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_4110150
_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            'C51 H50 F12 N7 O8 P2'
_chemical_formula_weight         1178.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 98.144(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7113(12)
_cell_length_b                   14.2665(17)
_cell_length_c                   36.270(4)
_cell_measurement_reflns_used    10332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.056
_cell_measurement_theta_min      4.444
_cell_volume                     5486.6(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1105
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            73032
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.9159
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       prism
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         13686
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.337
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+17.4489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2479
_reflns_number_gt                6349
_reflns_number_total             13686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074721asi20070627_023910.cif
_cod_data_source_block           0615218s
_cod_database_code               4110150