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_1553491
_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         'C61 H45 Cl3 N4 O4 Pd2'
_chemical_formula_sum            'C61 H45 Cl3 N4 O4 Pd2'
_chemical_formula_weight         1217.21
_chemical_name_common            2PdNAmX-1
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 113.6497(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   27.6181(17)
_cell_length_b                   13.0551(9)
_cell_length_c                   30.802(2)
_cell_measurement_reflns_used    60385
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     10173.2(12)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0632
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            89431
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4912.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.800
_refine_diff_density_min         -3.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11605
_refine_ls_number_restraints     60
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0409P)^2^+195.4855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                9780
_reflns_number_total             11605
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6qo00315j2.cif
_cod_data_source_block           2PdNAmX-1
_cod_database_code               1553491
_solvent_exptl_crystal_recrystallization_method CHCl3