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_4115095
_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_formula_sum            'C94.25 H48 N8 O25.6 P2'
_chemical_formula_weight         1763.95
_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                 102.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.817(4)
_cell_length_b                   29.334(6)
_cell_length_c                   17.757(4)
_cell_measurement_reflns_used    11540
_cell_measurement_temperature    119(2)
_cell_measurement_theta_max      44.49
_cell_measurement_theta_min      3.38
_cell_volume                     10060(4)
_computing_cell_refinement
;
SMART (Siemens, 1995), SAINT (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      293(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11540
_diffrn_reflns_theta_full        44.49
_diffrn_reflns_theta_max         44.49
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             3617
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      2.035
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.1418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4085
_refine_ls_wR_factor_ref         0.4256
_reflns_number_gt                2976
_reflns_number_total             3523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0204269_2.cif
_cod_data_source_block           pphos
_cod_original_formula_sum        'C94.25 H48 N8 O25.60 P2'
_cod_database_code               4115095