# Supplementary Information (SI) 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_2223k_0m
_database_code_depnum_ccdc_archive 'CCDC 2370447'
loop_
_audit_author_name
_audit_author_address
'jian chen'
;SOUTH EAST UNIVERSITY
China
;
_audit_update_record             
;
2024-07-13 deposited with the CCDC.	2024-08-29 downloaded from the CCDC.
;
_audit_creation_date             2024-06-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H19 Br N, Cl4 Fe'
_chemical_formula_sum            'C8 H19 Br Cl4 Fe N'
_chemical_formula_weight         406.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   7.5437(4)
_cell_length_b                   11.5570(5)
_cell_length_c                   18.4337(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.388(2)
_cell_angle_gamma                90
_cell_volume                     1605.70(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3069
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.888
_shelx_estimated_absorpt_T_min   0.737
_exptl_absorpt_coefficient_mu    4.067
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3167
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1207 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.4249.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12360
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         2.080
_diffrn_ambient_temperature      223.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  bruker
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2127
_reflns_number_total             3280
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.686
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0090(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0786P)²+2.7888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1732
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C7(H7A,H7B), C5(H5A,H5B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.16065(10) 0.44254(6) 0.13966(6) 0.0875(4) Uani 1 1 d . . . . .
N1 N 0.1560(5) 0.7395(3) 0.1121(2) 0.0351(10) Uani 1 1 d . . . . .
C3 C 0.0365(7) 0.8342(5) 0.1400(3) 0.0415(13) Uani 1 1 d . . . . .
H3A H -0.008155 0.809123 0.186635 0.050 Uiso 1 1 calc R U . . .
H3B H 0.108641 0.903574 0.149171 0.050 Uiso 1 1 calc R U . . .
C1 C 0.0531(7) 0.6287(5) 0.0996(3) 0.0449(14) Uani 1 1 d . . . . .
H1A H -0.039702 0.642369 0.061772 0.054 Uiso 1 1 calc R U . . .
H1B H 0.133487 0.569831 0.081370 0.054 Uiso 1 1 calc R U . . .
C7 C 0.3061(7) 0.7231(5) 0.1689(3) 0.0441(13) Uani 1 1 d . . . . .
H7A H 0.361535 0.798456 0.178755 0.053 Uiso 1 1 calc R U . . .
H7B H 0.255217 0.696456 0.214007 0.053 Uiso 1 1 calc R U . . .
C8 C 0.4465(8) 0.6400(5) 0.1487(3) 0.0499(15) Uani 1 1 d . . . . .
H8A H 0.510520 0.671100 0.108520 0.075 Uiso 1 1 calc R U . . .
H8B H 0.392291 0.566882 0.134394 0.075 Uiso 1 1 calc R U . . .
H8C H 0.528217 0.627710 0.190010 0.075 Uiso 1 1 calc R U . . .
C5 C 0.2294(8) 0.7736(5) 0.0394(3) 0.0483(14) Uani 1 1 d . . . . .
H5A H 0.304297 0.710616 0.022556 0.058 Uiso 1 1 calc R U . . .
H5B H 0.130149 0.782771 0.003804 0.058 Uiso 1 1 calc R U . . .
C4 C -0.1198(8) 0.8669(5) 0.0908(3) 0.0508(15) Uani 1 1 d . . . . .
H4A H -0.077947 0.894125 0.044737 0.076 Uiso 1 1 calc R U . . .
H4B H -0.186876 0.927784 0.113270 0.076 Uiso 1 1 calc R U . . .
H4C H -0.195309 0.799814 0.082548 0.076 Uiso 1 1 calc R U . . .
C6 C 0.3364(11) 0.8838(6) 0.0417(4) 0.072(2) Uani 1 1 d . . . . .
H6A H 0.386722 0.896700 -0.005192 0.108 Uiso 1 1 calc R U . . .
H6B H 0.431267 0.877318 0.078661 0.108 Uiso 1 1 calc R U . . .
H6C H 0.260176 0.948289 0.053153 0.108 Uiso 1 1 calc R U . . .
C2 C -0.0321(10) 0.5818(6) 0.1660(4) 0.0648(19) Uani 1 1 d . . . . .
H2A H -0.113428 0.639379 0.184990 0.078 Uiso 1 1 calc R U . . .
H2B H 0.059138 0.564602 0.203839 0.078 Uiso 1 1 calc R U . . .
Fe1 Fe 0.31781(11) 0.25090(7) 0.13945(4) 0.0427(3) Uani 1 1 d . . . . .
Cl3 Cl 0.3393(2) 0.35739(12) 0.04049(7) 0.0480(4) Uani 1 1 d . . . . .
Cl4 Cl 0.3169(2) 0.36372(12) 0.23538(7) 0.0480(4) Uani 1 1 d . . . . .
Cl1 Cl 0.0709(2) 0.14855(12) 0.13276(10) 0.0607(5) Uani 1 1 d . . . . .
Cl2 Cl 0.5478(3) 0.13419(17) 0.15057(9) 0.0765(6) 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
Br1 C2 1.930(6) . ?
N1 C3 1.522(6) . ?
N1 C1 1.510(7) . ?
N1 C7 1.522(7) . ?
N1 C5 1.523(7) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.506(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 C2 1.507(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 C8 1.489(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 C6 1.508(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
Fe1 Cl3 2.2121(16) . ?
Fe1 Cl4 2.1972(15) . ?
Fe1 Cl1 2.2054(18) . ?
Fe1 Cl2 2.2001(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
C3 N1 C5 110.7(4) . . ?
C1 N1 C3 110.7(4) . . ?
C1 N1 C7 111.3(4) . . ?
C1 N1 C5 106.8(4) . . ?
C7 N1 C3 106.9(4) . . ?
C7 N1 C5 110.5(4) . . ?
N1 C3 H3A 108.3 . . ?
N1 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 N1 115.9(4) . . ?
C4 C3 H3A 108.3 . . ?
C4 C3 H3B 108.3 . . ?
N1 C1 H1A 108.6 . . ?
N1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 N1 114.6(5) . . ?
C2 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
N1 C7 H7A 108.5 . . ?
N1 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 N1 115.1(5) . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C5 H5A 108.7 . . ?
N1 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C6 C5 N1 114.1(5) . . ?
C6 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Br1 C2 H2A 109.9 . . ?
Br1 C2 H2B 109.9 . . ?
C1 C2 Br1 108.8(5) . . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
Cl4 Fe1 Cl3 109.65(6) . . ?
Cl4 Fe1 Cl1 109.42(7) . . ?
Cl4 Fe1 Cl2 108.52(7) . . ?
Cl1 Fe1 Cl3 110.06(7) . . ?
Cl2 Fe1 Cl3 109.47(7) . . ?
Cl2 Fe1 Cl1 109.70(8) . . ?

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
N1 C1 C2 Br1 179.0(4) . . . . ?
C3 N1 C1 C2 -58.7(6) . . . . ?
C3 N1 C7 C8 -175.2(5) . . . . ?
C3 N1 C5 C6 59.2(7) . . . . ?
C1 N1 C3 C4 -60.2(6) . . . . ?
C1 N1 C7 C8 63.8(6) . . . . ?
C1 N1 C5 C6 179.8(5) . . . . ?
C7 N1 C3 C4 178.5(5) . . . . ?
C7 N1 C1 C2 60.0(6) . . . . ?
C7 N1 C5 C6 -59.0(6) . . . . ?
C5 N1 C3 C4 58.0(6) . . . . ?
C5 N1 C1 C2 -179.3(5) . . . . ?
C5 N1 C7 C8 -54.7(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
