π-Bonded molecular wires: self-assembly of mixed-valence cation-radical stacks within the nanochannels formed by inert tetrakis[3,5-bis(trifluoromethyl)phenyl]borate anions
Rosokha, Sergiy V.; Stern, Charlotte L.; Ritzert, Jeremy T.; CrystEngComm 15 (2013) 10638–; doi:10.1039/c3ce41719k

data_7211461
_publ_section_title
;
 \p-Bonded molecular wires: self-assembly of mixed-valence cation-radical
 stacks within the nanochannels formed by inert
 tetrakis[3,5-bis(trifluoromethyl)phenyl]borate anions
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              10638
_journal_paper_doi               10.1039/c3ce41719k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         '2(C20 H12), C32 H12 B F24'
_chemical_formula_sum            'C72 H36 B F24'
_chemical_formula_weight         1367.82
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-08-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.008(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.022(12)
_cell_length_b                   32.94(3)
_cell_length_c                   13.667(10)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      2.36
_cell_volume                     6394(9)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.24
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.5413
_exptl_absorpt_correction_T_min  0.4761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0937 before and 0.0814 after correction.
The Ratio of minimum to maximum transmission is 0.8795.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         9273
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0678P)^2^+2.8250P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5848
_reflns_number_total             9273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41719k.txt
_cod_data_source_block           n2959
_cod_database_code               7211461
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F2-C27 \\sim F3A-C27 \\sim F3-C27 \\sim F1A-C27 \\sim F1-C27 \\sim F2A-C27
 with sigma of 0.02
 F10A-C35 \\sim F11-C35 \\sim F11A-C35 \\sim F12-C35 \\sim F12A-C35 \\sim F10-C35
 with sigma of 0.02
3. Rigid bond restraints
 F3A, F2, F2A, F1, F1A, F3, F12, F12A, F10, F10A, F11, F11A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F3A \\sim F2 \\sim F2A \\sim F1 \\sim F1A \\sim F3 \\sim F12 \\sim F12A \\sim F10 \\sim F10A \\sim F11 \\sim F11A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C22(H22), C24(H24), C26(H26), C30(H30), C32(H32),
  C34(H34)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of the disordered solvent molecules from the refinement.
Only the atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 730.1 Ang^3 [11.4%]
Total electron count / cell = 224.6
;
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.946
_shelx_hkl_checksum              16852
_shelx_res_checksum              23992
_shelxl_version_number           2012-9