Selective and quantitative synthesis of a linear [3]catenane by two component coordination-driven self-assembly
Singh, Jatinder; Kim, Dong Hwan; Kim, Eun-Hee; Singh, Nem; Kim, Hyunuk; Hadiputra, Rizky; Jung, Jaehoon; Chi, Ki-Whan; Chemical Communications  (2019) –; doi:10.1039/C9CC03336J

data_7123482
_publ_section_title
;
 Selective and quantitative synthesis of a linear [3]catenane by two
 component coordination-driven self-assembly
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03336J
_journal_year                    2019
_chemical_formula_sum            'C104 H120.33 F8 N16 O20.5 Ru4 S2.67'
_chemical_formula_weight         2564.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-26 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   28.000(6)
_cell_length_b                   48.956(10)
_cell_length_c                   30.810(6)
_cell_measurement_reflns_used    183048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.63
_cell_volume                     40605(16)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.800
_diffrn_measured_fraction_theta_max 0.395
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.800
_diffrn_reflns_Laue_measured_fraction_max 0.395
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            107465
_diffrn_reflns_point_group_measured_fraction_full 0.769
_diffrn_reflns_point_group_measured_fraction_max 0.375
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.637
_diffrn_reflns_theta_min         1.354
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'HKL3000sm Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             15732
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.80(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4116
_refine_ls_number_reflns         58400
_refine_ls_number_restraints     2523
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1087
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2821
_refine_ls_wR_factor_ref         0.3212
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.738
_reflns_Friedel_fraction_max     0.356
_reflns_number_gt                30294
_reflns_number_total             58400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03336j2.cif
_cod_data_source_block           cc_sq
_cod_original_cell_volume        40605(15)
_cod_original_formula_sum        'C104 H120.33 F8 N16 O20.50 Ru4 S2.67'
_cod_database_code               7123482
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              25095
_shelx_hkl_checksum              65733
_shelx_fab_checksum              26922