Encapsulation of 4,4′-bipyridinium cations by two crown ether molecules: formation and structure of [3]pseudorotaxanes
Nikitin, Kirill; Müller-Bunz, Helge; New Journal of Chemistry 33 (2009) 2472–; doi:10.1039/b9nj00414a

data_7051756
_publ_section_title
;
 Encapsulation of 4,4&#x2032;-bipyridinium cations by two crown ether
 molecules: formation and structure of [3]pseudorotaxanes
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2472
_journal_paper_doi               10.1039/b9nj00414a
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety
'C16 H18 N2, 2 (C24 H32 O8), 2 (F6 P), 2 (C3 H6 O), 0.25(C2 H3 N), 0.25(H2 O)'
_chemical_formula_sum            'C70.5 H95.25 F12 N2.25 O18.25 P2'
_chemical_formula_weight         1556.18
_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                 97.301(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1988(10)
_cell_length_b                   32.459(2)
_cell_length_c                   16.0338(11)
_cell_measurement_reflns_used    7659
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      2.37
_cell_volume                     7329.7(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22023
_diffrn_reflns_theta_full        22.07
_diffrn_reflns_theta_max         22.07
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.9686
_exptl_absorpt_correction_T_min  0.7647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) for selected reflections was 0.043 before and 0.030 after
correction. The Ratio of minimum to maximum transmission is 0.789538.
The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0322P)^2^+35.7526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                4113
_reflns_number_total             4530
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b9nj00414a.txt
_cod_data_source_block           mjm263
_cod_depositor_comments
;

2018-09-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         6224.72
_cod_original_formula_moiety
'4 (C16 H18 N2), 8 (C24 H32 O8), 8 (F6 P), 8 (C3 H6 O), C2 H3 N, H2 O'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        7329.6(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C282 H381 N9 O73 F48 P8'
_cod_database_code               7051756