Orientational self-sorting: formation of structurally defined Pd<sub>4</sub>L<sub>8</sub> and Pd<sub>6</sub>L<sub>12</sub> cages from low-symmetry dipyridyl ligands.
Li, Ru-Jin; Marcus, Adam; Fadaei-Tirani, Farzaneh; Severin, Kay; Chemical communications (Cambridge, England) 57 (2021) 10023–10026; doi:10.1039/d1cc03828a

data_7128955
_publ_section_title
;
 Orientational self-sorting: formation of structurally defined
 Pd<sub>4</sub>L<sub>8</sub> and Pd<sub>6</sub>L<sub>12</sub> cages from
 low-symmetry dipyridyl ligands.
;
_journal_issue                   78
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10023
_journal_page_last               10026
_journal_paper_doi               10.1039/d1cc03828a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C128 H96 N16 Pd4, B4 F16 Na, 2(C24 H20 B), 3(B F4)'
_chemical_formula_sum            'C176 H136 B9 F28 N16 Na Pd4'
_chemical_formula_weight         3552.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-06-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-29 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.1520(5)
_cell_length_b                   39.3021(10)
_cell_length_c                   33.9980(6)
_cell_measurement_reflns_used    22489
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.7250
_cell_measurement_theta_min      3.1550
_cell_volume                     40288.9(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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    -60.00  12.00   1.00   12.50    --  -41.04  96.00  71.00   72
  2  \w     16.00  73.00   1.00   12.50    --   41.04 -96.00 -37.00   57
  3  \w     66.00 100.00   1.00   55.00    --  105.15 -96.00 -37.00   34
  4  \w    108.00 178.00   1.00   55.00    --  105.15  96.00  71.00   70
  5  \w   -110.00 -17.00   1.00   12.50    --  -41.04 -38.00-120.00   93
  6  \w     22.00  49.00   1.00   12.50    --   41.04  38.00 -90.00   27
  7  \w     63.00 107.00   1.00   12.50    --   41.04  38.00 -90.00   44
  8  \w      9.00  79.00   1.00   12.50    --   41.04 -99.00-180.00   70
  9  \w     64.00 144.00   1.00   55.00    --  105.15 178.00 150.00   80
 10  \w     30.00  85.00   1.00   55.00    --  105.15-111.00-120.00   55
 11  \w     42.00  80.00   1.00   55.00    --  105.15 -61.00 -30.00   38
 12  \w     77.00 177.00   1.00   55.00    --  105.15  61.00 120.00  100
 13  \w    104.00 143.00   1.00   55.00    --  105.15  77.00   0.00   39
 14  \w    104.00 169.00   1.00   55.00    --  105.15 111.00-150.00   65
 15  \w    109.00 143.00   1.00   55.00    --  105.15 111.00 -60.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159508000
_diffrn_orient_matrix_UB_12      -0.0350271000
_diffrn_orient_matrix_UB_13      -0.0146434000
_diffrn_orient_matrix_UB_21      -0.0484766000
_diffrn_orient_matrix_UB_22      -0.0108344000
_diffrn_orient_matrix_UB_23      -0.0070330000
_diffrn_orient_matrix_UB_31      0.0025095000
_diffrn_orient_matrix_UB_32      0.0138862000
_diffrn_orient_matrix_UB_33      -0.0422959000
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            97504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.696
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.311
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
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            'clear pale yellow'
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       prism
_exptl_crystal_F_000             14368
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.185
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         19734
_refine_ls_number_restraints     1847
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0985
_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^)+(0.1798P)^2^+212.6869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2831
_refine_ls_wR_factor_ref         0.3227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13293
_reflns_number_total             19734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03828a2.cif
_cod_data_source_block           rj-20
_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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7128954--7128955.cif.
;
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               7128955
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C176 H136 B10 F32 N16 Na Pd4'
_shelx_estimated_absorpt_t_max   0.422
_shelx_estimated_absorpt_t_min   0.344
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B2-F2 = B2-F3 = B2-F1 = B2-F4
 1.42 with sigma of 0.02
 F9A-B4 = F10B-B4 = F12B-B4 = F11A-B4 = F15B-B6 = F16B-B6
 1.42 with sigma of 0.02
 F10A-B4 = F9B-B4 = F12A-B4 = F11B-B4
 1.42 with sigma of 0.02
 F15B-B6 = F15A-B6 = F16B-B6 = F16A-B6
 1.42 with sigma of 0.02
 F14-B5 = F13-B5
 1.42 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(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(1)
 Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(1)
 Fixed Sof: F13(0.5) F14(0.5) B5(0.25) F15A(0.25) F15B(0.25) F16A(0.25)
 F16B(0.25) B6(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
  C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C43(H43),
  C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52),
 C53(H53), C55(H55), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62), C63(H63),
  C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72),
 C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C79(H79), C80(H80), C81(H81),
  C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64869
_shelx_fab_checksum              46666
_olex2_date_sample_data_collection 2021-04-15
_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 2.263
_oxdiff_exptl_absorpt_empirical_full_min 0.507