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_7719639
_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
'C216 H120 N24 Pd6, 8(B F4), 6(C2 H3 N), 4[B F4], 22[C2H3N]'
_chemical_formula_sum            'C272 H204 B12 F48 N52 Pd6'
_chemical_formula_weight         5533.74
_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             2025-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-25 deposited with the CCDC.	2025-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                102.0875(7)
_cell_angle_beta                 91.7048(7)
_cell_angle_gamma                99.1616(7)
_cell_formula_units_Z            2
_cell_length_a                   20.84690(17)
_cell_length_b                   21.52588(19)
_cell_length_c                   38.1140(3)
_cell_measurement_reflns_used    71998
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.2530
_cell_measurement_theta_min      2.1220
_cell_volume                     16475.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.44.103a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.102a 64-bit (release 28-03-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.103a (Rigaku OD, 2025)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.958
_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     36.00 108.00   0.50    2.50    --   66.04  15.00 150.00  144
  2  \w     28.00  63.00   0.50    2.50    --   66.04 -95.00 150.00   70
  3  \w     30.00  63.00   0.50    2.50    --   66.04 -95.00  90.00   66
  4  \w     30.00  59.00   0.50    2.50    --   66.04 -95.00-120.00   58
  5  \w     29.00  71.00   0.50    2.50    --   66.04 -95.00-180.00   84
  6  \w     30.00 103.00   0.50    2.50    --   66.04   0.00-120.00  146
  7  \w     37.00  64.00   0.50    2.50    --   66.04 -95.00   0.00   54
  8  \w     36.00 104.00   0.50    2.50    --   66.04  15.00 -60.00  136
  9  \w    -93.00 -66.00   0.50    2.50    --  -66.76 125.00   0.00   54
 10  \w    -92.00 -26.00   0.50    2.50    --  -66.76 125.00  90.00  132
 11  \w    -58.00 -33.00   0.50    2.50    --  -66.76 125.00   0.00   50
 12  \w   -109.00 -40.00   0.50    2.50    --  -66.76 -15.00 -90.00  138
 13  \w    -71.00 -35.00   0.50    2.50    --  -66.76   0.00 -30.00   72
 14  \w    -95.00 -51.00   0.50    2.50    --  -69.34 125.00 150.00   88
 15  \w    -96.00 -47.00   0.50    2.50    --  -69.34 125.00 -60.00   98
 16  \w    -96.00 -35.00   0.50    2.50    --  -69.34 125.00-120.00  122
 17  \w    -71.00 -34.00   0.50    2.50    --  -69.34   0.00 -60.00   74
 18  \w     47.00  78.00   0.50    2.50    --   69.57 -95.00 -90.00   62
 19  \w     39.00  72.00   0.50    2.50    --   69.57 -95.00-120.00   66
 20  \w     38.00 114.00   0.50    2.50    --   69.57  15.00 -90.00  152
 21  \w     51.00 103.00   0.50    2.50    --   69.57   0.00-180.00  104
 22  \w   -121.00 -38.00   0.50    2.50    --  -74.00 155.00 -45.16  166
 23  \w    -80.00 -37.00   0.50    2.50    --  -74.82 144.00-130.48   86
 24  \w   -108.00 -82.00   0.50    2.50    --  -74.82 135.00-158.30   52
 25  \w    -78.00 -40.00   0.50    2.50    --  -74.82 140.00  35.08   76
 26  \w   -112.00 -86.00   0.50    2.50    --  -74.82 140.00  35.08   52
 27  \w    -69.00 -44.00   0.50    2.50    --  -74.82 135.00-158.30   50
 28  \w   -110.00 -33.00   0.50    2.50    --  -74.82 138.00 120.47  154
 29  \w   -114.00 -88.00   0.50    2.50    --  -74.82 144.00-130.48   52
 30  \w     73.00 103.00   0.50    2.50    --   77.93-125.00-180.00   60
 31  \w     48.00  73.00   0.50    2.50    --   77.93-125.00 -60.00   50
 32  \w     41.00 105.00   0.50    2.50    --   77.93-125.00 120.00  128
 33  \w     80.00 105.00   0.50    2.50    --   77.93-125.00  60.00   50
 34  \w     36.00  66.00   0.50    2.50    --   77.93-125.00  60.00   60
 35  \w     80.00 105.00   0.50    2.50    --   77.93-125.00  90.00   50
 36  \w     39.00  64.00   0.50    2.50    --   77.93-125.00  90.00   50
 37  \w     66.00  92.00   0.50    2.50    --   77.93  15.00-180.00   52
 38  \w     80.00 105.00   0.50    2.50    --   77.93-125.00 150.00   50
 39  \w     80.00 105.00   0.50    2.50    --   77.93-125.00-120.00   50
 40  \w     43.00 103.00   0.50    2.50    --   77.93   0.00 -30.00  120
 41  \w     80.00 105.00   0.50    2.50    --   77.93-125.00-150.00   50
 42  \w     41.00  67.00   0.50    2.50    --   77.93 -95.00 -30.00   52
 43  \w     80.00 105.00   0.50    2.50    --   77.93-125.00 -30.00   50
 44  \w     60.00  95.00   0.50    2.50    --   77.93  15.00-150.00   70
 45  \w     45.00  70.00   0.50    2.50    --   77.93-125.00 -30.00   50
 46  \w     41.00  66.00   0.50    2.50    --   77.93 -95.00 120.00   50
 47  \w     80.00 105.00   0.50    2.50    --   77.93-125.00   0.00   50
 48  \w     62.00 121.00   0.50    2.50    --   77.93  15.00  30.00  118
 49  \w     53.00  94.00   0.50    2.50    --   77.93  15.00 -90.00   82
 50  \w     78.00 103.00   0.50    2.50    --   77.93  15.00  60.00   50
 51  \w     80.00 105.00   0.50    2.50    --   77.93-125.00 -60.00   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      -0.0553632000
_diffrn_orient_matrix_UB_12      0.0009391000
_diffrn_orient_matrix_UB_13      0.0258938000
_diffrn_orient_matrix_UB_21      0.0171321000
_diffrn_orient_matrix_UB_22      0.0740342000
_diffrn_orient_matrix_UB_23      0.0110447000
_diffrn_orient_matrix_UB_31      -0.0476291000
_diffrn_orient_matrix_UB_32      0.0057397000
_diffrn_orient_matrix_UB_33      -0.0303898000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            295421
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.826
_diffrn_reflns_theta_min         2.130
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.169
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.103a (Rigaku Oxford Diffraction, 2025)
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    1.115
_exptl_crystal_description       plate
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.860
_refine_diff_density_min         -2.783
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2403
_refine_ls_number_reflns         64878
_refine_ls_number_restraints     4503
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1799P)^2^+15.1296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2719
_refine_ls_wR_factor_ref         0.2919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42105
_reflns_number_total             64878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02223a2.cif
_cod_data_source_block           jm-513
_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               7719639
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_usercomment     'CD3CN, iPr2O'
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.584
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B8-F31 = B8-F29 = B8-F30 = B8-F32
 1.42 with sigma of 0.02
 B9-F34 = B9-F36 = B9-F35 = B9-F33
 1.42 with sigma of 0.02
 C242-C241
 1.46 with sigma of 0.02
 B7-F26 = B7-F27 = B7-F28 = B7-F25
 1.42 with sigma of 0.02
 B5-F17 = B5-F18 = B5-F19 = B5-F20
 1.42 with sigma of 0.02
 B6-F23 = B6-F21 = B6-F22 = B6-F24
 1.42 with sigma of 0.02
 B4-F16 = B4-F14 = B4-F15 = B4-F13
 1.42 with sigma of 0.02
 N45-C238
 1.14 with sigma of 0.02
 C238-C237
 1.46 with sigma of 0.02
 N39-C255
 1.14 with sigma of 0.02
 C255-C256
 1.46 with sigma of 0.02
 N35-C234
 1.14 with sigma of 0.02
 C234-C233
 1.46 with sigma of 0.02
 N40-C242
 1.14 with sigma of 0.02
 N44-C235
 1.14 with sigma of 0.02
 C235-C236
 1.46 with sigma of 0.02
 B2-F6 = B2-F7 = B2-F8 = B2-F5
 1.42 with sigma of 0.02
 B3-F12 = B3-F11 = B3-F9 = B3-F10
 1.42 with sigma of 0.02
 B1-F3 = B1-F4 = B1-F1 = B1-F2
 1.42 with sigma of 0.02
 N43-C240
 1.14 with sigma of 0.02
 C240-C239
 1.46 with sigma of 0.02
 N40-C241
 2.59 with sigma of 0.04
 N45-C237
 2.59 with sigma of 0.04
 N39-C256
 2.59 with sigma of 0.04
 N35-C233
 2.59 with sigma of 0.04
 N44-C236
 2.59 with sigma of 0.04
 N43-C239
 2.59 with sigma of 0.04
 F6-F7 \\sim F6-F8 \\sim F6-F5 \\sim F7-F8 \\sim F7-F5 \\sim F8-F5
 with sigma of 0.04
 B2-F6 \\sim B2-F7 \\sim B2-F8 \\sim B2-F5
 with sigma of 0.02
 F23-F21 \\sim F23-F22 \\sim F23-F24 \\sim F21-F22 \\sim F21-F24 \\sim F22-F24
 with sigma of 0.04
 B6-F23 \\sim B6-F21 \\sim B6-F22 \\sim B6-F24
 with sigma of 0.02
 F17-F18 \\sim F17-F19 \\sim F17-F20 \\sim F18-F19 \\sim F18-F20 \\sim F19-F20
 with sigma of 0.04
 B5-F17 \\sim B5-F18 \\sim B5-F19 \\sim B5-F20
 with sigma of 0.02
 F16-F14 \\sim F16-F15 \\sim F16-F13 \\sim F14-F15 \\sim F14-F13 \\sim F15-F13
 with sigma of 0.04
 B4-F16 \\sim B4-F14 \\sim B4-F15 \\sim B4-F13
 with sigma of 0.02
 F26-F27 \\sim F26-F28 \\sim F26-F25 \\sim F27-F28 \\sim F27-F25 \\sim F28-F25
 with sigma of 0.04
 B7-F26 \\sim B7-F27 \\sim B7-F28 \\sim B7-F25
 with sigma of 0.02
 F31-F29 \\sim F31-F30 \\sim F31-F32 \\sim F29-F30 \\sim F29-F32 \\sim F30-F32
 with sigma of 0.04
 B8-F31 \\sim B8-F29 \\sim B8-F30 \\sim B8-F32
 with sigma of 0.02
 F34-F36 \\sim F34-F35 \\sim F34-F33 \\sim F36-F35 \\sim F36-F33 \\sim F35-F33
 with sigma of 0.04
 B9-F34 \\sim B9-F36 \\sim B9-F35 \\sim B9-F33
 with sigma of 0.02
 F12-F11 \\sim F12-F9 \\sim F12-F10 \\sim F11-F9 \\sim F11-F10 \\sim F9-F10
 with sigma of 0.04
 B3-F12 \\sim B3-F11 \\sim B3-F9 \\sim B3-F10
 with sigma of 0.02
 F3-F4 \\sim F3-F1 \\sim F3-F2 \\sim F4-F1 \\sim F4-F2 \\sim F1-F2
 with sigma of 0.04
 B1-F3 \\sim B1-F4 \\sim B1-F1 \\sim B1-F2
 with sigma of 0.02
3. 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
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) B1(0.5) F21(0.5) F22(0.5) F23(0.5)
 F24(0.5) B6(0.5)
6.a Me refined with riding coordinates:
 C241(H24A,H24B,H24C)
6.b Aromatic/amide H refined with riding coordinates:
 C159(H159), C160(H160), C161(H161), C158(H158), C184(H184), C186(H186),
 C187(H187), C188(H188), C179(H179), C180(H180), C181(H181), C178(H178),
 C78(H78), C79(H79), C80(H80), C77(H77), C99(H99), C97(H97), C98(H98),
 C189(H189), C3(H3), C2(H2), C1(H1), C5(H5), C9(H9), C13(H13), C11(H11),
 C18(H18), C16(H16), C20(H20), C19(H19), C25(H25), C24(H24), C27(H27), C26(H26),
  C28(H28), C30(H30), C31(H31), C32(H32), C36(H36), C40(H40), C38(H38),
 C45(H45), C107(H107), C46(H46), C44(H44), C50(H50), C51(H51), C52(H52),
 C53(H53), C58(H58), C54(H54), C55(H55), C56(H56), C66(H66), C64(H64), C62(H62),
  C70(H70), C71(H71), C72(H72), C73(H73), C83(H83), C85(H85), C81(H81),
 C82(H82), C89(H89), C93(H93), C91(H91), C106(H106), C105(H105), C104(H104),
 C103(H103), C110(H110), C111(H111), C112(H112), C108(H108), C116(H116),
 C118(H118), C120(H120), C125(H125), C124(H124), C127(H127), C126(H126),
 C134(H134), C133(H133), C132(H132), C131(H131), C139(H139), C135(H135),
 C136(H136), C137(H137), C143(H143), C147(H147), C145(H145), C152(H152),
 C151(H151), C154(H154), C153(H153), C162(H162), C163(H163), C164(H164),
 C165(H165), C174(H174), C172(H172), C170(H170), C191(H191), C193(H193),
 C216(H216), C190(H190), C201(H201), C199(H199), C198(H198), C208(H208),
 C207(H207), C206(H206), C205(H205), C215(H215), C214(H214), C213(H213),
 C212(H212)
6.c Fitted hexagon refined as free rotating group:
 N13(C159,C160,C161,C157,C158), N14(C184,C185,C186,C187,C188), N17(C179,C180,
 C181,C177,C178), N18(C78,C79,C80,C76,C77), N19(C99,C96,C97,C98,C189), C3(C2,C1,
 N1,C5,C4), C9(C8,C13,C12,C11,C10), C18(C17,C16,N5,C20,C19), C25(N24,C24,C23,
 C27,C26), C28(C29,C30,C31,C32,N2), C36(C35,C40,C39,C38,C37), C45(C107,C46,C43,
 C44,N6), C49(C50,N9,C51,C52,C53), C57(C58,N3,C54,C55,C56), C61(C66,C65,C64,C63,
 C62), C69(C70,N10,C71,C72,C73), C83(C84,C85,N4,C81,C82), C90(C89,C88,C93,C92,
 C91), C106(C105,C104,N21,C103,C102), C109(C110,C111,C112,N7,C108), C116(C117,
 C118,C119,C120,C115), C125(N23,C124,C123,C127,C126), C130(C134,C133,C132,N16,
 C131), C138(C139,N12,C135,C136,C137), C143(C142,C147,C146,C145,C144), C152(N8,
 C151,C150,C154,C153), C166(C162,N11,C163,C164,C165), C169(C174,C173,C172,C171,
 C170), C191(C192,C193,N20,C216,C190), C196(C201,C200,C199,C197,C198),
 C204(C208,C207,C206,N15,C205), C211(C215,C214,C213,N22,C212)
6.d Idealised Me refined as rotating group:
 C233(H23A,H23B,H23C), C256(H25A,H25B,H25C), C239(H23D,H23E,H23F), C236(H23G,
 H23H,H23I), C237(H23J,H23K,H23L)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1300 electrons were 
found in a volume of 7715\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
22[C2H3N] per Asymmetric Unit 
which account for 968 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17247
_shelx_hkl_checksum              37687
_shelx_fab_checksum              29640
_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 2.323