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_7719638
_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
'C120 H96 N48 Pd6 S12, 12(B F4), 28(C2 H3 N), 2(C6 H14 O), 4[C2H3N], 2.5[C2H3N]'
_chemical_formula_sum            'C201 H227.5 B12 F48 N82.5 O2 Pd6 S12'
_chemical_formula_weight         5895.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-08-19
_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                 111.9603(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.51690(15)
_cell_length_b                   33.34179(13)
_cell_length_c                   22.84232(14)
_cell_measurement_reflns_used    80275
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.1720
_cell_measurement_theta_min      2.4710
_cell_volume                     13785.65(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.141a 64-bit (release 04-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.141a (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 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     75.00 100.00   0.50    0.50    --   76.61-125.00   0.00   50
  2  \w     77.00 103.00   0.50    0.50    --   76.61-125.00 -90.00   52
  3  \w     63.00  89.00   0.50    0.50    --   75.73-111.00 -90.00   52
  4  \w     40.00  66.00   0.50    0.50    --   76.61-125.00-120.00   52
  5  \w     66.00  92.00   0.50    0.50    --   75.73-111.00-150.00   52
  6  \w     53.00  79.00   0.50    0.50    --   76.61 -95.00-150.00   52
  7  \w     41.00  84.00   0.50    0.50    --   76.61 -95.00 -90.00   86
  8  \w     40.00  71.00   0.50    0.50    --   79.75 -65.00-151.36   62
  9  \w     26.00  68.00   0.50    0.50    --   63.87 -95.00 -30.00   84
 10  \w     58.00  83.00   0.50    0.50    --   76.61 -95.00 120.00   50
 11  \w     40.00  80.00   0.50    0.50    --   76.61 -95.00 150.00   80
 12  \w     41.00  67.00   0.50    0.50    --   79.75 -68.00 151.53   52
 13  \w     65.00  90.00   0.50    0.50    --   75.73   0.00  90.00   50
 14  \w     69.00  94.00   0.50    0.50    --   63.87  28.00 122.00   50
 15  \w     77.00 102.00   0.50    0.50    --   75.73  28.00 122.00   50
 16  \w     90.00 115.00   0.50    0.50    --   76.61  28.00 122.00   50
 17  \w     62.00 125.00   0.50    0.50    --   79.75  21.00  90.24  126
 18  \w     54.00 117.00   0.50    0.50    --   79.75  14.00  30.17  126
 19  \w     48.00 100.00   0.50    0.50    --   79.75  18.00 -19.57  104
 20  \w     88.00 114.00   0.50    0.50    --   79.75   5.00-132.23   52
 21  \w     64.00 124.00   0.50    0.50    --   79.75  22.00 -99.83  120
 22  \w     54.00 114.00   0.50    0.50    --   79.75  19.00-123.24  120
 23  \w     70.00 120.00   0.50    0.50    --   79.75   6.00 -24.49  100
 24  \w     58.00 111.00   0.50    0.50    --   79.75   1.00 108.21  106
 25  \w     58.00 118.00   0.50    0.50    --   79.75   5.00 158.87  120
 26  \w    -70.00 -41.00   0.50    0.50    --  -71.12   0.00 -30.00   58
 27  \w    -66.00 -35.00   0.50    0.50    --  -71.12   0.00-150.00   62
 28  \w    -71.00 -37.00   0.50    0.50    --  -71.12   0.00-180.00   68
 29  \w    -66.00 -35.00   0.50    0.50    --  -71.12   0.00-120.00   62
 30  \w    -71.00 -42.00   0.50    0.50    --  -71.12   0.00 -60.00   58
 31  \w    -92.00 -67.00   0.50    0.50    --  -64.59 -28.00 -39.00   50
 32  \w   -109.00 -80.00   0.50    0.50    --  -76.25 -78.00 -55.36   58
 33  \w   -111.00 -85.00   0.50    0.50    --  -76.25 -83.00-142.17   52
 34  \w   -111.00 -83.00   0.50    0.50    --  -76.25 -75.00-121.25   56
 35  \w   -111.00 -77.00   0.50    0.50    --  -71.12 -28.00 -39.00   68
 36  \w    -69.00 -41.00   0.50    0.50    --  -76.25  87.00-167.28   56
 37  \w    -75.00 -32.00   0.50    0.50    --  -71.12 111.00-180.00   86
 38  \w    -69.00 -41.00   0.50    0.50    --  -76.25 123.00-156.37   56
 39  \w    -80.00 -55.00   0.50    0.50    --  -76.25  88.00 -69.41   50
 40  \w    -86.00 -31.00   0.50    0.50    --  -71.12 111.00 120.00  110
;
_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      -0.0802403000
_diffrn_orient_matrix_UB_12      -0.0126596000
_diffrn_orient_matrix_UB_13      -0.0127758000
_diffrn_orient_matrix_UB_21      0.0222084000
_diffrn_orient_matrix_UB_22      -0.0114073000
_diffrn_orient_matrix_UB_23      0.0700320000
_diffrn_orient_matrix_UB_31      -0.0177092000
_diffrn_orient_matrix_UB_32      0.0429538000
_diffrn_orient_matrix_UB_33      0.0148386000
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            175849
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.774
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.764
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.141a (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    1.420
_exptl_crystal_description       prism
_exptl_crystal_F_000             5974
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.597
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1563
_refine_ls_number_reflns         28191
_refine_ls_number_restraints     2175
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1692P)^2^+24.5990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23438
_reflns_number_total             28191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02223a2.cif
_cod_data_source_block           jm-484
_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        13785.65(16)
_cod_original_formula_sum        'C201 H227.50 B12 F48 N82.50 O2 Pd6 S12'
_cod_database_code               7719638
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C188 H208 B12 F48 N76 O2 Pd6 S12'
_chemical_oxdiff_usercomment     'CRYSTALLISED FROM CD3CN AND iPr2O'
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.382
_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
 C89-C91 = C89-C90 = C94-C92 = C92-C93
 1.54 with sigma of 0.02
 N37-C85
 1.14 with sigma of 0.02
 C77-C78
 1.46 with sigma of 0.02
 C85-C86
 1.46 with sigma of 0.02
 N36-C83
 1.14 with sigma of 0.02
 C83-C84
 1.46 with sigma of 0.02
 N38-C87
 1.14 with sigma of 0.02
 C87-C88
 1.46 with sigma of 0.02
 N26-C63
 1.14 with sigma of 0.02
 C63-C64
 1.46 with sigma of 0.02
 N31-C73
 1.14 with sigma of 0.02
 C73-C74
 1.46 with sigma of 0.02
 N30-C71
 1.14 with sigma of 0.02
 C71-C72
 1.46 with sigma of 0.02
 N32-C75
 1.14 with sigma of 0.02
 C75-C76
 1.46 with sigma of 0.02
 N29-C69
 1.14 with sigma of 0.02
 C69-C70
 1.46 with sigma of 0.02
 N25-C61
 1.14 with sigma of 0.02
 C61-C62
 1.46 with sigma of 0.02
 N28-C67
 1.14 with sigma of 0.02
 C67-C68
 1.46 with sigma of 0.02
 N33-C77
 1.14 with sigma of 0.02
 N34-C79
 1.14 with sigma of 0.02
 C79-C80
 1.46 with sigma of 0.02
 N27-C65
 1.14 with sigma of 0.02
 C65-C66
 1.46 with sigma of 0.02
 F24-B6 = F22-B6 = F23-B6 = F21-B6 = F20-B5 = F19-B5 = F17-B5 = F18-B5 = F7-B2
 = F5-B2 = F6-B2 = F8-B2 = F3-B1 = F1-B1 = F2-B1 = F4-B1 = F16-B4 = F13-B4 =
 F14-B4 = F15-B4
 1.42 with sigma of 0.02
 N35-C81
 1.14 with sigma of 0.02
 C81-C82
 1.46 with sigma of 0.02
 F9-B3 = F12-B3 = F10-B3 = F11-B3
 1.42 with sigma of 0.02
 O1-C92 = O1-C89
 1.44 with sigma of 0.02
 N33-C78
 2.59 with sigma of 0.04
 N37-C86
 2.59 with sigma of 0.04
 N36-C84
 2.59 with sigma of 0.04
 N38-C88
 2.59 with sigma of 0.04
 N26-C64
 2.59 with sigma of 0.04
 N31-C74
 2.59 with sigma of 0.04
 N30-C72
 2.59 with sigma of 0.04
 N32-C76
 2.59 with sigma of 0.04
 N29-C70
 2.59 with sigma of 0.04
 N25-C62
 2.59 with sigma of 0.04
 N28-C68
 2.59 with sigma of 0.04
 N34-C80
 2.59 with sigma of 0.04
 N27-C66
 2.59 with sigma of 0.04
 N35-C82
 2.59 with sigma of 0.04
 C94-C93
 2.54 with sigma of 0.04
 C91-C90
 2.54 with sigma of 0.04
 F12-F9 \\sim F10-F11
 with sigma of 0.02
 F11-F9 \\sim F9-F10
 with sigma of 0.02
 F10-F11 \\sim F11-F9
 with sigma of 0.02
 F12-F11 \\sim F11-F10
 with sigma of 0.02
 F11-F10 \\sim F10-F12
 with sigma of 0.02
 C93-O1 \\sim O1-C94
 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.a Ternary CH refined with riding coordinates:
 C89(H89), C92(H92)
5.b Me refined with riding coordinates:
 C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C93(H93A,H93B,H93C), C94(H94A,H94B,
 H94C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C58(H58), C59(H59),
  C60(H60)
5.d Idealised Me refined as rotating group:
 C86(H86A,H86B,H86C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C72(H72A,H72B,
 H72C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C84(H84A,
 H84B,H84C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C),
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C88(H88A,H88B,H88C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 294 electrons were 
found in a volume of 1362\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4[C2H3N], 2.5[C2H3N] per Asymmetric Unit 
which account for 286 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11561
_shelx_hkl_checksum              77812
_shelx_fab_checksum              7068
_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 2.363
_oxdiff_exptl_absorpt_empirical_full_min 0.592