Planar-Chiral Metal Complexes Comprised of Square-Planar Metal and Achiral Tetradentate Ligands: Design, Optical Resolution, and Thermodynamics
Hidetoshi Goto; Teppei Hayakawa; Kanako Furutachi; Hiroshi Sugimoto; Shohei Inoue; Inorganic Chemistry 51 (2012) 4134–4142; doi:10.1021/ic2024742

data_4328783
_publ_section_title
;
 Planar-Chiral Metal Complexes Comprised of Square-Planar Metal and
 Achiral Tetradentate Ligands: Design, Optical Resolution, and
 Thermodynamics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4134
_journal_page_last               4142
_journal_paper_doi               10.1021/ic2024742
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C36 H28 N4 O4 Pd'
_chemical_formula_sum            'C36 H28 N4 O4 Pd'
_chemical_formula_weight         687.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 115.5300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5464(6)
_cell_length_b                   11.3534(4)
_cell_length_c                   17.6697(7)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.23
_cell_volume                     2995.29(19)
_computing_cell_refinement       'SMART (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT (Bruker AXS, 2003)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX 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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20554
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_correction_T_min  0.7313
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.805
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+2.6675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                6099
_reflns_number_total             6868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2024742_si_002_1.cif
_cod_data_source_block           PdL4
_cod_database_code               4328783