Octapi Interactions: Self-Assembly of a Pd-Based [2]Catenane Driven by Eightfold π Interactions
Jinzhen Lu; David R. Turner; Lindsay P. Harding; Lindsay T. Byrne; Murray V. Baker; Stuart R. Batten; Journal of the American Chemical Society 131 (2009) 10372–10373; doi:10.1021/ja9041912

data_4104786
_publ_section_title
;
 Octapi Interactions: Self-Assembly of a Pd-Based [2]Catenane Driven by
 Eightfold \p Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10372
_journal_page_last               10373
_journal_paper_doi               10.1021/ja9041912
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C127.5 H125.5 F12 N12 O12 P4 Pd2 Pt0 S4'
_chemical_formula_weight         2710.82
_chemical_name_common            {[(dppp)Pd(LPr)]2.4OTF}4.5Toluene
_chemical_name_systematic
; 
 {[(dppp)Pd(LPr)]2.4OTF}.4.5Toluene 
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n 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                   28.414(12)
_cell_length_b                   41.636(8)
_cell_length_c                   29.307(7)
_cell_measurement_reflns_used    324685
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      0.92
_cell_volume                     34672(18)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       Blu-Ice
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'ADSC Quantum 210r Detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.77343
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            324685
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_correction_T_min  0.9328
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_description       block
_exptl_crystal_F_000             11156
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.802
_refine_diff_density_min         -2.537
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1273
_refine_ls_number_reflns         23136
_refine_ls_number_restraints     1229
_refine_ls_restrained_S_all      2.343
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.1487
_refine_ls_shift/su_max          1.094
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.2000P)^2^+0.0000sin\q/\l] 
 where P = 0.00000Fo^2^ + 1.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4340
_refine_ls_wR_factor_ref         0.4549
_reflns_number_gt                17907
_reflns_number_total             23136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9041912_si_003.cif
_cod_data_source_block           squeezed
_cod_original_formula_sum        'C127.50 H125.50 F12 N12 O12 P4 Pd2 Pt0 S4'
_cod_database_code               4104786