Bis(benzimidazolium) axles and crown ether wheels: a versatile templating pair for the formation of [2]rotaxane molecular shuttles
Zhu, Kelong; Vukotic, V. Nicholas; Noujeim, Nadim; Loeb, Stephen J.; Chemical Science 3 (2012) 3265–; doi:10.1039/c2sc20986a

data_1515243
_publ_section_title
;
 Bis(benzimidazolium) axles and crown ether wheels: a versatile templating
 pair for the formation of [2]rotaxane molecular shuttles
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3265
_journal_paper_doi               10.1039/c2sc20986a
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C76.5 H96.5 B2 Cl1.5 F8 N4 O8'
_chemical_formula_weight         1426.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.751(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.833(2)
_cell_length_b                   29.043(4)
_cell_length_c                   38.755(6)
_cell_measurement_reflns_used    681
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.06
_cell_volume                     15428(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1179
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            70770
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.9669
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6040
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Both BF4- anoins were treated as rigid groups using DFIX, SADI, DELU and SIMU
restraints. One of the BF4- anions was disordered over two sites and refined
with sofs of 1/3 nd 2/3.
Residual electron density in the lattice appeared to be CHCL3 but could not
be modeled satisfactorily. The unit cell was calculated to contain an
estimated 4 molecules of CHCL3 which were treated as a diffuse contribution
to the overall scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.399
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         13565
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.2103
_refine_ls_R_factor_gt           0.1356
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1939P)^2^+35.8923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3416
_refine_ls_wR_factor_ref         0.3923
_reflns_number_gt                7009
_reflns_number_total             13565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20986a.txt
_cod_data_source_block           kz92
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C76.50 H96.50 B2 Cl1.50 F8 N4 O8'
_cod_database_code               1515243