Construction of Pd-based coordination cages with three geometrically distinct ligands.
Li, Ru-Jin; de Montmollin, Jean; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00248a

data_7712856
_publ_section_title
;
 Construction of Pd-based coordination cages with three geometrically
 distinct ligands.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00248a
_journal_year                    2023
_chemical_formula_moiety         'C136 H88 N16 Pd4'
_chemical_formula_sum            'C136 H88 N16 Pd4'
_chemical_formula_weight         2371.82
_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             2023-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2023-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                91.918(2)
_cell_angle_beta                 109.850(3)
_cell_angle_gamma                91.610(2)
_cell_formula_units_Z            2
_cell_length_a                   19.4282(7)
_cell_length_b                   21.0392(5)
_cell_length_c                   24.7683(6)
_cell_measurement_reflns_used    30138
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      68.6190
_cell_measurement_theta_min      2.4120
_cell_volume                     9508.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     29.00  54.00   0.50   10.00    --   66.35 -95.00 175.00   50
  2  \w    -56.00 -30.00   0.50   10.00    --  -67.54  95.00 -74.00   52
  3  \w     31.00  77.00   0.50   10.00    --   68.22 -95.00 175.00   92
  4  \w    -69.00 -32.00   0.50   10.00    --  -70.49  95.00 -74.00   74
  5  \w     40.00  65.00   0.50   17.00    --   78.25 -95.00 175.00   50
  6  \w     42.00  67.00   0.50   17.00    --   79.39 -95.00 175.00   50
  7  \w     31.00  74.00   0.50   10.00    --   66.35-125.00  30.00   86
  8  \w     36.00  74.00   0.50   10.00    --   66.35 -95.00 120.00   76
  9  \w     37.00 111.00   0.50   10.00    --   66.35  15.00 -60.00  148
 10  \w     37.00 102.00   0.50   10.00    --   66.35  15.00-120.00  130
 11  \w   -105.00 -80.00   0.50   10.00    --  -67.54   0.00  60.00   50
 12  \w     31.00  71.00   0.50   10.00    --   68.22 -95.00  30.00   80
 13  \w     70.00 108.00   0.50   10.00    --   68.22  15.00-180.00   76
 14  \w     32.00  57.00   0.50   10.00    --   68.22 -95.00-120.00   50
 15  \w     37.00  66.00   0.50   10.00    --   68.22  15.00-180.00   58
 16  \w     26.00  95.00   0.50   10.00    --   68.22-125.00 120.00  138
 17  \w   -107.00 -75.00   0.50   10.00    --  -70.49   0.00-150.00   64
 18  \w    -97.00 -33.00   0.50   10.00    --  -70.49 125.00   0.00  128
 19  \w   -108.00 -76.00   0.50   10.00    --  -70.49   0.00   0.00   64
 20  \w    -96.00 -30.00   0.50   10.00    --  -70.49 125.00-150.00  132
 21  \w   -106.00 -33.00   0.50   10.00    --  -70.49   0.00  90.00  146
 22  \w   -106.00 -74.00   0.50   10.00    --  -70.49   0.00  60.00   64
 23  \w     94.00 120.00   0.50   17.00    --   73.81-154.00  97.27   52
 24  \w   -112.00 -38.00   0.50   17.00    --  -75.68 141.00 133.68  148
 25  \w   -122.00 -50.00   0.50   17.00    --  -75.68 159.00  18.59  144
 26  \w    -60.00 -35.00   0.50   17.00    --  -75.68 145.00 -65.83   50
 27  \w   -115.00 -87.00   0.50   17.00    --  -75.68 145.00 -65.83   56
 28  \w     39.00  71.00   0.50   17.00    --   78.25-125.00  60.00   64
 29  \w     79.00 104.00   0.50   17.00    --   78.25-125.00  90.00   50
 30  \w     47.00 123.00   0.50   17.00    --   78.25  15.00  90.00  152
 31  \w     78.00 105.00   0.50   17.00    --   78.25-125.00   0.00   54
 32  \w     43.00  72.00   0.50   17.00    --   78.25 -95.00-120.00   58
 33  \w     58.00  87.00   0.50   17.00    --   78.25 -95.00 -90.00   58
 34  \w     47.00 121.00   0.50   17.00    --   78.25  15.00-120.00  148
 35  \w     44.00  69.00   0.50   17.00    --   78.25-125.00  90.00   50
 36  \w     52.00 103.00   0.50   17.00    --   78.25-125.00-180.00  102
 37  \w     37.00  63.00   0.50   17.00    --   78.25-125.00   0.00   52
 38  \w     54.00  80.00   0.50   17.00    --   78.25  15.00  30.00   52
 39  \w     74.00 105.00   0.50   17.00    --   78.25-125.00  60.00   62
 40  \w     38.00 105.00   0.50   17.00    --   78.25-125.00-150.00  134
 41  \w     52.00 104.00   0.50   17.00    --   79.39  15.00-180.00  104
 42  \w     65.00 124.00   0.50   17.00    --   79.39  15.00 -60.00  118
 43  \w     81.00 106.00   0.50   17.00    --   79.39-125.00-120.00   50
 44  \w     55.00  80.00   0.50   17.00    --   79.39-125.00-120.00   50
 45  \w     43.00 103.00   0.50   17.00    --   79.39-125.00 -30.00  120
 46  \w     81.00 106.00   0.50   17.00    --   79.39-125.00 -60.00   50
 47  \w     81.00 106.00   0.50   17.00    --   79.39-125.00 120.00   50
 48  \w     56.00  83.00   0.50   17.00    --   79.39 -95.00 -30.00   54
 49  \w     81.00 106.00   0.50   17.00    --   79.39-125.00  30.00   50
 50  \w     81.00 106.00   0.50   17.00    --   79.39-125.00 -90.00   50
 51  \w     46.00  73.00   0.50   17.00    --   79.39-125.00 -90.00   54
 52  \w     81.00 106.00   0.50   17.00    --   79.39-125.00 150.00   50
 53  \w     81.00 106.00   0.50   17.00    --   79.39-125.00-180.00   50
 54  \w     92.00 119.00   0.50   17.00    --   79.39  15.00 -30.00   54
;
_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      0.0467530000
_diffrn_orient_matrix_UB_12      0.0008129000
_diffrn_orient_matrix_UB_13      -0.0392968000
_diffrn_orient_matrix_UB_21      -0.0619863000
_diffrn_orient_matrix_UB_22      -0.0372433000
_diffrn_orient_matrix_UB_23      -0.0475506000
_diffrn_orient_matrix_UB_31      -0.0330393000
_diffrn_orient_matrix_UB_32      0.0631621000
_diffrn_orient_matrix_UB_33      -0.0240166000
_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  0.0789
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70982
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        39.973
_diffrn_reflns_theta_max         39.973
_diffrn_reflns_theta_min         2.420
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.278
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
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    0.828
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.671
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         11503
_refine_ls_number_restraints     2382
_refine_ls_restrained_S_all      1.574
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.1177
_refine_ls_shift/su_max          0.000
_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          0.3805
_refine_ls_wR_factor_ref         0.4032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7922
_reflns_number_total             11503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00248a2.cif
_cod_data_source_block           rj-100
_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 
;
_cod_original_cell_volume        9508.8(5)
_cod_database_code               7712856
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C136 H88 N16 Pd4 B8 F32'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.622
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C126-C124 = C132-C130 = C104-C103 = C102-C100 = C96-C95 = C94-C91 = C8-C7 =
 C6-C4 = C24-C22 = C18-C16 = C34-C31 = C36-C35 = C42-C40 = C44-C43 = C116-C115 =
  C114-C112 = C64-C63 = C62-C60 = C56-C55 = C54-C51 = C74-C71 = C76-C75 = C82-
 C80 = C84-C83
 1.5 with sigma of 0.01
 C115-C114 = C7-C6 = C43-C42 = C83-C82 = C75-C74 = C35-C34 = C95-C94 = C55-C54
 = C63-C62 = C103-C102
 1.15 with sigma of 0.01
 C127-C124 \\sim C124-C131
 with sigma of 0.02
 C129-C132 \\sim C132-C131
 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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C12(H12), C11(H11), C10(H10),
 C13(H13), C14(H14), C15(H15), C17(H17), C25(H25), C28(H28), C27(H27), C26(H26),
  C33(H33), C32(H32), C30(H30), C29(H29), C66(H66), C65(H65), C68(H68),
 C67(H67), C69(H69), C70(H70), C72(H72), C73(H73), C87(H87), C88(H88), C85(H85),
  C86(H86), C93(H93), C92(H92), C90(H90), C89(H89), C109(H109), C110(H110),
 C111(H111), C113(H113), C117(H117), C120(H120), C119(H119), C118(H118),
 C121(H121), C122(H122), C123(H123), C125(H125), C23(H23), C21(H21), C20(H20),
 C19(H19), C37(H37), C38(H38), C39(H39), C41(H41), C45(H45), C46(H46), C47(H47),
  C48(H48), C50(H50), C49(H49), C53(H53), C52(H52), C59(H59), C58(H58),
 C57(H57), C61(H61), C81(H81), C77(H77), C78(H78), C79(H79), C101(H101),
 C99(H99), C98(H98), C97(H97), C108(H108), C107(H107), C106(H106), C105(H105),
 C127(H127), C128(H128), C129(H129), C131(H131), C136(H136), C135(H135),
 C134(H134), C133(H133)
5.b Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C9,C8,C12,C11,C10), N3(C13,C14,C15,C16,C17), N4(C25,
 C24,C28,C27,C26), N5(C33,C32,C31,C30,C29), N8(C66,C65,C64,C68,C67), N9(C69,C70,
 C71,C72,C73), N10(C87,C88,C84,C85,C86), N11(C93,C92,C91,C90,C89), N13(C109,
 C110,C111,C112,C113), N14(C117,C116,C120,C119,C118), N15(C121,C122,C123,C124,
 C125), C18(C23,C22,C21,C20,C19), C36(C37,C38,C39,C40,C41), C51(C50,C49,N7,C53,
 C52), C60(C59,C58,C57,C56,C61), C80(C81,C76,C77,C78,C79), C96(C101,C100,C99,
 C98,C97), C104(C108,C107,N12,C106,C105), C126(C127,C128,C129,C130,C131),
 C132(C136,C135,C134,N16,C133)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78151
_shelx_hkl_checksum              980
_shelx_fab_checksum              88159
_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 12.104
_oxdiff_exptl_absorpt_empirical_full_min 0.193