Metal-Switching and Self-Inclusion of Functional Cavitands
Patrick Amrhein; Alexander Shivanyuk; Darren W. Johnson; Julius Rebek; Journal of the American Chemical Society 124 (2002) 10349–10358; doi:10.1021/ja0204269

data_4115094
_publ_contact_author
;
Julius Rebek, Jr.
Skaggs Institute for Chemical Biology (MB26)
The Scripps Research Institute
10550 N. Torrey Pines Road
La Jolla, CA  92037
;
_publ_contact_author_email       jrebek@scripps.edu
_publ_contact_author_fax         858-784-2876
_publ_contact_author_phone       858-784-2250
_publ_section_title
;
 Metal-Switching and Self-Inclusion of Functional Cavitands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10349
_journal_page_last               10358
_journal_paper_doi               10.1021/ja0204269
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        synthetic
_chemical_formula_sum            'C94 H62 Br8 N8 O16'
_chemical_formula_weight         2198.80
_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                87.653(2)
_cell_angle_beta                 71.100(2)
_cell_angle_gamma                83.745(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7937(6)
_cell_length_b                   17.8890(7)
_cell_length_c                   18.2308(8)
_cell_measurement_reflns_used    17486
_cell_measurement_temperature    117(2)
_cell_measurement_theta_max      49.23
_cell_measurement_theta_min      2.48
_cell_volume                     4537.3(3)
_computing_cell_refinement
;
SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SHELXL-97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      117(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  '3 circle diffractometer'
_diffrn_measurement_method
;
omega scans with profile analysis
;
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17483
_diffrn_reflns_theta_full        49.35
_diffrn_reflns_theta_max         49.35
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    4.811
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.622
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.1012
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1762P)^2^+69.1860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2716
_refine_ls_wR_factor_ref         0.2815
_reflns_number_gt                6649
_reflns_number_total             8122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0204269_1.cif
_cod_data_source_block           patbrs
_cod_database_code               4115094