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_4110155
_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            'C112.5 H136.25 F36 N12 O26 P6 Pd1.5 S0'
_chemical_formula_weight         3102.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   37.8491(10)
_cell_length_b                   37.8491(10)
_cell_length_c                   33.4157(17)
_cell_measurement_reflns_used    18694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.913
_cell_measurement_theta_min      4.643
_cell_volume                     41456(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.2073
_diffrn_reflns_av_sigmaI/netI    0.1798
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            171843
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         0.87
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.9409
_exptl_absorpt_correction_T_min  0.8899
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             19035
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         22653
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1882
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.339
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1455P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2623
_reflns_number_gt                9609
_reflns_number_total             22653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074721asi20070713_011142.cif
_cod_data_source_block           0700008s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Rombohedric' was replaced with
'rhombohedral' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C112.50 H136.25 F36 N12 O26 P6 Pd1.50 S0'
_cod_database_code               4110155