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_7128954
_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
'C168 H118 N24 Pd6 S12, 8(C24 H20 B), 4[BPh4]'
_chemical_formula_sum            'C360 H278 B8 N24 Pd6 S12'
_chemical_formula_weight         6049.65
_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             2021-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-25 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                65.278(5)
_cell_angle_beta                 69.004(4)
_cell_angle_gamma                67.104(4)
_cell_formula_units_Z            1
_cell_length_a                   22.4855(10)
_cell_length_b                   22.5246(9)
_cell_length_c                   25.9711(13)
_cell_measurement_reflns_used    15402
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      50.8740
_cell_measurement_theta_min      3.5690
_cell_volume                     10701.9(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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      1.00  58.00   1.00    7.00    --    0.00  63.00 -76.00   57
  2  \w    -10.00  26.00   1.00    7.00    --    0.00 -63.00 146.00   36
  3  \w    -71.00 -18.00   1.00    7.00    --    0.00 -63.00 146.00   53
  4  \w     86.00 132.00   1.00   28.00    --   61.04  63.00 -76.00   46
  5  \w     30.00  89.00   1.00   28.00    --   61.04 -63.00 146.00   59
  6  \w     -1.00  26.00   1.00   28.00    --   61.04 -63.00 146.00   27
  7  \w    -87.00 -56.00   1.00    7.00    --    0.00 178.00-120.00   31
  8  \w    -58.00 -33.00   1.00   28.00    --  -55.50  63.00 -76.00   25
  9  \w   -101.00 -76.00   1.00   28.00    --  -55.50 -63.00 146.00   25
 10  \w    -10.00  56.00   1.00   28.00    --   61.04 -57.00   0.00   66
 11  \w     53.00  80.00   1.00   28.00    --   61.04 -77.00  90.00   27
 12  \w     -5.00  57.00   1.00   28.00    --   61.04 -19.00 120.00   62
 13  \w     -9.00  36.00   1.00   28.00    --   61.04 -77.00  90.00   45
 14  \w    -11.00  17.00   1.00   28.00    --   61.04 -19.00   0.00   28
 15  \w     61.00 101.00   1.00   28.00    --   61.04 -19.00   0.00   40
 16  \w     61.00 102.00   1.00   28.00    --   61.04-125.00 -60.00   41
 17  \w     45.00 126.00   1.00   28.00    --   61.04  38.00 -90.00   81
 18  \w     95.00 132.00   1.00   28.00    --   61.04  57.00 -60.00   37
 19  \w     18.00 101.00   1.00   28.00    --   61.04 -99.00  90.00   83
 20  \w     20.00  93.00   1.00   28.00    --   61.04 -77.00 120.00   73
 21  \w     35.00  83.00   1.00   28.00    --   61.04  57.00 -60.00   48
 22  \w      7.00  91.00   1.00   28.00    --   61.04 -99.00   0.00   84
 23  \w     41.00  66.00   1.00   28.00    --   61.04-125.00 -30.00   25
 24  \w     45.00  70.00   1.00   28.00    --   61.04  57.00  30.00   25
 25  \w    104.00 133.00   1.00   28.00    --   61.04  57.00  30.00   29
 26  \w     31.00  85.00   1.00   28.00    --   61.04-125.00   0.00   54
;
_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      0.0175506000
_diffrn_orient_matrix_UB_12      0.0633675000
_diffrn_orient_matrix_UB_13      -0.0490627000
_diffrn_orient_matrix_UB_21      0.0623415000
_diffrn_orient_matrix_UB_22      -0.0462633000
_diffrn_orient_matrix_UB_23      -0.0287724000
_diffrn_orient_matrix_UB_31      -0.0407009000
_diffrn_orient_matrix_UB_32      -0.0019326000
_diffrn_orient_matrix_UB_33      -0.0357215000
_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  0.1222
_diffrn_reflns_av_unetI/netI     0.1467
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57926
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        50.721
_diffrn_reflns_theta_max         50.721
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (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 light yellow'
_exptl_crystal_density_diffrn    0.939
_exptl_crystal_description       plate
_exptl_crystal_F_000             3114
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.003
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1516
_refine_ls_number_reflns         21834
_refine_ls_number_restraints     2993
_refine_ls_restrained_S_all      1.785
_refine_ls_R_factor_all          0.2797
_refine_ls_R_factor_gt           0.2192
_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          0.5045
_refine_ls_wR_factor_ref         0.5476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13360
_reflns_number_total             21834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03828a2.cif
_cod_data_source_block           rj-19
_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_cell_volume        10702.0(10)
_cod_database_code               7128954
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C456 H360 B12 N24 Pd6 S12'
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.545
_reflns_odcompleteness_completeness 96.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C36-C37
 1.5 with sigma of 0.01
 C145-B3 = C139-B3 = C133-B3 = C151-B3 = C169-B4 = C175-B4 = C157-B4 = C163-B4
 = C109-B2 = C127-B2 = C121-B2 = C115-B2 = C85-B1 = C91-B1 = C97-B1 = C103-B1
 1.65 with sigma of 0.01
 C48-C46
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N11: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
Uanis(N9) = Uanis(N8)
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), C4(H4), C5(H5), C29(H29), C30(H30), C32(H32), C33(H33),
 C47(H47), C45(H45), C44(H44), C43(H43), C27(H27), C28(H28), C25(H25), C26(H26),
  C52(H52), C55(H55), C56(H56), C66(H66), C68(H68), C69(H69), C70(H70),
 C62(H62), C65(H65), C64(H64), C63(H63), C39(H39), C42(H42), C41(H41), C40(H40),
  C75(H75), C76(H76), C78(H78), C79(H79), C84(H84), C83(H83), C81(H81),
 C80(H80), C12(H12), C13(H13), C14(H14), C11(H11), C7(H7), C8(H8), C15(H15),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C35(H35), C36(H36), C49(H49),
  C50(H50), C58(H58), C59(H59), C72(H72), C73(H73), C90(H90), C89(H89),
 C88(H88), C87(H87), C86(H86), C96(H96), C95(H95), C94(H94), C93(H93), C92(H92),
  C102(H102), C101(H101), C100(H100), C99(H99), C98(H98), C108(H108),
 C107(H107), C106(H106), C105(H105), C104(H104), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), C150(H150), C149(H149),
 C148(H148), C147(H147), C146(H146), C152(H152), C153(H153), C154(H154),
 C155(H155), C156(H156), C158(H158), C159(H159), C160(H160), C161(H161),
 C162(H162), C168(H168), C167(H167), C166(H166), C165(H165), C164(H164),
 C170(H170), C171(H171), C172(H172), C173(H173), C174(H174), C176(H176),
 C177(H177), C178(H178), C179(H179), C180(H180)
5.b Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N3(C29,C30,C31,C32,C33), N4(C47,C46,C45,C44,C43), N5(C27,
 C28,C24,C25,C26), N6(C52,C53,C54,C55,C56), N7(C66,C67,C68,C69,C70), N8(C62,C61,
 C65,C64,C63), N9(C39,C38,C42,C41,C40), N10(C75,C76,C77,C78,C79), N11(C84,C83,
 C82,C81,C80), N12(C12,C13,C14,C10,C11), C85(C90,C89,C88,C87,C86), C91(C96,C95,
 C94,C93,C92), C97(C102,C101,C100,C99,C98), C103(C108,C107,C106,C105,C104),
 C109(C110,C111,C112,C113,C114), C115(C116,C117,C118,C119,C120), C121(C122,C123,
 C124,C125,C126), C127(C128,C129,C130,C131,C132), C133(C134,C135,C136,C137,
 C138), C139(C140,C141,C142,C143,C144), C145(C150,C149,C148,C147,C146),
 C151(C152,C153,C154,C155,C156), C157(C158,C159,C160,C161,C162), C163(C168,C167,
 C166,C165,C164), C169(C170,C171,C172,C173,C174), C175(C176,C177,C178,C179,C180)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6480
_shelx_fab_checksum              52447
_olex2_date_sample_data_collection 2021-03-08
_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 1.754
_oxdiff_exptl_absorpt_empirical_full_min 0.663