Selective Construction of Very Large Stacking-Interaction-Induced Molecular 818 Metalla-knots and Borromean Ring Using Curved Dipyridyl Ligands
Zhang, Hai-Ning; Lin, Yue-Jian; Jin, Guo-Xin; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11925

data_4135466
_publ_section_title
;
 Selective Construction of Very Large Stacking-Interaction-Induced
 Molecular 818 Metalla-knots and Borromean Ring Using Curved Dipyridyl
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11925
_journal_year                    2020
_chemical_formula_sum            'C150 H167 F12 N5 O26 Rh4 S4'
_chemical_formula_weight         3223.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                92.145(2)
_cell_angle_beta                 104.593(2)
_cell_angle_gamma                110.192(2)
_cell_formula_units_Z            1
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_cell_length_b                   18.5301(8)
_cell_length_c                   27.9838(12)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      54.87
_cell_measurement_theta_min      3.87
_cell_volume                     7401.9(6)
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_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            85932
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.952
_diffrn_reflns_theta_min         2.927
_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.320
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1761
_refine_ls_number_reflns         27993
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+14.7889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23794
_reflns_number_total             27993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11925_si_004.cif
_cod_data_source_block           4
_cod_database_code               4135466
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.266
_shelx_estimated_absorpt_t_max   0.426
_shelx_res_checksum              13384
_shelx_hkl_checksum              91671
_shelx_fab_checksum              86831