Stretching [8]cycloparaphenylene with encapsulated potassium cations: structural and theoretical insights into core perturbation upon four-fold reduction and complexation
Rogachev, Andrey Yu.; Zhou, Zheng; Liu, Shuyang; Wei, Zheng; Schaub, Tobias A.; Jasti, Ramesh; Petrukhina, Marina A.; Chemical Science  (2021) –; doi:10.1039/D1SC00713K

data_1561668
_publ_section_title
;
 Stretching [8]cycloparaphenylene with encapsulated potassium cations:
 structural and theoretical insights into core perturbation upon four-fold
 reduction and complexation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC00713K
_journal_year                    2021
_chemical_formula_moiety         '0.5(C160 H192 K8 O16)'
_chemical_formula_sum            'C80 H96 K4 O8'
_chemical_formula_weight         1341.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-23 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.196(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.330(7)
_cell_length_b                   10.120(3)
_cell_length_c                   31.991(8)
_cell_measurement_reflns_used    8534
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.84
_cell_volume                     7136(4)
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1743
_diffrn_reflns_av_unetI/netI     0.1248
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            39344
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.842
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.6885
_exptl_absorpt_correction_T_min  0.5580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was 
used for absorption correction. wR2(int) was 
0.0965 before and 0.0728 after correction. 
The Ratio of minimum to maximum transmission 
is 0.8105. The \l/2 correction factor is not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       plate
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6517
_refine_ls_number_restraints     1175
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.2049
_refine_ls_R_factor_gt           0.1508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+341.9939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3157
_refine_ls_wR_factor_ref         0.3469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4413
_reflns_number_total             6517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00713k2.cif
_cod_data_source_block           str2844
_cod_original_cell_volume        7136(3)
_cod_database_code               1561668
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.886(3)
 0.114(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C30-C29 = C31-C32 = C30-C31
 1.54 with sigma of 0.02
 O2-C32 = O2-C29
 1.43 with sigma of 0.02
 C31-C32 = C30-C31 = C30-C29
 1.54 with sigma of 0.02
 O1-C28 = O1X-C28X = O1-C25 = O1X-C25X
 1.43 with sigma of 0.02
 C27X-C28X = C27-C28 = C26-C27 = C26X-C27X = C25-C26 = C25X-C26X
 1.54 with sigma of 0.02
 O4-C37X = O4-C37 = O4-C40X = O4-C40
 1.43 with sigma of 0.02
 C38X-C37X = C38-C37 = C39X-C38X = C39-C38 = C39-C40 = C39X-C40X
 1.54 with sigma of 0.02
 O3-C36 = O3-C33
 1.43 with sigma of 0.02
 C34X-C33X = C35-C36 = C35-C34 = C35X-C34X = C34-C33 = C35X-C36X
 1.54 with sigma of 0.02
 O2-C29 = O2-C32
 1.43 with sigma of 0.02
 C30-C29 = C30X-C29X = C32-C31 = C32X-C31X = C31X-C30X = C31-C30
 1.54 with sigma of 0.02
 O2-C29 = O2-C29X = O2-C32 = O2-C32X
 1.43 with sigma of 0.02
 O3-C33X = O3-C36 = O3-C36X = O3-C33
 1.43 with sigma of 0.02
 O1-C28 \\sim O1X-C28X
 with sigma of 0.02
 O1-C25 \\sim O1X-C25X
 with sigma of 0.02
 C28-C27 \\sim C28X-C27X
 with sigma of 0.02
 C27-C26 \\sim C27X-C26X
 with sigma of 0.02
 C26-C25 \\sim C26X-C25X
 with sigma of 0.02
 O1-C27 \\sim O1X-C27X
 with sigma of 0.04
 O1-C26 \\sim O1X-C26X
 with sigma of 0.04
 C28-C26 \\sim C28X-C26X
 with sigma of 0.04
 C28-C25 \\sim C28X-C25X
 with sigma of 0.04
 C27-C25 \\sim C27X-C25X
 with sigma of 0.04
 C37-C38 \\sim C37X-C38X
 with sigma of 0.02
 C40-C39 \\sim C40X-C39X
 with sigma of 0.02
 C38-C39 \\sim C38X-C39X
 with sigma of 0.02
 C37-C40 \\sim C37X-C40X
 with sigma of 0.04
 C37-C39 \\sim C37X-C39X
 with sigma of 0.04
 C40-C38 \\sim C40X-C38X
 with sigma of 0.04
 C33-C34 \\sim C36X-C35X
 with sigma of 0.02
 C36-C35 \\sim C33X-C34X
 with sigma of 0.02
 C34-C35 \\sim C35X-C34X
 with sigma of 0.02
 C33-C36 \\sim C36X-C33X
 with sigma of 0.04
 C33-C35 \\sim C36X-C34X
 with sigma of 0.04
 C36-C34 \\sim C33X-C35X
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O3 \\sim C33 \\sim C36 \\sim C34 \\sim C35 \\sim C36X \\sim C33X \\sim C35X
\\sim C34X \\sim O4 \\sim C37 \\sim C40 \\sim C38 \\sim C39 \\sim C37X \\sim
C40X \\sim C38X \\sim C39X \\sim O1 \\sim C28 \\sim C27 \\sim C26 \\sim C25
\\sim O1X \\sim C28X \\sim C27X \\sim C26X \\sim C25X \\sim O2 \\sim C29 \\sim
C32 \\sim C31 \\sim C30: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C24 \\sim C23 \\sim C19 \\sim C22 \\sim C20 \\sim C21 \\sim C15 \\sim C17 \\sim
C16 \\sim C13 \\sim C14 \\sim C18 \\sim C9 \\sim C12 \\sim C10 \\sim C3 \\sim
C1 \\sim C6 \\sim C11 \\sim C7 \\sim C2 \\sim C8 \\sim C5 \\sim C4: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
O2 \\sim C29 \\sim C32 \\sim C31 \\sim C30 \\sim C31X \\sim C32X \\sim C30X
\\sim C29X: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) = Uanis(C17)
Uanis(C15) = Uanis(C18)
5. Rigid body (RIGU) restrains
 O3, C33, C36, C34, C35, C36X, C33X, C35X, C34X, O4, C37, C40, C38, C39, C37X,
 C40X, C38X, C39X, O1, C28, C27, C26, C25, O1X, C28X, C27X, C26X, C25X, O2, C29,
  C32, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C23, C19, C22, C20, C21, C15, C17, C16, C13, C14, C18, C9, C12, C10, C3,
 C1, C6, C11, C7, C2, C8, C5, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C29, C32, C31, C30, C31X, C32X, C30X, C29X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C31X)=Sof(H31C)=Sof(H31D)=Sof(C32X)=Sof(H32C)=Sof(H32D)=Sof(C30X)=
 Sof(H30C)=Sof(H30D)=Sof(C29X)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(1)
 Sof(O1X)=Sof(C28X)=Sof(H28C)=Sof(H28D)=Sof(C27X)=Sof(H27C)=Sof(H27D)=
 Sof(C26X)=Sof(H26C)=Sof(H26D)=Sof(C25X)=Sof(H25C)=Sof(H25D)=1-FVAR(2)
 Sof(O1)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(2)
 Sof(C37X)=Sof(H37C)=Sof(H37D)=Sof(C40X)=Sof(H40C)=Sof(H40D)=Sof(C38X)=
 Sof(H38C)=Sof(H38D)=Sof(C39X)=Sof(H39C)=Sof(H39D)=1-FVAR(3)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(3)
 Sof(C36X)=Sof(H36C)=Sof(H36D)=Sof(C33X)=Sof(H33C)=Sof(H33D)=Sof(C35X)=
 Sof(H35C)=Sof(H35D)=Sof(C34X)=Sof(H34C)=Sof(H34D)=1-FVAR(4)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C33(H33A,H33B), C28(H28A,H28B), C40(H40A,H40B), C36(H36A,
 H36B), C34(H34A,H34B), C27(H27A,H27B), C38(H38A,H38B), C26(H26A,H26B),
 C25(H25A,H25B), C39(H39A,H39B), C35(H35A,H35B), C29(H29A,H29B), C32(H32A,H32B),
  C31(H31A,H31B), C30(H30A,H30B), C28X(H28C,H28D), C27X(H27C,H27D), C26X(H26C,
 H26D), C25X(H25C,H25D), C37X(H37C,H37D), C40X(H40C,H40D), C38X(H38C,H38D),
 C39X(H39C,H39D), C36X(H36C,H36D), C33X(H33C,H33D), C35X(H35C,H35D), C34X(H34C,
 H34D), C31X(H31C,H31D), C32X(H32C,H32D), C30X(H30C,H30D), C29X(H29C,H29D)
7.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C9(H9), C17(H17), C12(H12), C24(H24), C14(H14), C1(H1), C18(H18),
 C23(H23), C11(H11), C2(H2), C8(H8), C5(H5), C4(H4), C20(H20), C21(H21)
;
_shelx_res_checksum              65104
_shelx_hkl_checksum              65666
_olex2_submission_special_instructions 'No special instructions were received'