Self-assembly of Cyclic Hexamers of γ-Cyclodextrin in a Metallosupramolecular Framework with D-Penicillamine
Somsri, Supattra; Kuwamura, Naoto; Kojima, Tatsuhiro; Yoshinari, Nobuto; Konno, Takumi; Chemical Science  (2020) –; doi:10.1039/D0SC03925J

data_1558864
_publ_section_title
;
 Self-assembly of Cyclic Hexamers of \g-Cyclodextrin in a
 Metallosupramolecular Framework with D-Penicillamine
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03925J
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C30 H54 Au3 Co2 N6 Na3.33 O45 S6'
_chemical_formula_weight         2196.54
_space_group_crystal_system      cubic
_space_group_IT_number           199
_space_group_name_Hall           'I 2b 2c 3'
_space_group_name_H-M_alt        'I 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-29 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   41.407(3)
_cell_length_b                   41.407(3)
_cell_length_c                   41.407(3)
_cell_measurement_reflns_used    141507
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.007
_cell_measurement_theta_min      0.588
_cell_volume                     70994(9)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'RIGAKU 1/4chi goniometer with PILATUS3 X CdTe 1M'
_diffrn_measurement_method       'w scan'
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4248
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            141507
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.766
_diffrn_reflns_theta_max         16.007
_diffrn_reflns_theta_min         0.588
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.617
_exptl_crystal_description       'truncated hexagonal pyramid'
_exptl_crystal_F_000             12716
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.749
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 5263 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         27154
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0428P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15051
_reflns_number_total             27154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03925j2.cif
_cod_data_source_block           2L
_cod_original_cell_volume        70996(17)
_cod_database_code               1558864
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.902
_shelx_res_checksum              84692
_shelx_fab_checksum              97169