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_4103458
_publ_contact_author_address
;Department of Chemistry
240 Reiss Building
Georgetown University
37th & O st, NW
Washington, DC, 20057
;
_publ_contact_author_email       kth7@georgetown.edu
_publ_contact_author_name        'K. Travis Holman'
_publ_contact_author_phone       '202 687 4027'
_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_sum            'C129 H158 F18 N9 O45 Ru6 S6'
_chemical_formula_weight         3695.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 125.01
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.8474(12)
_cell_length_b                   18.9252(9)
_cell_length_c                   17.7103(16)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.57
_cell_volume                     7095.7(8)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    '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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30623
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.8270
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1990)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3754
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7985
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+43.7172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1717
_reflns_number_gt                6905
_reflns_number_total             7985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1071515_si_003.cif
_cod_data_source_block           09078SQ
_cod_original_cell_volume        7095.5(8)
_cod_database_code               4103458