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_7211462
_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(C22 H26), C32 H12 B F24'
_chemical_formula_sum            'C76 H64 B F24'
_chemical_formula_weight         1444.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2013-04-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.821(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.960(4)
_cell_length_b                   32.662(7)
_cell_length_c                   14.213(3)
_cell_measurement_reflns_used    906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.90
_cell_measurement_theta_min      2.37
_cell_volume                     7733(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.797
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1218
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.797
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51989
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.577994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0832 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.5780.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       plate
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         11139
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0997P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5184
_reflns_number_total             11139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41719k.txt
_cod_data_source_block           ros105
_cod_database_code               7211462
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F2A, F3B, F3A, F1B, F1A, F2B, F24B, F23B, F22B, F20A, F19B, F19A, F21B, F21A,
 F20B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13A, F15, F15A, F14, F14A, F13, F24B, F24A, F22B, F22A, F23B, F23A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F2A \\sim F3B \\sim F3A \\sim F1B \\sim F1A \\sim F2B \\sim F24B \\sim F23B \\sim F22B \\sim F20A \\sim F19B \\sim F19A \\sim F21B \\sim F21A \\sim F20B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F13A \\sim F15 \\sim F15A \\sim F14 \\sim F14A \\sim F13 \\sim F24B \\sim F24A \\sim F22B \\sim F22A \\sim F23B \\sim F23A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1*Sof(F13)=1*Sof(F14)=1*Sof(F15)=1-1*Sof(F13A)=1-1*Sof(F14A)=1-1*Sof(F15A)
 1*Sof(F1A)=1*Sof(F2A)=1*Sof(F3A)=1-1*Sof(F1B)=1-1*Sof(F2B)=1-1*Sof(F3B)
 1*Sof(F19A)=1*Sof(F20A)=1*Sof(F21A)=1-1*Sof(F19B)=1-1*Sof(F20B)=1-1*Sof(F21B)
 1-1*Sof(F22A)=1-1*Sof(F23A)=1-1*Sof(F24A)=1*Sof(F22B)=1*Sof(F23B)=1*Sof(F24B)
5.a Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C26(H26), C33(H33), C46(H46), C48(H48), C50(H50), C54(H54),
 C56(H56), C58(H58), C62(H62), C64(H64), C66(H66), C70(H70), C72(H72), C74(H74)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C43(H43A,H43B,H43C)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 1428.4 Ang^3^ [18.5%]
Total electron count / cell = 311.9
;
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.978
_shelx_hkl_checksum              90062
_shelx_res_checksum              57697
_shelxl_version_number           2012-9