Synthesis, Optical Resolution, and Stereochemical Properties of a Rationally Designed Chiral C–N Palladacycle
See Leng Yap, Jeanette; Chen, Houguang Jeremy; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Organometallics 33 (2014) 930–; doi:10.1021/om401044z

data_4082409
_publ_section_title
;
 Synthesis, Optical Resolution, and Stereochemical Properties of a
 Rationally Designed Chiral C--N Palladacycle
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              930
_journal_paper_doi               10.1021/om401044z
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C23.4 H40 N2 O2.6 Pd'
_chemical_formula_weight         497.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 110.553(4)
_cell_angle_gamma                90
_cell_formula_units_Z            10
_cell_length_a                   15.002(2)
_cell_length_b                   32.905(4)
_cell_length_c                   15.089(2)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      23.2739
_cell_measurement_theta_min      2.3507
_cell_volume                     6974.4(16)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'Bruker Apex2'
_computing_publication_material  'Bruker Apex2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            120576
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.963
_refine_diff_density_min         -1.366
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1458
_refine_ls_number_reflns         33642
_refine_ls_number_restraints     598
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1798
_reflns_number_gt                24330
_reflns_number_total             33642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401044z_si_001.cif
_cod_data_source_block           I
_cod_original_cell_volume        6974.4(17)
_cod_original_formula_sum        'C23.40 H40 N2 O2.60 Pd'
_cod_database_code               4082409