Confinement of a Au‒N-heterocyclic carbene in a Pd6L12 metal‒organic cage
Zeng, Lihua; Sun, Shujian; Wei, Zhang-Wen; Xin, Yu; Liu, Liping; Zhang, Jianyong; RSC Advances 10 (2020) 39323–39327; doi:10.1039/D0RA07509D

data_7241660
_publ_section_title
;
 Confinement of a Au--N-heterocyclic carbene in a Pd6L12 metal--organic
 cage
;
_journal_issue                   64
_journal_name_full               'RSC Advances'
_journal_page_first              39323
_journal_page_last               39327
_journal_paper_doi               10.1039/D0RA07509D
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C74 H84 Au2 I2 N8 Pd'
_chemical_formula_sum            'C74 H84 Au2 I2 N8 Pd'
_chemical_formula_weight         1839.62
_chemical_name_common            Pd6L12
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-02 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   29.8768(16)
_cell_length_b                   29.8768(16)
_cell_length_c                   74.341(3)
_cell_measurement_reflns_used    3995
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      44.4570
_cell_measurement_theta_min      4.1550
_cell_volume                     57468(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  33.00   1.00   65.00    --  -40.08  19.00 -90.00  108
  2  \w    113.00 178.00   1.00   22.50    --  109.06  30.00  30.00   65
  3  \w     37.00 131.00   1.00   22.50    --  109.06 -62.00-142.00   94
  4  \w    104.00 178.00   1.00   22.50    --  109.06  85.00 -27.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0124014000
_diffrn_orient_matrix_UB_12      -0.0180403000
_diffrn_orient_matrix_UB_13      -0.0177573000
_diffrn_orient_matrix_UB_21      -0.0414641000
_diffrn_orient_matrix_UB_22      -0.0562160000
_diffrn_orient_matrix_UB_23      0.0043119000
_diffrn_orient_matrix_UB_31      -0.0408920000
_diffrn_orient_matrix_UB_32      0.0080458000
_diffrn_orient_matrix_UB_33      -0.0097785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            13205
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        39.969
_diffrn_reflns_theta_max         39.969
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_description       block
_exptl_crystal_F_000             16092
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: EtOAc-DMSO'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.603
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         7693
_refine_ls_number_restraints     825
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0888
_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^)+(0.1620P)^2^+1993.3063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2668
_refine_ls_wR_factor_ref         0.2821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5908
_reflns_number_total             7693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra07509d2.cif
_cod_data_source_block           Pd6L12
_cod_original_cell_volume        57468(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7241660
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     P20
_shelx_estimated_absorpt_t_max   0.256
_shelx_estimated_absorpt_t_min   0.256
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.93
_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
 C52-C53 = C52-C54
 1.49 with sigma of 0.01
 C53-C54
 2.75 with sigma of 0.01
 N5-C38 = C39-C38 = C40-C39 = C41-C40 = C42-C41 = N5-C42
 1.39 with sigma of 0.01
 C5-C4 = N1-C5 = N1-C7BA = C7BA-C0CA = C3-C0CA = C4-C3
 1.39 with sigma of 0.01
 C6-C4
 1.5 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(I1) \\sim Ueq, Uanis(Au1) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C27(H27), C30(H30), C49(H49), C52(H52), C64(H64), C67(H67)
5.b Me refined with riding coordinates:
 C14(H14A,H14B,H14C)
5.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C35(H35), C34(H34), C37(H37), C3(H3), C0CA(H0CA), C7BA(H7BA),
 C5(H5), C7(H7), C11(H11), C20(H20), C19(H19), C23(H23), C25(H25), C42(H42),
 C38(H38), C39(H39), C40(H40), C48(H48), C44(H44), C57(H57), C56(H56), C62(H62),
  C74(H74), C73(H73), C72(H72), C71(H71)
5.d Fitted pentagon refined as free rotating group:
 C20(N3,C18,N2,C19), C57(N7,C55,N6,C56)
5.e Fitted hexagon refined as free rotating group:
 N4(C36,C35,C34,C33,C37), C24(C23,C22,C21,C26,C25), C46(C47,C48,C43,C44,C45),
 C61(C62,C63,C58,C59,C60), C70(C74,N8,C73,C72,C71)
5.f Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.266
_oxdiff_exptl_absorpt_empirical_full_min 0.605