 0.268(5) GR . P 2
C9a C 0.4293(3) 1.0238(3) 0.7490(3) 0.0474(8) Uani 1.000000 . U . .
H9aa H 0.3812(3) 1.0154(3) 0.8127(3) 0.0569(9) Uiso 0.732(5) R . P 1
H9ab H 0.3868(3) 0.9978(3) 0.6829(3) 0.0569(9) Uiso 0.732(5) R . P 1
H9ac H 0.3742(3) 1.0181(3) 0.8071(3) 0.0569(9) Uiso 0.268(5) R . P 2
H9ad H 0.3927(3) 0.9973(3) 0.6799(3) 0.0569(9) Uiso 0.268(5) R . P 2
C10a C 0.520(2) 0.951(3) 0.776(3) 0.044(4) Uani 0.268(5) D U P 2
H10c H 0.544(2) 0.916(3) 0.707(3) 0.053(4) Uiso 0.268(5) R . P 2
H10d H 0.492(2) 0.890(3) 0.823(3) 0.053(4) Uiso 0.268(5) R . P 2


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 C2 1.953(3) . y
Fe1 C1 1.944(2) . y
Fe1 C6 1.939(3) . y
Fe1 C4 1.941(2) . y
Fe1 C3 1.941(2) . y
Fe1 C5 1.946(3) . y
K1 N2 2.956(2) 1_556 y
K1 N6 2.839(3) . y
K1 N5 2.840(2) 4_676 y
K1 N3 2.904(2) 4_576 y
K1 N1 2.906(2) 2_556 y
K1 N4 2.840(2) 2_546 y
O1 H1 0.8200 . ?
O1 C8 1.393(4) . ?
N2 C2 1.148(4) . ?
N6 C6 1.144(4) . ?
N7 H7a 0.8900 . ?
N7 H7b 0.8900 . ?
N7 H7c 0.8900 . ?
N7 C7 1.482(4) . ?
N8 H8a 0.8900 . ?
N8 H8b 0.8900 . ?
N8 H8c 0.8900 . ?
N8 C9a 1.462(4) . ?
C1 N1 1.143(3) . ?
C4 N4 1.145(3) . ?
N5 C5 1.148(4) . ?
N3 C3 1.148(3) . ?
O2 H2 0.8200 . ?
O2 C10 1.294(11) . ?
C7 H7d 0.9700 . ?
C7 H7e 0.9700 . ?
C7 C8 1.476(5) . ?
C8 H8d 0.9700 . ?
C8 H8e 0.9700 . ?
C10 H10a 0.9700 . ?
C10 H10b 0.9700 . ?
C10 C9a 1.509(12) . ?
O2a H2a 0.8200 . ?
O2a C10a 1.39(3) . ?
C9a H9aa 0.9700 . ?
C9a H9ab 0.9700 . ?
C9a H9ac 0.9700 . ?
C9a H9ad 0.9700 . ?
C9a C10a 1.40(3) . ?
C10a H10c 0.9700 . ?
C10a H10d 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C2 90.02(9) . . y
C6 Fe1 C2 178.05(10) . . y
C6 Fe1 C1 89.84(9) . . y
C4 Fe1 C2 88.70(9) . . y
C4 Fe1 C1 177.24(9) . . y
C4 Fe1 C6 91.52(9) . . y
C3 Fe1 C2 89.80(11) . . y
C3 Fe1 C1 91.26(11) . . y
C3 Fe1 C6 88.26(11) . . y
C3 Fe1 C4 91.19(11) . . y
C5 Fe1 C2 92.79(11) . . y
C5 Fe1 C1 89.70(10) . . y
C5 Fe1 C6 89.15(11) . . y
C5 Fe1 C4 87.91(10) . . y
C5 Fe1 C3 177.24(10) . . y
N6 K1 N2 177.24(8) . 1_556 y
N5 K1 N2 87.71(8) 4_676 1_556 y
N5 K1 N6 90.01(8) 4_676 . y
N3 K1 N2 85.36(7) 4_576 1_556 y
N3 K1 N6 96.78(8) 4_576 . y
N3 K1 N5 171.44(8) 4_576 4_676 y
N1 K1 N2 91.80(6) 2_556 1_556 y
N1 K1 N6 90.21(7) 2_556 . y
N1 K1 N5 102.95(8) 2_556 4_676 y
N1 K1 N3 82.32(8) 2_556 4_576 y
N4 K1 N2 90.97(6) 2_546 1_556 y
N4 K1 N6 87.75(6) 2_546 . y
N4 K1 N5 96.33(8) 2_546 4_676 y
N4 K1 N3 78.78(8) 2_546 4_576 y
N4 K1 N1 160.61(7) 2_546 2_556 y
C8 O1 H1 109.5 . . ?
C2 N2 K1 176.1(2) . 1_554 ?
C6 N6 K1 176.2(2) . . ?
H7b N7 H7a 109.5 . . ?
H7c N7 H7a 109.5 . . ?
H7c N7 H7b 109.5 . . ?
C7 N7 H7a 109.5 . . ?
C7 N7 H7b 109.5 . . ?
C7 N7 H7c 109.5 . . ?
N2 C2 Fe1 177.8(2) . . ?
H8b N8 H8a 109.5 . . ?
H8c N8 H8a 109.5 . . ?
H8c N8 H8b 109.5 . . ?
C9a N8 H8a 109.5 . . ?
C9a N8 H8b 109.5 . . ?
C9a N8 H8c 109.5 . . ?
N1 C1 Fe1 178.1(2) . . ?
N6 C6 Fe1 178.4(2) . . ?
N4 C4 Fe1 176.3(2) . . ?
C5 N5 K1 164.6(3) . 4_575 ?
C3 N3 K1 158.5(3) . 4_675 ?
C1 N1 K1 154.0(2) . 2_546 ?
C4 N4 K1 167.2(2) . 2_556 ?
N3 C3 Fe1 179.6(3) . . ?
N5 C5 Fe1 176.6(2) . . ?
C10 O2 H2 109.5 . . ?
H7d C7 N7 109.81(16) . . ?
H7e C7 N7 109.81(17) . . ?
H7e C7 H7d 108.3 . . ?
C8 C7 N7 109.3(3) . . ?
C8 C7 H7d 109.81(19) . . ?
C8 C7 H7e 109.8(2) . . ?
C7 C8 O1 111.6(3) . . ?
H8d C8 O1 109.29(17) . . ?
H8d C8 C7 109.3(2) . . ?
H8e C8 O1 109.29(19) . . ?
H8e C8 C7 109.3(2) . . ?
H8e C8 H8d 108.0 . . ?
H10a C10 O2 108.8(5) . . ?
H10b C10 O2 108.8(6) . . ?
H10b C10 H10a 107.7 . . ?
C9a C10 O2 113.8(9) . . ?
C9a C10 H10a 108.8(4) . . ?
C9a C10 H10b 108.8(5) . . ?
C10a O2a H2a 109.5 . . ?
C10 C9a N8 110.2(5) . . ?
H9aa C9a N8 109.62(16) . . ?
H9aa C9a C10 109.6(5) . . ?
H9ab C9a N8 109.62(17) . . ?
H9ab C9a C10 109.6(5) . . ?
H9ab C9a H9aa 108.1 . . ?
H9ac C9a N8 108.59(16) . . ?
H9ac C9a C10 115.5(5) . . ?
H9ac C9a H9aa 6.4 . . ?
H9ac C9a H9ab 103.0 . . ?
H9ad C9a N8 108.59(17) . . ?
H9ad C9a C10 106.2(5) . . ?
H9ad C9a H9aa 112.6 . . ?
H9ad C9a H9ab 4.7 . . ?
H9ad C9a H9ac 107.6 . . ?
C10a C9a N8 114.7(12) . . ?
C10a C9a C10 7.0(18) . . ?
C10a C9a H9aa 102.8(14) . . ?
C10a C9a H9ab 111.6(12) . . ?
C10a C9a H9ac 108.6(14) . . ?
C10a C9a H9ad 108.6(12) . . ?
C9a C10a O2a 118(2) . . ?
H10c C10a O2a 107.7(13) . . ?
H10c C10a C9a 107.7(13) . . ?
H10d C10a O2a 107.7(15) . . ?
H10d C10a C9a 107.7(14) . . ?
H10d C10a H10c 107.11156790(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C8 C7 N7 -51.4(3) . . . . ?
N8 C9a C10 O2 -48.1(4) . . . . ?
N8 C9a C10a O2a 25.2(6) . . . . ?
O2 C10 C9a C10a -179(6) . . . . ?
C10 C9a C10a O2a 76(13) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
N8 C10 1 2
N8 C10a 1 2
O2 C10 1 1
O2a C10a 1 1

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0200 1.3428 0.0488 0.0488
2 0.0400 2.4230 0.0139 0.0139

loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
N8 C10 0.004000 -0.011651 -0.009742 0.003104
N8 C9a 0.004000 -0.014129 -0.017377 -0.002998
N8 C10a 0.004000 -0.006818 -0.008684 -0.009486
O2 C10 0.004000 0.011380 0.000449 -0.011407
O2 C9a 0.004000 0.004561 -0.004158 -0.007083
C10 C9a 0.004000 0.015875 0.012608 -0.005297
C10 C10a 0.004000 0.000030 0.000003 0.000049
O2a C9a 0.004000 0.004769 0.015287 -0.016369
O2a C10a 0.004000 0.008652 -0.004704 -0.003463
C9a C10a 0.004000 -0.004737 -0.009575 0.006054

