A Cryptand/Bisparaquat [3]Pseudorotaxane by Cooperative Complexation
Feihe Huang; Frank R. Fronczek; Harry W. Gibson; Journal of the American Chemical Society 125 (2003) 9272–9273; doi:10.1021/ja0355877

data_4114035
_publ_contact_author_address
;
 Department of Chemistry
 Virginia Polytechnic Institute and State University
 Blacksburg, VA, USA, 24061
;
_publ_contact_author_email       hwgibson@vt.edu
_publ_contact_author_fax         540-231-8517
_publ_contact_author_name        'Harry W. Gibson'
_publ_contact_author_phone       540-231-5902
_publ_section_title
;
 A Cryptand/Bisparaquat [3]Pseudorotaxane by Cooperative Complexation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9272
_journal_page_last               9273
_journal_paper_doi               10.1021/ja0355877
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C114 H140 F24 N4 O38 P4 '
_chemical_formula_sum            'C114 H140 F24 N4 O38 P4'
_chemical_formula_weight         2754.22
_chemical_name_systematic
;                                                                               
?                                                                               
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_date             03-23-02
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                80.08(1)
_cell_angle_beta                 75.44(1)
_cell_angle_gamma                73.94(2)
_cell_formula_units_Z            1
_cell_length_a                   10.974(3)
_cell_length_b                   17.451(4)
_cell_length_c                   19.735(6)
_cell_measurement_reflns_used    12145
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.55
_cell_volume                     3493.8(17)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_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  0.03
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54676
_diffrn_reflns_theta_full        24.000
_diffrn_reflns_theta_max         25.532
_diffrn_reflns_theta_min         2.558
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             1432.0
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.77
_refine_ls_extinction_coef       11.7(708)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0585
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         5089
_refine_ls_R_factor_all          0.1832
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000156
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 2.46 2.32 1.80 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1269
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0779
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              21
_reflns_limit_k_min              -20
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5089
_reflns_number_total             12707
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ja0355877.cif
_cod_data_source_block           hfh60/hfh83
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C114 H140 F24 N4 O38 P4 '
_cod_database_code               4114035