Synthesis, Structure, and Catalytic Performance of Diastereopure Five-Coordinated NCN-Pincer Palladium(II) Complexes Bearing Bulky Amino Acid Substituents
Gosiewska, Silvia; Martinez Herreras, Sara; Lutz, Martin; Spek, Anthony L.; Havenith, Remco W. A.; van Klink, Gerard P. M.; van Koten, Gerard; Gebbink, Robertus J. M. Klein; Organometallics 27 (2008) 2549–; doi:10.1021/om701261q

data_4071102
_publ_section_title
;
 Synthesis, Structure, and Catalytic Performance of Diastereopure
 Five-Coordinated NCN-Pincer Palladium(II) Complexes Bearing Bulky Amino
 Acid Substituents
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2549
_journal_paper_doi               10.1021/om701261q
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H43 Br N2 O2'
_chemical_formula_sum            'C42 H43 Br N2 O2'
_chemical_formula_weight         687.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1480(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3438(1)
_cell_length_b                   36.4734(4)
_cell_length_c                   11.8353(1)
_cell_measurement_reflns_used    70714
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      1.02
_cell_volume                     3476.65(6)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL2000, SortAV'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33653
_diffrn_reflns_theta_full        23.52
_diffrn_reflns_theta_max         23.52
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         10274
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                8204
_reflns_number_total             10274
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om701261q-file002.cif
_cod_data_source_block           s3307a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4071102