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_1558866
_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            'C378 H613 Au9 Co6 N18 Na10 O301.5 S18'
_chemical_formula_weight         13167.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_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                90.00(4)
_cell_angle_beta                 97.93(4)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   48.570(8)
_cell_length_b                   28.050(8)
_cell_length_c                   52.051(10)
_cell_measurement_reflns_used    226850
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.821
_cell_measurement_theta_min      1.338
_cell_volume                     70236(3)
_computing_cell_refinement       HKL3000
_computing_data_collection
'<i>PAL BL2D-SMDC Program</i>(Shin et.al, 2016)'
_computing_data_reduction        HKL3000
_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_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.571
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_reflns_av_R_equivalents  0.1734
_diffrn_reflns_av_unetI/netI     0.3986
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.571
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            226850
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.509
_diffrn_reflns_theta_full        22.955
_diffrn_reflns_theta_max         29.821
_diffrn_reflns_theta_min         1.338
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       'hexagonal thin plate'
_exptl_crystal_F_000             26760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.850
_exptl_crystal_size_mid          0.670
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.571
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 13381 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.074(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6672
_refine_ls_number_reflns         134066
_refine_ls_number_restraints     44136
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.1974
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.2033
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.840
_reflns_Friedel_fraction_max     0.444
_reflns_number_gt                52614
_reflns_number_total             134066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03925j2.cif
_cod_data_source_block           3D
_cod_original_cell_volume        70236(28)
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C378 H613 Au9 Co6 N18 Na10 O301.50 S18'
_cod_database_code               1558866
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.338
_shelx_estimated_absorpt_t_max   0.829
_shelx_res_checksum              23987
_shelx_fab_checksum              31461