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_1515244
_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            'C89.5 H107.5 B2 Cl1.5 F8 N5 O12'
_chemical_formula_weight         1672.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.934(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.517(3)
_cell_length_b                   39.753(5)
_cell_length_c                   11.1884(15)
_cell_measurement_reflns_used    452
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.91
_cell_measurement_theta_min      1.97
_cell_volume                     9500(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1358
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            48976
_diffrn_reflns_theta_full        20.91
_diffrn_reflns_theta_max         20.91
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9628
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3532
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         9999
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.2158
_refine_ls_R_factor_gt           0.1563
_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^)+(0.0378P)^2^+107.4031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2932
_refine_ls_wR_factor_ref         0.3319
_reflns_number_gt                6600
_reflns_number_total             9999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20986a.txt
_cod_data_source_block           kz90z
_cod_original_cell_volume        9501(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C89.50 H107.50 B2 Cl1.50 F8 N5 O12'
_cod_database_code               1515244