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_4116574
_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            'C88 H52 Au2 Cl3 F12 N4 O P6'
_chemical_formula_weight         2095.44
_chemical_name_common            AuMacrocycle
_chemical_name_systematic
; 
 ? 
;
_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                 129.357(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.030(5)
_cell_length_b                   15.798(3)
_cell_length_c                   23.331(6)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      4.76
_cell_volume                     9413(4)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.1205
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7062
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.75
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.368
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.5139
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       Block
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .78
_exptl_crystal_size_min          .45
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.00002(4)
_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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                3410
_reflns_number_total             6134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991982e_3.cif
_cod_data_source_block           vjc330
_cod_depositor_comments
;

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1047.72
_cod_original_formula_units_Z            8
_cod_original_cell_volume        9413(3)
_cod_original_formula_sum        'C44 H26 Au Cl1.50 F6 N2 Na0 O0.50 P3'
_cod_database_code               4116574