Threading-Followed-by-Shrinking Protocol for the Synthesis of a [2]Rotaxane Incorporating a Pd(II)-Salophen Moiety
Il Yoon; Mamiko Narita; Toshimi Shimizu; Masumi Asakawa; Journal of the American Chemical Society 126 (2004) 16740–16741; doi:10.1021/ja0464490

data_4113354
_publ_section_title
;
 Threading-Followed-by-Shrinking Protocol for the Synthesis of a
 [2]Rotaxane Incorporating a Pd(II)-Salophen Moiety
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16740
_journal_page_last               16741
_journal_paper_doi               10.1021/ja0464490
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C56 H64 Cl N3 O12 Pd'
_chemical_formula_weight         1112.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                104.2930(10)
_cell_angle_beta                 96.2350(10)
_cell_angle_gamma                102.1140(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5559(7)
_cell_length_b                   14.3901(9)
_cell_length_c                   15.6599(9)
_cell_measurement_reflns_used    20658
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      1.51
_cell_volume                     2642.1(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20658
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9124
_exptl_absorpt_correction_T_min  0.8536
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         13141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.9553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                11670
_reflns_number_total             13141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0464490si20040616_035401.cif
_cod_data_source_block           sadf
_cod_database_code               4113354