The first quantitative synthesis of a closed three‒link chain (6<sup>3</sup><sub>1</sub>) using coordination and non-covalent interactions‒driven self‒assembly.
Singh, Jatinder; Kim, Dong Hwan; Kim, Eun-Hee; Kim, Hyunuk; Hadiputra, Rizky; Jung, Jaehoon; Chi, Ki-Whan; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01406

data_4134910
_publ_section_title
;
 The first quantitative synthesis of a closed three--link chain
 (6<sup>3</sup><sub>1</sub>) using coordination and non-covalent
 interactions--driven self--assembly.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01406
_journal_year                    2020
_chemical_formula_sum            'C115.01 H107.4 F12 N12.64 O23.65 Ru4 S4'
_chemical_formula_weight         2805.53
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   42.315(6)
_cell_length_b                   42.315(6)
_cell_length_c                   19.337(4)
_cell_measurement_reflns_used    71117
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      0.81
_cell_volume                     29985(9)
_computing_cell_refinement       'DENZO (Z. Otwinowski and W. Minor, 1997)'
_computing_data_collection       'ADSC Quantum software'
_computing_data_reduction        'HKL3000 (Z. Otwinowski and W. Minor, 1997)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  'Diamond 4'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39534
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        22.882
_diffrn_reflns_theta_max         22.882
_diffrn_reflns_theta_min         1.508
_diffrn_source                   synchrotron-PAL
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             12808
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.59(5)
_refine_ls_extinction_coef       0.0045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1571
_refine_ls_number_reflns         16752
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1953P)^2^+1.1765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2272
_refine_ls_wR_factor_ref         0.2367
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.840
_reflns_Friedel_fraction_max     0.840
_reflns_number_gt                15196
_reflns_number_total             16752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01406_si_002.cif
_cod_data_source_block           r3_sq
_cod_original_cell_volume        29986(10)
_cod_original_formula_sum        'C115.01 H107.40 F12 N12.64 O23.65 Ru4 S4'
_cod_database_code               4134910
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              8541
_shelx_hkl_checksum              98889
_shelx_fab_checksum              84790