Self-assembly and guest-induced disassembly of triply interlocked [2]catenanes.
Zhang, Ying-Ying; Qiu, Feng-Yi; Shi, Hua-Tian; Yu, Weibin; Chemical communications (Cambridge, England) 57 (2021) 3010–3013; doi:10.1039/d0cc08052g

data_7127913
_publ_section_title
;
 Self-assembly and guest-induced disassembly of triply interlocked
 [2]catenanes.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3010
_journal_page_last               3013
_journal_paper_doi               10.1039/d0cc08052g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C144 H132 N6 O12 Rh6, 4(C F3 O3 S), 2[C1F3O3S], 6[C2H3N], 4[C4H10O]'
_chemical_formula_sum            'C178 H190 F18 N12 O34 Rh6 S6'
_chemical_formula_weight         4193.23
_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_date             2021-02-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.01.30 svn.rb'd11e6e19' for OlexSys, GUI svn.r6224)
;
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                70.629(4)
_cell_angle_beta                 81.477(3)
_cell_angle_gamma                72.911(4)
_cell_formula_units_Z            2
_cell_length_a                   17.6122(10)
_cell_length_b                   22.2298(14)
_cell_length_c                   26.3632(14)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.61
_cell_measurement_theta_min      2.36
_cell_volume                     9292.7(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            243712
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.916
_diffrn_reflns_theta_min         1.779
_exptl_absorpt_coefficient_mu    5.620
_exptl_absorpt_correction_T_max  0.324
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4284
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1822
_refine_ls_number_reflns         37934
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1284P)^2^+0.4845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24530
_reflns_number_total             37934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08052g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7127913--7127914.cif.'
_cod_database_code               7127913
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.302
_shelx_estimated_absorpt_t_min   0.237
_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. Restrained distances
 S6-F3 = S6-F4 = S6-F5
 2.6 with sigma of 0.03
 O13-O14 = O13-O15 = O14-O15
 2.4 with sigma of 0.02
 S6-O13 = S6-O14 = S6-O15
 1.43 with sigma of 0.02
 S6-C1A
 1.8 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.04
 S2-F7 \\sim S2-F8 \\sim S2-F9
 with sigma of 0.04
 C1C-O19 \\sim C1C-O1A \\sim C1C-O1B
 with sigma of 0.04
 O19-O1A \\sim O1A-O1B \\sim O19-O1B
 with sigma of 0.04
 C1C-F7 \\sim C1C-F8 \\sim C1C-F9
 with sigma of 0.02
 S2-O19 \\sim S2-O1A \\sim S2-O1B
 with sigma of 0.02
 C1B-F1 \\sim C1B-F2 \\sim C1B-F6
 with sigma of 0.02
 C1B-O16 \\sim C1B-O17 \\sim C1B-O18
 with sigma of 0.04
 O1C-O1D \\sim O1D-O1E \\sim O1C-O1E
 with sigma of 0.04
 O16-O17 \\sim O17-O18 \\sim O16-O18
 with sigma of 0.04
 S3-F10 \\sim S3-F11 \\sim S3-F12
 with sigma of 0.04
 S1-O16 \\sim S1-O17 \\sim S1-O18
 with sigma of 0.02
 C1D-F10 \\sim C1D-F11 \\sim C1D-F12
 with sigma of 0.02
 S1-F1 \\sim S1-F2 \\sim S1-F6
 with sigma of 0.04
 F1-F2 \\sim F2-F6 \\sim F6-F1
 with sigma of 0.04
 C1D-O1C \\sim C1D-O1D \\sim C1D-O1E
 with sigma of 0.04
 C1A-O13 \\sim C1A-O14 \\sim C1A-O15
 with sigma of 0.04
 F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.04
 S3-O1C \\sim S3-O1D \\sim S3-O1E
 with sigma of 0.02
 C1A-F3 \\sim C1A-F4 \\sim C1A-F5
 with sigma of 0.02
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(S6) = Uanis(S3)
4.a Riding coordinates:
 C71(H71A,H71B,H71C), C140(H14A,H14B,H14C)
4.b Me refined with riding coordinates:
 C132(H13G,H13H,H13I)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C13(H13), C17(H17),
 C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C36(H36), C38(H38), C40(H40), C44(H44),
 C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56), C62(H62), C63(H63), C85(H85), C86(H86), C92(H92), C93(H93),
 C115(H115), C116(H116), C122(H122), C123(H123)
4.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,
 H74C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C), C84(H84A,H84B,H84C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C102(H10G,H10H,H10I), C103(H10J,H10K,H10L), C104(H10M,H10N,H10O), C110(H11A,
 H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C113(H11J,H11K,H11L),
 C114(H11M,H11N,H11O), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C133(H13J,
 H13K,H13L), C134(H13M,H13N,H13O), C141(H14D,H14E,H14F), C142(H14G,H14H,H14I),
 C143(H14J,H14K,H14L), C144(H14M,H14N,H14O)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 897 electrons were 
found in a volume of 3052\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C1F3O3S], 6[C2H3N] and
4[C4H10O] per Formula Unit which account for 892 electrons 
per unit cell.

The decision to mask two triflate counter ions was not taken lightly, but
all other chemical evidence as well as the requirement of the charge balance
leave no other conclusion: two triflates are hiding in the solvent sphere.
The full, un-masked hkl is embedded in the CIF and, if you can do better 
than us, please feel free to do so.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98069
_shelx_fab_checksum              66705
_olex2_submission_special_instructions 'No special instructions were received'