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_7211459
_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         '3(C10 H12 Se4), 2(C32 H12 B F24), C6 H14'
_chemical_formula_sum            'C100 H74 B2 F48 Se12'
_chemical_formula_weight         3156.73
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2013-05-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                75.3559(15)
_cell_angle_beta                 88.6776(15)
_cell_angle_gamma                68.4075(14)
_cell_formula_units_Z            2
_cell_length_a                   15.8147(5)
_cell_length_b                   18.6849(6)
_cell_length_c                   21.3439(7)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.68
_cell_measurement_theta_min      3.18
_cell_volume                     5656.8(3)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            101263
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.823
_diffrn_reflns_theta_min         2.146
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.5535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.7355.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       needle
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1544
_refine_ls_number_reflns         18797
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+11.7101P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14695
_reflns_number_total             18797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41719k.txt
_cod_data_source_block           n2789
_cod_database_code               7211459
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F42-C86 \\sim F42A-C86 \\sim F41-C86 \\sim F41A-C86 \\sim F40-C86 \\sim F40A-C86
 with sigma of 0.01
 F21-C61 \\sim F21A-C61 \\sim F19-C61 \\sim F19A-C61 \\sim F20-C61 \\sim F20A-C61
 with sigma of 0.01
 C99A-C1A \\sim C99-C100 \\sim C99A-C98 \\sim C99-C98
 with sigma of 0.02
3. Rigid bond restraints
 F40A, F42, F42A, F41, F41A, F40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F21, F21A, F19, F19A, F20, F20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99A, C99, C1A, C100
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F40A \\sim F42 \\sim F42A \\sim F41 \\sim F41A \\sim F40: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F21 \\sim F21A \\sim F19 \\sim F19A \\sim F20 \\sim F20A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C99A \\sim C99 \\sim C1A \\sim C100: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F40A)=Sof(F41A)=Sof(F42A)=1-FVAR(1)
 Sof(F40)=Sof(F41)=Sof(F42)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Sof(H98C)=Sof(H98D)=Sof(C99A)=Sof(H99C)=Sof(H99D)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=1-FVAR(3)
 Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C100)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C98(H98C,H98D), C99(H99A,
 H99B), C99A(H99C,H99D)
6.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C95(H95A,H95B,H95C), C100(H10A,H10B,
 H10C), C1A(H1AA,H1AB,H1AC)
6.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C34(H34), C36(H36), C40(H40), C42(H42), C44(H44), C48(H48),
 C50(H50), C52(H52), C56(H56), C58(H58), C60(H60), C64(H64), C66(H66), C68(H68),
  C72(H72), C74(H74), C76(H76), C80(H80), C82(H82), C84(H84), C88(H88),
 C90(H90), C92(H92)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10D,H10E,H10F),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C)
;
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.188
_shelx_hkl_checksum              64685
_shelx_res_checksum              16478
_shelxl_version_number           2012-9