# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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. 
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data_kai316a_6mcppcation_ch2cl2_auto
_database_code_depnum_ccdc_archive 'CCDC 2359239'
loop_
_audit_author_name
_audit_author_address
'Akiko Yagi'
;University
Japan
;
_audit_update_record             
;
2024-05-30 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2023-10-16
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2018.12.05 svn.r3537 for Rigaku Oxford Diffraction, GUI svn.r5625)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(F6 Sb), 5(C H2 Cl2), C42 H24'
_chemical_formula_sum            'C47 H34 Cl10 F12 Sb2'
_chemical_formula_weight         1424.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H Sb F Cl '
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0560(3)
_cell_length_b                   12.0361(2)
_cell_length_c                   12.1017(3)
_cell_angle_alpha                105.769(2)
_cell_angle_beta                 104.054(2)
_cell_angle_gamma                116.448(2)
_cell_volume                     1257.78(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    15461
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1280
_cell_measurement_theta_min      2.0660
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.751
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19722
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.921
_diffrn_reflns_theta_min         1.929
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  13.00   0.50   10.00    --    3.32 -62.00 -16.00  160
  2  ω     27.00  72.00   0.50   10.00    --    3.32  62.00 122.00   90
  3  ω    -19.00  30.00   0.50   10.00    --   -2.70  57.00-120.00   98
  4  ω    -17.00  77.00   0.50   10.00    --   -2.70  19.00 120.00  188
  5  ω     -6.00  38.00   0.50   10.00    --    3.32 -99.00-120.00   88
  6  ω    -11.00  14.00   0.50   10.00    --    3.32 -99.00 120.00   50
  7  ω    -12.00  37.00   0.50   10.00    --    3.32 -99.00 -30.00   98
  8  ω    -11.00  36.00   0.50   10.00    --    3.32 -99.00  60.00   94
  9  ω      8.00  33.00   0.50   10.00    --    3.32 -99.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0651557000
_diffrn_orient_matrix_UB_12      -0.0016870000
_diffrn_orient_matrix_UB_13      -0.0290724000
_diffrn_orient_matrix_UB_21      -0.0377379000
_diffrn_orient_matrix_UB_22      -0.0716765000
_diffrn_orient_matrix_UB_23      -0.0388761000
_diffrn_orient_matrix_UB_31      -0.0240735000
_diffrn_orient_matrix_UB_32      -0.0147319000
_diffrn_orient_matrix_UB_33      0.0464526000
_diffrn_oxdiff_digest_frames     
;
010980833ad92e22a1943d2d3712b2691500025b6e8
;
_diffrn_oxdiff_digest_hkl        
;
010cb771c33b3ba8a5aff1190c4d191e8df3ce
;
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5528
_reflns_number_total             5972
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+1.2796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl33-C32 = Cl34-C32
 1.76 with sigma of 0.01
3. Others
 Fixed Sof: Cl34(0.5) Cl33(0.5) C32(0.5) H2A(0.5) H2B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H00A,H00B), C1(H00C,H00D), C16(H00E,H00F), C35(H00G,H00K), C29(H01A,H01B),
 C32(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H00H), C4(H00I), C8(H00J), C11(H00N), C21(H00Q), C14(H00R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Sb22 Sb -0.06458(2) 0.63986(2) 0.20371(2) 0.01619(5) Uani 1 1 d . . . . .
Cl37 Cl -0.31988(7) 0.63107(6) 0.53999(6) 0.02940(12) Uani 1 1 d . . . . .
Cl36 Cl -0.17391(7) 0.90662(6) 0.54982(6) 0.03185(13) Uani 1 1 d . . . . .
Cl31 Cl -0.49088(9) 0.34353(9) -0.16062(8) 0.04907(18) Uani 1 1 d . . . . .
Cl30 Cl -0.35391(11) 0.36767(11) -0.33629(7) 0.0624(2) Uani 1 1 d . . . . .
F23 F -0.10858(16) 0.65428(14) 0.05048(12) 0.0289(3) Uani 1 1 d . . . . .
F24 F -0.02034(17) 0.62762(15) 0.35812(13) 0.0336(3) Uani 1 1 d . . . . .
F27 F 0.13615(17) 0.77593(18) 0.25874(17) 0.0475(5) Uani 1 1 d . . . . .
F26 F -0.0336(3) 0.50287(19) 0.13489(18) 0.0560(5) Uani 1 1 d . . . . .
F25 F -0.0968(3) 0.7776(2) 0.27184(17) 0.0544(5) Uani 1 1 d . . . . .
F28 F -0.26372(18) 0.5075(2) 0.15274(19) 0.0611(6) Uani 1 1 d . . . . .
C7 C 0.4920(2) 0.7126(2) 0.72443(19) 0.0162(4) Uani 1 1 d . . . . .
C2 C 0.9176(2) 1.0940(2) 1.04606(19) 0.0155(4) Uani 1 1 d . . . . .
C19 C 0.6015(2) 0.8438(2) 0.73709(19) 0.0160(4) Uani 1 1 d . . . . .
C18 C 0.5601(2) 0.9123(2) 0.67312(18) 0.0164(4) Uani 1 1 d . . . . .
H00H H 0.632254 0.988934 0.667047 0.020 Uiso 1 1 calc R . . . .
C4 C 0.7781(2) 0.8589(2) 1.0338(2) 0.0171(4) Uani 1 1 d . . . . .
H00I H 0.764609 0.798111 1.072662 0.021 Uiso 1 1 calc R . . . .
C8 C 0.3431(2) 0.6605(2) 0.66724(18) 0.0168(4) Uani 1 1 d . . . . .
H00J H 0.269541 0.571898 0.654909 0.020 Uiso 1 1 calc R . . . .
C15 C 0.2197(2) 0.8901(2) 0.63163(18) 0.0169(4) Uani 1 1 d . . . . .
C5 C 0.7069(2) 0.8104(2) 0.9054(2) 0.0163(4) Uani 1 1 d . . . . .
C3 C 0.8726(2) 1.0037(2) 1.10554(19) 0.0157(4) Uani 1 1 d . . . . .
C11 C 0.0846(2) 0.6969(2) 0.68378(18) 0.0165(4) Uani 1 1 d . . . . .
H00N H 0.043185 0.603071 0.668048 0.020 Uiso 1 1 calc R . . . .
C20 C 0.7335(2) 0.9036(2) 0.84806(19) 0.0156(4) Uani 1 1 d . . . . .
C12 C 0.0498(2) 0.7774(2) 0.75499(18) 0.0157(4) Uani 1 1 d . . . . .
C21 C 0.8512(2) 1.0445(2) 0.91730(19) 0.0160(4) Uani 1 1 d . . . . .
H00Q H 0.882671 1.102015 0.876284 0.019 Uiso 1 1 calc R . . . .
C14 C 0.1777(2) 0.9672(2) 0.69700(19) 0.0182(4) Uani 1 1 d . . . . .
H00R H 0.194870 1.050244 0.692717 0.022 Uiso 1 1 calc R . . . .
C9 C 0.3039(2) 0.7445(2) 0.62737(17) 0.0157(4) Uani 1 1 d . . . . .
C13 C 0.1070(2) 0.9167(2) 0.77153(19) 0.0161(4) Uani 1 1 d . . . . .
C6 C 0.5664(2) 0.6711(2) 0.8121(2) 0.0181(4) Uani 1 1 d . . . . .
H00A H 0.589308 0.606381 0.767002 0.022 Uiso 1 1 calc R . . . .
H00B H 0.504736 0.629156 0.854199 0.022 Uiso 1 1 calc R . . . .
C17 C 0.4118(2) 0.8633(2) 0.62031(18) 0.0163(4) Uani 1 1 d . . . . .
C10 C 0.1859(2) 0.7614(2) 0.63473(17) 0.0159(4) Uani 1 1 d . . . . .
C1 C 1.0053(2) 1.2427(2) 1.14475(19) 0.0172(4) Uani 1 1 d . . . . .
H00C H 1.114094 1.284173 1.176685 0.021 Uiso 1 1 calc R . . . .
H00D H 0.980141 1.300025 1.111751 0.021 Uiso 1 1 calc R . . . .
C16 C 0.3407(2) 0.9381(2) 0.58514(19) 0.0185(4) Uani 1 1 d . . . . .
H00E H 0.298728 0.908753 0.492629 0.022 Uiso 1 1 calc R . . . .
H00F H 0.411793 1.039546 0.629828 0.022 Uiso 1 1 calc R . . . .
C35 C -0.2253(3) 0.7352(3) 0.4728(2) 0.0275(5) Uani 1 1 d . . . . .
H00G H -0.134799 0.734425 0.478593 0.033 Uiso 1 1 calc R . . . .
H00K H -0.290514 0.695964 0.381967 0.033 Uiso 1 1 calc R . . . .
C29 C -0.3367(3) 0.3604(3) -0.1911(3) 0.0394(6) Uani 1 1 d . . . . .
H01A H -0.243895 0.445443 -0.122311 0.047 Uiso 1 1 calc R . . . .
H01B H -0.329716 0.280817 -0.192590 0.047 Uiso 1 1 calc R . . . .
Cl34 Cl -0.3876(2) 0.15226(19) 0.01577(18) 0.0572(4) Uani 0.5 1 d D . P A -1
Cl33 Cl -0.5267(3) -0.1060(3) 0.0418(2) 0.0619(5) Uani 0.5 1 d D . P A -1
C32 C -0.5427(6) -0.0122(6) -0.0409(6) 0.0487(15) Uani 0.5 1 d D . P A -1
H2A H -0.566404 -0.064993 -0.130129 0.058 Uiso 0.5 1 calc R . P A -1
H2B H -0.628216 -0.004669 -0.040422 0.058 Uiso 0.5 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb22 F23 1.8756(12) . ?
Sb22 F24 1.8768(13) . ?
Sb22 F27 1.8716(15) . ?
Sb22 F26 1.8509(16) . ?
Sb22 F25 1.8656(16) . ?
Sb22 F28 1.8568(16) . ?
Cl37 C35 1.768(2) . ?
Cl36 C35 1.762(3) . ?
Cl31 C29 1.767(3) . ?
Cl30 C29 1.751(3) . ?
C7 C19 1.435(3) . ?
C7 C8 1.369(3) . ?
C7 C6 1.511(3) . ?
C2 C3 1.437(3) . ?
C2 C21 1.368(3) . ?
C2 C1 1.516(3) . ?
C19 C18 1.413(3) . ?
C19 C20 1.428(3) . ?
C18 C17 1.368(3) . ?
C4 C5 1.371(3) . ?
C4 C3 1.414(3) . ?
C8 C9 1.413(3) . ?
C15 C14 1.367(3) . ?
C15 C10 1.436(3) . ?
C15 C16 1.514(3) . ?
C5 C20 1.434(3) . ?
C5 C6 1.516(3) . ?
C3 C13 1.433(3) 2_677 ?
C11 C12 1.367(3) . ?
C11 C10 1.417(3) . ?
C20 C21 1.416(3) . ?
C12 C13 1.436(3) . ?
C12 C1 1.513(3) 2_677 ?
C14 C13 1.418(3) . ?
C9 C17 1.440(3) . ?
C9 C10 1.426(3) . ?
C17 C16 1.512(3) . ?
Cl34 C32 1.731(6) . ?
Cl33 C32 1.736(5) . ?

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
F23 Sb22 F24 179.25(6) . . ?
F27 Sb22 F23 89.59(7) . . ?
F27 Sb22 F24 90.22(7) . . ?
F26 Sb22 F23 90.46(7) . . ?
F26 Sb22 F24 90.27(8) . . ?
F26 Sb22 F27 90.86(10) . . ?
F26 Sb22 F25 179.56(9) . . ?
F26 Sb22 F28 90.32(11) . . ?
F25 Sb22 F23 89.15(7) . . ?
F25 Sb22 F24 90.12(7) . . ?
F25 Sb22 F27 89.33(10) . . ?
F28 Sb22 F23 91.22(7) . . ?
F28 Sb22 F24 88.95(7) . . ?
F28 Sb22 F27 178.56(9) . . ?
F28 Sb22 F25 89.49(11) . . ?
C19 C7 C6 109.33(18) . . ?
C8 C7 C19 120.77(19) . . ?
C8 C7 C6 127.63(18) . . ?
C3 C2 C1 109.41(17) . . ?
C21 C2 C3 120.58(19) . . ?
C21 C2 C1 127.59(18) . . ?
C18 C19 C7 121.17(19) . . ?
C18 C19 C20 127.52(18) . . ?
C20 C19 C7 108.16(18) . . ?
C17 C18 C19 117.13(18) . . ?
C5 C4 C3 116.77(18) . . ?
C7 C8 C9 116.94(18) . . ?
C14 C15 C10 120.63(18) . . ?
C14 C15 C16 127.71(19) . . ?
C10 C15 C16 108.94(18) . . ?
C4 C5 C20 120.70(19) . . ?
C4 C5 C6 127.84(18) . . ?
C20 C5 C6 109.15(18) . . ?
C4 C3 C2 121.44(18) . . ?
C4 C3 C13 127.05(18) . 2_677 ?
C13 C3 C2 107.87(18) 2_677 . ?
C12 C11 C10 116.27(18) . . ?
C19 C20 C5 108.29(18) . . ?
C21 C20 C19 127.19(19) . . ?
C21 C20 C5 121.34(19) . . ?
C11 C12 C13 120.89(18) . . ?
C11 C12 C1 127.04(18) . 2_677 ?
C13 C12 C1 109.39(17) . 2_677 ?
C2 C21 C20 116.89(18) . . ?
C15 C14 C13 116.53(19) . . ?
C8 C9 C17 121.11(19) . . ?
C8 C9 C10 127.04(18) . . ?
C10 C9 C17 107.93(18) . . ?
C3 C13 C12 108.08(17) 2_677 . ?
C14 C13 C3 127.00(19) . 2_677 ?
C14 C13 C12 121.25(18) . . ?
C7 C6 C5 100.38(16) . . ?
C18 C17 C9 120.52(19) . . ?
C18 C17 C16 128.21(18) . . ?
C9 C17 C16 108.85(17) . . ?
C11 C10 C15 121.50(18) . . ?
C11 C10 C9 126.61(18) . . ?
C9 C10 C15 108.02(17) . . ?
C12 C1 C2 99.94(16) 2_677 . ?
C17 C16 C15 99.76(16) . . ?
Cl36 C35 Cl37 111.80(12) . . ?
Cl30 C29 Cl31 110.97(16) . . ?
Cl34 C32 Cl33 115.9(3) . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.720
_oxdiff_exptl_absorpt_empirical_full_min 0.608
