Tuning the separation and coupling of corannulene trianion-radicals through sizable alkali metal belts
Spisak, Sarah N.; Rogachev, Andrey Yu.; Zabula, Alexander V.; Filatov, Alexander S.; Clérac, Rodolphe; Petrukhina, Marina A.; Chem. Sci. 8 (2017) 3137–; doi:10.1039/C6SC05370J

data_1545678
_publ_section_title
;
 Tuning the separation and coupling of corannulene trianion-radicals
 through sizable alkali metal belts
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              3137
_journal_paper_doi               10.1039/C6SC05370J
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C32 H38 Cs K2 O6'
_chemical_formula_sum            'C32 H38 Cs K2 O6'
_chemical_formula_weight         729.73
_chemical_name_systematic
; 
 [?5:Cs(diglyme)?6-K:?3-K(diglyme)(corannulene trianion)]

;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-11-11 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                64.4920(10)
_cell_angle_beta                 78.4840(10)
_cell_angle_gamma                71.7550(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8938(9)
_cell_length_b                   13.3712(12)
_cell_length_c                   15.5210(14)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.41
_cell_volume                     1755.0(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15218
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.241
_diffrn_reflns_theta_min         1.746
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0307 after correction.
The Ratio of minimum to maximum transmission is 0.6570.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_platon_squeeze_details          (replace
_refine_diff_density_max         1.644
_refine_diff_density_min         -2.941
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7805
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0432P)^2^+5.7556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7039
_reflns_number_total             7805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05370j2.cif
_cod_data_source_block           final
_cod_database_code               1545678
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4A-C27A \\sim O4-C27 \\sim O6A-C32A \\sim O6-C32 \\sim O3-C26 \\sim O1-C21
 with sigma of 0.02
 O3-C25 \\sim O1-C22 \\sim O6-C31 \\sim O6A-C31A \\sim O4-C28 \\sim O4A-C28A
 with sigma of 0.02
 O2-C23 \\sim O2-C24 \\sim O5-C29 \\sim O5A-C29A \\sim O5A-C30A \\sim O5-C30
 with sigma of 0.02
 C23-C22 \\sim C25-C24 \\sim C31A-C30A \\sim C31-C30 \\sim C29A-C28A \\sim
C29-C28
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cs1) = Uanis(Cs1A)
Uanis(C31) = Uanis(C31A)
Uanis(C29) = Uanis(C29A)
Uanis(C28) = Uanis(C28A)
Uanis(C32) = Uanis(C32A)
Uanis(O5A) = Uanis(O5)
Uanis(O4) = Uanis(O4A)
Uanis(C29) = Uanis(C29A) = Uanis(C30A) = Uanis(C30)
4. Rigid body (RIGU) restrains
 C27, O4, C28, C29, O5, C30, C31, O6, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cs1A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=
 Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(Cs1)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C28A(H28C,
 H28D), C29A(H29C,H29D), C30A(H30C,H30D), C31A(H31C,H31D), C22(H22A,H22B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14)
6.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C27A(H27D,H27E,H27F), C32A(H32D,
 H32E,H32F), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C)
;
_platon_squeeze_void_probe_radius 1.20