Superbowl Container Molecules
Elizabeth S. Barrett; Jacob L. Irwin; Alison J. Edwards; Michael S. Sherburn; Journal of the American Chemical Society 126 (2004) 16747–16749; doi:10.1021/ja044405l

data_4113323
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       sherburn@rsc.anu.edu.au
_publ_contact_author_fax         '+61 2 6125 8114'
_publ_contact_author_name        'Michael S. Sherburn'
_publ_contact_author_phone       '+61 1 6125 4988'
_publ_section_title
;
 Superbowl Container Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16747
_journal_page_last               16749
_journal_paper_doi               10.1021/ja044405l
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C268 H316 Br4 O52, 4 C2H6O, 5 CHCl3, 3 O'
_chemical_formula_sum            'C281 H345 Br4 Cl15 O59'
_chemical_formula_weight         4688.96
_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 difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'geom difmap'
_audit_creation_date             04-27-07
_audit_creation_method           'maXus + CRYSTALS_ver_12-03-99'
_cell_angle_alpha                81.514(2)
_cell_angle_beta                 80.2321(14)
_cell_angle_gamma                78.3354(9)
_cell_formula_units_Z            2
_cell_length_a                   22.4832(6)
_cell_length_b                   25.2863(7)
_cell_length_c                   31.2864(8)
_cell_measurement_reflns_used    280650
_cell_measurement_temperature    120
_cell_measurement_theta_max      18.848
_cell_measurement_theta_min      2.910
_cell_volume                     17048.4(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
    CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
 CRYSTALS (Watkin et al 2003)  + maXus(Mackay et al., 1999)
;
_computing_structure_refinement
;
 CRYSTALS (Watkin et al 2003) 
PLATON (Spek 1990)
;
_computing_structure_solution
;
    SIR97 (Altomare et al, 1999)
;
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.04227
_diffrn_orient_matrix_UB_12      0.01630
_diffrn_orient_matrix_UB_13      0.00733
_diffrn_orient_matrix_UB_21      -0.00884
_diffrn_orient_matrix_UB_22      -0.01449
_diffrn_orient_matrix_UB_23      0.03695
_diffrn_orient_matrix_UB_31      0.00824
_diffrn_orient_matrix_UB_32      -0.02859
_diffrn_orient_matrix_UB_33      -0.01346
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            99800
_diffrn_reflns_theta_full        18.84
_diffrn_reflns_theta_max         18.84
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.70
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    'not known'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7362+
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0264
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         5282
_refine_ls_number_restraints     1046
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.1062
_refine_ls_shift/su_max          0.045
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.512E+04 -0.849E+04 0.439E+04 -0.138E+04 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0764
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0764
_reflns_d_resolution_high        1.15
_reflns_d_resolution_low         1.87
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                5282
_reflns_number_total             26105
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja044405lsi20040915_020926.cif
_cod_data_source_block           MSEB8z
_cod_original_cell_volume        17048.3(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113323