Synthesis and structural characterization of isomeric palladium(II) complexes with chiral N,O-bidentate ligands
Takashi Tsuno; Haruka Iwabe; Henri Brunner; Inorganica Chimica Acta 400 (2013) 262–266; doi:

data_1516961
_publ_section_title
;
 Synthesis and structural characterization of isomeric palladium(II)
 complexes with chiral N,O-bidentate ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              262
_journal_page_last               266
_journal_volume                  400
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H32 N2 O2 Pd'
_chemical_formula_sum            'C38 H32 N2 O2 Pd'
_chemical_formula_weight         655.06
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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
_cell_angle_alpha                88.127(16)
_cell_angle_beta                 84.123(18)
_cell_angle_gamma                79.058(19)
_cell_formula_units_Z            2
_cell_length_a                   6.683(4)
_cell_length_b                   15.639(7)
_cell_length_c                   15.685(7)
_cell_measurement_reflns_used    11393
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.14
_cell_measurement_wavelength     0.71073
_cell_volume                     1600.9(14)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF08 (Beurskens et al, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku RAPID-RAXIS'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.1075
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12141
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4203
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.507
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         9023
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+6.3637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                6854
_reflns_number_total             9023
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-400-262-266-2.cif
_cod_data_source_block           pdnap
_cod_database_code               1516961