Homochiral association of binuclear trans-bis(β-iminoaryloxy)palladium(ii) complexes doubly linked with m-xylylene spacers: drastic linker-dependence of the association chirality of chiral clothespin-shaped molecules
Naito, Masaya; Komiya, Naruyoshi; Naota, Takeshi; Organic Chemistry Frontiers 3 (2016) 1286–; doi:10.1039/C6QO00315J

data_1553490
_publ_section_title
;
 Homochiral association of binuclear
 trans-bis(\b-iminoaryloxy)palladium(ii) complexes doubly linked with
 m-xylylene spacers: drastic linker-dependence of the association
 chirality of chiral clothespin-shaped molecules
;
_journal_issue                   10
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1286
_journal_paper_doi               10.1039/C6QO00315J
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C60 H44 N4 O4 Pd2'
_chemical_formula_sum            'C60 H44 N4 O4 Pd2'
_chemical_formula_weight         1097.83
_chemical_name_common            2PdNAmX-2
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-04-30 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            12
_cell_length_a                   20.2007(6)
_cell_length_b                   25.2676(7)
_cell_length_c                   31.3498(8)
_cell_measurement_reflns_used    112720
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      3.06
_cell_volume                     16001.7(8)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1796
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            270470
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             6672.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.870
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     946
_refine_ls_number_reflns         18213
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1066P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1993
_reflns_number_gt                11469
_reflns_number_total             18213
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6qo00315j2.cif
_cod_data_source_block           2PdNAmX-2
_cod_database_code               1553490
_solvent_exptl_crystal_recrystallization_method CHCl3