Covalent Post-assembly Modification Triggers Structural Transformations of Borromean Rings.
Gao, Wen-Xi; Feng, Hui-Jun; Lin, Yue-Jian; Jin, Guo-Xin; Journal of the American Chemical Society 141 (2019) 9160–9164; doi:10.1021/jacs.9b02985

data_4128718
_publ_section_title
;
 Covalent Post-assembly Modification Triggers Structural Transformations
 of Borromean Rings.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9160
_journal_page_last               9164
_journal_paper_doi               10.1021/jacs.9b02985
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C76 H93 Cl4 F12 N8 O14.5 Rh4 S4'
_chemical_formula_weight         2260.26
_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   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                91.4880(10)
_cell_angle_beta                 100.9610(10)
_cell_angle_gamma                102.2630(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2462(4)
_cell_length_b                   18.9725(6)
_cell_length_c                   20.7122(6)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.88
_cell_measurement_theta_min      3.44
_cell_volume                     4605.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
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_diffrn_reflns_theta_max         54.894
_diffrn_reflns_theta_min         3.473
_exptl_absorpt_coefficient_mu    5.542
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             2282
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.420
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_refine_diff_density_max         2.055
_refine_diff_density_min         -1.835
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.00144(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         17265
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0716P)^2^+22.7131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15634
_reflns_number_total             17265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02985_si_003.cif
_cod_data_source_block           ga_90305f_a
_cod_original_formula_sum        'C76 H93 Cl4 F12 N8 O14.50 Rh4 S4'
_cod_database_code               4128718
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.168
_shelx_estimated_absorpt_t_max   0.247
_shelx_res_checksum              31644
_shelx_hkl_checksum              49032