Mixed-Metal Metallocryptands. Short Metal-Metal Separations Strengthened by a Dipolar Interaction
Vincent J. Catalano; Mark A. Malwitz; Journal of the American Chemical Society 126 (2004) 6560–6561; doi:10.1021/ja048800n

data_4112607
_publ_section_title
;
 Mixed-Metal Metallocryptands. Short Metal-Metal Separations Strengthened
 by a Dipolar Interaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6560
_journal_page_last               6561
_journal_paper_doi               10.1021/ja048800n
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C112 H84 Au Cl10 F12 N6 P8 Pd Tl'
_chemical_formula_weight         2851.85
_chemical_name_common            1.(PF6)2.2CHCl3.2CH2Cl2
_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                 90.0200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1939(5)
_cell_length_b                   30.6021(8)
_cell_length_c                   20.6077(6)
_cell_measurement_temperature    100(2)
_cell_volume                     10843.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            114960
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    3.434
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          .367
_exptl_crystal_size_mid          .558
_exptl_crystal_size_min          .63
_refine_diff_density_max         6.068
_refine_diff_density_min         -8.220
_refine_diff_density_rms         0.411
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   5.671
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1367
_refine_ls_number_reflns         24901
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      5.672
_refine_ls_R_factor_all          0.1605
_refine_ls_R_factor_gt           0.1572
_refine_ls_shift/su_max          13.397
_refine_ls_shift/su_mean         0.459
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+20.5655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3925
_refine_ls_wR_factor_ref         0.3930
_reflns_number_gt                23600
_reflns_number_total             24901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048800nsi20040227_034945_2.cif
_cod_data_source_block           unr05s
_cod_database_code               4112607