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_7719640
_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
'C264 H192 N48 Pd6, 10(B F4), 2(C4 H8 O2), 6(C2 H3 N), 2[BF4]'
_chemical_formula_sum            'C284 H226 B12 F48 N54 O4 Pd6'
_chemical_formula_weight         6139.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-09-05
_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                90
_cell_angle_beta                 97.7376(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.4258(3)
_cell_length_b                   34.96497(18)
_cell_length_c                   32.50283(12)
_cell_measurement_reflns_used    125103
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7430
_cell_measurement_theta_min      1.6580
_cell_volume                     47776.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.113a 64-bit (release 02-06-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.111a (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      100.00(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 0.998
_diffrn_measured_fraction_theta_max 0.976
_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     37.00  75.00   0.50    1.00    --   66.04 -95.00  90.00   76
  2  \w     28.00  71.00   0.50    1.00    --   66.04 -95.00-180.00   86
  3  \w     28.00  61.00   0.50    1.00    --   66.04 -95.00 -30.00   66
  4  \w     32.00  70.00   0.50    1.00    --   66.04 -95.00-120.00   76
  5  \w     28.00  54.00   0.50    1.00    --   66.04 -95.00  30.00   52
  6  \w     34.00  73.00   0.50    1.00    --   66.04 -95.00 120.00   78
  7  \w     28.00  75.00   0.50    1.00    --   66.04 -95.00 -60.00   94
  8  \w   -104.00 -74.00   0.50    1.00    --  -67.39   0.00  30.00   60
  9  \w   -103.00 -73.00   0.50    1.00    --  -67.39   0.00  60.00   60
 10  \w   -104.00 -72.00   0.50    1.00    --  -67.39   0.00  90.00   64
 11  \w    -70.00 -35.00   0.50    1.00    --  -67.39 125.00-180.00   70
 12  \w   -102.00 -72.00   0.50    1.00    --  -67.39   0.00 120.00   60
 13  \w   -103.00 -36.00   0.50    1.00    --  -67.39 -15.00 150.00  134
 14  \w    -77.00 -25.00   0.50    1.00    --  -67.39 125.00-150.00  104
 15  \w    -75.00 -26.00   0.50    1.00    --  -69.31 125.00   0.00   98
 16  \w   -105.00 -80.00   0.50    1.00    --  -69.31   0.00-180.00   50
 17  \w    -94.00 -48.00   0.50    1.00    --  -69.31 -15.00  60.00   92
 18  \w   -103.00 -75.00   0.50    1.00    --  -69.31   0.00 -30.00   56
 19  \w     49.00  77.00   0.50    1.00    --   69.52 -95.00 150.00   56
 20  \w     34.00  77.00   0.50    1.00    --   69.52 -95.00   0.00   86
 21  \w     39.00 114.00   0.50    1.00    --   69.52  15.00 150.00  150
 22  \w     41.00 115.00   0.50    1.00    --   69.52  15.00  60.00  148
 23  \w    -97.00 -55.00   0.50    1.00    --  -74.80 115.00 -70.16   84
 24  \w   -113.00 -45.00   0.50    1.00    --  -74.80 142.00  64.67  136
 25  \w   -113.00 -76.00   0.50    1.00    --  -74.80 142.00 108.92   74
 26  \w    -73.00 -47.00   0.50    1.00    --  -74.80 151.00 -54.50   52
 27  \w    -65.00 -38.00   0.50    1.00    --  -74.80 142.00 108.92   54
 28  \w   -104.00 -41.00   0.50    1.00    --  -74.80 126.00   4.21  126
 29  \w    -56.00 -31.00   0.50    1.00    --  -74.80 128.00-136.59   50
 30  \w   -119.00 -89.00   0.50    1.00    --  -74.80 151.00 -54.50   60
 31  \w   -105.00 -62.00   0.50    1.00    --  -74.80 128.00-136.59   86
 32  \w     81.00 106.00   0.50    1.00    --   77.97-125.00-180.00   50
 33  \w     47.00  73.00   0.50    1.00    --   77.97-125.00 120.00   52
 34  \w     49.00  74.00   0.50    1.00    --   77.97-125.00-180.00   50
 35  \w     72.00 123.00   0.50    1.00    --   77.97  15.00-120.00  102
 36  \w     52.00 109.00   0.50    1.00    --   77.97  15.00 120.00  114
 37  \w     40.00  65.00   0.50    1.00    --   77.97 -95.00  30.00   50
 38  \w     56.00  82.00   0.50    1.00    --   77.97 -95.00-180.00   52
 39  \w     67.00 107.00   0.50    1.00    --   77.97  15.00 -30.00   80
 40  \w     81.00 106.00   0.50    1.00    --   77.97-125.00 150.00   50
 41  \w     52.00 114.00   0.50    1.00    --   77.97  15.00-180.00  124
 42  \w     40.00  65.00   0.50    1.00    --   77.97 -95.00-150.00   50
 43  \w     39.00 106.00   0.50    1.00    --   77.97-125.00   0.00  134
 44  \w     78.00 106.00   0.50    1.00    --   77.97-125.00-120.00   56
 45  \w     39.00  64.00   0.50    1.00    --   77.97-125.00-120.00   50
 46  \w     81.00 106.00   0.50    1.00    --   77.97-125.00  90.00   50
 47  \w     81.00 106.00   0.50    1.00    --   77.97-125.00-150.00   50
 48  \w     39.00  66.00   0.50    1.00    --   77.97-125.00-150.00   54
 49  \w     43.00 106.00   0.50    1.00    --   77.97-125.00  30.00  126
 50  \w     81.00 106.00   0.50    1.00    --   77.97-125.00 -30.00   50
 51  \w     36.00 106.00   0.50    1.00    --   77.97-125.00 -90.00  140
 52  \w     47.00 120.00   0.50    1.00    --   77.97  15.00  30.00  146
;
_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      -0.0357978000
_diffrn_orient_matrix_UB_12      -0.0086452000
_diffrn_orient_matrix_UB_13      -0.0020044000
_diffrn_orient_matrix_UB_21      -0.0068291000
_diffrn_orient_matrix_UB_22      0.0430564000
_diffrn_orient_matrix_UB_23      0.0035610000
_diffrn_orient_matrix_UB_31      -0.0039504000
_diffrn_orient_matrix_UB_32      0.0035813000
_diffrn_orient_matrix_UB_33      -0.0476410000
_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  0.0251
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            434846
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.045
_diffrn_reflns_theta_min         1.643
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.276
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.111a (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    0.854
_exptl_crystal_description       prism
_exptl_crystal_F_000             12432
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.893
_refine_diff_density_min         -2.415
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.390
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1822
_refine_ls_number_reflns         48088
_refine_ls_number_restraints     3823
_refine_ls_restrained_S_all      1.434
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.005
_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          0.3136
_refine_ls_wR_factor_ref         0.3288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36863
_reflns_number_total             48088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02223a2.cif
_cod_data_source_block           jm-633_2
_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_original_cell_volume        47776.2(4)
_cod_database_code               7719640
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C264 N48 Pd6 B12 F48'
_chemical_oxdiff_usercomment     'ACD-d3, EtOAc, ETHER'
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.303
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C106-C109 = C206-C109
 1.5 with sigma of 0.01
 C103-N20 = C203-N20
 1.5 with sigma of 0.02
 C124-C113 = C124-C113
 1.5 with sigma of 0.01
 B3-F28 = B3-F11 = B3-F10 = B3-F9
 1.42 with sigma of 0.02
 C135-C136
 1.5 with sigma of 0.02
 B6-F20 = B6-F22 = B6-F23 = B6-F21
 1.42 with sigma of 0.02
 C82A-C78 = C78-C82B
 1.5 with sigma of 0.02
 N15-C85A = N15-C85B
 1.47 with sigma of 0.02
 O2-C134
 1.32 with sigma of 0.02
 O2-C135
 1.46 with sigma of 0.02
 O1-C134
 1.22 with sigma of 0.02
 N23-C227 = N23-C127
 1.4 with sigma of 0.02
 C133-C134
 1.49 with sigma of 0.02
 N27-C141
 1.14 with sigma of 0.02
 C141-C142
 1.46 with sigma of 0.02
 N26-C139
 1.14 with sigma of 0.02
 C139-C140
 1.46 with sigma of 0.02
 B5-F16 = B5-F19 = B5-F18 = B5-F17
 1.42 with sigma of 0.02
 N25-C137
 1.14 with sigma of 0.02
 C137-C138
 1.46 with sigma of 0.02
 B7-F24 = B7-F27 = B7-F26 = B7-F25
 1.42 with sigma of 0.02
 B2-F5 = B2-F8 = B2-F6 = B2-F7
 1.42 with sigma of 0.02
 B1-F2 = B1-F1 = B1-F4 = B1-F3
 1.42 with sigma of 0.02
 B4-F14 = B4-F15 = B4-F13 = B4-F12
 1.42 with sigma of 0.02
 O2-C136
 2.38 with sigma of 0.04
 O2-O1
 2.24 with sigma of 0.04
 O2-C133
 2.35 with sigma of 0.04
 O1-C133
 2.4 with sigma of 0.04
 N27-C142
 2.59 with sigma of 0.04
 N26-C140
 2.59 with sigma of 0.04
 N25-C138
 2.59 with sigma of 0.04
 C106-C109 \\sim C206-C109
 with sigma of 0.01
 C124-C113 \\sim C124-C113
 with sigma of 0.01
 N20-C203 \\sim N20-C103
 with sigma of 0.01
 N23-C127 \\sim N23-C227
 with sigma of 0.01
 F24-F27 \\sim F24-F26 \\sim F24-F25 \\sim F27-F26 \\sim F27-F25 \\sim F26-F25
 with sigma of 0.04
 B7-F24 \\sim B7-F27 \\sim B7-F26 \\sim B7-F25
 with sigma of 0.02
 F25-F24 \\sim F25-F27 \\sim F25-F26 \\sim F24-F27 \\sim F24-F26 \\sim F27-F26
 with sigma of 0.04
 B7-F25 \\sim B7-F24 \\sim B7-F27 \\sim B7-F26
 with sigma of 0.02
 F20-F22 \\sim F20-F23 \\sim F20-F21 \\sim F22-F23 \\sim F22-F21 \\sim F23-F21
 with sigma of 0.04
 B6-F20 \\sim B6-F22 \\sim B6-F23 \\sim B6-F21
 with sigma of 0.02
 F16-F19 \\sim F16-F18 \\sim F16-F17 \\sim F19-F18 \\sim F19-F17 \\sim F18-F17
 with sigma of 0.04
 B5-F16 \\sim B5-F19 \\sim B5-F18 \\sim B5-F17
 with sigma of 0.02
 F28-F11 \\sim F28-F10 \\sim F28-F9 \\sim F11-F10 \\sim F11-F9 \\sim F10-F9
 with sigma of 0.04
 B3-F28 \\sim B3-F11 \\sim B3-F10 \\sim B3-F9
 with sigma of 0.02
 F5-F8 \\sim F5-F6 \\sim F5-F7 \\sim F8-F6 \\sim F8-F7 \\sim F6-F7
 with sigma of 0.04
 B2-F5 \\sim B2-F8 \\sim B2-F6 \\sim B2-F7
 with sigma of 0.02
 F1-F4 \\sim F1-F2 \\sim F1-F3 \\sim F4-F2 \\sim F4-F3 \\sim F2-F3
 with sigma of 0.04
 B1-F1 \\sim B1-F4 \\sim B1-F2 \\sim B1-F3
 with sigma of 0.02
 F14-F15 \\sim F14-F13 \\sim F14-F12 \\sim F15-F13 \\sim F15-F12 \\sim F13-F12
 with sigma of 0.04
 B4-F14 \\sim B4-F15 \\sim B4-F13 \\sim B4-F12
 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 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C203)=Sof(C204)=Sof(H204)=Sof(C205)=Sof(H205)=Sof(C206)=Sof(C207)=
 Sof(H207)=Sof(C208)=Sof(H208)=Sof(C224)=Sof(C225)=Sof(H225)=Sof(C226)=
 Sof(H226)=Sof(C227)=Sof(C228)=Sof(H228)=Sof(C229)=Sof(H229)=1-FVAR(1)
 Sof(C106)=Sof(C107)=Sof(H107)=Sof(C108)=Sof(H108)=Sof(C103)=Sof(C104)=
 Sof(H104)=Sof(C105)=Sof(H105)=Sof(C127)=Sof(C128)=Sof(H128)=Sof(C129)=
 Sof(H129)=Sof(C124)=Sof(C125)=Sof(H125)=Sof(C126)=Sof(H126)=FVAR(1)
 Sof(C82B)=Sof(C87B)=Sof(H87B)=Sof(C86B)=Sof(H86B)=Sof(C85B)=Sof(C84B)=
 Sof(H84B)=Sof(C83B)=Sof(H83B)=1-FVAR(2)
 Sof(C82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=Sof(H84A)=Sof(C85A)=Sof(C86A)=
 Sof(H86A)=Sof(C87A)=Sof(H87A)=FVAR(2)
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) B1(0.5) F12(0.5) F13(0.5) F14(0.5)
 F15(0.5) B4(0.5) F16(0.5) F17(0.5) F18(0.5) F19(0.5) B5(0.5) F24(0.5) F25(0.5)
 F26(0.5) F27(0.5) B7(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C135(H13D,H13E)
6.b Me refined with riding coordinates:
 C136(H13F,H13G,H13H)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C5(H5), C9(H9), C8(H8), C11(H11), C15(H15),
 C13(H13), C20(H20), C21(H21), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C42(H42), C41(H41), C39(H39), C38(H38), C48(H48),
  C46(H46), C44(H44), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55),
 C56(H56), C57(H57), C63(H63), C62(H62), C60(H60), C59(H59), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68), C69(H69), C72(H72), C71(H71), C75(H75),
 C74(H74), C77(H77), C81(H81), C79(H79), C83A(H83A), C84A(H84A), C86A(H86A),
 C87A(H87A), C87B(H87B), C86B(H86B), C84B(H84B), C83B(H83B), C88(H88), C89(H89),
  C90(H90), C96(H96), C95(H95), C93(H93), C92(H92), C97(H97), C98(H98),
 C99(H99), C100(H100), C101(H101), C102(H102), C107(H107), C108(H108),
 C104(H104), C105(H105), C112(H112), C110(H110), C114(H114), C117(H117),
 C116(H116), C120(H120), C119(H119), C121(H121), C122(H122), C123(H123),
 C128(H128), C129(H129), C125(H125), C126(H126), C130(H130), C131(H131),
 C132(H132), C204(H204), C205(H205), C207(H207), C208(H208), C225(H225),
 C226(H226), C228(H228), C229(H229)
6.d Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C9,C8), C12(C11,C10,C15,C14,C13), C19(C20,C21,C16,C17,C18),
 C25(C26,C27,C28,C29,C30), C37(C42,C41,C40,C39,C38), C43(C48,C47,C46,C45,C44),
 C49(C50,C51,C52,C53,C54), C58(C63,C62,C61,C60,C59), C73(C72,C71,C70,C75,C74),
 C77(C76,C81,C80,C79,C78), C82A(C83A,C84A,C85A,C86A,C87A), C82B(C87B,C86B,C85B,
 C84B,C83B), C91(C96,C95,C94,C93,C92), C106(C107,C108,C103,C104,C105),
 C113(C112,C111,C110,C109,C114), C118(C117,C116,C115,C120,C119), C127(C128,C129,
 C124,C125,C126), C203(C204,C205,C206,C207,C208), C224(C225,C226,C227,C228,C229)
6.e Idealised Me refined as rotating group:
 C133(H13A,H13B,H13C), C138(H13I,H13J,H13K), C140(H14A,H14B,H14C), C142(H14D,
 H14E,H14F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 6377 electrons were 
found in a volume of 23817\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[BF4] per Asymmetric Unit 
which account for 328 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35286
_shelx_hkl_checksum              36686
_shelx_fab_checksum              32458
_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 1.570
_oxdiff_exptl_absorpt_empirical_full_min 0.670