Helicity Inversion from Left- to Right-Handed Square Planar Pd(II) Complexes: Synthesis of a Diastereomer Pair from a Single Chiral Ligand and their Structure Dynamism
Hiroyuki Miyake; Masashi Ueda; Saori Murota; Hideki Sugimoto; Hiroshi Tsukube; Chem.Commun. 48 (2012) 3721–; doi:10.1039/c2cc18154a

data_7107532
_publ_section_title
;
 Helicity Inversion from Left- to Right-Handed Square Planar Pd(II)
 Complexes: Synthesis of a Diastereomer Pair from a Single Chiral Ligand
 and their Structure Dynamism
;
_journal_name_full               Chem.Commun.
_journal_page_first              3721
_journal_paper_doi               10.1039/c2cc18154a
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C12 H26 Cl2 N4 O2 Pd'
_chemical_formula_sum            'C12 H26 Cl2 N4 O2 Pd'
_chemical_formula_weight         435.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   10.2009(10)
_cell_length_b                   12.1922(15)
_cell_length_c                   13.7244(16)
_cell_measurement_reflns_used    8818
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.1673
_cell_volume                     1706.9(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17076
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.8164
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.6678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                3827
_reflns_number_total             3883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc18154a.txt
_cod_data_source_block           '[Pd(H2L)Cl2]'
_cod_original_sg_symbol_H-M      'P 212121'
_cod_database_code               7107532