Highly selective synthesis and near-infrared photothermal conversion of metalla-Borromean ring and [2]catenane assemblies
Dang, Li-Long; Li, Ting-Ting; Zhang, Ting-Ting; Zhao, Ying; Chen, Tian; Gao, Xiang; Ma, Lufang; Jin, Guo-Xin; Chemical Science  (2022) –; doi:10.1039/D2SC00437B

data_1566751
_publ_section_title
;
 Highly selective synthesis and near-infrared photothermal conversion of
 metalla-Borromean ring and [2]catenane assemblies
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00437B
_journal_year                    2022
_chemical_formula_moiety         'C116 H116 N12 Rh4, 2(C F3 O3 S), 5[CF3SO3]'
_chemical_formula_sum            'C123 H116 F21 N12 O21 Rh4 S7'
_chemical_formula_weight         3133.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-01-06 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.206(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.6083(8)
_cell_length_b                   12.7106(5)
_cell_length_c                   23.5913(8)
_cell_measurement_reflns_used    8333
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      72.8690
_cell_measurement_theta_min      3.9260
_cell_volume                     6730.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -67.00  12.00   1.00    2.26    --  -40.73  57.00-120.00   79
  2  \w      1.00  49.00   1.00    2.26    --   40.73 -99.00 -60.00   48
  3  \w     35.00 133.00   1.00    4.00    --  107.58 -45.00 -90.00   98
  4  \w     95.00 172.00   1.00    4.00    --  107.58  30.00   0.00   77
  5  \w    103.00 176.00   1.00    4.00    --  107.58 125.00-120.00   73
  6  \w     98.00 178.00   1.00    4.00    --  107.58 125.00 -60.00   80
  7  \w    142.00 177.00   1.00    4.00    --  107.58 125.00 120.00   35
  8  \w     51.00 138.00   1.00    4.00    --  107.58 -77.00-180.00   87
  9  \w     49.00  99.00   1.00    4.00    --  107.58-125.00  90.00   50
 10  \w   -117.00  -8.00   1.00    2.26    --  -40.73 -77.00  90.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0604883000
_diffrn_orient_matrix_UB_12      0.0495507000
_diffrn_orient_matrix_UB_13      -0.0415947000
_diffrn_orient_matrix_UB_21      -0.0323969000
_diffrn_orient_matrix_UB_22      -0.0969712000
_diffrn_orient_matrix_UB_23      0.0103592000
_diffrn_orient_matrix_UB_31      -0.0026876000
_diffrn_orient_matrix_UB_32      0.0531967000
_diffrn_orient_matrix_UB_33      0.0574039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28919
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.311
_diffrn_reflns_theta_min         3.758
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       block
_exptl_crystal_F_000             3174
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.394
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         13295
_refine_ls_number_restraints     1143
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1217P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9136
_reflns_number_total             13295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00437b2.cif
_cod_data_source_block           p21c
_cod_database_code               1566751
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.570
_shelx_estimated_absorpt_t_min   0.499
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C16(H16), C26(H26), C28(H28), C31(H31), C32(H32),
 C35(H35), C37(H37), C40(H40), C41(H41), C45(H45), C48(H48), C51(H51), C52(H52)
4.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C),
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C43(H43A,H43B,
 H43C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 722 electrons were 
found in a volume of 2146\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[CF3SO3] per Asymmetric Unit 
which account for 730 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97020
_shelx_hkl_checksum              83393
_shelx_fab_checksum              32064
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.518
_oxdiff_exptl_absorpt_empirical_full_min 0.657