# Supplementary Information (SI) for ChemComm.
# 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. 
# 
#######################################################################

data_hyh-2_sq
_database_code_depnum_ccdc_archive 'CCDC 2417620'
loop_
_audit_author_name
_audit_author_address
'Lixuan Cai'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-01-21 deposited with the CCDC.	2025-04-25 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         ?
_chemical_formula_sum            'C198 H180 F0 N48 P0 Pd6'
_chemical_formula_weight         3870.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.0375 3.1039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'

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

_cell_length_a                   25.0141(9)
_cell_length_b                   25.0141(9)
_cell_length_c                   60.039(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     32534(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    275(2)
_cell_measurement_reflns_used    5795
_cell_measurement_theta_min      1.8040
_cell_measurement_theta_max      34.1580

_exptl_crystal_description       rodlike
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.395
_exptl_crystal_F_000             3960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.986
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      275(2)
_diffrn_radiation_wavelength     1.3405
_diffrn_radiation_type           GaK\a
_diffrn_source                   'micro-focus metaljet'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30958
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         1.773
_diffrn_reflns_theta_max         35.644
_diffrn_reflns_theta_full        35.644
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             4078
_reflns_number_gt                1753
_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       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.2000P)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         4078
_refine_ls_number_parameters     193
_refine_ls_number_restraints     172
_refine_ls_R_factor_all          0.1867
_refine_ls_R_factor_gt           0.1249
_refine_ls_wR_factor_ref         0.4294
_refine_ls_wR_factor_gt          0.3844
_refine_ls_goodness_of_fit_ref   1.379
_refine_ls_restrained_S_all      1.401
_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
Pd01 Pd 0.67920(8) 0.83960(4) 0.52308(4) 0.2684(15) Uani 1 2 d S T P . .
N1 N 0.6274(4) 0.7539(3) 0.5086(2) 0.231(5) Uani 1 1 d G U . . .
C2 C 0.6463(3) 0.7347(5) 0.4900(2) 0.268(8) Uani 1 1 d G U . . .
H2 H 0.684398 0.760964 0.483500 0.322 Uiso 1 1 calc R U . . .
C3 C 0.6084(5) 0.6764(5) 0.48108(15) 0.251(6) Uani 1 1 d G U . . .
H3 H 0.621043 0.663600 0.468611 0.301 Uiso 1 1 calc R U . . .
C4 C 0.5515(4) 0.6372(3) 0.49079(19) 0.224(6) Uani 1 1 d DG U . . .
C5 C 0.5325(3) 0.6563(4) 0.50942(18) 0.224(6) Uani 1 1 d G U . . .
H5 H 0.494424 0.630109 0.515918 0.268 Uiso 1 1 calc R U . . .
C6 C 0.5705(5) 0.7147(5) 0.51834(14) 0.246(6) Uani 1 1 d G U . . .
H6 H 0.557777 0.727472 0.530807 0.295 Uiso 1 1 calc R U . . .
C7 C 0.5133(5) 0.5768(5) 0.4832(2) 0.202(6) Uani 1 1 d D U . . .
N8 N 0.5359(5) 0.5568(5) 0.46724(19) 0.196(5) Uani 1 1 d D . . . .
C9 C 0.5017(4) 0.4983(4) 0.4600(3) 0.197(8) Uani 1 2 d DS TU P . .
N10 N 0.4577(3) 0.5423(3) 0.4914(3) 0.210(7) Uani 1 2 d DS T P . .
C11 C 0.5254(5) 0.4746(5) 0.4449(4) 0.238(11) Uani 1 2 d DS TU P . .
N12 N 0.7304(6) 0.9198(6) 0.5381(3) 0.346(7) Uani 1 1 d . U . . .
H12A H 0.754161 0.948063 0.528089 0.415 Uiso 1 1 calc R U . . .
H12B H 0.706111 0.932113 0.544343 0.415 Uiso 1 1 calc R U . . .
C12 C 0.5867(6) 0.5060(6) 0.4367(3) 0.251(7) Uani 1 1 d D U . . .
H12 H 0.610674 0.547342 0.440668 0.302 Uiso 1 1 calc R U . . .
C13 C 0.6124(7) 0.4844(7) 0.4246(3) 0.280(8) Uani 1 1 d D U . . .
H13 H 0.653032 0.509498 0.420066 0.336 Uiso 1 1 calc R U . . .
N14 N 0.5790(4) 0.4210(4) 0.4179(4) 0.295(10) Uani 1 2 d DS TU P . .
C14 C 0.6087(4) 0.3913(4) 0.4066(4) 0.302(7) Uani 1 2 d DS TU P . .
H14A H 0.588966 0.348325 0.411141 0.362 Uiso 0.5 1 calc R U P . .
H14B H 0.651675 0.411034 0.411141 0.362 Uiso 0.5 1 calc R U P . .
C15 C 0.6050(4) 0.3950(4) 0.3800(4) 0.316(7) Uani 1 2 d DS TU P . .
C16 C 0.6503(6) 0.4446(6) 0.3678(3) 0.354(8) Uani 1 1 d D U . . .
H16 H 0.682687 0.477411 0.375278 0.425 Uiso 1 1 calc R U . . .
C17 C 0.6475(7) 0.4455(7) 0.3452(3) 0.381(10) Uani 1 1 d D U . . .
H17 H 0.677614 0.480191 0.337741 0.457 Uiso 1 1 calc R U . . .
C18 C 0.6023(5) 0.3977(5) 0.3325(3) 0.472(12) Uani 1 2 d DS TU P . .
C19 C 0.6017(4) 0.3983(4) 0.3082(2) 0.487(11) Uani 1 2 d DS TU P . .
C20 C 0.6498(5) 0.4454(6) 0.29640(18) 0.511(10) Uani 1 1 d D U . . .
H20 H 0.685358 0.474116 0.303815 0.614 Uiso 1 1 calc R U . . .
C21 C 0.6450(6) 0.4498(6) 0.27344(13) 0.493(10) Uani 1 1 d D U . . .
H21 H 0.672228 0.485981 0.266036 0.592 Uiso 1 1 calc DR U . . .
C22 C 0.5997(8) 0.4003(8) 0.26164(13) 0.458(11) Uani 1 2 d DS TU P . .
C23 C 0.7685(8) 0.9146(5) 0.5548(3) 0.371(8) Uani 1 1 d D U . . .
H23A H 0.754703 0.920031 0.569310 0.445 Uiso 1 1 calc R U . . .
H23B H 0.810546 0.947953 0.552782 0.445 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
Pd01 N12 1.977(13) . ?
Pd01 N12 1.977(13) 21_565 ?
Pd01 N1 2.062(7) . ?
Pd01 N1 2.062(7) 21_565 ?
N1 C2 1.3900 . ?
N1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2 0.9300 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 C7 1.400(11) . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 N10 1.310(10) . ?
C7 N8 1.331(10) . ?
N8 C9 1.346(11) . ?
C9 C11 1.369(15) . ?
C11 C12 1.417(12) 19_665 ?
C11 C12 1.417(12) . ?
N12 C23 1.434(15) . ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
C12 C13 1.255(16) . ?
C12 H12 0.9300 . ?
C13 N14 1.432(14) . ?
C13 H13 0.9300 . ?
N14 C14 1.454(16) . ?
C14 C15 1.61(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.396(10) 19_665 ?
C15 C16 1.396(10) . ?
C16 C17 1.363(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.392(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.456(16) . ?
C19 C20 1.386(9) 19_665 ?
C19 C20 1.386(9) . ?
C20 C21 1.393(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.384(9) . ?
C21 H21 0.9300 . ?
C22 C22 1.398(16) 10_665 ?
C23 C23 1.519(17) 21_565 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N12 Pd01 N12 87.4(8) . 21_565 ?
N12 Pd01 N1 177.0(5) . . ?
N12 Pd01 N1 89.8(5) 21_565 . ?
N12 Pd01 N1 89.8(4) . 21_565 ?
N12 Pd01 N1 177.0(5) 21_565 21_565 ?
N1 Pd01 N1 93.0(4) . 21_565 ?
C2 N1 C6 120.0 . . ?
C2 N1 Pd01 123.5(7) . . ?
C6 N1 Pd01 116.5(7) . . ?
N1 C2 C3 120.0 . . ?
N1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C7 117.9(10) . . ?
C3 C4 C7 122.0(9) . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 N1 120.0 . . ?
C5 C6 H6 120.0 . . ?
N1 C6 H6 120.0 . . ?
N10 C7 N8 122.1(11) . . ?
N10 C7 C4 121.0(11) . . ?
N8 C7 C4 116.8(10) . . ?
C7 N8 C9 118.9(12) . . ?
N8 C9 N8 118.9(16) . 19_665 ?
N8 C9 C11 120.5(8) . . ?
N8 C9 C11 120.5(8) 19_665 . ?
C7 N10 C7 118.5(15) 19_665 . ?
C9 C11 C12 124.9(10) . 19_665 ?
C9 C11 C12 124.9(10) . . ?
C12 C11 C12 109.9(19) 19_665 . ?
C23 N12 Pd01 110.4(10) . . ?
C23 N12 H12A 109.6 . . ?
Pd01 N12 H12A 109.6 . . ?
C23 N12 H12B 109.6 . . ?
Pd01 N12 H12B 109.6 . . ?
H12A N12 H12B 108.1 . . ?
C13 C12 C11 127.3(15) . . ?
C13 C12 H12 116.4 . . ?
C11 C12 H12 116.4 . . ?
C12 C13 N14 120.0(16) . . ?
C12 C13 H13 120.0 . . ?
N14 C13 H13 120.0 . . ?
C13 N14 C13 115.4(19) . 19_665 ?
C13 N14 C14 122.2(9) . . ?
C13 N14 C14 122.2(9) 19_665 . ?
N14 C14 C15 111.9(19) . . ?
N14 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
N14 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C16 117(2) 19_665 . ?
C16 C15 C14 121.7(10) 19_665 . ?
C16 C15 C14 121.7(10) . . ?
C17 C16 C15 120.7(15) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 124.0(14) . . ?
C16 C17 H17 118.0 . . ?
C18 C17 H17 118.0 . . ?
C17 C18 C17 113.4(18) . 19_665 ?
C17 C18 C19 123.2(9) . . ?
C17 C18 C19 123.2(9) 19_665 . ?
C20 C19 C20 118.5(8) 19_665 . ?
C20 C19 C18 120.7(4) 19_665 . ?
C20 C19 C18 120.7(4) . . ?
C19 C20 C21 120.0(6) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.1(7) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C21 117.8(8) . 19_665 ?
C21 C22 C22 120.8(3) . 10_665 ?
C21 C22 C22 120.8(3) 19_665 10_665 ?
N12 C23 C23 115.0(7) . 21_565 ?
N12 C23 H23A 108.5 . . ?
C23 C23 H23A 108.5 21_565 . ?
N12 C23 H23B 108.5 . . ?
C23 C23 H23B 108.5 21_565 . ?
H23A C23 H23B 107.5 . . ?

_refine_diff_density_max         0.598
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.061



# start Validation Reply Form
_vrf_THETM01_hyh-2_sq            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals of this giant supramolecular assembly is very 
poorly diffracting,  possibly due to a large amount of amorphous solvents 
and highly-disordered counterions existing in the unit cell, which occupy 
  as much as 77.7% of the unit cell based on PLATON calculation.
;
_vrf_PLAT084_hyh-2_sq            
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.45 Report
RESPONSE: As stated above, the high R2 value is due to the poor diffraction 
ability of such cage complex and the existence of a large amount of amorphous 
solents and counter anions.
;
_vrf_PLAT260_hyh-2_sq            
;
PROBLEM: Large Average Ueq of Residue Including Pd01 0.311 Check 
RESPONSE: This alert is due to the poor diffraction quality of the crystals and 
some disordered counterions.
;
# end Validation Reply Form
