[(Pd-Pd)@Ge18]4-: A Palladium Dimer Inside the Largest Single-Cage Deltahedron
Jose M. Goicoechea; Slavi C. Sevov; Journal of the American Chemical Society 127 (2005) 7676–7677; doi:10.1021/ja051224q

data_4111729
_publ_section_title
;
 [(Pd-Pd)@Ge18]4-: A Palladium Dimer Inside the Largest Single-Cage
 Deltahedron
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7676
_journal_page_last               7677
_journal_paper_doi               10.1021/ja051224q
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         '4(C18 H36 K N2 O6), Ge18 Pd2, 2(C7 H8)'
_chemical_formula_sum            'C86 H160 Ge18 K4 N8 O24 Pd2'
_chemical_formula_weight         3366.04
_chemical_name_systematic
;
 (K-crypt)4(Pd2@Ge18)*2tol
;
_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                 115.333(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.324(3)
_cell_length_b                   27.519(5)
_cell_length_c                   15.849(3)
_cell_measurement_temperature    100(2)
_cell_volume                     6041(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    'Bruker SHELXTL-V5.1'
_computing_publication_material  'Bruker SHELXTL-V5.1'
_computing_structure_refinement  'Bruker SHELXTL-V5.1'
_computing_structure_solution    'Bruker SHELXTL-V5.1'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37883
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    4.893
_exptl_absorpt_correction_T_max  0.7920
_exptl_absorpt_correction_T_min  0.4124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R.H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       brick
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         11465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+8.2790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                8323
_reflns_number_total             11465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051224qsi20050413_120411.cif
_cod_data_source_block           p21nsadabs
_cod_original_cell_volume        6041.0(18)
_cod_database_code               4111729