Wide variability in the stability of Pd<sub>6</sub>L<sub><i>x</i></sub>-type coordination cages.
de Montmollin, Jean; Fadaei-Tirani, Farzaneh; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15773–15779; doi:10.1039/d5dt02223a

data_7719637
_publ_section_title
;
 Wide variability in the stability of
 Pd<sub>6</sub>L<sub><i>x</i></sub>-type coordination cages.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15773
_journal_page_last               15779
_journal_paper_doi               10.1039/d5dt02223a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C192 H158 N64 Pd8'
_chemical_formula_sum            'C192 H158 N64 Pd8'
_chemical_formula_weight         4213.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-08-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-12 deposited with the CCDC.	2025-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                96.6247(9)
_cell_angle_beta                 94.5683(9)
_cell_angle_gamma                112.7005(10)
_cell_formula_units_Z            2
_cell_length_a                   24.8049(3)
_cell_length_b                   27.3216(3)
_cell_length_c                   29.8355(3)
_cell_measurement_reflns_used    66731
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      48.3910
_cell_measurement_theta_min      1.8090
_cell_volume                     18358.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -7.00  29.00   0.50    5.00    --   29.66 -97.00-137.00   72
  2  \w     -7.00  18.00   0.50    5.00    --   30.82 -97.00-137.00   50
  3  \w    -28.00   6.00   0.50    5.00    --  -31.33  97.00 -29.00   68
  4  \w     -9.00  21.00   0.50    5.00    --    2.00 100.00-159.25   60
  5  \w    -11.00  30.00   0.50    5.00    --   -6.00  90.00 133.66   82
  6  \w     -4.00  22.00   0.50    5.00    --    6.00 100.00 -72.90   52
  7  \w     -4.00  21.00   0.50    5.00    --    6.00  99.00 -11.64   50
  8  \w    -23.00   2.00   0.50    5.00    --  -10.00 103.00 -63.01   50
  9  \w    -46.00 -21.00   0.50    5.00    --  -10.00 139.00 -34.37   50
 10  \w    -14.00  13.00   0.50    5.00    --  -10.00 102.00  43.29   54
 11  \w      6.00  34.00   0.50    5.00    --   14.00  94.00 150.11   56
 12  \w     16.00  41.00   0.50    5.00    --   18.00  86.00  99.72   50
 13  \w     12.00  37.00   0.50    5.00    --   18.00  92.00 -51.35   50
 14  \w     15.00  40.00   0.50    5.00    --   18.00  87.00-157.09   50
 15  \w     27.00  58.00   0.50    5.00    --   22.00  76.00-156.37   62
 16  \w     17.00  42.00   0.50    5.00    --   22.00  90.00 122.15   50
 17  \w     17.00  42.00   0.50    5.00    --   22.00  90.00  51.46   50
 18  \w     25.00  50.00   0.50    5.00    --   22.00  77.00   2.10   50
 19  \w     17.00  42.00   0.50    5.00    --   22.00  90.00   5.30   50
 20  \w     25.00  50.00   0.50    5.00    --   22.00  77.00 -46.69   50
 21  \w     17.00  42.00   0.50    5.00    --   22.00  90.00-125.96   50
 22  \w     30.00  55.00   0.50    5.00    --   26.00  76.00 -32.66   50
 23  \w     29.00  54.00   0.50    5.00    --   26.00  77.00 -96.67   50
 24  \w     31.00  56.00   0.50    5.00    --   26.00  76.00 142.55   50
 25  \w    -65.00 -33.00   0.50    5.00    --  -30.00 -77.00-141.65   64
 26  \w     36.00  63.00   0.50    5.00    --   30.24  73.00 135.57   54
 27  \w     35.00  60.00   0.50    5.00    --   30.24  75.00-130.41   50
 28  \w     34.00  59.00   0.50    5.00    --   30.24  76.00-166.75   50
 29  \w     34.00  59.00   0.50    5.00    --   30.24  76.00 -80.55   50
 30  \w     35.00  62.00   0.50    5.00    --   30.24  75.00  25.35   54
 31  \w     35.00  60.00   0.50    5.00    --   30.24  75.00  50.52   50
 32  \w     42.00  68.00   0.50    5.00    --   30.24  51.00 -54.79   52
 33  \w     43.00  70.00   0.50    5.00    --   30.24  66.00 108.08   54
 34  \w     34.00  59.00   0.50    5.00    --   30.24  77.00-154.99   50
 35  \w     36.00  66.00   0.50    5.00    --   30.24  75.00  62.76   60
 36  \w     34.00  59.00   0.50    5.00    --   30.24  76.00  -3.49   50
 37  \w     34.00  59.00   0.50    5.00    --   30.24  77.00  77.53   50
 38  \w     41.00  66.00   0.50    5.00    --   30.24  37.00 -89.16   50
 39  \w     34.00  59.00   0.50    5.00    --   30.24  76.00 -95.22   50
 40  \w     34.00  60.00   0.50    5.00    --   30.24  76.00 -30.01   52
 41  \w     36.00  64.00   0.50    5.00    --   30.24  77.00  31.64   56
 42  \w     34.00  61.00   0.50    5.00    --   30.24  76.00 173.89   54
 43  \w     35.00  60.00   0.50    5.00    --   30.24  77.00 -95.19   50
 44  \w     35.00  60.00   0.50    5.00    --   30.24  75.00 -48.44   50
 45  \w     43.00  74.00   0.50    5.00    --   30.24  38.00-142.46   62
 46  \w     34.00  59.00   0.50    5.00    --   30.24  76.00  96.81   50
 47  \w     34.00  60.00   0.50    5.00    --   30.24  77.00 -67.99   52
 48  \w     36.00  66.00   0.50    5.00    --   30.24  74.00 119.63   60
 49  \w     35.00  62.00   0.50    5.00    --   30.24  77.00 152.54   54
 50  \w     35.00  60.00   0.50    5.00    --   30.24  75.00-125.94   50
 51  \w    -14.00  18.00   0.50    5.00    --   30.82 -19.00 150.00   64
 52  \w    -65.00 -38.00   0.50    5.00    --  -31.33 -75.00 -63.48   54
 53  \w    -14.00  11.00   0.50    5.00    --  -31.33  19.00 -60.00   50
 54  \w    -31.00  -4.00   0.50    5.00    --  -31.33  82.00 134.48   54
 55  \w    -19.00  12.00   0.50    5.00    --  -31.33  53.00 -26.23   62
 56  \w    -17.00  14.00   0.50    5.00    --  -31.33  19.00 120.00   62
 57  \w    -66.00 -36.00   0.50    5.00    --  -31.33 -74.00-106.52   60
 58  \w    -11.00  15.00   0.50    5.00    --  -31.33  19.00 -90.00   52
 59  \w    -68.00 -27.00   0.50    5.00    --  -31.33   0.00-180.00   82
 60  \w    -14.00  15.00   0.50    5.00    --  -31.33  19.00   0.00   58
 61  \w    -22.00   4.00   0.50    5.00    --  -31.33  35.00-106.18   52
 62  \w    -16.00  12.00   0.50    5.00    --  -31.33  44.00 -55.38   56
 63  \w    -17.00  10.00   0.50    5.00    --  -31.33  19.00 150.00   54
 64  \w    -20.00  12.00   0.50    5.00    --  -31.33  52.00  33.70   64
 65  \w    -18.00  11.00   0.50    5.00    --  -31.33  51.00  57.19   58
 66  \w    -21.00   4.00   0.50    5.00    --  -31.33   0.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0677646000
_diffrn_orient_matrix_UB_12      0.0207824000
_diffrn_orient_matrix_UB_13      0.0052117000
_diffrn_orient_matrix_UB_21      -0.0038298000
_diffrn_orient_matrix_UB_22      -0.0272263000
_diffrn_orient_matrix_UB_23      -0.0490157000
_diffrn_orient_matrix_UB_31      0.0032177000
_diffrn_orient_matrix_UB_32      0.0515686000
_diffrn_orient_matrix_UB_33      -0.0179721000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            232490
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        51.425
_diffrn_reflns_theta_max         51.425
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.378
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.762
_exptl_crystal_description       prism
_exptl_crystal_F_000             4252
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.305
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1906
_refine_ls_number_reflns         39190
_refine_ls_number_restraints     4272
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.1137
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3637
_refine_ls_wR_factor_ref         0.3831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20931
_reflns_number_total             39190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02223a2.cif
_cod_data_source_block           jm-346-2nd-filtrate
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719637--7719640.cif.
;
_cod_database_code               7719637
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C144 H120 B16 N48 F64 Pd8 '
_chemical_oxdiff_usercomment     'crystallised from iPr2O diffusion into CD3NO2'
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.751
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C1(H1), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15),
 C14(H14), C22(H22), C24(H24), C23(H23), C26(H26), C27(H27), C25(H25), C34(H34),
  C35(H35), C36(H36), C39(H39), C38(H38), C37(H37), C48(H48), C47(H47),
 C46(H46), C49(H49), C50(H50), C51(H51), C60(H60), C59(H59), C58(H58), C84(H84),
  C83(H83), C82(H82), C61(H61), C62(H62), C63(H63), C71(H71), C72(H72),
 C70(H70), C87(H87), C86(H86), C85(H85), C94(H94), C96(H96), C95(H95), C98(H98),
  C99(H99), C97(H97), C106(H106), C107(H107), C108(H108), C191(H191),
 C192(H192), C190(H190), C116(H116), C117(H117), C115(H115), C120(H120),
 C119(H119), C118(H118), C127(H127), C128(H128), C129(H129), C131(H131),
 C132(H132), C130(H130), C140(H140), C141(H141), C139(H139), C143(H143),
 C144(H144), C142(H142), C153(H153), C152(H152), C151(H151), C156(H156),
 C155(H155), C154(H154), C165(H165), C164(H164), C163(H163), C168(H168),
 C167(H167), C166(H166), C177(H177), C176(H176), C175(H175), C179(H179),
 C180(H180), C178(H178), C6(H6), C5(H5), C9(H9), C8(H8), C20(H20), C21(H21),
 C17(H17), C18(H18), C32(H32), C33(H33), C29(H29), C30(H30), C42(H42), C41(H41),
  C45(H45), C44(H44), C53(H53), C54(H54), C56(H56), C57(H57), C69(H69),
 C68(H68), C66(H66), C65(H65), C75(H75), C80(H80), C81(H81), C77(H77), C78(H78),
  C93(H93), C92(H92), C90(H90), C89(H89), C101(H101), C102(H102), C104(H104),
 C105(H105), C110(H110), C111(H111), C113(H113), C114(H114), C122(H122),
 C123(H123), C125(H125), C126(H126), C134(H134), C135(H135), C137(H137),
 C138(H138), C149(H149), C148(H148), C146(H146), C147(H147), C159(H159),
 C158(H158), C162(H162), C161(H161), C171(H171), C170(H170), C174(H174),
 C173(H173), C186(H186), C185(H185), C183(H183), C182(H182), C187(H187),
 C189(H189), C188(H188)
4.b Fitted pentagon refined as free rotating group:
 N1(C2,C3,N2,C1), N4(C10,N3,C11,C12), N5(C13,N6,C15,C14), N7(C22,N8,C24,C23),
 N9(C26,C27,N10,C25), N12(C34,N11,C35,C36), N14(C39,C38,N13,C37), N16(C48,C47,
 N15,C46), N18(C49,N17,C50,C51), N20(C60,C59,N19,C58), N24(C84,C83,N23,C82),
 N26(C61,N25,C62,C63), N27(C71,C72,N28,C70), N30(C87,C86,N29,C85), N31(C94,N32,
 C96,C95), N33(C98,C99,N34,C97), N36(C106,N35,C107,C108), N37(C191,C192,N38,
 C190), N39(C116,C117,N40,C115), N42(C120,C119,N41,C118), N43(C127,N44,C128,
 C129), N45(C131,C132,N46,C130), N47(C140,C141,N48,C139), N49(C143,C144,N50,
 C142), N52(C153,C152,N51,C151), N54(C156,C155,N53,C154), N56(C165,C164,N55,
 C163), N58(C168,C167,N57,C166), N60(C177,C176,N59,C175), N62(C179,C180,N61,
 C178), C187(N64,C189,C188,N63)
4.c Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C9,C8), C19(C20,C21,C16,C17,C18), C31(C32,C33,C28,C29,C30),
 C43(C42,C41,C40,C45,C44), C52(C53,C54,C55,C56,C57), C64(C69,C68,C67,C66,C65),
 C79(C80,C81,C76,C77,C78), C88(C93,C92,C91,C90,C89), C100(C101,C102,C103,C104,
 C105), C110(C111,C112,C113,C114,C109), C121(C122,C123,C124,C125,C126),
 C133(C134,C135,C136,C137,C138), C150(C149,C148,C145,C146,C147), C160(C159,C158,
 C157,C162,C161), C172(C171,C170,C169,C174,C173), C181(C186,C185,C184,C183,C182)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58590
_shelx_hkl_checksum              35689
_shelx_fab_checksum              8761
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.040
_oxdiff_exptl_absorpt_empirical_full_min 0.661