Molecular Catenation via Metal-Directed Self-Assembly and π-Donor/π-Acceptor Interactions: Efficient One-Pot Synthesis, Characterization, and Crystal Structures of [3]Catenanes Based on Pd or Pt Dinuclear Metallocycles
Víctor Blanco; Marcos Chas; Dolores Abella; Carlos Peinador; José M. Quintela; Journal of the American Chemical Society 129 (2007) 13978–13986; doi:10.1021/ja074721a

data_4110153
_publ_section_title
;
 Molecular Catenation via Metal-Directed Self-Assembly and
 \p-Donor/\p-Acceptor Interactions: Efficient One-Pot Synthesis,
 Characterization, and Crystal Structures of [3]Catenanes Based on Pd or
 Pt Dinuclear Metallocycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13978
_journal_page_last               13986
_journal_paper_doi               10.1021/ja074721a
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C264 H280 F96 N38 O48 P16 Pt4'
_chemical_formula_weight         7853.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                90.000(5)
_cell_angle_beta                 125.982(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   38.981(5)
_cell_length_b                   21.921(5)
_cell_length_c                   24.767(5)
_cell_measurement_reflns_used    15979
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.148
_cell_measurement_theta_min      4.516
_cell_volume                     17126(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0930
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88110
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  0.7590
_exptl_absorpt_correction_T_min  0.7348
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             7860
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.969
_refine_diff_density_min         -2.124
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.706(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2094
_refine_ls_number_reflns         28369
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.571
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1909
_reflns_number_gt                19703
_reflns_number_total             28369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074721asi20070627_024007.cif
_cod_data_source_block           pvb73fm
_cod_original_cell_volume        17125(6)
_cod_database_code               4110153