Pd2@Sn184-: Fusion of Two Endohedral Stannaspherenes
Zhong-Ming Sun; Hai Xiao; Jun Li; Lai-Sheng Wang; Journal of the American Chemical Society 129 (2007) 9560–9561; doi:10.1021/ja0728674

data_4109747
_publ_section_title
;
 Pd2@Sn184-: Fusion of Two Endohedral Stannaspherenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9560
_journal_page_last               9561
_journal_paper_doi               10.1021/ja0728674
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C78 H168 K4 N14 O24 Pd2 Sn18'
_chemical_formula_weight         4191.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.71(3)
_cell_angle_beta                 98.62(3)
_cell_angle_gamma                100.53(3)
_cell_formula_units_Z            1
_cell_length_a                   14.913(3)
_cell_length_b                   15.930(3)
_cell_length_c                   16.270(3)
_cell_measurement_reflns_used    621
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      39.00
_cell_measurement_theta_min      3.12
_cell_volume                     3307.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Brucker Proteum Diffractometer'
_diffrn_measurement_method       'narrow frame method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10371
_diffrn_reflns_theta_full        39.00
_diffrn_reflns_theta_max         39.00
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    30.225
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            gray
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             1994
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+22.6913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                2803
_reflns_number_total             3605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0728674si20070424_060610.cif
_cod_data_source_block           1
_cod_original_cell_volume        3307.3(12)
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               4109747