Self-assembly of pseudo-rotaxane and rotaxane complexes using an electrostatic slippage approach.
Catalán, Aldo C; Tiburcio, Jorge; Chemical communications (Cambridge, England) 52 (2016) 9526–9529; doi:10.1039/c6cc04619c

data_7124782
_publ_section_title
;
 Self-assembly of pseudo-rotaxane and rotaxane complexes using an
 electrostatic slippage approach.
;
_journal_issue                   61
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9526
_journal_page_last               9529
_journal_paper_doi               10.1039/c6cc04619c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C21 H28 N2 O2, 2 (B F4)'
_chemical_formula_sum            'C21 H28 B2 F8 N2 O2'
_chemical_formula_weight         514.07
_chemical_name_common            'Piperidine axle'
_chemical_properties_physical    Heat-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-22 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                70.566(2)
_cell_angle_beta                 78.711(2)
_cell_angle_gamma                88.033(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8103(2)
_cell_length_b                   12.0335(4)
_cell_length_c                   15.7289(5)
_cell_measurement_reflns_used    33312
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1191.39(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26209
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  1.0622
_exptl_absorpt_correction_T_min  0.9210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0861P)^2^+0.5626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                4096
_reflns_number_total             5394
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6cc04619c2.cif
_cod_data_source_block           jtk155
_cod_database_code               7124782
_solvent_exptl_crystal_recrystallization_method nitromethane