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_1566752
_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
'2(C100 H92 Ir4 N4 O8), 4(C1 F3 O3 S1), O6 S2, C2 F6, 0.56[CF3SO3], 5.2[CF3SO3]'
_chemical_formula_sum            'C211.76 H184 F35.28 Ir8 N8 O51.28 S11.76'
_chemical_formula_weight         6246.20
_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   mixed
_audit_creation_date             2022-03-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-31 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.140(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   21.3182(15)
_cell_length_b                   15.4343(10)
_cell_length_c                   19.1459(14)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      52.99
_cell_measurement_theta_min      3.09
_cell_volume                     6219.6(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'Bruker BIS V6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_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_temperature      173.00
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON III'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45180
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.901
_diffrn_reflns_theta_min         3.089
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.505
_exptl_absorpt_correction_T_max  0.7363
_exptl_absorpt_correction_T_min  0.5913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1387 before and 0.1028 after correction.
The Ratio of minimum to maximum transmission is 0.8031.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             3042
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         11342
_refine_ls_number_restraints     2089
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0690P)^2^+9.2966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8310
_reflns_number_total             11342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00437b2.cif
_cod_data_source_block           a
_cod_database_code               1566752
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.509
_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. Shared sites
{S2, C52}
{O10, F4}
{O9, F5}
{O8, F6}
3. Restrained distances
 C51-F2 = C51-F1 = C51-F3
 1.33 with sigma of 0.02
 C51-S1
 1.82 with sigma of 0.02
 S1-O6 = S1-O5 = S1-O7
 1.44 with sigma of 0.02
 C51-O6
 2.58 with sigma of 0.04
 C51-O7
 2.57 with sigma of 0.04
 C51-O5
 2.56 with sigma of 0.04
 F2-F1 \\sim F1-F3 \\sim F3-F2
 with sigma of 0.04
 S1-F2 \\sim S1-F1 \\sim S1-F3
 with sigma of 0.04
 C51-F2 \\sim C51-F1 \\sim C51-F3
 with sigma of 0.02
 S1-O6 \\sim S1-O5 \\sim S1-O7
 with sigma of 0.02
 O6-O5 \\sim O5-O7 \\sim O6-O7
 with sigma of 0.04
 C51-O6 \\sim C51-O5 \\sim C51-O7
 with sigma of 0.04
 C49A-C43A \\sim C50A-C44A \\sim C45A-C46A \\sim C41A-C47A \\sim C42A-C48A
 with sigma of 0.02
 C50-C44 \\sim C49-C43 \\sim C42-C48 \\sim C41-C47 \\sim C45-C46
 with sigma of 0.02
 C49-C48 \\sim C50-C49 \\sim C50-C46 \\sim C47-C46 \\sim C47-C48
 with sigma of 0.02
 C47A-C48A \\sim C49A-C48A \\sim C50A-C49A \\sim C50A-C46A \\sim C47A-C46A
 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ir1, O2, O1, N2, C35, C31, C34, C33, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C35 \\sim C33 \\sim C40 \\sim C31 \\sim C34 \\sim C32 \\sim C37 \\sim C36 \\sim
C39 \\sim C38: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C51 \\sim F2 \\sim F1 \\sim F3 \\sim S1 \\sim O6 \\sim O5 \\sim O7: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F1 \\sim C51 \\sim F2 \\sim F3 \\sim S1 \\sim O6 \\sim O5 \\sim O7: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
S2 \\sim C52 \\sim O9 \\sim O10 \\sim O8 \\sim F4 \\sim F5 \\sim F6: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C22 \\sim C23 \\sim C24: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
F1 \\sim C51 \\sim F2 \\sim F3 \\sim S1 \\sim O6 \\sim O5 \\sim O7 \\sim F3A
\\sim O7A \\sim S1A \\sim C51A \\sim O5A \\sim O6A \\sim F2A \\sim F1A: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C43 \\sim C44 \\sim C45 \\sim C41 \\sim C42 \\sim C50 \\sim C49 \\sim C46 \\sim
C47 \\sim C48 \\sim C43A \\sim C44A \\sim C45A \\sim C41A \\sim C42A \\sim C50A
\\sim C49A \\sim C46A \\sim C47A \\sim C48A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C46A \\sim C45A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(S2) = Uanis(C52)
Uanis(O10) = Uanis(F4)
Uanis(O8) = Uanis(F6)
Uanis(O9) = Uanis(F5)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C51, F2, F1, F3, S1, O6, O5, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O7A)=Sof(C51A)=Sof(F3A)=Sof(F2A)=Sof(F1A)=Sof(S1A)=Sof(O5A)=Sof(O6A)=1-
 FVAR(1)
 Sof(C51)=Sof(F2)=Sof(F1)=Sof(F3)=Sof(S1)=Sof(O6)=Sof(O5)=Sof(O7)=FVAR(1)
 Sof(C43A)=Sof(C44A)=Sof(C45A)=Sof(C41A)=Sof(C42A)=Sof(C50A)=Sof(H50D)=
 Sof(H50E)=Sof(H50F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C46A)=
 Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(2)
 Sof(C43)=Sof(C44)=Sof(C45)=Sof(C41)=Sof(C42)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=FVAR(2)
 Fixed Sof: S2(0.5) C52(0.5) O9(0.5) O10(0.5) O8(0.5) F4(0.5) F5(0.5) F6(0.5)
8.a Riding coordinates:
 C50(H50A,H50B,H50C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
8.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C)
8.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C27(H27), C17(H17), C28(H28), C22(H22), C19(H19), C23(H23), C1(H1),
 C12(H12), C20(H20), C10(H10), C2(H2), C9(H9), C5(H5), C13(H13), C4(H4)
8.d Fitted pentagon refined as free rotating group:
 C34(C33,C32,C31,C35), C43(C44,C45,C41,C42), C43A(C44A,C45A,C41A,C42A)
8.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C50A(H50D,H50E,H50F),
 C49A(H49D,H49E,H49F), C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F), C48A(H48D,
 H48E,H48F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 411 electrons were 
found in a volume of 1552\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.56[CF3SO3], 5.2[CF3SO3] per Asymmetric Unit 
which account for 420 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24463
_shelx_hkl_checksum              99909
_shelx_fab_checksum              169
_olex2_submission_special_instructions 'No special instructions were received'