# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_1a(100K)
_database_code_depnum_ccdc_archive 'CCDC 2002656'
loop_
_audit_author_name
_audit_author_address
'Kil Sik Min'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Cl4 Fe N4 O2, N O3, H2 O'
_chemical_formula_sum            'C32 H20 Cl4 Fe N5 O6'
_chemical_formula_weight         768.18

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'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1453 0.1556 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3456 0.8258 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.4930(19)
_cell_length_b                   11.327(2)
_cell_length_c                   15.069(3)
_cell_angle_alpha                105.08(3)
_cell_angle_beta                 100.34(3)
_cell_angle_gamma                94.92(3)
_cell_volume                     1524.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27459
_cell_measurement_theta_min      0.40
_cell_measurement_theta_max      29.54

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             778
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.868
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_absorpt_special_details   
;
Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.932, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detertor'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14642
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.852
_diffrn_reflns_theta_max         29.491
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measured_fraction_theta_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_point_group_measured_fraction_full 0.932
_reflns_number_total             7484
_reflns_number_gt                5520
_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       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    "SHELXS-2013'(sheldrick, 2013)"
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_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)+(0.1568P)²] 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     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.094(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7484
_refine_ls_number_parameters     440
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.2092
_refine_ls_wR_factor_gt          0.1912
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.34796(5) 0.70663(4) 0.25377(3) 0.03948(18) Uani 1 1 d . . . . .
Cl1 Cl -0.06420(10) 0.24184(10) 0.38028(7) 0.0652(3) Uani 1 1 d . . . . .
Cl2 Cl 0.01135(9) 0.36824(8) 0.06959(6) 0.0521(2) Uani 1 1 d . . . . .
Cl3 Cl -0.28147(10) 0.98956(9) 0.12216(7) 0.0573(3) Uani 1 1 d . . . . .
Cl4 Cl -0.05023(9) 0.79162(8) 0.39416(5) 0.0506(2) Uani 1 1 d . . . . .
N1 N 0.4762(3) 0.8648(2) 0.32275(17) 0.0403(5) Uani 1 1 d . . . . .
N2 N 0.4022(3) 0.6701(2) 0.37168(17) 0.0387(5) Uani 1 1 d . . . . .
N3 N 0.5162(3) 0.6500(2) 0.20309(17) 0.0414(6) Uani 1 1 d . . . . .
N4 N 0.3031(3) 0.7533(2) 0.13793(17) 0.0420(6) Uani 1 1 d . . . . .
O1 O 0.2393(2) 0.5505(2) 0.19618(14) 0.0437(5) Uani 1 1 d . . . . .
O2 O 0.1882(2) 0.7671(2) 0.29896(14) 0.0429(5) Uani 1 1 d . . . . .
C1 C 0.5526(3) 0.8595(3) 0.4077(2) 0.0408(6) Uani 1 1 d . . . . .
C2 C 0.4984(3) 0.9665(3) 0.2964(2) 0.0437(7) Uani 1 1 d . . . . .
H2 H 0.444660 0.970303 0.237866 0.052 Uiso 1 1 calc R U . . .
C3 C 0.5981(4) 1.0685(3) 0.3518(2) 0.0479(7) Uani 1 1 d . . . . .
H3 H 0.610517 1.140398 0.331198 0.057 Uiso 1 1 calc R U . . .
C4 C 0.6782(4) 1.0643(3) 0.4362(2) 0.0463(7) Uani 1 1 d . . . . .
H4 H 0.746647 1.132989 0.474040 0.056 Uiso 1 1 calc R U . . .
C5 C 0.6580(3) 0.9570(3) 0.4664(2) 0.0446(7) Uani 1 1 d . . . . .
C6 C 0.7354(4) 0.9410(3) 0.5514(2) 0.0468(7) Uani 1 1 d . . . . .
H6 H 0.807604 1.004859 0.592076 0.056 Uiso 1 1 calc R U . . .
C7 C 0.7061(4) 0.8334(3) 0.5749(2) 0.0486(7) Uani 1 1 d . . . . .
H7 H 0.759219 0.823699 0.631694 0.058 Uiso 1 1 calc R U . . .
C8 C 0.5990(4) 0.7370(3) 0.5164(2) 0.0457(7) Uani 1 1 d . . . . .
H8 H 0.581032 0.662747 0.533154 0.055 Uiso 1 1 calc R U . . .
C9 C 0.5211(3) 0.7518(3) 0.4352(2) 0.0420(6) Uani 1 1 d . . . . .
C10 C 0.3293(3) 0.5907(3) 0.4002(2) 0.0440(7) Uani 1 1 d . . . . .
H10 H 0.356887 0.589503 0.463674 0.053 Uiso 1 1 calc R U . . .
C11 C 0.2083(3) 0.5041(3) 0.3400(2) 0.0446(7) Uani 1 1 d . . . . .
C12 C 0.1333(4) 0.4296(3) 0.3825(2) 0.0501(7) Uani 1 1 d . . . . .
H12 H 0.157711 0.442524 0.448608 0.060 Uiso 1 1 calc R U . . .
C13 C 0.0245(4) 0.3378(3) 0.3281(3) 0.0518(8) Uani 1 1 d . . . . .
C14 C -0.0146(4) 0.3181(3) 0.2315(3) 0.0502(8) Uani 1 1 d . . . . .
H14 H -0.090991 0.255334 0.194562 0.060 Uiso 1 1 calc R U . . .
C15 C 0.0604(3) 0.3920(3) 0.1901(2) 0.0462(7) Uani 1 1 d . . . . .
C16 C 0.1745(3) 0.4874(3) 0.2422(2) 0.0414(6) Uani 1 1 d . . . . .
C17 C 0.5177(4) 0.6682(3) 0.1169(2) 0.0441(7) Uani 1 1 d . . . . .
C18 C 0.6225(4) 0.5964(3) 0.2418(2) 0.0453(7) Uani 1 1 d . . . . .
H18 H 0.621814 0.583033 0.301396 0.054 Uiso 1 1 calc R U . . .
C19 C 0.7343(4) 0.5597(3) 0.1961(2) 0.0489(7) Uani 1 1 d . . . . .
H19 H 0.809056 0.523085 0.225395 0.059 Uiso 1 1 calc R U . . .
C20 C 0.7366(4) 0.5760(3) 0.1107(2) 0.0504(8) Uani 1 1 d . . . . .
H20 H 0.812629 0.550794 0.080108 0.061 Uiso 1 1 calc R U . . .
C21 C 0.6251(4) 0.6311(3) 0.0664(2) 0.0489(7) Uani 1 1 d . . . . .
C22 C 0.6137(4) 0.6483(3) -0.0236(2) 0.0518(8) Uani 1 1 d . . . . .
H22 H 0.684353 0.622792 -0.059153 0.062 Uiso 1 1 calc R U . . .
C23 C 0.5028(4) 0.7009(3) -0.0598(2) 0.0528(8) Uani 1 1 d . . . . .
H23 H 0.496862 0.711814 -0.120731 0.063 Uiso 1 1 calc R U . . .
C24 C 0.3964(4) 0.7397(3) -0.0094(2) 0.0487(7) Uani 1 1 d . . . . .
H24 H 0.319785 0.776737 -0.036191 0.058 Uiso 1 1 calc R U . . .
C25 C 0.4028(4) 0.7242(3) 0.0791(2) 0.0455(7) Uani 1 1 d . . . . .
C26 C 0.1971(3) 0.8129(3) 0.1157(2) 0.0439(7) Uani 1 1 d . . . . .
H26 H 0.193990 0.841300 0.061481 0.053 Uiso 1 1 calc R U . . .
C27 C 0.0847(4) 0.8389(3) 0.1671(2) 0.0444(7) Uani 1 1 d . . . . .
C28 C -0.0283(4) 0.8964(3) 0.1272(2) 0.0480(7) Uani 1 1 d . . . . .
H28 H -0.024635 0.918636 0.070956 0.058 Uiso 1 1 calc R U . . .
C29 C -0.1414(4) 0.9194(3) 0.1699(2) 0.0488(7) Uani 1 1 d . . . . .
C30 C -0.1494(4) 0.8860(3) 0.2520(2) 0.0485(7) Uani 1 1 d . . . . .
H30 H -0.230531 0.900502 0.280099 0.058 Uiso 1 1 calc R U . . .
C31 C -0.0400(4) 0.8323(3) 0.2922(2) 0.0455(7) Uani 1 1 d . . . . .
C32 C 0.0845(3) 0.8099(3) 0.2522(2) 0.0429(7) Uani 1 1 d . . . . .
N5 N 0.5483(4) 0.3565(3) 0.3150(2) 0.0559(7) Uani 1 1 d . . . . .
O3 O 0.5753(3) 0.4428(2) 0.38903(17) 0.0642(7) Uani 1 1 d . . . . .
O4 O 0.6446(3) 0.3229(3) 0.27270(19) 0.0635(7) Uani 1 1 d . . . . .
O5 O 0.4191(3) 0.3022(3) 0.28251(18) 0.0627(7) Uani 1 1 d . . . . .
O6 O 0.3175(4) 0.0804(3) 0.1326(2) 0.0808(9) Uani 1 1 d D . . . .
H6A H 0.345(5) 0.145(4) 0.187(2) 0.121 Uiso 1 1 d D U . . .
H6B H 0.233(4) 0.090(5) 0.095(3) 0.121 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.874(2) . ?
Fe1 O2 1.881(2) . ?
Fe1 N2 1.919(3) . ?
Fe1 N4 1.939(3) . ?
Fe1 N3 1.976(3) . ?
Fe1 N1 1.994(3) . ?
Cl1 C13 1.742(4) . ?
Cl2 C15 1.734(3) . ?
Cl3 C29 1.747(4) . ?
Cl4 C31 1.731(3) . ?
N1 C2 1.325(4) . ?
N1 C1 1.372(4) . ?
N2 C10 1.293(4) . ?
N2 C9 1.420(4) . ?
N3 C18 1.343(4) . ?
N3 C17 1.369(4) . ?
N4 C26 1.301(4) . ?
N4 C25 1.412(4) . ?
O1 C16 1.305(4) . ?
O2 C32 1.309(4) . ?
C1 C5 1.409(4) . ?
C1 C9 1.413(4) . ?
C2 C3 1.398(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.414(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.420(5) . ?
C6 C7 1.375(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.411(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.369(4) . ?
C8 H8 0.9500 . ?
C10 C11 1.441(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.405(5) . ?
C11 C16 1.409(4) . ?
C12 C13 1.374(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(5) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.417(4) . ?
C17 C21 1.407(5) . ?
C17 C25 1.414(5) . ?
C18 C19 1.401(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.351(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.425(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.405(5) . ?
C22 C23 1.354(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.403(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(5) . ?
C24 H24 0.9500 . ?
C26 C27 1.433(5) . ?
C26 H26 0.9500 . ?
C27 C32 1.405(5) . ?
C27 C28 1.425(5) . ?
C28 C29 1.358(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(5) . ?
C30 C31 1.375(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.432(4) . ?
N5 O4 1.237(4) . ?
N5 O3 1.246(4) . ?
N5 O5 1.273(4) . ?
O6 H6A 0.926(10) . ?
O6 H6B 0.927(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O2 90.81(10) . . ?
O1 Fe1 N2 92.65(10) . . ?
O2 Fe1 N2 86.20(10) . . ?
O1 Fe1 N4 91.15(10) . . ?
O2 Fe1 N4 94.60(11) . . ?
N2 Fe1 N4 176.10(10) . . ?
O1 Fe1 N3 90.83(10) . . ?
O2 Fe1 N3 177.04(10) . . ?
N2 Fe1 N3 96.18(11) . . ?
N4 Fe1 N3 82.91(11) . . ?
O1 Fe1 N1 174.38(11) . . ?
O2 Fe1 N1 91.79(10) . . ?
N2 Fe1 N1 82.55(11) . . ?
N4 Fe1 N1 93.60(11) . . ?
N3 Fe1 N1 86.79(11) . . ?
C2 N1 C1 119.0(3) . . ?
C2 N1 Fe1 129.4(2) . . ?
C1 N1 Fe1 111.6(2) . . ?
C10 N2 C9 119.6(3) . . ?
C10 N2 Fe1 125.4(2) . . ?
C9 N2 Fe1 114.4(2) . . ?
C18 N3 C17 118.9(3) . . ?
C18 N3 Fe1 128.2(2) . . ?
C17 N3 Fe1 112.9(2) . . ?
C26 N4 C25 120.7(3) . . ?
C26 N4 Fe1 125.1(2) . . ?
C25 N4 Fe1 114.0(2) . . ?
C16 O1 Fe1 122.94(19) . . ?
C32 O2 Fe1 125.7(2) . . ?
N1 C1 C5 122.2(3) . . ?
N1 C1 C9 117.3(3) . . ?
C5 C1 C9 120.5(3) . . ?
N1 C2 C3 122.3(3) . . ?
N1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C1 C5 C4 117.1(3) . . ?
C1 C5 C6 118.1(3) . . ?
C4 C5 C6 124.8(3) . . ?
C7 C6 C5 120.2(3) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 121.4(3) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C1 120.4(3) . . ?
C8 C9 N2 127.4(3) . . ?
C1 C9 N2 112.1(3) . . ?
N2 C10 C11 123.0(3) . . ?
N2 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C12 C11 C16 121.5(3) . . ?
C12 C11 C10 116.5(3) . . ?
C16 C11 C10 121.8(3) . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 121.3(3) . . ?
C12 C13 Cl1 119.7(3) . . ?
C14 C13 Cl1 119.0(3) . . ?
C15 C14 C13 118.6(3) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 122.9(3) . . ?
C14 C15 Cl2 118.7(2) . . ?
C16 C15 Cl2 118.4(3) . . ?
O1 C16 C11 126.0(3) . . ?
O1 C16 C15 118.0(3) . . ?
C11 C16 C15 116.0(3) . . ?
N3 C17 C21 122.6(3) . . ?
N3 C17 C25 116.6(3) . . ?
C21 C17 C25 120.8(3) . . ?
N3 C18 C19 121.4(3) . . ?
N3 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 120.2(3) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C22 C21 C17 118.5(3) . . ?
C22 C21 C20 124.9(3) . . ?
C17 C21 C20 116.5(3) . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 121.4(3) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 N4 127.7(3) . . ?
C24 C25 C17 118.7(3) . . ?
N4 C25 C17 113.5(3) . . ?
N4 C26 C27 124.9(3) . . ?
N4 C26 H26 117.6 . . ?
C27 C26 H26 117.6 . . ?
C32 C27 C28 121.1(3) . . ?
C32 C27 C26 122.5(3) . . ?
C28 C27 C26 116.4(3) . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.9(3) . . ?
C28 C29 Cl3 120.5(3) . . ?
C30 C29 Cl3 118.6(3) . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 121.5(3) . . ?
C30 C31 Cl4 119.9(3) . . ?
C32 C31 Cl4 118.6(3) . . ?
O2 C32 C27 126.1(3) . . ?
O2 C32 C31 117.3(3) . . ?
C27 C32 C31 116.6(3) . . ?
O4 N5 O3 121.2(3) . . ?
O4 N5 O5 119.6(3) . . ?
O3 N5 O5 119.2(3) . . ?
H6A O6 H6B 112(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Fe1 O1 C16 -56.3(3) . . . . ?
N2 Fe1 O1 C16 30.0(3) . . . . ?
N4 Fe1 O1 C16 -150.9(3) . . . . ?
N3 Fe1 O1 C16 126.2(3) . . . . ?
O1 Fe1 O2 C32 -84.7(2) . . . . ?
N2 Fe1 O2 C32 -177.3(2) . . . . ?
N4 Fe1 O2 C32 6.5(2) . . . . ?
N1 Fe1 O2 C32 100.3(2) . . . . ?
C2 N1 C1 C5 -2.4(4) . . . . ?
Fe1 N1 C1 C5 175.5(2) . . . . ?
C2 N1 C1 C9 177.1(3) . . . . ?
Fe1 N1 C1 C9 -5.0(3) . . . . ?
C1 N1 C2 C3 0.6(5) . . . . ?
Fe1 N1 C2 C3 -176.8(2) . . . . ?
N1 C2 C3 C4 0.8(5) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
N1 C1 C5 C4 2.7(4) . . . . ?
C9 C1 C5 C4 -176.8(3) . . . . ?
N1 C1 C5 C6 -177.7(3) . . . . ?
C9 C1 C5 C6 2.8(5) . . . . ?
C3 C4 C5 C1 -1.2(5) . . . . ?
C3 C4 C5 C6 179.1(3) . . . . ?
C1 C5 C6 C7 -0.5(5) . . . . ?
C4 C5 C6 C7 179.1(3) . . . . ?
C5 C6 C7 C8 -0.5(5) . . . . ?
C6 C7 C8 C9 -1.0(5) . . . . ?
C7 C8 C9 C1 3.3(5) . . . . ?
C7 C8 C9 N2 -174.6(3) . . . . ?
N1 C1 C9 C8 176.2(3) . . . . ?
C5 C1 C9 C8 -4.3(5) . . . . ?
N1 C1 C9 N2 -5.6(4) . . . . ?
C5 C1 C9 N2 173.9(3) . . . . ?
C10 N2 C9 C8 21.0(5) . . . . ?
Fe1 N2 C9 C8 -167.8(3) . . . . ?
C10 N2 C9 C1 -157.1(3) . . . . ?
Fe1 N2 C9 C1 14.1(3) . . . . ?
C9 N2 C10 C11 -179.4(3) . . . . ?
Fe1 N2 C10 C11 10.4(4) . . . . ?
N2 C10 C11 C12 -175.6(3) . . . . ?
N2 C10 C11 C16 9.7(5) . . . . ?
C16 C11 C12 C13 0.2(5) . . . . ?
C10 C11 C12 C13 -174.6(3) . . . . ?
C11 C12 C13 C14 -0.9(6) . . . . ?
C11 C12 C13 Cl1 177.7(3) . . . . ?
C12 C13 C14 C15 1.0(6) . . . . ?
Cl1 C13 C14 C15 -177.6(3) . . . . ?
C13 C14 C15 C16 -0.5(5) . . . . ?
C13 C14 C15 Cl2 -179.6(3) . . . . ?
Fe1 O1 C16 C11 -20.6(5) . . . . ?
Fe1 O1 C16 C15 160.2(2) . . . . ?
C12 C11 C16 O1 -178.8(3) . . . . ?
C10 C11 C16 O1 -4.4(5) . . . . ?
C12 C11 C16 C15 0.4(5) . . . . ?
C10 C11 C16 C15 174.8(3) . . . . ?
C14 C15 C16 O1 179.1(3) . . . . ?
Cl2 C15 C16 O1 -1.8(4) . . . . ?
C14 C15 C16 C11 -0.2(5) . . . . ?
Cl2 C15 C16 C11 179.0(2) . . . . ?
C18 N3 C17 C21 1.1(4) . . . . ?
Fe1 N3 C17 C21 -177.9(2) . . . . ?
C18 N3 C17 C25 179.6(3) . . . . ?
Fe1 N3 C17 C25 0.6(3) . . . . ?
C17 N3 C18 C19 0.3(4) . . . . ?
Fe1 N3 C18 C19 179.1(2) . . . . ?
N3 C18 C19 C20 -0.9(5) . . . . ?
C18 C19 C20 C21 0.1(5) . . . . ?
N3 C17 C21 C22 177.0(3) . . . . ?
C25 C17 C21 C22 -1.5(4) . . . . ?
N3 C17 C21 C20 -1.8(4) . . . . ?
C25 C17 C21 C20 179.7(3) . . . . ?
C19 C20 C21 C22 -177.5(3) . . . . ?
C19 C20 C21 C17 1.2(5) . . . . ?
C17 C21 C22 C23 0.9(5) . . . . ?
C20 C21 C22 C23 179.5(3) . . . . ?
C21 C22 C23 C24 0.0(5) . . . . ?
C22 C23 C24 C25 -0.3(5) . . . . ?
C23 C24 C25 N4 -177.5(3) . . . . ?
C23 C24 C25 C17 -0.3(5) . . . . ?
C26 N4 C25 C24 -7.5(5) . . . . ?
Fe1 N4 C25 C24 176.3(3) . . . . ?
C26 N4 C25 C17 175.2(3) . . . . ?
Fe1 N4 C25 C17 -1.0(3) . . . . ?
N3 C17 C25 C24 -177.3(3) . . . . ?
C21 C17 C25 C24 1.2(5) . . . . ?
N3 C17 C25 N4 0.2(4) . . . . ?
C21 C17 C25 N4 178.8(3) . . . . ?
C25 N4 C26 C27 175.3(3) . . . . ?
Fe1 N4 C26 C27 -9.0(4) . . . . ?
N4 C26 C27 C32 5.0(5) . . . . ?
N4 C26 C27 C28 -175.0(3) . . . . ?
C32 C27 C28 C29 -2.6(5) . . . . ?
C26 C27 C28 C29 177.4(3) . . . . ?
C27 C28 C29 C30 -0.8(5) . . . . ?
C27 C28 C29 Cl3 -179.9(2) . . . . ?
C28 C29 C30 C31 1.8(5) . . . . ?
Cl3 C29 C30 C31 -179.0(2) . . . . ?
C29 C30 C31 C32 0.5(5) . . . . ?
C29 C30 C31 Cl4 179.8(2) . . . . ?
Fe1 O2 C32 C27 -11.8(4) . . . . ?
Fe1 O2 C32 C31 169.7(2) . . . . ?
C28 C27 C32 O2 -173.8(3) . . . . ?
C26 C27 C32 O2 6.2(5) . . . . ?
C28 C27 C32 C31 4.7(4) . . . . ?
C26 C27 C32 C31 -175.3(3) . . . . ?
C30 C31 C32 O2 175.0(3) . . . . ?
Cl4 C31 C32 O2 -4.4(4) . . . . ?
C30 C31 C32 C27 -3.6(4) . . . . ?
Cl4 C31 C32 C27 177.0(2) . . . . ?

_refine_diff_density_max         1.614
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.127

# start Validation Reply Form
_vrf_PLAT029_1a100K              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.932 Why?  
RESPONSE: Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.932, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;
_vrf_PLAT420_1a100K              
;
PROBLEM: D-H Bond Without Acceptor  O6       --H6B      .     Please Check 
RESPONSE:  This alert is related to the hydrogen atoms of
lattice solvent molecules.It is very difficult to locate hydrogen atoms
accurately using X-ray data because these atoms have low scattering 
power.
;
# 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_1b(298K)
_database_code_depnum_ccdc_archive 'CCDC 2002657'
loop_
_audit_author_name
_audit_author_address
'Kil Sik Min'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Cl4 Fe N4 O2, N O3, H2 O'
_chemical_formula_sum            'C32 H20 Cl4 Fe N5 O6'
_chemical_formula_weight         768.18

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'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1453 0.1556 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3456 0.8258 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.5590(19)
_cell_length_b                   11.905(2)
_cell_length_c                   15.101(3)
_cell_angle_alpha                108.20(3)
_cell_angle_beta                 98.16(3)
_cell_angle_gamma                96.48(3)
_cell_volume                     1593.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    22291
_cell_measurement_theta_min      0.40
_cell_measurement_theta_max      29.54

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_F_000             778
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.831
_shelx_estimated_absorpt_T_min   0.922
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12123
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.799
_diffrn_reflns_theta_max         29.471
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.676
_diffrn_measured_fraction_theta_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.676
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.676
_diffrn_reflns_point_group_measured_fraction_full 0.927
_reflns_number_total             6283
_reflns_number_gt                4194
_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       'PAL ADSC Quatnrum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXs-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_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)+(0.1253P)²] 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     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.085(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6283
_refine_ls_number_parameters     440
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1770
_refine_ls_wR_factor_gt          0.1566
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.001
_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 0.34008(5) 0.68328(4) 0.25982(3) 0.0482(2) Uani 1 1 d . . . . .
Cl1 Cl -0.05895(13) 0.26866(12) 0.43443(10) 0.0906(4) Uani 1 1 d . . . . .
Cl2 Cl 0.00033(12) 0.33276(10) 0.10350(7) 0.0799(4) Uani 1 1 d . . . . .
Cl3 Cl -0.20072(16) 0.99824(13) 0.08931(11) 0.1063(5) Uani 1 1 d . . . . .
Cl4 Cl -0.07389(12) 0.81215(12) 0.36724(8) 0.0836(4) Uani 1 1 d . . . . .
N1 N 0.4852(3) 0.8515(2) 0.34278(18) 0.0488(6) Uani 1 1 d . . . . .
N2 N 0.4028(3) 0.6635(2) 0.39195(18) 0.0482(6) Uani 1 1 d . . . . .
N3 N 0.5215(3) 0.6237(2) 0.20516(18) 0.0525(7) Uani 1 1 d . . . . .
N4 N 0.3297(3) 0.7328(2) 0.13486(18) 0.0522(7) Uani 1 1 d . . . . .
O1 O 0.2354(3) 0.5227(2) 0.21973(15) 0.0579(6) Uani 1 1 d . . . . .
O2 O 0.1729(3) 0.7539(2) 0.28142(17) 0.0607(6) Uani 1 1 d . . . . .
C1 C 0.5591(4) 0.8480(3) 0.4263(2) 0.0476(7) Uani 1 1 d . . . . .
C2 C 0.5159(4) 0.9469(3) 0.3175(2) 0.0538(8) Uani 1 1 d . . . . .
H2 H 0.466296 0.949093 0.260566 0.065 Uiso 1 1 calc R U . . .
C3 C 0.6213(4) 1.0454(3) 0.3742(3) 0.0622(9) Uani 1 1 d . . . . .
H3 H 0.638920 1.111928 0.355104 0.075 Uiso 1 1 calc R U . . .
C4 C 0.6965(4) 1.0433(3) 0.4557(3) 0.0592(9) Uani 1 1 d . . . . .
H4 H 0.766820 1.107970 0.492855 0.071 Uiso 1 1 calc R U . . .
C5 C 0.6681(4) 0.9418(3) 0.4851(2) 0.0530(8) Uani 1 1 d . . . . .
C6 C 0.7421(4) 0.9288(3) 0.5682(3) 0.0604(9) Uani 1 1 d . . . . .
H6 H 0.814700 0.989855 0.607797 0.073 Uiso 1 1 calc R U . . .
C7 C 0.7095(4) 0.8296(3) 0.5911(3) 0.0639(10) Uani 1 1 d . . . . .
H7 H 0.761627 0.821984 0.645185 0.077 Uiso 1 1 calc R U . . .
C8 C 0.5964(4) 0.7369(3) 0.5336(2) 0.0589(9) Uani 1 1 d . . . . .
H8 H 0.573572 0.669066 0.550226 0.071 Uiso 1 1 calc R U . . .
C9 C 0.5213(4) 0.7475(3) 0.4537(2) 0.0488(8) Uani 1 1 d . . . . .
C10 C 0.3269(4) 0.5925(3) 0.4243(2) 0.0532(8) Uani 1 1 d . . . . .
H10 H 0.351079 0.602331 0.488399 0.064 Uiso 1 1 calc R U . . .
C11 C 0.2099(4) 0.5012(3) 0.3690(2) 0.0538(8) Uani 1 1 d . . . . .
C12 C 0.1366(4) 0.4388(3) 0.4199(3) 0.0621(9) Uani 1 1 d . . . . .
H12 H 0.164648 0.459948 0.485327 0.075 Uiso 1 1 calc R U . . .
C13 C 0.0253(4) 0.3481(3) 0.3725(3) 0.0655(10) Uani 1 1 d . . . . .
C14 C -0.0175(4) 0.3151(3) 0.2750(3) 0.0663(10) Uani 1 1 d . . . . .
H14 H -0.094104 0.253395 0.243202 0.080 Uiso 1 1 calc R U . . .
C15 C 0.0544(4) 0.3746(3) 0.2259(3) 0.0583(9) Uani 1 1 d . . . . .
C16 C 0.1700(4) 0.4692(3) 0.2697(2) 0.0523(8) Uani 1 1 d . . . . .
C17 C 0.5426(4) 0.6456(3) 0.1237(2) 0.0532(8) Uani 1 1 d . . . . .
C18 C 0.6123(4) 0.5685(3) 0.2441(3) 0.0624(9) Uani 1 1 d . . . . .
H18 H 0.596920 0.553257 0.298978 0.075 Uiso 1 1 calc R U . . .
C19 C 0.7318(5) 0.5321(4) 0.2044(3) 0.0755(11) Uani 1 1 d . . . . .
H19 H 0.793949 0.493120 0.232778 0.091 Uiso 1 1 calc R U . . .
C20 C 0.7547(5) 0.5544(4) 0.1250(3) 0.0718(11) Uani 1 1 d . . . . .
H20 H 0.834891 0.532889 0.099732 0.086 Uiso 1 1 calc R U . . .
C21 C 0.6581(4) 0.6103(3) 0.0797(3) 0.0627(10) Uani 1 1 d . . . . .
C22 C 0.6720(5) 0.6326(4) -0.0050(3) 0.0728(12) Uani 1 1 d . . . . .
H22 H 0.747561 0.609585 -0.035242 0.087 Uiso 1 1 calc R U . . .
C23 C 0.5759(5) 0.6871(4) -0.0417(3) 0.0766(12) Uani 1 1 d . . . . .
H23 H 0.586575 0.701658 -0.097609 0.092 Uiso 1 1 calc R U . . .
C24 C 0.4599(5) 0.7232(4) 0.0005(3) 0.0667(10) Uani 1 1 d . . . . .
H24 H 0.395003 0.760614 -0.027286 0.080 Uiso 1 1 calc R U . . .
C25 C 0.4422(4) 0.7026(3) 0.0842(2) 0.0544(8) Uani 1 1 d . . . . .
C26 C 0.2375(4) 0.7938(3) 0.1093(2) 0.0564(9) Uani 1 1 d . . . . .
H26 H 0.249232 0.816990 0.057055 0.068 Uiso 1 1 calc R U . . .
C27 C 0.1193(4) 0.8289(3) 0.1537(2) 0.0570(9) Uani 1 1 d . . . . .
C28 C 0.0302(4) 0.8915(4) 0.1093(3) 0.0675(10) Uani 1 1 d . . . . .
H28 H 0.052111 0.909304 0.056608 0.081 Uiso 1 1 calc R U . . .
C29 C -0.0888(5) 0.9253(4) 0.1454(3) 0.0767(12) Uani 1 1 d . . . . .
C30 C -0.1218(5) 0.9005(4) 0.2236(3) 0.0762(12) Uani 1 1 d . . . . .
H30 H -0.203061 0.923207 0.246783 0.091 Uiso 1 1 calc R U . . .
C31 C -0.0343(4) 0.8419(4) 0.2673(3) 0.0660(10) Uani 1 1 d . . . . .
C32 C 0.0897(4) 0.8048(3) 0.2345(2) 0.0563(9) Uani 1 1 d . . . . .
N5 N 0.5659(6) 0.3089(4) 0.2849(3) 0.0905(12) Uani 1 1 d . . . . .
O3 O 0.6354(6) 0.3865(4) 0.3537(3) 0.1427(19) Uani 1 1 d . . . . .
O4 O 0.6239(5) 0.2391(5) 0.2282(4) 0.1342(16) Uani 1 1 d . . . . .
O5 O 0.4352(5) 0.2990(6) 0.2671(3) 0.157(2) Uani 1 1 d . . . . .
O6 O 0.4266(7) 0.0203(4) 0.1111(5) 0.167(2) Uani 1 1 d D . . . .
H6A H 0.358(8) 0.062(8) 0.138(8) 0.250 Uiso 1 1 d D U . . .
H6B H 0.494(8) 0.066(7) 0.093(7) 0.250 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.910(3) . ?
Fe1 O1 1.923(2) . ?
Fe1 N2 2.093(3) . ?
Fe1 N3 2.124(3) . ?
Fe1 N4 2.138(3) . ?
Fe1 N1 2.194(3) . ?
Cl1 C13 1.735(4) . ?
Cl2 C15 1.740(4) . ?
Cl3 C29 1.740(5) . ?
Cl4 C31 1.735(5) . ?
N1 C2 1.324(4) . ?
N1 C1 1.371(4) . ?
N2 C10 1.303(4) . ?
N2 C9 1.420(4) . ?
N3 C18 1.325(5) . ?
N3 C17 1.372(4) . ?
N4 C26 1.295(5) . ?
N4 C25 1.421(4) . ?
O1 C16 1.308(4) . ?
O2 C32 1.311(5) . ?
C1 C5 1.405(4) . ?
C1 C9 1.411(5) . ?
C2 C3 1.408(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.344(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.423(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(5) . ?
C6 C7 1.347(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.417(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.361(5) . ?
C8 H8 0.9300 . ?
C10 C11 1.423(5) . ?
C10 H10 0.9300 . ?
C11 C16 1.409(5) . ?
C11 C12 1.423(5) . ?
C12 C13 1.361(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(6) . ?
C14 C15 1.373(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.405(5) . ?
C17 C25 1.405(5) . ?
C17 C21 1.405(5) . ?
C18 C19 1.412(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.348(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.418(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.405(6) . ?
C22 C23 1.337(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.390(5) . ?
C24 H24 0.9300 . ?
C26 C27 1.431(5) . ?
C26 H26 0.9300 . ?
C27 C32 1.395(5) . ?
C27 C28 1.422(6) . ?
C28 C29 1.377(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.373(7) . ?
C30 C31 1.373(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.412(5) . ?
N5 O3 1.200(5) . ?
N5 O5 1.224(6) . ?
N5 O4 1.235(6) . ?
O6 H6A 0.926(10) . ?
O6 H6B 0.923(10) . ?

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
O2 Fe1 O1 93.03(11) . . ?
O2 Fe1 N2 99.79(11) . . ?
O1 Fe1 N2 86.75(10) . . ?
O2 Fe1 N3 164.47(11) . . ?
O1 Fe1 N3 92.54(11) . . ?
N2 Fe1 N3 94.99(11) . . ?
O2 Fe1 N4 87.65(11) . . ?
O1 Fe1 N4 105.99(10) . . ?
N2 Fe1 N4 164.99(11) . . ?
N3 Fe1 N4 76.88(11) . . ?
O2 Fe1 N1 92.83(11) . . ?
O1 Fe1 N1 162.56(11) . . ?
N2 Fe1 N1 76.08(10) . . ?
N3 Fe1 N1 86.08(11) . . ?
N4 Fe1 N1 90.65(11) . . ?
C2 N1 C1 118.9(3) . . ?
C2 N1 Fe1 127.7(2) . . ?
C1 N1 Fe1 113.1(2) . . ?
C10 N2 C9 119.5(3) . . ?
C10 N2 Fe1 123.4(2) . . ?
C9 N2 Fe1 116.2(2) . . ?
C18 N3 C17 119.5(3) . . ?
C18 N3 Fe1 124.7(2) . . ?
C17 N3 Fe1 115.8(2) . . ?
C26 N4 C25 120.8(3) . . ?
C26 N4 Fe1 124.5(2) . . ?
C25 N4 Fe1 114.4(2) . . ?
C16 O1 Fe1 128.4(2) . . ?
C32 O2 Fe1 133.8(2) . . ?
N1 C1 C5 122.0(3) . . ?
N1 C1 C9 118.1(3) . . ?
C5 C1 C9 119.9(3) . . ?
N1 C2 C3 122.0(3) . . ?
N1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C1 C5 C6 118.2(3) . . ?
C1 C5 C4 117.2(3) . . ?
C6 C5 C4 124.6(3) . . ?
C7 C6 C5 121.2(3) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.6(4) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 119.7(4) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C1 120.3(3) . . ?
C8 C9 N2 125.4(3) . . ?
C1 C9 N2 114.3(3) . . ?
N2 C10 C11 125.0(3) . . ?
N2 C10 H10 117.5 . . ?
C11 C10 H10 117.5 . . ?
C16 C11 C10 123.4(3) . . ?
C16 C11 C12 120.9(3) . . ?
C10 C11 C12 115.6(3) . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 120.9(3) . . ?
C12 C13 Cl1 119.4(3) . . ?
C14 C13 Cl1 119.6(3) . . ?
C15 C14 C13 119.3(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 123.2(3) . . ?
C14 C15 Cl2 119.1(3) . . ?
C16 C15 Cl2 117.7(3) . . ?
O1 C16 C15 120.9(3) . . ?
O1 C16 C11 123.1(3) . . ?
C15 C16 C11 116.0(3) . . ?
N3 C17 C25 117.4(3) . . ?
N3 C17 C21 121.7(4) . . ?
C25 C17 C21 120.9(3) . . ?
N3 C18 C19 121.8(4) . . ?
N3 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C20 C19 C18 119.2(4) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 120.8(4) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C22 C21 C17 119.0(4) . . ?
C22 C21 C20 124.0(4) . . ?
C17 C21 C20 116.9(4) . . ?
C23 C22 C21 119.5(4) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 122.7(4) . . ?
C22 C23 H23 118.6 . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 119.6(4) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C17 118.3(3) . . ?
C24 C25 N4 126.2(4) . . ?
C17 C25 N4 115.5(3) . . ?
N4 C26 C27 126.2(3) . . ?
N4 C26 H26 116.9 . . ?
C27 C26 H26 116.9 . . ?
C32 C27 C28 120.9(4) . . ?
C32 C27 C26 124.0(4) . . ?
C28 C27 C26 115.1(4) . . ?
C29 C28 C27 119.1(4) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C30 C29 C28 121.1(4) . . ?
C30 C29 Cl3 119.6(4) . . ?
C28 C29 Cl3 119.3(4) . . ?
C29 C30 C31 119.7(4) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 122.3(4) . . ?
C30 C31 Cl4 119.9(3) . . ?
C32 C31 Cl4 117.7(3) . . ?
O2 C32 C27 123.3(3) . . ?
O2 C32 C31 119.8(4) . . ?
C27 C32 C31 116.9(4) . . ?
O3 N5 O5 120.8(7) . . ?
O3 N5 O4 121.3(6) . . ?
O5 N5 O4 117.9(5) . . ?
H6A O6 H6B 114(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
C2 N1 C1 C5 -1.1(5) . . . . ?
Fe1 N1 C1 C5 173.3(2) . . . . ?
C2 N1 C1 C9 177.7(3) . . . . ?
Fe1 N1 C1 C9 -7.9(4) . . . . ?
C1 N1 C2 C3 -0.5(5) . . . . ?
Fe1 N1 C2 C3 -174.0(3) . . . . ?
N1 C2 C3 C4 1.4(6) . . . . ?
C2 C3 C4 C5 -0.7(6) . . . . ?
N1 C1 C5 C6 -177.8(3) . . . . ?
C9 C1 C5 C6 3.4(5) . . . . ?
N1 C1 C5 C4 1.7(5) . . . . ?
C9 C1 C5 C4 -177.0(3) . . . . ?
C3 C4 C5 C1 -0.8(5) . . . . ?
C3 C4 C5 C6 178.7(4) . . . . ?
C1 C5 C6 C7 -0.2(5) . . . . ?
C4 C5 C6 C7 -179.7(4) . . . . ?
C5 C6 C7 C8 -1.9(6) . . . . ?
C6 C7 C8 C9 0.8(6) . . . . ?
C7 C8 C9 C1 2.4(5) . . . . ?
C7 C8 C9 N2 -177.6(3) . . . . ?
N1 C1 C9 C8 176.6(3) . . . . ?
C5 C1 C9 C8 -4.6(5) . . . . ?
N1 C1 C9 N2 -3.3(4) . . . . ?
C5 C1 C9 N2 175.5(3) . . . . ?
C10 N2 C9 C8 24.2(5) . . . . ?
Fe1 N2 C9 C8 -166.2(3) . . . . ?
C10 N2 C9 C1 -155.8(3) . . . . ?
Fe1 N2 C9 C1 13.7(4) . . . . ?
C9 N2 C10 C11 -177.1(3) . . . . ?
Fe1 N2 C10 C11 14.2(5) . . . . ?
N2 C10 C11 C16 6.0(6) . . . . ?
N2 C10 C11 C12 -176.4(4) . . . . ?
C16 C11 C12 C13 -0.9(6) . . . . ?
C10 C11 C12 C13 -178.5(4) . . . . ?
C11 C12 C13 C14 0.3(6) . . . . ?
C11 C12 C13 Cl1 177.5(3) . . . . ?
C12 C13 C14 C15 0.4(6) . . . . ?
Cl1 C13 C14 C15 -176.8(3) . . . . ?
C13 C14 C15 C16 -0.6(6) . . . . ?
C13 C14 C15 Cl2 179.9(3) . . . . ?
Fe1 O1 C16 C15 154.2(3) . . . . ?
Fe1 O1 C16 C11 -26.1(5) . . . . ?
C14 C15 C16 O1 179.7(4) . . . . ?
Cl2 C15 C16 O1 -0.8(5) . . . . ?
C14 C15 C16 C11 0.0(5) . . . . ?
Cl2 C15 C16 C11 179.5(3) . . . . ?
C10 C11 C16 O1 -1.5(6) . . . . ?
C12 C11 C16 O1 -179.0(3) . . . . ?
C10 C11 C16 C15 178.2(3) . . . . ?
C12 C11 C16 C15 0.7(5) . . . . ?
C18 N3 C17 C25 179.0(3) . . . . ?
Fe1 N3 C17 C25 -1.0(4) . . . . ?
C18 N3 C17 C21 0.4(5) . . . . ?
Fe1 N3 C17 C21 -179.6(2) . . . . ?
C17 N3 C18 C19 0.6(6) . . . . ?
Fe1 N3 C18 C19 -179.4(3) . . . . ?
N3 C18 C19 C20 0.3(7) . . . . ?
C18 C19 C20 C21 -2.0(7) . . . . ?
N3 C17 C21 C22 178.4(3) . . . . ?
C25 C17 C21 C22 -0.1(5) . . . . ?
N3 C17 C21 C20 -2.0(5) . . . . ?
C25 C17 C21 C20 179.4(3) . . . . ?
C19 C20 C21 C22 -177.7(4) . . . . ?
C19 C20 C21 C17 2.8(6) . . . . ?
C17 C21 C22 C23 0.2(6) . . . . ?
C20 C21 C22 C23 -179.3(4) . . . . ?
C21 C22 C23 C24 -0.3(7) . . . . ?
C22 C23 C24 C25 0.2(7) . . . . ?
C23 C24 C25 C17 -0.1(5) . . . . ?
C23 C24 C25 N4 -179.3(3) . . . . ?
N3 C17 C25 C24 -178.6(3) . . . . ?
C21 C17 C25 C24 0.0(5) . . . . ?
N3 C17 C25 N4 0.8(4) . . . . ?
C21 C17 C25 N4 179.4(3) . . . . ?
C26 N4 C25 C24 -6.1(5) . . . . ?
Fe1 N4 C25 C24 179.1(3) . . . . ?
C26 N4 C25 C17 174.6(3) . . . . ?
Fe1 N4 C25 C17 -0.2(4) . . . . ?
C25 N4 C26 C27 179.5(3) . . . . ?
Fe1 N4 C26 C27 -6.3(5) . . . . ?
N4 C26 C27 C32 2.2(6) . . . . ?
N4 C26 C27 C28 -177.5(3) . . . . ?
C32 C27 C28 C29 -1.9(5) . . . . ?
C26 C27 C28 C29 177.9(3) . . . . ?
C27 C28 C29 C30 0.5(6) . . . . ?
C27 C28 C29 Cl3 -178.3(3) . . . . ?
C28 C29 C30 C31 0.6(7) . . . . ?
Cl3 C29 C30 C31 179.4(3) . . . . ?
C29 C30 C31 C32 -0.4(6) . . . . ?
C29 C30 C31 Cl4 179.0(3) . . . . ?
Fe1 O2 C32 C27 -6.6(5) . . . . ?
Fe1 O2 C32 C31 175.7(2) . . . . ?
C28 C27 C32 O2 -175.8(3) . . . . ?
C26 C27 C32 O2 4.5(6) . . . . ?
C28 C27 C32 C31 2.0(5) . . . . ?
C26 C27 C32 C31 -177.7(3) . . . . ?
C30 C31 C32 O2 177.0(3) . . . . ?
Cl4 C31 C32 O2 -2.5(5) . . . . ?
C30 C31 C32 C27 -0.9(5) . . . . ?
Cl4 C31 C32 C27 179.6(3) . . . . ?

_refine_diff_density_max         0.575
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.098

# start Validation Reply Form
_vrf_PLAT029_1b298K              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.927 Why?  
RESPONSE: Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.927, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;
_vrf_PLAT420_1b298K              
;
PROBLEM: D-H Bond Without Acceptor  O6       --H6A      .     Please Check 
RESPONSE: This alert is related to the hydrogen atoms of
lattice solvent molecules.It is very difficult to locate hydrogen atoms
accurately using X-ray data because these atoms have low scattering 
power.
;
# 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_2a(100K)
_database_code_depnum_ccdc_archive 'CCDC 2002658'
loop_
_audit_author_name
_audit_author_address
'Kil Sik Min'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Cl4 Fe N4 O2, B F4, 2(C3 H6 O)'
_chemical_formula_sum            'C38 H30 B Cl4 F4 Fe N4 O4'
_chemical_formula_weight         891.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0050 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0140 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1230 0.1260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3241 0.6814 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.4580(19)
_cell_length_b                   12.391(3)
_cell_length_c                   16.320(3)
_cell_angle_alpha                95.32(3)
_cell_angle_beta                 103.38(3)
_cell_angle_gamma                97.00(3)
_cell_volume                     1832.3(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    51933
_cell_measurement_theta_min      0.36
_cell_measurement_theta_max      33.55

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_F_000             906
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.552
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.630
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28979
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.984
_diffrn_reflns_theta_max         33.320
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.732
_diffrn_measured_fraction_theta_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.732
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.732
_diffrn_reflns_point_group_measured_fraction_full 0.941
_reflns_number_total             14908
_reflns_number_gt                8986
_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       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_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)+(0.1575P)²] 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         14908
_refine_ls_number_parameters     509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.2541
_refine_ls_wR_factor_gt          0.2274
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_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 0.65447(4) 0.56247(4) 0.76665(2) 0.02070(11) Uani 1 1 d . . . . .
Cl1 Cl 1.22879(8) 0.24517(7) 0.72201(5) 0.03033(17) Uani 1 1 d . . . . .
Cl2 Cl 1.06142(8) 0.63116(7) 0.64730(4) 0.02885(16) Uani 1 1 d . . . . .
Cl3 Cl 1.14516(11) 1.06625(8) 0.90835(6) 0.0422(2) Uani 1 1 d . . . . .
Cl4 Cl 1.02466(7) 0.67241(7) 1.01303(4) 0.02876(17) Uani 1 1 d . . . . .
N1 N 0.4870(3) 0.5568(2) 0.82044(13) 0.0248(5) Uani 1 1 d . . . . .
N2 N 0.6778(2) 0.4257(2) 0.81275(13) 0.0220(5) Uani 1 1 d . . . . .
N3 N 0.5140(2) 0.4920(2) 0.65965(13) 0.0252(5) Uani 1 1 d . . . . .
N4 N 0.6222(3) 0.6958(2) 0.71616(13) 0.0250(5) Uani 1 1 d . . . . .
O1 O 0.8127(2) 0.56139(18) 0.71510(11) 0.0227(4) Uani 1 1 d . . . . .
O2 O 0.7784(2) 0.63734(18) 0.86715(11) 0.0237(4) Uani 1 1 d . . . . .
C1 C 0.4722(3) 0.4674(3) 0.86257(15) 0.0253(6) Uani 1 1 d . . . . .
C2 C 0.3940(3) 0.6283(3) 0.82236(17) 0.0295(6) Uani 1 1 d . . . . .
H2 H 0.403646 0.690896 0.793471 0.035 Uiso 1 1 calc R U . . .
C3 C 0.2812(3) 0.6150(3) 0.86572(18) 0.0337(7) Uani 1 1 d . . . . .
H3 H 0.216088 0.667717 0.865080 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2658(3) 0.5270(3) 0.90831(17) 0.0335(7) Uani 1 1 d . . . . .
H4 H 0.190247 0.517876 0.937727 0.040 Uiso 1 1 calc R U . . .
C5 C 0.3631(3) 0.4490(3) 0.90846(16) 0.0290(6) Uani 1 1 d . . . . .
C6 C 0.3583(3) 0.3553(3) 0.95130(18) 0.0343(7) Uani 1 1 d . . . . .
H6 H 0.285869 0.341268 0.982265 0.041 Uiso 1 1 calc R U . . .
C7 C 0.4571(3) 0.2851(3) 0.94835(18) 0.0335(7) Uani 1 1 d . . . . .
H7 H 0.452819 0.222536 0.977747 0.040 Uiso 1 1 calc R U . . .
C8 C 0.5671(3) 0.3027(3) 0.90234(18) 0.0303(7) Uani 1 1 d . . . . .
H8 H 0.634730 0.252266 0.900866 0.036 Uiso 1 1 calc R U . . .
C9 C 0.5743(3) 0.3938(3) 0.85992(15) 0.0243(6) Uani 1 1 d . . . . .
C10 C 0.7761(3) 0.3646(3) 0.80313(15) 0.0217(5) Uani 1 1 d . . . . .
H10 H 0.771804 0.296408 0.825389 0.026 Uiso 1 1 calc R U . . .
C11 C 0.8914(3) 0.3924(3) 0.76121(15) 0.0231(5) Uani 1 1 d . . . . .
C12 C 0.9909(3) 0.3173(3) 0.75999(16) 0.0242(5) Uani 1 1 d . . . . .
H12 H 0.978701 0.251914 0.785325 0.029 Uiso 1 1 calc R U . . .
C13 C 1.1056(3) 0.3376(3) 0.72255(16) 0.0237(5) Uani 1 1 d . . . . .
C14 C 1.1268(3) 0.4352(3) 0.68746(16) 0.0247(5) Uani 1 1 d . . . . .
H14 H 1.207873 0.450141 0.662945 0.030 Uiso 1 1 calc R U . . .
C15 C 1.0306(3) 0.5095(3) 0.68842(15) 0.0226(5) Uani 1 1 d . . . . .
C16 C 0.9054(3) 0.4908(3) 0.72296(14) 0.0215(5) Uani 1 1 d . . . . .
C17 C 0.4535(3) 0.5675(3) 0.61103(15) 0.0247(6) Uani 1 1 d . . . . .
C18 C 0.4750(3) 0.3867(3) 0.63147(16) 0.0264(6) Uani 1 1 d . . . . .
H18 H 0.519071 0.334487 0.664135 0.032 Uiso 1 1 calc R U . . .
C19 C 0.3691(3) 0.3491(3) 0.55378(17) 0.0328(7) Uani 1 1 d . . . . .
H19 H 0.343064 0.272749 0.535370 0.039 Uiso 1 1 calc R U . . .
C20 C 0.3053(3) 0.4218(3) 0.50586(17) 0.0339(7) Uani 1 1 d . . . . .
H20 H 0.235145 0.396862 0.453580 0.041 Uiso 1 1 calc R U . . .
C21 C 0.3439(3) 0.5357(3) 0.53441(16) 0.0307(7) Uani 1 1 d . . . . .
C22 C 0.2840(3) 0.6195(4) 0.49049(17) 0.0359(8) Uani 1 1 d . . . . .
H22 H 0.209412 0.600850 0.439216 0.043 Uiso 1 1 calc R U . . .
C23 C 0.3323(4) 0.7255(4) 0.52115(18) 0.0377(8) Uani 1 1 d . . . . .
H23 H 0.290075 0.780286 0.490814 0.045 Uiso 1 1 calc R U . . .
C24 C 0.4435(3) 0.7584(3) 0.59683(17) 0.0315(7) Uani 1 1 d . . . . .
H24 H 0.476040 0.833839 0.616966 0.038 Uiso 1 1 calc R U . . .
C25 C 0.5037(3) 0.6781(3) 0.64077(15) 0.0271(6) Uani 1 1 d . . . . .
C26 C 0.7065(3) 0.7881(3) 0.73923(17) 0.0275(6) Uani 1 1 d . . . . .
H26 H 0.687125 0.845974 0.705911 0.033 Uiso 1 1 calc R U . . .
C27 C 0.8285(3) 0.8089(3) 0.81252(17) 0.0262(6) Uani 1 1 d . . . . .
C28 C 0.9178(4) 0.9137(3) 0.8261(2) 0.0316(6) Uani 1 1 d . . . . .
H28 H 0.894871 0.965686 0.787636 0.038 Uiso 1 1 calc R U . . .
C29 C 1.0358(4) 0.9391(3) 0.8943(2) 0.0309(6) Uani 1 1 d . . . . .
C30 C 1.0711(3) 0.8657(3) 0.95242(18) 0.0309(6) Uani 1 1 d . . . . .
H30 H 1.153953 0.884050 0.999523 0.037 Uiso 1 1 calc R U . . .
C31 C 0.9822(3) 0.7645(3) 0.94009(16) 0.0254(6) Uani 1 1 d . . . . .
C32 C 0.8592(3) 0.7324(3) 0.87150(15) 0.0229(5) Uani 1 1 d . . . . .
B1 B 0.6299(6) 0.1056(4) 0.7030(3) 0.0426(9) Uani 1 1 d . . . . .
F1 F 0.5935(4) 0.0048(3) 0.6664(2) 0.0879(11) Uani 1 1 d . . . . .
F2 F 0.6602(6) 0.1746(4) 0.6494(3) 0.1252(19) Uani 1 1 d . . . . .
F3 F 0.5220(5) 0.1550(4) 0.7242(3) 0.1157(16) Uani 1 1 d . . . . .
F4 F 0.7400(4) 0.1123(3) 0.77395(19) 0.0686(8) Uani 1 1 d . . . . .
O3 O 0.3662(5) 0.8576(4) 0.9040(3) 0.0859(13) Uani 1 1 d . . . . .
O4 O 0.8250(6) 0.8577(4) 0.5782(3) 0.0902(14) Uani 1 1 d . . . . .
C33 C 0.3037(8) 0.9184(7) 0.7682(4) 0.090(2) Uani 1 1 d . . . . .
H33A H 0.228621 0.853254 0.756122 0.135 Uiso 1 1 calc R U . . .
H33B H 0.362376 0.915673 0.725957 0.135 Uiso 1 1 calc R U . . .
H33C H 0.256016 0.984324 0.765561 0.135 Uiso 1 1 calc R U . . .
C34 C 0.4019(7) 0.9213(5) 0.8552(4) 0.0703(15) Uani 1 1 d . . . . .
C35 C 0.5319(9) 0.9968(8) 0.8829(5) 0.122(3) Uani 1 1 d . . . . .
H35A H 0.560341 1.008261 0.945139 0.183 Uiso 1 1 calc R U . . .
H35B H 0.515579 1.066690 0.861408 0.183 Uiso 1 1 calc R U . . .
H35C H 0.610540 0.968251 0.861614 0.183 Uiso 1 1 calc R U . . .
C36 C 0.7034(9) 0.9735(6) 0.4809(4) 0.090(2) Uani 1 1 d . . . . .
H36A H 0.662500 0.905702 0.442452 0.135 Uiso 1 1 calc R U . . .
H36B H 0.746437 1.027821 0.450194 0.135 Uiso 1 1 calc R U . . .
H36C H 0.624982 1.002209 0.502420 0.135 Uiso 1 1 calc R U . . .
C37 C 0.8207(7) 0.9501(6) 0.5545(4) 0.0734(15) Uani 1 1 d . . . . .
C38 C 0.9293(8) 1.0412(6) 0.6021(5) 0.093(2) Uani 1 1 d . . . . .
H38A H 0.888642 1.079960 0.644403 0.140 Uiso 1 1 calc R U . . .
H38B H 0.954371 1.091819 0.563165 0.140 Uiso 1 1 calc R U . . .
H38C H 1.017823 1.013315 0.630844 0.140 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 O2 1.867(2) . ?
Fe1 O1 1.8792(18) . ?
Fe1 N2 1.933(3) . ?
Fe1 N4 1.939(3) . ?
Fe1 N1 1.978(2) . ?
Fe1 N3 1.984(2) . ?
Cl1 C13 1.731(3) . ?
Cl2 C15 1.725(3) . ?
Cl3 C29 1.741(4) . ?
Cl4 C31 1.739(3) . ?
N1 C2 1.325(4) . ?
N1 C1 1.367(4) . ?
N2 C10 1.296(4) . ?
N2 C9 1.421(3) . ?
N3 C18 1.321(4) . ?
N3 C17 1.374(4) . ?
N4 C26 1.282(4) . ?
N4 C25 1.439(3) . ?
O1 C16 1.307(3) . ?
O2 C32 1.311(4) . ?
C1 C9 1.412(4) . ?
C1 C5 1.418(4) . ?
C2 C3 1.412(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.358(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.413(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.411(5) . ?
C6 C7 1.358(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.424(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(4) . ?
C8 H8 0.9500 . ?
C10 C11 1.439(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.403(4) . ?
C11 C16 1.426(4) . ?
C12 C13 1.372(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.398(4) . ?
C14 C15 1.373(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.429(3) . ?
C17 C25 1.396(5) . ?
C17 C21 1.415(4) . ?
C18 C19 1.420(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.354(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.420(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.417(5) . ?
C22 C23 1.345(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.414(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.382(4) . ?
C24 H24 0.9500 . ?
C26 C27 1.435(4) . ?
C26 H26 0.9500 . ?
C27 C32 1.419(4) . ?
C27 C28 1.429(5) . ?
C28 C29 1.363(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(5) . ?
C30 C31 1.392(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.402(4) . ?
B1 F1 1.303(6) . ?
B1 F2 1.332(6) . ?
B1 F3 1.346(6) . ?
B1 F4 1.354(5) . ?
O3 C34 1.243(7) . ?
O4 C37 1.245(7) . ?
C33 C34 1.501(9) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.406(10) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.511(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.455(9) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 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
O2 Fe1 O1 91.18(9) . . ?
O2 Fe1 N2 89.32(10) . . ?
O1 Fe1 N2 95.03(9) . . ?
O2 Fe1 N4 93.46(10) . . ?
O1 Fe1 N4 85.81(10) . . ?
N2 Fe1 N4 177.08(10) . . ?
O2 Fe1 N1 89.91(9) . . ?
O1 Fe1 N1 177.60(11) . . ?
N2 Fe1 N1 82.84(10) . . ?
N4 Fe1 N1 96.27(11) . . ?
O2 Fe1 N3 175.72(10) . . ?
O1 Fe1 N3 91.13(9) . . ?
N2 Fe1 N3 94.07(11) . . ?
N4 Fe1 N3 83.11(11) . . ?
N1 Fe1 N3 87.92(9) . . ?
C2 N1 C1 118.1(2) . . ?
C2 N1 Fe1 128.7(2) . . ?
C1 N1 Fe1 113.13(19) . . ?
C10 N2 C9 120.3(2) . . ?
C10 N2 Fe1 125.57(17) . . ?
C9 N2 Fe1 114.07(19) . . ?
C18 N3 C17 119.0(2) . . ?
C18 N3 Fe1 128.81(19) . . ?
C17 N3 Fe1 112.2(2) . . ?
C26 N4 C25 121.6(3) . . ?
C26 N4 Fe1 124.98(19) . . ?
C25 N4 Fe1 112.8(2) . . ?
C16 O1 Fe1 125.76(16) . . ?
C32 O2 Fe1 123.65(16) . . ?
N1 C1 C9 116.5(2) . . ?
N1 C1 C5 122.8(3) . . ?
C9 C1 C5 120.8(3) . . ?
N1 C2 C3 122.5(3) . . ?
N1 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 124.2(3) . . ?
C6 C5 C1 118.6(3) . . ?
C4 C5 C1 117.2(3) . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 121.8(3) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C1 119.4(2) . . ?
C8 C9 N2 127.1(3) . . ?
C1 C9 N2 113.5(2) . . ?
N2 C10 C11 124.8(3) . . ?
N2 C10 H10 117.6 . . ?
C11 C10 H10 117.6 . . ?
C12 C11 C16 121.2(2) . . ?
C12 C11 C10 116.4(3) . . ?
C16 C11 C10 122.4(3) . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 120.0(3) . . ?
C12 C13 Cl1 120.4(2) . . ?
C14 C13 Cl1 119.6(2) . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 122.5(3) . . ?
C14 C15 Cl2 119.31(19) . . ?
C16 C15 Cl2 118.1(2) . . ?
O1 C16 C11 125.8(2) . . ?
O1 C16 C15 118.7(2) . . ?
C11 C16 C15 115.5(3) . . ?
N3 C17 C25 117.2(2) . . ?
N3 C17 C21 122.0(3) . . ?
C25 C17 C21 120.8(3) . . ?
N3 C18 C19 121.9(3) . . ?
N3 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C20 C19 C18 120.2(4) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.4(3) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C17 117.9(3) . . ?
C22 C21 C20 124.7(3) . . ?
C17 C21 C20 117.4(3) . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 122.5(3) . . ?
C22 C23 H23 118.8 . . ?
C24 C23 H23 118.8 . . ?
C25 C24 C23 118.3(4) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C24 C25 C17 120.2(3) . . ?
C24 C25 N4 126.2(3) . . ?
C17 C25 N4 113.5(2) . . ?
N4 C26 C27 123.8(3) . . ?
N4 C26 H26 118.1 . . ?
C27 C26 H26 118.1 . . ?
C32 C27 C28 120.2(3) . . ?
C32 C27 C26 123.1(3) . . ?
C28 C27 C26 116.8(3) . . ?
C29 C28 C27 120.0(3) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 121.5(3) . . ?
C28 C29 Cl3 119.2(3) . . ?
C30 C29 Cl3 119.4(3) . . ?
C29 C30 C31 118.5(3) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
C30 C31 C32 123.4(3) . . ?
C30 C31 Cl4 118.8(2) . . ?
C32 C31 Cl4 117.9(2) . . ?
O2 C32 C31 119.0(2) . . ?
O2 C32 C27 124.5(2) . . ?
C31 C32 C27 116.5(3) . . ?
F1 B1 F2 111.9(5) . . ?
F1 B1 F3 116.7(5) . . ?
F2 B1 F3 96.2(5) . . ?
F1 B1 F4 110.5(4) . . ?
F2 B1 F4 113.1(4) . . ?
F3 B1 F4 107.8(4) . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O3 C34 C35 119.6(7) . . ?
O3 C34 C33 119.6(6) . . ?
C35 C34 C33 120.8(6) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O4 C37 C38 118.7(6) . . ?
O4 C37 C36 123.0(6) . . ?
C38 C37 C36 118.2(7) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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
O2 Fe1 O1 C16 83.2(2) . . . . ?
N2 Fe1 O1 C16 -6.2(2) . . . . ?
N4 Fe1 O1 C16 176.6(2) . . . . ?
N3 Fe1 O1 C16 -100.4(2) . . . . ?
O1 Fe1 O2 C32 57.6(2) . . . . ?
N2 Fe1 O2 C32 152.6(2) . . . . ?
N4 Fe1 O2 C32 -28.3(2) . . . . ?
N1 Fe1 O2 C32 -124.6(2) . . . . ?
C2 N1 C1 C9 -179.3(3) . . . . ?
Fe1 N1 C1 C9 -1.1(3) . . . . ?
C2 N1 C1 C5 -0.6(4) . . . . ?
Fe1 N1 C1 C5 177.5(2) . . . . ?
C1 N1 C2 C3 -0.3(4) . . . . ?
Fe1 N1 C2 C3 -178.1(2) . . . . ?
N1 C2 C3 C4 0.7(5) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C3 C4 C5 C6 179.2(3) . . . . ?
C3 C4 C5 C1 -0.5(4) . . . . ?
N1 C1 C5 C6 -178.8(3) . . . . ?
C9 C1 C5 C6 -0.2(4) . . . . ?
N1 C1 C5 C4 1.0(4) . . . . ?
C9 C1 C5 C4 179.6(3) . . . . ?
C4 C5 C6 C7 -179.6(3) . . . . ?
C1 C5 C6 C7 0.2(5) . . . . ?
C5 C6 C7 C8 -0.3(5) . . . . ?
C6 C7 C8 C9 0.4(5) . . . . ?
C7 C8 C9 C1 -0.3(4) . . . . ?
C7 C8 C9 N2 178.5(3) . . . . ?
N1 C1 C9 C8 178.9(3) . . . . ?
C5 C1 C9 C8 0.2(4) . . . . ?
N1 C1 C9 N2 0.0(4) . . . . ?
C5 C1 C9 N2 -178.7(2) . . . . ?
C10 N2 C9 C8 2.8(4) . . . . ?
Fe1 N2 C9 C8 -177.7(2) . . . . ?
C10 N2 C9 C1 -178.3(2) . . . . ?
Fe1 N2 C9 C1 1.2(3) . . . . ?
C9 N2 C10 C11 -176.0(2) . . . . ?
Fe1 N2 C10 C11 4.6(4) . . . . ?
N2 C10 C11 C12 177.6(3) . . . . ?
N2 C10 C11 C16 -2.2(4) . . . . ?
C16 C11 C12 C13 0.7(4) . . . . ?
C10 C11 C12 C13 -179.1(3) . . . . ?
C11 C12 C13 C14 2.0(4) . . . . ?
C11 C12 C13 Cl1 179.5(2) . . . . ?
C12 C13 C14 C15 -1.8(4) . . . . ?
Cl1 C13 C14 C15 -179.3(2) . . . . ?
C13 C14 C15 C16 -1.2(4) . . . . ?
C13 C14 C15 Cl2 178.3(2) . . . . ?
Fe1 O1 C16 C11 10.1(4) . . . . ?
Fe1 O1 C16 C15 -172.08(18) . . . . ?
C12 C11 C16 O1 174.5(3) . . . . ?
C10 C11 C16 O1 -5.7(4) . . . . ?
C12 C11 C16 C15 -3.4(4) . . . . ?
C10 C11 C16 C15 176.4(2) . . . . ?
C14 C15 C16 O1 -174.4(2) . . . . ?
Cl2 C15 C16 O1 6.1(3) . . . . ?
C14 C15 C16 C11 3.6(4) . . . . ?
Cl2 C15 C16 C11 -175.85(19) . . . . ?
C18 N3 C17 C25 -176.5(2) . . . . ?
Fe1 N3 C17 C25 3.2(3) . . . . ?
C18 N3 C17 C21 4.1(4) . . . . ?
Fe1 N3 C17 C21 -176.2(2) . . . . ?
C17 N3 C18 C19 -2.0(4) . . . . ?
Fe1 N3 C18 C19 178.3(2) . . . . ?
N3 C18 C19 C20 0.3(4) . . . . ?
C18 C19 C20 C21 -0.6(4) . . . . ?
N3 C17 C21 C22 177.5(2) . . . . ?
C25 C17 C21 C22 -1.9(4) . . . . ?
N3 C17 C21 C20 -4.4(4) . . . . ?
C25 C17 C21 C20 176.3(2) . . . . ?
C19 C20 C21 C22 -179.4(3) . . . . ?
C19 C20 C21 C17 2.6(4) . . . . ?
C17 C21 C22 C23 0.7(4) . . . . ?
C20 C21 C22 C23 -177.3(3) . . . . ?
C21 C22 C23 C24 0.4(5) . . . . ?
C22 C23 C24 C25 -0.3(5) . . . . ?
C23 C24 C25 C17 -0.8(4) . . . . ?
C23 C24 C25 N4 176.7(3) . . . . ?
N3 C17 C25 C24 -177.4(3) . . . . ?
C21 C17 C25 C24 1.9(4) . . . . ?
N3 C17 C25 N4 4.8(3) . . . . ?
C21 C17 C25 N4 -175.9(2) . . . . ?
C26 N4 C25 C24 -16.4(4) . . . . ?
Fe1 N4 C25 C24 171.8(2) . . . . ?
C26 N4 C25 C17 161.2(3) . . . . ?
Fe1 N4 C25 C17 -10.6(3) . . . . ?
C25 N4 C26 C27 -178.3(3) . . . . ?
Fe1 N4 C26 C27 -7.4(4) . . . . ?
N4 C26 C27 C32 -6.4(5) . . . . ?
N4 C26 C27 C28 175.7(3) . . . . ?
C32 C27 C28 C29 2.2(5) . . . . ?
C26 C27 C28 C29 -179.8(3) . . . . ?
C27 C28 C29 C30 -0.9(5) . . . . ?
C27 C28 C29 Cl3 178.7(2) . . . . ?
C28 C29 C30 C31 -0.4(5) . . . . ?
Cl3 C29 C30 C31 180.0(2) . . . . ?
C29 C30 C31 C32 0.5(5) . . . . ?
C29 C30 C31 Cl4 -179.5(2) . . . . ?
Fe1 O2 C32 C31 -158.5(2) . . . . ?
Fe1 O2 C32 C27 23.8(4) . . . . ?
C30 C31 C32 O2 -177.1(3) . . . . ?
Cl4 C31 C32 O2 2.9(4) . . . . ?
C30 C31 C32 C27 0.7(4) . . . . ?
Cl4 C31 C32 C27 -179.3(2) . . . . ?
C28 C27 C32 O2 175.6(3) . . . . ?
C26 C27 C32 O2 -2.2(5) . . . . ?
C28 C27 C32 C31 -2.1(4) . . . . ?
C26 C27 C32 C31 -179.9(3) . . . . ?

_refine_diff_density_max         2.024
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.149

# start Validation Reply Form
_vrf_PLAT029_2a100K              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.941 Why?  
RESPONSE: Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.941, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;
# 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_2b(298k)(sqd)_sq
_database_code_depnum_ccdc_archive 'CCDC 2002659'
loop_
_audit_author_name
_audit_author_address
'Kil Sik Min'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Cl4 Fe N4 O2, B F4'
_chemical_formula_sum            'C32 H18 B Cl4 F4 Fe N4 O2'
_chemical_formula_weight         774.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0050 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0140 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1230 0.1260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3241 0.6814 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.5750(19)
_cell_length_b                   12.544(3)
_cell_length_c                   16.518(3)
_cell_angle_alpha                94.12(3)
_cell_angle_beta                 103.45(3)
_cell_angle_gamma                97.39(3)
_cell_volume                     1902.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    25533
_cell_measurement_theta_min      0.36
_cell_measurement_theta_max      33.55

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             778
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.520
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.630
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15631
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measured_fraction_theta_full 0.918
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_Laue_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.918
_reflns_number_total             9786
_reflns_number_gt                6035
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINFGX
_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)+(0.1331P)²] 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         9786
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0967
_refine_ls_wR_factor_ref         0.3042
_refine_ls_wR_factor_gt          0.2870
_refine_ls_goodness_of_fit_ref   1.500
_refine_ls_restrained_S_all      1.500
_refine_ls_shift/su_max          0.001
_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 0.65596(6) 0.55768(5) 0.76705(3) 0.0385(2) Uani 1 1 d . . . . .
Cl1 Cl 1.21992(15) 0.24398(14) 0.72327(11) 0.0746(4) Uani 1 1 d . . . . .
Cl2 Cl 1.05693(15) 0.62445(14) 0.64733(10) 0.0720(4) Uani 1 1 d . . . . .
Cl3 Cl 1.1316(2) 1.05990(16) 0.90841(15) 0.1012(6) Uani 1 1 d . . . . .
Cl4 Cl 1.02471(14) 0.66401(14) 1.00806(8) 0.0704(4) Uani 1 1 d . . . . .
N1 N 0.4888(4) 0.5499(3) 0.8223(2) 0.0465(9) Uani 1 1 d . . . . .
N2 N 0.6774(4) 0.4213(3) 0.8137(2) 0.0432(8) Uani 1 1 d . . . . .
N3 N 0.5127(4) 0.4914(3) 0.6598(2) 0.0422(8) Uani 1 1 d . . . . .
N4 N 0.6211(4) 0.6906(3) 0.7166(2) 0.0463(9) Uani 1 1 d . . . . .
O1 O 0.8121(3) 0.5548(3) 0.71604(19) 0.0484(7) Uani 1 1 d . . . . .
O2 O 0.7790(3) 0.6319(3) 0.86556(18) 0.0480(7) Uani 1 1 d . . . . .
C1 C 0.4749(4) 0.4613(4) 0.8640(3) 0.0468(10) Uani 1 1 d . . . . .
C2 C 0.3961(5) 0.6192(5) 0.8231(3) 0.0572(12) Uani 1 1 d . . . . .
H2 H 0.403748 0.678793 0.793209 0.069 Uiso 1 1 calc R U . . .
C3 C 0.2878(6) 0.6075(6) 0.8665(4) 0.0689(16) Uani 1 1 d . . . . .
H3 H 0.226457 0.659192 0.866916 0.083 Uiso 1 1 calc R U . . .
C4 C 0.2732(5) 0.5181(6) 0.9088(4) 0.0688(16) Uani 1 1 d . . . . .
H4 H 0.200821 0.508932 0.937761 0.083 Uiso 1 1 calc R U . . .
C5 C 0.3665(5) 0.4403(5) 0.9087(3) 0.0575(12) Uani 1 1 d . . . . .
C6 C 0.3647(6) 0.3462(6) 0.9523(4) 0.0708(16) Uani 1 1 d . . . . .
H6 H 0.296784 0.332183 0.983748 0.085 Uiso 1 1 calc R U . . .
C7 C 0.4591(6) 0.2783(5) 0.9484(4) 0.0661(14) Uani 1 1 d . . . . .
H7 H 0.455287 0.217241 0.977065 0.079 Uiso 1 1 calc R U . . .
C8 C 0.5663(6) 0.2964(5) 0.9017(3) 0.0622(14) Uani 1 1 d . . . . .
H8 H 0.630305 0.247116 0.899321 0.075 Uiso 1 1 calc R U . . .
C9 C 0.5744(4) 0.3878(4) 0.8598(3) 0.0455(10) Uani 1 1 d . . . . .
C10 C 0.7758(4) 0.3607(4) 0.8041(3) 0.0446(10) Uani 1 1 d . . . . .
H10 H 0.772292 0.294792 0.826489 0.054 Uiso 1 1 calc R U . . .
C11 C 0.8880(4) 0.3884(4) 0.7618(3) 0.0455(10) Uani 1 1 d . . . . .
C12 C 0.9851(5) 0.3140(4) 0.7613(3) 0.0488(10) Uani 1 1 d . . . . .
H12 H 0.972407 0.249911 0.785558 0.059 Uiso 1 1 calc R U . . .
C13 C 1.0994(5) 0.3361(5) 0.7247(3) 0.0543(11) Uani 1 1 d . . . . .
C14 C 1.1202(5) 0.4302(5) 0.6891(3) 0.0572(13) Uani 1 1 d . . . . .
H14 H 1.197661 0.444508 0.664408 0.069 Uiso 1 1 calc R U . . .
C15 C 1.0249(5) 0.5035(4) 0.6902(3) 0.0500(11) Uani 1 1 d . . . . .
C16 C 0.9032(4) 0.4842(4) 0.7234(2) 0.0432(9) Uani 1 1 d . . . . .
C17 C 0.4553(4) 0.5674(4) 0.6127(3) 0.0440(9) Uani 1 1 d . . . . .
C18 C 0.4718(5) 0.3883(4) 0.6321(3) 0.0475(10) Uani 1 1 d . . . . .
H18 H 0.511990 0.336794 0.664142 0.057 Uiso 1 1 calc R U . . .
C19 C 0.3694(5) 0.3534(5) 0.5555(3) 0.0567(12) Uani 1 1 d . . . . .
H19 H 0.344811 0.280171 0.536678 0.068 Uiso 1 1 calc R U . . .
C20 C 0.3074(5) 0.4274(5) 0.5098(3) 0.0602(13) Uani 1 1 d . . . . .
H20 H 0.237440 0.404816 0.460106 0.072 Uiso 1 1 calc R U . . .
C21 C 0.3465(5) 0.5362(5) 0.5360(3) 0.0524(12) Uani 1 1 d . . . . .
C22 C 0.2903(6) 0.6209(6) 0.4927(3) 0.0649(15) Uani 1 1 d . . . . .
H22 H 0.218557 0.604524 0.443030 0.078 Uiso 1 1 calc R U . . .
C23 C 0.3396(6) 0.7244(6) 0.5227(3) 0.0668(15) Uani 1 1 d . . . . .
H23 H 0.299838 0.777995 0.492882 0.080 Uiso 1 1 calc R U . . .
C24 C 0.4484(6) 0.7561(5) 0.5970(3) 0.0591(13) Uani 1 1 d . . . . .
H24 H 0.480192 0.828765 0.615941 0.071 Uiso 1 1 calc R U . . .
C25 C 0.5070(5) 0.6759(4) 0.6413(3) 0.0473(10) Uani 1 1 d . . . . .
C26 C 0.7043(6) 0.7839(4) 0.7394(3) 0.0549(11) Uani 1 1 d . . . . .
H26 H 0.685680 0.840279 0.706785 0.066 Uiso 1 1 calc R U . . .
C27 C 0.8227(5) 0.8035(4) 0.8124(3) 0.0545(11) Uani 1 1 d . . . . .
C28 C 0.9103(6) 0.9079(5) 0.8251(4) 0.0659(14) Uani 1 1 d . . . . .
H28 H 0.888718 0.957883 0.786864 0.079 Uiso 1 1 calc R U . . .
C29 C 1.0264(7) 0.9343(5) 0.8939(4) 0.0720(15) Uani 1 1 d . . . . .
C30 C 1.0651(6) 0.8582(5) 0.9495(4) 0.0682(15) Uani 1 1 d . . . . .
H30 H 1.147315 0.874533 0.993733 0.082 Uiso 1 1 calc R U . . .
C31 C 0.9785(5) 0.7574(5) 0.9378(3) 0.0556(12) Uani 1 1 d . . . . .
C32 C 0.8565(5) 0.7263(4) 0.8703(3) 0.0481(10) Uani 1 1 d . . . . .
B1 B 0.6412(17) 0.1018(7) 0.6962(10) 0.136(5) Uani 1 1 d . . . . .
F1 F 0.5975(11) 0.0050(7) 0.6712(6) 0.209(2) Uani 1 1 d . . . . .
F2 F 0.6467(12) 0.1722(7) 0.6513(6) 0.209(2) Uani 1 1 d . . . . .
F3 F 0.5294(12) 0.1578(7) 0.7114(6) 0.209(2) Uani 1 1 d . . . . .
F4 F 0.7307(12) 0.1087(7) 0.7725(7) 0.209(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.873(3) . ?
Fe1 O1 1.882(3) . ?
Fe1 N2 1.942(4) . ?
Fe1 N4 1.950(4) . ?
Fe1 N1 2.014(3) . ?
Fe1 N3 2.019(4) . ?
Cl1 C13 1.737(5) . ?
Cl2 C15 1.741(5) . ?
Cl3 C29 1.726(6) . ?
Cl4 C31 1.733(6) . ?
N1 C2 1.322(6) . ?
N1 C1 1.356(6) . ?
N2 C10 1.314(5) . ?
N2 C9 1.421(5) . ?
N3 C18 1.318(6) . ?
N3 C17 1.364(6) . ?
N4 C26 1.305(7) . ?
N4 C25 1.434(5) . ?
O1 C16 1.313(5) . ?
O2 C32 1.301(6) . ?
C1 C5 1.416(6) . ?
C1 C9 1.418(6) . ?
C2 C3 1.390(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.405(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.427(9) . ?
C6 C7 1.327(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.427(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(7) . ?
C8 H8 0.9300 . ?
C10 C11 1.433(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.401(6) . ?
C11 C16 1.405(7) . ?
C12 C13 1.376(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(8) . ?
C14 C15 1.378(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.401(6) . ?
C17 C25 1.394(7) . ?
C17 C21 1.434(6) . ?
C18 C19 1.410(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.348(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.378(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.416(7) . ?
C22 C23 1.340(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.407(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.386(6) . ?
C24 H24 0.9300 . ?
C26 C27 1.431(7) . ?
C26 H26 0.9300 . ?
C27 C32 1.425(7) . ?
C27 C28 1.434(8) . ?
C28 C29 1.379(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.397(9) . ?
C30 C31 1.394(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.405(6) . ?
B1 F2 1.198(14) . ?
B1 F1 1.240(13) . ?
B1 F4 1.338(15) . ?
B1 F3 1.413(16) . ?
F2 F3 1.665(13) . ?

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
O2 Fe1 O1 91.50(14) . . ?
O2 Fe1 N2 90.03(15) . . ?
O1 Fe1 N2 94.38(14) . . ?
O2 Fe1 N4 93.07(16) . . ?
O1 Fe1 N4 87.76(15) . . ?
N2 Fe1 N4 176.19(15) . . ?
O2 Fe1 N1 89.68(14) . . ?
O1 Fe1 N1 176.06(15) . . ?
N2 Fe1 N1 81.86(15) . . ?
N4 Fe1 N1 95.93(16) . . ?
O2 Fe1 N3 174.02(14) . . ?
O1 Fe1 N3 91.24(14) . . ?
N2 Fe1 N3 95.05(16) . . ?
N4 Fe1 N3 81.73(16) . . ?
N1 Fe1 N3 87.94(14) . . ?
C2 N1 C1 118.3(4) . . ?
C2 N1 Fe1 128.4(4) . . ?
C1 N1 Fe1 113.3(3) . . ?
C10 N2 C9 120.4(4) . . ?
C10 N2 Fe1 124.9(3) . . ?
C9 N2 Fe1 114.8(3) . . ?
C18 N3 C17 119.1(4) . . ?
C18 N3 Fe1 128.5(3) . . ?
C17 N3 Fe1 112.4(3) . . ?
C26 N4 C25 120.1(4) . . ?
C26 N4 Fe1 125.0(3) . . ?
C25 N4 Fe1 114.2(3) . . ?
C16 O1 Fe1 126.9(3) . . ?
C32 O2 Fe1 124.8(3) . . ?
N1 C1 C5 123.1(4) . . ?
N1 C1 C9 116.4(4) . . ?
C5 C1 C9 120.5(5) . . ?
N1 C2 C3 123.3(6) . . ?
N1 C2 H2 118.3 . . ?
C3 C2 H2 118.4 . . ?
C4 C3 C2 118.6(5) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 120.7(5) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C1 116.0(5) . . ?
C4 C5 C6 125.7(5) . . ?
C1 C5 C6 118.2(5) . . ?
C7 C6 C5 120.7(5) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 121.9(5) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 119.6(5) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C1 119.1(4) . . ?
C8 C9 N2 127.3(4) . . ?
C1 C9 N2 113.6(4) . . ?
N2 C10 C11 125.1(4) . . ?
N2 C10 H10 117.5 . . ?
C11 C10 H10 117.5 . . ?
C12 C11 C16 121.0(4) . . ?
C12 C11 C10 115.9(4) . . ?
C16 C11 C10 123.2(4) . . ?
C13 C12 C11 119.7(5) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 120.9(4) . . ?
C14 C13 Cl1 119.0(4) . . ?
C12 C13 Cl1 120.0(4) . . ?
C13 C14 C15 119.2(4) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 122.8(5) . . ?
C14 C15 Cl2 118.3(4) . . ?
C16 C15 Cl2 118.9(4) . . ?
O1 C16 C15 118.6(4) . . ?
O1 C16 C11 125.0(4) . . ?
C15 C16 C11 116.3(4) . . ?
N3 C17 C25 117.8(4) . . ?
N3 C17 C21 120.8(4) . . ?
C25 C17 C21 121.4(4) . . ?
N3 C18 C19 122.3(5) . . ?
N3 C18 H18 118.8 . . ?
C19 C18 H18 118.8 . . ?
C20 C19 C18 119.2(5) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 120.7(5) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C22 125.6(5) . . ?
C20 C21 C17 117.7(4) . . ?
C22 C21 C17 116.7(5) . . ?
C23 C22 C21 120.6(5) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 123.2(5) . . ?
C22 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C25 C24 C23 118.1(5) . . ?
C25 C24 H24 120.9 . . ?
C23 C24 H24 120.9 . . ?
C24 C25 C17 119.9(4) . . ?
C24 C25 N4 127.0(5) . . ?
C17 C25 N4 113.1(4) . . ?
N4 C26 C27 123.1(5) . . ?
N4 C26 H26 118.4 . . ?
C27 C26 H26 118.4 . . ?
C32 C27 C26 123.8(5) . . ?
C32 C27 C28 120.1(5) . . ?
C26 C27 C28 116.1(5) . . ?
C29 C28 C27 120.2(5) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 120.6(5) . . ?
C28 C29 Cl3 119.8(5) . . ?
C30 C29 Cl3 119.5(5) . . ?
C31 C30 C29 119.0(5) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C30 C31 C32 123.2(5) . . ?
C30 C31 Cl4 119.0(4) . . ?
C32 C31 Cl4 117.9(4) . . ?
O2 C32 C31 119.2(4) . . ?
O2 C32 C27 124.0(4) . . ?
C31 C32 C27 116.8(5) . . ?
F2 B1 F1 124.4(15) . . ?
F2 B1 F4 122.2(12) . . ?
F1 B1 F4 108.6(10) . . ?
F2 B1 F3 78.7(8) . . ?
F1 B1 F3 112.6(13) . . ?
F4 B1 F3 102.5(12) . . ?
B1 F2 F3 56.4(8) . . ?
B1 F3 F2 44.9(7) . . ?

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
O2 Fe1 O1 C16 84.1(4) . . . . ?
N2 Fe1 O1 C16 -6.1(4) . . . . ?
N4 Fe1 O1 C16 177.1(4) . . . . ?
N3 Fe1 O1 C16 -101.2(4) . . . . ?
O1 Fe1 O2 C32 60.1(4) . . . . ?
N2 Fe1 O2 C32 154.5(4) . . . . ?
N4 Fe1 O2 C32 -27.7(4) . . . . ?
N1 Fe1 O2 C32 -123.7(4) . . . . ?
C2 N1 C1 C5 -0.5(7) . . . . ?
Fe1 N1 C1 C5 178.8(4) . . . . ?
C2 N1 C1 C9 178.6(4) . . . . ?
Fe1 N1 C1 C9 -2.1(5) . . . . ?
C1 N1 C2 C3 1.9(7) . . . . ?
Fe1 N1 C2 C3 -177.3(4) . . . . ?
N1 C2 C3 C4 -1.9(8) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C3 C4 C5 C1 0.8(8) . . . . ?
C3 C4 C5 C6 177.9(5) . . . . ?
N1 C1 C5 C4 -0.9(7) . . . . ?
C9 C1 C5 C4 -179.9(4) . . . . ?
N1 C1 C5 C6 -178.2(5) . . . . ?
C9 C1 C5 C6 2.8(7) . . . . ?
C4 C5 C6 C7 -179.4(6) . . . . ?
C1 C5 C6 C7 -2.4(8) . . . . ?
C5 C6 C7 C8 0.5(9) . . . . ?
C6 C7 C8 C9 0.9(9) . . . . ?
C7 C8 C9 C1 -0.4(8) . . . . ?
C7 C8 C9 N2 176.9(5) . . . . ?
N1 C1 C9 C8 179.5(4) . . . . ?
C5 C1 C9 C8 -1.5(7) . . . . ?
N1 C1 C9 N2 1.8(6) . . . . ?
C5 C1 C9 N2 -179.1(4) . . . . ?
C10 N2 C9 C8 3.1(7) . . . . ?
Fe1 N2 C9 C8 -178.0(4) . . . . ?
C10 N2 C9 C1 -179.5(4) . . . . ?
Fe1 N2 C9 C1 -0.6(5) . . . . ?
C9 N2 C10 C11 -177.5(4) . . . . ?
Fe1 N2 C10 C11 3.7(6) . . . . ?
N2 C10 C11 C12 177.7(4) . . . . ?
N2 C10 C11 C16 -1.6(7) . . . . ?
C16 C11 C12 C13 1.7(7) . . . . ?
C10 C11 C12 C13 -177.6(4) . . . . ?
C11 C12 C13 C14 0.3(8) . . . . ?
C11 C12 C13 Cl1 -179.6(4) . . . . ?
C12 C13 C14 C15 0.1(8) . . . . ?
Cl1 C13 C14 C15 -179.9(4) . . . . ?
C13 C14 C15 C16 -2.7(8) . . . . ?
C13 C14 C15 Cl2 178.0(4) . . . . ?
Fe1 O1 C16 C15 -171.2(3) . . . . ?
Fe1 O1 C16 C11 9.6(6) . . . . ?
C14 C15 C16 O1 -174.8(4) . . . . ?
Cl2 C15 C16 O1 4.5(6) . . . . ?
C14 C15 C16 C11 4.5(7) . . . . ?
Cl2 C15 C16 C11 -176.2(3) . . . . ?
C12 C11 C16 O1 175.2(4) . . . . ?
C10 C11 C16 O1 -5.5(7) . . . . ?
C12 C11 C16 C15 -4.0(6) . . . . ?
C10 C11 C16 C15 175.3(4) . . . . ?
C18 N3 C17 C25 -176.3(4) . . . . ?
Fe1 N3 C17 C25 3.4(4) . . . . ?
C18 N3 C17 C21 3.1(6) . . . . ?
Fe1 N3 C17 C21 -177.2(3) . . . . ?
C17 N3 C18 C19 -0.7(6) . . . . ?
Fe1 N3 C18 C19 179.7(3) . . . . ?
N3 C18 C19 C20 -2.0(7) . . . . ?
C18 C19 C20 C21 2.0(7) . . . . ?
C19 C20 C21 C22 179.1(5) . . . . ?
C19 C20 C21 C17 0.4(7) . . . . ?
N3 C17 C21 C20 -3.0(6) . . . . ?
C25 C17 C21 C20 176.4(4) . . . . ?
N3 C17 C21 C22 178.1(4) . . . . ?
C25 C17 C21 C22 -2.5(6) . . . . ?
C20 C21 C22 C23 -177.9(5) . . . . ?
C17 C21 C22 C23 0.9(7) . . . . ?
C21 C22 C23 C24 0.4(8) . . . . ?
C22 C23 C24 C25 -0.1(8) . . . . ?
C23 C24 C25 C17 -1.5(7) . . . . ?
C23 C24 C25 N4 178.0(4) . . . . ?
N3 C17 C25 C24 -177.8(4) . . . . ?
C21 C17 C25 C24 2.8(6) . . . . ?
N3 C17 C25 N4 2.7(5) . . . . ?
C21 C17 C25 N4 -176.7(4) . . . . ?
C26 N4 C25 C24 -16.5(7) . . . . ?
Fe1 N4 C25 C24 172.8(4) . . . . ?
C26 N4 C25 C17 163.0(4) . . . . ?
Fe1 N4 C25 C17 -7.8(4) . . . . ?
C25 N4 C26 C27 -178.1(4) . . . . ?
Fe1 N4 C26 C27 -8.4(7) . . . . ?
N4 C26 C27 C32 -4.2(8) . . . . ?
N4 C26 C27 C28 175.3(5) . . . . ?
C32 C27 C28 C29 -0.7(8) . . . . ?
C26 C27 C28 C29 179.7(5) . . . . ?
C27 C28 C29 C30 3.4(9) . . . . ?
C27 C28 C29 Cl3 179.7(5) . . . . ?
C28 C29 C30 C31 -4.4(9) . . . . ?
Cl3 C29 C30 C31 179.3(4) . . . . ?
C29 C30 C31 C32 2.8(8) . . . . ?
C29 C30 C31 Cl4 -178.8(4) . . . . ?
Fe1 O2 C32 C31 -158.4(3) . . . . ?
Fe1 O2 C32 C27 24.1(6) . . . . ?
C30 C31 C32 O2 -177.8(5) . . . . ?
Cl4 C31 C32 O2 3.7(6) . . . . ?
C30 C31 C32 C27 -0.1(7) . . . . ?
Cl4 C31 C32 C27 -178.6(4) . . . . ?
C26 C27 C32 O2 -3.7(8) . . . . ?
C28 C27 C32 O2 176.7(5) . . . . ?
C26 C27 C32 C31 178.6(5) . . . . ?
C28 C27 C32 C31 -0.9(7) . . . . ?
F1 B1 F2 F3 109.8(18) . . . . ?
F4 B1 F2 F3 -97.7(15) . . . . ?
F1 B1 F3 F2 -122.7(17) . . . . ?
F4 B1 F3 F2 120.8(13) . . . . ?

_refine_diff_density_max         0.927
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.150


# start Validation Reply Form
_vrf_PLAT029_2b298ksqd_sq        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.918 Why?  
RESPONSE: Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.918, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;
# 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_3b(293k)_sq
_database_code_depnum_ccdc_archive 'CCDC 2002661'
loop_
_audit_author_name
_audit_author_address
'Kil Sik Min'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Cl4 Fe N4 O2, Cl O4'
_chemical_formula_sum            'C32 H18 Cl5 Fe N4 O6'
_chemical_formula_weight         787.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 '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 0.0050 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1230 0.1260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3241 0.6814 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.289(3)
_cell_length_b                   17.702(4)
_cell_length_c                   15.399(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.82(3)
_cell_angle_gamma                90
_cell_volume                     3708.1(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    78786
_cell_measurement_theta_min      0.36
_cell_measurement_theta_max      29.48

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_F_000             1588
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.579
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.630
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37942
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.599
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             9877
_reflns_number_gt                7465
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_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)+(0.1642P)²+3.1062P] 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     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9877
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.2486
_refine_ls_wR_factor_gt          0.2342
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_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 0.59712(3) 0.54583(2) 0.77687(3) 0.02972(16) Uani 1 1 d . . . . .
Cl1 Cl 0.75655(10) 0.92765(6) 0.83343(9) 0.0639(3) Uani 1 1 d . . . . .
Cl2 Cl 0.82183(9) 0.66576(6) 1.01884(7) 0.0658(4) Uani 1 1 d . . . . .
Cl3 Cl 1.11677(10) 0.51856(17) 0.8946(2) 0.1678(14) Uani 1 1 d . . . . .
Cl4 Cl 0.81956(8) 0.67057(7) 0.66273(8) 0.0647(3) Uani 1 1 d . . . . .
N1 N 0.52654(19) 0.48285(16) 0.67022(18) 0.0357(5) Uani 1 1 d . . . . .
N2 N 0.51914(18) 0.62572(16) 0.70322(17) 0.0336(5) Uani 1 1 d . . . . .
N3 N 0.49578(18) 0.51539(15) 0.83286(18) 0.0326(5) Uani 1 1 d . . . . .
N4 N 0.6694(2) 0.46327(14) 0.85021(19) 0.0336(5) Uani 1 1 d . . . . .
O1 O 0.65445(16) 0.61131(12) 0.87488(14) 0.0344(4) Uani 1 1 d . . . . .
O2 O 0.69590(16) 0.56835(14) 0.72453(15) 0.0358(5) Uani 1 1 d . . . . .
C1 C 0.4519(2) 0.5217(2) 0.6096(2) 0.0376(7) Uani 1 1 d . . . . .
C2 C 0.5410(3) 0.4106(2) 0.6538(3) 0.0437(7) Uani 1 1 d . . . . .
H2 H 0.591470 0.383949 0.695048 0.052 Uiso 1 1 calc R U . . .
C3 C 0.4819(3) 0.3738(2) 0.5758(3) 0.0518(9) Uani 1 1 d . . . . .
H3 H 0.494278 0.323587 0.565416 0.062 Uiso 1 1 calc R U . . .
C4 C 0.4063(3) 0.4110(3) 0.5148(3) 0.0529(10) Uani 1 1 d . . . . .
H4 H 0.367577 0.386398 0.462822 0.063 Uiso 1 1 calc R U . . .
C5 C 0.3875(3) 0.4870(3) 0.5311(2) 0.0470(8) Uani 1 1 d . . . . .
C6 C 0.3100(3) 0.5310(3) 0.4757(3) 0.0581(11) Uani 1 1 d . . . . .
H6 H 0.268057 0.510410 0.422337 0.070 Uiso 1 1 calc R U . . .
C7 C 0.2955(3) 0.6036(3) 0.4992(3) 0.0590(11) Uani 1 1 d . . . . .
H7 H 0.241277 0.630536 0.464003 0.071 Uiso 1 1 calc R U . . .
C8 C 0.3618(3) 0.6383(2) 0.5761(3) 0.0470(8) Uani 1 1 d . . . . .
H8 H 0.351433 0.687714 0.591423 0.056 Uiso 1 1 calc R U . . .
C9 C 0.4413(2) 0.5985(2) 0.6281(2) 0.0378(7) Uani 1 1 d . . . . .
C10 C 0.5406(2) 0.69626(19) 0.7131(2) 0.0381(7) Uani 1 1 d . . . . .
H10 H 0.501402 0.730020 0.671299 0.046 Uiso 1 1 calc R U . . .
C11 C 0.6222(2) 0.72619(19) 0.7854(2) 0.0365(6) Uani 1 1 d . . . . .
C12 C 0.6471(3) 0.8020(2) 0.7780(2) 0.0430(7) Uani 1 1 d . . . . .
H12 H 0.610688 0.830865 0.728795 0.052 Uiso 1 1 calc R U . . .
C13 C 0.7252(3) 0.83377(19) 0.8432(3) 0.0440(8) Uani 1 1 d . . . . .
C14 C 0.7796(3) 0.7919(2) 0.9168(3) 0.0451(8) Uani 1 1 d . . . . .
H14 H 0.833200 0.813328 0.960214 0.054 Uiso 1 1 calc R U . . .
C15 C 0.7537(3) 0.7178(2) 0.9254(2) 0.0408(7) Uani 1 1 d . . . . .
C16 C 0.6750(2) 0.68223(17) 0.8612(2) 0.0330(6) Uani 1 1 d . . . . .
C17 C 0.5200(2) 0.45187(17) 0.8848(2) 0.0338(6) Uani 1 1 d . . . . .
C18 C 0.4115(2) 0.5500(2) 0.8269(3) 0.0404(7) Uani 1 1 d . . . . .
H18 H 0.395586 0.593991 0.792407 0.049 Uiso 1 1 calc R U . . .
C19 C 0.3459(3) 0.5225(2) 0.8709(3) 0.0472(8) Uani 1 1 d . . . . .
H19 H 0.287777 0.548248 0.865659 0.057 Uiso 1 1 calc R U . . .
C20 C 0.3672(3) 0.4583(2) 0.9209(3) 0.0478(9) Uani 1 1 d . . . . .
H20 H 0.323114 0.439397 0.949100 0.057 Uiso 1 1 calc R U . . .
C21 C 0.4567(3) 0.42029(19) 0.9300(2) 0.0403(7) Uani 1 1 d . . . . .
C22 C 0.4882(3) 0.3544(2) 0.9818(3) 0.0503(9) Uani 1 1 d . . . . .
H22 H 0.447660 0.331672 1.011368 0.060 Uiso 1 1 calc R U . . .
C23 C 0.5787(3) 0.3234(2) 0.9890(3) 0.0505(9) Uani 1 1 d . . . . .
H23 H 0.598635 0.280193 1.024180 0.061 Uiso 1 1 calc R U . . .
C24 C 0.6417(3) 0.35552(19) 0.9445(3) 0.0435(7) Uani 1 1 d . . . . .
H24 H 0.702193 0.333342 0.949672 0.052 Uiso 1 1 calc R U . . .
C25 C 0.6132(2) 0.41993(17) 0.8934(2) 0.0358(6) Uani 1 1 d . . . . .
C26 C 0.7626(3) 0.4526(2) 0.8675(3) 0.0460(8) Uani 1 1 d . . . . .
H26 H 0.791097 0.412357 0.905111 0.055 Uiso 1 1 calc R U . . .
C27 C 0.8251(3) 0.4987(2) 0.8325(3) 0.0498(9) Uani 1 1 d . . . . .
C28 C 0.9264(3) 0.4863(3) 0.8705(4) 0.084(2) Uani 1 1 d . . . . .
H28 H 0.949476 0.448007 0.913052 0.101 Uiso 1 1 calc R U . . .
C29 C 0.9909(3) 0.5314(4) 0.8441(5) 0.095(2) Uani 1 1 d . . . . .
C30 C 0.9589(3) 0.5887(3) 0.7804(4) 0.0723(15) Uani 1 1 d . . . . .
H30 H 1.003757 0.619967 0.765214 0.087 Uiso 1 1 calc R U . . .
C31 C 0.8599(3) 0.5982(2) 0.7402(3) 0.0487(9) Uani 1 1 d . . . . .
C32 C 0.7889(2) 0.5548(2) 0.7660(2) 0.0385(7) Uani 1 1 d . . . . .
Cl5 Cl 0.73157(12) 0.24606(8) 0.73579(11) 0.0749(4) Uani 1 1 d . . . . .
O3 O 0.6301(6) 0.2375(5) 0.7227(7) 0.1881(19) Uani 1 1 d . . . . .
O4 O 0.7739(6) 0.1812(5) 0.7371(7) 0.1881(19) Uani 1 1 d . . . . .
O5 O 0.7770(6) 0.2805(5) 0.8207(8) 0.1881(19) Uani 1 1 d . . . . .
O6 O 0.7466(6) 0.3106(5) 0.6966(8) 0.1881(19) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.870(2) . ?
Fe1 O1 1.880(2) . ?
Fe1 N2 1.938(3) . ?
Fe1 N4 1.940(3) . ?
Fe1 N3 1.974(3) . ?
Fe1 N1 1.986(3) . ?
Cl1 C13 1.740(4) . ?
Cl2 C15 1.735(3) . ?
Cl3 C29 1.743(5) . ?
Cl4 C31 1.725(4) . ?
N1 C2 1.333(5) . ?
N1 C1 1.369(4) . ?
N2 C10 1.284(4) . ?
N2 C9 1.421(4) . ?
N3 C18 1.329(4) . ?
N3 C17 1.361(4) . ?
N4 C26 1.290(4) . ?
N4 C25 1.415(4) . ?
O1 C16 1.321(4) . ?
O2 C32 1.308(4) . ?
C1 C9 1.407(5) . ?
C1 C5 1.416(5) . ?
C2 C3 1.399(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.364(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.410(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.408(6) . ?
C6 C7 1.369(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.410(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.367(5) . ?
C8 H8 0.9300 . ?
C10 C11 1.444(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.403(5) . ?
C11 C16 1.413(4) . ?
C12 C13 1.372(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(5) . ?
C14 C15 1.380(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.399(4) . ?
C17 C21 1.415(4) . ?
C17 C25 1.415(5) . ?
C18 C19 1.401(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.353(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.414(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.407(5) . ?
C22 C23 1.378(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.408(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(5) . ?
C24 H24 0.9300 . ?
C26 C27 1.431(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.403(5) . ?
C27 C32 1.406(5) . ?
C28 C29 1.372(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.387(7) . ?
C30 C31 1.369(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.423(5) . ?
Cl5 O4 1.295(9) . ?
Cl5 O6 1.340(9) . ?
Cl5 O5 1.408(11) . ?
Cl5 O3 1.410(8) . ?

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
O2 Fe1 O1 90.79(10) . . ?
O2 Fe1 N2 88.10(11) . . ?
O1 Fe1 N2 92.93(11) . . ?
O2 Fe1 N4 94.25(11) . . ?
O1 Fe1 N4 88.49(11) . . ?
N2 Fe1 N4 177.24(11) . . ?
O2 Fe1 N3 176.39(11) . . ?
O1 Fe1 N3 90.87(10) . . ?
N2 Fe1 N3 95.02(11) . . ?
N4 Fe1 N3 82.58(11) . . ?
O2 Fe1 N1 91.29(11) . . ?
O1 Fe1 N1 174.95(11) . . ?
N2 Fe1 N1 82.54(12) . . ?
N4 Fe1 N1 95.95(12) . . ?
N3 Fe1 N1 87.32(11) . . ?
C2 N1 C1 119.1(3) . . ?
C2 N1 Fe1 128.8(2) . . ?
C1 N1 Fe1 112.0(2) . . ?
C10 N2 C9 121.7(3) . . ?
C10 N2 Fe1 124.5(2) . . ?
C9 N2 Fe1 113.3(2) . . ?
C18 N3 C17 118.9(3) . . ?
C18 N3 Fe1 127.9(2) . . ?
C17 N3 Fe1 113.2(2) . . ?
C26 N4 C25 121.5(3) . . ?
C26 N4 Fe1 124.2(2) . . ?
C25 N4 Fe1 113.9(2) . . ?
C16 O1 Fe1 121.42(19) . . ?
C32 O2 Fe1 122.6(2) . . ?
N1 C1 C9 117.2(3) . . ?
N1 C1 C5 122.1(4) . . ?
C9 C1 C5 120.6(3) . . ?
N1 C2 C3 121.4(4) . . ?
N1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 125.3(4) . . ?
C6 C5 C1 117.6(4) . . ?
C4 C5 C1 117.2(4) . . ?
C7 C6 C5 120.9(4) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 120.9(4) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C1 120.0(3) . . ?
C8 C9 N2 127.3(3) . . ?
C1 C9 N2 112.7(3) . . ?
N2 C10 C11 123.8(3) . . ?
N2 C10 H10 118.1 . . ?
C11 C10 H10 118.1 . . ?
C12 C11 C16 120.6(3) . . ?
C12 C11 C10 117.0(3) . . ?
C16 C11 C10 122.4(3) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 120.6(3) . . ?
C12 C13 Cl1 120.1(3) . . ?
C14 C13 Cl1 119.4(3) . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 122.8(3) . . ?
C14 C15 Cl2 119.0(3) . . ?
C16 C15 Cl2 118.2(3) . . ?
O1 C16 C15 119.0(3) . . ?
O1 C16 C11 124.5(3) . . ?
C15 C16 C11 116.5(3) . . ?
N3 C17 C21 122.0(3) . . ?
N3 C17 C25 116.6(3) . . ?
C21 C17 C25 121.4(3) . . ?
N3 C18 C19 122.1(4) . . ?
N3 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 125.0(3) . . ?
C22 C21 C17 117.7(3) . . ?
C20 C21 C17 117.3(3) . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 121.6(4) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C25 C24 C23 119.4(4) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C17 119.4(3) . . ?
C24 C25 N4 127.4(3) . . ?
C17 C25 N4 113.1(3) . . ?
N4 C26 C27 124.3(3) . . ?
N4 C26 H26 117.9 . . ?
C27 C26 H26 117.9 . . ?
C28 C27 C32 121.1(3) . . ?
C28 C27 C26 115.9(3) . . ?
C32 C27 C26 123.0(3) . . ?
C29 C28 C27 119.1(4) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
C28 C29 C30 121.9(4) . . ?
C28 C29 Cl3 119.2(4) . . ?
C30 C29 Cl3 118.9(4) . . ?
C31 C30 C29 118.7(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 122.2(4) . . ?
C30 C31 Cl4 119.0(3) . . ?
C32 C31 Cl4 118.6(3) . . ?
O2 C32 C27 125.2(3) . . ?
O2 C32 C31 118.0(3) . . ?
C27 C32 C31 116.8(3) . . ?
O4 Cl5 O6 128.6(6) . . ?
O4 Cl5 O5 106.8(6) . . ?
O6 Cl5 O5 87.5(6) . . ?
O4 Cl5 O3 111.3(5) . . ?
O6 Cl5 O3 109.1(5) . . ?
O5 Cl5 O3 109.9(5) . . ?

_refine_diff_density_max         1.920
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.117


# start Validation Reply Form
_vrf_PLAT029_3b293k_sq           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.958 Why?  
RESPONSE: Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.958, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;
# 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_3a(100k)_sq
_database_code_depnum_ccdc_archive 'CCDC 2002660'
loop_
_audit_author_name
_audit_author_address
'Kil Sik Min'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Cl4 Fe N4 O2, Cl O4'
_chemical_formula_sum            'C32 H18 Cl5 Fe N4 O6'
_chemical_formula_weight         787.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0012 '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 0.0047 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0086 0.0047 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1230 0.1262 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3241 0.6814 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.227(3)
_cell_length_b                   17.461(4)
_cell_length_c                   15.213(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.55(3)
_cell_angle_gamma                90
_cell_volume                     3603.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    101373
_cell_measurement_theta_min      0.36
_cell_measurement_theta_max      29.48

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             1588
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.595
_shelx_estimated_absorpt_T_min   0.916
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.630
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37245
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.618
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             9566
_reflns_number_gt                8284
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_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)+(0.0797P)²+9.7345P] 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         9566
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1619
_refine_ls_wR_factor_gt          0.1557
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_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 0.40169(2) 0.54601(2) 0.22336(2) 0.01346(18) Uani 1 1 d . . . . .
Cl1A Cl -0.12242(9) 0.52994(13) 0.08991(17) 0.0632(7) Uani 0.681(2) 1 d . . P A
1
Cl1B Cl -0.1115(2) 0.4916(3) 0.1468(4) 0.0632(7) Uani 0.319(2) 1 d . . P A 1
Cl2 Cl 0.17783(5) 0.67375(4) 0.33837(5) 0.0274(2) Uani 1 1 d . . . . .
Cl3 Cl 0.23709(5) 0.93190(4) 0.16540(5) 0.0264(2) Uani 1 1 d . . . . .
Cl4 Cl 0.17212(5) 0.66504(4) -0.01956(5) 0.0274(2) Uani 1 1 d . . . . .
N1 N 0.50352(15) 0.51575(12) 0.16638(15) 0.0157(4) Uani 1 1 d . . . . .
N2 N 0.32972(16) 0.46222(12) 0.15010(16) 0.0172(4) Uani 1 1 d . . . . .
N3 N 0.47294(15) 0.48290(12) 0.33103(15) 0.0163(4) Uani 1 1 d . . . . .
N4 N 0.48014(15) 0.62711(12) 0.29632(15) 0.0156(4) Uani 1 1 d . . . . .
O1 O 0.30261(13) 0.56876(11) 0.27686(13) 0.0172(4) Uani 1 1 d . . . . .
O2 O 0.34275(13) 0.61168(10) 0.12453(12) 0.0154(4) Uani 1 1 d . . . . .
C1 C 0.47955(19) 0.45044(14) 0.11438(18) 0.0166(5) Uani 1 1 d . . . . .
C2 C 0.58748(19) 0.55063(15) 0.17166(19) 0.0189(5) Uani 1 1 d . . . . .
H2 H 0.603361 0.596471 0.206647 0.023 Uiso 1 1 calc R U . . .
C3 C 0.6543(2) 0.52258(17) 0.1275(2) 0.0230(6) Uani 1 1 d . . . . .
H3 H 0.714044 0.549158 0.133150 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6327(2) 0.45685(16) 0.0766(2) 0.0230(6) Uani 1 1 d . . . . .
H4 H 0.677619 0.437121 0.046990 0.028 Uiso 1 1 calc R U . . .
C5 C 0.5427(2) 0.41849(15) 0.06826(19) 0.0199(5) Uani 1 1 d . . . . .
C6 C 0.5109(2) 0.35151(15) 0.0150(2) 0.0248(6) Uani 1 1 d . . . . .
H6 H 0.551970 0.328421 -0.016506 0.030 Uiso 1 1 calc R U . . .
C7 C 0.4207(2) 0.31995(15) 0.0088(2) 0.0252(6) Uani 1 1 d . . . . .
H7 H 0.400625 0.274803 -0.026767 0.030 Uiso 1 1 calc R U . . .
C8 C 0.3566(2) 0.35286(15) 0.0541(2) 0.0217(5) Uani 1 1 d . . . . .
H8 H 0.294398 0.330220 0.048619 0.026 Uiso 1 1 calc R U . . .
C9 C 0.38593(19) 0.41809(14) 0.10603(18) 0.0179(5) Uani 1 1 d . . . . .
C10 C 0.2359(2) 0.45112(17) 0.1321(3) 0.0306(7) Uani 1 1 d . . . . .
H10 H 0.207034 0.409173 0.093584 0.037 Uiso 1 1 calc R U . . .
C11 C 0.1728(2) 0.4987(2) 0.1670(3) 0.0402(4) Uani 1 1 d . . . . .
C12 C 0.0702(2) 0.4889(2) 0.1247(3) 0.0402(4) Uani 1 1 d . . . . .
H12 H 0.046535 0.451073 0.078474 0.048 Uiso 1 1 calc R U . . .
C13 C 0.0053(2) 0.5349(2) 0.1515(3) 0.0402(4) Uani 1 1 d . . . . .
C14 C 0.0377(2) 0.5907(2) 0.2191(3) 0.0402(4) Uani 1 1 d . . . . .
H14 H -0.008247 0.621637 0.237195 0.048 Uiso 1 1 calc R U . . .
C15 C 0.1379(2) 0.6005(2) 0.2597(3) 0.0402(4) Uani 1 1 d . . . . .
C16 C 0.2096(2) 0.5556(2) 0.2356(3) 0.0402(4) Uani 1 1 d . . . . .
C17 C 0.54909(18) 0.52197(15) 0.39112(18) 0.0183(5) Uani 1 1 d . . . . .
C18 C 0.4584(2) 0.41014(15) 0.3485(2) 0.0212(5) Uani 1 1 d . . . . .
H18 H 0.405733 0.382854 0.306963 0.025 Uiso 1 1 calc R U . . .
C19 C 0.5189(2) 0.37223(17) 0.4270(2) 0.0253(6) Uani 1 1 d . . . . .
H19 H 0.505816 0.320418 0.438415 0.030 Uiso 1 1 calc R U . . .
C20 C 0.5964(2) 0.40992(18) 0.4868(2) 0.0269(6) Uani 1 1 d . . . . .
H20 H 0.637487 0.384411 0.539646 0.032 Uiso 1 1 calc R U . . .
C21 C 0.6148(2) 0.48733(17) 0.4694(2) 0.0224(5) Uani 1 1 d . . . . .
C22 C 0.6947(2) 0.53164(19) 0.5235(2) 0.0269(6) Uani 1 1 d . . . . .
H22 H 0.739170 0.510176 0.577514 0.032 Uiso 1 1 calc R U . . .
C23 C 0.7085(2) 0.60533(19) 0.4985(2) 0.0264(6) Uani 1 1 d . . . . .
H23 H 0.764558 0.633279 0.533555 0.032 Uiso 1 1 calc R U . . .
C24 C 0.64031(19) 0.64034(16) 0.42147(19) 0.0209(5) Uani 1 1 d . . . . .
H24 H 0.650402 0.691490 0.405038 0.025 Uiso 1 1 calc R U . . .
C25 C 0.55947(18) 0.59977(15) 0.37063(17) 0.0171(5) Uani 1 1 d . . . . .
C26 C 0.45835(18) 0.69924(14) 0.28569(18) 0.0169(5) Uani 1 1 d . . . . .
H26 H 0.499145 0.734567 0.327735 0.020 Uiso 1 1 calc R U . . .
C27 C 0.37567(18) 0.72881(14) 0.21363(17) 0.0160(5) Uani 1 1 d . . . . .
C28 C 0.34968(19) 0.80581(14) 0.22105(18) 0.0186(5) Uani 1 1 d . . . . .
H28 H 0.387349 0.836231 0.271080 0.022 Uiso 1 1 calc R U . . .
C29 C 0.26993(19) 0.83695(14) 0.15603(19) 0.0188(5) Uani 1 1 d . . . . .
C30 C 0.2143(2) 0.79375(15) 0.08139(19) 0.0203(5) Uani 1 1 d . . . . .
H30 H 0.158776 0.815545 0.037062 0.024 Uiso 1 1 calc R U . . .
C31 C 0.24108(19) 0.71902(15) 0.07290(18) 0.0180(5) Uani 1 1 d . . . . .
C32 C 0.32179(17) 0.68315(13) 0.13812(17) 0.0144(5) Uani 1 1 d . . . . .
Cl5 Cl 0.26460(7) 0.25421(5) 0.76521(7) 0.0416(3) Uani 1 1 d . . . . .
O3 O 0.3689(2) 0.26247(16) 0.7790(2) 0.0501(8) Uani 1 1 d . . . . .
O4A O 0.2190(4) 0.2350(3) 0.6632(5) 0.0774(10) Uani 0.681(2) 1 d . . P A 2
O5A O 0.2281(4) 0.3215(3) 0.7794(6) 0.0774(10) Uani 0.681(2) 1 d . . P A 2
O6A O 0.2328(4) 0.1789(3) 0.7600(6) 0.0774(10) Uani 0.681(2) 1 d . . P A 2
O4B O 0.2094(9) 0.3124(7) 0.7079(12) 0.0774(10) Uani 0.319(2) 1 d . . P A 3
O5B O 0.2403(9) 0.2684(7) 0.8611(11) 0.0774(10) Uani 0.319(2) 1 d . . P A 3
O6B O 0.2577(9) 0.1942(8) 0.8242(12) 0.0774(10) Uani 0.319(2) 1 d . . P A 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.8706(18) . ?
Fe1 O2 1.8756(18) . ?
Fe1 N4 1.933(2) . ?
Fe1 N2 1.935(2) . ?
Fe1 N1 1.972(2) . ?
Fe1 N3 1.981(2) . ?
Cl1A Cl1B 1.068(6) . ?
Cl1A C13 1.778(4) . ?
Cl1B C13 1.808(5) . ?
Cl2 C15 1.727(3) . ?
Cl3 C29 1.740(3) . ?
Cl4 C31 1.731(3) . ?
N1 C2 1.322(3) . ?
N1 C1 1.371(3) . ?
N2 C10 1.294(4) . ?
N2 C9 1.416(3) . ?
N3 C18 1.327(3) . ?
N3 C17 1.370(3) . ?
N4 C26 1.295(3) . ?
N4 C25 1.418(3) . ?
O1 C16 1.303(4) . ?
O2 C32 1.314(3) . ?
C1 C5 1.411(3) . ?
C1 C9 1.417(4) . ?
C2 C3 1.406(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.417(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.417(4) . ?
C6 C7 1.373(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.419(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(4) . ?
C8 H8 0.9500 . ?
C10 C11 1.437(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.417(4) . ?
C11 C16 1.421(4) . ?
C12 C13 1.374(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(4) . ?
C14 C15 1.382(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.419(4) . ?
C17 C21 1.409(4) . ?
C17 C25 1.411(4) . ?
C18 C19 1.409(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.368(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.417(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.415(4) . ?
C22 C23 1.372(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.415(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.373(4) . ?
C24 H24 0.9500 . ?
C26 C27 1.440(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.408(3) . ?
C27 C32 1.418(3) . ?
C28 C29 1.373(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.394(4) . ?
C30 C31 1.376(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.417(3) . ?
Cl5 O5A 1.328(6) . ?
Cl5 O6A 1.385(6) . ?
Cl5 O6B 1.402(16) . ?
Cl5 O4B 1.412(16) . ?
Cl5 O3 1.442(3) . ?
Cl5 O4A 1.528(7) . ?
Cl5 O5B 1.616(15) . ?
O4A O6A 1.730(11) . ?
O5B O6B 1.462(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O2 90.32(8) . . ?
O1 Fe1 N4 88.57(9) . . ?
O2 Fe1 N4 93.07(9) . . ?
O1 Fe1 N2 94.24(9) . . ?
O2 Fe1 N2 88.25(9) . . ?
N4 Fe1 N2 176.89(9) . . ?
O1 Fe1 N1 176.65(9) . . ?
O2 Fe1 N1 91.23(8) . . ?
N4 Fe1 N1 94.31(9) . . ?
N2 Fe1 N1 82.84(9) . . ?
O1 Fe1 N3 91.33(9) . . ?
O2 Fe1 N3 175.25(9) . . ?
N4 Fe1 N3 82.52(9) . . ?
N2 Fe1 N3 96.06(10) . . ?
N1 Fe1 N3 87.36(9) . . ?
Cl1B Cl1A C13 74.2(3) . . ?
Cl1A Cl1B C13 71.2(3) . . ?
C2 N1 C1 118.8(2) . . ?
C2 N1 Fe1 128.35(19) . . ?
C1 N1 Fe1 112.88(17) . . ?
C10 N2 C9 120.8(2) . . ?
C10 N2 Fe1 124.63(18) . . ?
C9 N2 Fe1 114.07(17) . . ?
C18 N3 C17 118.9(2) . . ?
C18 N3 Fe1 128.8(2) . . ?
C17 N3 Fe1 112.28(17) . . ?
C26 N4 C25 122.0(2) . . ?
C26 N4 Fe1 124.45(18) . . ?
C25 N4 Fe1 113.21(17) . . ?
C16 O1 Fe1 122.85(19) . . ?
C32 O2 Fe1 121.49(16) . . ?
N1 C1 C5 122.1(2) . . ?
N1 C1 C9 116.5(2) . . ?
C5 C1 C9 121.3(2) . . ?
N1 C2 C3 122.6(3) . . ?
N1 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C1 C5 C4 117.6(3) . . ?
C1 C5 C6 118.0(3) . . ?
C4 C5 C6 124.4(2) . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 121.9(3) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 119.1(3) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 N2 127.2(2) . . ?
C8 C9 C1 119.7(2) . . ?
N2 C9 C1 113.0(2) . . ?
N2 C10 C11 123.7(3) . . ?
N2 C10 H10 118.2 . . ?
C11 C10 H10 118.2 . . ?
C12 C11 C16 121.2(3) . . ?
C12 C11 C10 115.8(3) . . ?
C16 C11 C10 122.9(3) . . ?
C13 C12 C11 119.2(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 121.7(3) . . ?
C12 C13 Cl1A 119.1(3) . . ?
C14 C13 Cl1A 118.8(2) . . ?
C12 C13 Cl1B 115.8(3) . . ?
C14 C13 Cl1B 114.7(3) . . ?
Cl1A C13 Cl1B 34.64(18) . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 122.8(3) . . ?
C14 C15 Cl2 118.7(2) . . ?
C16 C15 Cl2 118.4(2) . . ?
O1 C16 C15 118.9(3) . . ?
O1 C16 C11 124.9(3) . . ?
C15 C16 C11 116.2(3) . . ?
N3 C17 C21 122.7(2) . . ?
N3 C17 C25 116.5(2) . . ?
C21 C17 C25 120.8(3) . . ?
N3 C18 C19 121.8(3) . . ?
N3 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C17 C21 C22 117.9(3) . . ?
C17 C21 C20 117.0(3) . . ?
C22 C21 C20 125.0(3) . . ?
C23 C22 C21 120.5(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 121.0(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C17 119.8(2) . . ?
C24 C25 N4 127.3(2) . . ?
C17 C25 N4 112.9(2) . . ?
N4 C26 C27 123.6(2) . . ?
N4 C26 H26 118.2 . . ?
C27 C26 H26 118.2 . . ?
C28 C27 C32 120.7(2) . . ?
C28 C27 C26 117.1(2) . . ?
C32 C27 C26 122.2(2) . . ?
C29 C28 C27 120.0(2) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 121.0(2) . . ?
C28 C29 Cl3 120.2(2) . . ?
C30 C29 Cl3 118.8(2) . . ?
C31 C30 C29 119.0(2) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C30 C31 C32 122.8(2) . . ?
C30 C31 Cl4 119.2(2) . . ?
C32 C31 Cl4 117.99(19) . . ?
O2 C32 C31 119.0(2) . . ?
O2 C32 C27 124.6(2) . . ?
C31 C32 C27 116.4(2) . . ?
O5A Cl5 O6A 135.5(4) . . ?
O6B Cl5 O4B 143.1(7) . . ?
O5A Cl5 O3 108.9(3) . . ?
O6A Cl5 O3 114.0(3) . . ?
O6B Cl5 O3 104.4(5) . . ?
O4B Cl5 O3 111.9(5) . . ?
O5A Cl5 O4A 107.0(4) . . ?
O6A Cl5 O4A 72.7(4) . . ?
O3 Cl5 O4A 105.8(3) . . ?
O6B Cl5 O5B 57.4(7) . . ?
O4B Cl5 O5B 102.5(8) . . ?
O3 Cl5 O5B 110.2(5) . . ?
Cl5 O4A O6A 49.9(3) . . ?
Cl5 O6A O4A 57.5(3) . . ?
O6B O5B Cl5 53.9(8) . . ?
Cl5 O6B O5B 68.7(9) . . ?

_refine_diff_density_max         2.172
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.109


# start Validation Reply Form
_vrf_PLAT029_3a100k_sq           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.954 Why?  
RESPONSE: Since the Pohang Accelerator Laboratory goniostat has only one omega-axis,
diffrn_measured_fraction_theta_full is not fully covered as 0.954, especially
for the low symmetry such as a triclinic system. As this is an inherent
problem, other command and option were not helpful to
improve the completeness.
;
# end Validation Reply Form

