A Water-Soluble Xe@cryptophane-111 Complex Exhibits Very High Thermodynamic Stability and a Peculiar 129Xe NMR Chemical Shift
Robert M. Fairchild; Akil I. Joseph; K. Travis Holman; Heather A. Fogarty; Thierry Brotin; Jean-Pierre Dutasta; Céline Boutin; Gaspard Huber; Patrick Berthault; Journal of the American Chemical Society 132 (2010) 15505–15507; doi:10.1021/ja1071515

data_4103456
_publ_contact_author_email       kth7@georgetown.edu
_publ_contact_author_name        'K. Travis Holman'
_publ_section_title
;
 A Water-Soluble Xe@cryptophane-111 Complex Exhibits Very High
 Thermodynamic Stability and a Peculiar 129Xe NMR Chemical Shift
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15505
_journal_page_last               15507
_journal_paper_doi               10.1021/ja1071515
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C47 H38 O6, (H1.5 O0.75)'
_chemical_formula_sum            'C47 H39.5 Cl6 O6.75'
_chemical_formula_weight         924.99
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   51.168(5)
_cell_length_b                   10.0144(10)
_cell_length_c                   25.099(3)
_cell_measurement_reflns_used    11475
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.245
_cell_measurement_theta_min      4.549
_cell_volume                     12861(2)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics
'X-SEED, L.Barbour (1999); http://x-seed.net/'
_computing_publication_material
'X-SEED, L.Barbour (1999); http://x-seed.net/'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART, Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            78070
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5730
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         11310
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+9.3366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                8407
_reflns_number_total             11310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1071515_si_001.cif
_cod_data_source_block           g:\frames\guest\10001\work\001b
_cod_original_formula_sum        'C47 H39.50 Cl6 O6.75'
_cod_database_code               4103456