Synthesis and Characterization of Trigonal Gold(I) Cage Complexes: Luminescent Metallocryptates Encapsulating Tl(I) and Na+ Ions
Vincent J. Catalano; Byron L. Bennett; Heidi M. Kar; Bruce C. Noll; Journal of the American Chemical Society 121 (1999) 10235–10236; doi:10.1021/ja991982e

data_4116572
_publ_section_title
;
 Synthesis and Characterization of Trigonal Gold(I) Cage Complexes:
 Luminescent Metallocryptates Encapsulating Tl(I) and Na+ Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10235
_journal_page_last               10236
_journal_paper_doi               10.1021/ja991982e
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C128 H78 Au2 Cl5.5 N6 O12 P6 Tl'
_chemical_formula_weight         2871.06
_chemical_name_common            1
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.0130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1764(7)
_cell_length_b                   24.2486(9)
_cell_length_c                   26.3578(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      1.5
_cell_volume                     11403.3(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens Smart'
_diffrn_measurement_method       '\w scans'
_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  0.1310
_diffrn_reflns_av_sigmaI/netI    0.1548
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            84672
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    4.256
_exptl_absorpt_correction_T_max  .71
_exptl_absorpt_correction_T_min  .54
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             5626
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.838
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1473
_refine_ls_number_reflns         26165
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                13948
_reflns_number_total             26165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991982e_1.cif
_cod_data_source_block           bc283
_cod_original_formula_sum        'C128 H78 Au2 Cl5.50 N6 O12 P6 Tl'
_cod_database_code               4116572