[2]Rotaxanes containing pyridinium?phosphonium axles and 24-crown-8 ether wheels
Georges, Norma; Loeb, Stephen J.; Tiburcio, Jorge; Wisner, James A.; Organic & Biomolecular Chemistry 2 (2004) 2751–2756; doi:10.1039/b407653b

data_7153526
_publ_section_title
;
 [2]Rotaxanes containing pyridinium?phosphonium axles and 24-crown-8 ether
 wheels
;
_journal_issue                   19
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2751
_journal_page_last               2756
_journal_paper_doi               10.1039/b407653b
_journal_volume                  2
_journal_year                    2004
_chemical_formula_moiety
;
{[Et3PCH2CH2(4,4'-dipy)CH2(PhtBu))(24-crown-8)][BF4]3}
;
_chemical_formula_sum            'C45 H74.5 B3 F12 N2 O8.25 P'
_chemical_formula_weight         1066.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                90.638(7)
_cell_angle_beta                 102.614(7)
_cell_angle_gamma                105.370(8)
_cell_formula_units_Z            8
_cell_length_a                   16.912(6)
_cell_length_b                   21.522(8)
_cell_length_c                   31.460(12)
_cell_measurement_temperature    293(2)
_cell_volume                     10746(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0796
_diffrn_reflns_av_sigmaI/netI    0.2217
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            47619
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4500
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2566
_refine_ls_number_reflns         30431
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.2402
_refine_ls_R_factor_gt           0.1061
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2777
_refine_ls_wR_factor_ref         0.3365
_reflns_number_gt                10701
_reflns_number_total             30431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b407653bsup1.cif
_cod_data_source_block
{[Et3PCH2CH2(4,4'-dipy)CH2(PhtBu))(24-crown-8)][BF4]3}
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7153526