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_4112609
_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            'C112.5 H87 Au Cl11 N6 O0 P6 Pd Tl'
_chemical_formula_weight         2606.39
_chemical_name_common            1.Cl2.4.5CH2Cl2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.3585(14)
_cell_length_b                   26.8697(15)
_cell_length_c                   29.4776(16)
_cell_measurement_temperature    123(2)
_cell_volume                     21669(2)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            121155
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_T_max  0.7076
_exptl_absorpt_correction_T_min  0.3404
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            deep
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_meas      0
_exptl_crystal_description       shard
_exptl_crystal_F_000             10296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.668
_refine_diff_density_min         -2.028
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         22109
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0926P)^2^+99.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1827
_reflns_number_gt                16181
_reflns_number_total             22109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048800nsi20040227_034945_4.cif
_cod_data_source_block           ortabs
_cod_original_formula_sum        'C112.50 H87 Au Cl11 N6 O0 P6 Pd Tl'
_cod_database_code               4112609