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_4116573
_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            'C125.5 H78 Au2 Cl2 F18 N6 Na O2 P9'
_chemical_formula_weight         2810.49
_chemical_name_common            2
_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                 101.394(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4038(18)
_cell_length_b                   24.336(3)
_cell_length_c                   27.089(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      1.5
_cell_volume                     11893(2)
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            88725
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             5556
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.00021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1562
_refine_ls_number_reflns         27280
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.209
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+14.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                18645
_reflns_number_total             27280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991982e_2.cif
_cod_data_source_block           bc280
_cod_original_formula_sum        'C125.50 H78 Au2 Cl2 F18 N6 Na O2 P9'
_cod_database_code               4116573